# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_1_rt_mo
_audit_block_doi                 10.5517/ccdc.csd.cc2000wy
_database_code_depnum_ccdc_archive 'CCDC 1847069'
_audit_update_record             
;
2018-06-04 deposited with the CCDC.
2018-08-06 downloaded from the CCDC.
;
_audit_creation_date             2018-03-13
_audit_creation_method           
;
Olex2 1.2-ac21
(compiled 2015.09.16 svn.r134, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         '0.25(C42 H30 N6 O30 Pr4), H2 O'
_chemical_formula_sum            'C10.50 H9.50 N1.50 O8.50 Pr'
_chemical_formula_weight         433.61
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C52 H52 N8 O37 Pr4'
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'
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'
Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, -z'

_cell_length_a                   8.8422(7)
_cell_length_b                   10.7274(8)
_cell_length_c                   18.8231(16)
_cell_angle_alpha                75.375(7)
_cell_angle_beta                 83.809(7)
_cell_angle_gamma                69.205(7)
_cell_volume                     1614.7(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5016
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.8270
_cell_measurement_theta_min      2.1140
_exptl_absorpt_coefficient_mu    3.055
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89928
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.784
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       triclinic
_exptl_crystal_F_000             840
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-10 -8 -17 0.0720
-8 2 -16 0.0508
4 15 8 0.0068
3 -4 22 0.0679
-3 11 -6 0.0228
-10 3 6 0.0798
-7 2 20 0.1073
8 -2 16 0.0508
8 -3 -16 0.0956
9 9 20 0.0345
5 -10 6 0.0440
0 12 19 0.0466
3 7 26 0.0476
-8 -14 -12 0.0723

_exptl_crystal_size_max          0.233
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_min          0.08
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
-10.0014 -8.0143 -16.9219 -0.4561 0.8480 0.2070
-7.9976 1.9972 -15.9381 0.2132 0.9106 0.3087
3.9957 14.9732 7.9696 0.9559 -0.1617 0.2100
2.9909 -3.9983 21.9213 -0.4199 -0.9176 0.1322
-3.0011 10.9809 -5.9764 0.7606 0.5296 0.3492
-10.0114 2.9873 5.9875 0.0979 0.3081 0.9204
-7.0166 1.9863 19.9366 -0.0607 -0.2962 0.9600
7.9976 -1.9972 15.9381 -0.2132 -0.9106 -0.3087
8.0088 -2.9762 -15.9450 -0.0307 0.1043 -0.9746
8.9998 9.0104 19.9108 0.4937 -0.8819 -0.0509
5.0100 -9.9689 5.9828 -0.6824 -0.6010 -0.4728
-0.0128 11.9728 18.9347 0.6494 -0.3931 0.6556
2.9866 6.9810 25.9078 0.2795 -0.8449 0.4632
-7.9967 -13.9759 -11.9525 -0.8804 0.4878 0.0248

_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_av_unetI/netI     0.0546
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9020
_diffrn_reflns_theta_full        28.26
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         2.09
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9987
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.871
_diffrn_measured_fraction_theta_max 0.871
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -52.00  66.00   1.00    6.50    --   26.84 -77.00 150.00  118
  2  ω    -52.00  66.00   1.00    6.50    --   26.84 -77.00 -90.00  118
  3  ω    -52.00  66.00   1.00    6.50    --   26.84 -77.00  30.00  118
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0054305000
_diffrn_orient_matrix_UB_12      0.0665255000
_diffrn_orient_matrix_UB_13      -0.0077628000
_diffrn_orient_matrix_UB_21      -0.0446776000
_diffrn_orient_matrix_UB_22      0.0183783000
_diffrn_orient_matrix_UB_23      -0.0324128000
_diffrn_orient_matrix_UB_31      -0.0730779000
_diffrn_orient_matrix_UB_32      0.0227965000
_diffrn_orient_matrix_UB_33      0.0201599000
_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'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                6074
_reflns_number_total             6968
_reflns_odcompleteness_completeness 98.66
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         5.348
_refine_diff_density_min         -1.194
_refine_diff_density_rms         0.332
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         6968
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0560
_refine_ls_restrained_S_all      1.071
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0901P)²+24.7250P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1712
_refine_ls_wR_factor_ref         0.1772
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O1(H1A,H1B), O1AA(H1AB,H1AC)
2.b Rotating group:
 O3(H3A,H3B), O28(H28A,H28B), O30(H30A,H30B)
2.c Aromatic/amide H refined with riding coordinates:
 C1AA(H1AA), C2AA(H2AA), C5(H5), C15(H15), C24(H24), C26(H26), C33(H33),
 C39(H39), C42(H42)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
Pr1 Pr 0.10397(5) 1.46786(4) 0.77640(2) 0.01229(14) Uani 1 d . . .
Pr2 Pr 0.49814(5) 0.58847(4) 0.71293(2) 0.01206(14) Uani 1 d . . .
O2 O 0.2794(8) 0.6036(7) 0.8102(3) 0.0241(14) Uani 1 d . . .
O3 O 0.2989(9) 0.8284(8) 0.6898(5) 0.0389(18) Uani 1 d . . .
H3A H 0.3364 0.8837 0.6563 0.058 Uiso 1 d . . GR
H3B H 0.2801 0.8583 0.7301 0.058 Uiso 1 d . . GR
O6 O 0.0972(8) 0.6028(8) 1.1492(4) 0.0313(16) Uani 1 d . . .
O8 O 0.6093(8) 0.7308(7) 0.7591(4) 0.0253(14) Uani 1 d . . .
O9 O 0.4353(8) 0.3714(6) 0.7443(4) 0.0273(15) Uani 1 d . . .
O0AA O 0.7362(7) 0.4596(7) 0.6594(4) 0.0263(14) Uani 1 d . . .
O13 O 0.0040(8) 0.5902(7) 0.3177(3) 0.0253(14) Uani 1 d . . .
O16 O 0.6507(8) 0.4415(7) 0.8194(3) 0.0264(14) Uani 1 d . . .
O17 O 0.0703(8) 0.5907(8) 0.8807(4) 0.0298(16) Uani 1 d . . .
O20 O 0.8766(8) 0.6734(6) 0.7428(4) 0.0251(14) Uani 1 d . . .
O21 O 0.2943(8) 1.2379(7) 0.7478(5) 0.0338(17) Uani 1 d . . .
O24 O 0.4037(8) 0.5725(9) 0.5879(4) 0.0351(18) Uani 1 d . . .
O25 O 0.2031(8) 1.6065(6) 0.6680(3) 0.0210(13) Uani 1 d . . .
O28 O 0.5823(10) 0.7484(8) 0.6042(4) 0.0388(18) Uani 1 d . . .
H28A H 0.5001 0.7988 0.5756 0.058 Uiso 1 d . . GR
H28B H 0.6591 0.7013 0.5780 0.058 Uiso 1 d . . GR
O30 O 0.2457(9) 1.3040(9) 0.8866(4) 0.043(2) Uani 1 d . . .
H30A H 0.1984 1.2885 0.9354 0.064 Uiso 1 d . . GR
H30B H 0.3576 1.2445 0.8882 0.064 Uiso 1 d . . GR
N32 N 0.4754(11) 0.7075(10) 0.9683(5) 0.034(2) Uani 1 d . . .
C0AA C 0.7270(10) 0.8992(8) 0.7529(5) 0.0177(16) Uani 1 d . . .
N3 N -0.1404(9) 0.7113(8) 0.5130(4) 0.0232(16) Uani 1 d . . .
C1AA C 0.8688(11) 0.9282(10) 0.7557(6) 0.029(2) Uani 1 d . . .
H1AA H 0.9675 0.8572 0.7566 0.035 Uiso 1 calc . . R
N8 N 0.8704(10) 1.0510(9) 0.7569(6) 0.036(2) Uani 1 d . . .
C2AA C 0.4227(11) 0.6750(10) 1.0370(5) 0.0249(19) Uani 1 d . . .
H2AA H 0.4776 0.6819 1.0744 0.030 Uiso 1 calc . . R
C5 C 0.3981(12) 0.6917(11) 0.9159(5) 0.028(2) Uani 1 d . . .
H5 H 0.4329 0.7143 0.8674 0.034 Uiso 1 calc . . R
C3AA C 0.5813(10) 1.1340(9) 0.7500(5) 0.0197(17) Uani 1 d . . .
C9 C 0.2578(10) 0.5996(9) 0.6038(4) 0.0184(17) Uani 1 d . . .
C14 C 0.4281(11) 1.2564(8) 0.7462(5) 0.0195(17) Uani 1 d . . .
C15 C 0.7291(11) 1.1516(9) 0.7545(6) 0.029(2) Uani 1 d . . .
H15 H 0.7281 1.2379 0.7560 0.034 Uiso 1 calc . . R
C18 C 0.2903(10) 0.6313(9) 1.0560(4) 0.0177(16) Uani 1 d . . .
C20 C 0.2711(11) 0.6444(9) 0.9292(5) 0.0191(17) Uani 1 d . . .
C22 C 0.7388(11) 0.7556(8) 0.7521(5) 0.0190(17) Uani 1 d . . .
C24 C 0.1868(10) 0.5983(9) 0.4774(4) 0.0181(16) Uani 1 d . . .
H24 H 0.2959 0.5621 0.4653 0.022 Uiso 1 calc . . R
C26 C -0.0256(10) 0.6846(9) 0.5603(4) 0.0185(16) Uani 1 d . . .
H26 H -0.0573 0.7047 0.6061 0.022 Uiso 1 calc . . R
C27 C 0.1381(10) 0.6288(8) 0.5456(4) 0.0171(16) Uani 1 d . . .
C30 C 0.2413(10) 0.5942(8) 1.1358(4) 0.0167(16) Uani 1 d . . .
C31 C 0.1152(10) 0.5821(8) 0.3559(4) 0.0170(16) Uani 1 d . . .
C33 C 0.5826(10) 1.0047(9) 0.7504(5) 0.0206(17) Uani 1 d . . .
H33 H 0.4859 0.9894 0.7490 0.025 Uiso 1 calc . . R
C36 C 0.0689(10) 0.6234(8) 0.4281(4) 0.0157(16) Uani 1 d . . .
C37 C 0.1991(11) 0.6125(9) 0.8702(5) 0.0211(18) Uani 1 d . . .
C39 C -0.0915(10) 0.6811(9) 0.4478(5) 0.0196(17) Uani 1 d . . .
H39 H -0.1700 0.7000 0.4137 0.024 Uiso 1 calc . . R
C42 C 0.2105(10) 0.6165(9) 1.0013(5) 0.0183(16) Uani 1 d . . .
H42 H 0.1203 0.5891 1.0118 0.022 Uiso 1 calc . . R
O1 O 0.1887(12) 1.0162(14) 0.7705(11) 0.105(6) Uani 1 d . . .
H1A H 0.0964 1.0103 0.7848 0.158 Uiso 1 d . . G
H1B H 0.1810 1.0701 0.7283 0.158 Uiso 1 d . . G
O1AA O 0.5010(19) 0.7188(12) 0.4413(7) 0.079(3) Uani 1 d . . .
H1AB H 0.5238 0.6938 0.4865 0.119 Uiso 1 d . . G
H1AC H 0.5122 0.6489 0.4250 0.119 Uiso 1 d . . G


_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
Pr1 Pr2 4.0954(7) 1_565 ?
Pr1 O2 2.686(7) 1_565 ?
Pr1 O6 2.363(6) 2_577 ?
Pr1 O9 2.793(7) 1_565 ?
Pr1 O13 2.404(6) 2_576 ?
Pr1 O17 2.565(6) 1_565 ?
Pr1 O20 2.393(6) 1_465 ?
Pr1 O21 2.595(7) . ?
Pr1 O25 2.479(6) . ?
Pr1 O30 2.474(7) . ?
Pr1 C14 3.060(8) . ?
Pr1 C37 2.977(9) 1_565 ?
Pr2 Pr1 4.0954(7) 1_545 ?
Pr2 O2 2.507(6) . ?
Pr2 O3 2.509(7) . ?
Pr2 O8 2.445(6) . ?
Pr2 O9 2.497(6) . ?
Pr2 O0AA 2.353(6) . ?
Pr2 O16 2.408(6) . ?
Pr2 O24 2.646(7) . ?
Pr2 O25 2.756(6) 1_545 ?
Pr2 O28 2.548(7) . ?
Pr2 C9 3.065(8) . ?
O2 Pr1 2.686(7) 1_545 ?
O2 C37 1.273(10) . ?
O6 Pr1 2.363(6) 2_577 ?
O6 C30 1.246(11) . ?
O8 C22 1.251(11) . ?
O9 Pr1 2.793(7) 1_545 ?
O9 C14 1.249(10) 1_545 ?
O0AA C31 1.255(10) 2_666 ?
O13 Pr1 2.404(6) 2_576 ?
O13 C31 1.245(10) . ?
O16 C30 1.234(10) 2_667 ?
O17 Pr1 2.565(6) 1_545 ?
O17 C37 1.228(11) . ?
O20 Pr1 2.393(6) 1_645 ?
O20 C22 1.249(11) . ?
O21 C14 1.263(11) . ?
O24 C9 1.238(11) . ?
O25 Pr2 2.756(6) 1_565 ?
O25 C9 1.264(10) 1_565 ?
N32 C2AA 1.329(12) . ?
N32 C5 1.335(12) . ?
C0AA C1AA 1.403(12) . ?
C0AA C22 1.511(11) . ?
C0AA C33 1.369(12) . ?
N3 C26 1.329(11) . ?
N3 C39 1.335(11) . ?
C1AA N8 1.329(12) . ?
N8 C15 1.326(12) . ?
C2AA C18 1.390(12) . ?
C5 C20 1.364(13) . ?
C3AA C14 1.508(11) . ?
C3AA C15 1.400(12) . ?
C3AA C33 1.381(12) . ?
C9 O25 1.264(10) 1_545 ?
C9 C27 1.502(11) . ?
C14 O9 1.250(10) 1_565 ?
C18 C30 1.510(11) . ?
C18 C42 1.379(12) . ?
C20 C37 1.503(12) . ?
C20 C42 1.404(12) . ?
C24 C27 1.390(11) . ?
C24 C36 1.380(11) . ?
C26 C27 1.383(12) . ?
C30 O16 1.234(10) 2_667 ?
C31 O0AA 1.255(10) 2_666 ?
C31 C36 1.506(11) . ?
C36 C39 1.383(12) . ?
C37 Pr1 2.977(9) 1_545 ?

