# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_jj003_br_eu_otf_h2o_acet_red3
_database_code_depnum_ccdc_archive 'CCDC 1833428'
loop_
_audit_author_name
_audit_author_address
'Antti Tiihonen'
;University of Jyv?skyl?, Department of Chemistry
Finland
;
_audit_update_record             
;
2018-03-29 deposited with the CCDC.	2019-02-28 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_CHEMW03_I                   
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: The structure contains voids of unresolved electron density
which was treated using Olex2 solvent mask procedure (full details in 
_smtbx_masks_special_details). The 11 water molecules per asymmetric unit 
 are included in the formula and used in the calculations. 
;
_vrf_PLAT973_I                   
;
PROBLEM: Check Calcd Positive Resid. Density on       Eu1  
RESPONSE: Peak is located about 1 Angstrom from the metal atom and is caused by
the absorption effects. Data recorded with Cu-radiation. 
;
_vrf_PLAT420_I                   
;
PROBLEM: D-H Without Acceptor       O2W      --H2WA
RESPONSE: Hydrogen bond acceptor (water) have been removed among the other 
disordered solvent
 also water) from the voids (see vrf_CHEMW03_I).
;
_vrf_FORMU01_I                   
;
PROBLEM: There is a discrepancy between the atom counts in the
            _chemical_formula_sum and _chemical_formula_moiety.
RESPONSE: See explanation above (CHEMW03_ALERT2_A).
;
_vrf_CELLZ01_I                   
;
PROBLEM: Difference between formula and atom_site contents detected.
RESPONSE: See explanation above (CHEMW03_ALERT2_A).
;
_vrf_PLAT041_I                   
;
PROBLEM: Calculated and Reported SumFormula strings Differ ...    
RESPONSE: See explanation above (CHEMW03_ALERT2_A).
;
_vrf_PLAT042_I                   
;
PROBLEM: Calculated and Reported Moiety formula strings Differ by ...
RESPONSE: See explanation above (CHEMW03_ALERT2_A).
;
_vrf_PLAT068_I                   
;
PROBLEM: Reported F000 Differs from Calcd (or Missing)...
RESPONSE: See explanation above (CHEMW03_ALERT2_A).
;
_vrf_PLAT606_I                   
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure
RESPONSE: See explanation above (CHEMW03_ALERT2_A).
;
# end Validation Reply Form
_audit_creation_date             2018-03-26
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H31 Eu N3 O8, 2.13(Br), 0.87(C F3 O3 S)'
_chemical_formula_sum            'C30.88 H53 Br2.12 Eu F2.62 N3 O21.62 S0.88'
_chemical_formula_weight         1211.78
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C21 H25 O12 N3 F12 S3 Br1 Eu1'
_chemical_oxdiff_usercomment     'clear colorless block'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Eu Eu -8.9294 11.1857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.5897(3)
_cell_length_b                   14.3802(7)
_cell_length_c                   18.8257(8)
_cell_angle_alpha                107.624(4)
_cell_angle_beta                 103.176(3)
_cell_angle_gamma                99.794(3)
_cell_volume                     2327.76(18)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8356
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      76.7660
_cell_measurement_theta_min      3.3160
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    12.942
_exptl_absorpt_correction_T_max  0.495
_exptl_absorpt_correction_T_min  0.079
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.729
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1214
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 9 -7 0.0235
0 -4 -8 0.0358
0 4 8 0.0358
6 -2 -2 0.1193
-6 2 2 0.1193
-1 -9 7 0.0235

_exptl_crystal_size_max          0.245
_exptl_crystal_size_mid          0.086
_exptl_crystal_size_min          0.047
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.9999 9.0000 -6.9994 0.9893 0.2081 -0.2421
-0.0001 -3.9998 -8.0001 0.0285 -0.2536 0.9526
0.0001 3.9998 8.0001 -0.0285 0.2536 -0.9526
5.9999 -1.9994 -1.9997 -0.0436 0.9362 0.2346
-5.9999 1.9994 1.9997 0.0436 -0.9362 -0.2346
-0.9999 -9.0000 6.9994 -0.9893 -0.2081 0.2421

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_unetI/netI     0.0455
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            14473
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.998
_diffrn_reflns_theta_min         2.580
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3953
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     13.00 116.00   1.00    1.50    --   41.90  77.00   0.00  103
  2  ω     79.00 175.00   1.00    3.00    --  112.00  77.00 120.00   96
  3  ω    129.00 178.00   1.00    3.00    --  112.00 111.00 150.00   49
  4  ω     57.00 151.00   1.00    3.00    --  112.00 178.00  30.00   94
  5  ω    114.00 176.00   1.00    3.00    --  112.00  61.00-120.00   62
  6  ω    104.00 167.00   1.00    3.00    --  112.00  61.00-150.00   63
  7  ω     87.00 178.00   1.00    3.00    --  112.00  45.00-180.00   91
  8  ω     73.00 116.00   1.00    3.00    --  112.00-111.00-150.00   43
  9  ω     40.00 116.00   1.00    3.00    --  112.00-111.00   0.00   76
 10  ω     48.00 133.00   1.00    3.00    --  112.00 -45.00 150.00   85
 11  ω     36.00 137.00   1.00    3.00    --  112.00 -77.00  60.00  101
 12  ω    -70.00  31.00   1.00    1.50    --  -41.90  57.00 150.00  101
 13  ω    -74.00  31.00   1.00    1.50    --  -41.90  77.00 -90.00  105
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0043345000
_diffrn_orient_matrix_UB_12      0.0768020000
_diffrn_orient_matrix_UB_13      -0.0419653000
_diffrn_orient_matrix_UB_21      0.1700673000
_diffrn_orient_matrix_UB_22      0.0207961000
_diffrn_orient_matrix_UB_23      0.0213057000
_diffrn_orient_matrix_UB_31      -0.0147197000
_diffrn_orient_matrix_UB_32      -0.0848691000
_diffrn_orient_matrix_UB_33      -0.0766391000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8001
_reflns_number_total             8435
_reflns_odcompleteness_completeness 99.37
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         2.214
_refine_diff_density_min         -1.972
_refine_diff_density_rms         0.149
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     484
_refine_ls_number_reflns         8435
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0528
_refine_ls_restrained_S_all      1.078
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0937P)²+6.0740P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1478
_refine_ls_wR_factor_ref         0.1505
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Others
 Sof(Br3B)=1-FVAR(1)
 Sof(S1A)=Sof(F8A)=Sof(F6A)=Sof(O4A)=Sof(O3A)=Sof(F7A)=Sof(O2A)=Sof(C5A)=FVAR(1)
3.a Rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
3.b Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C10(H10A,H10B), C30(H30A,H30B)
3.c Aromatic/amide H refined with riding coordinates:
 C36(H36), C23(H23), C33(H33), C35(H35), C32(H32), C25(H25), C26(H26),
 C13(H13), C15(H15), C12(H12), C16(H16), C22(H22)
3.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Eu1 Eu 1.22776(3) 0.01237(2) 0.99442(2) 0.01501(11) Uani 1 1 d . . . . .
Br2 Br 1.21123(9) 0.58544(7) 0.70629(5) 0.0475(2) Uani 1 1 d . . . . .
Br1 Br 1.26852(9) 0.08124(7) 0.68771(5) 0.0474(2) Uani 1 1 d . . . . .
S1A S 0.2991(3) 0.25934(19) 0.39957(13) 0.0223(5) Uani 0.874(5) 1 d . . P A 1
O19 O 0.9095(4) 0.0308(3) 0.9253(2) 0.0229(8) Uani 1 1 d . . . . .
O38 O 0.6300(4) 0.0423(3) 0.0882(2) 0.0244(8) Uani 1 1 d . . . . .
O28 O 0.8387(4) 0.8420(3) 0.9385(2) 0.0233(8) Uani 1 1 d . . . . .
O18 O 1.1081(4) 0.0584(3) 0.8862(2) 0.0232(8) Uani 1 1 d . . . . .
O29 O 1.0466(4) 0.8592(3) 0.9024(2) 0.0219(8) Uani 1 1 d . . . . .
O39 O 0.4272(4) 0.0801(3) 0.1142(2) 0.0255(9) Uani 1 1 d . . . . .
F8A F 0.4031(6) 0.1120(3) 0.4270(3) 0.0437(12) Uani 0.874(5) 1 d . . P A 1
F6A F 0.1703(5) 0.0921(4) 0.4143(3) 0.0477(13) Uani 0.874(5) 1 d . . P A 1
O4A O 0.4462(6) 0.3225(4) 0.4319(3) 0.0324(12) Uani 0.874(5) 1 d . . P A 1
O3A O 0.1896(5) 0.3057(4) 0.4269(3) 0.0320(12) Uani 0.874(5) 1 d . . P A 1
F7A F 0.3331(6) 0.1970(4) 0.5203(3) 0.0459(12) Uani 0.874(5) 1 d . . P A 1
N31 N 0.7985(5) 0.2106(4) 0.3759(2) 0.0204(9) Uani 1 1 d . . . . .
O2A O 0.2510(7) 0.1992(5) 0.3172(3) 0.0432(14) Uani 0.874(5) 1 d . . P A 1
C20 C 0.6142(6) 0.4692(4) 0.6159(3) 0.0245(12) Uani 1 1 d . . . . .
H20A H 0.512651 0.443960 0.617517 0.029 Uiso 1 1 calc R . . . .
H20B H 0.605444 0.495524 0.572701 0.029 Uiso 1 1 calc R . . . .
C24 C 0.8411(6) 0.7221(4) 0.8227(3) 0.0201(10) Uani 1 1 d . . . . .
C36 C 0.6546(6) 0.2076(5) 0.3522(3) 0.0241(11) Uani 1 1 d . . . . .
H36 H 0.607162 0.235878 0.389540 0.029 Uiso 1 1 calc R . . . .
N21 N 0.6978(5) 0.5555(3) 0.6919(2) 0.0207(9) Uani 1 1 d . . . . .
C34 C 0.6457(6) 0.1255(4) 0.2198(3) 0.0181(10) Uani 1 1 d . . . . .
C23 C 0.6860(6) 0.6878(4) 0.7985(3) 0.0240(11) Uani 1 1 d . . . . .
H23 H 0.629547 0.721930 0.827921 0.029 Uiso 1 1 calc R . . . .
C37 C 0.5608(6) 0.0784(4) 0.1331(3) 0.0174(10) Uani 1 1 d . . . . .
C5 C 0.8007(6) 0.2760(5) 0.5171(3) 0.0235(11) Uani 1 1 d . . . . .
C3 C 0.6834(6) 0.3816(4) 0.5980(3) 0.0197(10) Uani 1 1 d . . . . .
C1 C 0.6838(6) 0.2143(4) 0.5996(3) 0.0219(11) Uani 1 1 d . . . . .
C33 C 0.7941(6) 0.1303(4) 0.2454(3) 0.0237(11) Uani 1 1 d . . . . .
H33 H 0.844172 0.104036 0.208842 0.028 Uiso 1 1 calc R . . . .
C35 C 0.5746(6) 0.1642(4) 0.2744(3) 0.0206(11) Uani 1 1 d . . . . .
H35 H 0.471859 0.160657 0.258244 0.025 Uiso 1 1 calc R . . . .
N11 N 0.7177(6) 0.1167(4) 0.6925(3) 0.0252(10) Uani 1 1 d . . . . .
C32 C 0.8699(6) 0.1729(5) 0.3235(3) 0.0278(12) Uani 1 1 d . . . . .
H32 H 0.972326 0.176121 0.340913 0.033 Uiso 1 1 calc R . . . .
C25 C 0.9201(6) 0.6697(4) 0.7799(3) 0.0232(11) Uani 1 1 d . . . . .
H25 H 1.025188 0.691373 0.795276 0.028 Uiso 1 1 calc R . . . .
C4 C 0.7625(6) 0.3679(4) 0.5433(3) 0.0231(11) Uani 1 1 d . . . . .
C6 C 0.7592(7) 0.1984(4) 0.5434(3) 0.0244(12) Uani 1 1 d . . . . .
C26 C 0.8445(6) 0.5848(4) 0.7140(3) 0.0226(11) Uani 1 1 d . . . . .
H26 H 0.898182 0.547458 0.684625 0.027 Uiso 1 1 calc R . . . .
C10 C 0.6185(7) 0.1273(4) 0.6220(3) 0.0274(12) Uani 1 1 d . . . . .
H10A H 0.524136 0.136421 0.632384 0.033 Uiso 1 1 calc R . . . .
H10B H 0.595098 0.063707 0.576925 0.033 Uiso 1 1 calc R . . . .
C13 C 0.9512(7) 0.1179(5) 0.7682(4) 0.0319(14) Uani 1 1 d . . . . .
H13 H 1.055689 0.132105 0.778209 0.038 Uiso 1 1 calc R . . . .
C14 C 0.8846(6) 0.0775(4) 0.8142(3) 0.0225(11) Uani 1 1 d . . . . .
C27 C 0.9160(6) 0.8163(4) 0.8940(3) 0.0196(10) Uani 1 1 d . . . . .
C15 C 0.7331(7) 0.0594(6) 0.7986(4) 0.0355(15) Uani 1 1 d . . . . .
H15 H 0.685479 0.034046 0.830469 0.043 Uiso 1 1 calc R . . . .
C2 C 0.6483(6) 0.3061(4) 0.6289(3) 0.0221(11) Uani 1 1 d . . . . .
C12 C 0.8643(7) 0.1371(6) 0.7077(4) 0.0333(14) Uani 1 1 d . . . . .
H12 H 0.909832 0.165327 0.676517 0.040 Uiso 1 1 calc R . . . .
C8 C 0.8032(8) 0.4491(5) 0.5109(4) 0.0367(15) Uani 1 1 d . . . . .
H8A H 0.911386 0.472836 0.525553 0.055 Uiso 1 1 calc GR . . . .
H8B H 0.762189 0.505622 0.532257 0.055 Uiso 1 1 calc GR . . . .
H8C H 0.762625 0.421626 0.453889 0.055 Uiso 1 1 calc GR . . . .
C7 C 0.5717(7) 0.3238(5) 0.6917(3) 0.0295(13) Uani 1 1 d . . . . .
H7A H 0.597888 0.396140 0.722373 0.044 Uiso 1 1 calc GR . . . .
H7B H 0.603262 0.287026 0.726047 0.044 Uiso 1 1 calc GR . . . .
H7C H 0.464081 0.299634 0.667522 0.044 Uiso 1 1 calc GR . . . .
C16 C 0.6510(7) 0.0779(5) 0.7369(4) 0.0342(15) Uani 1 1 d . . . . .
H16 H 0.546164 0.063303 0.725256 0.041 Uiso 1 1 calc R . . . .
C30 C 0.8910(7) 0.2618(5) 0.4602(3) 0.0293(13) Uani 1 1 d . . . . .
H30A H 0.951462 0.328672 0.466968 0.035 Uiso 1 1 calc R . . . .
H30B H 0.959851 0.221086 0.472897 0.035 Uiso 1 1 calc R . . . .
C9 C 0.7937(9) 0.0981(5) 0.5103(4) 0.0421(17) Uani 1 1 d . . . . .
H9A H 0.755783 0.073005 0.453170 0.063 Uiso 1 1 calc GR . . . .
H9B H 0.746553 0.049409 0.530013 0.063 Uiso 1 1 calc GR . . . .
H9C H 0.901276 0.107084 0.526176 0.063 Uiso 1 1 calc GR . . . .
C22 C 0.6161(6) 0.6042(4) 0.7317(3) 0.0246(11) Uani 1 1 d . . . . .
H22 H 0.511035 0.581284 0.713946 0.029 Uiso 1 1 calc R . . . .
C5A C 0.3019(8) 0.1595(6) 0.4416(5) 0.0341(16) Uani 0.874(5) 1 d . . P A 1
C17 C 0.9741(6) 0.0536(4) 0.8800(3) 0.0214(11) Uani 1 1 d . . . . .
O1W O 1.3031(6) -0.1329(4) 1.0192(3) 0.0381(11) Uani 1 1 d . . . . .
H1WA H 1.240481 -0.162537 1.037235 0.057 Uiso 1 1 d GR . . . .
H1WB H 1.390000 -0.113118 1.053193 0.057 Uiso 1 1 d GR . . . .
O2W O 1.3942(5) 0.1632(3) 0.9917(2) 0.0314(9) Uani 1 1 d . . . . .
H2WA H 1.439366 0.208803 1.039927 0.047 Uiso 1 1 d GR . . . .
H2WB H 1.344078 0.194351 0.963766 0.047 Uiso 1 1 d GR . . . .
Br3B Br 0.3216(18) 0.2934(11) 0.4251(10) 0.078(5) Uani 0.126(5) 1 d . . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Eu1 Eu1 4.3802(6) 2_757 ?
Eu1 O19 2.366(4) 2_757 ?
Eu1 O19 3.123(4) . ?
Eu1 O38 2.344(4) 2_756 ?
Eu1 O28 2.368(4) 2_767 ?
Eu1 O18 2.433(4) . ?
Eu1 O29 2.426(4) 1_545 ?
Eu1 O39 2.400(4) 1_656 ?
Eu1 C17 3.128(5) . ?
Eu1 O1W 2.461(5) . ?
Eu1 O2W 2.487(4) . ?
S1A O4A 1.422(6) . ?
S1A O3A 1.445(6) . ?
S1A O2A 1.446(6) . ?
S1A C5A 1.839(8) . ?
O19 C17 1.248(7) . ?
O38 C37 1.237(7) . ?
O28 C27 1.256(7) . ?
O18 C17 1.252(7) . ?
O29 C27 1.248(7) . ?
O39 C37 1.255(7) . ?
F8A C5A 1.311(9) . ?
F6A C5A 1.335(9) . ?
F7A C5A 1.353(9) . ?
N31 C36 1.339(7) . ?
N31 C32 1.358(7) . ?
N31 C30 1.508(6) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 N21 1.514(6) . ?
C20 C3 1.506(8) . ?
C24 C23 1.403(8) . ?
C24 C25 1.378(8) . ?
C24 C27 1.510(7) . ?
C36 H36 0.9500 . ?
C36 C35 1.376(8) . ?
N21 C26 1.325(7) . ?
N21 C22 1.342(7) . ?
C34 C37 1.524(7) . ?
C34 C33 1.377(8) . ?
C34 C35 1.391(7) . ?
C23 H23 0.9500 . ?
C23 C22 1.380(8) . ?
C5 C4 1.405(8) . ?
C5 C6 1.387(9) . ?
C5 C30 1.514(8) . ?
C3 C4 1.399(8) . ?
C3 C2 1.408(8) . ?
C1 C6 1.398(8) . ?
C1 C10 1.518(8) . ?
C1 C2 1.400(8) . ?
C33 H33 0.9500 . ?
C33 C32 1.371(8) . ?
C35 H35 0.9500 . ?
N11 C10 1.512(7) . ?
N11 C12 1.330(8) . ?
N11 C16 1.350(8) . ?
C32 H32 0.9500 . ?
C25 H25 0.9500 . ?
C25 C26 1.388(8) . ?
C4 C8 1.507(8) . ?
C6 C9 1.513(8) . ?
C26 H26 0.9500 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C13 H13 0.9500 . ?
C13 C14 1.388(8) . ?
C13 C12 1.379(9) . ?
C14 C15 1.377(9) . ?
C14 C17 1.504(7) . ?
C15 H15 0.9500 . ?
C15 C16 1.372(8) . ?
C2 C7 1.510(8) . ?
C12 H12 0.9500 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C16 H16 0.9500 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C22 H22 0.9500 . ?
O1W H1WA 0.8669 . ?
O1W H1WB 0.8663 . ?
O2W H2WA 0.8980 . ?
O2W H2WB 0.8987 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O19 Eu1 Eu1 31.45(7) . 2_757 ?
O19 Eu1 Eu1 43.52(9) 2_757 2_757 ?
O19 Eu1 O19 74.97(12) 2_757 . ?
O19 Eu1 O28 72.05(14) 2_757 2_767 ?
O19 Eu1 O18 119.75(13) 2_757 . ?
O19 Eu1 O29 78.72(13) 2_757 1_545 ?
O19 Eu1 O39 82.92(13) 2_757 1_656 ?
O19 Eu1 C17 98.00(14) 2_757 . ?
O19 Eu1 C17 23.03(13) . . ?
O19 Eu1 O1W 74.11(15) 2_757 . ?
O19 Eu1 O2W 138.99(14) 2_757 . ?
O38 Eu1 Eu1 143.39(9) 2_756 2_757 ?
O38 Eu1 O19 120.19(11) 2_756 . ?
O38 Eu1 O19 145.31(15) 2_756 2_757 ?
O38 Eu1 O28 142.21(15) 2_756 2_767 ?
O38 Eu1 O18 81.63(13) 2_756 . ?
O38 Eu1 O29 81.84(13) 2_756 1_545 ?
O38 Eu1 O39 96.74(13) 2_756 1_656 ?
O38 Eu1 C17 100.42(14) 2_756 . ?
O38 Eu1 O1W 72.60(15) 2_756 . ?
O38 Eu1 O2W 71.45(15) 2_756 . ?
O28 Eu1 Eu1 60.46(10) 2_767 2_757 ?
O28 Eu1 O19 62.74(12) 2_767 . ?
O28 Eu1 O18 79.01(13) 2_767 . ?
O28 Eu1 O29 122.94(13) 2_767 1_545 ?
O28 Eu1 O39 79.18(14) 2_767 1_656 ?
O28 Eu1 C17 70.02(14) 2_767 . ?
O28 Eu1 O1W 138.57(14) 2_767 . ?
O28 Eu1 O2W 71.57(15) 2_767 . ?
O18 Eu1 Eu1 76.23(9) . 2_757 ?
O18 Eu1 O19 44.79(11) . . ?
O18 Eu1 C17 21.76(14) . . ?
O18 Eu1 O1W 139.87(15) . . ?
O18 Eu1 O2W 70.38(14) . . ?
O29 Eu1 Eu1 64.47(9) 1_545 2_757 ?
O29 Eu1 O19 62.86(12) 1_545 . ?
O29 Eu1 O18 74.71(14) 1_545 . ?
O29 Eu1 C17 66.94(14) 1_545 . ?
O29 Eu1 O1W 71.65(16) 1_545 . ?
O29 Eu1 O2W 138.39(13) 1_545 . ?
O39 Eu1 Eu1 118.75(9) 1_656 2_757 ?
O39 Eu1 O19 140.17(12) 1_656 . ?
O39 Eu1 O18 141.07(15) 1_656 . ?
O39 Eu1 O29 143.91(14) 1_656 1_545 ?
O39 Eu1 C17 147.06(15) 1_656 . ?
O39 Eu1 O1W 73.55(16) 1_656 . ?
O39 Eu1 O2W 72.29(15) 1_656 . ?
C17 Eu1 Eu1 54.48(11) . 2_757 ?
O1W Eu1 Eu1 107.34(13) . 2_757 ?
O1W Eu1 O19 128.72(15) . . ?
O1W Eu1 C17 138.59(16) . . ?
O1W Eu1 O2W 126.06(17) . . ?
O2W Eu1 Eu1 125.45(11) . 2_757 ?
O2W Eu1 O19 103.99(13) . . ?
O2W Eu1 C17 86.82(15) . . ?
O4A S1A O3A 114.2(3) . . ?
O4A S1A O2A 117.6(4) . . ?
O4A S1A C5A 104.5(4) . . ?
O3A S1A O2A 114.3(4) . . ?
O3A S1A C5A 102.8(4) . . ?
O2A S1A C5A 100.4(4) . . ?
Eu1 O19 Eu1 105.03(12) 2_757 . ?
C17 O19 Eu1 176.2(4) . 2_757 ?
C17 O19 Eu1 78.7(3) . . ?
C37 O38 Eu1 175.3(4) . 2_756 ?
C27 O28 Eu1 139.8(4) . 2_767 ?
C17 O18 Eu1 112.2(3) . . ?
C27 O29 Eu1 135.7(3) . 1_565 ?
C37 O39 Eu1 134.8(3) . 1_454 ?
C36 N31 C32 120.8(5) . . ?
C36 N31 C30 122.1(5) . . ?
C32 N31 C30 117.0(5) . . ?
H20A C20 H20B 107.5 . . ?
N21 C20 H20A 108.5 . . ?
N21 C20 H20B 108.5 . . ?
C3 C20 H20A 108.5 . . ?
C3 C20 H20B 108.5 . . ?
C3 C20 N21 115.1(4) . . ?
C23 C24 C27 119.1(5) . . ?
C25 C24 C23 118.9(5) . . ?
C25 C24 C27 122.0(5) . . ?
N31 C36 H36 119.6 . . ?
N31 C36 C35 120.8(5) . . ?
C35 C36 H36 119.6 . . ?
C26 N21 C20 120.5(5) . . ?
C26 N21 C22 122.5(5) . . ?
C22 N21 C20 116.8(5) . . ?
C33 C34 C37 120.6(5) . . ?
C33 C34 C35 118.8(5) . . ?
C35 C34 C37 120.6(5) . . ?
C24 C23 H23 120.3 . . ?
C22 C23 C24 119.5(5) . . ?
C22 C23 H23 120.3 . . ?
O38 C37 O39 126.3(5) . . ?
O38 C37 C34 117.0(5) . . ?
O39 C37 C34 116.7(5) . . ?
C4 C5 C30 119.6(5) . . ?
C6 C5 C4 121.2(5) . . ?
C6 C5 C30 119.2(5) . . ?
C4 C3 C20 121.0(5) . . ?
C4 C3 C2 120.4(5) . . ?
C2 C3 C20 118.0(5) . . ?
C6 C1 C10 120.4(5) . . ?
C6 C1 C2 121.4(5) . . ?
C2 C1 C10 117.6(5) . . ?
C34 C33 H33 119.8 . . ?
C32 C33 C34 120.3(5) . . ?
C32 C33 H33 119.8 . . ?
C36 C35 C34 119.3(5) . . ?
C36 C35 H35 120.4 . . ?
C34 C35 H35 120.4 . . ?
C12 N11 C10 122.1(5) . . ?
C12 N11 C16 120.4(5) . . ?
C16 N11 C10 117.3(5) . . ?
N31 C32 C33 119.9(5) . . ?
N31 C32 H32 120.0 . . ?
C33 C32 H32 120.0 . . ?
C24 C25 H25 120.3 . . ?
C24 C25 C26 119.3(5) . . ?
C26 C25 H25 120.3 . . ?
C5 C4 C8 120.0(5) . . ?
C3 C4 C5 119.2(5) . . ?
C3 C4 C8 120.8(5) . . ?
C5 C6 C1 118.9(5) . . ?
C5 C6 C9 119.9(6) . . ?
C1 C6 C9 121.3(6) . . ?
N21 C26 C25 120.3(5) . . ?
N21 C26 H26 119.9 . . ?
C25 C26 H26 119.9 . . ?
C1 C10 H10A 108.6 . . ?
C1 C10 H10B 108.6 . . ?
N11 C10 C1 114.7(5) . . ?
N11 C10 H10A 108.6 . . ?
N11 C10 H10B 108.6 . . ?
H10A C10 H10B 107.6 . . ?
C14 C13 H13 120.3 . . ?
C12 C13 H13 120.3 . . ?
C12 C13 C14 119.4(6) . . ?
C13 C14 C17 121.5(5) . . ?
C15 C14 C13 118.5(5) . . ?
C15 C14 C17 119.9(5) . . ?
O28 C27 C24 115.4(5) . . ?
O29 C27 O28 127.5(5) . . ?
O29 C27 C24 117.1(5) . . ?
C14 C15 H15 120.0 . . ?
C16 C15 C14 119.9(6) . . ?
C16 C15 H15 120.0 . . ?
C3 C2 C7 120.3(5) . . ?
C1 C2 C3 118.8(5) . . ?
C1 C2 C7 121.0(5) . . ?
N11 C12 C13 121.0(6) . . ?
N11 C12 H12 119.5 . . ?
C13 C12 H12 119.5 . . ?
C4 C8 H8A 109.5 . . ?
C4 C8 H8B 109.5 . . ?
C4 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N11 C16 C15 120.6(6) . . ?
N11 C16 H16 119.7 . . ?
C15 C16 H16 119.7 . . ?
N31 C30 C5 113.8(5) . . ?
N31 C30 H30A 108.8 . . ?
N31 C30 H30B 108.8 . . ?
C5 C30 H30A 108.8 . . ?
C5 C30 H30B 108.8 . . ?
H30A C30 H30B 107.7 . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N21 C22 C23 119.5(5) . . ?
N21 C22 H22 120.3 . . ?
C23 C22 H22 120.3 . . ?
F8A C5A S1A 111.9(5) . . ?
F8A C5A F6A 108.6(7) . . ?
F8A C5A F7A 106.3(6) . . ?
F6A C5A S1A 111.1(5) . . ?
F6A C5A F7A 106.7(6) . . ?
F7A C5A S1A 111.9(5) . . ?
O19 C17 Eu1 78.3(3) . . ?
O19 C17 O18 124.3(5) . . ?
O19 C17 C14 117.6(5) . . ?
O18 C17 Eu1 46.1(2) . . ?
O18 C17 C14 118.1(5) . . ?
C14 C17 Eu1 164.1(4) . . ?
Eu1 O1W H1WA 110.2 . . ?
Eu1 O1W H1WB 110.2 . . ?
H1WA O1W H1WB 108.5 . . ?
Eu1 O2W H2WA 111.4 . . ?
Eu1 O2W H2WB 111.7 . . ?
H2WA O2W H2WB 107.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Eu1 O19 C17 O18 -1.4(5) . . . . ?
Eu1 O19 C17 C14 179.0(5) . . . . ?
Eu1 O28 C27 O29 48.0(9) 2_767 . . . ?
Eu1 O28 C27 C24 -132.6(5) 2_767 . . . ?
Eu1 O18 C17 O19 1.9(7) . . . . ?
Eu1 O18 C17 C14 -178.5(4) . . . . ?
Eu1 O29 C27 O28 -4.5(9) 1_565 . . . ?
Eu1 O29 C27 C24 176.1(3) 1_565 . . . ?
Eu1 O39 C37 O38 5.3(9) 1_454 . . . ?
Eu1 O39 C37 C34 -174.8(3) 1_454 . . . ?
O4A S1A C5A F8A -56.5(6) . . . . ?
O4A S1A C5A F6A -178.2(6) . . . . ?
O4A S1A C5A F7A 62.7(6) . . . . ?
O3A S1A C5A F8A -176.1(5) . . . . ?
O3A S1A C5A F6A 62.2(6) . . . . ?
O3A S1A C5A F7A -56.9(6) . . . . ?
N31 C36 C35 C34 -1.8(9) . . . . ?
O2A S1A C5A F8A 65.8(6) . . . . ?
O2A S1A C5A F6A -55.9(7) . . . . ?
O2A S1A C5A F7A -175.0(5) . . . . ?
C20 N21 C26 C25 174.1(5) . . . . ?
C20 N21 C22 C23 -175.6(5) . . . . ?
C20 C3 C4 C5 -167.9(5) . . . . ?
C20 C3 C4 C8 10.6(8) . . . . ?
C20 C3 C2 C1 166.1(5) . . . . ?
C20 C3 C2 C7 -13.1(7) . . . . ?
C24 C23 C22 N21 1.6(9) . . . . ?
C24 C25 C26 N21 1.1(9) . . . . ?
C36 N31 C32 C33 -0.7(9) . . . . ?
C36 N31 C30 C5 20.0(8) . . . . ?
N21 C20 C3 C4 -102.9(6) . . . . ?
N21 C20 C3 C2 86.3(6) . . . . ?
C34 C33 C32 N31 0.0(10) . . . . ?
C23 C24 C25 C26 0.2(8) . . . . ?
C23 C24 C27 O28 18.5(7) . . . . ?
C23 C24 C27 O29 -162.1(5) . . . . ?
C37 C34 C33 C32 179.9(5) . . . . ?
C37 C34 C35 C36 -179.0(5) . . . . ?
C3 C20 N21 C26 40.0(7) . . . . ?
C3 C20 N21 C22 -144.6(5) . . . . ?
C33 C34 C37 O38 2.4(8) . . . . ?
C33 C34 C37 O39 -177.5(5) . . . . ?
C33 C34 C35 C36 1.1(8) . . . . ?
C35 C34 C37 O38 -177.5(5) . . . . ?
C35 C34 C37 O39 2.6(8) . . . . ?
C35 C34 C33 C32 -0.2(9) . . . . ?
C32 N31 C36 C35 1.6(9) . . . . ?
C32 N31 C30 C5 -164.2(6) . . . . ?
C25 C24 C23 C22 -1.5(8) . . . . ?
C25 C24 C27 O28 -162.7(5) . . . . ?
C25 C24 C27 O29 16.8(8) . . . . ?
C4 C5 C6 C1 -2.9(8) . . . . ?
C4 C5 C6 C9 176.2(6) . . . . ?
C4 C5 C30 N31 -94.8(6) . . . . ?
C4 C3 C2 C1 -4.8(8) . . . . ?
C4 C3 C2 C7 176.1(5) . . . . ?
C6 C5 C4 C3 1.2(8) . . . . ?
C6 C5 C4 C8 -177.2(5) . . . . ?
C6 C5 C30 N31 86.2(7) . . . . ?
C6 C1 C10 N11 94.3(6) . . . . ?
C6 C1 C2 C3 3.1(8) . . . . ?
C6 C1 C2 C7 -177.8(5) . . . . ?
C26 N21 C22 C23 -0.3(9) . . . . ?
C10 C1 C6 C5 171.8(5) . . . . ?
C10 C1 C6 C9 -7.3(8) . . . . ?
C10 C1 C2 C3 -168.2(5) . . . . ?
C10 C1 C2 C7 10.9(8) . . . . ?
C10 N11 C12 C13 -173.9(6) . . . . ?
C10 N11 C16 C15 175.4(6) . . . . ?
C13 C14 C15 C16 2.2(10) . . . . ?
C13 C14 C17 Eu1 -13.4(17) . . . . ?
C13 C14 C17 O19 170.4(6) . . . . ?
C13 C14 C17 O18 -9.3(8) . . . . ?
C14 C13 C12 N11 -0.6(11) . . . . ?
C14 C15 C16 N11 -2.0(11) . . . . ?
C27 C24 C23 C22 177.4(5) . . . . ?
C27 C24 C25 C26 -178.7(5) . . . . ?
C15 C14 C17 Eu1 166.6(11) . . . . ?
C15 C14 C17 O19 -9.6(8) . . . . ?
C15 C14 C17 O18 170.7(6) . . . . ?
C2 C3 C4 C5 2.7(8) . . . . ?
C2 C3 C4 C8 -178.8(5) . . . . ?
C2 C1 C6 C5 0.7(8) . . . . ?
C2 C1 C6 C9 -178.3(6) . . . . ?
C2 C1 C10 N11 -94.3(6) . . . . ?
C12 N11 C10 C1 -35.3(8) . . . . ?
C12 N11 C16 C15 0.3(11) . . . . ?
C12 C13 C14 C15 -1.0(10) . . . . ?
C12 C13 C14 C17 179.0(6) . . . . ?
C16 N11 C10 C1 149.7(6) . . . . ?
C16 N11 C12 C13 1.0(10) . . . . ?
C30 N31 C36 C35 177.2(6) . . . . ?
C30 N31 C32 C33 -176.5(6) . . . . ?
C30 C5 C4 C3 -177.8(5) . . . . ?
C30 C5 C4 C8 3.7(8) . . . . ?
C30 C5 C6 C1 176.1(5) . . . . ?
C30 C5 C6 C9 -4.8(8) . . . . ?
C22 N21 C26 C25 -1.1(9) . . . . ?
C17 C14 C15 C16 -177.8(6) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.508 0.500 1.000 679.7 216.7 '22x water'

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.723
_oxdiff_exptl_absorpt_empirical_full_min 0.574
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_jj003_br_la_otf_h2o_acet_red3
_database_code_depnum_ccdc_archive 'CCDC 1833430'
loop_
_audit_author_name
_audit_author_address
'Antti Tiihonen'
;University of Jyv?skyl?, Department of Chemistry
Finland
;
_audit_update_record             
;
2018-03-29 deposited with the CCDC.	2019-02-28 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_CHEMW03_I                   
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: The structure contains voids of unresolved electron density
which was treated using Olex2 solvent mask procedure (full details in 
_smtbx_masks_special_details). The 10 water molecules per asymmetric unit 
 are included in the formula and used in the calculations. 
;
_vrf_PLAT973_I                   
;
PROBLEM: Check Calcd Positive Resid. Density on       La1  
RESPONSE: Peak is located about 1 Angstrom from the metal atom and is caused by
the absorption effects. Data recorded with Cu-radiation. 
;
_vrf_PLAT420_I                   
;
PROBLEM: D-H Without Acceptor       O1W      --H1WA
RESPONSE: Hydrogen bond acceptor (water) have been removed among the other 
disordered solvents (also water) from the voids (see vrf_CHEMW03_ALERT_2_A).
;
_vrf_FORMU01_I                   
;
PROBLEM: There is a discrepancy between the atom counts in the
            _chemical_formula_sum and _chemical_formula_moiety.
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_CELLZ01_I                   
;
PROBLEM: Difference between formula and atom_site contents detected.
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT041_I                   
;
PROBLEM: Calculated and Reported SumFormula strings Differ ...    
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT042_I                   
;
PROBLEM: Calculated and Reported Moiety formula strings Differ by ...
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT068_I                   
;
PROBLEM: Reported F000 Differs from Calcd (or Missing)...
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT606_I                   
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
# end Validation Reply Form
_audit_creation_date             2018-03-26
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H31 La N3 O8, 2.23(Br), 0.77(C F3 O3 S)'
_chemical_formula_sum            'C30.76 H51 Br2.24 F2.30 La N3 O20.30 S0.76'
_chemical_formula_weight         1173.28
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C21 H25 O12 N3 F12 S3 Br1 La1'
_chemical_oxdiff_usercomment     'clear colorless block'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
La La -1.4094 9.0376 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.6013(3)
_cell_length_b                   14.3577(3)
_cell_length_c                   18.7825(5)
_cell_angle_alpha                106.592(2)
_cell_angle_beta                 102.854(2)
_cell_angle_gamma                99.256(2)
_cell_volume                     2348.44(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8636
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      76.3530
_cell_measurement_theta_min      3.2790
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    10.314
_exptl_absorpt_correction_T_max  0.489
_exptl_absorpt_correction_T_min  0.137
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.659
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1174
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 -2 12 0.0361
1 5 -12 0.0311
-2 3 -10 0.0480
-2 -1 -9 0.0498
4 5 -8 0.0484
1 -2 -11 0.0433
-2 9 -1 0.0493
-6 0 3 0.1016
6 -4 -2 0.0784
-4 -4 0 0.0860
0 -9 7 0.0624
0 9 -7 0.0279

_exptl_crystal_size_max          0.202
_exptl_crystal_size_mid          0.132
_exptl_crystal_size_min          0.076
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.9964 -1.9934 11.9964 0.9421 -0.3030 -0.0043
0.9971 4.9951 -11.9969 -0.9353 0.2295 -0.3339
-2.0015 2.9941 -9.9980 -0.6724 0.6870 -0.1277
-2.0022 -1.0076 -8.9976 -0.6058 0.7419 0.3037
3.9971 4.9991 -7.9973 -0.7488 -0.4374 -0.4330
0.9957 -2.0083 -10.9960 -0.8755 0.3579 0.4356
-1.9972 9.0037 -1.0017 0.0221 0.1524 -0.9816
-5.9965 -0.0004 2.9974 0.4592 0.8600 -0.0187
5.9957 -4.0012 -1.9971 -0.3925 -0.8051 0.4500
-3.9993 -4.0040 -0.0004 0.1457 0.7574 0.4780
-0.0001 -9.0005 6.9993 0.5093 -0.0811 0.8768
0.0001 9.0005 -6.9993 -0.5093 0.0811 -0.8768

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            14614
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.990
_diffrn_reflns_theta_min         3.309
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -66.00  32.00   1.00    1.00    --  -41.65  37.00  60.00   98
  2  ω    -95.00  -2.00   1.00    1.00    --  -41.65 125.00  60.00   93
  3  ω    -95.00  -8.00   1.00    1.00    --  -41.65 125.00 150.00   87
  4  ω   -108.00 -17.00   1.00    1.00    --  -41.65 -37.00-120.00   91
  5  ω     37.00 145.00   1.00    2.00    --  112.00 -77.00-120.00  108
  6  ω     90.00 116.00   1.00    2.00    --  112.00-111.00 -30.00   26
  7  ω     94.00 141.00   1.00    2.00    --  112.00 -61.00  90.00   47
  8  ω     88.00 178.00   1.00    2.00    --  112.00  45.00 -30.00   90
  9  ω    101.00 151.00   1.00    2.00    --  112.00 111.00  60.00   50
 10  ω     83.00 178.00   1.00    2.00    --  112.00  61.00  30.00   95
 11  ω     44.00 140.00   1.00    2.00    --  112.00 -30.00   0.00   96
 12  ω     44.00  71.00   1.00    2.00    --  112.00 -61.00  90.00   27
 13  ω     31.00 108.00   1.00    2.00    --  112.00 -94.00  60.00   77
 14  ω     38.00  63.00   1.00    2.00    --  112.00-111.00 -30.00   25
 15  ω     37.00 116.00   1.00    2.00    --  112.00-111.00-180.00   79
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0387330000
_diffrn_orient_matrix_UB_12      0.0022839000
_diffrn_orient_matrix_UB_13      0.0756963000
_diffrn_orient_matrix_UB_21      -0.1649187000
_diffrn_orient_matrix_UB_22      -0.0244403000
_diffrn_orient_matrix_UB_23      -0.0430170000
_diffrn_orient_matrix_UB_31      -0.0066865000
_diffrn_orient_matrix_UB_32      -0.1126929000
_diffrn_orient_matrix_UB_33      -0.0196417000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8004
_reflns_number_total             8515
_reflns_odcompleteness_completeness 99.48
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         2.421
_refine_diff_density_min         -2.604
_refine_diff_density_rms         0.157
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     484
_refine_ls_number_reflns         8515
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0574
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0995P)²+10.2287P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1614
_refine_ls_wR_factor_ref         0.1649
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C10) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Sof(Br3B)=1-FVAR(1)
 Sof(S1A)=Sof(F7A)=Sof(F6A)=Sof(O2A)=Sof(O3A)=Sof(F8A)=Sof(O4A)=Sof(C5A)=FVAR(1)
4.a Rotating group:
 O2W(H2WA,H2WB), O1W(H1WA,H1WB)
4.b Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C20(H20A,H20B), C10(H10A,H10B)
4.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C16(H16), C35(H35), C13(H13), C36(H36), C33(H33), C23(H23),
 C12(H12), C22(H22), C25(H25), C32(H32), C26(H26)
4.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C7(H7A,H7B,H7C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
La1 La 0.27801(3) 0.99184(2) 1.00502(2) 0.02100(12) Uani 1 1 d . . . . .
Br2 Br -0.29698(9) 0.57376(7) 0.69839(5) 0.0474(2) Uani 1 1 d . . . . .
Br1 Br -0.21856(11) 1.07387(7) 0.68808(5) 0.0563(2) Uani 1 1 d . . . . .
S1A S 0.2027(6) 0.7384(4) 0.6027(2) 0.0251(10) Uani 0.766(6) 1 d . . P A 1
O29 O -0.6276(5) 0.9379(4) 0.1218(2) 0.0329(10) Uani 1 1 d . . . . .
O28 O -0.4364(5) 0.9724(3) 0.0777(2) 0.0274(9) Uani 1 1 d . . . . .
F7A F 0.3248(7) 0.9125(4) 0.5881(4) 0.0496(15) Uani 0.766(6) 1 d . . P A 1
F6A F 0.0878(7) 0.8856(4) 0.5731(4) 0.0502(16) Uani 0.766(6) 1 d . . P A 1
O2A O 0.3173(7) 0.7005(5) 0.5768(4) 0.0402(16) Uani 0.766(6) 1 d . . P A 1
C6 C -0.2551(7) 0.6278(4) 0.4561(3) 0.0270(13) Uani 1 1 d . . . . .
N11 N -0.2959(6) 0.7810(4) 0.6245(3) 0.0260(10) Uani 1 1 d . . . . .
C14 C -0.1437(6) 0.8692(4) 0.7780(3) 0.0210(11) Uani 1 1 d . . . . .
C27 C -0.4950(7) 0.9452(5) 0.1259(3) 0.0277(13) Uani 1 1 d . . . . .
N31 N -0.1898(6) 0.4487(4) 0.3065(3) 0.0257(10) Uani 1 1 d . . . . .
C1 C -0.2980(7) 0.7165(5) 0.4840(3) 0.0289(13) Uani 1 1 d . . . . .
N21 N -0.2235(6) 0.8866(4) 0.3121(3) 0.0272(11) Uani 1 1 d . . . . .
C5 C -0.1755(7) 0.6192(4) 0.4017(3) 0.0255(12) Uani 1 1 d . . . . .
C15 C -0.0727(7) 0.8314(4) 0.7236(3) 0.0244(12) Uani 1 1 d . . . . .
H15 H 0.030195 0.836671 0.739197 0.029 Uiso 1 1 calc R . . . .
O3A O 0.0601(7) 0.6766(5) 0.5685(4) 0.0374(15) Uani 0.766(6) 1 d . . P A 1
C3 C -0.1818(8) 0.7870(4) 0.4028(3) 0.0284(13) Uani 1 1 d . . . . .
F8A F 0.1678(8) 0.8091(5) 0.4832(4) 0.0564(17) Uani 0.766(6) 1 d . . P A 1
C24 C -0.3976(7) 0.9246(5) 0.1909(3) 0.0282(13) Uani 1 1 d . . . . .
C30 C -0.1047(7) 0.5319(4) 0.3806(4) 0.0296(13) Uani 1 1 d . . . . .
H30A H -0.005924 0.557397 0.376284 0.035 Uiso 1 1 calc R . . . .
H30B H -0.091098 0.503935 0.423420 0.035 Uiso 1 1 calc R . . . .
C16 C -0.1514(7) 0.7864(5) 0.6471(3) 0.0287(13) Uani 1 1 d . . . . .
H16 H -0.103105 0.758963 0.609981 0.034 Uiso 1 1 calc R . . . .
C35 C -0.4148(7) 0.3421(4) 0.2208(4) 0.0269(12) Uani 1 1 d . . . . .
H35 H -0.519280 0.324239 0.205974 0.032 Uiso 1 1 calc R . . . .
C13 C -0.2936(7) 0.8609(5) 0.7528(3) 0.0295(13) Uani 1 1 d . . . . .
H13 H -0.345162 0.885823 0.789019 0.035 Uiso 1 1 calc R . . . .
C36 C -0.3385(7) 0.4233(4) 0.2847(4) 0.0267(12) Uani 1 1 d . . . . .
H36 H -0.390589 0.462216 0.313980 0.032 Uiso 1 1 calc R . . . .
O4A O 0.2462(9) 0.7992(6) 0.6844(4) 0.0496(19) Uani 0.766(6) 1 d . . P A 1
C4 C -0.1425(7) 0.6971(4) 0.3725(3) 0.0258(12) Uani 1 1 d . . . . .
C33 C -0.1841(7) 0.3149(5) 0.2000(4) 0.0308(13) Uani 1 1 d . . . . .
H33 H -0.130156 0.278905 0.169977 0.037 Uiso 1 1 calc R . . . .
C8 C -0.0630(8) 0.6844(5) 0.3102(4) 0.0349(14) Uani 1 1 d . . . . .
H8A H 0.043505 0.705210 0.334495 0.052 Uiso 1 1 calc GR . . . .
H8B H -0.091288 0.725858 0.278619 0.052 Uiso 1 1 calc GR . . . .
H8C H -0.090108 0.613982 0.277108 0.052 Uiso 1 1 calc GR . . . .
C20 C -0.1223(8) 0.8753(5) 0.3806(4) 0.0330(14) Uani 1 1 d . . . . .
H20A H -0.101420 0.937226 0.425456 0.040 Uiso 1 1 calc R . . . .
H20B H -0.027937 0.868289 0.369182 0.040 Uiso 1 1 calc R . . . .
C23 C -0.2468(8) 0.9516(5) 0.2086(4) 0.0357(15) Uani 1 1 d . . . . .
H23 H -0.201935 0.983736 0.178758 0.043 Uiso 1 1 calc R . . . .
C12 C -0.3674(7) 0.8167(5) 0.6758(4) 0.0324(14) Uani 1 1 d . . . . .
H12 H -0.470136 0.811298 0.658637 0.039 Uiso 1 1 calc R . . . .
C22 C -0.1606(8) 0.9324(5) 0.2692(4) 0.0364(15) Uani 1 1 d . . . . .
H22 H -0.056411 0.951226 0.281026 0.044 Uiso 1 1 calc R . . . .
C2 C -0.2568(8) 0.7979(5) 0.4583(3) 0.0309(14) Uani 1 1 d . . . . .
C25 C -0.4597(8) 0.8773(6) 0.2349(4) 0.0394(16) Uani 1 1 d . . . . .
H25 H -0.563617 0.857956 0.224035 0.047 Uiso 1 1 calc R . . . .
C32 C -0.1123(7) 0.3953(5) 0.2651(4) 0.0279(13) Uani 1 1 d . . . . .
H32 H -0.007821 0.413941 0.281410 0.033 Uiso 1 1 calc R . . . .
C9 C -0.2932(10) 0.5424(5) 0.4867(4) 0.0426(17) Uani 1 1 d . . . . .
H9A H -0.247517 0.488581 0.465462 0.064 Uiso 1 1 calc GR . . . .
H9B H -0.400299 0.516779 0.470966 0.064 Uiso 1 1 calc GR . . . .
H9C H -0.256435 0.566937 0.543376 0.064 Uiso 1 1 calc GR . . . .
C10 C -0.3860(8) 0.7274(5) 0.5407(3) 0.0340(15) Uani 1 1 d . U . . .
H10A H -0.439505 0.659917 0.535939 0.041 Uiso 1 1 calc R . . . .
H10B H -0.460276 0.764609 0.527016 0.041 Uiso 1 1 calc R . . . .
C7 C -0.2962(11) 0.8956(6) 0.4933(4) 0.048(2) Uani 1 1 d . . . . .
H7A H -0.403365 0.884433 0.482138 0.073 Uiso 1 1 calc GR . . . .
H7B H -0.259312 0.944962 0.470890 0.073 Uiso 1 1 calc GR . . . .
H7C H -0.251308 0.920634 0.549507 0.073 Uiso 1 1 calc GR . . . .
C26 C -0.3689(9) 0.8584(6) 0.2952(4) 0.0392(16) Uani 1 1 d . . . . .
H26 H -0.411491 0.824648 0.324804 0.047 Uiso 1 1 calc R . . . .
C5A C 0.1989(10) 0.8427(6) 0.5598(6) 0.0348(19) Uani 0.766(6) 1 d . . P A 1
O19 O 0.0767(5) 0.9248(4) 0.8802(2) 0.0300(10) Uani 1 1 d . . . . .
O18 O -0.1296(5) 0.9486(3) 0.9096(2) 0.0255(9) Uani 1 1 d . . . . .
O38 O -0.3407(5) 0.1614(3) 0.0648(2) 0.0314(10) Uani 1 1 d . . . . .
O39 O -0.5512(5) 0.1549(3) 0.0997(2) 0.0284(9) Uani 1 1 d . . . . .
C17 C -0.0592(6) 0.9180(4) 0.8631(3) 0.0212(11) Uani 1 1 d . . . . .
C34 C -0.3379(7) 0.2860(4) 0.1779(3) 0.0255(12) Uani 1 1 d . . . . .
C37 C -0.4180(7) 0.1934(4) 0.1082(3) 0.0257(12) Uani 1 1 d . . . . .
O2W O 0.1039(6) 0.8337(3) 1.0036(3) 0.0366(11) Uani 1 1 d . . . . .
H2WA H 0.144309 0.783259 0.993174 0.055 Uiso 1 1 d GR . . . .
H2WB H 0.024619 0.817173 0.965099 0.055 Uiso 1 1 d GR . . . .
O1W O 0.2116(6) 1.1392(4) 0.9673(3) 0.0435(12) Uani 1 1 d . . . . .
H1WA H 0.225272 1.192954 1.009541 0.065 Uiso 1 1 d GR . . . .
H1WB H 0.114220 1.125584 0.943927 0.065 Uiso 1 1 d GR . . . .
Br3B Br 0.1943(13) 0.7260(9) 0.5920(7) 0.077(4) Uani 0.234(6) 1 d . . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
La1 O29 2.557(4) 1_656 ?
La1 O28 2.500(4) 2_576 ?
La1 O28 2.874(4) 1_656 ?
La1 C27 3.081(6) 1_656 ?
La1 O19 2.501(4) . ?
La1 O18 2.441(4) 2_577 ?
La1 O38 2.460(4) 2_566 ?
La1 O39 2.534(4) 1_666 ?
La1 O2W 2.583(5) . ?
La1 O1W 2.545(5) . ?
S1A O2A 1.422(8) . ?
S1A O3A 1.402(9) . ?
S1A O4A 1.458(8) . ?
S1A C5A 1.893(10) . ?
O29 C27 1.244(8) . ?
O28 C27 1.283(8) . ?
F7A C5A 1.329(11) . ?
F6A C5A 1.350(11) . ?
C6 C1 1.396(9) . ?
C6 C5 1.398(9) . ?
C6 C9 1.522(8) . ?
N11 C16 1.340(8) . ?
N11 C12 1.337(8) . ?
N11 C10 1.519(7) . ?
C14 C15 1.384(8) . ?
C14 C13 1.385(9) . ?
C14 C17 1.517(7) . ?
C27 C24 1.496(8) . ?
N31 C30 1.504(7) . ?
N31 C36 1.352(8) . ?
N31 C32 1.359(8) . ?
C1 C2 1.419(9) . ?
C1 C10 1.491(9) . ?
N21 C20 1.497(7) . ?
N21 C22 1.356(9) . ?
N21 C26 1.327(10) . ?
C5 C30 1.517(8) . ?
C5 C4 1.401(8) . ?
C15 H15 0.9500 . ?
C15 C16 1.372(8) . ?
C3 C4 1.402(8) . ?
C3 C20 1.511(9) . ?
C3 C2 1.382(10) . ?
F8A C5A 1.326(11) . ?
C24 C23 1.374(10) . ?
C24 C25 1.382(9) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C16 H16 0.9500 . ?
C35 H35 0.9500 . ?
C35 C36 1.367(8) . ?
C35 C34 1.388(8) . ?
C13 H13 0.9500 . ?
C13 C12 1.369(8) . ?
C36 H36 0.9500 . ?
C4 C8 1.519(9) . ?
C33 H33 0.9500 . ?
C33 C32 1.366(9) . ?
C33 C34 1.399(9) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C23 H23 0.9500 . ?
C23 C22 1.376(9) . ?
C12 H12 0.9500 . ?
C22 H22 0.9500 . ?
C2 C7 1.516(9) . ?
C25 H25 0.9500 . ?
C25 C26 1.389(9) . ?
C32 H32 0.9500 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C26 H26 0.9500 . ?
O19 C17 1.253(7) . ?
O18 C17 1.246(7) . ?
O38 C37 1.262(8) . ?
O39 C37 1.264(8) . ?
C34 C37 1.517(8) . ?
O2W H2WA 0.8699 . ?
O2W H2WB 0.8700 . ?
O1W H1WA 0.9024 . ?
O1W H1WB 0.9025 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O29 La1 O28 47.75(14) 1_656 1_656 ?
O29 La1 C27 23.18(17) 1_656 1_656 ?
O29 La1 O2W 67.37(16) 1_656 . ?
O28 La1 O29 122.19(14) 2_576 1_656 ?
O28 La1 O28 74.59(13) 2_576 1_656 ?
O28 La1 C27 99.11(16) 2_576 1_656 ?
O28 La1 C27 24.57(15) 1_656 1_656 ?
O28 La1 O19 84.07(14) 2_576 . ?
O28 La1 O39 81.20(14) 2_576 1_666 ?
O28 La1 O2W 134.73(15) 2_576 . ?
O28 La1 O1W 73.41(16) 2_576 . ?
O19 La1 O29 137.93(16) . 1_656 ?
O19 La1 O28 142.34(13) . 1_656 ?
O19 La1 C27 147.16(16) . 1_656 ?
O19 La1 O39 141.09(15) . 1_666 ?
O19 La1 O2W 70.99(15) . . ?
O19 La1 O1W 71.67(16) . . ?
O18 La1 O29 76.56(14) 2_577 1_656 ?
O18 La1 O28 116.66(12) 2_577 1_656 ?
O18 La1 O28 148.51(14) 2_577 2_576 ?
O18 La1 C27 96.07(15) 2_577 1_656 ?
O18 La1 O19 97.75(14) 2_577 . ?
O18 La1 O38 142.01(16) 2_577 2_566 ?
O18 La1 O39 77.87(14) 2_577 1_666 ?
O18 La1 O2W 73.98(15) 2_577 . ?
O18 La1 O1W 77.36(16) 2_577 . ?
O38 La1 O29 82.44(15) 2_566 1_656 ?
O38 La1 O28 69.22(15) 2_566 2_576 ?
O38 La1 O28 66.30(14) 2_566 1_656 ?
O38 La1 C27 73.51(15) 2_566 1_656 ?
O38 La1 O19 77.29(15) 2_566 . ?
O38 La1 O39 128.82(15) 2_566 1_666 ?
O38 La1 O2W 68.78(16) 2_566 . ?
O38 La1 O1W 133.17(16) 2_566 . ?
O39 La1 O29 79.32(15) 1_666 1_656 ?
O39 La1 O28 66.05(13) 1_666 1_656 ?
O39 La1 C27 71.11(15) 1_666 1_656 ?
O39 La1 O2W 140.29(15) 1_666 . ?
O39 La1 O1W 69.65(16) 1_666 . ?
O2W La1 O28 102.87(14) . 1_656 ?
O2W La1 C27 84.55(17) . 1_656 ?
O1W La1 O29 142.84(16) . 1_656 ?
O1W La1 O28 128.21(16) . 1_656 ?
O1W La1 C27 140.72(17) . 1_656 ?
O1W La1 O2W 128.52(18) . . ?
O2A S1A O4A 114.2(5) . . ?
O2A S1A C5A 99.8(5) . . ?
O3A S1A O2A 116.5(5) . . ?
O3A S1A O4A 119.4(5) . . ?
O3A S1A C5A 103.5(5) . . ?
O4A S1A C5A 98.5(5) . . ?
C27 O29 La1 102.8(4) . 1_454 ?
La1 O28 La1 105.41(13) 2_576 1_454 ?
C27 O28 La1 167.2(4) . 2_576 ?
C27 O28 La1 86.8(3) . 1_454 ?
C1 C6 C5 119.6(6) . . ?
C1 C6 C9 119.5(6) . . ?
C5 C6 C9 120.9(6) . . ?
C16 N11 C10 121.1(5) . . ?
C12 N11 C16 121.1(5) . . ?
C12 N11 C10 117.7(5) . . ?
C15 C14 C13 118.3(5) . . ?
C15 C14 C17 120.7(5) . . ?
C13 C14 C17 121.0(5) . . ?
O29 C27 La1 54.0(3) . 1_454 ?
O29 C27 O28 122.7(5) . . ?
O29 C27 C24 119.2(6) . . ?
O28 C27 La1 68.6(3) . 1_454 ?
O28 C27 C24 118.1(6) . . ?
C24 C27 La1 172.8(4) . 1_454 ?
C36 N31 C30 121.1(5) . . ?
C36 N31 C32 121.0(5) . . ?
C32 N31 C30 117.8(5) . . ?
C6 C1 C2 119.7(6) . . ?
C6 C1 C10 121.0(6) . . ?
C2 C1 C10 119.3(6) . . ?
C22 N21 C20 117.0(6) . . ?
C26 N21 C20 122.6(6) . . ?
C26 N21 C22 120.4(5) . . ?
C6 C5 C30 120.9(5) . . ?
C6 C5 C4 120.9(5) . . ?
C4 C5 C30 117.7(6) . . ?
C14 C15 H15 120.1 . . ?
C16 C15 C14 119.8(6) . . ?
C16 C15 H15 120.1 . . ?
C4 C3 C20 117.7(6) . . ?
C2 C3 C4 120.9(6) . . ?
C2 C3 C20 121.0(6) . . ?
C23 C24 C27 121.9(6) . . ?
C23 C24 C25 118.5(6) . . ?
C25 C24 C27 119.6(6) . . ?
N31 C30 C5 115.1(5) . . ?
N31 C30 H30A 108.5 . . ?
N31 C30 H30B 108.5 . . ?
C5 C30 H30A 108.5 . . ?
C5 C30 H30B 108.5 . . ?
H30A C30 H30B 107.5 . . ?
N11 C16 C15 120.4(6) . . ?
N11 C16 H16 119.8 . . ?
C15 C16 H16 119.8 . . ?
C36 C35 H35 120.3 . . ?
C36 C35 C34 119.3(6) . . ?
C34 C35 H35 120.3 . . ?
C14 C13 H13 120.0 . . ?
C12 C13 C14 119.9(6) . . ?
C12 C13 H13 120.0 . . ?
N31 C36 C35 120.7(6) . . ?
N31 C36 H36 119.7 . . ?
C35 C36 H36 119.7 . . ?
C5 C4 C3 118.9(6) . . ?
C5 C4 C8 120.3(5) . . ?
C3 C4 C8 120.8(6) . . ?
C32 C33 H33 120.3 . . ?
C32 C33 C34 119.3(6) . . ?
C34 C33 H33 120.3 . . ?
C4 C8 H8A 109.5 . . ?
C4 C8 H8B 109.5 . . ?
C4 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N21 C20 C3 114.2(5) . . ?
N21 C20 H20A 108.7 . . ?
N21 C20 H20B 108.7 . . ?
C3 C20 H20A 108.7 . . ?
C3 C20 H20B 108.7 . . ?
H20A C20 H20B 107.6 . . ?
C24 C23 H23 119.8 . . ?
C24 C23 C22 120.3(6) . . ?
C22 C23 H23 119.8 . . ?
N11 C12 C13 120.4(6) . . ?
N11 C12 H12 119.8 . . ?
C13 C12 H12 119.8 . . ?
N21 C22 C23 120.3(7) . . ?
N21 C22 H22 119.8 . . ?
C23 C22 H22 119.8 . . ?
C1 C2 C7 118.6(6) . . ?
C3 C2 C1 119.8(6) . . ?
C3 C2 C7 121.5(6) . . ?
C24 C25 H25 120.3 . . ?
C24 C25 C26 119.5(7) . . ?
C26 C25 H25 120.3 . . ?
N31 C32 C33 120.3(6) . . ?
N31 C32 H32 119.9 . . ?
C33 C32 H32 119.9 . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N11 C10 H10A 108.7 . . ?
N11 C10 H10B 108.7 . . ?
C1 C10 N11 114.4(5) . . ?
C1 C10 H10A 108.7 . . ?
C1 C10 H10B 108.7 . . ?
H10A C10 H10B 107.6 . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N21 C26 C25 121.0(6) . . ?
N21 C26 H26 119.5 . . ?
C25 C26 H26 119.5 . . ?
F7A C5A S1A 112.6(6) . . ?
F7A C5A F6A 109.4(7) . . ?
F6A C5A S1A 109.8(7) . . ?
F8A C5A S1A 112.3(6) . . ?
F8A C5A F7A 108.5(8) . . ?
F8A C5A F6A 103.8(7) . . ?
C17 O19 La1 133.7(4) . . ?
C17 O18 La1 177.0(4) . 2_577 ?
C37 O38 La1 142.9(4) . 2_566 ?
C37 O39 La1 130.9(4) . 1_444 ?
O19 C17 C14 116.5(5) . . ?
O18 C17 C14 117.8(5) . . ?
O18 C17 O19 125.7(5) . . ?
C35 C34 C33 119.3(5) . . ?
C35 C34 C37 121.1(6) . . ?
C33 C34 C37 119.6(5) . . ?
O38 C37 O39 126.5(5) . . ?
O38 C37 C34 114.9(6) . . ?
O39 C37 C34 118.6(5) . . ?
La1 O2W H2WA 109.4 . . ?
La1 O2W H2WB 109.4 . . ?
H2WA O2W H2WB 104.5 . . ?
La1 O1W H1WA 111.2 . . ?
La1 O1W H1WB 110.5 . . ?
H1WA O1W H1WB 103.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
La1 O29 C27 O28 -1.2(7) 1_454 . . . ?
La1 O29 C27 C24 176.9(4) 1_454 . . . ?
La1 O28 C27 La1 -162.7(18) 2_576 . . 1_454 ?
La1 O28 C27 O29 1.0(6) 1_454 . . . ?
La1 O28 C27 O29 -161.6(14) 2_576 . . . ?
La1 O28 C27 C24 20(2) 2_576 . . . ?
La1 O28 C27 C24 -177.1(5) 1_454 . . . ?
La1 O19 C17 C14 -178.8(4) . . . . ?
La1 O19 C17 O18 1.9(9) . . . . ?
La1 O38 C37 O39 -44.8(10) 2_566 . . . ?
La1 O38 C37 C34 133.8(5) 2_566 . . . ?
La1 O39 C37 O38 7.1(9) 1_444 . . . ?
La1 O39 C37 C34 -171.5(4) 1_444 . . . ?
O29 C27 C24 C23 -165.8(6) . . . . ?
O29 C27 C24 C25 14.1(9) . . . . ?
O28 C27 C24 C23 12.4(9) . . . . ?
O28 C27 C24 C25 -167.8(6) . . . . ?
O2A S1A C5A F7A -62.2(8) . . . . ?
O2A S1A C5A F6A 175.7(6) . . . . ?
O2A S1A C5A F8A 60.6(8) . . . . ?
C6 C1 C2 C3 3.6(9) . . . . ?
C6 C1 C2 C7 -176.1(6) . . . . ?
C6 C1 C10 N11 97.8(7) . . . . ?
C6 C5 C30 N31 99.6(7) . . . . ?
C6 C5 C4 C3 4.4(9) . . . . ?
C6 C5 C4 C8 -176.7(6) . . . . ?
C14 C15 C16 N11 1.6(9) . . . . ?
C14 C13 C12 N11 0.3(11) . . . . ?
C27 C24 C23 C22 179.4(6) . . . . ?
C27 C24 C25 C26 -180.0(6) . . . . ?
C1 C6 C5 C30 169.4(5) . . . . ?
C1 C6 C5 C4 -2.3(9) . . . . ?
C5 C6 C1 C2 -1.7(9) . . . . ?
C5 C6 C1 C10 178.6(5) . . . . ?
C15 C14 C13 C12 -0.4(10) . . . . ?
C15 C14 C17 O19 2.3(8) . . . . ?
C15 C14 C17 O18 -178.4(5) . . . . ?
O3A S1A C5A F7A 177.4(7) . . . . ?
O3A S1A C5A F6A 55.3(7) . . . . ?
O3A S1A C5A F8A -59.7(8) . . . . ?
C24 C23 C22 N21 0.0(11) . . . . ?
C24 C25 C26 N21 1.3(12) . . . . ?
C30 N31 C36 C35 -174.3(6) . . . . ?
C30 N31 C32 C33 175.8(6) . . . . ?
C30 C5 C4 C3 -167.6(5) . . . . ?
C30 C5 C4 C8 11.4(8) . . . . ?
C16 N11 C12 C13 0.8(10) . . . . ?
C16 N11 C10 C1 -21.5(9) . . . . ?
C35 C34 C37 O38 165.7(6) . . . . ?
C35 C34 C37 O39 -15.6(9) . . . . ?
C13 C14 C15 C16 -0.6(9) . . . . ?
C13 C14 C17 O19 -178.0(6) . . . . ?
C13 C14 C17 O18 1.3(8) . . . . ?
C36 N31 C30 C5 -35.3(8) . . . . ?
C36 N31 C32 C33 0.4(9) . . . . ?
C36 C35 C34 C33 -1.3(9) . . . . ?
C36 C35 C34 C37 178.0(6) . . . . ?
O4A S1A C5A F7A 54.2(8) . . . . ?
O4A S1A C5A F6A -67.9(7) . . . . ?
O4A S1A C5A F8A 177.1(7) . . . . ?
C4 C5 C30 N31 -88.5(7) . . . . ?
C4 C3 C20 N21 94.0(7) . . . . ?
C4 C3 C2 C1 -1.5(9) . . . . ?
C4 C3 C2 C7 178.2(6) . . . . ?
C33 C34 C37 O38 -15.1(8) . . . . ?
C33 C34 C37 O39 163.6(6) . . . . ?
C20 N21 C22 C23 -175.5(6) . . . . ?
C20 N21 C26 C25 174.7(7) . . . . ?
C20 C3 C4 C5 169.7(5) . . . . ?
C20 C3 C4 C8 -9.3(8) . . . . ?
C20 C3 C2 C1 -173.4(6) . . . . ?
C20 C3 C2 C7 6.3(10) . . . . ?
C23 C24 C25 C26 -0.1(11) . . . . ?
C12 N11 C16 C15 -1.8(10) . . . . ?
C12 N11 C10 C1 162.9(6) . . . . ?
C22 N21 C20 C3 -152.6(6) . . . . ?
C22 N21 C26 C25 -1.8(11) . . . . ?
C2 C1 C10 N11 -81.9(8) . . . . ?
C2 C3 C4 C5 -2.4(9) . . . . ?
C2 C3 C4 C8 178.6(6) . . . . ?
C2 C3 C20 N21 -93.9(7) . . . . ?
C25 C24 C23 C22 -0.5(10) . . . . ?
C32 N31 C30 C5 149.2(6) . . . . ?
C32 N31 C36 C35 1.0(9) . . . . ?
C32 C33 C34 C35 2.6(10) . . . . ?
C32 C33 C34 C37 -176.7(6) . . . . ?
C9 C6 C1 C2 177.1(6) . . . . ?
C9 C6 C1 C10 -2.6(9) . . . . ?
C9 C6 C5 C30 -9.4(9) . . . . ?
C9 C6 C5 C4 178.9(6) . . . . ?
C10 N11 C16 C15 -177.2(6) . . . . ?
C10 N11 C12 C13 176.4(6) . . . . ?
C10 C1 C2 C3 -176.7(6) . . . . ?
C10 C1 C2 C7 3.6(9) . . . . ?
C26 N21 C20 C3 30.8(9) . . . . ?
C26 N21 C22 C23 1.2(10) . . . . ?
C17 C14 C15 C16 179.2(5) . . . . ?
C17 C14 C13 C12 179.9(6) . . . . ?
C34 C35 C36 N31 -0.5(9) . . . . ?
C34 C33 C32 N31 -2.2(10) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.525 0.500 0.000 683.7 204.0 '20x water'

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.376
_oxdiff_exptl_absorpt_empirical_full_min 0.768
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_jj003_br_gd_otf_h2o_acet_red3
_database_code_depnum_ccdc_archive 'CCDC 1833429'
loop_
_audit_author_name
_audit_author_address
'Antti Tiihonen'
;University of Jyv?skyl?, Department of Chemistry
Finland
;
_audit_update_record             
;
2018-03-29 deposited with the CCDC.	2019-02-28 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_CHEMW03_I                   
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: The structure contains voids of unresolved electron density
which was treated using Olex2 solvent mask procedure (full details in 
_smtbx_masks_special_details). The 10 water molecules per asymmetric unit 
 are included in the formula and used in the calculations. 
;
_vrf_PLAT973_I                   
;
PROBLEM: Check Calcd Positive Resid. Density on       Gd1  
RESPONSE: Peak is located about 1 Angstrom from the metal atom and is caused by
the absorption effects. Data recorded with Cu-radiation. 
;
_vrf_PLAT420_I                   
;
PROBLEM: D-H Without Acceptor       O1W      --H1WB
RESPONSE: Hydrogen bond acceptor (water) have been removed among the other 
disordered solvents (also water) from the voids (see vrf_CHEMW03_I).
;
_vrf_FORMU01_I                   
;
PROBLEM: There is a discrepancy between the atom counts in the
            _chemical_formula_sum and _chemical_formula_moiety.
RESPONSE: See explanation above (CHEMW03_ALERT2_A).
;
_vrf_CELLZ01_I                   
;
PROBLEM: Difference between formula and atom_site contents detected.
RESPONSE: See explanation above (CHEMW03_ALERT2_A).
;
_vrf_PLAT041_I                   
;
PROBLEM: Calculated and Reported SumFormula strings Differ ...    
RESPONSE: See explanation above (CHEMW03_ALERT2_A).
;
_vrf_PLAT042_I                   
;
PROBLEM: Calculated and Reported Moiety formula strings Differ by ...
RESPONSE: See explanation above (CHEMW03_ALERT2_A).
;
_vrf_PLAT068_I                   
;
PROBLEM: Reported F000 Differs from Calcd (or Missing)...
RESPONSE: See explanation above (CHEMW03_ALERT2_A).
;
_vrf_PLAT606_I                   
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure
RESPONSE: See explanation above (CHEMW03_ALERT2_A).
;
# end Validation Reply Form
_audit_creation_date             2018-03-26
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H31 Gd N3 O8, 2(Br), C F3 O3 S'
_chemical_formula_sum            'C31 H51 Br2 F3 Gd N3 O21 S'
_chemical_formula_weight         1207.88
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C21 H25 O12 N3 F12 S3 Br1 Gd1'
_chemical_oxdiff_usercomment     'clear colorless block'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -8.8380 11.9157 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.5280(4)
_cell_length_b                   14.3123(6)
_cell_length_c                   18.8610(8)
_cell_angle_alpha                107.797(4)
_cell_angle_beta                 103.227(4)
_cell_angle_gamma                99.461(3)
_cell_volume                     2306.53(18)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7885
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      76.6790
_cell_measurement_theta_min      3.3350
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    12.555
_exptl_absorpt_correction_T_max  0.269
_exptl_absorpt_correction_T_min  0.061
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.739
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1206
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
4 6 -4 0.0516
-4 4 8 0.1341
0 -7 -4 0.0799
-3 9 -2 0.1159
6 -5 -2 0.1364
-1 -8 8 0.0734
-6 -1 7 0.1289
5 -3 3 0.1132
2 4 6 0.0771
0 2 -12 0.0624
1 -8 8 0.0709
0 8 -8 0.0582
-6 -1 3 0.1346
-1 -9 4 0.0794
0 9 -1 0.0661
0 3 9 0.0804
2 1 9 0.0777
4 -1 -10 0.1177
3 -9 3 0.0947

_exptl_crystal_size_max          0.283
_exptl_crystal_size_mid          0.164
_exptl_crystal_size_min          0.132
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
3.9995 6.0006 -4.0002 -0.6121 -0.7868 -0.1229
-4.0004 3.9998 8.0008 -0.5199 0.4196 0.7382
0.0006 -7.0003 -4.0005 0.8835 0.1996 -0.4334
-3.0004 9.0002 -1.9998 -0.2788 -0.4037 0.8994
6.0001 -4.9997 -2.0004 -0.0628 -0.2064 -1.0241
-0.9997 -8.0005 8.0004 0.1593 0.8951 -0.3475
-5.9999 -1.0006 7.0006 0.1797 0.7811 0.6717
4.9999 -2.9997 3.0001 -0.5036 -0.0137 -0.7722
1.9994 4.0003 6.0005 -0.9967 -0.0662 0.0172
0.0003 2.0002 -12.0008 0.7463 -0.6864 0.0942
1.0002 -8.0003 8.0003 -0.0503 0.7651 -0.5864
-0.0003 8.0004 -8.0003 -0.0545 -0.8301 0.4669
-5.9998 -1.0006 3.0003 0.4837 0.5895 0.6626
-0.9995 -9.0005 4.0000 0.5460 0.7594 -0.4172
-0.0000 9.0000 -1.0001 -0.6692 -0.5508 0.5433
-0.0000 3.0000 8.9999 -0.9323 0.2633 0.2021
2.0000 1.0000 8.9999 -0.9763 0.2451 -0.1580
4.0000 -1.0000 -10.0000 0.4235 -0.6829 -0.5608
3.0000 -9.0000 3.0001 0.2028 0.4516 -0.8970

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_unetI/netI     0.0508
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            14103
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.000
_diffrn_reflns_theta_min         2.577
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3953
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -70.00  31.00   1.00    1.00    --  -41.90  57.00 -30.00  101
  2  ω    -74.00  33.00   1.00    1.00    --  -41.90  77.00-180.00  107
  3  ω     52.00 103.00   1.00    1.00    --   41.90-138.00 117.00   51
  4  ω     61.00 141.00   1.00    2.00    --  112.00 -61.00 150.00   80
  5  ω     64.00 108.00   1.00    2.00    --  112.00 -94.00  60.00   44
  6  ω     51.00 136.00   1.00    2.00    --  112.00 -45.00  60.00   85
  7  ω     75.00 108.00   1.00    2.00    --  112.00 -94.00-120.00   33
  8  ω     65.00 115.00   1.00    2.00    --  112.00-111.00-180.00   50
  9  ω     41.00 132.00   1.00    2.00    --  112.00 -45.00 -30.00   91
 10  ω     29.00  55.00   1.00    2.00    --  112.00 -94.00-120.00   26
 11  ω     29.00 109.00   1.00    2.00    --  112.00 -94.00 -30.00   80
 12  ω     30.00 178.00   1.00    2.00    --  112.00   0.00 120.00  148
 13  ω    100.00 172.00   1.00    2.00    --  112.00 111.00 120.00   72
 14  ω   -113.00 -18.00   1.00    1.00    --  -41.90 -37.00  30.00   95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1048011000
_diffrn_orient_matrix_UB_12      -0.0828012000
_diffrn_orient_matrix_UB_13      -0.0759865000
_diffrn_orient_matrix_UB_21      -0.0649963000
_diffrn_orient_matrix_UB_22      -0.0558804000
_diffrn_orient_matrix_UB_23      0.0478813000
_diffrn_orient_matrix_UB_31      -0.1194279000
_diffrn_orient_matrix_UB_32      0.0606128000
_diffrn_orient_matrix_UB_33      0.0022511000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7753
_reflns_number_total             8343
_reflns_odcompleteness_completeness 99.32
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         2.858
_refine_diff_density_min         -1.928
_refine_diff_density_rms         0.206
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     484
_refine_ls_number_reflns         8343
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0686
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1298P)²+11.1175P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1930
_refine_ls_wR_factor_ref         0.1984
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Others
 Sof(Br2B)=1-FVAR(1)
 Sof(Br2A)=FVAR(1)
3.a Rotating group:
 O2W(H2WA,H2WB), O1W(H1WA,H1WB)
3.b Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C10(H10A,H10B), C30(H30A,H30B)
3.c Aromatic/amide H refined with riding coordinates:
 C16(H16), C23(H23), C32(H32), C25(H25), C22(H22), C15(H15), C12(H12),
 C13(H13), C33(H33), C36(H36), C26(H26), C35(H35)
3.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C7(H7A,H7B,H7C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd 0.73021(4) 0.51380(3) -0.00513(2) 0.01991(15) Uani 1 1 d . . . . .
Br1 Br 1.23644(14) 0.41713(10) 0.31308(7) 0.0606(3) Uani 1 1 d . . . . .
Br2A Br 1.28275(15) 0.91504(12) 0.29314(9) 0.0517(5) Uani 0.739(4) 1 d . . P A
2
S40 S 0.8026(2) 0.76522(16) 0.40202(12) 0.0340(4) Uani 1 1 d . . . . .
O18 O 0.9275(6) 0.5852(4) 0.1147(3) 0.0286(11) Uani 1 1 d . . . . .
O28 O 1.5503(5) 1.3602(4) 0.9043(3) 0.0243(10) Uani 1 1 d . . . . .
O29 O 1.3412(6) 1.3410(4) 0.9400(3) 0.0261(10) Uani 1 1 d . . . . .
O19 O 1.1291(5) 0.5416(4) 0.0882(3) 0.0273(11) Uani 1 1 d . . . . .
F46 F 0.6673(8) 0.5955(5) 0.4159(5) 0.075(2) Uani 1 1 d . . . . .
O41 O 0.6908(8) 0.8090(5) 0.4254(5) 0.0542(18) Uani 1 1 d . . . . .
F47 F 0.9035(8) 0.6129(5) 0.4270(4) 0.0663(17) Uani 1 1 d . . . . .
C20 C 1.1176(9) 0.9691(6) 0.6157(4) 0.0322(17) Uani 1 1 d . . . . .
H20A H 1.015227 0.944918 0.617205 0.039 Uiso 1 1 calc R . . . .
H20B H 1.109760 0.995894 0.572774 0.039 Uiso 1 1 calc R . . . .
O42 O 0.9465(8) 0.8240(5) 0.4311(4) 0.0506(16) Uani 1 1 d . . . . .
N21 N 1.2026(7) 1.0555(5) 0.6920(3) 0.0260(13) Uani 1 1 d . . . . .
N11 N 1.2994(7) 0.7085(5) 0.3751(3) 0.0249(12) Uani 1 1 d . . . . .
C24 C 1.3444(8) 1.2220(5) 0.8238(4) 0.0219(13) Uani 1 1 d . . . . .
O43 O 0.7517(11) 0.7019(7) 0.3183(5) 0.068(2) Uani 1 1 d . . . . .
F45 F 0.8334(9) 0.6997(6) 0.5202(4) 0.075(2) Uani 1 1 d . . . . .
C16 C 1.1570(9) 0.7064(6) 0.3527(4) 0.0319(17) Uani 1 1 d . . . . .
H16 H 1.109886 0.734316 0.390584 0.038 Uiso 1 1 calc R . . . .
C23 C 1.4262(8) 1.1704(6) 0.7813(4) 0.0272(15) Uani 1 1 d . . . . .
H23 H 1.531784 1.192812 0.797016 0.033 Uiso 1 1 calc R . . . .
C5 C 1.1847(8) 0.8801(5) 0.5971(4) 0.0247(14) Uani 1 1 d . . . . .
N31 N 1.2159(7) 0.6151(5) 0.6929(4) 0.0283(13) Uani 1 1 d . . . . .
C17 C 1.0616(8) 0.5803(5) 0.1334(4) 0.0223(14) Uani 1 1 d . . . . .
C6 C 1.2656(9) 0.8659(6) 0.5429(4) 0.0287(15) Uani 1 1 d . . . . .
C32 C 1.1473(9) 0.5798(8) 0.7378(5) 0.040(2) Uani 1 1 d . . . . .
H32 H 1.042158 0.567582 0.726729 0.048 Uiso 1 1 calc R . . . .
C25 C 1.1906(9) 1.1888(6) 0.7993(5) 0.0318(16) Uani 1 1 d . . . . .
H25 H 1.133698 1.223126 0.828718 0.038 Uiso 1 1 calc R . . . .
C3 C 1.1840(9) 0.7121(6) 0.5994(4) 0.0282(15) Uani 1 1 d . . . . .
C1 C 1.3024(8) 0.7717(6) 0.5160(4) 0.0281(15) Uani 1 1 d . . . . .
C22 C 1.3508(8) 1.0848(5) 0.7149(4) 0.0257(14) Uani 1 1 d . . . . .
H22 H 1.405466 1.047204 0.685855 0.031 Uiso 1 1 calc R . . . .
C2 C 1.2587(9) 0.6941(6) 0.5427(4) 0.0319(16) Uani 1 1 d . . . . .
C27 C 1.4204(8) 1.3166(5) 0.8957(4) 0.0243(14) Uani 1 1 d . . . . .
C15 C 1.0753(8) 0.6641(6) 0.2747(4) 0.0277(15) Uani 1 1 d . . . . .
H15 H 0.972052 0.661110 0.258852 0.033 Uiso 1 1 calc R . . . .
C14 C 1.1464(8) 0.6261(5) 0.2200(4) 0.0204(13) Uani 1 1 d . . . . .
C44 C 0.7988(10) 0.6552(10) 0.4331(10) 0.080(5) Uani 1 1 d . . . . .
C8 C 1.0737(9) 0.8258(7) 0.6920(4) 0.0343(17) Uani 1 1 d . . . . .
H8A H 1.113294 0.896761 0.726946 0.052 Uiso 1 1 calc GR . . . .
H8B H 1.092638 0.781359 0.721714 0.052 Uiso 1 1 calc GR . . . .
H8C H 0.966167 0.812534 0.668331 0.052 Uiso 1 1 calc GR . . . .
C4 C 1.1495(8) 0.8051(6) 0.6285(4) 0.0267(15) Uani 1 1 d . . . . .
C10 C 1.3942(9) 0.7561(7) 0.4599(4) 0.0355(18) Uani 1 1 d . . . . .
H10A H 1.459157 0.711945 0.471338 0.043 Uiso 1 1 calc R . . . .
H10B H 1.459159 0.822393 0.468222 0.043 Uiso 1 1 calc R . . . .
C12 C 1.3698(9) 0.6710(7) 0.3226(4) 0.0339(17) Uani 1 1 d . . . . .
H12 H 1.472327 0.672715 0.339782 0.041 Uiso 1 1 calc R . . . .
C13 C 1.2952(9) 0.6307(6) 0.2453(5) 0.0326(17) Uani 1 1 d . . . . .
H13 H 1.346121 0.605601 0.208555 0.039 Uiso 1 1 calc R . . . .
C33 C 1.2296(9) 0.5615(7) 0.7994(5) 0.0386(19) Uani 1 1 d . . . . .
H33 H 1.180865 0.537821 0.831606 0.046 Uiso 1 1 calc R . . . .
C36 C 1.3630(10) 0.6339(8) 0.7074(5) 0.042(2) Uani 1 1 d . . . . .
H36 H 1.409508 0.661015 0.675938 0.050 Uiso 1 1 calc R . . . .
C26 C 1.1197(8) 1.1051(6) 0.7315(5) 0.0302(16) Uani 1 1 d . . . . .
H26 H 1.014054 1.083206 0.713135 0.036 Uiso 1 1 calc R . . . .
C30 C 1.1171(9) 0.6262(6) 0.6224(5) 0.0348(18) Uani 1 1 d . . . . .
H30A H 1.022673 0.636896 0.632896 0.042 Uiso 1 1 calc R . . . .
H30B H 1.092343 0.561820 0.577554 0.042 Uiso 1 1 calc R . . . .
C9 C 1.3053(12) 0.9465(7) 0.5108(5) 0.045(2) Uani 1 1 d . . . . .
H9A H 1.357230 0.922644 0.472128 0.067 Uiso 1 1 calc GR . . . .
H9B H 1.370497 1.007855 0.553169 0.067 Uiso 1 1 calc GR . . . .
H9C H 1.214324 0.961900 0.485887 0.067 Uiso 1 1 calc GR . . . .
C7 C 1.2915(13) 0.5930(7) 0.5106(6) 0.048(2) Uani 1 1 d . . . . .
H7A H 1.254004 0.547849 0.535700 0.073 Uiso 1 1 calc GR . . . .
H7B H 1.399432 0.602199 0.520814 0.073 Uiso 1 1 calc GR . . . .
H7C H 1.242616 0.563149 0.454180 0.073 Uiso 1 1 calc GR . . . .
C35 C 1.4481(9) 0.6138(8) 0.7683(5) 0.0381(19) Uani 1 1 d . . . . .
H35 H 1.552980 0.625425 0.777858 0.046 Uiso 1 1 calc R . . . .
O38 O 1.4039(6) 0.5283(4) 0.9245(3) 0.0258(10) Uani 1 1 d . . . . .
O39 O 1.6075(6) 0.5589(4) 0.8876(3) 0.0278(11) Uani 1 1 d . . . . .
O2W O 0.8968(6) 0.6629(4) -0.0090(3) 0.0347(12) Uani 1 1 d . . . . .
H2WA H 0.925238 0.716777 0.037060 0.052 Uiso 1 1 d GR . . . .
H2WB H 0.852989 0.685487 -0.046950 0.052 Uiso 1 1 d GR . . . .
O1W O 0.8116(7) 0.3716(5) 0.0207(4) 0.0412(14) Uani 1 1 d . . . . .
H1WA H 0.737245 0.313488 -0.000588 0.062 Uiso 1 1 d GR . . . .
H1WB H 0.844543 0.383318 0.072633 0.062 Uiso 1 1 d GR . . . .
C34 C 1.3806(8) 0.5766(5) 0.8154(4) 0.0260(14) Uani 1 1 d . . . . .
C37 C 1.4713(8) 0.5522(5) 0.8803(4) 0.0249(14) Uani 1 1 d . . . . .
Br2B Br 1.1519(6) 0.8494(5) 0.1377(4) 0.0779(18) Uani 0.261(4) 1 d . . P A 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 O18 2.387(5) . ?
Gd1 O28 2.411(5) 1_444 ?
Gd1 O29 2.362(5) 2_776 ?
Gd1 O19 2.331(5) 2_765 ?
Gd1 O38 2.347(5) 2_766 ?
Gd1 O39 2.416(5) 1_454 ?
Gd1 O2W 2.472(6) . ?
Gd1 O1W 2.436(6) . ?
S40 O41 1.409(7) . ?
S40 O42 1.372(8) . ?
S40 O43 1.476(8) . ?
S40 C44 1.838(10) . ?
O18 C17 1.265(9) . ?
O28 C27 1.241(9) . ?
O29 C27 1.259(9) . ?
O19 C17 1.235(9) . ?
F46 C44 1.303(12) . ?
F47 C44 1.260(13) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 N21 1.518(9) . ?
C20 C5 1.500(11) . ?
N21 C22 1.331(10) . ?
N21 C26 1.346(10) . ?
N11 C16 1.318(10) . ?
N11 C10 1.520(9) . ?
N11 C12 1.348(10) . ?
C24 C23 1.382(10) . ?
C24 C25 1.383(10) . ?
C24 C27 1.517(9) . ?
F45 C44 1.501(19) . ?
C16 H16 0.9500 . ?
C16 C15 1.384(10) . ?
C23 H23 0.9500 . ?
C23 C22 1.396(10) . ?
C5 C6 1.402(11) . ?
C5 C4 1.407(11) . ?
N31 C32 1.343(11) . ?
N31 C36 1.329(11) . ?
N31 C30 1.513(9) . ?
C17 C14 1.522(9) . ?
C6 C1 1.420(11) . ?
C6 C9 1.494(11) . ?
C32 H32 0.9500 . ?
C32 C33 1.368(11) . ?
C25 H25 0.9500 . ?
C25 C26 1.389(11) . ?
C3 C2 1.400(12) . ?
C3 C4 1.401(11) . ?
C3 C30 1.516(11) . ?
C1 C2 1.396(12) . ?
C1 C10 1.508(11) . ?
C22 H22 0.9500 . ?
C2 C7 1.502(11) . ?
C15 H15 0.9500 . ?
C15 C14 1.385(10) . ?
C14 C13 1.372(10) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C8 C4 1.513(10) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C12 H12 0.9500 . ?
C12 C13 1.356(11) . ?
C13 H13 0.9500 . ?
C33 H33 0.9500 . ?
C33 C34 1.366(11) . ?
C36 H36 0.9500 . ?
C36 C35 1.383(11) . ?
C26 H26 0.9500 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C35 H35 0.9500 . ?
C35 C34 1.388(11) . ?
O38 C37 1.252(9) . ?
O39 C37 1.258(9) . ?
O2W H2WA 0.9154 . ?
O2W H2WB 0.9164 . ?
O1W H1WA 0.9093 . ?
O1W H1WB 0.9097 . ?
C34 C37 1.498(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O18 Gd1 O28 144.53(18) . 1_444 ?
O18 Gd1 O39 140.52(19) . 1_454 ?
O18 Gd1 O2W 71.92(19) . . ?
O18 Gd1 O1W 73.8(2) . . ?
O28 Gd1 O39 74.82(18) 1_444 1_454 ?
O28 Gd1 O2W 138.37(18) 1_444 . ?
O28 Gd1 O1W 72.4(2) 1_444 . ?
O29 Gd1 O18 78.79(18) 2_776 . ?
O29 Gd1 O28 122.19(17) 2_776 1_444 ?
O29 Gd1 O39 78.05(18) 2_776 1_454 ?
O29 Gd1 O2W 72.57(19) 2_776 . ?
O29 Gd1 O1W 138.96(19) 2_776 . ?
O19 Gd1 O18 98.19(17) 2_765 . ?
O19 Gd1 O28 81.57(17) 2_765 1_444 ?
O19 Gd1 O29 142.38(19) 2_765 2_776 ?
O19 Gd1 O38 145.30(19) 2_765 2_766 ?
O19 Gd1 O39 81.69(18) 2_765 1_454 ?
O19 Gd1 O2W 70.94(19) 2_765 . ?
O19 Gd1 O1W 72.4(2) 2_765 . ?
O38 Gd1 O18 82.13(18) 2_766 . ?
O38 Gd1 O28 78.87(18) 2_766 1_444 ?
O38 Gd1 O29 72.01(18) 2_766 2_776 ?
O38 Gd1 O39 119.68(17) 2_766 1_454 ?
O38 Gd1 O2W 139.31(18) 2_766 . ?
O38 Gd1 O1W 74.44(19) 2_766 . ?
O39 Gd1 O2W 70.84(19) 1_454 . ?
O39 Gd1 O1W 140.5(2) 1_454 . ?
O1W Gd1 O2W 124.6(2) . . ?
O41 S40 O43 111.6(5) . . ?
O41 S40 C44 106.0(5) . . ?
O42 S40 O41 118.0(4) . . ?
O42 S40 O43 116.6(5) . . ?
O42 S40 C44 107.5(4) . . ?
O43 S40 C44 93.3(7) . . ?
C17 O18 Gd1 133.1(4) . . ?
C27 O28 Gd1 136.4(4) . 1_666 ?
C27 O29 Gd1 139.0(5) . 2_776 ?
C17 O19 Gd1 173.9(5) . 2_765 ?
H20A C20 H20B 107.5 . . ?
N21 C20 H20A 108.4 . . ?
N21 C20 H20B 108.4 . . ?
C5 C20 H20A 108.4 . . ?
C5 C20 H20B 108.4 . . ?
C5 C20 N21 115.3(6) . . ?
C22 N21 C20 121.2(6) . . ?
C22 N21 C26 122.3(6) . . ?
C26 N21 C20 116.3(6) . . ?
C16 N11 C10 122.5(6) . . ?
C16 N11 C12 121.0(6) . . ?
C12 N11 C10 116.5(6) . . ?
C23 C24 C25 119.6(7) . . ?
C23 C24 C27 121.0(6) . . ?
C25 C24 C27 119.4(6) . . ?
N11 C16 H16 119.6 . . ?
N11 C16 C15 120.7(7) . . ?
C15 C16 H16 119.6 . . ?
C24 C23 H23 120.6 . . ?
C24 C23 C22 118.8(7) . . ?
C22 C23 H23 120.6 . . ?
C6 C5 C20 121.1(7) . . ?
C6 C5 C4 120.6(7) . . ?
C4 C5 C20 117.9(7) . . ?
C32 N31 C30 116.7(7) . . ?
C36 N31 C32 121.6(7) . . ?
C36 N31 C30 121.6(7) . . ?
O18 C17 C14 116.4(6) . . ?
O19 C17 O18 126.1(6) . . ?
O19 C17 C14 117.5(6) . . ?
C5 C6 C1 119.0(7) . . ?
C5 C6 C9 120.4(7) . . ?
C1 C6 C9 120.4(7) . . ?
N31 C32 H32 120.2 . . ?
N31 C32 C33 119.7(8) . . ?
C33 C32 H32 120.2 . . ?
C24 C25 H25 120.1 . . ?
C24 C25 C26 119.8(7) . . ?
C26 C25 H25 120.1 . . ?
C2 C3 C4 121.5(7) . . ?
C2 C3 C30 120.5(7) . . ?
C4 C3 C30 117.3(7) . . ?
C6 C1 C10 119.9(7) . . ?
C2 C1 C6 120.7(7) . . ?
C2 C1 C10 119.3(7) . . ?
N21 C22 C23 120.3(7) . . ?
N21 C22 H22 119.9 . . ?
C23 C22 H22 119.9 . . ?
C3 C2 C7 120.9(8) . . ?
C1 C2 C3 118.9(7) . . ?
C1 C2 C7 120.1(8) . . ?
O28 C27 O29 127.8(6) . . ?
O28 C27 C24 117.7(6) . . ?
O29 C27 C24 114.5(6) . . ?
C16 C15 H15 120.5 . . ?
C16 C15 C14 118.9(7) . . ?
C14 C15 H15 120.5 . . ?
C15 C14 C17 120.8(6) . . ?
C13 C14 C17 120.5(6) . . ?
C13 C14 C15 118.7(6) . . ?
F46 C44 S40 115.6(7) . . ?
F46 C44 F45 99.6(11) . . ?
F47 C44 S40 116.2(8) . . ?
F47 C44 F46 116.3(11) . . ?
F47 C44 F45 100.9(9) . . ?
F45 C44 S40 104.4(9) . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C4 C8 H8A 109.5 . . ?
C4 C8 H8B 109.5 . . ?
C4 C8 H8C 109.5 . . ?
C5 C4 C8 119.6(7) . . ?
C3 C4 C5 118.9(7) . . ?
C3 C4 C8 121.4(7) . . ?
N11 C10 H10A 109.0 . . ?
N11 C10 H10B 109.0 . . ?
C1 C10 N11 112.9(6) . . ?
C1 C10 H10A 109.0 . . ?
C1 C10 H10B 109.0 . . ?
H10A C10 H10B 107.8 . . ?
N11 C12 H12 119.8 . . ?
N11 C12 C13 120.5(7) . . ?
C13 C12 H12 119.8 . . ?
C14 C13 H13 119.9 . . ?
C12 C13 C14 120.2(7) . . ?
C12 C13 H13 119.9 . . ?
C32 C33 H33 119.4 . . ?
C34 C33 C32 121.2(8) . . ?
C34 C33 H33 119.4 . . ?
N31 C36 H36 120.1 . . ?
N31 C36 C35 119.8(8) . . ?
C35 C36 H36 120.1 . . ?
N21 C26 C25 119.2(7) . . ?
N21 C26 H26 120.4 . . ?
C25 C26 H26 120.4 . . ?
N31 C30 C3 114.9(6) . . ?
N31 C30 H30A 108.5 . . ?
N31 C30 H30B 108.5 . . ?
C3 C30 H30A 108.5 . . ?
C3 C30 H30B 108.5 . . ?
H30A C30 H30B 107.5 . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C36 C35 H35 119.9 . . ?
C36 C35 C34 120.1(8) . . ?
C34 C35 H35 119.9 . . ?
C37 O38 Gd1 177.6(5) . 2_766 ?
C37 O39 Gd1 112.9(4) . 1_656 ?
Gd1 O2W H2WA 112.2 . . ?
Gd1 O2W H2WB 112.6 . . ?
H2WA O2W H2WB 106.4 . . ?
Gd1 O1W H1WA 112.3 . . ?
Gd1 O1W H1WB 112.2 . . ?
H1WA O1W H1WB 106.5 . . ?
C33 C34 C35 117.7(7) . . ?
C33 C34 C37 121.8(7) . . ?
C35 C34 C37 120.5(7) . . ?
O38 C37 O39 125.1(7) . . ?
O38 C37 C34 116.2(6) . . ?
O39 C37 C34 118.7(7) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Gd1 O18 C17 O19 7.7(12) . . . . ?
Gd1 O18 C17 C14 -172.0(4) . . . . ?
Gd1 O28 C27 O29 -5.0(12) 1_666 . . . ?
Gd1 O28 C27 C24 175.0(4) 1_666 . . . ?
Gd1 O29 C27 O28 48.9(11) 2_776 . . . ?
Gd1 O29 C27 C24 -131.1(6) 2_776 . . . ?
Gd1 O39 C37 O38 2.3(9) 1_656 . . . ?
Gd1 O39 C37 C34 -179.2(5) 1_656 . . . ?
O18 C17 C14 C15 4.4(10) . . . . ?
O18 C17 C14 C13 -175.4(7) . . . . ?
O19 C17 C14 C15 -175.2(7) . . . . ?
O19 C17 C14 C13 4.9(11) . . . . ?
O41 S40 C44 F46 47.4(15) . . . . ?
O41 S40 C44 F47 -171.0(11) . . . . ?
O41 S40 C44 F45 -60.9(7) . . . . ?
C20 N21 C22 C23 173.8(7) . . . . ?
C20 N21 C26 C25 -176.1(7) . . . . ?
C20 C5 C6 C1 -168.0(6) . . . . ?
C20 C5 C6 C9 8.7(11) . . . . ?
C20 C5 C4 C3 166.7(6) . . . . ?
C20 C5 C4 C8 -12.5(10) . . . . ?
O42 S40 C44 F46 174.5(12) . . . . ?
O42 S40 C44 F47 -43.9(14) . . . . ?
O42 S40 C44 F45 66.2(7) . . . . ?
N21 C20 C5 C6 -102.1(8) . . . . ?
N21 C20 C5 C4 85.2(9) . . . . ?
N11 C16 C15 C14 -1.7(13) . . . . ?
N11 C12 C13 C14 -1.2(14) . . . . ?
C24 C23 C22 N21 1.9(11) . . . . ?
C24 C25 C26 N21 2.2(12) . . . . ?
O43 S40 C44 F46 -66.2(14) . . . . ?
O43 S40 C44 F47 75.4(13) . . . . ?
O43 S40 C44 F45 -174.5(7) . . . . ?
C16 N11 C10 C1 16.9(11) . . . . ?
C16 N11 C12 C13 0.4(13) . . . . ?
C16 C15 C14 C17 -179.1(7) . . . . ?
C16 C15 C14 C13 0.8(12) . . . . ?
C23 C24 C25 C26 -1.2(12) . . . . ?
C23 C24 C27 O28 17.5(10) . . . . ?
C23 C24 C27 O29 -162.5(7) . . . . ?
C5 C20 N21 C22 40.4(10) . . . . ?
C5 C20 N21 C26 -144.6(7) . . . . ?
C5 C6 C1 C2 0.1(11) . . . . ?
C5 C6 C1 C10 -177.8(7) . . . . ?
N31 C32 C33 C34 -1.3(15) . . . . ?
N31 C36 C35 C34 -1.7(15) . . . . ?
C17 C14 C13 C12 -179.5(8) . . . . ?
C6 C5 C4 C3 -6.0(10) . . . . ?
C6 C5 C4 C8 174.8(7) . . . . ?
C6 C1 C2 C3 -3.0(11) . . . . ?
C6 C1 C2 C7 176.8(8) . . . . ?
C6 C1 C10 N11 -93.1(9) . . . . ?
C32 N31 C36 C35 2.2(14) . . . . ?
C32 N31 C30 C3 148.4(8) . . . . ?
C32 C33 C34 C35 1.7(14) . . . . ?
C32 C33 C34 C37 -177.0(9) . . . . ?
C25 C24 C23 C22 -0.9(11) . . . . ?
C25 C24 C27 O28 -160.6(7) . . . . ?
C25 C24 C27 O29 19.4(10) . . . . ?
C22 N21 C26 C25 -1.2(12) . . . . ?
C2 C3 C4 C5 3.1(11) . . . . ?
C2 C3 C4 C8 -177.7(7) . . . . ?
C2 C3 C30 N31 94.7(9) . . . . ?
C2 C1 C10 N11 88.9(9) . . . . ?
C27 C24 C23 C22 -179.0(7) . . . . ?
C27 C24 C25 C26 177.0(7) . . . . ?
C15 C14 C13 C12 0.6(12) . . . . ?
C4 C5 C6 C1 4.4(10) . . . . ?
C4 C5 C6 C9 -178.9(7) . . . . ?
C4 C3 C2 C1 1.4(11) . . . . ?
C4 C3 C2 C7 -178.4(8) . . . . ?
C4 C3 C30 N31 -94.3(9) . . . . ?
C10 N11 C16 C15 178.7(8) . . . . ?
C10 N11 C12 C13 -177.4(8) . . . . ?
C10 C1 C2 C3 174.9(7) . . . . ?
C10 C1 C2 C7 -5.3(11) . . . . ?
C12 N11 C16 C15 1.1(13) . . . . ?
C12 N11 C10 C1 -165.4(7) . . . . ?
C33 C34 C37 O38 -7.9(11) . . . . ?
C33 C34 C37 O39 173.5(8) . . . . ?
C36 N31 C32 C33 -0.7(14) . . . . ?
C36 N31 C30 C3 -35.3(12) . . . . ?
C36 C35 C34 C33 -0.2(14) . . . . ?
C36 C35 C34 C37 178.5(8) . . . . ?
C26 N21 C22 C23 -0.8(11) . . . . ?
C30 N31 C32 C33 175.6(9) . . . . ?
C30 N31 C36 C35 -174.0(9) . . . . ?
C30 C3 C2 C1 172.0(7) . . . . ?
C30 C3 C2 C7 -7.8(11) . . . . ?
C30 C3 C4 C5 -167.8(6) . . . . ?
C30 C3 C4 C8 11.4(10) . . . . ?
C9 C6 C1 C2 -176.6(8) . . . . ?
C9 C6 C1 C10 5.5(11) . . . . ?
C35 C34 C37 O38 173.4(8) . . . . ?
C35 C34 C37 O39 -5.2(11) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.631 0.000 0.000 606.1 201.5 '20x water'

