# 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. 
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data_Ce_24DNB
_database_code_depnum_ccdc_archive 'CCDC 1584543'
_audit_update_record             
;
2018-02-08 deposited with the CCDC.
2018-02-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H24 Ce2 N12 O40'
_chemical_formula_sum            'C42 H24 Ce2 N12 O40'
_chemical_formula_weight         1616.97

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'
Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_H-M_alt        'C c'
_space_group_name_Hall           'C -2yc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   12.7786(18)
_cell_length_b                   47.775(7)
_cell_length_c                   9.2651(10)
_cell_angle_alpha                90
_cell_angle_beta                 92.972(5)
_cell_angle_gamma                90
_cell_volume                     5648.8(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    6258
_cell_measurement_theta_min      2.56
_cell_measurement_theta_max      27.35

_exptl_crystal_description       Needles
_exptl_crystal_colour            White
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.901
_exptl_crystal_F_000             3184
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    1.716
_shelx_estimated_absorpt_T_min   0.684
_shelx_estimated_absorpt_T_max   0.736
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.681
_exptl_absorpt_correction_T_max  0.742
_exptl_absorpt_process_details   
'SADABS-2014/2 - Bruker AXS area detector scaling and absorption correction'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            25602
_diffrn_reflns_av_unetI/netI     0.1034
_diffrn_reflns_av_R_equivalents  0.0688
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -55
_diffrn_reflns_limit_k_max       62
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.652
_diffrn_reflns_theta_max         27.791
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.841
_diffrn_reflns_point_group_measured_fraction_full 0.875
_reflns_number_total             11222
_reflns_number_gt                8916
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.697
_reflns_Friedel_fraction_max     0.692
_reflns_Friedel_fraction_full    0.753

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Sir-92 (Altomare et al., 1993)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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.All hydrogen atoms were 
fixed geometrically with their Uiso values 1.2 times of phenylene carbons. 
The hydrogen atoms of water molecules were located from the difference 
Fourier synthesis and were refined isotropically with distance of 0.82 Å 
with Uiso values 1.2 times that of their carrier oxygen atoms. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0846P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2841 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.027(16)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         11222
_refine_ls_number_parameters     883
_refine_ls_number_restraints     11
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0541
_refine_ls_wR_factor_ref         0.1451
_refine_ls_wR_factor_gt          0.1280
_refine_ls_goodness_of_fit_ref   0.901
_refine_ls_restrained_S_all      0.901
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3595(10) 0.9157(3) -0.0189(13) 0.033(3) Uani 1 1 d . . . . .
C2 C 0.4152(10) 0.9424(3) -0.0537(12) 0.032(3) Uani 1 1 d . . . . .
C3 C 0.3821(10) 0.9685(3) -0.0113(13) 0.033(3) Uani 1 1 d . . . . .
C4 C 0.4313(11) 0.9929(3) -0.0474(15) 0.041(3) Uani 1 1 d . . . . .
H4 H 0.407896 1.010109 -0.014928 0.049 Uiso 1 1 calc R U . . .
C5 C 0.5149(11) 0.9913(3) -0.1316(16) 0.046(3) Uani 1 1 d . . . . .
C6 C 0.5549(12) 0.9656(3) -0.1783(15) 0.047(3) Uani 1 1 d . . . . .
H6 H 0.613251 0.964779 -0.234251 0.056 Uiso 1 1 calc R U . . .
C7 C 0.5038(10) 0.9414(3) -0.1374(14) 0.040(3) Uani 1 1 d . . . . .
H7 H 0.528922 0.924134 -0.166187 0.049 Uiso 1 1 calc R U . . .
C8 C 0.1438(9) 0.9087(3) -0.2810(12) 0.030(2) Uani 1 1 d . . . . .
C9 C 0.0885(9) 0.9358(2) -0.2497(12) 0.029(2) Uani 1 1 d . . . . .
C10 C 0.1020(10) 0.9602(3) -0.3321(13) 0.034(3) Uani 1 1 d . . . . .
C11 C 0.0471(11) 0.9840(3) -0.3139(14) 0.038(3) Uani 1 1 d . . . . .
H11 H 0.057831 0.999625 -0.370831 0.046 Uiso 1 1 calc R U . . .
C12 C -0.0256(11) 0.9844(3) -0.2078(15) 0.041(3) Uani 1 1 d . . . . .
C13 C -0.0407(11) 0.9611(3) -0.1198(15) 0.045(3) Uani 1 1 d . . . . .
H13 H -0.087768 0.961590 -0.046635 0.054 Uiso 1 1 calc R U . . .
C14 C 0.0161(10) 0.9375(2) -0.1452(13) 0.035(3) Uani 1 1 d . . . . .
H14 H 0.005296 0.921824 -0.088701 0.042 Uiso 1 1 calc R U . . .
C15 C 0.4470(10) 0.8606(2) 0.2922(14) 0.028(3) Uani 1 1 d . . . . .
C16 C 0.5402(10) 0.8689(3) 0.2084(14) 0.034(3) Uani 1 1 d . . . . .
C17 C 0.5917(10) 0.8517(3) 0.1153(12) 0.032(3) Uani 1 1 d . . . . .
C18 C 0.6699(10) 0.8627(3) 0.0306(15) 0.036(3) Uani 1 1 d . . . . .
H18 H 0.703245 0.851353 -0.034493 0.044 Uiso 1 1 calc R U . . .
C19 C 0.6954(12) 0.8897(3) 0.0451(19) 0.046(4) Uani 1 1 d . . . . .
C20 C 0.6478(12) 0.9076(3) 0.1405(17) 0.051(4) Uani 1 1 d . . . . .
H20 H 0.668634 0.926157 0.149761 0.061 Uiso 1 1 calc R U . . .
C21 C 0.5695(11) 0.8971(3) 0.2202(16) 0.042(3) Uani 1 1 d . . . . .
H21 H 0.535366 0.908855 0.282624 0.051 Uiso 1 1 calc R U . . .
C22 C 0.3583(9) 0.8271(3) -0.2068(12) 0.030(2) Uani 1 1 d . . . . .
C23 C 0.4160(10) 0.8032(3) -0.2764(12) 0.034(3) Uani 1 1 d . . . . .
C24 C 0.5101(10) 0.8059(3) -0.3439(13) 0.039(3) Uani 1 1 d . . . . .
C25 C 0.5535(13) 0.7846(5) -0.4203(16) 0.068(6) Uani 1 1 d . . . . .
H25 H 0.615727 0.786881 -0.466615 0.082 Uiso 1 1 calc R U . . .
C26 C 0.4987(15) 0.7591(4) -0.4248(18) 0.066(6) Uani 1 1 d . . . . .
C27 C 0.4109(15) 0.7553(3) -0.3541(19) 0.060(5) Uani 1 1 d . . . . .
H27 H 0.378154 0.737916 -0.355783 0.072 Uiso 1 1 calc R U . . .
C28 C 0.3689(12) 0.7771(3) -0.2790(16) 0.051(4) Uani 1 1 d . . . . .
H28 H 0.308253 0.774229 -0.229579 0.061 Uiso 1 1 calc R U . . .
C29 C 0.2298(10) 0.8081(2) 0.2608(14) 0.034(3) Uani 1 1 d . . . . .
C30 C 0.2565(12) 0.7773(2) 0.2485(17) 0.030(2) Uani 1 1 d . . . . .
C31 C 0.2225(10) 0.7570(2) 0.3428(13) 0.030(2) Uani 1 1 d . . . . .
C32 C 0.2554(10) 0.7294(2) 0.3398(14) 0.035(3) Uani 1 1 d . . . . .
H32 H 0.232722 0.716283 0.405315 0.043 Uiso 1 1 calc R U . . .
C33 C 0.3240(10) 0.7223(3) 0.2342(15) 0.038(3) Uani 1 1 d . . . . .
C34 C 0.3579(11) 0.7410(3) 0.1349(16) 0.045(3) Uani 1 1 d . . . . .
H34 H 0.402075 0.735483 0.063559 0.054 Uiso 1 1 calc R U . . .
C35 C 0.3236(11) 0.7688(3) 0.1446(14) 0.039(3) Uani 1 1 d . . . . .
H35 H 0.346737 0.781881 0.079173 0.047 Uiso 1 1 calc R U . . .
C36 C 0.0557(10) 0.8769(3) 0.2125(14) 0.032(3) Uani 1 1 d . . . . .
C37 C -0.0350(9) 0.8841(2) 0.3083(13) 0.027(2) Uani 1 1 d . . . . .
C38 C -0.1170(11) 0.8667(3) 0.3421(16) 0.039(3) Uani 1 1 d . . . . .
C39 C -0.1988(11) 0.8755(3) 0.4242(16) 0.043(3) Uani 1 1 d . . . . .
H39 H -0.254220 0.863610 0.442758 0.052 Uiso 1 1 calc R U . . .
C40 C -0.1944(13) 0.9029(3) 0.4781(16) 0.047(4) Uani 1 1 d . . . . .
C41 C -0.1128(12) 0.9199(3) 0.4513(17) 0.051(4) Uani 1 1 d . . . . .
H41 H -0.110277 0.937814 0.490434 0.061 Uiso 1 1 calc R U . . .
C42 C -0.0338(11) 0.9111(3) 0.3671(16) 0.044(3) Uani 1 1 d . . . . .
H42 H 0.021080 0.923181 0.349072 0.053 Uiso 1 1 calc R U . . .
N1 N 0.2881(10) 0.9724(2) 0.0736(14) 0.042(3) Uani 1 1 d . . . . .
N2 N 0.5657(12) 1.0175(3) -0.1792(18) 0.069(5) Uani 1 1 d . . . . .
N3 N 0.1792(11) 0.9607(2) -0.4449(14) 0.047(3) Uani 1 1 d . . . . .
N4 N -0.0897(12) 1.0095(3) -0.1882(15) 0.057(3) Uani 1 1 d . . . . .
N5 N 0.5651(9) 0.8223(2) 0.1044(13) 0.039(3) Uani 1 1 d . . . . .
N6 N 0.7764(15) 0.9007(3) -0.046(3) 0.090(6) Uani 1 1 d . . . . .
N7 N 0.5713(9) 0.8325(3) -0.3279(13) 0.048(3) Uani 1 1 d . . . . .
N8 N 0.5433(19) 0.7364(5) -0.512(2) 0.098(8) Uani 1 1 d . . . . .
N9 N 0.1455(9) 0.7642(2) 0.4499(13) 0.040(3) Uani 1 1 d . . . . .
N10 N 0.3580(9) 0.6933(2) 0.2261(15) 0.051(3) Uani 1 1 d . . . . .
N11 N -0.1168(11) 0.8373(3) 0.2919(14) 0.053(3) Uani 1 1 d . . . . .
N12 N -0.2790(13) 0.9120(4) 0.5646(17) 0.068(4) Uani 1 1 d . . . . .
O1 O 0.3842(7) 0.89310(18) -0.0791(9) 0.035(2) Uani 1 1 d . . . . .
O2 O 0.2891(7) 0.91609(17) 0.0736(9) 0.0359(19) Uani 1 1 d . . . . .
O3 O 0.3033(11) 0.9762(3) 0.2028(13) 0.083(4) Uani 1 1 d . . . . .
O4 O 0.2040(9) 0.9731(3) 0.0084(14) 0.070(3) Uani 1 1 d . . . . .
O5 O 0.5430(13) 1.0389(3) -0.112(2) 0.102(5) Uani 1 1 d . . . . .
O6 O 0.6261(13) 1.0165(3) -0.2733(19) 0.099(5) Uani 1 1 d . . . . .
O7 O 0.1552(8) 0.89135(18) -0.1782(9) 0.041(2) Uani 1 1 d . . . . .
O8 O 0.1686(8) 0.90430(19) -0.4054(10) 0.040(2) Uani 1 1 d . . . . .
O9 O 0.2712(9) 0.9575(2) -0.4039(13) 0.062(3) Uani 1 1 d . . . . .
O10 O 0.1488(12) 0.9653(3) -0.5680(12) 0.080(4) Uani 1 1 d . . . . .
O11 O -0.0818(12) 1.0289(2) -0.2736(14) 0.077(4) Uani 1 1 d . . . . .
O12 O -0.1435(12) 1.0104(3) -0.0842(17) 0.091(5) Uani 1 1 d . . . . .
O13 O 0.3579(7) 0.86151(17) 0.2240(9) 0.0304(19) Uani 1 1 d . . . . .
O14 O 0.4576(8) 0.8562(2) 0.4244(9) 0.041(2) Uani 1 1 d . . . . .
O15 O 0.5146(9) 0.8121(2) 0.1995(12) 0.056(3) Uani 1 1 d . . . . .
O16 O 0.5948(9) 0.8086(2) 0.0019(12) 0.058(3) Uani 1 1 d . . . . .
O17 O 0.8198(12) 0.8861(3) -0.1267(18) 0.092(5) Uani 1 1 d . . . . .
O18 O 0.799(2) 0.9252(4) -0.023(3) 0.237(17) Uani 1 1 d . . . . .
O19 O 0.3581(8) 0.82797(19) -0.0731(9) 0.040(2) Uani 1 1 d . . . . .
O20 O 0.3068(7) 0.84315(18) -0.2910(9) 0.0368(19) Uani 1 1 d . . . . .
O21 O 0.5373(8) 0.8514(2) -0.2562(12) 0.054(3) Uani 1 1 d . . . . .
O22 O 0.6563(10) 0.8327(3) -0.3861(19) 0.097(5) Uani 1 1 d . . . . .
O23 O 0.6250(17) 0.7405(5) -0.569(2) 0.149(11) Uani 1 1 d . . . . .
O24 O 0.4953(17) 0.7145(4) -0.5161(19) 0.125(9) Uani 1 1 d . . . . .
O25 O 0.2003(7) 0.82019(17) 0.1465(9) 0.035(2) Uani 1 1 d . . . . .
O26 O 0.2433(8) 0.81880(17) 0.3836(9) 0.041(2) Uani 1 1 d . . . . .
O27 O 0.0708(9) 0.7790(3) 0.4078(13) 0.067(3) Uani 1 1 d . . . . .
O28 O 0.1558(10) 0.7545(3) 0.5701(12) 0.067(3) Uani 1 1 d . . . . .
O29 O 0.4035(11) 0.6861(2) 0.1198(16) 0.082(4) Uani 1 1 d . . . . .
O30 O 0.3399(11) 0.6777(2) 0.3268(17) 0.082(4) Uani 1 1 d . . . . .
O31 O 0.1467(6) 0.87710(18) 0.2652(9) 0.0315(18) Uani 1 1 d . . . . .
O32 O 0.0339(8) 0.8733(3) 0.0824(11) 0.054(3) Uani 1 1 d . . . . .
O33 O -0.0332(9) 0.8266(2) 0.2697(15) 0.066(3) Uani 1 1 d . . . . .
O34 O -0.2029(9) 0.8257(3) 0.2758(17) 0.080(4) Uani 1 1 d . . . . .
O35 O -0.2669(13) 0.9346(4) 0.6261(19) 0.115(6) Uani 1 1 d . . . . .
O36 O -0.3564(11) 0.8980(3) 0.5687(18) 0.089(5) Uani 1 1 d . . . . .
O1W O 0.0902(9) 0.8338(2) -0.1315(10) 0.054(3) Uani 1 1 d . . . . .
O2W O 0.3241(8) 0.91358(18) 0.3682(9) 0.040(2) Uani 1 1 d D . . . .
H21W H 0.306(11) 0.919(2) 0.287(6) 0.048 Uiso 1 1 d D U . . .
H22W H 0.328(12) 0.9282(15) 0.416(10) 0.048 Uiso 1 1 d D U . . .
O3W O 0.0991(8) 0.8452(2) 0.5570(10) 0.044(2) Uani 1 1 d D . . . .
H31W H 0.065(11) 0.834(2) 0.506(11) 0.052 Uiso 1 1 d D U . . .
H32W H 0.108(12) 0.836(2) 0.633(8) 0.052 Uiso 1 1 d D U . . .
O4W O 0.4008(7) 0.8960(2) 0.6289(9) 0.037(2) Uani 1 1 d D . . . .
H41W H 0.396(9) 0.902(3) 0.709(7) 0.045 Uiso 1 1 d D U . . .
H42W H 0.463(4) 0.892(3) 0.625(12) 0.045 Uiso 1 1 d D U . . .
Ce1 Ce 0.23113(4) 0.86394(2) 0.01584(5) 0.02513(17) Uani 1 1 d . . . . .
Ce2 Ce 0.26691(4) 0.86699(2) 0.47882(5) 0.02533(17) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.264(15) . ?
C1 O2 1.275(15) . ?
C1 C2 1.501(17) . ?
C2 C3 1.384(17) . ?
C2 C7 1.407(18) . ?
C3 C4 1.373(18) . ?
C3 N1 1.481(17) . ?
C4 C5 1.36(2) . ?
C4 H4 0.9300 . ?
C5 C6 1.41(2) . ?
C5 N2 1.488(18) . ?
C6 C7 1.388(19) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 O8 1.229(14) . ?
C8 O7 1.264(14) . ?
C8 C9 1.509(16) . ?
C9 C14 1.376(16) . ?
C9 C10 1.409(16) . ?
C10 C11 1.350(17) . ?
C10 N3 1.474(17) . ?
C11 C12 1.388(19) . ?
C11 H11 0.9300 . ?
C12 C13 1.398(18) . ?
C12 N4 1.471(17) . ?
C13 C14 1.365(18) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C15 O14 1.243(15) . ?
C15 O13 1.275(15) . ?
C15 C16 1.508(18) . ?
C16 C17 1.381(18) . ?
C16 C21 1.404(17) . ?
C17 C18 1.404(18) . ?
C17 N5 1.447(16) . ?
C18 C19 1.33(2) . ?
C18 H18 0.9300 . ?
C19 C20 1.39(2) . ?
C19 N6 1.47(2) . ?
C20 C21 1.37(2) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
C22 O19 1.239(14) . ?
C22 O20 1.257(14) . ?
C22 C23 1.519(17) . ?
C23 C28 1.386(19) . ?
C23 C24 1.390(19) . ?
C24 C25 1.38(2) . ?
C24 N7 1.494(19) . ?
C25 C26 1.40(3) . ?
C25 H25 0.9300 . ?
C26 C27 1.34(3) . ?
C26 N8 1.48(2) . ?
C27 C28 1.38(2) . ?
C27 H27 0.9300 . ?
C28 H28 0.9300 . ?
C29 O25 1.247(15) . ?
C29 O26 1.250(15) . ?
C29 C30 1.515(15) . ?
C30 C35 1.38(2) . ?
C30 C31 1.393(18) . ?
C31 C32 1.381(16) . ?
C31 N9 1.474(16) . ?
C32 C33 1.390(19) . ?
C32 H32 0.9300 . ?
C33 C34 1.368(19) . ?
C33 N10 1.458(16) . ?
C34 C35 1.402(18) . ?
C34 H34 0.9300 . ?
C35 H35 0.9300 . ?
C36 O32 1.235(16) . ?
C36 O31 1.237(14) . ?
C36 C37 1.537(17) . ?
C37 C38 1.387(18) . ?
C37 C42 1.398(18) . ?
C38 C39 1.39(2) . ?
C38 N11 1.479(18) . ?
C39 C40 1.40(2) . ?
C39 H39 0.9300 . ?
C40 C41 1.36(2) . ?
C40 N12 1.45(2) . ?
C41 C42 1.37(2) . ?
C41 H41 0.9300 . ?
C42 H42 0.9300 . ?
N1 O4 1.205(16) . ?
N1 O3 1.217(16) . ?
N2 O6 1.19(2) . ?
N2 O5 1.24(2) . ?
N3 O10 1.206(17) . ?
N3 O9 1.226(17) . ?
N4 O12 1.213(19) . ?
N4 O11 1.227(18) . ?
N5 O15 1.220(15) . ?
N5 O16 1.229(14) . ?
N6 O17 1.18(2) . ?
N6 O18 1.22(2) . ?
N7 O21 1.216(16) . ?
N7 O22 1.237(17) . ?
N8 O24 1.21(3) . ?
N8 O23 1.21(3) . ?
N9 O28 1.206(15) . ?
N9 O27 1.235(15) . ?
N10 O29 1.219(17) . ?
N10 O30 1.222(17) . ?
N11 O33 1.213(17) . ?
N11 O34 1.234(17) . ?
N12 O36 1.20(2) . ?
N12 O35 1.23(2) . ?
O1 Ce1 2.592(9) . ?
O2 Ce1 2.646(8) . ?
O7 Ce1 2.390(8) . ?
O8 Ce2 2.459(9) 1_554 ?
O13 Ce1 2.456(9) . ?
O13 Ce2 2.698(9) . ?
O14 Ce2 2.566(10) . ?
O19 Ce1 2.530(8) . ?
O20 Ce2 2.448(8) 1_554 ?
O25 Ce1 2.457(8) . ?
O26 Ce2 2.479(8) . ?
O31 Ce2 2.489(8) . ?
O31 Ce1 2.675(9) . ?
O32 Ce1 2.663(11) . ?
O1W Ce1 2.632(8) . ?
O2W Ce2 2.572(9) . ?
O2W H21W 0.82(3) . ?
O2W H22W 0.83(3) . ?
O3W Ce2 2.524(10) . ?
O3W H31W 0.82(3) . ?
O3W H32W 0.83(3) . ?
O4W Ce2 2.555(8) . ?
O4W H41W 0.81(3) . ?
O4W H42W 0.82(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
O1 C1 O2 120.6(11) . . ?
O1 C1 C2 119.9(11) . . ?
O2 C1 C2 119.5(11) . . ?
C3 C2 C7 116.9(12) . . ?
C3 C2 C1 123.4(11) . . ?
C7 C2 C1 119.7(11) . . ?
C4 C3 C2 123.1(12) . . ?
C4 C3 N1 114.8(11) . . ?
C2 C3 N1 122.0(11) . . ?
C5 C4 C3 118.5(13) . . ?
C5 C4 H4 120.7 . . ?
C3 C4 H4 120.7 . . ?
C4 C5 C6 122.3(13) . . ?
C4 C5 N2 119.5(15) . . ?
C6 C5 N2 118.2(14) . . ?
C7 C6 C5 117.3(13) . . ?
C7 C6 H6 121.4 . . ?
C5 C6 H6 121.4 . . ?
C6 C7 C2 121.9(13) . . ?
C6 C7 H7 119.1 . . ?
C2 C7 H7 119.1 . . ?
O8 C8 O7 124.8(11) . . ?
O8 C8 C9 118.1(10) . . ?
O7 C8 C9 117.0(10) . . ?
C14 C9 C10 115.8(11) . . ?
C14 C9 C8 121.8(11) . . ?
C10 C9 C8 122.3(10) . . ?
C11 C10 C9 123.4(12) . . ?
C11 C10 N3 116.4(11) . . ?
C9 C10 N3 120.2(11) . . ?
C10 C11 C12 118.1(12) . . ?
C10 C11 H11 120.9 . . ?
C12 C11 H11 120.9 . . ?
C11 C12 C13 121.3(12) . . ?
C11 C12 N4 119.8(12) . . ?
C13 C12 N4 118.9(13) . . ?
C14 C13 C12 117.7(12) . . ?
C14 C13 H13 121.2 . . ?
C12 C13 H13 121.2 . . ?
C13 C14 C9 123.7(12) . . ?
C13 C14 H14 118.1 . . ?
C9 C14 H14 118.1 . . ?
O14 C15 O13 122.9(12) . . ?
O14 C15 C16 120.2(12) . . ?
O13 C15 C16 116.4(11) . . ?
C17 C16 C21 119.1(12) . . ?
C17 C16 C15 125.4(11) . . ?
C21 C16 C15 115.3(12) . . ?
C16 C17 C18 120.2(12) . . ?
C16 C17 N5 120.2(11) . . ?
C18 C17 N5 119.6(11) . . ?
C19 C18 C17 118.8(13) . . ?
C19 C18 H18 120.6 . . ?
C17 C18 H18 120.6 . . ?
C18 C19 C20 123.0(15) . . ?
C18 C19 N6 117.7(14) . . ?
C20 C19 N6 119.4(14) . . ?
C21 C20 C19 118.3(14) . . ?
C21 C20 H20 120.8 . . ?
C19 C20 H20 120.8 . . ?
C20 C21 C16 120.6(14) . . ?
C20 C21 H21 119.7 . . ?
C16 C21 H21 119.7 . . ?
O19 C22 O20 124.8(11) . . ?
O19 C22 C23 118.5(10) . . ?
O20 C22 C23 116.4(10) . . ?
C28 C23 C24 117.4(13) . . ?
C28 C23 C22 117.6(12) . . ?
C24 C23 C22 124.9(12) . . ?
C25 C24 C23 123.0(15) . . ?
C25 C24 N7 117.3(14) . . ?
C23 C24 N7 119.7(12) . . ?
C24 C25 C26 116.5(16) . . ?
C24 C25 H25 121.8 . . ?
C26 C25 H25 121.8 . . ?
C27 C26 C25 122.0(14) . . ?
C27 C26 N8 122(2) . . ?
C25 C26 N8 116(2) . . ?
C26 C27 C28 120.3(16) . . ?
C26 C27 H27 119.8 . . ?
C28 C27 H27 119.8 . . ?
C27 C28 C23 120.6(16) . . ?
C27 C28 H28 119.7 . . ?
C23 C28 H28 119.7 . . ?
O25 C29 O26 127.3(11) . . ?
O25 C29 C30 116.4(11) . . ?
O26 C29 C30 116.3(11) . . ?
C35 C30 C31 117.1(10) . . ?
C35 C30 C29 119.2(12) . . ?
C31 C30 C29 123.6(13) . . ?
C32 C31 C30 123.2(12) . . ?
C32 C31 N9 116.9(11) . . ?
C30 C31 N9 119.9(10) . . ?
C31 C32 C33 116.8(12) . . ?
C31 C32 H32 121.6 . . ?
C33 C32 H32 121.6 . . ?
C34 C33 C32 123.2(12) . . ?
C34 C33 N10 118.8(12) . . ?
C32 C33 N10 118.0(12) . . ?
C33 C34 C35 117.7(12) . . ?
C33 C34 H34 121.2 . . ?
C35 C34 H34 121.2 . . ?
C30 C35 C34 122.1(12) . . ?
C30 C35 H35 119.0 . . ?
C34 C35 H35 119.0 . . ?
O32 C36 O31 123.1(13) . . ?
O32 C36 C37 117.2(11) . . ?
O31 C36 C37 119.5(11) . . ?
C38 C37 C42 117.3(12) . . ?
C38 C37 C36 126.6(11) . . ?
C42 C37 C36 116.1(11) . . ?
C39 C38 C37 122.8(13) . . ?
C39 C38 N11 118.1(13) . . ?
C37 C38 N11 119.1(13) . . ?
C38 C39 C40 117.4(14) . . ?
C38 C39 H39 121.3 . . ?
C40 C39 H39 121.3 . . ?
C41 C40 C39 120.8(14) . . ?
C41 C40 N12 121.7(15) . . ?
C39 C40 N12 117.5(16) . . ?
C40 C41 C42 121.1(15) . . ?
C40 C41 H41 119.5 . . ?
C42 C41 H41 119.5 . . ?
C41 C42 C37 120.6(14) . . ?
C41 C42 H42 119.7 . . ?
C37 C42 H42 119.7 . . ?
O4 N1 O3 125.6(14) . . ?
O4 N1 C3 117.6(12) . . ?
O3 N1 C3 116.7(13) . . ?
O6 N2 O5 125.3(16) . . ?
O6 N2 C5 119.4(17) . . ?
O5 N2 C5 115.3(16) . . ?
O10 N3 O9 124.9(14) . . ?
O10 N3 C10 118.7(14) . . ?
O9 N3 C10 116.4(13) . . ?
O12 N4 O11 123.8(14) . . ?
O12 N4 C12 117.9(14) . . ?
O11 N4 C12 118.2(14) . . ?
O15 N5 O16 122.8(12) . . ?
O15 N5 C17 118.0(11) . . ?
O16 N5 C17 119.3(12) . . ?
O17 N6 O18 124.1(19) . . ?
O17 N6 C19 121.5(15) . . ?
O18 N6 C19 114.2(18) . . ?
O21 N7 O22 125.4(15) . . ?
O21 N7 C24 119.1(11) . . ?
O22 N7 C24 115.5(14) . . ?
O24 N8 O23 125.0(19) . . ?
O24 N8 C26 116(2) . . ?
O23 N8 C26 119(3) . . ?
O28 N9 O27 123.8(13) . . ?
O28 N9 C31 119.1(12) . . ?
O27 N9 C31 117.0(11) . . ?
O29 N10 O30 124.2(13) . . ?
O29 N10 C33 117.7(13) . . ?
O30 N10 C33 118.0(13) . . ?
O33 N11 O34 125.2(15) . . ?
O33 N11 C38 118.2(13) . . ?
O34 N11 C38 116.7(14) . . ?
O36 N12 O35 124.2(16) . . ?
O36 N12 C40 119.5(17) . . ?
O35 N12 C40 116.3(17) . . ?
C1 O1 Ce1 95.8(7) . . ?
C1 O2 Ce1 93.0(7) . . ?
C8 O7 Ce1 162.2(9) . . ?
C8 O8 Ce2 134.0(8) . 1_554 ?
C15 O13 Ce1 158.0(8) . . ?
C15 O13 Ce2 89.1(7) . . ?
Ce1 O13 Ce2 112.7(3) . . ?
C15 O14 Ce2 96.0(8) . . ?
C22 O19 Ce1 112.6(8) . . ?
C22 O20 Ce2 154.7(8) . 1_554 ?
C29 O25 Ce1 139.7(8) . . ?
C29 O26 Ce2 135.3(7) . . ?
C36 O31 Ce2 147.2(8) . . ?
C36 O31 Ce1 94.0(7) . . ?
Ce2 O31 Ce1 112.4(3) . . ?
C36 O32 Ce1 94.7(8) . . ?
Ce2 O2W H21W 125(9) . . ?
Ce2 O2W H22W 122(9) . . ?
H21W O2W H22W 103(4) . . ?
Ce2 O3W H31W 122(10) . . ?
Ce2 O3W H32W 112(10) . . ?
H31W O3W H32W 102(4) . . ?
Ce2 O4W H41W 128(9) . . ?
Ce2 O4W H42W 117(9) . . ?
H41W O4W H42W 105(5) . . ?
O7 Ce1 O13 147.4(3) . . ?
O7 Ce1 O25 140.1(3) . . ?
O13 Ce1 O25 71.9(3) . . ?
O7 Ce1 O19 111.7(3) . . ?
O13 Ce1 O19 79.4(3) . . ?
O25 Ce1 O19 72.8(3) . . ?
O7 Ce1 O1 74.6(3) . . ?
O13 Ce1 O1 79.3(3) . . ?
O25 Ce1 O1 140.1(3) . . ?
O19 Ce1 O1 75.3(3) . . ?
O7 Ce1 O1W 70.7(3) . . ?
O13 Ce1 O1W 141.9(3) . . ?
O25 Ce1 O1W 70.6(3) . . ?
O19 Ce1 O1W 83.9(3) . . ?
O1 Ce1 O1W 128.8(3) . . ?
O7 Ce1 O2 74.6(3) . . ?
O13 Ce1 O2 73.7(3) . . ?
O25 Ce1 O2 138.7(3) . . ?
O19 Ce1 O2 121.9(3) . . ?
O1 Ce1 O2 49.8(3) . . ?
O1W Ce1 O2 142.8(3) . . ?
O7 Ce1 O32 74.3(3) . . ?
O13 Ce1 O32 114.8(3) . . ?
O25 Ce1 O32 81.4(3) . . ?
O19 Ce1 O32 145.1(4) . . ?
O1 Ce1 O32 136.7(3) . . ?
O1W Ce1 O32 65.2(4) . . ?
O2 Ce1 O32 93.1(3) . . ?
O7 Ce1 O31 110.8(3) . . ?
O13 Ce1 O31 67.2(3) . . ?
O25 Ce1 O31 72.1(3) . . ?
O19 Ce1 O31 137.3(3) . . ?
O1 Ce1 O31 120.8(3) . . ?
O1W Ce1 O31 106.3(3) . . ?
O2 Ce1 O31 74.1(3) . . ?
O32 Ce1 O31 48.1(3) . . ?
O20 Ce2 O8 92.6(3) 1_556 1_556 ?
O20 Ce2 O26 83.9(3) 1_556 . ?
O8 Ce2 O26 140.6(3) 1_556 . ?
O20 Ce2 O31 151.0(3) 1_556 . ?
O8 Ce2 O31 84.1(3) 1_556 . ?
O26 Ce2 O31 80.7(3) . . ?
O20 Ce2 O3W 72.5(3) 1_556 . ?
O8 Ce2 O3W 73.3(3) 1_556 . ?
O26 Ce2 O3W 68.3(3) . . ?
O31 Ce2 O3W 79.0(3) . . ?
O20 Ce2 O4W 71.0(3) 1_556 . ?
O8 Ce2 O4W 73.3(3) 1_556 . ?
O26 Ce2 O4W 139.7(3) . . ?
O31 Ce2 O4W 134.1(3) . . ?
O3W Ce2 O4W 128.5(3) . . ?
O20 Ce2 O14 85.5(3) 1_556 . ?
O8 Ce2 O14 138.0(3) 1_556 . ?
O26 Ce2 O14 81.0(3) . . ?
O31 Ce2 O14 115.8(3) . . ?
O3W Ce2 O14 143.5(4) . . ?
O4W Ce2 O14 66.4(3) . . ?
O20 Ce2 O2W 134.4(3) 1_556 . ?
O8 Ce2 O2W 73.1(3) 1_556 . ?
O26 Ce2 O2W 133.9(3) . . ?
O31 Ce2 O2W 72.0(3) . . ?
O3W Ce2 O2W 137.3(3) . . ?
O4W Ce2 O2W 63.4(3) . . ?
O14 Ce2 O2W 78.6(3) . . ?
O20 Ce2 O13 129.6(3) 1_556 . ?
O8 Ce2 O13 134.9(3) 1_556 . ?
O26 Ce2 O13 69.4(3) . . ?
O31 Ce2 O13 66.4(3) . . ?
O3W Ce2 O13 128.5(3) . . ?
O4W Ce2 O13 102.8(3) . . ?
O14 Ce2 O13 49.6(3) . . ?
O2W Ce2 O13 65.9(3) . . ?

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
O1 C1 C2 C3 169.2(12) . . . . ?
O2 C1 C2 C3 -12.2(18) . . . . ?
O1 C1 C2 C7 -8.7(18) . . . . ?
O2 C1 C2 C7 169.9(12) . . . . ?
C7 C2 C3 C4 0.2(19) . . . . ?
C1 C2 C3 C4 -177.8(12) . . . . ?
C7 C2 C3 N1 178.3(12) . . . . ?
C1 C2 C3 N1 0.3(19) . . . . ?
C2 C3 C4 C5 2(2) . . . . ?
N1 C3 C4 C5 -176.6(13) . . . . ?
C3 C4 C5 C6 -2(2) . . . . ?
C3 C4 C5 N2 176.5(12) . . . . ?
C4 C5 C6 C7 1(2) . . . . ?
N2 C5 C6 C7 -177.5(13) . . . . ?
C5 C6 C7 C2 0(2) . . . . ?
C3 C2 C7 C6 -1(2) . . . . ?
C1 C2 C7 C6 176.9(12) . . . . ?
O8 C8 C9 C14 148.3(12) . . . . ?
O7 C8 C9 C14 -27.4(17) . . . . ?
O8 C8 C9 C10 -27.1(18) . . . . ?
O7 C8 C9 C10 157.3(12) . . . . ?
C14 C9 C10 C11 -1.1(19) . . . . ?
C8 C9 C10 C11 174.4(12) . . . . ?
C14 C9 C10 N3 178.7(12) . . . . ?
C8 C9 C10 N3 -5.7(19) . . . . ?
C9 C10 C11 C12 0(2) . . . . ?
N3 C10 C11 C12 -179.4(13) . . . . ?
C10 C11 C12 C13 1(2) . . . . ?
C10 C11 C12 N4 -177.7(12) . . . . ?
C11 C12 C13 C14 -2(2) . . . . ?
N4 C12 C13 C14 176.8(13) . . . . ?
C12 C13 C14 C9 2(2) . . . . ?
C10 C9 C14 C13 0.1(19) . . . . ?
C8 C9 C14 C13 -175.5(13) . . . . ?
O14 C15 C16 C17 106.0(16) . . . . ?
O13 C15 C16 C17 -81.8(16) . . . . ?
O14 C15 C16 C21 -79.2(16) . . . . ?
O13 C15 C16 C21 93.0(14) . . . . ?
C21 C16 C17 C18 -2(2) . . . . ?
C15 C16 C17 C18 172.7(13) . . . . ?
C21 C16 C17 N5 178.1(12) . . . . ?
C15 C16 C17 N5 -7(2) . . . . ?
C16 C17 C18 C19 2(2) . . . . ?
N5 C17 C18 C19 -178.1(13) . . . . ?
C17 C18 C19 C20 0(2) . . . . ?
C17 C18 C19 N6 -179.1(16) . . . . ?
C18 C19 C20 C21 -2(3) . . . . ?
N6 C19 C20 C21 177.3(16) . . . . ?
C19 C20 C21 C16 2(2) . . . . ?
C17 C16 C21 C20 0(2) . . . . ?
C15 C16 C21 C20 -175.1(13) . . . . ?
O19 C22 C23 C28 75.5(15) . . . . ?
O20 C22 C23 C28 -98.7(14) . . . . ?
O19 C22 C23 C24 -107.8(14) . . . . ?
O20 C22 C23 C24 78.0(15) . . . . ?
C28 C23 C24 C25 4.6(19) . . . . ?
C22 C23 C24 C25 -172.1(12) . . . . ?
C28 C23 C24 N7 -172.0(11) . . . . ?
C22 C23 C24 N7 11.3(18) . . . . ?
C23 C24 C25 C26 -1(2) . . . . ?
N7 C24 C25 C26 175.2(12) . . . . ?
C24 C25 C26 C27 -2(2) . . . . ?
C24 C25 C26 N8 177.7(13) . . . . ?
C25 C26 C27 C28 3(3) . . . . ?
N8 C26 C27 C28 -177.2(15) . . . . ?
C26 C27 C28 C23 1(2) . . . . ?
C24 C23 C28 C27 -4(2) . . . . ?
C22 C23 C28 C27 172.8(12) . . . . ?
O25 C29 C30 C35 50.2(19) . . . . ?
O26 C29 C30 C35 -127.4(14) . . . . ?
O25 C29 C30 C31 -134.2(14) . . . . ?
O26 C29 C30 C31 48.2(19) . . . . ?
C35 C30 C31 C32 2(2) . . . . ?
C29 C30 C31 C32 -173.4(13) . . . . ?
C35 C30 C31 N9 -176.0(12) . . . . ?
C29 C30 C31 N9 8(2) . . . . ?
C30 C31 C32 C33 -1.4(19) . . . . ?
N9 C31 C32 C33 177.0(11) . . . . ?
C31 C32 C33 C34 -0.9(19) . . . . ?
C31 C32 C33 N10 -178.5(11) . . . . ?
C32 C33 C34 C35 2(2) . . . . ?
N10 C33 C34 C35 179.6(13) . . . . ?
C31 C30 C35 C34 -1(2) . . . . ?
C29 C30 C35 C34 174.9(13) . . . . ?
C33 C34 C35 C30 -1(2) . . . . ?
O32 C36 C37 C38 67.8(19) . . . . ?
O31 C36 C37 C38 -118.0(14) . . . . ?
O32 C36 C37 C42 -112.4(14) . . . . ?
O31 C36 C37 C42 61.8(17) . . . . ?
C42 C37 C38 C39 3(2) . . . . ?
C36 C37 C38 C39 -176.8(13) . . . . ?
C42 C37 C38 N11 -175.1(12) . . . . ?
C36 C37 C38 N11 5(2) . . . . ?
C37 C38 C39 C40 -2(2) . . . . ?
N11 C38 C39 C40 176.2(13) . . . . ?
C38 C39 C40 C41 0(2) . . . . ?
C38 C39 C40 N12 -179.6(14) . . . . ?
C39 C40 C41 C42 2(2) . . . . ?
N12 C40 C41 C42 -179.0(15) . . . . ?
C40 C41 C42 C37 -1(2) . . . . ?
C38 C37 C42 C41 -2(2) . . . . ?
C36 C37 C42 C41 178.3(13) . . . . ?
C4 C3 N1 O4 94.8(15) . . . . ?
C2 C3 N1 O4 -83.4(16) . . . . ?
C4 C3 N1 O3 -80.8(16) . . . . ?
C2 C3 N1 O3 100.9(16) . . . . ?
C4 C5 N2 O6 -166.5(18) . . . . ?
C6 C5 N2 O6 13(2) . . . . ?
C4 C5 N2 O5 16(2) . . . . ?
C6 C5 N2 O5 -165.3(17) . . . . ?
C11 C10 N3 O10 -60.3(17) . . . . ?
C9 C10 N3 O10 119.9(14) . . . . ?
C11 C10 N3 O9 117.1(14) . . . . ?
C9 C10 N3 O9 -62.8(16) . . . . ?
C11 C12 N4 O12 -171.6(16) . . . . ?
C13 C12 N4 O12 9(2) . . . . ?
C11 C12 N4 O11 5(2) . . . . ?
C13 C12 N4 O11 -174.1(15) . . . . ?
C16 C17 N5 O15 -15.6(19) . . . . ?
C18 C17 N5 O15 164.4(12) . . . . ?
C16 C17 N5 O16 165.0(12) . . . . ?
C18 C17 N5 O16 -14.9(18) . . . . ?
C18 C19 N6 O17 -2(3) . . . . ?
C20 C19 N6 O17 179(2) . . . . ?
C18 C19 N6 O18 -177(3) . . . . ?
C20 C19 N6 O18 4(4) . . . . ?
C25 C24 N7 O21 -177.2(12) . . . . ?
C23 C24 N7 O21 -0.3(18) . . . . ?
C25 C24 N7 O22 0.1(19) . . . . ?
C23 C24 N7 O22 176.9(13) . . . . ?
C27 C26 N8 O24 0(3) . . . . ?
C25 C26 N8 O24 -179.5(15) . . . . ?
C27 C26 N8 O23 -177.2(17) . . . . ?
C25 C26 N8 O23 3(3) . . . . ?
C32 C31 N9 O28 41.4(17) . . . . ?
C30 C31 N9 O28 -140.2(14) . . . . ?
C32 C31 N9 O27 -135.2(12) . . . . ?
C30 C31 N9 O27 43.2(18) . . . . ?
C34 C33 N10 O29 -10(2) . . . . ?
C32 C33 N10 O29 167.9(14) . . . . ?
C34 C33 N10 O30 169.6(14) . . . . ?
C32 C33 N10 O30 -12.7(19) . . . . ?
C39 C38 N11 O33 -153.0(15) . . . . ?
C37 C38 N11 O33 26(2) . . . . ?
C39 C38 N11 O34 27(2) . . . . ?
C37 C38 N11 O34 -154.3(14) . . . . ?
C41 C40 N12 O36 169.3(17) . . . . ?
C39 C40 N12 O36 -12(3) . . . . ?
C41 C40 N12 O35 -8(3) . . . . ?
C39 C40 N12 O35 170.8(17) . . . . ?
O2 C1 O1 Ce1 10.0(13) . . . . ?
C2 C1 O1 Ce1 -171.5(10) . . . . ?
O1 C1 O2 Ce1 -9.7(12) . . . . ?
C2 C1 O2 Ce1 171.7(10) . . . . ?
O8 C8 O7 Ce1 80(3) . . . . ?
C9 C8 O7 Ce1 -105(3) . . . . ?
O7 C8 O8 Ce2 -9(2) . . . 1_554 ?
C9 C8 O8 Ce2 175.5(8) . . . 1_554 ?
O14 C15 O13 Ce1 -172.0(14) . . . . ?
C16 C15 O13 Ce1 16(3) . . . . ?
O14 C15 O13 Ce2 15.7(12) . . . . ?
C16 C15 O13 Ce2 -156.2(9) . . . . ?
O13 C15 O14 Ce2 -16.7(13) . . . . ?
C16 C15 O14 Ce2 155.0(10) . . . . ?
O20 C22 O19 Ce1 4.1(15) . . . . ?
C23 C22 O19 Ce1 -169.6(8) . . . . ?
O19 C22 O20 Ce2 158.8(13) . . . 1_554 ?
C23 C22 O20 Ce2 -27(2) . . . 1_554 ?
O26 C29 O25 Ce1 43(2) . . . . ?
C30 C29 O25 Ce1 -134.7(11) . . . . ?
O25 C29 O26 Ce2 -18(2) . . . . ?
C30 C29 O26 Ce2 159.3(9) . . . . ?
O32 C36 O31 Ce2 -149.0(12) . . . . ?
C37 C36 O31 Ce2 37(2) . . . . ?
O32 C36 O31 Ce1 -4.4(14) . . . . ?
C37 C36 O31 Ce1 -178.3(10) . . . . ?
O31 C36 O32 Ce1 4.5(15) . . . . ?
C37 C36 O32 Ce1 178.5(10) . . . . ?