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
O2 Pr1 Pr2 36.43(13) 1_565 1_565 ?
O2 Pr1 O9 63.83(19) 1_565 1_565 ?
O2 Pr1 C14 86.2(2) 1_565 . ?
O2 Pr1 C37 25.3(2) 1_565 1_565 ?
O6 Pr1 Pr2 161.30(17) 2_577 1_565 ?
O6 Pr1 O2 126.8(2) 2_577 1_565 ?
O6 Pr1 O9 140.6(2) 2_577 1_565 ?
O6 Pr1 O13 83.4(2) 2_577 2_576 ?
O6 Pr1 O17 78.6(2) 2_577 1_565 ?
O6 Pr1 O20 81.0(2) 2_577 1_465 ?
O6 Pr1 O21 101.2(3) 2_577 . ?
O6 Pr1 O25 154.3(2) 2_577 . ?
O6 Pr1 O30 74.6(3) 2_577 . ?
O6 Pr1 C14 120.4(3) 2_577 . ?
O6 Pr1 C37 101.5(3) 2_577 1_565 ?
O9 Pr1 Pr2 36.71(13) 1_565 1_565 ?
O9 Pr1 C14 24.1(2) 1_565 . ?
O9 Pr1 C37 83.8(2) 1_565 1_565 ?
O13 Pr1 Pr2 115.00(16) 2_576 1_565 ?
O13 Pr1 O2 147.8(2) 2_576 1_565 ?
O13 Pr1 O9 101.3(2) 2_576 1_565 ?
O13 Pr1 O17 151.8(2) 2_576 1_565 ?
O13 Pr1 O21 68.7(2) 2_576 . ?
O13 Pr1 O25 81.8(2) 2_576 . ?
O13 Pr1 O30 125.4(3) 2_576 . ?
O13 Pr1 C14 86.6(2) 2_576 . ?
O13 Pr1 C37 165.3(2) 2_576 1_565 ?
O17 Pr1 Pr2 85.45(15) 1_565 1_565 ?
O17 Pr1 O2 49.02(19) 1_565 1_565 ?
O17 Pr1 O9 106.3(2) 1_565 1_565 ?
O17 Pr1 O21 136.0(2) 1_565 . ?
O17 Pr1 C14 121.2(2) 1_565 . ?
O17 Pr1 C37 24.2(2) 1_565 1_565 ?
O20 Pr1 Pr2 104.44(17) 1_465 1_565 ?
O20 Pr1 O2 92.3(2) 1_465 1_565 ?
O20 Pr1 O9 138.4(2) 1_465 1_565 ?
O20 Pr1 O13 80.7(2) 1_465 2_576 ?
O20 Pr1 O17 75.2(2) 1_465 1_565 ?
O20 Pr1 O21 148.7(2) 1_465 . ?
O20 Pr1 O25 75.9(2) 1_465 . ?
O20 Pr1 O30 140.6(3) 1_465 . ?
O20 Pr1 C14 153.7(2) 1_465 . ?
O20 Pr1 C37 86.3(2) 1_465 1_565 ?
O21 Pr1 Pr2 83.58(16) . 1_565 ?
O21 Pr1 O2 110.0(2) . 1_565 ?
O21 Pr1 O9 47.9(2) . 1_565 ?
O21 Pr1 C14 24.0(2) . . ?
O21 Pr1 C37 123.0(2) . 1_565 ?
O25 Pr1 Pr2 41.00(14) . 1_565 ?
O25 Pr1 O2 66.03(19) . 1_565 ?
O25 Pr1 O9 63.5(2) . 1_565 ?
O25 Pr1 O17 105.9(2) . 1_565 ?
O25 Pr1 O21 92.9(2) . . ?
O25 Pr1 C14 79.6(2) . . ?
O25 Pr1 C37 88.3(2) . 1_565 ?
O30 Pr1 Pr2 90.9(2) . 1_565 ?
O30 Pr1 O2 78.8(3) . 1_565 ?
O30 Pr1 O9 71.0(2) . 1_565 ?
O30 Pr1 O17 70.0(3) . 1_565 ?
O30 Pr1 O21 67.7(3) . . ?
O30 Pr1 O25 131.1(2) . . ?
O30 Pr1 C14 64.7(3) . . ?
O30 Pr1 C37 69.3(3) . 1_565 ?
C14 Pr1 Pr2 60.58(17) . 1_565 ?
C37 Pr1 Pr2 61.59(18) 1_565 1_565 ?
C37 Pr1 C14 102.4(2) 1_565 . ?
O2 Pr2 Pr1 39.51(15) . 1_545 ?
O2 Pr2 O3 70.7(2) . . ?
O2 Pr2 O24 112.2(2) . . ?
O2 Pr2 O25 64.59(19) . 1_545 ?
O2 Pr2 O28 138.2(2) . . ?
O2 Pr2 C9 88.9(2) . . ?
O3 Pr2 Pr1 85.70(19) . 1_545 ?
O3 Pr2 O24 86.8(3) . . ?
O3 Pr2 O25 67.3(2) . 1_545 ?
O3 Pr2 O28 67.6(3) . . ?
O3 Pr2 C9 74.4(2) . . ?
O8 Pr2 Pr1 132.23(16) . 1_545 ?
O8 Pr2 O2 92.8(2) . . ?
O8 Pr2 O3 71.5(2) . . ?
O8 Pr2 O9 144.6(2) . . ?
O8 Pr2 O24 139.5(2) . . ?
O8 Pr2 O25 137.5(2) . 1_545 ?
O8 Pr2 O28 71.1(3) . . ?
O8 Pr2 C9 143.1(2) . . ?
O9 Pr2 Pr1 41.97(15) . 1_545 ?
O9 Pr2 O2 70.8(2) . . ?
O9 Pr2 O3 127.0(2) . . ?
O9 Pr2 O24 75.6(2) . . ?
O9 Pr2 O25 63.9(2) . 1_545 ?
O9 Pr2 O28 141.0(3) . . ?
O9 Pr2 C9 69.8(2) . . ?
O0AA Pr2 Pr1 124.42(18) . 1_545 ?
O0AA Pr2 O2 150.3(2) . . ?
O0AA Pr2 O3 138.9(3) . . ?
O0AA Pr2 O8 98.6(2) . . ?
O0AA Pr2 O9 84.5(2) . . ?
O0AA Pr2 O16 78.1(2) . . ?
O0AA Pr2 O24 75.6(2) . . ?
O0AA Pr2 O25 119.0(2) . 1_545 ?
O0AA Pr2 O28 71.5(2) . . ?
O0AA Pr2 C9 97.9(2) . . ?
O16 Pr2 Pr1 93.76(16) . 1_545 ?
O16 Pr2 O2 78.9(2) . . ?
O16 Pr2 O3 132.2(3) . . ?
O16 Pr2 O8 74.1(2) . . ?
O16 Pr2 O9 72.0(2) . . ?
O16 Pr2 O24 139.7(3) . . ?
O16 Pr2 O25 129.5(2) . 1_545 ?
O16 Pr2 O28 128.9(3) . . ?
O16 Pr2 C9 141.9(2) . . ?
O24 Pr2 Pr1 77.14(16) . 1_545 ?
O24 Pr2 O25 47.79(19) . 1_545 ?
O24 Pr2 C9 23.6(2) . . ?
O25 Pr2 Pr1 36.18(12) 1_545 1_545 ?
O25 Pr2 C9 24.3(2) 1_545 . ?
O28 Pr2 Pr1 137.3(2) . 1_545 ?
O28 Pr2 O24 69.0(3) . . ?
O28 Pr2 O25 101.3(2) . 1_545 ?
O28 Pr2 C9 83.3(3) . . ?
C9 Pr2 Pr1 57.02(16) . 1_545 ?
Pr2 O2 Pr1 104.1(2) . 1_545 ?
C37 O2 Pr1 90.2(5) . 1_545 ?
C37 O2 Pr2 163.7(6) . . ?
C30 O6 Pr1 151.1(6) . 2_577 ?
C22 O8 Pr2 136.8(6) . . ?
Pr2 O9 Pr1 101.3(2) . 1_545 ?
C14 O9 Pr1 90.0(5) 1_545 1_545 ?
C14 O9 Pr2 165.1(6) 1_545 . ?
C31 O0AA Pr2 156.2(6) 2_666 . ?
C31 O13 Pr1 153.6(6) . 2_576 ?
C30 O16 Pr2 153.8(6) 2_667 . ?
C37 O17 Pr1 97.1(5) . 1_545 ?
C22 O20 Pr1 154.6(6) . 1_645 ?
C14 O21 Pr1 99.1(5) . . ?
C9 O24 Pr2 97.6(5) . . ?
Pr1 O25 Pr2 102.8(2) . 1_565 ?
C9 O25 Pr1 139.4(6) 1_565 . ?
C9 O25 Pr2 91.7(5) 1_565 1_565 ?
C2AA N32 C5 116.8(8) . . ?
C1AA C0AA C22 119.5(8) . . ?
C33 C0AA C1AA 117.7(8) . . ?
C33 C0AA C22 122.8(8) . . ?
C26 N3 C39 116.8(8) . . ?
N8 C1AA C0AA 123.8(8) . . ?
C15 N8 C1AA 117.5(8) . . ?
N32 C2AA C18 123.8(8) . . ?
N32 C5 C20 123.8(9) . . ?
C15 C3AA C14 118.5(8) . . ?
C33 C3AA C14 123.1(8) . . ?
C33 C3AA C15 118.4(8) . . ?
O24 C9 Pr2 58.8(5) . . ?
O24 C9 O25 122.2(8) . 1_545 ?
O24 C9 C27 120.3(8) . . ?
O25 C9 Pr2 64.0(5) 1_545 . ?
O25 C9 C27 117.5(8) 1_545 . ?
C27 C9 Pr2 170.7(6) . . ?
O9 C14 Pr1 65.9(5) 1_565 . ?
O9 C14 O21 121.6(8) 1_565 . ?
O9 C14 C3AA 120.0(8) 1_565 . ?
O21 C14 Pr1 56.8(4) . . ?
O21 C14 C3AA 118.3(8) . . ?
C3AA C14 Pr1 166.1(6) . . ?
N8 C15 C3AA 123.1(8) . . ?
C2AA C18 C30 120.0(7) . . ?
C42 C18 C2AA 118.8(8) . . ?
C42 C18 C30 121.1(8) . . ?
C5 C20 C37 122.4(8) . . ?
C5 C20 C42 119.4(8) . . ?
C42 C20 C37 118.1(8) . . ?
O8 C22 C0AA 117.0(8) . . ?
O20 C22 O8 126.0(8) . . ?
O20 C22 C0AA 117.0(8) . . ?
C36 C24 C27 118.2(8) . . ?
N3 C26 C27 123.9(8) . . ?
C24 C27 C9 121.8(8) . . ?
C26 C27 C9 119.6(7) . . ?
C26 C27 C24 118.5(8) . . ?
O6 C30 C18 116.9(7) . . ?
O16 C30 O6 127.2(8) 2_667 . ?
O16 C30 C18 115.9(8) 2_667 . ?
O0AA C31 C36 116.3(7) 2_666 . ?
O13 C31 O0AA 126.2(8) . 2_666 ?
O13 C31 C36 117.5(7) . . ?
C0AA C33 C3AA 119.6(8) . . ?
C24 C36 C31 120.1(7) . . ?
C24 C36 C39 118.7(8) . . ?
C39 C36 C31 121.1(7) . . ?
O2 C37 Pr1 64.5(5) . 1_545 ?
O2 C37 C20 117.6(8) . . ?
O17 C37 Pr1 58.8(5) . 1_545 ?
O17 C37 O2 121.4(8) . . ?
O17 C37 C20 120.9(8) . . ?
C20 C37 Pr1 163.6(6) . 1_545 ?
N3 C39 C36 123.8(8) . . ?
C18 C42 C20 117.2(8) . . ?

# start Validation Reply Form
_vrf_PLAT029_shelxl              
;
RESPONSE: This Alert is due to the low quality 
crystals are used for collecting single crystal X-ray data. 
;
_vrf_PLAT601_shelxl              
;
RESPONSE: This Alert is due to the presence of
residual electron density due to heavy metal atoms 
after refinement of structure. 
;
_vrf_PLAT094_shelxl              
;
RESPONSE: This Alert is due to the presence of
residual electron density due to heavy metal atoms 
after refinement of structure. 
;
# end Validation Reply Form


_olex2_date_sample_data_collection 2016-01-30
_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 1.212
_oxdiff_exptl_absorpt_empirical_full_min 0.782
####################################################################### 
# 
# 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_m5_rt_mo
_audit_block_doi                 10.5517/ccdc.csd.cc200114
_database_code_depnum_ccdc_archive 'CCDC 1847074'
_audit_update_record             
;
2018-06-04 deposited with the CCDC.
2018-08-06 downloaded from the CCDC.
;
_audit_creation_date             2018-03-16
_audit_creation_method           
;
Olex2 1.2-ac21
(compiled 2015.09.16 svn.r134, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C21 H15 N3 O15 Sm2, H2 O'
_chemical_formula_sum            'C21 H17 N3 O16 Sm2'
_chemical_formula_weight         868.08
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C336 H304 N80 O224 Sm32'
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'
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'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   14.5749(9)
_cell_length_b                   11.2005(6)
_cell_length_c                   14.8295(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.069(5)
_cell_angle_gamma                90.00
_cell_volume                     2414.8(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4658
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.0020
_cell_measurement_theta_min      1.8800
_exptl_absorpt_coefficient_mu    4.908
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52792
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    2.388
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       monoclinic
_exptl_crystal_F_000             1664
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-4 3 -20 0.0852
-3 -10 -15 0.0538
8 9 14 0.0945
12 -11 -8 0.0640
15 -4 12 0.1065
-1 -13 11 0.0429
-6 -14 8 0.0492
4 1 20 0.0856
-10 0 -18 0.0804
5 7 -18 0.0860
7 -14 7 0.0446
5 -14 -7 0.0346
17 0 -13 0.0977
-18 1 11 0.0914
-13 -9 12 0.0720
-19 -6 2 0.0937
-1 -15 -4 0.0377
0 16 0 0.0383
-7 -15 1 0.0399
4 -4 -20 0.0643

_exptl_crystal_size_max          0.237
_exptl_crystal_size_mid          0.166
_exptl_crystal_size_min          0.08
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
-3.9914 2.9998 -19.9959 0.0168 0.0180 -1.0105
-2.9924 -10.0000 -14.9984 0.7560 0.1629 -0.5961
7.9893 9.0003 13.9983 -0.7481 0.0877 0.6299
11.9951 -10.9990 -8.0003 0.5830 0.7724 -0.0621
14.9862 -3.9990 11.9968 -0.0286 0.5871 0.8030
-1.0014 -12.9999 10.9965 0.7182 -0.0166 0.6631
-5.9969 -14.0003 7.9971 0.8618 -0.1956 0.4721
3.9910 1.0002 19.9964 -0.2595 -0.0668 0.9577
-9.9875 -0.0006 -17.9964 0.2562 -0.2409 -0.9589
5.0013 7.0003 -17.9961 -0.3496 0.3536 -0.8518
6.9943 -13.9993 6.9968 0.7124 0.4054 0.5992
5.0000 -13.9994 -7.0006 0.8420 0.4799 -0.0698
16.9921 0.0013 -12.9983 -0.1073 0.9239 -0.3703
-17.9909 0.9987 10.9988 0.0737 -0.9578 0.2520
-12.9937 -9.0008 11.9972 0.6127 -0.6211 0.4965
-18.9867 -6.0012 1.9996 0.5784 -0.8116 -0.0818
-0.9966 -14.9998 -4.0011 0.9525 0.1847 0.0013
-0.0016 15.9998 0.0019 -0.9710 -0.1951 -0.2113
-6.9940 -15.0003 0.9983 0.9872 -0.1462 0.1508
4.0037 -3.9996 -19.9970 0.3450 0.4660 -0.8116

_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0485
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            7913
_diffrn_reflns_theta_full        28.35
_diffrn_reflns_theta_max         28.35
_diffrn_reflns_theta_min         1.89
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9974
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.871
_diffrn_measured_fraction_theta_max 0.871
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     55.00 111.00   1.00    7.50    --   26.84 178.00 -30.00   56
  2  ω     57.00 115.00   1.00    7.50    --   26.84 178.00-180.00   58
  3  ω    -31.00  73.00   1.00    7.50    --   26.84   0.00 150.00  104
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0120727000
_diffrn_orient_matrix_UB_12      -0.0606874000
_diffrn_orient_matrix_UB_13      -0.0075331000
_diffrn_orient_matrix_UB_21      0.0453580000
_diffrn_orient_matrix_UB_22      -0.0121861000
_diffrn_orient_matrix_UB_23      -0.0117842000
_diffrn_orient_matrix_UB_31      0.0133173000
_diffrn_orient_matrix_UB_32      -0.0132113000
_diffrn_orient_matrix_UB_33      0.0458947000
_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'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                4513
_reflns_number_total             5257
_reflns_odcompleteness_completeness 98.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         1.454
_refine_diff_density_min         -2.695
_refine_diff_density_rms         0.204
_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     385
_refine_ls_number_reflns         5257
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0389
_refine_ls_restrained_S_all      1.047
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0589P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0972
_refine_ls_wR_factor_ref         0.1067
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O32(H32A,H32B)
2.b Rotating group:
 O25(H25A,H25B), O40(H40A,H40B), O48(H48A,H48B)
2.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C0AA(H0AA), C15(H15), C20(H20), C25(H25), C48(H48), C57(H57),
 C62(H62), C68(H68)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
Sm2 Sm 0.136913(19) 0.15691(2) 0.514838(19) 0.01721(10) Uani 1 d . . .
Sm1 Sm 0.357205(19) 0.32532(2) 0.456443(19) 0.01670(10) Uani 1 d . . .
O3 O 0.2712(3) 0.1341(3) 0.4277(3) 0.0221(8) Uani 1 d . . .
O10 O 0.2301(3) -0.6550(3) 0.5505(3) 0.0199(8) Uani 1 d . . .
O11 O 0.1205(3) 0.2657(4) 0.3798(3) 0.0264(9) Uani 1 d . . .
O14 O 0.5189(3) 0.3449(3) 0.4559(3) 0.0259(9) Uani 1 d . . .
O16 O -0.0275(3) 0.1625(3) 0.5164(3) 0.0210(9) Uani 1 d . . .
O21 O 0.2236(3) 0.4105(4) 0.3641(2) 0.0246(9) Uani 1 d . . .
O25 O 0.3936(3) 0.3046(4) 0.3019(3) 0.0279(9) Uani 1 d . . .
H25A H 0.4312 0.2450 0.2966 0.042 Uiso 1 d . . GR
H25B H 0.4199 0.3692 0.2834 0.042 Uiso 1 d . . GR
O33 O 0.3956(3) 0.2458(4) 0.6020(2) 0.0254(9) Uani 1 d . . .
O40 O 0.0744(3) 0.0354(4) 0.3826(3) 0.0284(9) Uani 1 d . . .
H40A H 0.0421 0.0800 0.3442 0.043 Uiso 1 d . . GR
H40B H 0.0392 -0.0212 0.4007 0.043 Uiso 1 d . . GR
O42 O 0.4209(3) 0.1074(3) 0.4417(3) 0.0265(9) Uani 1 d . . .
O44 O 0.0811(3) -0.6218(4) 0.5445(3) 0.0276(9) Uani 1 d . . .
O48 O 0.1028(3) 0.1812(4) 0.6721(3) 0.0276(10) Uani 1 d . . .
H48A H 0.0746 0.2493 0.6803 0.041 Uiso 1 d . . GR
H48B H 0.1538 0.1807 0.7075 0.041 Uiso 1 d . . GR
N54 N 0.2365(4) 0.7837(4) 0.3360(3) 0.0272(11) Uani 1 d . . .
O2 O -0.2122(3) 0.3961(4) 0.1149(2) 0.0261(9) Uani 1 d . . .
C5 C 0.3260(4) -0.0637(5) 0.4161(3) 0.0197(11) Uani 1 d . . .
C9 C 0.1788(3) -0.4597(5) 0.5877(3) 0.0167(10) Uani 1 d . . .
C13 C 0.1235(4) -0.3672(5) 0.5527(4) 0.0194(11) Uani 1 d . . .
H13 H 0.0736 -0.3825 0.5117 0.023 Uiso 1 calc . . R
N16 N 0.2680(4) -0.3239(4) 0.6817(3) 0.0288(12) Uani 1 d . . .
C24 C 0.0707(4) 0.4292(5) 0.2938(3) 0.0196(11) Uani 1 d . . .
C11 C -0.0657(3) 0.4212(5) 0.1943(3) 0.0186(11) Uani 1 d . . .
C0AA C 0.0063(4) 0.3626(5) 0.2421(3) 0.0216(12) Uani 1 d . . .
H0AA H 0.0112 0.2799 0.2395 0.026 Uiso 1 calc . . R
C15 C 0.2162(4) -0.2344(5) 0.6456(4) 0.0250(12) Uani 1 d . . .
H15 H 0.2290 -0.1569 0.6653 0.030 Uiso 1 calc . . R
N18 N -0.0096(3) 0.6093(5) 0.2518(3) 0.0269(11) Uani 1 d . . .
C20 C -0.0709(4) 0.5440(5) 0.2025(4) 0.0245(12) Uani 1 d . . .
H20 H -0.1199 0.5832 0.1718 0.029 Uiso 1 calc . . R
C25 C 0.2556(4) 0.8991(5) 0.3555(4) 0.0243(12) Uani 1 d . . .
H25 H 0.2190 0.9572 0.3261 0.029 Uiso 1 calc . . R
C30 C -0.1343(4) 0.3521(5) 0.1327(3) 0.0210(12) Uani 1 d . . .
O32 O -0.0082(5) 0.0579(6) 0.2017(4) 0.075(2) Uani 1 d . . .
H32A H -0.0209 0.1199 0.1702 0.113 Uiso 1 d . . G
H32B H -0.0550 0.0372 0.2290 0.113 Uiso 1 d . . G
C35 C 0.1447(4) -0.2520(5) 0.5802(4) 0.0182(11) Uani 1 d . . .
C37 C 0.1453(4) 0.3644(5) 0.3496(3) 0.0195(11) Uani 1 d . . .
C41 C 0.1599(4) -0.5859(5) 0.5584(3) 0.0185(11) Uani 1 d . . .
C44 C 0.3588(4) 0.7289(5) 0.4453(3) 0.0178(11) Uani 1 d . . .
C48 C 0.3806(4) 0.8479(5) 0.4619(4) 0.0191(11) Uani 1 d . . .
H48 H 0.4299 0.8689 0.5020 0.023 Uiso 1 calc . . R
C57 C 0.0599(4) 0.5508(5) 0.2965(4) 0.0241(12) Uani 1 d . . .
H57 H 0.1032 0.5952 0.3313 0.029 Uiso 1 calc . . R
C62 C 0.2498(4) -0.4345(5) 0.6512(4) 0.0250(12) Uani 1 d . . .
H62 H 0.2867 -0.4969 0.6738 0.030 Uiso 1 calc . . R
C66 C 0.0955(4) -0.1455(5) 0.5381(4) 0.0178(11) Uani 1 d . . .
C68 C 0.2875(4) 0.7014(5) 0.3817(4) 0.0213(12) Uani 1 d . . .
H68 H 0.2744 0.6214 0.3702 0.026 Uiso 1 calc . . R
C70 C 0.3427(4) 0.0654(5) 0.4303(3) 0.0207(11) Uani 1 d . . .
C74 C 0.4097(4) 0.6295(5) 0.4961(4) 0.0193(11) Uani 1 d . . .
O1 O 0.3764(3) 0.5266(4) 0.4882(3) 0.0278(9) Uani 1 d . . .
O0AA O 0.1290(3) -0.0445(4) 0.5588(3) 0.0282(9) Uani 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
Sm2 Sm1 3.8745(4) . ?
Sm2 O3 2.434(4) . ?
Sm2 O10 2.542(4) 1_565 ?
Sm2 O11 2.341(4) . ?
Sm2 O16 2.398(4) . ?
Sm2 O40 2.505(4) . ?
Sm2 O44 2.655(4) 1_565 ?
Sm2 O48 2.434(4) . ?
Sm2 O2 2.632(4) 4_666 ?
Sm2 C41 2.966(5) 1_565 ?
Sm2 O0AA 2.353(4) . ?
Sm1 O3 2.503(4) . ?
Sm1 O10 2.406(4) 1_565 ?
Sm1 O14 2.368(4) . ?
Sm1 O21 2.489(4) . ?
Sm1 O25 2.400(4) . ?
Sm1 O33 2.366(4) . ?
Sm1 O42 2.626(4) . ?
Sm1 C70 2.943(6) . ?
Sm1 O1 2.316(4) . ?
O3 C70 1.294(6) . ?
O10 Sm2 2.541(4) 1_545 ?
O10 Sm1 2.406(4) 1_545 ?
O10 C41 1.296(6) . ?
O11 C37 1.256(6) . ?
O14 C74 1.251(6) 3_666 ?
O16 C66 1.249(7) 3_556 ?
O21 C37 1.258(6) . ?
O33 C30 1.276(7) 4_666 ?
O42 C70 1.234(6) . ?
O44 Sm2 2.655(4) 1_545 ?
O44 C41 1.220(6) . ?
N54 C25 1.349(7) . ?
N54 C68 1.337(7) . ?
O2 Sm2 2.632(4) 4_565 ?
O2 C30 1.248(7) . ?
C5 C25 1.380(7) 1_545 ?
C5 C48 1.413(7) 1_545 ?
C5 C70 1.479(8) . ?
C9 C13 1.390(7) . ?
C9 C41 1.499(7) . ?
C9 C62 1.378(7) . ?
C13 C35 1.382(7) . ?
N16 C15 1.343(7) . ?
N16 C62 1.338(7) . ?
C24 C0AA 1.388(7) . ?
C24 C37 1.505(7) . ?
C24 C57 1.371(8) . ?
C11 C0AA 1.389(7) . ?
C11 C20 1.384(8) . ?
C11 C30 1.518(7) . ?
C15 C35 1.386(7) . ?
N18 C20 1.332(7) . ?
N18 C57 1.341(7) . ?
C25 C5 1.380(7) 1_565 ?
C30 O33 1.276(7) 4_565 ?
C35 C66 1.506(7) . ?
C41 Sm2 2.966(5) 1_545 ?
C44 C48 1.387(7) . ?
C44 C68 1.388(7) . ?
C44 C74 1.510(7) . ?
C48 C5 1.413(7) 1_565 ?
C66 O16 1.248(7) 3_556 ?
C66 O0AA 1.261(6) . ?
C74 O14 1.251(6) 3_666 ?
C74 O1 1.253(6) . ?