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.708
_oxdiff_exptl_absorpt_empirical_full_min 0.600
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_jj003_br_tb_otf_h2o_acet_red3
_database_code_depnum_ccdc_archive 'CCDC 1833438'
loop_
_audit_author_name
_audit_author_address
'Antti Tiihonen'
;University of Jyv?skyl?, Department of Chemistry
Finland
;
_audit_update_record             
;
2018-03-29 deposited with the CCDC.	2019-02-28 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_CHEMW03_I                   
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: The structure contains voids of unresolved electron density
which was treated using Olex2 solvent mask procedure (full details in 
_smtbx_masks_special_details). The 9 water molecules per asymmetric unit 
 are included in the formula and used in the calculations. 
;
_vrf_PLAT420_I                   
;
PROBLEM: D-H Without Acceptor       O       --H 
RESPONSE: Hydrogen bond acceptors (water located in a void) have been removed 
among the other disordered solvents (also water) in the voids 
(see vrf_CHEMW03_ALERT_2_A).
;
_vrf_FORMU01_I                   
;
PROBLEM: There is a discrepancy between the atom counts in the
            _chemical_formula_sum and _chemical_formula_moiety.
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_CELLZ01_I                   
;
PROBLEM: Difference between formula and atom_site contents detected.
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT041_I                   
;
PROBLEM: Calculated and Reported SumFormula strings Differ ...    
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT042_I                   
;
PROBLEM: Calculated and Reported Moiety formula strings Differ by ...
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT068_I                   
;
PROBLEM: Reported F000 Differs from Calcd (or Missing)...
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT606_I                   
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
# end Validation Reply Form

_audit_creation_date             2018-03-26
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H31 N3 O8 Tb, 2(Br), C F3 O3 S'
_chemical_formula_sum            'C31 H49 Br2 F3 N3 O20 S Tb'
_chemical_formula_weight         1191.53
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C21 H25 O12 N3 F12 S3 Br1 Tb1'
_chemical_oxdiff_usercomment     'clear colorless block'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -9.1472 9.1891 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.5114(4)
_cell_length_b                   14.2612(6)
_cell_length_c                   18.8972(6)
_cell_angle_alpha                108.079(4)
_cell_angle_beta                 103.298(3)
_cell_angle_gamma                99.250(4)
_cell_volume                     2295.55(17)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7780
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      76.3710
_cell_measurement_theta_min      3.3660
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    10.819
_exptl_absorpt_correction_T_max  0.790
_exptl_absorpt_correction_T_min  0.566
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.724
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1188
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -8 10 0.0239
0 8 -10 0.0239
0 -4 -8 0.0353
0 4 8 0.0353
-6 1 5 0.0682
6 -1 -5 0.0413

_exptl_crystal_size_max          0.127
_exptl_crystal_size_mid          0.076
_exptl_crystal_size_min          0.048
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.0105 -8.0023 9.9911 0.8691 0.4699 -0.3202
-0.0105 8.0023 -9.9911 -0.8691 -0.4699 0.3202
-0.0054 -3.9954 -8.0022 -0.3247 -0.2547 -0.9006
0.0054 3.9954 8.0022 0.3247 0.2547 0.9006
-5.9986 0.9967 5.0081 0.6266 -0.7530 0.1445
5.9986 -0.9967 -5.0081 -0.6266 0.7530 -0.1445

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13793
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.995
_diffrn_reflns_theta_min         3.368
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3953
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -73.00  26.00   1.00    3.00    --  -41.90  69.00 -80.00   99
  2  ω      1.00  83.00   1.00    3.00    --   41.90 -99.00  30.00   82
  3  ω     44.00 140.00   1.00    6.00    --  112.00 -30.00  90.00   96
  4  ω     53.00 116.00   1.00    6.00    --  112.00-111.00  60.00   63
  5  ω     51.00 140.00   1.00    6.00    --  112.00 -30.00 -60.00   89
  6  ω     87.00 115.00   1.00    6.00    --  112.00-111.00-150.00   28
  7  ω     46.00 140.00   1.00    6.00    --  112.00 -30.00-150.00   94
  8  ω    100.00 155.00   1.00    6.00    --  112.00 111.00-120.00   55
  9  ω    101.00 132.00   1.00    6.00    --  112.00 111.00 -90.00   31
 10  ω    106.00 140.00   1.00    6.00    --  112.00 111.00  30.00   34
 11  ω     38.00 140.00   1.00    6.00    --  112.00 -77.00  90.00  102
 12  ω     36.00 135.00   1.00    6.00    --  112.00 -77.00-120.00   99
 13  ω   -115.00 -31.00   1.00    3.00    --  -41.90 -57.00 150.00   84
 14  ω   -115.00 -18.00   1.00    3.00    --  -41.90 -37.00  30.00   97
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0616006000
_diffrn_orient_matrix_UB_12      -0.0357110000
_diffrn_orient_matrix_UB_13      0.0584456000
_diffrn_orient_matrix_UB_21      0.1549335000
_diffrn_orient_matrix_UB_22      -0.0116432000
_diffrn_orient_matrix_UB_23      0.0375438000
_diffrn_orient_matrix_UB_31      0.0419721000
_diffrn_orient_matrix_UB_32      0.1112195000
_diffrn_orient_matrix_UB_33      0.0569855000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7799
_reflns_number_total             8301
_reflns_odcompleteness_completeness 99.33
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         3.157
_refine_diff_density_min         -2.302
_refine_diff_density_rms         0.187
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     484
_refine_ls_number_reflns         8301
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_gt           0.0688
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0836P)²+32.1568P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1859
_refine_ls_wR_factor_ref         0.1887
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N11) \\sim Ueq, Uanis(C10) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
3. Others
 Sof(Br2B)=1-FVAR(1)
 Sof(Br2A)=FVAR(1)
4.a Rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
4.b Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C30(H30A,H30B), C10(H10A,H10B)
4.c Aromatic/amide H refined with riding coordinates:
 C25(H25), C15(H15), C16(H16), C13(H13), C35(H35), C32(H32), C26(H26),
 C23(H23), C33(H33), C22(H22), C12(H12), C36(H36)
4.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.23112(4) 1.01383(3) 0.49505(2) 0.01625(15) Uani 1 1 d . . . . .
Br1 Br 0.73788(14) 0.91405(11) -0.18594(7) 0.0592(3) Uani 1 1 d . . . . .
Br2A Br 0.78086(17) 1.41619(15) 0.79152(10) 0.0563(6) Uani 0.734(4) 1 d . . P A
2
S40 S -0.3024(2) 0.73611(17) 0.09799(12) 0.0292(4) Uani 1 1 d . . . B 1
O18 O 0.3715(5) 0.9593(4) 0.4122(3) 0.0213(11) Uani 1 1 d . . . . .
O43 O -0.1921(8) 0.6896(6) 0.0760(5) 0.053(2) Uani 1 1 d . . . B 1
O42 O -0.4486(8) 0.6760(5) 0.0691(4) 0.0426(16) Uani 1 1 d . . . B 1
F47 F -0.1672(8) 0.9023(6) 0.0823(5) 0.077(2) Uani 1 1 d . . . B 1
C37 C 0.0304(8) 0.9462(6) -0.3817(4) 0.0210(15) Uani 1 1 d . . . . .
O41 O -0.2546(10) 0.8016(8) 0.1811(5) 0.071(3) Uani 1 1 d . . . B 1
F45 F -0.4045(8) 0.8857(5) 0.0711(5) 0.0677(19) Uani 1 1 d . . . B 1
C25 C 0.0744(8) 0.3300(6) -0.2798(4) 0.0214(15) Uani 1 1 d . . . . .
H25 H -0.031374 0.308007 -0.295502 0.026 Uiso 1 1 calc R . . . .
C17 C 0.4382(8) 0.9201(5) 0.3670(4) 0.0160(14) Uani 1 1 d . . . . .
C1 C 0.1954(9) 0.7279(6) -0.0164(4) 0.0251(17) Uani 1 1 d . . . . .
N21 N 0.2984(7) 0.4440(5) -0.1911(4) 0.0237(14) Uani 1 1 d . . . . .
C3 C 0.3140(9) 0.6194(5) -0.0969(4) 0.0213(15) Uani 1 1 d . . . . .
F46 F -0.3334(10) 0.7982(7) -0.0209(4) 0.083(3) Uani 1 1 d . . . B 1
C15 C 0.4232(9) 0.8367(6) 0.2255(4) 0.0234(16) Uani 1 1 d . . . . .
H15 H 0.526265 0.838561 0.241295 0.028 Uiso 1 1 calc R . . . .
C2 C 0.2336(9) 0.6352(6) -0.0422(4) 0.0262(17) Uani 1 1 d . . . . .
C34 C 0.1183(9) 0.9218(6) -0.3157(4) 0.0230(16) Uani 1 1 d . . . . .
N31 N 0.2829(8) 0.8847(5) -0.1933(4) 0.0267(15) Uani 1 1 d . . . . .
C20 C 0.3814(9) 0.5294(6) -0.1152(4) 0.0267(17) Uani 1 1 d . . . . .
H20A H 0.484585 0.553438 -0.115745 0.032 Uiso 1 1 calc R . . . .
H20B H 0.387486 0.502283 -0.072587 0.032 Uiso 1 1 calc R . . . .
C27 C 0.0790(8) 0.1818(5) -0.3957(4) 0.0199(15) Uani 1 1 d . . . . .
C16 C 0.3440(9) 0.7961(7) 0.1483(4) 0.0278(17) Uani 1 1 d . . . . .
H16 H 0.392065 0.769044 0.110589 0.033 Uiso 1 1 calc R . . . .
C13 C 0.2037(9) 0.8720(7) 0.2557(4) 0.0255(17) Uani 1 1 d . . . . .
H13 H 0.153132 0.897756 0.292495 0.031 Uiso 1 1 calc R . . . .
C35 C 0.2716(9) 0.9358(8) -0.3003(5) 0.036(2) Uani 1 1 d . . . . .
H35 H 0.320419 0.958363 -0.332806 0.043 Uiso 1 1 calc R . . . .
C24 C 0.1551(8) 0.2777(6) -0.3229(4) 0.0200(15) Uani 1 1 d . . . . .
C4 C 0.3489(8) 0.6947(6) -0.1283(4) 0.0224(16) Uani 1 1 d . . . . .
C5 C 0.3150(9) 0.7885(6) -0.0996(4) 0.0252(17) Uani 1 1 d . . . . .
C32 C 0.1368(10) 0.8671(8) -0.2080(5) 0.036(2) Uani 1 1 d . . . . .
H32 H 0.090423 0.841709 -0.175823 0.044 Uiso 1 1 calc R . . . .
C26 C 0.1486(9) 0.4138(6) -0.2142(4) 0.0236(16) Uani 1 1 d . . . . .
H26 H 0.093780 0.450931 -0.184695 0.028 Uiso 1 1 calc R . . . .
C14 C 0.3535(8) 0.8751(5) 0.2807(4) 0.0169(14) Uani 1 1 d . . . . .
C44 C -0.2999(11) 0.8415(10) 0.0641(10) 0.073(5) Uani 1 1 d . . . B 1
C23 C 0.3097(9) 0.3120(6) -0.2985(5) 0.0266(17) Uani 1 1 d . . . . .
H23 H 0.366712 0.278175 -0.328420 0.032 Uiso 1 1 calc R . . . .
C33 C 0.0507(9) 0.8850(8) -0.2692(5) 0.035(2) Uani 1 1 d . . . . .
H33 H -0.054503 0.872179 -0.279409 0.042 Uiso 1 1 calc R . . . .
C7 C 0.1934(12) 0.5542(7) -0.0091(6) 0.041(2) Uani 1 1 d . . . . .
H7A H 0.121054 0.571209 0.019180 0.062 Uiso 1 1 calc GR . . . .
H7B H 0.283508 0.550838 0.026702 0.062 Uiso 1 1 calc GR . . . .
H7C H 0.149624 0.487991 -0.051703 0.062 Uiso 1 1 calc GR . . . .
C22 C 0.3793(9) 0.3941(7) -0.2317(5) 0.0293(18) Uani 1 1 d . . . . .
H22 H 0.485200 0.416052 -0.213865 0.035 Uiso 1 1 calc R . . . .
C12 C 0.1281(9) 0.8313(7) 0.1770(4) 0.0288(18) Uani 1 1 d . . . . .
H12 H 0.025478 0.829799 0.159621 0.035 Uiso 1 1 calc R . . . .
C36 C 0.3522(10) 0.9175(7) -0.2387(5) 0.034(2) Uani 1 1 d . . . . .
H36 H 0.457331 0.927877 -0.227973 0.041 Uiso 1 1 calc R . . . .
C6 C 0.2390(10) 0.8071(7) -0.0430(4) 0.0299(18) Uani 1 1 d . . . . .
C8 C 0.4249(10) 0.6744(7) -0.1915(5) 0.0331(19) Uani 1 1 d . . . . .
H8A H 0.532729 0.688408 -0.167719 0.050 Uiso 1 1 calc GR . . . .
H8B H 0.404938 0.718749 -0.221191 0.050 Uiso 1 1 calc GR . . . .
H8C H 0.386283 0.602997 -0.226520 0.050 Uiso 1 1 calc GR . . . .
C30 C 0.3813(10) 0.8732(7) -0.1229(5) 0.034(2) Uani 1 1 d . . . . .
H30A H 0.475497 0.861656 -0.133616 0.041 Uiso 1 1 calc R . . . .
H30B H 0.406977 0.938222 -0.078142 0.041 Uiso 1 1 calc R . . . .
C9 C 0.2034(14) 0.9075(8) -0.0118(6) 0.049(3) Uani 1 1 d . . . . .
H9A H 0.094880 0.897754 -0.025250 0.074 Uiso 1 1 calc GR . . . .
H9B H 0.245358 0.954149 -0.034602 0.074 Uiso 1 1 calc GR . . . .
H9C H 0.246643 0.936408 0.045090 0.074 Uiso 1 1 calc GR . . . .
O28 O 0.1588(6) 0.1577(4) -0.4399(3) 0.0213(11) Uani 1 1 d . . . . .
O29 O -0.0516(5) 0.1391(4) -0.4046(3) 0.0201(11) Uani 1 1 d . . . . .
O39 O 0.0987(6) 0.9713(4) -0.4253(3) 0.0222(11) Uani 1 1 d . . . . .
O38 O -0.1063(6) 0.9412(4) -0.3894(3) 0.0214(11) Uani 1 1 d . . . . .
O19 O 0.5724(5) 0.9154(4) 0.3858(3) 0.0229(11) Uani 1 1 d . . . . .
Br2B Br 0.6528(6) 1.3510(4) 0.6375(3) 0.0632(16) Uani 0.266(4) 1 d . . P A 1
O1W O 0.3142(7) 0.8733(5) 0.5201(4) 0.0350(14) Uani 1 1 d . . . . .
H1WA H 0.239014 0.827549 0.517735 0.053 Uiso 1 1 d GR . . . .
H1WB H 0.377904 0.894249 0.566266 0.053 Uiso 1 1 d GR . . . .
O2W O 0.3959(7) 1.1636(4) 0.4913(3) 0.0292(12) Uani 1 1 d . . . . .
H2WA H 0.451605 1.202684 0.538321 0.044 Uiso 1 1 d GR . . . .
H2WB H 0.343652 1.199378 0.471466 0.044 Uiso 1 1 d GR . . . .
N11 N 0.1981(7) 0.7939(5) 0.1251(3) 0.0219(13) Uani 1 1 d . U . . .
C10 C 0.1058(9) 0.7465(7) 0.0411(4) 0.0294(18) Uani 1 1 d . U . . .
H10A H 0.041740 0.791427 0.029614 0.035 Uiso 1 1 calc R . . . .
H10B H 0.039426 0.680661 0.033014 0.035 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O18 2.319(5) . ?
Tb1 O28 2.339(5) 1_566 ?
Tb1 O29 2.396(5) 2_565 ?
Tb1 O39 2.327(5) 1_556 ?
Tb1 O38 2.399(5) 2_575 ?
Tb1 O19 2.373(5) 2_676 ?
Tb1 O1W 2.407(6) . ?
Tb1 O2W 2.468(6) . ?
S40 O43 1.402(7) . ?
S40 O42 1.395(7) . ?
S40 O41 1.473(8) . ?
S40 C44 1.806(10) . ?
O18 C17 1.229(9) . ?
F47 C44 1.315(12) . ?
C37 C34 1.503(10) . ?
C37 O39 1.257(9) . ?
C37 O38 1.263(9) . ?
F45 C44 1.271(14) . ?
C25 H25 0.9500 . ?
C25 C24 1.379(10) . ?
C25 C26 1.368(10) . ?
C17 C14 1.517(9) . ?
C17 O19 1.262(9) . ?
C1 C2 1.399(12) . ?
C1 C6 1.413(12) . ?
C1 C10 1.515(11) . ?
N21 C20 1.500(9) . ?
N21 C26 1.344(10) . ?
N21 C22 1.341(11) . ?
C3 C2 1.406(11) . ?
C3 C20 1.506(11) . ?
C3 C4 1.410(11) . ?
F46 C44 1.465(19) . ?
C15 H15 0.9500 . ?
C15 C16 1.364(10) . ?
C15 C14 1.381(10) . ?
C2 C7 1.512(11) . ?
C34 C35 1.387(11) . ?
C34 C33 1.377(11) . ?
N31 C32 1.319(12) . ?
N31 C36 1.343(11) . ?
N31 C30 1.511(10) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C27 C24 1.530(9) . ?
C27 O28 1.261(9) . ?
C27 O29 1.240(9) . ?
C16 H16 0.9500 . ?
C16 N11 1.347(10) . ?
C13 H13 0.9500 . ?
C13 C14 1.383(10) . ?
C13 C12 1.380(10) . ?
C35 H35 0.9500 . ?
C35 C36 1.361(12) . ?
C24 C23 1.389(11) . ?
C4 C5 1.399(12) . ?
C4 C8 1.510(11) . ?
C5 C6 1.406(12) . ?
C5 C30 1.505(11) . ?
C32 H32 0.9500 . ?
C32 C33 1.375(12) . ?
C26 H26 0.9500 . ?
C23 H23 0.9500 . ?
C23 C22 1.361(12) . ?
C33 H33 0.9500 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C22 H22 0.9500 . ?
C12 H12 0.9500 . ?
C12 N11 1.334(10) . ?
C36 H36 0.9500 . ?
C6 C9 1.496(13) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
O1W H1WA 0.8692 . ?
O1W H1WB 0.8685 . ?
O2W H2WA 0.8732 . ?
O2W H2WB 0.8737 . ?
N11 C10 1.499(9) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O18 Tb1 O28 142.36(19) . 1_566 ?
O18 Tb1 O29 81.88(17) . 2_565 ?
O18 Tb1 O39 145.4(2) . 1_556 ?
O18 Tb1 O38 82.04(18) . 2_575 ?
O18 Tb1 O19 98.18(17) . 2_676 ?
O18 Tb1 O1W 72.5(2) . . ?
O18 Tb1 O2W 70.75(19) . . ?
O28 Tb1 O29 121.73(17) 1_566 2_565 ?
O28 Tb1 O38 77.76(18) 1_566 2_575 ?
O28 Tb1 O19 79.03(18) 1_566 2_676 ?
O28 Tb1 O1W 138.92(19) 1_566 . ?
O28 Tb1 O2W 72.74(19) 1_566 . ?
O29 Tb1 O38 74.49(18) 2_565 2_575 ?
O29 Tb1 O1W 72.9(2) 2_565 . ?
O29 Tb1 O2W 138.15(18) 2_565 . ?
O39 Tb1 O28 71.95(19) 1_556 1_566 ?
O39 Tb1 O29 78.78(18) 1_556 2_565 ?
O39 Tb1 O38 119.27(18) 1_556 2_575 ?
O39 Tb1 O19 81.97(17) 1_556 2_676 ?
O39 Tb1 O1W 74.5(2) 1_556 . ?
O39 Tb1 O2W 139.47(19) 1_556 . ?
O38 Tb1 O1W 140.8(2) 2_575 . ?
O38 Tb1 O2W 70.93(19) 2_575 . ?
O19 Tb1 O29 144.52(19) 2_676 2_565 ?
O19 Tb1 O38 140.90(19) 2_676 2_575 ?
O19 Tb1 O1W 73.4(2) 2_676 . ?
O19 Tb1 O2W 72.35(19) 2_676 . ?
O1W Tb1 O2W 124.4(2) . . ?
O43 S40 O41 112.7(6) . . ?
O43 S40 C44 106.9(6) . . ?
O42 S40 O43 117.1(5) . . ?
O42 S40 O41 115.5(5) . . ?
O42 S40 C44 107.3(5) . . ?
O41 S40 C44 94.2(7) . . ?
C17 O18 Tb1 173.3(5) . . ?
O39 C37 C34 117.6(7) . . ?
O39 C37 O38 124.4(7) . . ?
O38 C37 C34 118.1(7) . . ?
C24 C25 H25 120.4 . . ?
C26 C25 H25 120.4 . . ?
C26 C25 C24 119.2(7) . . ?
O18 C17 C14 117.5(6) . . ?
O18 C17 O19 125.8(6) . . ?
O19 C17 C14 116.7(6) . . ?
C2 C1 C6 121.1(7) . . ?
C2 C1 C10 120.8(7) . . ?
C6 C1 C10 118.0(8) . . ?
C26 N21 C20 120.9(7) . . ?
C22 N21 C20 117.5(7) . . ?
C22 N21 C26 121.4(7) . . ?
C2 C3 C20 121.1(7) . . ?
C2 C3 C4 120.1(7) . . ?
C4 C3 C20 118.4(7) . . ?
C16 C15 H15 120.0 . . ?
C16 C15 C14 119.9(7) . . ?
C14 C15 H15 120.0 . . ?
C1 C2 C3 119.5(7) . . ?
C1 C2 C7 120.0(8) . . ?
C3 C2 C7 120.5(8) . . ?
C35 C34 C37 120.1(7) . . ?
C33 C34 C37 121.7(7) . . ?
C33 C34 C35 118.1(7) . . ?
C32 N31 C36 121.5(7) . . ?
C32 N31 C30 121.9(7) . . ?
C36 N31 C30 116.6(7) . . ?
N21 C20 C3 115.2(6) . . ?
N21 C20 H20A 108.5 . . ?
N21 C20 H20B 108.5 . . ?
C3 C20 H20A 108.5 . . ?
C3 C20 H20B 108.5 . . ?
H20A C20 H20B 107.5 . . ?
O28 C27 C24 114.4(6) . . ?
O29 C27 C24 117.2(6) . . ?
O29 C27 O28 128.5(7) . . ?
C15 C16 H16 119.7 . . ?
N11 C16 C15 120.7(7) . . ?
N11 C16 H16 119.7 . . ?
C14 C13 H13 120.2 . . ?
C12 C13 H13 120.2 . . ?
C12 C13 C14 119.6(7) . . ?
C34 C35 H35 119.9 . . ?
C36 C35 C34 120.3(8) . . ?
C36 C35 H35 119.9 . . ?
C25 C24 C27 121.7(7) . . ?
C25 C24 C23 119.0(7) . . ?
C23 C24 C27 119.3(7) . . ?
C3 C4 C8 120.0(7) . . ?
C5 C4 C3 119.6(7) . . ?
C5 C4 C8 120.5(7) . . ?
C4 C5 C6 121.1(7) . . ?
C4 C5 C30 117.4(8) . . ?
C6 C5 C30 120.9(8) . . ?
N31 C32 H32 119.6 . . ?
N31 C32 C33 120.8(8) . . ?
C33 C32 H32 119.6 . . ?
C25 C26 H26 119.7 . . ?
N21 C26 C25 120.5(7) . . ?
N21 C26 H26 119.7 . . ?
C15 C14 C17 121.2(6) . . ?
C15 C14 C13 118.6(7) . . ?
C13 C14 C17 120.2(6) . . ?
F47 C44 S40 115.0(7) . . ?
F47 C44 F46 99.9(11) . . ?
F45 C44 S40 115.7(9) . . ?
F45 C44 F47 115.3(11) . . ?
F45 C44 F46 101.4(10) . . ?
F46 C44 S40 106.7(9) . . ?
C24 C23 H23 120.0 . . ?
C22 C23 C24 119.9(7) . . ?
C22 C23 H23 120.0 . . ?
C34 C33 H33 120.3 . . ?
C32 C33 C34 119.5(8) . . ?
C32 C33 H33 120.3 . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N21 C22 C23 119.9(7) . . ?
N21 C22 H22 120.0 . . ?
C23 C22 H22 120.0 . . ?
C13 C12 H12 119.8 . . ?
N11 C12 C13 120.4(7) . . ?
N11 C12 H12 119.8 . . ?
N31 C36 C35 119.8(8) . . ?
N31 C36 H36 120.1 . . ?
C35 C36 H36 120.1 . . ?
C1 C6 C9 120.3(8) . . ?
C5 C6 C1 118.4(8) . . ?
C5 C6 C9 121.3(8) . . ?
C4 C8 H8A 109.5 . . ?
C4 C8 H8B 109.5 . . ?
C4 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N31 C30 H30A 108.4 . . ?
N31 C30 H30B 108.4 . . ?
C5 C30 N31 115.4(7) . . ?
C5 C30 H30A 108.4 . . ?
C5 C30 H30B 108.4 . . ?
H30A C30 H30B 107.5 . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C27 O28 Tb1 139.0(5) . 1_544 ?
C27 O29 Tb1 136.1(5) . 2_565 ?
C37 O39 Tb1 177.8(5) . 1_554 ?
C37 O38 Tb1 114.5(5) . 2_575 ?
C17 O19 Tb1 133.2(4) . 2_676 ?
Tb1 O1W H1WA 110.3 . . ?
Tb1 O1W H1WB 110.3 . . ?
H1WA O1W H1WB 108.5 . . ?
Tb1 O2W H2WA 110.3 . . ?
Tb1 O2W H2WB 110.8 . . ?
H2WA O2W H2WB 108.2 . . ?
C16 N11 C10 122.3(7) . . ?
C12 N11 C16 120.8(6) . . ?
C12 N11 C10 116.9(6) . . ?
C1 C10 H10A 108.6 . . ?
C1 C10 H10B 108.6 . . ?
N11 C10 C1 114.5(7) . . ?
N11 C10 H10A 108.6 . . ?
N11 C10 H10B 108.6 . . ?
H10A C10 H10B 107.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O18 C17 C14 C15 175.0(7) . . . . ?
O18 C17 C14 C13 -5.0(11) . . . . ?
O18 C17 O19 Tb1 -6.9(12) . . . 2_676 ?
O43 S40 C44 F47 -49.4(14) . . . . ?
O43 S40 C44 F45 172.3(11) . . . . ?
O43 S40 C44 F46 60.3(8) . . . . ?
O42 S40 C44 F47 -175.8(11) . . . . ?
O42 S40 C44 F45 45.8(14) . . . . ?
O42 S40 C44 F46 -66.1(8) . . . . ?
C37 C34 C35 C36 177.5(9) . . . . ?
C37 C34 C33 C32 -177.9(8) . . . . ?
O41 S40 C44 F47 65.9(13) . . . . ?
O41 S40 C44 F45 -72.5(12) . . . . ?
O41 S40 C44 F46 175.6(7) . . . . ?
C25 C24 C23 C22 2.0(13) . . . . ?
C3 C4 C5 C6 -3.7(11) . . . . ?
C3 C4 C5 C30 167.9(7) . . . . ?
C15 C16 N11 C12 -0.1(13) . . . . ?
C15 C16 N11 C10 -177.7(8) . . . . ?
C2 C1 C6 C5 3.4(11) . . . . ?
C2 C1 C6 C9 -177.0(8) . . . . ?
C2 C1 C10 N11 91.3(9) . . . . ?
C2 C3 C20 N21 103.6(8) . . . . ?
C2 C3 C4 C5 5.7(11) . . . . ?
C2 C3 C4 C8 -175.4(7) . . . . ?
C34 C37 O38 Tb1 178.5(5) . . . 2_575 ?
C34 C35 C36 N31 0.7(15) . . . . ?
N31 C32 C33 C34 0.0(16) . . . . ?
C20 N21 C26 C25 -173.9(7) . . . . ?
C20 N21 C22 C23 175.9(8) . . . . ?
C20 C3 C2 C1 168.7(7) . . . . ?
C20 C3 C2 C7 -9.0(11) . . . . ?
C20 C3 C4 C5 -166.5(7) . . . . ?
C20 C3 C4 C8 12.4(10) . . . . ?
C27 C24 C23 C22 -176.7(8) . . . . ?
C16 C15 C14 C17 179.5(7) . . . . ?
C16 C15 C14 C13 -0.5(12) . . . . ?
C16 N11 C10 C1 -15.9(11) . . . . ?
C13 C12 N11 C16 -0.6(13) . . . . ?
C13 C12 N11 C10 177.1(8) . . . . ?
C35 C34 C33 C32 2.3(14) . . . . ?
C24 C25 C26 N21 -1.1(12) . . . . ?
C24 C27 O28 Tb1 131.2(6) . . . 1_544 ?
C24 C27 O29 Tb1 -174.9(5) . . . 2_565 ?
C24 C23 C22 N21 -2.5(13) . . . . ?
C4 C3 C2 C1 -3.2(11) . . . . ?
C4 C3 C2 C7 179.0(7) . . . . ?
C4 C3 C20 N21 -84.3(9) . . . . ?
C4 C5 C6 C1 -0.9(11) . . . . ?
C4 C5 C6 C9 179.6(8) . . . . ?
C4 C5 C30 N31 94.6(9) . . . . ?
C32 N31 C36 C35 1.8(15) . . . . ?
C32 N31 C30 C5 35.1(12) . . . . ?
C26 C25 C24 C27 178.5(7) . . . . ?
C26 C25 C24 C23 -0.2(12) . . . . ?
C26 N21 C20 C3 -41.9(11) . . . . ?
C26 N21 C22 C23 1.1(13) . . . . ?
C14 C17 O19 Tb1 171.7(5) . . . 2_676 ?
C14 C15 C16 N11 0.7(13) . . . . ?
C14 C13 C12 N11 0.8(13) . . . . ?
C33 C34 C35 C36 -2.7(14) . . . . ?
C22 N21 C20 C3 143.4(8) . . . . ?
C22 N21 C26 C25 0.7(12) . . . . ?
C12 C13 C14 C17 179.8(7) . . . . ?
C12 C13 C14 C15 -0.2(12) . . . . ?
C12 N11 C10 C1 166.4(8) . . . . ?
C36 N31 C32 C33 -2.1(15) . . . . ?
C36 N31 C30 C5 -147.3(9) . . . . ?
C6 C1 C2 C3 -1.4(11) . . . . ?
C6 C1 C2 C7 176.4(8) . . . . ?
C6 C1 C10 N11 -88.8(9) . . . . ?
C6 C5 C30 N31 -93.8(9) . . . . ?
C8 C4 C5 C6 177.4(7) . . . . ?
C8 C4 C5 C30 -11.0(11) . . . . ?
C30 N31 C32 C33 175.3(9) . . . . ?
C30 N31 C36 C35 -175.8(9) . . . . ?
C30 C5 C6 C1 -172.2(7) . . . . ?
C30 C5 C6 C9 8.3(12) . . . . ?
O28 C27 C24 C25 162.4(7) . . . . ?
O28 C27 C24 C23 -18.9(10) . . . . ?
O28 C27 O29 Tb1 6.4(13) . . . 2_565 ?
O29 C27 C24 C25 -16.5(11) . . . . ?
O29 C27 C24 C23 162.2(7) . . . . ?
O29 C27 O28 Tb1 -50.0(12) . . . 1_544 ?
O39 C37 C34 C35 5.6(12) . . . . ?
O39 C37 C34 C33 -174.2(8) . . . . ?
O39 C37 O38 Tb1 -0.7(9) . . . 2_575 ?
O38 C37 C34 C35 -173.7(8) . . . . ?
O38 C37 C34 C33 6.5(12) . . . . ?
O19 C17 C14 C15 -3.7(10) . . . . ?
O19 C17 C14 C13 176.3(7) . . . . ?
C10 C1 C2 C3 178.6(7) . . . . ?
C10 C1 C2 C7 -3.7(12) . . . . ?
C10 C1 C6 C5 -176.5(7) . . . . ?
C10 C1 C6 C9 3.1(12) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.816 0.500 0.500 602.7 182.8 '18x water'

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.406
_oxdiff_exptl_absorpt_empirical_full_min 0.662
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_jj003_br_nd_otf_kotf_ii_h2o_acet_red2
_database_code_depnum_ccdc_archive 'CCDC 1833434'
loop_
_audit_author_name
_audit_author_address
'Antti Tiihonen'
;University of Jyv?skyl?, Department of Chemistry
Finland
;
_audit_update_record             
;
2018-03-29 deposited with the CCDC.	2019-02-28 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_CHEMW03_I                   
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: The structure contains voids of unresolved electron density
which was treated using Olex2 solvent mask procedure (full details in 
_smtbx_masks_special_details). The 6 water molecules per asymmetric unit 
 are included in the formula and used in the calculations. 
;
_vrf_PLAT420_I                   
;
PROBLEM: D-H Without Acceptor       O       --H 
RESPONSE: Hydrogen bond acceptors (water located in a void) have been removed 
among the other disordered solvents (also water) found in the voids 
(see vrf_CHEMW03_ALERT_2_A).
;
_vrf_FORMU01_I                   
;
PROBLEM: There is a discrepancy between the atom counts in the
            _chemical_formula_sum and _chemical_formula_moiety.
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_CELLZ01_I                   
;
PROBLEM: Difference between formula and atom_site contents detected.
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT041_I                   
;
PROBLEM: Calculated and Reported SumFormula strings Differ ...    
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT042_I                   
;
PROBLEM: Calculated and Reported Moiety formula strings Differ by ...
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT068_I                   
;
PROBLEM: Reported F000 Differs from Calcd (or Missing)...
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT606_I                   
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
# end Validation Reply Form
_audit_creation_date             2018-03-26
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C30 H31 N3 Nd O8, 1.35(Br), 1.65(C F3 O3 S), 0.35(O)'
_chemical_formula_sum            'C31.65 H43 Br1.35 F4.94 N3 Nd O19.29 S1.65'
_chemical_formula_weight         1173.14
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C32 H31 Br1 F5 N3 Nd1 O13 S2'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -3.1807 10.9079 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   18.7643(2)
_cell_length_b                   25.6962(3)
_cell_length_c                   9.85675(12)
_cell_angle_alpha                90
_cell_angle_beta                 102.8557(12)
_cell_angle_gamma                90
_cell_volume                     4633.50(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7481
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      76.5540
_cell_measurement_theta_min      4.1810
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    11.453
_exptl_absorpt_correction_T_max  0.821
_exptl_absorpt_correction_T_min  0.539
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.682
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2346
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
3 16 0 0.0148
-2 -16 -1 0.0373
6 9 -5 0.0273
3 -9 -5 0.0400
-5 -5 6 0.0322
11 -4 1 0.0033
-12 1 -1 0.0165

_exptl_crystal_size_max          0.083
_exptl_crystal_size_mid          0.059
_exptl_crystal_size_min          0.023
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
3.0000 16.0000 -0.0000 -0.6419 0.7536 -0.0634
-2.0000 -16.0000 -1.0000 0.6543 -0.7406 -0.0992
6.0000 9.0000 -5.0000 -0.3317 0.4425 -0.8378
3.0000 -9.0000 -5.0000 0.4083 -0.3800 -0.7725
-5.0000 -5.0000 6.0000 0.2184 -0.1827 0.9644
11.0000 -4.0000 1.0000 0.7563 0.6597 -0.0277
-12.0000 1.0000 -1.0000 -0.6568 -0.8306 0.0466

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            16990
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.994
_diffrn_reflns_theta_min         2.965
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3953
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -118.00  -9.00   1.00   20.00    --  -42.03 -77.00  90.00  109
  2  ω    -70.00  30.00   1.00   20.00    --  -42.03  57.00 -30.00  100
  3  ω    104.00 178.00   1.00   60.00    --  112.00 111.00   0.00   74
  4  ω     84.00 178.00   1.00   60.00    --  112.00  30.00   0.00   94
  5  ω     43.00 111.00   1.00   60.00    --  112.00-111.00 -60.00   68
  6  ω    104.00 143.00   1.00   60.00    --  112.00 111.00-150.00   39
  7  ω     33.00 105.00   1.00   60.00    --  112.00 -94.00  90.00   72
  8  ω     39.00 131.00   1.00   60.00    --  112.00 -45.00  60.00   92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0477035000
_diffrn_orient_matrix_UB_12      -0.0490615000
_diffrn_orient_matrix_UB_13      0.0352766000
_diffrn_orient_matrix_UB_21      0.0675415000
_diffrn_orient_matrix_UB_22      0.0344363000
_diffrn_orient_matrix_UB_23      0.0545311000
_diffrn_orient_matrix_UB_31      -0.0161690000
_diffrn_orient_matrix_UB_32      -0.0009329000
_diffrn_orient_matrix_UB_33      0.1464746000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6956
_reflns_number_total             8412
_reflns_odcompleteness_completeness 99.58
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         1.088
_refine_diff_density_min         -1.910
_refine_diff_density_rms         0.118
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     556
_refine_ls_number_reflns         8412
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0464
_refine_ls_restrained_S_all      1.068
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0792P)²+8.8951P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1295
_refine_ls_wR_factor_ref         0.1363
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O3B) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3. Others
 Sof(Br2B)=Sof(O3B)=1-FVAR(1)
 Sof(S48A)=Sof(O50A)=Sof(O49A)=Sof(O51A)=Sof(F53A)=Sof(F55A)=Sof(F54A)=
 Sof(C52A)=FVAR(1)
4.a Rotating group:
 O2W(H2WA,H2WB), O1W(H1WA,H1WB)
4.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C20(H20A,H20B), C30(H30A,H30B)
4.c Aromatic/amide H refined with riding coordinates:
 C16(H16), C15(H15), C12(H12), C23(H23), C26(H26), C13(H13), C22(H22),
 C25(H25), C35(H35), C36(H36), C32(H32), C33(H33)
4.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Nd1 Nd 0.61652(2) 0.75018(2) -0.23300(2) 0.01796(10) Uani 1 1 d . . . . .
Br1 Br 0.40114(5) 0.84615(4) -0.06366(10) 0.0750(3) Uani 1 1 d . . . . .
S40 S 1.00383(8) 0.85281(5) 0.63650(14) 0.0336(3) Uani 1 1 d . . . . .
O18 O 0.6968(2) 0.7870(2) -0.0336(4) 0.0438(11) Uani 1 1 d . . . . .
O43 O 0.9992(2) 0.87761(18) 0.7634(4) 0.0458(11) Uani 1 1 d . . . . .
F47 F 0.9610(2) 0.76762(15) 0.7395(4) 0.0507(9) Uani 1 1 d . . . . .
O42 O 0.9743(4) 0.88191(19) 0.5141(5) 0.0651(16) Uani 1 1 d . . . . .
F45 F 0.9431(3) 0.76750(17) 0.5198(5) 0.0771(15) Uani 1 1 d . . . . .
N11 N 0.9400(2) 0.87028(16) 0.0834(4) 0.0232(8) Uani 1 1 d . . . . .
C10 C 1.0090(3) 0.8997(3) 0.0771(6) 0.0402(15) Uani 1 1 d . . . . .
H10A H 1.033603 0.881940 0.011112 0.048 Uiso 1 1 calc R . . . .
H10B H 0.995585 0.935164 0.040786 0.048 Uiso 1 1 calc R . . . .
O41 O 1.0736(3) 0.8289(2) 0.6424(7) 0.079(2) Uani 1 1 d . . . . .
C4 C 1.1599(2) 0.91158(19) 0.4735(5) 0.0226(10) Uani 1 1 d . . . . .
F46 F 0.8734(2) 0.81261(17) 0.6222(6) 0.0711(13) Uani 1 1 d . . . . .
C14 C 0.8102(2) 0.8218(2) 0.0832(5) 0.0229(10) Uani 1 1 d . . . . .
C6 C 1.1064(2) 0.8611(2) 0.2661(5) 0.0237(10) Uani 1 1 d . . . . .
C8 C 1.2115(3) 0.9163(2) 0.6141(6) 0.0323(11) Uani 1 1 d . . . . .
H8A H 1.249256 0.889357 0.623486 0.048 Uiso 1 1 calc GR . . . .
H8B H 1.184164 0.911808 0.687238 0.048 Uiso 1 1 calc GR . . . .
H8C H 1.234498 0.950706 0.622820 0.048 Uiso 1 1 calc GR . . . .
C16 C 0.8944(3) 0.8585(2) -0.0381(5) 0.0262(10) Uani 1 1 d . . . . .
H16 H 0.907543 0.867264 -0.122952 0.031 Uiso 1 1 calc R . . . .
C15 C 0.8290(2) 0.8339(2) -0.0414(5) 0.0251(10) Uani 1 1 d . . . . .
H15 H 0.797216 0.825274 -0.127682 0.030 Uiso 1 1 calc R . . . .
C44 C 0.9425(4) 0.7975(2) 0.6278(7) 0.0427(14) Uani 1 1 d . . . . .
C17 C 0.7368(3) 0.7964(2) 0.0814(5) 0.0274(11) Uani 1 1 d . . . . .
C5 C 1.1536(2) 0.86522(19) 0.3986(5) 0.0234(10) Uani 1 1 d . . . . .
C12 C 0.9232(3) 0.8580(2) 0.2048(5) 0.0253(10) Uani 1 1 d . . . . .
H12 H 0.956244 0.866440 0.289806 0.030 Uiso 1 1 calc R . . . .
N21 N 1.1745(2) 1.04010(17) 0.4907(5) 0.0320(10) Uani 1 1 d . . . . .
C20 C 1.1166(3) 1.0014(2) 0.5089(7) 0.0382(14) Uani 1 1 d . . . . .
H20A H 1.125982 0.990721 0.607747 0.046 Uiso 1 1 calc R . . . .
H20B H 1.068228 1.018660 0.485647 0.046 Uiso 1 1 calc R . . . .
C7 C 1.0133(3) 0.9947(3) 0.2371(8) 0.0551(19) Uani 1 1 d . . . . .
H7A H 0.962589 0.982560 0.218544 0.083 Uiso 1 1 calc GR . . . .
H7B H 1.024401 1.007934 0.150792 0.083 Uiso 1 1 calc GR . . . .
H7C H 1.020060 1.022677 0.306492 0.083 Uiso 1 1 calc GR . . . .
C1 C 1.0614(2) 0.9040(2) 0.2157(5) 0.0281(11) Uani 1 1 d . . . . .
C23 C 1.2372(3) 1.0875(2) 0.3492(6) 0.0327(11) Uani 1 1 d . . . . .
H23 H 1.247830 1.093246 0.260576 0.039 Uiso 1 1 calc R . . . .
C3 C 1.1144(3) 0.95384(19) 0.4199(6) 0.0266(10) Uani 1 1 d . . . . .
C26 C 1.2050(4) 1.0687(2) 0.6034(7) 0.0426(14) Uani 1 1 d . . . . .
H26 H 1.193425 1.061977 0.690860 0.051 Uiso 1 1 calc R . . . .
C13 C 0.8585(3) 0.8334(2) 0.2068(5) 0.0249(10) Uani 1 1 d . . . . .
H13 H 0.846980 0.824470 0.293009 0.030 Uiso 1 1 calc R . . . .
C30 C 1.1917(2) 0.81773(19) 0.4690(6) 0.0271(11) Uani 1 1 d . . . . .
H30A H 1.187576 0.817857 0.567429 0.032 Uiso 1 1 calc R . . . .
H30B H 1.165732 0.786484 0.424356 0.032 Uiso 1 1 calc R . . . .
C9 C 1.1028(3) 0.8126(2) 0.1811(7) 0.0413(14) Uani 1 1 d . . . . .
H9A H 1.143469 0.789599 0.222966 0.062 Uiso 1 1 calc GR . . . .
H9B H 1.106295 0.821598 0.086219 0.062 Uiso 1 1 calc GR . . . .
H9C H 1.056384 0.794755 0.178579 0.062 Uiso 1 1 calc GR . . . .
C22 C 1.1895(3) 1.0485(2) 0.3669(6) 0.0349(12) Uani 1 1 d . . . . .
H22 H 1.167133 1.027504 0.289863 0.042 Uiso 1 1 calc R . . . .
C25 C 1.2536(3) 1.1081(2) 0.5897(6) 0.0385(13) Uani 1 1 d . . . . .
H25 H 1.276124 1.128122 0.668599 0.046 Uiso 1 1 calc R . . . .
C2 C 1.0645(3) 0.9498(2) 0.2922(6) 0.0329(12) Uani 1 1 d . . . . .
O19 O 0.7224(2) 0.78755(17) 0.1970(4) 0.0362(9) Uani 1 1 d . . . . .
N31 N 1.2706(2) 0.81308(16) 0.4655(4) 0.0247(9) Uani 1 1 d . . . . .
C35 C 1.3650(3) 0.8164(2) 0.3425(5) 0.0261(10) Uani 1 1 d . . . . .
H35 H 1.381621 0.825593 0.261401 0.031 Uiso 1 1 calc R . . . .
C36 C 1.2939(3) 0.8265(2) 0.3487(5) 0.0277(11) Uani 1 1 d . . . . .
H36 H 1.261391 0.842663 0.272667 0.033 Uiso 1 1 calc R . . . .
C27 C 1.3193(3) 1.1635(2) 0.4486(5) 0.0277(11) Uani 1 1 d . . . . .
C24 C 1.2694(3) 1.1182(2) 0.4619(5) 0.0284(11) Uani 1 1 d . . . . .
C32 C 1.3167(3) 0.7921(2) 0.5760(5) 0.0295(11) Uani 1 1 d . . . . .
H32 H 1.299644 0.784414 0.657618 0.035 Uiso 1 1 calc R . . . .
O28 O 1.3235(2) 1.17666(15) 0.3294(4) 0.0315(8) Uani 1 1 d . . . . .
O29 O 1.3513(2) 1.18354(17) 0.5622(4) 0.0391(10) Uani 1 1 d . . . . .
C37 C 1.4884(2) 0.77713(18) 0.4437(5) 0.0196(9) Uani 1 1 d . . . . .
C34 C 1.4125(2) 0.79305(19) 0.4525(5) 0.0214(9) Uani 1 1 d . . . . .
C33 C 1.3880(3) 0.7818(2) 0.5725(5) 0.0305(12) Uani 1 1 d . . . . .
H33 H 1.420374 0.767084 0.651196 0.037 Uiso 1 1 calc R . . . .
O39 O 1.50178(17) 0.77647(14) 0.3240(3) 0.0251(7) Uani 1 1 d . . . . .
O38 O 1.53199(18) 0.76483(15) 0.5527(4) 0.0262(7) Uani 1 1 d . . . . .
O2W O 0.5765(3) 0.66337(16) -0.3465(4) 0.0445(10) Uani 1 1 d . . . . .
H2WA H 0.573080 0.633624 -0.280356 0.067 Uiso 1 1 d GR . . . .
H2WB H 0.526264 0.662904 -0.412070 0.067 Uiso 1 1 d GR . . . .
O1W O 0.5539(2) 0.83168(16) -0.1858(5) 0.0443(10) Uani 1 1 d . . . . .
H1WA H 0.554276 0.858332 -0.252673 0.066 Uiso 1 1 d GR . . . .
H1WB H 0.503627 0.826912 -0.185072 0.066 Uiso 1 1 d GR . . . .
Br2B Br 1.1791(5) 1.0160(3) 0.9763(9) 0.053(2) Uani 0.353(4) 1 d . . P A 2
S48A S 1.1889(5) 1.0117(3) 0.9959(11) 0.0303(12) Uani 0.647(4) 1 d . . P A 1
O50A O 1.1271(3) 1.0168(3) 1.0642(7) 0.0415(16) Uani 0.647(4) 1 d . . P A 1
O49A O 1.1687(4) 1.0165(4) 0.8475(6) 0.054(2) Uani 0.647(4) 1 d . . P A 1
O51A O 1.2520(4) 1.0406(3) 1.0667(7) 0.0466(17) Uani 0.647(4) 1 d . . P A 1
F53A F 1.1589(4) 0.9135(3) 0.9588(9) 0.077(2) Uani 0.647(4) 1 d . . P A 1
F55A F 1.2713(4) 0.9350(3) 0.9657(10) 0.088(3) Uani 0.647(4) 1 d . . P A 1
F54A F 1.2333(4) 0.9319(3) 1.1530(8) 0.079(2) Uani 0.647(4) 1 d . . P A 1
C52A C 1.2140(6) 0.9461(5) 1.0242(13) 0.056(3) Uani 0.647(4) 1 d . . P A 1
O3B O 1.2487(13) 0.8746(10) 1.034(2) 0.110(7) Uani 0.353(4) 1 d . U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nd1 O18 2.389(3) . ?
Nd1 O19 2.444(3) 4_575 ?
Nd1 O28 2.486(3) 3_775 ?
Nd1 O29 2.383(4) 2_745 ?
Nd1 O39 2.441(3) 4_475 ?
Nd1 O38 2.372(3) 1_454 ?
Nd1 O2W 2.533(4) . ?
Nd1 O1W 2.495(4) . ?
S40 O43 1.424(4) . ?
S40 O42 1.423(5) . ?
S40 O41 1.436(5) . ?
S40 C44 1.819(7) . ?
O18 C17 1.236(6) . ?
F47 C44 1.323(8) . ?
F45 C44 1.317(7) . ?
N11 C10 1.512(6) . ?
N11 C16 1.342(6) . ?
N11 C12 1.341(6) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C1 1.499(7) . ?
C4 C8 1.508(7) . ?
C4 C5 1.392(7) . ?
C4 C3 1.410(7) . ?
F46 C44 1.343(8) . ?
C14 C15 1.386(7) . ?
C14 C17 1.521(6) . ?
C14 C13 1.380(7) . ?
C6 C5 1.410(7) . ?
C6 C1 1.410(7) . ?
C6 C9 1.494(8) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C16 H16 0.9500 . ?
C16 C15 1.374(7) . ?
C15 H15 0.9500 . ?
C17 O19 1.249(6) . ?
C5 C30 1.503(6) . ?
C12 H12 0.9500 . ?
C12 C13 1.373(7) . ?
N21 C20 1.512(6) . ?
N21 C26 1.349(8) . ?
N21 C22 1.329(8) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C3 1.500(8) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C7 C2 1.523(7) . ?
C1 C2 1.392(8) . ?
C23 H23 0.9500 . ?
C23 C22 1.380(8) . ?
C23 C24 1.387(7) . ?
C3 C2 1.395(7) . ?
C26 H26 0.9500 . ?
C26 C25 1.389(8) . ?
C13 H13 0.9500 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 N31 1.495(5) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C22 H22 0.9500 . ?
C25 H25 0.9500 . ?
C25 C24 1.381(8) . ?
N31 C36 1.363(6) . ?
N31 C32 1.343(6) . ?
C35 H35 0.9500 . ?
C35 C36 1.374(7) . ?
C35 C34 1.378(7) . ?
C36 H36 0.9500 . ?
C27 C24 1.518(7) . ?
C27 O28 1.242(6) . ?
C27 O29 1.257(6) . ?
C32 H32 0.9500 . ?
C32 C33 1.374(7) . ?
C37 C34 1.504(6) . ?
C37 O39 1.260(6) . ?
C37 O38 1.237(6) . ?
C34 C33 1.391(7) . ?
C33 H33 0.9500 . ?
O2W H2WA 1.0161 . ?
O2W H2WB 1.0168 . ?
O1W H1WA 0.9518 . ?
O1W H1WB 0.9535 . ?
S48A O50A 1.471(11) . ?
S48A O49A 1.432(12) . ?
S48A O51A 1.439(10) . ?
S48A C52A 1.757(13) . ?
F53A C52A 1.373(14) . ?
F55A C52A 1.358(13) . ?
F54A C52A 1.292(14) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O18 Nd1 O19 89.19(14) . 4_575 ?
O18 Nd1 O28 76.07(13) . 3_775 ?
O18 Nd1 O39 110.40(12) . 4_475 ?
O18 Nd1 O2W 141.49(16) . . ?
O18 Nd1 O1W 75.59(16) . . ?
O19 Nd1 O28 74.13(13) 4_575 3_775 ?
O19 Nd1 O2W 72.90(15) 4_575 . ?
O19 Nd1 O1W 146.25(15) 4_575 . ?
O28 Nd1 O2W 127.74(13) 3_775 . ?
O28 Nd1 O1W 73.04(14) 3_775 . ?
O29 Nd1 O18 71.86(16) 2_745 . ?
O29 Nd1 O19 79.65(12) 2_745 4_575 ?
O29 Nd1 O28 138.46(14) 2_745 3_775 ?
O29 Nd1 O39 74.55(12) 2_745 4_475 ?
O29 Nd1 O2W 71.53(15) 2_745 . ?
O29 Nd1 O1W 121.81(14) 2_745 . ?
O39 Nd1 O19 140.15(14) 4_475 4_575 ?
O39 Nd1 O28 142.89(12) 4_475 3_775 ?
O39 Nd1 O2W 70.40(14) 4_475 . ?
O39 Nd1 O1W 73.54(13) 4_475 . ?
O38 Nd1 O18 147.55(16) 1_454 . ?
O38 Nd1 O19 103.66(12) 1_454 4_575 ?
O38 Nd1 O28 79.01(12) 1_454 3_775 ?
O38 Nd1 O29 139.22(15) 1_454 2_745 ?
O38 Nd1 O39 78.48(11) 1_454 4_475 ?
O38 Nd1 O2W 70.89(14) 1_454 . ?
O38 Nd1 O1W 77.51(14) 1_454 . ?
O1W Nd1 O2W 135.71(15) . . ?
O43 S40 O41 112.9(4) . . ?
O43 S40 C44 103.3(3) . . ?
O42 S40 O43 114.9(3) . . ?
O42 S40 O41 116.1(4) . . ?
O42 S40 C44 104.3(3) . . ?
O41 S40 C44 103.2(3) . . ?
C17 O18 Nd1 167.2(4) . . ?
C16 N11 C10 117.3(4) . . ?
C12 N11 C10 121.8(4) . . ?
C12 N11 C16 120.9(4) . . ?
N11 C10 H10A 108.9 . . ?
N11 C10 H10B 108.9 . . ?
H10A C10 H10B 107.7 . . ?
C1 C10 N11 113.2(4) . . ?
C1 C10 H10A 108.9 . . ?
C1 C10 H10B 108.9 . . ?
C5 C4 C8 121.1(4) . . ?
C5 C4 C3 119.2(4) . . ?
C3 C4 C8 119.6(5) . . ?
C15 C14 C17 119.6(4) . . ?
C13 C14 C15 119.2(4) . . ?
C13 C14 C17 121.2(4) . . ?
C5 C6 C1 118.1(5) . . ?
C5 C6 C9 121.5(5) . . ?
C1 C6 C9 120.4(5) . . ?
C4 C8 H8A 109.5 . . ?
C4 C8 H8B 109.5 . . ?
C4 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N11 C16 H16 119.6 . . ?
N11 C16 C15 120.9(4) . . ?
C15 C16 H16 119.6 . . ?
C14 C15 H15 120.5 . . ?
C16 C15 C14 118.9(4) . . ?
C16 C15 H15 120.5 . . ?
F47 C44 S40 111.6(4) . . ?
F47 C44 F46 105.9(5) . . ?
F45 C44 S40 112.1(5) . . ?
F45 C44 F47 106.6(5) . . ?
F45 C44 F46 108.5(6) . . ?
F46 C44 S40 111.7(4) . . ?
O18 C17 C14 117.3(4) . . ?
O18 C17 O19 126.1(4) . . ?
O19 C17 C14 116.6(4) . . ?
C4 C5 C6 121.2(4) . . ?
C4 C5 C30 118.3(4) . . ?
C6 C5 C30 120.2(5) . . ?
N11 C12 H12 119.8 . . ?
N11 C12 C13 120.4(4) . . ?
C13 C12 H12 119.8 . . ?
C26 N21 C20 116.4(5) . . ?
C22 N21 C20 121.4(5) . . ?
C22 N21 C26 122.0(5) . . ?
N21 C20 H20A 108.9 . . ?
N21 C20 H20B 108.9 . . ?
H20A C20 H20B 107.8 . . ?
C3 C20 N21 113.2(4) . . ?
C3 C20 H20A 108.9 . . ?
C3 C20 H20B 108.9 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
C6 C1 C10 118.9(5) . . ?
C2 C1 C10 119.7(5) . . ?
C2 C1 C6 121.4(5) . . ?
C22 C23 H23 120.3 . . ?
C22 C23 C24 119.4(5) . . ?
C24 C23 H23 120.3 . . ?
C4 C3 C20 118.3(5) . . ?
C2 C3 C4 120.6(5) . . ?
C2 C3 C20 120.9(5) . . ?
N21 C26 H26 120.5 . . ?
N21 C26 C25 118.9(5) . . ?
C25 C26 H26 120.5 . . ?
C14 C13 H13 120.2 . . ?
C12 C13 C14 119.7(4) . . ?
C12 C13 H13 120.2 . . ?
C5 C30 H30A 108.5 . . ?
C5 C30 H30B 108.5 . . ?
H30A C30 H30B 107.5 . . ?
N31 C30 C5 115.2(4) . . ?
N31 C30 H30A 108.5 . . ?
N31 C30 H30B 108.5 . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N21 C22 C23 120.7(5) . . ?
N21 C22 H22 119.7 . . ?
C23 C22 H22 119.7 . . ?
C26 C25 H25 119.8 . . ?
C24 C25 C26 120.3(5) . . ?
C24 C25 H25 119.8 . . ?
C1 C2 C7 120.1(5) . . ?
C1 C2 C3 119.4(5) . . ?
C3 C2 C7 120.6(5) . . ?
C17 O19 Nd1 133.2(3) . 4_576 ?
C36 N31 C30 120.3(4) . . ?
C32 N31 C30 118.3(4) . . ?
C32 N31 C36 121.2(4) . . ?
C36 C35 H35 119.6 . . ?
C36 C35 C34 120.7(4) . . ?
C34 C35 H35 119.6 . . ?
N31 C36 C35 119.1(4) . . ?
N31 C36 H36 120.4 . . ?
C35 C36 H36 120.4 . . ?
O28 C27 C24 117.5(4) . . ?
O28 C27 O29 127.8(5) . . ?
O29 C27 C24 114.7(5) . . ?
C23 C24 C27 122.3(5) . . ?
C25 C24 C23 118.6(5) . . ?
C25 C24 C27 119.0(5) . . ?
N31 C32 H32 119.6 . . ?
N31 C32 C33 120.8(4) . . ?
C33 C32 H32 119.6 . . ?
C27 O28 Nd1 134.2(3) . 3_775 ?
C27 O29 Nd1 156.8(4) . 2_755 ?
O39 C37 C34 116.5(4) . . ?
O38 C37 C34 118.1(4) . . ?
O38 C37 O39 125.4(4) . . ?
C35 C34 C37 121.9(4) . . ?
C35 C34 C33 118.8(4) . . ?
C33 C34 C37 119.2(4) . . ?
C32 C33 C34 119.2(5) . . ?
C32 C33 H33 120.4 . . ?
C34 C33 H33 120.4 . . ?
C37 O39 Nd1 126.1(3) . 4_676 ?
C37 O38 Nd1 174.3(3) . 1_656 ?
Nd1 O2W H2WA 115.7 . . ?
Nd1 O2W H2WB 115.7 . . ?
H2WA O2W H2WB 102.6 . . ?
Nd1 O1W H1WA 113.5 . . ?
Nd1 O1W H1WB 113.7 . . ?
H1WA O1W H1WB 104.9 . . ?
O50A S48A C52A 102.8(6) . . ?
O49A S48A O50A 113.8(8) . . ?
O49A S48A O51A 117.0(7) . . ?
O49A S48A C52A 104.2(7) . . ?
O51A S48A O50A 112.3(7) . . ?
O51A S48A C52A 104.9(8) . . ?
F53A C52A S48A 111.3(8) . . ?
F55A C52A S48A 110.0(8) . . ?
F55A C52A F53A 104.9(10) . . ?
F54A C52A S48A 115.6(10) . . ?
F54A C52A F53A 107.9(9) . . ?
F54A C52A F55A 106.5(9) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Nd1 O18 C17 C14 133.4(14) . . . . ?
Nd1 O18 C17 O19 -47(2) . . . . ?
O18 C17 O19 Nd1 -0.3(10) . . . 4_576 ?
O43 S40 C44 F47 -56.5(5) . . . . ?
O43 S40 C44 F45 -176.0(5) . . . . ?
O43 S40 C44 F46 61.9(5) . . . . ?
O42 S40 C44 F47 -176.9(4) . . . . ?
O42 S40 C44 F45 63.6(6) . . . . ?
O42 S40 C44 F46 -58.5(5) . . . . ?
N11 C10 C1 C6 79.6(6) . . . . ?
N11 C10 C1 C2 -100.0(6) . . . . ?
N11 C16 C15 C14 0.7(8) . . . . ?
N11 C12 C13 C14 -0.7(8) . . . . ?
C10 N11 C16 C15 -177.0(5) . . . . ?
C10 N11 C12 C13 176.9(5) . . . . ?
C10 C1 C2 C7 1.6(8) . . . . ?
C10 C1 C2 C3 -178.8(4) . . . . ?
O41 S40 C44 F47 61.3(5) . . . . ?
O41 S40 C44 F45 -58.1(6) . . . . ?
O41 S40 C44 F46 179.7(5) . . . . ?
C4 C5 C30 N31 -83.6(6) . . . . ?
C4 C3 C2 C7 177.6(5) . . . . ?
C4 C3 C2 C1 -1.9(7) . . . . ?
C14 C17 O19 Nd1 179.0(3) . . . 4_576 ?
C6 C5 C30 N31 103.3(5) . . . . ?
C6 C1 C2 C7 -177.9(5) . . . . ?
C6 C1 C2 C3 1.7(7) . . . . ?
C8 C4 C5 C6 -178.8(4) . . . . ?
C8 C4 C5 C30 8.1(6) . . . . ?
C8 C4 C3 C20 -2.8(7) . . . . ?
C8 C4 C3 C2 -177.8(5) . . . . ?
C16 N11 C10 C1 -171.3(5) . . . . ?
C16 N11 C12 C13 -0.5(8) . . . . ?
C15 C14 C17 O18 0.8(8) . . . . ?
C15 C14 C17 O19 -178.5(5) . . . . ?
C15 C14 C13 C12 1.9(8) . . . . ?
C17 C14 C15 C16 177.7(5) . . . . ?
C17 C14 C13 C12 -177.7(5) . . . . ?
C5 C4 C3 C20 173.8(4) . . . . ?
C5 C4 C3 C2 -1.2(7) . . . . ?
C5 C6 C1 C10 -177.9(4) . . . . ?
C5 C6 C1 C2 1.7(7) . . . . ?
C5 C30 N31 C36 -39.6(7) . . . . ?
C5 C30 N31 C32 144.8(5) . . . . ?
C12 N11 C10 C1 11.2(8) . . . . ?
C12 N11 C16 C15 0.5(8) . . . . ?
N21 C20 C3 C4 88.1(6) . . . . ?
N21 C20 C3 C2 -96.9(6) . . . . ?
N21 C26 C25 C24 1.0(10) . . . . ?
C20 N21 C26 C25 -174.2(6) . . . . ?
C20 N21 C22 C23 173.6(5) . . . . ?
C20 C3 C2 C7 2.8(8) . . . . ?
C20 C3 C2 C1 -176.7(5) . . . . ?
C1 C6 C5 C4 -4.9(6) . . . . ?
C1 C6 C5 C30 168.1(4) . . . . ?
C3 C4 C5 C6 4.7(7) . . . . ?
C3 C4 C5 C30 -168.5(4) . . . . ?
C26 N21 C20 C3 -148.5(5) . . . . ?
C26 N21 C22 C23 -0.3(9) . . . . ?
C26 C25 C24 C23 -1.6(9) . . . . ?
C26 C25 C24 C27 176.4(6) . . . . ?
C13 C14 C15 C16 -1.9(8) . . . . ?
C13 C14 C17 O18 -179.6(5) . . . . ?
C13 C14 C17 O19 1.1(8) . . . . ?
C30 N31 C36 C35 -172.7(5) . . . . ?
C30 N31 C32 C33 172.9(5) . . . . ?
C9 C6 C5 C4 176.0(5) . . . . ?
C9 C6 C5 C30 -11.0(7) . . . . ?
C9 C6 C1 C10 1.3(7) . . . . ?
C9 C6 C1 C2 -179.2(5) . . . . ?
C22 N21 C20 C3 37.3(7) . . . . ?
C22 N21 C26 C25 -0.1(9) . . . . ?
C22 C23 C24 C25 1.2(8) . . . . ?
C22 C23 C24 C27 -176.8(5) . . . . ?
N31 C32 C33 C34 -0.2(9) . . . . ?
C35 C34 C33 C32 2.8(8) . . . . ?
C36 N31 C32 C33 -2.5(8) . . . . ?
C36 C35 C34 C37 174.4(5) . . . . ?
C36 C35 C34 C33 -2.6(8) . . . . ?
C24 C23 C22 N21 -0.3(9) . . . . ?
C24 C27 O28 Nd1 173.5(3) . . . 3_775 ?
C24 C27 O29 Nd1 -118.3(8) . . . 2_755 ?
C32 N31 C36 C35 2.7(8) . . . . ?
O28 C27 C24 C23 8.7(8) . . . . ?
O28 C27 C24 C25 -169.2(5) . . . . ?
O28 C27 O29 Nd1 61.2(11) . . . 2_755 ?
O29 C27 C24 C23 -171.7(5) . . . . ?
O29 C27 C24 C25 10.4(8) . . . . ?
O29 C27 O28 Nd1 -6.0(9) . . . 3_775 ?
C37 C34 C33 C32 -174.3(5) . . . . ?
C34 C35 C36 N31 -0.1(8) . . . . ?
C34 C37 O39 Nd1 -177.6(3) . . . 4_676 ?
O39 C37 C34 C35 -13.7(7) . . . . ?
O39 C37 C34 C33 163.3(5) . . . . ?
O38 C37 C34 C35 167.7(5) . . . . ?
O38 C37 C34 C33 -15.3(7) . . . . ?
O38 C37 O39 Nd1 0.9(7) . . . 4_676 ?
O50A S48A C52A F53A 63.9(10) . . . . ?
O50A S48A C52A F55A 179.7(9) . . . . ?
O50A S48A C52A F54A -59.7(11) . . . . ?
O49A S48A C52A F53A -55.0(10) . . . . ?
O49A S48A C52A F55A 60.8(11) . . . . ?
O49A S48A C52A F54A -178.6(9) . . . . ?
O51A S48A C52A F53A -178.5(8) . . . . ?
O51A S48A C52A F55A -62.7(11) . . . . ?
O51A S48A C52A F54A 57.9(11) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.221 0.708 0.333 15.7 12.9 ?
2 0.221 0.792 0.833 15.7 12.9 ?
3 0.500 0.500 -0.588 450.5 126.3 '12x water'
4 0.500 0.000 -0.273 450.5 126.3 '12x water'
5 0.779 0.208 0.167 15.7 12.4 ?
6 0.779 0.292 0.667 15.7 12.4 ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.175
_oxdiff_exptl_absorpt_empirical_full_min 0.889
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_jj003_br_nd_otf_koh_h2o_test1_red3
_database_code_depnum_ccdc_archive 'CCDC 1833433'
loop_
_audit_author_name
_audit_author_address
'Antti Tiihonen'
;University of Jyv?skyl?, Department of Chemistry
Finland
;
_audit_update_record             
;
2018-03-29 deposited with the CCDC.	2019-02-28 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT420_I                   
;
PROBLEM: D-H Without Acceptor       O       --H 
RESPONSE: Hydrogen bond acceptor (water) have been removed among the other 
disordered solvents (also water) from the voids (see vrf_CHEMW03_ALERT_2_A).
;
_vrf_PLAT417_I                   
;
PROBLEM: Short Inter D-H..H-D H1WA ..H29 
RESPONSE: hydrogen atoms generated with riding model to their
general (unoptimized) positions.
;
_vrf_PLAT772_I                   
;
PROBLEM: Suspect O-H Bond in CIF: O38A     --H38A 
RESPONSE:Hydrogen atom shared between dimerized carboxylic acid units 
("charged proton"). Location found in electron density map.
;
# end Validation Reply Form
_audit_creation_date             2018-03-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C60 H59 N6 O10, 5(Br), 4(H2 O), 2(O)'
_chemical_formula_sum            'C60 H67 Br5 N6 O16'
_chemical_formula_weight         1527.74
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.1828(6)
_cell_length_b                   13.1617(5)
_cell_length_c                   13.3823(7)
_cell_angle_alpha                103.662(4)
_cell_angle_beta                 114.054(5)
_cell_angle_gamma                106.336(4)
_cell_volume                     1581.63(14)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    5073
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      28.6490
_cell_measurement_theta_min      1.7620
_shelx_estimated_absorpt_T_max   0.795
_shelx_estimated_absorpt_T_min   0.364
_exptl_absorpt_coefficient_mu    3.248
_exptl_absorpt_correction_T_max  0.856
_exptl_absorpt_correction_T_min  0.559
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plank
_exptl_crystal_F_000             772
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-2 1 -15 0.0199
-2 18 -6 0.2068
1 -2 16 0.0478
-15 1 7 0.0440
1 -18 7 0.1787
-14 13 2 0.1377
9 -9 10 0.0894
1 -14 15 0.1364
5 1 -18 0.0484
15 0 -8 0.0661
12 -15 -3 0.1366
-5 12 10 0.1463
-9 9 14 0.1180
14 0 -2 0.0610
5 5 9 0.0877
2 3 13 0.0674

_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.131
_exptl_crystal_size_min          0.074
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-1.9861 1.0011 -15.0042 0.3455 0.9372 -0.1584
-1.9972 17.9958 -6.0029 -0.7080 0.4079 0.5444
0.9858 -2.0003 16.0046 -0.3358 -0.9500 0.0617
-15.0006 1.0069 7.0034 -0.3926 0.2466 -0.8680
0.9967 -17.9953 7.0033 0.6703 -0.4217 -0.6023
-13.9988 13.0030 2.0010 -0.8134 0.4749 -0.3636
8.9893 -9.0020 10.0026 0.2424 -0.9458 0.2629
0.9889 -13.9967 15.0053 0.2604 -0.8804 -0.4087
5.0139 0.9977 -18.0057 0.4993 0.8065 0.2661
15.0013 -0.0071 -8.0038 0.3728 -0.1908 0.9020
12.0023 -15.0040 -3.0020 0.9156 -0.3299 0.1558
-5.0119 12.0010 10.0047 -0.8951 -0.3658 0.2000
-9.0135 9.0030 14.0069 -0.9038 -0.4178 -0.1480
13.9960 -0.0064 -2.0021 0.1973 -0.4887 0.8681
4.9869 4.9970 9.0035 -0.4342 -0.7318 0.5505
1.9845 2.9985 13.0056 -0.4801 -0.8279 0.3039

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_av_unetI/netI     0.0471
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11112
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.997
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_min         1.759
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3953
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -57.00  35.00   1.00   15.00    --    8.98 -57.00 -90.00   92
  2  ω    -16.00  81.00   1.00   15.00    --    8.98  57.00  60.00   97
  3  ω    -20.00  50.00   1.00   15.00    --    8.98 -99.00-180.00   70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0101359000
_diffrn_orient_matrix_UB_12      -0.0474036000
_diffrn_orient_matrix_UB_13      -0.0275326000
_diffrn_orient_matrix_UB_21      -0.0430462000
_diffrn_orient_matrix_UB_22      -0.0010724000
_diffrn_orient_matrix_UB_23      -0.0568388000
_diffrn_orient_matrix_UB_31      0.0627336000
_diffrn_orient_matrix_UB_32      0.0388273000
_diffrn_orient_matrix_UB_33      0.0048443000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5077
_reflns_number_total             6149
_reflns_odcompleteness_completeness 97.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         1.126
_refine_diff_density_min         -0.864
_refine_diff_density_rms         0.088
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         6149
_refine_ls_number_restraints     47
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0402
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0313P)²+3.0141P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0869
_refine_ls_wR_factor_ref         0.0944
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O39A-H38A_$1
 1.4 with sigma of 0.02
 O38A-H38A
 1.3 with sigma of 0.02
 C37-O39C
 1.2 with sigma of 0.02
3. Restrained planarity
 O39C, C37, O38C, C34
 with sigma of 0.1
 O39B, O38B, C37, C34
 with sigma of 0.1
 O38C, C37, O39C, C34
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(O38B) \\sim Ueq, Uanis(O38A) \\sim Ueq, Uanis(O38C) \\sim Ueq,
Uanis(O39B) \\sim Ueq, Uanis(O39A) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(O39C)
\\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.006
Uanis(O38B) = Uanis(O38A) = Uanis(O38C)
Uanis(O39B) = Uanis(O39A) = Uanis(O39C)
5. Others
 Fixed Sof: O38A(0.5) H38A(0.5) O39A(0.5) O38B(0.3) O39B(0.3) O38C(0.2)
 O39C(0.2)
 Fixed Uiso: H38A(0.05)
6.a Free rotating group:
 O2W(H2WA,H2WB), O1W(H1WA,H1WB)
6.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C20(H20A,H20B), C30(H30A,H30B)
6.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C15(H15), C16(H16), C22(H22), C23(H23), C25(H25),
 C26(H26), C32(H32), C33(H33), C35(H35), C36(H36)
6.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C)
6.e Idealised tetrahedral OH refined as rotating group:
 O19(H19), O29(H29)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6174(4) 0.7147(3) 0.1271(3) 0.0196(7) Uani 1 1 d . . . . .
C2 C 0.4845(4) 0.6850(3) 0.1229(3) 0.0177(7) Uani 1 1 d . . . . .
C3 C 0.3562(4) 0.6301(3) 0.0124(3) 0.0186(7) Uani 1 1 d . . . . .
C4 C 0.3586(4) 0.5990(3) -0.0945(3) 0.0209(7) Uani 1 1 d . . . . .
C5 C 0.4921(4) 0.6221(3) -0.0881(3) 0.0221(7) Uani 1 1 d . . . . .
C6 C 0.6215(4) 0.6835(3) 0.0215(3) 0.0233(8) Uani 1 1 d . . . . .
C7 C 0.7649(4) 0.7175(4) 0.0257(4) 0.0360(10) Uani 1 1 d . . . . .
H7A H 0.830721 0.796752 0.084993 0.054 Uiso 1 1 calc GR . . . .
H7B H 0.749686 0.712880 -0.053032 0.054 Uiso 1 1 calc GR . . . .
H7C H 0.807364 0.664839 0.047844 0.054 Uiso 1 1 calc GR . . . .
C8 C 0.4798(4) 0.7146(3) 0.2373(3) 0.0221(7) Uani 1 1 d . . . . .
H8A H 0.481392 0.791485 0.261179 0.033 Uiso 1 1 calc GR . . . .
H8B H 0.564087 0.713962 0.300514 0.033 Uiso 1 1 calc GR . . . .
H8C H 0.391038 0.657324 0.224348 0.033 Uiso 1 1 calc GR . . . .
C9 C 0.2196(4) 0.5443(3) -0.2141(3) 0.0319(9) Uani 1 1 d . . . . .
H9A H 0.165179 0.463893 -0.230139 0.048 Uiso 1 1 calc GR . . . .
H9B H 0.242495 0.546454 -0.277123 0.048 Uiso 1 1 calc GR . . . .
H9C H 0.161062 0.587182 -0.212537 0.048 Uiso 1 1 calc GR . . . .
C10 C 0.7555(4) 0.7766(3) 0.2468(3) 0.0211(7) Uani 1 1 d . . . . .
H10A H 0.752435 0.731422 0.296011 0.025 Uiso 1 1 calc R . . . .
H10B H 0.838420 0.781439 0.235012 0.025 Uiso 1 1 calc R . . . .
C12 C 0.8136(4) 0.9295(3) 0.4275(3) 0.0255(8) Uani 1 1 d . . . . .
H12 H 0.816934 0.875647 0.463808 0.031 Uiso 1 1 calc R . . . .
C13 C 0.8450(4) 1.0407(3) 0.4929(3) 0.0248(8) Uani 1 1 d . . . . .
H13 H 0.868909 1.063688 0.573991 0.030 Uiso 1 1 calc R . . . .
C14 C 0.8414(4) 1.1188(3) 0.4399(3) 0.0223(7) Uani 1 1 d . . . . .
C15 C 0.8008(4) 1.0821(3) 0.3200(3) 0.0261(8) Uani 1 1 d . . . . .
H15 H 0.794081 1.133808 0.281177 0.031 Uiso 1 1 calc R . . . .
C16 C 0.7705(4) 0.9699(3) 0.2584(3) 0.0257(8) Uani 1 1 d . . . . .
H16 H 0.743706 0.944213 0.176649 0.031 Uiso 1 1 calc R . . . .
C17 C 0.8793(4) 1.2410(3) 0.5146(3) 0.0242(8) Uani 1 1 d . . . . .
C20 C 0.2132(4) 0.6012(3) 0.0084(3) 0.0217(7) Uani 1 1 d . . . . .
H20A H 0.133468 0.556463 -0.075619 0.026 Uiso 1 1 calc R . . . .
H20B H 0.205202 0.551732 0.052907 0.026 Uiso 1 1 calc R . . . .
C22 C 0.1525(4) 0.7097(3) 0.1407(3) 0.0249(8) Uani 1 1 d . . . . .
H22 H 0.140227 0.648725 0.167247 0.030 Uiso 1 1 calc R . . . .
C23 C 0.1258(4) 0.8001(3) 0.1843(3) 0.0255(8) Uani 1 1 d . . . . .
H23 H 0.097609 0.803168 0.242578 0.031 Uiso 1 1 calc R . . . .
C24 C 0.1400(4) 0.8868(3) 0.1432(3) 0.0236(8) Uani 1 1 d . . . . .
C25 C 0.1881(4) 0.8837(3) 0.0623(3) 0.0281(8) Uani 1 1 d . . . . .
H25 H 0.201391 0.944072 0.034996 0.034 Uiso 1 1 calc R . . . .
C26 C 0.2164(4) 0.7915(3) 0.0223(3) 0.0256(8) Uani 1 1 d . . . . .
H26 H 0.250293 0.788561 -0.032426 0.031 Uiso 1 1 calc R . . . .
C27 C 0.1003(4) 0.9818(3) 0.1875(3) 0.0271(8) Uani 1 1 d . . . . .
C30 C 0.4968(4) 0.5808(3) -0.2006(3) 0.0268(8) Uani 1 1 d . . . . .
H30A H 0.582638 0.564071 -0.181940 0.032 Uiso 1 1 calc R . . A .
H30B H 0.409781 0.507631 -0.258502 0.032 Uiso 1 1 calc R . . A .
C32 C 0.4979(4) 0.7667(3) -0.2141(3) 0.0319(9) Uani 1 1 d . . . B 1
H32 H 0.489399 0.785227 -0.144956 0.038 Uiso 1 1 calc R . . B 1
C33 C 0.5043(5) 0.8430(4) -0.2680(4) 0.0394(10) Uani 1 1 d . . . B 1
H33 H 0.500675 0.913917 -0.236032 0.047 Uiso 1 1 calc R . . B 1
C34 C 0.5160(5) 0.8171(4) -0.3678(4) 0.0444(11) Uani 1 1 d . . . B 1
C35 C 0.5216(7) 0.7144(5) -0.4102(5) 0.0673(17) Uani 1 1 d . . . B 1
H35 H 0.530043 0.694516 -0.479336 0.081 Uiso 1 1 calc R . . B 1
C36 C 0.5154(6) 0.6395(4) -0.3546(4) 0.0547(14) Uani 1 1 d . . . B 1
H36 H 0.519608 0.568555 -0.385182 0.066 Uiso 1 1 calc R . . B 1
C37 C 0.5325(7) 0.9038(6) -0.4213(6) 0.0719(17) Uani 1 1 d D U . B 1
N11 N 0.7783(3) 0.8965(2) 0.3125(2) 0.0197(6) Uani 1 1 d . . . . .
N21 N 0.1961(3) 0.7061(2) 0.0605(3) 0.0210(6) Uani 1 1 d . . . . .
N31 N 0.5033(3) 0.6659(3) -0.2578(3) 0.0271(7) Uani 1 1 d . . . B 1
O18 O 0.9329(3) 1.2748(2) 0.6214(2) 0.0322(6) Uani 1 1 d . . . . .
O19 O 0.8476(3) 1.3004(2) 0.4502(2) 0.0306(6) Uani 1 1 d . . . . .
H19 H 0.866588 1.366673 0.494344 0.046 Uiso 1 1 calc GR . . . .
O28 O 0.0431(3) 0.9754(2) 0.2470(2) 0.0353(7) Uani 1 1 d . . . . .
O29 O 0.1302(3) 1.0648(2) 0.1519(3) 0.0353(7) Uani 1 1 d . . . . .
H29 H 0.103879 1.114197 0.176914 0.053 Uiso 1 1 calc GR . . . .
O38A O 0.4960(11) 0.8745(7) -0.5262(8) 0.0683(18) Uani 0.5 1 d D U . B 1
H38A H 0.428(7) 0.935(6) -0.567(6) 0.050 Uiso 0.5 1 d D . . C 1
O39A O 0.5421(9) 1.0105(7) -0.3628(7) 0.0606(17) Uani 0.5 1 d D U . B 1
Br1 Br 0.500000 1.000000 0.000000 0.03580(15) Uani 1 2 d S T P . .
Br2 Br 0.83705(4) 1.55099(3) 0.80088(3) 0.02796(11) Uani 1 1 d . . . . .
Br3 Br 0.77530(4) 1.66882(3) 0.48340(3) 0.03024(11) Uani 1 1 d . . . . .
O2W O 0.9068(3) 1.5013(2) 0.5810(3) 0.0352(7) Uani 1 1 d . . . . .
H2WA H 0.887124 1.507611 0.636561 0.053 Uiso 1 1 d G . . . .
H2WB H 0.872458 1.537673 0.540923 0.053 Uiso 1 1 d G . . . .
O1W O 0.0426(3) 1.2094(2) 0.2263(2) 0.0329(6) Uani 1 1 d . . . . .
H1WA H 0.087695 1.229657 0.301485 0.049 Uiso 1 1 d G . . . .
H1WB H 0.065806 1.268246 0.210344 0.049 Uiso 1 1 d G . . . .
O38B O 0.6224(16) 0.9098(11) -0.4579(12) 0.0683(18) Uani 0.3 1 d . U . D 3
O39B O 0.4699(15) 0.9633(12) -0.4035(12) 0.0606(17) Uani 0.3 1 d . U . E 3
O38C O 0.407(3) 0.8381(18) -0.5598(19) 0.0683(18) Uani 0.2 1 d . U . F 2
O39C O 0.610(2) 0.9832(17) -0.3904(17) 0.0606(17) Uani 0.2 1 d D U . G 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.400(5) . ?
C1 C6 1.398(5) . ?
C1 C10 1.509(5) . ?
C2 C3 1.397(5) . ?
C2 C8 1.514(5) . ?
C3 C4 1.405(5) . ?
C3 C20 1.512(5) . ?
C4 C5 1.399(5) . ?
C4 C9 1.515(5) . ?
C5 C6 1.397(5) . ?
C5 C30 1.503(5) . ?
C6 C7 1.512(5) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 N11 1.504(4) . ?
C12 H12 0.9500 . ?
C12 C13 1.374(5) . ?
C12 N11 1.344(4) . ?
C13 H13 0.9500 . ?
C13 C14 1.381(5) . ?
C14 C15 1.389(5) . ?
C14 C17 1.509(5) . ?
C15 H15 0.9500 . ?
C15 C16 1.376(5) . ?
C16 H16 0.9500 . ?
C16 N11 1.338(4) . ?
C17 O18 1.204(4) . ?
C17 O19 1.306(4) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 N21 1.493(4) . ?
C22 H22 0.9500 . ?
C22 C23 1.363(5) . ?
C22 N21 1.344(4) . ?
C23 H23 0.9500 . ?
C23 C24 1.377(5) . ?
C24 C25 1.389(5) . ?
C24 C27 1.514(5) . ?
C25 H25 0.9500 . ?
C25 C26 1.380(5) . ?
C26 H26 0.9500 . ?
C26 N21 1.341(4) . ?
C27 O28 1.210(4) . ?
C27 O29 1.305(4) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 N31 1.500(5) . ?
C32 H32 0.9500 . ?
C32 C33 1.370(6) . ?
C32 N31 1.347(5) . ?
C33 H33 0.9500 . ?
C33 C34 1.367(6) . ?
C34 C35 1.367(7) . ?
C34 C37 1.491(7) . ?
C35 H35 0.9500 . ?
C35 C36 1.372(7) . ?
C36 H36 0.9500 . ?
C36 N31 1.331(5) . ?
C37 O38A 1.214(9) . ?
C37 O39A 1.388(10) . ?
O19 H19 0.8400 . ?
O29 H29 0.8400 . ?
O38A H38A 1.31(2) . ?
O2W H2WA 0.8496 . ?
O2W H2WB 0.8502 . ?
O1W H1WA 0.8496 . ?
O1W H1WB 0.8504 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C10 119.1(3) . . ?
C6 C1 C2 120.3(3) . . ?
C6 C1 C10 120.6(3) . . ?
C1 C2 C8 120.3(3) . . ?
C3 C2 C1 119.5(3) . . ?
C3 C2 C8 120.2(3) . . ?
C2 C3 C4 120.8(3) . . ?
C2 C3 C20 119.3(3) . . ?
C4 C3 C20 119.9(3) . . ?
C3 C4 C9 120.5(3) . . ?
C5 C4 C3 118.7(3) . . ?
C5 C4 C9 120.8(3) . . ?
C4 C5 C30 119.7(3) . . ?
C6 C5 C4 120.9(3) . . ?
C6 C5 C30 119.4(3) . . ?
C1 C6 C7 120.3(3) . . ?
C5 C6 C1 119.6(3) . . ?
C5 C6 C7 120.1(3) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C2 C8 H8A 109.5 . . ?
C2 C8 H8B 109.5 . . ?
C2 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C4 C9 H9A 109.5 . . ?
C4 C9 H9B 109.5 . . ?
C4 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C1 C10 H10A 109.2 . . ?
C1 C10 H10B 109.2 . . ?
H10A C10 H10B 107.9 . . ?
N11 C10 C1 112.2(3) . . ?
N11 C10 H10A 109.2 . . ?
N11 C10 H10B 109.2 . . ?
C13 C12 H12 119.8 . . ?
N11 C12 H12 119.8 . . ?
N11 C12 C13 120.4(3) . . ?
C12 C13 H13 120.3 . . ?
C12 C13 C14 119.5(3) . . ?
C14 C13 H13 120.3 . . ?
C13 C14 C15 119.2(3) . . ?
C13 C14 C17 118.3(3) . . ?
C15 C14 C17 122.4(3) . . ?
C14 C15 H15 120.5 . . ?
C16 C15 C14 119.0(3) . . ?
C16 C15 H15 120.5 . . ?
C15 C16 H16 119.7 . . ?
N11 C16 C15 120.6(3) . . ?
N11 C16 H16 119.7 . . ?
O18 C17 C14 120.9(3) . . ?
O18 C17 O19 126.7(3) . . ?
O19 C17 C14 112.3(3) . . ?
C3 C20 H20A 109.0 . . ?
C3 C20 H20B 109.0 . . ?
H20A C20 H20B 107.8 . . ?
N21 C20 C3 112.8(3) . . ?
N21 C20 H20A 109.0 . . ?
N21 C20 H20B 109.0 . . ?
C23 C22 H22 119.7 . . ?
N21 C22 H22 119.7 . . ?
N21 C22 C23 120.7(3) . . ?
C22 C23 H23 120.3 . . ?
C22 C23 C24 119.5(3) . . ?
C24 C23 H23 120.3 . . ?
C23 C24 C25 119.5(3) . . ?
C23 C24 C27 118.1(3) . . ?
C25 C24 C27 122.4(3) . . ?
C24 C25 H25 120.5 . . ?
C26 C25 C24 118.9(3) . . ?
C26 C25 H25 120.5 . . ?
C25 C26 H26 119.9 . . ?
N21 C26 C25 120.1(3) . . ?
N21 C26 H26 119.9 . . ?
O28 C27 C24 120.9(3) . . ?
O28 C27 O29 126.0(4) . . ?
O29 C27 C24 113.1(3) . . ?
C5 C30 H30A 108.9 . . ?
C5 C30 H30B 108.9 . . ?
H30A C30 H30B 107.7 . . ?
N31 C30 C5 113.6(3) . . ?
N31 C30 H30A 108.9 . . ?
N31 C30 H30B 108.9 . . ?
C33 C32 H32 119.5 . . ?
N31 C32 H32 119.5 . . ?
N31 C32 C33 120.9(4) . . ?
C32 C33 H33 120.0 . . ?
C34 C33 C32 120.0(4) . . ?
C34 C33 H33 120.0 . . ?
C33 C34 C37 119.6(5) . . ?
C35 C34 C33 117.9(4) . . ?
C35 C34 C37 122.3(5) . . ?
C34 C35 H35 119.5 . . ?
C34 C35 C36 121.0(4) . . ?
C36 C35 H35 119.5 . . ?
C35 C36 H36 119.9 . . ?
N31 C36 C35 120.3(5) . . ?
N31 C36 H36 119.9 . . ?
O38A C37 C34 121.3(7) . . ?
O38A C37 O39A 117.7(7) . . ?
O39A C37 C34 117.4(6) . . ?
C12 N11 C10 118.6(3) . . ?
C16 N11 C10 120.1(3) . . ?
C16 N11 C12 121.2(3) . . ?
C22 N21 C20 118.7(3) . . ?
C26 N21 C20 120.0(3) . . ?
C26 N21 C22 121.2(3) . . ?
C32 N31 C30 122.2(3) . . ?
C36 N31 C30 117.9(3) . . ?
C36 N31 C32 119.9(4) . . ?
C17 O19 H19 109.5 . . ?
C27 O29 H29 109.5 . . ?
C37 O38A H38A 107(3) . . ?
C37 O39A H38A 98(3) . 2_674 ?
H2WA O2W H2WB 109.5 . . ?
H1WA O1W H1WB 109.4 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C7 H7A O28 0.98 2.47 3.431(5) 165.1 1_655 yes
C7 H7B N31 0.98 2.75 3.468(5) 130.5 . yes
C9 H9A O18 0.98 2.59 3.445(4) 145.7 1_444 yes
C9 H9B N31 0.98 2.77 3.474(5) 129.5 . yes
C13 H13 O28 0.95 2.43 3.267(5) 146.5 2_676 yes
C23 H23 O18 0.95 2.38 3.226(4) 147.7 2_676 yes
O19 H19 O2W 0.84 1.69 2.525(4) 178.4 . yes
O29 H29 O1W 0.84 1.71 2.553(4) 177.1 . yes
O38A H38A O38A 1.31(2) 2.24(7) 3.177(17) 125(5) 2_674 yes
O38A H38A O39A 1.31(2) 1.40(2) 2.364(11) 122(2) 2_674 yes
O2W H2WA Br2 0.85 2.46 3.308(3) 173.0 . yes
O2W H2WB Br3 0.85 2.40 3.218(3) 162.0 . yes
O1W H1WA Br3 0.85 2.42 3.253(3) 166.9 2_686 yes
O1W H1WB Br2 0.85 2.39 3.232(2) 170.5 2_686 yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 3.4(5) . . . . ?
C1 C2 C3 C20 -178.3(3) . . . . ?
C1 C10 N11 C12 131.8(3) . . . . ?
C1 C10 N11 C16 -51.6(4) . . . . ?
C2 C1 C6 C5 -0.3(5) . . . . ?
C2 C1 C6 C7 178.9(3) . . . . ?
C2 C1 C10 N11 -66.8(4) . . . . ?
C2 C3 C4 C5 1.2(5) . . . . ?
C2 C3 C4 C9 -177.3(3) . . . . ?
C2 C3 C20 N21 64.0(4) . . . . ?
C3 C4 C5 C6 -5.4(5) . . . . ?
C3 C4 C5 C30 174.9(3) . . . . ?
C3 C20 N21 C22 -131.2(3) . . . . ?
C3 C20 N21 C26 52.4(4) . . . . ?
C4 C3 C20 N21 -117.7(3) . . . . ?
C4 C5 C6 C1 4.9(5) . . . . ?
C4 C5 C6 C7 -174.2(3) . . . . ?
C4 C5 C30 N31 89.5(4) . . . . ?
C5 C30 N31 C32 -3.2(5) . . . . ?
C5 C30 N31 C36 176.6(4) . . . . ?
C6 C1 C2 C3 -3.8(5) . . . . ?
C6 C1 C2 C8 177.6(3) . . . . ?
C6 C1 C10 N11 115.5(3) . . . . ?
C6 C5 C30 N31 -90.2(4) . . . . ?
C8 C2 C3 C4 -178.0(3) . . . . ?
C8 C2 C3 C20 0.3(4) . . . . ?
C9 C4 C5 C6 173.1(3) . . . . ?
C9 C4 C5 C30 -6.7(5) . . . . ?
C10 C1 C2 C3 178.5(3) . . . . ?
C10 C1 C2 C8 -0.1(4) . . . . ?
C10 C1 C6 C5 177.4(3) . . . . ?
C10 C1 C6 C7 -3.5(5) . . . . ?
C12 C13 C14 C15 2.4(5) . . . . ?
C12 C13 C14 C17 -178.7(3) . . . . ?
C13 C12 N11 C10 175.6(3) . . . . ?
C13 C12 N11 C16 -1.1(5) . . . . ?
C13 C14 C15 C16 -2.4(5) . . . . ?
C13 C14 C17 O18 11.5(5) . . . . ?
C13 C14 C17 O19 -168.7(3) . . . . ?
C14 C15 C16 N11 0.7(6) . . . . ?
C15 C14 C17 O18 -169.7(4) . . . . ?
C15 C14 C17 O19 10.1(5) . . . . ?
C15 C16 N11 C10 -175.5(3) . . . . ?
C15 C16 N11 C12 1.0(5) . . . . ?
C17 C14 C15 C16 178.8(3) . . . . ?
C20 C3 C4 C5 -177.1(3) . . . . ?
C20 C3 C4 C9 4.5(5) . . . . ?
C22 C23 C24 C25 -3.1(5) . . . . ?
C22 C23 C24 C27 176.1(3) . . . . ?
C23 C22 N21 C20 -175.4(3) . . . . ?
C23 C22 N21 C26 0.9(5) . . . . ?
C23 C24 C25 C26 1.9(5) . . . . ?
C23 C24 C27 O28 -7.8(5) . . . . ?
C23 C24 C27 O29 174.1(3) . . . . ?
C24 C25 C26 N21 0.6(5) . . . . ?
C25 C24 C27 O28 171.4(4) . . . . ?
C25 C24 C27 O29 -6.7(5) . . . . ?
C25 C26 N21 C20 174.2(3) . . . . ?
C25 C26 N21 C22 -2.1(5) . . . . ?
C27 C24 C25 C26 -177.3(3) . . . . ?
C30 C5 C6 C1 -175.3(3) . . . . ?
C30 C5 C6 C7 5.5(5) . . . . ?
C32 C33 C34 C35 -0.3(7) . . . . ?
C32 C33 C34 C37 -176.1(4) . . . . ?
C33 C32 N31 C30 179.9(4) . . . . ?
C33 C32 N31 C36 0.1(6) . . . . ?
C33 C34 C35 C36 0.2(8) . . . . ?
C33 C34 C37 O38A -155.2(7) . . . . ?
C33 C34 C37 O39A 2.9(8) . . . . ?
C34 C35 C36 N31 0.1(9) . . . . ?
C35 C34 C37 O38A 29.3(10) . . . . ?
C35 C34 C37 O39A -172.6(7) . . . . ?
C35 C36 N31 C30 180.0(5) . . . . ?
C35 C36 N31 C32 -0.2(7) . . . . ?
C37 C34 C35 C36 175.8(5) . . . . ?
N11 C12 C13 C14 -0.7(6) . . . . ?
N21 C22 C23 C24 1.7(5) . . . . ?
N31 C32 C33 C34 0.2(6) . . . . ?

