# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2020

####################################################################### 
# 
# 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_435-11Cd
_database_code_depnum_ccdc_archive 'CCDC 2012741'
_audit_update_record             
;
2020-06-28 deposited with the CCDC.	2021-01-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C25 H24 Cd N2 O10'
_chemical_formula_weight         624.86

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'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      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                   8.5006(7)
_cell_length_b                   11.4499(9)
_cell_length_c                   13.9188(10)
_cell_angle_alpha                72.721(7)
_cell_angle_beta                 79.726(7)
_cell_angle_gamma                78.478(7)
_cell_volume                     1257.22(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7747
_cell_measurement_theta_min      3.555
_cell_measurement_theta_max      25.050

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.651
_exptl_crystal_F_000             632
_exptl_transmission_factor_min   0.807
_exptl_transmission_factor_max   0.846
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    0.930
_shelx_estimated_absorpt_T_min   0.815
_shelx_estimated_absorpt_T_max   0.850
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.815
_exptl_absorpt_correction_T_max  0.850
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APE-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7747
_diffrn_reflns_av_unetI/netI     0.0951
_diffrn_reflns_av_R_equivalents  0.0483
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.555
_diffrn_reflns_theta_max         25.050
_diffrn_reflns_theta_full        25.050
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             4438
_reflns_number_gt                3348
_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    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0190P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4438
_refine_ls_number_parameters     344
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0748
_refine_ls_R_factor_gt           0.0518
_refine_ls_wR_factor_ref         0.0981
_refine_ls_wR_factor_gt          0.0826
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.000
_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
Cd1 Cd -0.30581(5) 0.76798(3) 0.17263(3) 0.03543(15) Uani 1 1 d . . . . .
N1 N -0.2839(5) 0.9550(4) 0.0538(3) 0.0362(11) Uani 1 1 d . . . . .
N2 N -0.5125(5) 0.9169(4) 0.2158(3) 0.0370(11) Uani 1 1 d . . . . .
O1 O -0.0615(4) 0.6589(3) 0.2257(3) 0.0444(10) Uani 1 1 d . . . . .
O2 O -0.1707(4) 0.7959(3) 0.3085(3) 0.0431(10) Uani 1 1 d . . . . .
O3 O 0.5171(5) 0.5592(3) 0.1393(3) 0.0523(11) Uani 1 1 d . . . . .
O4 O 0.5608(4) 0.6198(3) 0.2683(3) 0.0427(10) Uani 1 1 d . . . . .
O5 O 0.8187(5) 0.1071(3) 0.2274(3) 0.0512(11) Uani 1 1 d . . . . .
O6 O 0.7373(6) -0.0122(3) 0.3799(3) 0.0594(13) Uani 1 1 d . . . . .
H6 H 0.7864 -0.0683 0.3557 0.089 Uiso 1 1 calc R U . . .
O7 O -0.2266(5) 0.6834(3) 0.0389(3) 0.0570(12) Uani 1 1 d . . . . .
H1W H -0.1313 0.6819 0.0073 0.068 Uiso 1 1 d R U . . .
H2W H -0.2455 0.6329 0.0099 0.068 Uiso 1 1 d R U . . .
O8 O 0.9125(5) 0.3243(4) 0.0637(3) 0.0677(13) Uani 1 1 d . . . . .
H3W H 0.8854 0.2618 0.1102 0.081 Uiso 1 1 d R U . . .
H4W H 0.9281 0.3521 0.1044 0.081 Uiso 1 1 d R U . . .
O9 O 0.0306(5) 0.4132(4) 0.2045(3) 0.0693(13) Uani 1 1 d . . . . .
H5W H 0.0023 0.4861 0.2112 0.083 Uiso 1 1 d R U . . .
H6W H 0.1099 0.4359 0.1608 0.083 Uiso 1 1 d R U . . .
O10 O 0.2893(6) 0.4878(4) 0.0620(3) 0.0798(15) Uani 1 1 d . . . . .
H7W H 0.3602 0.5093 0.0865 0.096 Uiso 1 1 d R U . . .
H8W H 0.2287 0.5436 0.0236 0.096 Uiso 1 1 d R U . . .
C1 C -0.0648(6) 0.7065(5) 0.2975(4) 0.0326(13) Uani 1 1 d . . . . .
C2 C 0.0574(6) 0.6524(4) 0.3700(4) 0.0269(11) Uani 1 1 d . . . . .
C3 C 0.1829(6) 0.5614(4) 0.3494(3) 0.0278(12) Uani 1 1 d . . . . .
H3 H 0.1949 0.5422 0.2879 0.033 Uiso 1 1 calc R U . . .
C4 C 0.2911(6) 0.4981(4) 0.4190(4) 0.0276(12) Uani 1 1 d . . . . .
C5 C 0.2715(6) 0.5291(5) 0.5104(4) 0.0344(13) Uani 1 1 d . . . . .
H5 H 0.3403 0.4868 0.5588 0.041 Uiso 1 1 calc R U . . .
C6 C 0.1486(7) 0.6237(5) 0.5294(4) 0.0425(14) Uani 1 1 d . . . . .
H6A H 0.1382 0.6459 0.5896 0.051 Uiso 1 1 calc R U . . .
C7 C 0.0431(6) 0.6842(5) 0.4597(4) 0.0385(14) Uani 1 1 d . . . . .
H7 H -0.0384 0.7469 0.4731 0.046 Uiso 1 1 calc R U . . .
C8 C 0.4170(6) 0.3970(4) 0.3950(4) 0.0270(12) Uani 1 1 d . . . . .
C9 C 0.5164(6) 0.4147(4) 0.3022(4) 0.0262(11) Uani 1 1 d . . . . .
C10 C 0.5283(6) 0.5420(5) 0.2299(4) 0.0340(13) Uani 1 1 d . . . . .
C11 C 0.6178(6) 0.3161(4) 0.2770(4) 0.0329(13) Uani 1 1 d . . . . .
H11 H 0.6799 0.3287 0.2137 0.040 Uiso 1 1 calc R U . . .
C12 C 0.6302(6) 0.1977(4) 0.3434(4) 0.0307(12) Uani 1 1 d . . . . .
C13 C 0.7393(7) 0.0953(5) 0.3094(4) 0.0403(14) Uani 1 1 d . . . . .
C14 C 0.5367(6) 0.1819(4) 0.4376(4) 0.0357(13) Uani 1 1 d . . . . .
H14 H 0.5459 0.1045 0.4846 0.043 Uiso 1 1 calc R U . . .
C15 C 0.4310(6) 0.2791(4) 0.4621(4) 0.0332(13) Uani 1 1 d . . . . .
H15 H 0.3673 0.2659 0.5249 0.040 Uiso 1 1 calc R U . . .
C16 C -0.1731(7) 0.9677(5) -0.0277(4) 0.0418(14) Uani 1 1 d . . . . .
H16 H -0.1047 0.8974 -0.0388 0.050 Uiso 1 1 calc R U . . .
C17 C -0.1557(7) 1.0801(5) -0.0960(4) 0.0483(16) Uani 1 1 d . . . . .
H17 H -0.0768 1.0860 -0.1522 0.058 Uiso 1 1 calc R U . . .
C18 C -0.2560(8) 1.1825(5) -0.0799(4) 0.0529(17) Uani 1 1 d . . . . .
H18 H -0.2454 1.2599 -0.1245 0.063 Uiso 1 1 calc R U . . .
C19 C -0.3740(7) 1.1711(5) 0.0033(4) 0.0472(16) Uani 1 1 d . . . . .
H19 H -0.4454 1.2402 0.0143 0.057 Uiso 1 1 calc R U . . .
C20 C -0.3841(6) 1.0548(5) 0.0701(4) 0.0333(13) Uani 1 1 d . . . . .
C21 C -0.5108(6) 1.0353(4) 0.1607(4) 0.0356(13) Uani 1 1 d . . . . .
C22 C -0.6212(8) 1.1304(5) 0.1868(4) 0.0509(16) Uani 1 1 d . . . . .
H22 H -0.6185 1.2118 0.1481 0.061 Uiso 1 1 calc R U . . .
C23 C -0.7351(8) 1.1043(6) 0.2702(5) 0.065(2) Uani 1 1 d . . . . .
H23 H -0.8100 1.1677 0.2886 0.078 Uiso 1 1 calc R U . . .
C24 C -0.7372(8) 0.9848(6) 0.3255(5) 0.0596(18) Uani 1 1 d . . . . .
H24 H -0.8137 0.9652 0.3822 0.071 Uiso 1 1 calc R U . . .
C25 C -0.6248(7) 0.8930(5) 0.2966(4) 0.0513(16) Uani 1 1 d . . . . .
H25 H -0.6268 0.8113 0.3347 0.062 Uiso 1 1 calc R U . . .


_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
Cd1 O4 2.197(3) 1_455 ?
Cd1 O7 2.284(4) . ?
Cd1 N1 2.303(4) . ?
Cd1 O1 2.320(4) . ?
Cd1 N2 2.322(4) . ?
Cd1 O2 2.505(4) . ?
N1 C16 1.330(6) . ?
N1 C20 1.333(6) . ?
N2 C25 1.338(6) . ?
N2 C21 1.346(6) . ?
O1 C1 1.267(6) . ?
O2 C1 1.248(6) . ?
O3 C10 1.236(6) . ?
O4 C10 1.260(6) . ?
O4 Cd1 2.197(3) 1_655 ?
O5 C13 1.203(6) . ?
O6 C13 1.328(6) . ?
O6 H6 0.8200 . ?
O7 H1W 0.8500 . ?
O7 H2W 0.8499 . ?
O8 H3W 0.8499 . ?
O8 H4W 0.7698 . ?
O9 H5W 0.8500 . ?
O9 H6W 0.8500 . ?
O10 H7W 0.8500 . ?
O10 H8W 0.8500 . ?
C1 C2 1.492(7) . ?
C2 C7 1.380(7) . ?
C2 C3 1.389(6) . ?
C3 C4 1.393(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.394(7) . ?
C4 C8 1.484(6) . ?
C5 C6 1.398(7) . ?
C5 H5 0.9300 . ?
C6 C7 1.374(7) . ?
C6 H6A 0.9300 . ?
C7 H7 0.9300 . ?
C8 C15 1.391(6) . ?
C8 C9 1.395(6) . ?
C9 C11 1.371(6) . ?
C9 C10 1.517(6) . ?
C11 C12 1.393(6) . ?
C11 H11 0.9300 . ?
C12 C14 1.389(7) . ?
C12 C13 1.482(7) . ?
C14 C15 1.371(7) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C17 1.372(6) . ?
C16 H16 0.9300 . ?
C17 C18 1.356(8) . ?
C17 H17 0.9300 . ?
C18 C19 1.383(7) . ?
C18 H18 0.9300 . ?
C19 C20 1.388(6) . ?
C19 H19 0.9300 . ?
C20 C21 1.498(7) . ?
C21 C22 1.380(7) . ?
C22 C23 1.372(8) . ?
C22 H22 0.9300 . ?
C23 C24 1.359(8) . ?
C23 H23 0.9300 . ?
C24 C25 1.376(8) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?

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
O4 Cd1 O7 95.92(13) 1_455 . ?
O4 Cd1 N1 153.74(15) 1_455 . ?
O7 Cd1 N1 85.49(15) . . ?
O4 Cd1 O1 92.19(13) 1_455 . ?
O7 Cd1 O1 84.14(14) . . ?
N1 Cd1 O1 114.00(14) . . ?
O4 Cd1 N2 90.65(14) 1_455 . ?
O7 Cd1 N2 136.43(15) . . ?
N1 Cd1 N2 71.17(15) . . ?
O1 Cd1 N2 138.71(14) . . ?
O4 Cd1 O2 97.55(13) 1_455 . ?
O7 Cd1 O2 135.89(13) . . ?
N1 Cd1 O2 99.54(13) . . ?
O1 Cd1 O2 53.60(12) . . ?
N2 Cd1 O2 85.20(13) . . ?
C16 N1 C20 119.3(4) . . ?
C16 N1 Cd1 122.8(4) . . ?
C20 N1 Cd1 117.8(3) . . ?
C25 N2 C21 118.5(5) . . ?
C25 N2 Cd1 123.7(4) . . ?
C21 N2 Cd1 117.6(3) . . ?
C1 O1 Cd1 96.8(3) . . ?
C1 O2 Cd1 88.6(3) . . ?
C10 O4 Cd1 119.6(3) . 1_655 ?
C13 O6 H6 109.5 . . ?
Cd1 O7 H1W 122.4 . . ?
Cd1 O7 H2W 145.3 . . ?
H1W O7 H2W 90.2 . . ?
H3W O8 H4W 89.2 . . ?
H5W O9 H6W 90.7 . . ?
H7W O10 H8W 118.7 . . ?
O2 C1 O1 120.4(5) . . ?
O2 C1 C2 120.5(5) . . ?
O1 C1 C2 119.1(5) . . ?
C7 C2 C3 119.2(5) . . ?
C7 C2 C1 121.9(5) . . ?
C3 C2 C1 118.7(5) . . ?
C2 C3 C4 121.5(5) . . ?
C2 C3 H3 119.2 . . ?
C4 C3 H3 119.2 . . ?
C3 C4 C5 118.2(5) . . ?
C3 C4 C8 119.0(4) . . ?
C5 C4 C8 122.7(5) . . ?
C4 C5 C6 120.1(5) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C7 C6 C5 120.4(5) . . ?
C7 C6 H6A 119.8 . . ?
C5 C6 H6A 119.8 . . ?
C6 C7 C2 120.4(5) . . ?
C6 C7 H7 119.8 . . ?
C2 C7 H7 119.8 . . ?
C15 C8 C9 118.1(5) . . ?
C15 C8 C4 120.5(4) . . ?
C9 C8 C4 121.3(4) . . ?
C11 C9 C8 120.1(4) . . ?
C11 C9 C10 117.3(4) . . ?
C8 C9 C10 122.4(4) . . ?
O3 C10 O4 125.6(5) . . ?
O3 C10 C9 119.1(5) . . ?
O4 C10 C9 115.1(5) . . ?
C9 C11 C12 121.8(5) . . ?
C9 C11 H11 119.1 . . ?
C12 C11 H11 119.1 . . ?
C14 C12 C11 117.8(5) . . ?
C14 C12 C13 123.7(4) . . ?
C11 C12 C13 118.5(5) . . ?
O5 C13 O6 123.6(5) . . ?
O5 C13 C12 124.5(5) . . ?
O6 C13 C12 111.9(5) . . ?
C15 C14 C12 120.7(4) . . ?
C15 C14 H14 119.6 . . ?
C12 C14 H14 119.6 . . ?
C14 C15 C8 121.4(5) . . ?
C14 C15 H15 119.3 . . ?
C8 C15 H15 119.3 . . ?
N1 C16 C17 122.7(5) . . ?
N1 C16 H16 118.7 . . ?
C17 C16 H16 118.7 . . ?
C18 C17 C16 118.6(6) . . ?
C18 C17 H17 120.7 . . ?
C16 C17 H17 120.7 . . ?
C17 C18 C19 119.6(5) . . ?
C17 C18 H18 120.2 . . ?
C19 C18 H18 120.2 . . ?
C18 C19 C20 118.9(6) . . ?
C18 C19 H19 120.5 . . ?
C20 C19 H19 120.5 . . ?
N1 C20 C19 120.9(5) . . ?
N1 C20 C21 117.4(4) . . ?
C19 C20 C21 121.7(5) . . ?
N2 C21 C22 121.1(5) . . ?
N2 C21 C20 115.5(5) . . ?
C22 C21 C20 123.4(5) . . ?
C23 C22 C21 119.6(5) . . ?
C23 C22 H22 120.2 . . ?
C21 C22 H22 120.2 . . ?
C24 C23 C22 119.2(6) . . ?
C24 C23 H23 120.4 . . ?
C22 C23 H23 120.4 . . ?
C23 C24 C25 119.1(6) . . ?
C23 C24 H24 120.4 . . ?
C25 C24 H24 120.4 . . ?
N2 C25 C24 122.4(5) . . ?
N2 C25 H25 118.8 . . ?
C24 C25 H25 118.8 . . ?