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
O3 Sm2 Sm1 38.93(9) . . ?
O3 Sm2 O10 76.06(12) . 1_565 ?
O3 Sm2 O40 77.81(13) . . ?
O3 Sm2 O44 116.95(13) . 1_565 ?
O3 Sm2 O2 66.67(12) . 4_666 ?
O3 Sm2 C41 97.75(14) . 1_565 ?
O10 Sm2 Sm1 37.23(9) 1_565 . ?
O10 Sm2 O44 50.01(12) 1_565 1_565 ?
O10 Sm2 O2 69.93(12) 1_565 4_666 ?
O10 Sm2 C41 25.76(13) 1_565 1_565 ?
O11 Sm2 Sm1 65.88(9) . . ?
O11 Sm2 O3 68.76(13) . . ?
O11 Sm2 O10 76.53(13) . 1_565 ?
O11 Sm2 O16 87.33(13) . . ?
O11 Sm2 O40 66.65(14) . . ?
O11 Sm2 O44 69.03(13) . 1_565 ?
O11 Sm2 O48 138.24(14) . . ?
O11 Sm2 O2 129.02(13) . 4_666 ?
O11 Sm2 C41 71.57(14) . 1_565 ?
O11 Sm2 O0AA 137.02(14) . . ?
O16 Sm2 Sm1 146.47(9) . . ?
O16 Sm2 O3 148.15(13) . . ?
O16 Sm2 O10 119.73(12) . 1_565 ?
O16 Sm2 O40 73.38(13) . . ?
O16 Sm2 O44 69.88(12) . 1_565 ?
O16 Sm2 O48 73.50(14) . . ?
O16 Sm2 O2 142.74(12) . 4_666 ?
O16 Sm2 C41 94.01(13) . 1_565 ?
O40 Sm2 Sm1 110.51(9) . . ?
O40 Sm2 O10 140.55(13) . 1_565 ?
O40 Sm2 O44 122.57(13) . 1_565 ?
O40 Sm2 O2 124.17(13) . 4_666 ?
O40 Sm2 C41 136.65(14) . 1_565 ?
O44 Sm2 Sm1 81.43(9) 1_565 . ?
O44 Sm2 C41 24.27(13) 1_565 1_565 ?
O48 Sm2 Sm1 112.85(10) . . ?
O48 Sm2 O3 138.30(13) . . ?
O48 Sm2 O10 81.41(13) . 1_565 ?
O48 Sm2 O40 136.34(14) . . ?
O48 Sm2 O44 69.59(13) . 1_565 ?
O48 Sm2 O2 72.80(13) . 4_666 ?
O48 Sm2 C41 73.17(14) . 1_565 ?
O2 Sm2 Sm1 64.09(9) 4_666 . ?
O2 Sm2 O44 111.76(12) 4_666 1_565 ?
O2 Sm2 C41 91.11(13) 4_666 1_565 ?
C41 Sm2 Sm1 59.55(10) 1_565 . ?
O0AA Sm2 Sm1 125.91(10) . . ?
O0AA Sm2 O3 95.95(14) . . ?
O0AA Sm2 O10 140.62(12) . 1_565 ?
O0AA Sm2 O16 87.34(13) . . ?
O0AA Sm2 O40 70.97(13) . . ?
O0AA Sm2 O44 145.82(14) . 1_565 ?
O0AA Sm2 O48 79.88(14) . . ?
O0AA Sm2 O2 71.54(13) . 4_666 ?
O0AA Sm2 C41 151.37(14) . 1_565 ?
O3 Sm1 Sm2 37.68(9) . . ?
O3 Sm1 O42 50.67(12) . . ?
O3 Sm1 C70 25.91(13) . . ?
O10 Sm1 Sm2 39.72(9) 1_565 . ?
O10 Sm1 O3 77.30(12) 1_565 . ?
O10 Sm1 O21 71.30(12) 1_565 . ?
O10 Sm1 O42 115.13(12) 1_565 . ?
O10 Sm1 C70 96.65(14) 1_565 . ?
O14 Sm1 Sm2 152.46(9) . . ?
O14 Sm1 O3 124.40(13) . . ?
O14 Sm1 O10 143.23(14) . 1_565 ?
O14 Sm1 O21 134.63(13) . . ?
O14 Sm1 O25 73.62(14) . . ?
O14 Sm1 O42 74.19(13) . . ?
O14 Sm1 C70 98.80(14) . . ?
O21 Sm1 Sm2 71.42(9) . . ?
O21 Sm1 O3 82.64(12) . . ?
O21 Sm1 O42 125.30(12) . . ?
O21 Sm1 C70 105.12(14) . . ?
O25 Sm1 Sm2 114.16(10) . . ?
O25 Sm1 O3 84.07(14) . . ?
O25 Sm1 O10 142.52(13) . 1_565 ?
O25 Sm1 O21 74.29(13) . . ?
O25 Sm1 O42 74.17(13) . . ?
O25 Sm1 C70 78.31(14) . . ?
O33 Sm1 Sm2 76.05(9) . . ?
O33 Sm1 O3 85.19(13) . . ?
O33 Sm1 O10 69.39(13) . 1_565 ?
O33 Sm1 O14 82.34(14) . . ?
O33 Sm1 O21 140.50(13) . . ?
O33 Sm1 O25 141.34(14) . . ?
O33 Sm1 O42 70.35(13) . . ?
O33 Sm1 C70 75.97(14) . . ?
O42 Sm1 Sm2 82.52(9) . . ?
O42 Sm1 C70 24.77(13) . . ?
C70 Sm1 Sm2 59.67(11) . . ?
O1 Sm1 Sm2 121.24(10) . . ?
O1 Sm1 O3 156.87(13) . . ?
O1 Sm1 O10 83.11(13) . 1_565 ?
O1 Sm1 O14 78.73(13) . . ?
O1 Sm1 O21 79.49(13) . . ?
O1 Sm1 O25 104.87(15) . . ?
O1 Sm1 O33 99.41(14) . . ?
O1 Sm1 O42 152.02(13) . . ?
O1 Sm1 C70 175.08(14) . . ?
Sm2 O3 Sm1 103.39(14) . . ?
C70 O3 Sm2 136.3(3) . . ?
C70 O3 Sm1 96.4(3) . . ?
Sm1 O10 Sm2 103.06(13) 1_545 1_545 ?
C41 O10 Sm2 95.8(3) . 1_545 ?
C41 O10 Sm1 138.8(3) . 1_545 ?
C37 O11 Sm2 138.5(3) . . ?
C74 O14 Sm1 143.8(4) 3_666 . ?
C66 O16 Sm2 137.5(4) 3_556 . ?
C37 O21 Sm1 127.0(3) . . ?
C30 O33 Sm1 125.8(3) 4_666 . ?
C70 O42 Sm1 92.1(3) . . ?
C41 O44 Sm2 92.3(3) . 1_545 ?
C68 N54 C25 117.0(5) . . ?
C30 O2 Sm2 137.8(4) . 4_565 ?
C25 C5 C48 117.9(5) 1_545 1_545 ?
C25 C5 C70 119.7(5) 1_545 . ?
C48 C5 C70 122.4(5) 1_545 . ?
C13 C9 C41 120.3(5) . . ?
C62 C9 C13 119.4(5) . . ?
C62 C9 C41 120.4(5) . . ?
C35 C13 C9 118.2(5) . . ?
C62 N16 C15 117.7(5) . . ?
C0AA C24 C37 118.6(5) . . ?
C57 C24 C0AA 118.4(5) . . ?
C57 C24 C37 122.9(5) . . ?
C0AA C11 C30 120.5(5) . . ?
C20 C11 C0AA 118.0(5) . . ?
C20 C11 C30 121.5(5) . . ?
C24 C0AA C11 119.0(6) . . ?
N16 C15 C35 123.0(5) . . ?
C20 N18 C57 117.2(5) . . ?
N18 C20 C11 123.7(5) . . ?
N54 C25 C5 124.1(5) . 1_565 ?
O33 C30 C11 115.1(5) 4_565 . ?
O2 C30 O33 126.3(5) . 4_565 ?
O2 C30 C11 118.5(5) . . ?
C13 C35 C15 118.8(5) . . ?
C13 C35 C66 121.8(5) . . ?
C15 C35 C66 119.3(5) . . ?
O11 C37 O21 125.5(5) . . ?
O11 C37 C24 114.0(5) . . ?
O21 C37 C24 120.5(5) . . ?
O10 C41 Sm2 58.5(3) . 1_545 ?
O10 C41 C9 117.4(5) . . ?
O44 C41 Sm2 63.4(3) . 1_545 ?
O44 C41 O10 121.8(5) . . ?
O44 C41 C9 120.8(5) . . ?
C9 C41 Sm2 174.1(4) . 1_545 ?
C48 C44 C68 119.0(5) . . ?
C48 C44 C74 121.5(5) . . ?
C68 C44 C74 119.6(5) . . ?
C44 C48 C5 118.3(5) . 1_565 ?
N18 C57 C24 123.7(5) . . ?
N16 C62 C9 122.8(5) . . ?
O16 C66 C35 118.7(5) 3_556 . ?
O16 C66 O0AA 124.8(5) 3_556 . ?
O0AA C66 C35 116.4(5) . . ?
N54 C68 C44 123.6(5) . . ?
O3 C70 Sm1 57.7(3) . . ?
O3 C70 C5 117.0(5) . . ?
O42 C70 Sm1 63.1(3) . . ?
O42 C70 O3 120.7(5) . . ?
O42 C70 C5 122.3(5) . . ?
C5 C70 Sm1 174.6(4) . . ?
O14 C74 C44 118.3(5) 3_666 . ?
O14 C74 O1 124.4(5) 3_666 . ?
O1 C74 C44 117.3(5) . . ?
C74 O1 Sm1 162.8(4) . . ?
C66 O0AA Sm2 144.9(4) . . ?

# start Validation Reply Form
_vrf_PLAT029_shelxl              
;
RESPONSE: This Alert is due to the low
quality crystals are used for collecting 
data for single crystal X-ray crystallography.
;
_vrf_PLAT420_shelxl              
;
RESPONSE: This Alert is due to the presence of
residual electron density due to heavy metal atoms 
after refinement of structure. 
;
_vrf_PLAT415_shelxl              
;
RESPONSE: This Alert is due to the presence of
residual electron density due to heavy metal atoms 
after refinement of structure. 
;
# end Validation Reply Form


_olex2_date_sample_data_collection 2016-12-15
_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 1.879
_oxdiff_exptl_absorpt_empirical_full_min 0.720
####################################################################### 
# 
# 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_z5_rt_mo
_audit_block_doi                 10.5517/ccdc.csd.cc2000xz
_database_code_depnum_ccdc_archive 'CCDC 1847070'
_audit_update_record             
;
2018-06-04 deposited with the CCDC.
2018-08-06 downloaded from the CCDC.
;
_audit_creation_date             2018-03-16
_audit_creation_method           
;
Olex2 1.2-ac21
(compiled 2015.09.16 svn.r134, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C11 H11 Er N O8'
_chemical_formula_sum            'C11 H11 Er N O8'
_chemical_formula_weight         452.47
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C72 H80 Er8 N8 O64'
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'
Er Er -0.2586 4.9576 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y, -z+1/2'
3 'x+1/2, y+1/2, z'
4 '-x+1/2, y+1/2, -z+1/2'
5 '-x, -y, -z'
6 'x, -y, z-1/2'
7 '-x+1/2, -y+1/2, -z'
8 'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   19.2352(3)
_cell_length_b                   7.90393(14)
_cell_length_c                   16.7290(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.5518(15)
_cell_angle_gamma                90.00
_cell_volume                     2542.44(7)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    3074
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.8920
_cell_measurement_theta_min      2.1120
_exptl_absorpt_coefficient_mu    6.643
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68284
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    2.364
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       monoclinic
_exptl_crystal_F_000             1728
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-8 11 -1 0.1688
15 -9 0 0.1400
-3 0 23 0.0229
-14 0 -20 0.0399
13 -8 12 0.1173
0 0 24 0.0279
12 3 20 0.0295
24 5 -3 0.0434
2 -11 -7 0.1335
-27 0 2 0.0549
0 0 -24 0.0459
1 -11 2 0.1412
15 2 -19 0.0362

_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.155
_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
-8.0004 11.0000 -1.0000 0.0148 -0.0124 -1.0316
15.0004 -9.0000 -0.0000 -0.0220 -0.2889 0.9356
-3.0005 -0.0000 23.0000 0.9620 0.1770 0.0278
-13.9996 0.0000 -20.0000 -0.8849 0.4286 -0.2083
13.0001 -8.0000 11.9999 0.4859 -0.2077 0.8598
-0.0005 -0.0000 24.0000 1.0129 0.0749 0.0637
11.9995 3.0000 20.0000 0.9009 -0.4375 -0.0703
24.0000 5.0000 -3.0000 -0.0203 -0.9828 -0.1694
2.0006 -11.0000 -7.0000 -0.3699 0.1979 0.9438
-27.0002 -0.0000 2.0000 0.0058 0.9532 -0.2939
0.0005 0.0000 -24.0000 -1.0129 -0.0749 -0.0637
1.0004 -11.0000 1.9999 0.0070 0.2610 0.9567
15.0004 2.0000 -18.9999 -0.7436 -0.6381 -0.0552