_olex2_exptl_crystal_mounting_method 'Mitegen loop 100 micron'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.199
_oxdiff_exptl_absorpt_empirical_full_min 0.753
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_jj003_br_nd_oac_h2o_acet_12_red2
_database_code_depnum_ccdc_archive 'CCDC 1833431'
loop_
_audit_author_name
_audit_author_address
'Antti Tiihonen'
;University of Jyv?skyl?, Department of Chemistry
Finland
;
_audit_update_record             
;
2018-03-29 deposited with the CCDC.	2019-02-28 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_CHEMW03_I                   
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: The structure contains voids of unresolved electron density
which was treated using Olex2 solvent mask procedure (full details in 
_smtbx_masks_special_details). The 11 water molecules per asymmetric unit 
 are included in the formula and used in the calculations. 
;
_vrf_PLAT420_I                   
;
PROBLEM: D-H Without Acceptor       O2W      --H2WB
RESPONSE: Hydrogen bond acceptor (water) have been removed among the other 
disordered solvents (also water) from the voids (see vrf_CHEMW03_ALERT_2_A).
;
_vrf_FORMU01_I                   
;
PROBLEM: There is a discrepancy between the atom counts in the
            _chemical_formula_sum and _chemical_formula_moiety.
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_CELLZ01_I                   
;
PROBLEM: Difference between formula and atom_site contents detected.
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT041_I                   
;
PROBLEM: Calculated and Reported SumFormula strings Differ ...    
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT068_I                   
;
PROBLEM: Reported F000 Differs from Calcd (or Missing)...
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT606_I                   
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
# end Validation Reply Form
_audit_creation_date             2018-03-26
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C32 H34 N3 Nd O10, 2(Br)'
_chemical_formula_sum            'C32 H56 Br2 N3 Nd O21'
_chemical_formula_weight         1122.85
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C30 H30 N3 O12 Br3 Nd1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -3.1807 10.9079 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.1533(9)
_cell_length_b                   14.3573(13)
_cell_length_c                   18.8779(16)
_cell_angle_alpha                107.505(8)
_cell_angle_beta                 103.919(8)
_cell_angle_gamma                96.822(8)
_cell_volume                     2247.0(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5259
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      75.9880
_cell_measurement_theta_min      3.2570
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    11.590
_exptl_absorpt_correction_T_max  0.810
_exptl_absorpt_correction_T_min  0.494
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.660
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1134
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 8 -9 0.0180
6 -2 -1 0.0752
-6 2 1 0.0752
0 4 8 0.0322
0 -4 -8 0.0322
-1 -8 9 0.0180

_exptl_crystal_size_max          0.157
_exptl_crystal_size_mid          0.064
_exptl_crystal_size_min          0.036
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
1.0042 7.9941 -9.0056 0.9737 0.2354 0.0001
5.9955 -2.0009 -0.9988 -0.2056 0.9512 -0.3170
-5.9955 2.0009 0.9988 0.2056 -0.9512 0.3170
-0.0004 3.9977 8.0015 0.0510 -0.2180 -0.9479
0.0004 -3.9977 -8.0015 -0.0510 0.2180 0.9479
-1.0042 -7.9941 9.0056 -0.9737 -0.2354 -0.0001

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0427
_diffrn_reflns_av_unetI/netI     0.0653
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            13462
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.996
_diffrn_reflns_theta_min         3.299
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3953
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -66.00  32.00   2.00    2.00    --  -41.90  37.00 -90.00   49
  2  ω    -67.00  29.00   2.00    2.00    --  -41.90  57.00 120.00   48
  3  ω     45.00  97.00   2.00    2.00    --   41.90-125.00 -60.00   26
  4  ω     40.00 116.00   2.00    4.00    --  112.00-111.00  60.00   38
  5  ω     50.00  94.00   2.00    4.00    --  112.00-111.00 120.00   22
  6  ω     38.00 140.00   2.00    4.00    --  112.00 -30.00   0.00   51
  7  ω     88.00 178.00   2.00    4.00    --  112.00  45.00  30.00   45
  8  ω    111.00 163.00   2.00    4.00    --  112.00 111.00 -60.00   26
  9  ω    104.00 176.00   2.00    4.00    --  112.00 111.00 -30.00   36
 10  ω     40.00 140.00   2.00    4.00    --  112.00 -77.00-120.00   50
 11  ω     43.00 137.00   2.00    4.00    --  112.00 -30.00-150.00   47
 12  ω     36.00 116.00   2.00    4.00    --  112.00-111.00-180.00   40
 13  ω   -111.00 -17.00   2.00    2.00    --  -41.90 -57.00 -30.00   47
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0123039000
_diffrn_orient_matrix_UB_12      0.0835182000
_diffrn_orient_matrix_UB_13      -0.0353548000
_diffrn_orient_matrix_UB_21      0.1508765000
_diffrn_orient_matrix_UB_22      -0.0129235000
_diffrn_orient_matrix_UB_23      -0.0207832000
_diffrn_orient_matrix_UB_31      -0.0921469000
_diffrn_orient_matrix_UB_32      -0.0779771000
_diffrn_orient_matrix_UB_33      -0.0795076000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7156
_reflns_number_total             8126
_reflns_odcompleteness_completeness 99.06
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         1.213
_refine_diff_density_min         -1.939
_refine_diff_density_rms         0.127
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         8126
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0430
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0615P)²+0.0701P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1097
_refine_ls_wR_factor_ref         0.1163
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
2.b Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C10(H10A,H10B), C20(H20A,H20B)
2.c Aromatic/amide H refined with riding coordinates:
 C33(H33), C22(H22), C12(H12), C32(H32), C13(H13), C16(H16), C23(H23),
 C36(H36), C15(H15), C26(H26), C35(H35), C25(H25)
2.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C40(H40A,H40B,H40C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Nd1 Nd 0.71912(3) 1.01198(2) 0.49040(2) 0.01468(9) Uani 1 1 d . . . . .
Br1 Br 0.18978(6) 0.71675(4) 0.11293(3) 0.02382(13) Uani 1 1 d . . . . .
Br2 Br 0.70130(7) 0.49644(5) 0.17285(4) 0.03151(15) Uani 1 1 d . . . . .
O38 O 0.4374(4) 0.1615(2) -0.4146(2) 0.0188(7) Uani 1 1 d . . . . .
O29 O -0.0399(7) 0.8833(5) -0.3131(3) 0.0607(17) Uani 1 1 d . . . . .
O28 O -0.0623(6) 0.7192(5) -0.3613(4) 0.0600(16) Uani 1 1 d . . . . .
N11 N 0.6805(5) 0.7301(3) 0.1354(2) 0.0189(9) Uani 1 1 d . . . . .
C33 C 0.5587(6) 0.3545(4) -0.2998(3) 0.0209(10) Uani 1 1 d . . . . .
H33 H 0.449575 0.335699 -0.317284 0.025 Uiso 1 1 calc R . . . .
C5 C 0.7711(6) 0.6231(4) -0.1070(3) 0.0211(11) Uani 1 1 d . . . . .
N21 N 0.4611(6) 0.8377(4) -0.1731(3) 0.0324(11) Uani 1 1 d . . . . .
C6 C 0.7299(6) 0.6132(4) -0.0426(3) 0.0199(10) Uani 1 1 d . . . . .
N31 N 0.7846(5) 0.4662(3) -0.2110(2) 0.0183(9) Uani 1 1 d . . . . .
C34 C 0.6454(6) 0.2973(4) -0.3378(3) 0.0173(10) Uani 1 1 d . . . . .
C22 C 0.3621(7) 0.7497(5) -0.1983(4) 0.0345(14) Uani 1 1 d . . . . .
H22 H 0.393560 0.695725 -0.183740 0.041 Uiso 1 1 calc R . . . .
C4 C 0.7304(7) 0.6982(4) -0.1369(3) 0.0273(12) Uani 1 1 d . . . . .
C1 C 0.6472(6) 0.6801(4) -0.0073(3) 0.0175(10) Uani 1 1 d . . . . .
C12 C 0.8347(6) 0.7517(4) 0.1528(3) 0.0225(11) Uani 1 1 d . . . . .
H12 H 0.882756 0.727657 0.113425 0.027 Uiso 1 1 calc R . . . .
C9 C 0.7783(7) 0.5327(4) -0.0113(3) 0.0317(13) Uani 1 1 d . . . . .
H9A H 0.752001 0.468757 -0.054092 0.048 Uiso 1 1 calc GR . . . .
H9B H 0.724711 0.527121 0.026822 0.048 Uiso 1 1 calc GR . . . .
H9C H 0.889646 0.549983 0.013637 0.048 Uiso 1 1 calc GR . . . .
C32 C 0.6306(6) 0.4392(4) -0.2361(3) 0.0224(11) Uani 1 1 d . . . . .
H32 H 0.570641 0.478577 -0.209846 0.027 Uiso 1 1 calc R . . . .
C24 C 0.1679(8) 0.8153(6) -0.2667(4) 0.0401(16) Uani 1 1 d . . . . .
C13 C 0.9234(6) 0.8081(4) 0.2268(3) 0.0209(10) Uani 1 1 d . . . . .
H13 H 1.032296 0.822956 0.238661 0.025 Uiso 1 1 calc R . . . .
C16 C 0.6080(6) 0.7634(4) 0.1902(3) 0.0213(11) Uani 1 1 d . . . . .
H16 H 0.498965 0.747547 0.177213 0.026 Uiso 1 1 calc R . . . .
C7 C 0.5494(7) 0.8410(4) 0.0145(4) 0.0352(14) Uani 1 1 d . . . . .
H7A H 0.500416 0.815678 0.047695 0.053 Uiso 1 1 calc GR . . . .
H7B H 0.472399 0.859718 -0.021776 0.053 Uiso 1 1 calc GR . . . .
H7C H 0.630935 0.899621 0.046754 0.053 Uiso 1 1 calc GR . . . .
C30 C 0.8695(6) 0.5571(4) -0.1426(3) 0.0278(13) Uani 1 1 d . . . . .
H30A H 0.941762 0.597477 -0.158858 0.033 Uiso 1 1 calc R . . . .
H30B H 0.931688 0.535578 -0.102100 0.033 Uiso 1 1 calc R . . . .
C37 C 0.5724(6) 0.2017(4) -0.4078(3) 0.0191(10) Uani 1 1 d . . . . .
C23 C 0.2157(8) 0.7372(5) -0.2451(4) 0.0385(15) Uani 1 1 d . . . . .
H23 H 0.146720 0.674600 -0.262825 0.046 Uiso 1 1 calc R . . . .
C36 C 0.8717(6) 0.4100(4) -0.2467(3) 0.0218(11) Uani 1 1 d . . . . .
H36 H 0.980669 0.428925 -0.227570 0.026 Uiso 1 1 calc R . . . .
C2 C 0.6183(6) 0.7603(4) -0.0310(3) 0.0236(11) Uani 1 1 d . . . . .
C15 C 0.6941(6) 0.8202(4) 0.2647(3) 0.0212(11) Uani 1 1 d . . . . .
H15 H 0.644102 0.843969 0.303222 0.025 Uiso 1 1 calc R . . . .
C10 C 0.5837(6) 0.6640(4) 0.0561(3) 0.0219(11) Uani 1 1 d . . . . .
H10A H 0.478151 0.676936 0.047683 0.026 Uiso 1 1 calc R . . . .
H10B H 0.577479 0.593407 0.052852 0.026 Uiso 1 1 calc R . . . .
C20 C 0.6244(8) 0.8546(5) -0.1228(4) 0.0382(15) Uani 1 1 d . . . . .
H20A H 0.696136 0.867196 -0.152228 0.046 Uiso 1 1 calc R . . . .
H20B H 0.644182 0.914970 -0.076448 0.046 Uiso 1 1 calc R . . . .
C26 C 0.4181(8) 0.9163(5) -0.1926(4) 0.0362(14) Uani 1 1 d . . . . .
H26 H 0.489439 0.978160 -0.174210 0.043 Uiso 1 1 calc R . . . .
C8 C 0.7639(9) 0.7052(6) -0.2099(4) 0.0447(17) Uani 1 1 d . . . . .
H8A H 0.858862 0.754706 -0.195910 0.067 Uiso 1 1 calc GR . . . .
H8B H 0.678414 0.725536 -0.240021 0.067 Uiso 1 1 calc GR . . . .
H8C H 0.776029 0.640012 -0.241055 0.067 Uiso 1 1 calc GR . . . .
C3 C 0.6569(7) 0.7683(4) -0.0969(3) 0.0277(12) Uani 1 1 d . . . . .
C35 C 0.8034(6) 0.3257(4) -0.3106(3) 0.0214(11) Uani 1 1 d . . . . .
H35 H 0.865186 0.286900 -0.335885 0.026 Uiso 1 1 calc R . . . .
C25 C 0.2743(9) 0.9070(5) -0.2382(4) 0.0400(16) Uani 1 1 d . . . . .
H25 H 0.244892 0.962538 -0.251013 0.048 Uiso 1 1 calc R . . . .
C27 C 0.0082(9) 0.8061(6) -0.3184(4) 0.0445(17) Uani 1 1 d . . . . .
O18 O 0.8793(4) 0.9418(3) 0.4134(2) 0.0211(8) Uani 1 1 d . . . . .
O39 O 0.6554(4) 0.1728(2) -0.4505(2) 0.0208(8) Uani 1 1 d . . . . .
C17 C 0.9489(6) 0.9033(4) 0.3664(3) 0.0179(10) Uani 1 1 d . . . . .
C14 C 0.8532(6) 0.8433(4) 0.2842(3) 0.0172(10) Uani 1 1 d . . . . .
O1W O 0.8185(4) 0.8798(3) 0.5418(2) 0.0243(8) Uani 1 1 d . . . . .
H1WA H 0.752786 0.820420 0.519126 0.036 Uiso 1 1 d GR . . . .
H1WB H 0.832932 0.896771 0.593235 0.036 Uiso 1 1 d GR . . . .
O19 O 1.0905(4) 0.9091(3) 0.3807(2) 0.0219(8) Uani 1 1 d . . . . .
O2W O 0.8923(5) 1.1527(3) 0.4799(2) 0.0279(9) Uani 1 1 d . . . . .
H2WA H 0.997244 1.142598 0.481019 0.042 Uiso 1 1 d GR . . . .
H2WB H 0.909301 1.217168 0.521617 0.042 Uiso 1 1 d GR . . . .
C41 C 0.4577(6) 1.0112(4) 0.3627(3) 0.0205(10) Uani 1 1 d . . . . .
C40 C 0.3244(7) 0.9962(6) 0.2937(3) 0.0360(15) Uani 1 1 d . . . . .
H40A H 0.322088 0.935535 0.251652 0.054 Uiso 1 1 calc GR . . . .
H40B H 0.335234 1.053748 0.276279 0.054 Uiso 1 1 calc GR . . . .
H40C H 0.228531 0.989444 0.307916 0.054 Uiso 1 1 calc GR . . . .
O43 O 0.5931(4) 1.0234(3) 0.3585(2) 0.0261(8) Uani 1 1 d . . . . .
O42 O 0.4341(4) 1.0094(3) 0.42669(19) 0.0184(7) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nd1 Nd1 4.0971(6) 2_676 ?
Nd1 O38 2.515(3) 2_665 ?
Nd1 O18 2.402(3) . ?
Nd1 O39 2.450(3) 1_566 ?
Nd1 O1W 2.542(4) . ?
Nd1 O19 2.464(3) 2_776 ?
Nd1 O2W 2.503(4) . ?
Nd1 C41 2.956(5) . ?
Nd1 O43 2.543(4) . ?
Nd1 O42 2.399(3) 2_676 ?
Nd1 O42 2.587(4) . ?
O38 C37 1.259(6) . ?
O29 C27 1.226(10) . ?
O28 C27 1.257(10) . ?
N11 C12 1.345(7) . ?
N11 C16 1.360(7) . ?
N11 C10 1.495(6) . ?
C33 H33 0.9500 . ?
C33 C34 1.376(7) . ?
C33 C32 1.381(7) . ?
C5 C6 1.397(8) . ?
C5 C4 1.408(8) . ?
C5 C30 1.506(7) . ?
N21 C22 1.342(8) . ?
N21 C20 1.512(8) . ?
N21 C26 1.361(8) . ?
C6 C1 1.404(7) . ?
C6 C9 1.513(8) . ?
N31 C32 1.342(7) . ?
N31 C30 1.495(6) . ?
N31 C36 1.350(7) . ?
C34 C37 1.530(6) . ?
C34 C35 1.378(7) . ?
C22 H22 0.9500 . ?
C22 C23 1.373(9) . ?
C4 C8 1.510(8) . ?
C4 C3 1.409(9) . ?
C1 C2 1.385(8) . ?
C1 C10 1.516(7) . ?
C12 H12 0.9500 . ?
C12 C13 1.373(7) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C32 H32 0.9500 . ?
C24 C23 1.386(10) . ?
C24 C25 1.409(11) . ?
C24 C27 1.515(10) . ?
C13 H13 0.9500 . ?
C13 C14 1.388(7) . ?
C16 H16 0.9500 . ?
C16 C15 1.374(7) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C7 C2 1.521(7) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C37 O39 1.253(6) . ?
C23 H23 0.9500 . ?
C36 H36 0.9500 . ?
C36 C35 1.375(7) . ?
C2 C3 1.405(9) . ?
C15 H15 0.9500 . ?
C15 C14 1.386(7) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C3 1.498(8) . ?
C26 H26 0.9500 . ?
C26 C25 1.355(10) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C35 H35 0.9500 . ?
C25 H25 0.9500 . ?
O18 C17 1.249(6) . ?
C17 C14 1.510(7) . ?
C17 O19 1.246(6) . ?
O1W H1WA 0.8984 . ?
O1W H1WB 0.8982 . ?
O2W H2WA 0.9844 . ?
O2W H2WB 0.9843 . ?
C41 C40 1.496(7) . ?
C41 O43 1.256(7) . ?
C41 O42 1.284(6) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O38 Nd1 Nd1 68.91(8) 2_665 2_676 ?
O38 Nd1 O1W 66.62(12) 2_665 . ?
O38 Nd1 C41 68.45(13) 2_665 . ?
O38 Nd1 O43 76.94(12) 2_665 . ?
O38 Nd1 O42 66.99(12) 2_665 . ?
O18 Nd1 Nd1 144.89(8) . 2_676 ?
O18 Nd1 O38 78.24(12) . 2_665 ?
O18 Nd1 O39 140.23(13) . 1_566 ?
O18 Nd1 O1W 73.71(13) . . ?
O18 Nd1 O19 100.97(12) . 2_776 ?
O18 Nd1 O2W 71.96(13) . . ?
O18 Nd1 C41 98.09(13) . . ?
O18 Nd1 O43 76.86(12) . . ?
O18 Nd1 O42 121.14(11) . . ?
O39 Nd1 Nd1 66.42(9) 1_566 2_676 ?
O39 Nd1 O38 133.99(12) 1_566 2_665 ?
O39 Nd1 O1W 134.39(12) 1_566 . ?
O39 Nd1 O19 73.47(13) 1_566 2_776 ?
O39 Nd1 O2W 68.64(13) 1_566 . ?
O39 Nd1 C41 79.51(13) 1_566 . ?
O39 Nd1 O43 87.83(13) 1_566 . ?
O39 Nd1 O42 69.82(12) 1_566 . ?
O1W Nd1 Nd1 103.02(8) . 2_676 ?
O1W Nd1 C41 135.07(13) . . ?
O1W Nd1 O43 136.76(13) . . ?
O1W Nd1 O42 125.91(12) . . ?
O19 Nd1 Nd1 110.67(8) 2_776 2_676 ?
O19 Nd1 O38 134.49(12) 2_776 2_665 ?
O19 Nd1 O1W 69.57(13) 2_776 . ?
O19 Nd1 O2W 74.16(13) 2_776 . ?
O19 Nd1 C41 152.85(14) 2_776 . ?
O19 Nd1 O43 148.00(13) 2_776 . ?
O19 Nd1 O42 137.32(11) 2_776 . ?
O2W Nd1 Nd1 130.56(9) . 2_676 ?
O2W Nd1 O38 142.72(12) . 2_665 ?
O2W Nd1 O1W 123.08(13) . . ?
O2W Nd1 C41 93.83(14) . . ?
O2W Nd1 O43 74.91(13) . . ?
O2W Nd1 O42 110.59(13) . . ?
C41 Nd1 Nd1 58.88(11) . 2_676 ?
O43 Nd1 Nd1 83.83(8) . 2_676 ?
O43 Nd1 C41 24.98(14) . . ?
O43 Nd1 O42 50.57(11) . . ?
O42 Nd1 Nd1 33.27(8) . 2_676 ?
O42 Nd1 Nd1 36.28(9) 2_676 2_676 ?
O42 Nd1 O38 78.88(12) 2_676 2_665 ?
O42 Nd1 O18 147.10(13) 2_676 . ?
O42 Nd1 O39 71.86(12) 2_676 1_566 ?
O42 Nd1 O1W 75.65(12) 2_676 . ?
O42 Nd1 O19 79.03(12) 2_676 2_776 ?
O42 Nd1 O2W 137.01(12) 2_676 . ?
O42 Nd1 C41 95.12(14) 2_676 . ?
O42 Nd1 C41 25.70(13) . . ?
O42 Nd1 O43 120.09(12) 2_676 . ?
O42 Nd1 O42 69.54(13) 2_676 . ?
C37 O38 Nd1 131.9(3) . 2_665 ?
C12 N11 C16 121.2(4) . . ?
C12 N11 C10 120.9(4) . . ?
C16 N11 C10 117.8(4) . . ?
C34 C33 H33 120.1 . . ?
C34 C33 C32 119.8(5) . . ?
C32 C33 H33 120.1 . . ?
C6 C5 C4 121.1(5) . . ?
C6 C5 C30 120.2(5) . . ?
C4 C5 C30 118.6(5) . . ?
C22 N21 C20 122.4(5) . . ?
C22 N21 C26 120.8(6) . . ?
C26 N21 C20 116.8(5) . . ?
C5 C6 C1 118.9(5) . . ?
C5 C6 C9 119.5(5) . . ?
C1 C6 C9 121.5(5) . . ?
C32 N31 C30 123.1(4) . . ?
C32 N31 C36 120.5(4) . . ?
C36 N31 C30 116.4(4) . . ?
C33 C34 C37 122.2(5) . . ?
C33 C34 C35 118.8(5) . . ?
C35 C34 C37 118.9(5) . . ?
N21 C22 H22 119.8 . . ?
N21 C22 C23 120.4(6) . . ?
C23 C22 H22 119.8 . . ?
C5 C4 C8 121.8(6) . . ?
C5 C4 C3 118.4(5) . . ?
C3 C4 C8 119.8(6) . . ?
C6 C1 C10 120.2(5) . . ?
C2 C1 C6 121.0(5) . . ?
C2 C1 C10 118.7(5) . . ?
N11 C12 H12 119.7 . . ?
N11 C12 C13 120.6(5) . . ?
C13 C12 H12 119.7 . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C33 C32 H32 119.8 . . ?
N31 C32 C33 120.5(5) . . ?
N31 C32 H32 119.8 . . ?
C23 C24 C25 117.5(6) . . ?
C23 C24 C27 123.0(7) . . ?
C25 C24 C27 119.6(6) . . ?
C12 C13 H13 120.1 . . ?
C12 C13 C14 119.7(5) . . ?
C14 C13 H13 120.1 . . ?
N11 C16 H16 120.4 . . ?
N11 C16 C15 119.3(5) . . ?
C15 C16 H16 120.4 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
C5 C30 H30A 108.3 . . ?
C5 C30 H30B 108.3 . . ?
N31 C30 C5 115.8(4) . . ?
N31 C30 H30A 108.3 . . ?
N31 C30 H30B 108.3 . . ?
H30A C30 H30B 107.4 . . ?
O38 C37 C34 116.0(5) . . ?
O39 C37 O38 128.3(4) . . ?
O39 C37 C34 115.7(5) . . ?
C22 C23 C24 120.5(7) . . ?
C22 C23 H23 119.7 . . ?
C24 C23 H23 119.7 . . ?
N31 C36 H36 119.8 . . ?
N31 C36 C35 120.3(5) . . ?
C35 C36 H36 119.8 . . ?
C1 C2 C7 121.0(5) . . ?
C1 C2 C3 119.4(5) . . ?
C3 C2 C7 119.6(5) . . ?
C16 C15 H15 119.7 . . ?
C16 C15 C14 120.7(5) . . ?
C14 C15 H15 119.7 . . ?
N11 C10 C1 112.4(4) . . ?
N11 C10 H10A 109.1 . . ?
N11 C10 H10B 109.1 . . ?
C1 C10 H10A 109.1 . . ?
C1 C10 H10B 109.1 . . ?
H10A C10 H10B 107.9 . . ?
N21 C20 H20A 108.9 . . ?
N21 C20 H20B 108.9 . . ?
H20A C20 H20B 107.7 . . ?
C3 C20 N21 113.2(5) . . ?
C3 C20 H20A 108.9 . . ?
C3 C20 H20B 108.9 . . ?
N21 C26 H26 119.8 . . ?
C25 C26 N21 120.4(6) . . ?
C25 C26 H26 119.8 . . ?
C4 C8 H8A 109.5 . . ?
C4 C8 H8B 109.5 . . ?
C4 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C4 C3 C20 119.9(6) . . ?
C2 C3 C4 120.7(5) . . ?
C2 C3 C20 119.3(6) . . ?
C34 C35 H35 120.0 . . ?
C36 C35 C34 120.0(5) . . ?
C36 C35 H35 120.0 . . ?
C24 C25 H25 119.8 . . ?
C26 C25 C24 120.4(6) . . ?
C26 C25 H25 119.8 . . ?
O29 C27 O28 126.8(7) . . ?
O29 C27 C24 117.1(7) . . ?
O28 C27 C24 116.1(7) . . ?
C17 O18 Nd1 173.1(3) . . ?
C37 O39 Nd1 134.6(3) . 1_544 ?
O18 C17 C14 117.3(4) . . ?
O19 C17 O18 126.3(4) . . ?
O19 C17 C14 116.3(4) . . ?
C13 C14 C17 120.5(5) . . ?
C15 C14 C13 118.5(5) . . ?
C15 C14 C17 121.0(4) . . ?
Nd1 O1W H1WA 111.9 . . ?
Nd1 O1W H1WB 111.7 . . ?
H1WA O1W H1WB 107.1 . . ?
C17 O19 Nd1 125.7(3) . 2_776 ?
Nd1 O2W H2WA 115.0 . . ?
Nd1 O2W H2WB 114.8 . . ?
H2WA O2W H2WB 103.5 . . ?
C40 C41 Nd1 172.4(4) . . ?
O43 C41 Nd1 58.8(3) . . ?
O43 C41 C40 120.7(5) . . ?
O43 C41 O42 119.3(5) . . ?
O42 C41 Nd1 60.9(3) . . ?
O42 C41 C40 119.9(5) . . ?
C41 C40 H40A 109.5 . . ?
C41 C40 H40B 109.5 . . ?
C41 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C41 O43 Nd1 96.2(3) . . ?
Nd1 O42 Nd1 110.46(13) 2_676 . ?
C41 O42 Nd1 155.4(3) . 2_676 ?
C41 O42 Nd1 93.4(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1W H1WB O29 0.90 1.95 2.716(6) 142.7 1_656 yes
O2W H2WA O1W 0.98 1.88 2.845(6) 166.4 2_776 yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Nd1 O38 C37 C34 -161.5(3) 2_665 . . . ?
Nd1 O38 C37 O39 17.6(8) 2_665 . . . ?
Nd1 C41 O42 Nd1 -166.6(9) . . . 2_676 ?
O38 C37 O39 Nd1 -45.8(8) . . . 1_544 ?
N11 C12 C13 C14 -0.1(9) . . . . ?
N11 C16 C15 C14 -0.3(9) . . . . ?
C33 C34 C37 O38 -20.8(7) . . . . ?
C33 C34 C37 O39 159.9(5) . . . . ?
C33 C34 C35 C36 -0.4(8) . . . . ?
C5 C6 C1 C2 -5.7(7) . . . . ?
C5 C6 C1 C10 172.5(4) . . . . ?
C5 C4 C3 C2 -3.1(8) . . . . ?
C5 C4 C3 C20 174.6(5) . . . . ?
N21 C22 C23 C24 -0.2(11) . . . . ?
N21 C20 C3 C4 98.3(7) . . . . ?
N21 C20 C3 C2 -84.0(7) . . . . ?
N21 C26 C25 C24 -0.8(10) . . . . ?
C6 C5 C4 C8 -175.4(5) . . . . ?
C6 C5 C4 C3 4.7(8) . . . . ?
C6 C5 C30 N31 96.1(6) . . . . ?
C6 C1 C2 C7 -171.1(5) . . . . ?
C6 C1 C2 C3 7.3(7) . . . . ?
C6 C1 C10 N11 101.3(5) . . . . ?
N31 C36 C35 C34 -0.9(8) . . . . ?
C34 C33 C32 N31 0.0(8) . . . . ?
C34 C37 O39 Nd1 133.4(4) . . . 1_544 ?
C22 N21 C20 C3 -6.8(9) . . . . ?
C22 N21 C26 C25 -0.2(10) . . . . ?
C4 C5 C6 C1 -0.4(7) . . . . ?
C4 C5 C6 C9 -178.9(5) . . . . ?
C4 C5 C30 N31 -87.8(6) . . . . ?
C1 C2 C3 C4 -2.8(8) . . . . ?
C1 C2 C3 C20 179.5(5) . . . . ?
C12 N11 C16 C15 0.1(8) . . . . ?
C12 N11 C10 C1 -37.2(7) . . . . ?
C12 C13 C14 C15 -0.1(8) . . . . ?
C12 C13 C14 C17 178.5(5) . . . . ?
C9 C6 C1 C2 172.7(5) . . . . ?
C9 C6 C1 C10 -9.1(7) . . . . ?
C32 C33 C34 C37 178.8(5) . . . . ?
C32 C33 C34 C35 0.8(8) . . . . ?
C32 N31 C30 C5 -5.3(8) . . . . ?
C32 N31 C36 C35 1.7(8) . . . . ?
C16 N11 C12 C13 0.1(9) . . . . ?
C16 N11 C10 C1 146.1(5) . . . . ?
C16 C15 C14 C13 0.3(8) . . . . ?
C16 C15 C14 C17 -178.3(5) . . . . ?
C7 C2 C3 C4 175.6(5) . . . . ?
C7 C2 C3 C20 -2.1(8) . . . . ?
C30 C5 C6 C1 175.6(4) . . . . ?
C30 C5 C6 C9 -2.8(7) . . . . ?
C30 C5 C4 C8 8.5(8) . . . . ?
C30 C5 C4 C3 -171.4(5) . . . . ?
C30 N31 C32 C33 179.8(5) . . . . ?
C30 N31 C36 C35 -179.3(5) . . . . ?
C37 C34 C35 C36 -178.5(5) . . . . ?
C23 C24 C25 C26 1.1(10) . . . . ?
C23 C24 C27 O29 156.1(7) . . . . ?
C23 C24 C27 O28 -22.7(10) . . . . ?
C36 N31 C32 C33 -1.3(8) . . . . ?
C36 N31 C30 C5 175.7(5) . . . . ?
C2 C1 C10 N11 -80.5(6) . . . . ?
C10 N11 C12 C13 -176.5(5) . . . . ?
C10 N11 C16 C15 176.8(5) . . . . ?
C10 C1 C2 C7 10.7(7) . . . . ?
C10 C1 C2 C3 -171.0(5) . . . . ?
C20 N21 C22 C23 -178.8(6) . . . . ?
C20 N21 C26 C25 179.3(6) . . . . ?
C26 N21 C22 C23 0.7(10) . . . . ?
C26 N21 C20 C3 173.7(6) . . . . ?
C8 C4 C3 C2 177.0(5) . . . . ?
C8 C4 C3 C20 -5.3(8) . . . . ?
C35 C34 C37 O38 157.2(5) . . . . ?
C35 C34 C37 O39 -22.1(7) . . . . ?
C25 C24 C23 C22 -0.6(10) . . . . ?
C25 C24 C27 O29 -23.5(10) . . . . ?
C25 C24 C27 O28 157.8(7) . . . . ?
C27 C24 C23 C22 179.8(6) . . . . ?
C27 C24 C25 C26 -179.3(6) . . . . ?
O18 C17 C14 C13 172.5(5) . . . . ?
O18 C17 C14 C15 -9.0(8) . . . . ?
O18 C17 O19 Nd1 5.1(8) . . . 2_776 ?
C14 C17 O19 Nd1 -174.6(3) . . . 2_776 ?
O19 C17 C14 C13 -7.7(8) . . . . ?
O19 C17 C14 C15 170.8(5) . . . . ?
C40 C41 O43 Nd1 -171.1(5) . . . . ?
C40 C41 O42 Nd1 171.3(5) . . . . ?
C40 C41 O42 Nd1 4.7(12) . . . 2_676 ?
O43 C41 O42 Nd1 -173.7(5) . . . 2_676 ?
O43 C41 O42 Nd1 -7.1(5) . . . . ?
O42 C41 O43 Nd1 7.3(5) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.000 246.8 85.0 '9x water'
2 -0.042 0.500 0.500 444.3 130.7 '13x water'

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.358
_oxdiff_exptl_absorpt_empirical_full_min 0.853
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_jj003_br_nd_otf_h2o_acet_red3
_database_code_depnum_ccdc_archive 'CCDC 1833432'
loop_
_audit_author_name
_audit_author_address
'Antti Tiihonen'
;University of Jyv?skyl?, Department of Chemistry
Finland
;
_audit_update_record             
;
2018-03-29 deposited with the CCDC.	2019-02-28 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_CHEMW03_I                   
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: The structure contains voids of unresolved electron density
which was treated using Olex2 solvent mask procedure (full details in 
_smtbx_masks_special_details). The 11 water molecules per asymmetric unit 
 are included in the formula and used in the calculations. 
;
_vrf_PLAT973_I                   
;
PROBLEM: Check Calcd Positive Resid. Density on       Nd1  
RESPONSE: Peak is located about 1 Angstrom from the metal atom and is caused by
the absorption effects. Data recorded with Cu-radiation. 
;
_vrf_PLAT420_I                   
;
PROBLEM: D-H Without Acceptor       O      --H
RESPONSE: Hydrogen bond acceptor (water) have been removed among the other 
disordered solvents (also water) from the voids (see vrf_CHEMW03_ALERT_2_A).
;
_vrf_FORMU01_I                   
;
PROBLEM: There is a discrepancy between the atom counts in the
            _chemical_formula_sum and _chemical_formula_moiety.
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_CELLZ01_I                   
;
PROBLEM: Difference between formula and atom_site contents detected.
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT041_I                   
;
PROBLEM: Calculated and Reported SumFormula strings Differ ...    
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT042_I                   
;
PROBLEM: Calculated and Reported Moiety formula strings Differ by ...
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT068_I                   
;
PROBLEM: Reported F000 Differs from Calcd (or Missing)...
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT606_I                   
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
# end Validation Reply Form
_audit_creation_date             2018-03-26
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H31 N3 Nd O8, 2.31(Br), 0.69(C F3 O3 S)'
_chemical_formula_sum            'C30.68 H53 Br2.32 F2.06 N3 Nd O21.06 S0.69'
_chemical_formula_weight         1191.27
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C21 H25 O12 N3 F12 S3 Br1 Nd1'
_chemical_oxdiff_usercomment     'clear colorless block'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -3.1807 10.9079 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.5721(4)
_cell_length_b                   14.4092(6)
_cell_length_c                   18.7321(7)
_cell_angle_alpha                106.854(4)
_cell_angle_beta                 103.019(4)
_cell_angle_gamma                99.792(4)
_cell_volume                     2331.09(18)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8266
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      76.3980
_cell_measurement_theta_min      3.2780
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    11.862
_exptl_absorpt_correction_T_max  0.487
_exptl_absorpt_correction_T_min  0.204
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.697
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1194
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-2 0 11 0.0389
1 8 0 0.0509
3 0 9 0.0407
0 -8 -1 0.0772
-3 0 -8 0.0522
-3 -4 11 0.0492
2 5 -11 0.0441
6 -1 -4 0.0294
-6 1 6 0.0286
5 -7 -2 0.0438
-4 7 -5 0.0441
2 0 -12 0.0377

_exptl_crystal_size_max          0.145
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.063
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-2.0000 -0.0001 11.0002 0.0621 0.8170 -0.4744
0.9998 8.0006 0.0007 -0.8188 0.4796 0.2481
3.0000 0.0003 9.0004 -0.5950 0.4365 -0.7826
0.0002 -8.0005 -1.0007 0.6992 -0.5948 -0.2745
-3.0000 -0.0003 -8.0003 0.5753 -0.3713 0.7240
-2.9999 -4.0004 10.9998 0.5412 0.6022 -0.5559
1.9999 5.0004 -10.9998 -0.4868 -0.4860 0.6826
6.0001 -0.9997 -3.9999 -0.6722 -0.6271 -0.3177
-6.0001 0.9997 6.0000 0.6328 0.7575 0.2005
5.0002 -7.0001 -2.0004 -0.0626 -0.8440 -0.5997
-4.0002 7.0001 -4.9997 0.0611 0.3377 0.9248
2.0000 0.0000 -12.0002 -0.0424 -0.8822 0.5330

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_unetI/netI     0.0477
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            14235
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.999
_diffrn_reflns_theta_min         2.576
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3953
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      2.00  83.00   1.00    1.50    --   41.90 -99.00 -60.00   81
  2  ω     30.00 151.00   1.00    4.50    --  112.00 -15.00 -30.00  121
  3  ω     97.00 145.00   1.00    4.50    --  112.00 -77.00   0.00   48
  4  ω    101.00 137.00   1.00    4.50    --  112.00 -30.00 120.00   36
  5  ω     88.00 175.00   1.00    4.50    --  112.00  45.00 150.00   87
  6  ω     78.00 151.00   1.00    4.50    --  112.00 178.00  60.00   73
  7  ω     43.00  95.00   1.00    4.50    --  112.00 -30.00 120.00   52
  8  ω     47.00 116.00   1.00    4.50    --  112.00-111.00  90.00   69
  9  ω     36.00  83.00   1.00    4.50    --  112.00 -77.00   0.00   47
 10  ω     29.00 109.00   1.00    4.50    --  112.00 -94.00-180.00   80
 11  ω     47.00 133.00   1.00    4.50    --  112.00 -45.00-180.00   86
 12  ω    -68.00  31.00   1.00    1.50    --  -41.90  57.00-150.00   99
 13  ω   -115.00 -28.00   1.00    1.50    --  -41.90 -37.00  60.00   87
 14  ω   -113.00 -18.00   1.00    1.50    --  -41.90 -37.00 -30.00   95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1392943000
_diffrn_orient_matrix_UB_12      -0.0849328000
_diffrn_orient_matrix_UB_13      -0.0196797000
_diffrn_orient_matrix_UB_21      -0.0500447000
_diffrn_orient_matrix_UB_22      0.0661932000
_diffrn_orient_matrix_UB_23      0.0651734000
_diffrn_orient_matrix_UB_31      -0.0850732000
_diffrn_orient_matrix_UB_32      0.0416423000
_diffrn_orient_matrix_UB_33      -0.0585961000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7892
_reflns_number_total             8450
_reflns_odcompleteness_completeness 99.45
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         2.889
_refine_diff_density_min         -2.830
_refine_diff_density_rms         0.169
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     484
_refine_ls_number_reflns         8450
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0612
_refine_ls_restrained_S_all      1.047
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1163P)²+9.8672P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1752
_refine_ls_wR_factor_ref         0.1788
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Others
 Sof(Br3B)=1-FVAR(1)
 Sof(S1A)=Sof(F7A)=Sof(F6A)=Sof(O4A)=Sof(O3A)=Sof(F8A)=Sof(O2A)=Sof(C5A)=FVAR(1)
3.a Rotating group:
 O2W(H2WA,H2WB), O1W(H1WA,H1WB)
3.b Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C20(H20A,H20B), C10(H10A,H10B)
3.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C33(H33), C22(H22), C16(H16), C25(H25), C13(H13), C12(H12),
 C32(H32), C35(H35), C36(H36), C26(H26), C23(H23)
3.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Nd1 Nd 0.27757(4) -0.00925(2) 0.50570(2) 0.02151(13) Uani 1 1 d . . . . .
Br2 Br 0.70061(10) 0.57433(8) 1.19803(6) 0.0506(3) Uani 1 1 d . . . . .
Br1 Br 0.22339(14) -0.07615(9) 0.81162(6) 0.0612(3) Uani 1 1 d . . . . .
S1A S -0.2008(6) 0.2622(4) 0.8979(2) 0.0242(11) Uani 0.686(7) 1 d . . P A 1
O18 O 0.1322(5) 0.0481(4) 0.5890(2) 0.0270(10) Uani 1 1 d . . . . .
O28 O 0.6210(6) 0.0604(4) 1.3812(3) 0.0343(11) Uani 1 1 d . . . . .
O29 O 0.4285(6) 0.0297(4) 1.4247(3) 0.0293(10) Uani 1 1 d . . . . .
O19 O -0.0751(5) 0.0748(4) 0.6164(3) 0.0319(11) Uani 1 1 d . . . . .
F7A F -0.0919(8) 0.1135(5) 0.9263(4) 0.0435(17) Uani 0.686(7) 1 d . . P A 1
C6 C 0.2565(8) 0.3717(5) 1.0440(4) 0.0296(14) Uani 1 1 d . . . . .
F6A F -0.3272(8) 0.0873(6) 0.9120(4) 0.0501(19) Uani 0.686(7) 1 d . . P A 1
N31 N 0.1884(6) 0.5520(4) 1.1936(3) 0.0263(12) Uani 1 1 d . . . . .
C14 C 0.1446(7) 0.1297(4) 0.7206(3) 0.0209(12) Uani 1 1 d . . . . .
C27 C 0.4875(8) 0.0546(5) 1.3772(4) 0.0286(14) Uani 1 1 d . . . . .
N21 N 0.2198(7) 0.1150(4) 1.1902(3) 0.0275(12) Uani 1 1 d . . . . .
O4A O -0.3145(9) 0.3008(6) 0.9244(5) 0.0364(18) Uani 0.686(7) 1 d . . P A 1
N11 N 0.2955(7) 0.2186(5) 0.8753(3) 0.0279(12) Uani 1 1 d . . . . .
C15 C 0.0719(8) 0.1675(5) 0.7747(4) 0.0251(13) Uani 1 1 d . . . . .
H15 H -0.031455 0.162106 0.758550 0.030 Uiso 1 1 calc R . . . .
C5 C 0.1771(8) 0.3808(5) 1.0989(4) 0.0250(13) Uani 1 1 d . . . . .
C34 C 0.3376(8) 0.7174(5) 1.3230(4) 0.0255(13) Uani 1 1 d . . . . .
C3 C 0.1810(9) 0.2135(5) 1.0983(4) 0.0302(15) Uani 1 1 d . . . . .
C17 C 0.0603(7) 0.0808(4) 0.6346(3) 0.0212(12) Uani 1 1 d . . . . .
C33 C 0.4149(7) 0.6631(5) 1.2803(4) 0.0255(13) Uani 1 1 d . . . . .
H33 H 0.519973 0.683677 1.295047 0.031 Uiso 1 1 calc R . . . .
C24 C 0.3930(9) 0.0773(5) 1.3118(4) 0.0309(15) Uani 1 1 d . . . . .
C30 C 0.1052(8) 0.4671(5) 1.1188(4) 0.0285(14) Uani 1 1 d . . . . .
H30A H 0.092576 0.494184 1.075487 0.034 Uiso 1 1 calc R . . . .
H30B H 0.005164 0.440552 1.121849 0.034 Uiso 1 1 calc R . . . .
C22 C 0.3652(10) 0.1412(8) 1.2070(5) 0.046(2) Uani 1 1 d . . . . .
H22 H 0.408664 0.172895 1.176460 0.055 Uiso 1 1 calc R . . . .
C1 C 0.2979(8) 0.2829(6) 1.0166(4) 0.0314(15) Uani 1 1 d . . . . .
C16 C 0.1518(8) 0.2125(5) 0.8515(4) 0.0275(14) Uani 1 1 d . . . . .
H16 H 0.103371 0.239873 0.888642 0.033 Uiso 1 1 calc R . . . .
O3A O -0.0567(10) 0.3235(6) 0.9316(5) 0.0369(19) Uani 0.686(7) 1 d . . P A 1
C25 C 0.2413(9) 0.0509(6) 1.2942(4) 0.0378(17) Uani 1 1 d . . . . .
H25 H 0.195179 0.019139 1.323902 0.045 Uiso 1 1 calc R . . . .
C20 C 0.1205(9) 0.1258(5) 1.1205(4) 0.0354(17) Uani 1 1 d . . . . .
H20A H 0.024953 0.132194 1.130689 0.042 Uiso 1 1 calc R . . . .
H20B H 0.100085 0.063597 1.075417 0.042 Uiso 1 1 calc R . . . .
C13 C 0.2945(8) 0.1381(5) 0.7461(4) 0.0290(14) Uani 1 1 d . . . . .
H13 H 0.345842 0.112831 0.709872 0.035 Uiso 1 1 calc R . . . .
C12 C 0.3696(8) 0.1835(7) 0.8245(4) 0.0368(17) Uani 1 1 d . . . . .
H12 H 0.473035 0.189964 0.842390 0.044 Uiso 1 1 calc R . . . .
C32 C 0.3401(8) 0.5798(5) 1.2168(4) 0.0274(14) Uani 1 1 d . . . . .
H32 H 0.393575 0.540906 1.188630 0.033 Uiso 1 1 calc R . . . .
C4 C 0.1430(8) 0.3035(5) 1.1283(4) 0.0284(14) Uani 1 1 d . . . . .
C35 C 0.1826(8) 0.6858(6) 1.3000(4) 0.0313(15) Uani 1 1 d . . . . .
H35 H 0.127415 0.720526 1.329787 0.038 Uiso 1 1 calc R . . . .
C36 C 0.1117(8) 0.6045(5) 1.2343(4) 0.0280(14) Uani 1 1 d . . . . .
H36 H 0.006429 0.584898 1.217185 0.034 Uiso 1 1 calc R . . . .
F8A F -0.1662(9) 0.1921(6) 1.0186(4) 0.0506(19) Uani 0.686(7) 1 d . . P A 1
C26 C 0.1564(9) 0.0708(6) 1.2329(5) 0.0373(17) Uani 1 1 d . . . . .
H26 H 0.051409 0.052808 1.220846 0.045 Uiso 1 1 calc R . . . .
C23 C 0.4570(10) 0.1236(8) 1.2681(5) 0.046(2) Uani 1 1 d . . . . .
H23 H 0.561718 0.143156 1.279376 0.055 Uiso 1 1 calc R . . . .
C2 C 0.2578(9) 0.2022(5) 1.0420(4) 0.0326(16) Uani 1 1 d . . . . .
C10 C 0.3871(8) 0.2718(6) 0.9594(4) 0.0347(16) Uani 1 1 d . . . . .
H10A H 0.460589 0.234232 0.972873 0.042 Uiso 1 1 calc R . . . .
H10B H 0.442550 0.339262 0.964741 0.042 Uiso 1 1 calc R . . . .
C9 C 0.2955(11) 0.4569(6) 1.0145(5) 0.046(2) Uani 1 1 d . . . . .
H9A H 0.234851 0.438856 0.960434 0.069 Uiso 1 1 calc GR . . . .
H9B H 0.400580 0.469676 1.016737 0.069 Uiso 1 1 calc GR . . . .
H9C H 0.276419 0.517280 1.047055 0.069 Uiso 1 1 calc GR . . . .
C7 C 0.2967(13) 0.1050(7) 1.0080(5) 0.053(2) Uani 1 1 d . . . . .
H7A H 0.276905 0.061044 1.037769 0.080 Uiso 1 1 calc GR . . . .
H7B H 0.401948 0.118682 1.010647 0.080 Uiso 1 1 calc GR . . . .
H7C H 0.236562 0.072192 0.953485 0.080 Uiso 1 1 calc GR . . . .
C8 C 0.0646(9) 0.3165(6) 1.1916(4) 0.0333(15) Uani 1 1 d . . . . .
H8A H 0.091247 0.387416 1.224166 0.050 Uiso 1 1 calc GR . . . .
H8B H 0.095072 0.276723 1.223919 0.050 Uiso 1 1 calc GR . . . .
H8C H -0.042846 0.293902 1.167314 0.050 Uiso 1 1 calc GR . . . .
O2A O -0.2459(11) 0.1999(7) 0.8160(5) 0.045(2) Uani 0.686(7) 1 d . . P A 1
C5A C -0.1995(13) 0.1576(8) 0.9401(7) 0.035(2) Uani 0.686(7) 1 d . . P A 1
O39 O 0.5459(5) 0.8524(3) 1.4008(3) 0.0289(10) Uani 1 1 d . . . . .
O38 O 0.3354(6) 0.8416(4) 1.4352(3) 0.0321(11) Uani 1 1 d . . . . .
C37 C 0.4148(8) 0.8127(5) 1.3926(4) 0.0278(14) Uani 1 1 d . . . . .
O2W O 0.2090(7) 0.1360(5) 0.4746(3) 0.0448(14) Uani 1 1 d . . . . .
H2WA H 0.219092 0.134932 0.429041 0.067 Uiso 1 1 d GR . . . .
H2WB H 0.265822 0.192452 0.509802 0.067 Uiso 1 1 d GR . . . .
O1W O 0.1049(7) -0.1634(4) 0.5049(3) 0.0398(13) Uani 1 1 d . . . . .
H1WA H 0.151427 -0.209694 0.505816 0.060 Uiso 1 1 d GR . . . .
H1WB H 0.030287 -0.185903 0.463258 0.060 Uiso 1 1 d GR . . . .
Br3B Br -0.1865(11) 0.2806(8) 0.9094(6) 0.087(4) Uani 0.314(7) 1 d . . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nd1 O18 2.383(4) . ?
Nd1 O28 2.490(5) 2_657 ?
Nd1 O29 2.925(5) 2_657 ?
Nd1 O29 2.431(5) 1_554 ?
Nd1 O19 2.450(4) 2_556 ?
Nd1 C27 3.067(7) 2_657 ?
Nd1 O39 2.470(5) 2_667 ?
Nd1 O38 2.399(4) 1_544 ?
Nd1 O2W 2.480(6) . ?
Nd1 O1W 2.527(6) . ?
S1A O4A 1.425(10) . ?
S1A O3A 1.397(10) . ?
S1A O2A 1.455(9) . ?
S1A C5A 1.896(13) . ?
O18 C17 1.251(8) . ?
O28 C27 1.250(9) . ?
O29 C27 1.258(9) . ?
O19 C17 1.245(8) . ?
F7A C5A 1.335(14) . ?
C6 C5 1.400(10) . ?
C6 C1 1.394(10) . ?
C6 C9 1.510(11) . ?
F6A C5A 1.333(13) . ?
N31 C30 1.506(8) . ?
N31 C32 1.369(9) . ?
N31 C36 1.342(9) . ?
C14 C15 1.390(9) . ?
C14 C17 1.519(8) . ?
C14 C13 1.378(10) . ?
C27 C24 1.502(9) . ?
N21 C22 1.317(11) . ?
N21 C20 1.497(8) . ?
N21 C26 1.341(10) . ?
N11 C16 1.326(9) . ?
N11 C12 1.346(9) . ?
N11 C10 1.512(8) . ?
C15 H15 0.9500 . ?
C15 C16 1.368(9) . ?
C5 C30 1.515(9) . ?
C5 C4 1.401(10) . ?
C34 C33 1.377(9) . ?
C34 C35 1.401(10) . ?
C34 C37 1.522(9) . ?
C3 C20 1.506(10) . ?
C3 C4 1.399(10) . ?
C3 C2 1.405(11) . ?
C33 H33 0.9500 . ?
C33 C32 1.366(9) . ?
C24 C25 1.373(12) . ?
C24 C23 1.377(11) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C22 H22 0.9500 . ?
C22 C23 1.392(11) . ?
C1 C2 1.406(11) . ?
C1 C10 1.505(10) . ?
C16 H16 0.9500 . ?
C25 H25 0.9500 . ?
C25 C26 1.383(10) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C13 H13 0.9500 . ?
C13 C12 1.382(9) . ?
C12 H12 0.9500 . ?
C32 H32 0.9500 . ?
C4 C8 1.524(10) . ?
C35 H35 0.9500 . ?
C35 C36 1.365(10) . ?
C36 H36 0.9500 . ?
F8A C5A 1.349(13) . ?
C26 H26 0.9500 . ?
C23 H23 0.9500 . ?
C2 C7 1.507(10) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
O39 C37 1.243(9) . ?
O38 C37 1.255(9) . ?
O2W H2WA 0.8769 . ?
O2W H2WB 0.8771 . ?
O1W H1WA 0.8645 . ?
O1W H1WB 0.8644 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O18 Nd1 O28 78.46(16) . 2_657 ?
O18 Nd1 O29 147.01(17) . 1_554 ?
O18 Nd1 O29 118.71(14) . 2_657 ?
O18 Nd1 O19 96.54(15) . 2_556 ?
O18 Nd1 C27 98.24(17) . 2_657 ?
O18 Nd1 O39 79.62(16) . 2_667 ?
O18 Nd1 O38 142.15(18) . 1_544 ?
O18 Nd1 O2W 74.67(19) . . ?
O18 Nd1 O1W 73.28(17) . . ?
O28 Nd1 O29 47.24(15) 2_657 2_657 ?
O28 Nd1 C27 23.15(19) 2_657 2_657 ?
O28 Nd1 O1W 68.42(19) 2_657 . ?
O29 Nd1 O28 121.54(17) 1_554 2_657 ?
O29 Nd1 O29 74.34(16) 1_554 2_657 ?
O29 Nd1 O19 84.26(16) 1_554 2_556 ?
O29 Nd1 C27 24.09(17) 2_657 2_657 ?
O29 Nd1 C27 98.42(18) 1_554 2_657 ?
O29 Nd1 O39 79.90(16) 1_554 2_667 ?
O29 Nd1 O2W 74.22(18) 1_554 . ?
O29 Nd1 O1W 136.32(16) 1_554 . ?
O19 Nd1 O28 138.95(19) 2_556 2_657 ?
O19 Nd1 O29 141.63(15) 2_556 2_657 ?
O19 Nd1 C27 147.35(19) 2_556 2_657 ?
O19 Nd1 O39 142.22(18) 2_556 2_667 ?
O19 Nd1 O2W 72.3(2) 2_556 . ?
O19 Nd1 O1W 71.13(18) 2_556 . ?
O39 Nd1 O28 77.61(18) 2_667 2_657 ?
O39 Nd1 O29 64.93(15) 2_667 2_657 ?
O39 Nd1 C27 69.45(18) 2_667 2_657 ?
O39 Nd1 O2W 70.44(19) 2_667 . ?
O39 Nd1 O1W 139.83(16) 2_667 . ?
O38 Nd1 O28 82.23(17) 1_544 2_657 ?
O38 Nd1 O29 65.60(15) 1_544 2_657 ?
O38 Nd1 O29 70.35(17) 1_544 1_554 ?
O38 Nd1 O19 77.42(17) 1_544 2_556 ?
O38 Nd1 C27 73.05(17) 1_544 2_657 ?
O38 Nd1 O39 127.27(17) 1_544 2_667 ?
O38 Nd1 O2W 135.06(18) 1_544 . ?
O38 Nd1 O1W 69.40(18) 1_544 . ?
O2W Nd1 O28 141.17(18) . 2_657 ?
O2W Nd1 O29 128.72(18) . 2_657 ?
O2W Nd1 C27 139.9(2) . 2_657 ?
O2W Nd1 O1W 127.3(2) . . ?
O1W Nd1 O29 103.30(17) . 2_657 ?
O1W Nd1 C27 85.5(2) . 2_657 ?
O4A S1A O2A 114.7(6) . . ?
O4A S1A C5A 99.7(6) . . ?
O3A S1A O4A 116.6(6) . . ?
O3A S1A O2A 119.1(6) . . ?
O3A S1A C5A 103.9(6) . . ?
O2A S1A C5A 97.4(6) . . ?
C17 O18 Nd1 177.8(4) . . ?
C27 O28 Nd1 105.3(4) . 2_657 ?
Nd1 O29 Nd1 105.66(16) 1_556 2_657 ?
C27 O29 Nd1 84.3(4) . 2_657 ?
C27 O29 Nd1 169.9(5) . 1_556 ?
C17 O19 Nd1 135.3(4) . 2_556 ?
C5 C6 C9 120.4(7) . . ?
C1 C6 C5 119.1(7) . . ?
C1 C6 C9 120.6(7) . . ?
C32 N31 C30 120.4(6) . . ?
C36 N31 C30 119.0(6) . . ?
C36 N31 C32 120.4(6) . . ?
C15 C14 C17 120.5(6) . . ?
C13 C14 C15 119.1(6) . . ?
C13 C14 C17 120.5(6) . . ?
O28 C27 Nd1 51.5(3) . 2_657 ?
O28 C27 O29 123.1(6) . . ?
O28 C27 C24 118.2(6) . . ?
O29 C27 Nd1 71.6(4) . 2_657 ?
O29 C27 C24 118.6(7) . . ?
C24 C27 Nd1 169.6(5) . 2_657 ?
C22 N21 C20 122.0(6) . . ?
C22 N21 C26 119.9(6) . . ?
C26 N21 C20 117.9(7) . . ?
C16 N11 C12 121.4(6) . . ?
C16 N11 C10 122.1(6) . . ?
C12 N11 C10 116.4(6) . . ?
C14 C15 H15 120.6 . . ?
C16 C15 C14 118.9(6) . . ?
C16 C15 H15 120.6 . . ?
C6 C5 C30 120.7(6) . . ?
C6 C5 C4 121.1(6) . . ?
C4 C5 C30 117.5(6) . . ?
C33 C34 C35 119.0(6) . . ?
C33 C34 C37 122.1(6) . . ?
C35 C34 C37 118.8(6) . . ?
C4 C3 C20 118.1(7) . . ?
C4 C3 C2 120.5(6) . . ?
C2 C3 C20 120.9(7) . . ?
O18 C17 C14 117.2(6) . . ?
O19 C17 O18 126.2(6) . . ?
O19 C17 C14 116.6(6) . . ?
C34 C33 H33 120.1 . . ?
C32 C33 C34 119.9(6) . . ?
C32 C33 H33 120.1 . . ?
C25 C24 C27 120.3(7) . . ?
C25 C24 C23 119.1(7) . . ?
C23 C24 C27 120.6(7) . . ?
N31 C30 C5 115.5(6) . . ?
N31 C30 H30A 108.4 . . ?
N31 C30 H30B 108.4 . . ?
C5 C30 H30A 108.4 . . ?
C5 C30 H30B 108.4 . . ?
H30A C30 H30B 107.5 . . ?
N21 C22 H22 119.1 . . ?
N21 C22 C23 121.9(8) . . ?
C23 C22 H22 119.1 . . ?
C6 C1 C2 120.8(7) . . ?
C6 C1 C10 120.5(7) . . ?
C2 C1 C10 118.7(7) . . ?
N11 C16 C15 121.3(6) . . ?
N11 C16 H16 119.3 . . ?
C15 C16 H16 119.3 . . ?
C24 C25 H25 120.3 . . ?
C24 C25 C26 119.4(7) . . ?
C26 C25 H25 120.3 . . ?
N21 C20 C3 115.1(6) . . ?
N21 C20 H20A 108.5 . . ?
N21 C20 H20B 108.5 . . ?
C3 C20 H20A 108.5 . . ?
C3 C20 H20B 108.5 . . ?
H20A C20 H20B 107.5 . . ?
C14 C13 H13 120.2 . . ?
C14 C13 C12 119.7(6) . . ?
C12 C13 H13 120.2 . . ?
N11 C12 C13 119.7(7) . . ?
N11 C12 H12 120.2 . . ?
C13 C12 H12 120.2 . . ?
N31 C32 H32 119.9 . . ?
C33 C32 N31 120.3(6) . . ?
C33 C32 H32 119.9 . . ?
C5 C4 C8 120.7(6) . . ?
C3 C4 C5 119.1(7) . . ?
C3 C4 C8 120.2(6) . . ?
C34 C35 H35 120.3 . . ?
C36 C35 C34 119.3(6) . . ?
C36 C35 H35 120.3 . . ?
N31 C36 C35 121.0(6) . . ?
N31 C36 H36 119.5 . . ?
C35 C36 H36 119.5 . . ?
N21 C26 C25 121.0(8) . . ?
N21 C26 H26 119.5 . . ?
C25 C26 H26 119.5 . . ?
C24 C23 C22 118.7(8) . . ?
C24 C23 H23 120.7 . . ?
C22 C23 H23 120.7 . . ?
C3 C2 C1 119.2(7) . . ?
C3 C2 C7 121.2(7) . . ?
C1 C2 C7 119.6(7) . . ?
N11 C10 H10A 108.7 . . ?
N11 C10 H10B 108.7 . . ?
C1 C10 N11 114.1(6) . . ?
C1 C10 H10A 108.7 . . ?
C1 C10 H10B 108.7 . . ?
H10A C10 H10B 107.6 . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C4 C8 H8A 109.5 . . ?
C4 C8 H8B 109.5 . . ?
C4 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
F7A C5A S1A 110.3(8) . . ?
F7A C5A F8A 104.0(9) . . ?
F6A C5A S1A 113.5(8) . . ?
F6A C5A F7A 108.2(9) . . ?
F6A C5A F8A 108.1(10) . . ?
F8A C5A S1A 112.2(7) . . ?
C37 O39 Nd1 132.9(4) . 2_667 ?
C37 O38 Nd1 141.5(5) . 1_566 ?
O39 C37 C34 117.6(6) . . ?
O39 C37 O38 127.9(6) . . ?
O38 C37 C34 114.5(6) . . ?
Nd1 O2W H2WA 110.7 . . ?
Nd1 O2W H2WB 110.6 . . ?
H2WA O2W H2WB 108.2 . . ?
Nd1 O1W H1WA 109.9 . . ?
Nd1 O1W H1WB 110.2 . . ?
H1WA O1W H1WB 108.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Nd1 O28 C27 O29 1.6(8) 2_657 . . . ?
Nd1 O28 C27 C24 -177.7(5) 2_657 . . . ?
Nd1 O29 C27 Nd1 171(3) 1_556 . . 2_657 ?
Nd1 O29 C27 O28 170(2) 1_556 . . . ?
Nd1 O29 C27 O28 -1.3(7) 2_657 . . . ?
Nd1 O29 C27 C24 178.0(6) 2_657 . . . ?
Nd1 O29 C27 C24 -11(3) 1_556 . . . ?
Nd1 O19 C17 O18 -2.3(11) 2_556 . . . ?
Nd1 O19 C17 C14 179.6(4) 2_556 . . . ?
Nd1 C27 C24 C25 155(2) 2_657 . . . ?
Nd1 C27 C24 C23 -24(3) 2_657 . . . ?
Nd1 O39 C37 C34 175.6(4) 2_667 . . . ?
Nd1 O39 C37 O38 -4.4(11) 2_667 . . . ?
Nd1 O38 C37 C34 -138.3(6) 1_566 . . . ?
Nd1 O38 C37 O39 41.6(12) 1_566 . . . ?
O28 C27 C24 C25 165.3(7) . . . . ?
O28 C27 C24 C23 -13.7(11) . . . . ?
O29 C27 C24 C25 -14.0(10) . . . . ?
O29 C27 C24 C23 167.0(8) . . . . ?
C6 C5 C30 N31 -101.0(7) . . . . ?
C6 C5 C4 C3 -4.1(10) . . . . ?
C6 C5 C4 C8 176.3(6) . . . . ?
C6 C1 C2 C3 -2.9(11) . . . . ?
C6 C1 C2 C7 176.6(8) . . . . ?
C6 C1 C10 N11 -97.2(8) . . . . ?
C14 C15 C16 N11 -1.5(11) . . . . ?
C14 C13 C12 N11 0.4(12) . . . . ?
C27 C24 C25 C26 -178.8(7) . . . . ?
C27 C24 C23 C22 178.5(8) . . . . ?
N21 C22 C23 C24 0.2(15) . . . . ?
O4A S1A C5A F7A -176.1(7) . . . . ?
O4A S1A C5A F6A 62.3(9) . . . . ?
O4A S1A C5A F8A -60.6(9) . . . . ?
C15 C14 C17 O18 -179.8(6) . . . . ?
C15 C14 C17 O19 -1.5(9) . . . . ?
C15 C14 C13 C12 0.1(11) . . . . ?
C5 C6 C1 C2 1.5(10) . . . . ?
C5 C6 C1 C10 -178.2(6) . . . . ?
C34 C33 C32 N31 2.5(10) . . . . ?
C34 C35 C36 N31 3.0(11) . . . . ?
C17 C14 C15 C16 -179.0(6) . . . . ?
C17 C14 C13 C12 179.5(7) . . . . ?
C33 C34 C35 C36 -2.5(11) . . . . ?
C33 C34 C37 O39 14.5(10) . . . . ?
C33 C34 C37 O38 -165.5(6) . . . . ?
C24 C25 C26 N21 0.3(13) . . . . ?
C30 N31 C32 C33 173.2(6) . . . . ?
C30 N31 C36 C35 -176.1(7) . . . . ?
C30 C5 C4 C3 166.6(6) . . . . ?
C30 C5 C4 C8 -13.0(9) . . . . ?
C22 N21 C20 C3 -32.9(11) . . . . ?
C22 N21 C26 C25 -0.7(12) . . . . ?
C1 C6 C5 C30 -168.4(6) . . . . ?
C1 C6 C5 C4 2.0(10) . . . . ?
C16 N11 C12 C13 -1.5(12) . . . . ?
C16 N11 C10 C1 21.2(10) . . . . ?
O3A S1A C5A F7A -55.4(9) . . . . ?
O3A S1A C5A F6A -177.0(9) . . . . ?
O3A S1A C5A F8A 60.1(10) . . . . ?
C25 C24 C23 C22 -0.5(13) . . . . ?
C20 N21 C22 C23 -174.7(8) . . . . ?
C20 N21 C26 C25 174.6(7) . . . . ?
C20 C3 C4 C5 -169.7(6) . . . . ?
C20 C3 C4 C8 9.9(10) . . . . ?
C20 C3 C2 C1 172.9(7) . . . . ?
C20 C3 C2 C7 -6.6(11) . . . . ?
C13 C14 C15 C16 0.5(10) . . . . ?
C13 C14 C17 O18 0.8(9) . . . . ?
C13 C14 C17 O19 179.0(6) . . . . ?
C12 N11 C16 C15 2.1(11) . . . . ?
C12 N11 C10 C1 -163.2(7) . . . . ?
C32 N31 C30 C5 35.9(9) . . . . ?
C32 N31 C36 C35 -0.8(11) . . . . ?
C4 C5 C30 N31 88.3(8) . . . . ?
C4 C3 C20 N21 -93.2(8) . . . . ?
C4 C3 C2 C1 0.8(11) . . . . ?
C4 C3 C2 C7 -178.7(8) . . . . ?
C35 C34 C33 C32 -0.2(10) . . . . ?
C35 C34 C37 O39 -163.2(7) . . . . ?
C35 C34 C37 O38 16.8(9) . . . . ?
C36 N31 C30 C5 -148.8(7) . . . . ?
C36 N31 C32 C33 -2.0(10) . . . . ?
C26 N21 C22 C23 0.5(14) . . . . ?
C26 N21 C20 C3 151.9(7) . . . . ?
C23 C24 C25 C26 0.3(12) . . . . ?
C2 C3 C20 N21 94.5(8) . . . . ?
C2 C3 C4 C5 2.7(10) . . . . ?
C2 C3 C4 C8 -177.8(7) . . . . ?
C2 C1 C10 N11 83.1(9) . . . . ?
C10 N11 C16 C15 177.4(7) . . . . ?
C10 N11 C12 C13 -177.0(7) . . . . ?
C10 C1 C2 C3 176.8(6) . . . . ?
C10 C1 C2 C7 -3.7(11) . . . . ?
C9 C6 C5 C30 11.1(10) . . . . ?
C9 C6 C5 C4 -178.5(7) . . . . ?
C9 C6 C1 C2 -178.0(7) . . . . ?
C9 C6 C1 C10 2.3(11) . . . . ?
O2A S1A C5A F7A 67.1(9) . . . . ?
O2A S1A C5A F6A -54.5(10) . . . . ?
O2A S1A C5A F8A -177.4(9) . . . . ?
C37 C34 C33 C32 -177.9(6) . . . . ?
C37 C34 C35 C36 175.3(7) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.114 0.500 0.500 683.4 230.1 '22x water'

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.380
_oxdiff_exptl_absorpt_empirical_full_min 0.706
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_jj003_br_sm_otf_kotfx6_h2o_acet_mp_red2
_database_code_depnum_ccdc_archive 'CCDC 1833437'
loop_
_audit_author_name
_audit_author_address
'Antti Tiihonen'
;University of Jyv?skyl?, Department of Chemistry
Finland
;
_audit_update_record             
;
2018-03-29 deposited with the CCDC.	2019-02-28 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_CHEMW03_I                   
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: The structure contains voids of unresolved electron density
which was treated using Olex2 solvent mask procedure (full details in 
_smtbx_masks_special_details). The 8 water molecules per asymmetric unit 
 are included in the formula and used in the calculations. 
;
_vrf_PLAT412_I                   
;
PROBLEM: Short Intra XH3 .. XHn     H8B      ..H20B
RESPONSE:Hydrogen atoms generated by riding model to their unoptimized
positions.
;
_vrf_PLAT420_I                   
;
PROBLEM: D-H Without Acceptor       O       --H 
RESPONSE: Hydrogen bond acceptors (water located in a void) have been removed 
among the other disordered solvents (also water) in the voids 
(see vrf_CHEMW03_ALERT_2_A).
;
_vrf_FORMU01_I                   
;
PROBLEM: There is a discrepancy between the atom counts in the
            _chemical_formula_sum and _chemical_formula_moiety.
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_CELLZ01_I                   
;
PROBLEM: Difference between formula and atom_site contents detected.
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT041_I                   
;
PROBLEM: Calculated and Reported SumFormula strings Differ ...    
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT042_I                   
;
PROBLEM: Calculated and Reported Moiety formula strings Differ by ...
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT068_I                   
;
PROBLEM: Reported F000 Differs from Calcd (or Missing)...
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT606_I                   
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
# end Validation Reply Form

_audit_creation_date             2018-03-26
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H31 N3 O8 Sm, 1.39(Br), 1.61(C F3 O3 S)'
_chemical_formula_sum            'C31.61 H47 Br1.39 F4.84 N3 O20.84 S1.61 Sm'
_chemical_formula_weight         1207.22
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C32 H31 Br2 F5 N3 Sm1 O13 S1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sm Sm -5.3236 12.2178 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   18.7334(4)
_cell_length_b                   25.6590(5)
_cell_length_c                   9.82867(19)
_cell_angle_alpha                90
_cell_angle_beta                 102.696(2)
_cell_angle_gamma                90
_cell_volume                     4608.92(16)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8435
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      76.1920
_cell_measurement_theta_min      4.1820
_shelx_estimated_absorpt_T_max   0.825
_shelx_estimated_absorpt_T_min   0.188
_exptl_absorpt_coefficient_mu    12.543
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.285
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.43c (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.740
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2417
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
11 1 1 0.0082
-11 -1 -1 0.0082
-3 -5 6 0.0543
-1 16 2 0.0733
3 -7 -6 0.0332
0 -17 1 0.0942
2 13 -4 0.1037

_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.126
_exptl_crystal_size_min          0.016
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
11.0000 0.9998 1.0000 0.9551 -0.2006 0.0413
-11.0000 -0.9998 -1.0000 -0.9551 0.2006 -0.0413
-3.0000 -5.0000 6.0000 0.1482 0.4380 0.8725
-1.0000 16.0000 2.0000 0.2950 0.8466 -0.4683
3.0000 -7.0000 -6.0000 -0.3150 -0.9139 -0.3569
-0.0000 -17.0000 1.0000 -0.1607 -0.5831 0.8390
2.0000 13.0000 -4.0000 0.0356 0.0913 -0.9970

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            16613
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.996
_diffrn_reflns_theta_min         2.969
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -114.00 -14.00   1.00   10.00    --  -41.65 -57.00-180.00  100
  2  ω    -22.00  83.00   1.00   10.00    --   41.65 -19.00   0.00  105
  3  ω     84.00 178.00   1.00   50.00    --  112.00  30.00 150.00   94
  4  ω     59.00 116.00   1.00   50.00    --  112.00-111.00   0.00   57
  5  ω     42.00 113.00   1.00   50.00    --  112.00-111.00-150.00   71
  6  ω     39.00 138.00   1.00   50.00    --  112.00 -45.00 -30.00   99
  7  ω     43.00 100.00   1.00   50.00    --  112.00-111.00 -60.00   57
  8  ω    101.00 164.00   1.00   50.00    --  112.00 111.00 -30.00   63
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0786849000
_diffrn_orient_matrix_UB_12      0.0139017000
_diffrn_orient_matrix_UB_13      0.0756247000
_diffrn_orient_matrix_UB_21      -0.0301103000
_diffrn_orient_matrix_UB_22      0.0396544000
_diffrn_orient_matrix_UB_23      0.0909920000
_diffrn_orient_matrix_UB_31      -0.0022059000
_diffrn_orient_matrix_UB_32      -0.0429681000
_diffrn_orient_matrix_UB_33      0.1085102000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7190
_reflns_number_total             8360
_reflns_odcompleteness_completeness 99.36
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         0.974
_refine_diff_density_min         -1.831
_refine_diff_density_rms         0.125
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     547
_refine_ls_number_reflns         8360
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0529
_refine_ls_restrained_S_all      1.063
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0801P)²+17.8554P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1453
_refine_ls_wR_factor_ref         0.1502
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O43) \\sim Ueq, Uanis(O41) \\sim Ueq, Uanis(O42) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
3. Others
 Sof(Br2B)=1-FVAR(1)
 Sof(S48A)=Sof(F54A)=Sof(O50A)=Sof(O49A)=Sof(F53A)=Sof(F55A)=Sof(O51A)=
 Sof(C52A)=FVAR(1)
4.a Rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
4.b Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C20(H20A,H20B), C10(H10A,H10B)
4.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C13(H13), C35(H35), C12(H12), C32(H32), C36(H36), C25(H25),
 C16(H16), C22(H22), C26(H26), C33(H33), C23(H23)
4.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C8(H8A,H8B,H8C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sm1 Sm 0.38297(2) 0.75021(2) 0.23512(3) 0.01856(11) Uani 1 1 d . . . . .
Br1 Br 0.59780(6) 0.84615(5) 0.55970(11) 0.0770(3) Uani 1 1 d . . . . .
S48A S 0.8106(6) 0.4883(3) 0.0022(11) 0.0328(12) Uani 0.611(5) 1 d . . P A 1
S40 S 0.99672(9) 0.64685(6) 0.36701(16) 0.0357(3) Uani 1 1 d . . . . .
O19 O 0.49647(19) 0.72519(16) 0.6752(4) 0.0265(8) Uani 1 1 d . . . . .
O18 O 0.4661(2) 0.73421(17) 0.4452(4) 0.0272(8) Uani 1 1 d . . . . .
C17 C 0.5102(3) 0.7232(2) 0.5560(5) 0.0205(10) Uani 1 1 d . . . . .
F47 F 1.0393(2) 0.73160(17) 0.2613(5) 0.0508(10) Uani 1 1 d . . . . .
O43 O 1.0003(3) 0.6217(2) 0.2399(5) 0.0479(12) Uani 1 1 d . U . . .
F45 F 1.0583(4) 0.7322(2) 0.4816(5) 0.0820(18) Uani 1 1 d . . . . .
O41 O 1.0275(4) 0.6177(2) 0.4886(5) 0.0700(19) Uani 1 1 d . U . . .
F46 F 1.1270(2) 0.6868(2) 0.3772(6) 0.0706(14) Uani 1 1 d . . . . .
N11 N 0.7285(2) 0.68686(18) 0.5353(5) 0.0245(9) Uani 1 1 d . . . . .
O42 O 0.9273(4) 0.6708(3) 0.3619(9) 0.088(2) Uani 1 1 d . U . . .
C2 C 0.8395(3) 0.5886(2) 0.5282(6) 0.0240(11) Uani 1 1 d . . . . .
C15 C 0.6109(3) 0.7160(3) 0.4267(6) 0.0332(13) Uani 1 1 d . . . . .
H15 H 0.578036 0.729133 0.346337 0.040 Uiso 1 1 calc R . . . .
C34 C 1.1906(3) 0.6787(2) 0.9207(5) 0.0209(10) Uani 1 1 d . . . . .
N31 N 1.0600(2) 0.63032(19) 0.9191(5) 0.0248(9) Uani 1 1 d . . . . .
C13 C 0.6341(3) 0.6855(2) 0.6602(6) 0.0286(12) Uani 1 1 d . . . . .
H13 H 0.617737 0.677619 0.742747 0.034 Uiso 1 1 calc R . . . .
C44 C 1.0588(4) 0.7019(3) 0.3731(7) 0.0395(14) Uani 1 1 d . . . . .
C1 C 0.8457(3) 0.6355(2) 0.6021(6) 0.0227(10) Uani 1 1 d . . . . .
C35 C 1.1708(3) 0.6663(2) 1.0444(5) 0.0265(11) Uani 1 1 d . . . . .
H35 H 1.202234 0.674992 1.131155 0.032 Uiso 1 1 calc R . . . .
C30 C 0.9906(3) 0.6015(3) 0.9240(7) 0.0445(18) Uani 1 1 d . . . . .
H30A H 1.003447 0.566119 0.961378 0.053 Uiso 1 1 calc R . . . .
H30B H 0.965830 0.619760 0.989524 0.053 Uiso 1 1 calc R . . . .
C5 C 0.9382(3) 0.5968(2) 0.7863(6) 0.0296(12) Uani 1 1 d . . . . .
C7 C 0.7876(3) 0.5841(2) 0.3894(6) 0.0324(13) Uani 1 1 d . . . . .
H7A H 0.746283 0.607807 0.386000 0.049 Uiso 1 1 calc GR . . . .
H7B H 0.769648 0.548195 0.375643 0.049 Uiso 1 1 calc GR . . . .
H7C H 0.813032 0.593329 0.315580 0.049 Uiso 1 1 calc GR . . . .
C6 C 0.8932(3) 0.6396(2) 0.7348(6) 0.0251(11) Uani 1 1 d . . . . .
C12 C 0.7051(3) 0.6755(2) 0.6535(6) 0.0316(13) Uani 1 1 d . . . . .
H12 H 0.737940 0.660612 0.731379 0.038 Uiso 1 1 calc R . . . .
C3 C 0.8853(3) 0.5466(2) 0.5816(6) 0.0265(11) Uani 1 1 d . . . . .
C14 C 0.5866(3) 0.7068(2) 0.5478(5) 0.0246(11) Uani 1 1 d . . . . .
C32 C 1.0771(3) 0.6426(2) 0.7975(5) 0.0280(12) Uani 1 1 d . . . . .
H32 H 1.044080 0.634434 0.712208 0.034 Uiso 1 1 calc R . . . .
C36 C 1.1054(3) 0.6414(2) 1.0408(6) 0.0274(11) Uani 1 1 d . . . . .
H36 H 1.092305 0.631985 1.125614 0.033 Uiso 1 1 calc R . . . .
C25 C 0.7468(4) 0.3917(3) 0.4085(7) 0.0416(15) Uani 1 1 d . . . . .
H25 H 0.724979 0.371606 0.329074 0.050 Uiso 1 1 calc R . . . .
C16 C 0.6822(3) 0.7061(3) 0.4224(6) 0.0319(13) Uani 1 1 d . . . . .
H16 H 0.698859 0.712861 0.339577 0.038 Uiso 1 1 calc R . . . .
C22 C 0.8086(4) 0.4518(2) 0.6328(7) 0.0390(14) Uani 1 1 d . . . . .
H22 H 0.829716 0.473137 0.710226 0.047 Uiso 1 1 calc R . . . .
C9 C 0.8967(4) 0.6887(3) 0.8206(8) 0.0452(16) Uani 1 1 d . . . . .
H9A H 0.859401 0.713298 0.773165 0.068 Uiso 1 1 calc GR . . . .
H9B H 0.945256 0.704553 0.831632 0.068 Uiso 1 1 calc GR . . . .
H9C H 0.887742 0.680170 0.912531 0.068 Uiso 1 1 calc GR . . . .
N21 N 0.8250(3) 0.46026(19) 0.5091(6) 0.0340(11) Uani 1 1 d . . . . .
C24 C 0.7304(3) 0.3815(2) 0.5361(6) 0.0301(12) Uani 1 1 d . . . . .
C20 C 0.8830(3) 0.4986(3) 0.4925(8) 0.0397(16) Uani 1 1 d . . . . .
H20A H 0.874304 0.509325 0.393482 0.048 Uiso 1 1 calc R . . . .
H20B H 0.931254 0.481194 0.516581 0.048 Uiso 1 1 calc R . . . .
C26 C 0.7948(4) 0.4312(3) 0.3967(8) 0.0429(16) Uani 1 1 d . . . . .
H26 H 0.806750 0.438061 0.309258 0.051 Uiso 1 1 calc R . . . .
C8 C 0.9859(4) 0.5058(3) 0.7640(10) 0.063(2) Uani 1 1 d . . . . .
H8A H 1.036612 0.518235 0.786431 0.095 Uiso 1 1 calc GR . . . .
H8B H 0.980705 0.478492 0.692725 0.095 Uiso 1 1 calc GR . . . .
H8C H 0.973316 0.491542 0.848255 0.095 Uiso 1 1 calc GR . . . .
C33 C 1.1424(3) 0.6671(2) 0.7955(5) 0.0243(11) Uani 1 1 d . . . . .
H33 H 1.154263 0.676004 0.709308 0.029 Uiso 1 1 calc R . . . .
C23 C 0.7609(3) 0.4121(2) 0.6492(7) 0.0347(13) Uani 1 1 d . . . . .
H23 H 0.749448 0.406041 0.737285 0.042 Uiso 1 1 calc R . . . .
C4 C 0.9352(3) 0.5506(2) 0.7095(7) 0.0351(14) Uani 1 1 d . . . . .
C10 C 0.8072(3) 0.6825(2) 0.5324(7) 0.0307(12) Uani 1 1 d . . . . .
H10A H 0.832782 0.713885 0.577351 0.037 Uiso 1 1 calc R . . . .
H10B H 0.811613 0.682562 0.433815 0.037 Uiso 1 1 calc R . . . .
O28 O 0.6770(2) 0.32165(16) 0.6670(4) 0.0293(8) Uani 1 1 d . . . . .
O29 O 0.6488(2) 0.31681(19) 0.4342(4) 0.0378(10) Uani 1 1 d . . . . .
C27 C 0.6805(3) 0.3357(2) 0.5480(6) 0.0298(12) Uani 1 1 d . . . . .
F54A F 0.8419(5) 0.5860(4) 0.0469(10) 0.073(3) Uani 0.611(5) 1 d . . P A 1
O50A O 0.8726(4) 0.4832(4) -0.0653(8) 0.048(2) Uani 0.611(5) 1 d . . P A 1
O49A O 0.8318(4) 0.4818(4) 0.1517(7) 0.055(2) Uani 0.611(5) 1 d . . P A 1
F53A F 0.7299(5) 0.5650(3) 0.0395(11) 0.078(3) Uani 0.611(5) 1 d . . P A 1
F55A F 0.7659(5) 0.5686(4) -0.1483(10) 0.077(3) Uani 0.611(5) 1 d . . P A 1
O51A O 0.7478(4) 0.4596(3) -0.0661(8) 0.049(2) Uani 0.611(5) 1 d . . P A 1
C52A C 0.7860(7) 0.5543(5) -0.0204(15) 0.056(3) Uani 0.611(5) 1 d . . P A 1
Br2B Br 0.8223(4) 0.4832(3) 0.0256(8) 0.060(2) Uani 0.389(5) 1 d . . P A 2
O39 O 1.3022(2) 0.7147(2) 1.0389(4) 0.0464(13) Uani 1 1 d . . . . .
O38 O 1.2799(2) 0.71157(18) 0.8078(4) 0.0323(9) Uani 1 1 d . . . . .
C37 C 1.2638(3) 0.7043(2) 0.9234(6) 0.0270(12) Uani 1 1 d . . . . .
O1W O 0.4255(3) 0.83536(18) 0.3475(5) 0.0432(11) Uani 1 1 d . . . . .
H1WA H 0.429958 0.857554 0.285044 0.065 Uiso 1 1 d GR . . . .
H1WB H 0.468753 0.831933 0.397340 0.065 Uiso 1 1 d GR . . . .
O2W O 0.4418(3) 0.66861(18) 0.1847(5) 0.0446(11) Uani 1 1 d . . . . .
H2WA H 0.436088 0.644106 0.243494 0.067 Uiso 1 1 d GR . . . .
H2WB H 0.489335 0.672356 0.200416 0.067 Uiso 1 1 d GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sm1 O19 2.412(4) 4_575 ?
Sm1 O18 2.333(4) . ?
Sm1 O28 2.462(4) 3_666 ?
Sm1 O29 2.369(4) 2_655 ?
Sm1 O39 2.357(4) 1_454 ?
Sm1 O38 2.409(4) 4_475 ?
Sm1 O1W 2.498(4) . ?
Sm1 O2W 2.466(4) . ?
S48A O50A 1.464(13) . ?
S48A O49A 1.445(12) . ?
S48A O51A 1.427(11) . ?
S48A C52A 1.757(16) . ?
S40 O43 1.421(5) . ?
S40 O41 1.420(6) . ?
S40 O42 1.428(6) . ?
S40 C44 1.823(7) . ?
O19 C17 1.254(6) . ?
O18 C17 1.247(6) . ?
C17 C14 1.509(7) . ?
F47 C44 1.321(8) . ?
F45 C44 1.322(8) . ?
F46 C44 1.327(8) . ?
N11 C12 1.361(7) . ?
N11 C16 1.344(7) . ?
N11 C10 1.485(6) . ?
C2 C1 1.397(8) . ?
C2 C7 1.495(8) . ?
C2 C3 1.405(8) . ?
C15 H15 0.9500 . ?
C15 C14 1.385(7) . ?
C15 C16 1.368(8) . ?
C34 C35 1.383(7) . ?
C34 C33 1.389(7) . ?
C34 C37 1.516(7) . ?
N31 C30 1.506(7) . ?
N31 C32 1.341(7) . ?
N31 C36 1.337(7) . ?
C13 H13 0.9500 . ?
C13 C12 1.371(8) . ?
C13 C14 1.371(8) . ?
C1 C6 1.413(8) . ?
C1 C10 1.493(7) . ?
C35 H35 0.9500 . ?
C35 C36 1.377(8) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C5 1.491(8) . ?
C5 C6 1.409(8) . ?
C5 C4 1.400(9) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C6 C9 1.509(9) . ?
C12 H12 0.9500 . ?
C3 C20 1.506(8) . ?
C3 C4 1.396(8) . ?
C32 H32 0.9500 . ?
C32 C33 1.378(8) . ?
C36 H36 0.9500 . ?
C25 H25 0.9500 . ?
C25 C24 1.380(9) . ?
C25 C26 1.377(9) . ?
C16 H16 0.9500 . ?
C22 H22 0.9500 . ?
C22 N21 1.336(9) . ?
C22 C23 1.387(9) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
N21 C20 1.501(7) . ?
N21 C26 1.350(9) . ?
C24 C23 1.378(9) . ?
C24 C27 1.522(8) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C26 H26 0.9500 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C8 C4 1.512(9) . ?
C33 H33 0.9500 . ?
C23 H23 0.9500 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
O28 C27 1.239(7) . ?
O29 C27 1.244(7) . ?
F54A C52A 1.375(16) . ?
F53A C52A 1.340(15) . ?
F55A C52A 1.284(16) . ?
O39 C37 1.232(7) . ?
O38 C37 1.253(6) . ?
O1W H1WA 0.8551 . ?
O1W H1WB 0.8548 . ?
O2W H2WA 0.8760 . ?
O2W H2WB 0.8755 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O19 Sm1 O28 142.57(14) 4_575 3_666 ?
O19 Sm1 O1W 70.54(15) 4_575 . ?
O19 Sm1 O2W 73.53(15) 4_575 . ?
O18 Sm1 O19 79.02(13) . 4_575 ?
O18 Sm1 O28 78.22(13) . 3_666 ?
O18 Sm1 O29 139.87(16) . 2_655 ?
O18 Sm1 O39 147.13(18) . 1_454 ?
O18 Sm1 O38 103.40(14) . 4_475 ?
O18 Sm1 O1W 71.14(16) . . ?
O18 Sm1 O2W 77.74(16) . . ?
O28 Sm1 O1W 127.63(14) 3_666 . ?
O28 Sm1 O2W 72.85(15) 3_666 . ?
O29 Sm1 O19 74.82(14) 2_655 4_575 ?
O29 Sm1 O28 138.50(15) 2_655 3_666 ?
O29 Sm1 O38 79.68(13) 2_655 4_475 ?
O29 Sm1 O1W 71.71(17) 2_655 . ?
O29 Sm1 O2W 121.71(15) 2_655 . ?
O39 Sm1 O19 110.08(14) 1_454 4_575 ?
O39 Sm1 O28 76.36(14) 1_454 3_666 ?
O39 Sm1 O29 71.74(18) 1_454 2_655 ?
O39 Sm1 O38 89.27(16) 1_454 4_475 ?
O39 Sm1 O1W 141.66(19) 1_454 . ?
O39 Sm1 O2W 75.10(19) 1_454 . ?
O38 Sm1 O19 140.59(15) 4_475 4_575 ?
O38 Sm1 O28 74.02(14) 4_475 3_666 ?
O38 Sm1 O1W 73.20(16) 4_475 . ?
O38 Sm1 O2W 145.84(16) 4_475 . ?
O2W Sm1 O1W 135.92(17) . . ?
O50A S48A C52A 104.0(7) . . ?
O49A S48A O50A 112.5(8) . . ?
O49A S48A C52A 104.2(8) . . ?
O51A S48A O50A 113.3(8) . . ?
O51A S48A O49A 115.7(8) . . ?
O51A S48A C52A 105.8(9) . . ?
O43 S40 O42 112.5(5) . . ?
O43 S40 C44 103.2(3) . . ?
O41 S40 O43 114.3(3) . . ?
O41 S40 O42 117.0(4) . . ?
O41 S40 C44 104.0(4) . . ?
O42 S40 C44 103.7(4) . . ?
C17 O19 Sm1 127.7(3) . 4_576 ?
C17 O18 Sm1 177.0(4) . . ?
O19 C17 C14 116.9(4) . . ?
O18 C17 O19 125.0(5) . . ?
O18 C17 C14 118.0(4) . . ?
C12 N11 C10 120.5(5) . . ?
C16 N11 C12 120.9(5) . . ?
C16 N11 C10 118.4(4) . . ?
C1 C2 C7 120.3(5) . . ?
C1 C2 C3 119.5(5) . . ?
C3 C2 C7 120.2(5) . . ?
C14 C15 H15 119.9 . . ?
C16 C15 H15 119.9 . . ?
C16 C15 C14 120.2(5) . . ?
C35 C34 C33 118.8(5) . . ?
C35 C34 C37 120.0(5) . . ?
C33 C34 C37 121.2(4) . . ?
C32 N31 C30 121.4(5) . . ?
C36 N31 C30 117.3(5) . . ?
C36 N31 C32 121.2(5) . . ?
C12 C13 H13 119.9 . . ?
C12 C13 C14 120.1(5) . . ?
C14 C13 H13 119.9 . . ?
F47 C44 S40 111.2(5) . . ?
F47 C44 F45 106.4(6) . . ?
F47 C44 F46 106.5(6) . . ?
F45 C44 S40 111.4(5) . . ?
F45 C44 F46 109.0(6) . . ?
F46 C44 S40 112.1(5) . . ?
C2 C1 C6 120.6(5) . . ?
C2 C1 C10 118.7(5) . . ?
C6 C1 C10 120.4(5) . . ?
C34 C35 H35 120.2 . . ?
C36 C35 C34 119.5(5) . . ?
C36 C35 H35 120.2 . . ?
N31 C30 H30A 108.7 . . ?
N31 C30 H30B 108.7 . . ?
H30A C30 H30B 107.6 . . ?
C5 C30 N31 114.3(5) . . ?
C5 C30 H30A 108.7 . . ?
C5 C30 H30B 108.7 . . ?
C6 C5 C30 119.0(6) . . ?
C4 C5 C30 119.9(6) . . ?
C4 C5 C6 121.1(5) . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C1 C6 C9 121.3(5) . . ?
C5 C6 C1 118.6(5) . . ?
C5 C6 C9 120.1(5) . . ?
N11 C12 C13 119.9(5) . . ?
N11 C12 H12 120.0 . . ?
C13 C12 H12 120.0 . . ?
C2 C3 C20 118.2(5) . . ?
C4 C3 C2 120.9(5) . . ?
C4 C3 C20 120.7(5) . . ?
C15 C14 C17 119.6(5) . . ?
C13 C14 C17 121.5(5) . . ?
C13 C14 C15 118.8(5) . . ?
N31 C32 H32 119.8 . . ?
N31 C32 C33 120.4(5) . . ?
C33 C32 H32 119.8 . . ?
N31 C36 C35 120.6(5) . . ?
N31 C36 H36 119.7 . . ?
C35 C36 H36 119.7 . . ?
C24 C25 H25 120.1 . . ?
C26 C25 H25 120.1 . . ?
C26 C25 C24 119.8(6) . . ?
N11 C16 C15 120.0(5) . . ?
N11 C16 H16 120.0 . . ?
C15 C16 H16 120.0 . . ?
N21 C22 H22 119.8 . . ?
N21 C22 C23 120.5(6) . . ?
C23 C22 H22 119.8 . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C22 N21 C20 121.5(5) . . ?
C22 N21 C26 121.1(5) . . ?
C26 N21 C20 117.1(5) . . ?
C25 C24 C27 118.7(5) . . ?
C23 C24 C25 119.3(6) . . ?
C23 C24 C27 122.0(5) . . ?
C3 C20 H20A 108.8 . . ?
C3 C20 H20B 108.8 . . ?
N21 C20 C3 113.7(5) . . ?
N21 C20 H20A 108.8 . . ?
N21 C20 H20B 108.8 . . ?
H20A C20 H20B 107.7 . . ?
C25 C26 H26 120.0 . . ?
N21 C26 C25 120.0(6) . . ?
N21 C26 H26 120.0 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C4 C8 H8A 109.5 . . ?
C4 C8 H8B 109.5 . . ?
C4 C8 H8C 109.5 . . ?
C34 C33 H33 120.3 . . ?
C32 C33 C34 119.4(5) . . ?
C32 C33 H33 120.3 . . ?
C22 C23 H23 120.4 . . ?
C24 C23 C22 119.3(6) . . ?
C24 C23 H23 120.4 . . ?
C5 C4 C8 120.4(6) . . ?
C3 C4 C5 119.1(5) . . ?
C3 C4 C8 120.5(6) . . ?
N11 C10 C1 115.7(4) . . ?
N11 C10 H10A 108.4 . . ?
N11 C10 H10B 108.4 . . ?
C1 C10 H10A 108.4 . . ?
C1 C10 H10B 108.4 . . ?
H10A C10 H10B 107.4 . . ?
C27 O28 Sm1 135.2(4) . 3_666 ?
C27 O29 Sm1 155.5(5) . 2_645 ?
O28 C27 C24 117.2(5) . . ?
O28 C27 O29 128.4(5) . . ?
O29 C27 C24 114.3(5) . . ?
F54A C52A S48A 110.9(9) . . ?
F53A C52A S48A 110.6(10) . . ?
F53A C52A F54A 104.9(12) . . ?
F55A C52A S48A 114.3(12) . . ?
F55A C52A F54A 109.3(11) . . ?
F55A C52A F53A 106.4(11) . . ?
C37 O39 Sm1 167.8(5) . 1_656 ?
C37 O38 Sm1 134.3(4) . 4_676 ?
O39 C37 C34 116.9(5) . . ?
O39 C37 O38 126.5(5) . . ?
O38 C37 C34 116.5(5) . . ?
Sm1 O1W H1WA 109.7 . . ?
Sm1 O1W H1WB 109.5 . . ?
H1WA O1W H1WB 104.4 . . ?
Sm1 O2W H2WA 110.6 . . ?
Sm1 O2W H2WB 110.7 . . ?
H2WA O2W H2WB 103.2 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C26 H26 O49A 0.95 2.05 2.949(10) 157.3 . yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Sm1 O19 C17 O18 0.3(8) 4_576 . . . ?
Sm1 O19 C17 C14 179.5(3) 4_576 . . . ?
Sm1 O28 C27 C24 -175.1(4) 3_666 . . . ?
Sm1 O28 C27 O29 3.9(10) 3_666 . . . ?
Sm1 O29 C27 C24 120.5(8) 2_645 . . . ?
Sm1 O29 C27 O28 -58.6(12) 2_645 . . . ?
Sm1 O39 C37 C34 -145.4(19) 1_656 . . . ?
Sm1 O39 C37 O38 36(3) 1_656 . . . ?
Sm1 O38 C37 C34 179.1(4) 4_676 . . . ?
Sm1 O38 C37 O39 -2.7(10) 4_676 . . . ?
O19 C17 C14 C15 -164.2(5) . . . . ?
O19 C17 C14 C13 12.3(8) . . . . ?
O18 C17 C14 C15 15.1(8) . . . . ?
O18 C17 C14 C13 -168.4(5) . . . . ?
O43 S40 C44 F47 57.0(5) . . . . ?
O43 S40 C44 F45 175.5(5) . . . . ?
O43 S40 C44 F46 -62.0(6) . . . . ?
O41 S40 C44 F47 176.6(5) . . . . ?
O41 S40 C44 F45 -64.9(6) . . . . ?
O41 S40 C44 F46 57.6(6) . . . . ?
O42 S40 C44 F47 -60.5(6) . . . . ?
O42 S40 C44 F45 58.0(7) . . . . ?
O42 S40 C44 F46 -179.5(6) . . . . ?
C2 C1 C6 C5 4.7(7) . . . . ?
C2 C1 C6 C9 -175.6(5) . . . . ?
C2 C1 C10 N11 82.5(6) . . . . ?
C2 C3 C20 N21 -86.9(7) . . . . ?
C2 C3 C4 C5 1.4(8) . . . . ?
C2 C3 C4 C8 -178.1(6) . . . . ?
C34 C35 C36 N31 -1.7(9) . . . . ?
N31 C30 C5 C6 -79.9(8) . . . . ?
N31 C30 C5 C4 99.2(7) . . . . ?
N31 C32 C33 C34 0.4(9) . . . . ?
C1 C2 C3 C20 -173.6(5) . . . . ?
C1 C2 C3 C4 2.0(8) . . . . ?
C35 C34 C33 C32 -1.5(8) . . . . ?
C35 C34 C37 O39 -2.5(9) . . . . ?
C35 C34 C37 O38 175.9(5) . . . . ?
C30 N31 C32 C33 -177.4(6) . . . . ?
C30 N31 C36 C35 178.2(6) . . . . ?
C30 C5 C6 C1 177.8(5) . . . . ?
C30 C5 C6 C9 -1.9(8) . . . . ?
C30 C5 C4 C3 179.2(5) . . . . ?
C30 C5 C4 C8 -1.3(9) . . . . ?
C7 C2 C1 C6 178.4(5) . . . . ?
C7 C2 C1 C10 -7.8(7) . . . . ?
C7 C2 C3 C20 2.8(8) . . . . ?
C7 C2 C3 C4 178.5(5) . . . . ?
C6 C1 C10 N11 -103.7(6) . . . . ?
C6 C5 C4 C3 -1.8(8) . . . . ?
C6 C5 C4 C8 177.7(6) . . . . ?
C12 N11 C16 C15 2.0(10) . . . . ?
C12 N11 C10 C1 42.6(8) . . . . ?
C12 C13 C14 C17 -174.0(6) . . . . ?
C12 C13 C14 C15 2.6(9) . . . . ?
C3 C2 C1 C6 -5.1(7) . . . . ?
C3 C2 C1 C10 168.6(5) . . . . ?
C14 C15 C16 N11 0.9(10) . . . . ?
C14 C13 C12 N11 0.1(10) . . . . ?
C32 N31 C30 C5 -10.3(10) . . . . ?
C32 N31 C36 C35 0.6(9) . . . . ?
C36 N31 C30 C5 172.2(6) . . . . ?
C36 N31 C32 C33 0.1(9) . . . . ?
C25 C24 C23 C22 -1.3(10) . . . . ?
C25 C24 C27 O28 167.5(6) . . . . ?
C25 C24 C27 O29 -11.7(8) . . . . ?
C16 N11 C12 C13 -2.5(9) . . . . ?
C16 N11 C10 C1 -142.6(6) . . . . ?
C16 C15 C14 C17 173.5(6) . . . . ?
C16 C15 C14 C13 -3.1(10) . . . . ?
C22 N21 C20 C3 -37.0(8) . . . . ?
C22 N21 C26 C25 -0.7(10) . . . . ?
N21 C22 C23 C24 -0.2(10) . . . . ?
C24 C25 C26 N21 -0.9(11) . . . . ?
C20 C3 C4 C5 176.9(5) . . . . ?
C20 C3 C4 C8 -2.6(9) . . . . ?
C20 N21 C26 C25 173.5(6) . . . . ?
C26 C25 C24 C23 1.9(10) . . . . ?
C26 C25 C24 C27 -176.6(6) . . . . ?
C26 N21 C20 C3 148.8(6) . . . . ?
C33 C34 C35 C36 2.1(8) . . . . ?
C33 C34 C37 O39 177.7(6) . . . . ?
C33 C34 C37 O38 -3.9(8) . . . . ?
C23 C22 N21 C20 -172.7(6) . . . . ?
C23 C22 N21 C26 1.2(10) . . . . ?
C23 C24 C27 O28 -11.0(9) . . . . ?
C23 C24 C27 O29 169.9(6) . . . . ?
C4 C5 C6 C1 -1.2(8) . . . . ?
C4 C5 C6 C9 179.1(5) . . . . ?
C4 C3 C20 N21 97.4(7) . . . . ?
C10 N11 C12 C13 172.3(6) . . . . ?
C10 N11 C16 C15 -172.9(6) . . . . ?
C10 C1 C6 C5 -168.9(5) . . . . ?
C10 C1 C6 C9 10.7(8) . . . . ?
C27 C24 C23 C22 177.1(6) . . . . ?
O50A S48A C52A F54A -63.0(12) . . . . ?
O50A S48A C52A F53A -178.9(10) . . . . ?
O50A S48A C52A F55A 61.1(12) . . . . ?
O49A S48A C52A F54A 55.0(12) . . . . ?
O49A S48A C52A F53A -60.8(12) . . . . ?
O49A S48A C52A F55A 179.1(10) . . . . ?
O51A S48A C52A F54A 177.5(10) . . . . ?
O51A S48A C52A F53A 61.6(13) . . . . ?
O51A S48A C52A F55A -58.5(12) . . . . ?
C37 C34 C35 C36 -177.7(5) . . . . ?
C37 C34 C33 C32 178.3(5) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.222 0.190 0.415 44.6 15.3 '1x water'
2 0.222 0.310 0.915 44.6 15.8 '1x water'
3 0.500 0.000 -0.188 483.8 138.1 '14x water'
4 0.500 0.500 -0.146 483.8 138.1 '14x water'
5 0.778 0.690 0.085 44.6 13.8 '1x water'
6 0.778 0.810 0.585 44.6 14.3 '1x water'