_refine_diff_density_max         1.556
_refine_diff_density_min         -2.144
_refine_diff_density_rms         0.148

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1584550'
_audit_update_record             
;
2017-11-08 deposited with the CCDC.
2018-02-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C21 H13 N6 Nd O20, H2 O'
_chemical_formula_sum            'C21 H15 N6 Nd O21'
_chemical_formula_weight         831.63

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'
Nd Nd -0.1943 3.0179 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.2950(6)
_cell_length_b                   11.4720(8)
_cell_length_c                   13.8210(10)
_cell_angle_alpha                106.487(3)
_cell_angle_beta                 90.356(3)
_cell_angle_gamma                94.150(3)
_cell_volume                     1408.91(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    8025
_cell_measurement_theta_min      2.65
_cell_measurement_theta_max      27.18

_exptl_crystal_description       Rectangular
_exptl_crystal_colour            Pink
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.960
_exptl_crystal_F_000             822
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.170
_exptl_absorpt_coefficient_mu    1.952
_shelx_estimated_absorpt_T_min   0.673
_shelx_estimated_absorpt_T_max   0.733
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.668
_exptl_absorpt_correction_T_max  0.738
_exptl_absorpt_process_details   
'SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction'

_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            30525
_diffrn_reflns_av_unetI/netI     0.0651
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.537
_diffrn_reflns_theta_max         30.878
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measured_fraction_theta_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_point_group_measured_fraction_full 0.980
_reflns_number_total             8562
_reflns_number_gt                6921
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Sir-92 (Altomare et al., 1993)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0440P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8562
_refine_ls_number_parameters     460
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0406
_refine_ls_wR_factor_ref         0.0851
_refine_ls_wR_factor_gt          0.0784
_refine_ls_goodness_of_fit_ref   0.954
_refine_ls_restrained_S_all      0.954
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.0483(3) 0.2394(3) 0.5469(2) 0.0237(6) Uani 1 1 d . . . . .
C2 C -0.0065(3) 0.3640(3) 0.5828(2) 0.0233(6) Uani 1 1 d . . . . .
C3 C 0.0937(3) 0.4638(3) 0.6179(2) 0.0261(7) Uani 1 1 d . . . . .
H3 H 0.192046 0.453601 0.618657 0.031 Uiso 1 1 calc R U . . .
C4 C 0.0433(4) 0.5785(3) 0.6517(2) 0.0282(7) Uani 1 1 d . . . . .
C5 C -0.1002(4) 0.5996(3) 0.6509(3) 0.0320(7) Uani 1 1 d . . . . .
H5 H -0.131300 0.677644 0.674587 0.038 Uiso 1 1 calc R U . . .
C6 C -0.1962(4) 0.4982(3) 0.6128(2) 0.0288(7) Uani 1 1 d . . . . .
C7 C -0.1529(3) 0.3810(3) 0.5806(2) 0.0271(7) Uani 1 1 d . . . . .
H7 H -0.220451 0.314623 0.557847 0.033 Uiso 1 1 calc R U . . .
C8 C 0.4628(3) -0.1671(3) 0.3500(2) 0.0230(6) Uani 1 1 d . . . . .
C9 C 0.4952(3) -0.2783(3) 0.2684(2) 0.0221(6) Uani 1 1 d . . . . .
C10 C 0.6388(3) -0.3011(3) 0.2439(2) 0.0282(7) Uani 1 1 d . . . . .
H10 H 0.714141 -0.244818 0.274785 0.034 Uiso 1 1 calc R U . . .
C11 C 0.6660(3) -0.4083(3) 0.1735(2) 0.0302(7) Uani 1 1 d . . . . .
C12 C 0.5581(4) -0.4956(3) 0.1263(3) 0.0335(8) Uani 1 1 d . . . . .
H12 H 0.578647 -0.568292 0.079848 0.040 Uiso 1 1 calc R U . . .
C13 C 0.4184(3) -0.4694(3) 0.1517(2) 0.0277(7) Uani 1 1 d . . . . .
C14 C 0.3842(3) -0.3627(3) 0.2197(2) 0.0255(6) Uani 1 1 d . . . . .
H14 H 0.288370 -0.347174 0.232854 0.031 Uiso 1 1 calc R U . . .
C15 C -0.0245(3) -0.0345(3) 0.2961(2) 0.0240(6) Uani 1 1 d . . . . .
C16 C -0.0180(3) -0.0809(3) 0.1831(2) 0.0244(6) Uani 1 1 d . . . . .
C17 C -0.1344(4) -0.0829(3) 0.1206(2) 0.0283(7) Uani 1 1 d . . . . .
H17 H -0.221867 -0.056357 0.147134 0.034 Uiso 1 1 calc R U . . .
C18 C -0.1184(4) -0.1256(3) 0.0163(2) 0.0302(7) Uani 1 1 d . . . . .
C19 C 0.0076(4) -0.1692(3) -0.0267(2) 0.0323(7) Uani 1 1 d . . . . .
H19 H 0.015681 -0.199006 -0.096233 0.039 Uiso 1 1 calc R U . . .
C20 C 0.1209(4) -0.1663(3) 0.0389(3) 0.0316(7) Uani 1 1 d . . . . .
C21 C 0.1126(4) -0.1227(3) 0.1423(2) 0.0300(7) Uani 1 1 d . . . . .
H21 H 0.191991 -0.121040 0.184034 0.036 Uiso 1 1 calc R U . . .
N1 N 0.1502(4) 0.6840(3) 0.6873(2) 0.0369(7) Uani 1 1 d . . . . .
N2 N -0.3512(3) 0.5165(3) 0.6083(2) 0.0408(8) Uani 1 1 d . . . . .
N3 N 0.3006(3) -0.5611(3) 0.1044(2) 0.0392(7) Uani 1 1 d . . . . .
N4 N 0.8168(3) -0.4311(3) 0.1463(3) 0.0440(8) Uani 1 1 d . . . . .
N5 N 0.2608(4) -0.2083(3) -0.0033(3) 0.0448(8) Uani 1 1 d . . . . .
N6 N -0.2381(4) -0.1213(3) -0.0515(2) 0.0393(7) Uani 1 1 d . . . . .
O1 O 0.1812(2) 0.23343(19) 0.53359(19) 0.0338(5) Uani 1 1 d . . . . .
O2 O -0.0389(2) 0.14677(19) 0.53252(17) 0.0297(5) Uani 1 1 d . . . . .
O1W O 0.5251(5) 0.0674(6) 0.2083(3) 0.1138(18) Uani 1 1 d D . . . .
H11W H 0.481(8) 0.000(4) 0.184(6) 0.137 Uiso 1 1 d D U . . .
H12W H 0.496(8) 0.097(6) 0.165(4) 0.137 Uiso 1 1 d D U . . .
O3 O 0.2767(3) 0.6644(2) 0.6874(2) 0.0542(8) Uani 1 1 d . . . . .
O2W O 0.3816(3) 0.1319(2) 0.38824(19) 0.0341(5) Uani 1 1 d D . . . .
H21W H 0.361(4) 0.202(2) 0.396(3) 0.041 Uiso 1 1 d D U . . .
H22W H 0.401(4) 0.111(3) 0.3299(16) 0.041 Uiso 1 1 d D U . . .
O4 O 0.1060(3) 0.7858(2) 0.7137(2) 0.0537(8) Uani 1 1 d . . . . .
O3W O 0.3239(3) -0.1378(2) 0.56847(19) 0.0328(5) Uani 1 1 d D . . . .
H31W H 0.291(4) -0.140(3) 0.6229(19) 0.039 Uiso 1 1 d D U . . .
H32W H 0.409(2) -0.142(3) 0.574(3) 0.039 Uiso 1 1 d D U . . .
O5 O -0.3873(3) 0.6204(3) 0.6437(3) 0.0685(10) Uani 1 1 d . . . . .
O6 O -0.4343(3) 0.4275(3) 0.5725(2) 0.0543(8) Uani 1 1 d . . . . .
O7 O 0.3342(2) -0.1382(2) 0.35531(17) 0.0322(5) Uani 1 1 d . . . . .
O8 O 0.4378(2) 0.1113(2) 0.59028(17) 0.0316(5) Uani 1 1 d . . . . .
O9 O 0.1818(3) -0.5507(3) 0.1405(2) 0.0586(8) Uani 1 1 d . . . . .
O10 O 0.3296(3) -0.6447(2) 0.0312(2) 0.0563(8) Uani 1 1 d . . . . .
O11 O 0.9114(3) -0.3557(3) 0.1905(2) 0.0544(8) Uani 1 1 d . . . . .
O12 O 0.8383(3) -0.5228(3) 0.0801(3) 0.0916(14) Uani 1 1 d . . . . .
O13 O 0.0915(2) 0.0095(2) 0.34233(16) 0.0302(5) Uani 1 1 d . . . . .
O14 O 0.1455(2) 0.0451(2) 0.66466(16) 0.0277(5) Uani 1 1 d . . . . .
O15 O 0.3527(3) -0.2215(3) 0.0533(2) 0.0695(10) Uani 1 1 d . . . . .
O16 O 0.2749(4) -0.2281(3) -0.0934(2) 0.0713(10) Uani 1 1 d . . . . .
O17 O -0.3441(3) -0.0706(3) -0.0153(2) 0.0554(8) Uani 1 1 d . . . . .
O18 O -0.2252(4) -0.1668(3) -0.1420(2) 0.0611(8) Uani 1 1 d . . . . .
Nd1 Nd 0.22809(2) 0.01491(2) 0.49034(2) 0.02022(6) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.255(3) . ?
C1 O2 1.256(3) . ?
C1 C2 1.502(4) . ?
C2 C7 1.389(4) . ?
C2 C3 1.393(4) . ?
C3 C4 1.383(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.373(5) . ?
C4 N1 1.475(4) . ?
C5 C6 1.386(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.382(4) . ?
C6 N2 1.475(4) . ?
C7 H7 0.9300 . ?
C8 O8 1.245(4) 2_656 ?
C8 O7 1.260(3) . ?
C8 C9 1.495(4) . ?
C9 C14 1.390(4) . ?
C9 C10 1.403(4) . ?
C10 C11 1.376(4) . ?
C10 H10 0.9300 . ?
C11 C12 1.382(5) . ?
C11 N4 1.476(4) . ?
C12 C13 1.379(5) . ?
C12 H12 0.9300 . ?
C13 C14 1.375(4) . ?
C13 N3 1.472(4) . ?
C14 H14 0.9300 . ?
C15 O13 1.246(4) . ?
C15 O14 1.264(3) 2_556 ?
C15 C16 1.504(4) . ?
C16 C17 1.376(4) . ?
C16 C21 1.400(4) . ?
C17 C18 1.397(4) . ?
C17 H17 0.9300 . ?
C18 C19 1.378(5) . ?
C18 N6 1.463(5) . ?
C19 C20 1.377(5) . ?
C19 H19 0.9300 . ?
C20 C21 1.378(4) . ?
C20 N5 1.485(4) . ?
C21 H21 0.9300 . ?
N1 O3 1.214(4) . ?
N1 O4 1.224(4) . ?
N2 O6 1.216(4) . ?
N2 O5 1.225(4) . ?
N3 O9 1.214(4) . ?
N3 O10 1.228(4) . ?
N4 O12 1.212(4) . ?
N4 O11 1.216(4) . ?
N5 O15 1.201(4) . ?
N5 O16 1.211(4) . ?
N6 O17 1.217(4) . ?
N6 O18 1.222(4) . ?
O1 Nd1 2.478(2) . ?
O2 Nd1 2.413(2) 2_556 ?
O1W H11W 0.82(2) . ?
O1W H12W 0.81(2) . ?
O2W Nd1 2.579(2) . ?
O2W H21W 0.825(18) . ?
O2W H22W 0.799(18) . ?
O3W Nd1 2.513(2) . ?
O3W H31W 0.818(18) . ?
O3W H32W 0.796(18) . ?
O7 Nd1 2.440(2) . ?
O8 Nd1 2.392(2) . ?
O13 Nd1 2.385(2) . ?
O14 Nd1 2.470(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 C1 O2 123.0(3) . . ?
O1 C1 C2 117.5(3) . . ?
O2 C1 C2 119.5(3) . . ?
C7 C2 C3 120.2(3) . . ?
C7 C2 C1 121.6(3) . . ?
C3 C2 C1 118.2(3) . . ?
C4 C3 C2 118.3(3) . . ?
C4 C3 H3 120.9 . . ?
C2 C3 H3 120.9 . . ?
C5 C4 C3 123.6(3) . . ?
C5 C4 N1 118.4(3) . . ?
C3 C4 N1 118.0(3) . . ?
C4 C5 C6 116.4(3) . . ?
C4 C5 H5 121.8 . . ?
C6 C5 H5 121.8 . . ?
C7 C6 C5 122.8(3) . . ?
C7 C6 N2 118.8(3) . . ?
C5 C6 N2 118.4(3) . . ?
C6 C7 C2 118.8(3) . . ?
C6 C7 H7 120.6 . . ?
C2 C7 H7 120.6 . . ?
O8 C8 O7 124.3(3) 2_656 . ?
O8 C8 C9 118.5(3) 2_656 . ?
O7 C8 C9 117.1(3) . . ?
C14 C9 C10 119.5(3) . . ?
C14 C9 C8 120.3(3) . . ?
C10 C9 C8 120.0(3) . . ?
C11 C10 C9 118.8(3) . . ?
C11 C10 H10 120.6 . . ?
C9 C10 H10 120.6 . . ?
C10 C11 C12 122.9(3) . . ?
C10 C11 N4 118.8(3) . . ?
C12 C11 N4 118.3(3) . . ?
C13 C12 C11 116.6(3) . . ?
C13 C12 H12 121.7 . . ?
C11 C12 H12 121.7 . . ?
C14 C13 C12 123.2(3) . . ?
C14 C13 N3 118.6(3) . . ?
C12 C13 N3 118.2(3) . . ?
C13 C14 C9 118.9(3) . . ?
C13 C14 H14 120.6 . . ?
C9 C14 H14 120.6 . . ?
O13 C15 O14 126.3(3) . 2_556 ?
O13 C15 C16 116.3(3) . . ?
O14 C15 C16 117.4(3) 2_556 . ?
C17 C16 C21 120.2(3) . . ?
C17 C16 C15 122.3(3) . . ?
C21 C16 C15 117.5(3) . . ?
C16 C17 C18 118.6(3) . . ?
C16 C17 H17 120.7 . . ?
C18 C17 H17 120.7 . . ?
C19 C18 C17 122.9(3) . . ?
C19 C18 N6 117.7(3) . . ?
C17 C18 N6 119.4(3) . . ?
C20 C19 C18 116.5(3) . . ?
C20 C19 H19 121.8 . . ?
C18 C19 H19 121.8 . . ?
C19 C20 C21 123.3(3) . . ?
C19 C20 N5 118.8(3) . . ?
C21 C20 N5 117.9(3) . . ?
C20 C21 C16 118.6(3) . . ?
C20 C21 H21 120.7 . . ?
C16 C21 H21 120.7 . . ?
O3 N1 O4 124.0(3) . . ?
O3 N1 C4 117.9(3) . . ?
O4 N1 C4 118.1(3) . . ?
O6 N2 O5 124.7(3) . . ?
O6 N2 C6 118.0(3) . . ?
O5 N2 C6 117.3(3) . . ?
O9 N3 O10 124.0(3) . . ?
O9 N3 C13 118.6(3) . . ?
O10 N3 C13 117.4(3) . . ?
O12 N4 O11 124.2(3) . . ?
O12 N4 C11 117.9(3) . . ?
O11 N4 C11 117.9(3) . . ?
O15 N5 O16 123.8(3) . . ?
O15 N5 C20 118.5(3) . . ?
O16 N5 C20 117.6(3) . . ?
O17 N6 O18 123.4(3) . . ?
O17 N6 C18 118.6(3) . . ?
O18 N6 C18 118.0(3) . . ?
C1 O1 Nd1 107.00(18) . . ?
C1 O2 Nd1 173.3(2) . 2_556 ?
H11W O1W H12W 94(7) . . ?
Nd1 O2W H21W 114(3) . . ?
Nd1 O2W H22W 129(3) . . ?
H21W O2W H22W 102(4) . . ?
Nd1 O3W H31W 117(3) . . ?
Nd1 O3W H32W 120(3) . . ?
H31W O3W H32W 106(4) . . ?
C8 O7 Nd1 127.59(19) . . ?
C8 O8 Nd1 173.4(2) 2_656 . ?
C15 O13 Nd1 141.7(2) . . ?
C15 O14 Nd1 134.7(2) 2_556 . ?
O13 Nd1 O8 143.06(8) . . ?
O13 Nd1 O2 72.72(8) . 2_556 ?
O8 Nd1 O2 144.01(8) . 2_556 ?
O13 Nd1 O7 75.45(8) . . ?
O8 Nd1 O7 101.28(7) . . ?
O2 Nd1 O7 81.56(7) 2_556 . ?
O13 Nd1 O14 128.84(7) . . ?
O8 Nd1 O14 77.16(7) . . ?
O2 Nd1 O14 78.28(7) 2_556 . ?
O7 Nd1 O14 140.09(8) . . ?
O13 Nd1 O1 81.55(8) . . ?
O8 Nd1 O1 77.76(8) . . ?
O2 Nd1 O1 123.12(7) 2_556 . ?
O7 Nd1 O1 139.04(8) . . ?
O14 Nd1 O1 80.31(8) . . ?
O13 Nd1 O3W 136.78(8) . . ?
O8 Nd1 O3W 72.65(8) . . ?
O2 Nd1 O3W 74.07(8) 2_556 . ?
O7 Nd1 O3W 73.00(8) . . ?
O14 Nd1 O3W 68.51(8) . . ?
O1 Nd1 O3W 140.74(8) . . ?
O13 Nd1 O2W 72.18(8) . . ?
O8 Nd1 O2W 71.71(8) . . ?
O2 Nd1 O2W 140.86(8) 2_556 . ?
O7 Nd1 O2W 73.38(8) . . ?
O14 Nd1 O2W 138.86(8) . . ?
O1 Nd1 O2W 67.46(8) . . ?
O3W Nd1 O2W 124.00(8) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 C7 167.0(3) . . . . ?
O2 C1 C2 C7 -13.7(5) . . . . ?
O1 C1 C2 C3 -12.4(4) . . . . ?
O2 C1 C2 C3 167.0(3) . . . . ?
C7 C2 C3 C4 1.1(5) . . . . ?
C1 C2 C3 C4 -179.5(3) . . . . ?
C2 C3 C4 C5 -1.2(5) . . . . ?
C2 C3 C4 N1 -179.0(3) . . . . ?
C3 C4 C5 C6 -0.5(5) . . . . ?
N1 C4 C5 C6 177.3(3) . . . . ?
C4 C5 C6 C7 2.4(5) . . . . ?
C4 C5 C6 N2 -178.7(3) . . . . ?
C5 C6 C7 C2 -2.5(5) . . . . ?
N2 C6 C7 C2 178.6(3) . . . . ?
C3 C2 C7 C6 0.6(5) . . . . ?
C1 C2 C7 C6 -178.7(3) . . . . ?
O8 C8 C9 C14 160.9(3) 2_656 . . . ?
O7 C8 C9 C14 -16.9(4) . . . . ?
O8 C8 C9 C10 -15.9(4) 2_656 . . . ?
O7 C8 C9 C10 166.2(3) . . . . ?
C14 C9 C10 C11 -1.4(5) . . . . ?
C8 C9 C10 C11 175.5(3) . . . . ?
C9 C10 C11 C12 -0.8(5) . . . . ?
C9 C10 C11 N4 178.8(3) . . . . ?
C10 C11 C12 C13 1.3(5) . . . . ?
N4 C11 C12 C13 -178.2(3) . . . . ?
C11 C12 C13 C14 0.3(5) . . . . ?
C11 C12 C13 N3 -178.9(3) . . . . ?
C12 C13 C14 C9 -2.4(5) . . . . ?
N3 C13 C14 C9 176.8(3) . . . . ?
C10 C9 C14 C13 2.9(5) . . . . ?
C8 C9 C14 C13 -174.0(3) . . . . ?
O13 C15 C16 C17 -151.7(3) . . . . ?
O14 C15 C16 C17 29.2(4) 2_556 . . . ?
O13 C15 C16 C21 28.2(4) . . . . ?
O14 C15 C16 C21 -150.9(3) 2_556 . . . ?
C21 C16 C17 C18 -0.9(5) . . . . ?
C15 C16 C17 C18 179.0(3) . . . . ?
C16 C17 C18 C19 2.0(5) . . . . ?
C16 C17 C18 N6 -176.2(3) . . . . ?
C17 C18 C19 C20 -1.4(5) . . . . ?
N6 C18 C19 C20 176.7(3) . . . . ?
C18 C19 C20 C21 -0.1(5) . . . . ?
C18 C19 C20 N5 -178.0(3) . . . . ?
C19 C20 C21 C16 1.0(5) . . . . ?
N5 C20 C21 C16 178.9(3) . . . . ?
C17 C16 C21 C20 -0.5(5) . . . . ?
C15 C16 C21 C20 179.6(3) . . . . ?
C5 C4 N1 O3 -179.8(3) . . . . ?
C3 C4 N1 O3 -1.8(5) . . . . ?
C5 C4 N1 O4 -0.6(5) . . . . ?
C3 C4 N1 O4 177.3(3) . . . . ?
C7 C6 N2 O6 -2.9(5) . . . . ?
C5 C6 N2 O6 178.2(3) . . . . ?
C7 C6 N2 O5 175.1(3) . . . . ?
C5 C6 N2 O5 -3.8(5) . . . . ?
C14 C13 N3 O9 -14.0(5) . . . . ?
C12 C13 N3 O9 165.2(4) . . . . ?
C14 C13 N3 O10 167.0(3) . . . . ?
C12 C13 N3 O10 -13.8(5) . . . . ?
C10 C11 N4 O12 -176.0(4) . . . . ?
C12 C11 N4 O12 3.6(6) . . . . ?
C10 C11 N4 O11 2.8(5) . . . . ?
C12 C11 N4 O11 -177.7(4) . . . . ?
C19 C20 N5 O15 -169.9(4) . . . . ?
C21 C20 N5 O15 12.1(5) . . . . ?
C19 C20 N5 O16 9.5(5) . . . . ?
C21 C20 N5 O16 -168.5(4) . . . . ?
C19 C18 N6 O17 -171.9(3) . . . . ?
C17 C18 N6 O17 6.4(5) . . . . ?
C19 C18 N6 O18 6.7(5) . . . . ?
C17 C18 N6 O18 -175.1(3) . . . . ?
O2 C1 O1 Nd1 -4.4(4) . . . . ?
C2 C1 O1 Nd1 174.9(2) . . . . ?
O8 C8 O7 Nd1 -8.0(5) 2_656 . . . ?
C9 C8 O7 Nd1 169.70(19) . . . . ?
O14 C15 O13 Nd1 39.8(5) 2_556 . . . ?
C16 C15 O13 Nd1 -139.2(3) . . . . ?

_refine_diff_density_max         1.225
_refine_diff_density_min         -1.142
_refine_diff_density_rms         0.132

####################################################################### 
# 
# 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_Eu_24DNB
_database_code_depnum_ccdc_archive 'CCDC 1584544'
_audit_update_record             
;
2018-02-08 deposited with the CCDC.
2018-02-23 downloaded from the CCDC.
;
_audit_creation_date             2018-01-10
_audit_creation_method           
;
Olex2 1.2-dev
(compiled 2017.12.08 svn.r3473 for OlexSys, GUI svn.r5356)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C42 H30 Eu2 N12 O42'
_chemical_formula_sum            'C42 H30 Eu2 N12 O42'
_chemical_formula_weight         1678.66
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 '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'

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

_cell_length_a                   8.893(3)
_cell_length_b                   13.631(4)
_cell_length_c                   14.316(4)
_cell_angle_alpha                63.296(11)
_cell_angle_beta                 79.353(13)
_cell_angle_gamma                72.448(11)
_cell_volume                     1475.6(8)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    8401
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      32.99
_cell_measurement_theta_min      2.55
_shelx_estimated_absorpt_T_max   0.776
_shelx_estimated_absorpt_T_min   0.677
_exptl_absorpt_coefficient_mu    2.230
_exptl_absorpt_correction_T_max  0.781
_exptl_absorpt_correction_T_min  0.672
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   
'SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.889
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Rectangular
_exptl_crystal_F_000             828
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_unetI/netI     0.0346
_diffrn_reflns_Laue_measured_fraction_full 0.937
_diffrn_reflns_Laue_measured_fraction_max 0.931
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19834
_diffrn_reflns_point_group_measured_fraction_full 0.937
_diffrn_reflns_point_group_measured_fraction_max 0.931
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.499
_diffrn_reflns_theta_min         1.727
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.937
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5120
_reflns_number_total             5685
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'Sir-92 (Altomare et al., 1993)'
_refine_diff_density_max         1.897
_refine_diff_density_min         -2.148
_refine_diff_density_rms         0.206
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         5685
_refine_ls_number_restraints     51
_refine_ls_R_factor_all          0.0517
_refine_ls_R_factor_gt           0.0378
_refine_ls_restrained_S_all      1.159
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+15.9613P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0844
_refine_ls_wR_factor_ref         0.1108
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H,H) groups
2. Restrained distances
 O1W-H1WA = O1W-H1WB
 0.82 with sigma of 0.02
 O2W-H2WA = O2W-H2WB
 0.82 with sigma of 0.02
 O3W-H3WA = O3W-H3WB
 0.82 with sigma of 0.02
 H1WA-H1WB
 1.28 with sigma of 0.02
 H2WA-H2WB
 1.28 with sigma of 0.02
 H3WA-H3WB
 1.28 with sigma of 0.02
 C17-N5 \\sim C17-N5A
 with sigma of 0.02
 N5-O15 \\sim N5A-O15A
 with sigma of 0.02
 N5-O16' \\sim N5A-O16
 with sigma of 0.02
 C17-O15 \\sim C17-O15A
 with sigma of 0.04
 C17-O16' \\sim C17-O16
 with sigma of 0.04
 O15-O16' \\sim O15A-O16
 with sigma of 0.04
3. Rigid body (RIGU) restrains
 N5A, O15A, O16, C17
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N5, O16', O15, C17
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Fixed Sof: N5(0.25) O15(0.25) O16'(0.25) N5A(0.75) O15A(0.75) O16(0.75)
5.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C7(H7), C11(H11), C13(H13), C14(H14), C18(H18), C20(H20),
 C21(H21)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.8712(7) 0.2261(5) 0.9434(5) 0.0220(13) Uani 1 1 d . . . . .
C2 C 0.7971(8) 0.3511(5) 0.9101(5) 0.0236(13) Uani 1 1 d . . . . .
C3 C 0.6399(8) 0.3962(5) 0.8910(5) 0.0244(13) Uani 1 1 d . . . . .
C4 C 0.5639(9) 0.5071(5) 0.8697(6) 0.0310(15) Uani 1 1 d . . . . .
H4 H 0.456395 0.534945 0.858839 0.037 Uiso 1 1 calc R . . . .
C5 C 0.6545(9) 0.5748(5) 0.8653(5) 0.0307(15) Uani 1 1 d . . . . .
C6 C 0.8120(9) 0.5358(6) 0.8817(6) 0.0356(17) Uani 1 1 d . . . . .
H6 H 0.870029 0.584035 0.878007 0.043 Uiso 1 1 calc R . . . .
C7 C 0.8838(9) 0.4231(6) 0.9039(6) 0.0323(15) Uani 1 1 d . . . . .
H7 H 0.991284 0.395398 0.914838 0.039 Uiso 1 1 calc R . . . .
C8 C 0.8140(7) 0.0030(5) 0.8804(5) 0.0231(13) Uani 1 1 d . . . . .
C9 C 0.8002(8) 0.0166(6) 0.7708(5) 0.0299(15) Uani 1 1 d . . . . .
C10 C 0.8681(9) -0.0688(7) 0.7364(6) 0.0366(17) Uani 1 1 d . . . . .
C11 C 0.8506(12) -0.0536(8) 0.6385(7) 0.053(2) Uani 1 1 d . . . . .
H11 H 0.895665 -0.111632 0.616819 0.063 Uiso 1 1 calc R . . . .
C12 C 0.7659(12) 0.0478(10) 0.5731(6) 0.057(3) Uani 1 1 d . . . . .
C13 C 0.6939(12) 0.1345(9) 0.6020(7) 0.059(3) Uani 1 1 d . . . . .
H13 H 0.633686 0.202598 0.555802 0.071 Uiso 1 1 calc R . . . .
C14 C 0.7134(11) 0.1178(7) 0.7032(6) 0.0456(19) Uani 1 1 d . . . . .
H14 H 0.667137 0.175782 0.724722 0.055 Uiso 1 1 calc R . . . .
C15 C 0.8687(12) -0.2690(7) 1.3367(6) 0.050(2) Uani 1 1 d . . . . .
C16 C 0.9704(11) -0.3240(6) 1.4257(6) 0.045(2) Uani 1 1 d . . . . .
C17 C 0.9245(12) -0.3278(8) 1.5243(7) 0.0514(19) Uani 1 1 d D U . . .
C18 C 1.0280(13) -0.3757(8) 1.6041(7) 0.059(3) Uani 1 1 d . . . . .
H18 H 0.993998 -0.376322 1.669762 0.070 Uiso 1 1 calc R . . . .
C19 C 1.1784(13) -0.4209(7) 1.5823(8) 0.060(3) Uani 1 1 d . . . . .
C20 C 1.2316(14) -0.4210(9) 1.4874(10) 0.073(3) Uani 1 1 d . . . . .
H20 H 1.337038 -0.453593 1.475374 0.087 Uiso 1 1 calc R . . . .
C21 C 1.1279(14) -0.3722(9) 1.4087(8) 0.065(3) Uani 1 1 d . . . . .
H21 H 1.164330 -0.371592 1.343280 0.078 Uiso 1 1 calc R . . . .
N1 N 0.5458(7) 0.3266(5) 0.8875(5) 0.0331(14) Uani 1 1 d . . . . .
N2 N 0.5741(9) 0.6937(5) 0.8418(5) 0.0414(16) Uani 1 1 d . . . . .
N3 N 0.9538(10) -0.1806(6) 0.8088(7) 0.0518(19) Uani 1 1 d . . . . .
N4 N 0.7443(14) 0.0634(11) 0.4654(7) 0.083(3) Uani 1 1 d . . . . .
N5 N 0.756(3) -0.306(4) 1.553(2) 0.077(14) Uani 0.25 1 d D U P A 1
N6 N 1.2893(16) -0.4709(8) 1.6671(10) 0.087(3) Uani 1 1 d . . . . .
O1 O 0.7886(5) 0.1622(3) 1.0046(3) 0.0240(9) Uani 1 1 d . . . . .
O2 O 1.0073(6) 0.1998(4) 0.9073(4) 0.0306(11) Uani 1 1 d . . . . .
O3 O 0.5973(8) 0.2791(5) 0.8299(6) 0.0564(17) Uani 1 1 d . . . . .
O4 O 0.4239(7) 0.3221(5) 0.9405(5) 0.0523(15) Uani 1 1 d . . . . .
O5 O 0.4328(8) 0.7214(5) 0.8395(6) 0.0627(19) Uani 1 1 d . . . . .
O6 O 0.6550(8) 0.7578(4) 0.8269(5) 0.0584(18) Uani 1 1 d . . . . .
O7 O 0.6986(6) -0.0103(5) 0.9438(4) 0.0348(11) Uani 1 1 d . . . . .
O8 O 0.9359(5) 0.0114(4) 0.9031(4) 0.0277(10) Uani 1 1 d . . . . .
O9 O 0.9338(9) -0.2052(5) 0.9009(5) 0.0636(19) Uani 1 1 d . . . . .
O10 O 1.0369(11) -0.2439(7) 0.7706(7) 0.092(3) Uani 1 1 d . . . . .
O11 O 0.8025(15) -0.0190(9) 0.4454(7) 0.114(4) Uani 1 1 d . . . . .
O12 O 0.6836(15) 0.1571(11) 0.4057(7) 0.135(5) Uani 1 1 d . . . . .
O13 O 0.8071(12) -0.3290(6) 1.3206(6) 0.087(3) Uani 1 1 d . . . . .
O14 O 0.8604(7) -0.1655(4) 1.2786(4) 0.0452(14) Uani 1 1 d . . . . .
O15 O 0.704(4) -0.355(4) 1.640(2) 0.112(15) Uani 0.25 1 d D U P A 1
O16' O 0.674(3) -0.211(3) 1.491(2) 0.059(6) Uani 0.25 1 d D U P A 1
O17 O 1.2365(15) -0.4810(9) 1.7532(8) 0.115(4) Uani 1 1 d . . . . .
O18 O 1.4268(14) -0.5011(11) 1.6452(10) 0.137(5) Uani 1 1 d . . . . .
O1W O 0.6599(7) -0.1726(4) 1.1530(5) 0.0422(13) Uani 1 1 d D . . . .
H1WA H 0.616(10) -0.184(6) 1.115(5) 0.051 Uiso 1 1 d DR . . . .
H1WB H 0.689(10) -0.235(3) 1.200(4) 0.051 Uiso 1 1 d DR . . . .
O2W O 0.5352(6) 0.0559(5) 1.1133(5) 0.0425(14) Uani 1 1 d D . . . .
H2WA H 0.471(7) 0.050(7) 1.082(6) 0.051 Uiso 1 1 d DR . . . .
H2WB H 0.485(8) 0.107(5) 1.130(7) 0.051 Uiso 1 1 d DR . . . .
O3W O 0.7754(8) 0.0562(4) 1.2225(4) 0.0430(14) Uani 1 1 d D . . . .
H3WA H 0.715(9) 0.118(3) 1.212(5) 0.052 Uiso 1 1 d DR . . . .
H3WB H 0.767(10) 0.022(5) 1.2861(18) 0.052 Uiso 1 1 d DR . . . .
Eu1 Eu 0.81017(4) -0.03645(2) 1.10501(2) 0.01888(10) Uani 1 1 d . . . . .
N5A N 0.7642(14) -0.2735(14) 1.5477(11) 0.066(4) Uani 0.75 1 d D U P A 2
O15A O 0.7309(15) -0.2627(13) 1.6270(9) 0.096(4) Uani 0.75 1 d D U P A 2
O16 O 0.6666(16) -0.2543(15) 1.4830(11) 0.106(6) Uani 0.75 1 d D U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.508(8) . ?
C1 O1 1.235(7) . ?
C1 O2 1.239(8) . ?
C2 C3 1.370(9) . ?
C2 C7 1.385(9) . ?
C3 C4 1.371(9) . ?
C3 N1 1.463(8) . ?
C4 H4 0.9300 . ?
C4 C5 1.372(10) . ?
C5 C6 1.364(11) . ?
C5 N2 1.467(8) . ?
C6 H6 0.9300 . ?
C6 C7 1.383(9) . ?
C7 H7 0.9300 . ?
C8 C9 1.520(9) . ?
C8 O7 1.237(8) . ?
C8 O8 1.238(7) . ?
C8 Eu1 3.007(6) . ?
C9 C10 1.393(10) . ?
C9 C14 1.367(11) . ?
C10 C11 1.354(11) . ?
C10 N3 1.466(11) . ?
C11 H11 0.9300 . ?
C11 C12 1.351(14) . ?
C12 C13 1.366(14) . ?
C12 N4 1.499(11) . ?
C13 H13 0.9300 . ?
C13 C14 1.398(11) . ?
C14 H14 0.9300 . ?
C15 C16 1.470(12) . ?
C15 O13 1.229(11) . ?
C15 O14 1.262(9) . ?
C16 C17 1.377(12) . ?
C16 C21 1.384(14) . ?
C17 C18 1.390(12) . ?
C17 N5 1.46(2) . ?
C17 N5A 1.450(14) . ?
C18 H18 0.9300 . ?
C18 C19 1.337(15) . ?
C19 C20 1.354(15) . ?
C19 N6 1.485(13) . ?
C20 H20 0.9300 . ?
C20 C21 1.379(15) . ?
C21 H21 0.9300 . ?
N1 O3 1.212(8) . ?
N1 O4 1.204(8) . ?
N2 O5 1.200(9) . ?
N2 O6 1.218(9) . ?
N3 O9 1.198(10) . ?
N3 O10 1.216(10) . ?
N4 O11 1.224(14) . ?
N4 O12 1.194(14) . ?
N5 O15 1.19(2) . ?
N5 O16' 1.28(3) . ?
N6 O17 1.196(16) . ?
N6 O18 1.197(16) . ?
O1 Eu1 2.393(4) . ?
O2 Eu1 2.386(4) 2_757 ?
O7 Eu1 2.516(5) . ?
O8 Eu1 2.358(4) 2_757 ?
O8 Eu1 2.753(5) . ?
O14 Eu1 2.341(5) . ?
O1W H1WA 0.81(2) . ?
O1W H1WB 0.81(2) . ?
O1W Eu1 2.390(5) . ?
O2W H2WA 0.82(2) . ?
O2W H2WB 0.82(2) . ?
O2W Eu1 2.398(5) . ?
O3W H3WA 0.82(2) . ?
O3W H3WB 0.82(2) . ?
O3W Eu1 2.449(5) . ?
Eu1 Eu1 4.1247(12) 2_757 ?
N5A O15A 1.182(17) . ?
N5A O16 1.273(19) . ?