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
Cd1 O2 C1 O1 7.6(5) . . . . ?
Cd1 O2 C1 C2 -171.0(4) . . . . ?
Cd1 O1 C1 O2 -8.3(5) . . . . ?
Cd1 O1 C1 C2 170.3(3) . . . . ?
O2 C1 C2 C7 10.9(7) . . . . ?
O1 C1 C2 C7 -167.8(5) . . . . ?
O2 C1 C2 C3 -173.6(4) . . . . ?
O1 C1 C2 C3 7.7(7) . . . . ?
C7 C2 C3 C4 2.4(7) . . . . ?
C1 C2 C3 C4 -173.2(4) . . . . ?
C2 C3 C4 C5 -0.5(7) . . . . ?
C2 C3 C4 C8 176.7(4) . . . . ?
C3 C4 C5 C6 -1.7(7) . . . . ?
C8 C4 C5 C6 -178.8(4) . . . . ?
C4 C5 C6 C7 2.1(7) . . . . ?
C5 C6 C7 C2 -0.2(8) . . . . ?
C3 C2 C7 C6 -2.0(7) . . . . ?
C1 C2 C7 C6 173.4(4) . . . . ?
C3 C4 C8 C15 -124.8(5) . . . . ?
C5 C4 C8 C15 52.3(7) . . . . ?
C3 C4 C8 C9 50.5(6) . . . . ?
C5 C4 C8 C9 -132.5(5) . . . . ?
C15 C8 C9 C11 3.5(7) . . . . ?
C4 C8 C9 C11 -171.9(5) . . . . ?
C15 C8 C9 C10 -171.2(5) . . . . ?
C4 C8 C9 C10 13.4(7) . . . . ?
Cd1 O4 C10 O3 -24.3(7) 1_655 . . . ?
Cd1 O4 C10 C9 150.5(3) 1_655 . . . ?
C11 C9 C10 O3 53.3(7) . . . . ?
C8 C9 C10 O3 -131.9(5) . . . . ?
C11 C9 C10 O4 -121.9(5) . . . . ?
C8 C9 C10 O4 52.9(7) . . . . ?
C8 C9 C11 C12 -2.7(8) . . . . ?
C10 C9 C11 C12 172.3(5) . . . . ?
C9 C11 C12 C14 -0.4(8) . . . . ?
C9 C11 C12 C13 178.4(5) . . . . ?
C14 C12 C13 O5 178.5(5) . . . . ?
C11 C12 C13 O5 -0.2(9) . . . . ?
C14 C12 C13 O6 -0.4(8) . . . . ?
C11 C12 C13 O6 -179.1(5) . . . . ?
C11 C12 C14 C15 2.6(8) . . . . ?
C13 C12 C14 C15 -176.1(5) . . . . ?
C12 C14 C15 C8 -1.8(8) . . . . ?
C9 C8 C15 C14 -1.3(8) . . . . ?
C4 C8 C15 C14 174.2(5) . . . . ?
C20 N1 C16 C17 0.8(8) . . . . ?
Cd1 N1 C16 C17 -177.0(4) . . . . ?
N1 C16 C17 C18 -0.2(9) . . . . ?
C16 C17 C18 C19 -1.0(9) . . . . ?
C17 C18 C19 C20 1.7(9) . . . . ?
C16 N1 C20 C19 -0.1(8) . . . . ?
Cd1 N1 C20 C19 177.9(4) . . . . ?
C16 N1 C20 C21 177.8(5) . . . . ?
Cd1 N1 C20 C21 -4.3(6) . . . . ?
C18 C19 C20 N1 -1.2(8) . . . . ?
C18 C19 C20 C21 -178.9(5) . . . . ?
C25 N2 C21 C22 0.4(8) . . . . ?
Cd1 N2 C21 C22 -174.5(4) . . . . ?
C25 N2 C21 C20 -178.8(5) . . . . ?
Cd1 N2 C21 C20 6.4(6) . . . . ?
N1 C20 C21 N2 -1.4(7) . . . . ?
C19 C20 C21 N2 176.4(5) . . . . ?
N1 C20 C21 C22 179.5(5) . . . . ?
C19 C20 C21 C22 -2.7(8) . . . . ?
N2 C21 C22 C23 -0.1(9) . . . . ?
C20 C21 C22 C23 178.9(5) . . . . ?
C21 C22 C23 C24 -0.1(10) . . . . ?
C22 C23 C24 C25 0.1(10) . . . . ?
C21 N2 C25 C24 -0.4(9) . . . . ?
Cd1 N2 C25 C24 174.1(5) . . . . ?
C23 C24 C25 N2 0.1(10) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O10 H8W O8 0.85 1.98 2.827(7) 178.8 2_665
O10 H7W O3 0.85 1.88 2.734(6) 179.1 .
O9 H6W O10 0.85 1.92 2.773(6) 179.8 .
O9 H5W O1 0.85 2.00 2.854(5) 179.1 .
O8 H4W O9 0.77 2.11 2.861(6) 165.9 1_655
O8 H3W O5 0.85 2.12 2.965(5) 179.4 .
O7 H2W O10 0.85 2.05 2.902(6) 179.2 2_565
O7 H1W O8 0.85 1.94 2.792(5) 179.1 2_665
O6 H6 O2 0.82 1.81 2.601(5) 161.4 1_645
O10 H8W O8 0.85 1.98 2.827(7) 178.8 2_665
O10 H7W O3 0.85 1.88 2.734(6) 179.1 .
O9 H6W O10 0.85 1.92 2.773(6) 179.8 .
O9 H5W O1 0.85 2.00 2.854(5) 179.1 .
O8 H4W O9 0.77 2.11 2.861(6) 165.9 1_655
O8 H3W O5 0.85 2.12 2.965(5) 179.4 .
O7 H2W O10 0.85 2.05 2.902(6) 179.2 2_565
O7 H1W O8 0.85 1.94 2.792(5) 179.1 2_665
O6 H6 O2 0.82 1.81 2.601(5) 161.4 1_645
O10 H8W O8 0.85 1.98 2.827(7) 178.8 2_665
O10 H7W O3 0.85 1.88 2.734(6) 179.1 .
O9 H6W O10 0.85 1.92 2.773(6) 179.8 .
O9 H5W O1 0.85 2.00 2.854(5) 179.1 .
O8 H4W O9 0.77 2.11 2.861(6) 165.9 1_655
O8 H3W O5 0.85 2.12 2.965(5) 179.4 .
O7 H2W O10 0.85 2.05 2.902(6) 179.2 2_565
O7 H1W O8 0.85 1.94 2.792(5) 179.1 2_665
O6 H6 O2 0.82 1.81 2.601(5) 161.4 1_645
O6 H6 O2 0.82 1.81 2.601(5) 161.4 1_645
O7 H1W O8 0.85 1.94 2.792(5) 179.1 2_665
O7 H2W O10 0.85 2.05 2.902(6) 179.2 2_565
O8 H3W O5 0.85 2.12 2.965(5) 179.4 .
O8 H4W O9 0.77 2.11 2.861(6) 165.9 1_655
O9 H5W O1 0.85 2.00 2.854(5) 179.1 .
O9 H6W O10 0.85 1.92 2.773(6) 179.8 .
O10 H7W O3 0.85 1.88 2.734(6) 179.1 .
O10 H8W O8 0.85 1.98 2.827(7) 178.8 2_665
O6 H6 O2 0.82 1.81 2.601(5) 161.4 1_645
O7 H1W O8 0.85 1.94 2.792(5) 179.1 2_665
O7 H2W O10 0.85 2.05 2.902(6) 179.2 2_565
O8 H3W O5 0.85 2.12 2.965(5) 179.4 .
O8 H4W O9 0.77 2.11 2.861(6) 165.9 1_655
O9 H5W O1 0.85 2.00 2.854(5) 179.1 .
O9 H6W O10 0.85 1.92 2.773(6) 179.8 .
O10 H7W O3 0.85 1.88 2.734(6) 179.1 .
O10 H8W O8 0.85 1.98 2.827(7) 178.8 2_665
O6 H6 O2 0.82 1.81 2.601(5) 161.4 1_645
O7 H1W O8 0.85 1.94 2.792(5) 179.1 2_665
O7 H2W O10 0.85 2.05 2.902(6) 179.2 2_565
O8 H3W O5 0.85 2.12 2.965(5) 179.4 .
O8 H4W O9 0.77 2.11 2.861(6) 165.9 1_655
O9 H5W O1 0.85 2.00 2.854(5) 179.1 .
O9 H6W O10 0.85 1.92 2.773(6) 179.8 .
O10 H7W O3 0.85 1.88 2.734(6) 179.1 .
O10 H8W O8 0.85 1.98 2.827(7) 178.8 2_665

_refine_diff_density_max         0.661
_refine_diff_density_min         -0.660
_refine_diff_density_rms         0.100


# start Validation Reply Form
_vrf_PLAT910_I                   
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min) 12 Note
RESPONSE: Reduction of beam stop mask did not yield significant improvement.
Most of those missing srtong reflections appeared to be very strong and were
treated as overflows.
;
# end Validation Reply Form

####################################################################### 
# 
# 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_437-5Cd
_database_code_depnum_ccdc_archive 'CCDC 2012745'
_audit_update_record             
;
2020-06-28 deposited with the CCDC.	2021-01-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C39 H27 Cd2 Cl N4 O8'
_chemical_formula_weight         939.89

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'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   14.8198(7)
_cell_length_b                   14.3529(7)
_cell_length_c                   16.8168(7)
_cell_angle_alpha                90
_cell_angle_beta                 103.106(4)
_cell_angle_gamma                90
_cell_volume                     3483.9(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    12278
_cell_measurement_theta_min      3.433
_cell_measurement_theta_max      25.047