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.535
_oxdiff_exptl_absorpt_empirical_full_min 0.703
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_jj003_br_nd_otf_kotfx6_h2o_acet_red2
_database_code_depnum_ccdc_archive 'CCDC 1833435'
loop_
_audit_author_name
_audit_author_address
'Antti Tiihonen'
;University of Jyv?skyl?, Department of Chemistry
Finland
;
_audit_update_record             
;
2018-03-29 deposited with the CCDC.	2019-02-28 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_CHEMW03_I                   
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: The structure contains voids of unresolved electron density
which was treated using Olex2 solvent mask procedure (full details in 
_smtbx_masks_special_details). The 5.5 water molecules per asymmetric unit 
 are included in the formula and used in the calculations. 
;
_vrf_PLAT420_I                   
;
PROBLEM: D-H Without Acceptor       O       --H 
RESPONSE: Hydrogen bond acceptor (water located in a void) have been removed 
among the other disordered solvents (also water) in the voids 
(see vrf_CHEMW03_ALERT_2_B).
;
_vrf_FORMU01_I                   
;
PROBLEM: There is a discrepancy between the atom counts in the
            _chemical_formula_sum and _chemical_formula_moiety.
RESPONSE: See explanation above (CHEMW03_ALERT_2_B).
;
_vrf_CELLZ01_I                   
;
PROBLEM: Difference between formula and atom_site contents detected.
RESPONSE: See explanation above (CHEMW03_ALERT_2_B).
;
_vrf_PLAT041_I                   
;
PROBLEM: Calculated and Reported SumFormula strings Differ ...    
RESPONSE: See explanation above (CHEMW03_ALERT_2_B).
;
_vrf_PLAT042_I                   
;
PROBLEM: Calculated and Reported Moiety formula strings Differ by ...
RESPONSE: See explanation above (CHEMW03_ALERT_2_B).
;
_vrf_PLAT068_I                   
;
PROBLEM: Reported F000 Differs from Calcd (or Missing)...
RESPONSE: See explanation above (CHEMW03_ALERT_2_B).
;
_vrf_PLAT606_I                   
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure
RESPONSE: See explanation above (CHEMW03_ALERT_2_B).
;
# end Validation Reply Form
_audit_creation_date             2018-03-26
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H33 N3 Nd O9, 3(C F3 O3 S), H2 O, 0.5(O)'
_chemical_formula_sum            'C33 H46 F9 N3 Nd O25 S3'
_chemical_formula_weight         1296.15
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C33 H33 N3 O20 S3 F9 Nd1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -3.1807 10.9079 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.1157(3)
_cell_length_b                   14.2420(4)
_cell_length_c                   19.1578(7)
_cell_angle_alpha                110.861(3)
_cell_angle_beta                 101.670(3)
_cell_angle_gamma                91.706(3)
_cell_volume                     2510.09(16)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    10397
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      76.7370
_cell_measurement_theta_min      3.2900
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    10.144
_exptl_absorpt_correction_T_max  0.794
_exptl_absorpt_correction_T_min  0.462
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.43c (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plank
_exptl_crystal_F_000             1308
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 1 -11 0.0297
1 -2 12 0.0082
-5 -5 3 0.0565
-6 4 0 0.0706
0 -9 3 0.0111
0 9 -3 0.0403
7 1 -3 0.0618

_exptl_crystal_size_max          0.148
_exptl_crystal_size_mid          0.051
_exptl_crystal_size_min          0.042
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-1.0000 1.0000 -11.0001 0.9436 -0.2269 -0.1509
1.0000 -2.0000 12.0001 -1.0197 0.2113 0.0630
-5.0000 -5.0000 2.9998 0.1601 0.4251 -0.8413
-6.0000 4.0000 -0.0000 0.4461 0.8954 -0.0242
0.0000 -9.0000 2.9998 -0.2095 -0.3553 -0.8908
-0.0000 9.0000 -2.9998 0.2095 0.3553 0.8908
7.0000 1.0000 -2.9999 -0.3006 -0.8606 0.5708

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0595
_diffrn_reflns_av_unetI/netI     0.0725
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            15789
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.000
_diffrn_reflns_theta_min         3.342
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3953
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -66.00  11.00   1.00    1.50    --  -41.90  37.00 -30.00   77
  2  ω    -65.00  29.00   1.00    1.50    --  -41.90  37.00-150.00   94
  3  ω    -82.00  -8.00   1.00    1.50    --  -41.90 125.00 -60.00   74
  4  ω   -112.00 -18.00   1.00    1.50    --  -41.90 -37.00  30.00   94
  5  ω     57.00  90.00   1.00    1.50    --   41.90-125.00-150.00   33
  6  ω     54.00 145.00   1.00    4.50    --  112.00 -77.00-150.00   91
  7  ω     40.00 111.00   1.00    4.50    --  112.00 -45.00-150.00   71
  8  ω    106.00 175.00   1.00    4.50    --  112.00  30.00   0.00   69
  9  ω     52.00 138.00   1.00    4.50    --  112.00 -45.00 -60.00   86
 10  ω     73.00 141.00   1.00    4.50    --  112.00 -61.00   0.00   68
 11  ω     36.00 116.00   1.00    4.50    --  112.00-111.00-180.00   80
 12  ω     43.00 118.00   1.00    4.50    --  112.00 -45.00 120.00   75
 13  ω     60.00 116.00   1.00    4.50    --  112.00-111.00  30.00   56
 14  ω     35.00 169.00   1.00    4.50    --  112.00   0.00 150.00  134
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0764036000
_diffrn_orient_matrix_UB_12      -0.0030930000
_diffrn_orient_matrix_UB_13      -0.0791206000
_diffrn_orient_matrix_UB_21      -0.1149676000
_diffrn_orient_matrix_UB_22      0.0513947000
_diffrn_orient_matrix_UB_23      0.0357536000
_diffrn_orient_matrix_UB_31      0.0736963000
_diffrn_orient_matrix_UB_32      0.1044839000
_diffrn_orient_matrix_UB_33      0.0165198000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8463
_reflns_number_total             9109
_reflns_odcompleteness_completeness 99.56
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         2.152
_refine_diff_density_min         -2.245
_refine_diff_density_rms         0.141
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         9109
_refine_ls_number_restraints     96
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0526
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0903P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1363
_refine_ls_wR_factor_ref         0.1402
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C60B) \\sim Ueq, Uanis(S56B) \\sim Ueq, Uanis(O59B) \\sim Ueq,
Uanis(O58B) \\sim Ueq, Uanis(O57B) \\sim Ueq, Uanis(F63B) \\sim Ueq,
Uanis(F62B) \\sim Ueq, Uanis(F61B) \\sim Ueq, Uanis(F63A) \\sim Ueq,
Uanis(S56A) \\sim Ueq, Uanis(O58A) \\sim Ueq, Uanis(O59A) \\sim Ueq,
Uanis(O57A) \\sim Ueq, Uanis(C60A) \\sim Ueq, Uanis(F61A) \\sim Ueq,
Uanis(F62A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: S56B(0.5) O59B(0.5) O58B(0.5) F63B(0.5) F62B(0.5) F61B(0.5)
 C60B(0.5) S56A(0.5) O58A(0.5) O59A(0.5) O57A(0.5) F63A(0.5) F61A(0.5)
 C60A(0.5) F62A(0.5) O57B(0.5) O5W(0.5)
4.a Free rotating group:
 O4W(H4WA,H4WB)
4.b Rotating group:
 O2W(H2WA,H2WB), O1W(H1WA,H1WB), O3W(H3WA,H3WB)
4.c Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C30(H30A,H30B), C20(H20A,H20B)
4.d Aromatic/amide H refined with riding coordinates:
 C15(H15), C13(H13), C36(H36), C12(H12), C16(H16), C35(H35), C32(H32),
 C33(H33), C26(H26), C25(H25), C22(H22), C23(H23)
4.e Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Nd1 Nd 0.75395(2) 0.00993(2) 0.50231(2) 0.01219(10) Uani 1 1 d . . . . .
S48 S 0.59549(13) 0.18131(9) -0.09425(7) 0.0230(3) Uani 1 1 d . . . . .
S40 S 0.97637(12) 0.14058(10) 0.19510(7) 0.0228(3) Uani 1 1 d . . . . .
S56B S 0.8143(5) -0.4015(3) 0.2015(3) 0.0403(9) Uani 0.5 1 d . U P A 1
O19 O 0.3284(3) 0.0287(3) 0.40028(18) 0.0193(7) Uani 1 1 d . . . . .
O2W O 0.8634(3) 0.1503(3) 0.47794(19) 0.0200(7) Uani 1 1 d . . . . .
H2WA H 0.875687 0.208657 0.518604 0.030 Uiso 1 1 d GR . . . .
H2WB H 0.808559 0.165376 0.441333 0.030 Uiso 1 1 d GR . . . .
O1W O 0.5920(3) -0.1446(3) 0.4237(2) 0.0243(7) Uani 1 1 d . . . . .
H1WA H 0.511272 -0.134190 0.431004 0.036 Uiso 1 1 d GR . . . .
H1WB H 0.611902 -0.193110 0.439804 0.036 Uiso 1 1 d GR . . . .
O50 O 0.5016(4) 0.1479(3) -0.0590(2) 0.0294(8) Uani 1 1 d . . . . .
O18 O 0.5534(3) 0.0571(3) 0.44009(19) 0.0217(7) Uani 1 1 d . . . . .
O42 O 0.8306(4) 0.1247(3) 0.1724(2) 0.0332(9) Uani 1 1 d . . . . .
O39 O 0.3008(3) 0.8277(3) 0.40194(18) 0.0197(7) Uani 1 1 d . . . . .
F55 F 0.7619(4) 0.3461(3) -0.0504(2) 0.0494(10) Uani 1 1 d . . . . .
O38 O 0.1789(4) 0.6976(3) 0.4074(3) 0.0365(10) Uani 1 1 d . . . . .
F47 F 1.1499(5) 0.2883(3) 0.2094(3) 0.0640(13) Uani 1 1 d . . . . .
O41 O 1.0319(4) 0.1554(4) 0.2744(2) 0.0370(9) Uani 1 1 d . . . . .
F53 F 0.7103(5) 0.3133(4) 0.0429(2) 0.0673(14) Uani 1 1 d . . . . .
F46 F 0.9720(6) 0.2612(5) 0.1197(4) 0.0774(18) Uani 1 1 d . . . . .
O43 O 1.0464(4) 0.0737(3) 0.1423(2) 0.0367(10) Uani 1 1 d . . . . .
F45 F 0.9605(6) 0.3332(3) 0.2375(4) 0.0745(16) Uani 1 1 d . . . . .
O51 O 0.5391(5) 0.1945(4) -0.1645(3) 0.0466(12) Uani 1 1 d . . . . .
O49 O 0.7158(5) 0.1301(3) -0.0950(3) 0.0455(12) Uani 1 1 d . . . . .
F54 F 0.5660(5) 0.3708(3) -0.0240(3) 0.0598(12) Uani 1 1 d . . . . .
N11 N 0.4730(4) 0.0886(3) 0.1859(2) 0.0161(8) Uani 1 1 d . . . . .
N31 N 0.3978(5) 0.5252(3) 0.1959(2) 0.0241(9) Uani 1 1 d . . . . .
C14 C 0.4548(4) 0.0632(3) 0.3191(2) 0.0134(8) Uani 1 1 d . . . . .
C1 C 0.4002(5) 0.1732(4) 0.0921(2) 0.0161(9) Uani 1 1 d . . . . .
C17 C 0.4441(5) 0.0487(3) 0.3927(2) 0.0157(9) Uani 1 1 d . . . . .
C6 C 0.4549(5) 0.2757(4) 0.1261(3) 0.0179(9) Uani 1 1 d . . . . .
C10 C 0.4846(5) 0.0962(4) 0.1111(3) 0.0198(10) Uani 1 1 d . . . . .
H10A H 0.455072 0.029206 0.069466 0.024 Uiso 1 1 calc R . . . .
H10B H 0.580962 0.114785 0.113579 0.024 Uiso 1 1 calc R . . . .
C15 C 0.3425(5) 0.0834(4) 0.2744(3) 0.0190(9) Uani 1 1 d . . . . .
H15 H 0.258305 0.088697 0.289427 0.023 Uiso 1 1 calc R . . . .
C13 C 0.5759(5) 0.0556(4) 0.2962(3) 0.0205(10) Uani 1 1 d . . . . .
H13 H 0.653763 0.041873 0.326603 0.025 Uiso 1 1 calc R . . . .
C3 C 0.2054(5) 0.2147(4) 0.0170(2) 0.0170(9) Uani 1 1 d . . . . .
C30 C 0.4514(6) 0.4539(4) 0.1307(3) 0.0247(11) Uani 1 1 d . . . . .
H30A H 0.550668 0.455047 0.148183 0.030 Uiso 1 1 calc R . . . .
H30B H 0.435678 0.478399 0.087734 0.030 Uiso 1 1 calc R . . . .
C36 C 0.4099(6) 0.6246(4) 0.2072(3) 0.0294(12) Uani 1 1 d . . . . .
H36 H 0.448309 0.646803 0.173648 0.035 Uiso 1 1 calc R . . . .
C4 C 0.2612(5) 0.3167(4) 0.0475(3) 0.0192(10) Uani 1 1 d . . . . .
C12 C 0.5837(5) 0.0681(4) 0.2290(3) 0.0191(9) Uani 1 1 d . . . . .
H12 H 0.666913 0.062297 0.212801 0.023 Uiso 1 1 calc R . . . .
C2 C 0.2762(5) 0.1424(4) 0.0389(3) 0.0170(9) Uani 1 1 d . . . . .
C16 C 0.3541(5) 0.0958(4) 0.2078(3) 0.0210(10) Uani 1 1 d . . . . .
H16 H 0.277170 0.109625 0.176789 0.025 Uiso 1 1 calc R . . . .
C37 C 0.2583(5) 0.7352(4) 0.3808(3) 0.0215(10) Uani 1 1 d . . . . .
C35 C 0.3671(6) 0.6937(4) 0.2666(3) 0.0258(11) Uani 1 1 d . . . . .
H35 H 0.376239 0.763424 0.274305 0.031 Uiso 1 1 calc R . . . .
C5 C 0.3858(5) 0.3458(4) 0.1018(3) 0.0184(9) Uani 1 1 d . . . . .
C32 C 0.3475(6) 0.4926(4) 0.2438(3) 0.0310(12) Uani 1 1 d . . . . .
H32 H 0.341748 0.422672 0.235776 0.037 Uiso 1 1 calc R . . . .
C34 C 0.3103(5) 0.6615(4) 0.3156(3) 0.0219(10) Uani 1 1 d . . . . .
C9 C 0.5847(5) 0.3053(4) 0.1865(3) 0.0283(11) Uani 1 1 d . . . . .
H9A H 0.585857 0.265141 0.218882 0.042 Uiso 1 1 calc GR . . . .
H9B H 0.591197 0.377231 0.218223 0.042 Uiso 1 1 calc GR . . . .
H9C H 0.661905 0.292715 0.161970 0.042 Uiso 1 1 calc GR . . . .
C7 C 0.2195(5) 0.0322(4) 0.0037(3) 0.0254(11) Uani 1 1 d . . . . .
H7A H 0.231656 0.003160 -0.049005 0.038 Uiso 1 1 calc GR . . . .
H7B H 0.122575 0.026230 0.003230 0.038 Uiso 1 1 calc GR . . . .
H7C H 0.267629 -0.004363 0.033981 0.038 Uiso 1 1 calc GR . . . .
C33 C 0.3042(6) 0.5593(4) 0.3044(3) 0.0329(13) Uani 1 1 d . . . . .
H33 H 0.270037 0.535651 0.338531 0.039 Uiso 1 1 calc R . . . .
C52 C 0.6633(7) 0.3078(5) -0.0274(3) 0.0376(14) Uani 1 1 d . . . . .
C8 C 0.1899(6) 0.3937(4) 0.0215(3) 0.0352(13) Uani 1 1 d . . . . .
H8A H 0.225960 0.401070 -0.020248 0.053 Uiso 1 1 calc GR . . . .
H8B H 0.204910 0.458877 0.064568 0.053 Uiso 1 1 calc GR . . . .
H8C H 0.092310 0.371329 0.003348 0.053 Uiso 1 1 calc GR . . . .
C44 C 1.0163(7) 0.2627(5) 0.1911(4) 0.0437(16) Uani 1 1 d . . . . .
O59B O 0.7769(12) -0.4894(9) 0.2172(7) 0.062(3) Uani 0.5 1 d . U P A 1
O58B O 0.7187(9) -0.3760(9) 0.1472(7) 0.053(3) Uani 0.5 1 d . U P A 1
N21 N 0.0763(4) 0.1550(3) -0.1217(2) 0.0150(8) Uani 1 1 d . . . . .
C20 C 0.0700(5) 0.1820(4) -0.0398(3) 0.0199(10) Uani 1 1 d . . . . .
H20A H 0.025765 0.122689 -0.034477 0.024 Uiso 1 1 calc R . . . .
H20B H 0.011653 0.237301 -0.026293 0.024 Uiso 1 1 calc R . . . .
C26 C 0.1960(5) 0.1561(4) -0.1437(3) 0.0181(9) Uani 1 1 d . . . . .
H26 H 0.279150 0.175471 -0.106098 0.022 Uiso 1 1 calc R . . . .
O29 O 0.1881(3) 0.0543(3) -0.37717(17) 0.0180(7) Uani 1 1 d . . . . .
O28 O -0.0350(3) 0.0601(3) -0.40528(18) 0.0174(7) Uani 1 1 d . . . . .
C27 C 0.0758(5) 0.0697(3) -0.3594(2) 0.0146(9) Uani 1 1 d . . . . .
C24 C 0.0757(4) 0.1010(3) -0.2749(2) 0.0144(8) Uani 1 1 d . . . . .
C25 C 0.1972(4) 0.1292(4) -0.2200(3) 0.0170(9) Uani 1 1 d . . . . .
H25 H 0.281009 0.130021 -0.235028 0.020 Uiso 1 1 calc R . . . .
C22 C -0.0427(4) 0.1286(4) -0.1745(3) 0.0174(9) Uani 1 1 d . . . . .
H22 H -0.125571 0.128897 -0.158345 0.021 Uiso 1 1 calc R . . . .
C23 C -0.0457(4) 0.1012(4) -0.2516(3) 0.0165(9) Uani 1 1 d . . . . .
H23 H -0.129952 0.082747 -0.288281 0.020 Uiso 1 1 calc R . . . .
F63B F 1.0164(9) -0.3613(6) 0.1471(6) 0.056(2) Uani 0.5 1 d . U P A 1
F62B F 0.9180(9) -0.5116(7) 0.0883(5) 0.055(2) Uani 0.5 1 d . U P A 1
F61B F 1.0498(9) -0.4708(8) 0.1997(6) 0.068(3) Uani 0.5 1 d . U P A 1
C60B C 0.9562(15) -0.4371(11) 0.1591(9) 0.048(3) Uani 0.5 1 d . U P A 1
S56A S 0.7530(3) -0.3650(2) 0.31667(18) 0.0359(6) Uani 0.5 1 d . U P B 2
O58A O 0.6806(9) -0.2880(7) 0.2990(6) 0.042(2) Uani 0.5 1 d . U P B 2
O59A O 0.6724(9) -0.4595(7) 0.2974(6) 0.047(2) Uani 0.5 1 d . U P B 2
O57A O 0.8424(9) -0.3305(7) 0.3914(6) 0.049(2) Uani 0.5 1 d . U P B 2
O3W O 0.8602(3) -0.1423(3) 0.5022(2) 0.0228(7) Uani 1 1 d . . . . .
H3WA H 0.947209 -0.134930 0.502441 0.034 Uiso 1 1 d GR . . . .
H3WB H 0.827213 -0.193641 0.458745 0.034 Uiso 1 1 d GR . . . .
O4W O 0.8362(5) 0.2157(4) 0.3632(3) 0.0424(11) Uani 1 1 d . . . . .
H4WA H 0.900532 0.201709 0.339895 0.064 Uiso 1 1 d G . . . .
H4WB H 0.819514 0.276028 0.369659 0.064 Uiso 1 1 d G . . . .
F63A F 0.9474(11) -0.3168(7) 0.2603(7) 0.060(3) Uani 0.5 1 d . U P B 2
F61A F 0.9427(10) -0.4671(6) 0.2578(7) 0.064(3) Uani 0.5 1 d . U P B 2
C60A C 0.8701(15) -0.3964(11) 0.2523(10) 0.045(3) Uani 0.5 1 d . U P B 2
F62A F 0.786(2) -0.4295(16) 0.1758(11) 0.109(7) Uani 0.5 1 d . U P B 2
O57B O 0.8715(14) -0.3145(9) 0.2719(7) 0.051(3) Uani 0.5 1 d . U P A 1
O5W O 0.7138(10) -0.3114(8) 0.3782(6) 0.048(2) Uani 0.5 1 d . . P C 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nd1 O19 2.411(3) 2_656 ?
Nd1 O2W 2.487(3) . ?
Nd1 O1W 2.495(3) . ?
Nd1 O18 2.379(3) . ?
Nd1 O39 2.546(3) 2_666 ?
Nd1 O29 2.443(3) 2_655 ?
Nd1 O28 2.384(3) 1_656 ?
Nd1 O3W 2.448(3) . ?
S48 O50 1.430(4) . ?
S48 O51 1.430(5) . ?
S48 O49 1.437(4) . ?
S48 C52 1.812(6) . ?
S40 O42 1.437(4) . ?
S40 O41 1.445(4) . ?
S40 O43 1.441(4) . ?
S40 C44 1.805(7) . ?
S56B O59B 1.444(12) . ?
S56B O58B 1.426(11) . ?
S56B C60B 1.788(17) . ?
S56B O57B 1.463(13) . ?
O19 C17 1.246(6) . ?
O2W H2WA 0.8980 . ?
O2W H2WB 0.8959 . ?
O1W H1WA 0.8642 . ?
O1W H1WB 0.8643 . ?
O18 C17 1.253(6) . ?
O39 C37 1.265(6) . ?
F55 C52 1.342(7) . ?
O38 C37 1.236(7) . ?
F47 C44 1.330(8) . ?
F53 C52 1.309(8) . ?
F46 C44 1.343(9) . ?
F45 C44 1.310(8) . ?
F54 C52 1.347(8) . ?
N11 C10 1.503(5) . ?
N11 C12 1.356(6) . ?
N11 C16 1.346(6) . ?
N31 C30 1.513(6) . ?
N31 C36 1.351(7) . ?
N31 C32 1.340(7) . ?
C14 C17 1.519(6) . ?
C14 C15 1.382(6) . ?
C14 C13 1.378(6) . ?
C1 C6 1.410(7) . ?
C1 C10 1.510(7) . ?
C1 C2 1.392(6) . ?
C6 C5 1.394(7) . ?
C6 C9 1.499(7) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C15 H15 0.9500 . ?
C15 C16 1.375(7) . ?
C13 H13 0.9500 . ?
C13 C12 1.378(7) . ?
C3 C4 1.409(7) . ?
C3 C2 1.406(7) . ?
C3 C20 1.509(6) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C5 1.517(6) . ?
C36 H36 0.9500 . ?
C36 C35 1.370(8) . ?
C4 C5 1.405(7) . ?
C4 C8 1.503(7) . ?
C12 H12 0.9500 . ?
C2 C7 1.511(6) . ?
C16 H16 0.9500 . ?
C37 C34 1.518(7) . ?
C35 H35 0.9500 . ?
C35 C34 1.389(8) . ?
C32 H32 0.9500 . ?
C32 C33 1.373(8) . ?
C34 C33 1.391(8) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C33 H33 0.9500 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
N21 C20 1.493(5) . ?
N21 C26 1.361(6) . ?
N21 C22 1.350(6) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C26 H26 0.9500 . ?
C26 C25 1.376(6) . ?
O29 C27 1.254(6) . ?
O28 C27 1.247(6) . ?
C27 C24 1.520(6) . ?
C24 C25 1.388(6) . ?
C24 C23 1.389(6) . ?
C25 H25 0.9500 . ?
C22 H22 0.9500 . ?
C22 C23 1.380(6) . ?
C23 H23 0.9500 . ?
F63B C60B 1.335(17) . ?
F62B C60B 1.362(18) . ?
F61B C60B 1.314(16) . ?
S56A O58A 1.436(9) . ?
S56A O59A 1.439(9) . ?
S56A O57A 1.435(10) . ?
S56A C60A 1.832(16) . ?
O3W H3WA 0.8820 . ?
O3W H3WB 0.8821 . ?
O4W H4WA 0.8504 . ?
O4W H4WB 0.8499 . ?
F63A C60A 1.302(17) . ?
F61A C60A 1.286(17) . ?
C60A F62A 1.44(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O19 Nd1 O2W 142.30(11) 2_656 . ?
O19 Nd1 O1W 78.32(12) 2_656 . ?
O19 Nd1 O39 70.98(11) 2_656 2_666 ?
O19 Nd1 O29 147.35(12) 2_656 2_655 ?
O19 Nd1 O3W 77.35(12) 2_656 . ?
O2W Nd1 O1W 135.88(12) . . ?
O2W Nd1 O39 74.19(11) . 2_666 ?
O1W Nd1 O39 126.18(11) . 2_666 ?
O18 Nd1 O19 100.41(11) . 2_656 ?
O18 Nd1 O2W 82.35(12) . . ?
O18 Nd1 O1W 70.79(13) . . ?
O18 Nd1 O39 72.68(12) . 2_666 ?
O18 Nd1 O29 86.74(11) . 2_655 ?
O18 Nd1 O28 148.58(13) . 1_656 ?
O18 Nd1 O3W 139.79(13) . . ?
O29 Nd1 O2W 69.96(11) 2_655 . ?
O29 Nd1 O1W 74.07(11) 2_655 . ?
O29 Nd1 O39 140.62(11) 2_655 2_666 ?
O29 Nd1 O3W 76.89(12) 2_655 . ?
O28 Nd1 O19 84.52(11) 1_656 2_656 ?
O28 Nd1 O2W 75.55(11) 1_656 . ?
O28 Nd1 O1W 139.98(12) 1_656 . ?
O28 Nd1 O39 79.91(11) 1_656 2_666 ?
O28 Nd1 O29 105.84(11) 1_656 2_655 ?
O28 Nd1 O3W 71.63(12) 1_656 . ?
O3W Nd1 O2W 123.87(11) . . ?
O3W Nd1 O1W 69.46(12) . . ?
O3W Nd1 O39 138.99(12) . 2_666 ?
O50 S48 O51 116.5(3) . . ?
O50 S48 O49 113.4(2) . . ?
O50 S48 C52 104.5(3) . . ?
O51 S48 O49 114.4(3) . . ?
O51 S48 C52 104.2(3) . . ?
O49 S48 C52 101.5(3) . . ?
O42 S40 O41 114.7(2) . . ?
O42 S40 O43 115.6(2) . . ?
O42 S40 C44 103.4(3) . . ?
O41 S40 C44 103.4(3) . . ?
O43 S40 O41 113.8(3) . . ?
O43 S40 C44 103.9(3) . . ?
O59B S56B C60B 102.6(8) . . ?
O59B S56B O57B 112.0(7) . . ?
O58B S56B O59B 117.7(7) . . ?
O58B S56B C60B 105.9(7) . . ?
O58B S56B O57B 112.9(7) . . ?
O57B S56B C60B 104.0(8) . . ?
C17 O19 Nd1 133.3(3) . 2_656 ?
Nd1 O2W H2WA 111.6 . . ?
Nd1 O2W H2WB 111.3 . . ?
H2WA O2W H2WB 102.3 . . ?
Nd1 O1W H1WA 110.1 . . ?
Nd1 O1W H1WB 110.1 . . ?
H1WA O1W H1WB 103.8 . . ?
C17 O18 Nd1 159.2(3) . . ?
C37 O39 Nd1 133.9(3) . 2_666 ?
C12 N11 C10 118.1(4) . . ?
C16 N11 C10 121.2(4) . . ?
C16 N11 C12 120.5(4) . . ?
C36 N31 C30 117.6(4) . . ?
C32 N31 C30 121.6(4) . . ?
C32 N31 C36 120.8(5) . . ?
C15 C14 C17 120.1(4) . . ?
C13 C14 C17 120.4(4) . . ?
C13 C14 C15 119.5(4) . . ?
C6 C1 C10 118.0(4) . . ?
C2 C1 C6 121.5(4) . . ?
C2 C1 C10 120.4(4) . . ?
O19 C17 O18 125.8(4) . . ?
O19 C17 C14 117.5(4) . . ?
O18 C17 C14 116.7(4) . . ?
C1 C6 C9 119.1(5) . . ?
C5 C6 C1 118.4(4) . . ?
C5 C6 C9 122.5(4) . . ?
N11 C10 C1 112.7(4) . . ?
N11 C10 H10A 109.1 . . ?
N11 C10 H10B 109.1 . . ?
C1 C10 H10A 109.1 . . ?
C1 C10 H10B 109.1 . . ?
H10A C10 H10B 107.8 . . ?
C14 C15 H15 120.4 . . ?
C16 C15 C14 119.2(4) . . ?
C16 C15 H15 120.4 . . ?
C14 C13 H13 120.1 . . ?
C14 C13 C12 119.7(4) . . ?
C12 C13 H13 120.1 . . ?
C4 C3 C20 120.3(4) . . ?
C2 C3 C4 120.2(4) . . ?
C2 C3 C20 119.5(4) . . ?
N31 C30 H30A 108.9 . . ?
N31 C30 H30B 108.9 . . ?
N31 C30 C5 113.4(4) . . ?
H30A C30 H30B 107.7 . . ?
C5 C30 H30A 108.9 . . ?
C5 C30 H30B 108.9 . . ?
N31 C36 H36 119.7 . . ?
N31 C36 C35 120.5(5) . . ?
C35 C36 H36 119.7 . . ?
C3 C4 C8 120.7(5) . . ?
C5 C4 C3 119.2(4) . . ?
C5 C4 C8 120.1(5) . . ?
N11 C12 C13 120.2(4) . . ?
N11 C12 H12 119.9 . . ?
C13 C12 H12 119.9 . . ?
C1 C2 C3 119.3(4) . . ?
C1 C2 C7 120.4(4) . . ?
C3 C2 C7 120.3(4) . . ?
N11 C16 C15 120.9(4) . . ?
N11 C16 H16 119.6 . . ?
C15 C16 H16 119.6 . . ?
O39 C37 C34 116.8(4) . . ?
O38 C37 O39 127.3(5) . . ?
O38 C37 C34 115.9(4) . . ?
C36 C35 H35 120.0 . . ?
C36 C35 C34 119.9(5) . . ?
C34 C35 H35 120.0 . . ?
C6 C5 C30 119.0(4) . . ?
C6 C5 C4 121.3(4) . . ?
C4 C5 C30 119.6(4) . . ?
N31 C32 H32 119.7 . . ?
N31 C32 C33 120.6(5) . . ?
C33 C32 H32 119.7 . . ?
C35 C34 C37 121.5(5) . . ?
C35 C34 C33 118.2(5) . . ?
C33 C34 C37 120.3(5) . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C32 C33 C34 119.9(5) . . ?
C32 C33 H33 120.0 . . ?
C34 C33 H33 120.0 . . ?
F55 C52 S48 111.1(4) . . ?
F55 C52 F54 106.3(5) . . ?
F53 C52 S48 113.7(5) . . ?
F53 C52 F55 108.7(5) . . ?
F53 C52 F54 106.1(6) . . ?
F54 C52 S48 110.5(5) . . ?
C4 C8 H8A 109.5 . . ?
C4 C8 H8B 109.5 . . ?
C4 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
F47 C44 S40 111.1(5) . . ?
F47 C44 F46 106.3(6) . . ?
F46 C44 S40 110.8(6) . . ?
F45 C44 S40 111.4(5) . . ?
F45 C44 F47 108.8(7) . . ?
F45 C44 F46 108.2(6) . . ?
C26 N21 C20 122.4(4) . . ?
C22 N21 C20 117.3(4) . . ?
C22 N21 C26 120.4(4) . . ?
C3 C20 H20A 108.5 . . ?
C3 C20 H20B 108.5 . . ?
N21 C20 C3 115.1(4) . . ?
N21 C20 H20A 108.5 . . ?
N21 C20 H20B 108.5 . . ?
H20A C20 H20B 107.5 . . ?
N21 C26 H26 119.8 . . ?
N21 C26 C25 120.4(4) . . ?
C25 C26 H26 119.8 . . ?
C27 O29 Nd1 131.0(3) . 2_655 ?
C27 O28 Nd1 169.6(3) . 1_454 ?
O29 C27 C24 116.7(4) . . ?
O28 C27 O29 125.5(4) . . ?
O28 C27 C24 117.8(4) . . ?
C25 C24 C27 120.3(4) . . ?
C25 C24 C23 119.2(4) . . ?
C23 C24 C27 120.6(4) . . ?
C26 C25 C24 119.8(4) . . ?
C26 C25 H25 120.1 . . ?
C24 C25 H25 120.1 . . ?
N21 C22 H22 119.5 . . ?
N21 C22 C23 120.9(4) . . ?
C23 C22 H22 119.5 . . ?
C24 C23 H23 120.3 . . ?
C22 C23 C24 119.3(4) . . ?
C22 C23 H23 120.3 . . ?
F63B C60B S56B 112.5(10) . . ?
F63B C60B F62B 104.4(13) . . ?
F62B C60B S56B 111.8(10) . . ?
F61B C60B S56B 113.5(12) . . ?
F61B C60B F63B 107.6(12) . . ?
F61B C60B F62B 106.4(12) . . ?
O58A S56A O59A 115.3(6) . . ?
O58A S56A C60A 104.6(7) . . ?
O59A S56A C60A 104.0(6) . . ?
O57A S56A O58A 114.5(6) . . ?
O57A S56A O59A 113.5(6) . . ?
O57A S56A C60A 103.0(7) . . ?
Nd1 O3W H3WA 111.0 . . ?
Nd1 O3W H3WB 110.8 . . ?
H3WA O3W H3WB 102.9 . . ?
H4WA O4W H4WB 109.5 . . ?
F63A C60A S56A 111.6(12) . . ?
F63A C60A F62A 105.9(15) . . ?
F61A C60A S56A 114.3(12) . . ?
F61A C60A F63A 110.2(13) . . ?
F61A C60A F62A 108.8(16) . . ?
F62A C60A S56A 105.6(12) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Nd1 O19 C17 O18 -2.9(7) 2_656 . . . ?
Nd1 O19 C17 C14 176.5(3) 2_656 . . . ?
Nd1 O18 C17 O19 91.2(9) . . . . ?
Nd1 O18 C17 C14 -88.3(9) . . . . ?
Nd1 O39 C37 O38 -5.3(9) 2_666 . . . ?
Nd1 O39 C37 C34 174.8(3) 2_666 . . . ?
Nd1 O29 C27 O28 -4.8(7) 2_655 . . . ?
Nd1 O29 C27 C24 174.1(3) 2_655 . . . ?
Nd1 O28 C27 O29 78.6(18) 1_454 . . . ?
Nd1 O28 C27 C24 -100.3(16) 1_454 . . . ?
O50 S48 C52 F55 175.0(4) . . . . ?
O50 S48 C52 F53 52.0(6) . . . . ?
O50 S48 C52 F54 -67.3(5) . . . . ?
O42 S40 C44 F47 -178.8(5) . . . . ?
O42 S40 C44 F46 -60.8(5) . . . . ?
O42 S40 C44 F45 59.7(6) . . . . ?
O39 C37 C34 C35 -18.7(8) . . . . ?
O39 C37 C34 C33 160.1(5) . . . . ?
O38 C37 C34 C35 161.4(5) . . . . ?
O38 C37 C34 C33 -19.7(8) . . . . ?
O41 S40 C44 F47 61.4(6) . . . . ?
O41 S40 C44 F46 179.3(5) . . . . ?
O41 S40 C44 F45 -60.1(6) . . . . ?
O43 S40 C44 F47 -57.7(6) . . . . ?
O43 S40 C44 F46 60.2(5) . . . . ?
O43 S40 C44 F45 -179.2(6) . . . . ?
O51 S48 C52 F55 -62.2(5) . . . . ?
O51 S48 C52 F53 174.7(5) . . . . ?
O51 S48 C52 F54 55.4(5) . . . . ?
O49 S48 C52 F55 56.9(5) . . . . ?
O49 S48 C52 F53 -66.2(6) . . . . ?
O49 S48 C52 F54 174.6(4) . . . . ?
N31 C30 C5 C6 -99.9(5) . . . . ?
N31 C30 C5 C4 84.1(6) . . . . ?
N31 C36 C35 C34 -0.3(9) . . . . ?
N31 C32 C33 C34 1.1(10) . . . . ?
C14 C15 C16 N11 -0.1(8) . . . . ?
C14 C13 C12 N11 0.6(8) . . . . ?
C1 C6 C5 C30 -172.8(4) . . . . ?
C1 C6 C5 C4 3.1(7) . . . . ?
C17 C14 C15 C16 -179.6(4) . . . . ?
C17 C14 C13 C12 179.4(4) . . . . ?
C6 C1 C10 N11 82.1(5) . . . . ?
C6 C1 C2 C3 1.6(7) . . . . ?
C6 C1 C2 C7 -179.6(4) . . . . ?
C10 N11 C12 C13 -176.9(4) . . . . ?
C10 N11 C16 C15 176.5(4) . . . . ?
C10 C1 C6 C5 172.1(4) . . . . ?
C10 C1 C6 C9 -7.6(6) . . . . ?
C10 C1 C2 C3 -174.3(4) . . . . ?
C10 C1 C2 C7 4.5(6) . . . . ?
C15 C14 C17 O19 18.7(6) . . . . ?
C15 C14 C17 O18 -161.8(4) . . . . ?
C15 C14 C13 C12 -0.1(7) . . . . ?
C13 C14 C17 O19 -160.8(4) . . . . ?
C13 C14 C17 O18 18.7(6) . . . . ?
C13 C14 C15 C16 -0.1(7) . . . . ?
C3 C4 C5 C6 -0.1(7) . . . . ?
C3 C4 C5 C30 175.8(4) . . . . ?
C30 N31 C36 C35 -178.1(5) . . . . ?
C30 N31 C32 C33 177.5(5) . . . . ?
C36 N31 C30 C5 -156.5(5) . . . . ?
C36 N31 C32 C33 1.5(9) . . . . ?
C36 C35 C34 C37 -178.4(5) . . . . ?
C36 C35 C34 C33 2.7(8) . . . . ?
C4 C3 C2 C1 1.5(6) . . . . ?
C4 C3 C2 C7 -177.3(4) . . . . ?
C4 C3 C20 N21 87.2(5) . . . . ?
C12 N11 C10 C1 -146.2(4) . . . . ?
C12 N11 C16 C15 0.6(8) . . . . ?
C2 C1 C6 C5 -3.9(7) . . . . ?
C2 C1 C6 C9 176.4(4) . . . . ?
C2 C1 C10 N11 -101.8(5) . . . . ?
C2 C3 C4 C5 -2.2(7) . . . . ?
C2 C3 C4 C8 176.9(5) . . . . ?
C2 C3 C20 N21 -92.2(5) . . . . ?
C16 N11 C10 C1 37.8(6) . . . . ?
C16 N11 C12 C13 -0.8(7) . . . . ?
C37 C34 C33 C32 178.0(5) . . . . ?
C35 C34 C33 C32 -3.1(9) . . . . ?
C32 N31 C30 C5 27.4(7) . . . . ?
C32 N31 C36 C35 -1.9(9) . . . . ?
C9 C6 C5 C30 6.9(7) . . . . ?
C9 C6 C5 C4 -177.2(5) . . . . ?
C8 C4 C5 C6 -179.2(5) . . . . ?
C8 C4 C5 C30 -3.3(7) . . . . ?
O59B S56B C60B F63B -173.5(10) . . . . ?
O59B S56B C60B F62B 69.4(11) . . . . ?
O59B S56B C60B F61B -50.9(12) . . . . ?
O58B S56B C60B F63B 62.6(12) . . . . ?
O58B S56B C60B F62B -54.5(12) . . . . ?
O58B S56B C60B F61B -174.9(11) . . . . ?
N21 C26 C25 C24 0.1(7) . . . . ?
N21 C22 C23 C24 0.0(7) . . . . ?
C20 C3 C4 C5 178.4(4) . . . . ?
C20 C3 C4 C8 -2.6(7) . . . . ?
C20 C3 C2 C1 -179.1(4) . . . . ?
C20 C3 C2 C7 2.1(6) . . . . ?
C20 N21 C26 C25 179.0(4) . . . . ?
C20 N21 C22 C23 -179.1(4) . . . . ?
C26 N21 C20 C3 2.5(7) . . . . ?
C26 N21 C22 C23 0.7(7) . . . . ?
O29 C27 C24 C25 11.8(6) . . . . ?
O29 C27 C24 C23 -167.9(4) . . . . ?
O28 C27 C24 C25 -169.2(4) . . . . ?
O28 C27 C24 C23 11.1(7) . . . . ?
C27 C24 C25 C26 -179.1(4) . . . . ?
C27 C24 C23 C22 179.1(4) . . . . ?
C25 C24 C23 C22 -0.6(7) . . . . ?
C22 N21 C20 C3 -177.8(4) . . . . ?
C22 N21 C26 C25 -0.7(7) . . . . ?
C23 C24 C25 C26 0.6(7) . . . . ?
O58A S56A C60A F63A 55.9(13) . . . . ?
O58A S56A C60A F61A -178.2(11) . . . . ?
O58A S56A C60A F62A -58.7(13) . . . . ?
O59A S56A C60A F63A 177.3(11) . . . . ?
O59A S56A C60A F61A -56.8(13) . . . . ?
O59A S56A C60A F62A 62.7(13) . . . . ?
O57A S56A C60A F63A -64.1(13) . . . . ?
O57A S56A C60A F61A 61.8(13) . . . . ?
O57A S56A C60A F62A -178.7(12) . . . . ?
O57B S56B C60B F63B -56.6(12) . . . . ?
O57B S56B C60B F62B -173.7(10) . . . . ?
O57B S56B C60B F61B 66.0(12) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.885 0.500 0.500 380.5 109.2 '11x water'

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.561
_oxdiff_exptl_absorpt_empirical_full_min 0.662
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_jj003_y_no3_h2o_acet_red3
_database_code_depnum_ccdc_archive 'CCDC 1833444'
loop_
_audit_author_name
_audit_author_address
'Antti Tiihonen'
;University of Jyv?skyl?, Department of Chemistry
Finland
;
_audit_update_record             
;
2018-03-29 deposited with the CCDC.	2019-02-28 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_CHEMW03_I                   
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as...
RESPONSE: The structure contains voids of unresolved electron density
which was treated using Olex2 solvent mask procedure (full details in 
_smtbx_masks_special_details). The 10 water molecules per asymmetric unit 
 are included in the formula and used in the calculations. 
;
_vrf_PLAT412_I                   
;
PROBLEM: Short Intra XH3 .. XHn...
RESPONSE: Hydrogen atoms calculated using a riding model in their general
(unoptimized) geometry causing a proximity alert.
;
_vrf_PLAT420_I                   
;
PROBLEM: D-H Without Acceptor...
RESPONSE: Hydrogen bond acceptors (water) have been removed among
other disordered solvent from the voids (see CHEMW03_ALERT_2_A).
;
_vrf_FORMU01_I                   
;
PROBLEM: There is a discrepancy between the atom counts...
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_CELLZ01_I                   
;
PROBLEM: Difference between formula and atom_site...
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT041_I                   
;
PROBLEM: Calc. and Reported SumFormula Strings  Differ...
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT051_I                   
;
PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs...
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT068_I                   
;
PROBLEM: Reported F000 Differs from Calcd (or Missing)...
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT606_I                   
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure...
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
# end Validation Reply Form

_audit_creation_date             2018-03-28
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H31 N3 O8 Y, 3(N O3)'
_chemical_formula_sum            'C30 H41 N6 O22 Y'
_chemical_formula_weight         926.60
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C21 N6 H25 O14 Y'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Y Y -0.2670 2.0244 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.5796(3)
_cell_length_b                   12.0095(7)
_cell_length_c                   18.6284(5)
_cell_angle_alpha                104.551(4)
_cell_angle_beta                 98.841(3)
_cell_angle_gamma                102.169(4)
_cell_volume                     1978.82(16)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6822
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      76.5780
_cell_measurement_theta_min      3.9170
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.906
_exptl_absorpt_correction_T_max  0.890
_exptl_absorpt_correction_T_min  0.792
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             956
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2 6 2 0.0378
0 -8 1 0.0216
1 4 -12 0.0624
-4 -2 10 0.0427
-6 2 0 0.0293
-5 -3 3 0.0301
6 -1 -6 0.0434
1 -6 -5 0.0267
0 7 -1 0.0386
6 -2 1 0.0236

_exptl_crystal_size_max          0.136
_exptl_crystal_size_mid          0.061
_exptl_crystal_size_min          0.057
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
2.0005 5.9992 2.0005 0.7832 0.5627 0.3846
-0.0005 -7.9992 0.9992 -1.0319 -0.2348 -0.1930
0.9997 4.0003 -11.9991 0.4593 -0.7790 0.4979
-3.9995 -2.0003 9.9994 -0.2040 0.4588 -0.8613
-5.9997 1.9999 0.0002 0.2705 -0.3818 -0.8571
-4.9999 -2.9997 2.9996 -0.3650 -0.2506 -0.8797
5.9995 -0.9997 -5.9999 -0.1695 -0.0861 1.0097
0.9993 -5.9991 -5.0004 -0.8032 -0.5858 0.1309
0.0004 6.9993 -0.9993 0.9023 0.1949 0.1716
5.9997 -2.0000 0.9997 -0.2657 0.4664 0.8353

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_unetI/netI     0.0482
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            11727
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.999
_diffrn_reflns_theta_min         3.939
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -108.00   0.00   1.00    2.00    --  -41.40 -19.00-180.00  108
  2  ω   -116.00 -31.00   1.00    2.00    --  -41.40 -37.00 120.00   85
  3  ω      1.00  61.00   1.00    2.00    --   41.40 -99.00   0.00   60
  4  ω      2.00  67.00   1.00    2.00    --   41.40 -99.00  90.00   65
  5  ω     39.00  92.00   1.00    2.00    --   41.40-125.00-120.00   53
  6  ω     46.00 141.00   1.00   20.00    --  112.00 -61.00  30.00   95
  7  ω    107.00 140.00   1.00   20.00    --  112.00 -30.00 120.00   33
  8  ω     90.00 155.00   1.00   20.00    --  112.00  30.00   0.00   65
  9  ω     51.00  90.00   1.00   20.00    --  112.00 -30.00 120.00   39
 10  ω     50.00 145.00   1.00   20.00    --  112.00 -77.00-120.00   95
 11  ω     88.00 138.00   1.00   20.00    --  112.00 -45.00-180.00   50
 12  ω     38.00 116.00   1.00   20.00    --  112.00-111.00  60.00   78
 13  ω     41.00  70.00   1.00   20.00    --  112.00 -45.00-180.00   29
 14  ω     29.00 109.00   1.00   20.00    --  112.00 -94.00-180.00   80
 15  ω     32.00 159.00   1.00   20.00    --  112.00 -15.00 -30.00  127
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0018833000
_diffrn_orient_matrix_UB_12      0.1295943000
_diffrn_orient_matrix_UB_13      0.0047700000
_diffrn_orient_matrix_UB_21      0.0769427000
_diffrn_orient_matrix_UB_22      0.0399196000
_diffrn_orient_matrix_UB_23      0.0846443000
_diffrn_orient_matrix_UB_31      0.1499890000
_diffrn_orient_matrix_UB_32      0.0213852000
_diffrn_orient_matrix_UB_33      -0.0218692000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6564
_reflns_number_total             7185
_reflns_odcompleteness_completeness 99.38
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         1.862
_refine_diff_density_min         -0.967
_refine_diff_density_rms         0.112
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         7185
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0551
_refine_ls_restrained_S_all      1.110
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0599P)²+6.7601P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1496
_refine_ls_wR_factor_ref         0.1527
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 N44-O45 \\sim N44-O46 \\sim N44-O47
 with sigma of 0.02
 N48-O51 \\sim N48-O49 \\sim N48-O50
 with sigma of 0.02
 N40-O42 \\sim N40-O41 \\sim N40-O43
 with sigma of 0.02
3.a Rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
3.b Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C10(H10A,H10B), C20(H20A,H20B)
3.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C12(H12), C33(H33), C32(H32), C16(H16), C15(H15), C36(H36),
 C35(H35), C23(H23), C26(H26), C22(H22), C25(H25)
3.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C8(H8A,H8B,H8C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Y1 Y 0.26124(4) 0.48557(3) 0.49768(2) 0.02145(13) Uani 1 1 d . . . . .
O18 O 0.1734(3) 0.5008(3) 0.61049(15) 0.0268(7) Uani 1 1 d . . . . .
O28 O 0.2806(3) 1.3438(3) 1.38792(16) 0.0279(7) Uani 1 1 d . . . . .
O38 O 0.3744(3) 0.5929(3) 1.42266(17) 0.0294(7) Uani 1 1 d . . . . .
O29 O 0.5252(3) 1.3978(3) 1.41803(16) 0.0312(7) Uani 1 1 d . . . . .
O46 O 0.7370(4) 0.7391(3) 0.9258(2) 0.0413(8) Uani 1 1 d D . . . .
O49 O 0.0647(4) 0.6215(3) 1.1269(2) 0.0413(8) Uani 1 1 d D . . . .
O50 O -0.1049(4) 0.7083(4) 1.1480(3) 0.0516(10) Uani 1 1 d D . . . .
N11 N 0.0594(4) 0.6242(3) 0.86517(18) 0.0220(7) Uani 1 1 d . . . . .
N31 N 0.5231(4) 0.6817(3) 1.19681(19) 0.0238(7) Uani 1 1 d . . . . .
O45 O 0.5146(4) 0.6656(5) 0.9300(2) 0.0580(12) Uani 1 1 d D . . . .
C27 C 0.4042(5) 1.3388(4) 1.3754(2) 0.0272(9) Uani 1 1 d . . . . .
O47 O 0.6054(5) 0.5809(4) 0.8400(2) 0.0500(10) Uani 1 1 d D . . . .
N44 N 0.6182(4) 0.6613(4) 0.8987(2) 0.0295(8) Uani 1 1 d D . . . .
C2 C 0.2947(4) 0.6702(4) 1.0311(2) 0.0223(8) Uani 1 1 d . . . . .
N21 N 0.4228(5) 1.1189(3) 1.1610(2) 0.0310(8) Uani 1 1 d . . . . .
C13 C 0.1764(5) 0.5560(4) 0.7661(2) 0.0237(8) Uani 1 1 d . . . . .
H13 H 0.259058 0.534094 0.750438 0.028 Uiso 1 1 calc R . . . .
C6 C 0.2426(5) 0.8541(4) 1.0157(2) 0.0265(9) Uani 1 1 d . . . . .
O43 O -0.0979(5) 0.1391(5) 0.2178(3) 0.0668(14) Uani 1 1 d D . . . .
C4 C 0.4688(5) 0.8603(4) 1.0993(2) 0.0253(9) Uani 1 1 d . . . . .
C5 C 0.3765(5) 0.9191(4) 1.0652(2) 0.0270(9) Uani 1 1 d . . . . .
C17 C 0.0570(4) 0.5184(4) 0.6282(2) 0.0223(8) Uani 1 1 d . . . . .
C34 C 0.5093(5) 0.6570(4) 1.3382(2) 0.0238(8) Uani 1 1 d . . . . .
C3 C 0.4276(4) 0.7371(4) 1.0817(2) 0.0224(8) Uani 1 1 d . . . . .
O41 O -0.1733(7) 0.2192(5) 0.3158(3) 0.0740(15) Uani 1 1 d D . . . .
C1 C 0.2033(5) 0.7296(4) 0.9991(2) 0.0241(8) Uani 1 1 d . . . . .
C37 C 0.5002(5) 0.6278(4) 1.4122(2) 0.0254(9) Uani 1 1 d . . . . .
C12 C 0.1761(4) 0.5946(4) 0.8426(2) 0.0247(9) Uani 1 1 d . . . . .
H12 H 0.259684 0.600032 0.879444 0.030 Uiso 1 1 calc R . . . .
C30 C 0.5276(5) 0.6737(4) 1.1156(2) 0.0247(8) Uani 1 1 d . . . . .
H30A H 0.499334 0.588732 1.085275 0.030 Uiso 1 1 calc R . . . .
H30B H 0.629160 0.708577 1.112714 0.030 Uiso 1 1 calc R . . . .
C7 C 0.2582(5) 0.5364(4) 1.0111(2) 0.0268(9) Uani 1 1 d . . . . .
H7A H 0.334871 0.507867 0.988672 0.040 Uiso 1 1 calc GR . . . .
H7B H 0.164121 0.502186 0.974539 0.040 Uiso 1 1 calc GR . . . .
H7C H 0.251904 0.512090 1.057217 0.040 Uiso 1 1 calc GR . . . .
C14 C 0.0546(4) 0.5497(4) 0.7124(2) 0.0221(8) Uani 1 1 d . . . . .
C33 C 0.3866(5) 0.6637(4) 1.2905(2) 0.0260(9) Uani 1 1 d . . . . .
H33 H 0.296849 0.659711 1.306691 0.031 Uiso 1 1 calc R . . . .
N48 N 0.0155(5) 0.6897(5) 1.1677(3) 0.0544(14) Uani 1 1 d D . . . .
C32 C 0.3954(5) 0.6761(4) 1.2198(2) 0.0261(9) Uani 1 1 d . . . . .
H32 H 0.311770 0.680856 1.187118 0.031 Uiso 1 1 calc R . . . .
C24 C 0.4089(5) 1.2560(4) 1.3001(2) 0.0278(9) Uani 1 1 d . . . . .
C16 C -0.0612(5) 0.6153(4) 0.8140(2) 0.0254(9) Uani 1 1 d . . . . .
H16 H -0.143959 0.635029 0.830975 0.030 Uiso 1 1 calc R . . . .
C15 C -0.0657(5) 0.5776(4) 0.7366(2) 0.0268(9) Uani 1 1 d . . . . .
H15 H -0.151168 0.571021 0.700727 0.032 Uiso 1 1 calc R . . . .
C9 C 0.1389(7) 0.9143(5) 0.9790(3) 0.0432(13) Uani 1 1 d . . . . .
H9A H 0.051878 0.908254 1.000953 0.065 Uiso 1 1 calc GR . . . .
H9B H 0.109540 0.874879 0.924146 0.065 Uiso 1 1 calc GR . . . .
H9C H 0.188356 0.998412 0.988387 0.065 Uiso 1 1 calc GR . . . .
O42 O -0.0107(6) 0.1267(5) 0.3313(3) 0.0733(14) Uani 1 1 d D . . . .
C36 C 0.6446(5) 0.6816(4) 1.2437(3) 0.0294(9) Uani 1 1 d . . . . .
H36 H 0.734449 0.689774 1.227474 0.035 Uiso 1 1 calc R . . . .
C35 C 0.6405(5) 0.6700(5) 1.3148(3) 0.0309(10) Uani 1 1 d . . . . .
H35 H 0.727130 0.670861 1.347755 0.037 Uiso 1 1 calc R . . . .
C23 C 0.2849(5) 1.1722(5) 1.2532(3) 0.0347(10) Uani 1 1 d . . . . .
H23 H 0.194485 1.161488 1.268944 0.042 Uiso 1 1 calc R . . . .
C8 C 0.6140(5) 0.9305(5) 1.1532(3) 0.0382(11) Uani 1 1 d . . . . .
H8A H 0.652072 1.002850 1.139404 0.057 Uiso 1 1 calc GR . . . .
H8B H 0.683987 0.881521 1.149565 0.057 Uiso 1 1 calc GR . . . .
H8C H 0.599723 0.952503 1.205351 0.057 Uiso 1 1 calc GR . . . .
C26 C 0.5447(6) 1.1993(5) 1.2062(3) 0.0393(12) Uani 1 1 d . . . . .
H26 H 0.634033 1.208762 1.189340 0.047 Uiso 1 1 calc R . . . .
C22 C 0.2951(5) 1.1041(5) 1.1830(3) 0.0333(10) Uani 1 1 d . . . . .
H22 H 0.210873 1.046627 1.150253 0.040 Uiso 1 1 calc R . . . .
C25 C 0.5397(6) 1.2676(5) 1.2767(3) 0.0387(11) Uani 1 1 d . . . . .
H25 H 0.626089 1.322668 1.309226 0.046 Uiso 1 1 calc R . . . .
C10 C 0.0558(5) 0.6596(4) 0.9480(2) 0.0270(9) Uani 1 1 d . . . . .
H10A H 0.020834 0.586894 0.962965 0.032 Uiso 1 1 calc R . . . .
H10B H -0.015071 0.708361 0.955907 0.032 Uiso 1 1 calc R . . . .
C20 C 0.4287(6) 1.0528(4) 1.0821(3) 0.0343(10) Uani 1 1 d . . . . .
H20A H 0.530709 1.073757 1.075635 0.041 Uiso 1 1 calc R . . . .
H20B H 0.367322 1.078614 1.045010 0.041 Uiso 1 1 calc R . . . .
N40 N -0.0945(5) 0.1583(4) 0.2860(3) 0.0505(13) Uani 1 1 d D . . . .
O51 O 0.0730(9) 0.7241(9) 1.2375(4) 0.136(4) Uani 1 1 d D . . . .
O19 O -0.0546(3) 0.5167(3) 0.58355(16) 0.0288(7) Uani 1 1 d . . . . .
O39 O 0.6210(3) 0.6384(3) 1.45466(16) 0.0279(7) Uani 1 1 d . . . . .
O1W O 0.0779(3) 0.2990(3) 0.47763(19) 0.0331(7) Uani 1 1 d . . . . .
H1WA H 0.093638 0.268898 0.516201 0.050 Uiso 1 1 d GR . . . .
H1WB H 0.079578 0.244508 0.435611 0.050 Uiso 1 1 d GR . . . .
O2W O 0.2239(4) 0.6813(3) 0.53437(19) 0.0354(7) Uani 1 1 d . . . . .
H2WA H 0.238078 0.710339 0.584739 0.053 Uiso 1 1 d GR . . . .
H2WB H 0.132784 0.680892 0.514597 0.053 Uiso 1 1 d GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Y1 O18 2.361(3) . ?
Y1 O28 2.369(3) 1_544 ?
Y1 O38 2.361(3) 1_554 ?
Y1 O29 2.305(3) 2_677 ?
Y1 O19 2.290(3) 2_566 ?
Y1 O39 2.312(3) 2_667 ?
Y1 O1W 2.442(3) . ?
Y1 O2W 2.396(4) . ?
O18 C17 1.255(5) . ?
O28 C27 1.252(6) . ?
O38 C37 1.251(6) . ?
O29 C27 1.251(6) . ?
O46 N44 1.249(5) . ?
O49 N48 1.196(6) . ?
O50 N48 1.239(6) . ?
N11 C12 1.339(5) . ?
N11 C16 1.346(5) . ?
N11 C10 1.503(5) . ?
N31 C30 1.499(5) . ?
N31 C32 1.350(6) . ?
N31 C36 1.344(6) . ?
O45 N44 1.229(5) . ?
C27 C24 1.515(6) . ?
O47 N44 1.234(5) . ?
C2 C3 1.405(6) . ?
C2 C1 1.396(6) . ?
C2 C7 1.505(6) . ?
N21 C26 1.348(7) . ?
N21 C22 1.340(6) . ?
N21 C20 1.501(5) . ?
C13 H13 0.9500 . ?
C13 C12 1.383(6) . ?
C13 C14 1.391(6) . ?
C6 C5 1.399(7) . ?
C6 C1 1.402(7) . ?
C6 C9 1.523(6) . ?
O43 N40 1.226(6) . ?
C4 C5 1.413(6) . ?
C4 C3 1.387(7) . ?
C4 C8 1.518(6) . ?
C5 C20 1.512(7) . ?
C17 C14 1.523(5) . ?
C17 O19 1.243(5) . ?
C34 C37 1.515(6) . ?
C34 C33 1.390(6) . ?
C34 C35 1.383(6) . ?
C3 C30 1.505(6) . ?
O41 N40 1.253(7) . ?
C1 C10 1.514(6) . ?
C37 O39 1.260(5) . ?
C12 H12 0.9500 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C14 C15 1.374(6) . ?
C33 H33 0.9500 . ?
C33 C32 1.376(6) . ?
N48 O51 1.257(7) . ?
C32 H32 0.9500 . ?
C24 C23 1.386(7) . ?
C24 C25 1.380(7) . ?
C16 H16 0.9500 . ?
C16 C15 1.389(6) . ?
C15 H15 0.9500 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
O42 N40 1.257(6) . ?
C36 H36 0.9500 . ?
C36 C35 1.371(6) . ?
C35 H35 0.9500 . ?
C23 H23 0.9500 . ?
C23 C22 1.387(7) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C26 H26 0.9500 . ?
C26 C25 1.378(7) . ?
C22 H22 0.9500 . ?
C25 H25 0.9500 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
O1W H1WA 0.8886 . ?
O1W H1WB 0.8899 . ?
O2W H2WA 0.8927 . ?
O2W H2WB 0.8923 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O18 Y1 O28 141.95(12) . 1_544 ?
O18 Y1 O1W 73.12(11) . . ?
O18 Y1 O2W 74.33(12) . . ?
O28 Y1 O1W 71.28(11) 1_544 . ?
O28 Y1 O2W 139.50(12) 1_544 . ?
O38 Y1 O18 145.18(12) 1_554 . ?
O38 Y1 O28 72.86(11) 1_554 1_544 ?
O38 Y1 O1W 137.68(11) 1_554 . ?
O38 Y1 O2W 72.93(12) 1_554 . ?
O29 Y1 O18 82.25(11) 2_677 . ?
O29 Y1 O28 117.80(11) 2_677 1_544 ?
O29 Y1 O38 78.17(11) 2_677 1_554 ?
O29 Y1 O39 71.99(12) 2_677 2_667 ?
O29 Y1 O1W 139.46(12) 2_677 . ?
O29 Y1 O2W 74.99(12) 2_677 . ?
O19 Y1 O18 99.79(10) 2_566 . ?
O19 Y1 O28 81.26(11) 2_566 1_544 ?
O19 Y1 O38 81.67(11) 2_566 1_554 ?
O19 Y1 O29 145.90(13) 2_566 2_677 ?
O19 Y1 O39 142.11(12) 2_566 2_667 ?
O19 Y1 O1W 71.42(12) 2_566 . ?
O19 Y1 O2W 72.94(12) 2_566 . ?
O39 Y1 O18 81.22(11) 2_667 . ?
O39 Y1 O28 75.88(11) 2_667 1_544 ?
O39 Y1 O38 118.69(11) 2_667 1_554 ?
O39 Y1 O1W 72.79(11) 2_667 . ?
O39 Y1 O2W 141.03(11) 2_667 . ?
O2W Y1 O1W 125.81(12) . . ?
C17 O18 Y1 133.2(3) . . ?
C27 O28 Y1 119.8(3) . 1_566 ?
C37 O38 Y1 138.1(3) . 1_556 ?
C27 O29 Y1 175.7(3) . 2_677 ?
C12 N11 C16 120.8(3) . . ?
C12 N11 C10 120.7(3) . . ?
C16 N11 C10 118.4(3) . . ?
C32 N31 C30 120.3(3) . . ?
C36 N31 C30 118.5(3) . . ?
C36 N31 C32 120.8(4) . . ?
O28 C27 C24 117.2(4) . . ?
O29 C27 O28 126.5(4) . . ?
O29 C27 C24 116.3(4) . . ?
O45 N44 O46 120.2(4) . . ?
O45 N44 O47 120.4(4) . . ?
O47 N44 O46 119.4(4) . . ?
C3 C2 C7 118.8(4) . . ?
C1 C2 C3 119.0(4) . . ?
C1 C2 C7 122.2(4) . . ?
C26 N21 C20 118.7(4) . . ?
C22 N21 C26 121.4(4) . . ?
C22 N21 C20 119.7(4) . . ?
C12 C13 H13 120.3 . . ?
C12 C13 C14 119.4(4) . . ?
C14 C13 H13 120.3 . . ?
C5 C6 C1 118.9(4) . . ?
C5 C6 C9 122.1(4) . . ?
C1 C6 C9 119.1(4) . . ?
C5 C4 C8 120.7(4) . . ?
C3 C4 C5 119.5(4) . . ?
C3 C4 C8 119.9(4) . . ?
C6 C5 C4 120.5(4) . . ?
C6 C5 C20 121.4(4) . . ?
C4 C5 C20 118.1(4) . . ?
O18 C17 C14 117.0(3) . . ?
O19 C17 O18 125.8(4) . . ?
O19 C17 C14 117.1(4) . . ?
C33 C34 C37 121.6(4) . . ?
C35 C34 C37 119.5(4) . . ?
C35 C34 C33 118.7(4) . . ?
C2 C3 C30 119.3(4) . . ?
C4 C3 C2 120.9(4) . . ?
C4 C3 C30 119.8(4) . . ?
C2 C1 C6 121.3(4) . . ?
C2 C1 C10 119.7(4) . . ?
C6 C1 C10 118.9(4) . . ?
O38 C37 C34 116.5(4) . . ?
O38 C37 O39 127.9(4) . . ?
O39 C37 C34 115.6(4) . . ?
N11 C12 C13 120.7(4) . . ?
N11 C12 H12 119.7 . . ?
C13 C12 H12 119.7 . . ?
N31 C30 C3 112.7(3) . . ?
N31 C30 H30A 109.0 . . ?
N31 C30 H30B 109.0 . . ?
C3 C30 H30A 109.0 . . ?
C3 C30 H30B 109.0 . . ?
H30A C30 H30B 107.8 . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C13 C14 C17 120.5(4) . . ?
C15 C14 C13 119.0(4) . . ?
C15 C14 C17 120.4(4) . . ?
C34 C33 H33 120.1 . . ?
C32 C33 C34 119.9(4) . . ?
C32 C33 H33 120.1 . . ?
O49 N48 O50 123.1(5) . . ?
O49 N48 O51 117.6(5) . . ?
O50 N48 O51 117.6(5) . . ?
N31 C32 C33 120.0(4) . . ?
N31 C32 H32 120.0 . . ?
C33 C32 H32 120.0 . . ?
C23 C24 C27 121.9(4) . . ?
C25 C24 C27 118.6(4) . . ?
C25 C24 C23 119.4(4) . . ?
N11 C16 H16 119.7 . . ?
N11 C16 C15 120.5(4) . . ?
C15 C16 H16 119.7 . . ?
C14 C15 C16 119.5(4) . . ?
C14 C15 H15 120.3 . . ?
C16 C15 H15 120.3 . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N31 C36 H36 119.6 . . ?
N31 C36 C35 120.9(4) . . ?
C35 C36 H36 119.6 . . ?
C34 C35 H35 120.2 . . ?
C36 C35 C34 119.5(4) . . ?
C36 C35 H35 120.2 . . ?
C24 C23 H23 120.6 . . ?
C24 C23 C22 118.9(5) . . ?
C22 C23 H23 120.6 . . ?
C4 C8 H8A 109.5 . . ?
C4 C8 H8B 109.5 . . ?
C4 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N21 C26 H26 120.0 . . ?
N21 C26 C25 120.0(5) . . ?
C25 C26 H26 120.0 . . ?
N21 C22 C23 120.5(4) . . ?
N21 C22 H22 119.7 . . ?
C23 C22 H22 119.7 . . ?
C24 C25 H25 120.1 . . ?
C26 C25 C24 119.8(5) . . ?
C26 C25 H25 120.1 . . ?
N11 C10 C1 113.3(3) . . ?
N11 C10 H10A 108.9 . . ?
N11 C10 H10B 108.9 . . ?
C1 C10 H10A 108.9 . . ?
C1 C10 H10B 108.9 . . ?
H10A C10 H10B 107.7 . . ?
N21 C20 C5 112.8(4) . . ?
N21 C20 H20A 109.0 . . ?
N21 C20 H20B 109.0 . . ?
C5 C20 H20A 109.0 . . ?
C5 C20 H20B 109.0 . . ?
H20A C20 H20B 107.8 . . ?
O43 N40 O41 119.6(5) . . ?
O43 N40 O42 125.1(6) . . ?
O41 N40 O42 115.2(6) . . ?
C17 O19 Y1 179.4(3) . 2_566 ?
C37 O39 Y1 136.8(3) . 2_667 ?
Y1 O1W H1WA 111.3 . . ?
Y1 O1W H1WB 111.1 . . ?
H1WA O1W H1WB 107.5 . . ?
Y1 O2W H2WA 111.8 . . ?
Y1 O2W H2WB 111.1 . . ?
H2WA O2W H2WB 107.1 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1W H1WB O42 0.89 2.03 2.855(7) 154.0 . yes
O2W H2WA O41 0.89 2.08 2.905(6) 153.4 2_566 yes
O2W H2WB O1W 0.89 2.10 2.929(5) 153.3 2_566 yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Y1 O18 C17 C14 -166.7(3) . . . . ?
Y1 O18 C17 O19 10.6(7) . . . . ?
Y1 O28 C27 O29 4.7(7) 1_566 . . . ?
Y1 O28 C27 C24 -173.4(3) 1_566 . . . ?
Y1 O38 C37 C34 159.2(3) 1_556 . . . ?
Y1 O38 C37 O39 -18.4(8) 1_556 . . . ?
O18 C17 C14 C13 -1.0(6) . . . . ?
O18 C17 C14 C15 175.9(4) . . . . ?
O28 C27 C24 C23 -12.3(7) . . . . ?
O28 C27 C24 C25 165.5(5) . . . . ?
O38 C37 O39 Y1 61.1(7) . . . 2_667 ?
O29 C27 C24 C23 169.4(5) . . . . ?
O29 C27 C24 C25 -12.8(7) . . . . ?
N11 C16 C15 C14 -0.3(7) . . . . ?
N31 C36 C35 C34 0.6(8) . . . . ?
C27 C24 C23 C22 176.1(5) . . . . ?
C27 C24 C25 C26 -175.4(5) . . . . ?
C2 C3 C30 N31 -104.1(4) . . . . ?
C2 C1 C10 N11 -93.5(5) . . . . ?
N21 C26 C25 C24 -1.8(9) . . . . ?
C13 C14 C15 C16 2.3(7) . . . . ?
C6 C5 C20 N21 108.3(5) . . . . ?
C6 C1 C10 N11 89.2(5) . . . . ?
C4 C5 C20 N21 -73.3(5) . . . . ?
C4 C3 C30 N31 77.3(5) . . . . ?
C5 C6 C1 C2 0.2(6) . . . . ?
C5 C6 C1 C10 177.5(4) . . . . ?
C5 C4 C3 C2 -0.7(6) . . . . ?
C5 C4 C3 C30 177.9(4) . . . . ?
C17 C14 C15 C16 -174.7(4) . . . . ?
C34 C37 O39 Y1 -116.6(4) . . . 2_667 ?
C34 C33 C32 N31 0.1(7) . . . . ?
C3 C2 C1 C6 0.8(6) . . . . ?
C3 C2 C1 C10 -176.5(3) . . . . ?
C3 C4 C5 C6 1.8(6) . . . . ?
C3 C4 C5 C20 -176.6(4) . . . . ?
C1 C2 C3 C4 -0.6(6) . . . . ?
C1 C2 C3 C30 -179.2(3) . . . . ?
C1 C6 C5 C4 -1.5(6) . . . . ?
C1 C6 C5 C20 176.8(4) . . . . ?
C37 C34 C33 C32 -172.2(4) . . . . ?
C37 C34 C35 C36 171.9(5) . . . . ?
C12 N11 C16 C15 -1.4(7) . . . . ?
C12 N11 C10 C1 35.7(6) . . . . ?
C12 C13 C14 C17 174.5(4) . . . . ?
C12 C13 C14 C15 -2.5(7) . . . . ?
C30 N31 C32 C33 169.3(4) . . . . ?
C30 N31 C36 C35 -169.7(5) . . . . ?
C7 C2 C3 C4 177.3(4) . . . . ?
C7 C2 C3 C30 -1.3(5) . . . . ?
C7 C2 C1 C6 -177.0(4) . . . . ?
C7 C2 C1 C10 5.8(6) . . . . ?
C14 C13 C12 N11 0.9(7) . . . . ?
C33 C34 C37 O38 10.3(7) . . . . ?
C33 C34 C37 O39 -171.8(4) . . . . ?
C33 C34 C35 C36 -4.0(7) . . . . ?
C32 N31 C30 C3 37.7(6) . . . . ?
C32 N31 C36 C35 3.3(7) . . . . ?
C24 C23 C22 N21 0.3(8) . . . . ?
C16 N11 C12 C13 1.1(7) . . . . ?
C16 N11 C10 C1 -148.6(4) . . . . ?
C9 C6 C5 C4 178.8(4) . . . . ?
C9 C6 C5 C20 -2.9(6) . . . . ?
C9 C6 C1 C2 179.9(4) . . . . ?
C9 C6 C1 C10 -2.8(6) . . . . ?
C36 N31 C30 C3 -149.2(4) . . . . ?
C36 N31 C32 C33 -3.6(7) . . . . ?
C35 C34 C37 O38 -165.6(4) . . . . ?
C35 C34 C37 O39 12.4(6) . . . . ?
C35 C34 C33 C32 3.7(7) . . . . ?
C23 C24 C25 C26 2.4(8) . . . . ?
C8 C4 C5 C6 -179.8(4) . . . . ?
C8 C4 C5 C20 1.8(6) . . . . ?
C8 C4 C3 C2 -179.1(4) . . . . ?
C8 C4 C3 C30 -0.5(6) . . . . ?
C26 N21 C22 C23 0.3(8) . . . . ?
C26 N21 C20 C5 126.7(5) . . . . ?
C22 N21 C26 C25 0.5(8) . . . . ?
C22 N21 C20 C5 -58.5(6) . . . . ?
C25 C24 C23 C22 -1.6(8) . . . . ?
C10 N11 C12 C13 176.6(4) . . . . ?
C10 N11 C16 C15 -177.0(4) . . . . ?
C20 N21 C26 C25 175.2(5) . . . . ?
C20 N21 C22 C23 -174.3(5) . . . . ?
O19 C17 C14 C13 -178.6(4) . . . . ?
O19 C17 C14 C15 -1.6(6) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.604 0.000 0.500 417.7 95.4 '10x water'

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.220
_oxdiff_exptl_absorpt_empirical_full_min 0.830
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_jj003_br_sm_otf_h2o_acet_red3
_database_code_depnum_ccdc_archive 'CCDC 1833436'
loop_
_audit_author_name
_audit_author_address
'Antti Tiihonen'
;University of Jyv?skyl?, Department of Chemistry
Finland
;
_audit_update_record             
;
2018-03-29 deposited with the CCDC.	2019-02-28 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_CHEMW03_I                   
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: The structure contains voids of unresolved electron density
which was treated using Olex2 solvent mask procedure (full details in 
_smtbx_masks_special_details). The 11 water molecules per asymmetric unit 
 are included in the formula and used in the calculations. 
;
_vrf_PLAT973_I                   
;
PROBLEM: Check Calcd Positive Resid. Density on       Sm1  
RESPONSE: Peak is located about 1 Angstrom from the metal atom and is caused by
the absorption effects. Data recorded with Cu-radiation. 
;
_vrf_PLAT420_I                   
;
PROBLEM: D-H Without Acceptor       O       --H 
RESPONSE: Hydrogen bond acceptors (water located in a void) have been removed 
among the other disordered solvents (also water) in the voids 
(see vrf_CHEMW03_ALERT_2_A)
;
_vrf_PLAT414_I                   
;
PROBLEM: Short Intra D-H..H-X       H1WA     ..H13 
RESPONSE: Hydrogen atoms generated by riding model in to their
general unoptimized positions.  
;
_vrf_FORMU01_I                   
;
PROBLEM: There is a discrepancy between the atom counts in the
            _chemical_formula_sum and _chemical_formula_moiety.
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_CELLZ01_I                   
;
PROBLEM: Difference between formula and atom_site contents detected.
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT041_I                   
;
PROBLEM: Calculated and Reported SumFormula strings Differ ...    
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT042_I                   
;
PROBLEM: Calculated and Reported Moiety formula strings Differ by ...
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT068_I                   
;
PROBLEM: Reported F000 Differs from Calcd (or Missing)...
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT606_I                   
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
# end Validation Reply Form

_audit_creation_date             2018-03-26
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H31 N3 O8 Sm, 2.17(Br), 0.83(C F3 O3 S)'
_chemical_formula_sum            'C30.83 H53 Br2.17 F2.50 N3 O21.50 S0.83 Sm'
_chemical_formula_weight         1207.41
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C21 H25 O12 N3 F12 S3 Br1 Sm1'
_chemical_oxdiff_usercomment     'clear colorless block'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sm Sm -5.3236 12.2178 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.5251(3)
_cell_length_b                   14.2183(3)
_cell_length_c                   18.8650(7)
_cell_angle_alpha                107.596(3)
_cell_angle_beta                 102.916(3)
_cell_angle_gamma                99.489(2)
_cell_volume                     2298.27(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8378
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      76.5210
_cell_measurement_theta_min      3.3220
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    12.952
_exptl_absorpt_correction_T_max  0.579
_exptl_absorpt_correction_T_min  0.330
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.745
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1209
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 -8 8 0.0170
-6 2 1 0.0409
6 -1 -1 0.0296
-1 0 11 0.0140
1 8 -8 0.0269
1 0 -12 0.0259

_exptl_crystal_size_max          0.078
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.04
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.9982 -7.9987 7.9972 -0.6015 0.2383 0.7348
-5.9998 1.9995 1.0055 -0.3936 -0.8962 0.0533
5.9998 -0.9998 -1.0051 0.3901 0.8895 -0.1705
-0.9969 -0.0013 10.9997 -0.8455 0.3123 -0.2981
0.9982 7.9987 -7.9972 0.6015 -0.2383 -0.7348
0.9966 0.0014 -11.9996 0.9176 -0.3547 0.3301

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_unetI/netI     0.0545
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            13961
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.997
_diffrn_reflns_theta_min         2.568
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -67.00  27.00   1.00    2.50    --  -41.65  57.00  30.00   94
  2  ω    -65.00  33.00   1.00    2.50    --  -41.65  37.00-180.00   98
  3  ω    -96.00 -52.00   1.00    2.50    --  -41.65 125.00  90.00   44
  4  ω   -114.00 -20.00   1.00    2.50    --  -41.65 -57.00-120.00   94
  5  ω     40.00 136.00   1.00   10.00    --  112.00 -61.00-150.00   96
  6  ω     75.00 116.00   1.00   10.00    --  112.00-111.00 -30.00   41
  7  ω     61.00 113.00   1.00   10.00    --  112.00 -77.00   0.00   52
  8  ω     44.00 138.00   1.00   10.00    --  112.00 -45.00 -60.00   94
  9  ω    113.00 158.00   1.00   10.00    --  112.00  30.00-150.00   45
 10  ω     41.00 137.00   1.00   10.00    --  112.00 -61.00  60.00   96
 11  ω     81.00 113.00   1.00   10.00    --  112.00-111.00 150.00   32
 12  ω     37.00  62.00   1.00   10.00    --  112.00-111.00 150.00   25
 13  ω     36.00  61.00   1.00   10.00    --  112.00-111.00 -30.00   25
 14  ω     37.00 108.00   1.00   10.00    --  112.00-111.00-120.00   71
 15  ω     25.00 174.00   1.00   10.00    --  112.00   0.00-180.00  149
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0523614000
_diffrn_orient_matrix_UB_12      -0.0034423000
_diffrn_orient_matrix_UB_13      -0.0721196000
_diffrn_orient_matrix_UB_21      0.1542453000
_diffrn_orient_matrix_UB_22      -0.0066726000
_diffrn_orient_matrix_UB_23      0.0423721000
_diffrn_orient_matrix_UB_31      -0.0532852000
_diffrn_orient_matrix_UB_32      -0.1171619000
_diffrn_orient_matrix_UB_33      -0.0319473000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7711
_reflns_number_total             8320
_reflns_odcompleteness_completeness 99.45
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         1.969
_refine_diff_density_min         -2.865
_refine_diff_density_rms         0.164
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     484
_refine_ls_number_reflns         8320
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0606
_refine_ls_restrained_S_all      1.060
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1085P)²+8.2331P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1672
_refine_ls_wR_factor_ref         0.1719
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Others
 Sof(Br3B)=1-FVAR(1)
 Sof(S1A)=Sof(F7A)=Sof(O4A)=Sof(O2A)=Sof(F8A)=Sof(F6A)=Sof(O3A)=Sof(C5A)=FVAR(1)
3.a Rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
3.b Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C20(H20A,H20B), C10(H10A,H10B)
3.c Aromatic/amide H refined with riding coordinates:
 C33(H33), C13(H13), C35(H35), C32(H32), C15(H15), C12(H12), C36(H36),
 C16(H16), C25(H25), C22(H22), C26(H26), C23(H23)
3.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C8(H8A,H8B,H8C), C7(H7A,H7B,H7C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sm1 Sm 0.27105(3) 0.48627(2) 0.00537(2) 0.01946(13) Uani 1 1 d . . . . .
Br2 Br 0.23436(13) 0.41504(10) 0.31328(6) 0.0630(3) Uani 1 1 d . . . . .
Br1 Br 0.28580(14) -0.07649(14) 0.29472(9) 0.0830(4) Uani 1 1 d . . . . .
S1A S 0.7990(7) 0.7607(5) 0.3997(3) 0.0284(10) Uani 0.831(7) 1 d . . P A 1
O19 O 0.5902(5) 0.4712(4) 0.0753(3) 0.0263(10) Uani 1 1 d . . . . .
O18 O 0.3898(5) 0.4395(4) 0.1140(3) 0.0286(10) Uani 1 1 d . . . . .
F7A F 0.6667(8) 0.5953(6) 0.4170(6) 0.074(3) Uani 0.831(7) 1 d . . P A 1
O4A O 0.9447(7) 0.8242(5) 0.4319(4) 0.0353(15) Uani 0.831(7) 1 d . . P A 1
C17 C 0.5246(8) 0.4460(5) 0.1201(4) 0.0261(13) Uani 1 1 d . . . . .
C30 C 0.8869(8) 0.0297(5) 0.3847(4) 0.0298(14) Uani 1 1 d . . . . .
H30A H 0.989142 0.053906 0.382790 0.036 Uiso 1 1 calc R . . . .
H30B H 0.894587 0.002152 0.427349 0.036 Uiso 1 1 calc R . . . .
N31 N 0.8017(6) -0.0551(4) 0.3092(3) 0.0238(11) Uani 1 1 d . . . . .
O2A O 0.6855(8) 0.8066(6) 0.4216(6) 0.052(2) Uani 0.831(7) 1 d . . P A 1
C5 C 0.8186(8) 0.1194(5) 0.4033(3) 0.0256(13) Uani 1 1 d . . . . .
C14 C 0.6179(8) 0.4231(5) 0.1859(4) 0.0273(14) Uani 1 1 d . . . . .
C33 C 0.5769(8) -0.1670(5) 0.2214(4) 0.0259(13) Uani 1 1 d . . . . .
H33 H 0.471241 -0.186853 0.206135 0.031 Uiso 1 1 calc R . . . .
C3 C 0.6989(8) 0.2259(6) 0.4839(4) 0.0279(14) Uani 1 1 d . . . . .
C13 C 0.7684(9) 0.4393(6) 0.2009(4) 0.0365(17) Uani 1 1 d . . . . .
H13 H 0.816525 0.463016 0.168306 0.044 Uiso 1 1 calc R . . . .
F8A F 0.9058(9) 0.6147(5) 0.4280(5) 0.067(2) Uani 0.831(7) 1 d . . P A 1
C2 C 0.7417(9) 0.3049(6) 0.4581(4) 0.0326(15) Uani 1 1 d . . . . .
N11 N 0.7844(7) 0.3847(5) 0.3080(3) 0.0291(12) Uani 1 1 d . . . . .
C35 C 0.8105(8) -0.1879(6) 0.2011(4) 0.0339(16) Uani 1 1 d . . . . .
H35 H 0.866659 -0.222205 0.170898 0.041 Uiso 1 1 calc R . . . .
C4 C 0.7398(8) 0.1328(5) 0.4581(4) 0.0289(14) Uani 1 1 d . . . . .
C32 C 0.6538(8) -0.0843(5) 0.2871(4) 0.0273(14) Uani 1 1 d . . . . .
H32 H 0.600339 -0.047077 0.317356 0.033 Uiso 1 1 calc R . . . .
C1 C 0.8175(8) 0.2886(6) 0.4016(4) 0.0284(14) Uani 1 1 d . . . . .
C20 C 0.6079(9) 0.2411(7) 0.5411(4) 0.0379(18) Uani 1 1 d . . . . .
H20A H 0.544775 0.174115 0.533549 0.045 Uiso 1 1 calc R . . . .
H20B H 0.541188 0.284463 0.529564 0.045 Uiso 1 1 calc R . . . .
C15 C 0.5499(9) 0.3825(7) 0.2318(5) 0.0388(18) Uani 1 1 d . . . . .
H15 H 0.444747 0.367582 0.221073 0.047 Uiso 1 1 calc R . . . .
C9 C 0.9298(9) 0.1762(6) 0.3091(4) 0.0344(16) Uani 1 1 d . . . . .
H9A H 1.037744 0.201160 0.332689 0.052 Uiso 1 1 calc GR . . . .
H9B H 0.896649 0.212127 0.274110 0.052 Uiso 1 1 calc GR . . . .
H9C H 0.904939 0.102899 0.279513 0.052 Uiso 1 1 calc GR . . . .
C6 C 0.8525(8) 0.1952(5) 0.3725(4) 0.0270(14) Uani 1 1 d . . . . .
C12 C 0.8503(8) 0.4216(6) 0.2627(4) 0.0359(17) Uani 1 1 d . . . . .
H12 H 0.955460 0.435651 0.273828 0.043 Uiso 1 1 calc R . . . .
F6A F 0.8299(10) 0.6977(8) 0.5192(5) 0.080(3) Uani 0.831(7) 1 d . . P A 1
O3A O 0.7549(10) 0.6988(8) 0.3177(5) 0.064(2) Uani 0.831(7) 1 d . . P A 1
C36 C 0.8813(8) -0.1064(6) 0.2674(4) 0.0318(15) Uani 1 1 d . . . . .
H36 H 0.986900 -0.085501 0.284359 0.038 Uiso 1 1 calc R . . . .
C16 C 0.6353(9) 0.3639(8) 0.2925(5) 0.044(2) Uani 1 1 d . . . . .
H16 H 0.588869 0.336180 0.323959 0.053 Uiso 1 1 calc R . . . .
C10 C 0.8815(9) 0.3754(6) 0.3785(4) 0.0349(16) Uani 1 1 d . . . . .
H10A H 0.902495 0.439908 0.422677 0.042 Uiso 1 1 calc R . . . .
H10B H 0.977470 0.366734 0.368978 0.042 Uiso 1 1 calc R . . . .
C5A C 0.7980(11) 0.6621(9) 0.4420(8) 0.054(3) Uani 0.831(7) 1 d . . P A 1
C8 C 0.7005(11) 0.0498(7) 0.4908(5) 0.047(2) Uani 1 1 d . . . . .
H8A H 0.681038 -0.017170 0.450446 0.071 Uiso 1 1 calc GR . . . .
H8B H 0.611467 0.055946 0.507885 0.071 Uiso 1 1 calc GR . . . .
H8C H 0.783572 0.057083 0.535071 0.071 Uiso 1 1 calc GR . . . .
C7 C 0.7014(13) 0.4045(7) 0.4901(6) 0.054(2) Uani 1 1 d . . . . .
H7A H 0.592894 0.393197 0.474866 0.081 Uiso 1 1 calc GR . . . .
H7B H 0.744863 0.453762 0.469241 0.081 Uiso 1 1 calc GR . . . .
H7C H 0.740182 0.431166 0.546908 0.081 Uiso 1 1 calc GR . . . .
C34 C 0.6559(7) -0.2212(5) 0.1775(4) 0.0217(12) Uani 1 1 d . . . . .
N21 N 0.7017(6) 0.2899(4) 0.6253(3) 0.0252(11) Uani 1 1 d . . . . .
C25 C 0.9263(7) 0.3338(5) 0.7249(4) 0.0258(13) Uani 1 1 d . . . . .
H25 H 1.029040 0.335650 0.740531 0.031 Uiso 1 1 calc R . . . .
C37 C 0.5788(8) -0.3147(5) 0.1050(4) 0.0248(13) Uani 1 1 d . . . . .
C24 C 0.8555(7) 0.3725(5) 0.7800(3) 0.0210(12) Uani 1 1 d . . . . .
C22 C 0.6312(8) 0.3278(7) 0.6779(4) 0.0364(17) Uani 1 1 d . . . . .
H22 H 0.528569 0.325504 0.660872 0.044 Uiso 1 1 calc R . . . .
C26 C 0.8463(8) 0.2927(6) 0.6476(4) 0.0296(14) Uani 1 1 d . . . . .
H26 H 0.894238 0.266161 0.609645 0.035 Uiso 1 1 calc R . . . .
C23 C 0.7059(8) 0.3694(6) 0.7554(4) 0.0314(15) Uani 1 1 d . . . . .
H23 H 0.655557 0.396037 0.792154 0.038 Uiso 1 1 calc R . . . .
O29 O 1.0731(5) 0.4145(4) 0.8842(3) 0.0309(11) Uani 1 1 d . . . . .
C27 C 0.9410(7) 0.4187(5) 0.8662(3) 0.0209(12) Uani 1 1 d . . . . .
O28 O 0.8726(5) 0.4578(4) 0.9119(2) 0.0264(10) Uani 1 1 d . . . . .
O1W O 0.1898(7) 0.6301(5) -0.0224(3) 0.0434(14) Uani 1 1 d . . . . .
H1WA H 0.165148 0.619893 -0.074090 0.065 Uiso 1 1 d GR . . . .
H1WB H 0.261562 0.689674 0.001759 0.065 Uiso 1 1 d GR . . . .
O2W O 0.1021(6) 0.3332(4) 0.0078(3) 0.0365(12) Uani 1 1 d . . . . .
H2WA H 0.129727 0.325021 0.053189 0.055 Uiso 1 1 d GR . . . .
H2WB H 0.102163 0.276695 -0.028879 0.055 Uiso 1 1 d GR . . . .
O39 O 0.6579(5) -0.3391(4) 0.0605(3) 0.0284(10) Uani 1 1 d . . . . .
O38 O 0.4497(5) -0.3575(3) 0.0975(3) 0.0247(9) Uani 1 1 d . . . . .
Br3B Br 0.810(2) 0.7764(16) 0.4115(12) 0.077(7) Uani 0.169(7) 1 d . . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sm1 O19 2.371(5) 2_665 ?
Sm1 O18 2.441(4) . ?
Sm1 O29 2.419(4) 1_454 ?
Sm1 O28 2.345(4) 2_666 ?
Sm1 O1W 2.459(5) . ?
Sm1 O2W 2.503(5) . ?
Sm1 O39 2.377(4) 2_655 ?
Sm1 O38 2.439(4) 1_565 ?
S1A O4A 1.410(9) . ?
S1A O2A 1.426(9) . ?
S1A O3A 1.452(10) . ?
S1A C5A 1.811(12) . ?
O19 C17 1.256(8) . ?
O18 C17 1.248(9) . ?
F7A C5A 1.327(12) . ?
C17 C14 1.511(9) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 N31 1.504(8) . ?
C30 C5 1.509(10) . ?
N31 C32 1.331(9) . ?
N31 C36 1.353(9) . ?
C5 C4 1.394(10) . ?
C5 C6 1.397(10) . ?
C14 C13 1.363(11) . ?
C14 C15 1.390(10) . ?
C33 H33 0.9500 . ?
C33 C32 1.373(9) . ?
C33 C34 1.389(9) . ?
C3 C2 1.391(11) . ?
C3 C4 1.416(10) . ?
C3 C20 1.516(10) . ?
C13 H13 0.9500 . ?
C13 C12 1.366(10) . ?
F8A C5A 1.349(15) . ?
C2 C1 1.401(11) . ?
C2 C7 1.511(11) . ?
N11 C12 1.342(10) . ?
N11 C16 1.347(10) . ?
N11 C10 1.495(9) . ?
C35 H35 0.9500 . ?
C35 C36 1.360(10) . ?
C35 C34 1.393(9) . ?
C4 C8 1.520(10) . ?
C32 H32 0.9500 . ?
C1 C6 1.400(10) . ?
C1 C10 1.509(10) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 N21 1.517(8) . ?
C15 H15 0.9500 . ?
C15 C16 1.372(11) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C9 C6 1.520(9) . ?
C12 H12 0.9500 . ?
F6A C5A 1.331(16) . ?
C36 H36 0.9500 . ?
C16 H16 0.9500 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C34 C37 1.518(9) . ?
N21 C22 1.349(9) . ?
N21 C26 1.337(9) . ?
C25 H25 0.9500 . ?
C25 C24 1.389(9) . ?
C25 C26 1.376(9) . ?
C37 O39 1.260(8) . ?
C37 O38 1.236(8) . ?
C24 C23 1.386(9) . ?
C24 C27 1.524(8) . ?
C22 H22 0.9500 . ?
C22 C23 1.367(10) . ?
C26 H26 0.9500 . ?
C23 H23 0.9500 . ?
O29 C27 1.245(8) . ?
C27 O28 1.248(8) . ?
O1W H1WA 0.9095 . ?
O1W H1WB 0.9102 . ?
O2W H2WA 0.8860 . ?
O2W H2WB 0.8885 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O19 Sm1 O18 120.02(16) 2_665 . ?
O19 Sm1 O29 82.34(16) 2_665 1_454 ?
O19 Sm1 O1W 74.36(18) 2_665 . ?
O19 Sm1 O2W 138.55(17) 2_665 . ?
O19 Sm1 O39 71.68(17) 2_665 2_655 ?
O19 Sm1 O38 79.44(16) 2_665 1_565 ?
O18 Sm1 O1W 140.97(19) . . ?
O18 Sm1 O2W 70.55(17) . . ?
O29 Sm1 O18 140.28(18) 1_454 . ?
O29 Sm1 O1W 73.3(2) 1_454 . ?
O29 Sm1 O2W 71.62(18) 1_454 . ?
O29 Sm1 O38 144.43(17) 1_454 1_565 ?
O28 Sm1 O19 145.53(17) 2_666 2_665 ?
O28 Sm1 O18 81.22(16) 2_666 . ?
O28 Sm1 O29 98.02(15) 2_666 1_454 ?
O28 Sm1 O1W 72.83(18) 2_666 . ?
O28 Sm1 O2W 71.60(18) 2_666 . ?
O28 Sm1 O39 142.44(17) 2_666 2_655 ?
O28 Sm1 O38 80.92(15) 2_666 1_565 ?
O1W Sm1 O2W 124.9(2) . . ?
O39 Sm1 O18 78.82(16) 2_655 . ?
O39 Sm1 O29 78.39(17) 2_655 1_454 ?
O39 Sm1 O1W 138.03(18) 2_655 . ?
O39 Sm1 O2W 71.86(18) 2_655 . ?
O39 Sm1 O38 123.21(16) 2_655 1_565 ?
O38 Sm1 O18 75.05(17) 1_565 . ?
O38 Sm1 O1W 72.50(19) 1_565 . ?
O38 Sm1 O2W 138.48(16) 1_565 . ?
O4A S1A O2A 115.4(6) . . ?
O4A S1A O3A 117.1(5) . . ?
O4A S1A C5A 105.4(5) . . ?
O2A S1A O3A 112.4(7) . . ?
O2A S1A C5A 103.7(6) . . ?
O3A S1A C5A 100.2(7) . . ?
C17 O19 Sm1 175.7(4) . 2_665 ?
C17 O18 Sm1 111.1(4) . . ?
O19 C17 C14 116.6(6) . . ?
O18 C17 O19 124.6(6) . . ?
O18 C17 C14 118.7(6) . . ?
H30A C30 H30B 107.6 . . ?
N31 C30 H30A 108.7 . . ?
N31 C30 H30B 108.7 . . ?
N31 C30 C5 114.3(6) . . ?
C5 C30 H30A 108.7 . . ?
C5 C30 H30B 108.7 . . ?
C32 N31 C30 121.6(6) . . ?
C32 N31 C36 120.8(6) . . ?
C36 N31 C30 117.4(6) . . ?
C4 C5 C30 120.4(6) . . ?
C4 C5 C6 120.5(6) . . ?
C6 C5 C30 118.6(6) . . ?
C13 C14 C17 121.7(6) . . ?
C13 C14 C15 118.5(7) . . ?
C15 C14 C17 119.9(6) . . ?
C32 C33 H33 120.5 . . ?
C32 C33 C34 118.9(6) . . ?
C34 C33 H33 120.5 . . ?
C2 C3 C4 121.1(6) . . ?
C2 C3 C20 118.8(7) . . ?
C4 C3 C20 120.1(7) . . ?
C14 C13 H13 119.9 . . ?
C14 C13 C12 120.2(7) . . ?
C12 C13 H13 119.9 . . ?
C3 C2 C1 118.8(7) . . ?
C3 C2 C7 119.1(7) . . ?
C1 C2 C7 122.1(7) . . ?
C12 N11 C16 120.0(6) . . ?
C12 N11 C10 118.2(6) . . ?
C16 N11 C10 121.7(6) . . ?
C36 C35 H35 119.9 . . ?
C36 C35 C34 120.1(6) . . ?
C34 C35 H35 119.9 . . ?
C5 C4 C3 118.9(6) . . ?
C5 C4 C8 120.7(7) . . ?
C3 C4 C8 120.3(7) . . ?
N31 C32 C33 121.4(6) . . ?
N31 C32 H32 119.3 . . ?
C33 C32 H32 119.3 . . ?
C2 C1 C10 120.6(7) . . ?
C6 C1 C2 120.9(7) . . ?
C6 C1 C10 118.0(7) . . ?
C3 C20 H20A 108.9 . . ?
C3 C20 H20B 108.9 . . ?
C3 C20 N21 113.6(6) . . ?
H20A C20 H20B 107.7 . . ?
N21 C20 H20A 108.9 . . ?
N21 C20 H20B 108.9 . . ?
C14 C15 H15 120.1 . . ?
C16 C15 C14 119.7(7) . . ?
C16 C15 H15 120.1 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
C5 C6 C1 119.6(6) . . ?
C5 C6 C9 119.6(6) . . ?
C1 C6 C9 120.8(6) . . ?
C13 C12 H12 119.5 . . ?
N11 C12 C13 121.0(7) . . ?
N11 C12 H12 119.5 . . ?
N31 C36 C35 120.2(6) . . ?
N31 C36 H36 119.9 . . ?
C35 C36 H36 119.9 . . ?
N11 C16 C15 120.5(7) . . ?
N11 C16 H16 119.8 . . ?
C15 C16 H16 119.8 . . ?
N11 C10 C1 115.1(6) . . ?
N11 C10 H10A 108.5 . . ?
N11 C10 H10B 108.5 . . ?
C1 C10 H10A 108.5 . . ?
C1 C10 H10B 108.5 . . ?
H10A C10 H10B 107.5 . . ?
F7A C5A S1A 112.7(7) . . ?
F7A C5A F8A 110.8(10) . . ?
F7A C5A F6A 105.3(11) . . ?
F8A C5A S1A 109.8(9) . . ?
F6A C5A S1A 113.6(9) . . ?
F6A C5A F8A 104.3(9) . . ?
C4 C8 H8A 109.5 . . ?
C4 C8 H8B 109.5 . . ?
C4 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C33 C34 C35 118.5(6) . . ?
C33 C34 C37 122.0(6) . . ?
C35 C34 C37 119.5(6) . . ?
C22 N21 C20 116.7(6) . . ?
C26 N21 C20 122.3(6) . . ?
C26 N21 C22 121.0(6) . . ?
C24 C25 H25 120.3 . . ?
C26 C25 H25 120.3 . . ?
C26 C25 C24 119.4(6) . . ?
O39 C37 C34 114.4(6) . . ?
O38 C37 C34 117.1(6) . . ?
O38 C37 O39 128.5(6) . . ?
C25 C24 C27 120.7(6) . . ?
C23 C24 C25 118.9(6) . . ?
C23 C24 C27 120.4(6) . . ?
N21 C22 H22 119.7 . . ?
N21 C22 C23 120.7(7) . . ?
C23 C22 H22 119.7 . . ?
N21 C26 C25 120.6(6) . . ?
N21 C26 H26 119.7 . . ?
C25 C26 H26 119.7 . . ?
C24 C23 H23 120.3 . . ?
C22 C23 C24 119.5(6) . . ?
C22 C23 H23 120.3 . . ?
C27 O29 Sm1 132.8(4) . 1_656 ?
O29 C27 C24 116.6(5) . . ?
O29 C27 O28 126.2(6) . . ?
O28 C27 C24 117.2(6) . . ?
C27 O28 Sm1 174.0(5) . 2_666 ?
Sm1 O1W H1WA 112.1 . . ?
Sm1 O1W H1WB 112.4 . . ?
H1WA O1W H1WB 106.6 . . ?
Sm1 O2W H2WA 111.3 . . ?
Sm1 O2W H2WB 111.4 . . ?
H2WA O2W H2WB 107.7 . . ?
C37 O39 Sm1 138.8(5) . 2_655 ?
C37 O38 Sm1 134.8(4) . 1_545 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Sm1 O18 C17 O19 -1.4(8) . . . . ?
Sm1 O18 C17 C14 178.1(5) . . . . ?
Sm1 O29 C27 C24 173.0(4) 1_656 . . . ?
Sm1 O29 C27 O28 -6.4(11) 1_656 . . . ?
O19 C17 C14 C13 6.7(10) . . . . ?
O19 C17 C14 C15 -171.9(7) . . . . ?
O18 C17 C14 C13 -172.8(7) . . . . ?
O18 C17 C14 C15 8.5(10) . . . . ?
O4A S1A C5A F7A -179.9(10) . . . . ?
O4A S1A C5A F8A -55.9(10) . . . . ?
O4A S1A C5A F6A 60.5(10) . . . . ?
C17 C14 C13 C12 177.4(7) . . . . ?
C17 C14 C15 C16 -178.5(8) . . . . ?
C30 N31 C32 C33 -174.6(7) . . . . ?
C30 N31 C36 C35 175.9(7) . . . . ?
C30 C5 C4 C3 169.4(6) . . . . ?
C30 C5 C4 C8 -9.5(10) . . . . ?
C30 C5 C6 C1 -166.4(6) . . . . ?
C30 C5 C6 C9 12.3(9) . . . . ?
N31 C30 C5 C4 103.0(7) . . . . ?
N31 C30 C5 C6 -85.4(8) . . . . ?
O2A S1A C5A F7A 58.4(13) . . . . ?
O2A S1A C5A F8A -177.6(8) . . . . ?
O2A S1A C5A F6A -61.3(10) . . . . ?
C5 C30 N31 C32 -40.8(9) . . . . ?
C5 C30 N31 C36 144.4(7) . . . . ?
C14 C13 C12 N11 2.4(13) . . . . ?
C14 C15 C16 N11 -0.1(15) . . . . ?
C33 C34 C37 O39 161.8(6) . . . . ?
C33 C34 C37 O38 -19.2(9) . . . . ?
C3 C2 C1 C6 -1.3(10) . . . . ?
C3 C2 C1 C10 -173.0(6) . . . . ?
C3 C20 N21 C22 164.7(7) . . . . ?
C3 C20 N21 C26 -17.5(11) . . . . ?
C13 C14 C15 C16 2.8(13) . . . . ?
C2 C3 C4 C5 -2.8(10) . . . . ?
C2 C3 C4 C8 176.1(7) . . . . ?
C2 C3 C20 N21 -87.3(8) . . . . ?
C2 C1 C6 C5 -3.5(10) . . . . ?
C2 C1 C6 C9 177.8(6) . . . . ?
C2 C1 C10 N11 -95.6(8) . . . . ?
C35 C34 C37 O39 -18.0(9) . . . . ?
C35 C34 C37 O38 161.0(7) . . . . ?
C4 C5 C6 C1 5.2(10) . . . . ?
C4 C5 C6 C9 -176.1(6) . . . . ?
C4 C3 C2 C1 4.4(10) . . . . ?
C4 C3 C2 C7 -177.2(7) . . . . ?
C4 C3 C20 N21 92.2(8) . . . . ?
C32 N31 C36 C35 1.1(11) . . . . ?
C32 C33 C34 C35 -1.4(10) . . . . ?
C32 C33 C34 C37 178.8(6) . . . . ?
C20 C3 C2 C1 -176.0(6) . . . . ?
C20 C3 C2 C7 2.3(10) . . . . ?
C20 C3 C4 C5 177.6(6) . . . . ?
C20 C3 C4 C8 -3.4(10) . . . . ?
C20 N21 C22 C23 177.4(8) . . . . ?
C20 N21 C26 C25 -177.2(7) . . . . ?
C15 C14 C13 C12 -3.9(12) . . . . ?
C6 C5 C4 C3 -2.0(10) . . . . ?
C6 C5 C4 C8 179.0(7) . . . . ?
C6 C1 C10 N11 92.5(8) . . . . ?
C12 N11 C16 C15 -1.5(14) . . . . ?
C12 N11 C10 C1 -148.6(7) . . . . ?
O3A S1A C5A F7A -57.9(12) . . . . ?
O3A S1A C5A F8A 66.1(9) . . . . ?
O3A S1A C5A F6A -177.6(9) . . . . ?
C36 N31 C32 C33 0.0(11) . . . . ?
C36 C35 C34 C33 2.5(11) . . . . ?
C36 C35 C34 C37 -177.7(7) . . . . ?
C16 N11 C12 C13 0.4(13) . . . . ?
C16 N11 C10 C1 36.1(11) . . . . ?
C10 N11 C12 C13 -175.0(8) . . . . ?
C10 N11 C16 C15 173.6(8) . . . . ?
C10 C1 C6 C5 168.4(6) . . . . ?
C10 C1 C6 C9 -10.3(9) . . . . ?
C7 C2 C1 C6 -179.5(7) . . . . ?
C7 C2 C1 C10 8.7(11) . . . . ?
C34 C33 C32 N31 0.2(11) . . . . ?
C34 C35 C36 N31 -2.3(12) . . . . ?
C34 C37 O39 Sm1 130.1(6) . . . 2_655 ?
C34 C37 O38 Sm1 -173.8(4) . . . 1_545 ?
N21 C22 C23 C24 0.0(13) . . . . ?
C25 C24 C23 C22 0.5(11) . . . . ?
C25 C24 C27 O29 -3.8(9) . . . . ?
C25 C24 C27 O28 175.6(6) . . . . ?
C24 C25 C26 N21 0.0(11) . . . . ?
C22 N21 C26 C25 0.5(11) . . . . ?
C26 N21 C22 C23 -0.5(12) . . . . ?
C26 C25 C24 C23 -0.5(11) . . . . ?
C26 C25 C24 C27 -179.9(6) . . . . ?
C23 C24 C27 O29 176.7(7) . . . . ?
C23 C24 C27 O28 -3.8(9) . . . . ?
C27 C24 C23 C22 179.9(7) . . . . ?
O39 C37 O38 Sm1 5.0(11) . . . 1_545 ?
O38 C37 O39 Sm1 -48.8(10) . . . 2_655 ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.097 0.000 0.000 661.2 219.3 '22x water'