_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_unetI/netI     0.0416
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            4281
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.33
_diffrn_reflns_theta_min         2.12
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9974
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.868
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -10.00  72.00   1.00   12.00    --   26.84  57.00 -90.00   82
  2  ω     -6.00  98.00   1.00   12.00    --   26.84  57.00   0.00  104
  3  ω     63.00 104.00   1.00   12.00    --   26.84 178.00-120.00   41
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0029108000
_diffrn_orient_matrix_UB_12      0.0072983000
_diffrn_orient_matrix_UB_13      0.0422057000
_diffrn_orient_matrix_UB_21      -0.0350716000
_diffrn_orient_matrix_UB_22      -0.0263524000
_diffrn_orient_matrix_UB_23      0.0031196000
_diffrn_orient_matrix_UB_31      0.0110836000
_diffrn_orient_matrix_UB_32      -0.0854782000
_diffrn_orient_matrix_UB_33      0.0026557000
_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'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                2480
_reflns_number_total             2760
_reflns_odcompleteness_completeness 98.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         1.269
_refine_diff_density_min         -1.194
_refine_diff_density_rms         0.186
_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     186
_refine_ls_number_reflns         2760
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0299
_refine_ls_restrained_S_all      1.061
_refine_ls_shift/su_max          0.036
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0441P)²+3.7364P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0800
_refine_ls_wR_factor_ref         0.0847
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_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 O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C2) = Uanis(C1)
3.a Rotating group:
 O6(H6A,H6B), O29(H29A,H29B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C1AA(H1AA), C4(H4)
3.c X=CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
Er1 Er 0.455892(10) 0.81390(3) 0.434072(12) 0.02069(10) Uani 1 d . . .
O1 O 0.04874(18) 0.7930(4) 0.4313(2) 0.0277(8) Uani 1 d . . .
O6 O 0.4488(2) 0.5457(5) 0.3838(2) 0.0397(10) Uani 1 d . . .
H6A H 0.4880 0.5165 0.3634 0.060 Uiso 1 d . . GR
H6B H 0.4165 0.5398 0.3468 0.060 Uiso 1 d . . GR
O8 O 0.37157(18) 0.8635(5) 0.3438(2) 0.0361(9) Uani 1 d . . .
O20 O 0.14760(19) 0.7604(6) 0.4967(2) 0.0396(10) Uani 1 d . . .
N23 N 0.1456(2) 0.9388(7) 0.2249(3) 0.0367(11) Uani 1 d . . .
O30 O 0.3577(2) 0.9220(8) 0.2142(3) 0.0669(16) Uani 1 d . . .
C32 C 0.1144(3) 0.8000(6) 0.4341(3) 0.0246(11) Uani 1 d . . .
O34 O 0.56109(17) 0.9266(4) 0.5114(2) 0.0292(8) Uani 1 d . . .
C3 C 0.2247(3) 0.8448(6) 0.3593(3) 0.0259(11) Uani 1 d . . .
H3 H 0.2508 0.8121 0.4043 0.031 Uiso 1 calc . . R
C1AA C 0.1164(3) 0.8954(8) 0.2937(3) 0.0337(13) Uani 1 d . . .
H1AA H 0.0682 0.8977 0.2956 0.040 Uiso 1 calc . . R
C5 C 0.1528(2) 0.8479(6) 0.3610(3) 0.0248(10) Uani 1 d . . .
C9 C 0.2571(3) 0.8912(7) 0.2899(3) 0.0264(10) Uani 1 d . . .
C15 C 0.3357(3) 0.8914(8) 0.2819(3) 0.0311(12) Uani 1 d . . .
O29 O 0.5183(2) 0.9585(8) 0.3378(3) 0.0698(17) Uani 1 d . . .
H29A H 0.4905 0.9963 0.3003 0.105 Uiso 1 d . . GR
H29B H 0.5484 0.8918 0.3164 0.105 Uiso 1 d . . GR
C4 C 0.2158(3) 0.9358(7) 0.2240(3) 0.0318(12) Uani 1 d . . .
H4 H 0.2374 0.9651 0.1769 0.038 Uiso 1 calc . . R
O0AA O 0.5678(2) 0.6865(4) 0.4503(3) 0.0387(10) Uani 1 d . . .
C2AA C 0.5955(3) 0.7968(7) 0.4925(4) 0.0347(13) Uani 1 d A . .
C0AA C 0.6682(4) 0.7817(14) 0.5236(6) 0.078(3) Uani 1 d . . .
C1 C 0.7100(9) 0.849(3) 0.4693(18) 0.283(11) Uani 1 d A 2 .
H1A H 0.7429 0.7820 0.4448 0.340 Uiso 1 calc A 2 R
H1B H 0.7060 0.9631 0.4561 0.340 Uiso 1 calc A 2 R
C2 C 0.7011(9) 0.649(3) 0.5090(18) 0.283(11) Uani 1 d A 1 .
H2A H 0.7361 0.6510 0.4718 0.340 Uiso 1 calc A 1 R
H2B H 0.6905 0.5495 0.5354 0.340 Uiso 1 calc A 1 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
Er1 O1 2.410(4) 7_566 ?
Er1 O6 2.283(4) . ?
Er1 O8 2.220(4) . ?
Er1 O20 2.402(4) 7_566 ?
Er1 C32 2.768(5) 7_566 ?
Er1 O34 2.534(3) . ?
Er1 O34 2.271(3) 5_676 ?
Er1 O29 2.335(4) . ?
Er1 O0AA 2.385(4) . ?
Er1 C2AA 2.837(6) . ?
O1 Er1 2.410(4) 7_566 ?
O1 C32 1.263(6) . ?
O8 C15 1.249(6) . ?
O20 Er1 2.402(4) 7_566 ?
O20 C32 1.253(6) . ?
N23 C1AA 1.340(7) . ?
N23 C4 1.350(6) . ?
O30 C15 1.245(6) . ?
C32 Er1 2.768(5) 7_566 ?
C32 C5 1.494(7) . ?
O34 Er1 2.271(3) 5_676 ?
O34 C2AA 1.267(6) . ?
C3 C5 1.384(7) . ?
C3 C9 1.382(7) . ?
C1AA C5 1.363(7) . ?
C9 C15 1.521(6) . ?
C9 C4 1.387(7) . ?
O0AA C2AA 1.234(7) . ?
C2AA C0AA 1.483(9) . ?
C0AA C1 1.34(3) . ?
C0AA C2 1.25(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
O1 Er1 C32 27.12(14) 7_566 7_566 ?
O1 Er1 O34 72.25(12) 7_566 . ?
O1 Er1 C2AA 73.72(15) 7_566 . ?
O6 Er1 O1 90.88(13) . 7_566 ?
O6 Er1 O20 84.76(16) . 7_566 ?
O6 Er1 C32 88.06(15) . 7_566 ?
O6 Er1 O34 123.59(12) . . ?
O6 Er1 O29 103.12(19) . . ?
O6 Er1 O0AA 72.21(13) . . ?
O6 Er1 C2AA 97.40(15) . . ?
O8 Er1 O1 130.74(13) . 7_566 ?
O8 Er1 O6 83.03(15) . . ?
O8 Er1 O20 76.77(13) . 7_566 ?
O8 Er1 C32 103.64(15) . 7_566 ?
O8 Er1 O34 147.52(14) . . ?
O8 Er1 O34 90.17(14) . 5_676 ?
O8 Er1 O29 79.89(15) . . ?
O8 Er1 O0AA 142.41(15) . . ?
O8 Er1 C2AA 155.52(16) . . ?
O20 Er1 O1 53.98(12) 7_566 7_566 ?
O20 Er1 C32 26.87(14) 7_566 7_566 ?
O20 Er1 O34 120.03(13) 7_566 . ?
O20 Er1 C2AA 127.70(15) 7_566 . ?
C32 Er1 C2AA 100.83(17) 7_566 . ?
O34 Er1 O1 86.11(13) 5_676 7_566 ?
O34 Er1 O6 168.05(14) 5_676 . ?
O34 Er1 O20 84.11(15) 5_676 7_566 ?
O34 Er1 C32 96.17(14) . 7_566 ?
O34 Er1 C32 83.99(14) 5_676 7_566 ?
O34 Er1 O34 66.36(13) 5_676 . ?
O34 Er1 O29 85.24(18) 5_676 . ?
O34 Er1 O0AA 118.33(12) 5_676 . ?
O34 Er1 C2AA 26.52(13) . . ?
O34 Er1 C2AA 92.86(14) 5_676 . ?
O29 Er1 O1 148.16(14) . 7_566 ?
O29 Er1 O20 154.25(15) . 7_566 ?
O29 Er1 C32 168.67(18) . 7_566 ?
O29 Er1 O34 76.21(15) . . ?
O29 Er1 O0AA 78.81(16) . . ?
O29 Er1 C2AA 76.18(17) . . ?
O0AA Er1 O1 78.54(14) . 7_566 ?
O0AA Er1 O20 126.78(15) . 7_566 ?
O0AA Er1 C32 103.31(15) . 7_566 ?
O0AA Er1 O34 52.02(12) . . ?
O0AA Er1 C2AA 25.50(13) . . ?
C32 O1 Er1 92.4(3) . 7_566 ?
C15 O8 Er1 166.5(4) . . ?
C32 O20 Er1 93.1(3) . 7_566 ?
C1AA N23 C4 116.5(4) . . ?
O1 C32 Er1 60.4(3) . 7_566 ?
O1 C32 C5 119.8(5) . . ?
O20 C32 Er1 60.1(3) . 7_566 ?
O20 C32 O1 120.5(5) . . ?
O20 C32 C5 119.7(5) . . ?
C5 C32 Er1 175.7(3) . 7_566 ?
Er1 O34 Er1 113.63(13) 5_676 . ?
C2AA O34 Er1 156.0(4) . 5_676 ?
C2AA O34 Er1 90.2(3) . . ?
C9 C3 C5 119.1(5) . . ?
N23 C1AA C5 124.3(5) . . ?
C3 C5 C32 122.0(5) . . ?
C1AA C5 C32 119.4(4) . . ?
C1AA C5 C3 118.6(5) . . ?
C3 C9 C15 123.1(4) . . ?
C3 C9 C4 118.2(5) . . ?
C4 C9 C15 118.7(4) . . ?
O8 C15 C9 117.1(4) . . ?
O30 C15 O8 126.5(5) . . ?
O30 C15 C9 116.3(5) . . ?
N23 C4 C9 123.2(5) . . ?
C2AA O0AA Er1 98.2(3) . . ?
O34 C2AA Er1 63.3(3) . . ?
O34 C2AA C0AA 118.2(6) . . ?
O0AA C2AA Er1 56.3(3) . . ?
O0AA C2AA O34 119.6(5) . . ?
O0AA C2AA C0AA 122.2(5) . . ?
C0AA C2AA Er1 178.1(6) . . ?
C1 C0AA C2AA 107.9(12) . . ?
C2 C0AA C2AA 118.4(11) . . ?
C2 C0AA C1 83.4(15) . . ?

# start Validation Reply Form
_vrf_PLAT410_shelxl              
;
RESPONSE: This Alert is due to the presence of
residual electron density due to heavy metal atoms 
after refinement of structure. 
;
_vrf_PLAT417_shelxl              
;
RESPONSE: This Alert is due to the presence of
residual electron density due to heavy metal atoms 
after refinement of structure. 
;
_vrf_PLAT220_shelxl              
;
RESPONSE: This Alert is due to the presence of
residual electron density due to heavy metal atoms 
after refinement of structure. 
;
_vrf_PLAT230_shelxl              
;
RESPONSE: This Alert is due to the presence of
residual electron density due to heavy metal atoms 
after refinement of structure. 
;
_vrf_PLAT242_shelxl              
;
RESPONSE: This Alert is due to the presence of
residual electron density due to heavy metal atoms 
after refinement of structure. 
;
_vrf_PLAT250_shelxl              
;
RESPONSE: This Alert is due to the presence of
residual electron density due to heavy metal atoms 
after refinement of structure. 
;
# end Validation Reply Form


_olex2_date_sample_data_collection 2017-08-03
_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 1.454
_oxdiff_exptl_absorpt_empirical_full_min 0.828
####################################################################### 
# 
# 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_m2_rt_cu
_audit_block_doi                 10.5517/ccdc.csd.cc2000z1
_database_code_depnum_ccdc_archive 'CCDC 1847072'
_audit_update_record             
;
2018-06-04 deposited with the CCDC.
2018-08-06 downloaded from the CCDC.
;
_audit_creation_date             2018-03-15
_audit_creation_method           
;
Olex2 1.2-ac21
(compiled 2015.09.16 svn.r134, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C14 H10 Dy N2 O10, H2 O'
_chemical_formula_sum            'C14 H12 Dy N2 O11'
_chemical_formula_weight         546.76
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C28 H26 Dy2 N4 O24'
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'
Dy Dy -9.8046 9.8477 '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'

_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_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, -z'

_cell_length_a                   9.2117(6)
_cell_length_b                   9.5034(6)
_cell_length_c                   10.2696(6)
_cell_angle_alpha                96.241(5)
_cell_angle_beta                 94.321(5)
_cell_angle_gamma                93.127(5)
_cell_volume                     889.37(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3631
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      66.9640
_cell_measurement_theta_min      4.3430
_exptl_absorpt_coefficient_mu    23.085
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.19447
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    2.042
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       triclinic
_exptl_crystal_F_000             528
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 -6 1 0.0760
0 -1 7 0.1063
3 5 -1 0.0662
6 1 -1 0.0738
4 3 -4 0.1050
-1 6 -1 0.0760
-1 -4 -4 0.1110
-2 3 -5 0.0777
-6 0 1 0.0331
-2 1 6 0.1062
5 -3 1 0.0707
-1 5 3 0.0846
4 -5 -1 0.1041
-6 -1 -1 0.0116
5 1 2 0.0590
2 -1 6 0.1105
2 0 -6 0.1180

_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.152
_exptl_crystal_size_min          0.079
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 -6.0009 0.9998 -0.0799 -0.0627 0.9757
0.0001 -0.9996 7.0004 -0.0833 1.0137 0.2765
2.9999 5.0010 -1.0001 0.6946 0.0908 -0.6825
5.9997 1.0006 -1.0005 1.0271 -0.0124 0.0375
3.9998 3.0005 -4.0005 0.7978 -0.4199 -0.3924
-0.9999 6.0009 -0.9998 0.0799 0.0627 -0.9757
-1.0001 -4.0011 -4.0003 -0.2967 -0.7708 0.5107
-1.9999 3.0000 -5.0001 -0.1773 -0.6698 -0.6189
-5.9997 -0.0004 1.0005 -0.9876 0.0507 -0.1914
-1.9998 1.0005 6.0006 -0.3251 0.9068 -0.1184
4.9997 -3.0000 0.9996 0.6930 0.1185 0.6533
-0.9998 5.0010 3.0005 0.0153 0.6256 -0.7517
3.9997 -5.0006 -1.0006 0.4628 -0.2752 0.8912
-5.9997 -1.0007 -0.9996 -1.0146 -0.2881 -0.0726
4.9998 1.0007 1.9998 0.8448 0.4218 0.0553
1.9999 -0.9996 6.0002 0.2501 0.8966 0.3287
1.9998 -0.0003 -6.0006 0.3646 -0.8685 -0.0355

_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_unetI/netI     0.0430
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5221
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         67.00
_diffrn_reflns_theta_min         4.35
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9974
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      0.00  54.00   1.00    1.00    --   25.57 -57.00  60.00   54
  2  ω    -11.00 107.00   1.00    1.00    --   66.78 -77.00  60.00  118
  3  ω     90.00 128.00   1.00    1.00    --  108.00 -65.00   0.00   38
  4  ω    123.00 153.00   1.00    1.00    --  108.00 -89.00 -60.00   30
  5  ω    118.00 156.00   1.00    1.00    --  108.00 -89.00-120.00   38
  6  ω     70.00 131.00   1.00    1.00    --  108.00 -89.00   0.00   61
  7  ω     47.00 123.00   1.00    1.00    --  108.00-129.00 -95.86   76
  8  ω     32.00  67.00   1.00    1.00    --  108.00 -65.00   0.00   35
  9  ω     29.00  54.00   1.00    1.00    --  108.00 -89.00   0.00   25
 10  ω     23.00 104.00   1.00    1.00    --  108.00 -89.00 -60.00   81
 11  ω     26.00 104.00   1.00    1.00    --  108.00 -89.00-120.00   78
 12  ω     54.00 144.00   1.00    1.00    --  108.00  32.00-120.00   90
 13  ω    149.00 178.00   1.00    1.00    --  108.00  43.00 -90.00   29
 14  ω    120.00 169.00   1.00    1.00    --  108.00 104.00  30.00   49
 15  ω    124.00 151.00   1.00    1.00    --  108.00  54.00 120.00   27
 16  ω    100.00 145.00   1.00    1.00    --   66.78 111.00 150.00   45
 17  ω    109.00 144.00   1.00    1.00    --   66.78 154.00 112.00   35
 18  ω     92.00 142.00   1.00    1.00    --   66.78 178.00   0.00   50
 19  ω    103.00 178.00   1.00    1.00    --  108.00 138.00 -90.00   75
 20  ω    117.00 178.00   1.00    1.00    --  108.00  43.00-180.00   61
 21  ω    104.00 139.00   1.00    1.00    --   66.78 111.00 -30.00   35
 22  ω    102.00 175.00   1.00    1.00    --  108.00 104.00 -60.00   73
 23  ω     84.00 131.00   1.00    1.00    --  108.00  43.00 -90.00   47
 24  ω     66.00 149.00   1.00    1.00    --  108.00  43.00   0.00   83
 25  ω     78.00 104.00   1.00    1.00    --   66.78 154.00 112.00   26
 26  ω     70.00 107.00   1.00    1.00    --  108.00  54.00 120.00   37
 27  ω     69.00 173.00   1.00    1.00    --  108.00  43.00  90.00  104
 28  ω    -12.00 107.00   1.00    1.00    --   66.78 -45.00-150.00  119
 29  ω    -15.00 148.00   1.00    1.00    --   66.78 -15.00  30.00  163
 30  ω    -39.00  -3.00   1.00    1.00    --   25.57 -57.00  60.00   36
 31  ω    -44.00  59.00   1.00    1.00    --   25.57 -57.00 -60.00  103
 32  ω    -45.00  53.00   1.00    1.00    --   25.57 -77.00-150.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1635620000
_diffrn_orient_matrix_UB_12      0.0395197000
_diffrn_orient_matrix_UB_13      -0.0062521000
_diffrn_orient_matrix_UB_21      0.0166055000
_diffrn_orient_matrix_UB_22      0.0382507000
_diffrn_orient_matrix_UB_23      0.1502666000
_diffrn_orient_matrix_UB_31      0.0348418000
_diffrn_orient_matrix_UB_32      -0.1538658000
_diffrn_orient_matrix_UB_33      0.0175298000
_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'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                3053
_reflns_number_total             3122
_reflns_odcompleteness_completeness 98.27
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         8.343
_refine_diff_density_min         -9.150
_refine_diff_density_rms         0.400
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.303
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3122
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0991
_refine_ls_R_factor_gt           0.0986
_refine_ls_restrained_S_all      1.303
_refine_ls_shift/su_max          0.039
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2635
_refine_ls_wR_factor_ref         0.2656
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O15(H15A,H15B)
2.b Rotating group:
 O4(H4A,H4B), O3(H3A,H3B)
2.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C14(H14), C15(H15), C19(H19), C25(H25), C31(H31)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
Dy1 Dy 0.46998(5) 0.55740(5) 0.24116(4) 0.0117(4) Uiso 1 d . . .
O2 O 0.6719(9) 0.6453(10) 0.1449(8) 0.0295(19) Uani 1 d . . .
O4 O 0.4518(9) 0.7844(8) 0.3533(9) 0.032(2) Uani 1 d . . .
H4A H 0.4706 0.7856 0.4408 0.048 Uiso 1 d . . GR
H4B H 0.3621 0.8160 0.3401 0.048 Uiso 1 d . . GR
O6 O 0.3573(8) 0.7133(10) 0.0653(9) 0.0319(19) Uani 1 d . . .
O7 O 0.2207(9) 0.6148(9) 0.1993(9) 0.0308(19) Uani 1 d . . .
O9 O 0.3645(9) 0.4132(8) 0.5795(8) 0.0240(17) Uani 1 d . . .
O12 O 0.3317(10) 0.4321(9) 0.3666(9) 0.0283(19) Uani 1 d . . .
O15 O 0.4691(12) 0.1425(10) 0.3866(12) 0.047(3) Uani 1 d . . .
H15A H 0.5440 0.1511 0.4411 0.070 Uiso 1 d . . G
H15B H 0.4735 0.2078 0.3365 0.070 Uiso 1 d . . G
O17 O 0.3919(8) 0.3909(8) 0.0692(8) 0.0232(17) Uani 1 d . . .
O19 O 0.0241(9) 0.0404(8) 0.7150(9) 0.0294(18) Uani 1 d . . .
O0AA O -0.2116(9) 0.0535(9) 0.6656(10) 0.0332(19) Uani 1 d . . .
O3 O 0.6218(8) 0.3531(7) 0.2332(9) 0.0248(18) Uani 1 d . . .
H3A H 0.7044 0.3724 0.1993 0.037 Uiso 1 d . . GR
H3B H 0.5760 0.2801 0.1843 0.037 Uiso 1 d . . GR
N2 N 0.9832(10) 0.8633(9) -0.1209(10) 0.0209(19) Uani 1 d . . .
C3 C 0.6947(10) 0.6519(10) 0.0267(10) 0.014(2) Uani 1 d . . .
N5 N -0.1111(10) 0.3171(10) 0.3763(9) 0.0214(19) Uani 1 d . . .
C8 C 0.1333(10) 0.3372(10) 0.4726(10) 0.0126(19) Uani 1 d . . .
C10 C 0.0261(11) 0.3676(10) 0.3809(10) 0.016(2) Uani 1 d . . .
H10 H 0.0516 0.4269 0.3188 0.020 Uiso 1 calc . . R
C11 C 0.2881(10) 0.3995(10) 0.4735(9) 0.0115(18) Uani 1 d . . .
C14 C 0.9651(11) 0.6804(10) 0.0671(10) 0.016(2) Uani 1 d . . .
H14 H 0.9593 0.6225 0.1343 0.019 Uiso 1 calc . . R
C15 C 1.1035(11) 0.8269(10) -0.0564(11) 0.017(2) Uani 1 d . . .
H15 H 1.1932 0.8667 -0.0744 0.020 Uiso 1 calc . . R
C17 C 0.2337(12) 0.6844(11) 0.1052(12) 0.022(2) Uani 1 d . . .
C19 C 0.8527(12) 0.8104(12) -0.0945(11) 0.017(2) Uani 1 d . . .
H19 H 0.7690 0.8379 -0.1389 0.021 Uiso 1 calc . . R
C22 C -0.0430(11) 0.1916(11) 0.5597(11) 0.015(2) Uani 1 d . . .
C23 C 0.8396(11) 0.7138(10) -0.0006(10) 0.014(2) Uani 1 d . . .
C25 C 0.0989(12) 0.2486(11) 0.5647(10) 0.016(2) Uani 1 d . . .
H25 H 0.1691 0.2276 0.6284 0.019 Uiso 1 calc . . R
C28 C 1.0999(11) 0.7321(10) 0.0363(11) 0.017(2) Uani 1 d . . .
C29 C -0.0869(11) 0.0863(9) 0.6527(10) 0.017(2) Uani 1 d . . .
C31 C -0.1442(11) 0.2282(12) 0.4646(13) 0.021(2) Uani 1 d . . .
H31 H -0.2395 0.1895 0.4616 0.025 Uiso 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
Dy1 O2 2.328(8) . ?
Dy1 O4 2.353(7) . ?
Dy1 O6 2.646(9) . ?
Dy1 O7 2.407(8) . ?
Dy1 O9 2.283(8) 2_666 ?
Dy1 O12 2.261(8) . ?
Dy1 O17 2.284(7) . ?
Dy1 O3 2.452(7) . ?
Dy1 C17 2.888(11) . ?
O2 C3 1.255(13) . ?
O6 C17 1.265(15) . ?
O7 C17 1.238(16) . ?
O9 Dy1 2.283(8) 2_666 ?
O9 C11 1.241(12) . ?
O12 C11 1.261(13) . ?
O17 C3 1.237(12) 2_665 ?
O19 C29 1.287(13) . ?
O0AA C29 1.194(13) . ?
N2 C15 1.329(14) . ?
N2 C19 1.336(14) . ?
C3 O17 1.237(12) 2_665 ?
C3 C23 1.487(14) . ?
N5 C10 1.323(14) . ?
N5 C31 1.345(16) . ?
C8 C10 1.377(15) . ?
C8 C11 1.513(13) . ?
C8 C25 1.376(16) . ?
C14 C23 1.374(14) . ?
C14 C28 1.381(15) . ?
C15 C28 1.382(15) . ?
C17 C28 1.491(15) 1_455 ?
C19 C23 1.410(15) . ?
C22 C25 1.383(15) . ?
C22 C29 1.516(14) . ?
C22 C31 1.384(16) . ?
C28 C17 1.491(15) 1_655 ?