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.792
_exptl_crystal_F_000             1864
_exptl_transmission_factor_min   0.729
_exptl_transmission_factor_max   0.752
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.210
_exptl_absorpt_coefficient_mu    1.360
_shelx_estimated_absorpt_T_min   0.736
_shelx_estimated_absorpt_T_max   0.763
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.736
_exptl_absorpt_correction_T_max  0.763
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APE-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12278
_diffrn_reflns_av_unetI/netI     0.0701
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.433
_diffrn_reflns_theta_max         25.047
_diffrn_reflns_theta_full        25.047
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             6153
_reflns_number_gt                4497
_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    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0370P)²+1.1078P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6153
_refine_ls_number_parameters     487
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0450
_refine_ls_wR_factor_ref         0.1125
_refine_ls_wR_factor_gt          0.0950
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.000
_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
Cd1 Cd 0.08325(3) 0.59043(3) 0.24311(2) 0.04041(15) Uani 1 1 d . . . . .
Cd2 Cd 0.33677(3) 0.60993(3) 0.28339(2) 0.03588(14) Uani 1 1 d . . . . .
N1 N 0.0643(3) 0.6823(3) 0.3521(3) 0.0398(12) Uani 1 1 d . . . . .
N2 N 0.1206(3) 0.5007(3) 0.3622(3) 0.0366(11) Uani 1 1 d . . . . .
N3 N 0.3252(3) 0.6844(3) 0.4050(3) 0.0436(12) Uani 1 1 d . . . . .
N4 N 0.3721(3) 0.5032(3) 0.3897(3) 0.0380(11) Uani 1 1 d . . . . .
O1 O 0.1157(3) 0.4973(3) 0.1469(3) 0.0538(12) Uani 1 1 d . . . . .
O2 O 0.2635(3) 0.4857(3) 0.2112(2) 0.0453(10) Uani 1 1 d . . . . .
O3 O 0.0799(3) 0.4763(3) -0.1985(2) 0.0494(11) Uani 1 1 d . . . . .
O4 O 0.0358(2) 0.3467(3) -0.1476(2) 0.0445(10) Uani 1 1 d . . . . .
O5 O 0.5341(3) 0.2885(3) -0.2875(3) 0.0595(13) Uani 1 1 d . . . . .
O6 O 0.5432(3) 0.4172(3) -0.2164(3) 0.0560(12) Uani 1 1 d . . . . .
Cl1 Cl 0.20203(11) 0.70471(12) 0.21260(11) 0.0602(5) Uani 1 1 d . . . . .
O7 O 0.5492(5) 0.0942(4) 0.6673(5) 0.129(3) Uani 1 1 d . . . . .
H1W H 0.5242 0.0450 0.6806 0.154 Uiso 1 1 d R U . . .
H2W H 0.5454 0.1514 0.6794 0.154 Uiso 1 1 d R U . . .
O8 O 0.2314(8) 0.5812(7) 0.7720(7) 0.273(6) Uani 1 1 d . . . . .
H3W H 0.1858 0.5495 0.7801 0.328 Uiso 1 1 d R U . . .
H4W H 0.2901 0.5841 0.7864 0.328 Uiso 1 1 d R U . . .
C1 C 0.1986(4) 0.4808(4) 0.1481(3) 0.0364(13) Uani 1 1 d . . . . .
C2 C 0.2223(4) 0.4509(3) 0.0702(3) 0.0305(12) Uani 1 1 d . . . . .
C3 C 0.1545(3) 0.4438(3) -0.0013(3) 0.0295(12) Uani 1 1 d . . . . .
H3 H 0.0937 0.4582 0.0000 0.035 Uiso 1 1 calc R U . . .
C4 C 0.1738(4) 0.4159(3) -0.0749(3) 0.0317(12) Uani 1 1 d . . . . .
C5 C 0.0919(4) 0.4132(4) -0.1468(3) 0.0320(13) Uani 1 1 d . . . . .
C6 C 0.2653(3) 0.3928(3) -0.0777(3) 0.0290(12) Uani 1 1 d . . . . .
C7 C 0.3332(4) 0.4008(4) -0.0054(3) 0.0347(13) Uani 1 1 d . . . . .
H7 H 0.3942 0.3860 -0.0059 0.042 Uiso 1 1 calc R U . . .
C8 C 0.3126(4) 0.4301(4) 0.0669(4) 0.0382(14) Uani 1 1 d . . . . .
H8 H 0.3599 0.4358 0.1136 0.046 Uiso 1 1 calc R U . . .
C9 C 0.2899(3) 0.3551(3) -0.1522(3) 0.0285(12) Uani 1 1 d . . . . .
C10 C 0.3779(3) 0.3707(4) -0.1664(3) 0.0316(12) Uani 1 1 d . . . . .
H10 H 0.4185 0.4108 -0.1323 0.038 Uiso 1 1 calc R U . . .
C11 C 0.4059(3) 0.3271(4) -0.2306(3) 0.0306(12) Uani 1 1 d . . . . .
C12 C 0.5016(4) 0.3454(5) -0.2446(3) 0.0409(15) Uani 1 1 d . . . . .
C13 C 0.3448(4) 0.2700(4) -0.2832(3) 0.0391(14) Uani 1 1 d . . . . .
H13 H 0.3636 0.2405 -0.3259 0.047 Uiso 1 1 calc R U . . .
C14 C 0.2558(4) 0.2565(4) -0.2725(3) 0.0394(14) Uani 1 1 d . . . . .
H14 H 0.2141 0.2194 -0.3087 0.047 Uiso 1 1 calc R U . . .
C15 C 0.2295(4) 0.2987(3) -0.2077(3) 0.0337(13) Uani 1 1 d . . . . .
H15 H 0.1697 0.2893 -0.2007 0.040 Uiso 1 1 calc R U . . .
C16 C 0.0397(4) 0.7714(4) 0.3473(4) 0.0504(17) Uani 1 1 d . . . . .
H16 H 0.0301 0.8008 0.2967 0.060 Uiso 1 1 calc R U . . .
C17 C 0.0279(5) 0.8223(5) 0.4134(4) 0.0595(19) Uani 1 1 d . . . . .
H17 H 0.0104 0.8846 0.4072 0.071 Uiso 1 1 calc R U . . .
C18 C 0.0422(5) 0.7805(5) 0.4885(4) 0.0583(18) Uani 1 1 d . . . . .
H18 H 0.0338 0.8141 0.5336 0.070 Uiso 1 1 calc R U . . .
C19 C 0.0697(4) 0.6861(4) 0.4969(3) 0.0398(14) Uani 1 1 d . . . . .
C20 C 0.0798(3) 0.6403(4) 0.4255(3) 0.0341(13) Uani 1 1 d . . . . .
C21 C 0.0847(4) 0.6370(5) 0.5727(4) 0.0490(16) Uani 1 1 d . . . . .
H21 H 0.0756 0.6673 0.6192 0.059 Uiso 1 1 calc R U . . .
C22 C 0.1118(4) 0.5480(5) 0.5773(4) 0.0487(16) Uani 1 1 d . . . . .
H22 H 0.1220 0.5175 0.6273 0.058 Uiso 1 1 calc R U . . .
C23 C 0.1254(4) 0.4982(4) 0.5067(3) 0.0398(14) Uani 1 1 d . . . . .
C24 C 0.1091(3) 0.5440(4) 0.4308(3) 0.0331(13) Uani 1 1 d . . . . .
C25 C 0.1533(4) 0.4050(4) 0.5086(4) 0.0528(18) Uani 1 1 d . . . . .
H25 H 0.1653 0.3725 0.5577 0.063 Uiso 1 1 calc R U . . .
C26 C 0.1631(5) 0.3620(5) 0.4394(5) 0.0592(19) Uani 1 1 d . . . . .
H26 H 0.1803 0.2996 0.4402 0.071 Uiso 1 1 calc R U . . .
C27 C 0.1470(4) 0.4124(4) 0.3677(4) 0.0516(17) Uani 1 1 d . . . . .
H27 H 0.1552 0.3828 0.3206 0.062 Uiso 1 1 calc R U . . .
C28 C 0.3046(5) 0.7730(4) 0.4114(5) 0.069(2) Uani 1 1 d . . . . .
H28 H 0.2924 0.8096 0.3646 0.083 Uiso 1 1 calc R U . . .
C29 C 0.3003(6) 0.8141(6) 0.4854(6) 0.088(3) Uani 1 1 d . . . . .
H29 H 0.2871 0.8771 0.4884 0.106 Uiso 1 1 calc R U . . .
C30 C 0.3159(5) 0.7596(6) 0.5534(5) 0.077(2) Uani 1 1 d . . . . .
H30 H 0.3121 0.7852 0.6033 0.092 Uiso 1 1 calc R U . . .
C31 C 0.3373(4) 0.6661(5) 0.5486(4) 0.0545(18) Uani 1 1 d . . . . .
C32 C 0.3424(4) 0.6304(4) 0.4723(3) 0.0376(14) Uani 1 1 d . . . . .
C33 C 0.3543(5) 0.6059(6) 0.6177(4) 0.070(2) Uani 1 1 d . . . . .
H33 H 0.3501 0.6290 0.6684 0.083 Uiso 1 1 calc R U . . .
C34 C 0.3765(5) 0.5152(6) 0.6100(4) 0.069(2) Uani 1 1 d . . . . .
H34 H 0.3864 0.4770 0.6558 0.083 Uiso 1 1 calc R U . . .
C35 C 0.3851(4) 0.4765(5) 0.5337(4) 0.0497(16) Uani 1 1 d . . . . .
C36 C 0.3669(3) 0.5345(4) 0.4645(3) 0.0342(13) Uani 1 1 d . . . . .
C37 C 0.4120(4) 0.3859(5) 0.5238(5) 0.061(2) Uani 1 1 d . . . . .
H37 H 0.4266 0.3464 0.5687 0.073 Uiso 1 1 calc R U . . .
C38 C 0.4170(4) 0.3542(4) 0.4486(5) 0.0553(18) Uani 1 1 d . . . . .
H38 H 0.4340 0.2929 0.4416 0.066 Uiso 1 1 calc R U . . .
C39 C 0.3963(4) 0.4152(4) 0.3822(4) 0.0499(17) Uani 1 1 d . . . . .
H39 H 0.3997 0.3934 0.3309 0.060 Uiso 1 1 calc R U . . .


_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
Cd1 O1 2.234(4) . ?
Cd1 O4 2.285(4) 3_565 ?
Cd1 N1 2.327(4) . ?
Cd1 N2 2.339(5) . ?
Cd1 Cl1 2.5420(17) . ?
Cd1 O3 2.550(4) 3_565 ?
Cd1 C5 2.731(5) 3_565 ?
Cd2 O2 2.288(4) . ?
Cd2 N4 2.322(5) . ?
Cd2 O6 2.344(4) 3_665 ?
Cd2 N3 2.347(5) . ?
Cd2 O5 2.394(4) 3_665 ?
Cd2 Cl1 2.4854(17) . ?
Cd2 C12 2.698(6) 3_665 ?
N1 C16 1.327(7) . ?
N1 C20 1.346(7) . ?
N2 C27 1.323(7) . ?
N2 C24 1.355(7) . ?
N3 C28 1.319(7) . ?
N3 C32 1.348(7) . ?
N4 C39 1.326(7) . ?
N4 C36 1.355(7) . ?
O1 C1 1.247(6) . ?
O2 C1 1.263(6) . ?
O3 C5 1.240(6) . ?
O3 Cd1 2.550(4) 3_565 ?
O4 C5 1.264(6) . ?
O4 Cd1 2.285(4) 3_565 ?
O5 C12 1.255(7) . ?
O5 Cd2 2.394(4) 3_665 ?
O6 C12 1.239(7) . ?
O6 Cd2 2.344(4) 3_665 ?
O7 H1W 0.8500 . ?
O7 H2W 0.8499 . ?
O8 H3W 0.8500 . ?
O8 H4W 0.8501 . ?
C1 C2 1.494(7) . ?
C2 C8 1.385(7) . ?
C2 C3 1.385(7) . ?
C3 C4 1.390(7) . ?
C3 H3 0.9300 . ?
C4 C6 1.408(7) . ?
C4 C5 1.507(7) . ?
C5 Cd1 2.731(5) 3_565 ?
C6 C7 1.396(7) . ?
C6 C9 1.484(7) . ?
C7 C8 1.384(7) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C9 C15 1.395(7) . ?
C9 C10 1.397(7) . ?
C10 C11 1.390(7) . ?
C10 H10 0.9300 . ?
C11 C13 1.381(7) . ?
C11 C12 1.513(7) . ?
C12 Cd2 2.698(6) 3_665 ?
C13 C14 1.386(7) . ?
C13 H13 0.9300 . ?
C14 C15 1.378(7) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C17 1.374(8) . ?
C16 H16 0.9300 . ?
C17 C18 1.370(9) . ?
C17 H17 0.9300 . ?
C18 C19 1.414(8) . ?
C18 H18 0.9300 . ?
C19 C20 1.406(7) . ?
C19 C21 1.429(8) . ?
C20 C24 1.445(7) . ?
C21 C22 1.336(8) . ?
C21 H21 0.9300 . ?
C22 C23 1.439(8) . ?
C22 H22 0.9300 . ?
C23 C25 1.397(7) . ?
C23 C24 1.408(7) . ?
C25 C26 1.354(9) . ?
C25 H25 0.9300 . ?
C26 C27 1.382(9) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
C28 C29 1.391(10) . ?
C28 H28 0.9300 . ?
C29 C30 1.361(11) . ?
C29 H29 0.9300 . ?
C30 C31 1.385(9) . ?
C30 H30 0.9300 . ?
C31 C32 1.399(8) . ?
C31 C33 1.424(9) . ?
C32 C36 1.437(8) . ?
C33 C34 1.356(9) . ?
C33 H33 0.9300 . ?
C34 C35 1.430(9) . ?
C34 H34 0.9300 . ?
C35 C37 1.380(9) . ?
C35 C36 1.406(8) . ?
C37 C38 1.363(9) . ?
C37 H37 0.9300 . ?
C38 C39 1.398(9) . ?
C38 H38 0.9300 . ?
C39 H39 0.9300 . ?