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.240
_oxdiff_exptl_absorpt_empirical_full_min 0.792
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_jj003_br_yb_otf_h2o_acet_red3
_database_code_depnum_ccdc_archive 'CCDC 1833439'
loop_
_audit_author_name
_audit_author_address
'Antti Tiihonen'
;University of Jyv?skyl?, Department of Chemistry
Finland
;
_audit_update_record             
;
2018-03-29 deposited with the CCDC.	2019-02-28 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_CHEMW03_I                   
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: The structure contains voids of unresolved electron density
which was treated using Olex2 solvent mask procedure (full details in 
_smtbx_masks_special_details). The 6.5 water molecules per asymmetric unit 
 are included in the formula and used in the calculations. 
;
_vrf_PLAT420_I                   
;
PROBLEM: D-H Without Acceptor       O       --H 
RESPONSE: Hydrogen bond acceptors (water located in a void) have been removed 
among the other disordered solvents (also water) in the voids 
(see vrf_CHEMW03_ALERT_2_A).
;
_vrf_FORMU01_I                   
;
PROBLEM: There is a discrepancy between the atom counts in the
            _chemical_formula_sum and _chemical_formula_moiety.
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_CELLZ01_I                   
;
PROBLEM: Difference between formula and atom_site contents detected.
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT041_I                   
;
PROBLEM: Calculated and Reported SumFormula strings Differ ...    
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT068_I                   
;
PROBLEM: Reported F000 Differs from Calcd (or Missing)...
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT606_I                   
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
# end Validation Reply Form

_audit_creation_date             2018-03-26
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H31 N3 O8 Yb, 3(Br), O'
_chemical_formula_sum            'C30 H45 Br3 N3 O15 Yb'
_chemical_formula_weight         1100.46
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C21 H25 O12 N3 F12 S3 Br1 Yb1'
_chemical_oxdiff_usercomment     'clear colorless block'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Yb Yb -7.2108 4.4329 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.2767(3)
_cell_length_b                   13.0591(5)
_cell_length_c                   18.3855(8)
_cell_angle_alpha                107.284(4)
_cell_angle_beta                 98.961(3)
_cell_angle_gamma                94.147(3)
_cell_volume                     2084.10(14)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7206
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      76.8190
_cell_measurement_theta_min      3.6620
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    8.081
_exptl_absorpt_correction_T_max  0.918
_exptl_absorpt_correction_T_min  0.800
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.754
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1082
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 -5 -6 0.0247
5 -4 -3 0.0328
0 -7 9 0.0084
-6 3 2 0.0399
-4 5 5 0.0351
5 0 3 0.0285
0 7 -9 0.0151

_exptl_crystal_size_max          0.089
_exptl_crystal_size_mid          0.077
_exptl_crystal_size_min          0.023
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.9997 -5.0001 -5.9997 0.4796 0.8069 -0.3026
5.0000 -3.9997 -3.0002 0.0342 0.0075 -0.9641
-0.0000 -6.9999 9.0004 -0.8079 0.5105 -0.2326
-6.0000 2.9997 2.0003 0.0731 0.2296 1.0129
-4.0001 4.9998 5.0001 -0.2237 -0.2720 0.9370
4.9998 0.0003 2.9997 -0.4204 -0.5898 -0.5913
0.0000 6.9999 -9.0004 0.8079 -0.5105 0.2326

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_unetI/netI     0.0418
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12920
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.994
_diffrn_reflns_theta_min         3.573
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3953
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -70.00  31.00   1.00    2.50    --  -41.65  57.00  30.00  101
  2  ω    -69.00  31.00   1.00    2.50    --  -41.65  57.00 150.00  100
  3  ω    -74.00  34.00   1.00    2.50    --  -41.65  77.00-120.00  108
  4  ω     36.00 117.00   1.00    5.00    --  112.00 -77.00-150.00   81
  5  ω     74.00 115.00   1.00    5.00    --  112.00-111.00-180.00   41
  6  ω     52.00 140.00   1.00    5.00    --  112.00 -30.00-180.00   88
  7  ω     89.00 117.00   1.00    5.00    --  112.00  61.00   0.00   28
  8  ω    135.00 167.00   1.00    5.00    --  112.00  61.00   0.00   32
  9  ω    107.00 149.00   1.00    5.00    --  112.00  45.00  60.00   42
 10  ω     57.00 103.00   1.00    5.00    --  112.00 -94.00  60.00   46
 11  ω     40.00 140.00   1.00    5.00    --  112.00 -61.00  60.00  100
 12  ω     39.00 134.00   1.00    5.00    --  112.00 -45.00 -60.00   95
 13  ω     37.00 116.00   1.00    5.00    --  112.00-111.00   0.00   79
 14  ω     39.00 165.00   1.00    5.00    --  112.00 -15.00  30.00  126
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0347557000
_diffrn_orient_matrix_UB_12      0.0096919000
_diffrn_orient_matrix_UB_13      -0.0822290000
_diffrn_orient_matrix_UB_21      -0.1015036000
_diffrn_orient_matrix_UB_22      -0.1081867000
_diffrn_orient_matrix_UB_23      -0.0274230000
_diffrn_orient_matrix_UB_31      -0.1311778000
_diffrn_orient_matrix_UB_32      0.0609173000
_diffrn_orient_matrix_UB_33      0.0215314000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6738
_reflns_number_total             7538
_reflns_odcompleteness_completeness 99.35
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         1.441
_refine_diff_density_min         -1.151
_refine_diff_density_rms         0.114
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         7538
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0327
_refine_ls_restrained_S_all      1.034
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0520P)²+0.1267P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0847
_refine_ls_wR_factor_ref         0.0879
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Others
 Sof(Br3B)=Sof(O3WB)=1-FVAR(1)
 Sof(Br3A)=Sof(O3WA)=FVAR(1)
3.a Rotating group:
 O2W(H2WA,H2WB), O1W(H1WA,H1WB)
3.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C20(H20A,H20B), C30(H30A,H30B)
3.c Aromatic/amide H refined with riding coordinates:
 C35(H35), C15(H15), C32(H32), C25(H25), C33(H33), C22(H22), C13(H13),
 C23(H23), C12(H12), C16(H16), C26(H26), C36(H36)
3.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C7(H7A,H7B,H7C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Yb2 Yb 0.23670(2) -0.48296(2) 0.49894(2) 0.01480(7) Uani 1 1 d . . . . .
Br2 Br 0.06668(4) -0.28326(4) 0.88927(3) 0.02974(11) Uani 1 1 d . . . . .
Br1 Br 0.54048(5) -0.04878(4) 0.80906(3) 0.03335(11) Uani 1 1 d . . . . .
Br3A Br 0.56907(7) 0.36142(6) 0.80209(5) 0.0443(2) Uani 0.7243(18) 1 d . . P A
1
O19 O 0.1923(3) -0.3296(2) 0.59140(14) 0.0194(5) Uani 1 1 d . . . . .
N31 N 0.0673(3) 0.3997(2) 0.83954(17) 0.0167(6) Uani 1 1 d . . . . .
N11 N 0.0067(3) -0.0757(3) 0.80399(17) 0.0181(6) Uani 1 1 d . . . . .
C34 C 0.0550(4) 0.4168(3) 0.69403(19) 0.0169(7) Uani 1 1 d . . . . .
C27 C 0.4360(4) 0.4384(3) 1.36632(19) 0.0163(7) Uani 1 1 d . . . . .
N21 N 0.4506(3) 0.2811(2) 1.12882(16) 0.0150(6) Uani 1 1 d . . . . .
C1 C 0.0886(4) 0.0979(3) 0.91396(19) 0.0168(7) Uani 1 1 d . . . . .
C17 C 0.0631(4) -0.3229(3) 0.60404(19) 0.0181(7) Uani 1 1 d . . . . .
C35 C -0.0653(4) 0.4343(3) 0.7302(2) 0.0206(7) Uani 1 1 d . . . . .
H35 H -0.153413 0.450791 0.704633 0.025 Uiso 1 1 calc R . . . .
C4 C 0.2702(4) 0.2969(3) 0.9747(2) 0.0190(7) Uani 1 1 d . . . . .
C3 C 0.3144(4) 0.2057(3) 0.99224(19) 0.0172(7) Uani 1 1 d . . . . .
C15 C 0.1640(4) -0.1649(3) 0.7235(2) 0.0203(7) Uani 1 1 d . . . . .
H15 H 0.260473 -0.173211 0.713240 0.024 Uiso 1 1 calc R . . . .
C24 C 0.4431(4) 0.3872(3) 1.28159(19) 0.0159(7) Uani 1 1 d . . . . .
C32 C 0.1858(4) 0.3835(3) 0.8057(2) 0.0212(7) Uani 1 1 d . . . . .
H32 H 0.271549 0.365002 0.832057 0.025 Uiso 1 1 calc R . . . .
C6 C 0.0415(4) 0.1892(3) 0.89592(19) 0.0175(7) Uani 1 1 d . . . . .
C10 C -0.0134(4) -0.0077(3) 0.8824(2) 0.0185(7) Uani 1 1 d . . . . .
H10A H 0.003846 -0.049573 0.919147 0.022 Uiso 1 1 calc R . . . .
H10B H -0.116451 0.008350 0.879091 0.022 Uiso 1 1 calc R . . . .
C25 C 0.3138(4) 0.3512(3) 1.2273(2) 0.0180(7) Uani 1 1 d . . . . .
H25 H 0.221649 0.363835 1.242374 0.022 Uiso 1 1 calc R . . . .
C33 C 0.1833(4) 0.3935(3) 0.7330(2) 0.0203(7) Uani 1 1 d . . . . .
H33 H 0.268055 0.384561 0.709753 0.024 Uiso 1 1 calc R . . . .
C22 C 0.5773(4) 0.3175(3) 1.1800(2) 0.0181(7) Uani 1 1 d . . . . .
H22 H 0.668233 0.307328 1.162910 0.022 Uiso 1 1 calc R . . . .
C37 C 0.0431(4) 0.4282(3) 0.6136(2) 0.0170(7) Uani 1 1 d . . . . .
C8 C 0.3696(4) 0.4028(3) 1.0061(2) 0.0249(8) Uani 1 1 d . . . . .
H8A H 0.346623 0.444675 1.055853 0.037 Uiso 1 1 calc GR . . . .
H8B H 0.354477 0.443716 0.969318 0.037 Uiso 1 1 calc GR . . . .
H8C H 0.472338 0.388765 1.013743 0.037 Uiso 1 1 calc GR . . . .
C14 C 0.0428(4) -0.2302(3) 0.6720(2) 0.0178(7) Uani 1 1 d . . . . .
C5 C 0.1309(4) 0.2883(3) 0.92803(19) 0.0169(7) Uani 1 1 d . . . . .
C13 C -0.0978(4) -0.2118(3) 0.6863(2) 0.0221(8) Uani 1 1 d . . . . .
H13 H -0.182143 -0.252212 0.650097 0.027 Uiso 1 1 calc R . . . .
C23 C 0.5769(4) 0.3698(3) 1.2575(2) 0.0186(7) Uani 1 1 d . . . . .
H23 H 0.666812 0.393519 1.293737 0.022 Uiso 1 1 calc R . . . .
C12 C -0.1131(4) -0.1344(3) 0.7534(2) 0.0220(8) Uani 1 1 d . . . . .
H12 H -0.208525 -0.122324 0.764070 0.026 Uiso 1 1 calc R . . . .
C2 C 0.2241(4) 0.1051(3) 0.96232(19) 0.0174(7) Uani 1 1 d . . . . .
C16 C 0.1428(4) -0.0884(3) 0.7890(2) 0.0212(7) Uani 1 1 d . . . . .
H16 H 0.225306 -0.043818 0.824372 0.025 Uiso 1 1 calc R . . . .
C26 C 0.3200(4) 0.2968(3) 1.1511(2) 0.0174(7) Uani 1 1 d . . . . .
H26 H 0.231426 0.270240 1.114112 0.021 Uiso 1 1 calc R . . . .
C36 C -0.0544(4) 0.4272(3) 0.8050(2) 0.0203(7) Uani 1 1 d . . . . .
H36 H -0.134317 0.442065 0.831581 0.024 Uiso 1 1 calc R . . . .
C9 C -0.1041(4) 0.1778(3) 0.8427(2) 0.0252(8) Uani 1 1 d . . . . .
H9A H -0.098274 0.132922 0.790240 0.038 Uiso 1 1 calc GR . . . .
H9B H -0.127092 0.249458 0.841515 0.038 Uiso 1 1 calc GR . . . .
H9C H -0.181553 0.143673 0.861624 0.038 Uiso 1 1 calc GR . . . .
C20 C 0.4572(4) 0.2170(3) 1.0469(2) 0.0199(7) Uani 1 1 d . . . . .
H20A H 0.536221 0.253137 1.029270 0.024 Uiso 1 1 calc R . . . .
H20B H 0.482452 0.144240 1.045669 0.024 Uiso 1 1 calc R . . . .
C30 C 0.0722(4) 0.3910(3) 0.9195(2) 0.0202(7) Uani 1 1 d . . . . .
H30A H -0.028130 0.392156 0.931575 0.024 Uiso 1 1 calc R . . . .
H30B H 0.135522 0.454510 0.957644 0.024 Uiso 1 1 calc R . . . .
C7 C 0.2784(4) 0.0083(3) 0.9812(2) 0.0246(8) Uani 1 1 d . . . . .
H7A H 0.303624 0.024817 1.037579 0.037 Uiso 1 1 calc GR . . . .
H7B H 0.365862 -0.009220 0.958467 0.037 Uiso 1 1 calc GR . . . .
H7C H 0.201201 -0.053532 0.959805 0.037 Uiso 1 1 calc GR . . . .
O29 O 0.3151(3) 0.4669(2) 1.38082(13) 0.0192(5) Uani 1 1 d . . . . .
O38 O 0.1618(3) 0.4591(2) 0.59704(14) 0.0198(5) Uani 1 1 d . . . . .
O28 O 0.5503(3) 0.4489(2) 1.41464(14) 0.0209(5) Uani 1 1 d . . . . .
O39 O -0.0831(3) 0.4063(2) 0.57373(14) 0.0196(5) Uani 1 1 d . . . . .
O18 O -0.0474(3) -0.3878(2) 0.56738(14) 0.0201(5) Uani 1 1 d . . . . .
O2W O 0.3210(3) -0.6515(2) 0.48551(16) 0.0226(5) Uani 1 1 d . . . . .
H2WA H 0.273126 -0.689666 0.509822 0.034 Uiso 1 1 d GR . . . .
H2WB H 0.416936 -0.644576 0.505623 0.034 Uiso 1 1 d GR . . . .
O1W O 0.3824(3) -0.3272(2) 0.48974(15) 0.0211(5) Uani 1 1 d . . . . .
H1WA H 0.391597 -0.266968 0.533392 0.032 Uiso 1 1 d GR . . . .
H1WB H 0.343146 -0.304418 0.448192 0.032 Uiso 1 1 d GR . . . .
Br3B Br 0.5629(2) 0.2952(2) 0.68838(14) 0.0547(7) Uani 0.2757(18) 1 d . . P A 2
O3WA O 0.6545(8) 0.2450(6) 0.6308(3) 0.077(2) Uani 0.7243(18) 1 d . . P A 1
O3WB O 0.5168(16) 0.2368(12) 0.8527(9) 0.051(3) Uani 0.2757(18) 1 d . . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Yb2 O19 2.321(3) . ?
Yb2 C17 3.123(4) . ?
Yb2 O29 2.321(2) 1_544 ?
Yb2 O38 2.331(2) 1_545 ?
Yb2 O28 2.258(2) 2_657 ?
Yb2 O39 2.286(2) 2_556 ?
Yb2 O18 2.258(2) 2_546 ?
Yb2 O2W 2.346(3) . ?
Yb2 O1W 2.423(3) . ?
O19 C17 1.260(5) . ?
N31 C32 1.344(5) . ?
N31 C36 1.334(5) . ?
N31 C30 1.503(4) . ?
N11 C10 1.499(4) . ?
N11 C12 1.349(5) . ?
N11 C16 1.345(5) . ?
C34 C35 1.385(5) . ?
C34 C33 1.393(5) . ?
C34 C37 1.518(5) . ?
C27 C24 1.516(4) . ?
C27 O29 1.250(4) . ?
C27 O28 1.244(4) . ?
N21 C22 1.342(5) . ?
N21 C26 1.349(5) . ?
N21 C20 1.503(4) . ?
C1 C6 1.409(5) . ?
C1 C10 1.517(5) . ?
C1 C2 1.401(5) . ?
C17 C14 1.507(5) . ?
C17 O18 1.243(5) . ?
C35 H35 0.9500 . ?
C35 C36 1.394(5) . ?
C4 C3 1.397(5) . ?
C4 C8 1.507(5) . ?
C4 C5 1.412(5) . ?
C3 C2 1.414(5) . ?
C3 C20 1.502(5) . ?
C15 H15 0.9500 . ?
C15 C14 1.392(5) . ?
C15 C16 1.369(5) . ?
C24 C25 1.387(5) . ?
C24 C23 1.393(5) . ?
C32 H32 0.9500 . ?
C32 C33 1.379(5) . ?
C6 C5 1.396(5) . ?
C6 C9 1.510(5) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C25 H25 0.9500 . ?
C25 C26 1.382(5) . ?
C33 H33 0.9500 . ?
C22 H22 0.9500 . ?
C22 C23 1.385(5) . ?
C37 O38 1.257(5) . ?
C37 O39 1.245(4) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C14 C13 1.393(5) . ?
C5 C30 1.524(5) . ?
C13 H13 0.9500 . ?
C13 C12 1.378(5) . ?
C23 H23 0.9500 . ?
C12 H12 0.9500 . ?
C2 C7 1.506(5) . ?
C16 H16 0.9500 . ?
C26 H26 0.9500 . ?
C36 H36 0.9500 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
O2W H2WA 0.8984 . ?
O2W H2WB 0.8962 . ?
O1W H1WA 0.9297 . ?
O1W H1WB 0.9324 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O19 Yb2 C17 20.80(9) . . ?
O19 Yb2 O29 140.15(9) . 1_544 ?
O19 Yb2 O38 73.65(9) . 1_545 ?
O19 Yb2 O2W 142.06(9) . . ?
O19 Yb2 O1W 71.34(9) . . ?
O29 Yb2 C17 145.31(9) 1_544 . ?
O29 Yb2 O38 146.19(10) 1_544 1_545 ?
O29 Yb2 O2W 73.77(10) 1_544 . ?
O29 Yb2 O1W 72.07(9) 1_544 . ?
O38 Yb2 C17 65.54(9) 1_545 . ?
O38 Yb2 O2W 74.21(9) 1_545 . ?
O38 Yb2 O1W 137.03(9) 1_545 . ?
O28 Yb2 O19 79.95(9) 2_657 . ?
O28 Yb2 C17 97.05(9) 2_657 . ?
O28 Yb2 O29 102.68(9) 2_657 1_544 ?
O28 Yb2 O38 78.79(9) 2_657 1_545 ?
O28 Yb2 O39 142.99(10) 2_657 2_556 ?
O28 Yb2 O2W 74.49(10) 2_657 . ?
O28 Yb2 O1W 71.32(9) 2_657 . ?
O39 Yb2 O19 77.62(9) 2_556 . ?
O39 Yb2 C17 69.63(9) 2_556 . ?
O39 Yb2 O29 77.53(9) 2_556 1_544 ?
O39 Yb2 O38 121.53(9) 2_556 1_545 ?
O39 Yb2 O2W 137.65(9) 2_556 . ?
O39 Yb2 O1W 73.77(9) 2_556 . ?
O18 Yb2 O19 119.26(9) 2_546 . ?
O18 Yb2 C17 98.47(9) 2_546 . ?
O18 Yb2 O29 82.33(9) 2_546 1_544 ?
O18 Yb2 O38 77.84(9) 2_546 1_545 ?
O18 Yb2 O28 143.34(10) 2_546 2_657 ?
O18 Yb2 O39 73.67(10) 2_546 2_556 ?
O18 Yb2 O2W 72.20(9) 2_546 . ?
O18 Yb2 O1W 142.05(9) 2_546 . ?
O2W Yb2 C17 139.75(9) . . ?
O2W Yb2 O1W 123.85(9) . . ?
O1W Yb2 C17 87.97(9) . . ?
C17 O19 Yb2 118.4(2) . . ?
C32 N31 C30 119.9(3) . . ?
C36 N31 C32 121.7(3) . . ?
C36 N31 C30 118.3(3) . . ?
C12 N11 C10 118.2(3) . . ?
C16 N11 C10 120.1(3) . . ?
C16 N11 C12 121.1(3) . . ?
C35 C34 C33 119.6(3) . . ?
C35 C34 C37 118.1(3) . . ?
C33 C34 C37 122.3(3) . . ?
O29 C27 C24 116.5(3) . . ?
O28 C27 C24 117.3(3) . . ?
O28 C27 O29 126.2(3) . . ?
C22 N21 C26 120.9(3) . . ?
C22 N21 C20 118.4(3) . . ?
C26 N21 C20 120.6(3) . . ?
C6 C1 C10 118.4(3) . . ?
C2 C1 C6 121.1(3) . . ?
C2 C1 C10 120.4(3) . . ?
O19 C17 Yb2 40.84(17) . . ?
O19 C17 C14 116.7(3) . . ?
C14 C17 Yb2 156.6(2) . . ?
O18 C17 Yb2 85.3(2) . . ?
O18 C17 O19 126.0(3) . . ?
O18 C17 C14 117.3(3) . . ?
C34 C35 H35 120.7 . . ?
C34 C35 C36 118.7(3) . . ?
C36 C35 H35 120.7 . . ?
C3 C4 C8 120.0(3) . . ?
C3 C4 C5 118.9(3) . . ?
C5 C4 C8 121.0(3) . . ?
C4 C3 C2 121.0(3) . . ?
C4 C3 C20 118.8(3) . . ?
C2 C3 C20 120.0(3) . . ?
C14 C15 H15 120.3 . . ?
C16 C15 H15 120.3 . . ?
C16 C15 C14 119.3(3) . . ?
C25 C24 C27 119.6(3) . . ?
C25 C24 C23 119.0(3) . . ?
C23 C24 C27 121.3(3) . . ?
N31 C32 H32 119.9 . . ?
N31 C32 C33 120.3(3) . . ?
C33 C32 H32 119.9 . . ?
C1 C6 C9 119.5(3) . . ?
C5 C6 C1 119.0(3) . . ?
C5 C6 C9 121.5(3) . . ?
N11 C10 C1 113.4(3) . . ?
N11 C10 H10A 108.9 . . ?
N11 C10 H10B 108.9 . . ?
C1 C10 H10A 108.9 . . ?
C1 C10 H10B 108.9 . . ?
H10A C10 H10B 107.7 . . ?
C24 C25 H25 120.2 . . ?
C26 C25 C24 119.5(3) . . ?
C26 C25 H25 120.2 . . ?
C34 C33 H33 120.4 . . ?
C32 C33 C34 119.2(3) . . ?
C32 C33 H33 120.4 . . ?
N21 C22 H22 119.6 . . ?
N21 C22 C23 120.8(3) . . ?
C23 C22 H22 119.6 . . ?
O38 C37 C34 115.4(3) . . ?
O39 C37 C34 115.2(3) . . ?
O39 C37 O38 129.4(3) . . ?
C4 C8 H8A 109.5 . . ?
C4 C8 H8B 109.5 . . ?
C4 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C15 C14 C17 120.6(3) . . ?
C15 C14 C13 119.0(3) . . ?
C13 C14 C17 120.3(3) . . ?
C4 C5 C30 118.9(3) . . ?
C6 C5 C4 121.1(3) . . ?
C6 C5 C30 119.8(3) . . ?
C14 C13 H13 120.4 . . ?
C12 C13 C14 119.3(3) . . ?
C12 C13 H13 120.4 . . ?
C24 C23 H23 120.4 . . ?
C22 C23 C24 119.2(3) . . ?
C22 C23 H23 120.4 . . ?
N11 C12 C13 120.3(3) . . ?
N11 C12 H12 119.9 . . ?
C13 C12 H12 119.9 . . ?
C1 C2 C3 118.8(3) . . ?
C1 C2 C7 122.1(3) . . ?
C3 C2 C7 119.1(3) . . ?
N11 C16 C15 120.8(3) . . ?
N11 C16 H16 119.6 . . ?
C15 C16 H16 119.6 . . ?
N21 C26 C25 120.6(3) . . ?
N21 C26 H26 119.7 . . ?
C25 C26 H26 119.7 . . ?
N31 C36 C35 120.4(3) . . ?
N31 C36 H36 119.8 . . ?
C35 C36 H36 119.8 . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N21 C20 H20A 109.1 . . ?
N21 C20 H20B 109.1 . . ?
C3 C20 N21 112.4(3) . . ?
C3 C20 H20A 109.1 . . ?
C3 C20 H20B 109.1 . . ?
H20A C20 H20B 107.9 . . ?
N31 C30 C5 112.6(3) . . ?
N31 C30 H30A 109.1 . . ?
N31 C30 H30B 109.1 . . ?
C5 C30 H30A 109.1 . . ?
C5 C30 H30B 109.1 . . ?
H30A C30 H30B 107.8 . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C27 O29 Yb2 129.1(2) . 1_566 ?
C37 O38 Yb2 137.6(2) . 1_565 ?
C27 O28 Yb2 174.7(3) . 2_657 ?
C37 O39 Yb2 138.0(2) . 2_556 ?
C17 O18 Yb2 175.2(3) . 2_546 ?
Yb2 O2W H2WA 111.8 . . ?
Yb2 O2W H2WB 111.8 . . ?
H2WA O2W H2WB 106.9 . . ?
Yb2 O1W H1WA 112.9 . . ?
Yb2 O1W H1WB 113.3 . . ?
H1WA O1W H1WB 105.2 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O2W H2WB O1W 0.90 1.92 2.766(4) 157.3 2_646 yes
O1W H1WB O3WA 0.93 1.84 2.723(6) 156.8 2_656 yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Yb2 O19 C17 C14 171.5(2) . . . . ?
Yb2 O19 C17 O18 -5.7(5) . . . . ?
Yb2 C17 C14 C15 5.9(8) . . . . ?
Yb2 C17 C14 C13 -171.2(5) . . . . ?
O19 C17 C14 C15 -8.2(5) . . . . ?
O19 C17 C14 C13 174.8(3) . . . . ?
N31 C32 C33 C34 -2.2(6) . . . . ?
C34 C35 C36 N31 -2.8(6) . . . . ?
C34 C37 O38 Yb2 -170.1(2) . . . 1_565 ?
C34 C37 O39 Yb2 130.2(3) . . . 2_556 ?
C27 C24 C25 C26 -174.9(3) . . . . ?
C27 C24 C23 C22 176.6(3) . . . . ?
N21 C22 C23 C24 -1.9(6) . . . . ?
C1 C6 C5 C4 3.3(5) . . . . ?
C1 C6 C5 C30 -170.6(3) . . . . ?
C17 C14 C13 C12 172.8(3) . . . . ?
C35 C34 C33 C32 2.9(6) . . . . ?
C35 C34 C37 O38 149.8(3) . . . . ?
C35 C34 C37 O39 -29.7(5) . . . . ?
C4 C3 C2 C1 0.4(5) . . . . ?
C4 C3 C2 C7 178.4(3) . . . . ?
C4 C3 C20 N21 69.6(4) . . . . ?
C4 C5 C30 N31 110.5(4) . . . . ?
C3 C4 C5 C6 -3.7(5) . . . . ?
C3 C4 C5 C30 170.3(3) . . . . ?
C15 C14 C13 C12 -4.3(6) . . . . ?
C24 C27 O29 Yb2 167.0(2) . . . 1_566 ?
C24 C25 C26 N21 -1.8(6) . . . . ?
C32 N31 C36 C35 3.5(6) . . . . ?
C32 N31 C30 C5 -48.7(5) . . . . ?
C6 C1 C10 N11 89.1(4) . . . . ?
C6 C1 C2 C3 -0.8(5) . . . . ?
C6 C1 C2 C7 -178.7(3) . . . . ?
C6 C5 C30 N31 -75.4(4) . . . . ?
C10 N11 C12 C13 -168.8(3) . . . . ?
C10 N11 C16 C15 168.1(3) . . . . ?
C10 C1 C6 C5 176.6(3) . . . . ?
C10 C1 C6 C9 -3.3(5) . . . . ?
C10 C1 C2 C3 -178.4(3) . . . . ?
C10 C1 C2 C7 3.7(5) . . . . ?
C25 C24 C23 C22 0.3(6) . . . . ?
C33 C34 C35 C36 -0.4(6) . . . . ?
C33 C34 C37 O38 -27.8(5) . . . . ?
C33 C34 C37 O39 152.6(4) . . . . ?
C22 N21 C26 C25 0.2(5) . . . . ?
C22 N21 C20 C3 -165.7(3) . . . . ?
C37 C34 C35 C36 -178.1(3) . . . . ?
C37 C34 C33 C32 -179.5(4) . . . . ?
C8 C4 C3 C2 -178.9(3) . . . . ?
C8 C4 C3 C20 4.0(5) . . . . ?
C8 C4 C5 C6 177.1(3) . . . . ?
C8 C4 C5 C30 -9.0(5) . . . . ?
C14 C15 C16 N11 -0.2(6) . . . . ?
C14 C13 C12 N11 1.3(6) . . . . ?
C5 C4 C3 C2 1.8(5) . . . . ?
C5 C4 C3 C20 -175.2(3) . . . . ?
C23 C24 C25 C26 1.5(6) . . . . ?
C12 N11 C10 C1 -144.7(3) . . . . ?
C12 N11 C16 C15 -2.9(6) . . . . ?
C2 C1 C6 C5 -1.0(5) . . . . ?
C2 C1 C6 C9 179.1(3) . . . . ?
C2 C1 C10 N11 -93.3(4) . . . . ?
C2 C3 C20 N21 -107.4(4) . . . . ?
C16 N11 C10 C1 44.0(5) . . . . ?
C16 N11 C12 C13 2.4(6) . . . . ?
C16 C15 C14 C17 -173.3(3) . . . . ?
C16 C15 C14 C13 3.8(6) . . . . ?
C26 N21 C22 C23 1.7(6) . . . . ?
C26 N21 C20 C3 17.6(5) . . . . ?
C36 N31 C32 C33 -1.0(6) . . . . ?
C36 N31 C30 C5 133.5(3) . . . . ?
C9 C6 C5 C4 -176.8(3) . . . . ?
C9 C6 C5 C30 9.3(5) . . . . ?
C20 N21 C22 C23 -175.1(3) . . . . ?
C20 N21 C26 C25 176.8(3) . . . . ?
C20 C3 C2 C1 177.4(3) . . . . ?
C20 C3 C2 C7 -4.6(5) . . . . ?
C30 N31 C32 C33 -178.7(4) . . . . ?
C30 N31 C36 C35 -178.8(3) . . . . ?
O29 C27 C24 C25 -15.1(5) . . . . ?
O29 C27 C24 C23 168.6(3) . . . . ?
O38 C37 O39 Yb2 -49.3(6) . . . 2_556 ?
O28 C27 C24 C25 165.4(3) . . . . ?
O28 C27 C24 C23 -10.9(5) . . . . ?
O28 C27 O29 Yb2 -13.5(6) . . . 1_566 ?
O39 C37 O38 Yb2 9.4(7) . . . 1_565 ?
O18 C17 C14 C15 169.3(3) . . . . ?
O18 C17 C14 C13 -7.8(5) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.505 0.000 0.500 434.1 132.3 '13x water'
2 0.269 0.636 0.019 12.2 11.1 ?
3 0.731 0.364 0.981 12.2 11.1 ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.450
_oxdiff_exptl_absorpt_empirical_full_min 0.694
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_jj003_la_no3_h2o-acet_red3
_database_code_depnum_ccdc_archive 'CCDC 1833441'
loop_
_audit_author_name
_audit_author_address
'Antti Tiihonen'
;University of Jyv?skyl?, Department of Chemistry
Finland
;
_audit_update_record             
;
2018-03-29 deposited with the CCDC.	2019-02-28 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_CHEMW03_I                   
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as...
RESPONSE: The structure contains voids of unresolved electron density
which was treated using Olex2 solvent mask procedure (full details in 
_smtbx_masks_special_details). The 7 water molecules per asymmetric unit 
 are included in the formula and used in the calculations. 
;
_vrf_PLAT420_I                   
;
PROBLEM: D-H Without Acceptor...
RESPONSE: Hydrogen bond acceptors (water) have been removed among
other disordered solvent from the voids (see CHEMW03_ALERT_2_A).
;
_vrf_PLAT412_I                   
;
PROBLEM: Short Intra XH3 .. XHn...
RESPONSE: Hydrogen atoms calculated using a riding model in their general
(unoptimized) geometry causing a proximity alert.
;
_vrf_FORMU01_I                   
;
PROBLEM: There is a discrepancy between the atom counts...
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_CELLZ01_I                   
;
PROBLEM: Difference between formula and atom_site...
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT041_I                   
;
PROBLEM: Calc. and Reported SumFormula Strings  Differ...
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT044_I                   
;
PROBLEM: Calculated and Reported Density Dx Differ...
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT051_I                   
;
PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs...
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT068_I                   
;
PROBLEM: Reported F000 Differs from Calcd (or Missing)...
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT606_I                   
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure...
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
# end Validation Reply Form

_audit_creation_date             2018-03-28
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H31 La N3 O8, 3(N O3)'
_chemical_formula_sum            'C30 H45 La N6 O24'
_chemical_formula_weight         1012.63
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C21 H25 N4 O12 La1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
La La -1.4094 9.0376 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.6393(4)
_cell_length_b                   12.2016(6)
_cell_length_c                   19.0185(7)
_cell_angle_alpha                105.771(4)
_cell_angle_beta                 99.826(3)
_cell_angle_gamma                99.967(4)
_cell_volume                     2063.50(16)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6508
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      75.5620
_cell_measurement_theta_min      3.8550
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    8.855
_exptl_absorpt_correction_T_max  0.644
_exptl_absorpt_correction_T_min  0.470
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1032
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 1 -12 0.0235
3 6 -3 0.0394
-6 1 5 0.0374
6 0 -5 0.0236
1 8 -5 0.0410
-3 -6 2 0.0363
1 -1 12 0.0187
0 -8 5 0.0207

_exptl_crystal_size_max          0.086
_exptl_crystal_size_mid          0.064
_exptl_crystal_size_min          0.042
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.9997 1.0001 -12.0000 -0.3400 -0.9750 0.1971
3.0004 5.9995 -2.9985 0.0275 0.2851 0.9421
-5.9993 0.9993 4.9992 0.8441 -0.2765 -0.4379
5.9994 0.0006 -4.9990 -0.7717 0.3048 0.5481
1.0009 7.9992 -4.9984 0.2750 -0.0321 1.0307
-3.0004 -5.9995 1.9985 -0.0697 -0.3593 -0.9282
0.9997 -1.0001 12.0000 0.3400 0.9750 -0.1971
-0.0010 -7.9991 4.9986 -0.3685 0.1447 -0.9510

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_unetI/netI     0.0532
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12441
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.999
_diffrn_reflns_theta_min         3.870
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -63.00  27.00   1.00    2.50    --  -41.65  57.00   0.00   90
  2  ω      3.00  61.00   1.00    2.50    --   41.65 -99.00  60.00   58
  3  ω     41.00 140.00   1.00    5.00    --  112.00 -77.00  30.00   99
  4  ω     79.00 116.00   1.00    5.00    --  112.00-111.00 150.00   37
  5  ω     45.00 140.00   1.00    5.00    --  112.00 -30.00 150.00   95
  6  ω     43.00 136.00   1.00    5.00    --  112.00 -30.00   0.00   93
  7  ω     56.00 116.00   1.00    5.00    --  112.00-111.00 -60.00   60
  8  ω     26.00  73.00   1.00    2.50    --   41.65-125.00-120.00   47
  9  ω     86.00 178.00   1.00    5.00    --  112.00  45.00-180.00   92
 10  ω    108.00 172.00   1.00    5.00    --  112.00 111.00  90.00   64
 11  ω    108.00 178.00   1.00    5.00    --  112.00 111.00 120.00   70
 12  ω     44.00 110.00   1.00    5.00    --  112.00 -61.00 150.00   66
 13  ω   -114.00 -16.00   1.00    2.50    --  -41.65 -57.00-150.00   98
 14  ω   -112.00 -17.00   1.00    2.50    --  -41.65 -57.00  90.00   95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0935072000
_diffrn_orient_matrix_UB_12      0.0724205000
_diffrn_orient_matrix_UB_13      0.0421571000
_diffrn_orient_matrix_UB_21      0.1126519000
_diffrn_orient_matrix_UB_22      0.0282750000
_diffrn_orient_matrix_UB_23      0.0742249000
_diffrn_orient_matrix_UB_31      0.0797726000
_diffrn_orient_matrix_UB_32      0.1101941000
_diffrn_orient_matrix_UB_33      -0.0138881000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6502
_reflns_number_total             7466
_reflns_odcompleteness_completeness 99.36
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         2.677
_refine_diff_density_min         -2.394
_refine_diff_density_rms         0.138
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     438
_refine_ls_number_reflns         7466
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0736
_refine_ls_R_factor_gt           0.0671
_refine_ls_restrained_S_all      1.098
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1130P)²+4.6111P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1801
_refine_ls_wR_factor_ref         0.1883
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N31) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(La1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O45) = Uanis(N44) = Uanis(O47) = Uanis(O46)
Uanis(O50) = Uanis(N48) = Uanis(O51) = Uanis(O49)
Uanis(O41) = Uanis(O43) = Uanis(N40) = Uanis(O42)
3.a Rotating group:
 O2W(H2WA,H2WB), O1W(H1WA,H1WB)
3.b Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C20(H20A,H20B), C10(H10A,H10B)
3.c Aromatic/amide H refined with riding coordinates:
 C35(H35), C36(H36), C13(H13), C32(H32), C25(H25), C15(H15), C26(H26),
 C33(H33), C12(H12), C22(H22), C16(H16), C23(H23)
3.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C8(H8A,H8B,H8C), C7(H7A,H7B,H7C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
La1 La 0.23446(3) -0.48338(4) 0.00334(2) 0.03835(16) Uani 1 1 d . U . . .
O38 O 0.5439(5) 0.4811(5) 0.9121(2) 0.0465(12) Uani 1 1 d . . . . .
O39 O 0.3134(5) 0.4929(5) 0.8817(2) 0.0502(13) Uani 1 1 d . . . . .
O19 O -0.0031(5) -0.3972(5) 0.0825(3) 0.0477(12) Uani 1 1 d . . . . .
O29 O 0.1360(5) 0.4062(6) 0.0847(3) 0.0564(15) Uani 1 1 d . . . . .
O18 O 0.2348(5) -0.3272(5) 0.1214(2) 0.0483(13) Uani 1 1 d . . . . .
O43 O 0.2339(7) -0.2539(7) 0.4288(4) 0.0734(10) Uani 1 1 d . . . . .
C37 C 0.4313(7) 0.4740(7) 0.8665(3) 0.0382(15) Uani 1 1 d . . . . .
C17 C 0.1084(7) -0.3290(7) 0.1299(3) 0.0404(15) Uani 1 1 d . . . . .
O41 O 0.0204(7) -0.3352(7) 0.4311(4) 0.0734(10) Uani 1 1 d . . . . .
O45 O -0.3966(8) -0.1423(8) 0.2884(4) 0.0839(11) Uani 1 1 d . . . . .
N31 N 0.4323(5) 0.3593(5) 0.6338(3) 0.0320(11) Uani 1 1 d . U . . .
O47 O -0.3514(8) -0.2082(8) 0.1798(4) 0.0839(11) Uani 1 1 d . . . . .
N21 N -0.0113(6) 0.3330(5) 0.3075(3) 0.0339(11) Uani 1 1 d . . . . .
N40 N 0.1200(8) -0.3321(9) 0.4008(5) 0.0734(10) Uani 1 1 d . . . . .
N11 N 0.0598(6) -0.1154(5) 0.3367(3) 0.0382(12) Uani 1 1 d . . . . .
O46 O -0.4842(8) -0.0867(8) 0.1950(4) 0.0839(11) Uani 1 1 d . . . . .
O42 O 0.1113(7) -0.4073(7) 0.3415(4) 0.0734(10) Uani 1 1 d . . . . .
C4 C 0.2094(6) 0.3272(6) 0.4701(3) 0.0331(13) Uani 1 1 d . . . . .
C30 C 0.4383(7) 0.3193(7) 0.5518(3) 0.0417(16) Uani 1 1 d . . . . .
H30A H 0.480720 0.387877 0.537716 0.050 Uiso 1 1 calc R . . . .
H30B H 0.502741 0.264116 0.545006 0.050 Uiso 1 1 calc R . . . .
C3 C 0.0731(6) 0.2694(6) 0.4188(3) 0.0326(13) Uani 1 1 d . . . . .
C35 C 0.3106(6) 0.4241(6) 0.7294(3) 0.0372(14) Uani 1 1 d . . . . .
H35 H 0.225147 0.441306 0.743764 0.045 Uiso 1 1 calc R . . . .
C14 C 0.0905(7) -0.2504(6) 0.2022(4) 0.0401(15) Uani 1 1 d . . . . .
C6 C 0.2417(7) 0.1376(6) 0.4823(3) 0.0361(14) Uani 1 1 d . . . . .
C9 C 0.3347(9) 0.0706(8) 0.5174(4) 0.0499(18) Uani 1 1 d . . . . .
H9A H 0.283613 -0.011903 0.502063 0.075 Uiso 1 1 calc GR . . . .
H9B H 0.355237 0.103224 0.572213 0.075 Uiso 1 1 calc GR . . . .
H9C H 0.425774 0.076820 0.500853 0.075 Uiso 1 1 calc GR . . . .
C1 C 0.1067(7) 0.0828(6) 0.4322(3) 0.0331(13) Uani 1 1 d . . . . .
C36 C 0.3129(6) 0.3843(6) 0.6547(3) 0.0354(14) Uani 1 1 d . . . . .
H36 H 0.228484 0.374541 0.617428 0.043 Uiso 1 1 calc R . . . .
C34 C 0.4338(7) 0.4385(6) 0.7831(3) 0.0373(14) Uani 1 1 d . . . . .
C5 C 0.2913(6) 0.2602(6) 0.5000(3) 0.0363(14) Uani 1 1 d . . . . .
C20 C -0.0183(7) 0.3408(6) 0.3876(4) 0.0390(14) Uani 1 1 d . . . . .
H20A H 0.015031 0.423691 0.419429 0.047 Uiso 1 1 calc R . . . .
H20B H -0.120049 0.313073 0.389386 0.047 Uiso 1 1 calc R . . . .
C13 C 0.2080(7) -0.1763(7) 0.2544(4) 0.0439(16) Uani 1 1 d . . . . .
H13 H 0.301449 -0.171757 0.244035 0.053 Uiso 1 1 calc R . . . .
C32 C 0.5568(6) 0.3772(6) 0.6856(3) 0.0387(15) Uani 1 1 d . . . . .
H32 H 0.642025 0.362240 0.669927 0.046 Uiso 1 1 calc R . . . .
C25 C 0.1264(7) 0.3480(6) 0.2179(4) 0.0394(14) Uani 1 1 d . . . . .
H25 H 0.216711 0.353046 0.203839 0.047 Uiso 1 1 calc R . . . .
C15 C -0.0447(8) -0.2540(8) 0.2171(4) 0.055(2) Uani 1 1 d . . . . .
H15 H -0.128237 -0.303049 0.180795 0.066 Uiso 1 1 calc R . . . .
C2 C 0.0239(6) 0.1494(6) 0.4002(3) 0.0332(13) Uani 1 1 d . . . . .
C26 C 0.1160(7) 0.3389(6) 0.2880(4) 0.0395(14) Uani 1 1 d . . . . .
H26 H 0.199238 0.336937 0.322077 0.047 Uiso 1 1 calc R . . . .
C10 C 0.0464(8) -0.0470(6) 0.4127(4) 0.0426(15) Uani 1 1 d . . . . .
H10A H 0.097903 -0.076069 0.450970 0.051 Uiso 1 1 calc R . . . .
H10B H -0.057024 -0.060997 0.414424 0.051 Uiso 1 1 calc R . . . .
C8 C 0.2555(7) 0.4587(7) 0.4918(3) 0.0452(17) Uani 1 1 d . . . . .
H8A H 0.257632 0.482253 0.446621 0.068 Uiso 1 1 calc GR . . . .
H8B H 0.352222 0.485691 0.525337 0.068 Uiso 1 1 calc GR . . . .
H8C H 0.186642 0.493738 0.517697 0.068 Uiso 1 1 calc GR . . . .
C24 C 0.0035(8) 0.3498(7) 0.1684(4) 0.0439(16) Uani 1 1 d . . . . .
N44 N -0.4088(10) -0.1435(10) 0.2236(6) 0.0839(11) Uani 1 1 d . . . . .
C33 C 0.5588(7) 0.4169(6) 0.7606(3) 0.0371(14) Uani 1 1 d . . . . .
H33 H 0.645519 0.429638 0.797020 0.045 Uiso 1 1 calc R . . . .
C27 C 0.0118(8) 0.3709(8) 0.0943(4) 0.0466(17) Uani 1 1 d . . . . .
C12 C 0.1924(7) -0.1080(7) 0.3220(4) 0.0430(15) Uani 1 1 d . . . . .
H12 H 0.274593 -0.056080 0.357992 0.052 Uiso 1 1 calc R . . . .
C7 C -0.1214(7) 0.0892(7) 0.3453(4) 0.0436(16) Uani 1 1 d . . . . .
H7A H -0.186273 0.143066 0.349665 0.065 Uiso 1 1 calc GR . . . .
H7B H -0.164306 0.019219 0.356896 0.065 Uiso 1 1 calc GR . . . .
H7C H -0.107103 0.066559 0.293963 0.065 Uiso 1 1 calc GR . . . .
C22 C -0.1300(8) 0.3328(7) 0.2603(4) 0.0449(16) Uani 1 1 d . . . . .
H22 H -0.219073 0.327151 0.275606 0.054 Uiso 1 1 calc R . . . .
C16 C -0.0575(8) -0.1860(7) 0.2850(4) 0.0534(19) Uani 1 1 d . . . . .
H16 H -0.150549 -0.188849 0.295713 0.064 Uiso 1 1 calc R . . . .
C23 C -0.1274(8) 0.3404(8) 0.1898(4) 0.0508(18) Uani 1 1 d . . . . .
H23 H -0.213406 0.339297 0.156471 0.061 Uiso 1 1 calc R . . . .
O28 O -0.1068(5) 0.3561(5) 0.0497(3) 0.0516(13) Uani 1 1 d . . . . .
O2W O 0.2750(6) -0.6880(6) -0.0373(3) 0.0623(15) Uani 1 1 d . . . . .
H2WA H 0.186018 -0.752681 -0.050934 0.093 Uiso 1 1 d GR . . . .
H2WB H 0.342617 -0.708601 0.000759 0.093 Uiso 1 1 d GR . . . .
O1W O 0.4229(6) -0.2919(6) 0.0221(4) 0.0644(15) Uani 1 1 d . . . . .
H1WA H 0.439605 -0.238190 0.070339 0.097 Uiso 1 1 d GR . . . .
H1WB H 0.394803 -0.251378 -0.011510 0.097 Uiso 1 1 d GR . . . .
O49 O 0.4618(9) 0.3241(9) 0.2634(5) 0.1049(15) Uani 1 1 d . . . A 2
O50 O 0.6140(9) 0.2916(9) 0.3491(5) 0.1049(15) Uani 1 1 d . . . A 2
O51 O 0.4445(9) 0.3783(10) 0.3738(5) 0.1049(15) Uani 1 1 d . . . A 2
N48 N 0.5033(12) 0.3326(12) 0.3324(7) 0.1049(15) Uani 1 1 d . . . A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
La1 O38 2.436(4) 2_656 ?
La1 O39 2.515(4) 1_544 ?
La1 O19 2.470(5) 2_545 ?
La1 O29 2.510(5) 1_545 ?
La1 O18 2.518(5) . ?
La1 O28 2.455(5) 2 ?
La1 O2W 2.525(6) . ?
La1 O1W 2.596(6) . ?
O38 C37 1.243(8) . ?
O39 C37 1.263(8) . ?
O19 C17 1.270(8) . ?
O29 C27 1.261(9) . ?
O18 C17 1.253(8) . ?
O43 N40 1.249(10) . ?
C37 C34 1.532(8) . ?
C17 C14 1.505(9) . ?
O41 N40 1.202(9) . ?
O45 N44 1.214(12) . ?
N31 C30 1.518(7) . ?
N31 C36 1.336(8) . ?
N31 C32 1.359(8) . ?
O47 N44 1.254(13) . ?
N21 C20 1.514(8) . ?
N21 C26 1.338(8) . ?
N21 C22 1.329(8) . ?
N40 O42 1.224(10) . ?
N11 C10 1.498(8) . ?
N11 C12 1.348(9) . ?
N11 C16 1.346(9) . ?
O46 N44 1.244(13) . ?
C4 C3 1.429(8) . ?
C4 C5 1.393(10) . ?
C4 C8 1.508(10) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C5 1.510(8) . ?
C3 C20 1.502(9) . ?
C3 C2 1.383(10) . ?
C35 H35 0.9500 . ?
C35 C36 1.376(8) . ?
C35 C34 1.379(8) . ?
C14 C13 1.364(10) . ?
C14 C15 1.377(10) . ?
C6 C9 1.504(10) . ?
C6 C1 1.406(9) . ?
C6 C5 1.416(10) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C1 C2 1.413(9) . ?
C1 C10 1.508(10) . ?
C36 H36 0.9500 . ?
C34 C33 1.389(9) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C13 H13 0.9500 . ?
C13 C12 1.377(9) . ?
C32 H32 0.9500 . ?
C32 C33 1.371(8) . ?
C25 H25 0.9500 . ?
C25 C26 1.386(9) . ?
C25 C24 1.389(9) . ?
C15 H15 0.9500 . ?
C15 C16 1.370(10) . ?
C2 C7 1.523(8) . ?
C26 H26 0.9500 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C24 C27 1.514(10) . ?
C24 C23 1.386(10) . ?
C33 H33 0.9500 . ?
C27 O28 1.255(8) . ?
C12 H12 0.9500 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C22 H22 0.9500 . ?
C22 C23 1.372(10) . ?
C16 H16 0.9500 . ?
C23 H23 0.9500 . ?
O2W H2WA 1.0024 . ?
O2W H2WB 1.0041 . ?
O1W H1WA 0.9407 . ?
O1W H1WB 0.9408 . ?
O49 N48 1.275(14) . ?
O50 N48 1.283(14) . ?
O51 N48 1.129(14) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O38 La1 O39 101.49(15) 2_656 1_544 ?
O38 La1 O19 146.6(2) 2_656 2_545 ?
O38 La1 O29 78.68(17) 2_656 1_545 ?
O38 La1 O18 77.79(16) 2_656 . ?
O38 La1 O28 142.4(2) 2_656 2 ?
O38 La1 O2W 73.82(18) 2_656 . ?
O38 La1 O1W 71.6(2) 2_656 . ?
O39 La1 O18 140.8(2) 1_544 . ?
O39 La1 O2W 73.7(2) 1_544 . ?
O39 La1 O1W 73.7(2) 1_544 . ?
O19 La1 O39 81.98(16) 2_545 1_544 ?
O19 La1 O29 79.46(18) 2_545 1_545 ?
O19 La1 O18 120.14(15) 2_545 . ?
O19 La1 O2W 75.47(18) 2_545 . ?
O19 La1 O1W 139.2(2) 2_545 . ?
O29 La1 O39 143.6(2) 1_545 1_544 ?
O29 La1 O18 75.4(2) 1_545 . ?
O29 La1 O2W 71.5(2) 1_545 . ?
O29 La1 O1W 137.3(2) 1_545 . ?
O18 La1 O2W 139.67(19) . . ?
O18 La1 O1W 68.91(19) . . ?
O28 La1 O39 78.58(17) 2 1_544 ?
O28 La1 O19 70.96(19) 2 2_545 ?
O28 La1 O29 123.23(16) 2 1_545 ?
O28 La1 O18 79.34(18) 2 . ?
O28 La1 O2W 138.82(19) 2 . ?
O28 La1 O1W 72.47(19) 2 . ?
O2W La1 O1W 125.7(2) . . ?
C37 O38 La1 176.5(5) . 2_656 ?
C37 O39 La1 129.2(4) . 1_566 ?
C17 O19 La1 174.2(4) . 2_545 ?
C27 O29 La1 135.0(4) . 1_565 ?
C17 O18 La1 110.6(4) . . ?
O38 C37 O39 126.6(6) . . ?
O38 C37 C34 117.4(5) . . ?
O39 C37 C34 116.0(5) . . ?
O19 C17 C14 119.0(6) . . ?
O18 C17 O19 123.5(6) . . ?
O18 C17 C14 117.5(6) . . ?
C36 N31 C30 121.6(5) . . ?
C36 N31 C32 121.1(5) . . ?
C32 N31 C30 117.1(5) . . ?
C26 N21 C20 119.8(5) . . ?
C22 N21 C20 118.6(5) . . ?
C22 N21 C26 121.3(6) . . ?
O41 N40 O43 121.4(8) . . ?
O41 N40 O42 119.8(8) . . ?
O42 N40 O43 118.8(7) . . ?
C12 N11 C10 118.7(6) . . ?
C16 N11 C10 120.8(6) . . ?
C16 N11 C12 120.5(6) . . ?
C3 C4 C8 118.5(6) . . ?
C5 C4 C3 118.7(6) . . ?
C5 C4 C8 122.8(6) . . ?
N31 C30 H30A 109.0 . . ?
N31 C30 H30B 109.0 . . ?
H30A C30 H30B 107.8 . . ?
C5 C30 N31 112.8(5) . . ?
C5 C30 H30A 109.0 . . ?
C5 C30 H30B 109.0 . . ?
C4 C3 C20 119.3(6) . . ?
C2 C3 C4 120.2(6) . . ?
C2 C3 C20 120.5(6) . . ?
C36 C35 H35 120.4 . . ?
C36 C35 C34 119.1(6) . . ?
C34 C35 H35 120.4 . . ?
C13 C14 C17 120.5(6) . . ?
C13 C14 C15 119.1(6) . . ?
C15 C14 C17 120.3(6) . . ?
C1 C6 C9 122.4(7) . . ?
C1 C6 C5 118.5(6) . . ?
C5 C6 C9 119.1(6) . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C6 C1 C2 120.3(6) . . ?
C6 C1 C10 120.9(6) . . ?
C2 C1 C10 118.8(6) . . ?
N31 C36 C35 120.9(5) . . ?
N31 C36 H36 119.5 . . ?
C35 C36 H36 119.5 . . ?
C35 C34 C37 120.3(5) . . ?
C35 C34 C33 119.2(5) . . ?
C33 C34 C37 120.5(5) . . ?
C4 C5 C30 119.3(7) . . ?
C4 C5 C6 121.8(6) . . ?
C6 C5 C30 118.9(6) . . ?
N21 C20 H20A 109.2 . . ?
N21 C20 H20B 109.2 . . ?
C3 C20 N21 112.2(5) . . ?
C3 C20 H20A 109.2 . . ?
C3 C20 H20B 109.2 . . ?
H20A C20 H20B 107.9 . . ?
C14 C13 H13 119.7 . . ?
C14 C13 C12 120.6(6) . . ?
C12 C13 H13 119.7 . . ?
N31 C32 H32 120.2 . . ?
N31 C32 C33 119.6(6) . . ?
C33 C32 H32 120.2 . . ?
C26 C25 H25 120.3 . . ?
C26 C25 C24 119.3(6) . . ?
C24 C25 H25 120.3 . . ?
C14 C15 H15 120.4 . . ?
C16 C15 C14 119.3(7) . . ?
C16 C15 H15 120.4 . . ?
C3 C2 C1 120.5(6) . . ?
C3 C2 C7 119.5(6) . . ?
C1 C2 C7 119.9(6) . . ?
N21 C26 C25 119.9(6) . . ?
N21 C26 H26 120.0 . . ?
C25 C26 H26 120.0 . . ?
N11 C10 C1 113.3(5) . . ?
N11 C10 H10A 108.9 . . ?
N11 C10 H10B 108.9 . . ?
C1 C10 H10A 108.9 . . ?
C1 C10 H10B 108.9 . . ?
H10A C10 H10B 107.7 . . ?
C4 C8 H8A 109.5 . . ?
C4 C8 H8B 109.5 . . ?
C4 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C25 C24 C27 121.3(6) . . ?
C23 C24 C25 119.2(7) . . ?
C23 C24 C27 119.4(6) . . ?
O45 N44 O47 121.2(11) . . ?
O45 N44 O46 123.1(11) . . ?
O46 N44 O47 115.7(9) . . ?
C34 C33 H33 120.0 . . ?
C32 C33 C34 119.9(5) . . ?
C32 C33 H33 120.0 . . ?
O29 C27 C24 117.2(6) . . ?
O28 C27 O29 126.6(7) . . ?
O28 C27 C24 116.2(6) . . ?
N11 C12 C13 119.5(6) . . ?
N11 C12 H12 120.2 . . ?
C13 C12 H12 120.2 . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N21 C22 H22 119.2 . . ?
N21 C22 C23 121.7(7) . . ?
C23 C22 H22 119.2 . . ?
N11 C16 C15 121.0(7) . . ?
N11 C16 H16 119.5 . . ?
C15 C16 H16 119.5 . . ?
C24 C23 H23 120.7 . . ?
C22 C23 C24 118.6(7) . . ?
C22 C23 H23 120.7 . . ?
C27 O28 La1 135.2(6) . 2 ?
La1 O2W H2WA 115.3 . . ?
La1 O2W H2WB 115.7 . . ?
H2WA O2W H2WB 102.8 . . ?
La1 O1W H1WA 112.6 . . ?
La1 O1W H1WB 113.2 . . ?
H1WA O1W H1WB 105.6 . . ?
O49 N48 O50 116.0(12) . . ?
O51 N48 O49 118.5(12) . . ?
O51 N48 O50 125.5(12) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
La1 O39 C37 O38 -12.1(12) 1_566 . . . ?
La1 O39 C37 C34 167.6(5) 1_566 . . . ?
La1 O29 C27 C24 -156.5(6) 1_565 . . . ?
La1 O29 C27 O28 20.2(14) 1_565 . . . ?
La1 O18 C17 O19 -3.4(9) . . . . ?
La1 O18 C17 C14 173.2(5) . . . . ?
O38 C37 C34 C35 177.1(7) . . . . ?
O38 C37 C34 C33 -0.8(11) . . . . ?
O39 C37 C34 C35 -2.7(11) . . . . ?
O39 C37 C34 C33 179.4(7) . . . . ?
O19 C17 C14 C13 179.8(7) . . . . ?
O19 C17 C14 C15 1.2(12) . . . . ?
O29 C27 O28 La1 -62.2(11) . . . 2 ?
O18 C17 C14 C13 3.0(11) . . . . ?
O18 C17 C14 C15 -175.6(8) . . . . ?
C37 C34 C33 C32 175.4(7) . . . . ?
C17 C14 C13 C12 -177.1(7) . . . . ?
C17 C14 C15 C16 176.6(8) . . . . ?
N31 C30 C5 C4 91.1(7) . . . . ?
N31 C30 C5 C6 -89.9(7) . . . . ?
N31 C32 C33 C34 0.0(11) . . . . ?
N21 C22 C23 C24 -0.7(13) . . . . ?
C4 C3 C20 N21 103.4(6) . . . . ?
C4 C3 C2 C1 0.8(8) . . . . ?
C4 C3 C2 C7 -179.8(5) . . . . ?
C30 N31 C36 C35 -177.9(7) . . . . ?
C30 N31 C32 C33 178.0(7) . . . . ?
C3 C4 C5 C30 177.5(5) . . . . ?
C3 C4 C5 C6 -1.5(8) . . . . ?
C35 C34 C33 C32 -2.6(11) . . . . ?
C14 C13 C12 N11 0.5(12) . . . . ?
C14 C15 C16 N11 0.6(14) . . . . ?
C6 C1 C2 C3 -1.3(8) . . . . ?
C6 C1 C2 C7 179.3(5) . . . . ?
C6 C1 C10 N11 -103.5(7) . . . . ?
C9 C6 C1 C2 -179.4(5) . . . . ?
C9 C6 C1 C10 1.6(9) . . . . ?
C9 C6 C5 C4 -179.2(5) . . . . ?
C9 C6 C5 C30 1.9(8) . . . . ?
C1 C6 C5 C4 1.0(8) . . . . ?
C1 C6 C5 C30 -178.0(5) . . . . ?
C36 N31 C30 C5 -26.0(10) . . . . ?
C36 N31 C32 C33 2.7(11) . . . . ?
C36 C35 C34 C37 -175.5(7) . . . . ?
C36 C35 C34 C33 2.4(11) . . . . ?
C34 C35 C36 N31 0.3(11) . . . . ?
C5 C4 C3 C20 178.4(5) . . . . ?
C5 C4 C3 C2 0.6(8) . . . . ?
C5 C6 C1 C2 0.4(8) . . . . ?
C5 C6 C1 C10 -178.5(5) . . . . ?
C20 N21 C26 C25 -171.1(6) . . . . ?
C20 N21 C22 C23 171.8(7) . . . . ?
C20 C3 C2 C1 -177.0(5) . . . . ?
C20 C3 C2 C7 2.4(8) . . . . ?
C13 C14 C15 C16 -2.1(13) . . . . ?
C32 N31 C30 C5 158.8(6) . . . . ?
C32 N31 C36 C35 -2.9(11) . . . . ?
C25 C24 C27 O29 -11.7(12) . . . . ?
C25 C24 C27 O28 171.3(7) . . . . ?
C25 C24 C23 C22 1.7(13) . . . . ?
C15 C14 C13 C12 1.6(12) . . . . ?
C2 C3 C20 N21 -78.9(7) . . . . ?
C2 C1 C10 N11 77.6(7) . . . . ?
C26 N21 C20 C3 -43.1(8) . . . . ?
C26 N21 C22 C23 -1.0(12) . . . . ?
C26 C25 C24 C27 174.2(7) . . . . ?
C26 C25 C24 C23 -1.1(12) . . . . ?
C10 N11 C12 C13 175.6(7) . . . . ?
C10 N11 C16 C15 -176.1(8) . . . . ?
C10 C1 C2 C3 177.7(5) . . . . ?
C10 C1 C2 C7 -1.7(8) . . . . ?
C8 C4 C3 C20 0.8(8) . . . . ?
C8 C4 C3 C2 -177.0(5) . . . . ?
C8 C4 C5 C30 -5.0(8) . . . . ?
C8 C4 C5 C6 176.0(5) . . . . ?
C24 C25 C26 N21 -0.6(11) . . . . ?
C24 C27 O28 La1 114.6(7) . . . 2 ?
C27 C24 C23 C22 -173.7(8) . . . . ?
C12 N11 C10 C1 58.0(9) . . . . ?
C12 N11 C16 C15 1.6(13) . . . . ?
C22 N21 C20 C3 144.0(6) . . . . ?
C22 N21 C26 C25 1.7(11) . . . . ?
C16 N11 C10 C1 -124.3(8) . . . . ?
C16 N11 C12 C13 -2.1(11) . . . . ?
C23 C24 C27 O29 163.6(8) . . . . ?
C23 C24 C27 O28 -13.4(12) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.708 0.000 0.000 473.8 153.0 '14x water'

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.460
_oxdiff_exptl_absorpt_empirical_full_min 0.660
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_jj003-01-sm-otf-h2o-red6
_database_code_depnum_ccdc_archive 'CCDC 1833446'
loop_
_audit_author_name
_audit_author_address
'Antti Tiihonen'
;University of Jyv?skyl?, Department of Chemistry
Finland
;
_audit_update_record             
;
2018-03-29 deposited with the CCDC.	2019-02-28 downloaded from the CCDC.
;
_vrf_CHEMW03_I                   
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as...
RESPONSE: The structure contains voids of unresolved electron density
which was treated using Olex2 solvent mask procedure (full details in 
_smtbx_masks_special_details). The 12 water molecules per asymmetric unit 
 are included in the formula and used in the calculations. 
;
_vrf_PLAT420_I                   
;
PROBLEM: D-H Without Acceptor...
RESPONSE: Hydrogen bond acceptors (water) have been removed among
other disordered solvent from the voids (see CHEMW03_ALERT_2_B).
;
_vrf_PLAT973_I                   
;
PROBLEM: Check Calcd Positive Resid. Density on Sm1...
RESPONSE: Peak is located about 0.8 angstroms from the Sm1 atom
and is caused by the absorption effects. Data is recorded with Cu
radiation.
;
_vrf_PLAT412_I                   
;
PROBLEM: Short Intra XH3 .. XHn...
RESPONSE: Hydrogen atoms calculated using a riding model in their general
(unoptimized) geometry causing a proximity alert.
;
_vrf_FORMU01_I                   
;
PROBLEM: There is a discrepancy between the atom counts...
RESPONSE: See explanation above (CHEMW03_ALERT_2_B).
;
_vrf_CELLZ01_I                   
;
PROBLEM: Difference between formula and atom_site...
RESPONSE: See explanation above (CHEMW03_ALERT_2_B).
;
_vrf_PLAT041_I                   
;
PROBLEM: Calc. and Reported SumFormula Strings  Differ...
RESPONSE: See explanation above (CHEMW03_ALERT_2_B).
;
_vrf_PLAT042_I                   
;
PROBLEM: Calc. and Reported MoietyFormula Strings Differ...
RESPONSE: See explanation above (CHEMW03_ALERT_2_B).
;
_vrf_PLAT044_I                   
;
PROBLEM: Calculated and Reported Density Dx Differ...
RESPONSE: See explanation above (CHEMW03_ALERT_2_B).
;
_vrf_PLAT051_I                   
;
PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs...
RESPONSE: See explanation above (CHEMW03_ALERT_2_B).
;
_vrf_PLAT068_I                   
;
PROBLEM: Reported F000 Differs from Calcd (or Missing)...
RESPONSE: See explanation above (CHEMW03_ALERT_2_B).
;
_vrf_PLAT606_I                   
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure...
RESPONSE: See explanation above (CHEMW03_ALERT_2_B).
;
# end Validation Reply Form

_audit_creation_date             2018-03-28
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C60 H62 N6 O17 Sm2, 0.1(Br), 5.9(C F3 O3 S), 0.75(O)'
_chemical_formula_sum            'C65.90 H86 Br0.10 F17.70 N6 O47.45 S5.90 Sm2'
_chemical_formula_weight         2555.55
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C21 H20 O9 N3 F3 Sm S2'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sm Sm -5.3236 12.2178 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.1269(3)
_cell_length_b                   14.2176(4)
_cell_length_c                   34.2981(6)
_cell_angle_alpha                89.1178(19)
_cell_angle_beta                 87.111(2)
_cell_angle_gamma                87.308(3)
_cell_volume                     4926.1(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9569
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      76.5740
_cell_measurement_theta_min      2.5520
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    11.237
_exptl_absorpt_correction_T_max  0.736
_exptl_absorpt_correction_T_min  0.410
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.723
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2568
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2 1 21 0.0443
2 9 0 0.0203
-2 -9 -7 0.0169
-1 -9 2 0.0197
0 -9 6 0.0248
1 9 6 0.0235
0 8 -9 0.0322
-1 -9 -8 0.0250
6 -1 3 0.0706
-6 2 -2 0.0689
1 -2 -21 0.0323

_exptl_crystal_size_max          0.167
_exptl_crystal_size_mid          0.109
_exptl_crystal_size_min          0.046
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
1.9961 1.0102 21.0031 -0.0392 -0.0403 -0.9795
2.0150 9.0001 0.0167 0.5772 0.7993 -0.2187
-2.0134 -9.0037 -7.0165 -0.6008 -0.6913 0.5135
-1.0158 -8.9993 1.9843 -0.6684 -0.7205 0.0946
-0.0171 -8.9976 5.9852 -0.7529 -0.6725 -0.1137
1.0140 9.0034 6.0154 0.6954 0.5970 -0.4315
0.0161 7.9960 -8.9868 0.6569 0.6543 0.2555
-1.0135 -9.0045 -8.0154 -0.7021 -0.5661 0.5157
5.9952 -1.0003 3.0048 -0.6636 0.5477 -0.3502
-5.9937 2.0009 -2.0032 0.7528 -0.4988 0.2927
1.0009 -2.0112 -21.0015 -0.3405 0.3051 0.8753

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0610
_diffrn_reflns_av_unetI/netI     0.0940
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            29760
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.000
_diffrn_reflns_theta_min         3.112
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3953
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -118.00  -9.00   1.00    8.00    --  -41.78 -77.00  90.00  109
  2  ω   -116.00 -17.00   1.00    8.00    --  -41.78 -37.00 -30.00   99
  3  ω      1.00  83.00   1.00    8.00    --   41.78 -99.00 -60.00   82
  4  ω      1.00  62.00   1.00    8.00    --   41.78 -99.00-150.00   61
  5  ω     36.00 145.00   1.00   50.00    --  112.00 -77.00 -30.00  109
  6  ω     41.00 116.00   1.00   50.00    --  112.00-111.00 150.00   75
  7  ω     38.00  77.00   1.00   50.00    --  112.00 -30.00 -60.00   39
  8  ω     31.00 165.00   1.00   50.00    --  112.00 -15.00  90.00  134
  9  ω     31.00 109.00   1.00   50.00    --  112.00 -94.00 -90.00   78
 10  ω     45.00  91.00   1.00   50.00    --  112.00 -30.00 -30.00   46
 11  ω    106.00 169.00   1.00   50.00    --  112.00 111.00  60.00   63
 12  ω     41.00 126.00   1.00   50.00    --  112.00 -61.00 120.00   85
 13  ω     86.00 174.00   1.00   50.00    --  112.00  45.00 120.00   88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0979786000
_diffrn_orient_matrix_UB_12      0.0860599000
_diffrn_orient_matrix_UB_13      0.0033042000
_diffrn_orient_matrix_UB_21      0.1098259000
_diffrn_orient_matrix_UB_22      0.0642542000
_diffrn_orient_matrix_UB_23      -0.0154456000
_diffrn_orient_matrix_UB_31      -0.0398664000
_diffrn_orient_matrix_UB_32      -0.0153006000
_diffrn_orient_matrix_UB_33      -0.0421132000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                14021
_reflns_number_total             17807
_reflns_odcompleteness_completeness 99.35
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         1.639
_refine_diff_density_min         -1.386
_refine_diff_density_rms         0.143
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1256
_refine_ls_number_reflns         17807
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0845
_refine_ls_R_factor_gt           0.0694
_refine_ls_restrained_S_all      1.023
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0990P)²+8.1554P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1760
_refine_ls_wR_factor_ref         0.1891
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Shared sites
{O38A, O39B}
3. Restrained distances
 C34B-C37B
 1.53 with sigma of 0.02
 C37B-O38B
 1.25 with sigma of 0.02
 C37B-O39B
 1.25 with sigma of 0.02
 H4WA-O11A
 1.7 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(O38A) = Uanis(O39B)
Uanis(C35B) = Uanis(C36B) = Uanis(N31B) = Uanis(C32B) = Uanis(C33B) =
Uanis(C34B) = Uanis(C37B) = Uanis(O38B)
Uanis(O12B) = Uanis(O10A)
Uanis(F16B) = Uanis(C13B) = Uanis(F14B) = Uanis(F15B)
Uanis(F16A) = Uanis(C13A) = Uanis(F15A) = Uanis(F14A)
Uanis(C5A) = Uanis(F7A) = Uanis(F7B) = Uanis(F6A)
Uanis(C5B) = Uanis(F6B) = Uanis(F7B) = Uanis(F8B)
Uanis(O3B) = Uanis(O2B) = Uanis(O4B)
Uanis(C32A) = Uanis(C33A) = Uanis(C36A) = Uanis(C35A) = Uanis(C35B) =
Uanis(N31A) = Uanis(C37A) = Uanis(O39B) = Uanis(O39A)
Uanis(O6WA) = Uanis(O6WB)
5. Others
 Sof(C5B)=Sof(F8B)=Sof(F6B)=Sof(F7B)=Sof(O4B)=Sof(O3B)=Sof(O2B)=Sof(S1B)=1-
 FVAR(1)
 Sof(C5A)=Sof(F7A)=Sof(F8A)=Sof(F6A)=Sof(O4A)=Sof(O2A)=Sof(O3A)=Sof(S1A)=FVAR(1)
 Sof(C35B)=Sof(H35B)=Sof(C36B)=Sof(H36B)=Sof(N31B)=Sof(C32B)=Sof(H32B)=
 Sof(C33B)=Sof(H33B)=Sof(C34B)=Sof(C37B)=Sof(O38B)=Sof(O39B)=1-FVAR(2)
 Sof(C32A)=Sof(H32A)=Sof(C33A)=Sof(H33A)=Sof(C34A)=Sof(C35A)=Sof(H35A)=
 Sof(C36A)=Sof(H36A)=Sof(C37A)=Sof(N31A)=Sof(O38A)=Sof(O39A)=FVAR(2)
 Fixed Sof: Br1C(0.1) C13A(0.65) F14A(0.65) F16A(0.65) F15A(0.65) O10A(0.65)
 O12A(0.65) O11A(0.65) S9A(0.65) C13B(0.25) F14B(0.25) F16B(0.25) F15B(0.25)
 O12B(0.25) O10B(0.25) O11B(0.25) S9B(0.25) O6WB(0.375) O6WA(0.375)
6.a Rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB), O4W(H4WA,H4WB), O5W(H5WA,H5WB)
6.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C20(H20A,H20B), C49(H49A,H49B), C59(H59A,H59B), C69(H69A,H69B)
6.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C15(H15), C16(H16), C22(H22), C23(H23), C25(H25),
 C26(H26), C32A(H32A), C33A(H33A), C35A(H35A), C35B(H35B), C36B(H36B),
 C32B(H32B), C33B(H33B), C36A(H36A), C51(H51), C52(H52), C54(H54), C55(H55),
 C61(H61), C62(H62), C64(H64), C65(H65), C71(H71), C72(H72), C74(H74), C75(H75)
6.d Fitted hexagon refined as free rotating group:
 C35B(C36B,N31B,C32B,C33B,C34B)
6.e Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C46(H46A,H46B,H46C),
 C47(H47A,H47B,H47C), C48(H48A,H48B,H48C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.1946(7) 0.2940(6) 1.00966(19) 0.0309(15) Uani 1 1 d . . . . .
C2 C 0.2581(7) 0.3750(5) 1.02133(19) 0.0278(14) Uani 1 1 d . . . . .
C3 C 0.3566(7) 0.3641(6) 1.0487(2) 0.0330(16) Uani 1 1 d . . . . .
C4 C 0.3919(8) 0.2756(7) 1.0645(2) 0.0412(19) Uani 1 1 d . . . . .
C5 C 0.3339(9) 0.1955(7) 1.0508(2) 0.046(2) Uani 1 1 d . . . . .
C6 C 0.2327(9) 0.2053(6) 1.0247(2) 0.0380(18) Uani 1 1 d . . . . .
C7 C 0.2271(8) 0.4699(6) 1.0030(3) 0.0415(18) Uani 1 1 d . . . . .
H7A H 0.267223 0.471938 0.976413 0.062 Uiso 1 1 calc GR . . . .
H7B H 0.263009 0.519122 1.018547 0.062 Uiso 1 1 calc GR . . . .
H7C H 0.130980 0.480483 1.002127 0.062 Uiso 1 1 calc GR . . . .
C8 C 0.4950(11) 0.2675(12) 1.0943(3) 0.074(4) Uani 1 1 d . . . . .
H8A H 0.486553 0.322621 1.111226 0.111 Uiso 1 1 calc GR . . . .
H8B H 0.583176 0.264242 1.081117 0.111 Uiso 1 1 calc GR . . . .
H8C H 0.482816 0.210290 1.110157 0.111 Uiso 1 1 calc GR . . . .
C9 C 0.1659(12) 0.1201(8) 1.0104(3) 0.065(3) Uani 1 1 d . . . . .
H9A H 0.069653 0.129873 1.014217 0.097 Uiso 1 1 calc GR . . . .
H9B H 0.195364 0.064111 1.025153 0.097 Uiso 1 1 calc GR . . . .
H9C H 0.189289 0.111310 0.982582 0.097 Uiso 1 1 calc GR . . . .
C10 C 0.0898(7) 0.3047(6) 0.9810(2) 0.0330(16) Uani 1 1 d . . . . .
H10A H 0.046835 0.368400 0.983650 0.040 Uiso 1 1 calc R . . . .
H10B H 0.021728 0.258561 0.987780 0.040 Uiso 1 1 calc R . . . .
C12 C 0.2666(7) 0.2816(6) 0.9287(2) 0.0291(15) Uani 1 1 d . . . . .
H12 H 0.330515 0.282604 0.947984 0.035 Uiso 1 1 calc R . . . .
C13 C 0.3064(7) 0.2704(6) 0.88972(19) 0.0285(15) Uani 1 1 d . . . . .
H13 H 0.397962 0.264530 0.882219 0.034 Uiso 1 1 calc R . . . .
C14 C 0.2130(7) 0.2676(5) 0.86172(19) 0.0243(13) Uani 1 1 d . . . . .
C15 C 0.0810(7) 0.2773(6) 0.8734(2) 0.0316(16) Uani 1 1 d . . . . .
H15 H 0.014985 0.276301 0.854670 0.038 Uiso 1 1 calc R . . . .
C16 C 0.0455(7) 0.2886(6) 0.9125(2) 0.0322(16) Uani 1 1 d . . . . .
H16 H -0.045523 0.294702 0.920725 0.039 Uiso 1 1 calc R . . . .
C17 C 0.2556(7) 0.2559(5) 0.81877(19) 0.0269(14) Uani 1 1 d . . . . .
C20 C 0.4337(8) 0.4481(8) 1.0592(2) 0.046(2) Uani 1 1 d . . . . .
H20A H 0.527768 0.427438 1.061340 0.055 Uiso 1 1 calc R . . . .
H20B H 0.429065 0.495240 1.037671 0.055 Uiso 1 1 calc R . . . .
C22 C 0.2537(8) 0.5027(8) 1.1065(3) 0.052(3) Uani 1 1 d . . . . .
H22 H 0.191720 0.473036 1.091448 0.063 Uiso 1 1 calc R . . . .
C23 C 0.2100(7) 0.5546(7) 1.1387(2) 0.041(2) Uani 1 1 d . . . . .
H23 H 0.118166 0.559934 1.145821 0.049 Uiso 1 1 calc R . . . .
C24 C 0.2978(7) 0.5980(6) 1.1602(2) 0.0344(17) Uani 1 1 d . . . . .
C25 C 0.4316(7) 0.5886(7) 1.1494(2) 0.041(2) Uani 1 1 d . . . . .
H25 H 0.494757 0.617748 1.164202 0.049 Uiso 1 1 calc R . . . .
C26 C 0.4715(7) 0.5369(7) 1.1172(2) 0.0365(18) Uani 1 1 d . . . . .
H26 H 0.563064 0.531558 1.109558 0.044 Uiso 1 1 calc R . . . .
C27 C 0.2534(7) 0.6588(7) 1.1950(2) 0.0384(19) Uani 1 1 d . . . . .
C30 C 0.3940(11) 0.1004(9) 1.0604(4) 0.065(3) Uani 1 1 d . . . . .
C32A C 0.2309(13) 0.0647(10) 1.1111(4) 0.0567(10) Uani 0.724(6) 1 d . . P A 1
H32A H 0.175677 0.113842 1.100789 0.068 Uiso 0.724(6) 1 calc R . P A 1
C33A C 0.1850(14) 0.0099(10) 1.1441(4) 0.0567(10) Uani 0.724(6) 1 d . . P A 1
H33A H 0.095398 0.016018 1.153662 0.068 Uiso 0.724(6) 1 calc R . P A 1
C34A C 0.2728(11) -0.0514(9) 1.1614(3) 0.037(3) Uani 0.724(6) 1 d . . P A 1
C35A C 0.3907(14) -0.0701(11) 1.1422(4) 0.0567(10) Uani 0.724(6) 1 d . . P A 1
H35A H 0.449856 -0.117958 1.151677 0.068 Uiso 0.724(6) 1 calc R . P A 1
C35B C 0.274(3) -0.0544(12) 1.1482(7) 0.0567(10) Uani 0.276(6) 1 d . . P A 2
H35B H 0.276487 -0.120157 1.153677 0.068 Uiso 0.276(6) 1 calc R . P A 2
C36B C 0.326(3) -0.0213(14) 1.1125(6) 0.0567(10) Uani 0.276(6) 1 d G . P A 2
H36B H 0.363168 -0.064359 1.093620 0.068 Uiso 0.276(6) 1 calc R . P A 2
N31B N 0.323(2) 0.0749(15) 1.1045(5) 0.0567(10) Uani 0.276(6) 1 d G . P A 2
C32B C 0.268(2) 0.1379(12) 1.1321(6) 0.0567(10) Uani 0.276(6) 1 d G . P A 2
H32B H 0.266434 0.203648 1.126575 0.068 Uiso 0.276(6) 1 calc R . P A 2
C33B C 0.217(2) 0.1048(14) 1.1678(5) 0.0567(10) Uani 0.276(6) 1 d G . P A 2
H33B H 0.179753 0.147853 1.186631 0.068 Uiso 0.276(6) 1 calc R . P A 2
C34B C 0.220(3) 0.0086(16) 1.1758(6) 0.0567(10) Uani 0.276(6) 1 d DG . P A 2
C36A C 0.4250(14) -0.0200(10) 1.1089(4) 0.0567(10) Uani 0.724(6) 1 d . . P A 1
H36A H 0.507358 -0.035141 1.095423 0.068 Uiso 0.724(6) 1 calc R . P A 1
C37A C 0.2343(13) -0.1067(11) 1.1981(4) 0.0567(10) Uani 0.724(6) 1 d . . P A 1
C37B C 0.159(3) -0.0334(15) 1.2137(6) 0.0567(10) Uani 0.276(6) 1 d D . P A 2
C40 C 0.3008(7) 0.2976(5) 0.49308(18) 0.0239(13) Uani 1 1 d . . . . .
C41 C 0.2667(8) 0.2106(5) 0.4781(2) 0.0314(16) Uani 1 1 d . . . . .
C42 C 0.1687(8) 0.2091(5) 0.4511(2) 0.0297(15) Uani 1 1 d . . . . .
C43 C 0.1062(7) 0.2922(5) 0.4382(2) 0.0267(14) Uani 1 1 d . . . . .
C44 C 0.1392(6) 0.3781(5) 0.45376(19) 0.0231(13) Uani 1 1 d . . . . .
C45 C 0.2351(6) 0.3819(5) 0.48131(19) 0.0235(13) Uani 1 1 d . . . . .
C46 C 0.3357(10) 0.1193(6) 0.4913(3) 0.048(2) Uani 1 1 d . . . . .
H46A H 0.410064 0.133491 0.507124 0.072 Uiso 1 1 calc GR . . . .
H46B H 0.368558 0.083191 0.468452 0.072 Uiso 1 1 calc GR . . . .
H46C H 0.272791 0.082162 0.507010 0.072 Uiso 1 1 calc GR . . . .
C47 C 0.0040(9) 0.2910(6) 0.4069(2) 0.0399(19) Uani 1 1 d . . . . .
H47A H -0.085124 0.300350 0.419131 0.060 Uiso 1 1 calc GR . . . .
H47B H 0.011390 0.230152 0.393706 0.060 Uiso 1 1 calc GR . . . .
H47C H 0.020192 0.341592 0.387782 0.060 Uiso 1 1 calc GR . . . .
C48 C 0.2676(8) 0.4735(5) 0.4991(2) 0.0331(16) Uani 1 1 d . . . . .
H48A H 0.255614 0.468665 0.527625 0.050 Uiso 1 1 calc GR . . . .
H48B H 0.208668 0.524277 0.489450 0.050 Uiso 1 1 calc GR . . . .
H48C H 0.359684 0.487150 0.491975 0.050 Uiso 1 1 calc GR . . . .
C49 C 0.4080(7) 0.3023(6) 0.5217(2) 0.0317(15) Uani 1 1 d . . . . .
H49A H 0.444077 0.365825 0.520132 0.038 Uiso 1 1 calc R . . . .
H49B H 0.480811 0.256291 0.514044 0.038 Uiso 1 1 calc R . . . .
C51 C 0.2353(7) 0.2684(5) 0.57422(19) 0.0252(13) Uani 1 1 d . . . . .
H51 H 0.170878 0.268099 0.555024 0.030 Uiso 1 1 calc R . . . .
C52 C 0.1976(6) 0.2546(5) 0.61337(19) 0.0237(13) Uani 1 1 d . . . . .
H52 H 0.107497 0.246282 0.621110 0.028 Uiso 1 1 calc R . . . .
C53 C 0.2925(6) 0.2532(4) 0.64077(18) 0.0213(12) Uani 1 1 d . . . . .
C54 C 0.4240(7) 0.2662(5) 0.6290(2) 0.0269(14) Uani 1 1 d . . . . .
H54 H 0.490536 0.264971 0.647627 0.032 Uiso 1 1 calc R . . . .
C55 C 0.4564(6) 0.2809(5) 0.58962(19) 0.0241(13) Uani 1 1 d . . . . .
H55 H 0.545729 0.290119 0.581177 0.029 Uiso 1 1 calc R . . . .
C56 C 0.2543(7) 0.2406(5) 0.68377(19) 0.0255(14) Uani 1 1 d . . . . .
C59 C 0.1227(9) 0.1150(6) 0.4377(2) 0.0370(17) Uani 1 1 d . . . . .
H59A H 0.131979 0.068124 0.459180 0.044 Uiso 1 1 calc R . . . .
H59B H 0.027715 0.122037 0.432210 0.044 Uiso 1 1 calc R . . . .
C61 C 0.2739(11) 0.1343(7) 0.3788(3) 0.055(2) Uani 1 1 d . . . . .
H61 H 0.281672 0.198442 0.385349 0.066 Uiso 1 1 calc R . . . .
C62 C 0.3386(11) 0.0989(8) 0.3458(3) 0.057(3) Uani 1 1 d . . . . .
H62 H 0.390130 0.138864 0.329380 0.069 Uiso 1 1 calc R . . . .
C63 C 0.3297(9) 0.0060(7) 0.3364(3) 0.045(2) Uani 1 1 d . . . . .
C64 C 0.2509(9) -0.0494(6) 0.3602(3) 0.0410(19) Uani 1 1 d . . . . .
H64 H 0.242808 -0.113969 0.354413 0.049 Uiso 1 1 calc R . . . .
C65 C 0.1845(9) -0.0110(5) 0.3922(2) 0.0361(17) Uani 1 1 d . . . . .
H65 H 0.126817 -0.048389 0.407904 0.043 Uiso 1 1 calc R . . . .
C66 C 0.4048(10) -0.0339(7) 0.2998(3) 0.052(2) Uani 1 1 d . . . . .
C69 C 0.0591(7) 0.4655(5) 0.44163(19) 0.0243(13) Uani 1 1 d . . . . .
H69A H -0.033351 0.448474 0.438367 0.029 Uiso 1 1 calc R . . . .
H69B H 0.057859 0.511985 0.462863 0.029 Uiso 1 1 calc R . . . .
C71 C 0.2410(7) 0.5175(5) 0.3971(2) 0.0282(14) Uani 1 1 d . . . . .
H71 H 0.301407 0.487988 0.414266 0.034 Uiso 1 1 calc R . . . .
C72 C 0.2886(7) 0.5660(5) 0.3651(2) 0.0272(14) Uani 1 1 d . . . . .
H72 H 0.381396 0.568446 0.359783 0.033 Uiso 1 1 calc R . . . .
C73 C 0.2010(7) 0.6119(5) 0.34033(19) 0.0245(13) Uani 1 1 d . . . . .
C74 C 0.0660(7) 0.6013(6) 0.3481(2) 0.0334(16) Uani 1 1 d . . . . .
H74 H 0.003439 0.629524 0.331221 0.040 Uiso 1 1 calc R . . . .
C75 C 0.0239(7) 0.5500(5) 0.3802(2) 0.0278(14) Uani 1 1 d . . . . .
H75 H -0.068094 0.542116 0.385181 0.033 Uiso 1 1 calc R . . . .
C76 C 0.2510(7) 0.6720(5) 0.30637(19) 0.0268(14) Uani 1 1 d . . . . .
N11 N 0.1371(6) 0.2910(4) 0.93888(16) 0.0238(11) Uani 1 1 d . . . . .
N21 N 0.3855(6) 0.4939(6) 1.09613(18) 0.0354(15) Uani 1 1 d . . . . .
N31A N 0.3498(12) 0.0465(9) 1.0954(4) 0.0567(10) Uani 0.724(6) 1 d . . P A 1
N50 N 0.3623(5) 0.2822(4) 0.56345(16) 0.0220(11) Uani 1 1 d . . . . .
N60 N 0.1995(7) 0.0787(5) 0.40177(19) 0.0363(15) Uani 1 1 d . . . . .
N70 N 0.1106(5) 0.5108(4) 0.40460(16) 0.0225(11) Uani 1 1 d . . . . .
O1W O 0.1419(8) 0.0769(6) 0.7574(4) 0.095(4) Uani 1 1 d . . . . .
H1WA H 0.232163 0.077637 0.752699 0.143 Uiso 1 1 d GR . . . .
H1WB H 0.133008 0.018572 0.747103 0.143 Uiso 1 1 d GR . . . .
O2W O -0.0568(12) 0.0983(6) 0.7077(3) 0.095(4) Uani 1 1 d . . . . .
H2WA H -0.157454 0.089317 0.703406 0.143 Uiso 1 1 d GR . . . .
H2WB H -0.034169 0.029816 0.716795 0.143 Uiso 1 1 d GR . . . .
O3W O 0.0532(6) 0.3879(4) 0.74573(17) 0.0436(13) Uani 1 1 d . . . . .
H3WA H -0.006473 0.443571 0.749090 0.065 Uiso 1 1 d GR . . . .
H3WB H 0.139869 0.413251 0.739176 0.065 Uiso 1 1 d GR . . . .
O4W O 0.4075(7) 0.0872(5) 0.7684(2) 0.0559(17) Uani 1 1 d . . . . .
H4WA H 0.371390 0.079663 0.797494 0.084 Uiso 1 1 d DGR . . . .
H4WB H 0.469196 0.025932 0.767586 0.084 Uiso 1 1 d GR . . . .
O5W O 0.4147(6) 0.3983(4) 0.74968(16) 0.0416(13) Uani 1 1 d . . . . .
H5WA H 0.350426 0.423161 0.766127 0.062 Uiso 1 1 d GR . . . .
H5WB H 0.434369 0.445754 0.732950 0.062 Uiso 1 1 d GR . . . .
O18 O 0.3772(5) 0.2578(4) 0.80980(14) 0.0293(10) Uani 1 1 d . . . . .
O19 O 0.1662(5) 0.2454(4) 0.79603(14) 0.0341(12) Uani 1 1 d . . . . .
O28 O 0.1361(5) 0.6841(5) 1.19888(15) 0.0427(14) Uani 1 1 d . . . . .
O29 O 0.3474(6) 0.6680(6) 1.21770(19) 0.057(2) Uani 1 1 d . . . . .
O38A O 0.1150(7) -0.1133(5) 1.2078(2) 0.0567(10) Uani 0.724(6) 1 d . . P A 1
O38B O 0.143(2) 0.0213(16) 1.2423(6) 0.0567(10) Uani 0.276(6) 1 d D . P A 2
O39A O 0.3267(9) -0.1445(7) 1.2159(3) 0.0567(10) Uani 0.724(6) 1 d . . P A 1
O39B O 0.1150(7) -0.1133(5) 1.2078(2) 0.0567(10) Uani 0.276(6) 1 d D . P A 2
O57 O 0.3456(6) 0.2344(4) 0.70703(15) 0.0389(13) Uani 1 1 d . . . . .
O58 O 0.1339(5) 0.2386(4) 0.69336(15) 0.0329(11) Uani 1 1 d . . . . .
O67 O 0.4516(10) 0.0258(6) 0.2742(3) 0.082(3) Uani 1 1 d . . . . .
O68 O 0.3987(7) -0.1209(4) 0.29542(18) 0.0504(16) Uani 1 1 d . . . . .
O77 O 0.3735(5) 0.6774(4) 0.30161(14) 0.0285(10) Uani 1 1 d . . . . .
O78 O 0.1647(5) 0.7123(5) 0.28644(15) 0.0399(13) Uani 1 1 d . . . . .
Sm1 Sm -0.00123(3) 0.22295(3) 0.75235(2) 0.02395(11) Uani 1 1 d . . . . .
Sm2 Sm 0.51381(3) 0.23715(3) 0.75035(2) 0.02251(11) Uani 1 1 d . . . . .
Br1C Br 0.3085(16) 0.0035(11) 0.8767(5) 0.076(4) Uani 0.1 1 d . . P B 3
C107 C -0.3307(15) 0.1720(10) 0.9830(3) 0.074(4) Uani 1 1 d . . . . .
F108 F -0.2220(11) 0.1227(7) 0.9693(3) 0.111(3) Uani 1 1 d . . . . .
F109 F -0.4346(12) 0.1178(6) 0.9839(3) 0.120(4) Uani 1 1 d . . . . .
F110 F -0.3163(11) 0.1934(7) 1.0190(2) 0.105(3) Uani 1 1 d . . . . .
O104 O -0.2359(7) 0.3204(6) 0.9520(3) 0.078(3) Uani 1 1 d . . . . .
O105 O -0.3844(10) 0.2304(8) 0.9161(2) 0.086(3) Uani 1 1 d . . . . .
O106 O -0.4666(6) 0.3272(5) 0.9697(2) 0.0535(16) Uani 1 1 d . . . . .
S103 S -0.35823(19) 0.27471(17) 0.95132(6) 0.0419(4) Uani 1 1 d . . . . .
C13A C 0.163(3) -0.0129(19) 0.9042(7) 0.097(3) Uani 0.65 1 d . . P C 1
F14A F 0.2753(15) 0.0074(10) 0.9310(4) 0.097(3) Uani 0.65 1 d . . P C 1
F16A F 0.1213(18) -0.0773(11) 0.9214(4) 0.097(3) Uani 0.65 1 d . . P C 1
F15A F 0.0931(15) 0.0656(10) 0.9085(4) 0.097(3) Uani 0.65 1 d . . P C 1
O10A O 0.3504(16) -0.1019(11) 0.8626(5) 0.076(4) Uani 0.65 1 d . . P C 1
O12A O 0.1260(17) -0.0466(15) 0.8379(7) 0.118(7) Uani 0.65 1 d . . P C 1
O11A O 0.3029(11) 0.0612(7) 0.8462(3) 0.054(3) Uani 0.65 1 d D . P C 1
S9A S 0.2477(6) -0.0270(3) 0.85834(15) 0.0591(10) Uani 0.65 1 d . . P C 1
C99 C 0.0823(12) 0.6798(9) 0.9044(4) 0.066(3) Uani 1 1 d . . . . .
F100 F 0.0976(10) 0.7099(6) 0.9388(3) 0.100(3) Uani 1 1 d . . . . .
F101 F 0.1636(9) 0.7233(6) 0.8792(3) 0.100(3) Uani 1 1 d . . . . .
F102 F -0.0439(8) 0.7044(7) 0.8967(3) 0.107(3) Uani 1 1 d . . . . .
O96 O 0.2473(7) 0.5404(6) 0.9099(2) 0.064(2) Uani 1 1 d . . . . .
O97 O 0.0788(9) 0.5374(8) 0.8619(3) 0.085(3) Uani 1 1 d . . . . .
O98 O 0.0185(6) 0.5172(5) 0.9305(2) 0.0577(18) Uani 1 1 d . . . . .
S95 S 0.1107(2) 0.55256(16) 0.90151(7) 0.0428(5) Uani 1 1 d . . . . .
C5B C 0.302(5) -0.016(3) 0.5958(15) 0.086(2) Uani 0.403(7) 1 d . . P D 2
F8B F 0.362(3) -0.0907(17) 0.5828(7) 0.086(2) Uani 0.403(7) 1 d . . P D 2
F6B F 0.212(3) 0.0267(15) 0.5732(7) 0.086(2) Uani 0.403(7) 1 d . . P D 2
F7B F 0.380(4) 0.056(3) 0.5932(14) 0.086(2) Uani 0.403(7) 1 d . . P D 2
O4B O 0.316(3) -0.0872(17) 0.6646(7) 0.088(5) Uani 0.403(7) 1 d . . P D 2
O3B O 0.189(4) 0.042(3) 0.6607(10) 0.088(5) Uani 0.403(7) 1 d . . P D 2
O2B O 0.108(4) -0.103(3) 0.6360(9) 0.088(5) Uani 0.403(7) 1 d . . P D 2
S1B S 0.2098(9) -0.0381(4) 0.64438(17) 0.063(2) Uani 0.403(7) 1 d . . P D 2
C5A C 0.347(3) -0.029(2) 0.5999(10) 0.086(2) Uani 0.597(7) 1 d . . P D 1
F7A F 0.4040(15) -0.0814(9) 0.6257(4) 0.086(2) Uani 0.597(7) 1 d . . P D 1
F8A F 0.4120(16) 0.0460(13) 0.5974(8) 0.072(5) Uani 0.597(7) 1 d . . P D 1
F6A F 0.3545(18) -0.0758(11) 0.5657(5) 0.086(2) Uani 0.597(7) 1 d . . P D 1
O4A O 0.169(2) 0.0504(12) 0.6463(4) 0.061(4) Uani 0.597(7) 1 d . . P D 1
O2A O 0.1300(14) 0.0481(10) 0.5783(4) 0.063(3) Uani 0.597(7) 1 d . . P D 1
O3A O 0.1220(15) -0.0957(10) 0.6181(5) 0.061(4) Uani 0.597(7) 1 d . . P D 1
S1A S 0.1725(4) -0.0034(3) 0.61168(12) 0.0454(10) Uani 0.597(7) 1 d . . P D 1
C13B C 0.066(6) -0.046(5) 0.9110(15) 0.071(4) Uani 0.25 1 d . . P E 2
F14B F 0.012(3) -0.099(2) 0.8980(8) 0.071(4) Uani 0.25 1 d . . P E 2
F16B F 0.143(3) -0.075(2) 0.9417(9) 0.071(4) Uani 0.25 1 d . . P E 2
F15B F 0.004(3) 0.028(2) 0.9229(8) 0.071(4) Uani 0.25 1 d . . P E 2
O12B O 0.294(4) -0.086(3) 0.8695(14) 0.076(4) Uani 0.25 1 d . . P E 2
O10B O 0.118(4) 0.039(2) 0.8472(9) 0.064(8) Uani 0.25 1 d . . P E 2
O11B O 0.283(7) 0.065(3) 0.9053(13) 0.13(2) Uani 0.25 1 d . . P E 2
S9B S 0.2029(12) 0.0030(8) 0.8776(4) 0.058(3) Uani 0.25 1 d . . P E 2
C83 C 0.8389(9) 0.1664(6) 0.5154(2) 0.0401(18) Uani 1 1 d . . . . .
F84 F 0.9445(7) 0.1063(4) 0.51680(16) 0.0589(15) Uani 1 1 d . . . . .
F85 F 0.8336(6) 0.1949(4) 0.47845(15) 0.0559(14) Uani 1 1 d . . . . .
F86 F 0.7323(7) 0.1178(4) 0.52532(18) 0.0617(16) Uani 1 1 d . . . . .
O80 O 0.9636(5) 0.3129(4) 0.53329(18) 0.0376(12) Uani 1 1 d . . . . .
O81 O 0.7263(5) 0.3145(4) 0.54419(19) 0.0422(13) Uani 1 1 d . . . . .
O82 O 0.8654(8) 0.2186(5) 0.58580(17) 0.0511(16) Uani 1 1 d . . . . .
S79 S 0.85081(18) 0.26437(12) 0.54859(5) 0.0299(3) Uani 1 1 d . . . . .
C91 C 0.4059(10) 0.6715(7) 0.5886(3) 0.050(2) Uani 1 1 d . . . . .
F92 F 0.5312(6) 0.6937(5) 0.5944(2) 0.0691(18) Uani 1 1 d . . . . .
F93 F 0.3807(7) 0.6917(6) 0.5521(2) 0.077(2) Uani 1 1 d . . . . .
F94 F 0.3267(7) 0.7236(5) 0.6122(2) 0.0737(19) Uani 1 1 d . . . . .
O88 O 0.4786(6) 0.5005(5) 0.5717(2) 0.0459(15) Uani 1 1 d . . . . .
O89 O 0.2488(5) 0.5340(4) 0.59348(17) 0.0394(13) Uani 1 1 d . . . . .
O90 O 0.4210(7) 0.5380(6) 0.6397(2) 0.0556(17) Uani 1 1 d . . . . .
S87 S 0.38646(17) 0.54675(14) 0.59914(6) 0.0336(4) Uani 1 1 d . . . . .
O6WB O 0.012(3) 0.0876(14) 1.2622(7) 0.071(5) Uani 0.375 1 d . . P F 4
O6WA O 0.131(3) 0.0802(14) 1.2580(7) 0.071(5) Uani 0.375 1 d . . P G 3