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
O2 Dy1 O4 89.0(3) . . ?
O2 Dy1 O6 76.0(3) . . ?
O2 Dy1 O7 126.7(3) . . ?
O2 Dy1 O3 78.8(3) . . ?
O2 Dy1 C17 102.0(3) . . ?
O4 Dy1 O6 73.9(3) . . ?
O4 Dy1 O7 73.9(3) . . ?
O4 Dy1 O3 142.2(3) . . ?
O4 Dy1 C17 73.1(3) . . ?
O6 Dy1 C17 26.0(3) . . ?
O7 Dy1 O6 50.9(3) . . ?
O7 Dy1 O3 140.8(3) . . ?
O7 Dy1 C17 25.0(3) . . ?
O9 Dy1 O2 80.6(3) 2_666 . ?
O9 Dy1 O4 71.4(3) 2_666 . ?
O9 Dy1 O6 138.0(3) 2_666 . ?
O9 Dy1 O7 134.9(3) 2_666 . ?
O9 Dy1 O17 139.7(3) 2_666 . ?
O9 Dy1 O3 71.4(3) 2_666 . ?
O9 Dy1 C17 144.3(3) 2_666 . ?
O12 Dy1 O2 161.0(4) . . ?
O12 Dy1 O4 98.2(3) . . ?
O12 Dy1 O6 122.9(3) . . ?
O12 Dy1 O7 72.2(3) . . ?
O12 Dy1 O9 85.1(3) . 2_666 ?
O12 Dy1 O17 87.1(3) . . ?
O12 Dy1 O3 84.8(3) . . ?
O12 Dy1 C17 97.0(3) . . ?
O17 Dy1 O2 95.8(3) . . ?
O17 Dy1 O4 149.0(3) . . ?
O17 Dy1 O6 77.6(3) . . ?
O17 Dy1 O7 78.8(3) . . ?
O17 Dy1 O3 68.5(3) . . ?
O17 Dy1 C17 75.9(3) . . ?
O3 Dy1 O6 135.0(3) . . ?
O3 Dy1 C17 144.3(3) . . ?
C3 O2 Dy1 131.4(7) . . ?
C17 O6 Dy1 87.7(7) . . ?
C17 O7 Dy1 99.8(7) . . ?
C11 O9 Dy1 172.6(7) . 2_666 ?
C11 O12 Dy1 154.6(7) . . ?
C3 O17 Dy1 150.7(7) 2_665 . ?
C15 N2 C19 120.0(9) . . ?
O2 C3 C23 117.2(9) . . ?
O17 C3 O2 125.6(9) 2_665 . ?
O17 C3 C23 117.2(9) 2_665 . ?
C10 N5 C31 117.1(9) . . ?
C10 C8 C11 121.1(9) . . ?
C25 C8 C10 119.4(9) . . ?
C25 C8 C11 119.6(9) . . ?
N5 C10 C8 123.6(9) . . ?
O9 C11 O12 124.3(9) . . ?
O9 C11 C8 117.6(9) . . ?
O12 C11 C8 118.0(8) . . ?
C23 C14 C28 120.5(10) . . ?
N2 C15 C28 122.4(9) . . ?
O6 C17 Dy1 66.3(6) . . ?
O6 C17 C28 119.7(11) . 1_455 ?
O7 C17 Dy1 55.2(6) . . ?
O7 C17 O6 121.4(10) . . ?
O7 C17 C28 118.9(11) . 1_455 ?
C28 C17 Dy1 172.3(8) 1_455 . ?
N2 C19 C23 121.2(9) . . ?
C25 C22 C29 121.1(9) . . ?
C25 C22 C31 118.8(10) . . ?
C31 C22 C29 120.1(9) . . ?
C14 C23 C3 120.9(9) . . ?
C14 C23 C19 117.8(10) . . ?
C19 C23 C3 121.3(9) . . ?
C8 C25 C22 118.1(10) . . ?
C14 C28 C17 118.7(10) . 1_655 ?
C15 C28 C14 118.0(9) . . ?
C15 C28 C17 123.3(10) . 1_655 ?
O19 C29 C22 112.3(9) . . ?
O0AA C29 O19 125.4(10) . . ?
O0AA C29 C22 122.2(10) . . ?
N5 C31 C22 123.0(10) . . ?

# start Validation Reply Form
_vrf_PLAT213_shelxl              
;
RESPONSE: This Alert is due to the presence of
residual electron density due to heavy metal atoms 
after refinement of structure. 
;
_vrf_PLAT417_shelxl              
;
RESPONSE: This Alert is due to the presence of
residual electron density due to heavy metal atoms 
after refinement of structure. 
;
_vrf_PLAT097_shelxl              
;
RESPONSE: This Alert is due to the presence of
residual electron density due to heavy metal atoms 
after refinement of structure. 
;
_vrf_PLAT098_shelxl              
;
RESPONSE: This Alert is due to the presence of
residual electron density due to heavy metal atoms 
after refinement of structure. 
;
_vrf_PLAT201_shelxl              
;
RESPONSE: This Alert is due to the presence of
residual electron density due to heavy metal atoms 
after refinement of structure. 
;
_vrf_PLAT415_shelxl              
;
RESPONSE: This Alert is due to the presence of
residual electron density due to heavy metal atoms 
after refinement of structure. 
;
# end Validation Reply Form


_olex2_date_sample_data_collection 2016-09-02
_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 3.697
_oxdiff_exptl_absorpt_empirical_full_min 0.518
####################################################################### 
# 
# 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_g1_lt_mo
_audit_block_doi                 10.5517/ccdc.csd.cc2000y0
_database_code_depnum_ccdc_archive 'CCDC 1847071'
_audit_update_record             
;
2018-06-04 deposited with the CCDC.
2018-08-06 downloaded from the CCDC.
;
_audit_creation_date             2018-03-08
_audit_creation_method           
;
Olex2 1.2-ac21
(compiled 2015.09.16 svn.r134, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C23 H18 Eu2 N3 O16, 2(H2 O), C3 H7 N O'
_chemical_formula_sum            'C26 H29 Eu2 N4 O19'
_chemical_formula_weight         1005.45
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C100 H100 Eu8 N16 O80 '
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'
Eu Eu -0.1578 3.6682 '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'

_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_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'