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 C1 C2 115.6(5) . . ?
O1 C1 O2 128.0(6) . . ?
O2 C1 C2 116.4(5) . . ?
C3 C2 C1 121.3(6) . . ?
C3 C2 C7 117.7(6) . . ?
C7 C2 C1 120.9(6) . . ?
C2 C3 C4 123.5(6) . . ?
C2 C3 N1 120.0(5) . . ?
C4 C3 N1 116.4(6) . . ?
C3 C4 H4 121.7 . . ?
C3 C4 C5 116.6(7) . . ?
C5 C4 H4 121.7 . . ?
C4 C5 N2 116.8(7) . . ?
C6 C5 C4 122.9(6) . . ?
C6 C5 N2 120.3(6) . . ?
C5 C6 H6 120.6 . . ?
C5 C6 C7 118.7(6) . . ?
C7 C6 H6 120.6 . . ?
C2 C7 H7 119.7 . . ?
C6 C7 C2 120.6(7) . . ?
C6 C7 H7 119.7 . . ?
C9 C8 Eu1 173.4(4) . . ?
O7 C8 C9 118.7(6) . . ?
O7 C8 O8 121.2(6) . . ?
O7 C8 Eu1 55.2(3) . . ?
O8 C8 C9 120.0(6) . . ?
O8 C8 Eu1 66.3(3) . . ?
C10 C9 C8 123.7(7) . . ?
C14 C9 C8 117.7(6) . . ?
C14 C9 C10 118.6(7) . . ?
C9 C10 N3 120.0(7) . . ?
C11 C10 C9 121.7(8) . . ?
C11 C10 N3 118.2(8) . . ?
C10 C11 H11 120.8 . . ?
C12 C11 C10 118.3(8) . . ?
C12 C11 H11 120.8 . . ?
C11 C12 C13 123.0(8) . . ?
C11 C12 N4 118.2(10) . . ?
C13 C12 N4 118.7(10) . . ?
C12 C13 H13 121.0 . . ?
C12 C13 C14 117.9(9) . . ?
C14 C13 H13 121.0 . . ?
C9 C14 C13 120.3(8) . . ?
C9 C14 H14 119.8 . . ?
C13 C14 H14 119.8 . . ?
O13 C15 C16 117.5(7) . . ?
O13 C15 O14 125.0(9) . . ?
O14 C15 C16 117.3(8) . . ?
C17 C16 C15 125.7(9) . . ?
C17 C16 C21 116.5(9) . . ?
C21 C16 C15 117.8(8) . . ?
C16 C17 C18 123.3(10) . . ?
C16 C17 N5 117(2) . . ?
C16 C17 N5A 120.4(10) . . ?
C18 C17 N5 117.6(17) . . ?
C18 C17 N5A 116.2(10) . . ?
C17 C18 H18 121.5 . . ?
C19 C18 C17 117.1(9) . . ?
C19 C18 H18 121.5 . . ?
C18 C19 C20 122.9(10) . . ?
C18 C19 N6 117.1(11) . . ?
C20 C19 N6 120.0(11) . . ?
C19 C20 H20 120.3 . . ?
C19 C20 C21 119.4(11) . . ?
C21 C20 H20 120.3 . . ?
C16 C21 H21 119.5 . . ?
C20 C21 C16 120.9(10) . . ?
C20 C21 H21 119.5 . . ?
O3 N1 C3 116.6(6) . . ?
O4 N1 C3 117.8(6) . . ?
O4 N1 O3 125.5(6) . . ?
O5 N2 C5 118.1(7) . . ?
O5 N2 O6 124.1(6) . . ?
O6 N2 C5 117.8(7) . . ?
O9 N3 C10 118.5(7) . . ?
O9 N3 O10 124.4(9) . . ?
O10 N3 C10 117.1(8) . . ?
O11 N4 C12 116.4(11) . . ?
O12 N4 C12 116.6(11) . . ?
O12 N4 O11 126.7(10) . . ?
O15 N5 C17 122(2) . . ?
O15 N5 O16' 120(3) . . ?
O16' N5 C17 115(3) . . ?
O17 N6 C19 118.5(13) . . ?
O17 N6 O18 123.9(12) . . ?
O18 N6 C19 117.5(14) . . ?
C1 O1 Eu1 139.0(4) . . ?
C1 O2 Eu1 138.6(4) . 2_757 ?
C8 O7 Eu1 101.0(4) . . ?
C8 O8 Eu1 89.4(4) . . ?
C8 O8 Eu1 163.2(4) . 2_757 ?
Eu1 O8 Eu1 107.36(17) 2_757 . ?
C15 O14 Eu1 138.8(6) . . ?
H1WA O1W H1WB 104(3) . . ?
Eu1 O1W H1WA 128(6) . . ?
Eu1 O1W H1WB 118(6) . . ?
H2WA O2W H2WB 103(3) . . ?
Eu1 O2W H2WA 121(5) . . ?
Eu1 O2W H2WB 135(5) . . ?
H3WA O3W H3WB 103(3) . . ?
Eu1 O3W H3WA 123(6) . . ?
Eu1 O3W H3WB 122(6) . . ?
C8 Eu1 Eu1 57.37(12) . 2_757 ?
O1 Eu1 C8 74.59(15) . . ?
O1 Eu1 O7 80.95(16) . . ?
O1 Eu1 O8 68.18(14) . . ?
O1 Eu1 O2W 73.67(18) . . ?
O1 Eu1 O3W 70.16(16) . . ?
O1 Eu1 Eu1 66.26(11) . 2_757 ?
O2 Eu1 C8 74.86(17) 2_757 . ?
O2 Eu1 O1 132.20(15) 2_757 . ?
O2 Eu1 O7 85.57(18) 2_757 . ?
O2 Eu1 O8 68.79(15) 2_757 . ?
O2 Eu1 O1W 74.33(18) 2_757 . ?
O2 Eu1 O2W 144.18(17) 2_757 . ?
O2 Eu1 O3W 133.90(18) 2_757 . ?
O2 Eu1 Eu1 66.43(11) 2_757 2_757 ?
O7 Eu1 C8 23.82(16) . . ?
O7 Eu1 O8 48.05(14) . . ?
O7 Eu1 Eu1 81.09(11) . 2_757 ?
O8 Eu1 C8 24.31(15) . . ?
O8 Eu1 C8 96.95(17) 2_757 . ?
O8 Eu1 O1 74.32(15) 2_757 . ?
O8 Eu1 O2 73.92(16) 2_757 2_757 ?
O8 Eu1 O7 120.63(16) 2_757 . ?
O8 Eu1 O8 72.64(17) 2_757 . ?
O8 Eu1 O1W 144.95(17) 2_757 . ?
O8 Eu1 O2W 141.86(16) 2_757 . ?
O8 Eu1 O3W 77.35(19) 2_757 . ?
O8 Eu1 Eu1 39.58(12) 2_757 2_757 ?
O8 Eu1 Eu1 33.07(9) . 2_757 ?
O14 Eu1 C8 148.10(17) . . ?
O14 Eu1 O1 135.57(16) . . ?
O14 Eu1 O2 75.21(18) . 2_757 ?
O14 Eu1 O7 142.24(18) . . ?
O14 Eu1 O8 85.14(19) . 2_757 ?
O14 Eu1 O8 141.58(17) . . ?
O14 Eu1 O1W 72.7(2) . . ?
O14 Eu1 O2W 103.9(2) . . ?
O14 Eu1 O3W 67.07(18) . . ?
O14 Eu1 Eu1 118.33(16) . 2_757 ?
O1W Eu1 C8 88.76(19) . . ?
O1W Eu1 O1 139.92(17) . . ?
O1W Eu1 O7 70.90(19) . . ?
O1W Eu1 O8 108.74(18) . . ?
O1W Eu1 O2W 71.43(19) . . ?
O1W Eu1 O3W 116.1(2) . . ?
O1W Eu1 Eu1 133.03(16) . 2_757 ?
O2W Eu1 C8 94.0(2) . . ?
O2W Eu1 O7 73.67(19) . . ?
O2W Eu1 O8 113.04(18) . . ?
O2W Eu1 O3W 72.7(2) . . ?
O2W Eu1 Eu1 135.30(16) . 2_757 ?
O3W Eu1 C8 144.54(17) . . ?
O3W Eu1 O7 140.45(18) . . ?
O3W Eu1 O8 133.62(17) . . ?
O3W Eu1 Eu1 109.59(16) . 2_757 ?
O15A N5A C17 120.3(14) . . ?
O15A N5A O16 125.6(12) . . ?
O16 N5A C17 113.5(14) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 173.9(6) . . . . ?
C1 C2 C3 N1 -9.1(9) . . . . ?
C1 C2 C7 C6 -174.7(7) . . . . ?
C2 C1 O1 Eu1 -174.1(4) . . . . ?
C2 C1 O2 Eu1 -167.8(4) . . . 2_757 ?
C2 C3 C4 C5 1.7(11) . . . . ?
C2 C3 N1 O3 -52.4(9) . . . . ?
C2 C3 N1 O4 128.4(7) . . . . ?
C3 C2 C7 C6 1.5(11) . . . . ?
C3 C4 C5 C6 -0.5(11) . . . . ?
C3 C4 C5 N2 179.5(6) . . . . ?
C4 C3 N1 O3 124.8(7) . . . . ?
C4 C3 N1 O4 -54.4(9) . . . . ?
C4 C5 C6 C7 -0.1(12) . . . . ?
C4 C5 N2 O5 8.2(10) . . . . ?
C4 C5 N2 O6 -172.6(7) . . . . ?
C5 C6 C7 C2 -0.4(12) . . . . ?
C6 C5 N2 O5 -171.8(8) . . . . ?
C6 C5 N2 O6 7.4(11) . . . . ?
C7 C2 C3 C4 -2.3(10) . . . . ?
C7 C2 C3 N1 174.7(6) . . . . ?
C8 C9 C10 C11 178.8(7) . . . . ?
C8 C9 C10 N3 2.3(11) . . . . ?
C8 C9 C14 C13 -178.7(8) . . . . ?
C9 C8 O7 Eu1 177.1(5) . . . . ?
C9 C8 O8 Eu1 0.0(18) . . . 2_757 ?
C9 C8 O8 Eu1 -177.9(5) . . . . ?
C9 C10 C11 C12 0.6(13) . . . . ?
C9 C10 N3 O9 16.9(12) . . . . ?
C9 C10 N3 O10 -165.5(8) . . . . ?
C10 C9 C14 C13 0.0(13) . . . . ?
C10 C11 C12 C13 -1.8(15) . . . . ?
C10 C11 C12 N4 -178.9(9) . . . . ?
C11 C10 N3 O9 -159.7(8) . . . . ?
C11 C10 N3 O10 17.9(12) . . . . ?
C11 C12 C13 C14 2.0(16) . . . . ?
C11 C12 N4 O11 1.8(16) . . . . ?
C11 C12 N4 O12 -172.3(12) . . . . ?
C12 C13 C14 C9 -1.0(15) . . . . ?
C13 C12 N4 O11 -175.4(11) . . . . ?
C13 C12 N4 O12 10.4(17) . . . . ?
C14 C9 C10 C11 0.2(12) . . . . ?
C14 C9 C10 N3 -176.3(7) . . . . ?
C15 C16 C17 C18 -176.3(8) . . . . ?
C15 C16 C17 N5 19(3) . . . . ?
C15 C16 C17 N5A -0.8(16) . . . . ?
C15 C16 C21 C20 177.2(9) . . . . ?
C16 C15 O14 Eu1 153.1(7) . . . . ?
C16 C17 C18 C19 -0.8(14) . . . . ?
C16 C17 N5 O15 143(6) . . . . ?
C16 C17 N5 O16' -56(6) . . . . ?
C16 C17 N5A O15A -169.2(14) . . . . ?
C16 C17 N5A O16 19(2) . . . . ?
C17 C16 C21 C20 0.0(15) . . . . ?
C17 C18 C19 C20 0.3(15) . . . . ?
C17 C18 C19 N6 179.3(8) . . . . ?
C18 C17 N5 O15 -22(8) . . . . ?
C18 C17 N5 O16' 138(4) . . . . ?
C18 C17 N5A O15A 7(2) . . . . ?
C18 C17 N5A O16 -164.9(15) . . . . ?
C18 C19 C20 C21 0.3(17) . . . . ?
C18 C19 N6 O17 9.0(15) . . . . ?
C18 C19 N6 O18 -172.6(11) . . . . ?
C19 C20 C21 C16 -0.5(17) . . . . ?
C20 C19 N6 O17 -172.0(11) . . . . ?
C20 C19 N6 O18 6.5(16) . . . . ?
C21 C16 C17 C18 0.7(14) . . . . ?
C21 C16 C17 N5 -164(3) . . . . ?
C21 C16 C17 N5A 176.2(12) . . . . ?
N1 C3 C4 C5 -175.4(6) . . . . ?
N2 C5 C6 C7 179.8(7) . . . . ?
N3 C10 C11 C12 177.2(8) . . . . ?
N4 C12 C13 C14 179.1(9) . . . . ?
N5 C17 C18 C19 164(3) . . . . ?
N6 C19 C20 C21 -178.7(10) . . . . ?
O1 C1 C2 C3 -38.3(9) . . . . ?
O1 C1 C2 C7 137.7(7) . . . . ?
O1 C1 O2 Eu1 13.0(12) . . . 2_757 ?
O2 C1 C2 C3 142.3(7) . . . . ?
O2 C1 C2 C7 -41.6(9) . . . . ?
O2 C1 O1 Eu1 5.1(11) . . . . ?
O7 C8 C9 C10 -104.2(8) . . . . ?
O7 C8 C9 C14 74.4(9) . . . . ?
O7 C8 O8 Eu1 -176.1(10) . . . 2_757 ?
O7 C8 O8 Eu1 6.1(6) . . . . ?
O8 C8 C9 C10 79.7(8) . . . . ?
O8 C8 C9 C14 -101.7(8) . . . . ?
O8 C8 O7 Eu1 -6.8(7) . . . . ?
O13 C15 C16 C17 -96.4(12) . . . . ?
O13 C15 C16 C21 86.7(12) . . . . ?
O13 C15 O14 Eu1 -21.7(17) . . . . ?
O14 C15 C16 C17 88.5(11) . . . . ?
O14 C15 C16 C21 -88.5(11) . . . . ?
Eu1 C8 O8 Eu1 177.9(15) . . . 2_757 ?
N5A C17 C18 C19 -176.5(11) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_Gd_24dnb
_database_code_depnum_ccdc_archive 'CCDC 1584547'
_audit_update_record             
;
2018-02-08 deposited with the CCDC.
2018-02-23 downloaded from the CCDC.
;
_audit_creation_date             2018-01-10
_audit_creation_method           
;
Olex2 1.2-dev
(compiled 2017.12.08 svn.r3473 for OlexSys, GUI svn.r5356)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C42 H30 Gd2 N12 O42'
_chemical_formula_sum            'C42 H30 Gd2 N12 O42'
_chemical_formula_weight         1689.24
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 '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'

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

_cell_length_a                   8.9350(7)
_cell_length_b                   13.6750(12)
_cell_length_c                   14.3180(13)
_cell_angle_alpha                63.305(3)
_cell_angle_beta                 79.447(4)
_cell_angle_gamma                72.332(3)
_cell_volume                     1487.0(2)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    9810
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.03
_cell_measurement_theta_min      2.40
_shelx_estimated_absorpt_T_max   0.767
_shelx_estimated_absorpt_T_min   0.679
_exptl_absorpt_coefficient_mu    2.334
_exptl_absorpt_correction_T_max  0.772
_exptl_absorpt_correction_T_min  0.671
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   
'SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.886
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needles
_exptl_crystal_F_000             830
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0213
_diffrn_reflns_av_unetI/netI     0.0193
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26132
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.044
_diffrn_reflns_theta_min         1.594
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6773
_reflns_number_total             7111
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'Sir-92 (Altomare et al., 1993)'
_refine_diff_density_max         0.678
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       0.00081(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         7111
_refine_ls_number_restraints     51
_refine_ls_R_factor_all          0.0188
_refine_ls_R_factor_gt           0.0174
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0203P)²+0.7963P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0428
_refine_ls_wR_factor_ref         0.0436
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H,H) groups
2. Restrained distances
 O1W-H1WA = O1W-H1WB
 0.82 with sigma of 0.02
 O2W-H2WA = O2W-H2WB
 0.82 with sigma of 0.02
 O3W-H3WA = O3W-H3WB
 0.82 with sigma of 0.02
 H1WA-H1WB
 1.28 with sigma of 0.02
 H2WA-H2WB
 1.28 with sigma of 0.02
 H3WA-H3WB
 1.28 with sigma of 0.02
 C10-N3 \\sim C10-N3A
 with sigma of 0.02
 N3-O9' \\sim N3A-O9'A
 with sigma of 0.02
 N3-O10' \\sim N3A-O9
 with sigma of 0.02
 C10-O9' \\sim C10-O9'A
 with sigma of 0.04
 C10-O10' \\sim C10-O9
 with sigma of 0.04
 O9'-O10' \\sim O9'A-O9
 with sigma of 0.04
3. Rigid body (RIGU) restrains
 N3, O9', O10', C10
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O9, N3A, O9'A, C10
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Fixed Sof: N3(0.75) O9'(0.75) O10'(0.75) O9(0.25) N3A(0.25) O9'A(0.25)
5.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C7(H7), C11(H11), C13(H13), C14(H14), C18(H18), C20(H20),
 C21(H21)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.1272(2) 0.77503(15) 0.55669(15) 0.0244(3) Uani 1 1 d . . . . .
C2 C 0.2016(2) 0.64949(15) 0.59003(15) 0.0259(4) Uani 1 1 d . . . . .
C3 C 0.3600(2) 0.60322(15) 0.60936(15) 0.0267(4) Uani 1 1 d . . . . .
C4 C 0.4363(2) 0.49240(16) 0.63099(16) 0.0313(4) Uani 1 1 d . . . . .
H4 H 0.543073 0.464043 0.642788 0.038 Uiso 1 1 calc R . . . .
C5 C 0.3449(3) 0.42576(16) 0.63415(17) 0.0329(4) Uani 1 1 d . . . . .
C6 C 0.1865(3) 0.46501(18) 0.61806(19) 0.0393(5) Uani 1 1 d . . . . .
H6 H 0.128490 0.417058 0.621866 0.047 Uiso 1 1 calc R . . . .
C7 C 0.1153(2) 0.57770(17) 0.59604(19) 0.0358(5) Uani 1 1 d . . . . .
H7 H 0.008215 0.605596 0.585151 0.043 Uiso 1 1 calc R . . . .
C8 C 0.1340(3) 1.2680(2) 0.16571(18) 0.0470(6) Uani 1 1 d . . . . .
C9 C 0.0284(3) 1.32365(19) 0.07463(19) 0.0454(5) Uani 1 1 d . . . . .
C10 C 0.0756(3) 1.3280(2) -0.0236(2) 0.0517(6) Uani 1 1 d D U . . .
C11 C -0.0264(4) 1.3755(3) -0.1033(2) 0.0623(8) Uani 1 1 d . . . . .
H11 H 0.008270 1.376186 -0.168904 0.075 Uiso 1 1 calc R . . . .
C12 C -0.1777(4) 1.4208(2) -0.0825(2) 0.0611(8) Uani 1 1 d . . . . .
C13 C -0.2321(4) 1.4218(3) 0.0128(3) 0.0745(9) Uani 1 1 d . . . . .
H13 H -0.336905 1.455290 0.024288 0.089 Uiso 1 1 calc R . . . .
C14 C -0.1286(4) 1.3723(3) 0.0917(2) 0.0665(8) Uani 1 1 d . . . . .
H14 H -0.164631 1.371512 0.157189 0.080 Uiso 1 1 calc R . . . .
C15 C 0.1842(2) 0.99671(15) 0.62049(15) 0.0253(4) Uani 1 1 d . . . . .
C16 C 0.1984(2) 0.98352(18) 0.72909(16) 0.0307(4) Uani 1 1 d . . . . .
C17 C 0.1311(3) 1.0684(2) 0.76383(18) 0.0388(5) Uani 1 1 d . . . . .
C18 C 0.1480(3) 1.0538(3) 0.8630(2) 0.0534(6) Uani 1 1 d . . . . .
H18 H 0.101823 1.111364 0.884964 0.064 Uiso 1 1 calc R . . . .
C19 C 0.2346(3) 0.9523(3) 0.9279(2) 0.0583(7) Uani 1 1 d . . . . .
C20 C 0.3056(3) 0.8650(3) 0.8985(2) 0.0610(7) Uani 1 1 d . . . . .
H20 H 0.364787 0.796625 0.944738 0.073 Uiso 1 1 calc R . . . .
C21 C 0.2863(3) 0.8820(2) 0.79816(19) 0.0480(6) Uani 1 1 d . . . . .
H21 H 0.333260 0.824159 0.776801 0.058 Uiso 1 1 calc R . . . .
N1 N 0.4533(2) 0.67343(14) 0.61244(15) 0.0356(4) Uani 1 1 d . . . . .
N2 N 0.4239(3) 0.30653(15) 0.65825(16) 0.0425(4) Uani 1 1 d . . . . .
N3 N 0.2379(6) 1.2730(6) -0.0471(5) 0.0697(16) Uani 0.75 1 d D U P A 1
N4 N -0.2878(4) 1.4711(3) -0.1671(3) 0.0870(10) Uani 1 1 d . . . . .
N5 N 0.0455(3) 1.18057(19) 0.6923(2) 0.0544(6) Uani 1 1 d . . . . .
N6 N 0.2559(4) 0.9357(4) 1.0345(2) 0.0880(10) Uani 1 1 d . . . . .
O1 O -0.00891(15) 0.80121(11) 0.59241(12) 0.0317(3) Uani 1 1 d . . . . .
O2 O 0.21073(15) 0.83852(10) 0.49484(11) 0.0283(3) Uani 1 1 d . . . . .
O3 O 0.4030(2) 0.72043(16) 0.67035(16) 0.0546(5) Uani 1 1 d . . . . .
O4 O 0.5760(2) 0.67807(16) 0.55944(16) 0.0539(5) Uani 1 1 d . . . . .
O5 O 0.5667(2) 0.27852(15) 0.65959(18) 0.0628(5) Uani 1 1 d . . . . .
O6 O 0.3441(2) 0.24275(14) 0.67278(17) 0.0598(5) Uani 1 1 d . . . . .
O7 O 0.1393(2) 1.16554(12) 0.22107(12) 0.0419(4) Uani 1 1 d . . . . .
O8 O 0.1943(4) 1.32835(18) 0.18162(19) 0.0904(9) Uani 1 1 d . . . . .
O9' O 0.3343(9) 1.2526(7) 0.0160(6) 0.122(3) Uani 0.75 1 d D U P A 1
O10' O 0.2695(5) 1.2627(5) -0.1267(3) 0.1046(14) Uani 0.75 1 d D U P A 1
O11 O -0.4257(4) 1.5002(3) -0.1449(3) 0.1394(15) Uani 1 1 d . . . . .
O12 O -0.2349(4) 1.4806(3) -0.2538(3) 0.1158(12) Uani 1 1 d . . . . .
O13 O 0.30002(16) 1.01053(14) 0.55697(11) 0.0361(3) Uani 1 1 d . . . . .
O14 O 0.06227(15) 0.98780(11) 0.59791(11) 0.0303(3) Uani 1 1 d . . . . .
O15 O 0.0643(3) 1.20504(16) 0.60023(17) 0.0692(6) Uani 1 1 d . . . . .
O16 O -0.0388(3) 1.2442(2) 0.7305(2) 0.0960(9) Uani 1 1 d . . . . .
O17 O 0.1987(5) 1.0185(3) 1.0558(2) 0.1234(13) Uani 1 1 d . . . . .
O18 O 0.3191(4) 0.8424(4) 1.0951(2) 0.1423(16) Uani 1 1 d . . . . .
O1W O 0.46486(16) 0.94349(14) 0.38832(16) 0.0455(4) Uani 1 1 d D . . . .
H1WA H 0.536(3) 0.952(2) 0.410(2) 0.055 Uiso 1 1 d DR . . . .
H1WB H 0.508(3) 0.8902(19) 0.374(2) 0.055 Uiso 1 1 d DR . . . .
O2W O 0.34067(19) 1.17162(13) 0.34858(15) 0.0439(4) Uani 1 1 d D . . . .
H2WA H 0.383(3) 1.189(2) 0.3810(18) 0.053 Uiso 1 1 d DR . . . .
H2WB H 0.313(3) 1.2271(19) 0.2966(16) 0.053 Uiso 1 1 d DR . . . .
O3W O 0.2261(2) 0.94398(14) 0.27781(13) 0.0434(4) Uani 1 1 d D . . . .
H3WA H 0.283(3) 0.8817(15) 0.288(2) 0.052 Uiso 1 1 d DR . . . .
H3WB H 0.247(3) 0.9847(18) 0.2182(15) 0.052 Uiso 1 1 d DR . . . .
Gd1 Gd 0.19055(2) 1.03620(2) 0.39544(2) 0.01908(4) Uani 1 1 d . . . . .
O9 O 0.3020(15) 1.3484(16) -0.1394(8) 0.129(6) Uani 0.25 1 d D U P A 2
N3A N 0.2499(15) 1.3054(17) -0.0501(12) 0.076(6) Uani 0.25 1 d D U P A 2
O9'A O 0.327(3) 1.2111(18) 0.0126(18) 0.095(7) Uani 0.25 1 d D U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.518(2) . ?
C1 O1 1.241(2) . ?
C1 O2 1.248(2) . ?
C2 C3 1.386(3) . ?
C2 C7 1.388(3) . ?
C3 C4 1.373(3) . ?
C3 N1 1.468(2) . ?
C4 H4 0.9300 . ?
C4 C5 1.378(3) . ?
C5 C6 1.376(3) . ?
C5 N2 1.470(2) . ?
C6 H6 0.9300 . ?
C6 C7 1.386(3) . ?
C7 H7 0.9300 . ?
C8 C9 1.514(3) . ?
C8 O7 1.253(3) . ?
C8 O8 1.227(3) . ?
C9 C10 1.372(4) . ?
C9 C14 1.387(4) . ?
C10 C11 1.382(4) . ?
C10 N3 1.472(6) . ?
C10 N3A 1.504(13) . ?
C11 H11 0.9300 . ?
C11 C12 1.345(5) . ?
C12 C13 1.367(5) . ?
C12 N4 1.478(4) . ?
C13 H13 0.9300 . ?
C13 C14 1.380(4) . ?
C14 H14 0.9300 . ?
C15 C16 1.508(3) . ?
C15 O13 1.246(2) . ?
C15 O14 1.245(2) . ?
C15 Gd1 3.0109(19) . ?
C16 C17 1.394(3) . ?
C16 C21 1.382(3) . ?
C17 C18 1.373(3) . ?
C17 N5 1.466(3) . ?
C18 H18 0.9300 . ?
C18 C19 1.357(4) . ?
C19 C20 1.378(4) . ?
C19 N6 1.479(3) . ?
C20 H20 0.9300 . ?
C20 C21 1.383(3) . ?
C21 H21 0.9300 . ?
N1 O3 1.212(3) . ?
N1 O4 1.214(3) . ?
N2 O5 1.217(3) . ?
N2 O6 1.214(3) . ?
N3 O9' 1.243(9) . ?
N3 O10' 1.184(7) . ?
N4 O11 1.205(5) . ?
N4 O12 1.207(5) . ?
N5 O15 1.198(3) . ?
N5 O16 1.226(3) . ?
N6 O17 1.240(5) . ?
N6 O18 1.204(5) . ?
O1 Gd1 2.3793(13) 2_576 ?
O2 Gd1 2.3889(13) . ?
O7 Gd1 2.3519(15) . ?
O13 Gd1 2.5139(14) . ?
O14 Gd1 2.3586(12) 2_576 ?
O14 Gd1 2.7704(15) . ?
O1W H1WA 0.815(16) . ?
O1W H1WB 0.807(16) . ?
O1W Gd1 2.4007(14) . ?
O2W H2WA 0.796(16) . ?
O2W H2WB 0.797(16) . ?
O2W Gd1 2.3960(14) . ?
O3W H3WA 0.811(16) . ?
O3W H3WB 0.807(16) . ?
O3W Gd1 2.4489(15) . ?
O9 N3A 1.213(13) . ?
N3A O9'A 1.260(17) . ?

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 C1 C2 116.33(16) . . ?
O1 C1 O2 128.55(16) . . ?
O2 C1 C2 115.10(15) . . ?
C3 C2 C1 121.62(16) . . ?
C3 C2 C7 117.34(17) . . ?
C7 C2 C1 120.92(16) . . ?
C2 C3 N1 119.33(16) . . ?
C4 C3 C2 124.03(18) . . ?
C4 C3 N1 116.57(17) . . ?
C3 C4 H4 122.0 . . ?
C3 C4 C5 115.93(18) . . ?
C5 C4 H4 122.0 . . ?
C4 C5 N2 116.82(19) . . ?
C6 C5 C4 123.36(18) . . ?
C6 C5 N2 119.81(19) . . ?
C5 C6 H6 120.8 . . ?
C5 C6 C7 118.41(19) . . ?
C7 C6 H6 120.8 . . ?
C2 C7 H7 119.5 . . ?
C6 C7 C2 120.90(19) . . ?
C6 C7 H7 119.5 . . ?
O7 C8 C9 114.5(2) . . ?
O8 C8 C9 117.7(2) . . ?
O8 C8 O7 127.5(2) . . ?
C10 C9 C8 124.9(2) . . ?
C10 C9 C14 117.2(2) . . ?
C14 C9 C8 117.9(2) . . ?
C9 C10 C11 123.0(3) . . ?
C9 C10 N3 120.8(3) . . ?
C9 C10 N3A 116.3(8) . . ?
C11 C10 N3 116.0(4) . . ?
C11 C10 N3A 119.1(7) . . ?
C10 C11 H11 121.3 . . ?
C12 C11 C10 117.5(3) . . ?
C12 C11 H11 121.3 . . ?
C11 C12 C13 122.6(3) . . ?
C11 C12 N4 117.8(3) . . ?
C13 C12 N4 119.5(3) . . ?
C12 C13 H13 120.6 . . ?
C12 C13 C14 118.8(3) . . ?
C14 C13 H13 120.6 . . ?
C9 C14 H14 119.6 . . ?
C13 C14 C9 120.8(3) . . ?
C13 C14 H14 119.6 . . ?
C16 C15 Gd1 172.78(12) . . ?
O13 C15 C16 118.17(15) . . ?
O13 C15 Gd1 55.05(9) . . ?
O14 C15 C16 120.06(17) . . ?
O14 C15 O13 121.66(17) . . ?
O14 C15 Gd1 66.91(10) . . ?
C17 C16 C15 124.05(19) . . ?
C21 C16 C15 118.31(19) . . ?
C21 C16 C17 117.6(2) . . ?
C16 C17 N5 120.4(2) . . ?
C18 C17 C16 122.5(2) . . ?
C18 C17 N5 117.1(2) . . ?
C17 C18 H18 121.3 . . ?
C19 C18 C17 117.5(2) . . ?
C19 C18 H18 121.3 . . ?
C18 C19 C20 123.2(2) . . ?
C18 C19 N6 118.2(3) . . ?
C20 C19 N6 118.7(3) . . ?
C19 C20 H20 121.0 . . ?
C19 C20 C21 118.1(3) . . ?
C21 C20 H20 121.0 . . ?
C16 C21 C20 121.2(2) . . ?
C16 C21 H21 119.4 . . ?
C20 C21 H21 119.4 . . ?
O3 N1 C3 116.85(18) . . ?
O3 N1 O4 124.90(19) . . ?
O4 N1 C3 118.22(18) . . ?
O5 N2 C5 117.57(19) . . ?
O6 N2 C5 118.5(2) . . ?
O6 N2 O5 123.92(19) . . ?
O9' N3 C10 114.6(7) . . ?
O10' N3 C10 119.5(5) . . ?
O10' N3 O9' 125.5(6) . . ?
O11 N4 C12 117.5(4) . . ?
O11 N4 O12 124.0(3) . . ?
O12 N4 C12 118.5(4) . . ?
O15 N5 C17 118.1(2) . . ?
O15 N5 O16 124.1(3) . . ?
O16 N5 C17 117.8(3) . . ?
O17 N6 C19 116.8(3) . . ?
O18 N6 C19 117.9(4) . . ?
O18 N6 O17 125.2(3) . . ?
C1 O1 Gd1 138.44(12) . 2_576 ?
C1 O2 Gd1 138.79(11) . . ?
C8 O7 Gd1 136.71(15) . . ?
C15 O13 Gd1 100.97(11) . . ?
C15 O14 Gd1 163.71(13) . 2_576 ?
C15 O14 Gd1 88.67(11) . . ?
Gd1 O14 Gd1 107.59(5) 2_576 . ?
H1WA O1W H1WB 103(2) . . ?
Gd1 O1W H1WA 126.5(18) . . ?
Gd1 O1W H1WB 129.8(19) . . ?
H2WA O2W H2WB 107(2) . . ?
Gd1 O2W H2WA 134(2) . . ?
Gd1 O2W H2WB 113.0(19) . . ?
H3WA O3W H3WB 106(2) . . ?
Gd1 O3W H3WA 124.5(19) . . ?
Gd1 O3W H3WB 112(2) . . ?
O1 Gd1 C15 74.65(5) 2_576 . ?
O1 Gd1 O2 132.08(5) 2_576 . ?
O1 Gd1 O13 85.26(5) 2_576 . ?
O1 Gd1 O14 68.73(5) 2_576 . ?
O1 Gd1 O1W 144.12(5) 2_576 . ?
O1 Gd1 O2W 74.39(5) 2_576 . ?
O1 Gd1 O3W 134.00(5) 2_576 . ?
O2 Gd1 C15 74.80(5) . . ?
O2 Gd1 O13 81.44(5) . . ?
O2 Gd1 O14 68.13(4) . . ?
O2 Gd1 O1W 73.88(5) . . ?
O2 Gd1 O2W 140.11(5) . . ?
O2 Gd1 O3W 69.95(5) . . ?
O7 Gd1 C15 148.04(5) . . ?
O7 Gd1 O1 75.16(5) . 2_576 ?
O7 Gd1 O2 135.15(5) . . ?
O7 Gd1 O13 142.32(5) . . ?
O7 Gd1 O14 84.63(6) . 2_576 ?
O7 Gd1 O14 141.23(5) . . ?
O7 Gd1 O1W 104.25(7) . . ?
O7 Gd1 O2W 73.17(6) . . ?
O7 Gd1 O3W 67.03(5) . . ?
O13 Gd1 C15 23.98(4) . . ?
O13 Gd1 O14 48.33(4) . . ?
O14 Gd1 C15 96.83(5) 2_576 . ?
O14 Gd1 C15 24.42(4) . . ?
O14 Gd1 O1 73.87(5) 2_576 2_576 ?
O14 Gd1 O2 74.14(4) 2_576 . ?
O14 Gd1 O13 120.70(5) 2_576 . ?
O14 Gd1 O14 72.41(5) 2_576 . ?
O14 Gd1 O1W 141.96(5) 2_576 . ?
O14 Gd1 O2W 144.94(5) 2_576 . ?
O14 Gd1 O3W 77.35(6) 2_576 . ?
O1W Gd1 C15 94.17(6) . . ?
O1W Gd1 O13 73.76(6) . . ?
O1W Gd1 O14 113.15(6) . . ?
O1W Gd1 O3W 72.74(6) . . ?
O2W Gd1 C15 88.79(6) . . ?
O2W Gd1 O13 70.66(6) . . ?
O2W Gd1 O14 108.96(5) . . ?
O2W Gd1 O1W 71.34(6) . . ?
O2W Gd1 O3W 116.16(7) . . ?
O3W Gd1 C15 144.55(5) . . ?
O3W Gd1 O13 140.66(5) . . ?
O3W Gd1 O14 133.35(5) . . ?
O9 N3A C10 121.1(12) . . ?
O9 N3A O9'A 119.5(18) . . ?
O9'A N3A C10 113.5(17) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 -174.24(19) . . . . ?
C1 C2 C3 N1 8.9(3) . . . . ?
C1 C2 C7 C6 174.6(2) . . . . ?
C2 C1 O1 Gd1 167.73(13) . . . 2_576 ?
C2 C1 O2 Gd1 174.77(12) . . . . ?
C2 C3 C4 C5 -0.8(3) . . . . ?
C2 C3 N1 O3 53.0(3) . . . . ?
C2 C3 N1 O4 -128.8(2) . . . . ?
C3 C2 C7 C6 -1.5(3) . . . . ?
C3 C4 C5 C6 -0.7(3) . . . . ?
C3 C4 C5 N2 -179.39(18) . . . . ?
C4 C3 N1 O3 -124.1(2) . . . . ?
C4 C3 N1 O4 54.1(3) . . . . ?
C4 C5 C6 C7 1.0(4) . . . . ?
C4 C5 N2 O5 -9.8(3) . . . . ?
C4 C5 N2 O6 172.2(2) . . . . ?
C5 C6 C7 C2 0.2(4) . . . . ?
C6 C5 N2 O5 171.5(2) . . . . ?
C6 C5 N2 O6 -6.6(3) . . . . ?
C7 C2 C3 C4 1.9(3) . . . . ?
C7 C2 C3 N1 -175.02(19) . . . . ?
C8 C9 C10 C11 177.2(3) . . . . ?
C8 C9 C10 N3 2.3(5) . . . . ?
C8 C9 C10 N3A -17.7(10) . . . . ?
C8 C9 C14 C13 -178.3(3) . . . . ?
C9 C8 O7 Gd1 -153.98(18) . . . . ?
C9 C10 C11 C12 1.2(5) . . . . ?
C9 C10 N3 O9' -19.3(9) . . . . ?
C9 C10 N3 O10' 168.4(5) . . . . ?
C9 C10 N3A O9 -150(2) . . . . ?
C9 C10 N3A O9'A 57(3) . . . . ?
C10 C9 C14 C13 0.6(5) . . . . ?
C10 C11 C12 C13 0.5(5) . . . . ?
C10 C11 C12 N4 -179.6(3) . . . . ?
C11 C10 N3 O9' 165.5(7) . . . . ?
C11 C10 N3 O10' -6.9(8) . . . . ?
C11 C10 N3A O9 15(3) . . . . ?
C11 C10 N3A O9'A -137.4(19) . . . . ?
C11 C12 C13 C14 -1.5(5) . . . . ?
C11 C12 N4 O11 172.1(4) . . . . ?
C11 C12 N4 O12 -7.9(5) . . . . ?
C12 C13 C14 C9 0.9(5) . . . . ?
C13 C12 N4 O11 -8.0(5) . . . . ?
C13 C12 N4 O12 172.0(4) . . . . ?
C14 C9 C10 C11 -1.6(4) . . . . ?
C14 C9 C10 N3 -176.6(4) . . . . ?
C14 C9 C10 N3A 163.5(10) . . . . ?
C15 C16 C17 C18 -179.2(2) . . . . ?
C15 C16 C17 N5 -2.7(3) . . . . ?
C15 C16 C21 C20 179.2(2) . . . . ?
C16 C15 O13 Gd1 -177.08(14) . . . . ?
C16 C15 O14 Gd1 177.88(16) . . . . ?
C16 C15 O14 Gd1 1.7(6) . . . 2_576 ?
C16 C17 C18 C19 0.3(4) . . . . ?
C16 C17 N5 O15 -16.3(3) . . . . ?
C16 C17 N5 O16 164.9(3) . . . . ?
C17 C16 C21 C20 0.6(4) . . . . ?
C17 C18 C19 C20 0.3(4) . . . . ?
C17 C18 C19 N6 179.1(3) . . . . ?
C18 C17 N5 O15 160.4(2) . . . . ?
C18 C17 N5 O16 -18.3(4) . . . . ?
C18 C19 C20 C21 -0.5(5) . . . . ?
C18 C19 N6 O17 -3.4(5) . . . . ?
C18 C19 N6 O18 172.7(4) . . . . ?
C19 C20 C21 C16 0.0(4) . . . . ?
C20 C19 N6 O17 175.5(3) . . . . ?
C20 C19 N6 O18 -8.5(5) . . . . ?
C21 C16 C17 C18 -0.7(3) . . . . ?
C21 C16 C17 N5 175.8(2) . . . . ?
N1 C3 C4 C5 176.16(18) . . . . ?
N2 C5 C6 C7 179.7(2) . . . . ?
N3 C10 C11 C12 176.3(4) . . . . ?
N4 C12 C13 C14 178.6(3) . . . . ?
N5 C17 C18 C19 -176.4(2) . . . . ?
N6 C19 C20 C21 -179.3(3) . . . . ?
O1 C1 C2 C3 -142.94(19) . . . . ?
O1 C1 C2 C7 41.1(3) . . . . ?
O1 C1 O2 Gd1 -3.6(3) . . . . ?
O2 C1 C2 C3 38.4(3) . . . . ?
O2 C1 C2 C7 -137.5(2) . . . . ?
O2 C1 O1 Gd1 -13.9(3) . . . 2_576 ?
O7 C8 C9 C10 -89.7(3) . . . . ?
O7 C8 C9 C14 89.2(3) . . . . ?
O8 C8 C9 C10 95.5(4) . . . . ?
O8 C8 C9 C14 -85.7(4) . . . . ?
O8 C8 O7 Gd1 20.3(5) . . . . ?
O13 C15 C16 C17 103.8(2) . . . . ?
O13 C15 C16 C21 -74.7(3) . . . . ?
O13 C15 O14 Gd1 -5.98(19) . . . . ?
O13 C15 O14 Gd1 177.8(3) . . . 2_576 ?
O14 C15 C16 C17 -79.9(3) . . . . ?
O14 C15 C16 C21 101.6(2) . . . . ?
O14 C15 O13 Gd1 6.7(2) . . . . ?
Gd1 C15 O14 Gd1 -176.2(5) . . . 2_576 ?
N3A C10 C11 C12 -163.6(11) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_Sm_24DNb
_database_code_depnum_ccdc_archive 'CCDC 1584552'
_audit_update_record             
;
2018-02-08 deposited with the CCDC.
2018-02-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H18 N12 O40 Sm2'
_chemical_formula_sum            'C42 H18 N12 O40 Sm2'
_chemical_formula_weight         1631.41