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 Cd1 O4 89.18(15) . 3_565 ?
O1 Cd1 N1 173.93(15) . . ?
O4 Cd1 N1 96.79(15) 3_565 . ?
O1 Cd1 N2 104.06(16) . . ?
O4 Cd1 N2 144.52(14) 3_565 . ?
N1 Cd1 N2 71.63(16) . . ?
O1 Cd1 Cl1 88.12(12) . . ?
O4 Cd1 Cl1 93.61(11) 3_565 . ?
N1 Cd1 Cl1 90.36(12) . . ?
N2 Cd1 Cl1 119.19(11) . . ?
O1 Cd1 O3 84.70(14) . 3_565 ?
O4 Cd1 O3 53.99(13) 3_565 3_565 ?
N1 Cd1 O3 99.71(15) . 3_565 ?
N2 Cd1 O3 94.00(14) . 3_565 ?
Cl1 Cd1 O3 146.79(10) . 3_565 ?
O1 Cd1 C5 83.75(14) . 3_565 ?
O4 Cd1 C5 27.38(14) 3_565 3_565 ?
N1 Cd1 C5 102.08(15) . 3_565 ?
N2 Cd1 C5 120.39(16) . 3_565 ?
Cl1 Cd1 C5 120.08(13) . 3_565 ?
O3 Cd1 C5 26.88(13) 3_565 3_565 ?
O2 Cd2 N4 83.74(14) . . ?
O2 Cd2 O6 86.35(15) . 3_665 ?
N4 Cd2 O6 101.40(16) . 3_665 ?
O2 Cd2 N3 134.20(15) . . ?
N4 Cd2 N3 71.22(16) . . ?
O6 Cd2 N3 135.03(16) 3_665 . ?
O2 Cd2 O5 140.36(14) . 3_665 ?
N4 Cd2 O5 109.90(15) . 3_665 ?
O6 Cd2 O5 54.98(14) 3_665 3_665 ?
N3 Cd2 O5 85.03(16) . 3_665 ?
O2 Cd2 Cl1 86.52(11) . . ?
N4 Cd2 Cl1 138.26(12) . . ?
O6 Cd2 Cl1 118.38(12) 3_665 . ?
N3 Cd2 Cl1 87.64(12) . . ?
O5 Cd2 Cl1 103.34(11) 3_665 . ?
O2 Cd2 C12 113.45(17) . 3_665 ?
N4 Cd2 C12 106.58(16) . 3_665 ?
O6 Cd2 C12 27.32(15) 3_665 3_665 ?
N3 Cd2 C12 110.24(18) . 3_665 ?
O5 Cd2 C12 27.71(15) 3_665 3_665 ?
Cl1 Cd2 C12 114.51(13) . 3_665 ?
C16 N1 C20 118.4(5) . . ?
C16 N1 Cd1 125.3(4) . . ?
C20 N1 Cd1 116.3(4) . . ?
C27 N2 C24 118.2(5) . . ?
C27 N2 Cd1 126.5(4) . . ?
C24 N2 Cd1 115.2(3) . . ?
C28 N3 C32 119.2(6) . . ?
C28 N3 Cd2 125.1(5) . . ?
C32 N3 Cd2 115.7(4) . . ?
C39 N4 C36 118.5(5) . . ?
C39 N4 Cd2 125.0(4) . . ?
C36 N4 Cd2 116.5(4) . . ?
C1 O1 Cd1 118.4(4) . . ?
C1 O2 Cd2 132.0(4) . . ?
C5 O3 Cd1 84.7(3) . 3_565 ?
C5 O4 Cd1 96.4(3) . 3_565 ?
C12 O5 Cd2 89.8(4) . 3_665 ?
C12 O6 Cd2 92.5(4) . 3_665 ?
Cd2 Cl1 Cd1 93.90(6) . . ?
H1W O7 H2W 133.1 . . ?
H3W O8 H4W 141.4 . . ?
O1 C1 O2 124.2(5) . . ?
O1 C1 C2 117.9(5) . . ?
O2 C1 C2 117.9(5) . . ?
C8 C2 C3 117.9(5) . . ?
C8 C2 C1 121.3(5) . . ?
C3 C2 C1 120.9(5) . . ?
C2 C3 C4 122.6(5) . . ?
C2 C3 H3 118.7 . . ?
C4 C3 H3 118.7 . . ?
C3 C4 C6 119.5(5) . . ?
C3 C4 C5 115.6(4) . . ?
C6 C4 C5 124.9(5) . . ?
O3 C5 O4 123.7(5) . . ?
O3 C5 C4 120.3(5) . . ?
O4 C5 C4 115.9(5) . . ?
O3 C5 Cd1 68.4(3) . 3_565 ?
O4 C5 Cd1 56.2(3) . 3_565 ?
C4 C5 Cd1 163.8(4) . 3_565 ?
C7 C6 C4 117.4(5) . . ?
C7 C6 C9 119.9(4) . . ?
C4 C6 C9 122.5(5) . . ?
C8 C7 C6 122.1(5) . . ?
C8 C7 H7 118.9 . . ?
C6 C7 H7 118.9 . . ?
C7 C8 C2 120.5(5) . . ?
C7 C8 H8 119.7 . . ?
C2 C8 H8 119.7 . . ?
C15 C9 C10 117.5(5) . . ?
C15 C9 C6 122.2(4) . . ?
C10 C9 C6 120.2(4) . . ?
C11 C10 C9 121.0(5) . . ?
C11 C10 H10 119.5 . . ?
C9 C10 H10 119.5 . . ?
C13 C11 C10 119.8(5) . . ?
C13 C11 C12 120.3(5) . . ?
C10 C11 C12 119.9(5) . . ?
O6 C12 O5 122.6(5) . . ?
O6 C12 C11 119.2(5) . . ?
O5 C12 C11 118.2(6) . . ?
O6 C12 Cd2 60.2(3) . 3_665 ?
O5 C12 Cd2 62.5(3) . 3_665 ?
C11 C12 Cd2 173.7(4) . 3_665 ?
C11 C13 C14 120.3(5) . . ?
C11 C13 H13 119.8 . . ?
C14 C13 H13 119.8 . . ?
C15 C14 C13 119.3(5) . . ?
C15 C14 H14 120.4 . . ?
C13 C14 H14 120.4 . . ?
C14 C15 C9 122.1(5) . . ?
C14 C15 H15 119.0 . . ?
C9 C15 H15 119.0 . . ?
N1 C16 C17 123.1(6) . . ?
N1 C16 H16 118.5 . . ?
C17 C16 H16 118.5 . . ?
C18 C17 C16 119.4(6) . . ?
C18 C17 H17 120.3 . . ?
C16 C17 H17 120.3 . . ?
C17 C18 C19 119.5(6) . . ?
C17 C18 H18 120.2 . . ?
C19 C18 H18 120.2 . . ?
C20 C19 C18 116.5(6) . . ?
C20 C19 C21 120.4(5) . . ?
C18 C19 C21 123.0(6) . . ?
N1 C20 C19 123.0(5) . . ?
N1 C20 C24 118.1(5) . . ?
C19 C20 C24 118.9(5) . . ?
C22 C21 C19 120.4(6) . . ?
C22 C21 H21 119.8 . . ?
C19 C21 H21 119.8 . . ?
C21 C22 C23 121.6(6) . . ?
C21 C22 H22 119.2 . . ?
C23 C22 H22 119.2 . . ?
C25 C23 C24 117.2(6) . . ?
C25 C23 C22 123.5(6) . . ?
C24 C23 C22 119.2(5) . . ?
N2 C24 C23 121.9(5) . . ?
N2 C24 C20 118.7(5) . . ?
C23 C24 C20 119.4(5) . . ?
C26 C25 C23 120.4(6) . . ?
C26 C25 H25 119.8 . . ?
C23 C25 H25 119.8 . . ?
C25 C26 C27 118.7(6) . . ?
C25 C26 H26 120.6 . . ?
C27 C26 H26 120.6 . . ?
N2 C27 C26 123.5(6) . . ?
N2 C27 H27 118.2 . . ?
C26 C27 H27 118.2 . . ?
N3 C28 C29 122.7(7) . . ?
N3 C28 H28 118.6 . . ?
C29 C28 H28 118.6 . . ?
C30 C29 C28 118.3(7) . . ?
C30 C29 H29 120.8 . . ?
C28 C29 H29 120.8 . . ?
C29 C30 C31 120.3(7) . . ?
C29 C30 H30 119.8 . . ?
C31 C30 H30 119.8 . . ?
C30 C31 C32 118.0(7) . . ?
C30 C31 C33 122.7(7) . . ?
C32 C31 C33 119.3(7) . . ?
N3 C32 C31 121.3(6) . . ?
N3 C32 C36 118.5(5) . . ?
C31 C32 C36 120.1(6) . . ?
C34 C33 C31 120.4(7) . . ?
C34 C33 H33 119.8 . . ?
C31 C33 H33 119.8 . . ?
C33 C34 C35 122.1(7) . . ?
C33 C34 H34 118.9 . . ?
C35 C34 H34 118.9 . . ?
C37 C35 C36 117.7(6) . . ?
C37 C35 C34 124.1(7) . . ?
C36 C35 C34 118.2(6) . . ?
N4 C36 C35 122.1(5) . . ?
N4 C36 C32 118.1(5) . . ?
C35 C36 C32 119.8(5) . . ?
C38 C37 C35 120.3(7) . . ?
C38 C37 H37 119.8 . . ?
C35 C37 H37 119.8 . . ?
C37 C38 C39 119.0(6) . . ?
C37 C38 H38 120.5 . . ?
C39 C38 H38 120.5 . . ?
N4 C39 C38 122.4(6) . . ?
N4 C39 H39 118.8 . . ?
C38 C39 H39 118.8 . . ?

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
Cd1 O1 C1 O2 24.4(8) . . . . ?
Cd1 O1 C1 C2 -157.1(4) . . . . ?
Cd2 O2 C1 O1 -74.1(7) . . . . ?
Cd2 O2 C1 C2 107.5(5) . . . . ?
O1 C1 C2 C8 -179.1(5) . . . . ?
O2 C1 C2 C8 -0.6(8) . . . . ?
O1 C1 C2 C3 1.3(8) . . . . ?
O2 C1 C2 C3 179.8(5) . . . . ?
C8 C2 C3 C4 0.6(8) . . . . ?
C1 C2 C3 C4 -179.7(5) . . . . ?
C2 C3 C4 C6 0.8(8) . . . . ?
C2 C3 C4 C5 -179.2(5) . . . . ?
Cd1 O3 C5 O4 11.0(5) 3_565 . . . ?
Cd1 O3 C5 C4 -164.8(4) 3_565 . . . ?
Cd1 O4 C5 O3 -12.3(6) 3_565 . . . ?
Cd1 O4 C5 C4 163.7(4) 3_565 . . . ?
C3 C4 C5 O3 102.6(6) . . . . ?
C6 C4 C5 O3 -77.4(7) . . . . ?
C3 C4 C5 O4 -73.5(6) . . . . ?
C6 C4 C5 O4 106.5(6) . . . . ?
C3 C4 C5 Cd1 -16.5(16) . . . 3_565 ?
C6 C4 C5 Cd1 163.5(11) . . . 3_565 ?
C3 C4 C6 C7 -1.1(7) . . . . ?
C5 C4 C6 C7 178.9(5) . . . . ?
C3 C4 C6 C9 174.8(5) . . . . ?
C5 C4 C6 C9 -5.2(8) . . . . ?
C4 C6 C7 C8 0.1(8) . . . . ?
C9 C6 C7 C8 -175.9(5) . . . . ?
C6 C7 C8 C2 1.3(8) . . . . ?
C3 C2 C8 C7 -1.6(8) . . . . ?
C1 C2 C8 C7 178.7(5) . . . . ?
C7 C6 C9 C15 143.6(5) . . . . ?
C4 C6 C9 C15 -32.2(8) . . . . ?
C7 C6 C9 C10 -32.4(7) . . . . ?
C4 C6 C9 C10 151.8(5) . . . . ?
C15 C9 C10 C11 -3.7(8) . . . . ?
C6 C9 C10 C11 172.4(5) . . . . ?
C9 C10 C11 C13 2.4(8) . . . . ?
C9 C10 C11 C12 179.9(5) . . . . ?
Cd2 O6 C12 O5 4.3(6) 3_665 . . . ?
Cd2 O6 C12 C11 -172.8(4) 3_665 . . . ?
Cd2 O5 C12 O6 -4.2(6) 3_665 . . . ?
Cd2 O5 C12 C11 173.0(4) 3_665 . . . ?
C13 C11 C12 O6 156.1(5) . . . . ?
C10 C11 C12 O6 -21.3(8) . . . . ?
C13 C11 C12 O5 -21.1(8) . . . . ?
C10 C11 C12 O5 161.4(5) . . . . ?
C10 C11 C13 C14 0.4(8) . . . . ?
C12 C11 C13 C14 -177.1(5) . . . . ?
C11 C13 C14 C15 -1.7(9) . . . . ?
C13 C14 C15 C9 0.2(9) . . . . ?
C10 C9 C15 C14 2.4(8) . . . . ?
C6 C9 C15 C14 -173.6(5) . . . . ?
C20 N1 C16 C17 -1.1(9) . . . . ?
Cd1 N1 C16 C17 178.9(5) . . . . ?
N1 C16 C17 C18 0.3(11) . . . . ?
C16 C17 C18 C19 0.6(10) . . . . ?
C17 C18 C19 C20 -0.7(9) . . . . ?
C17 C18 C19 C21 -179.1(6) . . . . ?
C16 N1 C20 C19 1.0(8) . . . . ?
Cd1 N1 C20 C19 -179.0(4) . . . . ?
C16 N1 C20 C24 -178.2(5) . . . . ?
Cd1 N1 C20 C24 1.8(6) . . . . ?
C18 C19 C20 N1 -0.1(8) . . . . ?
C21 C19 C20 N1 178.3(5) . . . . ?
C18 C19 C20 C24 179.1(5) . . . . ?
C21 C19 C20 C24 -2.5(8) . . . . ?
C20 C19 C21 C22 2.4(9) . . . . ?
C18 C19 C21 C22 -179.2(6) . . . . ?
C19 C21 C22 C23 -0.9(9) . . . . ?
C21 C22 C23 C25 -179.8(6) . . . . ?
C21 C22 C23 C24 -0.6(8) . . . . ?
C27 N2 C24 C23 0.7(8) . . . . ?
Cd1 N2 C24 C23 177.7(4) . . . . ?
C27 N2 C24 C20 -179.7(5) . . . . ?
Cd1 N2 C24 C20 -2.8(6) . . . . ?
C25 C23 C24 N2 -0.6(8) . . . . ?
C22 C23 C24 N2 -179.9(5) . . . . ?
C25 C23 C24 C20 179.8(5) . . . . ?
C22 C23 C24 C20 0.5(8) . . . . ?
N1 C20 C24 N2 0.7(7) . . . . ?
C19 C20 C24 N2 -178.6(5) . . . . ?
N1 C20 C24 C23 -179.7(5) . . . . ?
C19 C20 C24 C23 1.0(7) . . . . ?
C24 C23 C25 C26 -0.5(9) . . . . ?
C22 C23 C25 C26 178.7(6) . . . . ?
C23 C25 C26 C27 1.5(10) . . . . ?
C24 N2 C27 C26 0.3(9) . . . . ?
Cd1 N2 C27 C26 -176.2(5) . . . . ?
C25 C26 C27 N2 -1.4(10) . . . . ?
C32 N3 C28 C29 0.5(11) . . . . ?
Cd2 N3 C28 C29 -178.8(6) . . . . ?
N3 C28 C29 C30 -1.6(13) . . . . ?
C28 C29 C30 C31 1.3(13) . . . . ?
C29 C30 C31 C32 0.1(11) . . . . ?
C29 C30 C31 C33 180.0(7) . . . . ?
C28 N3 C32 C31 1.1(9) . . . . ?
Cd2 N3 C32 C31 -179.6(4) . . . . ?
C28 N3 C32 C36 -178.6(5) . . . . ?
Cd2 N3 C32 C36 0.7(6) . . . . ?
C30 C31 C32 N3 -1.4(9) . . . . ?
C33 C31 C32 N3 178.8(6) . . . . ?
C30 C31 C32 C36 178.3(6) . . . . ?
C33 C31 C32 C36 -1.5(9) . . . . ?
C30 C31 C33 C34 -178.9(7) . . . . ?
C32 C31 C33 C34 0.9(10) . . . . ?
C31 C33 C34 C35 0.9(11) . . . . ?
C33 C34 C35 C37 176.7(7) . . . . ?
C33 C34 C35 C36 -2.1(10) . . . . ?
C39 N4 C36 C35 -0.9(8) . . . . ?
Cd2 N4 C36 C35 179.0(4) . . . . ?
C39 N4 C36 C32 178.7(5) . . . . ?
Cd2 N4 C36 C32 -1.4(6) . . . . ?
C37 C35 C36 N4 2.1(8) . . . . ?
C34 C35 C36 N4 -179.0(5) . . . . ?
C37 C35 C36 C32 -177.5(5) . . . . ?
C34 C35 C36 C32 1.4(8) . . . . ?
N3 C32 C36 N4 0.4(7) . . . . ?
C31 C32 C36 N4 -179.2(5) . . . . ?
N3 C32 C36 C35 -180.0(5) . . . . ?
C31 C32 C36 C35 0.4(8) . . . . ?
C36 C35 C37 C38 -2.2(9) . . . . ?
C34 C35 C37 C38 179.0(6) . . . . ?
C35 C37 C38 C39 1.2(9) . . . . ?
C36 N4 C39 C38 -0.3(8) . . . . ?
Cd2 N4 C39 C38 179.8(4) . . . . ?
C37 C38 C39 N4 0.2(9) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C28 H28 O8 0.93 2.25 3.146(13) 161.8 4_575
C17 H17 O1 0.93 2.48 3.299(8) 146.6 2
O8 H4W O7 0.85 2.34 3.185(13) 177.0 2_656
O8 H3W O3 0.85 1.99 2.838(11) 178.7 1_556
O7 H2W O5 0.85 2.06 2.912(7) 177.7 1_556
O7 H1W O6 0.85 2.24 3.086(8) 179.0 2_645
C28 H28 O8 0.93 2.25 3.146(13) 161.8 4_575
C17 H17 O1 0.93 2.48 3.299(8) 146.6 2
O8 H4W O7 0.85 2.34 3.185(13) 177.0 2_656
O8 H3W O3 0.85 1.99 2.838(11) 178.7 1_556
O7 H2W O5 0.85 2.06 2.912(7) 177.7 1_556
O7 H1W O6 0.85 2.24 3.086(8) 179.0 2_645
O7 H1W O6 0.85 2.24 3.086(8) 179.0 2_645
O7 H2W O5 0.85 2.06 2.912(7) 177.7 1_556
O8 H3W O3 0.85 1.99 2.838(11) 178.7 1_556
O8 H4W O7 0.85 2.34 3.185(13) 177.0 2_656
C17 H17 O1 0.93 2.48 3.299(8) 146.6 2
C28 H28 O8 0.93 2.25 3.146(13) 161.8 4_575