_cell_length_a                   10.082(3)
_cell_length_b                   20.2060(11)
_cell_length_c                   20.535(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 129.27(4)
_cell_angle_gamma                90.00
_cell_volume                     3238.3(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4648
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      28.0820
_cell_measurement_theta_min      2.2800
_exptl_absorpt_coefficient_mu    3.930
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49701
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    2.062
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       monoclinic
_exptl_crystal_F_000             1964
_exptl_crystal_size_max          0.255
_exptl_crystal_size_mid          0.0657
_exptl_crystal_size_min          0.0492
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0810
_diffrn_reflns_av_unetI/netI     0.1022
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            10796
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         2.22
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9987
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.867
_diffrn_measured_fraction_theta_max 0.867
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -10.00 103.00   1.00   10.70    --   26.92  77.00 -60.00  113
  2  ω    -49.00  59.00   1.00   10.70    --   26.92 -57.00  90.00  108
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0618857000
_diffrn_orient_matrix_UB_12      0.0081334000
_diffrn_orient_matrix_UB_13      0.0431688000
_diffrn_orient_matrix_UB_21      -0.0106410000
_diffrn_orient_matrix_UB_22      0.0340752000
_diffrn_orient_matrix_UB_23      -0.0107081000
_diffrn_orient_matrix_UB_31      -0.0654832000
_diffrn_orient_matrix_UB_32      0.0022928000
_diffrn_orient_matrix_UB_33      0.0035476000
_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'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                5412
_reflns_number_total             7015
_reflns_odcompleteness_completeness 98.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         5.143
_refine_diff_density_min         -7.347
_refine_diff_density_rms         0.595
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     261
_refine_ls_number_reflns         7015
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1091
_refine_ls_R_factor_gt           0.0892
_refine_ls_restrained_S_all      1.082
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2540
_refine_ls_wR_factor_ref         0.2922
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_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:
 O1AA(H1AA,H1AB), O2AA(H2AA,H2AB)
2.b Rotating group:
 O20(H20A,H20B), O28(H28A,H28B), O32(H32A,H32B)
2.c Aromatic/amide H refined with riding coordinates:
 C75(H75), C20(H20), C65(H65), C83(H83), C107(H107), C111(H111), C5AA(H5AA),
 C10(H10), C5(H5), C6(H6), C4AA(H4AA)
2.d X=CH2 refined with riding coordinates:
 C1(H1A,H1B)
2.e Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C9(H9A,H9B,H9C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
Eu1 Eu 0.24864(6) 0.45453(2) 0.68044(3) 0.0115(2) Uani 1 d . . .
Eu2 Eu 0.72115(6) 0.36782(3) 0.82642(3) 0.0122(2) Uani 1 d . . .
O12 O 0.2726(11) 0.4434(4) 0.5711(5) 0.0193(17) Uiso 1 d . . .
O18 O 0.2418(10) 0.3362(4) 0.6681(4) 0.0149(16) Uiso 1 d . . .
O20 O 0.1116(11) 0.5531(4) 0.6005(5) 0.0223(18) Uiso 1 d . . .
H20A H 0.0577 0.5711 0.6152 0.033 Uiso 1 d . . GR
H20B H 0.0413 0.5436 0.5483 0.033 Uiso 1 d . . GR
O28 O 0.2121(11) 0.5297(4) 0.7599(5) 0.0214(17) Uiso 1 d . . .
H28A H 0.3096 0.5372 0.8090 0.032 Uiso 1 d . . GR
H28B H 0.1429 0.5125 0.7666 0.032 Uiso 1 d . . GR
O32 O 0.7714(13) 0.2853(5) 0.7609(6) 0.032(2) Uiso 1 d . . .
H32A H 0.6833 0.2593 0.7304 0.049 Uiso 1 d . . GR
H32B H 0.8602 0.2617 0.7986 0.049 Uiso 1 d . . GR
O35 O 0.5236(10) 0.4074(4) 0.6867(4) 0.0165(16) Uiso 1 d . . .
O41 O 0.4743(11) 0.5365(4) 0.7396(5) 0.0204(17) Uiso 1 d . . .
O45 O 1.0195(11) 0.3954(4) 0.9471(5) 0.0235(18) Uiso 1 d . . .
O49 O 0.4981(11) 0.2882(4) 0.7685(5) 0.0213(17) Uiso 1 d . . .
O52 O 1.4570(10) 0.4128(4) 0.8197(4) 0.0150(15) Uiso 1 d . . .
O59 O 1.0076(10) 0.4158(4) 0.6741(4) 0.0174(16) Uiso 1 d . . .
O73 O -0.0507(10) 0.4232(4) 0.5513(5) 0.0166(16) Uiso 1 d . . .
C75 C 0.6475(16) 0.6611(5) 0.7928(7) 0.019(2) Uiso 1 d . . .
H75 H 0.5293 0.6623 0.7505 0.023 Uiso 1 calc . . R
C0AA C 0.7287(13) 0.6019(6) 0.8244(6) 0.014(2) Uiso 1 d . . .
O16 O 1.7104(10) 0.3918(4) 0.9410(4) 0.0168(16) Uiso 1 d . . .
C20 C 0.6628(14) 0.4111(5) 0.5997(7) 0.016(2) Uiso 1 d . . .
H20 H 0.7439 0.4071 0.6579 0.019 Uiso 1 calc . . R
N25 N 1.5353(13) 0.4242(5) 1.0749(6) 0.021(2) Uiso 1 d . . .
C2AA C 0.3390(13) 0.2885(5) 0.7062(6) 0.0104(19) Uiso 1 d . . .
C C 0.6340(14) 0.5354(5) 0.7979(6) 0.012(2) Uiso 1 d . . .
C38 C 1.5554(14) 0.4070(5) 0.8981(6) 0.013(2) Uiso 1 d . . .
C43 C 0.4850(15) 0.4158(6) 0.5597(7) 0.016(2) Uiso 1 d . . .
C51 C 1.4822(14) 0.4146(5) 0.9426(6) 0.015(2) Uiso 1 d . . .
C55 C 0.8986(14) 0.4170(5) 0.5929(6) 0.016(2) Uiso 1 d . . .
C59 C 1.0588(13) 0.4069(5) 0.9006(6) 0.012(2) Uiso 1 d . . .
C65 C 1.3037(14) 0.4133(5) 0.8978(7) 0.017(2) Uiso 1 d . . .
H65 H 1.2273 0.4112 0.8394 0.020 Uiso 1 calc . . R
C76 C 0.7117(14) 0.4127(5) 0.5516(6) 0.014(2) Uiso 1 d . . .
C78 C 0.4223(14) 0.4216(5) 0.6089(6) 0.016(2) Uiso 1 d . . .
N1AA N 0.4171(12) 0.4215(5) 0.4243(6) 0.0173(19) Uiso 1 d . . .
C83 C 1.3652(15) 0.4210(6) 1.0322(7) 0.019(2) Uiso 1 d . . .
H83 H 1.3248 0.4226 1.0622 0.022 Uiso 1 calc . . R
C89 C 1.2451(15) 0.4154(6) 0.9436(7) 0.018(2) Uiso 1 d . . .
C107 C 1.5911(16) 0.4200(6) 1.0312(7) 0.022(2) Uiso 1 d . . .
H107 H 1.7087 0.4207 1.0607 0.027 Uiso 1 calc . . R
C111 C 0.5832(15) 0.4161(6) 0.4639(7) 0.019(2) Uiso 1 d . . .
H111 H 0.6173 0.4143 0.4312 0.023 Uiso 1 calc . . R
N3AA N 0.9962(12) 0.6567(4) 0.9179(6) 0.0157(19) Uiso 1 d . . .
O0AA O 0.7270(10) 0.4853(4) 0.8353(5) 0.0206(18) Uiso 1 d . . .
C3 C 0.7401(14) 0.7197(6) 0.8235(6) 0.016(2) Uiso 1 d . . .
O5 O 0.9495(10) 0.4101(4) 0.8208(5) 0.0197(17) Uiso 1 d . . .
O6 O 0.8362(12) 0.2736(4) 0.9207(5) 0.027(2) Uiso 1 d . . .
C5AA C 0.9061(14) 0.6010(5) 0.8891(6) 0.016(2) Uiso 1 d . . .
H5AA H 0.9618 0.5608 0.9123 0.019 Uiso 1 calc . . R
C10 C 0.9166(14) 0.7162(5) 0.8866(6) 0.013(2) Uiso 1 d . . .
H10 H 0.9809 0.7549 0.9075 0.016 Uiso 1 calc . . R
C1 C 0.8155(12) 0.1820(5) 0.8542(6) 0.0073(18) Uiso 1 d . . .
H1A H 0.7825 0.2043 0.8063 0.009 Uiso 1 calc . . R
H1B H 0.8269 0.1362 0.8572 0.009 Uiso 1 calc . . R
C5 C 0.3719(14) 0.4236(5) 0.4719(6) 0.016(2) Uiso 1 d . . .
H5 H 0.2568 0.4308 0.4455 0.019 Uiso 1 calc . . R
C6 C 0.8440(18) 0.2128(7) 0.9127(9) 0.033(3) Uiso 1 d . . .
H6 H 0.8765 0.1872 0.9584 0.039 Uiso 1 calc . . R
O1AA O -0.0841(12) 0.5400(5) 0.7458(6) 0.028(2) Uani 1 d . . .
H1AA H 0.0051 0.5511 0.7524 0.043 Uiso 1 d . . G
H1AB H -0.0830 0.4985 0.7526 0.043 Uiso 1 d . . G
O2AA O 0.9728(12) 0.2838(5) 0.7169(6) 0.032(2) Uani 1 d . . .
H2AA H 1.0290 0.3155 0.7175 0.048 Uiso 1 d . . G
H2AB H 0.8818 0.2773 0.6668 0.048 Uiso 1 d . . G
O1 O 0.7107(12) 0.2393(5) 0.5539(7) 0.042(3) Uani 1 d . . .
N2 N 0.4227(15) 0.2520(6) 0.4700(8) 0.042(3) Uani 1 d . . .
C4AA C 0.574(3) 0.2470(9) 0.5407(13) 0.067(6) Uani 1 d . . .
H4AA H 0.5818 0.2496 0.5882 0.080 Uiso 1 calc . . R
C7 C 0.255(2) 0.2614(9) 0.4462(15) 0.074(7) Uani 1 d . . .
H7A H 0.2502 0.2395 0.4860 0.111 Uiso 1 calc . . GR
H7B H 0.1700 0.2432 0.3912 0.111 Uiso 1 calc . . GR
H7C H 0.2346 0.3079 0.4456 0.111 Uiso 1 calc . . GR
C9 C 0.406(3) 0.2530(9) 0.3884(12) 0.073(7) Uani 1 d . . .
H9A H 0.3972 0.2980 0.3709 0.109 Uiso 1 calc . . GR
H9B H 0.3054 0.2290 0.3444 0.109 Uiso 1 calc . . GR
H9C H 0.5053 0.2327 0.4002 0.109 Uiso 1 calc . . 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
Eu1 Eu2 4.083(2) . ?
Eu1 O12 2.416(8) . ?
Eu1 O18 2.400(7) . ?
Eu1 O20 2.387(8) . ?
Eu1 O28 2.422(8) . ?
Eu1 O35 2.857(8) . ?
Eu1 O41 2.428(9) . ?
Eu1 O52 2.386(7) 1_455 ?
Eu1 O59 2.476(8) 1_455 ?
Eu1 O73 2.531(8) . ?
Eu1 C55 2.869(12) 1_455 ?
Eu1 C78 2.986(11) . ?
Eu2 O32 2.390(9) . ?
Eu2 O35 2.367(7) . ?
Eu2 O45 2.462(9) . ?
Eu2 O49 2.381(8) . ?
Eu2 O52 2.733(8) 1_455 ?
Eu2 O16 2.471(8) 1_455 ?
Eu2 C38 2.949(11) 1_455 ?
Eu2 C59 2.822(11) . ?
Eu2 O0AA 2.379(9) . ?
Eu2 O5 2.526(9) . ?
Eu2 O6 2.424(9) . ?
O12 C78 1.261(14) . ?
O18 C2AA 1.237(12) . ?
O35 C78 1.270(13) . ?
O41 C 1.259(13) . ?
O45 C59 1.266(13) . ?
O49 C2AA 1.270(13) . ?
O52 Eu1 2.386(7) 1_655 ?
O52 Eu2 2.733(8) 1_655 ?
O52 C38 1.252(12) . ?
O59 Eu1 2.476(8) 1_655 ?
O59 C55 1.291(13) . ?
O73 C55 1.249(14) 1_455 ?
C75 C0AA 1.359(15) . ?
C75 C3 1.388(16) . ?
C0AA C 1.533(15) . ?
C0AA C5AA 1.399(15) . ?
O16 Eu2 2.471(8) 1_655 ?
O16 C38 1.253(13) . ?
C20 C43 1.426(16) . ?
C20 C76 1.355(15) . ?
N25 C83 1.346(15) . ?
N25 C107 1.329(15) . ?
C2AA C3 1.525(15) 2_646 ?
C O0AA 1.258(13) . ?
C38 Eu2 2.949(11) 1_655 ?
C38 C51 1.504(15) . ?
C43 C78 1.498(15) . ?
C43 C5 1.405(14) . ?
C51 C65 1.411(15) . ?
C51 C107 1.414(15) . ?
C55 Eu1 2.869(11) 1_655 ?
C55 O73 1.249(14) 1_655 ?
C55 C76 1.501(15) . ?
C59 C89 1.496(15) . ?
C59 O5 1.271(12) . ?
C65 C89 1.391(16) . ?
C76 C111 1.405(14) . ?
N1AA C111 1.324(15) . ?
N1AA C5 1.315(14) . ?
C83 C89 1.414(15) . ?
N3AA C5AA 1.326(14) . ?
N3AA C10 1.360(13) . ?
C3 C2AA 1.525(15) 2_656 ?
C3 C10 1.390(14) . ?
O6 C6 1.248(16) . ?
C1 C6 1.216(16) . ?
O1 C4AA 1.24(2) . ?
N2 C4AA 1.28(2) . ?
N2 C7 1.44(2) . ?
N2 C9 1.57(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
O12 Eu1 Eu2 83.4(2) . . ?
O12 Eu1 O28 146.3(3) . . ?
O12 Eu1 O35 49.1(2) . . ?
O12 Eu1 O41 85.2(3) . . ?
O12 Eu1 O59 126.4(3) . 1_455 ?
O12 Eu1 O73 76.0(3) . . ?
O12 Eu1 C55 101.5(3) . 1_455 ?
O12 Eu1 C78 24.2(3) . . ?
O18 Eu1 Eu2 65.95(19) . . ?
O18 Eu1 O12 79.8(3) . . ?
O18 Eu1 O28 133.6(3) . . ?
O18 Eu1 O35 68.6(2) . . ?
O18 Eu1 O41 133.4(3) . . ?
O18 Eu1 O59 73.6(3) . 1_455 ?
O18 Eu1 O73 72.8(3) . . ?
O18 Eu1 C55 74.2(3) . 1_455 ?
O18 Eu1 C78 73.3(3) . . ?
O20 Eu1 Eu2 139.6(2) . . ?
O20 Eu1 O12 78.1(3) . . ?
O20 Eu1 O18 142.4(3) . . ?
O20 Eu1 O28 70.8(3) . . ?
O20 Eu1 O35 115.6(3) . . ?
O20 Eu1 O41 74.1(3) . . ?
O20 Eu1 O52 143.7(3) . 1_455 ?
O20 Eu1 O59 96.1(3) . 1_455 ?
O20 Eu1 O73 72.6(3) . . ?
O20 Eu1 C55 81.0(3) . 1_455 ?
O20 Eu1 C78 96.4(3) . . ?
O28 Eu1 Eu2 112.3(2) . . ?
O28 Eu1 O35 137.4(3) . . ?
O28 Eu1 O41 74.3(3) . . ?
O28 Eu1 O59 70.8(3) . 1_455 ?
O28 Eu1 O73 105.9(3) . . ?
O28 Eu1 C55 86.4(3) . 1_455 ?
O28 Eu1 C78 149.0(3) . . ?
O35 Eu1 Eu2 34.49(15) . . ?
O35 Eu1 C55 135.5(3) . 1_455 ?
O35 Eu1 C78 25.0(2) . . ?
O41 Eu1 Eu2 68.7(2) . . ?
O41 Eu1 O35 68.3(3) . . ?
O41 Eu1 O59 145.0(3) . 1_455 ?
O41 Eu1 O73 144.4(3) . . ?
O41 Eu1 C55 152.3(3) . 1_455 ?
O41 Eu1 C78 75.1(3) . . ?
O52 Eu1 Eu2 40.15(19) 1_455 . ?
O52 Eu1 O12 123.4(3) 1_455 . ?
O52 Eu1 O18 73.7(2) 1_455 . ?
O52 Eu1 O28 79.0(3) 1_455 . ?
O52 Eu1 O35 74.6(2) 1_455 . ?
O52 Eu1 O41 78.8(3) 1_455 . ?
O52 Eu1 O59 92.4(3) 1_455 1_455 ?
O52 Eu1 O73 136.7(3) 1_455 . ?
O52 Eu1 C55 117.2(3) 1_455 1_455 ?
O52 Eu1 C78 99.5(3) 1_455 . ?
O59 Eu1 Eu2 123.58(18) 1_455 . ?
O59 Eu1 O35 142.1(3) 1_455 . ?
O59 Eu1 O73 52.1(2) 1_455 . ?
O59 Eu1 C55 26.7(3) 1_455 1_455 ?
O59 Eu1 C78 139.9(3) 1_455 . ?
O73 Eu1 Eu2 136.46(18) . . ?
O73 Eu1 O35 116.3(2) . . ?
O73 Eu1 C55 25.8(3) . 1_455 ?
O73 Eu1 C78 96.3(3) . . ?
C55 Eu1 Eu2 138.4(2) 1_455 . ?
C55 Eu1 C78 120.3(3) 1_455 . ?
C78 Eu1 Eu2 59.4(2) . . ?
O32 Eu2 Eu1 116.8(2) . . ?
O32 Eu2 O45 99.5(3) . . ?
O32 Eu2 O52 138.6(3) . 1_455 ?
O32 Eu2 O16 145.6(3) . 1_455 ?
O32 Eu2 C38 149.0(3) . 1_455 ?
O32 Eu2 C59 83.5(3) . . ?
O32 Eu2 O5 71.7(3) . . ?
O32 Eu2 O6 74.7(3) . . ?
O35 Eu2 Eu1 43.1(2) . . ?
O35 Eu2 O32 82.5(3) . . ?
O35 Eu2 O45 134.3(3) . . ?
O35 Eu2 O49 79.6(3) . . ?
O35 Eu2 O52 77.4(2) . 1_455 ?
O35 Eu2 O16 125.3(3) . 1_455 ?
O35 Eu2 C38 101.9(3) . 1_455 ?
O35 Eu2 C59 111.2(3) . . ?
O35 Eu2 O0AA 73.5(3) . . ?
O35 Eu2 O5 85.5(3) . . ?
O35 Eu2 O6 147.5(3) . . ?
O45 Eu2 Eu1 139.1(2) . . ?
O45 Eu2 O52 120.4(3) . 1_455 ?
O45 Eu2 O16 76.1(3) . 1_455 ?
O45 Eu2 C38 98.9(3) . 1_455 ?
O45 Eu2 C59 26.6(3) . . ?
O45 Eu2 O5 53.2(3) . . ?
O49 Eu2 Eu1 68.2(2) . . ?
O49 Eu2 O32 73.6(3) . . ?
O49 Eu2 O45 145.2(3) . . ?
O49 Eu2 O52 67.5(3) . 1_455 ?
O49 Eu2 O16 90.6(3) . 1_455 ?
O49 Eu2 C38 77.1(3) . 1_455 ?
O49 Eu2 C59 153.3(3) . . ?
O49 Eu2 O0AA 133.0(3) . . ?
O49 Eu2 O5 143.7(3) . . ?
O49 Eu2 O6 72.0(3) . . ?
O52 Eu2 Eu1 34.26(15) 1_455 . ?
O52 Eu2 C38 25.1(2) 1_455 1_455 ?
O52 Eu2 C59 137.6(3) 1_455 . ?
O16 Eu2 Eu1 83.16(18) 1_455 . ?
O16 Eu2 O52 49.8(2) 1_455 1_455 ?
O16 Eu2 C38 24.8(3) 1_455 1_455 ?
O16 Eu2 C59 101.3(3) 1_455 . ?
O16 Eu2 O5 124.6(3) 1_455 . ?
C38 Eu2 Eu1 59.0(2) 1_455 . ?
C59 Eu2 Eu1 136.4(2) . . ?
C59 Eu2 C38 121.8(3) . 1_455 ?
O0AA Eu2 Eu1 65.7(2) . . ?
O0AA Eu2 O32 137.4(3) . . ?
O0AA Eu2 O45 75.1(3) . . ?
O0AA Eu2 O52 69.4(3) . 1_455 ?
O0AA Eu2 O16 75.3(3) . 1_455 ?
O0AA Eu2 C38 71.9(3) . 1_455 ?
O0AA Eu2 C59 73.5(3) . . ?
O0AA Eu2 O5 71.7(3) . . ?
O0AA Eu2 O6 138.3(3) . . ?
O5 Eu2 Eu1 119.67(18) . . ?
O5 Eu2 O52 140.6(3) . 1_455 ?
O5 Eu2 C38 138.8(3) . 1_455 ?
O5 Eu2 C59 26.8(3) . . ?
O6 Eu2 Eu1 132.0(2) . . ?
O6 Eu2 O45 73.2(3) . . ?
O6 Eu2 O52 105.0(3) . 1_455 ?
O6 Eu2 O16 71.4(3) . 1_455 ?
O6 Eu2 C38 87.0(3) . 1_455 ?
O6 Eu2 C59 89.2(3) . . ?
O6 Eu2 O5 108.3(3) . . ?
C78 O12 Eu1 104.2(7) . . ?
C2AA O18 Eu1 138.7(7) . . ?
Eu2 O35 Eu1 102.4(3) . . ?
C78 O35 Eu1 83.2(6) . . ?
C78 O35 Eu2 172.4(7) . . ?
C O41 Eu1 133.9(7) . . ?
C59 O45 Eu2 92.8(6) . . ?
C2AA O49 Eu2 133.7(7) . . ?
Eu1 O52 Eu2 105.6(3) 1_655 1_655 ?
C38 O52 Eu1 162.5(7) . 1_655 ?
C38 O52 Eu2 87.1(6) . 1_655 ?
C55 O59 Eu1 93.9(7) . 1_655 ?
C55 O73 Eu1 92.4(6) 1_455 . ?
C0AA C75 C3 120.4(11) . . ?
C75 C0AA C 123.3(10) . . ?
C75 C0AA C5AA 119.1(11) . . ?
C5AA C0AA C 117.4(10) . . ?
C38 O16 Eu2 99.5(6) . 1_655 ?
C76 C20 C43 118.9(10) . . ?
C107 N25 C83 117.8(10) . . ?
O18 C2AA O49 129.1(10) . . ?
O18 C2AA C3 117.0(9) . 2_646 ?
O49 C2AA C3 114.0(9) . 2_646 ?
O41 C C0AA 117.2(9) . . ?
O0AA C O41 127.2(10) . . ?
O0AA C C0AA 115.6(9) . . ?
O52 C38 Eu2 67.8(6) . 1_655 ?
O52 C38 O16 123.3(10) . . ?
O52 C38 C51 118.6(10) . . ?
O16 C38 Eu2 55.7(5) . 1_655 ?
O16 C38 C51 118.1(9) . . ?
C51 C38 Eu2 169.3(7) . 1_655 ?
C20 C43 C78 122.0(10) . . ?
C5 C43 C20 116.7(10) . . ?
C5 C43 C78 120.7(10) . . ?
C65 C51 C38 121.1(9) . . ?
C65 C51 C107 118.1(10) . . ?
C107 C51 C38 120.8(10) . . ?
O59 C55 Eu1 59.4(6) . 1_655 ?
O59 C55 C76 117.8(10) . . ?
O73 C55 Eu1 61.8(6) 1_655 1_655 ?
O73 C55 O59 120.1(11) 1_655 . ?
O73 C55 C76 122.1(9) 1_655 . ?
C76 C55 Eu1 167.2(8) . 1_655 ?
O45 C59 Eu2 60.6(6) . . ?
O45 C59 C89 116.8(9) . . ?
O45 C59 O5 123.5(10) . . ?
C89 C59 Eu2 170.2(7) . . ?
O5 C59 Eu2 63.5(6) . . ?
O5 C59 C89 119.7(10) . . ?
C89 C65 C51 118.1(10) . . ?
C20 C76 C55 119.7(9) . . ?
C20 C76 C111 118.0(11) . . ?
C111 C76 C55 122.0(10) . . ?
O12 C78 Eu1 51.7(6) . . ?
O12 C78 O35 123.4(10) . . ?
O12 C78 C43 117.6(9) . . ?
O35 C78 Eu1 71.8(6) . . ?
O35 C78 C43 118.9(10) . . ?
C43 C78 Eu1 168.1(8) . . ?
C5 N1AA C111 116.4(9) . . ?
N25 C83 C89 122.9(11) . . ?
C65 C89 C59 120.6(9) . . ?
C65 C89 C83 119.2(11) . . ?
C83 C89 C59 120.1(10) . . ?
N25 C107 C51 124.0(12) . . ?
N1AA C111 C76 125.0(11) . . ?
C5AA N3AA C10 120.4(10) . . ?
C O0AA Eu2 141.6(7) . . ?
C75 C3 C2AA 124.5(10) . 2_656 ?
C75 C3 C10 118.4(11) . . ?
C10 C3 C2AA 117.1(10) . 2_656 ?
C59 O5 Eu2 89.7(7) . . ?
C6 O6 Eu2 134.9(9) . . ?
N3AA C5AA C0AA 121.1(10) . . ?
N3AA C10 C3 120.6(10) . . ?
N1AA C5 C43 124.7(11) . . ?
C1 C6 O6 129.7(14) . . ?
C4AA N2 C7 134(2) . . ?
C4AA N2 C9 117.1(17) . . ?
C7 N2 C9 108.9(14) . . ?
O1 C4AA N2 128(2) . . ?