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.417(11) . ?
C1 C6 1.400(12) . ?
C1 C10 1.483(10) . ?
C2 C3 1.406(11) . ?
C2 C7 1.507(12) . ?
C3 C4 1.400(13) . ?
C3 C20 1.514(12) . ?
C4 C5 1.403(15) . ?
C4 C8 1.498(12) . ?
C5 C6 1.395(13) . ?
C5 C30 1.495(14) . ?
C6 C9 1.514(14) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 N11 1.513(8) . ?
C12 H12 0.9500 . ?
C12 C13 1.385(10) . ?
C12 N11 1.342(9) . ?
C13 H13 0.9500 . ?
C13 C14 1.384(10) . ?
C14 C15 1.377(10) . ?
C14 C17 1.523(9) . ?
C15 H15 0.9500 . ?
C15 C16 1.383(10) . ?
C16 H16 0.9500 . ?
C16 N11 1.329(9) . ?
C17 O18 1.255(9) . ?
C17 O19 1.240(9) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 N21 1.484(9) . ?
C22 H22 0.9500 . ?
C22 C23 1.379(12) . ?
C22 N21 1.364(11) . ?
C23 H23 0.9500 . ?
C23 C24 1.359(11) . ?
C24 C25 1.386(10) . ?
C24 C27 1.523(10) . ?
C25 H25 0.9500 . ?
C25 C26 1.371(11) . ?
C26 H26 0.9500 . ?
C26 N21 1.335(10) . ?
C27 O28 1.226(10) . ?
C27 O29 1.272(10) . ?
C30 N31B 1.684(17) . ?
C30 N31A 1.476(14) . ?
C32A H32A 0.9500 . ?
C32A C33A 1.434(16) . ?
C32A N31A 1.310(17) . ?
C33A H33A 0.9500 . ?
C33A C34A 1.366(17) . ?
C34A C35A 1.352(17) . ?
C34A C37A 1.518(15) . ?
C35A H35A 0.9500 . ?
C35A C36A 1.375(17) . ?
C35B H35B 0.9500 . ?
C35B C36B 1.3900 . ?
C35B C34B 1.3900 . ?
C36B H36B 0.9500 . ?
C36B N31B 1.3900 . ?
N31B C32B 1.3900 . ?
C32B H32B 0.9500 . ?
C32B C33B 1.3900 . ?
C33B H33B 0.9500 . ?
C33B C34B 1.3900 . ?
C34B C37B 1.536(17) . ?
C36A H36A 0.9500 . ?
C36A N31A 1.281(17) . ?
C37A O38A 1.244(15) . ?
C37A O39A 1.240(17) . ?
C37B O38B 1.262(18) . ?
C37B O39B 1.261(18) . ?
C40 C41 1.410(10) . ?
C40 C45 1.407(10) . ?
C40 C49 1.505(10) . ?
C41 C42 1.392(11) . ?
C41 C46 1.520(10) . ?
C42 C43 1.391(11) . ?
C42 C59 1.521(10) . ?
C43 C44 1.401(10) . ?
C43 C47 1.529(10) . ?
C44 C45 1.392(10) . ?
C44 C69 1.517(9) . ?
C45 C48 1.504(10) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C49 N50 1.509(8) . ?
C51 H51 0.9500 . ?
C51 C52 1.391(9) . ?
C51 N50 1.343(9) . ?
C52 H52 0.9500 . ?
C52 C53 1.377(9) . ?
C53 C54 1.392(9) . ?
C53 C56 1.516(8) . ?
C54 H54 0.9500 . ?
C54 C55 1.390(9) . ?
C55 H55 0.9500 . ?
C55 N50 1.341(8) . ?
C56 O57 1.250(9) . ?
C56 O58 1.248(9) . ?
C59 H59A 0.9900 . ?
C59 H59B 0.9900 . ?
C59 N60 1.510(10) . ?
C61 H61 0.9500 . ?
C61 C62 1.368(14) . ?
C61 N60 1.338(12) . ?
C62 H62 0.9500 . ?
C62 C63 1.373(14) . ?
C63 C64 1.377(14) . ?
C63 C66 1.538(13) . ?
C64 H64 0.9500 . ?
C64 C65 1.366(12) . ?
C65 H65 0.9500 . ?
C65 N60 1.339(10) . ?
C66 O67 1.299(13) . ?
C66 O68 1.253(12) . ?
C69 H69A 0.9900 . ?
C69 H69B 0.9900 . ?
C69 N70 1.496(8) . ?
C71 H71 0.9500 . ?
C71 C72 1.365(10) . ?
C71 N70 1.341(9) . ?
C72 H72 0.9500 . ?
C72 C73 1.392(10) . ?
C73 C74 1.395(10) . ?
C73 C76 1.515(9) . ?
C74 H74 0.9500 . ?
C74 C75 1.373(10) . ?
C75 H75 0.9500 . ?
C75 N70 1.340(9) . ?
C76 O77 1.249(9) . ?
C76 O78 1.249(9) . ?
O1W H1WA 0.9209 . ?
O1W H1WB 0.9163 . ?
O1W Sm1 2.484(9) . ?
O2W H2WA 1.0515 . ?
O2W H2WB 1.0363 . ?
O2W Sm1 2.463(7) . ?
O3W H3WA 0.9782 . ?
O3W H3WB 0.9787 . ?
O3W Sm1 2.438(6) . ?
O4W H4WA 1.0506 . ?
O4W H4WB 1.0480 . ?
O4W Sm2 2.489(7) . ?
O5W H5WA 0.9023 . ?
O5W H5WB 0.9021 . ?
O5W Sm2 2.458(6) . ?
O18 Sm2 2.419(5) . ?
O19 Sm1 2.354(5) . ?
O28 Sm1 2.465(5) 2_567 ?
O29 Sm2 2.318(6) 2_667 ?
O38A Sm1 2.361(6) 2_557 ?
O39A Sm2 2.371(9) 2_657 ?
O39B Sm1 2.361(6) 2_557 ?
O57 Sm2 2.318(5) . ?
O58 Sm1 2.398(5) . ?
O68 Sm2 2.404(6) 2_656 ?
O77 Sm2 2.411(5) 2_666 ?
O78 Sm1 2.323(5) 2_566 ?
C107 F108 1.345(16) . ?
C107 F109 1.332(18) . ?
C107 F110 1.290(15) . ?
C107 S103 1.826(14) . ?
O104 S103 1.427(8) . ?
O105 S103 1.414(9) . ?
O106 S103 1.424(7) . ?
C13A F14A 1.53(4) . ?
C13A F16A 1.17(3) . ?
C13A F15A 1.30(3) . ?
C13A S9A 1.76(2) . ?
O10A S9A 1.464(15) . ?
O12A S9A 1.488(17) . ?
O11A S9A 1.443(10) . ?
C99 F100 1.280(15) . ?
C99 F101 1.330(13) . ?
C99 F102 1.347(15) . ?
C99 S95 1.822(13) . ?
O96 S95 1.428(7) . ?
O97 S95 1.435(9) . ?
O98 S95 1.432(8) . ?
C5B F8B 1.27(5) . ?
C5B F6B 1.35(5) . ?
C5B F7B 1.32(7) . ?
C5B S1B 1.90(6) . ?
O4B S1B 1.46(3) . ?
O3B S1B 1.28(4) . ?
O2B S1B 1.46(4) . ?
C5A F7A 1.29(3) . ?
C5A F8A 1.28(4) . ?
C5A F6A 1.36(4) . ?
C5A S1A 1.82(3) . ?
O4A S1A 1.419(18) . ?
O2A S1A 1.425(13) . ?
O3A S1A 1.441(14) . ?
C13B F14B 1.05(7) . ?
C13B F16B 1.39(5) . ?
C13B F15B 1.26(7) . ?
C13B S9B 1.91(6) . ?
O12B S9B 1.55(4) . ?
O10B S9B 1.46(3) . ?
O11B S9B 1.58(4) . ?
C83 F84 1.339(11) . ?
C83 F85 1.326(10) . ?
C83 F86 1.336(11) . ?
C83 S79 1.825(8) . ?
O80 S79 1.435(6) . ?
O81 S79 1.432(6) . ?
O82 S79 1.435(6) . ?
C91 F92 1.347(12) . ?
C91 F93 1.315(13) . ?
C91 F94 1.321(12) . ?
C91 S87 1.823(10) . ?
O88 S87 1.436(6) . ?
O89 S87 1.438(5) . ?
O90 S87 1.453(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C10 119.2(7) . . ?
C6 C1 C2 119.9(7) . . ?
C6 C1 C10 120.9(8) . . ?
C1 C2 C7 120.8(7) . . ?
C3 C2 C1 118.7(7) . . ?
C3 C2 C7 120.4(7) . . ?
C2 C3 C20 119.6(8) . . ?
C4 C3 C2 121.2(8) . . ?
C4 C3 C20 119.0(7) . . ?
C3 C4 C5 119.2(7) . . ?
C3 C4 C8 119.5(10) . . ?
C5 C4 C8 121.2(10) . . ?
C4 C5 C30 118.8(9) . . ?
C6 C5 C4 120.1(9) . . ?
C6 C5 C30 120.6(10) . . ?
C1 C6 C9 118.3(8) . . ?
C5 C6 C1 120.6(8) . . ?
C5 C6 C9 121.0(9) . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C4 C8 H8A 109.5 . . ?
C4 C8 H8B 109.5 . . ?
C4 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C1 C10 H10A 108.5 . . ?
C1 C10 H10B 108.5 . . ?
C1 C10 N11 115.0(6) . . ?
H10A C10 H10B 107.5 . . ?
N11 C10 H10A 108.5 . . ?
N11 C10 H10B 108.5 . . ?
C13 C12 H12 120.3 . . ?
N11 C12 H12 120.3 . . ?
N11 C12 C13 119.4(6) . . ?
C12 C13 H13 119.9 . . ?
C14 C13 C12 120.1(6) . . ?
C14 C13 H13 119.9 . . ?
C13 C14 C17 120.6(6) . . ?
C15 C14 C13 118.7(6) . . ?
C15 C14 C17 120.7(6) . . ?
C14 C15 H15 120.3 . . ?
C14 C15 C16 119.4(6) . . ?
C16 C15 H15 120.3 . . ?
C15 C16 H16 119.6 . . ?
N11 C16 C15 120.8(6) . . ?
N11 C16 H16 119.6 . . ?
O18 C17 C14 117.2(6) . . ?
O19 C17 C14 116.5(6) . . ?
O19 C17 O18 126.3(6) . . ?
C3 C20 H20A 108.8 . . ?
C3 C20 H20B 108.8 . . ?
H20A C20 H20B 107.7 . . ?
N21 C20 C3 114.0(7) . . ?
N21 C20 H20A 108.8 . . ?
N21 C20 H20B 108.8 . . ?
C23 C22 H22 119.8 . . ?
N21 C22 H22 119.8 . . ?
N21 C22 C23 120.3(7) . . ?
C22 C23 H23 119.9 . . ?
C24 C23 C22 120.3(7) . . ?
C24 C23 H23 119.9 . . ?
C23 C24 C25 118.9(7) . . ?
C23 C24 C27 122.0(7) . . ?
C25 C24 C27 119.0(7) . . ?
C24 C25 H25 120.4 . . ?
C26 C25 C24 119.2(7) . . ?
C26 C25 H25 120.4 . . ?
C25 C26 H26 119.1 . . ?
N21 C26 C25 121.9(7) . . ?
N21 C26 H26 119.1 . . ?
O28 C27 C24 118.1(7) . . ?
O28 C27 O29 130.3(7) . . ?
O29 C27 C24 111.3(7) . . ?
C5 C30 N31B 103.5(10) . . ?
N31A C30 C5 121.9(10) . . ?
C33A C32A H32A 120.3 . . ?
N31A C32A H32A 120.3 . . ?
N31A C32A C33A 119.5(12) . . ?
C32A C33A H33A 120.7 . . ?
C34A C33A C32A 118.6(12) . . ?
C34A C33A H33A 120.7 . . ?
C33A C34A C37A 121.7(11) . . ?
C35A C34A C33A 117.6(11) . . ?
C35A C34A C37A 120.2(10) . . ?
C34A C35A H35A 120.0 . . ?
C34A C35A C36A 120.0(12) . . ?
C36A C35A H35A 120.0 . . ?
C36B C35B H35B 120.0 . . ?
C36B C35B C34B 120.0 . . ?
C34B C35B H35B 120.0 . . ?
C35B C36B H36B 120.0 . . ?
N31B C36B C35B 120.0 . . ?
N31B C36B H36B 120.0 . . ?
C36B N31B C30 112.5(13) . . ?
C32B N31B C30 127.4(13) . . ?
C32B N31B C36B 120.0 . . ?
N31B C32B H32B 120.0 . . ?
C33B C32B N31B 120.0 . . ?
C33B C32B H32B 120.0 . . ?
C32B C33B H33B 120.0 . . ?
C32B C33B C34B 120.0 . . ?
C34B C33B H33B 120.0 . . ?
C35B C34B C37B 117.0(16) . . ?
C33B C34B C35B 120.0 . . ?
C33B C34B C37B 122.9(16) . . ?
C35A C36A H36A 118.8 . . ?
N31A C36A C35A 122.3(12) . . ?
N31A C36A H36A 118.8 . . ?
O38A C37A C34A 119.1(11) . . ?
O39A C37A C34A 116.2(11) . . ?
O39A C37A O38A 124.7(11) . . ?
O38B C37B C34B 116.3(19) . . ?
O39B C37B C34B 110.9(18) . . ?
O39B C37B O38B 132(2) . . ?
C41 C40 C49 120.9(7) . . ?
C45 C40 C41 120.4(6) . . ?
C45 C40 C49 118.7(6) . . ?
C40 C41 C46 120.5(7) . . ?
C42 C41 C40 119.4(7) . . ?
C42 C41 C46 120.1(7) . . ?
C41 C42 C59 119.5(7) . . ?
C43 C42 C41 120.8(7) . . ?
C43 C42 C59 119.5(7) . . ?
C42 C43 C44 119.3(6) . . ?
C42 C43 C47 120.8(7) . . ?
C44 C43 C47 119.9(7) . . ?
C43 C44 C69 117.2(6) . . ?
C45 C44 C43 121.3(6) . . ?
C45 C44 C69 121.4(6) . . ?
C40 C45 C48 119.7(6) . . ?
C44 C45 C40 118.8(6) . . ?
C44 C45 C48 121.5(6) . . ?
C41 C46 H46A 109.5 . . ?
C41 C46 H46B 109.5 . . ?
C41 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C43 C47 H47A 109.5 . . ?
C43 C47 H47B 109.5 . . ?
C43 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C45 C48 H48A 109.5 . . ?
C45 C48 H48B 109.5 . . ?
C45 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C40 C49 H49A 108.8 . . ?
C40 C49 H49B 108.8 . . ?
C40 C49 N50 113.9(6) . . ?
H49A C49 H49B 107.7 . . ?
N50 C49 H49A 108.8 . . ?
N50 C49 H49B 108.8 . . ?
C52 C51 H51 119.9 . . ?
N50 C51 H51 119.9 . . ?
N50 C51 C52 120.3(6) . . ?
C51 C52 H52 120.4 . . ?
C53 C52 C51 119.2(6) . . ?
C53 C52 H52 120.4 . . ?
C52 C53 C54 119.8(6) . . ?
C52 C53 C56 120.5(6) . . ?
C54 C53 C56 119.7(6) . . ?
C53 C54 H54 120.6 . . ?
C55 C54 C53 118.9(6) . . ?
C55 C54 H54 120.6 . . ?
C54 C55 H55 119.8 . . ?
N50 C55 C54 120.4(6) . . ?
N50 C55 H55 119.8 . . ?
O57 C56 C53 117.6(6) . . ?
O58 C56 C53 117.5(6) . . ?
O58 C56 O57 124.9(6) . . ?
C42 C59 H59A 109.0 . . ?
C42 C59 H59B 109.0 . . ?
H59A C59 H59B 107.8 . . ?
N60 C59 C42 113.0(7) . . ?
N60 C59 H59A 109.0 . . ?
N60 C59 H59B 109.0 . . ?
C62 C61 H61 120.0 . . ?
N60 C61 H61 120.0 . . ?
N60 C61 C62 120.0(9) . . ?
C61 C62 H62 119.8 . . ?
C61 C62 C63 120.5(10) . . ?
C63 C62 H62 119.8 . . ?
C62 C63 C64 118.4(9) . . ?
C62 C63 C66 120.3(9) . . ?
C64 C63 C66 121.4(8) . . ?
C63 C64 H64 120.2 . . ?
C65 C64 C63 119.6(8) . . ?
C65 C64 H64 120.2 . . ?
C64 C65 H65 119.5 . . ?
N60 C65 C64 120.9(8) . . ?
N60 C65 H65 119.5 . . ?
O67 C66 C63 117.6(9) . . ?
O68 C66 C63 115.3(8) . . ?
O68 C66 O67 126.3(9) . . ?
C44 C69 H69A 108.7 . . ?
C44 C69 H69B 108.7 . . ?
H69A C69 H69B 107.6 . . ?
N70 C69 C44 114.0(5) . . ?
N70 C69 H69A 108.7 . . ?
N70 C69 H69B 108.7 . . ?
C72 C71 H71 119.4 . . ?
N70 C71 H71 119.4 . . ?
N70 C71 C72 121.2(6) . . ?
C71 C72 H72 120.0 . . ?
C71 C72 C73 119.9(6) . . ?
C73 C72 H72 120.0 . . ?
C72 C73 C74 117.8(6) . . ?
C72 C73 C76 121.0(6) . . ?
C74 C73 C76 121.2(6) . . ?
C73 C74 H74 120.2 . . ?
C75 C74 C73 119.7(7) . . ?
C75 C74 H74 120.2 . . ?
C74 C75 H75 119.5 . . ?
N70 C75 C74 121.0(6) . . ?
N70 C75 H75 119.5 . . ?
O77 C76 C73 116.9(6) . . ?
O77 C76 O78 126.9(7) . . ?
O78 C76 C73 116.2(6) . . ?
C12 N11 C10 121.0(6) . . ?
C16 N11 C10 117.4(6) . . ?
C16 N11 C12 121.6(6) . . ?
C22 N21 C20 121.3(7) . . ?
C26 N21 C20 118.9(6) . . ?
C26 N21 C22 119.3(7) . . ?
C32A N31A C30 119.1(11) . . ?
C36A N31A C30 120.0(11) . . ?
C36A N31A C32A 120.9(12) . . ?
C51 N50 C49 122.7(6) . . ?
C55 N50 C49 115.8(5) . . ?
C55 N50 C51 121.5(6) . . ?
C61 N60 C59 122.1(7) . . ?
C61 N60 C65 120.5(8) . . ?
C65 N60 C59 117.2(7) . . ?
C71 N70 C69 120.7(6) . . ?
C75 N70 C69 118.8(6) . . ?
C75 N70 C71 120.3(6) . . ?
H1WA O1W H1WB 95.7 . . ?
Sm1 O1W H1WA 121.3 . . ?
Sm1 O1W H1WB 130.1 . . ?
H2WA O2W H2WB 96.6 . . ?
Sm1 O2W H2WA 117.7 . . ?
Sm1 O2W H2WB 115.9 . . ?
H3WA O3W H3WB 104.4 . . ?
Sm1 O3W H3WA 127.8 . . ?
Sm1 O3W H3WB 127.8 . . ?
H4WA O4W H4WB 96.9 . . ?
Sm2 O4W H4WA 116.9 . . ?
Sm2 O4W H4WB 116.5 . . ?
H5WA O5W H5WB 104.6 . . ?
Sm2 O5W H5WA 127.7 . . ?
Sm2 O5W H5WB 127.7 . . ?
C17 O18 Sm2 135.3(4) . . ?
C17 O19 Sm1 179.0(5) . . ?
C27 O28 Sm1 134.6(5) . 2_567 ?
C27 O29 Sm2 150.3(8) . 2_667 ?
C37A O38A Sm1 132.2(7) . 2_557 ?
C37A O39A Sm2 171.7(11) . 2_657 ?
C56 O57 Sm2 175.1(5) . . ?
C56 O58 Sm1 137.5(5) . . ?
C66 O68 Sm2 137.2(6) . 2_656 ?
C76 O77 Sm2 125.5(4) . 2_666 ?
C76 O78 Sm1 176.0(6) . 2_566 ?
O2W Sm1 O1W 66.3(3) . . ?
O2W Sm1 O28 132.2(3) . 2_567 ?
O3W Sm1 O1W 131.3(2) . . ?
O3W Sm1 O2W 135.9(2) . . ?
O3W Sm1 O28 70.9(2) . 2_567 ?
O19 Sm1 O1W 70.1(3) . . ?
O19 Sm1 O2W 136.2(3) . . ?
O19 Sm1 O3W 73.7(2) . . ?
O19 Sm1 O28 82.33(18) . 2_567 ?
O19 Sm1 O38A 95.6(2) . 2_557 ?
O19 Sm1 O58 96.88(18) . . ?
O28 Sm1 O1W 132.7(3) 2_567 . ?
O38A Sm1 O1W 71.6(3) 2_557 . ?
O38A Sm1 O2W 75.0(3) 2_557 . ?
O38A Sm1 O3W 144.1(2) 2_557 . ?
O38A Sm1 O28 73.8(2) 2_557 2_567 ?
O38A Sm1 O58 143.3(2) 2_557 . ?
O58 Sm1 O1W 80.5(3) . . ?
O58 Sm1 O2W 72.1(3) . . ?
O58 Sm1 O3W 72.6(2) . . ?
O58 Sm1 O28 142.2(2) . 2_567 ?
O78 Sm1 O1W 139.4(3) 2_566 . ?
O78 Sm1 O2W 73.4(3) 2_566 . ?
O78 Sm1 O3W 76.5(2) 2_566 . ?
O78 Sm1 O19 148.9(2) 2_566 . ?
O78 Sm1 O28 79.6(2) 2_566 2_567 ?
O78 Sm1 O38A 103.3(2) 2_566 2_557 ?
O78 Sm1 O58 82.60(18) 2_566 . ?
O5W Sm2 O4W 128.9(2) . . ?
O18 Sm2 O4W 70.3(2) . . ?
O18 Sm2 O5W 72.16(18) . . ?
O29 Sm2 O4W 133.3(3) 2_667 . ?
O29 Sm2 O5W 72.4(3) 2_667 . ?
O29 Sm2 O18 82.50(18) 2_667 . ?
O29 Sm2 O39A 69.2(4) 2_667 2_657 ?
O29 Sm2 O57 145.3(3) 2_667 . ?
O29 Sm2 O68 121.1(2) 2_667 2_656 ?
O29 Sm2 O77 75.9(2) 2_667 2_666 ?
O39A Sm2 O4W 74.0(3) 2_657 . ?
O39A Sm2 O5W 139.8(3) 2_657 . ?
O39A Sm2 O18 91.1(2) 2_657 . ?
O39A Sm2 O68 74.3(3) 2_657 2_656 ?
O39A Sm2 O77 108.5(2) 2_657 2_666 ?
O57 Sm2 O4W 77.5(2) . . ?
O57 Sm2 O5W 74.7(2) . . ?
O57 Sm2 O18 98.03(19) . . ?
O57 Sm2 O39A 145.1(3) . 2_657 ?
O57 Sm2 O68 78.4(2) . 2_656 ?
O57 Sm2 O77 83.85(17) . 2_666 ?
O68 Sm2 O4W 73.1(2) 2_656 . ?
O68 Sm2 O5W 138.7(2) 2_656 . ?
O68 Sm2 O18 143.1(2) 2_656 . ?
O68 Sm2 O77 73.9(2) 2_656 2_666 ?
O77 Sm2 O4W 144.7(2) 2_666 . ?
O77 Sm2 O5W 72.64(18) 2_666 . ?
O77 Sm2 O18 142.84(18) 2_666 . ?
F108 C107 S103 108.6(9) . . ?
F109 C107 F108 109.7(12) . . ?
F109 C107 S103 110.6(11) . . ?
F110 C107 F108 109.2(13) . . ?
F110 C107 F109 105.2(12) . . ?
F110 C107 S103 113.4(10) . . ?
O104 S103 C107 102.8(7) . . ?
O105 S103 C107 100.6(6) . . ?
O105 S103 O104 116.5(6) . . ?
O105 S103 O106 115.9(5) . . ?
O106 S103 C107 105.1(5) . . ?
O106 S103 O104 113.4(5) . . ?
F14A C13A S9A 102.8(17) . . ?
F16A C13A F14A 98(2) . . ?
F16A C13A F15A 115(2) . . ?
F16A C13A S9A 121(2) . . ?
F15A C13A F14A 99(2) . . ?
F15A C13A S9A 115.1(17) . . ?
O10A S9A C13A 107.3(11) . . ?
O10A S9A O12A 119.5(12) . . ?
O12A S9A C13A 94.1(15) . . ?
O11A S9A C13A 109.1(11) . . ?
O11A S9A O10A 111.9(9) . . ?
O11A S9A O12A 112.8(11) . . ?
F100 C99 F101 109.2(11) . . ?
F100 C99 F102 105.4(11) . . ?
F100 C99 S95 111.9(9) . . ?
F101 C99 F102 109.3(11) . . ?
F101 C99 S95 110.6(9) . . ?
F102 C99 S95 110.3(9) . . ?
O96 S95 C99 102.3(6) . . ?
O96 S95 O97 116.3(5) . . ?
O96 S95 O98 115.9(5) . . ?
O97 S95 C99 100.5(6) . . ?
O98 S95 C99 103.5(5) . . ?
O98 S95 O97 115.0(5) . . ?
F8B C5B F6B 117(4) . . ?
F8B C5B F7B 111(4) . . ?
F8B C5B S1B 112(3) . . ?
F6B C5B S1B 105(3) . . ?
F7B C5B F6B 93(4) . . ?
F7B C5B S1B 118(4) . . ?
O4B S1B C5B 98.6(17) . . ?
O3B S1B C5B 107(2) . . ?
O3B S1B O4B 106.7(19) . . ?
O3B S1B O2B 125(3) . . ?
O2B S1B C5B 105(2) . . ?
O2B S1B O4B 110.6(18) . . ?
F7A C5A F6A 108(2) . . ?
F7A C5A S1A 113(2) . . ?
F8A C5A F7A 106(2) . . ?
F8A C5A F6A 111(3) . . ?
F8A C5A S1A 112(2) . . ?
F6A C5A S1A 106(2) . . ?
O4A S1A C5A 104.9(14) . . ?
O4A S1A O2A 114.1(9) . . ?
O4A S1A O3A 112.8(10) . . ?
O2A S1A C5A 103.2(12) . . ?
O2A S1A O3A 117.1(9) . . ?
O3A S1A C5A 102.7(13) . . ?
F14B C13B F16B 117(6) . . ?
F14B C13B F15B 119(6) . . ?
F14B C13B S9B 114(5) . . ?
F16B C13B S9B 98(4) . . ?
F15B C13B F16B 104(5) . . ?
F15B C13B S9B 102(4) . . ?
O12B S9B C13B 102(3) . . ?
O12B S9B O11B 105(3) . . ?
O10B S9B C13B 97(2) . . ?
O10B S9B O12B 119(3) . . ?
O10B S9B O11B 126(3) . . ?
O11B S9B C13B 105(3) . . ?
F84 C83 S79 111.4(6) . . ?
F85 C83 F84 106.2(7) . . ?
F85 C83 F86 109.4(7) . . ?
F85 C83 S79 112.3(6) . . ?
F86 C83 F84 107.1(7) . . ?
F86 C83 S79 110.2(6) . . ?
O80 S79 C83 104.2(4) . . ?
O80 S79 O82 115.6(4) . . ?
O81 S79 C83 101.6(4) . . ?
O81 S79 O80 114.6(3) . . ?
O81 S79 O82 115.0(4) . . ?
O82 S79 C83 103.4(4) . . ?
F92 C91 S87 109.7(7) . . ?
F93 C91 F92 108.4(9) . . ?
F93 C91 F94 109.7(9) . . ?
F93 C91 S87 110.8(7) . . ?
F94 C91 F92 107.7(8) . . ?
F94 C91 S87 110.5(7) . . ?
O88 S87 C91 103.7(4) . . ?
O88 S87 O89 115.9(4) . . ?
O88 S87 O90 115.0(4) . . ?
O89 S87 C91 103.8(4) . . ?
O89 S87 O90 113.6(4) . . ?
O90 S87 C91 102.7(5) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 -0.2(10) . . . . ?
C1 C2 C3 C20 175.0(6) . . . . ?
C1 C10 N11 C12 -7.7(11) . . . . ?
C1 C10 N11 C16 172.2(7) . . . . ?
C2 C1 C6 C5 -0.8(11) . . . . ?
C2 C1 C6 C9 -177.9(8) . . . . ?
C2 C1 C10 N11 93.3(8) . . . . ?
C2 C3 C4 C5 4.1(11) . . . . ?
C2 C3 C4 C8 -178.6(7) . . . . ?
C2 C3 C20 N21 99.3(9) . . . . ?
C3 C4 C5 C6 -6.4(12) . . . . ?
C3 C4 C5 C30 165.6(8) . . . . ?
C3 C20 N21 C22 -37.8(13) . . . . ?
C3 C20 N21 C26 150.3(8) . . . . ?
C4 C3 C20 N21 -85.5(10) . . . . ?
C4 C5 C6 C1 4.8(12) . . . . ?
C4 C5 C6 C9 -178.2(9) . . . . ?
C4 C5 C30 N31B 85.9(13) . . . . ?
C4 C5 C30 N31A 91.8(14) . . . . ?
C5 C30 N31B C36B 157.7(13) . . . . ?
C5 C30 N31B C32B -24.1(19) . . . . ?
C5 C30 N31A C32A 23(2) . . . . ?
C5 C30 N31A C36A -160.0(15) . . . . ?
C6 C1 C2 C3 -1.5(10) . . . . ?
C6 C1 C2 C7 174.7(7) . . . . ?
C6 C1 C10 N11 -85.7(9) . . . . ?
C6 C5 C30 N31B -102.1(13) . . . . ?
C6 C5 C30 N31A -96.2(15) . . . . ?
C7 C2 C3 C4 -176.4(7) . . . . ?
C7 C2 C3 C20 -1.3(10) . . . . ?
C8 C4 C5 C6 176.3(8) . . . . ?
C8 C4 C5 C30 -11.7(12) . . . . ?
C10 C1 C2 C3 179.5(6) . . . . ?
C10 C1 C2 C7 -4.3(10) . . . . ?
C10 C1 C6 C5 178.2(7) . . . . ?
C10 C1 C6 C9 1.1(11) . . . . ?
C12 C13 C14 C15 0.7(12) . . . . ?
C12 C13 C14 C17 179.6(7) . . . . ?
C13 C12 N11 C10 -179.2(7) . . . . ?
C13 C12 N11 C16 0.9(12) . . . . ?
C13 C14 C15 C16 -0.6(12) . . . . ?
C13 C14 C17 O18 -6.4(10) . . . . ?
C13 C14 C17 O19 173.5(7) . . . . ?
C14 C15 C16 N11 0.6(13) . . . . ?
C14 C17 O18 Sm2 176.5(4) . . . . ?
C15 C14 C17 O18 172.5(7) . . . . ?
C15 C14 C17 O19 -7.6(10) . . . . ?
C15 C16 N11 C10 179.3(7) . . . . ?
C15 C16 N11 C12 -0.8(12) . . . . ?
C17 C14 C15 C16 -179.5(7) . . . . ?
C20 C3 C4 C5 -171.0(7) . . . . ?
C20 C3 C4 C8 6.3(11) . . . . ?
C22 C23 C24 C25 -0.5(15) . . . . ?
C22 C23 C24 C27 177.8(10) . . . . ?
C23 C22 N21 C20 -172.7(10) . . . . ?
C23 C22 N21 C26 -0.9(16) . . . . ?
C23 C24 C25 C26 0.8(14) . . . . ?
C23 C24 C27 O28 -14.7(14) . . . . ?
C23 C24 C27 O29 159.6(9) . . . . ?
C24 C25 C26 N21 -1.1(14) . . . . ?
C24 C27 O28 Sm1 178.4(6) . . . 2_567 ?
C24 C27 O29 Sm2 121.8(10) . . . 2_667 ?
C25 C24 C27 O28 163.5(9) . . . . ?
C25 C24 C27 O29 -22.1(12) . . . . ?
C25 C26 N21 C20 173.2(9) . . . . ?
C25 C26 N21 C22 1.2(14) . . . . ?
C27 C24 C25 C26 -177.6(8) . . . . ?
C30 C5 C6 C1 -167.1(8) . . . . ?
C30 C5 C6 C9 9.9(13) . . . . ?
C30 N31B C32B C33B -178(2) . . . . ?
C32A C33A C34A C35A -12(2) . . . . ?
C32A C33A C34A C37A 175.6(16) . . . . ?
C33A C32A N31A C30 177.3(15) . . . . ?
C33A C32A N31A C36A 0(3) . . . . ?
C33A C34A C35A C36A 8(3) . . . . ?
C33A C34A C37A O38A 16(2) . . . . ?
C33A C34A C37A O39A -165.4(16) . . . . ?
C34A C35A C36A N31A 1(3) . . . . ?
C34A C37A O38A Sm1 158.0(9) . . . 2_557 ?
C35A C34A C37A O38A -155.4(16) . . . . ?
C35A C34A C37A O39A 23(2) . . . . ?
C35A C36A N31A C30 177.6(16) . . . . ?
C35A C36A N31A C32A -6(3) . . . . ?
C35B C36B N31B C30 178.3(19) . . . . ?
C35B C36B N31B C32B 0.0 . . . . ?
C35B C34B C37B O38B 161(2) . . . . ?
C35B C34B C37B O39B -29(3) . . . . ?
C36B C35B C34B C33B 0.0 . . . . ?
C36B C35B C34B C37B 177(3) . . . . ?
C36B N31B C32B C33B 0.0 . . . . ?
N31B C32B C33B C34B 0.0 . . . . ?
C32B C33B C34B C35B 0.0 . . . . ?
C32B C33B C34B C37B -177(3) . . . . ?
C33B C34B C37B O38B -22(4) . . . . ?
C33B C34B C37B O39B 148(2) . . . . ?
C34B C35B C36B N31B 0.0 . . . . ?
C34B C37B O39B Sm1 -177.3(12) . . . 2_557 ?
C37A C34A C35A C36A 179.9(16) . . . . ?
C40 C41 C42 C43 1.4(11) . . . . ?
C40 C41 C42 C59 -174.3(7) . . . . ?
C40 C49 N50 C51 -4.7(10) . . . . ?
C40 C49 N50 C55 176.7(6) . . . . ?
C41 C40 C45 C44 -2.0(10) . . . . ?
C41 C40 C45 C48 176.8(6) . . . . ?
C41 C40 C49 N50 -82.7(8) . . . . ?
C41 C42 C43 C44 -2.5(11) . . . . ?
C41 C42 C43 C47 176.6(7) . . . . ?
C41 C42 C59 N60 -91.1(8) . . . . ?
C42 C43 C44 C45 1.3(10) . . . . ?
C42 C43 C44 C69 -174.3(6) . . . . ?
C42 C59 N60 C61 -16.5(12) . . . . ?
C42 C59 N60 C65 167.4(7) . . . . ?
C43 C42 C59 N60 93.1(9) . . . . ?
C43 C44 C45 C40 1.0(9) . . . . ?
C43 C44 C45 C48 -177.9(6) . . . . ?
C43 C44 C69 N70 -86.9(7) . . . . ?
C44 C69 N70 C71 -40.3(9) . . . . ?
C44 C69 N70 C75 143.9(6) . . . . ?
C45 C40 C41 C42 0.8(10) . . . . ?
C45 C40 C41 C46 -178.8(7) . . . . ?
C45 C40 C49 N50 97.6(8) . . . . ?
C45 C44 C69 N70 97.6(7) . . . . ?
C46 C41 C42 C43 -178.9(7) . . . . ?
C46 C41 C42 C59 5.3(11) . . . . ?
C47 C43 C44 C45 -177.8(7) . . . . ?
C47 C43 C44 C69 6.7(10) . . . . ?
C49 C40 C41 C42 -178.9(6) . . . . ?
C49 C40 C41 C46 1.5(11) . . . . ?
C49 C40 C45 C44 177.7(6) . . . . ?
C49 C40 C45 C48 -3.5(9) . . . . ?
C51 C52 C53 C54 0.4(10) . . . . ?
C51 C52 C53 C56 178.6(6) . . . . ?
C52 C51 N50 C49 -176.9(7) . . . . ?
C52 C51 N50 C55 1.6(11) . . . . ?
C52 C53 C54 C55 0.4(11) . . . . ?
C52 C53 C56 O57 176.0(7) . . . . ?
C52 C53 C56 O58 -5.2(10) . . . . ?
C53 C54 C55 N50 -0.3(11) . . . . ?
C53 C56 O58 Sm1 -179.4(5) . . . . ?
C54 C53 C56 O57 -5.8(10) . . . . ?
C54 C53 C56 O58 173.0(7) . . . . ?
C54 C55 N50 C49 177.9(7) . . . . ?
C54 C55 N50 C51 -0.8(11) . . . . ?
C56 C53 C54 C55 -177.8(6) . . . . ?
C59 C42 C43 C44 173.3(7) . . . . ?
C59 C42 C43 C47 -7.7(11) . . . . ?
C61 C62 C63 C64 2.0(17) . . . . ?
C61 C62 C63 C66 -178.8(10) . . . . ?
C62 C61 N60 C59 -178.1(10) . . . . ?
C62 C61 N60 C65 -2.0(16) . . . . ?
C62 C63 C64 C65 0.0(14) . . . . ?
C62 C63 C66 O67 -14.7(16) . . . . ?
C62 C63 C66 O68 174.6(10) . . . . ?
C63 C64 C65 N60 -3.0(13) . . . . ?
C63 C66 O68 Sm2 -178.3(6) . . . 2_656 ?
C64 C63 C66 O67 164.5(10) . . . . ?
C64 C63 C66 O68 -6.2(15) . . . . ?
C64 C65 N60 C59 -179.7(7) . . . . ?
C64 C65 N60 C61 4.1(13) . . . . ?
C66 C63 C64 C65 -179.2(9) . . . . ?
C69 C44 C45 C40 176.3(6) . . . . ?
C69 C44 C45 C48 -2.5(9) . . . . ?
C71 C72 C73 C74 -3.9(11) . . . . ?
C71 C72 C73 C76 175.5(7) . . . . ?
C72 C71 N70 C69 -174.1(7) . . . . ?
C72 C71 N70 C75 1.6(11) . . . . ?
C72 C73 C74 C75 2.5(11) . . . . ?
C72 C73 C76 O77 0.7(10) . . . . ?
C72 C73 C76 O78 -178.2(7) . . . . ?
C73 C74 C75 N70 0.9(12) . . . . ?
C73 C76 O77 Sm2 178.1(4) . . . 2_666 ?
C74 C73 C76 O77 -180.0(7) . . . . ?
C74 C73 C76 O78 1.1(11) . . . . ?
C74 C75 N70 C69 172.7(7) . . . . ?
C74 C75 N70 C71 -3.1(11) . . . . ?
C76 C73 C74 C75 -176.9(7) . . . . ?
N11 C12 C13 C14 -0.9(12) . . . . ?
N21 C22 C23 C24 0.6(17) . . . . ?
N31A C32A C33A C34A 9(3) . . . . ?
N50 C51 C52 C53 -1.4(11) . . . . ?
N60 C61 C62 C63 -1.0(18) . . . . ?
N70 C71 C72 C73 1.9(11) . . . . ?
O19 C17 O18 Sm2 -3.4(12) . . . . ?
O28 C27 O29 Sm2 -64.7(17) . . . 2_667 ?
O29 C27 O28 Sm1 5.3(17) . . . 2_567 ?
O38B C37B O39B Sm1 -10(5) . . . 2_557 ?
O39A C37A O38A Sm1 -20(3) . . . 2_557 ?
O57 C56 O58 Sm1 -0.7(12) . . . . ?
O67 C66 O68 Sm2 12(2) . . . 2_656 ?
O78 C76 O77 Sm2 -3.2(11) . . . 2_666 ?
F108 C107 S103 O104 -56.0(11) . . . . ?
F108 C107 S103 O105 64.5(11) . . . . ?
F108 C107 S103 O106 -174.8(9) . . . . ?
F109 C107 S103 O104 -176.5(8) . . . . ?
F109 C107 S103 O105 -56.0(10) . . . . ?
F109 C107 S103 O106 64.7(9) . . . . ?
F110 C107 S103 O104 65.6(13) . . . . ?
F110 C107 S103 O105 -173.9(12) . . . . ?
F110 C107 S103 O106 -53.2(13) . . . . ?
F14A C13A S9A O10A 56.6(17) . . . . ?
F14A C13A S9A O12A 179.3(15) . . . . ?
F14A C13A S9A O11A -64.8(16) . . . . ?
F16A C13A S9A O10A -51(3) . . . . ?
F16A C13A S9A O12A 71(3) . . . . ?
F16A C13A S9A O11A -173(3) . . . . ?
F15A C13A S9A O10A 163(2) . . . . ?
F15A C13A S9A O12A -74(3) . . . . ?
F15A C13A S9A O11A 41(3) . . . . ?
F100 C99 S95 O96 -63.7(9) . . . . ?
F100 C99 S95 O97 176.2(9) . . . . ?
F100 C99 S95 O98 57.1(10) . . . . ?
F101 C99 S95 O96 58.2(11) . . . . ?
F101 C99 S95 O97 -61.9(11) . . . . ?
F101 C99 S95 O98 179.0(9) . . . . ?
F102 C99 S95 O96 179.3(8) . . . . ?
F102 C99 S95 O97 59.2(9) . . . . ?
F102 C99 S95 O98 -59.9(9) . . . . ?
F8B C5B S1B O4B 50(4) . . . . ?
F8B C5B S1B O3B 160(4) . . . . ?
F8B C5B S1B O2B -64(4) . . . . ?
F6B C5B S1B O4B 178(3) . . . . ?
F6B C5B S1B O3B -72(4) . . . . ?
F6B C5B S1B O2B 63(3) . . . . ?
F7B C5B S1B O4B -81(3) . . . . ?
F7B C5B S1B O3B 30(4) . . . . ?
F7B C5B S1B O2B 165(3) . . . . ?
F7A C5A S1A O4A 65(2) . . . . ?
F7A C5A S1A O2A -176(2) . . . . ?
F7A C5A S1A O3A -54(3) . . . . ?
F8A C5A S1A O4A -55(2) . . . . ?
F8A C5A S1A O2A 65(2) . . . . ?
F8A C5A S1A O3A -173(2) . . . . ?
F6A C5A S1A O4A -176.5(18) . . . . ?
F6A C5A S1A O2A -57(2) . . . . ?
F6A C5A S1A O3A 65(2) . . . . ?
F84 C83 S79 O80 64.5(7) . . . . ?
F84 C83 S79 O81 -176.2(6) . . . . ?
F84 C83 S79 O82 -56.8(7) . . . . ?
F85 C83 S79 O80 -54.5(7) . . . . ?
F85 C83 S79 O81 64.8(7) . . . . ?
F85 C83 S79 O82 -175.8(7) . . . . ?
F86 C83 S79 O80 -176.8(6) . . . . ?
F86 C83 S79 O81 -57.5(7) . . . . ?
F86 C83 S79 O82 61.9(7) . . . . ?
F92 C91 S87 O88 -60.9(8) . . . . ?
F92 C91 S87 O89 177.6(7) . . . . ?
F92 C91 S87 O90 59.1(8) . . . . ?
F93 C91 S87 O88 58.7(8) . . . . ?
F93 C91 S87 O89 -62.9(8) . . . . ?
F93 C91 S87 O90 178.7(7) . . . . ?
F94 C91 S87 O88 -179.5(7) . . . . ?
F94 C91 S87 O89 58.9(8) . . . . ?
F94 C91 S87 O90 -59.5(8) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.515 0.329 0.252 392.2 122.6 '12x water'
2 -0.287 0.671 0.748 392.2 127.5 '12x water'

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.384
_oxdiff_exptl_absorpt_empirical_full_min 0.718
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_jj003-01-eu-otf-h2o_red4
_database_code_depnum_ccdc_archive 'CCDC 1833445'
loop_
_audit_author_name
_audit_author_address
'Antti Tiihonen'
;University of Jyv?skyl?, Department of Chemistry
Finland
;
_audit_update_record             
;
2018-03-29 deposited with the CCDC.	2019-02-28 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_CHEMW03_I                   
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as...
RESPONSE: The structure contains voids of unresolved electron density
which was treated using Olex2 solvent mask procedure (full details in 
_smtbx_masks_special_details). The 6 water molecules per asymmetric unit 
 are included in the formula and used in the calculations. 
;
_vrf_PLAT412_I                   
;
PROBLEM: Short Intra XH3 .. XHn...
RESPONSE: Hydrogen atoms calculated using a riding model in their general
(unoptimized) geometry causing a proximity alert.
;
_vrf_PLAT420_I                   
;
PROBLEM: D-H Without Acceptor...
RESPONSE: Hydrogen bond acceptors (water) have been removed among
other disordered solvent from the voids (see CHEMW03_ALERT_2_A).
;
_vrf_PLAT973_I                   
;
PROBLEM: Check Calcd Positive Resid. Density on Eu1...
RESPONSE: Peak is located about 0.8 angstroms from the Eu1 atom
and is caused by the absorption effects. Data is recorded with Cu
radiation.
;
_vrf_FORMU01_I                   
;
PROBLEM: There is a discrepancy between the atom counts...
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_CELLZ01_I                   
;
PROBLEM: Difference between formula and atom_site...
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT041_I                   
;
PROBLEM: Calc. and Reported SumFormula Strings  Differ...
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT042_I                   
;
PROBLEM: Calc. and Reported MoietyFormula Strings  Differ...
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT051_I                   
;
PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs...
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT068_I                   
;
PROBLEM: Reported F000 Differs from Calcd (or Missing)...
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT606_I                   
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure...
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
# end Validation Reply Form
_audit_creation_date             2018-03-28
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C30 H31 Eu N3 O8, 1.55(C F3 O3 S), 1.45(Br), 0.45(O)'
_chemical_formula_sum            'C31.55 H43 Br1.45 Eu F4.64 N3 O19.10 S1.55'
_chemical_formula_weight         1175.63
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C21 H20 O6 N3 F6 Eu'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Eu Eu -8.9294 11.1857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   18.6774(6)
_cell_length_b                   25.6718(7)
_cell_length_c                   9.7560(3)
_cell_angle_alpha                90
_cell_angle_beta                 102.421(3)
_cell_angle_gamma                90
_cell_volume                     4568.3(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4818
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      76.6530
_cell_measurement_theta_min      4.1870
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    12.813
_exptl_absorpt_correction_T_max  0.866
_exptl_absorpt_correction_T_min  0.325
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.709
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2346
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 17 0 0.0720
12 -2 0 0.0098
-12 2 0 0.0041
-1 -17 -1 0.0932
2 -10 -5 0.0759
-3 6 6 0.0925
-3 -7 6 0.0811
-2 -16 1 0.0850
3 -2 -6 0.0661

_exptl_crystal_size_max          0.168
_exptl_crystal_size_mid          0.161
_exptl_crystal_size_min          0.014
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.9937 16.9986 0.0185 -0.1794 0.6112 -0.8012
12.0022 -2.0181 0.0154 -0.9855 -0.2616 0.0672
-12.0022 2.0181 -0.0154 0.9855 0.2616 -0.0672
-0.9933 -16.9984 -1.0190 0.1887 -0.4839 0.9005
2.0062 -10.0020 -5.0095 -0.0632 0.2366 0.9618
-3.0053 6.0033 6.0045 0.1597 -0.4957 -0.8709
-2.9992 -6.9995 5.9925 0.2333 -0.9754 -0.2598
-1.9947 -16.0046 0.9819 0.2476 -0.6863 0.6575
3.0024 -2.0041 -6.0016 -0.1823 0.6434 0.6830

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0598
_diffrn_reflns_av_unetI/netI     0.0870
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            14324
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.998
_diffrn_reflns_theta_min         2.972
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -117.00 -11.00   1.00   12.50    --  -41.40 -77.00-120.00  106
  2  ω    -32.00  68.00   1.00   12.50    --   41.40 -19.00  60.00  100
  3  ω     44.00  88.00   1.00   70.00    --  112.00 -30.00-150.00   44
  4  ω     50.00  89.00   1.00   70.00    --  112.00 -30.00 -60.00   39
  5  ω    102.00 175.00   1.00   70.00    --  112.00 111.00  30.00   73
  6  ω     98.00 177.00   1.00   70.00    --  112.00  30.00 -30.00   79
  7  ω     38.00 143.00   1.00   70.00    --  112.00 -77.00  30.00  105
  8  ω     45.00  98.00   1.00   70.00    --  112.00 -45.00 -90.00   53
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0830577000
_diffrn_orient_matrix_UB_12      -0.0056889000
_diffrn_orient_matrix_UB_13      -0.0092795000
_diffrn_orient_matrix_UB_21      -0.0154113000
_diffrn_orient_matrix_UB_22      0.0369971000
_diffrn_orient_matrix_UB_23      -0.1272646000
_diffrn_orient_matrix_UB_31      -0.0021569000
_diffrn_orient_matrix_UB_32      -0.0469015000
_diffrn_orient_matrix_UB_33      -0.0992229000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6299
_reflns_number_total             8271
_reflns_odcompleteness_completeness 99.32
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         1.936
_refine_diff_density_min         -1.596
_refine_diff_density_rms         0.188
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         8271
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0987
_refine_ls_R_factor_gt           0.0835
_refine_ls_restrained_S_all      1.081
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1396P)²+20.6764P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2359
_refine_ls_wR_factor_ref         0.2492
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 H1WA-Br1
 2.4 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C30) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O39) = Uanis(O38) = Uanis(C37)
Uanis(O18) = Uanis(C17) = Uanis(O19)
4. Others
 Sof(Br2B)=Sof(O3B)=1-FVAR(1)
 Sof(O51A)=Sof(F53A)=Sof(O50A)=Sof(F54A)=Sof(F55A)=Sof(O49A)=Sof(C52A)=
 Sof(S48A)=FVAR(1)
5.a Rotating group:
 O2W(H2WA,H2WB), O1W(H1WA,H1WB)
5.b Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C10(H10A,H10B), C20(H20A,H20B)
5.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C16(H16), C13(H13), C15(H15), C32(H32), C23(H23), C35(H35),
 C33(H33), C26(H26), C22(H22), C36(H36), C25(H25)
5.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C7(H7A,H7B,H7C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Eu1 Eu 0.38254(2) 0.25086(2) 0.73096(5) 0.01720(19) Uani 1 1 d . . . . .
S40 S 0.99718(16) 0.35179(10) 0.8632(3) 0.0397(6) Uani 1 1 d . . . . .
O18 O 0.4665(3) 0.2660(3) 0.9404(6) 0.0244(8) Uani 1 1 d . . . . .
O42 O 0.9974(5) 0.3762(4) 0.7338(9) 0.053(2) Uani 1 1 d . . . . .
F45 F 1.0399(4) 0.2676(3) 0.7551(8) 0.0568(18) Uani 1 1 d . . . . .
F47 F 1.1270(4) 0.3130(4) 0.8679(11) 0.076(3) Uani 1 1 d . . . . .
N11 N 0.7300(4) 0.3128(3) 1.0351(8) 0.0264(16) Uani 1 1 d . . . . .
C12 C 0.7052(5) 0.3253(3) 1.1496(10) 0.0276(19) Uani 1 1 d . . . . .
H12 H 0.737592 0.340796 1.227329 0.033 Uiso 1 1 calc R . . . .
C17 C 0.5103(4) 0.2768(4) 1.0520(9) 0.0244(8) Uani 1 1 d . . . . .
N31 N 1.0609(4) 0.3715(3) 1.4162(8) 0.0271(16) Uani 1 1 d . . . . .
F46 F 1.0620(7) 0.2671(3) 0.9767(10) 0.086(3) Uani 1 1 d . . . . .
C16 C 0.6826(6) 0.2926(4) 0.9198(11) 0.036(2) Uani 1 1 d . . . . .
H16 H 0.699801 0.285078 0.837141 0.043 Uiso 1 1 calc R . . . .
C30 C 0.9917(6) 0.4020(4) 1.4198(11) 0.038(2) Uani 1 1 d . U . . .
H30A H 0.966794 0.385547 1.488699 0.046 Uiso 1 1 calc R . . . .
H30B H 1.005431 0.437836 1.452572 0.046 Uiso 1 1 calc R . . . .
C8 C 0.9848(7) 0.4958(5) 1.2608(16) 0.068(4) Uani 1 1 d . . . . .
H8A H 0.974511 0.507363 1.350348 0.102 Uiso 1 1 calc GR . . . .
H8B H 0.975976 0.524540 1.193288 0.102 Uiso 1 1 calc GR . . . .
H8C H 1.036054 0.484646 1.275217 0.102 Uiso 1 1 calc GR . . . .
O43 O 1.0276(8) 0.3814(3) 0.9819(10) 0.075(3) Uani 1 1 d . . . . .
C13 C 0.6331(5) 0.3159(4) 1.1565(11) 0.0295(19) Uani 1 1 d . . . . .
H13 H 0.616315 0.324875 1.238606 0.035 Uiso 1 1 calc R . . . .
C5 C 0.9390(5) 0.4047(4) 1.2807(11) 0.036(2) Uani 1 1 d . . . . .
C2 C 0.8394(5) 0.4112(3) 1.0231(11) 0.0265(19) Uani 1 1 d . . . . .
C6 C 0.8937(5) 0.3619(4) 1.2330(11) 0.030(2) Uani 1 1 d . . . . .
C15 C 0.6113(6) 0.2834(4) 0.9233(10) 0.033(2) Uani 1 1 d . . . . .
H15 H 0.578793 0.270042 0.842404 0.040 Uiso 1 1 calc R . . . .
C32 C 1.0776(5) 0.3579(4) 1.2935(10) 0.0294(19) Uani 1 1 d . . . . .
H32 H 1.044686 0.366224 1.207699 0.035 Uiso 1 1 calc R . . . .
C1 C 0.8459(4) 0.3650(3) 1.0982(11) 0.0277(19) Uani 1 1 d . . . . .
C23 C 0.7441(6) 0.6079(4) 0.9054(13) 0.042(3) Uani 1 1 d . . . . .
H23 H 0.721613 0.628132 0.826376 0.051 Uiso 1 1 calc R . . . .
C35 C 1.1712(4) 0.3351(4) 1.5410(9) 0.0242(17) Uani 1 1 d . . . . .
H35 H 1.203263 0.327103 1.627988 0.029 Uiso 1 1 calc R . . . .
C14 C 0.5856(5) 0.2933(3) 1.0439(8) 0.0225(17) Uani 1 1 d . . . . .
C9 C 0.8971(6) 0.3122(5) 1.3191(13) 0.046(3) Uani 1 1 d . . . . .
H9A H 0.948285 0.301334 1.350383 0.068 Uiso 1 1 calc GR . . . .
H9B H 0.869323 0.284684 1.261361 0.068 Uiso 1 1 calc GR . . . .
H9C H 0.875830 0.318648 1.401052 0.068 Uiso 1 1 calc GR . . . .
O41 O 0.9294(8) 0.3268(5) 0.8664(18) 0.106(6) Uani 1 1 d . . . . .
C33 C 1.1414(5) 0.3324(4) 1.2910(9) 0.0263(18) Uani 1 1 d . . . . .
H33 H 1.152280 0.321946 1.204311 0.032 Uiso 1 1 calc R . . . .
C7 C 0.7880(6) 0.4152(4) 0.8840(12) 0.038(2) Uani 1 1 d . . . . .
H7A H 0.814611 0.408440 0.809538 0.057 Uiso 1 1 calc GR . . . .
H7B H 0.766912 0.450319 0.872423 0.057 Uiso 1 1 calc GR . . . .
H7C H 0.748618 0.389567 0.878373 0.057 Uiso 1 1 calc GR . . . .
C10 C 0.8085(5) 0.3175(4) 1.0315(11) 0.032(2) Uani 1 1 d . . . . .
H10A H 0.813018 0.316618 0.932261 0.039 Uiso 1 1 calc R . . . .
H10B H 0.834581 0.286625 1.078669 0.039 Uiso 1 1 calc R . . . .
C44 C 1.0604(7) 0.2971(5) 0.8681(13) 0.047(3) Uani 1 1 d . . . . .
C26 C 0.8072(6) 0.5478(4) 1.1307(13) 0.040(3) Uani 1 1 d . . . . .
H26 H 0.828565 0.526077 1.207419 0.048 Uiso 1 1 calc R . . . .
C22 C 0.7925(6) 0.5682(4) 0.8911(13) 0.042(2) Uani 1 1 d . . . . .
H22 H 0.803803 0.561314 0.802497 0.051 Uiso 1 1 calc R . . . .
C34 C 1.1899(4) 0.3218(4) 1.4160(9) 0.0220(17) Uani 1 1 d . . . . .
C20 C 0.8807(5) 0.5014(4) 0.9838(13) 0.040(3) Uani 1 1 d . . . . .
H20A H 0.928996 0.518966 1.003994 0.048 Uiso 1 1 calc R . . . .
H20B H 0.870412 0.490150 0.884461 0.048 Uiso 1 1 calc R . . . .
C36 C 1.1060(5) 0.3601(4) 1.5386(9) 0.0294(19) Uani 1 1 d . . . . .
H36 H 1.092752 0.369188 1.624234 0.035 Uiso 1 1 calc R . . . .
C25 C 0.7601(6) 0.5872(4) 1.1497(12) 0.038(2) Uani 1 1 d . . . . .
H25 H 0.749494 0.593178 1.239337 0.046 Uiso 1 1 calc R . . . .
C3 C 0.8848(5) 0.4538(4) 1.0762(13) 0.039(2) Uani 1 1 d . . . . .
C4 C 0.9351(5) 0.4506(4) 1.2047(13) 0.038(2) Uani 1 1 d . . . . .
O38 O 1.2780(4) 0.2854(3) 1.3023(7) 0.0366(11) Uani 1 1 d . . . . .
O19 O 0.4954(3) 0.2745(3) 1.1699(6) 0.0244(8) Uani 1 1 d . . . . .
C37 C 1.2641(5) 0.2958(5) 1.4190(10) 0.0366(11) Uani 1 1 d . . . . .
C27 C 0.6791(5) 0.6641(4) 1.0494(10) 0.0277(19) Uani 1 1 d . . . . .
C24 C 0.7287(5) 0.6177(4) 1.0366(10) 0.0285(19) Uani 1 1 d . . . . .
O39 O 1.3043(4) 0.2878(3) 1.5353(7) 0.0366(11) Uani 1 1 d . . . . .
N21 N 0.8230(5) 0.5399(3) 1.0033(10) 0.036(2) Uani 1 1 d . . . . .
O29 O 0.6748(4) 0.6767(3) 1.1723(7) 0.0327(15) Uani 1 1 d . . . . .
O28 O 0.6507(4) 0.6856(3) 0.9395(7) 0.0405(18) Uani 1 1 d . . . . .
Br1 Br 0.59880(11) 0.34576(7) 0.5607(2) 0.0797(6) Uani 1 1 d D . . A 1
O2W O 0.4218(5) 0.1653(3) 0.8431(8) 0.0464(19) Uani 1 1 d . . . . .
H2WA H 0.418402 0.141425 0.778609 0.070 Uiso 1 1 d GR . . . .
H2WB H 0.390839 0.155503 0.893426 0.070 Uiso 1 1 d GR . . . .
O1W O 0.4437(5) 0.3314(3) 0.6807(9) 0.050(2) Uani 1 1 d . . . . .
H1WA H 0.500000 0.337226 0.681590 0.075 Uiso 1 1 d DGR . . . .
H1WB H 0.419809 0.368555 0.652902 0.075 Uiso 1 1 d GR . . . .
Br2B Br 0.8182(3) 0.5158(4) 0.5148(9) 0.047(2) Uani 0.452(8) 1 d . . P B 2
O51A O 0.8309(9) 0.5181(8) 0.6484(16) 0.057(4) Uani 0.548(8) 1 d . . P B 1
F53A F 0.8385(10) 0.4128(7) 0.541(2) 0.078(5) Uani 0.548(8) 1 d . . P B 1
O50A O 0.8712(9) 0.5153(7) 0.4320(16) 0.049(4) Uani 0.548(8) 1 d . . P B 1
F54A F 0.7637(10) 0.4316(7) 0.346(2) 0.084(6) Uani 0.548(8) 1 d . . P B 1
F55A F 0.7266(10) 0.4357(7) 0.532(3) 0.093(7) Uani 0.548(8) 1 d . . P B 1
O49A O 0.7481(8) 0.5407(6) 0.4294(16) 0.048(4) Uani 0.548(8) 1 d . . P B 1
C52A C 0.7834(15) 0.4450(10) 0.475(3) 0.063(7) Uani 0.548(8) 1 d . . P B 1
S48A S 0.8190(9) 0.5080(7) 0.5181(15) 0.049(4) Uani 0.548(8) 1 d . . P B 1
O3B O 0.7571(15) 0.3798(13) 0.466(3) 0.082(8) Uani 0.452(8) 1 d . . P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Eu1 O18 2.325(6) . ?
Eu1 O38 2.397(6) 4_465 ?
Eu1 O19 2.400(6) 4_565 ?
Eu1 O39 2.341(6) 1_454 ?
Eu1 O29 2.435(7) 3_667 ?
Eu1 O28 2.348(7) 2_646 ?
Eu1 O2W 2.492(7) . ?
Eu1 O1W 2.463(7) . ?
S40 O42 1.410(9) . ?
S40 O43 1.399(10) . ?
S40 O41 1.426(12) . ?
S40 C44 1.829(13) . ?
O18 C17 1.245(11) . ?
F45 C44 1.324(15) . ?
F47 C44 1.311(15) . ?
N11 C12 1.336(12) . ?
N11 C16 1.373(13) . ?
N11 C10 1.480(11) . ?
C12 H12 0.9500 . ?
C12 C13 1.384(13) . ?
C17 C14 1.487(12) . ?
C17 O19 1.241(11) . ?
N31 C30 1.518(11) . ?
N31 C32 1.347(12) . ?
N31 C36 1.338(12) . ?
F46 C44 1.304(14) . ?
C16 H16 0.9500 . ?
C16 C15 1.361(14) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C5 1.497(14) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C8 C4 1.510(14) . ?
C13 H13 0.9500 . ?
C13 C14 1.382(12) . ?
C5 C6 1.405(14) . ?
C5 C4 1.386(16) . ?
C2 C1 1.385(14) . ?
C2 C7 1.488(14) . ?
C2 C3 1.413(13) . ?
C6 C1 1.424(14) . ?
C6 C9 1.520(16) . ?
C15 H15 0.9500 . ?
C15 C14 1.386(12) . ?
C32 H32 0.9500 . ?
C32 C33 1.365(12) . ?
C1 C10 1.485(12) . ?
C23 H23 0.9500 . ?
C23 C22 1.388(15) . ?
C23 C24 1.394(15) . ?
C35 H35 0.9500 . ?
C35 C34 1.383(12) . ?
C35 C36 1.372(13) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C33 H33 0.9500 . ?
C33 C34 1.380(12) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C26 H26 0.9500 . ?
C26 C25 1.378(14) . ?
C26 N21 1.353(15) . ?
C22 H22 0.9500 . ?
C22 N21 1.335(15) . ?
C34 C37 1.533(11) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C3 1.510(16) . ?
C20 N21 1.503(12) . ?
C36 H36 0.9500 . ?
C25 H25 0.9500 . ?
C25 C24 1.377(14) . ?
C3 C4 1.399(16) . ?
O38 C37 1.249(11) . ?
C37 O39 1.236(12) . ?
C27 C24 1.531(12) . ?
C27 O29 1.261(12) . ?
C27 O28 1.220(12) . ?
O2W H2WA 0.8718 . ?
O2W H2WB 0.8720 . ?
O1W H1WA 1.0601 . ?
O1W H1WB 1.0621 . ?
O51A S48A 1.27(2) . ?
F53A C52A 1.37(4) . ?
O50A S48A 1.43(2) . ?
F54A C52A 1.28(3) . ?
F55A C52A 1.32(3) . ?
O49A S48A 1.65(2) . ?
C52A S48A 1.77(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O18 Eu1 O38 104.3(2) . 4_465 ?
O18 Eu1 O19 78.6(2) . 4_565 ?
O18 Eu1 O39 146.5(3) . 1_454 ?
O18 Eu1 O29 78.5(2) . 3_667 ?
O18 Eu1 O28 140.1(3) . 2_646 ?
O18 Eu1 O2W 71.5(3) . . ?
O18 Eu1 O1W 77.3(3) . . ?
O38 Eu1 O19 141.3(3) 4_465 4_565 ?
O38 Eu1 O29 74.3(3) 4_465 3_667 ?
O38 Eu1 O2W 73.2(3) 4_465 . ?
O38 Eu1 O1W 145.6(3) 4_465 . ?
O19 Eu1 O29 141.8(2) 4_565 3_667 ?
O19 Eu1 O2W 71.3(3) 4_565 . ?
O19 Eu1 O1W 73.1(3) 4_565 . ?
O39 Eu1 O38 89.4(2) 1_454 4_465 ?
O39 Eu1 O19 109.6(2) 1_454 4_565 ?
O39 Eu1 O29 75.9(2) 1_454 3_667 ?
O39 Eu1 O28 71.8(3) 1_454 2_646 ?
O39 Eu1 O2W 142.0(3) 1_454 . ?
O39 Eu1 O1W 74.5(3) 1_454 . ?
O29 Eu1 O2W 127.9(3) 3_667 . ?
O29 Eu1 O1W 72.4(3) 3_667 . ?
O28 Eu1 O38 79.7(2) 2_646 4_465 ?
O28 Eu1 O19 75.1(2) 2_646 4_565 ?
O28 Eu1 O29 138.4(3) 2_646 3_667 ?
O28 Eu1 O2W 72.0(3) 2_646 . ?
O28 Eu1 O1W 121.4(3) 2_646 . ?
O1W Eu1 O2W 136.2(3) . . ?
O42 S40 O41 113.2(9) . . ?
O42 S40 C44 103.9(5) . . ?
O43 S40 O42 114.8(6) . . ?
O43 S40 O41 115.5(8) . . ?
O43 S40 C44 104.5(7) . . ?
O41 S40 C44 103.0(7) . . ?
C17 O18 Eu1 176.7(7) . . ?
C12 N11 C16 119.8(7) . . ?
C12 N11 C10 121.5(8) . . ?
C16 N11 C10 118.5(8) . . ?
N11 C12 H12 119.5 . . ?
N11 C12 C13 120.9(8) . . ?
C13 C12 H12 119.5 . . ?
O18 C17 C14 117.9(7) . . ?
O19 C17 O18 124.2(8) . . ?
O19 C17 C14 117.8(7) . . ?
C32 N31 C30 121.1(8) . . ?
C36 N31 C30 117.9(8) . . ?
C36 N31 C32 121.0(8) . . ?
N11 C16 H16 119.8 . . ?
C15 C16 N11 120.4(8) . . ?
C15 C16 H16 119.8 . . ?
N31 C30 H30A 108.9 . . ?
N31 C30 H30B 108.9 . . ?
H30A C30 H30B 107.7 . . ?
C5 C30 N31 113.6(8) . . ?
C5 C30 H30A 108.9 . . ?
C5 C30 H30B 108.9 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C4 C8 H8A 109.5 . . ?
C4 C8 H8B 109.5 . . ?
C4 C8 H8C 109.5 . . ?
C12 C13 H13 120.0 . . ?
C14 C13 C12 120.0(8) . . ?
C14 C13 H13 120.0 . . ?
C6 C5 C30 119.7(10) . . ?
C4 C5 C30 118.3(9) . . ?
C4 C5 C6 122.0(9) . . ?
C1 C2 C7 120.5(8) . . ?
C1 C2 C3 119.4(9) . . ?
C3 C2 C7 120.0(10) . . ?
C5 C6 C1 118.3(9) . . ?
C5 C6 C9 121.5(10) . . ?
C1 C6 C9 120.1(9) . . ?
C16 C15 H15 119.7 . . ?
C16 C15 C14 120.5(9) . . ?
C14 C15 H15 119.7 . . ?
N31 C32 H32 119.6 . . ?
N31 C32 C33 120.7(9) . . ?
C33 C32 H32 119.7 . . ?
C2 C1 C6 120.2(8) . . ?
C2 C1 C10 119.5(9) . . ?
C6 C1 C10 120.0(9) . . ?
C22 C23 H23 120.2 . . ?
C22 C23 C24 119.5(10) . . ?
C24 C23 H23 120.2 . . ?
C34 C35 H35 120.2 . . ?
C36 C35 H35 120.2 . . ?
C36 C35 C34 119.5(8) . . ?
C13 C14 C17 122.0(8) . . ?
C13 C14 C15 118.1(8) . . ?
C15 C14 C17 119.8(8) . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C32 C33 H33 120.4 . . ?
C32 C33 C34 119.3(8) . . ?
C34 C33 H33 120.4 . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N11 C10 C1 115.6(7) . . ?
N11 C10 H10A 108.4 . . ?
N11 C10 H10B 108.4 . . ?
C1 C10 H10A 108.4 . . ?
C1 C10 H10B 108.4 . . ?
H10A C10 H10B 107.4 . . ?
F45 C44 S40 110.3(9) . . ?
F47 C44 S40 111.6(9) . . ?
F47 C44 F45 106.4(10) . . ?
F46 C44 S40 112.1(9) . . ?
F46 C44 F45 106.9(10) . . ?
F46 C44 F47 109.3(13) . . ?
C25 C26 H26 119.8 . . ?
N21 C26 H26 119.8 . . ?
N21 C26 C25 120.4(10) . . ?
C23 C22 H22 120.3 . . ?
N21 C22 C23 119.3(11) . . ?
N21 C22 H22 120.3 . . ?
C35 C34 C37 119.4(7) . . ?
C33 C34 C35 119.2(7) . . ?
C33 C34 C37 121.4(8) . . ?
H20A C20 H20B 107.7 . . ?
C3 C20 H20A 108.8 . . ?
C3 C20 H20B 108.8 . . ?
N21 C20 H20A 108.8 . . ?
N21 C20 H20B 108.8 . . ?
N21 C20 C3 113.7(9) . . ?
N31 C36 C35 120.3(8) . . ?
N31 C36 H36 119.9 . . ?
C35 C36 H36 119.9 . . ?
C26 C25 H25 120.5 . . ?
C24 C25 C26 118.9(11) . . ?
C24 C25 H25 120.5 . . ?
C2 C3 C20 117.3(10) . . ?
C4 C3 C2 121.3(10) . . ?
C4 C3 C20 121.3(9) . . ?
C5 C4 C8 120.1(10) . . ?
C5 C4 C3 118.4(9) . . ?
C3 C4 C8 121.5(10) . . ?
C37 O38 Eu1 133.6(6) . 4_666 ?
C17 O19 Eu1 128.9(5) . 4_566 ?
O38 C37 C34 116.1(8) . . ?
O39 C37 C34 117.2(8) . . ?
O39 C37 O38 126.7(8) . . ?
O29 C27 C24 116.1(8) . . ?
O28 C27 C24 115.8(8) . . ?
O28 C27 O29 128.0(8) . . ?
C23 C24 C27 117.6(8) . . ?
C25 C24 C23 119.7(9) . . ?
C25 C24 C27 122.6(9) . . ?
C37 O39 Eu1 164.9(8) . 1_656 ?
C26 N21 C20 121.3(9) . . ?
C22 N21 C26 122.1(9) . . ?
C22 N21 C20 116.5(10) . . ?
C27 O29 Eu1 133.4(6) . 3_667 ?
C27 O28 Eu1 160.5(8) . 2_656 ?
Eu1 O2W H2WA 109.5 . . ?
Eu1 O2W H2WB 109.5 . . ?
H2WA O2W H2WB 104.4 . . ?
Eu1 O1W H1WA 128.1 . . ?
Eu1 O1W H1WB 128.1 . . ?
H1WA O1W H1WB 103.8 . . ?
F53A C52A S48A 103.7(18) . . ?
F54A C52A F53A 109(2) . . ?
F54A C52A F55A 106(2) . . ?
F54A C52A S48A 120(2) . . ?
F55A C52A F53A 107(2) . . ?
F55A C52A S48A 111.1(19) . . ?
O51A S48A O50A 124.6(15) . . ?
O51A S48A O49A 111.7(14) . . ?
O51A S48A C52A 113.6(18) . . ?
O50A S48A O49A 101.4(13) . . ?
O50A S48A C52A 104.5(13) . . ?
O49A S48A C52A 97.0(14) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C22 H22 O51A 0.95 2.02 2.917(19) 157.1 . yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Eu1 O38 C37 C34 177.0(6) 4_666 . . . ?
Eu1 O38 C37 O39 -2(2) 4_666 . . . ?
O18 C17 C14 C13 166.9(9) . . . . ?
O18 C17 C14 C15 -16.9(14) . . . . ?
O18 C17 O19 Eu1 0.4(14) . . . 4_566 ?
O42 S40 C44 F45 -55.3(10) . . . . ?
O42 S40 C44 F47 62.7(11) . . . . ?
O42 S40 C44 F46 -174.4(10) . . . . ?
N11 C12 C13 C14 -0.1(15) . . . . ?
N11 C16 C15 C14 -1.1(18) . . . . ?
C12 N11 C16 C15 -2.5(16) . . . . ?
C12 N11 C10 C1 -41.6(13) . . . . ?
C12 C13 C14 C17 172.8(9) . . . . ?
C12 C13 C14 C15 -3.5(14) . . . . ?
N31 C30 C5 C6 79.0(12) . . . . ?
N31 C30 C5 C4 -103.1(10) . . . . ?
N31 C32 C33 C34 -1.9(15) . . . . ?
C16 N11 C12 C13 3.1(15) . . . . ?
C16 N11 C10 C1 141.6(10) . . . . ?
C16 C15 C14 C17 -172.3(10) . . . . ?
C16 C15 C14 C13 4.1(16) . . . . ?
C30 N31 C32 C33 177.4(9) . . . . ?
C30 N31 C36 C35 -176.4(9) . . . . ?
C30 C5 C6 C1 -177.9(8) . . . . ?
C30 C5 C6 C9 -0.5(13) . . . . ?
C30 C5 C4 C8 1.7(15) . . . . ?
C30 C5 C4 C3 -178.5(9) . . . . ?
O43 S40 C44 F45 -176.0(9) . . . . ?
O43 S40 C44 F47 -58.0(11) . . . . ?
O43 S40 C44 F46 64.9(12) . . . . ?
C5 C6 C1 C2 -6.5(12) . . . . ?
C5 C6 C1 C10 167.6(8) . . . . ?
C2 C1 C10 N11 -82.2(11) . . . . ?
C2 C3 C4 C8 178.9(11) . . . . ?
C2 C3 C4 C5 -0.8(15) . . . . ?
C6 C5 C4 C8 179.6(11) . . . . ?
C6 C5 C4 C3 -0.7(14) . . . . ?
C6 C1 C10 N11 103.6(10) . . . . ?
C32 N31 C30 C5 12.1(14) . . . . ?
C32 N31 C36 C35 1.5(14) . . . . ?
C32 C33 C34 C35 3.1(14) . . . . ?
C32 C33 C34 C37 -176.8(10) . . . . ?
C1 C2 C3 C20 174.2(8) . . . . ?
C1 C2 C3 C4 -1.5(14) . . . . ?
C23 C22 N21 C26 1.4(16) . . . . ?
C23 C22 N21 C20 -173.9(10) . . . . ?
C35 C34 C37 O38 -179.0(10) . . . . ?
C35 C34 C37 O39 0.0(15) . . . . ?
C14 C17 O19 Eu1 -179.2(6) . . . 4_566 ?
C9 C6 C1 C2 176.1(8) . . . . ?
C9 C6 C1 C10 -9.8(12) . . . . ?
O41 S40 C44 F45 62.9(11) . . . . ?
O41 S40 C44 F47 -179.1(11) . . . . ?
O41 S40 C44 F46 -56.2(13) . . . . ?
C33 C34 C37 O38 0.8(16) . . . . ?
C33 C34 C37 O39 179.9(10) . . . . ?
C7 C2 C1 C6 -178.2(8) . . . . ?
C7 C2 C1 C10 7.7(12) . . . . ?
C7 C2 C3 C20 -2.4(13) . . . . ?
C7 C2 C3 C4 -178.1(9) . . . . ?
C10 N11 C12 C13 -173.5(9) . . . . ?
C10 N11 C16 C15 174.2(10) . . . . ?
C26 C25 C24 C23 0.9(15) . . . . ?
C26 C25 C24 C27 -176.6(9) . . . . ?
C22 C23 C24 C25 -1.7(16) . . . . ?
C22 C23 C24 C27 175.9(10) . . . . ?
C34 C35 C36 N31 -0.2(15) . . . . ?
C34 C37 O39 Eu1 132(2) . . . 1_656 ?
C20 C3 C4 C8 3.4(16) . . . . ?
C20 C3 C4 C5 -176.3(9) . . . . ?
C36 N31 C30 C5 -169.9(9) . . . . ?
C36 N31 C32 C33 -0.5(15) . . . . ?
C36 C35 C34 C33 -2.1(14) . . . . ?
C36 C35 C34 C37 177.8(9) . . . . ?
C25 C26 N21 C22 -2.3(16) . . . . ?
C25 C26 N21 C20 172.8(9) . . . . ?
C3 C2 C1 C6 5.2(13) . . . . ?
C3 C2 C1 C10 -168.9(8) . . . . ?
C3 C20 N21 C26 34.8(13) . . . . ?
C3 C20 N21 C22 -149.8(10) . . . . ?
C4 C5 C6 C1 4.2(13) . . . . ?
C4 C5 C6 C9 -178.4(9) . . . . ?
O38 C37 O39 Eu1 -49(3) . . . 1_656 ?
O19 C17 C14 C13 -13.5(14) . . . . ?
O19 C17 C14 C15 162.7(9) . . . . ?
C24 C23 C22 N21 0.5(17) . . . . ?
C24 C27 O29 Eu1 173.3(6) . . . 3_667 ?
C24 C27 O28 Eu1 -122.2(17) . . . 2_656 ?
N21 C26 C25 C24 1.1(16) . . . . ?
N21 C20 C3 C2 88.6(12) . . . . ?
N21 C20 C3 C4 -95.6(11) . . . . ?
O29 C27 C24 C23 -169.9(9) . . . . ?
O29 C27 C24 C25 7.6(14) . . . . ?
O29 C27 O28 Eu1 55(2) . . . 2_656 ?
O28 C27 C24 C23 7.5(14) . . . . ?
O28 C27 C24 C25 -175.0(10) . . . . ?
O28 C27 O29 Eu1 -3.7(16) . . . 3_667 ?
F53A C52A S48A O51A -64(2) . . . . ?
F53A C52A S48A O50A 75(2) . . . . ?
F53A C52A S48A O49A 178.7(17) . . . . ?
F54A C52A S48A O51A 174(2) . . . . ?
F54A C52A S48A O50A -47(3) . . . . ?
F54A C52A S48A O49A 57(2) . . . . ?
F55A C52A S48A O51A 50(3) . . . . ?
F55A C52A S48A O50A -171(2) . . . . ?
F55A C52A S48A O49A -67(2) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.214 0.705 0.342 17.8 15.2 ?
2 0.214 0.795 0.842 17.8 15.2 ?
3 0.500 0.500 -0.810 433.8 125.3 '12x water'
4 0.500 0.000 -0.498 433.8 125.3 '12x water'
5 0.786 0.205 0.158 17.8 14.6 ?
6 0.786 0.295 0.658 17.8 14.6 ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.529
_oxdiff_exptl_absorpt_empirical_full_min 0.657
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_jj003_nd_br_h2o_acet_red3
_database_code_depnum_ccdc_archive 'CCDC 1833442'
loop_
_audit_author_name
_audit_author_address
'Antti Tiihonen'
;University of Jyv?skyl?, Department of Chemistry
Finland
;
_audit_update_record             
;
2018-03-29 deposited with the CCDC.	2019-02-28 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_CHEMW03_I                   
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as...
RESPONSE: The structure contains voids of unresolved electron density
which was treated using Olex2 solvent mask procedure (full details in 
_smtbx_masks_special_details). The 7 water molecules per asymmetric unit 
 are included in the formula and used in the calculations. 
;
_vrf_PLAT420_I                   
;
PROBLEM: D-H Without Acceptor...
RESPONSE: Hydrogen bond acceptors (water) have been removed among
other disordered solvent from the voids (see CHEMW03_ALERT_2_A).
;
_vrf_PLAT412_I                   
;
PROBLEM: Short Intra XH3 .. XHn...
RESPONSE: Hydrogen atoms calculated using a riding model in their general
(unoptimized) geometry causing a proximity alert.
;
_vrf_FORMU01_I                   
;
PROBLEM: There is a discrepancy between the atom counts...
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_CELLZ01_I                   
;
PROBLEM: Difference between formula and atom_site...
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT041_I                   
;
PROBLEM: Calc. and Reported SumFormula Strings  Differ...
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT044_I                   
;
PROBLEM: Calculated and Reported Density Dx Differ...
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT051_I                   
;
PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs...
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT068_I                   
;
PROBLEM: Reported F000 Differs from Calcd (or Missing)...
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT606_I                   
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure...
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
# end Validation Reply Form

_audit_creation_date             2018-03-28
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H31 N3 Nd O8, 3(Br)'
_chemical_formula_sum            'C30 H45 Br3 N3 Nd O15'
_chemical_formula_weight         1071.66
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C21 H25 O8 Nd Br3 N3'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -3.1807 10.9079 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.4378(3)
_cell_length_b                   12.3546(3)
_cell_length_c                   18.8810(4)
_cell_angle_alpha                104.683(2)
_cell_angle_beta                 98.809(2)
_cell_angle_gamma                99.428(2)
_cell_volume                     2056.71(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8623
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      76.0950
_cell_measurement_theta_min      3.8560
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    13.614
_exptl_absorpt_correction_T_max  0.422
_exptl_absorpt_correction_T_min  0.117
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.730
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1062
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-6 3 0 0.0448
1 -8 1 0.0688
0 -8 5 0.0492
1 7 -1 0.0415
6 0 -4 0.0230
-1 -2 12 0.0700
-3 -6 5 0.0525
3 6 -5 0.0558
1 1 11 0.0902
-1 0 -11 0.1367
6 -3 -4 0.0525
-6 3 2 0.0337

_exptl_crystal_size_max          0.231
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.073
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-6.0035 2.9956 -0.0093 -0.8594 -0.5128 0.1198
1.0023 -8.0076 1.0250 -0.1294 0.9719 0.2604
0.0013 -8.0014 5.0260 -0.3149 0.9693 -0.0385
0.9988 7.0091 -1.0218 0.4158 -0.8009 -0.3003
6.0034 0.0009 -4.0010 0.9906 0.1365 0.0770
-1.0018 -1.9813 12.0093 -0.3057 0.2806 -0.8878
-3.0006 -6.0029 5.0198 -0.7269 0.6542 -0.0030
3.0006 6.0029 -5.0198 0.7269 -0.6542 0.0030
0.9986 1.0238 10.9998 0.1290 -0.0240 -1.0372
-0.9988 -0.0224 -11.0029 -0.0935 -0.0933 0.9884
6.0041 -3.0032 -3.9917 0.8840 0.4886 0.2235
-6.0038 2.9994 1.9912 -0.8717 -0.5007 -0.0519

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_unetI/netI     0.0405
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12580
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.992
_diffrn_reflns_theta_min         3.785
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -66.00  27.00   1.00    1.00    --  -41.65  57.00  60.00   93
  2  ω      1.00  82.00   1.00    1.00    --   41.65 -99.00 150.00   81
  3  ω     36.00  63.00   1.00    1.50    --  112.00-111.00  30.00   27
  4  ω     83.00 115.00   1.00    1.50    --  112.00-111.00  30.00   32
  5  ω     66.00 105.00   1.00    1.50    --  112.00 -94.00 -60.00   39
  6  ω     57.00 141.00   1.00    1.50    --  112.00 -61.00 -30.00   84
  7  ω     65.00 171.00   1.00    1.50    --  112.00  15.00  60.00  106
  8  ω    149.00 178.00   1.00    1.50    --  112.00  61.00 -30.00   29
  9  ω    110.00 177.00   1.00    1.50    --  112.00  61.00 -60.00   67
 10  ω     87.00 168.00   1.00    1.50    --  112.00  45.00 -90.00   81
 11  ω     83.00 115.00   1.00    1.50    --  112.00  61.00 -30.00   32
 12  ω     45.00 135.00   1.00    1.50    --  112.00 -61.00-180.00   90
 13  ω     50.00 116.00   1.00    1.50    --  112.00-111.00-150.00   66
 14  ω     42.00 102.00   1.00    1.50    --  112.00-111.00 150.00   60
 15  ω   -115.00 -17.00   1.00    1.00    --  -41.65 -37.00 150.00   98
 16  ω   -113.00 -20.00   1.00    1.00    --  -41.65 -57.00 -90.00   93
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1608776000
_diffrn_orient_matrix_UB_12      0.0355007000
_diffrn_orient_matrix_UB_13      -0.0061775000
_diffrn_orient_matrix_UB_21      0.0269374000
_diffrn_orient_matrix_UB_22      -0.1171922000
_diffrn_orient_matrix_UB_23      0.0062767000
_diffrn_orient_matrix_UB_31      -0.0442825000
_diffrn_orient_matrix_UB_32      -0.0490283000
_diffrn_orient_matrix_UB_33      -0.0857078000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7176
_reflns_number_total             7446
_reflns_odcompleteness_completeness 99.44
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         1.727
_refine_diff_density_min         -1.438
_refine_diff_density_rms         0.127
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         7446
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0449
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0652P)²+6.7132P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1163
_refine_ls_wR_factor_ref         0.1179
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Others
 Sof(Br3B)=1-FVAR(1)
 Sof(Br3A)=FVAR(1)
3.a Rotating group:
 O2W(H2WA,H2WB), O1W(H1WA,H1WB)
3.b Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C30(H30A,H30B), C10(H10A,H10B)
3.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C16(H16), C15(H15), C35(H35), C32(H32), C33(H33), C23(H23),
 C13(H13), C36(H36), C22(H22), C26(H26), C25(H25)
3.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Nd1 Nd 0.23509(3) 0.51767(2) 0.50335(2) 0.01810(9) Uani 1 1 d . . . . .
Br1 Br 0.90043(6) 0.33483(5) 0.09927(4) 0.03437(15) Uani 1 1 d . . . . .
Br2 Br 0.51184(7) 0.36023(6) -0.17755(4) 0.04445(18) Uani 1 1 d . . . . .
O18 O 0.5428(4) 0.4618(3) 0.41111(18) 0.0244(7) Uani 1 1 d . . . . .
O19 O 0.3089(4) 0.4715(4) 0.38161(19) 0.0332(9) Uani 1 1 d . . . . .
O28 O 0.1449(4) 0.4409(3) -0.40060(19) 0.0257(8) Uani 1 1 d . . . . .
O39 O 0.2260(4) -0.3142(3) -0.39537(19) 0.0262(8) Uani 1 1 d . . . . .
C37 C 0.0975(6) -0.3160(4) -0.3863(3) 0.0226(10) Uani 1 1 d . . . . .
N31 N 0.0320(5) -0.1066(4) -0.1843(2) 0.0242(9) Uani 1 1 d . . . . .
N11 N 0.4256(5) 0.3226(4) 0.1333(2) 0.0235(9) Uani 1 1 d . . . . .
C34 C 0.0736(6) -0.2357(4) -0.3173(3) 0.0235(10) Uani 1 1 d . . . . .
C1 C 0.2825(6) 0.2292(5) 0.0002(3) 0.0245(11) Uani 1 1 d . . . . .
C17 C 0.4266(5) 0.4513(4) 0.3656(3) 0.0213(10) Uani 1 1 d . . . . .
C3 C 0.0791(6) 0.2719(4) -0.0740(3) 0.0208(10) Uani 1 1 d . . . . .
C20 C -0.0023(6) 0.3586(5) -0.0960(3) 0.0257(11) Uani 1 1 d . . . . .
H20A H -0.106126 0.338221 -0.092093 0.031 Uiso 1 1 calc R . . . .
H20B H 0.041118 0.435257 -0.060601 0.031 Uiso 1 1 calc R . . . .
C12 C 0.5546(6) 0.3522(5) 0.1835(3) 0.0251(11) Uani 1 1 d . . . . .
H12 H 0.643151 0.343343 0.166875 0.030 Uiso 1 1 calc R . . . .
C16 C 0.2997(5) 0.3387(4) 0.1551(3) 0.0219(10) Uani 1 1 d . . . . .
H16 H 0.210912 0.319206 0.118935 0.026 Uiso 1 1 calc R . . . .
C2 C 0.2149(6) 0.3097(4) -0.0247(3) 0.0233(10) Uani 1 1 d . . . . .
N21 N 0.0040(5) 0.3634(4) -0.1738(2) 0.0223(9) Uani 1 1 d . . . . .
C15 C 0.2988(5) 0.3834(4) 0.2300(3) 0.0216(10) Uani 1 1 d . . . . .
H15 H 0.209957 0.395600 0.245257 0.026 Uiso 1 1 calc R . . . .
C8 C -0.1273(6) 0.1159(5) -0.1607(3) 0.0318(12) Uani 1 1 d . . . . .
H8A H -0.180774 0.178181 -0.156287 0.048 Uiso 1 1 calc GR . . . .
H8B H -0.187913 0.049365 -0.152797 0.048 Uiso 1 1 calc GR . . . .
H8C H -0.104828 0.094933 -0.210779 0.048 Uiso 1 1 calc GR . . . .
C35 C 0.1923(6) -0.1788(5) -0.2592(3) 0.0282(11) Uani 1 1 d . . . . .
H35 H 0.289232 -0.183964 -0.265361 0.034 Uiso 1 1 calc R . . . .
C30 C 0.0083(7) -0.0501(4) -0.1070(3) 0.0287(11) Uani 1 1 d . . . . .
H30A H 0.046212 -0.090939 -0.071818 0.034 Uiso 1 1 calc R . . . .
H30B H -0.098254 -0.057270 -0.108721 0.034 Uiso 1 1 calc R . . . .
C32 C -0.0844(6) -0.1560(5) -0.2407(3) 0.0274(11) Uani 1 1 d . . . . .
H32 H -0.179661 -0.146140 -0.233951 0.033 Uiso 1 1 calc R . . . .
C27 C 0.0214(6) 0.4046(4) -0.3890(3) 0.0226(10) Uani 1 1 d . . . . .
C33 C -0.0659(6) -0.2203(5) -0.3076(3) 0.0290(11) Uani 1 1 d . . . . .
H33 H -0.148180 -0.254620 -0.347588 0.035 Uiso 1 1 calc R . . . .
C23 C 0.1413(6) 0.3784(4) -0.2665(3) 0.0233(10) Uani 1 1 d . . . . .
H23 H 0.232123 0.381696 -0.282515 0.028 Uiso 1 1 calc R . . . .
C13 C 0.5574(6) 0.3953(5) 0.2590(3) 0.0245(10) Uani 1 1 d . . . . .
H13 H 0.647530 0.414490 0.294212 0.029 Uiso 1 1 calc R . . . .
C6 C 0.2176(6) 0.1123(5) -0.0251(3) 0.0256(11) Uani 1 1 d . . . . .
C36 C 0.1686(6) -0.1149(5) -0.1926(3) 0.0301(12) Uani 1 1 d . . . . .
H36 H 0.249318 -0.076627 -0.152391 0.036 Uiso 1 1 calc R . . . .
C7 C 0.2875(7) 0.4357(5) 0.0026(4) 0.0394(14) Uani 1 1 d . . . . .
H7A H 0.238383 0.475417 0.040325 0.059 Uiso 1 1 calc GR . . . .
H7B H 0.279914 0.468550 -0.039528 0.059 Uiso 1 1 calc GR . . . .
H7C H 0.391107 0.444538 0.024854 0.059 Uiso 1 1 calc GR . . . .
C14 C 0.4293(5) 0.4104(4) 0.2831(3) 0.0204(10) Uani 1 1 d . . . . .
C24 C 0.0152(6) 0.3866(4) -0.3133(3) 0.0233(10) Uani 1 1 d . . . . .
C22 C 0.1309(5) 0.3656(4) -0.1972(3) 0.0232(10) Uani 1 1 d . . . . .
H22 H 0.214977 0.358308 -0.165441 0.028 Uiso 1 1 calc R . . . .
C4 C 0.0145(5) 0.1551(4) -0.1024(3) 0.0207(10) Uani 1 1 d . . . . .
C5 C 0.0836(6) 0.0758(4) -0.0778(3) 0.0234(10) Uani 1 1 d . . . . .
C26 C -0.1191(6) 0.3718(5) -0.2175(3) 0.0303(12) Uani 1 1 d . . . . .
H26 H -0.208005 0.370073 -0.199688 0.036 Uiso 1 1 calc R . . . .
C10 C 0.4309(6) 0.2700(6) 0.0526(3) 0.0322(13) Uani 1 1 d . . . . .
H10A H 0.479520 0.204232 0.049552 0.039 Uiso 1 1 calc R . . . .
H10B H 0.492057 0.327215 0.035305 0.039 Uiso 1 1 calc R . . . .
C25 C -0.1146(6) 0.3827(5) -0.2875(3) 0.0306(12) Uani 1 1 d . . . . .
H25 H -0.201176 0.387580 -0.318526 0.037 Uiso 1 1 calc R . . . .
C9 C 0.2927(8) 0.0287(6) 0.0031(3) 0.0407(15) Uani 1 1 d . . . . .
H9A H 0.372056 0.013663 -0.023451 0.061 Uiso 1 1 calc GR . . . .
H9B H 0.221651 -0.043050 -0.005559 0.061 Uiso 1 1 calc GR . . . .
H9C H 0.333540 0.060945 0.056842 0.061 Uiso 1 1 calc GR . . . .
O38 O -0.0149(4) -0.3863(3) -0.43087(19) 0.0268(8) Uani 1 1 d . . . . .
O29 O -0.1005(4) 0.3819(3) -0.4332(2) 0.0280(8) Uani 1 1 d . . . . .
O2W O 0.4095(4) 0.6937(4) 0.4971(2) 0.0376(9) Uani 1 1 d . . . . .
H2WA H 0.381583 0.758446 0.518125 0.056 Uiso 1 1 d GR . . . .
H2WB H 0.413996 0.692498 0.449672 0.056 Uiso 1 1 d GR . . . .
O1W O 0.2847(5) 0.3232(4) 0.4831(3) 0.0486(12) Uani 1 1 d . . . . .
H1WA H 0.225322 0.277803 0.503168 0.073 Uiso 1 1 d GR . . . .
H1WB H 0.379182 0.323843 0.504128 0.073 Uiso 1 1 d GR . . . .
Br3A Br 0.5683(3) -0.1044(3) -0.2050(2) 0.0954(13) Uani 0.372(3) 1 d . . P . .
Br3B Br -0.0030(3) 0.07120(14) -0.34921(10) 0.0908(7) Uani 0.628(3) 1 d . . P .
.