_refine_diff_density_max         0.679
_refine_diff_density_min         -0.674
_refine_diff_density_rms         0.102


# start Validation Reply Form
_vrf_PLAT910_I                   
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min) 18 Note
RESPONSE: Reduction of beam stop mask did not yield significant improvement.
Most of those missing srtong reflections appeared to be very strong and were
treated as overflows.
;
# end Validation Reply Form

####################################################################### 
# 
# 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_441-14Zn
_database_code_depnum_ccdc_archive 'CCDC 2012748'
_audit_update_record             
;
2020-06-28 deposited with the CCDC.	2021-01-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H40 N12 O16 Zn3'
_chemical_formula_weight         1237.03

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'
Zn Zn 0.2839 1.4301 '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                   7.5238(5)
_cell_length_b                   11.9010(9)
_cell_length_c                   13.6601(10)
_cell_angle_alpha                98.488(6)
_cell_angle_beta                 94.317(6)
_cell_angle_gamma                95.756(6)
_cell_volume                     1198.59(15)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7235
_cell_measurement_theta_min      3.403
_cell_measurement_theta_max      25.050

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.714
_exptl_crystal_F_000             630
_exptl_transmission_factor_min   0.703
_exptl_transmission_factor_max   0.723
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    1.578
_shelx_estimated_absorpt_T_min   0.713
_shelx_estimated_absorpt_T_max   0.743
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.713
_exptl_absorpt_correction_T_max  0.743
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APE-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7235
_diffrn_reflns_av_unetI/netI     0.0815
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.403
_diffrn_reflns_theta_max         25.050
_diffrn_reflns_theta_full        25.050
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4222
_reflns_number_gt                3083
_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    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0267P)²+0.7348P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4222
_refine_ls_number_parameters     374
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0514
_refine_ls_wR_factor_ref         0.1147
_refine_ls_wR_factor_gt          0.0961
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.048
_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
Zn1 Zn 0.5000 0.5000 1.0000 0.0472(3) Uani 1 2 d S . P . .
Zn2 Zn 0.67687(6) 0.90972(4) 0.71024(4) 0.03100(18) Uani 1 1 d . . . . .
N1 N 0.7144(4) 0.4692(3) 1.1008(3) 0.0294(9) Uani 1 1 d . . . . .
N2 N 1.0013(5) 0.5131(3) 1.1471(3) 0.0338(10) Uani 1 1 d . . . . .
N3 N 0.9605(5) 0.7235(3) 1.0315(3) 0.0318(10) Uani 1 1 d . . . . .
N4 N 0.6867(4) 0.6384(3) 0.9898(3) 0.0299(9) Uani 1 1 d . . . . .
N5 N 0.4643(4) 0.9342(3) 0.6132(3) 0.0295(9) Uani 1 1 d . . . . .
N6 N 0.2569(4) 0.9510(3) 0.4952(3) 0.0307(9) Uani 1 1 d . . . . .
O1 O 0.6835(4) 0.2053(3) 0.8802(3) 0.0504(11) Uani 1 1 d . . . . .
O2 O 0.6550(4) 0.3880(2) 0.8767(3) 0.0401(9) Uani 1 1 d . . . . .
O3 O -0.1343(3) 0.0296(2) 0.6940(2) 0.0344(8) Uani 1 1 d . . . . .
O4 O 0.0295(4) -0.0062(3) 0.8254(3) 0.0431(9) Uani 1 1 d . . . . .
O5 O 0.7944(4) 0.7619(3) 0.6202(3) 0.0607(12) Uani 1 1 d . . . . .
O6 O 0.5868(5) 0.7445(3) 0.7210(3) 0.0499(10) Uani 1 1 d . . . . .
O7 O 0.6141(4) 0.9797(3) 0.8444(2) 0.0376(8) Uani 1 1 d . . . . .
H1W H 0.4996 0.9660 0.8498 0.056 Uiso 1 1 d R U . . .
H2W H 0.6311 1.0540 0.8510 0.056 Uiso 1 1 d R U . . .
C1 C 0.6046(5) 0.2830(4) 0.8506(4) 0.0304(11) Uani 1 1 d . . . . .
C2 C 0.4354(5) 0.2524(3) 0.7801(4) 0.0279(11) Uani 1 1 d . . . . .
C3 C 0.3056(5) 0.1678(3) 0.7983(3) 0.0258(10) Uani 1 1 d . . . . .
H3 H 0.3286 0.1265 0.8497 0.031 Uiso 1 1 calc R U . . .
C4 C 0.1428(5) 0.1443(4) 0.7406(4) 0.0306(11) Uani 1 1 d . . . . .
C5 C 0.0065(5) 0.0489(4) 0.7583(4) 0.0288(11) Uani 1 1 d . . . . .
C6 C 0.1081(6) 0.2087(4) 0.6682(4) 0.0508(16) Uani 1 1 d . . . . .
H6 H -0.0045 0.1979 0.6329 0.061 Uiso 1 1 calc R U . . .
C7 C 0.2374(6) 0.2897(4) 0.6467(5) 0.0564(17) Uani 1 1 d . . . . .
H7 H 0.2129 0.3303 0.5950 0.068 Uiso 1 1 calc R U . . .
C8 C 0.4043(5) 0.3113(4) 0.7013(4) 0.0340(12) Uani 1 1 d . . . . .
C9 C 0.5441(6) 0.3874(4) 0.6637(4) 0.0353(12) Uani 1 1 d . . . . .
C10 C 0.5538(6) 0.5053(4) 0.6814(4) 0.0348(12) Uani 1 1 d . . . . .
H10 H 0.4781 0.5402 0.7242 0.042 Uiso 1 1 calc R U . . .
C11 C 0.6755(6) 0.5728(4) 0.6360(4) 0.0331(11) Uani 1 1 d . . . . .
C12 C 0.6875(6) 0.7014(4) 0.6598(4) 0.0386(13) Uani 1 1 d . . . . .
C13 C 0.7883(6) 0.5219(4) 0.5741(5) 0.0511(15) Uani 1 1 d . . . . .
H13 H 0.8707 0.5663 0.5443 0.061 Uiso 1 1 calc R U . . .
C14 C 0.7795(8) 0.4046(5) 0.5560(6) 0.080(2) Uani 1 1 d . . . . .
H14 H 0.8561 0.3698 0.5137 0.096 Uiso 1 1 calc R U . . .
C15 C 0.6588(7) 0.3387(4) 0.5997(6) 0.068(2) Uani 1 1 d . . . . .
H15 H 0.6539 0.2595 0.5860 0.081 Uiso 1 1 calc R U . . .
C16 C 0.7703(5) 0.3899(4) 1.1550(4) 0.0352(12) Uani 1 1 d . . . . .
H16 H 0.6981 0.3275 1.1694 0.042 Uiso 1 1 calc R U . . .
C17 C 0.9471(6) 0.4161(4) 1.1846(4) 0.0389(13) Uani 1 1 d . . . . .
H17 H 1.0179 0.3761 1.2229 0.047 Uiso 1 1 calc R U . . .
C18 C 0.8580(5) 0.5428(4) 1.0960(3) 0.0269(10) Uani 1 1 d . . . . .
C19 C 0.8423(5) 0.6345(4) 1.0414(3) 0.0267(10) Uani 1 1 d . . . . .
C20 C 0.8760(6) 0.7883(4) 0.9724(4) 0.0386(12) Uani 1 1 d . . . . .
H20 H 0.9246 0.8560 0.9535 0.046 Uiso 1 1 calc R U . . .
O8 O 0.3120(5) 0.9096(4) 0.9165(3) 0.0705(13) Uani 1 1 d G . . . .
H3W H 0.3013 0.9007 0.9765 0.106 Uiso 1 1 d G U . . .
H4W H 0.2215 0.9387 0.8943 0.106 Uiso 1 1 d G U . . .
C21 C 0.7083(6) 0.7355(4) 0.9464(4) 0.0358(12) Uani 1 1 d . . . . .
H21 H 0.6211 0.7607 0.9056 0.043 Uiso 1 1 calc R U . . .
C22 C 0.2990(5) 0.8874(4) 0.6352(4) 0.0363(12) Uani 1 1 d . . . . .
H22 H 0.2777 0.8545 0.6915 0.044 Uiso 1 1 calc R U . . .
C23 C 0.1742(5) 0.8971(4) 0.5621(4) 0.0317(11) Uani 1 1 d . . . . .
H23 H 0.0527 0.8713 0.5585 0.038 Uiso 1 1 calc R U . . .
C24 C 0.4345(5) 0.9722(4) 0.5277(4) 0.0278(11) Uani 1 1 d . . . . .
H1 H 1.103(7) 0.541(4) 1.146(4) 0.060(18) Uiso 1 1 d . . . . .
H2 H 1.072(6) 0.735(4) 1.059(4) 0.039(14) Uiso 1 1 d . . . . .
H4 H 0.212(7) 0.962(5) 0.428(5) 0.077(19) Uiso 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
Zn1 N4 2.083(3) . ?
Zn1 N4 2.083(3) 2_667 ?
Zn1 N1 2.136(3) . ?
Zn1 N1 2.136(3) 2_667 ?
Zn1 O2 2.432(3) . ?
Zn1 O2 2.432(3) 2_667 ?
Zn2 O3 1.958(3) 1_665 ?
Zn2 O7 2.009(3) . ?
Zn2 O6 2.044(3) . ?
Zn2 N5 2.071(3) . ?
Zn2 O5 2.286(4) . ?
N1 C18 1.333(5) . ?
N1 C16 1.362(5) . ?
N2 C18 1.345(5) . ?
N2 C17 1.368(6) . ?
N2 H1 0.80(5) . ?
N3 C19 1.342(5) . ?
N3 C20 1.363(6) . ?
N3 H2 0.88(4) . ?
N4 C19 1.329(5) . ?
N4 C21 1.375(5) . ?
N5 C24 1.324(6) . ?
N5 C22 1.384(5) . ?
N6 C23 1.347(6) . ?
N6 C24 1.363(5) . ?
N6 H4 0.99(6) . ?
O1 C1 1.247(5) . ?
O2 C1 1.260(5) . ?
O3 C5 1.303(5) . ?
O3 Zn2 1.958(3) 1_445 ?
O4 C5 1.215(5) . ?
O5 C12 1.234(6) . ?
O6 C12 1.259(6) . ?
O7 H1W 0.8714 . ?
O7 H2W 0.8708 . ?
C1 C2 1.516(6) . ?
C2 C8 1.386(6) . ?
C2 C3 1.393(6) . ?
C3 C4 1.386(5) . ?
C3 H3 0.9300 . ?
C4 C6 1.363(7) . ?
C4 C5 1.512(6) . ?
C6 C7 1.379(6) . ?
C6 H6 0.9300 . ?
C7 C8 1.392(6) . ?
C7 H7 0.9300 . ?
C8 C9 1.490(6) . ?
C9 C10 1.381(6) . ?
C9 C15 1.382(7) . ?
C10 C11 1.398(6) . ?
C10 H10 0.9300 . ?
C11 C13 1.366(7) . ?
C11 C12 1.508(6) . ?
C13 C14 1.375(7) . ?
C13 H13 0.9300 . ?
C14 C15 1.368(8) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C17 1.352(6) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
C18 C19 1.420(6) . ?
C20 C21 1.350(6) . ?
C20 H20 0.9300 . ?
O8 H3W 0.8501 . ?
O8 H4W 0.8500 . ?
C21 H21 0.9300 . ?
C22 C23 1.344(6) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 C24 1.454(9) 2_676 ?