# start Validation Reply Form
_vrf_PLAT029_shelxl              
;
RESPONSE: This Alert is due to the low quality 
crystals are used for collecting single crystal X-ray data. 
;
_vrf_PLAT201_shelxl              
;
RESPONSE: This Alert is due to the low quality 
crystals are used for collecting single crystal X-ray data. 
;
_vrf_PLAT415_shelxl              
;
RESPONSE: This Alert is due to the presence of
residual electron density due to heavy metal atoms 
after refinement of structure. 
;
_vrf_PLAT098_shelxl              
;
RESPONSE: This Alert is due to the presence of
residual electron density due to heavy metal atoms 
after refinement of structure. 
;
# end Validation Reply Form


_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 1.539
_oxdiff_exptl_absorpt_empirical_full_min 0.728
####################################################################### 
# 
# 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_m3_rt_mo
_audit_block_doi                 10.5517/ccdc.csd.cc200103
_database_code_depnum_ccdc_archive 'CCDC 1847073'
_audit_update_record             
;
2018-06-04 deposited with the CCDC.
2018-08-06 downloaded from the CCDC.
;
_audit_creation_date             2018-03-15
_audit_creation_method           
;
Olex2 1.2-ac21
(compiled 2015.09.16 svn.r134, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C21 H13 Gd2 N3 O14, 1.33(H2 O)'
_chemical_formula_sum            'C21 H15.67 Gd2 N3 O15.33'
_chemical_formula_weight         869.87
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C189 H126 Gd18 N27 O141'
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'
Gd Gd -0.1653 3.9035 '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'

_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_H-M_alt        'R 3'
_space_group_name_Hall           'R 3'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-y, x-y, z'
3 '-x+y, -x, z'
4 'x+2/3, y+1/3, z+1/3'
5 '-y+2/3, x-y+1/3, z+1/3'
6 '-x+y+2/3, -x+1/3, z+1/3'
7 'x+1/3, y+2/3, z+2/3'
8 '-y+1/3, x-y+2/3, z+2/3'
9 '-x+y+1/3, -x+2/3, z+2/3'

_cell_length_a                   19.5746(2)
_cell_length_b                   19.5746(2)
_cell_length_c                   21.7740(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     7225.27(15)
_cell_formula_units_Z            9
_cell_measurement_reflns_used    3965
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.1330
_cell_measurement_theta_min      2.2170
_exptl_absorpt_coefficient_mu    4.161
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71351
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.799
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       trigonal
_exptl_crystal_F_000             3720
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-14 10 26 0.0582
14 -10 -26 0.0582
16 -3 25 0.0512
22 -20 15 0.0478
16 -27 0 0.0523
-15 3 25 0.0618
15 -3 -25 0.0618
-12 11 27 0.0584
9 18 2 0.0290
-14 -14 1 0.0403
3 -22 15 0.0559
11 15 11 0.0267
-16 3 -25 0.0512
22 -5 17 0.0484
-10 19 -22 0.0377
-27 15 9 0.0717
-7 22 18 0.0360

_exptl_crystal_size_max          0.142
_exptl_crystal_size_mid          0.113
_exptl_crystal_size_min          0.081
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
-13.9983 9.9618 25.9749 0.1329 0.5363 0.8273
13.9983 -9.9618 -25.9749 -0.1329 -0.5363 -0.8273
15.9684 -3.0052 25.0033 0.2350 0.9800 -0.1618
21.9570 -19.9728 15.0128 0.6719 0.5501 -0.5082
15.9662 -26.9562 0.0138 0.8176 -0.1125 -0.5327
-15.0022 2.9712 24.9740 0.3963 0.3598 0.8409
15.0022 -2.9712 -24.9740 -0.3963 -0.3598 -0.8409
-11.9997 10.9608 26.9764 0.0831 0.6278 0.7777
9.0055 17.9794 2.0087 -0.7651 0.5899 -0.2501
-14.0004 -13.9892 0.9853 0.7154 -0.5561 0.4564
2.9706 -21.9798 14.9945 0.9847 0.0673 0.1027
10.9956 14.9781 11.0062 -0.5611 0.8196 -0.1884
-15.9684 3.0052 -25.0033 -0.2350 -0.9800 0.1618
21.9673 -4.9940 17.0127 0.1324 0.8742 -0.4702
-9.9627 18.9850 -21.9981 -0.8743 -0.4704 0.0213
-26.9727 14.9603 8.9708 -0.1120 -0.1263 1.0075
-6.9892 21.9550 17.9861 -0.5098 0.7074 0.4956

_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0162
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4567
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         27.96
_diffrn_reflns_theta_min         2.08
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9974
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.895
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -24.00  97.00   1.00   66.00    --   26.84  19.00 -90.00  121
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0125001000
_diffrn_orient_matrix_UB_12      -0.0377262000
_diffrn_orient_matrix_UB_13      0.0128484000
_diffrn_orient_matrix_UB_21      0.0234911000
_diffrn_orient_matrix_UB_22      0.0180993000
_diffrn_orient_matrix_UB_23      0.0263664000
_diffrn_orient_matrix_UB_31      -0.0322606000
_diffrn_orient_matrix_UB_32      0.0006620000
_diffrn_orient_matrix_UB_33      0.0142115000
_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'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                3877
_reflns_number_total             3893
_reflns_odcompleteness_completeness 98.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.351
_refine_diff_density_min         -2.554
_refine_diff_density_rms         0.250
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(3)
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         3893
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0424
_refine_ls_restrained_S_all      1.096
_refine_ls_shift/su_max          4.556
_refine_ls_shift/su_mean         0.155
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0882P)²+104.8366P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1257
_refine_ls_wR_factor_ref         0.1258
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: H1A(0.33333) H1B(0.33333)
3.a Free rotating group:
 O1(H1A,H1B), O0AA(H0AA,H0AB)
3.b Rotating group:
 O39(H39A,H39B), O40(H40A,H40B)
3.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C20(H20), C8(H8), C16(H16), C18(H18), C4(H4), C32(H32), C28(H28),
 C30(H30)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Gd1 Gd 0.86633(3) 0.73002(3) 0.60476(2) 0.01097(15) Uani 1 d . . 1 . . .
Gd2 Gd 0.80438(3) 0.60992(3) 0.423672(19) 0.01080(15) Uani 1 d . . 1 . . .
O11 O 0.8181(6) 0.7853(6) 0.5349(5) 0.026(2) Uani 1 d . . 1 . . .
O14 O 0.9586(6) 0.7729(6) 0.5240(5) 0.025(2) Uani 1 d . . 1 . . .
O10 O 0.7941(7) 0.7192(6) 0.4479(6) 0.035(3) Uani 1 d . . 1 . . .
O26 O 0.7044(6) 0.5611(7) 0.4962(6) 0.040(3) Uani 1 d . . 1 . . .
O13 O 0.9379(6) 0.7026(6) 0.4395(6) 0.033(3) Uani 1 d . . 1 . . .
O25 O 0.7355(5) 0.6295(6) 0.5853(6) 0.030(2) Uani 1 d . . 1 . . .
O23 O 0.8374(7) 0.5434(7) 0.4989(6) 0.036(3) Uani 1 d . . 1 . . .
O22 O 0.8774(8) 0.6173(7) 0.5833(6) 0.036(3) Uani 1 d . . 1 . . .
O38 O 0.9855(5) 0.7608(6) 0.6569(6) 0.029(2) Uani 1 d . . 1 . . .
C12 C 0.9802(7) 0.7599(7) 0.4739(7) 0.019(3) Uani 1 d . . 1 . . .
C24 C 0.6922(7) 0.5741(8) 0.5516(7) 0.023(3) Uani 1 d . . 1 . . .
O34 O 0.6866(7) 0.5859(6) 0.3694(7) 0.045(3) Uani 1 d . . 1 . . .
C19 C 0.6106(7) 0.5134(7) 0.5758(6) 0.018(2) Uani 1 d . . 1 . . .
N3 N 0.8181(6) 0.6437(7) 0.7071(6) 0.024(2) Uani 1 d . . 1 . . .
C9 C 0.7945(8) 0.7713(8) 0.4798(8) 0.026(3) Uani 1 d . . 1 . . .
N15 N 0.8507(7) 0.6969(8) 0.3199(6) 0.027(2) Uani 1 d . . 1 . . .
C7 C 1.0602(8) 0.8166(7) 0.4515(7) 0.022(3) Uani 1 d . . 1 . . .
C5 C 0.7644(8) 0.8222(8) 0.4528(6) 0.018(2) Uani 1 d . . 1 . . .
C17 C 0.4925(8) 0.3886(8) 0.5769(7) 0.028(3) Uani 1 d . . 1 . . .
O39 O 0.8029(7) 0.7793(7) 0.6696(5) 0.040(3) Uani 1 d . . 1 . . .
H39A H 0.7741 0.8142 0.6493 0.060 Uiso 1 d . . 1 GR . .
H39B H 0.8376 0.8241 0.7083 0.060 Uiso 1 d . . 1 GR . .
C6 C 1.1057(7) 0.8886(7) 0.4788(6) 0.017(2) Uani 1 d . . 1 . . .
H6 H 1.0885 0.9015 0.5144 0.020 Uiso 1 calc . . 1 R . .
C20 C 0.7989(9) 0.7151(9) 0.2949(8) 0.029(3) Uani 1 d . . 1 . . .
H20 H 0.7491 0.6954 0.3122 0.035 Uiso 1 calc . . 1 R . .
C8 C 1.0898(8) 0.8010(8) 0.4001(6) 0.022(3) Uani 1 d . . 1 . . .
H8 H 1.0584 0.7523 0.3816 0.027 Uiso 1 calc . . 1 R . .
C16 C 0.4713(9) 0.4129(8) 0.6268(8) 0.035(4) Uani 1 d . . 1 . . .
H16 H 0.4231 0.3777 0.6445 0.042 Uiso 1 calc . . 1 R . .
C18 C 0.5625(8) 0.4408(9) 0.5483(7) 0.027(3) Uani 1 d . . 1 . . .
H18 H 0.5770 0.4277 0.5114 0.032 Uiso 1 calc . . 1 R . .
C4 C 0.7180(8) 0.7986(7) 0.3986(6) 0.020(3) Uani 1 d . . 1 . . .
H4 H 0.7072 0.7516 0.3798 0.025 Uiso 1 calc . . 1 R . .
O35 O 0.7010(6) 0.4819(6) 0.3820(6) 0.041(3) Uani 1 d . . 1 . . .
C32 C 0.5240(8) 0.4914(8) 0.3430(6) 0.030(3) Uani 1 d . . 1 . . .
H32 H 0.5474 0.5445 0.3325 0.036 Uiso 1 calc . . 1 R . .
C27 C 0.5706(8) 0.4590(8) 0.3600(6) 0.028(3) Uani 1 d . . 1 . . .
C31 C 1.1122(8) 0.7791(7) 0.6751(7) 0.027(3) Uani 1 d . . 1 . . .
C28 C 0.5350(8) 0.3833(9) 0.3735(7) 0.034(3) Uani 1 d . . 1 . . .
H28 H 0.5661 0.3620 0.3855 0.041 Uiso 1 calc . . 1 R . .
C33 C 0.6589(8) 0.5150(9) 0.3699(6) 0.031(3) Uani 1 d . . 1 . . .
C36 C 1.0583(8) 0.8100(8) 0.6554(7) 0.034(3) Uani 1 d . . 1 . . .
C30 C 1.0825(9) 0.7020(9) 0.6890(8) 0.037(3) Uani 1 d . . 1 . . .
H30 H 1.0280 0.6702 0.6873 0.044 Uiso 1 calc . . 1 R . .
N29 N 1.1217(8) 0.6675(6) 0.7043(7) 0.033(3) Uani 1 d . . 1 . . .
O37 O 1.0861(7) 0.8812(6) 0.6435(7) 0.055(4) Uani 1 d . . 1 . . .
C21 C 0.8677(8) 0.5594(8) 0.5496(7) 0.020(3) Uani 1 d . . 1 . . .
O40 O 0.9467(6) 0.8760(6) 0.6113(5) 0.038(2) Uani 1 d . . 1 . . .
H40A H 0.9181 0.9016 0.6254 0.057 Uiso 1 d . . 1 GR . .
H40B H 0.9697 0.9017 0.5726 0.057 Uiso 1 d . . 1 GR . .
O1 O 1.0000 1.0000 0.515(2) 0.096(10) Uiso 1 d . . 3 S T P
H1A H 0.9752 1.0249 0.5204 0.144 Uiso 0.33 d . . 1 G . .
H1B H 1.0158 1.0057 0.4780 0.144 Uiso 0.33 d . . 1 G . .
O0AA O 0.5919(18) 0.640(2) 0.4446(18) 0.153(10) Uiso 1 d . . 1 . . .
H0AA H 0.5860 0.6165 0.4787 0.230 Uiso 1 d . . 1 G . .
H0AB H 0.5776 0.6743 0.4484 0.230 Uiso 1 d . . 1 G . .


_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 O11 2.324(10) . ?
Gd1 O14 2.354(10) . ?
Gd1 O25 2.360(9) . ?
Gd1 O22 2.368(10) . ?
Gd1 O38 2.385(9) . ?
Gd1 N3 2.667(11) . ?
Gd1 O39 2.379(9) . ?
Gd1 O40 2.483(10) . ?
Gd2 O10 2.308(10) . ?
Gd2 O26 2.317(10) . ?
Gd2 O13 2.345(10) . ?
Gd2 O23 2.374(10) . ?
Gd2 O34 2.418(11) . ?
Gd2 N15 2.699(13) . ?
Gd2 O35 2.475(10) . ?
Gd2 C33 2.765(14) . ?
Gd2 N29 2.633(12) 9_664 ?
O11 C9 1.27(2) . ?
O14 C12 1.241(18) . ?
O10 C9 1.229(18) . ?
O26 C24 1.281(19) . ?
O13 C12 1.256(17) . ?
O25 C24 1.230(17) . ?
O23 C21 1.217(19) . ?
O22 C21 1.283(17) . ?
O38 C36 1.261(16) . ?
C12 C7 1.478(17) . ?
C24 C19 1.530(16) . ?
O34 C33 1.211(19) . ?
C19 C20 1.411(19) 6_565 ?
C19 C18 1.388(18) . ?
N3 C8 1.331(17) 5_655 ?
N3 C4 1.324(16) 6_565 ?
C9 C5 1.508(17) . ?
N15 C20 1.346(18) . ?
N15 C16 1.322(18) 8_654 ?
C7 C6 1.371(16) . ?
C7 C8 1.36(2) . ?
C5 C6 1.389(17) 3_675 ?
C5 C4 1.418(18) . ?
C17 C16 1.33(2) . ?
C17 C18 1.382(19) . ?
C17 C21 1.502(16) 2_655 ?
O39 H39A 1.1680 . ?
O39 H39B 1.1616 . ?
C6 C5 1.389(17) 2_765 ?
C6 H6 0.9300 . ?
C20 C19 1.411(19) 8_654 ?
C20 H20 0.9300 . ?
C8 N3 1.331(17) 9_664 ?
C8 H8 0.9300 . ?
C16 N15 1.322(18) 6_565 ?
C16 H16 0.9300 . ?
C18 H18 0.9300 . ?
C4 N3 1.324(16) 8_654 ?
C4 H4 0.9300 . ?
O35 C33 1.306(17) . ?
C32 H32 0.9300 . ?
C32 C27 1.398(18) . ?
C32 C31 1.337(19) 7_444 ?
C27 C28 1.32(2) . ?
C27 C33 1.529(19) . ?
C31 C32 1.337(19) 4 ?
C31 C36 1.516(17) . ?
C31 C30 1.353(19) . ?
C28 H28 0.9300 . ?
C28 N29 1.369(19) 7_444 ?
C36 O37 1.245(18) . ?
C30 H30 0.9300 . ?
C30 N29 1.292(19) . ?
N29 Gd2 2.633(12) 5_655 ?
N29 C28 1.369(19) 4 ?
C21 C17 1.502(16) 3_665 ?
O40 H40A 0.9700 . ?
O40 H40B 0.9682 . ?
O1 H1A 0.8501 . ?
O1 H1B 0.8498 . ?
O0AA H0AA 0.8501 . ?
O0AA H0AB 0.8501 . ?