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nd1 O18 2.377(3) 2_666 ?
Nd1 O19 2.460(3) . ?
Nd1 O28 2.449(3) 1_556 ?
Nd1 O39 2.464(3) 1_566 ?
Nd1 O38 2.393(3) 2 ?
Nd1 O29 2.396(4) 2_565 ?
Nd1 O2W 2.544(4) . ?
Nd1 O1W 2.470(4) . ?
O18 C17 1.252(6) . ?
O19 C17 1.242(6) . ?
O28 C27 1.250(6) . ?
O39 C37 1.248(6) . ?
C37 C34 1.496(7) . ?
C37 O38 1.282(6) . ?
N31 C30 1.517(6) . ?
N31 C32 1.344(7) . ?
N31 C36 1.339(7) . ?
N11 C12 1.356(6) . ?
N11 C16 1.344(6) . ?
N11 C10 1.510(6) . ?
C34 C35 1.388(7) . ?
C34 C33 1.393(7) . ?
C1 C2 1.404(7) . ?
C1 C6 1.401(8) . ?
C1 C10 1.512(7) . ?
C17 C14 1.517(6) . ?
C3 C20 1.518(7) . ?
C3 C2 1.395(7) . ?
C3 C4 1.400(7) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 N21 1.495(6) . ?
C12 H12 0.9500 . ?
C12 C13 1.383(7) . ?
C16 H16 0.9500 . ?
C16 C15 1.383(7) . ?
C2 C7 1.515(8) . ?
N21 C22 1.336(7) . ?
N21 C26 1.352(7) . ?
C15 H15 0.9500 . ?
C15 C14 1.396(7) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C8 C4 1.518(7) . ?
C35 H35 0.9500 . ?
C35 C36 1.377(8) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C5 1.520(7) . ?
C32 H32 0.9500 . ?
C32 C33 1.365(8) . ?
C27 C24 1.510(7) . ?
C27 O29 1.257(6) . ?
C33 H33 0.9500 . ?
C23 H23 0.9500 . ?
C23 C24 1.403(7) . ?
C23 C22 1.374(7) . ?
C13 H13 0.9500 . ?
C13 C14 1.380(7) . ?
C6 C5 1.412(7) . ?
C6 C9 1.502(7) . ?
C36 H36 0.9500 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C24 C25 1.384(8) . ?
C22 H22 0.9500 . ?
C4 C5 1.397(7) . ?
C26 H26 0.9500 . ?
C26 C25 1.367(8) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C25 H25 0.9500 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
O2W H2WA 0.8982 . ?
O2W H2WB 0.8998 . ?
O1W H1WA 0.9175 . ?
O1W H1WB 0.9163 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O18 Nd1 O19 102.68(12) 2_666 . ?
O18 Nd1 O28 78.44(12) 2_666 1_556 ?
O18 Nd1 O39 78.58(12) 2_666 1_566 ?
O18 Nd1 O38 144.49(13) 2_666 2 ?
O18 Nd1 O29 142.94(13) 2_666 2_565 ?
O18 Nd1 O2W 73.23(13) 2_666 . ?
O18 Nd1 O1W 74.42(13) 2_666 . ?
O19 Nd1 O39 139.86(14) . 1_566 ?
O19 Nd1 O2W 72.10(15) . . ?
O19 Nd1 O1W 74.28(17) . . ?
O28 Nd1 O19 145.69(14) 1_556 . ?
O28 Nd1 O39 74.37(13) 1_556 1_566 ?
O28 Nd1 O2W 137.89(13) 1_556 . ?
O28 Nd1 O1W 73.09(16) 1_556 . ?
O39 Nd1 O2W 69.99(14) 1_566 . ?
O39 Nd1 O1W 141.03(15) 1_566 . ?
O38 Nd1 O19 81.34(13) 2 . ?
O38 Nd1 O28 79.23(12) 2 1_556 ?
O38 Nd1 O39 120.89(12) 2 1_566 ?
O38 Nd1 O29 72.53(13) 2 2_565 ?
O38 Nd1 O2W 139.09(13) 2 . ?
O38 Nd1 O1W 72.85(14) 2 . ?
O29 Nd1 O19 76.09(13) 2_565 . ?
O29 Nd1 O28 123.42(12) 2_565 1_556 ?
O29 Nd1 O39 79.73(13) 2_565 1_566 ?
O29 Nd1 O2W 71.25(13) 2_565 . ?
O29 Nd1 O1W 137.05(14) 2_565 . ?
O1W Nd1 O2W 125.92(16) . . ?
C17 O18 Nd1 179.4(3) . 2_666 ?
C17 O19 Nd1 130.4(3) . . ?
C27 O28 Nd1 135.4(3) . 1_554 ?
C37 O39 Nd1 110.5(3) . 1_544 ?
O39 C37 C34 118.3(4) . . ?
O39 C37 O38 123.8(5) . . ?
O38 C37 C34 117.9(4) . . ?
C32 N31 C30 119.6(4) . . ?
C36 N31 C30 118.4(4) . . ?
C36 N31 C32 121.7(4) . . ?
C12 N11 C10 116.7(4) . . ?
C16 N11 C12 121.1(4) . . ?
C16 N11 C10 122.2(4) . . ?
C35 C34 C37 119.5(5) . . ?
C35 C34 C33 118.4(5) . . ?
C33 C34 C37 122.0(5) . . ?
C2 C1 C10 118.9(5) . . ?
C6 C1 C2 121.0(5) . . ?
C6 C1 C10 120.0(5) . . ?
O18 C17 C14 117.2(4) . . ?
O19 C17 O18 126.1(4) . . ?
O19 C17 C14 116.8(4) . . ?
C2 C3 C20 119.7(5) . . ?
C2 C3 C4 121.0(5) . . ?
C4 C3 C20 119.2(5) . . ?
C3 C20 H20A 109.1 . . ?
C3 C20 H20B 109.1 . . ?
H20A C20 H20B 107.9 . . ?
N21 C20 C3 112.3(4) . . ?
N21 C20 H20A 109.1 . . ?
N21 C20 H20B 109.1 . . ?
N11 C12 H12 120.0 . . ?
N11 C12 C13 120.1(5) . . ?
C13 C12 H12 120.0 . . ?
N11 C16 H16 119.8 . . ?
N11 C16 C15 120.3(4) . . ?
C15 C16 H16 119.8 . . ?
C1 C2 C7 120.3(5) . . ?
C3 C2 C1 119.0(5) . . ?
C3 C2 C7 120.7(5) . . ?
C22 N21 C20 120.0(4) . . ?
C22 N21 C26 121.7(4) . . ?
C26 N21 C20 118.2(4) . . ?
C16 C15 H15 120.2 . . ?
C16 C15 C14 119.6(4) . . ?
C14 C15 H15 120.2 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C4 C8 H8A 109.5 . . ?
C4 C8 H8B 109.5 . . ?
C4 C8 H8C 109.5 . . ?
C34 C35 H35 120.2 . . ?
C36 C35 C34 119.6(5) . . ?
C36 C35 H35 120.2 . . ?
N31 C30 H30A 109.0 . . ?
N31 C30 H30B 109.0 . . ?
N31 C30 C5 112.9(4) . . ?
H30A C30 H30B 107.8 . . ?
C5 C30 H30A 109.0 . . ?
C5 C30 H30B 109.0 . . ?
N31 C32 H32 120.0 . . ?
N31 C32 C33 120.1(5) . . ?
C33 C32 H32 120.0 . . ?
O28 C27 C24 117.3(4) . . ?
O28 C27 O29 127.5(5) . . ?
O29 C27 C24 115.2(4) . . ?
C34 C33 H33 120.0 . . ?
C32 C33 C34 120.0(5) . . ?
C32 C33 H33 120.0 . . ?
C24 C23 H23 120.6 . . ?
C22 C23 H23 120.6 . . ?
C22 C23 C24 118.8(5) . . ?
C12 C13 H13 120.0 . . ?
C14 C13 C12 119.9(5) . . ?
C14 C13 H13 120.0 . . ?
C1 C6 C5 118.8(5) . . ?
C1 C6 C9 119.6(5) . . ?
C5 C6 C9 121.6(5) . . ?
N31 C36 C35 120.1(5) . . ?
N31 C36 H36 119.9 . . ?
C35 C36 H36 119.9 . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C15 C14 C17 119.7(4) . . ?
C13 C14 C17 121.5(4) . . ?
C13 C14 C15 118.8(4) . . ?
C23 C24 C27 121.0(5) . . ?
C25 C24 C27 120.3(4) . . ?
C25 C24 C23 118.7(5) . . ?
N21 C22 C23 120.8(5) . . ?
N21 C22 H22 119.6 . . ?
C23 C22 H22 119.6 . . ?
C3 C4 C8 119.8(5) . . ?
C5 C4 C3 119.4(5) . . ?
C5 C4 C8 120.8(5) . . ?
C6 C5 C30 121.0(5) . . ?
C4 C5 C30 118.4(5) . . ?
C4 C5 C6 120.6(5) . . ?
N21 C26 H26 120.2 . . ?
N21 C26 C25 119.6(5) . . ?
C25 C26 H26 120.2 . . ?
N11 C10 C1 114.4(4) . . ?
N11 C10 H10A 108.7 . . ?
N11 C10 H10B 108.7 . . ?
C1 C10 H10A 108.7 . . ?
C1 C10 H10B 108.7 . . ?
H10A C10 H10B 107.6 . . ?
C24 C25 H25 119.8 . . ?
C26 C25 C24 120.4(5) . . ?
C26 C25 H25 119.8 . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C37 O38 Nd1 174.2(3) . 2 ?
C27 O29 Nd1 136.0(3) . 2_565 ?
Nd1 O2W H2WA 111.5 . . ?
Nd1 O2W H2WB 111.8 . . ?
H2WA O2W H2WB 107.3 . . ?
Nd1 O1W H1WA 112.8 . . ?
Nd1 O1W H1WB 112.4 . . ?
H1WA O1W H1WB 106.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Nd1 O19 C17 O18 -7.9(8) . . . . ?
Nd1 O19 C17 C14 172.2(3) . . . . ?
Nd1 O28 C27 C24 -167.9(3) 1_554 . . . ?
Nd1 O28 C27 O29 11.2(9) 1_554 . . . ?
Nd1 O39 C37 C34 167.2(4) 1_544 . . . ?
Nd1 O39 C37 O38 -9.6(6) 1_544 . . . ?
O18 C17 C14 C15 172.0(5) . . . . ?
O18 C17 C14 C13 -5.7(7) . . . . ?
O19 C17 C14 C15 -8.1(7) . . . . ?
O19 C17 C14 C13 174.2(5) . . . . ?
O28 C27 C24 C23 -18.0(7) . . . . ?
O28 C27 C24 C25 159.3(5) . . . . ?
O28 C27 O29 Nd1 -55.0(8) . . . 2_565 ?
O39 C37 C34 C35 -12.7(7) . . . . ?
O39 C37 C34 C33 170.8(5) . . . . ?
C37 C34 C35 C36 -172.8(5) . . . . ?
C37 C34 C33 C32 172.8(5) . . . . ?
N31 C30 C5 C6 -101.5(6) . . . . ?
N31 C30 C5 C4 80.7(6) . . . . ?
N31 C32 C33 C34 0.6(8) . . . . ?
N11 C12 C13 C14 -1.3(8) . . . . ?
N11 C16 C15 C14 -0.8(8) . . . . ?
C34 C35 C36 N31 -0.8(9) . . . . ?
C1 C6 C5 C30 -179.9(4) . . . . ?
C1 C6 C5 C4 -2.1(7) . . . . ?
C3 C20 N21 C22 -44.9(7) . . . . ?
C3 C20 N21 C26 138.7(5) . . . . ?
C3 C4 C5 C30 177.6(4) . . . . ?
C3 C4 C5 C6 -0.2(7) . . . . ?
C20 C3 C2 C1 174.3(4) . . . . ?
C20 C3 C2 C7 -4.6(7) . . . . ?
C20 C3 C4 C8 6.5(7) . . . . ?
C20 C3 C4 C5 -175.0(4) . . . . ?
C20 N21 C22 C23 -175.2(5) . . . . ?
C20 N21 C26 C25 176.4(5) . . . . ?
C12 N11 C16 C15 -1.6(8) . . . . ?
C12 N11 C10 C1 174.9(5) . . . . ?
C12 C13 C14 C17 176.6(5) . . . . ?
C12 C13 C14 C15 -1.1(8) . . . . ?
C16 N11 C12 C13 2.7(8) . . . . ?
C16 N11 C10 C1 -4.4(8) . . . . ?
C16 C15 C14 C17 -175.6(5) . . . . ?
C16 C15 C14 C13 2.1(8) . . . . ?
C2 C1 C6 C5 1.4(7) . . . . ?
C2 C1 C6 C9 -179.7(5) . . . . ?
C2 C1 C10 N11 79.9(6) . . . . ?
C2 C3 C20 N21 105.6(5) . . . . ?
C2 C3 C4 C8 -175.1(5) . . . . ?
C2 C3 C4 C5 3.4(7) . . . . ?
N21 C26 C25 C24 -0.8(9) . . . . ?
C8 C4 C5 C30 -3.9(7) . . . . ?
C8 C4 C5 C6 178.2(5) . . . . ?
C35 C34 C33 C32 -3.7(8) . . . . ?
C30 N31 C32 C33 -171.1(5) . . . . ?
C30 N31 C36 C35 171.3(5) . . . . ?
C32 N31 C30 C5 -121.7(5) . . . . ?
C32 N31 C36 C35 -2.5(8) . . . . ?
C27 C24 C25 C26 -177.0(5) . . . . ?
C33 C34 C35 C36 3.8(8) . . . . ?
C23 C24 C25 C26 0.4(9) . . . . ?
C6 C1 C2 C3 1.7(7) . . . . ?
C6 C1 C2 C7 -179.4(5) . . . . ?
C6 C1 C10 N11 -102.9(6) . . . . ?
C36 N31 C30 C5 64.3(6) . . . . ?
C36 N31 C32 C33 2.6(8) . . . . ?
C24 C27 O29 Nd1 124.2(4) . . . 2_565 ?
C24 C23 C22 N21 -1.4(8) . . . . ?
C22 N21 C26 C25 0.1(8) . . . . ?
C22 C23 C24 C27 178.0(5) . . . . ?
C22 C23 C24 C25 0.7(8) . . . . ?
C4 C3 C20 N21 -76.0(6) . . . . ?
C4 C3 C2 C1 -4.1(7) . . . . ?
C4 C3 C2 C7 176.9(5) . . . . ?
C26 N21 C22 C23 1.0(8) . . . . ?
C10 N11 C12 C13 -176.6(5) . . . . ?
C10 N11 C16 C15 177.6(5) . . . . ?
C10 C1 C2 C3 178.9(4) . . . . ?
C10 C1 C2 C7 -2.1(7) . . . . ?
C10 C1 C6 C5 -175.8(4) . . . . ?
C10 C1 C6 C9 3.1(7) . . . . ?
C9 C6 C5 C30 1.3(8) . . . . ?
C9 C6 C5 C4 179.0(5) . . . . ?
O38 C37 C34 C35 164.2(5) . . . . ?
O38 C37 C34 C33 -12.3(8) . . . . ?
O29 C27 C24 C23 162.7(5) . . . . ?
O29 C27 C24 C25 -20.0(7) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.471 0.000 0.500 475.1 151.0 '14x water'

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.369
_oxdiff_exptl_absorpt_empirical_full_min 0.778
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_jj003_tb_otf_h2o_2_red3
_database_code_depnum_ccdc_archive 'CCDC 1833443'
loop_
_audit_author_name
_audit_author_address
'Antti Tiihonen'
;University of Jyv?skyl?, Department of Chemistry
Finland
;
_audit_update_record             
;
2018-03-29 deposited with the CCDC.	2019-02-28 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_CHEMW03_I                   
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as...
RESPONSE: The structure contains voids of unresolved electron density
which was treated using Olex2 solvent mask procedure (full details in 
_smtbx_masks_special_details). The 8 water molecules per asymmetric unit 
 are included in the formula and used in the calculations. 
;
_vrf_PLAT412_I                   
;
PROBLEM: Short Intra XH3 .. XHn...
RESPONSE: Hydrogen atoms calculated using a riding model in their general
(unoptimized) geometry causing a proximity alert.
;
_vrf_PLAT420_I                   
;
PROBLEM: D-H Without Acceptor...
RESPONSE: Hydrogen bond acceptors (water) have been removed among
other disordered solvent from the voids (see CHEMW03_ALERT_2_A).
;
_vrf_PLAT973_I                   
;
PROBLEM: Check Calcd Positive Resid. Density on Tb1...
RESPONSE: Peak is located about 0.6 angstroms from the Tb1 atom
and is caused by the absorption effects. Data is recorded with Cu
radiation.
;
_vrf_FORMU01_I                   
;
PROBLEM: There is a discrepancy between the atom counts...
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_CELLZ01_I                   
;
PROBLEM: Difference between formula and atom_site...
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT041_I                   
;
PROBLEM: Calc. and Reported SumFormula Strings  Differ...
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT042_I                   
;
PROBLEM: Calc. and Reported MoietyFormula Strings  Differ...
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT044_I                   
;
PROBLEM: Calculated and Reported Density Dx Differ...
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT051_I                   
;
PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs...
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT068_I                   
;
PROBLEM: Reported F000 Differs from Calcd (or Missing)...
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT606_I                   
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure...
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
# end Validation Reply Form
_audit_creation_date             2018-03-28
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C30 H31 N3 O8 Tb, 1.58(C F3 O3 S), 1.42(Br), 0.42(O)'
_chemical_formula_sum            'C31.58 H47 Br1.42 F4.73 N3 O21.15 S1.58 Tb'
_chemical_formula_weight         1220.21
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C20 N3 O9 H25 F6 S2 Tb1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -9.1472 9.1891 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   18.5943(2)
_cell_length_b                   25.8101(4)
_cell_length_c                   9.77200(13)
_cell_angle_alpha                90
_cell_angle_beta                 102.3429(13)
_cell_angle_gamma                90
_cell_volume                     4581.37(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7639
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      76.3460
_cell_measurement_theta_min      2.9380
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    10.608
_exptl_absorpt_correction_T_max  0.836
_exptl_absorpt_correction_T_min  0.699
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.769
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2437
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
12 -4 -1 0.0203
6 12 -4 0.0560
4 9 4 0.0346
0 -5 6 0.0425
-4 15 -1 0.0493
4 -15 1 0.0476
-3 6 6 0.0374
-2 -16 -1 0.0419
11 8 0 0.0445
3 16 1 0.0492
-12 2 1 0.0228
1 1 -6 0.0415

_exptl_crystal_size_max          0.101
_exptl_crystal_size_mid          0.085
_exptl_crystal_size_min          0.049
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
11.9997 -3.9991 -1.0004 -0.2647 0.7894 -0.5964
5.9997 12.0006 -3.9996 -0.9101 0.3225 0.3401
3.9998 8.9992 4.0004 0.2773 0.7708 0.4925
-0.0000 -5.0009 5.9999 0.9230 0.4110 -0.0767
-4.0000 14.9995 -0.9993 -0.3880 -0.1647 0.8882
4.0000 -14.9995 0.9993 0.3880 0.1647 -0.8882
-3.0000 5.9986 6.0004 0.7393 0.3446 0.5999
-1.9998 -15.9994 -1.0007 0.2455 -0.4782 -0.8303
10.9996 8.0003 0.0002 -0.3700 0.9744 0.1073
2.9998 15.9995 1.0007 -0.2635 0.5557 0.8011
-11.9996 1.9992 1.0003 0.3079 -0.8197 0.4893
1.0000 1.0011 -6.0001 -0.8546 -0.3939 -0.1667

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_unetI/netI     0.0538
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            15165
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.995
_diffrn_reflns_theta_min         2.975
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     14.00  63.00   1.00    2.00    --   41.90  77.00   0.00   49
  2  ω     90.00 175.00   1.00    8.00    --  112.00  45.00  60.00   85
  3  ω     54.00 108.00   1.00    8.00    --  112.00-111.00 -30.00   54
  4  ω     43.00  97.00   1.00    8.00    --  112.00 -45.00 -60.00   54
  5  ω     37.00  84.00   1.00    8.00    --  112.00 -34.00-113.00   47
  6  ω     36.00  91.00   1.00    8.00    --  112.00 -30.00 120.00   55
  7  ω     40.00 138.00   1.00    8.00    --  112.00 -77.00 150.00   98
  8  ω    -98.00 -44.00   1.00    2.00    --  -41.90 -37.00-180.00   54
  9  ω   -113.00 -17.00   1.00    2.00    --  -41.90 -77.00 120.00   96
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0179333000
_diffrn_orient_matrix_UB_12      -0.0216006000
_diffrn_orient_matrix_UB_13      0.1358388000
_diffrn_orient_matrix_UB_21      0.0775860000
_diffrn_orient_matrix_UB_22      0.0151156000
_diffrn_orient_matrix_UB_23      0.0811028000
_diffrn_orient_matrix_UB_31      -0.0291975000
_diffrn_orient_matrix_UB_32      0.0535506000
_diffrn_orient_matrix_UB_33      0.0318431000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7099
_reflns_number_total             8286
_reflns_odcompleteness_completeness 99.39
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         1.787
_refine_diff_density_min         -1.704
_refine_diff_density_rms         0.149
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     556
_refine_ls_number_reflns         8286
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0637
_refine_ls_R_factor_gt           0.0571
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1033P)²+7.2275P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1567
_refine_ls_wR_factor_ref         0.1651
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Others
 Sof(Br2B)=Sof(O3B)=1-FVAR(1)
 Sof(F54A)=Sof(F53A)=Sof(F55A)=Sof(C52A)=Sof(S48A)=Sof(O51A)=Sof(O49A)=
 Sof(O50A)=FVAR(1)
3.a Rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
3.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C30(H30A,H30B), C20(H20A,H20B)
3.c Aromatic/amide H refined with riding coordinates:
 C33(H33), C35(H35), C23(H23), C15(H15), C12(H12), C16(H16), C25(H25),
 C32(H32), C13(H13), C36(H36), C22(H22), C26(H26)
3.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.88082(2) 0.25094(2) 1.22984(3) 0.01566(13) Uani 1 1 d . . . . .
S40 S 0.49612(9) 0.14802(6) 0.86308(15) 0.0364(3) Uani 1 1 d . . . . .
O28 O 0.1760(2) 0.67809(15) 0.6716(4) 0.0279(8) Uani 1 1 d . . . . .
O18 O 0.8024(2) 0.28722(19) 1.0369(4) 0.0366(10) Uani 1 1 d . . . . .
O19 O 0.77831(19) 0.28537(17) 0.8039(4) 0.0320(9) Uani 1 1 d . . . . .
O29 O 0.1521(2) 0.68647(17) 0.4383(4) 0.0329(9) Uani 1 1 d . . . . .
F47 F 0.5384(2) 0.23195(18) 0.7539(5) 0.0527(10) Uani 1 1 d . . . . .
F46 F 0.5600(4) 0.2324(2) 0.9759(6) 0.0844(19) Uani 1 1 d . . . . .
F45 F 0.6268(2) 0.1870(2) 0.8682(6) 0.0702(14) Uani 1 1 d . . . . .
O43 O 0.4978(3) 0.1229(2) 0.7353(5) 0.0513(13) Uani 1 1 d . . . . .
N31 N 0.2275(2) 0.31333(17) 0.5327(5) 0.0240(9) Uani 1 1 d . . . . .
N11 N 0.5596(2) 0.37141(17) 0.9151(4) 0.0227(9) Uani 1 1 d . . . . .
C8 C 0.2864(3) 0.4158(2) 0.3833(6) 0.0336(12) Uani 1 1 d . . . . .
H8A H 0.311884 0.404934 0.310066 0.050 Uiso 1 1 calc GR . . . .
H8B H 0.269674 0.451683 0.366503 0.050 Uiso 1 1 calc GR . . . .
H8C H 0.243856 0.393207 0.381747 0.050 Uiso 1 1 calc GR . . . .
C4 C 0.3383(3) 0.4120(2) 0.5241(6) 0.0265(11) Uani 1 1 d . . . . .
O41 O 0.5271(5) 0.1187(2) 0.9830(6) 0.078(2) Uani 1 1 d . . . . .
C44 C 0.5584(4) 0.2032(3) 0.8670(7) 0.0414(14) Uani 1 1 d . . . . .
C33 C 0.1311(3) 0.3149(2) 0.6566(5) 0.0251(10) Uani 1 1 d . . . . .
H33 H 0.113974 0.322737 0.739105 0.030 Uiso 1 1 calc R . . . .
C17 C 0.7629(2) 0.2953(2) 0.9189(5) 0.0245(11) Uani 1 1 d . . . . .
C5 C 0.3450(2) 0.36575(19) 0.6012(6) 0.0236(10) Uani 1 1 d . . . . .
C7 C 0.4843(4) 0.4955(3) 0.7598(10) 0.068(3) Uani 1 1 d . . . . .
H7A H 0.477211 0.523171 0.689487 0.102 Uiso 1 1 calc GR . . . .
H7B H 0.535625 0.483841 0.778351 0.102 Uiso 1 1 calc GR . . . .
H7C H 0.472617 0.508639 0.846595 0.102 Uiso 1 1 calc GR . . . .
C6 C 0.3924(3) 0.3623(2) 0.7338(6) 0.0269(11) Uani 1 1 d . . . . .
C14 C 0.6897(2) 0.3216(2) 0.9163(5) 0.0205(10) Uani 1 1 d . . . . .
C35 C 0.1091(3) 0.2837(2) 0.4213(5) 0.0301(12) Uani 1 1 d . . . . .
H35 H 0.076654 0.270628 0.340030 0.036 Uiso 1 1 calc R . . . .
C23 C 0.2602(3) 0.5881(2) 0.6492(7) 0.0360(13) Uani 1 1 d . . . . .
H23 H 0.248678 0.594006 0.738055 0.043 Uiso 1 1 calc R . . . .
C15 C 0.6712(3) 0.3354(2) 1.0419(5) 0.0227(10) Uani 1 1 d . . . . .
H15 H 0.703035 0.327216 1.128938 0.027 Uiso 1 1 calc R . . . .
C12 C 0.5767(3) 0.3581(2) 0.7929(5) 0.0245(10) Uani 1 1 d . . . . .
H12 H 0.543962 0.366475 0.707077 0.029 Uiso 1 1 calc R . . . .
C16 C 0.6056(3) 0.3611(2) 1.0377(5) 0.0249(10) Uani 1 1 d . . . . .
H16 H 0.592988 0.371735 1.122654 0.030 Uiso 1 1 calc R . . . .
C25 C 0.2464(4) 0.6086(2) 0.4068(7) 0.0388(13) Uani 1 1 d . . . . .
H25 H 0.225090 0.629125 0.327761 0.047 Uiso 1 1 calc R . . . .
C10 C 0.4907(3) 0.4022(3) 0.9209(7) 0.0435(17) Uani 1 1 d . . . . .
H10A H 0.465957 0.386131 0.990428 0.052 Uiso 1 1 calc R . . . .
H10B H 0.505126 0.437850 0.953114 0.052 Uiso 1 1 calc R . . . .
C3 C 0.3833(3) 0.4540(2) 0.5764(7) 0.0318(12) Uani 1 1 d . . . . .
C27 C 0.1811(3) 0.6653(2) 0.5509(5) 0.0234(10) Uani 1 1 d . . . . .
O42 O 0.4265(4) 0.1723(3) 0.8622(10) 0.101(3) Uani 1 1 d . . . . .
C30 C 0.3073(3) 0.3181(2) 0.5307(6) 0.0273(11) Uani 1 1 d . . . . .
H30A H 0.312491 0.317887 0.431943 0.033 Uiso 1 1 calc R . . . .
H30B H 0.333216 0.287127 0.576793 0.033 Uiso 1 1 calc R . . . .
C32 C 0.2025(3) 0.3252(2) 0.6497(5) 0.0259(10) Uani 1 1 d . . . . .
H32 H 0.234726 0.340813 0.727358 0.031 Uiso 1 1 calc R . . . .
C13 C 0.6414(3) 0.3323(2) 0.7912(5) 0.0243(10) Uani 1 1 d . . . . .
H13 H 0.652706 0.321996 0.704849 0.029 Uiso 1 1 calc R . . . .
C20 C 0.3813(3) 0.5016(2) 0.4869(8) 0.0442(18) Uani 1 1 d . . . . .
H20A H 0.430043 0.518679 0.510125 0.053 Uiso 1 1 calc R . . . .
H20B H 0.372230 0.490932 0.387343 0.053 Uiso 1 1 calc R . . . .
C34 C 0.0838(2) 0.2927(2) 0.5416(5) 0.0206(10) Uani 1 1 d . . . . .
C1 C 0.4374(3) 0.4049(2) 0.7820(6) 0.0338(13) Uani 1 1 d . . . . .
N21 N 0.3233(3) 0.53994(19) 0.5052(6) 0.0373(12) Uani 1 1 d . . . . .
C36 C 0.1820(3) 0.2936(2) 0.4191(6) 0.0313(12) Uani 1 1 d . . . . .
H36 H 0.199887 0.286555 0.336990 0.038 Uiso 1 1 calc R . . . .
C22 C 0.3075(4) 0.5484(2) 0.6316(7) 0.0397(14) Uani 1 1 d . . . . .
H22 H 0.328825 0.527030 0.708847 0.048 Uiso 1 1 calc R . . . .
C24 C 0.2301(3) 0.6189(2) 0.5366(6) 0.0277(11) Uani 1 1 d . . . . .
C26 C 0.2933(4) 0.5689(3) 0.3933(8) 0.0442(15) Uani 1 1 d . . . . .
H26 H 0.304536 0.561831 0.304800 0.053 Uiso 1 1 calc R . . . .
C9 C 0.3966(3) 0.3136(3) 0.8188(7) 0.0407(14) Uani 1 1 d . . . . .
H9A H 0.348560 0.296358 0.798796 0.061 Uiso 1 1 calc GR . . . .
H9B H 0.410265 0.322259 0.918676 0.061 Uiso 1 1 calc GR . . . .
H9C H 0.433733 0.290459 0.794574 0.061 Uiso 1 1 calc GR . . . .
C2 C 0.4340(3) 0.4505(2) 0.7056(8) 0.0404(15) Uani 1 1 d . . . . .
O38 O -0.00696(17) 0.27346(15) 0.6683(3) 0.0230(7) Uani 1 1 d . . . . .
C37 C 0.0068(2) 0.27607(18) 0.5479(5) 0.0167(9) Uani 1 1 d . . . . .
O39 O -0.03595(18) 0.26591(16) 0.4358(4) 0.0246(7) Uani 1 1 d . . . . .
O1W O 0.9214(3) 0.16712(18) 1.3388(5) 0.0451(11) Uani 1 1 d . . . . .
H1WA H 0.923559 0.143471 1.274807 0.068 Uiso 1 1 d GR . . . .
H1WB H 0.890860 0.155961 1.390088 0.068 Uiso 1 1 d GR . . . .
O2W O 0.9407(2) 0.33075(18) 1.1815(5) 0.0441(11) Uani 1 1 d . . . . .
H2WA H 0.991383 0.336240 1.185206 0.066 Uiso 1 1 d GR . . . .
H2WB H 0.918493 0.363210 1.154741 0.066 Uiso 1 1 d GR . . . .
Br1 Br 1.09648(6) 0.34515(4) 1.05747(10) 0.0698(3) Uani 1 1 d . . . . .
F54A F 0.7732(5) 0.5636(4) 0.9584(11) 0.075(3) Uani 0.577(5) 1 d . . P A 1
F53A F 0.6614(5) 0.5868(3) 0.9562(11) 0.070(2) Uani 0.577(5) 1 d . . P A 1
F55A F 0.7366(5) 0.5700(3) 1.1473(10) 0.069(2) Uani 0.577(5) 1 d . . P A 1
C52A C 0.7156(7) 0.5543(5) 1.0204(15) 0.053(3) Uani 0.577(5) 1 d . . P A 1
S48A S 0.6863(5) 0.4892(2) 0.9959(10) 0.0265(13) Uani 0.577(5) 1 d . . P A 1
O51A O 0.7524(4) 0.4606(3) 1.0712(8) 0.0427(18) Uani 0.577(5) 1 d . . P A 1
O49A O 0.6274(4) 0.4855(4) 1.0672(8) 0.043(2) Uani 0.577(5) 1 d . . P A 1
O50A O 0.6707(4) 0.4816(4) 0.8513(8) 0.054(3) Uani 0.577(5) 1 d . . P A 1
Br2B Br 0.6790(4) 0.4853(2) 0.9772(7) 0.0576(19) Uani 0.423(5) 1 d . . P A 2
O3B O 0.7448(10) 0.6222(8) 1.0302(15) 0.086(5) Uani 0.423(5) 1 d . . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O28 2.415(4) 3_667 ?
Tb1 O18 2.321(4) . ?
Tb1 O19 2.372(3) 4_566 ?
Tb1 O29 2.327(4) 2_646 ?
Tb1 O38 2.377(3) 4_666 ?
Tb1 O39 2.294(3) 1_656 ?
Tb1 O1W 2.458(4) . ?
Tb1 O2W 2.435(4) . ?
S40 O43 1.414(5) . ?
S40 O41 1.411(6) . ?
S40 C44 1.832(7) . ?
S40 O42 1.436(6) . ?
O28 C27 1.248(6) . ?
O18 C17 1.245(6) . ?
O19 C17 1.245(6) . ?
O29 C27 1.243(6) . ?
F47 C44 1.317(8) . ?
F46 C44 1.299(8) . ?
F45 C44 1.338(8) . ?
N31 C30 1.492(6) . ?
N31 C32 1.359(7) . ?
N31 C36 1.343(7) . ?
N11 C12 1.345(7) . ?
N11 C16 1.341(7) . ?
N11 C10 1.519(6) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C8 C4 1.505(8) . ?
C4 C5 1.403(8) . ?
C4 C3 1.398(7) . ?
C33 H33 0.9500 . ?
C33 C32 1.369(7) . ?
C33 C34 1.393(7) . ?
C17 C14 1.517(6) . ?
C5 C6 1.405(8) . ?
C5 C30 1.509(7) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C7 C2 1.515(8) . ?
C6 C1 1.401(8) . ?
C6 C9 1.499(9) . ?
C14 C15 1.389(7) . ?
C14 C13 1.381(7) . ?
C35 H35 0.9500 . ?
C35 C34 1.376(7) . ?
C35 C36 1.384(7) . ?
C23 H23 0.9500 . ?
C23 C22 1.385(8) . ?
C23 C24 1.376(8) . ?
C15 H15 0.9500 . ?
C15 C16 1.382(7) . ?
C12 H12 0.9500 . ?
C12 C13 1.378(7) . ?
C16 H16 0.9500 . ?
C25 H25 0.9500 . ?
C25 C24 1.391(8) . ?
C25 C26 1.371(9) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C1 1.502(8) . ?
C3 C20 1.504(9) . ?
C3 C2 1.407(9) . ?
C27 C24 1.528(7) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C32 H32 0.9500 . ?
C13 H13 0.9500 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 N21 1.503(7) . ?
C34 C37 1.509(6) . ?
C1 C2 1.387(10) . ?
N21 C22 1.348(9) . ?
N21 C26 1.343(9) . ?
C36 H36 0.9500 . ?
C22 H22 0.9500 . ?
C26 H26 0.9500 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
O38 C37 1.258(6) . ?
C37 O39 1.236(6) . ?
O1W H1WA 0.8810 . ?
O1W H1WB 0.8819 . ?
O2W H2WA 0.9459 . ?
O2W H2WB 0.9458 . ?
F54A C52A 1.361(16) . ?
F53A C52A 1.358(17) . ?
F55A C52A 1.284(16) . ?
C52A S48A 1.767(15) . ?
S48A O51A 1.487(11) . ?
S48A O49A 1.422(11) . ?
S48A O50A 1.394(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O28 Tb1 O1W 127.92(15) 3_667 . ?
O28 Tb1 O2W 72.12(15) 3_667 . ?
O18 Tb1 O28 76.45(13) . 3_667 ?
O18 Tb1 O19 90.04(14) . 4_566 ?
O18 Tb1 O29 71.93(16) . 2_646 ?
O18 Tb1 O38 109.56(12) . 4_666 ?
O18 Tb1 O1W 142.06(16) . . ?
O18 Tb1 O2W 74.64(17) . . ?
O19 Tb1 O28 74.31(14) 4_566 3_667 ?
O19 Tb1 O38 141.15(15) 4_566 4_666 ?
O19 Tb1 O1W 73.27(16) 4_566 . ?
O19 Tb1 O2W 145.50(16) 4_566 . ?
O29 Tb1 O28 138.81(14) 2_646 3_667 ?
O29 Tb1 O19 79.94(13) 2_646 4_566 ?
O29 Tb1 O38 75.21(13) 2_646 4_666 ?
O29 Tb1 O1W 71.73(15) 2_646 . ?
O29 Tb1 O2W 122.02(15) 2_646 . ?
O38 Tb1 O28 141.65(13) 4_666 3_667 ?
O38 Tb1 O1W 70.83(15) 4_666 . ?
O38 Tb1 O2W 73.29(15) 4_666 . ?
O39 Tb1 O28 78.04(13) 1_656 3_667 ?
O39 Tb1 O18 146.51(16) 1_656 . ?
O39 Tb1 O19 103.54(13) 1_656 4_566 ?
O39 Tb1 O29 140.02(15) 1_656 2_646 ?
O39 Tb1 O38 78.62(12) 1_656 4_666 ?
O39 Tb1 O1W 71.40(15) 1_656 . ?
O39 Tb1 O2W 77.14(15) 1_656 . ?
O2W Tb1 O1W 135.89(16) . . ?
O43 S40 C44 104.0(3) . . ?
O43 S40 O42 112.7(5) . . ?
O41 S40 O43 113.9(4) . . ?
O41 S40 C44 104.8(4) . . ?
O41 S40 O42 116.5(5) . . ?
O42 S40 C44 103.1(4) . . ?
C27 O28 Tb1 134.9(3) . 3_667 ?
C17 O18 Tb1 164.6(4) . . ?
C17 O19 Tb1 135.4(3) . 4_565 ?
C27 O29 Tb1 159.7(4) . 2_656 ?
C32 N31 C30 120.8(4) . . ?
C36 N31 C30 118.2(4) . . ?
C36 N31 C32 120.8(4) . . ?
C12 N11 C10 121.9(4) . . ?
C16 N11 C12 121.0(4) . . ?
C16 N11 C10 116.9(4) . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C4 C8 H8A 109.5 . . ?
C4 C8 H8B 109.5 . . ?
C4 C8 H8C 109.5 . . ?
C5 C4 C8 120.8(5) . . ?
C3 C4 C8 120.1(5) . . ?
C3 C4 C5 119.0(5) . . ?
F47 C44 S40 110.9(5) . . ?
F47 C44 F45 106.3(6) . . ?
F46 C44 S40 111.8(5) . . ?
F46 C44 F47 108.3(6) . . ?
F46 C44 F45 108.7(7) . . ?
F45 C44 S40 110.7(5) . . ?
C32 C33 H33 120.3 . . ?
C32 C33 C34 119.4(5) . . ?
C34 C33 H33 120.3 . . ?
O18 C17 C14 116.1(4) . . ?
O19 C17 O18 126.7(4) . . ?
O19 C17 C14 117.1(4) . . ?
C4 C5 C6 121.0(5) . . ?
C4 C5 C30 118.0(5) . . ?
C6 C5 C30 120.6(5) . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
C5 C6 C9 120.8(5) . . ?
C1 C6 C5 118.2(5) . . ?
C1 C6 C9 121.0(5) . . ?
C15 C14 C17 119.3(4) . . ?
C13 C14 C17 121.0(4) . . ?
C13 C14 C15 119.7(4) . . ?
C34 C35 H35 120.1 . . ?
C34 C35 C36 119.7(5) . . ?
C36 C35 H35 120.1 . . ?
C22 C23 H23 120.4 . . ?
C24 C23 H23 120.4 . . ?
C24 C23 C22 119.3(6) . . ?
C14 C15 H15 120.7 . . ?
C16 C15 C14 118.7(4) . . ?
C16 C15 H15 120.7 . . ?
N11 C12 H12 119.8 . . ?
N11 C12 C13 120.5(4) . . ?
C13 C12 H12 119.8 . . ?
N11 C16 C15 120.8(4) . . ?
N11 C16 H16 119.6 . . ?
C15 C16 H16 119.6 . . ?
C24 C25 H25 120.1 . . ?
C26 C25 H25 120.1 . . ?
C26 C25 C24 119.9(6) . . ?
N11 C10 H10A 109.0 . . ?
N11 C10 H10B 109.0 . . ?
H10A C10 H10B 107.8 . . ?
C1 C10 N11 113.0(4) . . ?
C1 C10 H10A 109.0 . . ?
C1 C10 H10B 109.0 . . ?
C4 C3 C20 118.8(5) . . ?
C4 C3 C2 120.8(6) . . ?
C2 C3 C20 120.2(5) . . ?
O28 C27 C24 117.5(4) . . ?
O29 C27 O28 127.9(5) . . ?
O29 C27 C24 114.7(5) . . ?
N31 C30 C5 115.3(4) . . ?
N31 C30 H30A 108.5 . . ?
N31 C30 H30B 108.5 . . ?
C5 C30 H30A 108.5 . . ?
C5 C30 H30B 108.5 . . ?
H30A C30 H30B 107.5 . . ?
N31 C32 C33 120.5(5) . . ?
N31 C32 H32 119.8 . . ?
C33 C32 H32 119.8 . . ?
C14 C13 H13 120.3 . . ?
C12 C13 C14 119.3(4) . . ?
C12 C13 H13 120.3 . . ?
C3 C20 H20A 108.9 . . ?
C3 C20 H20B 108.9 . . ?
H20A C20 H20B 107.7 . . ?
N21 C20 C3 113.5(5) . . ?
N21 C20 H20A 108.9 . . ?
N21 C20 H20B 108.9 . . ?
C33 C34 C37 121.6(4) . . ?
C35 C34 C33 119.1(4) . . ?
C35 C34 C37 119.2(4) . . ?
C6 C1 C10 119.9(6) . . ?
C2 C1 C6 122.0(5) . . ?
C2 C1 C10 118.1(6) . . ?
C22 N21 C20 121.2(6) . . ?
C26 N21 C20 117.0(6) . . ?
C26 N21 C22 121.5(5) . . ?
N31 C36 C35 120.3(5) . . ?
N31 C36 H36 119.9 . . ?
C35 C36 H36 119.9 . . ?
C23 C22 H22 119.9 . . ?
N21 C22 C23 120.1(6) . . ?
N21 C22 H22 119.9 . . ?
C23 C24 C25 119.2(5) . . ?
C23 C24 C27 121.9(5) . . ?
C25 C24 C27 118.9(5) . . ?
C25 C26 H26 120.0 . . ?
N21 C26 C25 120.0(6) . . ?
N21 C26 H26 120.0 . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C3 C2 C7 120.6(6) . . ?
C1 C2 C7 120.6(6) . . ?
C1 C2 C3 118.8(5) . . ?
C37 O38 Tb1 128.0(3) . 4_465 ?
O38 C37 C34 116.0(4) . . ?
O39 C37 C34 117.4(4) . . ?
O39 C37 O38 126.6(4) . . ?
C37 O39 Tb1 176.8(4) . 1_454 ?
Tb1 O1W H1WA 111.0 . . ?
Tb1 O1W H1WB 111.0 . . ?
H1WA O1W H1WB 108.1 . . ?
Tb1 O2W H2WA 127.8 . . ?
Tb1 O2W H2WB 127.7 . . ?
H2WA O2W H2WB 104.5 . . ?
F54A C52A S48A 110.9(10) . . ?
F53A C52A F54A 105.1(12) . . ?
F53A C52A S48A 110.5(9) . . ?
F55A C52A F54A 105.5(11) . . ?
F55A C52A F53A 107.0(11) . . ?
F55A C52A S48A 117.0(12) . . ?
O51A S48A C52A 101.9(8) . . ?
O49A S48A C52A 104.1(7) . . ?
O49A S48A O51A 111.5(7) . . ?
O50A S48A C52A 105.1(8) . . ?
O50A S48A O51A 113.8(6) . . ?
O50A S48A O49A 118.2(8) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Tb1 O28 C27 O29 -4.7(9) 3_667 . . . ?
Tb1 O28 C27 C24 173.8(3) 3_667 . . . ?
Tb1 O18 C17 O19 -44.5(18) . . . . ?
Tb1 O18 C17 C14 137.6(12) . . . . ?
Tb1 O19 C17 O18 -0.6(10) 4_565 . . . ?
Tb1 O19 C17 C14 177.3(4) 4_565 . . . ?
Tb1 O29 C27 O28 54.5(12) 2_656 . . . ?
Tb1 O29 C27 C24 -124.0(9) 2_656 . . . ?
Tb1 O38 C37 C34 -179.7(3) 4_465 . . . ?
Tb1 O38 C37 O39 -0.6(7) 4_465 . . . ?
O28 C27 C24 C23 8.0(8) . . . . ?
O28 C27 C24 C25 -170.0(5) . . . . ?
O18 C17 C14 C15 0.6(8) . . . . ?
O18 C17 C14 C13 -179.8(5) . . . . ?
O19 C17 C14 C15 -177.5(5) . . . . ?
O19 C17 C14 C13 2.1(8) . . . . ?
O29 C27 C24 C23 -173.3(5) . . . . ?
O29 C27 C24 C25 8.7(7) . . . . ?
O43 S40 C44 F47 55.5(5) . . . . ?
O43 S40 C44 F46 176.5(6) . . . . ?
O43 S40 C44 F45 -62.2(6) . . . . ?
N11 C12 C13 C14 -1.9(8) . . . . ?
N11 C10 C1 C6 77.6(7) . . . . ?
N11 C10 C1 C2 -102.9(7) . . . . ?
C8 C4 C5 C6 -178.9(5) . . . . ?
C8 C4 C5 C30 8.6(7) . . . . ?
C8 C4 C3 C20 -2.8(8) . . . . ?
C8 C4 C3 C2 -177.8(5) . . . . ?
C4 C5 C6 C1 -5.2(7) . . . . ?
C4 C5 C6 C9 177.0(5) . . . . ?
C4 C5 C30 N31 -82.9(6) . . . . ?
C4 C3 C20 N21 88.1(7) . . . . ?
C4 C3 C2 C7 178.1(6) . . . . ?
C4 C3 C2 C1 -1.5(8) . . . . ?
O41 S40 C44 F47 175.4(5) . . . . ?
O41 S40 C44 F46 -63.6(6) . . . . ?
O41 S40 C44 F45 57.7(6) . . . . ?
C33 C34 C37 O38 -14.0(7) . . . . ?
C33 C34 C37 O39 166.8(5) . . . . ?
C17 C14 C15 C16 177.4(5) . . . . ?
C17 C14 C13 C12 -177.4(5) . . . . ?
C5 C4 C3 C20 174.0(5) . . . . ?
C5 C4 C3 C2 -1.0(8) . . . . ?
C5 C6 C1 C10 -177.9(4) . . . . ?
C5 C6 C1 C2 2.7(8) . . . . ?
C6 C5 C30 N31 104.5(5) . . . . ?
C6 C1 C2 C7 -179.0(6) . . . . ?
C6 C1 C2 C3 0.6(8) . . . . ?
C14 C15 C16 N11 1.9(8) . . . . ?
C35 C34 C37 O38 163.2(5) . . . . ?
C35 C34 C37 O39 -16.1(7) . . . . ?
C15 C14 C13 C12 2.2(8) . . . . ?
C12 N11 C16 C15 -1.7(8) . . . . ?
C12 N11 C10 C1 13.2(9) . . . . ?
C16 N11 C12 C13 1.6(8) . . . . ?
C16 N11 C10 C1 -171.4(6) . . . . ?
C10 N11 C12 C13 176.8(6) . . . . ?
C10 N11 C16 C15 -177.1(6) . . . . ?
C10 C1 C2 C7 1.6(9) . . . . ?
C10 C1 C2 C3 -178.9(5) . . . . ?
C3 C4 C5 C6 4.4(7) . . . . ?
C3 C4 C5 C30 -168.2(5) . . . . ?
C3 C20 N21 C22 37.2(8) . . . . ?
C3 C20 N21 C26 -149.1(6) . . . . ?
O42 S40 C44 F47 -62.3(6) . . . . ?
O42 S40 C44 F46 58.7(7) . . . . ?
O42 S40 C44 F45 -180.0(6) . . . . ?
C30 N31 C32 C33 -172.0(5) . . . . ?
C30 N31 C36 C35 173.5(6) . . . . ?
C30 C5 C6 C1 167.2(4) . . . . ?
C30 C5 C6 C9 -10.7(7) . . . . ?
C32 N31 C30 C5 -41.9(7) . . . . ?
C32 N31 C36 C35 -2.0(9) . . . . ?
C32 C33 C34 C35 -2.7(8) . . . . ?
C32 C33 C34 C37 174.4(5) . . . . ?
C13 C14 C15 C16 -2.2(8) . . . . ?
C20 C3 C2 C7 3.2(9) . . . . ?
C20 C3 C2 C1 -176.4(5) . . . . ?
C20 N21 C22 C23 172.4(6) . . . . ?
C20 N21 C26 C25 -172.5(6) . . . . ?
C34 C33 C32 N31 -0.9(9) . . . . ?
C34 C35 C36 N31 -1.7(10) . . . . ?
C36 N31 C30 C5 142.7(5) . . . . ?
C36 N31 C32 C33 3.3(8) . . . . ?
C36 C35 C34 C33 4.0(9) . . . . ?
C36 C35 C34 C37 -173.2(5) . . . . ?
C22 C23 C24 C25 1.6(9) . . . . ?
C22 C23 C24 C27 -176.3(5) . . . . ?
C22 N21 C26 C25 1.2(10) . . . . ?
C24 C23 C22 N21 -0.4(9) . . . . ?
C24 C25 C26 N21 0.1(10) . . . . ?
C26 C25 C24 C23 -1.4(9) . . . . ?
C26 C25 C24 C27 176.6(6) . . . . ?
C26 N21 C22 C23 -1.0(10) . . . . ?
C9 C6 C1 C10 0.0(8) . . . . ?
C9 C6 C1 C2 -179.5(5) . . . . ?
C2 C3 C20 N21 -96.9(6) . . . . ?
F54A C52A S48A O51A 63.2(12) . . . . ?
F54A C52A S48A O49A 179.3(10) . . . . ?
F54A C52A S48A O50A -55.7(12) . . . . ?
F53A C52A S48A O51A 179.4(10) . . . . ?
F53A C52A S48A O49A -64.5(12) . . . . ?
F53A C52A S48A O50A 60.4(11) . . . . ?
F55A C52A S48A O51A -57.9(12) . . . . ?
F55A C52A S48A O49A 58.2(12) . . . . ?
F55A C52A S48A O50A -176.8(10) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 -0.693 492.8 141.4 '14x water'
2 0.000 0.500 -0.815 492.8 141.4 '14x water'
3 0.319 0.208 0.635 44.8 11.4 '1x water'
4 0.319 0.292 0.135 44.8 11.7 '1x water'
5 0.681 0.708 0.865 44.8 12.4 '1x water'
6 0.681 0.792 0.365 44.8 12.7 '1x water'

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.378
_oxdiff_exptl_absorpt_empirical_full_min 0.742
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_jj003_br_nd_otf_h2o_acet_evac_ii_red2
_database_code_depnum_ccdc_archive 'CCDC 1842357'
loop_
_audit_author_name
_audit_author_address
'Antti Tiihonen'
;University of Jyv?skyl?, Department of Chemistry
Finland
;
_audit_update_record             
;
2018-05-09 deposited with the CCDC.	2019-02-28 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT601_I                   
;
PROBLEM: Structure Contains Solvent Accessible VOIDS...
RESPONSE: Crystal has been subjected to vacuum and evacuated from
diffuse water previously in a channel. Thus formed void is isolated by
nearby disordered anions, and contains no clear indication of any solvent.
;
# end Validation Reply Form
_audit_creation_date             2018-05-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C30.57 H28.7 F1.72 N3 Nd O8.57 S0.57, 2(Br), 0.43(C1 F3 O3 S1), 1.15(H2 O)'
_chemical_formula_sum            'C31 H31 Br2 F3 N3 Nd O11 S'
_chemical_formula_weight         1014.71
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C33 H30 N3 O12 S1 F3 Nd1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -3.1807 10.9079 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.4141(3)
_cell_length_b                   12.0776(3)
_cell_length_c                   18.7454(5)
_cell_angle_alpha                105.103(2)
_cell_angle_beta                 98.057(2)
_cell_angle_gamma                99.489(2)
_cell_volume                     1991.69(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8785
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      76.1580
_cell_measurement_theta_min      3.8660
_shelx_estimated_absorpt_T_max   0.637
_shelx_estimated_absorpt_T_min   0.259
_exptl_absorpt_coefficient_mu    13.409
_exptl_absorpt_correction_T_max  0.793
_exptl_absorpt_correction_T_min  0.456
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.43c (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.692
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             998
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-6 0 6 0.0183
6 0 -6 0.0183
-2 0 -10 0.0521
2 0 10 0.0521
1 -7 -2 0.0380
-1 7 2 0.0380
1 7 -1 0.0368
-4 0 10 0.0223
3 -7 6 0.0661

_exptl_crystal_size_max          0.138
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.037
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-6.0000 -0.0000 6.0000 -1.0389 0.0273 0.1299
6.0000 0.0000 -6.0000 1.0389 -0.0273 -0.1299
-2.0000 -0.0000 -10.0000 -0.0650 0.8560 -0.4926
2.0000 0.0000 10.0000 0.0650 -0.8560 0.4926
1.0000 -7.0000 -2.0000 0.0209 -0.1149 -0.9781
-1.0000 7.0000 2.0000 -0.0209 0.1149 0.9781
1.0000 7.0000 -1.0000 0.3488 0.1763 0.8902
-4.0000 -0.0000 10.0000 -0.8332 -0.4053 0.3545
3.0000 -7.0000 6.0000 0.1328 -0.8297 -0.5749

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12783
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.989
_diffrn_reflns_theta_min         3.878
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -116.00 -17.00   1.00    2.00    --  -41.65 -37.00  90.00   99
  2  ω   -114.00 -15.00   1.00    2.00    --  -41.65 -57.00-150.00   99
  3  ω    -62.00  23.00   1.00    2.00    --  -41.65  57.00   0.00   85
  4  ω      1.00  83.00   1.00    2.00    --   41.65 -99.00  90.00   82
  5  ω     41.00 141.00   1.00    8.00    --  112.00 -61.00-150.00  100
  6  ω     58.00 116.00   1.00    8.00    --  112.00-111.00 150.00   58
  7  ω     35.00  61.00   1.00    8.00    --  112.00 -94.00 -30.00   26
  8  ω     39.00  90.00   1.00    8.00    --  112.00 -45.00 150.00   51
  9  ω     43.00 129.00   1.00    8.00    --  112.00 -45.00   0.00   86
 10  ω     30.00 106.00   1.00    8.00    --  112.00 -94.00  30.00   76
 11  ω     91.00 176.00   1.00    8.00    --  112.00  30.00 -60.00   85
 12  ω     70.00 101.00   1.00    8.00    --  112.00 -94.00 -30.00   31
 13  ω     30.00  96.00   1.00    8.00    --  112.00 -94.00-180.00   66
 14  ω    114.00 141.00   1.00    8.00    --  112.00 111.00 -60.00   27
 15  ω     77.00 114.00   1.00    8.00    --  112.00-111.00 -90.00   37
 16  ω     60.00 178.00   1.00    8.00    --  112.00  15.00  60.00  118
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1497051000
_diffrn_orient_matrix_UB_12      0.0250949000
_diffrn_orient_matrix_UB_13      -0.0234399000
_diffrn_orient_matrix_UB_21      -0.0751209000
_diffrn_orient_matrix_UB_22      0.0258400000
_diffrn_orient_matrix_UB_23      -0.0705738000
_diffrn_orient_matrix_UB_31      0.0230132000
_diffrn_orient_matrix_UB_32      0.1302635000
_diffrn_orient_matrix_UB_33      0.0446568000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7009
_reflns_number_total             7241
_reflns_odcompleteness_completeness 99.56
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         1.608
_refine_diff_density_min         -1.108
_refine_diff_density_rms         0.095
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     562
_refine_ls_number_reflns         7241
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0367
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0477P)²+3.4615P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0944
_refine_ls_wR_factor_ref         0.0952
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Shared sites
{O1WB, O51A}
{O2WB, O50A}
3. Restrained distances
 H4WA-Br2B
 2.55 with sigma of 0.04
 H4WB-Br1B
 2.55 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
Uanis(O41A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O1WB) = Uanis(O51A)
Uanis(O2WB) = Uanis(O50A)
5. Others
 Sof(S40A)=Sof(F45A)=Sof(F47A)=Sof(F46A)=Sof(C44A)=Sof(Br1B)=Sof(O42A)=
 Sof(O41A)=Sof(H1WA)=Sof(H1WB)=Sof(O2WB)=Sof(H2WA)=Sof(H2WB)=Sof(O43A)=
 Sof(O1WB)=1-FVAR(1)
 Sof(Br2B)=Sof(S48A)=Sof(O49A)=Sof(F54A)=Sof(F53A)=Sof(F55A)=Sof(C52A)=
 Sof(O3WA)=Sof(H3WA)=Sof(H3WB)=Sof(O51A)=Sof(O4WB)=Sof(H4WA)=Sof(H4WB)=
 Sof(O50A)=FVAR(1)
6.a Free rotating group:
 O3WA(H3WA,H3WB), O4WB(H4WA,H4WB)
6.b Rotating group:
 O51A(H1WA,H1WB), O2WB(H2WA,H2WB)
6.c Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C30(H30A,H30B), C10(H10A,H10B)
6.d Aromatic/amide H refined with riding coordinates:
 C26(H26), C35(H35), C32(H32), C33(H33), C22(H22), C25(H25), C23(H23),
 C36(H36), C13(H13), C16(H16), C12(H12), C15(H15)
6.e Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C8(H8A,H8B,H8C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Nd1 Nd 0.23859(2) 0.51295(2) 0.50295(2) 0.02854(9) Uani 1 1 d . . . . .
Br3 Br 0.08760(5) 0.65925(4) 0.89392(3) 0.03173(12) Uani 1 1 d . . . . .
Br2B Br 0.50386(9) 1.32536(7) 0.83888(5) 0.0368(3) Uani 0.5743(17) 1 d D . P A
2
O18 O 0.1294(3) 0.4081(3) 0.58409(17) 0.0347(7) Uani 1 1 d . . . . .
N21 N 0.0459(4) -0.1060(3) 0.82843(18) 0.0213(6) Uani 1 1 d . . . . .
C6 C 0.2124(5) 0.3252(3) 0.9713(2) 0.0223(8) Uani 1 1 d . . . . .
C1 C 0.0747(4) 0.2777(3) 0.9251(2) 0.0215(7) Uani 1 1 d . . . . .
C5 C 0.2908(4) 0.2509(3) 0.99817(19) 0.0211(8) Uani 1 1 d . . . . .
N31 N 0.4385(4) 0.3485(3) 1.12973(17) 0.0192(6) Uani 1 1 d . . . . .
C4 C 0.2341(4) 0.1296(3) 0.9792(2) 0.0204(7) Uani 1 1 d . . . . .
C3 C 0.0970(4) 0.0836(3) 0.9310(2) 0.0204(7) Uani 1 1 d . . . . .
N11 N -0.0133(4) 0.3474(3) 0.81609(19) 0.0256(7) Uani 1 1 d . . . . .
C26 C -0.0735(5) -0.1699(4) 0.7784(2) 0.0274(8) Uani 1 1 d . . . . .
H26 H -0.167776 -0.167758 0.790663 0.033 Uiso 1 1 calc R . . . .
C2 C 0.0172(4) 0.1570(3) 0.9039(2) 0.0211(7) Uani 1 1 d . . . . .
C14 C -0.0028(5) 0.3574(4) 0.6727(2) 0.0280(9) Uani 1 1 d . . . . .
C35 C 0.5692(5) 0.4142(4) 1.2553(2) 0.0288(9) Uani 1 1 d . . . . .
H35 H 0.658641 0.429740 1.290190 0.035 Uiso 1 1 calc R . . . .
C24 C 0.0769(5) -0.2426(4) 0.6933(2) 0.0245(8) Uani 1 1 d . . . . .
C32 C 0.3138(4) 0.3687(3) 1.1528(2) 0.0211(7) Uani 1 1 d . . . . .
H32 H 0.225786 0.353036 1.116863 0.025 Uiso 1 1 calc R . . . .
C20 C 0.0310(5) -0.0473(3) 0.9068(2) 0.0240(8) Uani 1 1 d . . . . .
H20A H 0.080519 -0.084085 0.941865 0.029 Uiso 1 1 calc R . . . .
H20B H -0.074303 -0.059386 0.909988 0.029 Uiso 1 1 calc R . . . .
C33 C 0.3130(4) 0.4118(3) 1.2283(2) 0.0214(7) Uani 1 1 d . . . . .
H33 H 0.224758 0.426530 1.244335 0.026 Uiso 1 1 calc R . . . .
C22 C 0.1799(5) -0.1037(4) 0.8122(2) 0.0265(8) Uani 1 1 d . . . . .
H22 H 0.262888 -0.054695 0.847896 0.032 Uiso 1 1 calc R . . . .
C25 C -0.0615(5) -0.2390(4) 0.7092(2) 0.0286(9) Uani 1 1 d . . . . .
H25 H -0.146637 -0.283227 0.673135 0.034 Uiso 1 1 calc R . . . .
C23 C 0.1989(5) -0.1718(4) 0.7443(2) 0.0284(9) Uani 1 1 d . . . . .
H23 H 0.294200 -0.170039 0.732723 0.034 Uiso 1 1 calc R . . . .
C36 C 0.5659(4) 0.3723(3) 1.1797(2) 0.0232(8) Uani 1 1 d . . . . .
H36 H 0.653568 0.359953 1.162186 0.028 Uiso 1 1 calc R . . . .
C7 C 0.2780(6) 0.4549(4) 0.9915(3) 0.0403(11) Uani 1 1 d . . . . .
H7A H 0.273035 0.479648 0.945583 0.060 Uiso 1 1 calc GR . . . .
H7B H 0.380719 0.470233 1.016811 0.060 Uiso 1 1 calc GR . . . .
H7C H 0.222875 0.498970 1.025268 0.060 Uiso 1 1 calc GR . . . .
C13 C -0.1337(5) 0.3541(4) 0.6985(3) 0.0334(10) Uani 1 1 d . . . . .
H13 H -0.221089 0.354348 0.666397 0.040 Uiso 1 1 calc R . . . .
C30 C 0.4421(4) 0.3018(4) 1.0473(2) 0.0259(8) Uani 1 1 d . . . . .
H30A H 0.500767 0.240265 1.040832 0.031 Uiso 1 1 calc R . . . .
H30B H 0.491808 0.366175 1.030087 0.031 Uiso 1 1 calc R . . . .
C10 C -0.0148(5) 0.3559(4) 0.8972(2) 0.0272(8) Uani 1 1 d . . . . .
H10A H -0.117328 0.333706 0.903404 0.033 Uiso 1 1 calc R . . . .
H10B H 0.024791 0.438192 0.928152 0.033 Uiso 1 1 calc R . . . .
C16 C 0.1142(5) 0.3455(4) 0.7907(2) 0.0287(9) Uani 1 1 d . . . . .
H16 H 0.198949 0.340333 0.822758 0.034 Uiso 1 1 calc R . . . .
C17 C 0.0044(5) 0.3767(4) 0.5955(2) 0.0309(9) Uani 1 1 d . . . . .
C9 C 0.3235(5) 0.0533(4) 1.0101(2) 0.0328(9) Uani 1 1 d . . . . .
H9A H 0.410456 0.049828 0.987056 0.049 Uiso 1 1 calc GR . . . .
H9B H 0.263728 -0.025977 0.998515 0.049 Uiso 1 1 calc GR . . . .
H9C H 0.354084 0.086718 1.064813 0.049 Uiso 1 1 calc GR . . . .
C34 C 0.4412(4) 0.4338(4) 1.2808(2) 0.0257(8) Uani 1 1 d . . . . .
C8 C -0.1285(5) 0.1076(4) 0.8510(3) 0.0373(11) Uani 1 1 d . . . . .
H8A H -0.190722 0.165553 0.858918 0.056 Uiso 1 1 calc GR . . . .
H8B H -0.176368 0.036089 0.860774 0.056 Uiso 1 1 calc GR . . . .
H8C H -0.113256 0.089054 0.798918 0.056 Uiso 1 1 calc GR . . . .
C12 C -0.1363(5) 0.3504(4) 0.7714(3) 0.0311(9) Uani 1 1 d . . . . .
H12 H -0.225262 0.349985 0.789882 0.037 Uiso 1 1 calc R . . . .
C15 C 0.1223(5) 0.3511(4) 0.7188(2) 0.0298(9) Uani 1 1 d . . . . .
H15 H 0.212060 0.350681 0.701179 0.036 Uiso 1 1 calc R . . . .
O38 O 0.3163(4) 0.4864(4) 1.38113(16) 0.0414(9) Uani 1 1 d . . . . .
O28 O 0.2244(3) -0.3332(3) 0.61388(16) 0.0354(7) Uani 1 1 d . . . . .
C27 C 0.0956(5) -0.3287(4) 0.6225(2) 0.0275(9) Uani 1 1 d . . . . .
O39 O 0.5537(4) 0.4872(4) 1.40923(17) 0.0517(11) Uani 1 1 d . . . . .
C37 C 0.4374(5) 0.4731(5) 1.3642(2) 0.0361(11) Uani 1 1 d . . . . .
O29 O -0.0176(3) -0.3939(3) 0.57794(15) 0.0327(7) Uani 1 1 d . . . . .
O19 O -0.1168(3) 0.3617(3) 0.55311(17) 0.0352(7) Uani 1 1 d . . . . .
S48A S 0.4178(2) 0.26255(16) 0.44108(10) 0.0292(4) Uani 0.5743(17) 1 d . . P A
1
O49A O 0.4084(7) 0.2239(6) 0.3619(3) 0.0479(16) Uani 0.5743(17) 1 d . . P A 1
F54A F 0.3831(11) 0.1501(8) 0.5393(4) 0.089(3) Uani 0.5743(17) 1 d . . P A 1
F53A F 0.4773(12) 0.0642(8) 0.4487(6) 0.105(3) Uani 0.5743(17) 1 d . . P A 1
F55A F 0.2410(11) 0.0668(7) 0.4300(6) 0.103(3) Uani 0.5743(17) 1 d . . P A 1
C52A C 0.3772(15) 0.1295(10) 0.4675(7) 0.064(3) Uani 0.5743(17) 1 d . . P A 1
S40A S 0.5131(3) -0.1972(3) 0.17126(15) 0.0372(6) Uani 0.4257(17) 1 d . . P A 1
F45A F 0.3969(10) -0.1190(8) 0.2902(5) 0.067(3) Uani 0.4257(17) 1 d . . P A 1
F47A F 0.5182(13) -0.2476(11) 0.2982(5) 0.082(3) Uani 0.4257(17) 1 d . . P A 1
F46A F 0.6239(13) -0.0692(13) 0.3116(5) 0.103(4) Uani 0.4257(17) 1 d . . P A 1
C44A C 0.5139(17) -0.1488(16) 0.2747(7) 0.065(5) Uani 0.4257(17) 1 d . . P A 1
Br1B Br 0.58789(18) 0.87044(16) 0.70357(12) 0.0733(6) Uani 0.4257(17) 1 d D . P
A 2
O3WA O 0.4147(6) 0.1334(5) 0.2062(3) 0.0344(12) Uani 0.5743(17) 1 d . . P A 1
H3WA H 0.445691 0.068333 0.193192 0.052 Uiso 0.5743(17) 1 d G . P A 1
H3WB H 0.431381 0.153708 0.255160 0.052 Uiso 0.5743(17) 1 d G . P A 1
O42A O 0.3797(11) -0.2875(7) 0.1415(5) 0.045(2) Uani 0.4257(17) 1 d . . P A 1
O41A O 0.6480(13) -0.2311(14) 0.1668(7) 0.088(4) Uani 0.4257(17) 1 d . U P A 1
O51A O 0.2939(4) 0.3125(4) 0.4641(2) 0.0482(9) Uani 0.5743(17) 1 d . . P A 1
H1WA H 0.210962 0.256761 0.462457 0.072 Uiso 0.4257(17) 1 d GR . P A 2
H1WB H 0.365961 0.292166 0.495530 0.072 Uiso 0.4257(17) 1 d GR . P A 2
O2WB O 0.4318(4) 0.6939(5) 0.5179(2) 0.0604(12) Uani 0.4257(17) 1 d . . P A 2
H2WA H 0.404072 0.746260 0.483692 0.091 Uiso 0.4257(17) 1 d GR . P A 2
H2WB H 0.448013 0.757629 0.569492 0.091 Uiso 0.4257(17) 1 d GR . P A 2
O4WB O 0.4907(16) 1.0529(11) 0.8584(8) 0.052(3) Uani 0.5743(17) 1 d . . P A 2
H4WA H 0.466495 1.115201 0.849347 0.078 Uiso 0.5743(17) 1 d DG . P A 2
H4WB H 0.510688 1.014128 0.816207 0.078 Uiso 0.5743(17) 1 d DG . P A 2
O43A O 0.502(2) -0.0918(14) 0.1518(10) 0.048(4) Uani 0.4257(17) 1 d . . P A 1
O50A O 0.4318(4) 0.6939(5) 0.5179(2) 0.0604(12) Uani 0.5743(17) 1 d . . P A 1
O1WB O 0.2939(4) 0.3125(4) 0.4641(2) 0.0482(9) Uani 0.4257(17) 1 d . . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nd1 O18 2.447(3) . ?
Nd1 O38 2.453(3) 1_554 ?
Nd1 O28 2.437(3) 1_565 ?
Nd1 O39 2.374(3) 2_667 ?
Nd1 O29 2.385(3) 2_556 ?
Nd1 O19 2.402(3) 2_566 ?
Nd1 O51A 2.503(4) . ?
Nd1 O2WB 2.528(4) . ?
Nd1 O50A 2.528(4) . ?
Nd1 O1WB 2.503(4) . ?
O18 C17 1.241(6) . ?
N21 C26 1.334(5) . ?
N21 C20 1.493(5) . ?
N21 C22 1.336(5) . ?
C6 C1 1.393(6) . ?
C6 C5 1.398(6) . ?
C6 C7 1.512(5) . ?
C1 C2 1.398(5) . ?
C1 C10 1.507(5) . ?
C5 C4 1.406(6) . ?
C5 C30 1.517(5) . ?
N31 C32 1.344(5) . ?
N31 C36 1.352(5) . ?
N31 C30 1.508(5) . ?
C4 C3 1.402(6) . ?
C4 C9 1.513(6) . ?
C3 C2 1.399(5) . ?
C3 C20 1.522(5) . ?
N11 C10 1.499(5) . ?
N11 C16 1.353(6) . ?
N11 C12 1.342(6) . ?
C26 H26 0.9500 . ?
C26 C25 1.380(6) . ?
C2 C8 1.503(6) . ?
C14 C13 1.384(7) . ?
C14 C17 1.533(6) . ?
C14 C15 1.385(6) . ?
C35 H35 0.9500 . ?
C35 C36 1.369(6) . ?
C35 C34 1.390(6) . ?
C24 C25 1.382(6) . ?
C24 C23 1.381(6) . ?
C24 C27 1.510(5) . ?
C32 H32 0.9500 . ?
C32 C33 1.375(5) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C33 H33 0.9500 . ?
C33 C34 1.386(5) . ?
C22 H22 0.9500 . ?
C22 C23 1.377(6) . ?
C25 H25 0.9500 . ?
C23 H23 0.9500 . ?
C36 H36 0.9500 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C13 H13 0.9500 . ?
C13 C12 1.382(6) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C16 H16 0.9500 . ?
C16 C15 1.380(6) . ?
C17 O19 1.253(5) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C34 C37 1.518(5) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C12 H12 0.9500 . ?
C15 H15 0.9500 . ?
O38 C37 1.250(5) . ?
O28 C27 1.254(5) . ?
C27 O29 1.258(5) . ?
O39 C37 1.243(5) . ?
S48A O49A 1.420(6) . ?
S48A C52A 1.799(12) . ?
S48A O51A 1.465(4) . ?
S48A O50A 1.454(4) 2_666 ?
F54A C52A 1.296(15) . ?
F53A C52A 1.351(16) . ?
F55A C52A 1.364(15) . ?
S40A C44A 1.873(14) . ?
S40A O42A 1.453(10) . ?
S40A O41A 1.403(10) . ?
S40A O43A 1.428(14) . ?
F45A C44A 1.26(2) . ?
F47A C44A 1.38(2) . ?
F46A C44A 1.265(17) . ?
O3WA H3WA 0.8708 . ?
O3WA H3WB 0.8705 . ?
O2WB H2WA 1.0477 . ?
O2WB H2WB 1.0407 . ?
O4WB H4WA 0.8706 . ?
O4WB H4WB 0.8702 . ?
O1WB H1WA 0.9347 . ?
O1WB H1WB 0.9414 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O18 Nd1 O38 143.63(13) . 1_554 ?
O18 Nd1 O51A 74.63(13) . . ?
O18 Nd1 O2WB 137.80(12) . . ?
O18 Nd1 O50A 137.80(12) . . ?
O18 Nd1 O1WB 74.63(13) . . ?
O38 Nd1 O51A 72.17(13) 1_554 . ?
O38 Nd1 O2WB 74.08(13) 1_554 . ?
O38 Nd1 O50A 74.08(13) 1_554 . ?
O38 Nd1 O1WB 72.17(13) 1_554 . ?
O28 Nd1 O18 75.32(12) 1_565 . ?
O28 Nd1 O38 141.04(13) 1_565 1_554 ?
O28 Nd1 O51A 141.85(12) 1_565 . ?
O28 Nd1 O2WB 70.59(13) 1_565 . ?
O28 Nd1 O50A 70.59(13) 1_565 . ?
O28 Nd1 O1WB 141.85(12) 1_565 . ?
O39 Nd1 O18 77.38(13) 2_667 . ?
O39 Nd1 O38 106.27(11) 2_667 1_554 ?
O39 Nd1 O28 77.79(12) 2_667 1_565 ?
O39 Nd1 O29 144.12(15) 2_667 2_556 ?
O39 Nd1 O19 143.09(15) 2_667 2_566 ?
O39 Nd1 O51A 73.16(13) 2_667 . ?
O39 Nd1 O2WB 71.79(15) 2_667 . ?
O39 Nd1 O50A 71.79(15) 2_667 . ?
O39 Nd1 O1WB 73.16(13) 2_667 . ?
O29 Nd1 O18 77.44(11) 2_556 . ?
O29 Nd1 O38 80.43(11) 2_556 1_554 ?
O29 Nd1 O28 119.36(10) 2_556 1_565 ?
O29 Nd1 O19 72.71(12) 2_556 2_566 ?
O29 Nd1 O51A 75.80(11) 2_556 . ?
O29 Nd1 O2WB 141.73(12) 2_556 . ?
O29 Nd1 O50A 141.73(12) 2_556 . ?
O29 Nd1 O1WB 75.80(11) 2_556 . ?
O19 Nd1 O18 122.68(11) 2_566 . ?
O19 Nd1 O38 76.38(11) 2_566 1_554 ?
O19 Nd1 O28 78.49(11) 2_566 1_565 ?
O19 Nd1 O51A 138.42(11) 2_566 . ?
O19 Nd1 O2WB 73.85(13) 2_566 . ?
O19 Nd1 O50A 73.85(13) 2_566 . ?
O19 Nd1 O1WB 138.42(11) 2_566 . ?
O51A Nd1 O50A 120.93(15) . . ?
O1WB Nd1 O2WB 120.93(15) . . ?
C17 O18 Nd1 136.6(3) . . ?
C26 N21 C20 119.2(3) . . ?
C26 N21 C22 121.3(3) . . ?
C22 N21 C20 119.1(3) . . ?
C1 C6 C5 119.1(3) . . ?
C1 C6 C7 120.8(4) . . ?
C5 C6 C7 120.0(4) . . ?
C6 C1 C2 120.7(4) . . ?
C6 C1 C10 120.4(4) . . ?
C2 C1 C10 118.9(4) . . ?
C6 C5 C4 121.4(4) . . ?
C6 C5 C30 119.3(4) . . ?
C4 C5 C30 119.3(4) . . ?
C32 N31 C36 121.0(3) . . ?
C32 N31 C30 121.3(3) . . ?
C36 N31 C30 117.8(3) . . ?
C5 C4 C9 119.2(4) . . ?
C3 C4 C5 118.4(3) . . ?
C3 C4 C9 122.4(4) . . ?
C4 C3 C20 121.0(3) . . ?
C2 C3 C4 120.8(3) . . ?
C2 C3 C20 118.2(4) . . ?
C16 N11 C10 119.4(4) . . ?
C12 N11 C10 119.2(4) . . ?
C12 N11 C16 121.2(4) . . ?
N21 C26 H26 119.7 . . ?
N21 C26 C25 120.7(4) . . ?
C25 C26 H26 119.7 . . ?
C1 C2 C3 119.6(4) . . ?
C1 C2 C8 119.5(4) . . ?
C3 C2 C8 120.9(4) . . ?
C13 C14 C17 119.5(4) . . ?
C13 C14 C15 119.7(4) . . ?
C15 C14 C17 120.7(4) . . ?
C36 C35 H35 120.1 . . ?
C36 C35 C34 119.8(4) . . ?
C34 C35 H35 120.1 . . ?
C25 C24 C27 120.2(4) . . ?
C23 C24 C25 119.8(4) . . ?
C23 C24 C27 119.9(4) . . ?
N31 C32 H32 119.8 . . ?
N31 C32 C33 120.4(3) . . ?
C33 C32 H32 119.8 . . ?
N21 C20 C3 112.1(3) . . ?
N21 C20 H20A 109.2 . . ?
N21 C20 H20B 109.2 . . ?
C3 C20 H20A 109.2 . . ?
C3 C20 H20B 109.2 . . ?
H20A C20 H20B 107.9 . . ?
C32 C33 H33 120.1 . . ?
C32 C33 C34 119.8(4) . . ?
C34 C33 H33 120.1 . . ?
N21 C22 H22 119.7 . . ?
N21 C22 C23 120.6(4) . . ?
C23 C22 H22 119.7 . . ?
C26 C25 C24 118.6(4) . . ?
C26 C25 H25 120.7 . . ?
C24 C25 H25 120.7 . . ?
C24 C23 H23 120.6 . . ?
C22 C23 C24 118.8(4) . . ?
C22 C23 H23 120.6 . . ?
N31 C36 C35 120.4(4) . . ?
N31 C36 H36 119.8 . . ?
C35 C36 H36 119.8 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C14 C13 H13 120.2 . . ?
C12 C13 C14 119.5(4) . . ?
C12 C13 H13 120.2 . . ?
C5 C30 H30A 108.9 . . ?
C5 C30 H30B 108.9 . . ?
N31 C30 C5 113.3(3) . . ?
N31 C30 H30A 108.9 . . ?
N31 C30 H30B 108.9 . . ?
H30A C30 H30B 107.7 . . ?
C1 C10 H10A 109.2 . . ?
C1 C10 H10B 109.2 . . ?
N11 C10 C1 112.2(3) . . ?
N11 C10 H10A 109.2 . . ?
N11 C10 H10B 109.2 . . ?
H10A C10 H10B 107.9 . . ?
N11 C16 H16 119.7 . . ?
N11 C16 C15 120.6(4) . . ?
C15 C16 H16 119.7 . . ?
O18 C17 C14 115.7(4) . . ?
O18 C17 O19 128.7(4) . . ?
O19 C17 C14 115.6(4) . . ?
C4 C9 H9A 109.5 . . ?
C4 C9 H9B 109.5 . . ?
C4 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C35 C34 C37 121.7(4) . . ?
C33 C34 C35 118.6(4) . . ?
C33 C34 C37 119.6(4) . . ?
C2 C8 H8A 109.5 . . ?
C2 C8 H8B 109.5 . . ?
C2 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N11 C12 C13 120.1(4) . . ?
N11 C12 H12 120.0 . . ?
C13 C12 H12 120.0 . . ?
C14 C15 H15 120.6 . . ?
C16 C15 C14 118.9(4) . . ?
C16 C15 H15 120.6 . . ?
C37 O38 Nd1 129.9(3) . 1_556 ?
C27 O28 Nd1 113.5(3) . 1_545 ?
O28 C27 C24 117.0(4) . . ?
O28 C27 O29 124.5(4) . . ?
O29 C27 C24 118.4(4) . . ?
C37 O39 Nd1 171.6(4) . 2_667 ?
O38 C37 C34 116.6(4) . . ?
O39 C37 C34 117.4(4) . . ?
O39 C37 O38 126.0(4) . . ?
C27 O29 Nd1 177.4(3) . 2_556 ?
C17 O19 Nd1 133.9(3) . 2_566 ?
O49A S48A C52A 104.4(5) . . ?
O49A S48A O51A 114.2(3) . . ?
O49A S48A O50A 112.6(3) . 2_666 ?
O51A S48A C52A 98.2(5) . . ?
O50A S48A C52A 98.8(5) 2_666 . ?
O50A S48A O51A 123.7(3) 2_666 . ?
F54A C52A S48A 112.1(8) . . ?
F54A C52A F53A 107.4(10) . . ?
F54A C52A F55A 109.4(12) . . ?
F53A C52A S48A 109.3(10) . . ?
F53A C52A F55A 108.9(11) . . ?
F55A C52A S48A 109.7(8) . . ?
O42A S40A C44A 103.4(6) . . ?
O41A S40A C44A 104.1(8) . . ?
O41A S40A O42A 118.0(8) . . ?
O41A S40A O43A 114.8(10) . . ?
O43A S40A C44A 101.1(10) . . ?
O43A S40A O42A 112.7(9) . . ?
F45A C44A S40A 113.5(10) . . ?
F45A C44A F47A 105.0(11) . . ?
F45A C44A F46A 110.3(17) . . ?
F47A C44A S40A 105.2(12) . . ?
F46A C44A S40A 113.3(10) . . ?
F46A C44A F47A 109.0(13) . . ?
H3WA O3WA H3WB 104.5 . . ?
S48A O51A Nd1 136.6(3) . . ?
Nd1 O2WB H2WA 115.2 . . ?
Nd1 O2WB H2WB 114.4 . . ?
H2WA O2WB H2WB 97.3 . . ?
H4WA O4WB H4WB 104.5 . . ?
S48A O50A Nd1 133.8(3) 2_666 . ?
Nd1 O1WB H1WA 109.1 . . ?
Nd1 O1WB H1WB 119.5 . . ?
H1WA O1WB H1WB 101.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Nd1 O18 C17 C14 -156.1(3) . . . . ?
Nd1 O18 C17 O19 21.8(8) . . . . ?
Nd1 O38 C37 C34 167.7(3) 1_556 . . . ?
Nd1 O38 C37 O39 -11.1(9) 1_556 . . . ?
Nd1 O28 C27 C24 175.1(3) 1_545 . . . ?
Nd1 O28 C27 O29 -2.0(6) 1_545 . . . ?
O18 C17 O19 Nd1 -59.7(7) . . . 2_566 ?
N21 C26 C25 C24 1.4(7) . . . . ?
N21 C22 C23 C24 -0.1(7) . . . . ?
C6 C1 C2 C3 1.8(6) . . . . ?
C6 C1 C2 C8 -177.1(4) . . . . ?
C6 C1 C10 N11 104.4(4) . . . . ?
C6 C5 C4 C3 1.3(5) . . . . ?
C6 C5 C4 C9 -179.7(4) . . . . ?
C6 C5 C30 N31 86.4(4) . . . . ?
C1 C6 C5 C4 0.3(6) . . . . ?
C1 C6 C5 C30 178.8(3) . . . . ?
C5 C6 C1 C2 -1.9(6) . . . . ?
C5 C6 C1 C10 178.1(3) . . . . ?
C5 C4 C3 C2 -1.4(5) . . . . ?
C5 C4 C3 C20 178.6(3) . . . . ?
N31 C32 C33 C34 -0.5(6) . . . . ?
C4 C5 C30 N31 -95.1(4) . . . . ?
C4 C3 C2 C1 -0.1(6) . . . . ?
C4 C3 C2 C8 178.8(4) . . . . ?
C4 C3 C20 N21 -102.8(4) . . . . ?
N11 C16 C15 C14 -0.7(7) . . . . ?
C26 N21 C20 C3 -126.2(4) . . . . ?
C26 N21 C22 C23 -2.9(6) . . . . ?
C2 C1 C10 N11 -75.6(5) . . . . ?
C2 C3 C20 N21 77.2(4) . . . . ?
C14 C13 C12 N11 -1.5(7) . . . . ?
C14 C17 O19 Nd1 118.2(4) . . . 2_566 ?
C35 C34 C37 O38 -178.9(5) . . . . ?
C35 C34 C37 O39 0.0(8) . . . . ?
C32 N31 C36 C35 2.1(6) . . . . ?
C32 N31 C30 C5 -15.6(5) . . . . ?
C32 C33 C34 C35 1.6(6) . . . . ?
C32 C33 C34 C37 -175.6(4) . . . . ?
C20 N21 C26 C25 -170.4(4) . . . . ?
C20 N21 C22 C23 169.8(4) . . . . ?
C20 C3 C2 C1 179.9(3) . . . . ?
C20 C3 C2 C8 -1.2(6) . . . . ?
C33 C34 C37 O38 -1.7(7) . . . . ?
C33 C34 C37 O39 177.2(5) . . . . ?
C22 N21 C26 C25 2.3(6) . . . . ?
C22 N21 C20 C3 61.0(5) . . . . ?
C25 C24 C23 C22 3.8(6) . . . . ?
C25 C24 C27 O28 -175.3(4) . . . . ?
C25 C24 C27 O29 2.0(6) . . . . ?
C23 C24 C25 C26 -4.4(6) . . . . ?
C23 C24 C27 O28 1.2(6) . . . . ?
C23 C24 C27 O29 178.4(4) . . . . ?
C36 N31 C32 C33 -1.4(6) . . . . ?
C36 N31 C30 C5 166.1(3) . . . . ?
C36 C35 C34 C33 -1.0(7) . . . . ?
C36 C35 C34 C37 176.2(4) . . . . ?
C7 C6 C1 C2 177.1(4) . . . . ?
C7 C6 C1 C10 -2.9(6) . . . . ?
C7 C6 C5 C4 -178.7(4) . . . . ?
C7 C6 C5 C30 -0.2(6) . . . . ?
C13 C14 C17 O18 162.4(4) . . . . ?
C13 C14 C17 O19 -15.8(6) . . . . ?
C13 C14 C15 C16 -2.1(7) . . . . ?
C30 C5 C4 C3 -177.2(3) . . . . ?
C30 C5 C4 C9 1.8(5) . . . . ?
C30 N31 C32 C33 -179.7(4) . . . . ?
C30 N31 C36 C35 -179.6(4) . . . . ?
C10 C1 C2 C3 -178.2(3) . . . . ?
C10 C1 C2 C8 2.9(6) . . . . ?
C10 N11 C16 C15 -172.7(4) . . . . ?
C10 N11 C12 C13 173.8(4) . . . . ?
C16 N11 C10 C1 -42.8(5) . . . . ?
C16 N11 C12 C13 -1.4(6) . . . . ?
C17 C14 C13 C12 -172.5(4) . . . . ?
C17 C14 C15 C16 173.5(4) . . . . ?
C9 C4 C3 C2 179.6(4) . . . . ?
C9 C4 C3 C20 -0.4(6) . . . . ?
C34 C35 C36 N31 -0.9(7) . . . . ?
C12 N11 C10 C1 141.9(4) . . . . ?
C12 N11 C16 C15 2.5(6) . . . . ?
C15 C14 C13 C12 3.2(7) . . . . ?
C15 C14 C17 O18 -13.2(6) . . . . ?
C15 C14 C17 O19 168.6(4) . . . . ?
C27 C24 C25 C26 172.1(4) . . . . ?
C27 C24 C23 C22 -172.7(4) . . . . ?
O49A S48A C52A F54A 179.2(9) . . . . ?
O49A S48A C52A F53A 60.2(9) . . . . ?
O49A S48A C52A F55A -59.1(11) . . . . ?
O49A S48A O51A Nd1 -94.9(4) . . . . ?
C52A S48A O51A Nd1 155.2(5) . . . . ?
O42A S40A C44A F45A -53.5(13) . . . . ?
O42A S40A C44A F47A 60.8(11) . . . . ?
O42A S40A C44A F46A 179.7(14) . . . . ?
O41A S40A C44A F45A -177.3(13) . . . . ?
O41A S40A C44A F47A -63.0(12) . . . . ?
O41A S40A C44A F46A 55.9(17) . . . . ?
O51A S48A C52A F54A -63.1(10) . . . . ?
O51A S48A C52A F53A 177.9(8) . . . . ?
O51A S48A C52A F55A 58.6(10) . . . . ?
O43A S40A C44A F45A 63.3(14) . . . . ?
O43A S40A C44A F47A 177.6(12) . . . . ?
O43A S40A C44A F46A -63.5(18) . . . . ?
O50A S48A C52A F54A 63.0(10) 2_666 . . . ?
O50A S48A C52A F53A -56.0(9) 2_666 . . . ?
O50A S48A C52A F55A -175.3(9) 2_666 . . . ?
O50A S48A O51A Nd1 48.8(5) 2_666 . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.216
_oxdiff_exptl_absorpt_empirical_full_min 0.806
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_jj003_ndoac_dry_h2o_acet_red2
_database_code_depnum_ccdc_archive 'CCDC 1894870'
loop_
_audit_author_name
_audit_author_address
'Antti Tiihonen'
;Department of Chemistry, University of Jyvaskyla
Finland
;
_audit_update_record             
;
2019-01-31 deposited with the CCDC.	2019-02-28 downloaded from the CCDC.
;
_audit_creation_date             2019-01-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C32 H30 N3 Nd O8, 2(Br), 7(H2 O)'
_chemical_formula_sum            'C32 H44 Br2 N3 Nd O15'
_chemical_formula_weight         1014.76
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C32 H30 N3 O18 Nd1 Br2'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -3.1807 10.9079 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.7309(9)
_cell_length_b                   12.2707(11)
_cell_length_c                   19.3079(11)
_cell_angle_alpha                106.661(7)
_cell_angle_beta                 100.429(7)
_cell_angle_gamma                91.716(8)
_cell_volume                     1941.6(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6499
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      75.5370
_cell_measurement_theta_min      3.7280
_shelx_estimated_absorpt_T_max   0.558
_shelx_estimated_absorpt_T_min   0.240
_exptl_absorpt_coefficient_mu    13.225
_exptl_absorpt_correction_T_max  0.793
_exptl_absorpt_correction_T_min  0.298
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.43c (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.736
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1014
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -8 2 0.0295
1 8 -2 0.0115
-1 6 5 0.0228
0 8 -7 0.0220
-5 2 -4 0.0579
0 1 -12 0.0525
6 0 -3 0.0542
3 -7 5 0.0478
0 -6 11 0.0502

_exptl_crystal_size_max          0.151
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.05
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.0036 -7.9974 1.9926 -1.0053 -0.1379 0.0005
1.0040 7.9980 -1.9909 1.0395 -0.0343 0.0401
-0.9944 6.0043 5.0012 0.7958 0.3040 0.5055
0.0011 7.9922 -6.9905 0.9468 0.1162 -0.4208
-5.0030 1.9929 -4.0052 0.0392 0.8803 -0.4973
-0.0055 0.9874 -11.9943 -0.0119 -0.0339 -0.9879
6.0010 0.0002 -2.9886 0.1703 -1.0463 -0.0087
2.9997 -6.9927 4.9973 -0.7389 -0.6232 0.3954
0.0021 -5.9882 10.9906 -0.6428 -0.0621 0.7990