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           9
_space_group_name_H-M_alt        'C c'
_space_group_name_Hall           'C -2yc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   12.8390(14)
_cell_length_b                   47.454(6)
_cell_length_c                   9.2030(9)
_cell_angle_alpha                90
_cell_angle_beta                 92.811(4)
_cell_angle_gamma                90
_cell_volume                     5600.3(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3264
_cell_measurement_theta_min      2.58
_cell_measurement_theta_max      20.97

_exptl_crystal_description       Needles
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.935
_exptl_crystal_F_000             3192
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    2.202
_shelx_estimated_absorpt_T_min   0.693
_shelx_estimated_absorpt_T_max   0.734
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.690
_exptl_absorpt_correction_T_max  0.741
_exptl_absorpt_process_details   
'SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26340
_diffrn_reflns_av_unetI/netI     0.1059
_diffrn_reflns_av_R_equivalents  0.0798
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -60
_diffrn_reflns_limit_k_max       62
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.645
_diffrn_reflns_theta_max         27.967
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.742
_diffrn_reflns_point_group_measured_fraction_full 0.804
_reflns_number_total             10017
_reflns_number_gt                7653
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.488
_reflns_Friedel_fraction_max     0.488
_reflns_Friedel_fraction_full    0.607

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Sir-92 (Altomare et al., 1993)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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.The disorder in the nitro 
 groups of Ligand was resolved by splitting each of the affected 
 atoms in two parts (using PART) with their site occupancy factors and
 Uiso values refined as free variables and constraints on their distances
All hydrogen atoms were fixed geometrically with their Uiso values 1.2 
times of phenylene carbons.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0757P)²+3.9381P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2172 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.001(15)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         10017
_refine_ls_number_parameters     885
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0522
_refine_ls_wR_factor_ref         0.1343
_refine_ls_wR_factor_gt          0.1174
_refine_ls_goodness_of_fit_ref   0.878
_refine_ls_restrained_S_all      0.878
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.7198(11) 0.0851(3) 0.8501(14) 0.031(3) Uani 1 1 d . . . . .
C2 C 0.6609(12) 0.0584(3) 0.8860(13) 0.033(3) Uani 1 1 d . . . . .
C3 C 0.6925(11) 0.0315(3) 0.8435(15) 0.034(3) Uani 1 1 d . . . . .
C4 C 0.6426(12) 0.0073(3) 0.8815(17) 0.041(4) Uani 1 1 d . . . . .
H4 H 0.664802 -0.010298 0.851531 0.050 Uiso 1 1 calc R U . . .
C5 C 0.5581(12) 0.0103(3) 0.9659(18) 0.044(4) Uani 1 1 d . . . . .
C6 C 0.5228(13) 0.0356(3) 1.0106(15) 0.041(4) Uani 1 1 d . . . . .
H6 H 0.465552 0.036661 1.068595 0.049 Uiso 1 1 calc R U . . .
C7 C 0.5722(11) 0.0597(3) 0.9694(16) 0.041(3) Uani 1 1 d . . . . .
H7 H 0.546827 0.077127 0.997012 0.049 Uiso 1 1 calc R U . . .
C8 C 0.8413(12) 0.1915(3) 0.5730(18) 0.036(3) Uani 1 1 d . . . . .
C9 C 0.8159(14) 0.2223(2) 0.5816(19) 0.028(3) Uani 1 1 d . . . . .
C10 C 0.7501(12) 0.2308(3) 0.6887(16) 0.040(4) Uani 1 1 d . . . . .
H10 H 0.727753 0.217542 0.754734 0.049 Uiso 1 1 calc R U . . .
C11 C 0.7168(13) 0.2586(3) 0.7002(16) 0.046(4) Uani 1 1 d . . . . .
H11 H 0.672593 0.264053 0.772116 0.055 Uiso 1 1 calc R U . . .
C12 C 0.7515(11) 0.2774(3) 0.6014(16) 0.037(3) Uani 1 1 d . . . . .
C13 C 0.8173(12) 0.2704(3) 0.4938(15) 0.039(3) Uani 1 1 d . . . . .
H13 H 0.838411 0.283686 0.426912 0.046 Uiso 1 1 calc R U . . .
C14 C 0.8503(12) 0.2432(3) 0.4894(15) 0.034(3) Uani 1 1 d . . . . .
C15 C 0.7193(10) 0.1723(3) 1.0491(15) 0.031(3) Uani 1 1 d . . . . .
C16 C 0.6578(11) 0.1970(3) 1.1110(13) 0.034(3) Uani 1 1 d . . . . .
C17 C 0.5666(13) 0.1950(3) 1.1788(16) 0.046(4) Uani 1 1 d . . . . .
C18 C 0.5248(16) 0.2166(5) 1.2523(18) 0.068(6) Uani 1 1 d . . . . .
H18 H 0.461894 0.214652 1.297152 0.082 Uiso 1 1 calc R U . . .
C19 C 0.5776(16) 0.2411(5) 1.258(2) 0.061(6) Uani 1 1 d . . . . .
C20 C 0.6628(17) 0.2455(4) 1.182(2) 0.063(6) Uani 1 1 d . . . . .
H20 H 0.692295 0.263370 1.177762 0.075 Uiso 1 1 calc R U . . .
C21 C 0.7062(14) 0.2229(3) 1.1100(17) 0.053(4) Uani 1 1 d . . . . .
H21 H 0.767452 0.225232 1.061489 0.063 Uiso 1 1 calc R U . . .
C22 C 0.9282(10) 0.0923(3) 1.1106(13) 0.028(3) Uani 1 1 d . . . . .
C23 C 0.9809(10) 0.0655(3) 1.0809(13) 0.027(3) Uani 1 1 d . . . . .
C24 C 0.9694(10) 0.0408(3) 1.1644(14) 0.032(3) Uani 1 1 d . . . . .
C25 C 1.0260(13) 0.0168(3) 1.1458(15) 0.039(3) Uani 1 1 d . . . . .
H25 H 1.016761 0.000958 1.203330 0.047 Uiso 1 1 calc R U . . .
C26 C 1.0966(12) 0.0170(3) 1.0393(16) 0.041(4) Uani 1 1 d . . . . .
C27 C 1.1106(11) 0.0396(3) 0.9517(17) 0.044(4) Uani 1 1 d . . . . .
H27 H 1.157649 0.038756 0.878148 0.052 Uiso 1 1 calc R U . . .
C28 C 1.0539(12) 0.0642(3) 0.9733(16) 0.042(4) Uani 1 1 d . . . . .
H28 H 1.064706 0.079932 0.915443 0.050 Uiso 1 1 calc R U . . .
C29 C 1.0119(13) 0.1232(3) 0.6172(15) 0.036(3) Uani 1 1 d . . . . .
C30 C 1.1049(11) 0.1164(3) 0.5260(14) 0.032(3) Uani 1 1 d . . . . .
C31 C 1.1037(13) 0.0891(3) 0.4654(18) 0.048(4) Uani 1 1 d . . . . .
H31 H 1.047798 0.077186 0.480739 0.057 Uiso 1 1 calc R U . . .
C32 C 1.1835(14) 0.0799(3) 0.3845(18) 0.053(4) Uani 1 1 d . . . . .
H32 H 1.181664 0.061771 0.346118 0.064 Uiso 1 1 calc R U . . .
C33 C 1.2662(15) 0.0972(4) 0.3595(17) 0.049(5) Uani 1 1 d . . . . .
C34 C 1.2698(13) 0.1243(3) 0.4132(18) 0.041(4) Uani 1 1 d . . . . .
H34 H 1.324713 0.136352 0.394676 0.049 Uiso 1 1 calc R U . . .
C35 C 1.1904(13) 0.1327(3) 0.4938(17) 0.037(4) Uani 1 1 d . . . . .
C36 C 0.6306(11) 0.1392(3) 0.5432(16) 0.029(3) Uani 1 1 d . . . . .
C37 C 0.5342(12) 0.1304(3) 0.6233(15) 0.034(3) Uani 1 1 d . . . . .
C38 C 0.5089(13) 0.1018(3) 0.6114(18) 0.049(4) Uani 1 1 d . . . . .
H38 H 0.545699 0.089762 0.552654 0.059 Uiso 1 1 calc R U . . .
C39 C 0.4268(13) 0.0920(4) 0.6905(18) 0.051(4) Uani 1 1 d . . . . .
H39 H 0.404939 0.073350 0.680187 0.061 Uiso 1 1 calc R U . . .
C40 C 0.3781(13) 0.1095(4) 0.7833(19) 0.043(4) Uani 1 1 d . . . . .
C41 C 0.4063(12) 0.1368(3) 0.8042(18) 0.041(4) Uani 1 1 d . . . . .
H41 H 0.374687 0.147994 0.872514 0.049 Uiso 1 1 calc R U . . .
C42 C 0.4833(11) 0.1475(3) 0.7208(16) 0.038(3) Uani 1 1 d . . . . .
N1 N 0.7874(11) 0.0277(2) 0.7599(15) 0.042(3) Uani 1 1 d . . . . .
N2 N 0.5078(14) -0.0159(4) 1.011(2) 0.067(5) Uani 1 1 d . . . . .
N3 N 0.9264(10) 0.2353(3) 0.3800(14) 0.041(3) Uani 1 1 d . . . . .
N4 N 0.7177(11) 0.3072(3) 0.6127(18) 0.056(4) Uani 1 1 d . . . . .
N5 N 0.5048(12) 0.1688(3) 1.1682(16) 0.056(4) Uani 1 1 d . . . . .
N6 N 0.536(2) 0.2659(6) 1.337(2) 0.089(7) Uani 1 1 d . . . . .
N7 N 0.8895(13) 0.0399(2) 1.2740(14) 0.049(4) Uani 1 1 d . . . . .
N8 N 1.1605(13) -0.0088(3) 1.0217(17) 0.056(4) Uani 1 1 d . . . . .
N9 N 1.1896(11) 0.1625(3) 0.5452(15) 0.046(3) Uani 1 1 d . . . . .
N10 N 1.3511(15) 0.0872(5) 0.270(2) 0.071(5) Uani 1 1 d . . . . .
N11 N 0.5115(10) 0.1778(3) 0.7327(15) 0.041(3) Uani 1 1 d . . . . .
N12 N 0.296(2) 0.0985(5) 0.870(3) 0.098(8) Uani 1 1 d . . . . .
O1 O 0.6964(8) 0.1080(2) 0.9126(10) 0.039(2) Uani 1 1 d . . . . .
O2 O 0.7890(8) 0.08460(19) 0.7598(9) 0.037(2) Uani 1 1 d . . . . .
O1W O 0.6751(8) 0.10462(19) 0.2069(9) 0.038(2) Uani 1 1 d . . . . .
O3 O 0.7733(12) 0.0239(3) 0.6296(14) 0.086(5) Uani 1 1 d . . . . .
O2W O 0.9694(10) 0.1670(2) 0.9636(11) 0.062(3) Uani 1 1 d . . . . .
O4 O 0.8705(10) 0.0269(3) 0.8215(15) 0.068(4) Uani 1 1 d . . . . .
O3W O 0.7516(8) 0.0866(2) 0.4669(10) 0.040(2) Uani 1 1 d . . . . .
O5 O 0.5301(14) -0.0373(3) 0.950(2) 0.099(5) Uani 1 1 d . . . . .
O6 O 0.4451(14) -0.0145(3) 1.105(2) 0.102(6) Uani 1 1 d . . . . .
O4W O 0.9719(8) 0.1546(2) 0.2785(11) 0.040(2) Uani 1 1 d . . . . .
O7 O 0.8717(8) 0.17932(18) 0.6878(10) 0.035(2) Uani 1 1 d . . . . .
O8 O 0.8277(9) 0.1803(2) 0.4493(10) 0.041(3) Uani 1 1 d . . . . .
O9 O 0.9166(10) 0.2463(3) 0.2593(12) 0.064(3) Uani 1 1 d . . . . .
O10 O 0.9989(10) 0.2200(3) 0.4213(14) 0.065(3) Uani 1 1 d . . . . .
O11 O 0.6718(13) 0.3140(3) 0.7170(18) 0.095(5) Uani 1 1 d . . . . .
O12 O 0.7382(14) 0.3226(3) 0.5136(18) 0.093(5) Uani 1 1 d . . . . .
O13 O 0.7648(8) 0.1568(2) 0.1393(10) 0.039(2) Uani 1 1 d . . . . .
O14 O 0.7223(9) 0.1708(2) 0.9126(9) 0.041(3) Uani 1 1 d . . . . .
O15 O 0.421(5) 0.1728(11) 1.232(9) 0.082(8) Uani 0.52(6) 1 d . . P A 1
O15' O 0.424(5) 0.1623(11) 1.230(10) 0.082(8) Uani 0.48(6) 1 d . . P A 2
O16 O 0.5361(9) 0.1486(3) 1.0938(13) 0.055(3) Uani 1 1 d . . . . .
O17 O 0.462(4) 0.2658(12) 1.383(5) 0.089(13) Uani 0.64(7) 1 d . . P B 1
O17' O 0.446(8) 0.2536(19) 1.425(8) 0.089(13) Uani 0.36(7) 1 d . . P B 2
O18 O 0.609(5) 0.2921(11) 1.348(8) 0.077(11) Uani 0.46(5) 1 d . . P B 1
O18' O 0.569(5) 0.2842(9) 1.342(6) 0.077(11) Uani 0.54(5) 1 d . . P B 2
O19 O 0.7188(8) 0.13801(18) 0.6123(11) 0.031(2) Uani 1 1 d . . . . .
O20 O 0.6229(9) 0.1433(2) 0.4110(10) 0.038(2) Uani 1 1 d . . . . .
O21 O 0.5624(11) 0.1876(2) 0.6380(15) 0.067(4) Uani 1 1 d . . . . .
O22 O 0.4812(9) 0.1909(2) 0.8371(13) 0.058(3) Uani 1 1 d . . . . .
O23 O 0.2576(14) 0.1123(4) 0.957(2) 0.107(6) Uani 1 1 d . . . . .
O24 O 0.306(3) 0.0707(7) 0.886(5) 0.105(10) Uani 0.50(2) 1 d . . P C 1
O24' O 0.244(2) 0.0781(7) 0.811(5) 0.105(10) Uani 0.50(2) 1 d . . P C 2
O25 O 0.9242(7) 0.12309(19) 0.5630(10) 0.032(2) Uani 1 1 d . . . . .
O26 O 1.0335(9) 0.1270(2) 0.7535(12) 0.047(3) Uani 1 1 d . . . . .
O27 O 1.1053(10) 0.1741(3) 0.5628(16) 0.064(4) Uani 1 1 d . . . . .
O28 O 1.2748(9) 0.1740(3) 0.5667(19) 0.082(4) Uani 1 1 d . . . . .
O29 O 1.4276(12) 0.1015(4) 0.2685(19) 0.091(5) Uani 1 1 d . . . . .
O30 O 1.3387(14) 0.0647(4) 0.211(2) 0.119(7) Uani 1 1 d . . . . .
O31 O 0.9159(8) 0.10968(19) 1.0078(9) 0.040(2) Uani 1 1 d . . . . .
O32 O 0.9019(8) 0.09678(19) 0.2370(10) 0.037(2) Uani 1 1 d . . . . .
O33 O 0.7983(9) 0.0430(2) 1.2323(15) 0.062(3) Uani 1 1 d . . . . .
O34 O 0.9230(12) 0.0359(3) 1.4004(13) 0.074(4) Uani 1 1 d . . . . .
O35 O 1.1517(13) -0.0279(3) 1.1029(17) 0.080(5) Uani 1 1 d . . . . .
O36 O 1.2149(12) -0.0091(3) 0.9112(18) 0.089(5) Uani 1 1 d . . . . .
Sm1 Sm 0.80641(5) 0.13279(2) 0.35745(5) 0.02666(19) Uani 1 1 d . . . . .
Sm2 Sm 0.84281(5) 0.13623(2) 0.81417(5) 0.02692(19) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O2 1.246(15) . ?
C1 O1 1.274(15) . ?
C1 C2 1.521(18) . ?
C2 C3 1.400(19) . ?
C2 C7 1.405(19) . ?
C3 C4 1.37(2) . ?
C3 N1 1.48(2) . ?
C4 C5 1.37(2) . ?
C4 H4 0.9300 . ?
C5 C6 1.35(2) . ?
C5 N2 1.47(2) . ?
C6 C7 1.37(2) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 O7 1.250(18) . ?
C8 O8 1.260(18) . ?
C8 C9 1.500(17) . ?
C9 C10 1.39(2) . ?
C9 C14 1.39(2) . ?
C10 C11 1.391(19) . ?
C10 H10 0.9300 . ?
C11 C12 1.37(2) . ?
C11 H11 0.9300 . ?
C12 C13 1.374(19) . ?
C12 N4 1.482(17) . ?
C13 C14 1.361(18) . ?
C13 H13 0.9300 . ?
C14 N3 1.485(18) . ?
C15 O13 1.234(15) 1_556 ?
C15 O14 1.260(15) . ?
C15 C16 1.541(18) . ?
C16 C17 1.36(2) . ?
C16 C21 1.38(2) . ?
C17 C18 1.36(2) . ?
C17 N5 1.47(2) . ?
C18 C19 1.34(3) . ?
C18 H18 0.9300 . ?
C19 C20 1.34(3) . ?
C19 N6 1.50(2) . ?
C20 C21 1.39(2) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
C22 O32 1.246(15) 1_556 ?
C22 O31 1.260(15) . ?
C22 C23 1.470(18) . ?
C23 C28 1.398(18) . ?
C23 C24 1.413(17) . ?
C24 C25 1.367(18) . ?
C24 N7 1.475(18) . ?
C25 C26 1.37(2) . ?
C25 H25 0.9300 . ?
C26 C27 1.36(2) . ?
C26 N8 1.486(18) . ?
C27 C28 1.39(2) . ?
C27 H27 0.9300 . ?
C28 H28 0.9300 . ?
C29 O25 1.209(17) . ?
C29 O26 1.285(17) . ?
C29 C30 1.53(2) . ?
C30 C35 1.39(2) . ?
C30 C31 1.41(2) . ?
C31 C32 1.37(2) . ?
C31 H31 0.9300 . ?
C32 C33 1.37(2) . ?
C32 H32 0.9300 . ?
C33 C34 1.38(2) . ?
C33 N10 1.48(2) . ?
C34 C35 1.35(2) . ?
C34 H34 0.9300 . ?
C35 N9 1.490(18) . ?
C36 O20 1.231(17) . ?
C36 O19 1.274(17) . ?
C36 C37 1.53(2) . ?
C37 C42 1.396(19) . ?
C37 C38 1.40(2) . ?
C38 C39 1.39(2) . ?
C38 H38 0.9300 . ?
C39 C40 1.37(2) . ?
C39 H39 0.9300 . ?
C40 C41 1.36(2) . ?
C40 N12 1.45(2) . ?
C41 C42 1.38(2) . ?
C41 H41 0.9300 . ?
C42 N11 1.484(19) . ?
N1 O4 1.183(17) . ?
N1 O3 1.217(16) . ?
N2 O5 1.20(2) . ?
N2 O6 1.21(2) . ?
N3 O10 1.227(16) . ?
N3 O9 1.229(15) . ?
N4 O11 1.195(18) . ?
N4 O12 1.208(19) . ?
N5 O15' 1.24(6) . ?
N5 O16 1.258(18) . ?
N5 O15 1.27(6) . ?
N6 O18' 0.97(5) . ?
N6 O17 1.06(5) . ?
N6 O17' 1.55(11) . ?
N6 O18 1.56(6) . ?
N7 O33 1.222(18) . ?
N7 O34 1.235(18) . ?
N8 O35 1.182(19) . ?
N8 O36 1.26(2) . ?
N9 O28 1.230(17) . ?
N9 O27 1.234(17) . ?
N10 O29 1.19(2) . ?
N10 O30 1.21(2) . ?
N11 O21 1.209(17) . ?
N11 O22 1.224(16) . ?
N12 O23 1.17(3) . ?
N12 O24' 1.28(4) . ?
N12 O24 1.33(4) . ?
O1 Sm2 2.513(10) . ?
O2 Sm2 2.588(9) . ?
O1W Sm1 2.514(9) . ?
O2W Sm2 2.539(11) . ?
O3W Sm1 2.528(10) . ?
O4W Sm1 2.503(10) . ?
O7 Sm2 2.391(9) . ?
O8 Sm1 2.419(9) . ?
O13 Sm1 2.347(9) . ?
O14 Sm2 2.457(9) . ?
O19 Sm2 2.388(10) . ?
O19 Sm1 2.662(10) . ?
O20 Sm1 2.481(11) . ?
O25 Sm1 2.408(9) . ?
O25 Sm2 2.658(9) . ?
O26 Sm2 2.576(11) . ?
O31 Sm2 2.341(9) . ?
O32 Sm1 2.405(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 C1 O1 120.6(12) . . ?
O2 C1 C2 120.6(11) . . ?
O1 C1 C2 118.9(12) . . ?
C3 C2 C7 116.6(13) . . ?
C3 C2 C1 123.0(13) . . ?
C7 C2 C1 120.5(12) . . ?
C4 C3 C2 123.1(14) . . ?
C4 C3 N1 115.9(13) . . ?
C2 C3 N1 120.9(12) . . ?
C3 C4 C5 116.8(14) . . ?
C3 C4 H4 121.6 . . ?
C5 C4 H4 121.6 . . ?
C6 C5 C4 123.4(14) . . ?
C6 C5 N2 120.4(15) . . ?
C4 C5 N2 116.1(15) . . ?
C5 C6 C7 119.2(14) . . ?
C5 C6 H6 120.4 . . ?
C7 C6 H6 120.4 . . ?
C6 C7 C2 120.9(14) . . ?
C6 C7 H7 119.5 . . ?
C2 C7 H7 119.5 . . ?
O7 C8 O8 126.3(12) . . ?
O7 C8 C9 117.7(13) . . ?
O8 C8 C9 115.9(14) . . ?
C10 C9 C14 116.6(12) . . ?
C10 C9 C8 117.5(13) . . ?
C14 C9 C8 125.9(15) . . ?
C9 C10 C11 122.0(13) . . ?
C9 C10 H10 119.0 . . ?
C11 C10 H10 119.0 . . ?
C12 C11 C10 117.3(13) . . ?
C12 C11 H11 121.4 . . ?
C10 C11 H11 121.4 . . ?
C11 C12 C13 123.6(13) . . ?
C11 C12 N4 118.2(13) . . ?
C13 C12 N4 118.3(13) . . ?
C14 C13 C12 117.1(13) . . ?
C14 C13 H13 121.5 . . ?
C12 C13 H13 121.5 . . ?
C13 C14 C9 123.4(14) . . ?
C13 C14 N3 118.4(12) . . ?
C9 C14 N3 118.2(12) . . ?
O13 C15 O14 126.9(13) 1_556 . ?
O13 C15 C16 116.0(12) 1_556 . ?
O14 C15 C16 116.9(11) . . ?
C17 C16 C21 117.8(14) . . ?
C17 C16 C15 125.8(14) . . ?
C21 C16 C15 116.0(13) . . ?
C18 C17 C16 123.2(19) . . ?
C18 C17 N5 116.5(17) . . ?
C16 C17 N5 120.2(14) . . ?
C19 C18 C17 118(2) . . ?
C19 C18 H18 121.2 . . ?
C17 C18 H18 121.2 . . ?
C18 C19 C20 122.5(17) . . ?
C18 C19 N6 120(2) . . ?
C20 C19 N6 117(2) . . ?
C19 C20 C21 118.8(18) . . ?
C19 C20 H20 120.6 . . ?
C21 C20 H20 120.6 . . ?
C16 C21 C20 119.5(17) . . ?
C16 C21 H21 120.2 . . ?
C20 C21 H21 120.2 . . ?
O32 C22 O31 123.9(12) 1_556 . ?
O32 C22 C23 118.1(11) 1_556 . ?
O31 C22 C23 117.9(11) . . ?
C28 C23 C24 116.1(12) . . ?
C28 C23 C22 120.0(12) . . ?
C24 C23 C22 123.6(11) . . ?
C25 C24 C23 123.6(13) . . ?
C25 C24 N7 116.9(12) . . ?
C23 C24 N7 119.4(12) . . ?
C24 C25 C26 117.3(13) . . ?
C24 C25 H25 121.3 . . ?
C26 C25 H25 121.3 . . ?
C27 C26 C25 122.7(13) . . ?
C27 C26 N8 119.8(14) . . ?
C25 C26 N8 117.5(14) . . ?
C26 C27 C28 119.5(14) . . ?
C26 C27 H27 120.3 . . ?
C28 C27 H27 120.3 . . ?
C27 C28 C23 120.7(14) . . ?
C27 C28 H28 119.7 . . ?
C23 C28 H28 119.7 . . ?
O25 C29 O26 123.8(14) . . ?
O25 C29 C30 120.7(12) . . ?
O26 C29 C30 115.4(13) . . ?
C35 C30 C31 114.9(14) . . ?
C35 C30 C29 130.6(13) . . ?
C31 C30 C29 114.6(13) . . ?
C32 C31 C30 121.0(16) . . ?
C32 C31 H31 119.5 . . ?
C30 C31 H31 119.5 . . ?
C31 C32 C33 120.5(16) . . ?
C31 C32 H32 119.8 . . ?
C33 C32 H32 119.8 . . ?
C32 C33 C34 120.8(16) . . ?
C32 C33 N10 120.0(17) . . ?
C34 C33 N10 119.2(18) . . ?
C35 C34 C33 117.3(16) . . ?
C35 C34 H34 121.3 . . ?
C33 C34 H34 121.3 . . ?
C34 C35 C30 125.5(14) . . ?
C34 C35 N9 118.1(14) . . ?
C30 C35 N9 116.3(13) . . ?
O20 C36 O19 121.8(14) . . ?
O20 C36 C37 119.5(13) . . ?
O19 C36 C37 117.9(13) . . ?
C42 C37 C38 120.1(15) . . ?
C42 C37 C36 124.5(13) . . ?
C38 C37 C36 114.7(13) . . ?
C39 C38 C37 117.6(15) . . ?
C39 C38 H38 121.2 . . ?
C37 C38 H38 121.2 . . ?
C40 C39 C38 120.3(16) . . ?
C40 C39 H39 119.9 . . ?
C38 C39 H39 119.9 . . ?
C41 C40 C39 123.0(16) . . ?
C41 C40 N12 117.7(17) . . ?
C39 C40 N12 119.3(18) . . ?
C40 C41 C42 117.8(15) . . ?
C40 C41 H41 121.1 . . ?
C42 C41 H41 121.1 . . ?
C41 C42 C37 121.1(15) . . ?
C41 C42 N11 119.5(13) . . ?
C37 C42 N11 119.4(13) . . ?
O4 N1 O3 123.7(16) . . ?
O4 N1 C3 119.9(13) . . ?
O3 N1 C3 116.3(14) . . ?
O5 N2 O6 124.0(18) . . ?
O5 N2 C5 117.9(18) . . ?
O6 N2 C5 118.1(17) . . ?
O10 N3 O9 125.2(14) . . ?
O10 N3 C14 117.0(12) . . ?
O9 N3 C14 117.6(13) . . ?
O11 N4 O12 125.3(15) . . ?
O11 N4 C12 118.0(14) . . ?
O12 N4 C12 116.7(14) . . ?
O15' N5 O16 111(4) . . ?
O16 N5 O15 132(3) . . ?
O15' N5 C17 129(4) . . ?
O16 N5 C17 119.6(14) . . ?
O15 N5 C17 108(3) . . ?
O18' N6 C19 124(4) . . ?
O17 N6 C19 122(4) . . ?
O18' N6 O17' 131(5) . . ?
C19 N6 O17' 104(4) . . ?
O17 N6 O18 122(4) . . ?
C19 N6 O18 116(3) . . ?
O33 N7 O34 126.7(15) . . ?
O33 N7 C24 118.0(14) . . ?
O34 N7 C24 115.3(16) . . ?
O35 N8 O36 125.1(15) . . ?
O35 N8 C26 119.4(16) . . ?
O36 N8 C26 115.2(14) . . ?
O28 N9 O27 124.0(14) . . ?
O28 N9 C35 116.9(13) . . ?
O27 N9 C35 119.1(13) . . ?
O29 N10 O30 126.1(19) . . ?
O29 N10 C33 117(2) . . ?
O30 N10 C33 116.7(19) . . ?
O21 N11 O22 124.9(14) . . ?
O21 N11 C42 117.4(13) . . ?
O22 N11 C42 117.7(13) . . ?
O23 N12 O24' 119(3) . . ?
O23 N12 O24 121(3) . . ?
O23 N12 C40 121(2) . . ?
O24' N12 C40 115(3) . . ?
O24 N12 C40 111(2) . . ?
C1 O1 Sm2 95.4(8) . . ?
C1 O2 Sm2 92.7(7) . . ?
C8 O7 Sm2 139.2(9) . . ?
C8 O8 Sm1 135.8(9) . . ?
C15 O13 Sm1 160.9(9) 1_554 . ?
C15 O14 Sm2 117.1(8) . . ?
C36 O19 Sm2 158.9(9) . . ?
C36 O19 Sm1 88.2(8) . . ?
Sm2 O19 Sm1 112.8(4) . . ?
C36 O20 Sm1 97.7(9) . . ?
C29 O25 Sm1 149.3(9) . . ?
C29 O25 Sm2 92.2(9) . . ?
Sm1 O25 Sm2 112.3(4) . . ?
C29 O26 Sm2 94.2(9) . . ?
C22 O31 Sm2 162.8(10) . . ?
C22 O32 Sm1 136.1(9) 1_554 . ?
O13 Sm1 O32 92.9(3) . . ?
O13 Sm1 O25 150.8(3) . . ?
O32 Sm1 O25 84.9(3) . . ?
O13 Sm1 O8 82.2(3) . . ?
O32 Sm1 O8 140.5(4) . . ?
O25 Sm1 O8 81.2(3) . . ?
O13 Sm1 O20 83.9(3) . . ?
O32 Sm1 O20 138.2(4) . . ?
O25 Sm1 O20 116.6(3) . . ?
O8 Sm1 O20 80.5(4) . . ?
O13 Sm1 O4W 73.3(3) . . ?
O32 Sm1 O4W 72.6(3) . . ?
O25 Sm1 O4W 78.3(3) . . ?
O8 Sm1 O4W 68.5(4) . . ?
O20 Sm1 O4W 143.3(4) . . ?
O13 Sm1 O1W 70.6(3) . . ?
O32 Sm1 O1W 73.2(3) . . ?
O25 Sm1 O1W 135.2(3) . . ?
O8 Sm1 O1W 138.6(3) . . ?
O20 Sm1 O1W 66.4(3) . . ?
O4W Sm1 O1W 128.0(3) . . ?
O13 Sm1 O3W 134.9(3) . . ?
O32 Sm1 O3W 74.1(3) . . ?
O25 Sm1 O3W 72.4(3) . . ?
O8 Sm1 O3W 134.3(3) . . ?
O20 Sm1 O3W 79.0(3) . . ?
O4W Sm1 O3W 137.0(3) . . ?
O1W Sm1 O3W 64.3(3) . . ?
O13 Sm1 O19 128.3(3) . . ?
O32 Sm1 O19 136.0(3) . . ?
O25 Sm1 O19 66.5(3) . . ?
O8 Sm1 O19 69.5(3) . . ?
O20 Sm1 O19 50.2(3) . . ?
O4W Sm1 O19 128.2(3) . . ?
O1W Sm1 O19 103.5(3) . . ?
O3W Sm1 O19 65.9(3) . . ?
O31 Sm2 O19 147.0(3) . . ?
O31 Sm2 O7 139.9(3) . . ?
O19 Sm2 O7 72.8(3) . . ?
O31 Sm2 O14 108.3(3) . . ?
O19 Sm2 O14 81.7(3) . . ?
O7 Sm2 O14 74.0(3) . . ?
O31 Sm2 O1 73.6(4) . . ?
O19 Sm2 O1 79.5(3) . . ?
O7 Sm2 O1 140.2(3) . . ?
O14 Sm2 O1 74.2(3) . . ?
O31 Sm2 O2W 71.0(4) . . ?
O19 Sm2 O2W 141.8(3) . . ?
O7 Sm2 O2W 70.2(3) . . ?
O14 Sm2 O2W 79.3(4) . . ?
O1 Sm2 O2W 125.5(3) . . ?
O31 Sm2 O26 74.0(4) . . ?
O19 Sm2 O26 116.2(4) . . ?
O7 Sm2 O26 82.4(4) . . ?
O14 Sm2 O26 144.6(4) . . ?
O1 Sm2 O26 136.4(4) . . ?
O2W Sm2 O26 68.0(4) . . ?
O31 Sm2 O2 74.4(3) . . ?
O19 Sm2 O2 73.8(3) . . ?
O7 Sm2 O2 139.7(3) . . ?
O14 Sm2 O2 122.4(3) . . ?
O1 Sm2 O2 50.8(3) . . ?
O2W Sm2 O2 143.8(3) . . ?
O26 Sm2 O2 92.6(3) . . ?
O31 Sm2 O25 112.1(3) . . ?
O19 Sm2 O25 66.9(3) . . ?
O7 Sm2 O25 72.6(3) . . ?
O14 Sm2 O25 139.4(3) . . ?
O1 Sm2 O25 121.4(3) . . ?
O2W Sm2 O25 109.7(3) . . ?
O26 Sm2 O25 49.7(3) . . ?
O2 Sm2 O25 73.9(3) . . ?