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
O11 Gd1 O14 76.3(4) . . ?
O11 Gd1 O25 75.3(4) . . ?
O11 Gd1 O22 123.5(4) . . ?
O11 Gd1 O38 140.2(4) . . ?
O11 Gd1 N3 138.1(4) . . ?
O11 Gd1 O39 77.5(4) . . ?
O11 Gd1 O40 70.9(4) . . ?
O14 Gd1 O25 118.8(4) . . ?
O14 Gd1 O22 76.9(4) . . ?
O14 Gd1 O38 77.7(4) . . ?
O14 Gd1 N3 144.6(4) . . ?
O14 Gd1 O39 139.6(4) . . ?
O14 Gd1 O40 72.6(4) . . ?
O25 Gd1 O22 75.8(4) . . ?
O25 Gd1 O38 144.3(4) . . ?
O25 Gd1 N3 74.3(4) . . ?
O25 Gd1 O39 82.9(4) . . ?
O25 Gd1 O40 140.2(4) . . ?
O22 Gd1 O38 78.2(4) . . ?
O22 Gd1 N3 75.1(4) . . ?
O22 Gd1 O39 143.5(4) . . ?
O22 Gd1 O40 141.5(4) . . ?
O38 Gd1 N3 75.8(3) . . ?
O38 Gd1 O40 72.9(4) . . ?
O39 Gd1 O38 105.0(4) . . ?
O39 Gd1 N3 70.7(4) . . ?
O39 Gd1 O40 70.0(4) . . ?
O40 Gd1 N3 120.1(4) . . ?
O10 Gd2 O26 77.2(5) . . ?
O10 Gd2 O13 80.2(4) . . ?
O10 Gd2 O23 121.6(4) . . ?
O10 Gd2 O34 77.0(4) . . ?
O10 Gd2 N15 76.4(4) . . ?
O10 Gd2 O35 128.0(4) . . ?
O10 Gd2 C33 100.5(4) . . ?
O10 Gd2 N29 151.0(4) . 9_664 ?
O26 Gd2 O13 127.2(4) . . ?
O26 Gd2 O23 73.1(4) . . ?
O26 Gd2 O34 74.1(5) . . ?
O26 Gd2 N15 141.1(4) . . ?
O26 Gd2 O35 74.8(4) . . ?
O26 Gd2 C33 68.7(4) . . ?
O26 Gd2 N29 131.0(4) . 9_664 ?
O13 Gd2 O23 79.5(4) . . ?
O13 Gd2 O34 143.9(4) . . ?
O13 Gd2 N15 75.1(4) . . ?
O13 Gd2 O35 150.2(4) . . ?
O13 Gd2 C33 163.2(4) . . ?
O13 Gd2 N29 76.3(4) . 9_664 ?
O23 Gd2 O34 136.5(4) . . ?
O23 Gd2 N15 145.7(4) . . ?
O23 Gd2 O35 90.4(4) . . ?
O23 Gd2 C33 113.3(4) . . ?
O23 Gd2 N29 70.5(4) . 9_664 ?
O34 Gd2 N15 72.5(4) . . ?
O34 Gd2 O35 53.6(4) . . ?
O34 Gd2 C33 25.9(4) . . ?
O34 Gd2 N29 113.5(5) . 9_664 ?
N15 Gd2 C33 88.7(4) . . ?
O35 Gd2 N15 100.3(4) . . ?
O35 Gd2 C33 28.2(4) . . ?
O35 Gd2 N29 73.9(4) . 9_664 ?
N29 Gd2 N15 81.2(4) 9_664 . ?
N29 Gd2 C33 97.2(4) 9_664 . ?
C9 O11 Gd1 135.1(9) . . ?
C12 O14 Gd1 149.6(9) . . ?
C9 O10 Gd2 158.5(11) . . ?
C24 O26 Gd2 139.8(10) . . ?
C12 O13 Gd2 139.5(10) . . ?
C24 O25 Gd1 145.6(10) . . ?
C21 O23 Gd2 135.7(10) . . ?
C21 O22 Gd1 153.5(10) . . ?
C36 O38 Gd1 140.3(9) . . ?
O14 C12 O13 124.6(12) . . ?
O14 C12 C7 118.6(13) . . ?
O13 C12 C7 116.8(13) . . ?
O26 C24 C19 113.3(12) . . ?
O25 C24 O26 128.4(12) . . ?
O25 C24 C19 118.2(13) . . ?
C33 O34 Gd2 93.2(9) . . ?
C20 C19 C24 117.1(12) 6_565 . ?
C18 C19 C24 123.8(12) . . ?
C18 C19 C20 119.0(12) . 6_565 ?
C8 N3 Gd1 118.7(8) 5_655 . ?
C4 N3 Gd1 124.9(8) 6_565 . ?
C4 N3 C8 116.2(11) 6_565 5_655 ?
O11 C9 C5 116.5(12) . . ?
O10 C9 O11 124.4(13) . . ?
O10 C9 C5 119.1(14) . . ?
C20 N15 Gd2 116.5(9) . . ?
C16 N15 Gd2 125.4(9) 8_654 . ?
C16 N15 C20 118.1(13) 8_654 . ?
C6 C7 C12 121.9(13) . . ?
C8 C7 C12 120.9(12) . . ?
C8 C7 C6 117.1(12) . . ?
C6 C5 C9 121.5(12) 3_675 . ?
C6 C5 C4 118.1(11) 3_675 . ?
C4 C5 C9 120.4(12) . . ?
C16 C17 C18 118.3(12) . . ?
C16 C17 C21 121.8(12) . 2_655 ?
C18 C17 C21 119.8(12) . 2_655 ?
Gd1 O39 H39A 121.0 . . ?
Gd1 O39 H39B 120.8 . . ?
H39A O39 H39B 95.9 . . ?
C7 C6 C5 119.4(12) . 2_765 ?
C7 C6 H6 120.3 . . ?
C5 C6 H6 120.3 2_765 . ?
C19 C20 H20 120.0 8_654 . ?
N15 C20 C19 120.2(13) . 8_654 ?
N15 C20 H20 119.8 . . ?
N3 C8 C7 126.6(12) 9_664 . ?
N3 C8 H8 116.8 9_664 . ?
C7 C8 H8 116.6 . . ?
N15 C16 C17 125.7(13) 6_565 . ?
N15 C16 H16 117.1 6_565 . ?
C17 C16 H16 117.2 . . ?
C19 C18 H18 120.8 . . ?
C17 C18 C19 118.5(13) . . ?
C17 C18 H18 120.7 . . ?
N3 C4 C5 122.4(11) 8_654 . ?
N3 C4 H4 118.8 8_654 . ?
C5 C4 H4 118.7 . . ?
C33 O35 Gd2 88.4(8) . . ?
C27 C32 H32 120.1 . . ?
C31 C32 H32 120.3 7_444 . ?
C31 C32 C27 119.6(13) 7_444 . ?
C32 C27 C33 118.1(13) . . ?
C28 C27 C32 118.2(13) . . ?
C28 C27 C33 123.2(13) . . ?
C32 C31 C36 122.3(12) 4 . ?
C32 C31 C30 116.8(12) 4 . ?
C30 C31 C36 120.9(12) . . ?
C27 C28 H28 118.1 . . ?
C27 C28 N29 123.9(14) . 7_444 ?
N29 C28 H28 118.0 7_444 . ?
O34 C33 Gd2 60.9(8) . . ?
O34 C33 O35 122.5(13) . . ?
O34 C33 C27 121.3(13) . . ?
O35 C33 Gd2 63.5(7) . . ?
O35 C33 C27 116.1(13) . . ?
C27 C33 Gd2 163.0(10) . . ?
O38 C36 C31 115.7(12) . . ?
O37 C36 O38 123.7(13) . . ?
O37 C36 C31 120.3(12) . . ?
C31 C30 H30 116.5 . . ?
N29 C30 C31 127.2(14) . . ?
N29 C30 H30 116.3 . . ?
C28 N29 Gd2 120.1(10) 4 5_655 ?
C30 N29 Gd2 123.4(11) . 5_655 ?
C30 N29 C28 114.3(12) . 4 ?
O23 C21 O22 125.7(12) . . ?
O23 C21 C17 118.8(12) . 3_665 ?
O22 C21 C17 115.5(12) . 3_665 ?
Gd1 O40 H40A 114.5 . . ?
Gd1 O40 H40B 114.2 . . ?
H40A O40 H40B 104.2 . . ?
H1A O1 H1B 109.5 . . ?
H0AA O0AA H0AB 109.5 . . ?

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
Gd1 O11 C9 O10 -2(2) . . . . ?
Gd1 O11 C9 C5 177.6(8) . . . . ?
Gd1 O14 C12 O13 12(3) . . . . ?
Gd1 O14 C12 C7 -170.2(13) . . . . ?
Gd1 O25 C24 O26 -22(3) . . . . ?
Gd1 O25 C24 C19 161.3(12) . . . . ?
Gd1 O22 C21 O23 0(3) . . . . ?
Gd1 O22 C21 C17 -178.9(18) . . . 3_665 ?
Gd1 O38 C36 C31 -147.9(12) . . . . ?
Gd1 O38 C36 O37 38(3) . . . . ?
Gd2 O10 C9 O11 10(4) . . . . ?
Gd2 O10 C9 C5 -170(2) . . . . ?
Gd2 O26 C24 O25 8(3) . . . . ?
Gd2 O26 C24 C19 -175.2(11) . . . . ?
Gd2 O13 C12 O14 19(2) . . . . ?
Gd2 O13 C12 C7 -159.2(11) . . . . ?
Gd2 O23 C21 O22 15(2) . . . . ?
Gd2 O23 C21 C17 -165.6(11) . . . 3_665 ?
Gd2 O34 C33 O35 -15.9(16) . . . . ?
Gd2 O34 C33 C27 160.5(12) . . . . ?
Gd2 N15 C20 C19 176.6(12) . . . 8_654 ?
Gd2 O35 C33 O34 15.5(16) . . . . ?
Gd2 O35 C33 C27 -161.1(11) . . . . ?
O11 Gd1 O14 C12 -88.2(19) . . . . ?
O11 Gd1 O25 C24 86.7(18) . . . . ?
O11 Gd1 O22 C21 -5(3) . . . . ?
O11 Gd1 O38 C36 -14(2) . . . . ?
O11 Gd1 N3 C8 178.5(10) . . . 5_655 ?
O11 Gd1 N3 C4 3.7(15) . . . 6_565 ?
O11 C9 C5 C6 18.8(19) . . . 3_675 ?
O11 C9 C5 C4 -163.1(13) . . . . ?
O14 Gd1 O11 C9 61.1(13) . . . . ?
O14 Gd1 O25 C24 21.8(19) . . . . ?
O14 Gd1 O22 C21 -68(2) . . . . ?
O14 Gd1 O38 C36 36.4(17) . . . . ?
O14 Gd1 N3 C8 15.6(15) . . . 5_655 ?
O14 Gd1 N3 C4 -159.2(10) . . . 6_565 ?
O14 C12 C7 C6 -11(2) . . . . ?
O14 C12 C7 C8 173.1(14) . . . . ?
O10 Gd2 O26 C24 -57.1(17) . . . . ?
O10 Gd2 O13 C12 36.9(15) . . . . ?
O10 Gd2 O23 C21 -18.6(16) . . . . ?
O10 Gd2 O34 C33 -154.0(11) . . . . ?
O10 Gd2 N15 C20 -57.0(12) . . . . ?
O10 Gd2 N15 C16 120.4(15) . . . 8_654 ?
O10 Gd2 O35 C33 13.4(11) . . . . ?
O10 Gd2 C33 O34 25.7(11) . . . . ?
O10 Gd2 C33 O35 -169.3(9) . . . . ?
O10 Gd2 C33 C27 -76(3) . . . . ?
O10 C9 C5 C6 -161.8(14) . . . 3_675 ?
O10 C9 C5 C4 16(2) . . . . ?
O26 Gd2 O10 C9 59(3) . . . . ?
O26 Gd2 O13 C12 -28.7(17) . . . . ?
O26 Gd2 O23 C21 -81.3(15) . . . . ?
O26 Gd2 O34 C33 -73.9(10) . . . . ?
O26 Gd2 N15 C20 -8.6(16) . . . . ?
O26 Gd2 N15 C16 168.8(13) . . . 8_654 ?
O26 Gd2 O35 C33 73.2(9) . . . . ?
O26 Gd2 C33 O34 97.4(11) . . . . ?
O26 Gd2 C33 O35 -97.5(9) . . . . ?
O26 Gd2 C33 C27 -5(3) . . . . ?
O26 C24 C19 C20 -162.0(15) . . . 6_565 ?
O26 C24 C19 C18 16(2) . . . . ?
O13 Gd2 O10 C9 -73(3) . . . . ?
O13 Gd2 O26 C24 9.9(19) . . . . ?
O13 Gd2 O23 C21 53.0(15) . . . . ?
O13 Gd2 O34 C33 153.7(9) . . . . ?
O13 Gd2 N15 C20 -140.3(13) . . . . ?
O13 Gd2 N15 C16 37.1(14) . . . 8_654 ?
O13 Gd2 O35 C33 -145.1(9) . . . . ?
O13 Gd2 C33 O34 -65.0(19) . . . . ?
O13 Gd2 C33 O35 100.0(16) . . . . ?
O13 Gd2 C33 C27 -167(3) . . . . ?
O13 C12 C7 C6 167.2(13) . . . . ?
O13 C12 C7 C8 -9(2) . . . . ?
O25 Gd1 O11 C9 -64.1(13) . . . . ?
O25 Gd1 O14 C12 -24(2) . . . . ?
O25 Gd1 O22 C21 57(2) . . . . ?
O25 Gd1 O38 C36 159.3(15) . . . . ?
O25 Gd1 N3 C8 133.6(12) . . . 5_655 ?
O25 Gd1 N3 C4 -41.3(12) . . . 6_565 ?
O25 C24 C19 C20 15(2) . . . 6_565 ?
O25 C24 C19 C18 -166.8(14) . . . . ?
O23 Gd2 O10 C9 -1(3) . . . . ?
O23 Gd2 O26 C24 72.0(17) . . . . ?
O23 Gd2 O13 C12 -88.0(15) . . . . ?
O23 Gd2 O34 C33 -31.4(14) . . . . ?
O23 Gd2 N15 C20 176.0(11) . . . . ?
O23 Gd2 N15 C16 -6.6(18) . . . 8_654 ?
O23 Gd2 O35 C33 145.6(9) . . . . ?
O23 Gd2 C33 O34 157.0(10) . . . . ?
O23 Gd2 C33 O35 -38.0(10) . . . . ?
O23 Gd2 C33 C27 55(4) . . . . ?
O22 Gd1 O11 C9 -2.7(15) . . . . ?
O22 Gd1 O14 C12 41.7(19) . . . . ?
O22 Gd1 O25 C24 -44.2(18) . . . . ?
O22 Gd1 O38 C36 115.4(18) . . . . ?
O22 Gd1 N3 C8 54.5(11) . . . 5_655 ?
O22 Gd1 N3 C4 -120.3(12) . . . 6_565 ?
O38 Gd1 O11 C9 111.7(14) . . . . ?
O38 Gd1 O14 C12 122.2(19) . . . . ?
O38 Gd1 O25 C24 -88.6(19) . . . . ?
O38 Gd1 O22 C21 -148(2) . . . . ?
O38 Gd1 N3 C8 -26.9(11) . . . 5_655 ?
O38 Gd1 N3 C4 158.3(13) . . . 6_565 ?
C12 C7 C6 C5 -174.7(13) . . . 2_765 ?
C12 C7 C8 N3 176.6(15) . . . 9_664 ?
C24 C19 C18 C17 175.3(15) . . . . ?
O34 Gd2 O10 C9 136(3) . . . . ?
O34 Gd2 O26 C24 -137.1(17) . . . . ?
O34 Gd2 O13 C12 88.4(17) . . . . ?
O34 Gd2 O23 C21 -124.0(15) . . . . ?
O34 Gd2 N15 C20 23.4(12) . . . . ?
O34 Gd2 N15 C16 -159.1(16) . . . 8_654 ?
O34 Gd2 O35 C33 -8.1(8) . . . . ?
O34 Gd2 C33 O35 165.0(16) . . . . ?
O34 Gd2 C33 C27 -102(4) . . . . ?
N3 Gd1 O11 C9 -108.8(14) . . . . ?
N3 Gd1 O14 C12 80(2) . . . . ?
N3 Gd1 O25 C24 -122.5(19) . . . . ?
N3 Gd1 O22 C21 134(2) . . . . ?
N3 Gd1 O38 C36 -167.2(18) . . . . ?
C9 C5 C4 N3 179.2(13) . . . 8_654 ?
N15 Gd2 O10 C9 -149(3) . . . . ?
N15 Gd2 O26 C24 -105.3(17) . . . . ?
N15 Gd2 O13 C12 115.3(15) . . . . ?
N15 Gd2 O23 C21 95.7(16) . . . . ?
N15 Gd2 O34 C33 126.4(11) . . . . ?
N15 Gd2 O35 C33 -67.2(9) . . . . ?
N15 Gd2 C33 O34 -50.2(11) . . . . ?
N15 Gd2 C33 O35 114.8(9) . . . . ?
N15 Gd2 C33 C27 -152(3) . . . . ?
O39 Gd1 O11 C9 -149.9(14) . . . . ?
O39 Gd1 O14 C12 -139.1(18) . . . . ?
O39 Gd1 O25 C24 165.6(19) . . . . ?
O39 Gd1 O22 C21 113(2) . . . . ?
O39 Gd1 O38 C36 -102.0(17) . . . . ?
O39 Gd1 N3 C8 -138.6(12) . . . 5_655 ?
O39 Gd1 N3 C4 46.5(12) . . . 6_565 ?
C6 C7 C8 N3 1(2) . . . 9_664 ?
C6 C5 C4 N3 -3(2) 3_675 . . 8_654 ?
C20 C19 C18 C17 -6(2) 6_565 . . . ?
C8 C7 C6 C5 1(2) . . . 2_765 ?
C16 N15 C20 C19 -1(3) 8_654 . . 8_654 ?
C16 C17 C18 C19 6(2) . . . . ?
C18 C17 C16 N15 -2(3) . . . 6_565 ?
O35 Gd2 O10 C9 118(3) . . . . ?
O35 Gd2 O26 C24 167.2(18) . . . . ?
O35 Gd2 O13 C12 -160.1(13) . . . . ?
O35 Gd2 O23 C21 -155.3(15) . . . . ?
O35 Gd2 O34 C33 8.7(9) . . . . ?
O35 Gd2 N15 C20 69.9(13) . . . . ?
O35 Gd2 N15 C16 -112.7(14) . . . 8_654 ?
O35 Gd2 C33 O34 -165.0(16) . . . . ?
O35 Gd2 C33 C27 93(4) . . . . ?
C32 C27 C28 N29 1(2) . . . 7_444 ?
C32 C27 C33 Gd2 100(3) . . . . ?
C32 C27 C33 O34 8(2) . . . . ?
C32 C27 C33 O35 -175.8(13) . . . . ?
C32 C31 C36 O38 -179.4(15) 4 . . . ?
C32 C31 C36 O37 -5(2) 4 . . . ?
C32 C31 C30 N29 1(3) 4 . . . ?
C31 C32 C27 C28 1(2) 7_444 . . . ?
C31 C32 C27 C33 -171.3(13) 7_444 . . . ?
C31 C30 N29 Gd2 163.7(14) . . . 5_655 ?
C31 C30 N29 C28 1(3) . . . 4 ?
C28 C27 C33 Gd2 -72(4) . . . . ?
C28 C27 C33 O34 -164.4(16) . . . . ?
C28 C27 C33 O35 12(2) . . . . ?
C33 Gd2 O10 C9 124(3) . . . . ?
C33 Gd2 O26 C24 -163.8(18) . . . . ?
C33 Gd2 O13 C12 130.6(17) . . . . ?
C33 Gd2 O23 C21 -138.4(14) . . . . ?
C33 Gd2 N15 C20 44.1(13) . . . . ?
C33 Gd2 N15 C16 -138.5(15) . . . 8_654 ?
C33 C27 C28 N29 172.9(14) . . . 7_444 ?
C36 C31 C30 N29 177.5(16) . . . . ?
C30 C31 C36 O38 5(2) . . . . ?
C30 C31 C36 O37 179.0(17) . . . . ?
N29 Gd2 O10 C9 -109(3) 9_664 . . . ?
N29 Gd2 O26 C24 115.4(17) 9_664 . . . ?
N29 Gd2 O13 C12 -160.3(16) 9_664 . . . ?
N29 Gd2 O23 C21 132.0(16) 9_664 . . . ?
N29 Gd2 O34 C33 54.5(11) 9_664 . . . ?
N29 Gd2 N15 C20 141.6(13) 9_664 . . . ?
N29 Gd2 N15 C16 -41.0(15) 9_664 . . 8_654 ?
N29 Gd2 O35 C33 -144.9(10) 9_664 . . . ?
N29 Gd2 C33 O34 -131.2(11) 9_664 . . . ?
N29 Gd2 C33 O35 33.8(9) 9_664 . . . ?
N29 Gd2 C33 C27 127(3) 9_664 . . . ?
C21 C17 C16 N15 -179.2(16) 2_655 . . 6_565 ?
C21 C17 C18 C19 -177.6(14) 2_655 . . . ?
O40 Gd1 O11 C9 137.1(14) . . . . ?
O40 Gd1 O14 C12 -162(2) . . . . ?
O40 Gd1 O25 C24 119.1(18) . . . . ?
O40 Gd1 O22 C21 -106(2) . . . . ?
O40 Gd1 O38 C36 -38.9(17) . . . . ?
O40 Gd1 N3 C8 -87.0(11) . . . 5_655 ?
O40 Gd1 N3 C4 98.2(12) . . . 6_565 ?

# start Validation Reply Form
_vrf_PLAT080_shelxl              
;
RESPONSE: This Alert is due to the presence of
residual electron density due to heavy metal atoms 
after refinement of structure. 
;
_vrf_PLAT213_shelxl              
;
RESPONSE: This Alert is due to the presence of
residual electron density due to heavy metal atoms 
after refinement of structure. 
;
_vrf_PLAT602_shelxl              
;
RESPONSE: This Alert is due to the presence of
residual electron density due to heavy metal atoms 
after refinement of structure. 
;
_vrf_PLAT420_shelxl              
;
RESPONSE: This Alert is due to the presence of
residual electron density due to heavy metal atoms 
after refinement of structure. 
;
_vrf_PLAT241_shelxl              
;
RESPONSE: This Alert is due to the presence of
residual electron density due to heavy metal atoms 
after refinement of structure. 
;
_vrf_PLAT242_shelxl              
;
RESPONSE: This Alert is due to the presence of
residual electron density due to heavy metal atoms 
after refinement of structure. 
;
# end Validation Reply Form

_olex2_date_sample_data_collection 2016-12-12
_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 1.275
_oxdiff_exptl_absorpt_empirical_full_min 0.812