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12498
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.991
_diffrn_reflns_theta_min         3.774
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3953
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -115.00 -17.00   2.00    3.00    --  -41.78 -37.00 120.00   49
  2  ω    -54.00  -2.00   2.00    3.00    --  -41.78 125.00   0.00   26
  3  ω    -66.00  24.00   2.00    3.00    --  -41.78  37.00 -60.00   45
  4  ω      1.00  71.00   2.00    3.00    --   41.78 -99.00   0.00   35
  5  ω     38.00  98.00   2.00    3.00    --   41.78-125.00-180.00   30
  6  ω     72.00 176.00   2.00    6.00    --  112.00  15.00-120.00   52
  7  ω    146.00 178.00   2.00    6.00    --  112.00 111.00  60.00   16
  8  ω     38.00 118.00   2.00    6.00    --  112.00 -30.00-150.00   40
  9  ω    101.00 129.00   2.00    6.00    --  112.00 111.00  60.00   14
 10  ω     50.00 116.00   2.00    6.00    --  112.00-111.00 120.00   33
 11  ω     36.00 116.00   2.00    6.00    --  112.00-111.00 -90.00   40
 12  ω     84.00 178.00   2.00    6.00    --  112.00  30.00 150.00   47
 13  ω     77.00 103.00   2.00    6.00    --  112.00 -94.00-180.00   13
 14  ω     33.00 109.00   2.00    6.00    --  112.00 -94.00   0.00   38
 15  ω     41.00 137.00   2.00    6.00    --  112.00 -45.00 -30.00   48
 16  ω     49.00 139.00   2.00    6.00    --  112.00 -61.00  90.00   45
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0341239000
_diffrn_orient_matrix_UB_12      0.1285673000
_diffrn_orient_matrix_UB_13      0.0115588000
_diffrn_orient_matrix_UB_21      -0.1721524000
_diffrn_orient_matrix_UB_22      0.0184291000
_diffrn_orient_matrix_UB_23      0.0044246000
_diffrn_orient_matrix_UB_31      0.0404110000
_diffrn_orient_matrix_UB_32      0.0208641000
_diffrn_orient_matrix_UB_33      0.0840614000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6658
_reflns_number_total             7055
_reflns_odcompleteness_completeness 99.46
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         0.718
_refine_diff_density_min         -0.715
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     503
_refine_ls_number_reflns         7055
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0251
_refine_ls_restrained_S_all      1.007
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0277P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0589
_refine_ls_wR_factor_ref         0.0600
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Free rotating group:
 O6W(H6WA,H6WB), O1W(H1WA,H1WB), O7W(H7WA,H7WB), O2W(H2WA,H2WB), O4W(H4WA,
 H4WB), O0AA(H0AA,H0AB), O5W(H5WA,H5WB)
2.b Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C10(H10A,H10B), C20(H20A,H20B)
2.c Aromatic/amide H refined with riding coordinates:
 C23(H23), C35(H35), C13(H13), C16(H16), C26(H26), C33(H33), C22(H22),
 C25(H25), C15(H15), C12(H12), C36(H36), C32(H32)
2.d Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C9(H9A,H9B,H9C), C8(H8A,H8B,H8C), C7(H7A,H7B,H7C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Nd1 Nd -0.26695(2) 0.97507(2) -0.00112(2) 0.01054(5) Uani 1 1 d . . . . .
Br1 Br -0.11060(4) 0.81099(3) 0.58975(2) 0.02035(8) Uani 1 1 d . . . . .
Br2 Br -0.49231(4) 0.50270(3) 0.34585(2) 0.02123(8) Uani 1 1 d . . . . .
O18 O -0.0266(2) 0.98422(18) 0.08289(11) 0.0160(4) Uani 1 1 d . . . . .
O39 O 0.3100(2) 0.91706(18) 0.87359(11) 0.0157(4) Uani 1 1 d . . . . .
O38 O 0.5492(2) 0.85142(18) 0.88819(11) 0.0154(4) Uani 1 1 d . . . . .
O43 O -0.3256(2) 0.81617(18) 0.05634(12) 0.0180(4) Uani 1 1 d . . . . .
O29 O 0.1334(2) 0.19336(18) 0.05921(11) 0.0165(4) Uani 1 1 d . . . . .
O6W O -0.4379(3) 0.8860(2) 0.32369(14) 0.0275(5) Uani 1 1 d . . . . .
H6WA H -0.404912 0.862033 0.361549 0.041 Uiso 1 1 d G . . . .
H6WB H -0.485571 0.825758 0.289649 0.041 Uiso 1 1 d G . . . .
O28 O -0.1295(2) 0.16669(17) 0.03010(11) 0.0138(4) Uani 1 1 d . . . . .
O1W O -0.2031(3) 0.6276(2) 0.09569(16) 0.0341(6) Uani 1 1 d . . . . .
H1WA H -0.235226 0.692995 0.093227 0.051 Uiso 1 1 d G . . . .
H1WB H -0.276112 0.597002 0.111304 0.051 Uiso 1 1 d G . . . .
O7W O -0.3564(3) 0.7803(2) 0.43429(13) 0.0275(5) Uani 1 1 d . . . . .
H7WA H -0.384855 0.707448 0.417003 0.041 Uiso 1 1 d G . . . .
H7WB H -0.284400 0.786869 0.473200 0.041 Uiso 1 1 d G . . . .
O2W O -0.4332(3) 0.5184(2) 0.14323(16) 0.0353(6) Uani 1 1 d . . . . .
H2WA H -0.472466 0.569113 0.175161 0.053 Uiso 1 1 d G . . . .
H2WB H -0.513498 0.473420 0.115223 0.053 Uiso 1 1 d G . . . .
O4W O -0.8932(4) 0.5900(3) 0.15590(16) 0.0442(7) Uani 1 1 d . . . . .
H4WA H -0.870231 0.539862 0.118050 0.066 Uiso 1 1 d G . . . .
H4WB H -0.983723 0.610359 0.139109 0.066 Uiso 1 1 d G . . . .
O0AA O -0.6021(3) 0.6723(2) 0.24313(15) 0.0364(6) Uani 1 1 d . . . . .
H0AA H -0.699307 0.660159 0.220290 0.055 Uiso 1 1 d G . . . .
H0AB H -0.585299 0.629518 0.272251 0.055 Uiso 1 1 d G . . . .
C40 C -0.5742(4) 0.7492(3) 0.0721(2) 0.0330(9) Uani 1 1 d . . . . .
H40A H -0.683387 0.761075 0.055057 0.049 Uiso 1 1 calc GR . . . .
H40B H -0.552946 0.764702 0.125742 0.049 Uiso 1 1 calc GR . . . .
H40C H -0.555313 0.669969 0.048683 0.049 Uiso 1 1 calc GR . . . .
N21 N -0.0362(3) 0.4242(2) 0.28352(13) 0.0140(5) Uani 1 1 d . . . . .
N11 N 0.0283(3) 0.9055(2) 0.32336(13) 0.0134(5) Uani 1 1 d . . . . .
C6 C -0.0041(3) 0.6855(3) 0.37635(15) 0.0131(6) Uani 1 1 d . . . . .
O5W O -0.7399(4) 0.4199(2) 0.06147(15) 0.0351(6) Uani 1 1 d . . . . .
H5WA H -0.773700 0.424956 0.017279 0.053 Uiso 1 1 d G . . . .
H5WB H -0.756736 0.347763 0.057104 0.053 Uiso 1 1 d G . . . .
N31 N 0.4132(3) 0.7641(2) 0.61861(13) 0.0125(5) Uani 1 1 d . . . . .
C17 C 0.0936(3) 0.9717(2) 0.12580(16) 0.0135(6) Uani 1 1 d . . . . .
C2 C 0.2137(3) 0.8041(2) 0.46676(15) 0.0122(6) Uani 1 1 d . . . . .
C37 C 0.4270(3) 0.8724(2) 0.85122(16) 0.0128(6) Uani 1 1 d . . . . .
C3 C 0.2628(3) 0.7071(3) 0.48576(15) 0.0138(6) Uani 1 1 d . . . . .
C9 C 0.2244(4) 0.4996(3) 0.47986(17) 0.0193(6) Uani 1 1 d . . . . .
H9A H 0.281592 0.451404 0.445149 0.029 Uiso 1 1 calc GR . . . .
H9B H 0.131238 0.455283 0.482188 0.029 Uiso 1 1 calc GR . . . .
H9C H 0.291874 0.526496 0.528919 0.029 Uiso 1 1 calc GR . . . .
C34 C 0.4182(4) 0.8367(2) 0.76808(16) 0.0137(6) Uani 1 1 d . . . . .
C14 C 0.0697(4) 0.9445(2) 0.19475(15) 0.0137(6) Uani 1 1 d . . . . .
C41 C -0.4685(4) 0.8284(3) 0.05164(16) 0.0162(6) Uani 1 1 d . . . . .
C4 C 0.1759(4) 0.6007(2) 0.45423(15) 0.0135(6) Uani 1 1 d . . . . .
C23 C 0.1219(4) 0.3358(3) 0.19973(17) 0.0174(6) Uani 1 1 d . . . . .
H23 H 0.222419 0.318975 0.189508 0.021 Uiso 1 1 calc R . . . .
C1 C 0.0768(3) 0.7930(2) 0.41318(15) 0.0133(6) Uani 1 1 d . . . . .
C35 C 0.5559(4) 0.8257(3) 0.74169(16) 0.0165(6) Uani 1 1 d . . . . .
H35 H 0.653645 0.842825 0.775206 0.020 Uiso 1 1 calc R . . . .
C13 C -0.0771(4) 0.9460(3) 0.21253(16) 0.0149(6) Uani 1 1 d . . . . .
H13 H -0.164843 0.959318 0.179876 0.018 Uiso 1 1 calc R . . . .
C8 C 0.3103(4) 0.9176(3) 0.50397(17) 0.0202(6) Uani 1 1 d . . . . .
H8A H 0.317094 0.937527 0.557411 0.030 Uiso 1 1 calc GR . . . .
H8B H 0.260636 0.977029 0.485448 0.030 Uiso 1 1 calc GR . . . .
H8C H 0.415646 0.911487 0.493080 0.030 Uiso 1 1 calc GR . . . .
C5 C 0.0441(3) 0.5904(2) 0.39782(15) 0.0130(6) Uani 1 1 d . . . . .
C16 C 0.1714(4) 0.9014(3) 0.30636(17) 0.0181(6) Uani 1 1 d . . . . .
H16 H 0.256458 0.884744 0.338933 0.022 Uiso 1 1 calc R . . . .
C26 C -0.1662(4) 0.3949(2) 0.22912(16) 0.0152(6) Uani 1 1 d . . . . .
H26 H -0.264519 0.418123 0.239574 0.018 Uiso 1 1 calc R . . . .
C33 C 0.2772(3) 0.8144(2) 0.71748(16) 0.0145(6) Uani 1 1 d . . . . .
H33 H 0.181308 0.824940 0.734175 0.017 Uiso 1 1 calc R . . . .
C22 C 0.1059(4) 0.3985(3) 0.26919(16) 0.0173(6) Uani 1 1 d . . . . .
H22 H 0.195893 0.423762 0.307406 0.021 Uiso 1 1 calc R . . . .
C25 C -0.1556(4) 0.3319(2) 0.15908(16) 0.0153(6) Uani 1 1 d . . . . .
H25 H -0.246182 0.312040 0.120902 0.018 Uiso 1 1 calc R . . . .
C15 C 0.1956(4) 0.9208(3) 0.24289(16) 0.0165(6) Uani 1 1 d . . . . .
H15 H 0.297076 0.918333 0.231457 0.020 Uiso 1 1 calc R . . . .
C12 C -0.0949(4) 0.9280(3) 0.27792(16) 0.0161(6) Uani 1 1 d . . . . .
H12 H -0.194694 0.931420 0.291120 0.019 Uiso 1 1 calc R . . . .
C7 C -0.1401(4) 0.6714(3) 0.31257(16) 0.0168(6) Uani 1 1 d . . . . .
H7A H -0.187916 0.743775 0.317806 0.025 Uiso 1 1 calc GR . . . .
H7B H -0.217835 0.612087 0.312569 0.025 Uiso 1 1 calc GR . . . .
H7C H -0.102459 0.649084 0.266060 0.025 Uiso 1 1 calc GR . . . .
C30 C 0.4174(4) 0.7170(3) 0.53840(15) 0.0148(6) Uani 1 1 d . . . . .
H30A H 0.456436 0.640290 0.529923 0.018 Uiso 1 1 calc R . . . .
H30B H 0.493674 0.766432 0.526229 0.018 Uiso 1 1 calc R . . . .
C24 C -0.0121(4) 0.2973(2) 0.14432(16) 0.0148(6) Uani 1 1 d . . . . .
C27 C -0.0019(3) 0.2121(2) 0.07070(16) 0.0142(6) Uani 1 1 d . . . . .
C36 C 0.5513(3) 0.7898(3) 0.66658(16) 0.0152(6) Uani 1 1 d . . . . .
H36 H 0.646036 0.783288 0.648651 0.018 Uiso 1 1 calc R . . . .
C10 C 0.0078(4) 0.8962(3) 0.39653(15) 0.0161(6) Uani 1 1 d . . . . .
H10A H -0.105096 0.891768 0.397555 0.019 Uiso 1 1 calc R . . . .
H10B H 0.058276 0.965879 0.435488 0.019 Uiso 1 1 calc R . . . .
C20 C -0.0511(4) 0.4764(2) 0.36148(15) 0.0148(6) Uani 1 1 d . . . . .
H20A H -0.017025 0.423097 0.390065 0.018 Uiso 1 1 calc R . . . .
H20B H -0.162558 0.487047 0.363007 0.018 Uiso 1 1 calc R . . . .
C32 C 0.2774(3) 0.7767(2) 0.64268(16) 0.0145(6) Uani 1 1 d . . . . .
H32 H 0.181073 0.759716 0.608110 0.017 Uiso 1 1 calc R . . . .
O19 O 0.2308(2) 0.98454(18) 0.11767(11) 0.0157(4) Uani 1 1 d . . . . .
O42 O -0.5263(2) 0.90842(17) 0.02832(11) 0.0145(4) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nd1 O18 2.387(2) . ?
Nd1 O39 2.540(2) 2_576 ?
Nd1 O38 2.490(2) 1_454 ?
Nd1 O43 2.585(2) . ?
Nd1 O29 2.486(2) 2_565 ?
Nd1 O28 2.467(2) 1_565 ?
Nd1 O19 2.509(2) 2_575 ?
Nd1 O42 2.412(2) 2_475 ?
Nd1 O42 2.596(2) . ?
O18 C17 1.257(4) . ?
O39 C37 1.261(4) . ?
O38 C37 1.249(4) . ?
O43 C41 1.251(4) . ?
O29 C27 1.257(4) . ?
O6W H6WA 0.8694 . ?
O6W H6WB 0.8692 . ?
O28 C27 1.250(4) . ?
O1W H1WA 0.8695 . ?
O1W H1WB 0.8702 . ?
O7W H7WA 0.8703 . ?
O7W H7WB 0.8701 . ?
O2W H2WA 0.8687 . ?
O2W H2WB 0.8699 . ?
O4W H4WA 0.8694 . ?
O4W H4WB 0.8702 . ?
O0AA H0AA 0.8697 . ?
O0AA H0AB 0.8703 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C40 C41 1.500(4) . ?
N21 C26 1.360(4) . ?
N21 C22 1.346(4) . ?
N21 C20 1.488(4) . ?
N11 C16 1.347(4) . ?
N11 C12 1.348(4) . ?
N11 C10 1.491(4) . ?
C6 C1 1.404(4) . ?
C6 C5 1.397(4) . ?
C6 C7 1.514(4) . ?
O5W H5WA 0.8716 . ?
O5W H5WB 0.8696 . ?
N31 C30 1.498(3) . ?
N31 C36 1.348(4) . ?
N31 C32 1.347(4) . ?
C17 C14 1.509(4) . ?
C17 O19 1.246(4) . ?
C2 C3 1.400(4) . ?
C2 C1 1.407(4) . ?
C2 C8 1.517(4) . ?
C37 C34 1.525(4) . ?
C3 C4 1.404(4) . ?
C3 C30 1.514(4) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C9 C4 1.506(4) . ?
C34 C35 1.384(4) . ?
C34 C33 1.391(4) . ?
C14 C13 1.385(4) . ?
C14 C15 1.401(4) . ?
C41 O42 1.273(4) . ?
C4 C5 1.409(4) . ?
C23 H23 0.9500 . ?
C23 C22 1.375(4) . ?
C23 C24 1.400(4) . ?
C1 C10 1.509(4) . ?
C35 H35 0.9500 . ?
C35 C36 1.382(4) . ?
C13 H13 0.9500 . ?
C13 C12 1.377(4) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C5 C20 1.516(4) . ?
C16 H16 0.9500 . ?
C16 C15 1.365(4) . ?
C26 H26 0.9500 . ?
C26 C25 1.373(4) . ?
C33 H33 0.9500 . ?
C33 C32 1.385(4) . ?
C22 H22 0.9500 . ?
C25 H25 0.9500 . ?
C25 C24 1.387(4) . ?
C15 H15 0.9500 . ?
C12 H12 0.9500 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C24 C27 1.523(4) . ?
C36 H36 0.9500 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C32 H32 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O18 Nd1 O39 73.19(7) . 2_576 ?
O18 Nd1 O38 144.65(7) . 1_454 ?
O18 Nd1 O43 78.49(7) . . ?
O18 Nd1 O29 74.32(7) . 2_565 ?
O18 Nd1 O28 71.04(7) . 1_565 ?
O18 Nd1 O19 113.20(7) . 2_575 ?
O18 Nd1 O42 119.50(7) . . ?
O18 Nd1 O42 141.11(7) . 2_475 ?
O39 Nd1 O43 75.89(7) 2_576 . ?
O39 Nd1 O42 66.24(7) 2_576 . ?
O38 Nd1 O39 131.25(7) 1_454 2_576 ?
O38 Nd1 O43 83.72(7) 1_454 . ?
O38 Nd1 O19 67.59(7) 1_454 2_575 ?
O38 Nd1 O42 66.74(7) 1_454 . ?
O43 Nd1 O42 49.88(6) . . ?
O29 Nd1 O39 138.32(7) 2_565 2_576 ?
O29 Nd1 O38 71.28(7) 2_565 1_454 ?
O29 Nd1 O43 72.63(7) 2_565 . ?
O29 Nd1 O19 78.58(7) 2_565 2_575 ?
O29 Nd1 O42 109.98(7) 2_565 . ?
O28 Nd1 O39 73.86(7) 1_565 2_576 ?
O28 Nd1 O38 134.06(7) 1_565 1_454 ?
O28 Nd1 O43 141.91(7) 1_565 . ?
O28 Nd1 O29 118.38(7) 1_565 2_565 ?
O28 Nd1 O19 70.83(7) 1_565 2_575 ?
O28 Nd1 O42 131.28(7) 1_565 . ?
O19 Nd1 O39 138.86(7) 2_575 2_576 ?
O19 Nd1 O43 144.59(7) 2_575 . ?
O19 Nd1 O42 127.01(6) 2_575 . ?
O42 Nd1 O39 77.53(7) 2_475 2_576 ?
O42 Nd1 O38 74.22(7) 2_475 1_454 ?
O42 Nd1 O43 118.39(7) 2_475 . ?
O42 Nd1 O29 142.23(7) 2_475 2_565 ?
O42 Nd1 O28 76.66(7) 2_475 1_565 ?
O42 Nd1 O19 74.43(7) 2_475 2_575 ?
O42 Nd1 O42 68.59(8) 2_475 . ?
C17 O18 Nd1 170.4(2) . . ?
C37 O39 Nd1 132.26(18) . 2_576 ?
C37 O38 Nd1 130.97(19) . 1_656 ?
C41 O43 Nd1 95.63(18) . . ?
C27 O29 Nd1 136.46(19) . 2_565 ?
H6WA O6W H6WB 104.7 . . ?
C27 O28 Nd1 133.03(18) . 1_545 ?
H1WA O1W H1WB 104.5 . . ?
H7WA O7W H7WB 104.5 . . ?
H2WA O2W H2WB 104.6 . . ?
H4WA O4W H4WB 104.5 . . ?
H0AA O0AA H0AB 109.4 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C41 C40 H40A 109.5 . . ?
C41 C40 H40B 109.5 . . ?
C41 C40 H40C 109.5 . . ?
C26 N21 C20 119.9(3) . . ?
C22 N21 C26 121.1(3) . . ?
C22 N21 C20 118.7(2) . . ?
C16 N11 C12 120.9(3) . . ?
C16 N11 C10 119.8(2) . . ?
C12 N11 C10 119.0(3) . . ?
C1 C6 C7 120.6(3) . . ?
C5 C6 C1 119.5(3) . . ?
C5 C6 C7 119.9(3) . . ?
H5WA O5W H5WB 104.5 . . ?
C36 N31 C30 117.3(2) . . ?
C32 N31 C30 121.8(2) . . ?
C32 N31 C36 120.8(2) . . ?
O18 C17 C14 117.0(3) . . ?
O19 C17 O18 125.5(3) . . ?
O19 C17 C14 117.5(3) . . ?
C3 C2 C1 118.8(3) . . ?
C3 C2 C8 119.1(3) . . ?
C1 C2 C8 122.1(3) . . ?
O39 C37 C34 116.3(3) . . ?
O38 C37 O39 128.5(3) . . ?
O38 C37 C34 115.2(3) . . ?
C2 C3 C4 121.4(3) . . ?
C2 C3 C30 118.7(3) . . ?
C4 C3 C30 119.8(3) . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C4 C9 H9A 109.5 . . ?
C4 C9 H9B 109.5 . . ?
C4 C9 H9C 109.5 . . ?
C35 C34 C37 118.8(3) . . ?
C35 C34 C33 118.5(3) . . ?
C33 C34 C37 122.7(3) . . ?
C13 C14 C17 120.3(3) . . ?
C13 C14 C15 118.8(3) . . ?
C15 C14 C17 120.8(3) . . ?
O43 C41 C40 121.1(3) . . ?
O43 C41 O42 119.8(3) . . ?
O42 C41 C40 119.1(3) . . ?
C3 C4 C9 120.4(3) . . ?
C3 C4 C5 118.6(3) . . ?
C5 C4 C9 121.0(3) . . ?
C22 C23 H23 120.5 . . ?
C22 C23 C24 119.1(3) . . ?
C24 C23 H23 120.5 . . ?
C6 C1 C2 120.6(3) . . ?
C6 C1 C10 118.0(3) . . ?
C2 C1 C10 121.3(3) . . ?
C34 C35 H35 120.0 . . ?
C36 C35 C34 120.0(3) . . ?
C36 C35 H35 120.0 . . ?
C14 C13 H13 120.3 . . ?
C12 C13 C14 119.5(3) . . ?
C12 C13 H13 120.3 . . ?
C2 C8 H8A 109.5 . . ?
C2 C8 H8B 109.5 . . ?
C2 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C6 C5 C4 120.8(3) . . ?
C6 C5 C20 119.0(3) . . ?
C4 C5 C20 120.2(3) . . ?
N11 C16 H16 119.6 . . ?
N11 C16 C15 120.8(3) . . ?
C15 C16 H16 119.6 . . ?
N21 C26 H26 120.0 . . ?
N21 C26 C25 120.1(3) . . ?
C25 C26 H26 120.0 . . ?
C34 C33 H33 120.1 . . ?
C32 C33 C34 119.7(3) . . ?
C32 C33 H33 120.1 . . ?
N21 C22 C23 120.6(3) . . ?
N21 C22 H22 119.7 . . ?
C23 C22 H22 119.7 . . ?
C26 C25 H25 120.1 . . ?
C26 C25 C24 119.7(3) . . ?
C24 C25 H25 120.1 . . ?
C14 C15 H15 120.3 . . ?
C16 C15 C14 119.4(3) . . ?
C16 C15 H15 120.3 . . ?
N11 C12 C13 120.5(3) . . ?
N11 C12 H12 119.8 . . ?
C13 C12 H12 119.8 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N31 C30 C3 115.5(2) . . ?
N31 C30 H30A 108.4 . . ?
N31 C30 H30B 108.4 . . ?
C3 C30 H30A 108.4 . . ?
C3 C30 H30B 108.4 . . ?
H30A C30 H30B 107.5 . . ?
C23 C24 C27 120.4(3) . . ?
C25 C24 C23 119.1(3) . . ?
C25 C24 C27 120.4(3) . . ?
O29 C27 C24 116.2(3) . . ?
O28 C27 O29 128.0(3) . . ?
O28 C27 C24 115.8(3) . . ?
N31 C36 C35 120.4(3) . . ?
N31 C36 H36 119.8 . . ?
C35 C36 H36 119.8 . . ?
N11 C10 C1 112.6(2) . . ?
N11 C10 H10A 109.1 . . ?
N11 C10 H10B 109.1 . . ?
C1 C10 H10A 109.1 . . ?
C1 C10 H10B 109.1 . . ?
H10A C10 H10B 107.8 . . ?
N21 C20 C5 113.2(2) . . ?
N21 C20 H20A 108.9 . . ?
N21 C20 H20B 108.9 . . ?
C5 C20 H20A 108.9 . . ?
C5 C20 H20B 108.9 . . ?
H20A C20 H20B 107.7 . . ?
N31 C32 C33 120.4(3) . . ?
N31 C32 H32 119.8 . . ?
C33 C32 H32 119.8 . . ?
C17 O19 Nd1 116.81(18) . 2_575 ?
Nd1 O42 Nd1 111.41(8) 2_475 . ?
C41 O42 Nd1 154.1(2) . 2_475 ?
C41 O42 Nd1 94.51(18) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O6W H6WA O7W 0.87 1.94 2.801(3) 168.5 . yes
O6W H6WB O0AA 0.87 1.99 2.825(4) 159.8 . yes
O1W H1WA O43 0.87 1.97 2.817(3) 163.0 . yes
O2W H2WA O0AA 0.87 2.07 2.928(4) 170.0 . yes
O2W H2WB O5W 0.87 2.05 2.882(4) 159.6 . yes
O4W H4WA O5W 0.87 2.07 2.889(4) 156.6 . yes
O0AA H0AA O4W 0.87 1.92 2.764(4) 162.8 . yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Nd1 O39 C37 O38 13.9(5) 2_576 . . . ?
Nd1 O39 C37 C34 -167.42(18) 2_576 . . . ?
Nd1 O38 C37 O39 -51.2(4) 1_656 . . . ?
Nd1 O38 C37 C34 130.1(2) 1_656 . . . ?
Nd1 O43 C41 C40 174.9(3) . . . . ?
Nd1 O43 C41 O42 -4.2(3) . . . . ?
Nd1 O29 C27 O28 -36.1(5) 2_565 . . . ?
Nd1 O29 C27 C24 141.4(2) 2_565 . . . ?
Nd1 O28 C27 O29 72.9(4) 1_545 . . . ?
Nd1 O28 C27 C24 -104.6(3) 1_545 . . . ?
O18 C17 C14 C13 -6.7(4) . . . . ?
O18 C17 C14 C15 175.2(3) . . . . ?
O18 C17 O19 Nd1 -4.6(4) . . . 2_575 ?
O39 C37 C34 C35 157.4(3) . . . . ?
O39 C37 C34 C33 -22.8(4) . . . . ?
O38 C37 C34 C35 -23.7(4) . . . . ?
O38 C37 C34 C33 156.1(3) . . . . ?
O43 C41 O42 Nd1 4.2(3) . . . . ?
O43 C41 O42 Nd1 -173.6(3) . . . 2_475 ?
C40 C41 O42 Nd1 7.3(6) . . . 2_475 ?
C40 C41 O42 Nd1 -174.9(3) . . . . ?
N21 C26 C25 C24 0.7(4) . . . . ?
N11 C16 C15 C14 -0.4(5) . . . . ?
C6 C1 C10 N11 -74.8(3) . . . . ?
C6 C5 C20 N21 71.5(3) . . . . ?
C17 C14 C13 C12 -176.0(3) . . . . ?
C17 C14 C15 C16 177.2(3) . . . . ?
C2 C3 C4 C9 -175.2(3) . . . . ?
C2 C3 C4 C5 5.5(4) . . . . ?
C2 C3 C30 N31 82.1(3) . . . . ?
C2 C1 C10 N11 108.5(3) . . . . ?
C37 C34 C35 C36 177.8(3) . . . . ?
C37 C34 C33 C32 -176.7(3) . . . . ?
C3 C2 C1 C6 -3.7(4) . . . . ?
C3 C2 C1 C10 173.0(3) . . . . ?
C3 C4 C5 C6 -3.4(4) . . . . ?
C3 C4 C5 C20 178.9(3) . . . . ?
C9 C4 C5 C6 177.4(3) . . . . ?
C9 C4 C5 C20 -0.3(4) . . . . ?
C34 C35 C36 N31 -0.8(5) . . . . ?
C34 C33 C32 N31 -1.5(4) . . . . ?
C14 C17 O19 Nd1 178.56(18) . . . 2_575 ?
C14 C13 C12 N11 -2.1(5) . . . . ?
C4 C3 C30 N31 -101.1(3) . . . . ?
C4 C5 C20 N21 -110.8(3) . . . . ?
C23 C24 C27 O29 -10.5(4) . . . . ?
C23 C24 C27 O28 167.3(3) . . . . ?
C1 C6 C5 C4 -2.1(4) . . . . ?
C1 C6 C5 C20 175.6(3) . . . . ?
C1 C2 C3 C4 -2.0(4) . . . . ?
C1 C2 C3 C30 174.7(3) . . . . ?
C35 C34 C33 C32 3.1(4) . . . . ?
C13 C14 C15 C16 -0.9(4) . . . . ?
C8 C2 C3 C4 178.5(3) . . . . ?
C8 C2 C3 C30 -4.7(4) . . . . ?
C8 C2 C1 C6 175.8(3) . . . . ?
C8 C2 C1 C10 -7.6(4) . . . . ?
C5 C6 C1 C2 5.7(4) . . . . ?
C5 C6 C1 C10 -171.0(3) . . . . ?
C16 N11 C12 C13 0.8(4) . . . . ?
C16 N11 C10 C1 -52.3(4) . . . . ?
C26 N21 C22 C23 -3.8(5) . . . . ?
C26 N21 C20 C5 -124.3(3) . . . . ?
C26 C25 C24 C23 -5.5(4) . . . . ?
C26 C25 C24 C27 170.3(3) . . . . ?
C33 C34 C35 C36 -2.0(4) . . . . ?
C22 N21 C26 C25 4.1(4) . . . . ?
C22 N21 C20 C5 61.0(4) . . . . ?
C22 C23 C24 C25 5.8(4) . . . . ?
C22 C23 C24 C27 -170.0(3) . . . . ?
C25 C24 C27 O29 173.7(3) . . . . ?
C25 C24 C27 O28 -8.5(4) . . . . ?
C15 C14 C13 C12 2.1(4) . . . . ?
C12 N11 C16 C15 0.5(5) . . . . ?
C12 N11 C10 C1 133.5(3) . . . . ?
C7 C6 C1 C2 -172.8(3) . . . . ?
C7 C6 C1 C10 10.5(4) . . . . ?
C7 C6 C5 C4 176.3(3) . . . . ?
C7 C6 C5 C20 -5.9(4) . . . . ?
C30 N31 C36 C35 -175.3(3) . . . . ?
C30 N31 C32 C33 176.3(3) . . . . ?
C30 C3 C4 C9 8.1(4) . . . . ?
C30 C3 C4 C5 -171.2(3) . . . . ?
C24 C23 C22 N21 -1.2(5) . . . . ?
C36 N31 C30 C3 -170.6(3) . . . . ?
C36 N31 C32 C33 -1.3(4) . . . . ?
C10 N11 C16 C15 -173.5(3) . . . . ?
C10 N11 C12 C13 174.9(3) . . . . ?
C20 N21 C26 C25 -170.4(3) . . . . ?
C20 N21 C22 C23 170.8(3) . . . . ?
C32 N31 C30 C3 11.7(4) . . . . ?
C32 N31 C36 C35 2.5(4) . . . . ?
O19 C17 C14 C13 170.4(3) . . . . ?
O19 C17 C14 C15 -7.7(4) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.183
_oxdiff_exptl_absorpt_empirical_full_min 0.819
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_jj003_br_yb_otf_kotfx6_h2o_acet_red3_clark
_database_code_depnum_ccdc_archive 'CCDC 1833440'
loop_
_audit_author_name
_audit_author_address
'Antti Tiihonen'
;University of Jyv?skyl?, Department of Chemistry
Finland
;
_audit_update_record             
;
2018-03-29 deposited with the CCDC.	2019-02-28 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_CHEMW03_I                   
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: The structure contains voids of unresolved electron density
which was treated using Olex2 solvent mask procedure (full details in 
_smtbx_masks_special_details). The 5 water molecules per asymmetric unit 
 are included in the formula and used in the calculations. 
;
_vrf_DIFMN02_I                   
;
PROBLEM: The minimum difference density is < -0.1*ZMAX*1.00 
RESPONSE: Absorption effect of heavy Yb atom due to Cu-radiation.
;
_vrf_PLAT098_I                   
;
PROBLEM: Large Reported Min.  (Negative) Residual Density
RESPONSE: See vrf_DIFMN02_I).
;
_vrf_PLAT420_I                   
;
PROBLEM: D-H Without Acceptor       O       --H 
RESPONSE: Hydrogen bond acceptor (water located in a void) have been removed 
among the other disordered solvents (also water) in the voids 
(see vrf_CHEMW03_ALERT_2_B).
;
_vrf_FORMU01_I                   
;
PROBLEM: There is a discrepancy between the atom counts in the
            _chemical_formula_sum and _chemical_formula_moiety.
RESPONSE: See explanation above (CHEMW03_ALERT_2_B).
;
_vrf_CELLZ01_I                   
;
PROBLEM: Difference between formula and atom_site contents detected.
RESPONSE: See explanation above (CHEMW03_ALERT_2_B).
;
_vrf_PLAT041_I                   
;
PROBLEM: Calculated and Reported SumFormula strings Differ ...    
RESPONSE: See explanation above (CHEMW03_ALERT_2_B).
;
_vrf_PLAT042_I                   
;
PROBLEM: Calculated and Reported Moiety formula strings Differ by ...
RESPONSE: See explanation above (CHEMW03_ALERT_2_B).
;
_vrf_PLAT068_I                   
;
PROBLEM: Reported F000 Differs from Calcd (or Missing)...
RESPONSE: See explanation above (CHEMW03_ALERT_2_B).
;
_vrf_PLAT606_I                   
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure
RESPONSE: See explanation above (CHEMW03_ALERT_2_B).
;
# end Validation Reply Form

_audit_creation_date             2018-03-26
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H31 N3 O8 Yb, 2.9(C F3 O3 S), 0.1(Br)'
_chemical_formula_sum            'C32.90 H41 Br0.10 F8.70 N3 O21.70 S2.90 Yb'
_chemical_formula_weight         1264.99
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C33 H34 F9 N3 O17 S3 Yb1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Yb Yb -7.2108 4.4329 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.0256(3)
_cell_length_b                   14.2571(4)
_cell_length_c                   18.5311(5)
_cell_angle_alpha                109.018(3)
_cell_angle_beta                 105.086(3)
_cell_angle_gamma                95.287(2)
_cell_volume                     2372.01(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    10585
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      76.3350
_cell_measurement_theta_min      4.5710
_shelx_estimated_absorpt_T_max   0.796
_shelx_estimated_absorpt_T_min   0.503
_exptl_absorpt_coefficient_mu    5.989
_exptl_absorpt_correction_T_max  0.828
_exptl_absorpt_correction_T_min  0.655
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.43c (Rigaku Oxford Diffraction, 2018)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.771
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1262
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-6 -1 -1 0.0418
6 1 1 0.0418
-1 -8 9 0.0236
0 -1 -11 0.0118
0 9 -6 0.0223
0 1 10 0.0282

_exptl_crystal_size_max          0.133
_exptl_crystal_size_mid          0.059
_exptl_crystal_size_min          0.04
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-6.0005 -0.9960 -1.0027 -0.5736 -0.7631 0.4069
6.0005 0.9960 1.0027 0.5736 0.7631 -0.4069
-1.0044 -8.0002 9.0088 -0.5874 0.5831 0.5604
0.0069 -0.9981 -11.0017 0.5236 -0.6990 0.6085
0.0022 9.0003 -6.0096 0.3467 -0.5220 -0.7691
-0.0063 0.9983 10.0015 -0.4754 0.6341 -0.5637

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_av_unetI/netI     0.0577
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            14829
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.995
_diffrn_reflns_theta_min         3.428
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -116.00 -17.00   1.00    2.50    --  -41.78 -37.00-180.00   99
  2  ω   -116.00 -23.00   1.00    2.50    --  -41.78 -37.00  90.00   93
  3  ω      1.00  49.00   1.00    2.50    --   41.78 -99.00  60.00   48
  4  ω      1.00  62.00   1.00    2.50    --   41.78 -99.00 -30.00   61
  5  ω     53.00  97.00   1.00    2.50    --   41.78-125.00-180.00   44
  6  ω     66.00 109.00   1.00    7.50    --  112.00 -94.00-120.00   43
  7  ω     50.00 109.00   1.00    7.50    --  112.00 -94.00 -60.00   59
  8  ω     65.00 150.00   1.00    7.50    --  112.00 178.00-180.00   85
  9  ω    148.00 176.00   1.00    7.50    --  112.00 111.00 120.00   28
 10  ω     73.00 149.00   1.00    7.50    --  112.00 178.00 150.00   76
 11  ω     83.00 166.00   1.00    7.50    --  112.00  61.00 -90.00   83
 12  ω     32.00 151.00   1.00    7.50    --  112.00 -15.00  90.00  119
 13  ω     40.00 116.00   1.00    7.50    --  112.00-111.00 150.00   76
 14  ω     44.00 136.00   1.00    7.50    --  112.00 -61.00 120.00   92
 15  ω     36.00 140.00   1.00    7.50    --  112.00 -30.00-120.00  104
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1025755000
_diffrn_orient_matrix_UB_12      0.0063778000
_diffrn_orient_matrix_UB_13      -0.0481056000
_diffrn_orient_matrix_UB_21      0.1187461000
_diffrn_orient_matrix_UB_22      -0.0146606000
_diffrn_orient_matrix_UB_23      0.0649433000
_diffrn_orient_matrix_UB_31      -0.0411655000
_diffrn_orient_matrix_UB_32      -0.1154024000
_diffrn_orient_matrix_UB_33      -0.0448677000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7681
_reflns_number_total             8573
_reflns_odcompleteness_completeness 99.16
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         2.995
_refine_diff_density_min         -7.199
_refine_diff_density_rms         0.282
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.184
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     682
_refine_ls_number_reflns         8573
_refine_ls_number_restraints     222
_refine_ls_R_factor_all          0.0913
_refine_ls_R_factor_gt           0.0822
_refine_ls_restrained_S_all      1.172
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1894P)²+10.0617P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2401
_refine_ls_wR_factor_ref         0.2745
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 H2WB-O59A
 2 with sigma of 0.02
 O58A_$1-H1WB
 1.95 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F53A) \\sim Ueq, Uanis(O50A) \\sim Ueq, Uanis(S48A) \\sim Ueq,
Uanis(C52A) \\sim Ueq, Uanis(O49A) \\sim Ueq, Uanis(O51A) \\sim Ueq,
Uanis(F55A) \\sim Ueq, Uanis(F54A) \\sim Ueq, Uanis(F53B) \\sim Ueq,
Uanis(S48B) \\sim Ueq, Uanis(O49B) \\sim Ueq, Uanis(O51B) \\sim Ueq,
Uanis(C52B) \\sim Ueq, Uanis(O50B) \\sim Ueq, Uanis(F54B) \\sim Ueq,
Uanis(F55B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O19) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(O29) \\sim Ueq, Uanis(C27)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 F53B, S48B, O49B, O51B, C52B, O50B, F54B, F55B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F53A, O50A, S48A, C52A, O49A, O51A, F55A, F54A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(S48B)=Sof(O49B)=Sof(F54B)=Sof(O51B)=Sof(F55B)=Sof(C52B)=Sof(F53B)=
 Sof(O50B)=1-FVAR(1)
 Sof(O50A)=Sof(F53A)=Sof(C52A)=Sof(F55A)=Sof(S48A)=Sof(O49A)=Sof(O51A)=
 Sof(F54A)=FVAR(1)
 Fixed Sof: S56A(0.9) O58A(0.9) O59A(0.9) F61A(0.9) F63A(0.9) O57A(0.9)
 F62A(0.9) C60A(0.9) Br1B(0.1)
6.a Rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
6.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C20(H20A,H20B), C30(H30A,H30B)
6.c Aromatic/amide H refined with riding coordinates:
 C25(H25), C12(H12), C26(H26), C13(H13), C32(H32), C33(H33), C35(H35),
 C22(H22), C23(H23), C36(H36), C16(H16), C15(H15)
6.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Yb1 Yb 0.24629(4) -0.00946(3) 0.50272(2) 0.0212(2) Uani 1 1 d . . . . .
S40 S 0.1907(2) 0.77100(16) 1.08999(14) 0.0303(5) Uani 1 1 d . . . . .
S48B S 0.280(2) 0.4425(16) 0.7886(13) 0.031(3) Uani 0.38(2) 1 d . U P A 2
O38 O 0.3906(7) 0.9380(5) 0.5917(4) 0.0320(14) Uani 1 1 d . . . . .
O18 O 0.4274(6) 0.1273(4) 0.5803(3) 0.0242(12) Uani 1 1 d . . . . .
O19 O 0.6263(6) 0.0793(4) 0.5792(4) 0.0250(12) Uani 1 1 d . U . . .
O41 O 0.0592(7) 0.7010(5) 1.0537(5) 0.0389(16) Uani 1 1 d . . . . .
O42 O 0.2032(12) 0.8507(7) 1.1634(6) 0.067(3) Uani 1 1 d . . . . .
O49B O 0.399(4) 0.432(2) 0.846(2) 0.040(6) Uani 0.38(2) 1 d . U P A 2
O43 O 0.3103(8) 0.7242(6) 1.0914(7) 0.065(3) Uani 1 1 d . . . . .
O50A O 0.167(3) 0.4435(16) 0.8156(18) 0.043(5) Uani 0.62(2) 1 d . U P A 1
F47 F 0.1706(14) 0.7804(9) 0.9498(5) 0.109(5) Uani 1 1 d . . . . .
F46 F 0.3216(10) 0.8990(7) 1.0466(5) 0.077(3) Uani 1 1 d . . . . .
F54B F 0.232(3) 0.569(2) 0.7118(19) 0.072(7) Uani 0.38(2) 1 d . U P A 2
F45 F 0.0974(11) 0.8963(7) 1.0223(7) 0.106(4) Uani 1 1 d . . . . .
O39 O 0.3851(9) 0.7769(5) 0.5201(4) 0.0461(19) Uani 1 1 d . . . . .
N11 N 0.7897(8) 0.4037(5) 0.8018(4) 0.0234(14) Uani 1 1 d . . . . .
O51B O 0.236(4) 0.368(2) 0.709(2) 0.061(7) Uani 0.38(2) 1 d . U P A 2
N31 N 0.7249(9) 0.8306(6) 0.7838(5) 0.0350(19) Uani 1 1 d . . . . .
F55B F 0.445(3) 0.545(2) 0.7411(18) 0.072(7) Uani 0.38(2) 1 d . U P A 2
C6 C 0.8351(10) 0.6494(7) 0.8587(5) 0.0259(18) Uani 1 1 d . . . . .
C25 C 0.7049(9) 0.8395(6) 1.2524(5) 0.0268(17) Uani 1 1 d . U . . .
H25 H 0.657060 0.856422 1.291567 0.032 Uiso 1 1 calc R . . . .
C3 C 0.6889(9) 0.6933(7) 0.9726(5) 0.0278(18) Uani 1 1 d . . . . .
C1 C 0.8104(8) 0.5814(6) 0.8957(5) 0.0235(17) Uani 1 1 d . . . . .
C12 C 0.6480(10) 0.3881(7) 0.7779(5) 0.0302(19) Uani 1 1 d . . . . .
H12 H 0.600915 0.433902 0.807168 0.036 Uiso 1 1 calc R . . . .
C26 C 0.6289(10) 0.7931(8) 1.1744(5) 0.034(2) Uani 1 1 d . . . . .
H26 H 0.529018 0.778019 1.159124 0.041 Uiso 1 1 calc R . . . .
C2 C 0.7395(9) 0.6021(6) 0.9521(5) 0.0236(16) Uani 1 1 d . . . . .
F53A F 0.3310(18) 0.6536(10) 0.8786(9) 0.070(5) Uani 0.62(2) 1 d . U P A 1
N21 N 0.6964(8) 0.7678(6) 1.1175(4) 0.0275(16) Uani 1 1 d . . . . .
C13 C 0.5710(10) 0.3051(6) 0.7105(5) 0.0294(19) Uani 1 1 d . . . . .
H13 H 0.471291 0.295618 0.691695 0.035 Uiso 1 1 calc R . . . .
C14 C 0.6393(9) 0.2371(6) 0.6713(5) 0.0230(16) Uani 1 1 d . . . . .
C4 C 0.7167(10) 0.7643(7) 0.9388(5) 0.030(2) Uani 1 1 d . . . . .
C32 C 0.7314(11) 0.9180(7) 0.7717(6) 0.032(2) Uani 1 1 d . . . . .
H32 H 0.804169 0.973956 0.807189 0.039 Uiso 1 1 calc R . . . .
C33 C 0.6325(11) 0.9280(7) 0.7076(6) 0.039(2) Uani 1 1 d . . . . .
H33 H 0.634070 0.991644 0.701434 0.047 Uiso 1 1 calc R . . . .
C35 C 0.5278(12) 0.7565(8) 0.6680(7) 0.044(3) Uani 1 1 d . . . . .
H35 H 0.455915 0.699567 0.633237 0.053 Uiso 1 1 calc R . . . .
C22 C 0.8358(9) 0.7908(7) 1.1394(5) 0.0301(19) Uani 1 1 d . . . . .
H22 H 0.881657 0.773933 1.099365 0.036 Uiso 1 1 calc R . . . .
C23 C 0.9165(9) 0.8388(7) 1.2190(5) 0.0288(18) Uani 1 1 d . . . . .
H23 H 1.016231 0.854654 1.233259 0.035 Uiso 1 1 calc R . . . .
C5 C 0.7921(9) 0.7435(6) 0.8831(5) 0.0259(17) Uani 1 1 d . . . . .
C10 C 0.8743(9) 0.4881(6) 0.8786(5) 0.0282(19) Uani 1 1 d . . . . .
H10A H 0.970083 0.506184 0.875848 0.034 Uiso 1 1 calc R . . . .
H10B H 0.883517 0.463718 0.923639 0.034 Uiso 1 1 calc R . . . .
C36 C 0.6242(13) 0.7498(8) 0.7315(7) 0.053(3) Uani 1 1 d . . . . .
H36 H 0.621283 0.687315 0.739635 0.063 Uiso 1 1 calc R . . . .
C17 C 0.5566(9) 0.1398(6) 0.6039(5) 0.0250(17) Uani 1 1 d . . . . .
C16 C 0.8565(10) 0.3407(7) 0.7616(6) 0.033(2) Uani 1 1 d . . . . .
H16 H 0.956504 0.354407 0.778284 0.040 Uiso 1 1 calc R . . . .
C8 C 0.7218(11) 0.5287(8) 0.9936(6) 0.037(2) Uani 1 1 d . . . . .
H8A H 0.809698 0.537782 1.035847 0.055 Uiso 1 1 calc GR . . . .
H8B H 0.698765 0.459355 0.954439 0.055 Uiso 1 1 calc GR . . . .
H8C H 0.645570 0.541370 1.017353 0.055 Uiso 1 1 calc GR . . . .
C37 C 0.4263(10) 0.8526(7) 0.5811(6) 0.032(2) Uani 1 1 d . . . . .
C20 C 0.6054(10) 0.7152(8) 1.0306(5) 0.034(2) Uani 1 1 d . . . . .
H20A H 0.549418 0.650751 1.024886 0.040 Uiso 1 1 calc R . . . .
H20B H 0.538665 0.758236 1.016650 0.040 Uiso 1 1 calc R . . . .
C34 C 0.5331(10) 0.8458(7) 0.6534(6) 0.033(2) Uani 1 1 d . . . . .
C30 C 0.8358(11) 0.8225(7) 0.8517(6) 0.039(2) Uani 1 1 d . . . . .
H30A H 0.865087 0.889042 0.896253 0.047 Uiso 1 1 calc R . . . .
H30B H 0.918911 0.807125 0.833916 0.047 Uiso 1 1 calc R . . . .
C15 C 0.7840(10) 0.2557(7) 0.6961(6) 0.034(2) Uani 1 1 d . . . . .
H15 H 0.833308 0.210396 0.668248 0.041 Uiso 1 1 calc R . . . .
C7 C 0.9073(12) 0.6214(8) 0.7948(7) 0.040(2) Uani 1 1 d . . . . .
H7A H 1.009412 0.635496 0.820203 0.061 Uiso 1 1 calc GR . . . .
H7B H 0.884094 0.661281 0.760599 0.061 Uiso 1 1 calc GR . . . .
H7C H 0.875174 0.549269 0.762007 0.061 Uiso 1 1 calc GR . . . .
C44 C 0.1983(14) 0.8360(10) 1.0223(7) 0.059(4) Uani 1 1 d . . . . .
C9 C 0.6676(13) 0.8632(8) 0.9610(8) 0.050(3) Uani 1 1 d . . . . .
H9A H 0.565212 0.851388 0.937131 0.075 Uiso 1 1 calc GR . . . .
H9B H 0.713342 0.908635 0.940942 0.075 Uiso 1 1 calc GR . . . .
H9C H 0.692067 0.894088 1.019552 0.075 Uiso 1 1 calc GR . . . .
C52B C 0.342(4) 0.559(3) 0.770(2) 0.048(6) Uani 0.38(2) 1 d . U P A 2
C24 C 0.8504(9) 0.8631(6) 1.2772(5) 0.0239(16) Uani 1 1 d . . . . .
C27 C 0.9324(8) 0.9127(6) 1.3655(5) 0.0191(15) Uani 1 1 d . U . . .
O28 O 1.0642(6) 0.9257(4) 1.3824(3) 0.0256(12) Uani 1 1 d . . . . .
O29 O 0.8657(7) 0.9329(5) 1.4091(4) 0.0276(13) Uani 1 1 d . U . . .
O1W O 0.2147(7) 0.1159(5) 0.4496(4) 0.0335(15) Uani 1 1 d . . . . .
H1WA H 0.193045 0.169290 0.483363 0.050 Uiso 1 1 d GR . . . .
H1WB H 0.138506 0.094880 0.405804 0.050 Uiso 1 1 d DGR . . . .
O2W O 0.1117(7) -0.1484(5) 0.5045(4) 0.0341(14) Uani 1 1 d . . . . .
H2WA H 0.015245 -0.154400 0.480620 0.051 Uiso 1 1 d GR . . . .
H2WB H 0.114457 -0.143582 0.556329 0.051 Uiso 1 1 d DGR . . . .
C52A C 0.324(2) 0.5900(18) 0.8075(15) 0.048(4) Uani 0.62(2) 1 d . U P A 1
F55A F 0.4457(14) 0.6116(13) 0.7899(10) 0.069(5) Uani 0.62(2) 1 d . U P A 1
F53B F 0.376(3) 0.642(2) 0.8334(19) 0.076(7) Uani 0.38(2) 1 d . U P A 2
S48A S 0.3006(14) 0.4641(10) 0.8024(8) 0.035(2) Uani 0.62(2) 1 d . U P A 1
O49A O 0.425(2) 0.4653(16) 0.8626(12) 0.043(5) Uani 0.62(2) 1 d . U P A 1
O50B O 0.165(4) 0.473(3) 0.817(3) 0.039(7) Uani 0.38(2) 1 d . U P A 2
O51A O 0.2962(18) 0.4018(13) 0.7199(9) 0.050(4) Uani 0.62(2) 1 d . U P A 1
F54A F 0.2224(15) 0.6036(11) 0.7506(10) 0.060(4) Uani 0.62(2) 1 d . U P A 1
S56A S 0.0919(4) -0.1688(3) 0.6953(2) 0.0503(8) Uani 0.9 1 d . . P B 1
O58A O 0.0313(11) -0.0894(8) 0.6779(8) 0.081(4) Uani 0.9 1 d D . P B 1
O59A O 0.1738(12) -0.2048(9) 0.6403(7) 0.065(3) Uani 0.9 1 d D . P B 1
F61A F 0.2978(13) -0.1690(8) 0.8144(6) 0.094(4) Uani 0.9 1 d . . P B 1
F63A F 0.3206(11) -0.0364(9) 0.7882(7) 0.092(4) Uani 0.9 1 d . . P B 1
O57A O 0.0066(13) -0.2413(8) 0.7078(6) 0.067(3) Uani 0.9 1 d . . P B 1
F62A F 0.1754(15) -0.0645(11) 0.8484(7) 0.106(4) Uani 0.9 1 d . . P B 1
C60A C 0.2349(19) -0.1103(12) 0.7866(10) 0.061(4) Uani 0.9 1 d . . P B 1
Br1B Br 0.0569(18) -0.1197(13) 0.7283(12) 0.065(4) Uani 0.1 1 d . . P C 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Yb1 O38 2.266(6) 1_545 ?
Yb1 O18 2.308(6) . ?
Yb1 O19 2.277(6) 2_656 ?
Yb1 O28 2.321(5) 1_444 ?
Yb1 O29 2.267(6) 2_667 ?
Yb1 O1W 2.314(6) . ?
Yb1 O2W 2.306(6) . ?
S40 O41 1.430(7) . ?
S40 O42 1.427(9) . ?
S40 O43 1.424(9) . ?
S40 C44 1.798(12) . ?
S48B O49B 1.44(4) . ?
S48B O51B 1.43(4) . ?
S48B C52B 1.88(4) . ?
S48B O50B 1.43(4) . ?
O38 C37 1.269(11) . ?
O18 C17 1.230(10) . ?
O19 C17 1.209(11) . ?
O50A S48A 1.44(3) . ?
F47 C44 1.258(16) . ?
F46 C44 1.334(15) . ?
F54B C52B 1.38(4) . ?
F45 C44 1.386(19) . ?
O39 C37 1.221(12) . ?
N11 C12 1.346(12) . ?
N11 C10 1.504(10) . ?
N11 C16 1.321(12) . ?
N31 C32 1.336(12) . ?
N31 C36 1.354(13) . ?
N31 C30 1.490(12) . ?
F55B C52B 1.28(4) . ?
C6 C1 1.397(12) . ?
C6 C5 1.415(13) . ?
C6 C7 1.509(14) . ?
C25 H25 0.9500 . ?
C25 C26 1.348(12) . ?
C25 C24 1.383(12) . ?
C3 C2 1.412(12) . ?
C3 C4 1.395(14) . ?
C3 C20 1.501(13) . ?
C1 C2 1.381(13) . ?
C1 C10 1.506(11) . ?
C12 H12 0.9500 . ?
C12 C13 1.388(12) . ?
C26 H26 0.9500 . ?
C26 N21 1.368(12) . ?
C2 C8 1.509(13) . ?
F53A C52A 1.31(3) . ?
N21 C22 1.326(12) . ?
N21 C20 1.520(10) . ?
C13 H13 0.9500 . ?
C13 C14 1.362(12) . ?
C14 C17 1.515(11) . ?
C14 C15 1.374(12) . ?
C4 C5 1.405(14) . ?
C4 C9 1.502(13) . ?
C32 H32 0.9500 . ?
C32 C33 1.392(13) . ?
C33 H33 0.9500 . ?
C33 C34 1.368(14) . ?
C35 H35 0.9500 . ?
C35 C36 1.351(15) . ?
C35 C34 1.385(14) . ?
C22 H22 0.9500 . ?
C22 C23 1.384(12) . ?
C23 H23 0.9500 . ?
C23 C24 1.375(13) . ?
C5 C30 1.506(13) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C36 H36 0.9500 . ?
C16 H16 0.9500 . ?
C16 C15 1.375(12) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C37 C34 1.518(12) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C15 H15 0.9500 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C52B F53B 1.31(5) . ?
C24 C27 1.515(11) . ?
C27 O28 1.256(10) . ?
C27 O29 1.161(10) . ?
O1W H1WA 0.8988 . ?
O1W H1WB 0.8990 . ?
O2W H2WA 0.9354 . ?
O2W H2WB 0.9339 . ?
C52A F55A 1.37(3) . ?
C52A S48A 1.76(3) . ?
C52A F54A 1.34(2) . ?
S48A O49A 1.43(2) . ?
S48A O51A 1.48(2) . ?
S56A O58A 1.422(10) . ?
S56A O59A 1.465(12) . ?
S56A O57A 1.396(10) . ?
S56A C60A 1.792(17) . ?
F61A C60A 1.254(17) . ?
F63A C60A 1.284(19) . ?
F62A C60A 1.43(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O38 Yb1 O18 74.7(2) 1_545 . ?
O38 Yb1 O19 84.4(2) 1_545 2_656 ?
O38 Yb1 O28 140.4(2) 1_545 1_444 ?
O38 Yb1 O29 93.3(2) 1_545 2_667 ?
O38 Yb1 O1W 146.6(2) 1_545 . ?
O38 Yb1 O2W 74.5(2) 1_545 . ?
O18 Yb1 O28 142.6(2) . 1_444 ?
O18 Yb1 O1W 72.3(2) . . ?
O19 Yb1 O18 92.2(2) 2_656 . ?
O19 Yb1 O28 81.8(2) 2_656 1_444 ?
O19 Yb1 O1W 91.8(2) 2_656 . ?
O19 Yb1 O2W 103.3(2) 2_656 . ?
O29 Yb1 O18 83.9(2) 2_667 . ?
O29 Yb1 O19 175.84(19) 2_667 2_656 ?
O29 Yb1 O28 102.1(2) 2_667 1_444 ?
O29 Yb1 O1W 88.2(2) 2_667 . ?
O29 Yb1 O2W 79.4(2) 2_667 . ?
O1W Yb1 O28 71.0(2) . 1_444 ?
O2W Yb1 O18 143.8(2) . . ?
O2W Yb1 O28 72.8(2) . 1_444 ?
O2W Yb1 O1W 138.2(2) . . ?
O41 S40 C44 105.5(5) . . ?
O42 S40 O41 115.7(6) . . ?
O42 S40 C44 103.4(6) . . ?
O43 S40 O41 113.8(5) . . ?
O43 S40 O42 114.1(6) . . ?
O43 S40 C44 102.4(7) . . ?
O49B S48B C52B 105(2) . . ?
O51B S48B O49B 117(2) . . ?
O51B S48B C52B 101(2) . . ?
O50B S48B O49B 116(3) . . ?
O50B S48B O51B 114(3) . . ?
O50B S48B C52B 100(2) . . ?
C37 O38 Yb1 129.3(6) . 1_565 ?
C17 O18 Yb1 135.1(5) . . ?
C17 O19 Yb1 153.5(6) . 2_656 ?
C12 N11 C10 120.5(7) . . ?
C16 N11 C12 120.7(7) . . ?
C16 N11 C10 118.6(7) . . ?
C32 N31 C36 119.6(8) . . ?
C32 N31 C30 118.7(8) . . ?
C36 N31 C30 121.5(8) . . ?
C1 C6 C5 118.5(9) . . ?
C1 C6 C7 119.5(8) . . ?
C5 C6 C7 122.0(8) . . ?
C26 C25 H25 119.0 . . ?
C26 C25 C24 121.9(8) . . ?
C24 C25 H25 119.0 . . ?
C2 C3 C20 120.8(9) . . ?
C4 C3 C2 119.8(9) . . ?
C4 C3 C20 119.4(8) . . ?
C6 C1 C10 118.5(8) . . ?
C2 C1 C6 121.5(8) . . ?
C2 C1 C10 119.8(8) . . ?
N11 C12 H12 120.1 . . ?
N11 C12 C13 119.8(9) . . ?
C13 C12 H12 120.1 . . ?
C25 C26 H26 120.2 . . ?
C25 C26 N21 119.7(8) . . ?
N21 C26 H26 120.2 . . ?
C3 C2 C8 120.6(8) . . ?
C1 C2 C3 119.8(8) . . ?
C1 C2 C8 119.6(8) . . ?
C26 N21 C20 117.3(8) . . ?
C22 N21 C26 119.6(7) . . ?
C22 N21 C20 123.1(8) . . ?
C12 C13 H13 120.2 . . ?
C14 C13 C12 119.6(8) . . ?
C14 C13 H13 120.2 . . ?
C13 C14 C17 120.3(8) . . ?
C13 C14 C15 119.3(8) . . ?
C15 C14 C17 120.4(8) . . ?
C3 C4 C5 119.8(8) . . ?
C3 C4 C9 121.1(10) . . ?
C5 C4 C9 119.1(10) . . ?
N31 C32 H32 119.7 . . ?
N31 C32 C33 120.7(9) . . ?
C33 C32 H32 119.7 . . ?
C32 C33 H33 120.1 . . ?
C34 C33 C32 119.8(9) . . ?
C34 C33 H33 120.1 . . ?
C36 C35 H35 119.8 . . ?
C36 C35 C34 120.4(10) . . ?
C34 C35 H35 119.8 . . ?
N21 C22 H22 119.0 . . ?
N21 C22 C23 122.0(8) . . ?
C23 C22 H22 119.0 . . ?
C22 C23 H23 120.4 . . ?
C24 C23 C22 119.1(8) . . ?
C24 C23 H23 120.4 . . ?
C6 C5 C30 118.6(9) . . ?
C4 C5 C6 120.4(8) . . ?
C4 C5 C30 120.9(9) . . ?
N11 C10 C1 113.4(7) . . ?
N11 C10 H10A 108.9 . . ?
N11 C10 H10B 108.9 . . ?
C1 C10 H10A 108.9 . . ?
C1 C10 H10B 108.9 . . ?
H10A C10 H10B 107.7 . . ?
N31 C36 H36 119.4 . . ?
C35 C36 N31 121.3(10) . . ?
C35 C36 H36 119.4 . . ?
O18 C17 C14 118.9(7) . . ?
O19 C17 O18 125.7(7) . . ?
O19 C17 C14 115.3(7) . . ?
N11 C16 H16 119.4 . . ?
N11 C16 C15 121.2(9) . . ?
C15 C16 H16 119.4 . . ?
C2 C8 H8A 109.5 . . ?
C2 C8 H8B 109.5 . . ?
C2 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O38 C37 C34 115.1(8) . . ?
O39 C37 O38 127.5(8) . . ?
O39 C37 C34 117.4(8) . . ?
C3 C20 N21 113.3(7) . . ?
C3 C20 H20A 108.9 . . ?
C3 C20 H20B 108.9 . . ?
N21 C20 H20A 108.9 . . ?
N21 C20 H20B 108.9 . . ?
H20A C20 H20B 107.7 . . ?
C33 C34 C35 118.1(9) . . ?
C33 C34 C37 121.5(8) . . ?
C35 C34 C37 120.3(9) . . ?
N31 C30 C5 114.9(8) . . ?
N31 C30 H30A 108.6 . . ?
N31 C30 H30B 108.6 . . ?
C5 C30 H30A 108.6 . . ?
C5 C30 H30B 108.6 . . ?
H30A C30 H30B 107.5 . . ?
C14 C15 C16 119.2(9) . . ?
C14 C15 H15 120.4 . . ?
C16 C15 H15 120.4 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
F47 C44 S40 115.5(10) . . ?
F47 C44 F46 109.9(13) . . ?
F47 C44 F45 104.3(12) . . ?
F46 C44 S40 111.4(8) . . ?
F46 C44 F45 105.7(11) . . ?
F45 C44 S40 109.2(11) . . ?
C4 C9 H9A 109.5 . . ?
C4 C9 H9B 109.5 . . ?
C4 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
F54B C52B S48B 107(2) . . ?
F55B C52B S48B 109(3) . . ?
F55B C52B F54B 108(3) . . ?
F55B C52B F53B 111(3) . . ?
F53B C52B S48B 114(3) . . ?
F53B C52B F54B 108(3) . . ?
C25 C24 C27 120.5(8) . . ?
C23 C24 C25 117.6(8) . . ?
C23 C24 C27 121.9(7) . . ?
O28 C27 C24 115.8(7) . . ?
O29 C27 C24 116.0(7) . . ?
O29 C27 O28 128.2(8) . . ?
C27 O28 Yb1 133.1(5) . 1_666 ?
C27 O29 Yb1 166.7(6) . 2_667 ?
Yb1 O1W H1WA 111.1 . . ?
Yb1 O1W H1WB 110.7 . . ?
H1WA O1W H1WB 103.0 . . ?
Yb1 O2W H2WA 113.0 . . ?
Yb1 O2W H2WB 112.6 . . ?
H2WA O2W H2WB 101.2 . . ?
F53A C52A F55A 110(2) . . ?
F53A C52A S48A 111.7(16) . . ?
F53A C52A F54A 109.8(19) . . ?
F55A C52A S48A 108.8(17) . . ?
F54A C52A F55A 104.4(18) . . ?
F54A C52A S48A 111.6(17) . . ?
O50A S48A C52A 106.3(14) . . ?
O50A S48A O51A 111.1(14) . . ?
O49A S48A O50A 117.3(18) . . ?
O49A S48A C52A 102.1(12) . . ?
O49A S48A O51A 113.1(15) . . ?
O51A S48A C52A 105.7(14) . . ?
O58A S56A O59A 107.8(8) . . ?
O58A S56A C60A 106.5(7) . . ?
O59A S56A C60A 98.6(8) . . ?
O57A S56A O58A 117.7(8) . . ?
O57A S56A O59A 117.7(7) . . ?
O57A S56A C60A 106.2(7) . . ?
F61A C60A S56A 116.2(12) . . ?
F61A C60A F63A 112.2(15) . . ?
F61A C60A F62A 100.4(14) . . ?
F63A C60A S56A 115.2(11) . . ?
F63A C60A F62A 103.7(15) . . ?
F62A C60A S56A 107.1(12) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1W H1WB O58A 0.90 1.96 2.831(10) 163.8 2_556 yes
O2W H2WB O59A 0.93 2.01 2.822(12) 144.6 . yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Yb1 O38 C37 O39 -3.5(17) 1_565 . . . ?
Yb1 O38 C37 C34 176.3(6) 1_565 . . . ?
Yb1 O18 C17 O19 13.2(15) . . . . ?
Yb1 O18 C17 C14 -164.8(5) . . . . ?
Yb1 O19 C17 O18 92.6(15) 2_656 . . . ?
Yb1 O19 C17 C14 -89.3(13) 2_656 . . . ?
O38 C37 C34 C33 -31.2(15) . . . . ?
O38 C37 C34 C35 145.8(11) . . . . ?
O41 S40 C44 F47 -49.0(14) . . . . ?
O41 S40 C44 F46 -175.4(10) . . . . ?
O41 S40 C44 F45 68.1(9) . . . . ?
O42 S40 C44 F47 -170.9(13) . . . . ?
O42 S40 C44 F46 62.7(13) . . . . ?
O42 S40 C44 F45 -53.8(10) . . . . ?
O49B S48B C52B F54B 177(3) . . . . ?
O49B S48B C52B F55B 61(3) . . . . ?
O49B S48B C52B F53B -64(3) . . . . ?
O43 S40 C44 F47 70.3(13) . . . . ?
O43 S40 C44 F46 -56.2(12) . . . . ?
O43 S40 C44 F45 -172.6(8) . . . . ?
O39 C37 C34 C33 148.6(11) . . . . ?
O39 C37 C34 C35 -34.4(16) . . . . ?
N11 C12 C13 C14 3.3(14) . . . . ?
N11 C16 C15 C14 1.1(16) . . . . ?
O51B S48B C52B F54B 55(3) . . . . ?
O51B S48B C52B F55B -62(3) . . . . ?
O51B S48B C52B F53B 174(3) . . . . ?
N31 C32 C33 C34 -4.2(18) . . . . ?
C6 C1 C2 C3 0.7(12) . . . . ?
C6 C1 C2 C8 -176.9(8) . . . . ?
C6 C1 C10 N11 -82.4(10) . . . . ?
C6 C5 C30 N31 100.4(11) . . . . ?
C25 C26 N21 C22 -1.2(14) . . . . ?
C25 C26 N21 C20 179.7(9) . . . . ?
C25 C24 C27 O28 175.8(8) . . . . ?
C25 C24 C27 O29 -3.3(12) . . . . ?
C3 C4 C5 C6 2.6(12) . . . . ?
C3 C4 C5 C30 -174.0(8) . . . . ?
C1 C6 C5 C4 -4.9(12) . . . . ?
C1 C6 C5 C30 171.8(8) . . . . ?
C12 N11 C10 C1 -35.7(12) . . . . ?
C12 N11 C16 C15 -2.3(15) . . . . ?
C12 C13 C14 C17 172.7(8) . . . . ?
C12 C13 C14 C15 -4.5(14) . . . . ?
C26 C25 C24 C23 0.8(14) . . . . ?
C26 C25 C24 C27 -178.4(8) . . . . ?
C26 N21 C22 C23 1.0(15) . . . . ?
C26 N21 C20 C3 178.3(9) . . . . ?
C2 C3 C4 C5 1.4(12) . . . . ?
C2 C3 C4 C9 -178.4(8) . . . . ?
C2 C3 C20 N21 88.8(10) . . . . ?
C2 C1 C10 N11 102.9(9) . . . . ?
F53A C52A S48A O50A 62(2) . . . . ?
F53A C52A S48A O49A -61(2) . . . . ?
F53A C52A S48A O51A -179.6(16) . . . . ?
N21 C22 C23 C24 0.2(15) . . . . ?
C13 C14 C17 O18 6.5(13) . . . . ?
C13 C14 C17 O19 -171.8(8) . . . . ?
C13 C14 C15 C16 2.3(15) . . . . ?
C4 C3 C2 C1 -3.1(11) . . . . ?
C4 C3 C2 C8 174.5(8) . . . . ?
C4 C3 C20 N21 -91.1(10) . . . . ?
C4 C5 C30 N31 -82.9(11) . . . . ?
C32 N31 C36 C35 -1(2) . . . . ?
C32 N31 C30 C5 155.3(10) . . . . ?
C32 C33 C34 C35 4.9(18) . . . . ?
C32 C33 C34 C37 -178.0(10) . . . . ?
C22 N21 C20 C3 -0.8(14) . . . . ?
C22 C23 C24 C25 -1.0(13) . . . . ?
C22 C23 C24 C27 178.1(8) . . . . ?
C23 C24 C27 O28 -3.3(12) . . . . ?
C23 C24 C27 O29 177.5(8) . . . . ?
C5 C6 C1 C2 3.3(12) . . . . ?
C5 C6 C1 C10 -171.3(7) . . . . ?
C10 N11 C12 C13 -174.7(9) . . . . ?
C10 N11 C16 C15 172.5(9) . . . . ?
C10 C1 C2 C3 175.2(7) . . . . ?
C10 C1 C2 C8 -2.4(11) . . . . ?
C36 N31 C32 C33 2.4(17) . . . . ?
C36 N31 C30 C5 -29.2(16) . . . . ?
C36 C35 C34 C33 -4.0(19) . . . . ?
C36 C35 C34 C37 178.8(12) . . . . ?
C17 C14 C15 C16 -174.8(9) . . . . ?
C16 N11 C12 C13 0.1(14) . . . . ?
C16 N11 C10 C1 149.5(9) . . . . ?
C20 C3 C2 C1 177.0(7) . . . . ?
C20 C3 C2 C8 -5.5(12) . . . . ?
C20 C3 C4 C5 -178.6(7) . . . . ?
C20 C3 C4 C9 1.6(12) . . . . ?
C20 N21 C22 C23 -179.9(9) . . . . ?
C34 C35 C36 N31 2(2) . . . . ?
C30 N31 C32 C33 178.0(11) . . . . ?
C30 N31 C36 C35 -177.0(12) . . . . ?
C15 C14 C17 O18 -176.5(9) . . . . ?
C15 C14 C17 O19 5.3(13) . . . . ?
C7 C6 C1 C2 -177.2(8) . . . . ?
C7 C6 C1 C10 8.2(12) . . . . ?
C7 C6 C5 C4 175.7(8) . . . . ?
C7 C6 C5 C30 -7.7(13) . . . . ?
C9 C4 C5 C6 -177.6(8) . . . . ?
C9 C4 C5 C30 5.8(13) . . . . ?
C24 C25 C26 N21 0.3(15) . . . . ?
C24 C27 O28 Yb1 -177.7(5) . . . 1_666 ?
C24 C27 O29 Yb1 -108(3) . . . 2_667 ?
O28 C27 O29 Yb1 73(3) . . . 2_667 ?
O29 C27 O28 Yb1 1.3(13) . . . 1_666 ?
F55A C52A S48A O50A -175.9(18) . . . . ?
F55A C52A S48A O49A 61(2) . . . . ?
F55A C52A S48A O51A -57.8(18) . . . . ?
O50B S48B C52B F54B -62(3) . . . . ?
O50B S48B C52B F55B -179(3) . . . . ?
O50B S48B C52B F53B 57(4) . . . . ?
F54A C52A S48A O50A -61(2) . . . . ?
F54A C52A S48A O49A 175(2) . . . . ?
F54A C52A S48A O51A 57(2) . . . . ?
O58A S56A C60A F61A 176.4(15) . . . . ?
O58A S56A C60A F63A -49.5(17) . . . . ?
O58A S56A C60A F62A 65.2(13) . . . . ?
O59A S56A C60A F61A -72.1(16) . . . . ?
O59A S56A C60A F63A 62.0(15) . . . . ?
O59A S56A C60A F62A 176.7(10) . . . . ?
O57A S56A C60A F61A 50.2(18) . . . . ?
O57A S56A C60A F63A -175.8(14) . . . . ?
O57A S56A C60A F62A -61.0(12) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.137 0.500 0.500 352.2 104.9 '10x water'

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.800
_oxdiff_exptl_absorpt_empirical_full_min 0.628
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_jj003_no3_nd_no3_agno3_h2o_acet_red2
_database_code_depnum_ccdc_archive 'CCDC 1842358'
loop_
_audit_author_name
_audit_author_address
'Antti Tiihonen'
;University of Jyv?skyl?, Department of Chemistry
Finland
;
_audit_update_record             
;
2018-05-09 deposited with the CCDC.	2019-02-28 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_CHEMW03_I                   
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: The structure contains voids of unresolved electron density
which was treated using Olex2 solvent mask procedure (full details in 
_smtbx_masks_special_details). The 6 water molecules per asymmetric unit 
 are included in the formula and used in the calculations.
;
_vrf_PLAT420_I                   
;
PROBLEM: D-H Without Acceptor...
RESPONSE: Hydrogen bond acceptors (water) have been removed among
other disordered solvent from the voids (see CHEMW03_ALERT_2_A).
;
_vrf_FORMU01_I                   
;
PROBLEM: There is a discrepancy between the atom counts...
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_CELLZ01_I                   
;
PROBLEM: Difference between formula and atom_site...
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT041_I                   
;
PROBLEM: Calc. and Reported SumFormula Strings  Differ...
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT051_I                   
;
PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs...
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
_vrf_PLAT068_I                   
;
PROBLEM: Reported F000 Differs from Calcd (or Missing)...
RESPONSE: See explanation above (CHEMW03_ALERT_2_A).
;
# end Validation Reply Form
_audit_creation_date             2018-05-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H31 N3 Nd O8, 3(N O3), O'
_chemical_formula_sum            'C30 H43 N6 Nd O23'
_chemical_formula_weight         999.94
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C30 H32 O16 N6 Nd1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -3.1807 10.9079 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.5948(6)
_cell_length_b                   12.3229(9)
_cell_length_c                   18.8983(13)
_cell_angle_alpha                106.033(6)
_cell_angle_beta                 99.619(6)
_cell_angle_gamma                99.928(6)
_cell_volume                     2060.2(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8244
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      75.9390
_cell_measurement_theta_min      3.7810
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    10.441
_exptl_absorpt_correction_T_max  0.697
_exptl_absorpt_correction_T_min  0.240
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.43c (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1018
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-6 -1 1 0.0472
6 1 0 0.0244
0 -7 -3 0.0615
0 0 -11 0.0898
-6 1 2 0.0669
-2 -1 12 0.0930
5 -6 3 0.0673
-6 1 -1 0.0721
1 7 -8 0.0920
4 3 -11 0.0800
3 6 -2 0.0608
-2 7 1 0.0942
-5 -4 3 0.0542

_exptl_crystal_size_max          0.215
_exptl_crystal_size_mid          0.169
_exptl_crystal_size_min          0.078
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-6.0001 -0.9994 0.9984 0.7951 -0.5556 -0.3285
6.0001 0.9994 0.0016 -0.8575 0.5266 0.2750
-0.0000 -6.9995 -3.0009 0.3739 -0.5841 0.7851
0.0001 0.0004 -11.0002 0.6858 0.3189 0.5879
-6.0001 1.0004 1.9986 0.6794 -0.3929 -0.5604
-2.0002 -1.0002 11.9996 -0.4446 -0.5873 -0.6735
5.0001 -6.0003 3.0006 -0.7192 -0.3032 0.6788
-6.0001 1.0006 -1.0014 0.8664 -0.3059 -0.4001
1.0001 6.9998 -7.9991 0.1734 0.9747 -0.1365
4.0002 2.9999 -10.9988 0.0519 0.8936 0.5630
3.0001 5.9995 -1.9986 -0.4509 0.8485 -0.2465
-2.0000 6.9998 1.0003 0.0277 0.4985 -0.7997
-5.0002 -3.9994 2.9983 0.6121 -0.8294 -0.1069

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            13092
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.975
_diffrn_reflns_theta_min         3.836
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -67.00  31.00   2.00    2.00    --  -41.78  70.00 -89.00   49
  2  ω   -107.00 -13.00   2.00    2.00    --  -41.78 -77.00 150.00   47
  3  ω    -74.00  34.00   2.00    2.00    --  -41.78  77.00  30.00   54
  4  ω     47.00  73.00   2.00    2.00    --   41.78 -77.00  30.00   13
  5  ω    -34.00  -8.00   2.00    2.00    --   41.78 -77.00  30.00   13
  6  ω     73.00 115.00   2.00    4.00    --  112.00-111.00  30.00   21
  7  ω     92.00 178.00   2.00    4.00    --  112.00  61.00 -30.00   43
  8  ω    110.00 166.00   2.00    4.00    --  112.00  30.00  60.00   28
  9  ω    106.00 178.00   2.00    4.00    --  112.00  30.00  30.00   36
 10  ω     41.00 115.00   2.00    4.00    --  112.00-111.00-150.00   37
 11  ω     83.00 109.00   2.00    4.00    --  112.00-111.00 120.00   13
 12  ω     41.00  69.00   2.00    4.00    --  112.00 -61.00 -90.00   14
 13  ω     78.00 140.00   2.00    4.00    --  112.00 -61.00 -90.00   31
 14  ω     83.00 131.00   2.00    4.00    --  112.00  61.00 -90.00   24
 15  ω     90.00 176.00   2.00    4.00    --  112.00  30.00 120.00   43
 16  ω     42.00 140.00   2.00    4.00    --  112.00 -61.00  30.00   49
 17  ω     36.00 134.00   2.00    4.00    --  112.00 -77.00-150.00   49
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1384483000
_diffrn_orient_matrix_UB_12      -0.0266909000
_diffrn_orient_matrix_UB_13      -0.0623495000
_diffrn_orient_matrix_UB_21      0.0718105000
_diffrn_orient_matrix_UB_22      0.0958710000
_diffrn_orient_matrix_UB_23      -0.0289829000
_diffrn_orient_matrix_UB_31      0.0607149000
_diffrn_orient_matrix_UB_32      -0.0892576000
_diffrn_orient_matrix_UB_33      -0.0534480000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7147
_reflns_number_total             7471
_reflns_odcompleteness_completeness 99.51
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         1.800
_refine_diff_density_min         -1.732
_refine_diff_density_rms         0.107
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     549
_refine_ls_number_reflns         7471
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0401
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0749P)²+1.9810P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1081
_refine_ls_wR_factor_ref         0.1098
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 N48A-O49A \\sim N48A-O51A \\sim N48A-O50A
 with sigma of 0.02
 N48B-O51B \\sim N48B-O50B \\sim N48B-O49B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N48A) = Uanis(O50A) = Uanis(O49A) = Uanis(O51A)
Uanis(O49B) = Uanis(N48B) = Uanis(O51B) = Uanis(O50B)
4. Others
 Sof(N48B)=Sof(O51B)=Sof(O50B)=Sof(O49B)=Sof(O3WB)=1-FVAR(1)
 Sof(O3WA)=Sof(O3WC)=0.5*FVAR(2)
 Sof(N48A)=Sof(O49A)=Sof(O50A)=Sof(O51A)=FVAR(1)
 Sof(O42B)=Sof(O43B)=1-FVAR(2)
 Sof(O43A)=Sof(O42A)=FVAR(2)
 Sof(O47B)=1-FVAR(3)
 Sof(O47A)=FVAR(3)
5.a Rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
5.b Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C20(H20A,H20B), C10(H10A,H10B)
5.c Aromatic/amide H refined with riding coordinates:
 C32(H32), C33(H33), C35(H35), C36(H36), C16(H16), C23(H23), C13(H13),
 C12(H12), C15(H15), C22(H22), C25(H25), C26(H26)
5.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Nd1 Nd 0.26445(2) -0.51660(2) -0.00348(2) 0.02169(9) Uani 1 1 d . . . . .
O28 O 0.3907(3) 0.3617(3) 0.04946(17) 0.0329(6) Uani 1 1 d . . . . .
O29 O 0.6346(3) 0.4128(3) 0.08418(17) 0.0333(7) Uani 1 1 d . . . . .
N31 N 0.9338(4) 0.3580(3) 0.63373(18) 0.0255(7) Uani 1 1 d . . . . .
O41 O 0.2692(4) 0.2511(4) 0.5703(2) 0.0573(10) Uani 1 1 d . . . . .
N11 N 0.5558(4) -0.1139(3) 0.33521(19) 0.0285(7) Uani 1 1 d . . . . .
N21 N 0.4896(4) 0.3351(3) 0.30699(19) 0.0262(7) Uani 1 1 d . . . . .
C3 C 0.5764(4) 0.2695(3) 0.4183(2) 0.0229(7) Uani 1 1 d . . . . .
C6 C 0.7413(4) 0.1375(4) 0.4814(2) 0.0280(8) Uani 1 1 d . . . . .
C32 C 0.8123(4) 0.3810(4) 0.6549(2) 0.0278(8) Uani 1 1 d . . . . .
H32 H 0.726482 0.368693 0.617613 0.033 Uiso 1 1 calc R . . . .
C30 C 0.9404(4) 0.3170(5) 0.5516(2) 0.0338(10) Uani 1 1 d . . . . .
H30A H 1.004185 0.261528 0.544989 0.041 Uiso 1 1 calc R . . . .
H30B H 0.984040 0.384210 0.537139 0.041 Uiso 1 1 calc R . . . .
C5 C 0.7918(4) 0.2587(4) 0.4993(2) 0.0270(8) Uani 1 1 d . . . . .
C1 C 0.6057(4) 0.0837(3) 0.4309(2) 0.0257(8) Uani 1 1 d . . . . .
C33 C 0.8114(4) 0.4221(4) 0.7300(2) 0.0270(8) Uani 1 1 d . . . . .
H33 H 0.725789 0.439852 0.744578 0.032 Uiso 1 1 calc R . . . .
C4 C 0.7110(4) 0.3255(3) 0.4690(2) 0.0247(8) Uani 1 1 d . . . . .
C35 C 1.0609(4) 0.4156(4) 0.7618(2) 0.0266(8) Uani 1 1 d . . . . .
H35 H 1.147914 0.427700 0.798305 0.032 Uiso 1 1 calc R . . . .
C14 C 0.5848(4) -0.2522(4) 0.2000(2) 0.0281(8) Uani 1 1 d . . . . .
N40 N 0.3826(4) 0.3302(4) 0.5983(2) 0.0386(9) Uani 1 1 d . . . . .
C20 C 0.4844(4) 0.3417(4) 0.3882(2) 0.0294(8) Uani 1 1 d . . . . .
H20A H 0.518752 0.423567 0.420781 0.035 Uiso 1 1 calc R . . . .
H20B H 0.382522 0.314549 0.390583 0.035 Uiso 1 1 calc R . . . .
C2 C 0.5238(4) 0.1498(3) 0.3986(2) 0.0230(7) Uani 1 1 d . . . . .
C7 C 0.8336(5) 0.0705(5) 0.5167(2) 0.0394(10) Uani 1 1 d . . . . .
H7A H 0.923391 0.073227 0.498299 0.059 Uiso 1 1 calc GR . . . .
H7B H 0.780000 -0.010320 0.502887 0.059 Uiso 1 1 calc GR . . . .
H7C H 0.857465 0.105158 0.571783 0.059 Uiso 1 1 calc GR . . . .
C8 C 0.3787(5) 0.0917(4) 0.3432(2) 0.0338(9) Uani 1 1 d . . . . .
H8A H 0.326756 0.150975 0.335800 0.051 Uiso 1 1 calc GR . . . .
H8B H 0.320749 0.038927 0.363365 0.051 Uiso 1 1 calc GR . . . .
H8C H 0.394946 0.047715 0.294722 0.051 Uiso 1 1 calc GR . . . .
C24 C 0.5038(4) 0.3556(4) 0.1683(2) 0.0294(8) Uani 1 1 d . . . . .
C36 C 1.0585(4) 0.3761(4) 0.6859(2) 0.0262(8) Uani 1 1 d . . . . .
H36 H 1.144125 0.361475 0.670016 0.031 Uiso 1 1 calc R . . . .
C16 C 0.4361(5) -0.1815(4) 0.2830(3) 0.0383(10) Uani 1 1 d . . . . .
H16 H 0.342740 -0.181508 0.293594 0.046 Uiso 1 1 calc R . . . .
C23 C 0.6274(4) 0.3516(4) 0.2166(2) 0.0284(8) Uani 1 1 d . . . . .
H23 H 0.717442 0.356131 0.201727 0.034 Uiso 1 1 calc R . . . .
C13 C 0.7049(5) -0.1793(4) 0.2529(2) 0.0321(9) Uani 1 1 d . . . . .
H13 H 0.798867 -0.176761 0.242671 0.039 Uiso 1 1 calc R . . . .
C10 C 0.5427(5) -0.0448(4) 0.4115(2) 0.0317(9) Uani 1 1 d . . . . .
H10A H 0.593133 -0.073709 0.450230 0.038 Uiso 1 1 calc R . . . .
H10B H 0.438782 -0.057223 0.413318 0.038 Uiso 1 1 calc R . . . .
C12 C 0.6887(5) -0.1098(4) 0.3208(2) 0.0329(9) Uani 1 1 d . . . . .
H12 H 0.771378 -0.059074 0.357161 0.040 Uiso 1 1 calc R . . . .
C15 C 0.4487(5) -0.2503(4) 0.2147(3) 0.0389(10) Uani 1 1 d . . . . .
H15 H 0.364194 -0.296337 0.177595 0.047 Uiso 1 1 calc R . . . .
C27 C 0.5113(5) 0.3780(4) 0.0937(2) 0.0307(9) Uani 1 1 d . . . . .
C22 C 0.6176(4) 0.3409(4) 0.2866(2) 0.0288(8) Uani 1 1 d . . . . .
H22 H 0.701195 0.337565 0.320130 0.035 Uiso 1 1 calc R . . . .
C9 C 0.7604(5) 0.4568(4) 0.4916(2) 0.0354(10) Uani 1 1 d . . . . .
H9A H 0.762459 0.480328 0.446270 0.053 Uiso 1 1 calc GR . . . .
H9B H 0.857870 0.482188 0.524801 0.053 Uiso 1 1 calc GR . . . .
H9C H 0.692609 0.492666 0.518486 0.053 Uiso 1 1 calc GR . . . .
C25 C 0.3725(5) 0.3448(5) 0.1906(3) 0.0393(10) Uani 1 1 d . . . . .
H25 H 0.285907 0.343560 0.157299 0.047 Uiso 1 1 calc R . . . .
C26 C 0.3690(5) 0.3359(4) 0.2611(3) 0.0358(10) Uani 1 1 d . . . . .
H26 H 0.280058 0.330292 0.277120 0.043 Uiso 1 1 calc R . . . .
O38 O 1.0452(3) 0.4786(3) 0.91351(14) 0.0281(6) Uani 1 1 d . . . . .
O39 O 0.8169(3) 0.4927(3) 0.88500(15) 0.0351(7) Uani 1 1 d . . . . .
C34 C 0.9357(4) 0.4377(4) 0.7848(2) 0.0249(8) Uani 1 1 d . . . . .
C37 C 0.9329(4) 0.4727(3) 0.8682(2) 0.0236(7) Uani 1 1 d . . . . .
O1W O 0.0800(3) -0.7019(3) -0.0229(2) 0.0413(7) Uani 1 1 d . . . . .
H1WA H 0.114714 -0.755934 0.004689 0.062 Uiso 1 1 d GR . . . .
H1WB H 0.050307 -0.759487 -0.076222 0.062 Uiso 1 1 d GR . . . .
O2W O 0.2185(4) -0.3194(3) 0.0328(2) 0.0446(8) Uani 1 1 d . . . . .
H2WA H 0.282610 -0.274616 0.074109 0.067 Uiso 1 1 d GR . . . .
H2WB H 0.134669 -0.321557 0.046142 0.067 Uiso 1 1 d GR . . . .
O46 O -0.1364(6) -0.7892(4) -0.1769(2) 0.0705(13) Uani 1 1 d . . . . .
O19 O 0.7271(3) -0.3328(3) 0.11861(15) 0.0316(6) Uani 1 1 d . . . . .
O18 O 0.4877(3) -0.3967(3) 0.08078(16) 0.0315(6) Uani 1 1 d . . . . .
C17 C 0.6015(4) -0.3324(4) 0.1275(2) 0.0274(8) Uani 1 1 d . . . . .
N48A N 0.0091(8) -0.6682(8) 0.3322(5) 0.0703(12) Uani 0.661(5) 1 d D . P A 1
O49A O -0.0515(7) -0.6186(7) 0.3673(4) 0.0703(12) Uani 0.661(5) 1 d D . P A 1
O50A O 0.1116(7) -0.7100(7) 0.3478(4) 0.0703(12) Uani 0.661(5) 1 d D . P A 1
O51A O -0.0270(7) -0.6692(7) 0.2668(4) 0.0703(12) Uani 0.661(5) 1 d D . P A 1
O42B O 0.378(2) 0.4113(11) 0.6461(16) 0.080(6) Uani 0.59(4) 1 d . . P B 2
O43B O 0.4831(8) 0.308(2) 0.5710(6) 0.066(6) Uani 0.59(4) 1 d . . P B 2
N48B N -0.0072(17) -0.7521(15) 0.1346(8) 0.069(2) Uani 0.339(5) 1 d D . P A 2
O51B O 0.0138(16) -0.7505(13) 0.2005(8) 0.069(2) Uani 0.339(5) 1 d D . P A 2
O50B O -0.1163(15) -0.7159(13) 0.1194(8) 0.069(2) Uani 0.339(5) 1 d D . P A 2
O49B O 0.0472(16) -0.8057(14) 0.0869(8) 0.069(2) Uani 0.339(5) 1 d D . P A 2
O3WB O 0.1545(10) -0.7302(8) 0.4218(5) 0.033(2) Uani 0.339(5) 1 d . . P A 2
O3WA O 0.0923(18) -0.8678(12) 0.0407(9) 0.074(4) Uani 0.331(2) 1 d . . P A 1
O43A O 0.4778(12) 0.374(2) 0.5665(6) 0.044(4) Uani 0.41(4) 1 d . . P B 1
O42A O 0.414(3) 0.386(3) 0.6698(10) 0.073(7) Uani 0.41(4) 1 d . . P B 1
O45 O -0.1019(4) -0.8594(3) -0.2889(2) 0.0478(9) Uani 1 1 d . . . . .
N44 N -0.0837(5) -0.8552(4) -0.2224(3) 0.0514(11) Uani 1 1 d . . . . .
O47B O 0.0062(12) -0.8887(19) -0.1764(15) 0.069(5) Uani 0.50(4) 1 d . . P C 2
O47A O -0.0252(18) -0.9407(18) -0.2167(14) 0.058(5) Uani 0.50(4) 1 d . . P C 1
O3WC O 0.054(2) -0.874(2) 0.1709(16) 0.130(9) Uani 0.331(2) 1 d . . P A 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nd1 O28 2.401(3) 1_545 ?
Nd1 O29 2.459(3) 2_655 ?
Nd1 O38 2.386(3) 1_444 ?
Nd1 O39 2.451(3) 2_656 ?
Nd1 O1W 2.531(3) . ?
Nd1 O2W 2.474(3) . ?
Nd1 O19 2.463(3) 2_645 ?
Nd1 O18 2.403(3) . ?
O28 C27 1.258(5) . ?
O29 C27 1.247(5) . ?
N31 C32 1.344(5) . ?
N31 C30 1.510(5) . ?
N31 C36 1.359(5) . ?
O41 N40 1.253(6) . ?
N11 C16 1.351(6) . ?
N11 C10 1.497(5) . ?
N11 C12 1.343(5) . ?
N21 C20 1.524(5) . ?
N21 C22 1.344(5) . ?
N21 C26 1.329(6) . ?
C3 C4 1.406(5) . ?
C3 C20 1.509(6) . ?
C3 C2 1.396(6) . ?
C6 C5 1.413(6) . ?
C6 C1 1.407(6) . ?
C6 C7 1.506(6) . ?
C32 H32 0.9500 . ?
C32 C33 1.371(5) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C5 1.519(5) . ?
C5 C4 1.393(6) . ?
C1 C2 1.411(6) . ?
C1 C10 1.511(6) . ?
C33 H33 0.9500 . ?
C33 C34 1.389(5) . ?
C4 C9 1.520(6) . ?
C35 H35 0.9500 . ?
C35 C36 1.376(5) . ?
C35 C34 1.389(5) . ?
C14 C13 1.377(6) . ?
C14 C15 1.382(6) . ?
C14 C17 1.504(5) . ?
N40 O42B 1.162(16) . ?
N40 O43B 1.203(9) . ?
N40 O43A 1.297(13) . ?
N40 O42A 1.291(19) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C2 C8 1.516(5) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C24 C23 1.387(6) . ?
C24 C27 1.521(6) . ?
C24 C25 1.390(6) . ?
C36 H36 0.9500 . ?
C16 H16 0.9500 . ?
C16 C15 1.371(6) . ?
C23 H23 0.9500 . ?
C23 C22 1.381(6) . ?
C13 H13 0.9500 . ?
C13 C12 1.382(6) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C12 H12 0.9500 . ?
C15 H15 0.9500 . ?
C22 H22 0.9500 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C25 H25 0.9500 . ?
C25 C26 1.371(6) . ?
C26 H26 0.9500 . ?
O38 C37 1.236(5) . ?
O39 C37 1.253(5) . ?
C34 C37 1.520(5) . ?
O1W H1WA 1.0176 . ?
O1W H1WB 1.0196 . ?
O2W H2WA 0.8807 . ?
O2W H2WB 0.8805 . ?
O46 N44 1.248(7) . ?
O19 C17 1.245(5) . ?
O18 C17 1.262(5) . ?
N48A O49A 1.086(9) . ?
N48A O50A 1.217(9) . ?
N48A O51A 1.222(9) . ?
N48B O51B 1.222(14) . ?
N48B O50B 1.228(14) . ?
N48B O49B 1.212(14) . ?
O45 N44 1.225(6) . ?
N44 O47B 1.319(13) . ?
N44 O47A 1.298(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O28 Nd1 O29 121.96(10) 1_545 2_655 ?
O28 Nd1 O39 79.08(10) 1_545 2_656 ?
O28 Nd1 O1W 72.95(11) 1_545 . ?
O28 Nd1 O2W 140.21(11) 1_545 . ?
O28 Nd1 O19 78.77(10) 1_545 2_645 ?
O28 Nd1 O18 71.95(10) 1_545 . ?
O29 Nd1 O1W 136.69(11) 2_655 . ?
O29 Nd1 O2W 71.96(12) 2_655 . ?
O29 Nd1 O19 73.95(11) 2_655 2_645 ?
O38 Nd1 O28 142.17(11) 1_444 1_545 ?
O38 Nd1 O29 80.18(10) 1_444 2_655 ?
O38 Nd1 O39 100.28(9) 1_444 2_656 ?
O38 Nd1 O1W 70.69(11) 1_444 . ?
O38 Nd1 O2W 72.51(11) 1_444 . ?
O38 Nd1 O19 79.25(9) 1_444 2_645 ?
O38 Nd1 O18 145.85(11) 1_444 . ?
O39 Nd1 O29 144.40(12) 2_656 2_655 ?
O39 Nd1 O1W 73.84(11) 2_656 . ?
O39 Nd1 O2W 74.31(12) 2_656 . ?
O39 Nd1 O19 141.48(11) 2_656 2_645 ?
O2W Nd1 O1W 125.08(12) . . ?
O19 Nd1 O1W 69.72(11) 2_645 . ?
O19 Nd1 O2W 138.63(11) 2_645 . ?
O18 Nd1 O29 78.62(10) . 2_655 ?
O18 Nd1 O39 82.38(10) . 2_656 ?
O18 Nd1 O1W 140.56(11) . . ?
O18 Nd1 O2W 75.60(10) . . ?
O18 Nd1 O19 119.42(9) . 2_645 ?
C27 O28 Nd1 134.7(3) . 1_565 ?
C27 O29 Nd1 136.2(3) . 2_655 ?
C32 N31 C30 121.9(3) . . ?
C32 N31 C36 120.9(3) . . ?
C36 N31 C30 117.1(3) . . ?
C16 N11 C10 120.2(4) . . ?
C12 N11 C16 121.0(4) . . ?
C12 N11 C10 118.7(4) . . ?
C22 N21 C20 119.4(3) . . ?
C26 N21 C20 118.0(3) . . ?
C26 N21 C22 122.2(4) . . ?
C4 C3 C20 119.0(4) . . ?
C2 C3 C4 121.2(4) . . ?
C2 C3 C20 119.7(3) . . ?
C5 C6 C7 119.2(4) . . ?
C1 C6 C5 118.5(4) . . ?
C1 C6 C7 122.3(4) . . ?
N31 C32 H32 119.8 . . ?
N31 C32 C33 120.5(4) . . ?
C33 C32 H32 119.8 . . ?
N31 C30 H30A 109.1 . . ?
N31 C30 H30B 109.1 . . ?
N31 C30 C5 112.7(3) . . ?
H30A C30 H30B 107.8 . . ?
C5 C30 H30A 109.1 . . ?
C5 C30 H30B 109.1 . . ?
C6 C5 C30 118.9(4) . . ?
C4 C5 C6 121.9(4) . . ?
C4 C5 C30 119.2(4) . . ?
C6 C1 C2 120.3(4) . . ?
C6 C1 C10 121.2(4) . . ?
C2 C1 C10 118.5(4) . . ?
C32 C33 H33 120.0 . . ?
C32 C33 C34 120.0(4) . . ?
C34 C33 H33 120.0 . . ?
C3 C4 C9 119.3(4) . . ?
C5 C4 C3 118.5(4) . . ?
C5 C4 C9 122.2(4) . . ?
C36 C35 H35 120.1 . . ?
C36 C35 C34 119.7(3) . . ?
C34 C35 H35 120.1 . . ?
C13 C14 C15 118.9(4) . . ?
C13 C14 C17 120.5(4) . . ?
C15 C14 C17 120.6(4) . . ?
O41 N40 O43A 130.7(7) . . ?
O41 N40 O42A 119.5(11) . . ?
O42B N40 O41 117.5(9) . . ?
O42B N40 O43B 129.5(14) . . ?
O43B N40 O41 113.0(10) . . ?
O42A N40 O43A 109.6(12) . . ?
N21 C20 H20A 109.1 . . ?
N21 C20 H20B 109.1 . . ?
C3 C20 N21 112.5(3) . . ?
C3 C20 H20A 109.1 . . ?
C3 C20 H20B 109.1 . . ?
H20A C20 H20B 107.8 . . ?
C3 C2 C1 119.6(3) . . ?
C3 C2 C8 120.0(4) . . ?
C1 C2 C8 120.4(4) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C2 C8 H8A 109.5 . . ?
C2 C8 H8B 109.5 . . ?
C2 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C23 C24 C27 121.1(4) . . ?
C23 C24 C25 119.1(4) . . ?
C25 C24 C27 119.7(4) . . ?
N31 C36 C35 120.1(3) . . ?
N31 C36 H36 119.9 . . ?
C35 C36 H36 119.9 . . ?
N11 C16 H16 119.9 . . ?
N11 C16 C15 120.3(4) . . ?
C15 C16 H16 119.9 . . ?
C24 C23 H23 120.5 . . ?
C22 C23 C24 119.1(4) . . ?
C22 C23 H23 120.5 . . ?
C14 C13 H13 120.0 . . ?
C14 C13 C12 119.9(4) . . ?
C12 C13 H13 120.0 . . ?
N11 C10 C1 113.2(3) . . ?
N11 C10 H10A 108.9 . . ?
N11 C10 H10B 108.9 . . ?
C1 C10 H10A 108.9 . . ?
C1 C10 H10B 108.9 . . ?
H10A C10 H10B 107.8 . . ?
N11 C12 C13 119.9(4) . . ?
N11 C12 H12 120.0 . . ?
C13 C12 H12 120.0 . . ?
C14 C15 H15 120.1 . . ?
C16 C15 C14 119.7(4) . . ?
C16 C15 H15 120.1 . . ?
O28 C27 C24 115.4(4) . . ?
O29 C27 O28 127.6(4) . . ?
O29 C27 C24 116.9(4) . . ?
N21 C22 C23 119.8(4) . . ?
N21 C22 H22 120.1 . . ?
C23 C22 H22 120.1 . . ?
C4 C9 H9A 109.5 . . ?
C4 C9 H9B 109.5 . . ?
C4 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C24 C25 H25 120.3 . . ?
C26 C25 C24 119.5(4) . . ?
C26 C25 H25 120.3 . . ?
N21 C26 C25 120.2(4) . . ?
N21 C26 H26 119.9 . . ?
C25 C26 H26 119.9 . . ?
C37 O38 Nd1 177.4(3) . 1_666 ?
C37 O39 Nd1 131.1(3) . 2_656 ?
C33 C34 C37 120.7(3) . . ?
C35 C34 C33 118.7(3) . . ?
C35 C34 C37 120.6(3) . . ?
O38 C37 O39 125.7(3) . . ?
O38 C37 C34 117.2(3) . . ?
O39 C37 C34 117.1(3) . . ?
Nd1 O1W H1WA 115.4 . . ?
Nd1 O1W H1WB 116.3 . . ?
H1WA O1W H1WB 97.9 . . ?
Nd1 O2W H2WA 110.1 . . ?
Nd1 O2W H2WB 110.0 . . ?
H2WA O2W H2WB 104.0 . . ?
C17 O19 Nd1 113.2(2) . 2_645 ?
C17 O18 Nd1 177.2(3) . . ?
O19 C17 C14 117.6(3) . . ?
O19 C17 O18 124.6(4) . . ?
O18 C17 C14 117.8(4) . . ?
O49A N48A O50A 131.8(9) . . ?
O49A N48A O51A 110.4(8) . . ?
O50A N48A O51A 117.3(8) . . ?
O51B N48B O50B 109.3(14) . . ?
O49B N48B O51B 125.3(15) . . ?
O49B N48B O50B 123.2(15) . . ?
O46 N44 O47B 101.5(12) . . ?
O46 N44 O47A 131.1(10) . . ?
O45 N44 O46 121.6(5) . . ?
O45 N44 O47B 135.5(11) . . ?
O45 N44 O47A 106.4(11) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1W H1WA O49B 1.02 1.98 2.754(14) 130.4 . yes
O1W H1WA O3WA 1.02 1.70 2.651(13) 154.7 . yes
O2W H2WB O1W 0.88 2.12 2.901(5) 147.5 2_545 yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Nd1 O28 C27 O29 -61.1(6) 1_565 . . . ?
Nd1 O28 C27 C24 116.9(4) 1_565 . . . ?
Nd1 O29 C27 O28 19.2(8) 2_655 . . . ?
Nd1 O29 C27 C24 -158.8(3) 2_655 . . . ?
Nd1 O39 C37 O38 -12.5(7) 2_656 . . . ?
Nd1 O39 C37 C34 167.3(3) 2_656 . . . ?
Nd1 O19 C17 C14 173.8(3) 2_645 . . . ?
Nd1 O19 C17 O18 -4.4(5) 2_645 . . . ?
N31 C32 C33 C34 -1.5(7) . . . . ?
N31 C30 C5 C6 -90.6(5) . . . . ?
N31 C30 C5 C4 91.0(5) . . . . ?
N11 C16 C15 C14 1.5(8) . . . . ?
C6 C5 C4 C3 -0.9(5) . . . . ?
C6 C5 C4 C9 176.2(4) . . . . ?
C6 C1 C2 C3 -1.5(5) . . . . ?
C6 C1 C2 C8 179.1(4) . . . . ?
C6 C1 C10 N11 -103.6(4) . . . . ?
C32 N31 C30 C5 -23.8(6) . . . . ?
C32 N31 C36 C35 1.8(6) . . . . ?
C32 C33 C34 C35 2.7(6) . . . . ?
C32 C33 C34 C37 -174.5(4) . . . . ?
C30 N31 C32 C33 -177.6(4) . . . . ?
C30 N31 C36 C35 178.8(4) . . . . ?
C30 C5 C4 C3 177.5(3) . . . . ?
C30 C5 C4 C9 -5.4(5) . . . . ?
C5 C6 C1 C2 0.7(5) . . . . ?
C5 C6 C1 C10 -177.7(3) . . . . ?
C1 C6 C5 C30 -177.9(3) . . . . ?
C1 C6 C5 C4 0.5(5) . . . . ?
C33 C34 C37 O38 176.0(4) . . . . ?
C33 C34 C37 O39 -3.8(6) . . . . ?
C4 C3 C20 N21 103.8(4) . . . . ?
C4 C3 C2 C1 1.2(5) . . . . ?
C4 C3 C2 C8 -179.4(3) . . . . ?
C35 C34 C37 O38 -1.1(6) . . . . ?
C35 C34 C37 O39 179.1(4) . . . . ?
C14 C13 C12 N11 0.3(7) . . . . ?
C20 N21 C22 C23 -170.8(4) . . . . ?
C20 N21 C26 C25 171.8(4) . . . . ?
C20 C3 C4 C5 176.9(3) . . . . ?
C20 C3 C4 C9 -0.2(5) . . . . ?
C20 C3 C2 C1 -175.7(3) . . . . ?
C20 C3 C2 C8 3.7(5) . . . . ?
C2 C3 C4 C5 0.0(5) . . . . ?
C2 C3 C4 C9 -177.1(3) . . . . ?
C2 C3 C20 N21 -79.3(4) . . . . ?
C2 C1 C10 N11 77.9(5) . . . . ?
C7 C6 C5 C30 2.1(5) . . . . ?
C7 C6 C5 C4 -179.5(4) . . . . ?
C7 C6 C1 C2 -179.3(4) . . . . ?
C7 C6 C1 C10 2.3(6) . . . . ?
C24 C23 C22 N21 -0.3(6) . . . . ?
C24 C25 C26 N21 -1.5(8) . . . . ?
C36 N31 C32 C33 -0.8(6) . . . . ?
C36 N31 C30 C5 159.3(4) . . . . ?
C36 C35 C34 C33 -1.7(6) . . . . ?
C36 C35 C34 C37 175.4(4) . . . . ?
C16 N11 C10 C1 -123.1(4) . . . . ?
C16 N11 C12 C13 -2.9(7) . . . . ?
C23 C24 C27 O28 169.3(4) . . . . ?
C23 C24 C27 O29 -12.5(6) . . . . ?
C23 C24 C25 C26 3.1(7) . . . . ?
C13 C14 C15 C16 -4.0(8) . . . . ?
C13 C14 C17 O19 2.3(6) . . . . ?
C13 C14 C17 O18 -179.4(4) . . . . ?
C10 N11 C16 C15 -176.0(4) . . . . ?
C10 N11 C12 C13 175.1(4) . . . . ?
C10 C1 C2 C3 176.9(3) . . . . ?
C10 C1 C2 C8 -2.5(5) . . . . ?
C12 N11 C16 C15 2.0(7) . . . . ?
C12 N11 C10 C1 58.9(5) . . . . ?
C15 C14 C13 C12 3.1(7) . . . . ?
C15 C14 C17 O19 -177.8(4) . . . . ?
C15 C14 C17 O18 0.4(7) . . . . ?
C27 C24 C23 C22 174.6(4) . . . . ?
C27 C24 C25 C26 -173.7(4) . . . . ?
C22 N21 C20 C3 -43.0(5) . . . . ?
C22 N21 C26 C25 -1.1(7) . . . . ?
C25 C24 C23 C22 -2.2(7) . . . . ?
C25 C24 C27 O28 -14.0(6) . . . . ?
C25 C24 C27 O29 164.2(4) . . . . ?
C26 N21 C20 C3 143.8(4) . . . . ?
C26 N21 C22 C23 2.0(6) . . . . ?
C34 C35 C36 N31 -0.5(6) . . . . ?
C17 C14 C13 C12 -177.1(4) . . . . ?
C17 C14 C15 C16 176.2(5) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.500 0.000 0.000 362.3 113.1 11xWater

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.310
_oxdiff_exptl_absorpt_empirical_full_min 0.818