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
O2 C1 C2 C3 12(2) . . . . ?
O1 C1 C2 C3 -168.4(13) . . . . ?
O2 C1 C2 C7 -169.8(13) . . . . ?
O1 C1 C2 C7 9(2) . . . . ?
C7 C2 C3 C4 -1(2) . . . . ?
C1 C2 C3 C4 176.8(13) . . . . ?
C7 C2 C3 N1 -177.7(13) . . . . ?
C1 C2 C3 N1 0(2) . . . . ?
C2 C3 C4 C5 0(2) . . . . ?
N1 C3 C4 C5 176.4(14) . . . . ?
C3 C4 C5 C6 1(2) . . . . ?
C3 C4 C5 N2 -177.6(14) . . . . ?
C4 C5 C6 C7 1(3) . . . . ?
N2 C5 C6 C7 178.8(14) . . . . ?
C5 C6 C7 C2 -2(2) . . . . ?
C3 C2 C7 C6 2(2) . . . . ?
C1 C2 C7 C6 -175.6(13) . . . . ?
O7 C8 C9 C10 -50(2) . . . . ?
O8 C8 C9 C10 128.8(16) . . . . ?
O7 C8 C9 C14 131.7(16) . . . . ?
O8 C8 C9 C14 -50(2) . . . . ?
C14 C9 C10 C11 2(3) . . . . ?
C8 C9 C10 C11 -176.0(15) . . . . ?
C9 C10 C11 C12 0(3) . . . . ?
C10 C11 C12 C13 0(3) . . . . ?
C10 C11 C12 N4 -179.4(14) . . . . ?
C11 C12 C13 C14 -1(2) . . . . ?
N4 C12 C13 C14 177.6(13) . . . . ?
C12 C13 C14 C9 4(2) . . . . ?
C12 C13 C14 N3 -176.4(13) . . . . ?
C10 C9 C14 C13 -4(2) . . . . ?
C8 C9 C14 C13 173.8(15) . . . . ?
C10 C9 C14 N3 175.9(14) . . . . ?
C8 C9 C14 N3 -6(2) . . . . ?
O13 C15 C16 C17 -72.6(18) 1_556 . . . ?
O14 C15 C16 C17 111.0(16) . . . . ?
O13 C15 C16 C21 100.2(15) 1_556 . . . ?
O14 C15 C16 C21 -76.2(16) . . . . ?
C21 C16 C17 C18 -4(2) . . . . ?
C15 C16 C17 C18 168.6(14) . . . . ?
C21 C16 C17 N5 172.5(13) . . . . ?
C15 C16 C17 N5 -15(2) . . . . ?
C16 C17 C18 C19 0(2) . . . . ?
N5 C17 C18 C19 -177.2(15) . . . . ?
C17 C18 C19 C20 7(3) . . . . ?
C17 C18 C19 N6 179.9(16) . . . . ?
C18 C19 C20 C21 -9(3) . . . . ?
N6 C19 C20 C21 178.2(16) . . . . ?
C17 C16 C21 C20 2(2) . . . . ?
C15 C16 C21 C20 -171.1(14) . . . . ?
C19 C20 C21 C16 4(3) . . . . ?
O32 C22 C23 C28 -149.1(13) 1_556 . . . ?
O31 C22 C23 C28 28.3(19) . . . . ?
O32 C22 C23 C24 25(2) 1_556 . . . ?
O31 C22 C23 C24 -157.6(13) . . . . ?
C28 C23 C24 C25 1(2) . . . . ?
C22 C23 C24 C25 -173.4(13) . . . . ?
C28 C23 C24 N7 -176.3(13) . . . . ?
C22 C23 C24 N7 9(2) . . . . ?
C23 C24 C25 C26 -1(2) . . . . ?
N7 C24 C25 C26 176.7(14) . . . . ?
C24 C25 C26 C27 -1(2) . . . . ?
C24 C25 C26 N8 178.2(13) . . . . ?
C25 C26 C27 C28 2(2) . . . . ?
N8 C26 C27 C28 -177.0(14) . . . . ?
C26 C27 C28 C23 -2(2) . . . . ?
C24 C23 C28 C27 0(2) . . . . ?
C22 C23 C28 C27 174.8(13) . . . . ?
O25 C29 C30 C35 118.6(17) . . . . ?
O26 C29 C30 C35 -65(2) . . . . ?
O25 C29 C30 C31 -62(2) . . . . ?
O26 C29 C30 C31 114.1(15) . . . . ?
C35 C30 C31 C32 1(2) . . . . ?
C29 C30 C31 C32 -178.2(14) . . . . ?
C30 C31 C32 C33 -1(3) . . . . ?
C31 C32 C33 C34 -1(3) . . . . ?
C31 C32 C33 N10 -179.0(16) . . . . ?
C32 C33 C34 C35 2(3) . . . . ?
N10 C33 C34 C35 179.6(16) . . . . ?
C33 C34 C35 C30 -1(3) . . . . ?
C33 C34 C35 N9 -176.4(14) . . . . ?
C31 C30 C35 C34 -1(2) . . . . ?
C29 C30 C35 C34 178.7(16) . . . . ?
C31 C30 C35 N9 174.9(13) . . . . ?
C29 C30 C35 N9 -6(2) . . . . ?
O20 C36 C37 C42 -110.1(17) . . . . ?
O19 C36 C37 C42 80.0(18) . . . . ?
O20 C36 C37 C38 80.1(17) . . . . ?
O19 C36 C37 C38 -89.9(16) . . . . ?
C42 C37 C38 C39 5(2) . . . . ?
C36 C37 C38 C39 175.4(13) . . . . ?
C37 C38 C39 C40 -4(2) . . . . ?
C38 C39 C40 C41 0(3) . . . . ?
C38 C39 C40 N12 -176.9(18) . . . . ?
C39 C40 C41 C42 4(3) . . . . ?
N12 C40 C41 C42 -179.3(18) . . . . ?
C40 C41 C42 C37 -3(2) . . . . ?
C40 C41 C42 N11 175.8(14) . . . . ?
C38 C37 C42 C41 -1(2) . . . . ?
C36 C37 C42 C41 -170.8(14) . . . . ?
C38 C37 C42 N11 179.7(13) . . . . ?
C36 C37 C42 N11 10(2) . . . . ?
C4 C3 N1 O4 -94.2(17) . . . . ?
C2 C3 N1 O4 82.6(18) . . . . ?
C4 C3 N1 O3 81.8(17) . . . . ?
C2 C3 N1 O3 -101.4(17) . . . . ?
C6 C5 N2 O5 167.9(19) . . . . ?
C4 C5 N2 O5 -14(2) . . . . ?
C6 C5 N2 O6 -11(3) . . . . ?
C4 C5 N2 O6 167.5(19) . . . . ?
C13 C14 N3 O10 136.6(15) . . . . ?
C9 C14 N3 O10 -44(2) . . . . ?
C13 C14 N3 O9 -38(2) . . . . ?
C9 C14 N3 O9 141.9(15) . . . . ?
C11 C12 N4 O11 8(2) . . . . ?
C13 C12 N4 O11 -170.5(17) . . . . ?
C11 C12 N4 O12 -170.7(17) . . . . ?
C13 C12 N4 O12 10(2) . . . . ?
C18 C17 N5 O15' -9(5) . . . . ?
C16 C17 N5 O15' 174(5) . . . . ?
C18 C17 N5 O16 175.6(14) . . . . ?
C16 C17 N5 O16 -1(2) . . . . ?
C18 C17 N5 O15 1(4) . . . . ?
C16 C17 N5 O15 -176(4) . . . . ?
C18 C19 N6 O18' -178(4) . . . . ?
C20 C19 N6 O18' -5(5) . . . . ?
C18 C19 N6 O17 -5(5) . . . . ?
C20 C19 N6 O17 168(4) . . . . ?
C18 C19 N6 O17' 12(4) . . . . ?
C20 C19 N6 O17' -175(3) . . . . ?
C18 C19 N6 O18 175(3) . . . . ?
C20 C19 N6 O18 -12(4) . . . . ?
C25 C24 N7 O33 -116.9(15) . . . . ?
C23 C24 N7 O33 60.5(17) . . . . ?
C25 C24 N7 O34 63.1(17) . . . . ?
C23 C24 N7 O34 -119.5(14) . . . . ?
C27 C26 N8 O35 176.1(17) . . . . ?
C25 C26 N8 O35 -3(2) . . . . ?
C27 C26 N8 O36 -9(2) . . . . ?
C25 C26 N8 O36 171.5(16) . . . . ?
C34 C35 N9 O28 -30(2) . . . . ?
C30 C35 N9 O28 154.2(15) . . . . ?
C34 C35 N9 O27 149.9(16) . . . . ?
C30 C35 N9 O27 -26(2) . . . . ?
C32 C33 N10 O29 -169.8(19) . . . . ?
C34 C33 N10 O29 12(3) . . . . ?
C32 C33 N10 O30 6(3) . . . . ?
C34 C33 N10 O30 -172(2) . . . . ?
C41 C42 N11 O21 -164.7(15) . . . . ?
C37 C42 N11 O21 14(2) . . . . ?
C41 C42 N11 O22 15(2) . . . . ?
C37 C42 N11 O22 -166.1(14) . . . . ?
C41 C40 N12 O23 -2(4) . . . . ?
C39 C40 N12 O23 175(2) . . . . ?
C41 C40 N12 O24' 153(3) . . . . ?
C39 C40 N12 O24' -30(4) . . . . ?
C41 C40 N12 O24 -154(3) . . . . ?
C39 C40 N12 O24 23(4) . . . . ?
O2 C1 O1 Sm2 -7.6(14) . . . . ?
C2 C1 O1 Sm2 173.2(10) . . . . ?
O1 C1 O2 Sm2 7.4(13) . . . . ?
C2 C1 O2 Sm2 -173.4(11) . . . . ?
O8 C8 O7 Sm2 -43(2) . . . . ?
C9 C8 O7 Sm2 136.0(12) . . . . ?
O7 C8 O8 Sm1 18(2) . . . . ?
C9 C8 O8 Sm1 -160.7(11) . . . . ?
O13 C15 O14 Sm2 -5.7(18) 1_556 . . . ?
C16 C15 O14 Sm2 170.2(9) . . . . ?
O20 C36 O19 Sm2 169.8(16) . . . . ?
C37 C36 O19 Sm2 -20(3) . . . . ?
O20 C36 O19 Sm1 -14.6(13) . . . . ?
C37 C36 O19 Sm1 155.1(11) . . . . ?
O19 C36 O20 Sm1 15.9(14) . . . . ?
C37 C36 O20 Sm1 -153.7(10) . . . . ?
O26 C29 O25 Sm1 147.9(13) . . . . ?
C30 C29 O25 Sm1 -37(3) . . . . ?
O26 C29 O25 Sm2 3.8(16) . . . . ?
C30 C29 O25 Sm2 179.4(13) . . . . ?
O25 C29 O26 Sm2 -4.0(16) . . . . ?
C30 C29 O26 Sm2 -179.8(11) . . . . ?
O32 C22 O31 Sm2 -83(3) 1_556 . . . ?
C23 C22 O31 Sm2 100(3) . . . . ?

_refine_diff_density_max         2.284
_refine_diff_density_min         -1.224
_refine_diff_density_rms         0.160

####################################################################### 
# 
# 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_Nd_24DNB
_database_code_depnum_ccdc_archive 'CCDC 1584549'
_audit_update_record             
;
2018-02-08 deposited with the CCDC.
2018-02-23 downloaded from the CCDC.
;
_audit_creation_date             2018-01-10
_audit_creation_method           
;
Olex2 1.2-dev
(compiled 2017.12.08 svn.r3473 for OlexSys, GUI svn.r5356)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C16 H13 N4 Nd O16'
_chemical_formula_sum            'C16 H13 N4 Nd O16'
_chemical_formula_weight         661.53
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   8.9260(9)
_cell_length_b                   8.9830(8)
_cell_length_c                   16.6560(16)
_cell_angle_alpha                75.642(3)
_cell_angle_beta                 77.479(3)
_cell_angle_gamma                61.240(3)
_cell_volume                     1126.70(19)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9991
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      32.25
_cell_measurement_theta_min      2.54
_shelx_estimated_absorpt_T_max   0.672
_shelx_estimated_absorpt_T_min   0.597
_exptl_absorpt_coefficient_mu    2.395
_exptl_absorpt_correction_T_max  0.677
_exptl_absorpt_correction_T_min  0.592
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   
'SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.950
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needles
_exptl_crystal_F_000             650
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_unetI/netI     0.0343
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            30227
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.605
_diffrn_reflns_theta_min         2.541
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7151
_reflns_number_total             8090
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'Sir-92 (Altomare et al., 1993)'
_refine_diff_density_max         2.580
_refine_diff_density_min         -0.957
_refine_diff_density_rms         0.139
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         8090
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0315
_refine_ls_restrained_S_all      1.089
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0465P)²+0.3739P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0772
_refine_ls_wR_factor_ref         0.0839
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H2WA,H2WB} of O2W
 At 1.5 times of:
  All C(H,H,H) groups, {H1WA,H1WB} of O1W
2. Restrained distances
 O2W-H2WA = O2W-H2WB
 0.82 with sigma of 0.02
 O1W-H1WA = O1W-H1WB
 0.85 with sigma of 0.02
 H1WA-H1WB
 1.34 with sigma of 0.04
 Nd1-H1WA \\sim Nd1-H1WB
 with sigma of 0.02
3.a Me refined with riding coordinates:
 C15(H15A,H15B,H15C)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C7(H7), C11(H11), C13(H13), C14(H14)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.5372(3) 1.0306(3) 0.12051(16) 0.0243(4) Uani 1 1 d . . . . .
C2 C 0.5907(3) 0.9815(3) 0.20709(16) 0.0279(5) Uani 1 1 d . . . . .
C3 C 0.4913(4) 0.9407(4) 0.27760(18) 0.0314(5) Uani 1 1 d . . . . .
C4 C 0.5300(4) 0.9094(4) 0.35780(19) 0.0392(6) Uani 1 1 d . . . . .
H4 H 0.461848 0.882780 0.403982 0.047 Uiso 1 1 calc R . . . .
C5 C 0.6746(4) 0.9198(4) 0.36579(19) 0.0406(7) Uani 1 1 d . . . . .
C6 C 0.7803(4) 0.9560(5) 0.2990(2) 0.0446(8) Uani 1 1 d . . . . .
H6 H 0.878009 0.960314 0.306891 0.054 Uiso 1 1 calc R . . . .
C7 C 0.7366(4) 0.9858(4) 0.21925(19) 0.0364(6) Uani 1 1 d . . . . .
H7 H 0.807086 1.009054 0.173234 0.044 Uiso 1 1 calc R . . . .
C8 C 1.0995(3) 0.5433(3) -0.17487(15) 0.0251(4) Uani 1 1 d . . . . .
C9 C 1.1399(3) 0.5681(3) -0.26918(16) 0.0271(5) Uani 1 1 d . . . . .
C10 C 1.2756(4) 0.6001(4) -0.31366(18) 0.0311(5) Uani 1 1 d . . . . .
C11 C 1.3020(4) 0.6277(4) -0.39960(19) 0.0375(6) Uani 1 1 d . . . . .
H11 H 1.392799 0.650087 -0.428117 0.045 Uiso 1 1 calc R . . . .
C12 C 1.1894(4) 0.6210(4) -0.44160(18) 0.0370(6) Uani 1 1 d . . . . .
C13 C 1.0538(5) 0.5887(5) -0.4015(2) 0.0433(7) Uani 1 1 d . . . . .
H13 H 0.980318 0.583904 -0.431652 0.052 Uiso 1 1 calc R . . . .
C14 C 1.0289(4) 0.5635(4) -0.31479(18) 0.0383(6) Uani 1 1 d . . . . .
H14 H 0.936656 0.543140 -0.286768 0.046 Uiso 1 1 calc R . . . .
C15 C 1.2990(4) 0.5351(4) 0.1085(2) 0.0450(8) Uani 1 1 d . . . . .
H15A H 1.360740 0.414702 0.104935 0.067 Uiso 1 1 calc R . . . .
H15B H 1.375966 0.586469 0.089940 0.067 Uiso 1 1 calc R . . . .
H15C H 1.252074 0.548961 0.165258 0.067 Uiso 1 1 calc R . . . .
C16 C 1.1569(3) 0.6209(3) 0.05473(16) 0.0256(5) Uani 1 1 d . . . . .
N1 N 0.3397(4) 0.9237(4) 0.26901(16) 0.0392(6) Uani 1 1 d . . . . .
N2 N 0.7145(4) 0.8933(4) 0.45131(19) 0.0528(8) Uani 1 1 d . . . . .
N3 N 1.3962(4) 0.6076(4) -0.26896(17) 0.0399(6) Uani 1 1 d . . . . .
N4 N 1.2169(4) 0.6493(4) -0.53368(17) 0.0484(7) Uani 1 1 d . . . . .
O1 O 0.6548(2) 0.9989(2) 0.06114(12) 0.0275(4) Uani 1 1 d . . . . .
O2 O 0.3798(2) 1.1055(2) 0.11473(12) 0.0295(4) Uani 1 1 d . . . . .
O1W O 0.5521(3) 0.7333(3) 0.04969(13) 0.0331(4) Uani 1 1 d D . . . .
H1WA H 0.543(4) 0.706(5) 0.0991(11) 0.050 Uiso 1 1 d DR . . . .
H1WB H 0.467(3) 0.823(3) 0.030(2) 0.050 Uiso 1 1 d DR . . . .
O3 O 0.3630(4) 0.8143(4) 0.22974(15) 0.0521(6) Uani 1 1 d . . . . .
O2W O 0.8677(3) 1.0043(3) -0.09667(13) 0.0382(5) Uani 1 1 d D . . . .
H2WA H 0.900(5) 1.067(4) -0.084(2) 0.046 Uiso 1 1 d DR . . . .
H2WB H 0.847(5) 1.033(5) -0.1437(13) 0.046 Uiso 1 1 d DR . . . .
O4 O 0.2016(3) 1.0148(4) 0.30328(19) 0.0621(7) Uani 1 1 d . . . . .
O5 O 0.6618(4) 0.8065(5) 0.50642(17) 0.0727(9) Uani 1 1 d . . . . .
O6 O 0.7962(5) 0.9617(5) 0.46160(19) 0.0760(10) Uani 1 1 d . . . . .
O7 O 0.8324(3) 0.6093(2) 0.13722(12) 0.0299(4) Uani 1 1 d . . . . .
O8 O 0.9926(3) 0.6746(2) -0.14557(12) 0.0349(4) Uani 1 1 d . . . . .
O9 O 1.3709(4) 0.5879(4) -0.19260(15) 0.0523(6) Uani 1 1 d . . . . .
O10 O 1.5134(4) 0.6351(5) -0.3097(2) 0.0721(9) Uani 1 1 d . . . . .
O11 O 1.3375(4) 0.6791(4) -0.56753(16) 0.0669(8) Uani 1 1 d . . . . .
O12 O 1.1192(5) 0.6395(5) -0.57074(17) 0.0730(9) Uani 1 1 d . . . . .
O13 O 1.1320(2) 0.5308(2) 0.01588(12) 0.0263(4) Uani 1 1 d . . . . .
O14 O 1.0565(3) 0.7800(2) 0.04863(14) 0.0353(4) Uani 1 1 d . . . . .
Nd1 Nd 0.82962(2) 0.75269(2) -0.01103(2) 0.01952(4) Uani 1 1 d 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
C1 C2 1.511(3) . ?
C1 O1 1.250(3) . ?
C1 O2 1.246(3) . ?
C2 C3 1.396(4) . ?
C2 C7 1.380(4) . ?
C3 C4 1.379(4) . ?
C3 N1 1.473(4) . ?
C4 H4 0.9300 . ?
C4 C5 1.374(5) . ?
C5 C6 1.377(5) . ?
C5 N2 1.477(4) . ?
C6 H6 0.9300 . ?
C6 C7 1.391(4) . ?
C7 H7 0.9300 . ?
C8 C9 1.518(4) . ?
C8 O7 1.257(3) 2_765 ?
C8 O8 1.241(3) . ?
C9 C10 1.392(4) . ?
C9 C14 1.394(4) . ?
C10 C11 1.378(4) . ?
C10 N3 1.470(4) . ?
C11 H11 0.9300 . ?
C11 C12 1.374(4) . ?
C12 C13 1.374(5) . ?
C12 N4 1.477(4) . ?
C13 H13 0.9300 . ?
C13 C14 1.391(4) . ?
C14 H14 0.9300 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C15 C16 1.488(4) . ?
C16 O13 1.272(3) . ?
C16 O14 1.262(3) . ?
C16 Nd1 2.925(2) . ?
N1 O3 1.225(4) . ?
N1 O4 1.213(4) . ?
N2 O5 1.218(5) . ?
N2 O6 1.215(4) . ?
N3 O9 1.226(4) . ?
N3 O10 1.214(4) . ?
N4 O11 1.220(4) . ?
N4 O12 1.218(4) . ?
O1 Nd1 2.4404(17) . ?
O2 Nd1 2.4735(18) 2_675 ?
O1W H1WA 0.797(17) . ?
O1W H1WB 0.846(17) . ?
O1W Nd1 2.536(2) . ?
O2W H2WA 0.828(18) . ?
O2W H2WB 0.796(18) . ?
O2W Nd1 2.487(2) . ?
O7 Nd1 2.4852(19) . ?
O8 Nd1 2.452(2) . ?
O13 Nd1 2.4210(17) 2_765 ?
O13 Nd1 2.5226(18) . ?
O14 Nd1 2.5736(19) . ?

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 C1 C2 116.9(2) . . ?
O2 C1 C2 116.9(2) . . ?
O2 C1 O1 126.1(2) . . ?
C3 C2 C1 122.1(2) . . ?
C7 C2 C1 120.2(3) . . ?
C7 C2 C3 117.6(2) . . ?
C2 C3 N1 120.5(2) . . ?
C4 C3 C2 123.1(3) . . ?
C4 C3 N1 116.3(3) . . ?
C3 C4 H4 121.8 . . ?
C5 C4 C3 116.4(3) . . ?
C5 C4 H4 121.8 . . ?
C4 C5 C6 123.5(3) . . ?
C4 C5 N2 117.2(3) . . ?
C6 C5 N2 119.2(3) . . ?
C5 C6 H6 121.0 . . ?
C5 C6 C7 118.0(3) . . ?
C7 C6 H6 121.0 . . ?
C2 C7 C6 121.3(3) . . ?
C2 C7 H7 119.4 . . ?
C6 C7 H7 119.4 . . ?
O7 C8 C9 115.9(2) 2_765 . ?
O8 C8 C9 115.6(2) . . ?
O8 C8 O7 128.2(2) . 2_765 ?
C10 C9 C8 125.3(2) . . ?
C10 C9 C14 117.5(3) . . ?
C14 C9 C8 117.1(2) . . ?
C9 C10 N3 120.0(3) . . ?
C11 C10 C9 122.6(3) . . ?
C11 C10 N3 117.4(3) . . ?
C10 C11 H11 121.2 . . ?
C12 C11 C10 117.6(3) . . ?
C12 C11 H11 121.2 . . ?
C11 C12 N4 118.1(3) . . ?
C13 C12 C11 122.8(3) . . ?
C13 C12 N4 119.1(3) . . ?
C12 C13 H13 120.8 . . ?
C12 C13 C14 118.4(3) . . ?
C14 C13 H13 120.8 . . ?
C9 C14 H14 119.5 . . ?
C13 C14 C9 121.1(3) . . ?
C13 C14 H14 119.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C16 C15 H15A 109.5 . . ?
C16 C15 H15B 109.5 . . ?
C16 C15 H15C 109.5 . . ?
C15 C16 Nd1 164.3(2) . . ?
O13 C16 C15 119.3(2) . . ?
O13 C16 Nd1 59.22(12) . . ?
O14 C16 C15 121.8(2) . . ?
O14 C16 O13 118.8(2) . . ?
O14 C16 Nd1 61.50(13) . . ?
O3 N1 C3 117.4(3) . . ?
O4 N1 C3 118.1(3) . . ?
O4 N1 O3 124.5(3) . . ?
O5 N2 C5 117.9(3) . . ?
O6 N2 C5 117.4(3) . . ?
O6 N2 O5 124.8(3) . . ?
O9 N3 C10 117.9(3) . . ?
O10 N3 C10 118.2(3) . . ?
O10 N3 O9 123.9(3) . . ?
O11 N4 C12 117.6(3) . . ?
O12 N4 C12 118.0(3) . . ?
O12 N4 O11 124.4(3) . . ?
C1 O1 Nd1 134.69(16) . . ?
C1 O2 Nd1 142.05(17) . 2_675 ?
H1WA O1W H1WB 115(3) . . ?
Nd1 O1W H1WA 114(2) . . ?
Nd1 O1W H1WB 110(2) . . ?
H2WA O2W H2WB 111(4) . . ?
Nd1 O2W H2WA 130(3) . . ?
Nd1 O2W H2WB 118(3) . . ?
C8 O7 Nd1 135.46(17) 2_765 . ?
C8 O8 Nd1 138.64(17) . . ?
C16 O13 Nd1 146.11(17) . 2_765 ?
C16 O13 Nd1 95.12(14) . . ?
Nd1 O13 Nd1 109.82(6) 2_765 . ?
C16 O14 Nd1 92.98(14) . . ?
O1 Nd1 O2 87.70(6) . 2_675 ?
O1 Nd1 O1W 73.99(7) . . ?
O1 Nd1 O2W 71.96(7) . . ?
O1 Nd1 O7 78.44(6) . . ?
O1 Nd1 O8 142.40(6) . . ?
O1 Nd1 O13 124.75(6) . . ?
O1 Nd1 O14 77.52(6) . . ?
O2 Nd1 O1W 69.35(7) 2_675 . ?
O2 Nd1 O2W 71.87(7) 2_675 . ?
O2 Nd1 O7 136.46(7) 2_675 . ?
O2 Nd1 O13 144.97(6) 2_675 . ?
O2 Nd1 O14 143.58(7) 2_675 . ?
O1W Nd1 O14 134.67(7) . . ?
O2W Nd1 O1W 128.54(7) . . ?
O2W Nd1 O13 103.48(7) . . ?
O2W Nd1 O14 71.93(7) . . ?
O7 Nd1 O1W 67.18(7) . . ?
O7 Nd1 O2W 138.02(6) . . ?
O7 Nd1 O13 70.15(6) . . ?
O7 Nd1 O14 73.12(7) . . ?
O8 Nd1 O2 73.37(7) . 2_675 ?
O8 Nd1 O1W 125.26(8) . . ?
O8 Nd1 O2W 71.37(7) . . ?
O8 Nd1 O7 136.91(6) . . ?
O8 Nd1 O13 72.37(6) . . ?
O8 Nd1 O14 98.61(7) . . ?
O13 Nd1 O1 142.29(6) 2_765 . ?
O13 Nd1 O2 92.63(6) 2_765 2_675 ?
O13 Nd1 O1W 70.96(6) 2_765 . ?
O13 Nd1 O1W 127.62(6) . . ?
O13 Nd1 O2W 143.24(7) 2_765 . ?
O13 Nd1 O7 75.59(6) 2_765 . ?
O13 Nd1 O8 72.30(7) 2_765 . ?
O13 Nd1 O13 70.18(6) 2_765 . ?
O13 Nd1 O14 119.29(6) 2_765 . ?
O13 Nd1 O14 50.67(6) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 -174.5(3) . . . . ?
C1 C2 C3 N1 7.4(4) . . . . ?
C1 C2 C7 C6 174.3(3) . . . . ?
C2 C1 O1 Nd1 89.4(3) . . . . ?
C2 C1 O2 Nd1 174.85(19) . . . 2_675 ?
C2 C3 C4 C5 -0.2(5) . . . . ?
C2 C3 N1 O3 59.8(4) . . . . ?
C2 C3 N1 O4 -122.5(3) . . . . ?
C3 C2 C7 C6 -2.0(5) . . . . ?
C3 C4 C5 C6 -1.2(5) . . . . ?
C3 C4 C5 N2 177.7(3) . . . . ?
C4 C3 N1 O3 -118.5(3) . . . . ?
C4 C3 N1 O4 59.3(4) . . . . ?
C4 C5 C6 C7 0.9(5) . . . . ?
C4 C5 N2 O5 25.9(5) . . . . ?
C4 C5 N2 O6 -153.3(4) . . . . ?
C5 C6 C7 C2 0.8(5) . . . . ?
C6 C5 N2 O5 -155.1(4) . . . . ?
C6 C5 N2 O6 25.7(5) . . . . ?
C7 C2 C3 C4 1.7(4) . . . . ?
C7 C2 C3 N1 -176.4(3) . . . . ?
C8 C9 C10 C11 -177.6(3) . . . . ?
C8 C9 C10 N3 1.7(4) . . . . ?
C8 C9 C14 C13 178.6(3) . . . . ?
C9 C8 O8 Nd1 171.29(19) . . . . ?
C9 C10 C11 C12 -0.7(5) . . . . ?
C9 C10 N3 O9 -1.2(4) . . . . ?
C9 C10 N3 O10 179.7(3) . . . . ?
C10 C9 C14 C13 0.5(5) . . . . ?
C10 C11 C12 C13 0.2(5) . . . . ?
C10 C11 C12 N4 -179.7(3) . . . . ?
C11 C10 N3 O9 178.0(3) . . . . ?
C11 C10 N3 O10 -1.0(5) . . . . ?
C11 C12 C13 C14 0.6(5) . . . . ?
C11 C12 N4 O11 -0.8(5) . . . . ?
C11 C12 N4 O12 178.4(3) . . . . ?
C12 C13 C14 C9 -0.9(5) . . . . ?
C13 C12 N4 O11 179.4(3) . . . . ?
C13 C12 N4 O12 -1.5(5) . . . . ?
C14 C9 C10 C11 0.4(4) . . . . ?
C14 C9 C10 N3 179.6(3) . . . . ?
C15 C16 O13 Nd1 161.9(2) . . . . ?
C15 C16 O13 Nd1 23.9(5) . . . 2_765 ?
C15 C16 O14 Nd1 -162.2(3) . . . . ?
N1 C3 C4 C5 178.0(3) . . . . ?
N2 C5 C6 C7 -178.0(3) . . . . ?
N3 C10 C11 C12 -179.9(3) . . . . ?
N4 C12 C13 C14 -179.6(3) . . . . ?
O1 C1 C2 C3 -152.3(3) . . . . ?
O1 C1 C2 C7 31.6(4) . . . . ?
O1 C1 O2 Nd1 -1.9(5) . . . 2_675 ?
O2 C1 C2 C3 30.6(4) . . . . ?
O2 C1 C2 C7 -145.5(3) . . . . ?
O2 C1 O1 Nd1 -93.9(3) . . . . ?
O7 C8 C9 C10 -91.4(3) 2_765 . . . ?
O7 C8 C9 C14 90.6(3) 2_765 . . . ?
O7 C8 O8 Nd1 -2.3(5) 2_765 . . . ?
O8 C8 C9 C10 94.1(3) . . . . ?
O8 C8 C9 C14 -83.8(3) . . . . ?
O13 C16 O14 Nd1 15.5(3) . . . . ?
O14 C16 O13 Nd1 -15.8(3) . . . . ?
O14 C16 O13 Nd1 -153.9(2) . . . 2_765 ?
Nd1 C16 O13 Nd1 -138.1(3) . . . 2_765 ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_GDAC_24dnb
_database_code_depnum_ccdc_archive 'CCDC 1584546'
_audit_update_record             
;
2018-02-08 deposited with the CCDC.
2018-02-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H26 Gd2 N4 O24'
_chemical_formula_sum            'C22 H26 Gd2 N4 O24'
_chemical_formula_weight         1044.95

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1650 3.9040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   14.1321(4)
_cell_length_b                   8.8970(3)
_cell_length_c                   25.7568(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3238.49(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9938
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      35.42

_exptl_crystal_description       Needles
_exptl_crystal_colour            White
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.143
_exptl_crystal_F_000             2024
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.130
_exptl_absorpt_coefficient_mu    4.166
_shelx_estimated_absorpt_T_min   0.538
_shelx_estimated_absorpt_T_max   0.613
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.531
_exptl_absorpt_correction_T_max  0.619
_exptl_absorpt_process_details   
'SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction'

_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            30138
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         1.581
_diffrn_reflns_theta_max         35.442
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             7216
_reflns_number_gt                6412
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Sir-92 (Altomare et al., 1993)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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.All hydrogen atoms were 
fixed geometrically with their Uiso values 1.2 times of phenylene carbons. 
The hydrogen atoms of water molecules were located from the difference 
Fourier synthesis and were refined isotropically with distance of 0.82 Å 
with Uiso values 1.2 times that of their carrier oxygen atoms.
hydrogen atoms of methyl groups of coordinated acetate group were fixed 
geometrically with their Uiso values 1.5 times of their carrier carbons
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0140P)²+7.9895P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7216
_refine_ls_number_parameters     249
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0270
_refine_ls_wR_factor_ref         0.0626
_refine_ls_wR_factor_gt          0.0603
_refine_ls_goodness_of_fit_ref   1.243
_refine_ls_restrained_S_all      1.243
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.11099(15) 0.2019(2) 0.14651(8) 0.0118(3) Uani 1 1 d . . . . .
C2 C 0.13510(16) 0.2920(2) 0.19423(8) 0.0122(3) Uani 1 1 d . . . . .
C3 C 0.07515(15) 0.3103(2) 0.23688(9) 0.0129(3) Uani 1 1 d . . . . .
C4 C 0.10220(16) 0.3831(3) 0.28205(9) 0.0138(3) Uani 1 1 d . . . . .
H4 H 0.060840 0.391735 0.310979 0.017 Uiso 1 1 calc R U . . .
C5 C 0.19256(16) 0.4427(2) 0.28280(8) 0.0136(3) Uani 1 1 d . . . . .
C6 C 0.25460(16) 0.4305(3) 0.24165(9) 0.0153(4) Uani 1 1 d . . . . .
H6 H 0.315831 0.474293 0.243446 0.018 Uiso 1 1 calc R U . . .
C7 C 0.22581(16) 0.3529(3) 0.19745(9) 0.0152(4) Uani 1 1 d . . . . .
H7 H 0.268405 0.341296 0.169202 0.018 Uiso 1 1 calc R U . . .
C8 C 0.00842(18) -0.4141(3) 0.11371(12) 0.0219(5) Uani 1 1 d . . . . .
H8A H 0.042998 -0.447601 0.144586 0.033 Uiso 1 1 calc R U . . .
H8B H 0.019735 -0.484509 0.085130 0.033 Uiso 1 1 calc R U . . .
H8C H -0.059446 -0.410414 0.121433 0.033 Uiso 1 1 calc R U . . .
C9 C 0.04182(15) -0.2614(2) 0.09847(8) 0.0112(3) Uani 1 1 d . . . . .
C10 C 0.13824(18) -0.2957(3) -0.07441(10) 0.0191(4) Uani 1 1 d . . . . .
H10A H 0.085006 -0.292377 -0.098765 0.029 Uiso 1 1 calc R U . . .
H10B H 0.140985 -0.395032 -0.058026 0.029 Uiso 1 1 calc R U . . .
H10C H 0.197368 -0.276858 -0.093199 0.029 Uiso 1 1 calc R U . . .
C11 C 0.12509(15) -0.1781(2) -0.03360(8) 0.0110(3) Uani 1 1 d . . . . .
N1 N -0.02322(14) 0.2569(2) 0.23459(8) 0.0172(4) Uani 1 1 d . . . . .
N2 N 0.22350(15) 0.5206(2) 0.33008(8) 0.0171(3) Uani 1 1 d . . . . .
O1 O 0.07903(13) 0.07085(19) 0.15133(7) 0.0168(3) Uani 1 1 d . . . . .
O2 O 0.12944(12) 0.25841(18) 0.10255(7) 0.0135(3) Uani 1 1 d . . . . .
O3 O -0.06515(14) 0.2682(3) 0.19324(8) 0.0245(4) Uani 1 1 d . . . . .
O4 O -0.05804(15) 0.2069(3) 0.27469(9) 0.0301(5) Uani 1 1 d . . . . .
O5 O 0.17888(16) 0.4979(2) 0.36993(8) 0.0259(4) Uani 1 1 d . . . . .
O6 O 0.29287(15) 0.6034(2) 0.32684(8) 0.0272(4) Uani 1 1 d . . . . .
O7 O -0.01657(12) -0.16315(19) 0.08374(7) 0.0153(3) Uani 1 1 d . . . . .
O8 O 0.12992(11) -0.23125(18) 0.09860(7) 0.0148(3) Uani 1 1 d . . . . .
O9 O 0.04563(11) -0.11297(18) -0.02752(7) 0.0130(3) Uani 1 1 d . . . . .
O10 O 0.19237(12) -0.1459(2) -0.00347(7) 0.0170(3) Uani 1 1 d . . . . .
O1W O 0.26321(11) 0.02264(18) 0.08334(7) 0.0147(3) Uani 1 1 d D . . . .
H11W H 0.298(2) -0.049(2) 0.0874(14) 0.018 Uiso 1 1 d D U . . .
H12W H 0.298(2) 0.095(2) 0.0879(13) 0.018 Uiso 1 1 d D U . . .
O2W O 0.14759(12) 0.1904(2) -0.00825(7) 0.0171(3) Uani 1 1 d D . . . .
H22W H 0.122(2) 0.191(4) -0.0367(9) 0.021 Uiso 1 1 d D U . . .
H21W H 0.1943(17) 0.242(3) -0.0111(12) 0.021 Uiso 1 1 d D U . . .
Gd1 Gd 0.10294(2) 0.01653(2) 0.05664(2) 0.00852(3) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.256(3) . ?
C1 O2 1.266(3) . ?
C1 C2 1.507(3) . ?
C2 C7 1.394(3) . ?
C2 C3 1.397(3) . ?
C3 C4 1.386(3) . ?
C3 N1 1.470(3) . ?
C4 C5 1.383(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.380(3) . ?
C5 N2 1.468(3) . ?
C6 C7 1.392(3) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C9 1.490(3) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 O7 1.261(3) . ?
C9 O8 1.274(3) . ?
C10 C11 1.495(3) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 O10 1.260(3) . ?
C11 O9 1.273(3) . ?
N1 O3 1.223(3) . ?
N1 O4 1.228(3) . ?
N2 O5 1.222(3) . ?
N2 O6 1.229(3) . ?
O1 Gd1 2.5093(18) . ?
O2 Gd1 2.4839(16) . ?
O7 Gd1 2.4280(17) . ?
O8 Gd1 2.4847(17) . ?
O9 Gd1 2.3890(16) 5 ?
O9 Gd1 2.5850(17) . ?
O10 Gd1 2.4664(17) . ?
O1W Gd1 2.3678(16) . ?
O1W H11W 0.815(17) . ?
O1W H12W 0.812(17) . ?
O2W Gd1 2.3629(17) . ?
O2W H22W 0.814(17) . ?
O2W H21W 0.807(17) . ?

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 C1 O2 122.1(2) . . ?
O1 C1 C2 119.6(2) . . ?
O2 C1 C2 118.13(19) . . ?
C7 C2 C3 117.8(2) . . ?
C7 C2 C1 117.60(19) . . ?
C3 C2 C1 124.5(2) . . ?
C4 C3 C2 123.2(2) . . ?
C4 C3 N1 116.5(2) . . ?
C2 C3 N1 120.3(2) . . ?
C5 C4 C3 116.5(2) . . ?
C5 C4 H4 121.8 . . ?
C3 C4 H4 121.8 . . ?
C6 C5 C4 123.1(2) . . ?
C6 C5 N2 119.0(2) . . ?
C4 C5 N2 117.9(2) . . ?
C5 C6 C7 118.8(2) . . ?
C5 C6 H6 120.6 . . ?
C7 C6 H6 120.6 . . ?
C6 C7 C2 120.7(2) . . ?
C6 C7 H7 119.7 . . ?
C2 C7 H7 119.7 . . ?
C9 C8 H8A 109.5 . . ?
C9 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C9 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O7 C9 O8 119.6(2) . . ?
O7 C9 C8 120.3(2) . . ?
O8 C9 C8 120.1(2) . . ?
C11 C10 H10A 109.5 . . ?
C11 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C11 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O10 C11 O9 119.11(19) . . ?
O10 C11 C10 119.9(2) . . ?
O9 C11 C10 121.0(2) . . ?
O3 N1 O4 124.6(2) . . ?
O3 N1 C3 117.8(2) . . ?
O4 N1 C3 117.5(2) . . ?
O5 N2 O6 124.6(2) . . ?
O5 N2 C5 117.7(2) . . ?
O6 N2 C5 117.7(2) . . ?
C1 O1 Gd1 91.96(14) . . ?
C1 O2 Gd1 92.89(13) . . ?
C9 O7 Gd1 95.05(13) . . ?
C9 O8 Gd1 92.05(13) . . ?
C11 O9 Gd1 154.15(15) . 5 ?
C11 O9 Gd1 91.69(13) . . ?
Gd1 O9 Gd1 112.25(6) 5 . ?
C11 O10 Gd1 97.64(13) . . ?
Gd1 O1W H11W 127(2) . . ?
Gd1 O1W H12W 129(2) . . ?
H11W O1W H12W 104(2) . . ?
Gd1 O2W H22W 122(2) . . ?
Gd1 O2W H21W 131(2) . . ?
H22W O2W H21W 106(2) . . ?
O2W Gd1 O1W 86.27(6) . . ?
O2W Gd1 O9 77.15(6) . 5 ?
O1W Gd1 O9 157.47(6) . 5 ?
O2W Gd1 O7 145.09(6) . . ?
O1W Gd1 O7 126.65(6) . . ?
O9 Gd1 O7 73.47(6) 5 . ?
O2W Gd1 O10 78.62(7) . . ?
O1W Gd1 O10 72.88(6) . . ?
O9 Gd1 O10 117.63(6) 5 . ?
O7 Gd1 O10 98.69(6) . . ?
O2W Gd1 O2 74.30(6) . . ?
O1W Gd1 O2 72.40(6) . . ?
O9 Gd1 O2 88.33(6) 5 . ?
O7 Gd1 O2 122.58(6) . . ?
O10 Gd1 O2 136.83(6) . . ?
O2W Gd1 O8 147.94(6) . . ?
O1W Gd1 O8 75.36(6) . . ?
O9 Gd1 O8 126.17(5) 5 . ?
O7 Gd1 O8 52.95(5) . . ?
O10 Gd1 O8 71.01(6) . . ?
O2 Gd1 O8 122.58(6) . . ?
O2W Gd1 O1 126.68(6) . . ?
O1W Gd1 O1 80.91(6) . . ?
O9 Gd1 O1 96.76(6) 5 . ?
O7 Gd1 O1 75.74(6) . . ?
O10 Gd1 O1 142.37(6) . . ?
O2 Gd1 O1 52.46(5) . . ?
O8 Gd1 O1 76.62(6) . . ?
O2W Gd1 O9 77.43(6) . . ?
O1W Gd1 O9 123.61(6) . . ?
O9 Gd1 O9 67.75(6) 5 . ?
O7 Gd1 O9 74.31(6) . . ?
O10 Gd1 O9 51.17(5) . . ?
O2 Gd1 O9 146.37(5) . . ?
O8 Gd1 O9 91.00(5) . . ?
O1 Gd1 O9 149.17(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
O1 C1 C2 C7 126.3(2) . . . . ?
O2 C1 C2 C7 -49.4(3) . . . . ?
O1 C1 C2 C3 -49.2(3) . . . . ?
O2 C1 C2 C3 135.1(2) . . . . ?
C7 C2 C3 C4 -1.2(3) . . . . ?
C1 C2 C3 C4 174.4(2) . . . . ?
C7 C2 C3 N1 176.2(2) . . . . ?
C1 C2 C3 N1 -8.3(3) . . . . ?
C2 C3 C4 C5 1.9(3) . . . . ?
N1 C3 C4 C5 -175.6(2) . . . . ?
C3 C4 C5 C6 -0.8(3) . . . . ?
C3 C4 C5 N2 -180.0(2) . . . . ?
C4 C5 C6 C7 -1.0(4) . . . . ?
N2 C5 C6 C7 178.2(2) . . . . ?
C5 C6 C7 C2 1.7(3) . . . . ?
C3 C2 C7 C6 -0.7(3) . . . . ?
C1 C2 C7 C6 -176.5(2) . . . . ?
C4 C3 N1 O3 141.4(2) . . . . ?
C2 C3 N1 O3 -36.2(3) . . . . ?
C4 C3 N1 O4 -37.2(3) . . . . ?
C2 C3 N1 O4 145.3(2) . . . . ?
C6 C5 N2 O5 -161.7(2) . . . . ?
C4 C5 N2 O5 17.6(3) . . . . ?
C6 C5 N2 O6 17.9(3) . . . . ?
C4 C5 N2 O6 -162.9(2) . . . . ?
O2 C1 O1 Gd1 8.0(2) . . . . ?
C2 C1 O1 Gd1 -167.52(17) . . . . ?
O1 C1 O2 Gd1 -8.1(2) . . . . ?
C2 C1 O2 Gd1 167.50(16) . . . . ?
O8 C9 O7 Gd1 5.8(2) . . . . ?
C8 C9 O7 Gd1 -171.8(2) . . . . ?
O7 C9 O8 Gd1 -5.6(2) . . . . ?
C8 C9 O8 Gd1 172.0(2) . . . . ?
O10 C11 O9 Gd1 152.2(2) . . . 5 ?
C10 C11 O9 Gd1 -30.2(5) . . . 5 ?
O10 C11 O9 Gd1 -6.1(2) . . . . ?
C10 C11 O9 Gd1 171.44(19) . . . . ?
O9 C11 O10 Gd1 6.5(2) . . . . ?
C10 C11 O10 Gd1 -171.12(18) . . . . ?