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
N4 Zn1 N4 180.0 . 2_667 ?
N4 Zn1 N1 79.84(13) . . ?
N4 Zn1 N1 100.16(13) 2_667 . ?
N4 Zn1 N1 100.16(13) . 2_667 ?
N4 Zn1 N1 79.84(13) 2_667 2_667 ?
N1 Zn1 N1 180.0 . 2_667 ?
N4 Zn1 O2 87.24(12) . . ?
N4 Zn1 O2 92.76(12) 2_667 . ?
N1 Zn1 O2 83.66(13) . . ?
N1 Zn1 O2 96.34(13) 2_667 . ?
N4 Zn1 O2 92.75(12) . 2_667 ?
N4 Zn1 O2 87.24(12) 2_667 2_667 ?
N1 Zn1 O2 96.34(13) . 2_667 ?
N1 Zn1 O2 83.66(13) 2_667 2_667 ?
O2 Zn1 O2 180.0 . 2_667 ?
O3 Zn2 O7 97.33(13) 1_665 . ?
O3 Zn2 O6 152.30(14) 1_665 . ?
O7 Zn2 O6 96.60(14) . . ?
O3 Zn2 N5 103.86(13) 1_665 . ?
O7 Zn2 N5 104.29(14) . . ?
O6 Zn2 N5 95.71(14) . . ?
O3 Zn2 O5 96.52(13) 1_665 . ?
O7 Zn2 O5 146.60(14) . . ?
O6 Zn2 O5 59.95(14) . . ?
N5 Zn2 O5 101.64(15) . . ?
C18 N1 C16 106.5(3) . . ?
C18 N1 Zn1 109.4(3) . . ?
C16 N1 Zn1 142.6(3) . . ?
C18 N2 C17 107.8(4) . . ?
C18 N2 H1 124(4) . . ?
C17 N2 H1 127(4) . . ?
C19 N3 C20 107.4(3) . . ?
C19 N3 H2 124(3) . . ?
C20 N3 H2 128(3) . . ?
C19 N4 C21 105.8(3) . . ?
C19 N4 Zn1 112.3(3) . . ?
C21 N4 Zn1 141.9(3) . . ?
C24 N5 C22 105.8(3) . . ?
C24 N5 Zn2 139.8(3) . . ?
C22 N5 Zn2 114.0(3) . . ?
C23 N6 C24 107.4(4) . . ?
C23 N6 H4 130(3) . . ?
C24 N6 H4 122(3) . . ?
C1 O2 Zn1 119.8(3) . . ?
C5 O3 Zn2 118.1(3) . 1_445 ?
C12 O5 Zn2 84.2(3) . . ?
C12 O6 Zn2 94.6(3) . . ?
Zn2 O7 H1W 111.0 . . ?
Zn2 O7 H2W 110.3 . . ?
H1W O7 H2W 103.1 . . ?
O1 C1 O2 124.0(4) . . ?
O1 C1 C2 119.5(4) . . ?
O2 C1 C2 116.4(4) . . ?
C8 C2 C3 119.8(4) . . ?
C8 C2 C1 120.9(4) . . ?
C3 C2 C1 119.2(4) . . ?
C4 C3 C2 120.8(4) . . ?
C4 C3 H3 119.6 . . ?
C2 C3 H3 119.6 . . ?
C6 C4 C3 118.9(4) . . ?
C6 C4 C5 120.8(4) . . ?
C3 C4 C5 120.2(4) . . ?
O4 C5 O3 123.4(4) . . ?
O4 C5 C4 122.5(4) . . ?
O3 C5 C4 114.1(4) . . ?
C4 C6 C7 120.9(4) . . ?
C4 C6 H6 119.5 . . ?
C7 C6 H6 119.5 . . ?
C6 C7 C8 120.8(5) . . ?
C6 C7 H7 119.6 . . ?
C8 C7 H7 119.6 . . ?
C2 C8 C7 118.5(4) . . ?
C2 C8 C9 124.3(4) . . ?
C7 C8 C9 116.9(5) . . ?
C10 C9 C15 117.7(5) . . ?
C10 C9 C8 123.2(4) . . ?
C15 C9 C8 118.8(4) . . ?
C9 C10 C11 121.1(5) . . ?
C9 C10 H10 119.5 . . ?
C11 C10 H10 119.5 . . ?
C13 C11 C10 119.6(4) . . ?
C13 C11 C12 120.5(4) . . ?
C10 C11 C12 119.8(5) . . ?
O5 C12 O6 121.3(5) . . ?
O5 C12 C11 120.4(5) . . ?
O6 C12 C11 118.3(5) . . ?
C11 C13 C14 119.7(5) . . ?
C11 C13 H13 120.2 . . ?
C14 C13 H13 120.2 . . ?
C15 C14 C13 120.5(6) . . ?
C15 C14 H14 119.7 . . ?
C13 C14 H14 119.7 . . ?
C14 C15 C9 121.4(5) . . ?
C14 C15 H15 119.3 . . ?
C9 C15 H15 119.3 . . ?
C17 C16 N1 109.5(4) . . ?
C17 C16 H16 125.3 . . ?
N1 C16 H16 125.3 . . ?
C16 C17 N2 106.3(4) . . ?
C16 C17 H17 126.8 . . ?
N2 C17 H17 126.8 . . ?
N1 C18 N2 109.8(4) . . ?
N1 C18 C19 119.6(3) . . ?
N2 C18 C19 130.5(4) . . ?
N4 C19 N3 110.7(4) . . ?
N4 C19 C18 118.2(4) . . ?
N3 C19 C18 131.1(4) . . ?
C21 C20 N3 106.8(4) . . ?
C21 C20 H20 126.6 . . ?
N3 C20 H20 126.6 . . ?
H3W O8 H4W 109.5 . . ?
C20 C21 N4 109.2(4) . . ?
C20 C21 H21 125.4 . . ?
N4 C21 H21 125.4 . . ?
C23 C22 N5 109.0(4) . . ?
C23 C22 H22 125.5 . . ?
N5 C22 H22 125.5 . . ?
N6 C23 C22 107.7(4) . . ?
N6 C23 H23 126.2 . . ?
C22 C23 H23 126.2 . . ?
N5 C24 N6 110.1(4) . . ?
N5 C24 C24 127.4(5) . 2_676 ?
N6 C24 C24 122.4(5) . 2_676 ?

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
Zn1 O2 C1 O1 -102.6(5) . . . . ?
Zn1 O2 C1 C2 76.3(5) . . . . ?
O1 C1 C2 C8 -139.5(5) . . . . ?
O2 C1 C2 C8 41.6(6) . . . . ?
O1 C1 C2 C3 43.8(6) . . . . ?
O2 C1 C2 C3 -135.1(4) . . . . ?
C8 C2 C3 C4 -2.3(7) . . . . ?
C1 C2 C3 C4 174.4(4) . . . . ?
C2 C3 C4 C6 -2.8(7) . . . . ?
C2 C3 C4 C5 177.4(4) . . . . ?
Zn2 O3 C5 O4 2.8(6) 1_445 . . . ?
Zn2 O3 C5 C4 -178.9(3) 1_445 . . . ?
C6 C4 C5 O4 -176.2(5) . . . . ?
C3 C4 C5 O4 3.7(7) . . . . ?
C6 C4 C5 O3 5.5(7) . . . . ?
C3 C4 C5 O3 -174.6(4) . . . . ?
C3 C4 C6 C7 5.3(9) . . . . ?
C5 C4 C6 C7 -174.8(5) . . . . ?
C4 C6 C7 C8 -2.9(9) . . . . ?
C3 C2 C8 C7 4.7(7) . . . . ?
C1 C2 C8 C7 -172.0(4) . . . . ?
C3 C2 C8 C9 -168.3(4) . . . . ?
C1 C2 C8 C9 15.0(7) . . . . ?
C6 C7 C8 C2 -2.2(9) . . . . ?
C6 C7 C8 C9 171.4(5) . . . . ?
C2 C8 C9 C10 -105.4(6) . . . . ?
C7 C8 C9 C10 81.5(7) . . . . ?
C2 C8 C9 C15 81.4(7) . . . . ?
C7 C8 C9 C15 -91.7(6) . . . . ?
C15 C9 C10 C11 0.0(7) . . . . ?
C8 C9 C10 C11 -173.3(4) . . . . ?
C9 C10 C11 C13 -0.8(7) . . . . ?
C9 C10 C11 C12 -177.8(4) . . . . ?
Zn2 O5 C12 O6 -1.2(5) . . . . ?
Zn2 O5 C12 C11 179.3(4) . . . . ?
Zn2 O6 C12 O5 1.3(5) . . . . ?
Zn2 O6 C12 C11 -179.1(3) . . . . ?
C13 C11 C12 O5 3.0(7) . . . . ?
C10 C11 C12 O5 180.0(4) . . . . ?
C13 C11 C12 O6 -176.6(5) . . . . ?
C10 C11 C12 O6 0.4(7) . . . . ?
C10 C11 C13 C14 0.8(8) . . . . ?
C12 C11 C13 C14 177.8(5) . . . . ?
C11 C13 C14 C15 -0.1(10) . . . . ?
C13 C14 C15 C9 -0.7(11) . . . . ?
C10 C9 C15 C14 0.7(10) . . . . ?
C8 C9 C15 C14 174.3(6) . . . . ?
C18 N1 C16 C17 1.0(6) . . . . ?
Zn1 N1 C16 C17 164.3(4) . . . . ?
N1 C16 C17 N2 -0.5(6) . . . . ?
C18 N2 C17 C16 -0.2(6) . . . . ?
C16 N1 C18 N2 -1.1(5) . . . . ?
Zn1 N1 C18 N2 -170.5(3) . . . . ?
C16 N1 C18 C19 178.4(4) . . . . ?
Zn1 N1 C18 C19 9.0(5) . . . . ?
C17 N2 C18 N1 0.8(5) . . . . ?
C17 N2 C18 C19 -178.6(5) . . . . ?
C21 N4 C19 N3 -0.7(5) . . . . ?
Zn1 N4 C19 N3 178.6(3) . . . . ?
C21 N4 C19 C18 179.1(4) . . . . ?
Zn1 N4 C19 C18 -1.6(5) . . . . ?
C20 N3 C19 N4 1.1(5) . . . . ?
C20 N3 C19 C18 -178.6(5) . . . . ?
N1 C18 C19 N4 -5.4(7) . . . . ?
N2 C18 C19 N4 174.0(5) . . . . ?
N1 C18 C19 N3 174.3(5) . . . . ?
N2 C18 C19 N3 -6.3(9) . . . . ?
C19 N3 C20 C21 -1.0(6) . . . . ?
N3 C20 C21 N4 0.6(6) . . . . ?
C19 N4 C21 C20 0.0(6) . . . . ?
Zn1 N4 C21 C20 -179.0(4) . . . . ?
C24 N5 C22 C23 0.7(5) . . . . ?
Zn2 N5 C22 C23 -173.3(3) . . . . ?
C24 N6 C23 C22 1.0(5) . . . . ?
N5 C22 C23 N6 -1.1(5) . . . . ?
C22 N5 C24 N6 0.0(5) . . . . ?
Zn2 N5 C24 N6 171.5(3) . . . . ?
C22 N5 C24 C24 -179.4(6) . . . 2_676 ?
Zn2 N5 C24 C24 -7.9(9) . . . 2_676 ?
C23 N6 C24 N5 -0.6(5) . . . . ?
C23 N6 C24 C24 178.8(5) . . . 2_676 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N6 H4 O3 0.99(6) 1.74(6) 2.728(5) 175(5) 2_566
N3 H2 O1 0.88(4) 1.98(4) 2.846(4) 169(4) 2_767
N2 H1 O2 0.80(5) 2.00(5) 2.795(5) 172(6) 2_767
C23 H23 O5 0.93 2.50 3.344(5) 151.1 1_455
C21 H21 O6 0.93 2.49 3.165(6) 129.5 .
O8 H4W O4 0.85 1.89 2.733(5) 171.1 1_565
O8 H3W O7 0.85 2.64 3.320(6) 137.8 2_677
O8 H3W O1 0.85 2.48 3.270(6) 154.7 2_667
O7 H2W O1 0.87 1.78 2.647(4) 172.1 1_565
O7 H1W O8 0.87 1.86 2.652(5) 150.3 .

_refine_diff_density_max         0.408
_refine_diff_density_min         -0.464
_refine_diff_density_rms         0.085

####################################################################### 
# 
# 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_435-16Cd
_database_code_depnum_ccdc_archive 'CCDC 2012744'
_audit_update_record             
;
2020-06-28 deposited with the CCDC.	2021-01-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C50 H40 Cd2 N4 O16'
_chemical_formula_weight         1177.66

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'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      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                   7.8254(6)
_cell_length_b                   8.9550(7)
_cell_length_c                   17.9632(17)
_cell_angle_alpha                94.442(7)
_cell_angle_beta                 98.969(7)
_cell_angle_gamma                109.430(7)
_cell_volume                     1161.24(18)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6951
_cell_measurement_theta_min      3.478
_cell_measurement_theta_max      25.048