_refine_diff_density_max         2.483
_refine_diff_density_min         -1.556
_refine_diff_density_rms         0.136

####################################################################### 
# 
# 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_La_24DNB
_database_code_depnum_ccdc_archive 'CCDC 1584548'
_audit_update_record             
;
2018-02-08 deposited with the CCDC.
2018-02-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C45 H31 La2 N13 O40'
_chemical_formula_sum            'C45 H31 La2 N13 O40'
_chemical_formula_weight         1671.65

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'
La La -0.2871 2.4523 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.9791(13)
_cell_length_b                   14.499(2)
_cell_length_c                   23.157(4)
_cell_angle_alpha                81.559(8)
_cell_angle_beta                 89.492(7)
_cell_angle_gamma                81.411(7)
_cell_volume                     2948.5(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9965
_cell_measurement_theta_min      2.44
_cell_measurement_theta_max      29.32

_exptl_crystal_description       Needles
_exptl_crystal_colour            White
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.883
_exptl_crystal_F_000             1652
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.160
_exptl_absorpt_coefficient_mu    1.553
_shelx_estimated_absorpt_T_min   0.757
_shelx_estimated_absorpt_T_max   0.789
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.751
_exptl_absorpt_correction_T_max  0.795
_exptl_absorpt_process_details   
'SADABS-2014/2 - Bruker AXS area detector scaling and absorption correction'

_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            68102
_diffrn_reflns_av_unetI/netI     0.0561
_diffrn_reflns_av_R_equivalents  0.0530
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         1.574
_diffrn_reflns_theta_max         30.250
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             17467
_reflns_number_gt                13249
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Sir-92 (Altomare et al., 1993)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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.All hydrogen atoms were 
fixed geometrically with their Uiso values 1.2 times of phenylene carbons. 
The hydrogen atoms of water molecules were located from the difference 
Fourier synthesis and were refined isotropically with distance of 0.82 Å 
with Uiso values 1.2 times that of their carrier oxygen atoms.. In complex
, hydrogen atoms of methyl groups of coordinated DMF solvent were fixed 
geometrically with their Uiso values 1.5 times of their carrier carbons. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0374P)²+1.9003P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         17467
_refine_ls_number_parameters     921
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0381
_refine_ls_wR_factor_ref         0.0902
_refine_ls_wR_factor_gt          0.0810
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_restrained_S_all      1.001
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2695(3) 0.6789(2) 0.84462(13) 0.0256(6) Uani 1 1 d . . . . .
C2 C 0.2890(3) 0.6252(2) 0.90647(13) 0.0268(6) Uani 1 1 d . . . . .
C3 C 0.2240(3) 0.5459(2) 0.92778(13) 0.0290(7) Uani 1 1 d . . . . .
C4 C 0.2368(4) 0.5044(2) 0.98577(14) 0.0332(8) Uani 1 1 d . . . . .
H4 H 0.192580 0.451284 0.999102 0.040 Uiso 1 1 calc R U . . .
C5 C 0.3177(4) 0.5449(3) 1.02279(14) 0.0323(7) Uani 1 1 d . . . . .
C6 C 0.3857(4) 0.6222(3) 1.00435(15) 0.0365(8) Uani 1 1 d . . . . .
H6 H 0.439157 0.648140 1.030531 0.044 Uiso 1 1 calc R U . . .
C7 C 0.3736(4) 0.6613(2) 0.94572(15) 0.0343(8) Uani 1 1 d . . . . .
H7 H 0.422630 0.712386 0.932447 0.041 Uiso 1 1 calc R U . . .
C8 C 0.1827(3) 0.9409(2) 0.80470(13) 0.0258(6) Uani 1 1 d . . . . .
C9 C 0.2435(3) 1.0213(2) 0.82629(14) 0.0279(7) Uani 1 1 d . . . . .
C10 C 0.3143(4) 1.0173(2) 0.87965(15) 0.0315(7) Uani 1 1 d . . . . .
C11 C 0.3618(4) 1.0955(3) 0.89767(18) 0.0454(10) Uani 1 1 d . . . . .
H11 H 0.408332 1.092000 0.933814 0.054 Uiso 1 1 calc R U . . .
C12 C 0.3369(4) 1.1777(3) 0.8596(2) 0.0532(11) Uani 1 1 d . . . . .
C13 C 0.2731(5) 1.1844(3) 0.8051(2) 0.0578(12) Uani 1 1 d . . . . .
H13 H 0.262556 1.240975 0.779634 0.069 Uiso 1 1 calc R U . . .
C14 C 0.2253(4) 1.1061(3) 0.78878(17) 0.0426(9) Uani 1 1 d . . . . .
H14 H 0.180319 1.110030 0.752297 0.051 Uiso 1 1 calc R U . . .
C15 C 0.7193(3) 0.8145(2) 0.85277(12) 0.0251(6) Uani 1 1 d . . . . .
C16 C 0.8109(3) 0.8190(2) 0.90677(13) 0.0273(7) Uani 1 1 d . . . . .
C17 C 0.8096(4) 0.8986(3) 0.93408(14) 0.0314(7) Uani 1 1 d . . . . .
C18 C 0.8870(4) 0.8957(3) 0.98609(15) 0.0394(9) Uani 1 1 d . . . . .
H18 H 0.883940 0.949305 1.003993 0.047 Uiso 1 1 calc R U . . .
C19 C 0.9676(4) 0.8119(3) 1.01011(14) 0.0393(9) Uani 1 1 d . . . . .
C20 C 0.9753(4) 0.7318(3) 0.98460(15) 0.0404(9) Uani 1 1 d . . . . .
H20 H 1.031736 0.675576 1.001844 0.049 Uiso 1 1 calc R U . . .
C21 C 0.8975(4) 0.7361(3) 0.93272(14) 0.0356(8) Uani 1 1 d . . . . .
H21 H 0.903312 0.682266 0.914852 0.043 Uiso 1 1 calc R U . . .
C22 C -0.1899(3) 0.7745(2) 0.64028(12) 0.0265(6) Uani 1 1 d . . . . .
C23 C -0.2682(4) 0.7382(3) 0.59233(13) 0.0331(8) Uani 1 1 d . . . . .
C24 C -0.3364(5) 0.7958(4) 0.54379(18) 0.0595(12) Uani 1 1 d . . . . .
C25 C -0.4021(7) 0.7589(5) 0.4998(2) 0.097(2) Uani 1 1 d . . . . .
H25 H -0.449709 0.797763 0.467648 0.117 Uiso 1 1 calc R U . . .
C26 C -0.3936(6) 0.6634(5) 0.5058(2) 0.0785(19) Uani 1 1 d . . . . .
C27 C -0.3279(5) 0.6050(4) 0.5523(2) 0.0698(15) Uani 1 1 d . . . . .
H27 H -0.323927 0.540142 0.554600 0.084 Uiso 1 1 calc R U . . .
C28 C -0.2666(5) 0.6427(3) 0.5963(2) 0.0548(11) Uani 1 1 d . . . . .
H28 H -0.223765 0.602904 0.629067 0.066 Uiso 1 1 calc R U . . .
C29 C 0.3382(3) 0.6828(2) 0.68171(12) 0.0229(6) Uani 1 1 d . . . . .
C30 C 0.2669(3) 0.6021(2) 0.66524(14) 0.0281(7) Uani 1 1 d . . . . .
C31 C 0.1886(4) 0.6023(3) 0.61454(16) 0.0405(8) Uani 1 1 d . . . . .
C32 C 0.1150(5) 0.5274(3) 0.6055(2) 0.0613(13) Uani 1 1 d . . . . .
H32 H 0.062905 0.527760 0.570955 0.074 Uiso 1 1 calc R U . . .
C33 C 0.1229(5) 0.4533(3) 0.6501(3) 0.0611(13) Uani 1 1 d . . . . .
C34 C 0.1990(5) 0.4495(3) 0.7004(2) 0.0554(11) Uani 1 1 d . . . . .
H34 H 0.201603 0.397768 0.729533 0.066 Uiso 1 1 calc R U . . .
C35 C 0.2726(4) 0.5236(3) 0.70770(17) 0.0392(8) Uani 1 1 d . . . . .
H35 H 0.327556 0.520981 0.741919 0.047 Uiso 1 1 calc R U . . .
C36 C -0.3089(3) 1.0048(2) 0.72879(13) 0.0259(6) Uani 1 1 d . . . . .
C37 C -0.3084(3) 1.1085(2) 0.73304(14) 0.0266(6) Uani 1 1 d . . . . .
C38 C -0.4079(3) 1.1833(2) 0.70454(14) 0.0292(7) Uani 1 1 d . . . . .
C39 C -0.4028(4) 1.2765(2) 0.71004(16) 0.0351(8) Uani 1 1 d . . . . .
H39 H -0.471550 1.325271 0.690603 0.042 Uiso 1 1 calc R U . . .
C40 C -0.2912(4) 1.2938(2) 0.74556(15) 0.0327(7) Uani 1 1 d . . . . .
C41 C -0.1902(4) 1.2223(2) 0.77537(15) 0.0351(8) Uani 1 1 d . . . . .
H41 H -0.117130 1.235871 0.799725 0.042 Uiso 1 1 calc R U . . .
C42 C -0.1985(4) 1.1308(2) 0.76872(14) 0.0313(7) Uani 1 1 d . . . . .
H42 H -0.129449 1.082447 0.788418 0.038 Uiso 1 1 calc R U . . .
C43 C 0.0719(17) 1.1312(6) 0.6124(5) 0.280(9) Uani 1 1 d . . . . .
H43A H 0.087782 1.113822 0.653712 0.419 Uiso 1 1 calc R U . . .
H43B H 0.011902 1.192340 0.604558 0.419 Uiso 1 1 calc R U . . .
H43C H 0.167276 1.132723 0.593498 0.419 Uiso 1 1 calc R U . . .
C44 C -0.1015(9) 1.1066(7) 0.5440(4) 0.236(7) Uani 1 1 d . . . . .
H44A H -0.139438 1.057237 0.527851 0.354 Uiso 1 1 calc R U . . .
H44B H -0.048669 1.142096 0.514406 0.354 Uiso 1 1 calc R U . . .
H44C H -0.184010 1.147650 0.557619 0.354 Uiso 1 1 calc R U . . .
C45 C 0.0189(6) 0.9835(4) 0.6170(3) 0.099(2) Uani 1 1 d . . . . .
H45 H -0.037100 0.943415 0.601813 0.119 Uiso 1 1 calc R U . . .
N1 N 0.1404(4) 0.5010(2) 0.88841(13) 0.0411(7) Uani 1 1 d . . . . .
N2 N 0.3334(4) 0.5020(2) 1.08469(13) 0.0421(8) Uani 1 1 d . . . . .
N3 N 0.3376(4) 0.9292(2) 0.92076(13) 0.0409(7) Uani 1 1 d . . . . .
N4 N 0.3779(5) 1.2635(3) 0.8787(3) 0.0922(18) Uani 1 1 d . . . . .
N5 N 0.7248(3) 0.9896(2) 0.90820(14) 0.0410(7) Uani 1 1 d . . . . .
N6 N 1.0454(4) 0.8073(3) 1.06666(15) 0.0573(10) Uani 1 1 d . . . . .
N7 N -0.3345(7) 0.8958(4) 0.5352(2) 0.106(2) Uani 1 1 d . . . . .
N8 N -0.4610(10) 0.6251(7) 0.4585(2) 0.141(3) Uani 1 1 d . . . . .
N9 N 0.1833(5) 0.6810(3) 0.56694(15) 0.0597(10) Uani 1 1 d . . . . .
N10 N 0.0380(6) 0.3760(4) 0.6417(3) 0.1042(19) Uani 1 1 d . . . . .
N11 N -0.5213(4) 1.1664(2) 0.66331(14) 0.0438(8) Uani 1 1 d . . . . .
N12 N -0.2770(4) 1.3918(2) 0.75088(16) 0.0493(9) Uani 1 1 d . . . . .
N13 N -0.0013(5) 1.0665(3) 0.59146(19) 0.0760(13) Uani 1 1 d . . . . .
O1 O 0.3890(2) 0.68571(16) 0.81761(10) 0.0321(5) Uani 1 1 d . . . . .
O2 O 0.1385(2) 0.71376(16) 0.82822(9) 0.0318(5) Uani 1 1 d . . . . .
O3 O 0.1675(3) 0.51182(19) 0.83658(11) 0.0474(7) Uani 1 1 d . . . . .
O4 O 0.0476(5) 0.4541(3) 0.90999(14) 0.0962(15) Uani 1 1 d . . . . .
O5 O 0.2780(4) 0.4317(2) 1.09994(12) 0.0666(9) Uani 1 1 d . . . . .
O6 O 0.4032(4) 0.5369(2) 1.11753(13) 0.0702(10) Uani 1 1 d . . . . .
O7 O 0.2698(2) 0.88671(16) 0.77708(10) 0.0304(5) Uani 1 1 d . . . . .
O8 O 0.0457(2) 0.93718(17) 0.80963(11) 0.0366(6) Uani 1 1 d . . . . .
O9 O 0.2510(3) 0.8733(2) 0.91651(14) 0.0597(8) Uani 1 1 d . . . . .
O10 O 0.4416(3) 0.9167(2) 0.95593(12) 0.0618(8) Uani 1 1 d . . . . .
O11 O 0.3896(6) 1.2635(3) 0.9313(3) 0.129(2) Uani 1 1 d . . . . .
O12 O 0.3912(6) 1.3302(3) 0.8402(3) 0.130(2) Uani 1 1 d . . . . .
O13 O 0.7891(2) 0.80097(16) 0.80669(9) 0.0278(5) Uani 1 1 d . . . . .
O14 O 0.5806(2) 0.81673(19) 0.85695(9) 0.0379(6) Uani 1 1 d . . . . .
O15 O 0.6772(3) 0.99620(19) 0.85864(11) 0.0464(6) Uani 1 1 d . . . . .
O16 O 0.7068(4) 1.0537(2) 0.93807(15) 0.0705(10) Uani 1 1 d . . . . .
O17 O 1.0164(4) 0.8748(3) 1.09313(13) 0.0777(11) Uani 1 1 d . . . . .
O18 O 1.1349(5) 0.7363(3) 1.08366(15) 0.0921(13) Uani 1 1 d . . . . .
O19 O -0.0571(2) 0.7875(2) 0.63298(10) 0.0396(6) Uani 1 1 d . . . . .
O20 O -0.2590(2) 0.78404(15) 0.68706(9) 0.0263(5) Uani 1 1 d . . . . .
O21 O -0.3109(4) 0.9339(2) 0.57488(15) 0.0695(9) Uani 1 1 d . . . . .
O22 O -0.3502(13) 0.9392(5) 0.4861(3) 0.316(7) Uani 1 1 d . . . . .
O23 O -0.5606(9) 0.6768(7) 0.4279(2) 0.223(5) Uani 1 1 d . . . . .
O24 O -0.4115(7) 0.5420(6) 0.4539(3) 0.178(4) Uani 1 1 d . . . . .
O25 O 0.4778(2) 0.67481(16) 0.68362(10) 0.0325(5) Uani 1 1 d . . . . .
O26 O 0.2522(2) 0.74983(15) 0.69904(9) 0.0280(5) Uani 1 1 d . . . . .
O27 O 0.2671(4) 0.7396(2) 0.57031(12) 0.0595(8) Uani 1 1 d . . . . .
O28 O 0.0910(6) 0.6846(3) 0.52726(16) 0.1092(16) Uani 1 1 d . . . . .
O29 O -0.0258(10) 0.3807(5) 0.5973(4) 0.249(5) Uani 1 1 d . . . . .
O30 O 0.0398(5) 0.3114(3) 0.6815(2) 0.1123(17) Uani 1 1 d . . . . .
O31 O -0.4271(2) 0.97055(16) 0.73946(10) 0.0321(5) Uani 1 1 d . . . . .
O32 O -0.1835(2) 0.96213(16) 0.71646(11) 0.0355(5) Uani 1 1 d . . . . .
O33 O -0.4878(4) 1.1025(2) 0.63469(13) 0.0576(8) Uani 1 1 d . . . . .
O34 O -0.6414(3) 1.2187(2) 0.65913(17) 0.0779(11) Uani 1 1 d . . . . .
O35 O -0.3723(4) 1.4536(2) 0.72700(18) 0.0833(12) Uani 1 1 d . . . . .
O36 O -0.1722(4) 1.4068(2) 0.77826(18) 0.0793(12) Uani 1 1 d . . . . .
O37 O 0.1002(3) 0.94572(19) 0.65900(11) 0.0418(6) Uani 1 1 d . . . . .
O1W O 0.6795(3) 0.62893(16) 0.77625(10) 0.0290(5) Uani 1 1 d D . . . .
H11W H 0.656(4) 0.589(2) 0.7591(12) 0.035 Uiso 1 1 d D U . . .
H12W H 0.675(4) 0.608(2) 0.8105(7) 0.035 Uiso 1 1 d D U . . .
O2W O 0.4163(3) 0.89945(18) 0.65212(11) 0.0378(6) Uani 1 1 d D . . . .
H21W H 0.327(2) 0.908(2) 0.6490(17) 0.045 Uiso 1 1 d D U . . .
H22W H 0.445(4) 0.9494(17) 0.6454(17) 0.045 Uiso 1 1 d D U . . .
O3W O -0.0301(2) 0.64533(17) 0.74511(11) 0.0338(5) Uani 1 1 d D . . . .
H31W H -0.116(2) 0.632(2) 0.7495(15) 0.041 Uiso 1 1 d D U . . .
H32W H 0.015(3) 0.609(2) 0.7723(12) 0.041 Uiso 1 1 d D U . . .
La1 La 0.51522(2) 0.80072(2) 0.74938(2) 0.01927(5) Uani 1 1 d . . . . .
La2 La 0.00877(2) 0.81983(2) 0.73834(2) 0.01976(5) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.247(3) . ?
C1 O2 1.248(3) . ?
C1 C2 1.524(4) . ?
C2 C3 1.391(4) . ?
C2 C7 1.396(4) . ?
C3 C4 1.387(4) . ?
C3 N1 1.467(4) . ?
C4 C5 1.376(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.368(5) . ?
C5 N2 1.476(4) . ?
C6 C7 1.391(5) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 O8 1.243(4) . ?
C8 O7 1.262(4) . ?
C8 C9 1.507(4) . ?
C9 C10 1.384(4) . ?
C9 C14 1.386(5) . ?
C10 C11 1.389(5) . ?
C10 N3 1.465(5) . ?
C11 C12 1.364(6) . ?
C11 H11 0.9300 . ?
C12 C13 1.376(6) . ?
C12 N4 1.477(5) . ?
C13 C14 1.375(5) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C15 O14 1.244(3) . ?
C15 O13 1.258(3) . ?
C15 C16 1.518(4) . ?
C16 C21 1.389(5) . ?
C16 C17 1.394(5) . ?
C17 C18 1.388(4) . ?
C17 N5 1.467(5) . ?
C18 C19 1.362(5) . ?
C18 H18 0.9300 . ?
C19 C20 1.371(5) . ?
C19 N6 1.478(4) . ?
C20 C21 1.384(4) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
C22 O19 1.241(4) . ?
C22 O20 1.259(3) . ?
C22 C23 1.517(4) . ?
C23 C28 1.372(6) . ?
C23 C24 1.385(5) . ?
C24 C25 1.392(6) . ?
C24 N7 1.438(7) . ?
C25 C26 1.361(9) . ?
C25 H25 0.9300 . ?
C26 C27 1.348(8) . ?
C26 N8 1.472(6) . ?
C27 C28 1.381(6) . ?
C27 H27 0.9300 . ?
C28 H28 0.9300 . ?
C29 O25 1.242(3) . ?
C29 O26 1.260(3) . ?
C29 C30 1.511(4) . ?
C30 C31 1.373(5) . ?
C30 C35 1.386(5) . ?
C31 C32 1.394(5) . ?
C31 N9 1.461(5) . ?
C32 C33 1.370(7) . ?
C32 H32 0.9300 . ?
C33 C34 1.345(7) . ?
C33 N10 1.482(6) . ?
C34 C35 1.375(5) . ?
C34 H34 0.9300 . ?
C35 H35 0.9300 . ?
C36 O31 1.246(4) . ?
C36 O32 1.253(4) . ?
C36 C37 1.522(4) . ?
C37 C38 1.386(4) . ?
C37 C42 1.396(4) . ?
C38 C39 1.383(4) . ?
C38 N11 1.473(4) . ?
C39 C40 1.376(5) . ?
C39 H39 0.9300 . ?
C40 C41 1.377(5) . ?
C40 N12 1.468(4) . ?
C41 C42 1.371(5) . ?
C41 H41 0.9300 . ?
C42 H42 0.9300 . ?
C43 N13 1.367(9) . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C44 N13 1.426(7) . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C45 O37 1.230(5) . ?
C45 N13 1.249(6) . ?
C45 H45 0.9300 . ?
N1 O4 1.211(4) . ?
N1 O3 1.215(4) . ?
N2 O6 1.202(4) . ?
N2 O5 1.206(4) . ?
N3 O9 1.219(4) . ?
N3 O10 1.220(4) . ?
N4 O11 1.223(7) . ?
N4 O12 1.235(7) . ?
N5 O15 1.214(4) . ?
N5 O16 1.229(4) . ?
N6 O17 1.224(5) . ?
N6 O18 1.225(5) . ?
N7 O21 1.175(5) . ?
N7 O22 1.215(7) . ?
N8 O23 1.232(13) . ?
N8 O24 1.241(12) . ?
N9 O27 1.227(5) . ?
N9 O28 1.233(5) . ?
N10 O29 1.170(8) . ?
N10 O30 1.212(7) . ?
N11 O33 1.217(4) . ?
N11 O34 1.219(4) . ?
N12 O36 1.204(4) . ?
N12 O35 1.214(4) . ?
O1 La1 2.514(2) . ?
O2 La2 2.573(2) . ?
O7 La1 2.492(2) . ?
O7 La2 2.865(2) . ?
O8 La2 2.595(2) . ?
O13 La2 2.540(2) 1_655 ?
O13 La1 2.805(2) . ?
O14 La1 2.615(2) . ?
O19 La2 2.640(2) . ?
O20 La1 2.481(2) 1_455 ?
O20 La2 2.840(2) . ?
O25 La1 2.602(2) . ?
O26 La2 2.492(2) . ?
O26 La1 2.881(2) . ?
O31 La1 2.568(2) 1_455 ?
O32 La2 2.478(2) . ?
O37 La2 2.611(2) . ?
O1W La1 2.689(2) . ?
O1W H11W 0.808(17) . ?
O1W H12W 0.808(17) . ?
O2W La1 2.573(2) . ?
O2W H21W 0.798(17) . ?
O2W H22W 0.796(18) . ?
O3W La2 2.587(2) . ?
O3W H31W 0.823(17) . ?
O3W H32W 0.826(17) . ?

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 C1 O2 128.1(3) . . ?
O1 C1 C2 115.0(3) . . ?
O2 C1 C2 116.8(3) . . ?
C3 C2 C7 117.3(3) . . ?
C3 C2 C1 125.5(3) . . ?
C7 C2 C1 117.1(3) . . ?
C4 C3 C2 122.7(3) . . ?
C4 C3 N1 116.9(3) . . ?
C2 C3 N1 120.3(3) . . ?
C5 C4 C3 117.3(3) . . ?
C5 C4 H4 121.3 . . ?
C3 C4 H4 121.3 . . ?
C6 C5 C4 122.7(3) . . ?
C6 C5 N2 118.8(3) . . ?
C4 C5 N2 118.4(3) . . ?
C5 C6 C7 118.8(3) . . ?
C5 C6 H6 120.6 . . ?
C7 C6 H6 120.6 . . ?
C6 C7 C2 121.1(3) . . ?
C6 C7 H7 119.4 . . ?
C2 C7 H7 119.4 . . ?
O8 C8 O7 123.0(3) . . ?
O8 C8 C9 118.2(3) . . ?
O7 C8 C9 118.3(3) . . ?
C10 C9 C14 118.2(3) . . ?
C10 C9 C8 125.7(3) . . ?
C14 C9 C8 116.1(3) . . ?
C9 C10 C11 122.5(3) . . ?
C9 C10 N3 120.5(3) . . ?
C11 C10 N3 116.9(3) . . ?
C12 C11 C10 116.6(4) . . ?
C12 C11 H11 121.7 . . ?
C10 C11 H11 121.7 . . ?
C11 C12 C13 123.1(4) . . ?
C11 C12 N4 118.1(5) . . ?
C13 C12 N4 118.8(5) . . ?
C14 C13 C12 118.9(4) . . ?
C14 C13 H13 120.5 . . ?
C12 C13 H13 120.5 . . ?
C13 C14 C9 120.5(4) . . ?
C13 C14 H14 119.7 . . ?
C9 C14 H14 119.7 . . ?
O14 C15 O13 122.7(3) . . ?
O14 C15 C16 119.0(3) . . ?
O13 C15 C16 118.0(3) . . ?
C21 C16 C17 117.2(3) . . ?
C21 C16 C15 117.4(3) . . ?
C17 C16 C15 125.3(3) . . ?
C18 C17 C16 122.1(3) . . ?
C18 C17 N5 117.5(3) . . ?
C16 C17 N5 120.4(3) . . ?
C19 C18 C17 118.0(3) . . ?
C19 C18 H18 121.0 . . ?
C17 C18 H18 121.0 . . ?
C18 C19 C20 122.4(3) . . ?
C18 C19 N6 118.3(4) . . ?
C20 C19 N6 119.2(4) . . ?
C19 C20 C21 118.8(4) . . ?
C19 C20 H20 120.6 . . ?
C21 C20 H20 120.6 . . ?
C20 C21 C16 121.4(3) . . ?
C20 C21 H21 119.3 . . ?
C16 C21 H21 119.3 . . ?
O19 C22 O20 123.0(3) . . ?
O19 C22 C23 118.3(3) . . ?
O20 C22 C23 118.6(3) . . ?
C28 C23 C24 118.3(4) . . ?
C28 C23 C22 118.0(3) . . ?
C24 C23 C22 123.7(4) . . ?
C23 C24 C25 121.6(5) . . ?
C23 C24 N7 121.2(4) . . ?
C25 C24 N7 117.1(5) . . ?
C26 C25 C24 117.1(5) . . ?
C26 C25 H25 121.4 . . ?
C24 C25 H25 121.4 . . ?
C27 C26 C25 123.0(4) . . ?
C27 C26 N8 120.3(7) . . ?
C25 C26 N8 116.6(7) . . ?
C26 C27 C28 119.3(5) . . ?
C26 C27 H27 120.4 . . ?
C28 C27 H27 120.4 . . ?
C23 C28 C27 120.6(5) . . ?
C23 C28 H28 119.7 . . ?
C27 C28 H28 119.7 . . ?
O25 C29 O26 123.5(3) . . ?
O25 C29 C30 118.6(3) . . ?
O26 C29 C30 117.4(3) . . ?
C31 C30 C35 117.7(3) . . ?
C31 C30 C29 126.3(3) . . ?
C35 C30 C29 115.8(3) . . ?
C30 C31 C32 122.0(4) . . ?
C30 C31 N9 120.6(3) . . ?
C32 C31 N9 117.3(4) . . ?
C33 C32 C31 116.8(4) . . ?
C33 C32 H32 121.6 . . ?
C31 C32 H32 121.6 . . ?
C34 C33 C32 123.4(4) . . ?
C34 C33 N10 119.8(5) . . ?
C32 C33 N10 116.8(5) . . ?
C33 C34 C35 118.6(4) . . ?
C33 C34 H34 120.7 . . ?
C35 C34 H34 120.7 . . ?
C34 C35 C30 121.4(4) . . ?
C34 C35 H35 119.3 . . ?
C30 C35 H35 119.3 . . ?
O31 C36 O32 127.0(3) . . ?
O31 C36 C37 119.0(3) . . ?
O32 C36 C37 113.9(3) . . ?
C38 C37 C42 116.8(3) . . ?
C38 C37 C36 125.7(3) . . ?
C42 C37 C36 117.5(3) . . ?
C39 C38 C37 123.4(3) . . ?
C39 C38 N11 116.3(3) . . ?
C37 C38 N11 120.2(3) . . ?
C40 C39 C38 117.0(3) . . ?
C40 C39 H39 121.5 . . ?
C38 C39 H39 121.5 . . ?
C39 C40 C41 122.2(3) . . ?
C39 C40 N12 119.0(3) . . ?
C41 C40 N12 118.8(3) . . ?
C42 C41 C40 119.2(3) . . ?
C42 C41 H41 120.4 . . ?
C40 C41 H41 120.4 . . ?
C41 C42 C37 121.4(3) . . ?
C41 C42 H42 119.3 . . ?
C37 C42 H42 119.3 . . ?
N13 C43 H43A 109.5 . . ?
N13 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
N13 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
N13 C44 H44A 109.5 . . ?
N13 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
N13 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
O37 C45 N13 130.9(6) . . ?
O37 C45 H45 114.5 . . ?
N13 C45 H45 114.5 . . ?
O4 N1 O3 123.5(3) . . ?
O4 N1 C3 117.3(3) . . ?
O3 N1 C3 119.2(3) . . ?
O6 N2 O5 122.7(3) . . ?
O6 N2 C5 119.1(3) . . ?
O5 N2 C5 118.2(3) . . ?
O9 N3 O10 124.9(4) . . ?
O9 N3 C10 116.6(3) . . ?
O10 N3 C10 118.5(3) . . ?
O11 N4 O12 125.9(5) . . ?
O11 N4 C12 117.1(6) . . ?
O12 N4 C12 117.0(6) . . ?
O15 N5 O16 124.5(4) . . ?
O15 N5 C17 117.6(3) . . ?
O16 N5 C17 117.9(3) . . ?
O17 N6 O18 124.6(4) . . ?
O17 N6 C19 117.8(4) . . ?
O18 N6 C19 117.7(4) . . ?
O21 N7 O22 120.8(6) . . ?
O21 N7 C24 120.1(4) . . ?
O22 N7 C24 119.0(5) . . ?
O23 N8 O24 126.2(6) . . ?
O23 N8 C26 118.3(10) . . ?
O24 N8 C26 115.5(9) . . ?
O27 N9 O28 125.1(4) . . ?
O27 N9 C31 117.9(3) . . ?
O28 N9 C31 117.0(4) . . ?
O29 N10 O30 124.1(6) . . ?
O29 N10 C33 118.4(7) . . ?
O30 N10 C33 117.6(6) . . ?
O33 N11 O34 124.2(3) . . ?
O33 N11 C38 118.0(3) . . ?
O34 N11 C38 117.7(3) . . ?
O36 N12 O35 123.5(3) . . ?
O36 N12 C40 118.8(3) . . ?
O35 N12 C40 117.8(3) . . ?
C45 N13 C43 118.5(6) . . ?
C45 N13 C44 128.1(6) . . ?
C43 N13 C44 113.2(7) . . ?
C1 O1 La1 141.6(2) . . ?
C1 O2 La2 137.4(2) . . ?
C8 O7 La1 156.4(2) . . ?
C8 O7 La2 87.88(17) . . ?
La1 O7 La2 114.95(8) . . ?
C8 O8 La2 101.23(19) . . ?
C15 O13 La2 151.75(19) . 1_655 ?
C15 O13 La1 90.04(17) . . ?
La2 O13 La1 113.97(7) 1_655 . ?
C15 O14 La1 99.46(18) . . ?
C22 O19 La2 99.88(18) . . ?
C22 O20 La1 155.02(19) . 1_455 ?
C22 O20 La2 89.88(17) . . ?
La1 O20 La2 114.69(7) 1_455 . ?
C29 O25 La1 101.00(18) . . ?
C29 O26 La2 152.33(19) . . ?
C29 O26 La1 87.33(16) . . ?
La2 O26 La1 114.40(8) . . ?
C36 O31 La1 132.2(2) . 1_455 ?
C36 O32 La2 147.3(2) . . ?
C45 O37 La2 120.9(3) . . ?
La1 O1W H11W 116(3) . . ?
La1 O1W H12W 112(3) . . ?
H11W O1W H12W 105(3) . . ?
La1 O2W H21W 114(3) . . ?
La1 O2W H22W 114(3) . . ?
H21W O2W H22W 108(3) . . ?
La2 O3W H31W 119(3) . . ?
La2 O3W H32W 116(3) . . ?
H31W O3W H32W 101(2) . . ?
O20 La1 O7 152.51(7) 1_655 . ?
O20 La1 O1 133.56(7) 1_655 . ?
O7 La1 O1 72.69(7) . . ?
O20 La1 O31 81.07(7) 1_655 1_655 ?
O7 La1 O31 78.61(7) . 1_655 ?
O1 La1 O31 140.26(8) . 1_655 ?
O20 La1 O2W 78.09(7) 1_655 . ?
O7 La1 O2W 77.19(8) . . ?
O1 La1 O2W 128.95(7) . . ?
O31 La1 O2W 67.81(8) 1_655 . ?
O20 La1 O25 73.48(7) 1_655 . ?
O7 La1 O25 111.69(7) . . ?
O1 La1 O25 77.90(8) . . ?
O31 La1 O25 139.45(8) 1_655 . ?
O2W La1 O25 76.28(8) . . ?
O20 La1 O14 112.77(7) 1_655 . ?
O7 La1 O14 80.66(7) . . ?
O1 La1 O14 71.15(7) . . ?
O31 La1 O14 77.63(8) 1_655 . ?
O2W La1 O14 141.82(9) . . ?
O25 La1 O14 141.42(8) . . ?
O20 La1 O1W 69.05(7) 1_655 . ?
O7 La1 O1W 138.08(7) . . ?
O1 La1 O1W 65.50(7) . . ?
O31 La1 O1W 134.65(7) 1_655 . ?
O2W La1 O1W 132.92(8) . . ?
O25 La1 O1W 62.83(7) . . ?
O14 La1 O1W 83.33(8) . . ?
O20 La1 O13 65.14(6) 1_655 . ?
O7 La1 O13 123.66(7) . . ?
O1 La1 O13 103.21(7) . . ?
O31 La1 O13 70.86(7) 1_655 . ?
O2W La1 O13 127.81(7) . . ?
O25 La1 O13 122.45(6) . . ?
O14 La1 O13 47.63(6) . . ?
O1W La1 O13 65.94(7) . . ?
O20 La1 O26 113.56(6) 1_655 . ?
O7 La1 O26 64.73(7) . . ?
O1 La1 O26 66.66(7) . . ?
O31 La1 O26 123.59(7) 1_655 . ?
O2W La1 O26 63.43(7) . . ?
O25 La1 O26 47.05(6) . . ?
O14 La1 O26 131.33(6) . . ?
O1W La1 O26 99.84(7) . . ?
O13 La1 O26 165.53(6) . . ?
O32 La2 O26 139.11(8) . . ?
O32 La2 O13 71.59(8) . 1_455 ?
O26 La2 O13 148.89(7) . 1_455 ?
O32 La2 O2 138.50(8) . . ?
O26 La2 O2 76.84(7) . . ?
O13 La2 O2 77.98(7) 1_455 . ?
O32 La2 O3W 127.66(7) . . ?
O26 La2 O3W 79.20(7) . . ?
O13 La2 O3W 74.22(7) 1_455 . ?
O2 La2 O3W 66.67(8) . . ?
O32 La2 O8 70.82(8) . . ?
O26 La2 O8 112.19(7) . . ?
O13 La2 O8 78.77(7) 1_455 . ?
O2 La2 O8 76.17(8) . . ?
O3W La2 O8 137.56(8) . . ?
O32 La2 O37 68.28(8) . . ?
O26 La2 O37 71.42(8) . . ?
O13 La2 O37 139.68(8) 1_455 . ?
O2 La2 O37 132.94(7) . . ?
O3W La2 O37 136.09(8) . . ?
O8 La2 O37 84.63(8) . . ?
O32 La2 O19 85.06(8) . . ?
O26 La2 O19 74.80(7) . . ?
O13 La2 O19 110.81(7) 1_455 . ?
O2 La2 O19 132.85(8) . . ?
O3W La2 O19 71.55(8) . . ?
O8 La2 O19 150.05(8) . . ?
O37 La2 O19 69.74(8) . . ?
O32 La2 O20 66.70(7) . . ?
O26 La2 O20 116.98(7) . . ?
O13 La2 O20 63.92(6) 1_455 . ?
O2 La2 O20 122.81(7) . . ?
O3W La2 O20 63.03(7) . . ?
O8 La2 O20 130.02(6) . . ?
O37 La2 O20 102.50(7) . . ?
O19 La2 O20 47.10(6) . . ?
O32 La2 O7 105.13(7) . . ?
O26 La2 O7 64.98(7) . . ?
O13 La2 O7 120.04(6) 1_455 . ?
O2 La2 O7 66.99(7) . . ?
O3W La2 O7 126.20(7) . . ?
O8 La2 O7 47.24(6) . . ?
O37 La2 O7 68.43(7) . . ?
O19 La2 O7 128.85(6) . . ?
O20 La2 O7 170.06(6) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 C3 -122.9(3) . . . . ?
O2 C1 C2 C3 60.1(4) . . . . ?
O1 C1 C2 C7 60.2(4) . . . . ?
O2 C1 C2 C7 -116.8(3) . . . . ?
C7 C2 C3 C4 1.9(5) . . . . ?
C1 C2 C3 C4 -175.0(3) . . . . ?
C7 C2 C3 N1 -176.7(3) . . . . ?
C1 C2 C3 N1 6.4(5) . . . . ?
C2 C3 C4 C5 0.1(5) . . . . ?
N1 C3 C4 C5 178.7(3) . . . . ?
C3 C4 C5 C6 -0.9(5) . . . . ?
C3 C4 C5 N2 -179.8(3) . . . . ?
C4 C5 C6 C7 -0.3(6) . . . . ?
N2 C5 C6 C7 178.6(3) . . . . ?
C5 C6 C7 C2 2.4(5) . . . . ?
C3 C2 C7 C6 -3.2(5) . . . . ?
C1 C2 C7 C6 174.0(3) . . . . ?
O8 C8 C9 C10 98.4(4) . . . . ?
O7 C8 C9 C10 -88.9(4) . . . . ?
O8 C8 C9 C14 -81.3(4) . . . . ?
O7 C8 C9 C14 91.3(4) . . . . ?
C14 C9 C10 C11 2.6(5) . . . . ?
C8 C9 C10 C11 -177.2(3) . . . . ?
C14 C9 C10 N3 -179.5(3) . . . . ?
C8 C9 C10 N3 0.7(5) . . . . ?
C9 C10 C11 C12 -0.7(5) . . . . ?
N3 C10 C11 C12 -178.7(3) . . . . ?
C10 C11 C12 C13 -2.3(6) . . . . ?
C10 C11 C12 N4 176.5(4) . . . . ?
C11 C12 C13 C14 3.3(7) . . . . ?
N4 C12 C13 C14 -175.5(4) . . . . ?
C12 C13 C14 C9 -1.2(6) . . . . ?
C10 C9 C14 C13 -1.6(5) . . . . ?
C8 C9 C14 C13 178.2(4) . . . . ?
O14 C15 C16 C21 105.4(4) . . . . ?
O13 C15 C16 C21 -69.0(4) . . . . ?
O14 C15 C16 C17 -71.4(4) . . . . ?
O13 C15 C16 C17 114.3(4) . . . . ?
C21 C16 C17 C18 -2.1(5) . . . . ?
C15 C16 C17 C18 174.7(3) . . . . ?
C21 C16 C17 N5 177.9(3) . . . . ?
C15 C16 C17 N5 -5.3(5) . . . . ?
C16 C17 C18 C19 0.8(5) . . . . ?
N5 C17 C18 C19 -179.2(3) . . . . ?
C17 C18 C19 C20 0.5(5) . . . . ?
C17 C18 C19 N6 -177.6(3) . . . . ?
C18 C19 C20 C21 -0.4(6) . . . . ?
N6 C19 C20 C21 177.7(3) . . . . ?
C19 C20 C21 C16 -0.9(5) . . . . ?
C17 C16 C21 C20 2.1(5) . . . . ?
C15 C16 C21 C20 -174.9(3) . . . . ?
O19 C22 C23 C28 93.8(4) . . . . ?
O20 C22 C23 C28 -81.6(4) . . . . ?
O19 C22 C23 C24 -83.8(5) . . . . ?
O20 C22 C23 C24 100.8(4) . . . . ?
C28 C23 C24 C25 -0.1(7) . . . . ?
C22 C23 C24 C25 177.5(4) . . . . ?
C28 C23 C24 N7 -176.4(5) . . . . ?
C22 C23 C24 N7 1.2(7) . . . . ?
C23 C24 C25 C26 -1.4(9) . . . . ?
N7 C24 C25 C26 175.1(5) . . . . ?
C24 C25 C26 C27 1.3(9) . . . . ?
C24 C25 C26 N8 -179.0(5) . . . . ?
C25 C26 C27 C28 0.4(8) . . . . ?
N8 C26 C27 C28 -179.4(5) . . . . ?
C24 C23 C28 C27 1.7(6) . . . . ?
C22 C23 C28 C27 -176.0(4) . . . . ?
C26 C27 C28 C23 -1.9(7) . . . . ?
O25 C29 C30 C31 -110.9(4) . . . . ?
O26 C29 C30 C31 76.9(4) . . . . ?
O25 C29 C30 C35 74.2(4) . . . . ?
O26 C29 C30 C35 -98.1(3) . . . . ?
C35 C30 C31 C32 0.9(6) . . . . ?
C29 C30 C31 C32 -174.0(4) . . . . ?
C35 C30 C31 N9 -177.4(3) . . . . ?
C29 C30 C31 N9 7.8(6) . . . . ?
C30 C31 C32 C33 0.6(7) . . . . ?
N9 C31 C32 C33 178.9(4) . . . . ?
C31 C32 C33 C34 -1.1(7) . . . . ?
C31 C32 C33 N10 176.9(4) . . . . ?
C32 C33 C34 C35 0.0(7) . . . . ?
N10 C33 C34 C35 -177.9(4) . . . . ?
C33 C34 C35 C30 1.5(6) . . . . ?
C31 C30 C35 C34 -2.0(5) . . . . ?
C29 C30 C35 C34 173.4(3) . . . . ?
O31 C36 C37 C38 -54.0(5) . . . . ?
O32 C36 C37 C38 128.5(3) . . . . ?
O31 C36 C37 C42 126.0(3) . . . . ?
O32 C36 C37 C42 -51.5(4) . . . . ?
C42 C37 C38 C39 -0.1(5) . . . . ?
C36 C37 C38 C39 179.8(3) . . . . ?
C42 C37 C38 N11 176.3(3) . . . . ?
C36 C37 C38 N11 -3.8(5) . . . . ?
C37 C38 C39 C40 0.5(5) . . . . ?
N11 C38 C39 C40 -176.0(3) . . . . ?
C38 C39 C40 C41 -1.1(5) . . . . ?
C38 C39 C40 N12 177.4(3) . . . . ?
C39 C40 C41 C42 1.3(6) . . . . ?
N12 C40 C41 C42 -177.2(3) . . . . ?
C40 C41 C42 C37 -0.9(5) . . . . ?
C38 C37 C42 C41 0.3(5) . . . . ?
C36 C37 C42 C41 -179.7(3) . . . . ?
C4 C3 N1 O4 24.7(5) . . . . ?
C2 C3 N1 O4 -156.6(4) . . . . ?
C4 C3 N1 O3 -154.8(3) . . . . ?
C2 C3 N1 O3 23.8(5) . . . . ?
C6 C5 N2 O6 1.4(5) . . . . ?
C4 C5 N2 O6 -179.7(4) . . . . ?
C6 C5 N2 O5 -177.1(4) . . . . ?
C4 C5 N2 O5 1.8(5) . . . . ?
C9 C10 N3 O9 -25.0(5) . . . . ?
C11 C10 N3 O9 153.0(3) . . . . ?
C9 C10 N3 O10 154.2(3) . . . . ?
C11 C10 N3 O10 -27.8(5) . . . . ?
C11 C12 N4 O11 -20.8(7) . . . . ?
C13 C12 N4 O11 158.0(5) . . . . ?
C11 C12 N4 O12 162.1(5) . . . . ?
C13 C12 N4 O12 -19.1(7) . . . . ?
C18 C17 N5 O15 168.6(3) . . . . ?
C16 C17 N5 O15 -11.4(5) . . . . ?
C18 C17 N5 O16 -11.5(5) . . . . ?
C16 C17 N5 O16 168.5(3) . . . . ?
C18 C19 N6 O17 10.3(6) . . . . ?
C20 C19 N6 O17 -167.9(4) . . . . ?
C18 C19 N6 O18 -169.5(4) . . . . ?
C20 C19 N6 O18 12.3(6) . . . . ?
C23 C24 N7 O21 -19.7(9) . . . . ?
C25 C24 N7 O21 163.8(6) . . . . ?
C23 C24 N7 O22 156.7(8) . . . . ?
C25 C24 N7 O22 -19.8(11) . . . . ?
C27 C26 N8 O23 156.0(6) . . . . ?
C25 C26 N8 O23 -23.8(9) . . . . ?
C27 C26 N8 O24 -23.3(8) . . . . ?
C25 C26 N8 O24 156.9(6) . . . . ?
C30 C31 N9 O27 10.0(6) . . . . ?
C32 C31 N9 O27 -168.4(4) . . . . ?
C30 C31 N9 O28 -167.8(4) . . . . ?
C32 C31 N9 O28 13.8(6) . . . . ?
C34 C33 N10 O29 -179.2(8) . . . . ?
C32 C33 N10 O29 2.8(10) . . . . ?
C34 C33 N10 O30 0.4(8) . . . . ?
C32 C33 N10 O30 -177.6(5) . . . . ?
C39 C38 N11 O33 143.2(4) . . . . ?
C37 C38 N11 O33 -33.5(5) . . . . ?
C39 C38 N11 O34 -35.2(5) . . . . ?
C37 C38 N11 O34 148.2(4) . . . . ?
C39 C40 N12 O36 -174.2(4) . . . . ?
C41 C40 N12 O36 4.4(6) . . . . ?
C39 C40 N12 O35 5.6(6) . . . . ?
C41 C40 N12 O35 -175.8(4) . . . . ?
O37 C45 N13 C43 -2.6(13) . . . . ?
O37 C45 N13 C44 -177.7(8) . . . . ?
O2 C1 O1 La1 37.1(6) . . . . ?
C2 C1 O1 La1 -139.4(3) . . . . ?
O1 C1 O2 La2 -1.6(6) . . . . ?
C2 C1 O2 La2 174.9(2) . . . . ?
O8 C8 O7 La1 -158.3(4) . . . . ?
C9 C8 O7 La1 29.5(7) . . . . ?
O8 C8 O7 La2 7.8(3) . . . . ?
C9 C8 O7 La2 -164.5(3) . . . . ?
O7 C8 O8 La2 -8.7(3) . . . . ?
C9 C8 O8 La2 163.5(2) . . . . ?
O14 C15 O13 La2 153.1(3) . . . 1_655 ?
C16 C15 O13 La2 -32.7(6) . . . 1_655 ?
O14 C15 O13 La1 3.9(3) . . . . ?
C16 C15 O13 La1 178.0(3) . . . . ?
O13 C15 O14 La1 -4.2(4) . . . . ?
C16 C15 O14 La1 -178.3(2) . . . . ?
O20 C22 O19 La2 4.4(4) . . . . ?
C23 C22 O19 La2 -170.8(3) . . . . ?
O19 C22 O20 La1 165.9(3) . . . 1_455 ?
C23 C22 O20 La1 -18.9(7) . . . 1_455 ?
O19 C22 O20 La2 -4.0(3) . . . . ?
C23 C22 O20 La2 171.1(3) . . . . ?
O26 C29 O25 La1 12.0(3) . . . . ?
C30 C29 O25 La1 -159.7(2) . . . . ?
O25 C29 O26 La2 -153.9(3) . . . . ?
C30 C29 O26 La2 17.9(6) . . . . ?
O25 C29 O26 La1 -10.7(3) . . . . ?
C30 C29 O26 La1 161.2(2) . . . . ?
O32 C36 O31 La1 4.5(5) . . . 1_455 ?
C37 C36 O31 La1 -172.72(19) . . . 1_455 ?
O31 C36 O32 La2 -43.6(6) . . . . ?
C37 C36 O32 La2 133.7(3) . . . . ?
N13 C45 O37 La2 141.5(6) . . . . ?

_refine_diff_density_max         1.075
_refine_diff_density_min         -0.739
_refine_diff_density_rms         0.110

####################################################################### 
# 
# 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_Pr_24DNB
_database_code_depnum_ccdc_archive 'CCDC 1584551'
_audit_update_record             
;
2018-02-08 deposited with the CCDC.
2018-02-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H18 N12 O40 Pr2'
_chemical_formula_sum            'C42 H18 N12 O40 Pr2'
_chemical_formula_weight         1612.51

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      monoclinic
_space_group_IT_number           9
_space_group_name_H-M_alt        'C c'
_space_group_name_Hall           'C -2yc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   12.771(3)
_cell_length_b                   47.712(9)
_cell_length_c                   9.221(2)
_cell_angle_alpha                90
_cell_angle_beta                 92.452(11)
_cell_angle_gamma                90
_cell_volume                     5613(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    7108
_cell_measurement_theta_min      2.56
_cell_measurement_theta_max      25.01

_exptl_crystal_description       Prism
_exptl_crystal_colour            'light green'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.908
_exptl_crystal_F_000             3168
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    1.841
_shelx_estimated_absorpt_T_min   0.757
_shelx_estimated_absorpt_T_max   0.809
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.751
_exptl_absorpt_correction_T_max  0.814
_exptl_absorpt_process_details   
'SADABS-2014/2 - Bruker AXS area detector scaling and absorption correction'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            24423
_diffrn_reflns_av_unetI/netI     0.0787
_diffrn_reflns_av_R_equivalents  0.0547
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -54
_diffrn_reflns_limit_k_max       60
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.652
_diffrn_reflns_theta_max         27.259
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.764
_diffrn_reflns_point_group_measured_fraction_full 0.796
_reflns_number_total             9624
_reflns_number_gt                7950
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.543
_reflns_Friedel_fraction_max     0.539
_reflns_Friedel_fraction_full    0.591

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Sir-92 (Altomare et al., 1993)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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.All hydrogen atoms were 
fixed geometrically with their Uiso values 1.2 times of phenylene carbons. 
.we couldn't able to locate hydrogen atoms of water molecules from 
the difference Fourier synthesis 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0268P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2457 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.012(11)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         9624
_refine_ls_number_parameters     865
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0390
_refine_ls_wR_factor_ref         0.0785
_refine_ls_wR_factor_gt          0.0731
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_restrained_S_all      0.974
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6401(7) 0.08464(18) 0.0124(9) 0.030(2) Uani 1 1 d . . . . .
C2 C 0.5843(7) 0.05793(16) 0.0509(9) 0.0243(19) Uani 1 1 d . . . . .
C3 C 0.6173(7) 0.03151(17) 0.0075(10) 0.027(2) Uani 1 1 d . . . . .
C4 C 0.5676(7) 0.00742(18) 0.0462(11) 0.035(2) Uani 1 1 d . . . . .
H4 H 0.591556 -0.009950 0.016089 0.042 Uiso 1 1 calc R U . . .
C5 C 0.4836(8) 0.0093(2) 0.1285(12) 0.043(3) Uani 1 1 d . . . . .
C6 C 0.4460(8) 0.0345(2) 0.1758(11) 0.042(3) Uani 1 1 d . . . . .
H6 H 0.388524 0.035221 0.234252 0.051 Uiso 1 1 calc R U . . .
C7 C 0.4960(7) 0.05907(19) 0.1341(10) 0.035(2) Uani 1 1 d . . . . .
H7 H 0.470040 0.076360 0.162185 0.043 Uiso 1 1 calc R U . . .
C8 C 0.8545(6) 0.09153(16) 0.2755(9) 0.0221(18) Uani 1 1 d . . . . .
C9 C 0.9077(6) 0.06434(16) 0.2463(9) 0.0240(19) Uani 1 1 d . . . . .
C10 C 0.8944(7) 0.04019(17) 0.3289(9) 0.029(2) Uani 1 1 d . . . . .
C11 C 0.9511(8) 0.01604(18) 0.3102(10) 0.037(2) Uani 1 1 d . . . . .
H11 H 0.941655 0.000256 0.367340 0.045 Uiso 1 1 calc R U . . .
C12 C 1.0223(8) 0.01642(19) 0.2029(11) 0.041(2) Uani 1 1 d . . . . .
C13 C 1.0358(7) 0.03915(19) 0.1183(11) 0.043(2) Uani 1 1 d . . . . .
H13 H 1.083561 0.038484 0.045012 0.051 Uiso 1 1 calc R U . . .
C14 C 0.9799(7) 0.06306(17) 0.1395(10) 0.034(2) Uani 1 1 d . . . . .
H14 H 0.990638 0.078639 0.081375 0.040 Uiso 1 1 calc R U . . .
C15 C 0.6395(6) 0.17254(16) 0.2058(9) 0.0244(19) Uani 1 1 d . . . . .
C16 C 0.5820(7) 0.19679(18) 0.2746(10) 0.033(2) Uani 1 1 d . . . . .
C17 C 0.4886(8) 0.1945(2) 0.3428(10) 0.039(2) Uani 1 1 d . . . . .
C18 C 0.4483(9) 0.2159(3) 0.4194(11) 0.056(3) Uani 1 1 d . . . . .
H18 H 0.387202 0.213759 0.469699 0.067 Uiso 1 1 calc R U . . .
C19 C 0.5009(11) 0.2409(3) 0.4197(13) 0.059(4) Uani 1 1 d . . . . .
C20 C 0.5864(10) 0.2447(2) 0.3471(13) 0.057(4) Uani 1 1 d . . . . .
H20 H 0.617633 0.262315 0.344750 0.068 Uiso 1 1 calc R U . . .
C21 C 0.6287(8) 0.22293(19) 0.2760(11) 0.045(3) Uani 1 1 d . . . . .
H21 H 0.690228 0.225593 0.227236 0.054 Uiso 1 1 calc R U . . .
C22 C 0.7670(7) 0.19148(16) -0.2633(11) 0.028(2) Uani 1 1 d . . . . .
C23 C 0.7409(9) 0.22269(14) -0.2548(13) 0.0246(17) Uani 1 1 d . . . . .
C24 C 0.7761(7) 0.24278(17) -0.3468(10) 0.028(2) Uani 1 1 d . . . . .
C25 C 0.7420(7) 0.27047(17) -0.3391(10) 0.036(2) Uani 1 1 d . . . . .
H25 H 0.764715 0.283841 -0.404116 0.043 Uiso 1 1 calc R U . . .
C26 C 0.6754(7) 0.27744(17) -0.2355(10) 0.032(2) Uani 1 1 d . . . . .
C27 C 0.6419(8) 0.25879(17) -0.1380(11) 0.040(2) Uani 1 1 d . . . . .
H27 H 0.597489 0.264266 -0.065855 0.048 Uiso 1 1 calc R U . . .
C28 C 0.6753(8) 0.23107(18) -0.1481(10) 0.037(2) Uani 1 1 d . . . . .
H28 H 0.652907 0.217963 -0.081538 0.045 Uiso 1 1 calc R U . . .
C29 C 0.9408(7) 0.12295(18) -0.2161(10) 0.028(2) Uani 1 1 d . . . . .
C30 C 1.0306(7) 0.11573(18) -0.3107(10) 0.027(2) Uani 1 1 d . . . . .
C31 C 1.1148(7) 0.13310(17) -0.3422(10) 0.031(2) Uani 1 1 d . . . . .
C32 C 1.1939(8) 0.1247(2) -0.4212(11) 0.037(2) Uani 1 1 d . . . . .
H32 H 1.250315 0.136398 -0.437738 0.044 Uiso 1 1 calc R U . . .
C33 C 1.1891(9) 0.0981(3) -0.4772(13) 0.048(3) Uani 1 1 d . . . . .
C34 C 1.1079(8) 0.0798(2) -0.4519(12) 0.047(3) Uani 1 1 d . . . . .
H34 H 1.106974 0.061732 -0.489832 0.056 Uiso 1 1 calc R U . . .
C35 C 1.0285(7) 0.08931(19) -0.3684(11) 0.038(2) Uani 1 1 d . . . . .
H35 H 0.972408 0.077554 -0.350793 0.046 Uiso 1 1 calc R U . . .
C36 C 0.5531(7) 0.13943(16) -0.2943(10) 0.022(2) Uani 1 1 d . . . . .
C37 C 0.4586(7) 0.13063(16) -0.2120(10) 0.027(2) Uani 1 1 d . . . . .
C38 C 0.4078(7) 0.14729(18) -0.1157(10) 0.030(2) Uani 1 1 d . . . . .
C39 C 0.3303(8) 0.1372(2) -0.0338(12) 0.041(3) Uani 1 1 d . . . . .
H39 H 0.296258 0.148425 0.031704 0.050 Uiso 1 1 calc R U . . .
C40 C 0.3052(8) 0.1095(2) -0.0530(14) 0.041(3) Uani 1 1 d . . . . .
C41 C 0.3515(8) 0.0918(2) -0.1468(12) 0.048(3) Uani 1 1 d . . . . .
H41 H 0.329958 0.073309 -0.157369 0.057 Uiso 1 1 calc R U . . .
C42 C 0.4315(8) 0.10262(19) -0.2254(11) 0.037(2) Uani 1 1 d . . . . .
H42 H 0.467417 0.091065 -0.287567 0.044 Uiso 1 1 calc R U . . .
N1 N 0.7097(7) 0.02764(15) -0.0745(9) 0.036(2) Uani 1 1 d . . . . .
N2 N 0.4334(8) -0.0173(2) 0.1760(13) 0.061(3) Uani 1 1 d . . . . .
N3 N 0.8175(8) 0.03951(14) 0.4399(9) 0.041(2) Uani 1 1 d . . . . .
N4 N 1.0858(8) -0.0092(2) 0.1831(12) 0.054(3) Uani 1 1 d . . . . .
N5 N 0.4277(7) 0.1681(2) 0.3282(11) 0.050(2) Uani 1 1 d . . . . .
N6 N 0.4556(12) 0.2643(3) 0.5044(13) 0.084(5) Uani 1 1 d . . . . .
N7 N 0.8519(7) 0.23577(15) -0.4535(10) 0.040(2) Uani 1 1 d . . . . .
N8 N 0.6419(6) 0.30686(17) -0.2263(12) 0.047(2) Uani 1 1 d . . . . .
N9 N 1.1145(7) 0.16244(17) -0.2898(10) 0.044(2) Uani 1 1 d . . . . .
N10 N 1.2757(10) 0.0876(3) -0.5642(12) 0.064(3) Uani 1 1 d . . . . .
N11 N 0.4348(6) 0.17748(17) -0.1049(10) 0.038(2) Uani 1 1 d . . . . .
N12 N 0.2230(11) 0.0976(3) 0.0317(19) 0.093(5) Uani 1 1 d . . . . .
O1 O 0.6146(5) 0.10699(12) 0.0761(6) 0.0311(15) Uani 1 1 d . . . . .
O2 O 0.7093(5) 0.08409(11) -0.0764(6) 0.0304(14) Uani 1 1 d . . . . .
O1W O 0.8972(6) 0.16716(14) 0.1294(7) 0.060(2) Uani 1 1 d . . . . .
O3 O 0.6957(7) 0.02422(17) -0.2050(8) 0.076(3) Uani 1 1 d . . . . .
O2W O 0.6766(5) 0.08590(12) -0.3701(6) 0.0362(15) Uani 1 1 d . . . . .
O4 O 0.7933(6) 0.02704(15) -0.0129(10) 0.064(2) Uani 1 1 d . . . . .
O3W O 0.5972(5) 0.10424(11) -0.6323(6) 0.0330(15) Uani 1 1 d . . . . .
O5 O 0.4555(8) -0.03842(18) 0.1128(13) 0.096(3) Uani 1 1 d . . . . .
O4W O 0.8992(5) 0.15492(13) -0.5597(7) 0.0356(16) Uani 1 1 d . . . . .
O6 O 0.3721(8) -0.0155(2) 0.2721(13) 0.095(4) Uani 1 1 d . . . . .
O7 O 0.8418(5) 0.10862(12) 0.1718(7) 0.0387(17) Uani 1 1 d . . . . .
O8 O 0.8279(5) 0.09586(12) 0.4018(7) 0.0341(15) Uani 1 1 d . . . . .
O9 O 0.7254(6) 0.04293(15) 0.3983(10) 0.061(2) Uani 1 1 d . . . . .
O10 O 0.8465(8) 0.03552(17) 0.5641(9) 0.077(3) Uani 1 1 d . . . . .
O11 O 1.0768(8) -0.02829(16) 0.2687(10) 0.073(3) Uani 1 1 d . . . . .
O12 O 1.1406(7) -0.00981(16) 0.0805(11) 0.082(3) Uani 1 1 d . . . . .
O13 O 0.6403(5) 0.17132(12) 0.0722(6) 0.0358(16) Uani 1 1 d . . . . .
O14 O 0.6892(5) 0.15693(11) 0.2925(6) 0.0340(15) Uani 1 1 d . . . . .
O15 O 0.4606(5) 0.14838(17) 0.2556(8) 0.0513(19) Uani 1 1 d . . . . .
O16 O 0.3441(7) 0.1684(2) 0.3872(13) 0.093(4) Uani 1 1 d . . . . .
O17 O 0.3770(10) 0.2605(3) 0.5670(14) 0.126(6) Uani 1 1 d . . . . .
O18 O 0.5055(10) 0.2861(2) 0.5110(12) 0.114(5) Uani 1 1 d . . . . .
O19 O 0.7972(5) 0.17986(11) -0.1486(7) 0.0307(16) Uani 1 1 d . . . . .
O20 O 0.7529(5) 0.18074(11) -0.3863(7) 0.0359(17) Uani 1 1 d . . . . .
O21 O 0.9256(6) 0.22082(15) -0.4122(9) 0.060(2) Uani 1 1 d . . . . .
O22 O 0.8415(6) 0.24581(16) -0.5751(8) 0.064(2) Uani 1 1 d . . . . .
O23 O 0.5965(7) 0.31389(15) -0.1207(11) 0.074(3) Uani 1 1 d . . . . .
O24 O 0.6612(8) 0.32265(15) -0.3233(11) 0.079(3) Uani 1 1 d . . . . .
O25 O 0.8505(5) 0.12253(12) -0.2690(6) 0.0280(14) Uani 1 1 d . . . . .
O26 O 0.9614(6) 0.12733(15) -0.0828(8) 0.0474(19) Uani 1 1 d . . . . .
O27 O 1.0315(6) 0.17386(15) -0.2747(10) 0.060(2) Uani 1 1 d . . . . .
O28 O 1.1993(6) 0.17413(15) -0.2697(11) 0.075(3) Uani 1 1 d . . . . .
O29 O 1.3546(7) 0.1017(2) -0.5661(12) 0.086(3) Uani 1 1 d . . . . .
O30 O 1.2650(8) 0.0651(2) -0.6254(12) 0.110(4) Uani 1 1 d . . . . .
O31 O 0.6418(5) 0.13861(11) -0.2278(7) 0.0242(14) Uani 1 1 d . . . . .
O32 O 0.5427(5) 0.14375(14) -0.4258(7) 0.0319(15) Uani 1 1 d . . . . .
O33 O 0.4852(6) 0.18778(14) -0.1993(9) 0.053(2) Uani 1 1 d . . . . .
O34 O 0.4037(6) 0.19051(15) -0.0013(9) 0.056(2) Uani 1 1 d . . . . .
O35 O 0.1989(12) 0.0745(3) 0.008(2) 0.215(9) Uani 1 1 d . . . . .
O36 O 0.1844(9) 0.1120(2) 0.1196(13) 0.100(4) Uani 1 1 d . . . . .
Pr1 Pr 0.76618(3) 0.13632(2) -0.01973(4) 0.02217(13) Uani 1 1 d . . . . .
Pr2 Pr 0.73097(3) 0.13290(2) -0.48078(4) 0.02203(13) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O2 1.231(11) . ?
C1 O1 1.266(11) . ?
C1 C2 1.510(12) . ?
C2 C7 1.392(13) . ?
C2 C3 1.393(11) . ?
C3 C4 1.368(12) . ?
C3 N1 1.441(12) . ?
C4 C5 1.343(14) . ?
C4 H4 0.9300 . ?
C5 C6 1.374(14) . ?
C5 N2 1.495(13) . ?
C6 C7 1.396(13) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 O8 1.244(10) . ?
C8 O7 1.261(9) . ?
C8 C9 1.494(11) . ?
C9 C14 1.379(12) . ?
C9 C10 1.395(12) . ?
C10 C11 1.376(12) . ?
C10 N3 1.449(12) . ?
C11 C12 1.372(14) . ?
C11 H11 0.9300 . ?
C12 C13 1.351(14) . ?
C12 N4 1.483(13) . ?
C13 C14 1.364(12) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C15 O13 1.234(10) . ?
C15 O14 1.246(9) . ?
C15 C16 1.523(12) . ?
C16 C17 1.376(14) . ?
C16 C21 1.383(13) . ?
C17 C18 1.359(14) . ?
C17 N5 1.482(13) . ?
C18 C19 1.369(17) . ?
C18 H18 0.9300 . ?
C19 C20 1.317(18) . ?
C19 N6 1.491(14) . ?
C20 C21 1.354(14) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
C22 O19 1.241(10) . ?
C22 O20 1.250(11) . ?
C22 C23 1.529(10) . ?
C23 C24 1.368(14) . ?
C23 C28 1.378(16) . ?
C24 C25 1.394(11) . ?
C24 N7 1.449(13) . ?
C25 C26 1.348(13) . ?
C25 H25 0.9300 . ?
C26 C27 1.347(13) . ?
C26 N8 1.471(11) . ?
C27 C28 1.394(12) . ?
C27 H27 0.9300 . ?
C28 H28 0.9300 . ?
C29 O25 1.233(10) . ?
C29 O26 1.264(11) . ?
C29 C30 1.510(13) . ?
C30 C35 1.368(12) . ?
C30 C31 1.398(13) . ?
C31 C32 1.333(14) . ?
C31 N9 1.481(11) . ?
C32 C33 1.370(15) . ?
C32 H32 0.9300 . ?
C33 C34 1.383(16) . ?
C33 N10 1.479(16) . ?
C34 C35 1.376(14) . ?
C34 H34 0.9300 . ?
C35 H35 0.9300 . ?
C36 O32 1.232(10) . ?
C36 O31 1.265(10) . ?
C36 C37 1.512(14) . ?
C37 C38 1.374(13) . ?
C37 C42 1.384(12) . ?
C38 C39 1.359(14) . ?
C38 N11 1.484(11) . ?
C39 C40 1.367(14) . ?
C39 H39 0.9300 . ?
C40 C41 1.361(16) . ?
C40 N12 1.452(17) . ?
C41 C42 1.378(15) . ?
C41 H41 0.9300 . ?
C42 H42 0.9300 . ?
N1 O4 1.188(10) . ?
N1 O3 1.220(10) . ?
N2 O5 1.203(14) . ?
N2 O6 1.210(15) . ?
N3 O10 1.204(11) . ?
N3 O9 1.232(11) . ?
N4 O12 1.201(13) . ?
N4 O11 1.213(12) . ?
N5 O16 1.219(13) . ?
N5 O15 1.238(11) . ?
N6 O17 1.194(19) . ?
N6 O18 1.219(17) . ?
N7 O22 1.221(10) . ?
N7 O21 1.228(10) . ?
N8 O23 1.202(12) . ?
N8 O24 1.203(12) . ?
N9 O27 1.205(10) . ?
N9 O28 1.225(10) . ?
N10 O29 1.211(14) . ?
N10 O30 1.219(14) . ?
N11 O33 1.209(11) . ?
N11 O34 1.220(10) . ?
N12 O35 1.163(14) . ?
N12 O36 1.188(16) . ?
O1 Pr1 2.575(6) . ?
O2 Pr1 2.642(5) . ?
O1W Pr1 2.581(6) . ?
O2W Pr2 2.571(6) . ?
O3W Pr2 2.557(5) . ?
O4W Pr2 2.526(6) . ?
O7 Pr1 2.378(6) . ?
O8 Pr2 2.438(6) 1_556 ?
O13 Pr1 2.492(6) . ?
O14 Pr2 2.424(6) 1_556 ?
O19 Pr1 2.435(6) . ?
O20 Pr2 2.455(5) . ?
O25 Pr2 2.477(6) . ?
O25 Pr1 2.662(6) . ?
O26 Pr1 2.620(8) . ?
O31 Pr1 2.441(6) . ?
O31 Pr2 2.653(6) . ?
O32 Pr2 2.532(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 C1 O1 122.2(8) . . ?
O2 C1 C2 119.9(8) . . ?
O1 C1 C2 117.9(9) . . ?
C7 C2 C3 117.1(8) . . ?
C7 C2 C1 119.9(8) . . ?
C3 C2 C1 123.0(8) . . ?
C4 C3 C2 122.4(9) . . ?
C4 C3 N1 115.4(8) . . ?
C2 C3 N1 122.1(8) . . ?
C5 C4 C3 118.9(9) . . ?
C5 C4 H4 120.6 . . ?
C3 C4 H4 120.6 . . ?
C4 C5 C6 122.4(9) . . ?
C4 C5 N2 118.2(10) . . ?
C6 C5 N2 119.4(11) . . ?
C5 C6 C7 118.6(10) . . ?
C5 C6 H6 120.7 . . ?
C7 C6 H6 120.7 . . ?
C2 C7 C6 120.6(9) . . ?
C2 C7 H7 119.7 . . ?
C6 C7 H7 119.7 . . ?
O8 C8 O7 124.8(8) . . ?
O8 C8 C9 117.2(7) . . ?
O7 C8 C9 118.0(8) . . ?
C14 C9 C10 117.0(8) . . ?
C14 C9 C8 119.3(8) . . ?
C10 C9 C8 123.5(8) . . ?
C11 C10 C9 123.1(9) . . ?
C11 C10 N3 116.5(8) . . ?
C9 C10 N3 120.4(8) . . ?
C12 C11 C10 116.6(9) . . ?
C12 C11 H11 121.7 . . ?
C10 C11 H11 121.7 . . ?
C13 C12 C11 122.1(9) . . ?
C13 C12 N4 120.5(10) . . ?
C11 C12 N4 117.4(9) . . ?
C12 C13 C14 120.5(10) . . ?
C12 C13 H13 119.7 . . ?
C14 C13 H13 119.7 . . ?
C13 C14 C9 120.6(9) . . ?
C13 C14 H14 119.7 . . ?
C9 C14 H14 119.7 . . ?
O13 C15 O14 125.9(8) . . ?
O13 C15 C16 118.4(7) . . ?
O14 C15 C16 115.4(8) . . ?
C17 C16 C21 116.8(9) . . ?
C17 C16 C15 124.9(9) . . ?
C21 C16 C15 118.2(9) . . ?
C18 C17 C16 122.2(11) . . ?
C18 C17 N5 118.6(11) . . ?
C16 C17 N5 119.2(9) . . ?
C17 C18 C19 117.4(12) . . ?
C17 C18 H18 121.3 . . ?
C19 C18 H18 121.3 . . ?
C20 C19 C18 122.4(11) . . ?
C20 C19 N6 120.8(14) . . ?
C18 C19 N6 116.7(14) . . ?
C19 C20 C21 119.9(12) . . ?
C19 C20 H20 120.1 . . ?
C21 C20 H20 120.1 . . ?
C20 C21 C16 121.0(12) . . ?
C20 C21 H21 119.5 . . ?
C16 C21 H21 119.5 . . ?
O19 C22 O20 128.1(7) . . ?
O19 C22 C23 116.8(8) . . ?
O20 C22 C23 115.0(8) . . ?
C24 C23 C28 117.7(8) . . ?
C24 C23 C22 124.9(10) . . ?
C28 C23 C22 117.4(9) . . ?
C23 C24 C25 121.4(9) . . ?
C23 C24 N7 120.4(8) . . ?
C25 C24 N7 118.2(8) . . ?
C26 C25 C24 118.5(9) . . ?
C26 C25 H25 120.7 . . ?
C24 C25 H25 120.7 . . ?
C27 C26 C25 122.5(8) . . ?
C27 C26 N8 119.4(9) . . ?
C25 C26 N8 118.1(9) . . ?
C26 C27 C28 118.4(10) . . ?
C26 C27 H27 120.8 . . ?
C28 C27 H27 120.8 . . ?
C23 C28 C27 121.3(9) . . ?
C23 C28 H28 119.3 . . ?
C27 C28 H28 119.3 . . ?
O25 C29 O26 122.7(9) . . ?
O25 C29 C30 119.2(8) . . ?
O26 C29 C30 117.9(8) . . ?
C35 C30 C31 117.9(9) . . ?
C35 C30 C29 115.6(8) . . ?
C31 C30 C29 126.5(8) . . ?
C32 C31 C30 122.8(9) . . ?
C32 C31 N9 118.5(9) . . ?
C30 C31 N9 118.7(9) . . ?
C31 C32 C33 117.6(10) . . ?
C31 C32 H32 121.2 . . ?
C33 C32 H32 121.2 . . ?
C32 C33 C34 122.8(11) . . ?
C32 C33 N10 119.6(12) . . ?
C34 C33 N10 117.5(11) . . ?
C35 C34 C33 117.5(10) . . ?
C35 C34 H34 121.2 . . ?
C33 C34 H34 121.2 . . ?
C30 C35 C34 121.3(9) . . ?
C30 C35 H35 119.4 . . ?
C34 C35 H35 119.4 . . ?
O32 C36 O31 122.6(9) . . ?
O32 C36 C37 119.1(8) . . ?
O31 C36 C37 117.8(8) . . ?
C38 C37 C42 119.6(9) . . ?
C38 C37 C36 124.9(7) . . ?
C42 C37 C36 115.1(8) . . ?
C39 C38 C37 121.9(8) . . ?
C39 C38 N11 118.7(9) . . ?
C37 C38 N11 119.4(8) . . ?
C38 C39 C40 116.3(10) . . ?
C38 C39 H39 121.9 . . ?
C40 C39 H39 121.9 . . ?
C41 C40 C39 125.1(11) . . ?
C41 C40 N12 116.2(11) . . ?
C39 C40 N12 118.7(11) . . ?
C40 C41 C42 117.1(10) . . ?
C40 C41 H41 121.5 . . ?
C42 C41 H41 121.5 . . ?
C41 C42 C37 120.0(10) . . ?
C41 C42 H42 120.0 . . ?
C37 C42 H42 120.0 . . ?
O4 N1 O3 124.0(10) . . ?
O4 N1 C3 119.5(8) . . ?
O3 N1 C3 116.5(9) . . ?
O5 N2 O6 125.9(11) . . ?
O5 N2 C5 117.2(12) . . ?
O6 N2 C5 116.9(11) . . ?
O10 N3 O9 124.6(10) . . ?
O10 N3 C10 119.0(10) . . ?
O9 N3 C10 116.4(9) . . ?
O12 N4 O11 124.7(10) . . ?
O12 N4 C12 117.1(10) . . ?
O11 N4 C12 118.1(11) . . ?
O16 N5 O15 125.1(10) . . ?
O16 N5 C17 114.5(10) . . ?
O15 N5 C17 120.4(9) . . ?
O17 N6 O18 123.6(13) . . ?
O17 N6 C19 119.6(16) . . ?
O18 N6 C19 116.7(15) . . ?
O22 N7 O21 124.4(10) . . ?
O22 N7 C24 118.9(8) . . ?
O21 N7 C24 116.7(8) . . ?
O23 N8 O24 123.3(9) . . ?
O23 N8 C26 117.7(9) . . ?
O24 N8 C26 119.0(10) . . ?
O27 N9 O28 123.6(9) . . ?
O27 N9 C31 118.7(8) . . ?
O28 N9 C31 117.7(9) . . ?
O29 N10 O30 123.9(12) . . ?
O29 N10 C33 117.6(12) . . ?
O30 N10 C33 118.5(12) . . ?
O33 N11 O34 123.9(9) . . ?
O33 N11 C38 118.4(8) . . ?
O34 N11 C38 117.7(9) . . ?
O35 N12 O36 124.4(15) . . ?
O35 N12 C40 117.6(14) . . ?
O36 N12 C40 118.0(12) . . ?
C1 O1 Pr1 95.0(6) . . ?
C1 O2 Pr1 92.7(5) . . ?
C8 O7 Pr1 163.2(6) . . ?
C8 O8 Pr2 134.4(5) . 1_556 ?
C15 O13 Pr1 113.9(5) . . ?
C15 O14 Pr2 157.4(6) . 1_556 ?
C22 O19 Pr1 138.3(5) . . ?
C22 O20 Pr2 135.5(5) . . ?
C29 O25 Pr2 147.5(6) . . ?
C29 O25 Pr1 93.5(5) . . ?
Pr2 O25 Pr1 111.9(2) . . ?
C29 O26 Pr1 94.7(6) . . ?
C36 O31 Pr1 157.1(6) . . ?
C36 O31 Pr2 89.2(5) . . ?
Pr1 O31 Pr2 113.4(2) . . ?
C36 O32 Pr2 95.7(5) . . ?
O7 Pr1 O19 140.1(2) . . ?
O7 Pr1 O31 147.03(19) . . ?
O19 Pr1 O31 72.06(19) . . ?
O7 Pr1 O13 111.5(2) . . ?
O19 Pr1 O13 73.5(2) . . ?
O31 Pr1 O13 80.19(19) . . ?
O7 Pr1 O1 74.3(2) . . ?
O19 Pr1 O1 140.5(2) . . ?
O31 Pr1 O1 79.7(2) . . ?
O13 Pr1 O1 75.0(2) . . ?
O7 Pr1 O1W 71.8(2) . . ?
O19 Pr1 O1W 70.0(2) . . ?
O31 Pr1 O1W 141.15(19) . . ?
O13 Pr1 O1W 81.4(2) . . ?
O1 Pr1 O1W 127.3(2) . . ?
O7 Pr1 O26 73.4(2) . . ?
O19 Pr1 O26 81.7(2) . . ?
O31 Pr1 O26 115.2(2) . . ?
O13 Pr1 O26 145.0(2) . . ?
O1 Pr1 O26 136.4(2) . . ?
O1W Pr1 O26 67.0(2) . . ?
O7 Pr1 O2 73.87(18) . . ?
O19 Pr1 O2 139.25(18) . . ?
O31 Pr1 O2 73.88(17) . . ?
O13 Pr1 O2 121.6(2) . . ?
O1 Pr1 O2 49.53(18) . . ?
O1W Pr1 O2 144.1(2) . . ?
O26 Pr1 O2 93.3(2) . . ?
O7 Pr1 O25 109.7(2) . . ?
O19 Pr1 O25 73.08(19) . . ?
O31 Pr1 O25 66.80(18) . . ?
O13 Pr1 O25 138.60(18) . . ?
O1 Pr1 O25 119.99(18) . . ?
O1W Pr1 O25 108.9(2) . . ?
O26 Pr1 O25 49.00(19) . . ?
O2 Pr1 O25 73.38(18) . . ?
O14 Pr2 O8 93.3(2) 1_554 1_554 ?
O14 Pr2 O20 83.33(19) 1_554 . ?
O8 Pr2 O20 141.2(2) 1_554 . ?
O14 Pr2 O25 151.7(2) 1_554 . ?
O8 Pr2 O25 84.1(2) 1_554 . ?
O20 Pr2 O25 81.3(2) . . ?
O14 Pr2 O4W 73.3(2) 1_554 . ?
O8 Pr2 O4W 73.7(2) 1_554 . ?
O20 Pr2 O4W 68.3(2) . . ?
O25 Pr2 O4W 78.89(19) . . ?
O14 Pr2 O32 84.3(2) 1_554 . ?
O8 Pr2 O32 137.9(2) 1_554 . ?
O20 Pr2 O32 80.4(2) . . ?
O25 Pr2 O32 116.2(2) . . ?
O4W Pr2 O32 143.0(2) . . ?
O14 Pr2 O3W 70.39(19) 1_554 . ?
O8 Pr2 O3W 73.1(2) 1_554 . ?
O20 Pr2 O3W 139.0(2) . . ?
O25 Pr2 O3W 134.35(19) . . ?
O4W Pr2 O3W 128.4(2) . . ?
O32 Pr2 O3W 66.5(2) . . ?
O14 Pr2 O2W 134.58(18) 1_554 . ?
O8 Pr2 O2W 72.3(2) 1_554 . ?
O20 Pr2 O2W 134.3(2) . . ?
O25 Pr2 O2W 71.37(19) . . ?
O4W Pr2 O2W 136.4(2) . . ?
O32 Pr2 O2W 79.9(2) . . ?
O3W Pr2 O2W 64.23(18) . . ?
O14 Pr2 O31 128.52(19) 1_554 . ?
O8 Pr2 O31 135.26(19) 1_554 . ?
O20 Pr2 O31 68.8(2) . . ?
O25 Pr2 O31 66.46(18) . . ?
O4W Pr2 O31 127.79(18) . . ?
O32 Pr2 O31 49.90(18) . . ?
O3W Pr2 O31 103.51(19) . . ?
O2W Pr2 O31 66.87(18) . . ?