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.684
_exptl_crystal_F_000             592
_exptl_transmission_factor_min   0.803
_exptl_transmission_factor_max   0.828
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    0.995
_shelx_estimated_absorpt_T_min   0.811
_shelx_estimated_absorpt_T_max   0.833
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.811
_exptl_absorpt_correction_T_max  0.833
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APE-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6951
_diffrn_reflns_av_unetI/netI     0.0842
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.478
_diffrn_reflns_theta_max         25.049
_diffrn_reflns_theta_full        25.049
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             4103
_reflns_number_gt                3224
_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    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0146P)²+2.6548P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4103
_refine_ls_number_parameters     325
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.0737
_refine_ls_R_factor_gt           0.0535
_refine_ls_wR_factor_ref         0.1053
_refine_ls_wR_factor_gt          0.0912
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.000
_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
Cd1 Cd 0.35732(6) 0.31685(5) 0.09000(2) 0.03636(15) Uani 1 1 d . . . . .
N1 N 0.5016(6) 0.5656(5) 0.1637(3) 0.0343(11) Uani 1 1 d . . . . .
N2 N 0.7336(15) 1.2757(14) 0.4148(7) 0.127(4) Uani 1 1 d . U . . .
O1 O 0.3844(6) 0.1653(5) 0.1912(2) 0.0422(10) Uani 1 1 d . . . . .
O2 O 0.1545(5) 0.2549(4) 0.1745(2) 0.0415(10) Uani 1 1 d . . . . .
O3 O 0.2885(9) 0.5431(8) 0.4499(3) 0.1046(18) Uani 1 1 d . U . . .
H1 H 0.2982 0.6121 0.4847 0.157 Uiso 1 1 calc R U . . .
O4 O 0.2010(8) 0.3902(8) 0.5359(4) 0.1040(18) Uani 1 1 d . U . . .
O5 O -0.2199(5) -0.4297(4) 0.0052(2) 0.0421(10) Uani 1 1 d . . . . .
O6 O -0.1654(5) -0.1720(4) 0.0245(2) 0.0407(10) Uani 1 1 d . . . . .
O7 O 0.6002(5) 0.2910(5) 0.0502(2) 0.0479(11) Uani 1 1 d . . . . .
H1W H 0.6565 0.3795 0.0360 0.058 Uiso 1 1 d R U . . .
H2W H 0.6647 0.2335 0.0623 0.058 Uiso 1 1 d R U . . .
O8 O 0.7994(6) 0.1151(5) 0.0874(3) 0.0716(16) Uani 1 1 d . . . . .
H3W H 0.9075 0.1582 0.1141 0.086 Uiso 1 1 d R U . . .
H4W H 0.8090 0.0289 0.0684 0.086 Uiso 1 1 d R U . . .
C1 C 0.2524(8) 0.1884(6) 0.2129(3) 0.0303(13) Uani 1 1 d . . . . .
C2 C 0.2101(7) 0.1540(6) 0.2902(3) 0.0296(13) Uani 1 1 d . . . . .
C3 C 0.2422(8) 0.2851(7) 0.3436(4) 0.0424(16) Uani 1 1 d . . . . .
H3 H 0.2852 0.3872 0.3299 0.051 Uiso 1 1 calc R U . . .
C4 C 0.2121(9) 0.2683(9) 0.4164(4) 0.0492(18) Uani 1 1 d . . . . .
C5 C 0.2352(14) 0.4061(13) 0.4720(6) 0.0986(19) Uani 1 1 d . U . . .
C6 C 0.1505(9) 0.1168(9) 0.4360(4) 0.0543(19) Uani 1 1 d . . . . .
H6 H 0.1322 0.1039 0.4854 0.065 Uiso 1 1 calc R U . . .
C7 C 0.1152(8) -0.0170(8) 0.3838(3) 0.0406(15) Uani 1 1 d . . . . .
H7 H 0.0723 -0.1182 0.3985 0.049 Uiso 1 1 calc R U . . .
C8 C 0.1434(7) -0.0022(6) 0.3091(3) 0.0300(13) Uani 1 1 d . . . . .
C9 C 0.0957(7) -0.1465(6) 0.2527(3) 0.0254(12) Uani 1 1 d . . . . .
C10 C 0.0061(7) -0.1538(6) 0.1784(3) 0.0243(11) Uani 1 1 d . . . . .
H10 H -0.0235 -0.0664 0.1642 0.029 Uiso 1 1 calc R U . . .
C11 C -0.0401(7) -0.2883(6) 0.1251(3) 0.0250(12) Uani 1 1 d . . . . .
C12 C -0.1453(7) -0.2963(7) 0.0473(3) 0.0314(13) Uani 1 1 d . . . . .
C13 C 0.0049(8) -0.4181(7) 0.1463(3) 0.0376(14) Uani 1 1 d . . . . .
H13 H -0.0229 -0.5083 0.1109 0.045 Uiso 1 1 calc R U . . .
C14 C 0.0908(8) -0.4134(7) 0.2199(4) 0.0393(15) Uani 1 1 d . . . . .
H14 H 0.1197 -0.5012 0.2340 0.047 Uiso 1 1 calc R U . . .
C15 C 0.1347(7) -0.2796(6) 0.2731(3) 0.0327(13) Uani 1 1 d . . . . .
H15 H 0.1905 -0.2790 0.3229 0.039 Uiso 1 1 calc R U . . .
C16 C 0.5769(8) 0.5744(7) 0.2366(3) 0.0372(14) Uani 1 1 d . . . . .
H16 H 0.5943 0.4839 0.2533 0.045 Uiso 1 1 calc R U . . .
C17 C 0.6300(8) 0.7106(7) 0.2879(3) 0.0372(14) Uani 1 1 d . . . . .
H17 H 0.6794 0.7107 0.3385 0.045 Uiso 1 1 calc R U . . .
C18 C 0.6094(7) 0.8487(6) 0.2639(3) 0.0320(13) Uani 1 1 d . . . . .
C19 C 0.5362(7) 0.8403(7) 0.1880(3) 0.0351(14) Uani 1 1 d . . . . .
H19 H 0.5228 0.9304 0.1691 0.042 Uiso 1 1 calc R U . . .
C20 C 0.4833(8) 0.6989(7) 0.1406(3) 0.0390(14) Uani 1 1 d . . . . .
H20 H 0.4321 0.6954 0.0899 0.047 Uiso 1 1 calc R U . . .
C21 C 0.6591(8) 0.9979(8) 0.3172(4) 0.0480(18) Uani 1 1 d . . . . .
C22 C 0.6187(9) 0.9917(10) 0.3898(4) 0.071(2) Uani 1 1 d . . . . .
H22 H 0.5663 0.8942 0.4067 0.085 Uiso 1 1 calc R U . . .
C23 C 0.6589(14) 1.1365(16) 0.4370(6) 0.116(5) Uani 1 1 d . . . . .
H23 H 0.6317 1.1335 0.4856 0.140 Uiso 1 1 calc R U . . .
C24 C 0.7772(13) 1.2835(11) 0.3480(8) 0.112(5) Uani 1 1 d . . . . .
H24 H 0.8351 1.3833 0.3343 0.134 Uiso 1 1 calc R U . . .
C25 C 0.7398(9) 1.1465(8) 0.2960(5) 0.070(2) Uani 1 1 d . . . . .
H25 H 0.7688 1.1555 0.2478 0.084 Uiso 1 1 calc R U . . .


_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
Cd1 O7 2.206(4) . ?
Cd1 N1 2.322(4) . ?
Cd1 O2 2.329(4) . ?
Cd1 O6 2.344(4) 2 ?
Cd1 O5 2.349(4) 2 ?
Cd1 O1 2.376(4) . ?
Cd1 C12 2.705(6) 2 ?
N1 C16 1.335(7) . ?
N1 C20 1.338(7) . ?
N2 C24 1.298(15) . ?
N2 C23 1.312(15) . ?
O1 C1 1.232(6) . ?
O2 C1 1.273(6) . ?
O3 C5 1.274(12) . ?
O3 H1 0.8200 . ?
O4 C5 1.227(12) . ?
O5 C12 1.264(6) . ?
O5 Cd1 2.349(4) 2 ?
O6 C12 1.265(6) . ?
O6 Cd1 2.344(4) 2 ?
O7 H1W 0.8499 . ?
O7 H2W 0.8500 . ?
O8 H3W 0.8500 . ?
O8 H4W 0.8500 . ?
C1 C2 1.508(7) . ?
C2 C3 1.385(7) . ?
C2 C8 1.410(7) . ?
C3 C4 1.375(9) . ?
C3 H3 0.9300 . ?
C4 C6 1.374(9) . ?
C4 C5 1.469(9) . ?
C6 C7 1.384(8) . ?
C6 H6 0.9300 . ?
C7 C8 1.404(7) . ?
C7 H7 0.9300 . ?
C8 C9 1.481(7) . ?
C9 C15 1.387(7) . ?
C9 C10 1.394(7) . ?
C10 C11 1.386(7) . ?
C10 H10 0.9300 . ?
C11 C13 1.385(7) . ?
C11 C12 1.492(7) . ?
C12 Cd1 2.705(6) 2 ?
C13 C14 1.377(8) . ?
C13 H13 0.9300 . ?
C14 C15 1.383(7) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C17 1.371(7) . ?
C16 H16 0.9300 . ?
C17 C18 1.390(7) . ?
C17 H17 0.9300 . ?
C18 C19 1.381(8) . ?
C18 C21 1.480(7) . ?
C19 C20 1.369(7) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
C21 C25 1.382(10) . ?
C21 C22 1.390(10) . ?
C22 C23 1.405(11) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 C25 1.401(11) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?

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
O7 Cd1 N1 98.50(15) . . ?
O7 Cd1 O2 148.35(14) . . ?
N1 Cd1 O2 87.67(15) . . ?
O7 Cd1 O6 90.50(15) . 2 ?
N1 Cd1 O6 146.65(15) . 2 ?
O2 Cd1 O6 101.29(14) . 2 ?
O7 Cd1 O5 105.26(15) . 2 ?
N1 Cd1 O5 90.99(14) . 2 ?
O2 Cd1 O5 105.65(14) . 2 ?
O6 Cd1 O5 55.68(12) 2 2 ?
O7 Cd1 O1 92.91(14) . . ?
N1 Cd1 O1 95.86(16) . . ?
O2 Cd1 O1 55.49(13) . . ?
O6 Cd1 O1 115.78(14) 2 . ?
O5 Cd1 O1 159.43(14) 2 . ?
O7 Cd1 C12 98.36(16) . 2 ?
N1 Cd1 C12 118.81(17) . 2 ?
O2 Cd1 C12 105.77(15) . 2 ?
O6 Cd1 C12 27.85(14) 2 2 ?
O5 Cd1 C12 27.84(13) 2 2 ?
O1 Cd1 C12 141.10(16) . 2 ?
C16 N1 C20 117.1(5) . . ?
C16 N1 Cd1 119.4(4) . . ?
C20 N1 Cd1 122.3(4) . . ?
C24 N2 C23 120.3(11) . . ?
C1 O1 Cd1 90.4(3) . . ?
C1 O2 Cd1 91.5(3) . . ?
C5 O3 H1 109.5 . . ?
C12 O5 Cd1 91.9(3) . 2 ?
C12 O6 Cd1 92.2(3) . 2 ?
Cd1 O7 H1W 106.5 . . ?
Cd1 O7 H2W 131.9 . . ?
H1W O7 H2W 116.1 . . ?
H3W O8 H4W 98.9 . . ?
O1 C1 O2 122.0(5) . . ?
O1 C1 C2 121.4(5) . . ?
O2 C1 C2 116.4(5) . . ?
C3 C2 C8 120.5(5) . . ?
C3 C2 C1 116.6(5) . . ?
C8 C2 C1 122.9(5) . . ?
C4 C3 C2 121.6(6) . . ?
C4 C3 H3 119.2 . . ?
C2 C3 H3 119.2 . . ?
C6 C4 C3 118.5(6) . . ?
C6 C4 C5 119.5(8) . . ?
C3 C4 C5 122.0(8) . . ?
O4 C5 O3 121.6(8) . . ?
O4 C5 C4 121.9(11) . . ?
O3 C5 C4 116.5(9) . . ?
C4 C6 C7 121.4(6) . . ?
C4 C6 H6 119.3 . . ?
C7 C6 H6 119.3 . . ?
C6 C7 C8 120.9(6) . . ?
C6 C7 H7 119.5 . . ?
C8 C7 H7 119.5 . . ?
C7 C8 C2 117.1(5) . . ?
C7 C8 C9 120.4(5) . . ?
C2 C8 C9 122.5(5) . . ?
C15 C9 C10 118.2(5) . . ?
C15 C9 C8 120.7(5) . . ?
C10 C9 C8 121.0(5) . . ?
C11 C10 C9 121.6(5) . . ?
C11 C10 H10 119.2 . . ?
C9 C10 H10 119.2 . . ?
C13 C11 C10 119.1(5) . . ?
C13 C11 C12 120.4(5) . . ?
C10 C11 C12 120.4(5) . . ?
O6 C12 O5 120.2(5) . . ?
O6 C12 C11 120.4(5) . . ?
O5 C12 C11 119.4(5) . . ?
O6 C12 Cd1 60.0(3) . 2 ?
O5 C12 Cd1 60.2(3) . 2 ?
C11 C12 Cd1 176.1(4) . 2 ?
C14 C13 C11 119.9(5) . . ?
C14 C13 H13 120.0 . . ?
C11 C13 H13 120.0 . . ?
C13 C14 C15 120.8(5) . . ?
C13 C14 H14 119.6 . . ?
C15 C14 H14 119.6 . . ?
C14 C15 C9 120.3(5) . . ?
C14 C15 H15 119.8 . . ?
C9 C15 H15 119.8 . . ?
N1 C16 C17 123.1(5) . . ?
N1 C16 H16 118.4 . . ?
C17 C16 H16 118.4 . . ?
C16 C17 C18 119.6(5) . . ?
C16 C17 H17 120.2 . . ?
C18 C17 H17 120.2 . . ?
C19 C18 C17 117.1(5) . . ?
C19 C18 C21 120.9(6) . . ?
C17 C18 C21 122.0(6) . . ?
C20 C19 C18 119.8(5) . . ?
C20 C19 H19 120.1 . . ?
C18 C19 H19 120.1 . . ?
N1 C20 C19 123.3(6) . . ?
N1 C20 H20 118.4 . . ?
C19 C20 H20 118.4 . . ?
C25 C21 C22 118.0(7) . . ?
C25 C21 C18 121.7(7) . . ?
C22 C21 C18 120.2(7) . . ?
C21 C22 C23 118.3(9) . . ?
C21 C22 H22 120.8 . . ?
C23 C22 H22 120.8 . . ?
N2 C23 C22 122.1(11) . . ?
N2 C23 H23 118.9 . . ?
C22 C23 H23 118.9 . . ?
N2 C24 C25 122.2(11) . . ?
N2 C24 H24 118.9 . . ?
C25 C24 H24 118.9 . . ?
C21 C25 C24 119.0(9) . . ?
C21 C25 H25 120.5 . . ?
C24 C25 H25 120.5 . . ?