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
O2 C1 C2 C7 -170.4(7) . . . . ?
O1 C1 C2 C7 11.0(11) . . . . ?
O2 C1 C2 C3 9.9(12) . . . . ?
O1 C1 C2 C3 -168.7(7) . . . . ?
C7 C2 C3 C4 -1.4(12) . . . . ?
C1 C2 C3 C4 178.3(8) . . . . ?
C7 C2 C3 N1 -177.8(8) . . . . ?
C1 C2 C3 N1 1.9(12) . . . . ?
C2 C3 C4 C5 0.4(13) . . . . ?
N1 C3 C4 C5 177.0(9) . . . . ?
C3 C4 C5 C6 -0.3(15) . . . . ?
C3 C4 C5 N2 -177.0(8) . . . . ?
C4 C5 C6 C7 1.3(15) . . . . ?
N2 C5 C6 C7 177.9(8) . . . . ?
C3 C2 C7 C6 2.4(12) . . . . ?
C1 C2 C7 C6 -177.4(8) . . . . ?
C5 C6 C7 C2 -2.3(14) . . . . ?
O8 C8 C9 C14 -149.7(8) . . . . ?
O7 C8 C9 C14 28.9(11) . . . . ?
O8 C8 C9 C10 25.3(12) . . . . ?
O7 C8 C9 C10 -156.1(8) . . . . ?
C14 C9 C10 C11 1.5(12) . . . . ?
C8 C9 C10 C11 -173.6(8) . . . . ?
C14 C9 C10 N3 -177.9(8) . . . . ?
C8 C9 C10 N3 7.0(12) . . . . ?
C9 C10 C11 C12 -0.9(13) . . . . ?
N3 C10 C11 C12 178.5(8) . . . . ?
C10 C11 C12 C13 -0.7(14) . . . . ?
C10 C11 C12 N4 178.7(8) . . . . ?
C11 C12 C13 C14 1.6(15) . . . . ?
N4 C12 C13 C14 -177.8(8) . . . . ?
C12 C13 C14 C9 -0.9(14) . . . . ?
C10 C9 C14 C13 -0.6(12) . . . . ?
C8 C9 C14 C13 174.7(8) . . . . ?
O13 C15 C16 C17 108.1(11) . . . . ?
O14 C15 C16 C17 -77.7(10) . . . . ?
O13 C15 C16 C21 -75.4(10) . . . . ?
O14 C15 C16 C21 98.8(10) . . . . ?
C21 C16 C17 C18 -5.8(13) . . . . ?
C15 C16 C17 C18 170.7(8) . . . . ?
C21 C16 C17 N5 171.9(7) . . . . ?
C15 C16 C17 N5 -11.6(13) . . . . ?
C16 C17 C18 C19 3.8(14) . . . . ?
N5 C17 C18 C19 -173.9(8) . . . . ?
C17 C18 C19 C20 1.3(17) . . . . ?
C17 C18 C19 N6 -180.0(9) . . . . ?
C18 C19 C20 C21 -4.1(18) . . . . ?
N6 C19 C20 C21 177.2(10) . . . . ?
C19 C20 C21 C16 1.9(16) . . . . ?
C17 C16 C21 C20 2.9(14) . . . . ?
C15 C16 C21 C20 -173.8(9) . . . . ?
O19 C22 C23 C24 131.5(10) . . . . ?
O20 C22 C23 C24 -49.9(13) . . . . ?
O19 C22 C23 C28 -49.9(13) . . . . ?
O20 C22 C23 C28 128.6(10) . . . . ?
C28 C23 C24 C25 -3.8(15) . . . . ?
C22 C23 C24 C25 174.8(8) . . . . ?
C28 C23 C24 N7 174.9(9) . . . . ?
C22 C23 C24 N7 -6.5(15) . . . . ?
C23 C24 C25 C26 2.0(13) . . . . ?
N7 C24 C25 C26 -176.8(8) . . . . ?
C24 C25 C26 C27 1.0(14) . . . . ?
C24 C25 C26 N8 178.6(8) . . . . ?
C25 C26 C27 C28 -1.9(15) . . . . ?
N8 C26 C27 C28 -179.5(8) . . . . ?
C24 C23 C28 C27 2.8(16) . . . . ?
C22 C23 C28 C27 -175.8(8) . . . . ?
C26 C27 C28 C23 -0.1(15) . . . . ?
O25 C29 C30 C35 -61.0(11) . . . . ?
O26 C29 C30 C35 114.3(9) . . . . ?
O25 C29 C30 C31 120.1(9) . . . . ?
O26 C29 C30 C31 -64.6(13) . . . . ?
C35 C30 C31 C32 -2.3(14) . . . . ?
C29 C30 C31 C32 176.6(9) . . . . ?
C35 C30 C31 N9 175.6(8) . . . . ?
C29 C30 C31 N9 -5.5(13) . . . . ?
C30 C31 C32 C33 2.3(15) . . . . ?
N9 C31 C32 C33 -175.5(9) . . . . ?
C31 C32 C33 C34 -1.7(17) . . . . ?
C31 C32 C33 N10 -179.3(9) . . . . ?
C32 C33 C34 C35 1.0(16) . . . . ?
N10 C33 C34 C35 178.7(9) . . . . ?
C31 C30 C35 C34 1.5(14) . . . . ?
C29 C30 C35 C34 -177.5(9) . . . . ?
C33 C34 C35 C30 -0.9(15) . . . . ?
O32 C36 C37 C38 -108.5(10) . . . . ?
O31 C36 C37 C38 80.2(11) . . . . ?
O32 C36 C37 C42 79.2(10) . . . . ?
O31 C36 C37 C42 -92.2(9) . . . . ?
C42 C37 C38 C39 -0.8(13) . . . . ?
C36 C37 C38 C39 -172.9(9) . . . . ?
C42 C37 C38 N11 -178.2(7) . . . . ?
C36 C37 C38 N11 9.8(13) . . . . ?
C37 C38 C39 C40 -0.4(14) . . . . ?
N11 C38 C39 C40 177.0(8) . . . . ?
C38 C39 C40 C41 -0.1(16) . . . . ?
C38 C39 C40 N12 180.0(11) . . . . ?
C39 C40 C41 C42 1.7(17) . . . . ?
N12 C40 C41 C42 -178.3(11) . . . . ?
C40 C41 C42 C37 -2.9(15) . . . . ?
C38 C37 C42 C41 2.5(13) . . . . ?
C36 C37 C42 C41 175.3(8) . . . . ?
C4 C3 N1 O4 -94.5(10) . . . . ?
C2 C3 N1 O4 82.2(11) . . . . ?
C4 C3 N1 O3 83.1(10) . . . . ?
C2 C3 N1 O3 -100.2(10) . . . . ?
C4 C5 N2 O5 -16.2(15) . . . . ?
C6 C5 N2 O5 167.1(11) . . . . ?
C4 C5 N2 O6 165.7(11) . . . . ?
C6 C5 N2 O6 -11.0(15) . . . . ?
C11 C10 N3 O10 61.7(11) . . . . ?
C9 C10 N3 O10 -118.9(9) . . . . ?
C11 C10 N3 O9 -117.8(9) . . . . ?
C9 C10 N3 O9 61.6(11) . . . . ?
C13 C12 N4 O12 -7.6(15) . . . . ?
C11 C12 N4 O12 173.0(10) . . . . ?
C13 C12 N4 O11 174.4(10) . . . . ?
C11 C12 N4 O11 -5.0(14) . . . . ?
C18 C17 N5 O16 0.7(13) . . . . ?
C16 C17 N5 O16 -177.0(9) . . . . ?
C18 C17 N5 O15 177.9(8) . . . . ?
C16 C17 N5 O15 0.1(13) . . . . ?
C20 C19 N6 O17 178.6(11) . . . . ?
C18 C19 N6 O17 0(2) . . . . ?
C20 C19 N6 O18 -5.0(19) . . . . ?
C18 C19 N6 O18 176.2(9) . . . . ?
C23 C24 N7 O22 139.5(9) . . . . ?
C25 C24 N7 O22 -41.8(12) . . . . ?
C23 C24 N7 O21 -43.5(12) . . . . ?
C25 C24 N7 O21 135.3(8) . . . . ?
C27 C26 N8 O23 9.3(14) . . . . ?
C25 C26 N8 O23 -168.4(9) . . . . ?
C27 C26 N8 O24 -170.9(10) . . . . ?
C25 C26 N8 O24 11.3(14) . . . . ?
C32 C31 N9 O27 149.1(10) . . . . ?
C30 C31 N9 O27 -28.8(14) . . . . ?
C32 C31 N9 O28 -28.0(14) . . . . ?
C30 C31 N9 O28 154.0(9) . . . . ?
C32 C33 N10 O29 10.0(17) . . . . ?
C34 C33 N10 O29 -167.8(11) . . . . ?
C32 C33 N10 O30 -172.6(12) . . . . ?
C34 C33 N10 O30 9.7(17) . . . . ?
C39 C38 N11 O33 -163.3(9) . . . . ?
C37 C38 N11 O33 14.1(12) . . . . ?
C39 C38 N11 O34 16.0(12) . . . . ?
C37 C38 N11 O34 -166.5(8) . . . . ?
C41 C40 N12 O35 -4(3) . . . . ?
C39 C40 N12 O35 175.8(17) . . . . ?
C41 C40 N12 O36 176.5(14) . . . . ?
C39 C40 N12 O36 -4(2) . . . . ?
O2 C1 O1 Pr1 -8.2(8) . . . . ?
C2 C1 O1 Pr1 170.4(6) . . . . ?
O1 C1 O2 Pr1 7.9(8) . . . . ?
C2 C1 O2 Pr1 -170.6(6) . . . . ?
O8 C8 O7 Pr1 -75(2) . . . . ?
C9 C8 O7 Pr1 106(2) . . . . ?
O7 C8 O8 Pr2 6.4(13) . . . 1_556 ?
C9 C8 O8 Pr2 -175.2(5) . . . 1_556 ?
O14 C15 O13 Pr1 -5.2(11) . . . . ?
C16 C15 O13 Pr1 168.4(6) . . . . ?
O13 C15 O14 Pr2 -157.0(10) . . . 1_556 ?
C16 C15 O14 Pr2 29.3(18) . . . 1_556 ?
O20 C22 O19 Pr1 -42.1(15) . . . . ?
C23 C22 O19 Pr1 136.2(8) . . . . ?
O19 C22 O20 Pr2 17.4(15) . . . . ?
C23 C22 O20 Pr2 -161.0(7) . . . . ?
O26 C29 O25 Pr2 145.9(8) . . . . ?
C30 C29 O25 Pr2 -39.1(15) . . . . ?
O26 C29 O25 Pr1 3.7(9) . . . . ?
C30 C29 O25 Pr1 178.7(7) . . . . ?
O25 C29 O26 Pr1 -3.7(9) . . . . ?
C30 C29 O26 Pr1 -178.8(7) . . . . ?
O32 C36 O31 Pr1 172.1(8) . . . . ?
C37 C36 O31 Pr1 -16.8(17) . . . . ?
O32 C36 O31 Pr2 -16.3(8) . . . . ?
C37 C36 O31 Pr2 154.8(6) . . . . ?
O31 C36 O32 Pr2 17.1(8) . . . . ?
C37 C36 O32 Pr2 -153.8(6) . . . . ?

_refine_diff_density_max         1.235
_refine_diff_density_min         -1.041
_refine_diff_density_rms         0.116

####################################################################### 
# 
# 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_Eu_35DNb
_database_code_depnum_ccdc_archive 'CCDC 1584545'
_audit_update_record             
;
2018-02-08 deposited with the CCDC.
2018-02-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C21 H13 Eu N6 O20, H2 O'
_chemical_formula_sum            'C21 H15 Eu N6 O21'
_chemical_formula_weight         839.35

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'
Eu Eu -0.1578 3.6682 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.2090(17)
_cell_length_b                   11.329(2)
_cell_length_c                   13.664(3)
_cell_angle_alpha                106.024(8)
_cell_angle_beta                 90.136(9)
_cell_angle_gamma                94.491(9)
_cell_volume                     1365.5(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4010
_cell_measurement_theta_min      2.22
_cell_measurement_theta_max      27.16

_exptl_crystal_description       Rectangular
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.041
_exptl_crystal_F_000             828
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    2.409
_shelx_estimated_absorpt_T_min   0.699
_shelx_estimated_absorpt_T_max   0.795
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.692
_exptl_absorpt_correction_T_max  0.799
_exptl_absorpt_process_details   
'SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            28187
_diffrn_reflns_av_unetI/netI     0.1742
_diffrn_reflns_av_R_equivalents  0.1450
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.551
_diffrn_reflns_theta_max         31.810
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measured_fraction_theta_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             8849
_reflns_number_gt                5676
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Sir-92 (Altomare et al., 1993)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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.
All hydrogen atoms were fixed geometrically with their Uiso values 1.2 
times of phenylene carbons. The hydrogen atoms of water molecules were
 located from the difference Fourier synthesis and were refined 
isotropically with distance of 0.82 Å with Uiso values 1.2 times that 
of their carrier oxygen atoms.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1327P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8849
_refine_ls_number_parameters     460
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.1269
_refine_ls_R_factor_gt           0.0685
_refine_ls_wR_factor_ref         0.2518
_refine_ls_wR_factor_gt          0.1649
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_restrained_S_all      1.084
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.9515(9) 0.7641(8) 0.9534(7) 0.0141(16) Uani 1 1 d . . . . .
C2 C 1.0054(10) 0.6366(9) 0.9173(7) 0.0166(17) Uani 1 1 d . . . . .
C3 C 0.9063(10) 0.5351(9) 0.8813(7) 0.0182(18) Uani 1 1 d . . . . .
H3 H 0.804996 0.545752 0.880651 0.022 Uiso 1 1 calc R U . . .
C4 C 0.9535(10) 0.4196(9) 0.8465(7) 0.0179(18) Uani 1 1 d . . . . .
C5 C 1.0997(10) 0.3982(9) 0.8478(7) 0.0171(17) Uani 1 1 d . . . . .
H5 H 1.131066 0.317575 0.823372 0.021 Uiso 1 1 calc R U . . .
C6 C 1.1982(10) 0.5003(9) 0.8865(7) 0.0178(18) Uani 1 1 d . . . . .
C7 C 1.1532(10) 0.6187(9) 0.9195(6) 0.0167(17) Uani 1 1 d . . . . .
H7 H 1.222857 0.687174 0.943576 0.020 Uiso 1 1 calc R U . . .
C8 C 0.4603(8) 0.8345(9) 0.8506(7) 0.0139(16) Uani 1 1 d . . . . .
C9 C 0.4935(10) 0.7222(9) 0.7677(7) 0.0182(18) Uani 1 1 d . . . . .
C10 C 0.3812(10) 0.6377(9) 0.7187(6) 0.0164(17) Uani 1 1 d . . . . .
H10 H 0.282203 0.653345 0.731460 0.020 Uiso 1 1 calc R U . . .
C11 C 0.4182(10) 0.5302(9) 0.6509(7) 0.0182(18) Uani 1 1 d . . . . .
C12 C 0.5586(10) 0.5034(9) 0.6252(7) 0.0173(18) Uani 1 1 d . . . . .
H12 H 0.580143 0.428253 0.578030 0.021 Uiso 1 1 calc R U . . .
C13 C 0.6648(9) 0.5920(9) 0.6720(7) 0.0169(18) Uani 1 1 d . . . . .
C14 C 0.6416(10) 0.6987(9) 0.7442(7) 0.0165(17) Uani 1 1 d . . . . .
H14 H 0.720310 0.754880 0.777330 0.020 Uiso 1 1 calc R U . . .
C15 C 1.0270(10) 1.0328(8) 1.2030(6) 0.0152(17) Uani 1 1 d . . . . .
C16 C 1.0174(10) 1.0799(8) 1.3171(7) 0.0164(17) Uani 1 1 d . . . . .
C17 C 1.1371(10) 1.0812(9) 1.3796(7) 0.0179(18) Uani 1 1 d . . . . .
H17 H 1.226936 1.053744 1.351678 0.021 Uiso 1 1 calc R U . . .
C18 C 1.1212(11) 1.1242(9) 1.4853(7) 0.0195(18) Uani 1 1 d . . . . .
C19 C 0.9922(10) 1.1686(9) 1.5277(7) 0.0177(18) Uani 1 1 d . . . . .
H19 H 0.983548 1.199203 1.599307 0.021 Uiso 1 1 calc R U . . .
C20 C 0.8770(10) 1.1666(8) 1.4619(7) 0.0168(17) Uani 1 1 d . . . . .
C21 C 0.8857(10) 1.1218(9) 1.3573(7) 0.0183(18) Uani 1 1 d . . . . .
H21 H 0.804130 1.119518 1.313979 0.022 Uiso 1 1 calc R U . . .
N1 N 1.3547(9) 0.4823(8) 0.8917(7) 0.0224(18) Uani 1 1 d . . . . .
N2 N 0.8475(9) 0.3137(8) 0.8114(6) 0.0208(17) Uani 1 1 d . . . . .
N3 N 0.2989(9) 0.4365(8) 0.6042(6) 0.0198(16) Uani 1 1 d . . . . .
N4 N 0.8188(9) 0.5687(8) 0.6428(7) 0.0241(18) Uani 1 1 d . . . . .
N5 N 0.7371(9) 1.2091(8) 1.5031(6) 0.0212(17) Uani 1 1 d . . . . .
N6 N 1.2408(9) 1.1206(8) 1.5543(6) 0.0206(16) Uani 1 1 d . . . . .
O1 O 0.8174(6) 0.7680(6) 0.9667(5) 0.0175(13) Uani 1 1 d . . . . .
O2 O 1.0400(8) 0.8557(6) 0.9670(5) 0.0226(15) Uani 1 1 d . . . . .
O3 O 1.3907(8) 0.3775(7) 0.8562(7) 0.0330(19) Uani 1 1 d . . . . .
O4 O 1.4381(7) 0.5727(7) 0.9288(6) 0.0257(16) Uani 1 1 d . . . . .
O5 O 0.7191(7) 0.3334(7) 0.8118(6) 0.0240(15) Uani 1 1 d . . . . .
O6 O 0.8900(8) 0.2096(6) 0.7841(6) 0.0240(15) Uani 1 1 d . . . . .
O7 O 0.6665(7) 1.1362(6) 1.1446(5) 0.0186(13) Uani 1 1 d . . . . .
O8 O 0.5635(7) 0.8893(6) 0.9113(5) 0.0202(14) Uani 1 1 d . . . . .
O9 O 0.1753(8) 0.4478(7) 0.6408(6) 0.0293(17) Uani 1 1 d . . . . .
O10 O 0.3263(7) 0.3535(7) 0.5297(5) 0.0255(16) Uani 1 1 d . . . . .
O11 O 0.8398(9) 0.4774(8) 0.5736(7) 0.042(2) Uani 1 1 d . . . . .
O12 O 0.9141(8) 0.6443(7) 0.6907(6) 0.0284(17) Uani 1 1 d . . . . .
O13 O 0.9063(7) 0.9855(7) 1.1563(5) 0.0188(13) Uani 1 1 d . . . . .
O14 O 0.8530(7) 0.9544(6) 0.8372(5) 0.0190(13) Uani 1 1 d . . . . .
O15 O 0.6414(8) 1.2200(8) 1.4448(6) 0.0347(19) Uani 1 1 d . . . . .
O16 O 0.7244(9) 1.2332(8) 1.5966(6) 0.0340(19) Uani 1 1 d . . . . .
O17 O 1.2284(9) 1.1712(8) 1.6462(5) 0.0310(18) Uani 1 1 d . . . . .
O18 O 1.3466(8) 1.0672(7) 1.5187(5) 0.0279(17) Uani 1 1 d . . . . .
O1W O 0.6795(7) 1.1364(7) 0.9331(5) 0.0213(15) Uani 1 1 d D . . . .
H11W H 0.681(11) 1.130(11) 0.871(2) 0.026 Uiso 1 1 d D U . . .
H12W H 0.604(7) 1.170(10) 0.949(7) 0.026 Uiso 1 1 d D U . . .
O2W O 0.6154(7) 0.8686(7) 1.1116(5) 0.0195(13) Uani 1 1 d D . . . .
H21W H 0.631(12) 0.901(8) 1.173(2) 0.023 Uiso 1 1 d D U . . .
H22W H 0.633(12) 0.797(3) 1.106(7) 0.023 Uiso 1 1 d D U . . .
O3W O 0.5299(10) 0.0719(13) 0.7104(7) 0.054(3) Uani 1 1 d D . . . .
H31W H 0.601(11) 0.111(11) 0.697(11) 0.065 Uiso 1 1 d D U . . .
H32W H 0.526(16) 0.006(7) 0.666(10) 0.065 Uiso 1 1 d D U . . .
Eu1 Eu 0.77143(5) 0.98451(4) 1.01074(3) 0.01308(14) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O2 1.240(11) . ?
C1 O1 1.251(9) . ?
C1 C2 1.516(12) . ?
C2 C3 1.385(14) . ?
C2 C7 1.393(13) . ?
C3 C4 1.369(13) . ?
C3 H3 0.9500 . ?
C4 C5 1.387(12) . ?
C4 N2 1.456(13) . ?
C5 C6 1.391(14) . ?
C5 H5 0.9500 . ?
C6 C7 1.388(13) . ?
C6 N1 1.476(11) . ?
C7 H7 0.9500 . ?
C8 O7 1.235(10) 2_677 ?
C8 O8 1.264(11) . ?
C8 C9 1.504(13) . ?
C9 C10 1.386(14) . ?
C9 C14 1.431(13) . ?
C10 C11 1.379(13) . ?
C10 H10 0.9500 . ?
C11 C12 1.376(13) . ?
C11 N3 1.477(12) . ?
C12 C13 1.365(14) . ?
C12 H12 0.9500 . ?
C13 C14 1.365(13) . ?
C13 N4 1.498(11) . ?
C14 H14 0.9500 . ?
C15 O14 1.251(11) 2_777 ?
C15 O13 1.283(11) . ?
C15 C16 1.506(12) . ?
C16 C17 1.390(13) . ?
C16 C21 1.396(12) . ?
C17 C18 1.403(13) . ?
C17 H17 0.9500 . ?
C18 C19 1.391(12) . ?
C18 N6 1.458(13) . ?
C19 C20 1.384(13) . ?
C19 H19 0.9500 . ?
C20 C21 1.383(12) . ?
C20 N5 1.469(11) . ?
C21 H21 0.9500 . ?
N1 O4 1.218(11) . ?
N1 O3 1.224(11) . ?
N2 O5 1.221(10) . ?
N2 O6 1.229(10) . ?
N3 O10 1.221(10) . ?
N3 O9 1.246(10) . ?
N4 O11 1.222(11) . ?
N4 O12 1.226(11) . ?
N5 O15 1.222(11) . ?
N5 O16 1.238(10) . ?
N6 O18 1.218(10) . ?
N6 O17 1.238(10) . ?
O1 Eu1 2.431(6) . ?
O2 Eu1 2.364(7) 2_777 ?
O2 Eu1 2.949(7) . ?
O7 Eu1 2.402(6) . ?
O8 Eu1 2.352(7) . ?
O13 Eu1 2.339(6) . ?
O14 Eu1 2.430(6) . ?
O1W Eu1 2.456(7) . ?
O1W H11W 0.83(2) . ?
O1W H12W 0.82(2) . ?
O2W Eu1 2.530(7) . ?
O2W H21W 0.82(2) . ?
O2W H22W 0.83(2) . ?
O3W H31W 0.81(2) . ?
O3W H32W 0.82(2) . ?
Eu1 Eu1 4.2146(11) 2_777 ?

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 C1 O1 124.8(8) . . ?
O2 C1 C2 119.2(8) . . ?
O1 C1 C2 116.0(8) . . ?
C3 C2 C7 118.9(8) . . ?
C3 C2 C1 119.7(8) . . ?
C7 C2 C1 121.4(9) . . ?
C4 C3 C2 120.3(9) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C3 C4 C5 122.4(9) . . ?
C3 C4 N2 119.6(8) . . ?
C5 C4 N2 118.0(8) . . ?
C4 C5 C6 116.9(8) . . ?
C4 C5 H5 121.6 . . ?
C6 C5 H5 121.6 . . ?
C7 C6 C5 121.7(8) . . ?
C7 C6 N1 119.2(9) . . ?
C5 C6 N1 119.1(8) . . ?
C6 C7 C2 119.7(9) . . ?
C6 C7 H7 120.1 . . ?
C2 C7 H7 120.1 . . ?
O7 C8 O8 125.4(9) 2_677 . ?
O7 C8 C9 117.3(8) 2_677 . ?
O8 C8 C9 117.3(7) . . ?
C10 C9 C14 120.0(8) . . ?
C10 C9 C8 120.0(8) . . ?
C14 C9 C8 119.8(8) . . ?
C11 C10 C9 117.8(9) . . ?
C11 C10 H10 121.1 . . ?
C9 C10 H10 121.1 . . ?
C12 C11 C10 124.5(9) . . ?
C12 C11 N3 117.8(8) . . ?
C10 C11 N3 117.7(8) . . ?
C13 C12 C11 115.4(8) . . ?
C13 C12 H12 122.3 . . ?
C11 C12 H12 122.3 . . ?
C14 C13 C12 125.1(8) . . ?
C14 C13 N4 117.8(8) . . ?
C12 C13 N4 117.1(8) . . ?
C13 C14 C9 117.0(9) . . ?
C13 C14 H14 121.5 . . ?
C9 C14 H14 121.5 . . ?
O14 C15 O13 126.3(8) 2_777 . ?
O14 C15 C16 118.8(8) 2_777 . ?
O13 C15 C16 114.8(8) . . ?
C17 C16 C21 121.5(8) . . ?
C17 C16 C15 120.4(8) . . ?
C21 C16 C15 118.1(8) . . ?
C16 C17 C18 117.9(8) . . ?
C16 C17 H17 121.0 . . ?
C18 C17 H17 121.0 . . ?
C19 C18 C17 121.9(9) . . ?
C19 C18 N6 118.0(8) . . ?
C17 C18 N6 120.0(8) . . ?
C20 C19 C18 117.8(8) . . ?
C20 C19 H19 121.1 . . ?
C18 C19 H19 121.1 . . ?
C21 C20 C19 122.5(8) . . ?
C21 C20 N5 117.6(8) . . ?
C19 C20 N5 119.8(8) . . ?
C20 C21 C16 118.3(9) . . ?
C20 C21 H21 120.8 . . ?
C16 C21 H21 120.8 . . ?
O4 N1 O3 125.1(9) . . ?
O4 N1 C6 117.8(8) . . ?
O3 N1 C6 117.1(9) . . ?
O5 N2 O6 123.2(9) . . ?
O5 N2 C4 117.5(8) . . ?
O6 N2 C4 119.4(8) . . ?
O10 N3 O9 123.4(8) . . ?
O10 N3 C11 117.9(8) . . ?
O9 N3 C11 118.6(8) . . ?
O11 N4 O12 125.3(8) . . ?
O11 N4 C13 118.2(9) . . ?
O12 N4 C13 116.6(8) . . ?
O15 N5 O16 123.8(8) . . ?
O15 N5 C20 119.2(8) . . ?
O16 N5 C20 116.9(8) . . ?
O18 N6 O17 123.6(8) . . ?
O18 N6 C18 118.4(8) . . ?
O17 N6 C18 118.0(8) . . ?
C1 O1 Eu1 106.2(6) . . ?
C1 O2 Eu1 173.9(6) . 2_777 ?
C1 O2 Eu1 81.7(5) . . ?
Eu1 O2 Eu1 104.5(2) 2_777 . ?
C8 O7 Eu1 127.5(6) 2_677 . ?
C8 O8 Eu1 174.3(6) . . ?
C15 O13 Eu1 140.1(6) . . ?
C15 O14 Eu1 135.2(6) 2_777 . ?
Eu1 O1W H11W 124(7) . . ?
Eu1 O1W H12W 124(7) . . ?
H11W O1W H12W 102(3) . . ?
Eu1 O2W H21W 109(8) . . ?
Eu1 O2W H22W 116(8) . . ?
H21W O2W H22W 102(3) . . ?
H31W O3W H32W 104(3) . . ?
O13 Eu1 O8 142.7(2) . . ?
O13 Eu1 O2 73.2(2) . 2_777 ?
O8 Eu1 O2 144.0(2) . 2_777 ?
O13 Eu1 O7 76.2(2) . . ?
O8 Eu1 O7 101.4(2) . . ?
O2 Eu1 O7 81.6(2) 2_777 . ?
O13 Eu1 O14 128.7(2) . . ?
O8 Eu1 O14 76.6(2) . . ?
O2 Eu1 O14 78.7(2) 2_777 . ?
O7 Eu1 O14 140.3(2) . . ?
O13 Eu1 O1 81.0(2) . . ?
O8 Eu1 O1 77.7(2) . . ?
O2 Eu1 O1 122.7(2) 2_777 . ?
O7 Eu1 O1 139.6(2) . . ?
O14 Eu1 O1 79.5(2) . . ?
O13 Eu1 O1W 137.6(2) . . ?
O8 Eu1 O1W 72.7(2) . . ?
O2 Eu1 O1W 74.0(2) 2_777 . ?
O7 Eu1 O1W 73.1(2) . . ?
O14 Eu1 O1W 68.5(2) . . ?
O1 Eu1 O1W 140.3(2) . . ?
O13 Eu1 O2W 72.4(2) . . ?
O8 Eu1 O2W 71.4(2) . . ?
O2 Eu1 O2W 141.1(2) 2_777 . ?
O7 Eu1 O2W 73.1(2) . . ?
O14 Eu1 O2W 138.4(2) . . ?
O1 Eu1 O2W 68.4(2) . . ?
O1W Eu1 O2W 123.6(2) . . ?
O13 Eu1 O2 66.1(2) . . ?
O8 Eu1 O2 116.3(2) . . ?
O2 Eu1 O2 75.5(2) 2_777 . ?
O7 Eu1 O2 140.0(2) . . ?
O14 Eu1 O2 65.9(2) . . ?
O1 Eu1 O2 47.22(19) . . ?
O1W Eu1 O2 128.80(19) . . ?
O2W Eu1 O2 105.9(2) . . ?
O13 Eu1 C1 72.9(2) . . ?
O8 Eu1 C1 96.6(2) . . ?
O2 Eu1 C1 99.4(2) 2_777 . ?
O7 Eu1 C1 147.2(2) . . ?
O14 Eu1 C1 70.6(2) . . ?
O1 Eu1 C1 23.4(2) . . ?
O1W Eu1 C1 139.0(2) . . ?
O2W Eu1 C1 87.3(2) . . ?
O2 Eu1 C1 23.9(2) . . ?
O13 Eu1 Eu1 63.49(16) . 2_777 ?
O8 Eu1 Eu1 139.84(15) . 2_777 ?
O2 Eu1 Eu1 42.65(17) 2_777 2_777 ?
O7 Eu1 Eu1 117.03(16) . 2_777 ?
O14 Eu1 Eu1 66.66(16) . 2_777 ?
O1 Eu1 Eu1 80.10(14) . 2_777 ?
O1W Eu1 Eu1 106.50(16) . 2_777 ?
O2W Eu1 Eu1 128.91(15) . 2_777 ?
O2 Eu1 Eu1 32.89(14) . 2_777 ?
C1 Eu1 Eu1 56.78(18) . 2_777 ?

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
O2 C1 C2 C3 -166.3(8) . . . . ?
O1 C1 C2 C3 13.2(12) . . . . ?
Eu1 C1 C2 C3 -1(3) . . . . ?
O2 C1 C2 C7 13.9(13) . . . . ?
O1 C1 C2 C7 -166.7(8) . . . . ?
Eu1 C1 C2 C7 179(2) . . . . ?
C7 C2 C3 C4 -1.4(13) . . . . ?
C1 C2 C3 C4 178.8(8) . . . . ?
C2 C3 C4 C5 1.5(14) . . . . ?
C2 C3 C4 N2 178.4(8) . . . . ?
C3 C4 C5 C6 0.1(14) . . . . ?
N2 C4 C5 C6 -176.8(8) . . . . ?
C4 C5 C6 C7 -1.9(13) . . . . ?
C4 C5 C6 N1 178.7(8) . . . . ?
C5 C6 C7 C2 2.1(13) . . . . ?
N1 C6 C7 C2 -178.6(8) . . . . ?
C3 C2 C7 C6 -0.4(13) . . . . ?
C1 C2 C7 C6 179.4(8) . . . . ?
O7 C8 C9 C10 -17.6(13) 2_677 . . . ?
O8 C8 C9 C10 160.7(9) . . . . ?
O7 C8 C9 C14 166.5(8) 2_677 . . . ?
O8 C8 C9 C14 -15.2(13) . . . . ?
C14 C9 C10 C11 2.5(13) . . . . ?
C8 C9 C10 C11 -173.4(8) . . . . ?
C9 C10 C11 C12 -2.9(14) . . . . ?
C9 C10 C11 N3 175.8(8) . . . . ?
C10 C11 C12 C13 0.0(14) . . . . ?
N3 C11 C12 C13 -178.7(8) . . . . ?
C11 C12 C13 C14 3.6(14) . . . . ?
C11 C12 C13 N4 -177.5(8) . . . . ?
C12 C13 C14 C9 -4.0(14) . . . . ?
N4 C13 C14 C9 177.1(8) . . . . ?
C10 C9 C14 C13 0.7(13) . . . . ?
C8 C9 C14 C13 176.6(8) . . . . ?
O14 C15 C16 C17 -31.0(13) 2_777 . . . ?
O13 C15 C16 C17 151.0(9) . . . . ?
O14 C15 C16 C21 149.0(9) 2_777 . . . ?
O13 C15 C16 C21 -29.0(12) . . . . ?
C21 C16 C17 C18 1.0(14) . . . . ?
C15 C16 C17 C18 -179.0(9) . . . . ?
C16 C17 C18 C19 -2.2(14) . . . . ?
C16 C17 C18 N6 176.4(9) . . . . ?
C17 C18 C19 C20 1.4(15) . . . . ?
N6 C18 C19 C20 -177.2(9) . . . . ?
C18 C19 C20 C21 0.5(15) . . . . ?
C18 C19 C20 N5 178.2(9) . . . . ?
C19 C20 C21 C16 -1.6(14) . . . . ?
N5 C20 C21 C16 -179.4(8) . . . . ?
C17 C16 C21 C20 0.8(14) . . . . ?
C15 C16 C21 C20 -179.2(8) . . . . ?
C7 C6 N1 O4 2.9(13) . . . . ?
C5 C6 N1 O4 -177.7(9) . . . . ?
C7 C6 N1 O3 -175.8(9) . . . . ?
C5 C6 N1 O3 3.6(13) . . . . ?
C3 C4 N2 O5 2.1(13) . . . . ?
C5 C4 N2 O5 179.1(8) . . . . ?
C3 C4 N2 O6 -177.1(9) . . . . ?
C5 C4 N2 O6 -0.1(13) . . . . ?
C12 C11 N3 O10 -15.9(13) . . . . ?
C10 C11 N3 O10 165.3(9) . . . . ?
C12 C11 N3 O9 166.0(9) . . . . ?
C10 C11 N3 O9 -12.8(13) . . . . ?
C14 C13 N4 O11 -175.3(9) . . . . ?
C12 C13 N4 O11 5.7(13) . . . . ?
C14 C13 N4 O12 4.3(13) . . . . ?
C12 C13 N4 O12 -174.7(9) . . . . ?
C21 C20 N5 O15 -10.2(14) . . . . ?
C19 C20 N5 O15 172.0(10) . . . . ?
C21 C20 N5 O16 170.4(9) . . . . ?
C19 C20 N5 O16 -7.4(14) . . . . ?
C19 C18 N6 O18 170.4(9) . . . . ?
C17 C18 N6 O18 -8.3(14) . . . . ?
C19 C18 N6 O17 -8.8(14) . . . . ?
C17 C18 N6 O17 172.5(9) . . . . ?
O2 C1 O1 Eu1 3.8(11) . . . . ?
C2 C1 O1 Eu1 -175.6(6) . . . . ?
O1 C1 O2 Eu1 -3.1(9) . . . . ?
C2 C1 O2 Eu1 176.3(8) . . . . ?
O14 C15 O13 Eu1 -40.7(15) 2_777 . . . ?
C16 C15 O13 Eu1 137.2(7) . . . . ?

_refine_diff_density_max         4.489
_refine_diff_density_min         -6.413
_refine_diff_density_rms         0.444

# start Validation Reply Form
_vrf_PLAT971_shelxl              
;
RESPONSE: This Alert is due to the presence of
heavy metal atoms.
;
_vrf_PLAT972_shelxl              
;
RESPONSE: This Alert is due to the presence of
heavy metal atoms.
;
_vrf_PLAT973_shelxl              
;
RESPONSE: This Alert is due to the presence of
heavy metal atoms.
;
_vrf_PLAT975_shelxl              
;
RESPONSE: This Alert is due to the presence of
heavy metal atoms.
;
_vrf_PLAT976_shelxl              
;
RESPONSE: This Alert is due to the presence of
heavy metal atoms.
;
_vrf_PLAT029_shelxl              
;
RESPONSE: This Alert is due to the presence of
heavy metal atoms.
;
_vrf_PLAT098_shelxl              
;
RESPONSE: This Alert is due to the presence of
heavy metal atoms.
;
_vrf_PLAT924_shelxl              
;
RESPONSE: This Alert may be due to the
presence of electron density around heavy 
metal atom
in the difference fourier.
;
_vrf_PLAT925_shelxl              
;
RESPONSE: This Alert may be due to the
 presence of
electron density around heavy metal atom
in the difference fourier.
;
# end Validation Reply Form