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
Cd1 O1 C1 O2 7.8(5) . . . . ?
Cd1 O1 C1 C2 -166.1(4) . . . . ?
Cd1 O2 C1 O1 -8.0(5) . . . . ?
Cd1 O2 C1 C2 166.2(4) . . . . ?
O1 C1 C2 C3 109.5(6) . . . . ?
O2 C1 C2 C3 -64.7(7) . . . . ?
O1 C1 C2 C8 -69.7(7) . . . . ?
O2 C1 C2 C8 116.1(6) . . . . ?
C8 C2 C3 C4 0.6(8) . . . . ?
C1 C2 C3 C4 -178.7(5) . . . . ?
C2 C3 C4 C6 0.7(9) . . . . ?
C2 C3 C4 C5 -176.3(6) . . . . ?
C6 C4 C5 O4 0.0(13) . . . . ?
C3 C4 C5 O4 177.0(8) . . . . ?
C6 C4 C5 O3 -178.4(7) . . . . ?
C3 C4 C5 O3 -1.4(12) . . . . ?
C3 C4 C6 C7 -1.4(10) . . . . ?
C5 C4 C6 C7 175.7(6) . . . . ?
C4 C6 C7 C8 0.8(9) . . . . ?
C6 C7 C8 C2 0.5(8) . . . . ?
C6 C7 C8 C9 -176.7(5) . . . . ?
C3 C2 C8 C7 -1.2(8) . . . . ?
C1 C2 C8 C7 178.1(5) . . . . ?
C3 C2 C8 C9 176.0(5) . . . . ?
C1 C2 C8 C9 -4.7(8) . . . . ?
C7 C8 C9 C15 -41.0(7) . . . . ?
C2 C8 C9 C15 141.9(5) . . . . ?
C7 C8 C9 C10 137.2(5) . . . . ?
C2 C8 C9 C10 -39.9(7) . . . . ?
C15 C9 C10 C11 -1.5(7) . . . . ?
C8 C9 C10 C11 -179.7(5) . . . . ?
C9 C10 C11 C13 -0.3(8) . . . . ?
C9 C10 C11 C12 176.6(5) . . . . ?
Cd1 O6 C12 O5 1.9(5) 2 . . . ?
Cd1 O6 C12 C11 -175.5(4) 2 . . . ?
Cd1 O5 C12 O6 -1.9(5) 2 . . . ?
Cd1 O5 C12 C11 175.5(4) 2 . . . ?
C13 C11 C12 O6 -170.6(5) . . . . ?
C10 C11 C12 O6 12.4(8) . . . . ?
C13 C11 C12 O5 11.9(8) . . . . ?
C10 C11 C12 O5 -165.0(5) . . . . ?
C10 C11 C13 C14 1.4(8) . . . . ?
C12 C11 C13 C14 -175.6(5) . . . . ?
C11 C13 C14 C15 -0.6(9) . . . . ?
C13 C14 C15 C9 -1.2(9) . . . . ?
C10 C9 C15 C14 2.2(8) . . . . ?
C8 C9 C15 C14 -179.5(5) . . . . ?
C20 N1 C16 C17 1.9(8) . . . . ?
Cd1 N1 C16 C17 -166.0(4) . . . . ?
N1 C16 C17 C18 -1.5(9) . . . . ?
C16 C17 C18 C19 -0.4(8) . . . . ?
C16 C17 C18 C21 178.2(5) . . . . ?
C17 C18 C19 C20 1.6(8) . . . . ?
C21 C18 C19 C20 -177.0(5) . . . . ?
C16 N1 C20 C19 -0.6(8) . . . . ?
Cd1 N1 C20 C19 167.0(4) . . . . ?
C18 C19 C20 N1 -1.2(9) . . . . ?
C19 C18 C21 C25 -39.1(8) . . . . ?
C17 C18 C21 C25 142.4(6) . . . . ?
C19 C18 C21 C22 138.4(6) . . . . ?
C17 C18 C21 C22 -40.1(8) . . . . ?
C25 C21 C22 C23 1.1(10) . . . . ?
C18 C21 C22 C23 -176.5(6) . . . . ?
C24 N2 C23 C22 -1.7(18) . . . . ?
C21 C22 C23 N2 -0.4(14) . . . . ?
C23 N2 C24 C25 2.9(17) . . . . ?
C22 C21 C25 C24 0.0(10) . . . . ?
C18 C21 C25 C24 177.6(6) . . . . ?
N2 C24 C25 C21 -2.1(13) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C20 H20 O7 0.93 2.51 3.402(7) 161.7 2_665
C17 H17 O4 0.93 2.65 3.537(9) 160.7 2_666
O8 H4W O6 0.85 1.99 2.843(5) 179.3 1_655
O8 H3W O2 0.85 1.94 2.786(6) 179.4 1_655
O7 H2W O8 0.85 1.76 2.613(6) 179.7 .
O7 H1W O5 0.85 1.84 2.686(5) 179.4 1_665
O3 H1 N2 0.82 2.09 2.877(12) 161.6 2_676
C20 H20 O7 0.93 2.51 3.402(7) 161.7 2_665
C17 H17 O4 0.93 2.65 3.537(9) 160.7 2_666
O8 H4W O6 0.85 1.99 2.843(5) 179.3 1_655
O8 H3W O2 0.85 1.94 2.786(6) 179.4 1_655
O7 H2W O8 0.85 1.76 2.613(6) 179.7 .
O7 H1W O5 0.85 1.84 2.686(5) 179.4 1_665
O3 H1 N2 0.82 2.09 2.877(12) 161.6 2_676
O3 H1 N2 0.82 2.09 2.877(12) 161.6 2_676
O7 H1W O5 0.85 1.84 2.686(5) 179.4 1_665
O7 H2W O8 0.85 1.76 2.613(6) 179.7 .
O8 H3W O2 0.85 1.94 2.786(6) 179.4 1_655
O8 H4W O6 0.85 1.99 2.843(5) 179.3 1_655
C17 H17 O4 0.93 2.65 3.537(9) 160.7 2_666
C20 H20 O7 0.93 2.51 3.402(7) 161.7 2_665
O3 H1 N2 0.82 2.09 2.877(12) 161.6 2_676
O7 H1W O5 0.85 1.84 2.686(5) 179.4 1_665
O7 H2W O8 0.85 1.76 2.613(6) 179.7 .
O8 H3W O2 0.85 1.94 2.786(6) 179.4 1_655
O8 H4W O6 0.85 1.99 2.843(5) 179.3 1_655
C17 H17 O4 0.93 2.65 3.537(9) 160.7 2_666
C20 H20 O7 0.93 2.51 3.402(7) 161.7 2_665
O3 H1 N2 0.82 2.09 2.877(12) 161.6 2_676
O7 H1W O5 0.85 1.84 2.686(5) 179.4 1_665
O7 H2W O8 0.85 1.76 2.613(6) 179.7 .
O8 H3W O2 0.85 1.94 2.786(6) 179.4 1_655
O8 H4W O6 0.85 1.99 2.843(5) 179.3 1_655
C17 H17 O4 0.93 2.65 3.537(9) 160.7 2_666
C20 H20 O7 0.93 2.51 3.402(7) 161.7 2_665

_refine_diff_density_max         0.948
_refine_diff_density_min         -1.117
_refine_diff_density_rms         0.110


# start Validation Reply Form
_vrf_PLAT910_I                   
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min) 13 Note
RESPONSE: Reduction of beam stop mask did not yield significant improvement.
Most of those missing srtong reflections appeared to be very strong and were
treated as overflows.
;
# end Validation Reply Form

####################################################################### 
# 
# 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_430-18Zn
_database_code_depnum_ccdc_archive 'CCDC 2012743'
_audit_update_record             
;
2020-06-28 deposited with the CCDC.	2021-01-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C50 H40 N4 O16 Zn2'
_chemical_formula_weight         1083.60

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'
Zn Zn 0.2839 1.4301 '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                   7.8589(6)
_cell_length_b                   8.9034(7)
_cell_length_c                   17.5184(15)
_cell_angle_alpha                92.449(7)
_cell_angle_beta                 100.099(7)
_cell_angle_gamma                108.539(7)
_cell_volume                     1137.78(17)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7030
_cell_measurement_theta_min      3.364
_cell_measurement_theta_max      25.046

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_F_000             556
_exptl_transmission_factor_min   0.769
_exptl_transmission_factor_max   0.788
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.210
_exptl_absorpt_coefficient_mu    1.135
_shelx_estimated_absorpt_T_min   0.772
_shelx_estimated_absorpt_T_max   0.796
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.772
_exptl_absorpt_correction_T_max  0.796
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APE-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7030
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.364
_diffrn_reflns_theta_max         25.046
_diffrn_reflns_theta_full        25.046
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             4032
_reflns_number_gt                3339
_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    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0475P)²+3.9071P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4032
_refine_ls_number_parameters     325
_refine_ls_number_restraints     22
_refine_ls_R_factor_all          0.0737
_refine_ls_R_factor_gt           0.0607
_refine_ls_wR_factor_ref         0.1501
_refine_ls_wR_factor_gt          0.1395
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.000
_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
Zn1 Zn 0.36573(8) 0.33920(6) 0.09521(3) 0.0374(2) Uani 1 1 d . U . . .
N1 N 0.4819(5) 0.5670(4) 0.1595(2) 0.0359(9) Uani 1 1 d . . . . .
N2 N 0.7372(12) 1.2853(11) 0.4027(7) 0.121(3) Uani 1 1 d . U . . .
O1 O 0.3723(5) 0.1889(4) 0.1860(2) 0.0488(9) Uani 1 1 d . . . . .
O2 O 0.1400(5) 0.2756(4) 0.1667(2) 0.0481(8) Uani 1 1 d . U . . .
O3 O 0.1997(7) 0.3957(7) 0.5381(3) 0.1022(16) Uani 1 1 d . U . . .
H1 H 0.2204 0.4815 0.5634 0.153 Uiso 1 1 calc R U . . .
O4 O 0.2937(8) 0.5564(7) 0.4503(3) 0.1034(16) Uani 1 1 d . U . . .
O5 O -0.2325(5) -0.4097(4) 0.00019(18) 0.0394(8) Uani 1 1 d . . . . .
O6 O -0.1864(5) -0.1539(4) 0.01407(19) 0.0460(9) Uani 1 1 d . . . . .
O7 O 0.5958(5) 0.3288(4) 0.0660(2) 0.0497(9) Uani 1 1 d . . . . .
H1W H 0.6416 0.2563 0.0769 0.060 Uiso 1 1 d R U . . .
H2W H 0.6510 0.4143 0.0518 0.060 Uiso 1 1 d R U . . .
O8 O 0.7950(6) 0.1428(5) 0.0667(3) 0.0919(18) Uani 1 1 d . . . . .
H3W H 0.7622 0.0583 0.0344 0.110 Uiso 1 1 d R U . . .
H4W H 0.8991 0.1805 0.0970 0.110 Uiso 1 1 d R U . . .
C1 C 0.2381(7) 0.2093(5) 0.2074(3) 0.0362(11) Uani 1 1 d . . . . .
C2 C 0.2007(6) 0.1693(5) 0.2867(3) 0.0321(10) Uani 1 1 d . . . . .
C3 C 0.2365(7) 0.2982(6) 0.3417(3) 0.0435(12) Uani 1 1 d . . . . .
H3 H 0.2794 0.4009 0.3273 0.052 Uiso 1 1 calc R U . . .
C4 C 0.2102(7) 0.2784(7) 0.4168(3) 0.0495(14) Uani 1 1 d . . . . .
C5 C 0.2377(12) 0.4193(12) 0.4718(5) 0.0961(17) Uani 1 1 d . U . . .
C6 C 0.1462(8) 0.1262(8) 0.4374(3) 0.0537(15) Uani 1 1 d . . . . .
H6 H 0.1268 0.1108 0.4878 0.064 Uiso 1 1 calc R U . . .
C7 C 0.1104(7) -0.0045(6) 0.3838(3) 0.0421(12) Uani 1 1 d . . . . .
H7A H 0.0693 -0.1064 0.3990 0.051 Uiso 1 1 calc R U . . .
C8 C 0.1348(6) 0.0140(5) 0.3071(2) 0.0296(9) Uani 1 1 d . . . . .
C9 C 0.0862(6) -0.1285(5) 0.2502(2) 0.0278(9) Uani 1 1 d . . . . .
C10 C -0.0051(6) -0.1329(5) 0.1738(2) 0.0277(9) Uani 1 1 d . . . . .
H10 H -0.0345 -0.0444 0.1580 0.033 Uiso 1 1 calc R U . . .
C11 C -0.0525(6) -0.2675(5) 0.1209(3) 0.0284(9) Uani 1 1 d . . . . .
C12 C -0.1612(6) -0.2733(5) 0.0407(3) 0.0321(10) Uani 1 1 d . . . . .
C13 C -0.0037(7) -0.3980(5) 0.1443(3) 0.0411(12) Uani 1 1 d . . . . .
H13 H -0.0299 -0.4869 0.1088 0.049 Uiso 1 1 calc R U . . .
C14 C 0.0837(7) -0.3955(6) 0.2201(3) 0.0442(12) Uani 1 1 d . . . . .
H14 H 0.1128 -0.4843 0.2357 0.053 Uiso 1 1 calc R U . . .
C15 C 0.1284(6) -0.2637(5) 0.2727(3) 0.0359(11) Uani 1 1 d . . . . .
H15 H 0.1869 -0.2641 0.3237 0.043 Uiso 1 1 calc R U . . .
C16 C 0.5666(7) 0.5780(6) 0.2334(3) 0.0423(12) Uani 1 1 d . . . . .
H16 H 0.5875 0.4880 0.2521 0.051 Uiso 1 1 calc R U . . .
C17 C 0.6244(7) 0.7150(6) 0.2834(3) 0.0413(12) Uani 1 1 d . . . . .
H17 H 0.6824 0.7166 0.3347 0.050 Uiso 1 1 calc R U . . .
C18 C 0.5956(6) 0.8520(5) 0.2567(3) 0.0338(10) Uani 1 1 d . . . . .
C19 C 0.5117(7) 0.8427(6) 0.1795(3) 0.0387(11) Uani 1 1 d . . . . .
H19 H 0.4934 0.9321 0.1588 0.046 Uiso 1 1 calc R U . . .
C20 C 0.4556(7) 0.6991(6) 0.1338(3) 0.0422(12) Uani 1 1 d . . . . .
H20 H 0.3964 0.6937 0.0824 0.051 Uiso 1 1 calc R U . . .
C21 C 0.6472(7) 1.0008(6) 0.3096(3) 0.0443(13) Uani 1 1 d . . . . .
C22 C 0.6092(9) 0.9953(9) 0.3835(4) 0.076(2) Uani 1 1 d . . . . .
H22 H 0.5561 0.8992 0.4026 0.091 Uiso 1 1 calc R U . . .
C23 C 0.6560(12) 1.1462(16) 0.4300(5) 0.117(4) Uani 1 1 d . . . . .
H23 H 0.6296 1.1475 0.4796 0.140 Uiso 1 1 calc R U . . .
C24 C 0.7738(11) 1.2829(9) 0.3356(7) 0.112(4) Uani 1 1 d . . . . .
H24 H 0.8333 1.3798 0.3187 0.135 Uiso 1 1 calc R U . . .
C25 C 0.7322(8) 1.1482(7) 0.2859(4) 0.069(2) Uani 1 1 d . . . . .
H25 H 0.7606 1.1551 0.2365 0.083 Uiso 1 1 calc R U . . .


_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
Zn1 O7 1.992(4) . ?
Zn1 O5 2.044(3) 2 ?
Zn1 N1 2.117(4) . ?
Zn1 O1 2.126(4) . ?
Zn1 O2 2.288(4) . ?
Zn1 O6 2.383(3) 2 ?
Zn1 C12 2.557(4) 2 ?
N1 C16 1.332(6) . ?
N1 C20 1.340(6) . ?
N2 C24 1.259(14) . ?
N2 C23 1.350(14) . ?
O1 C1 1.241(6) . ?
O2 C1 1.260(6) . ?
O3 C5 1.259(11) . ?
O3 H1 0.8200 . ?
O4 C5 1.258(11) . ?
O5 C12 1.284(5) . ?
O5 Zn1 2.044(3) 2 ?
O6 C12 1.237(6) . ?
O6 Zn1 2.383(3) 2 ?
O7 H1W 0.8468 . ?
O7 H2W 0.8200 . ?
O8 H3W 0.8606 . ?
O8 H4W 0.8494 . ?
C1 C2 1.503(6) . ?
C2 C3 1.389(6) . ?
C2 C8 1.399(6) . ?
C3 C4 1.377(8) . ?
C3 H3 0.9300 . ?
C4 C6 1.376(8) . ?
C4 C5 1.484(8) . ?
C6 C7 1.387(7) . ?
C6 H6 0.9300 . ?
C7 C8 1.399(6) . ?
C7 H7A 0.9300 . ?
C8 C9 1.482(6) . ?
C9 C10 1.397(6) . ?
C9 C15 1.401(6) . ?
C10 C11 1.390(6) . ?
C10 H10 0.9300 . ?
C11 C13 1.390(6) . ?
C11 C12 1.500(6) . ?
C12 Zn1 2.557(4) 2 ?
C13 C14 1.379(7) . ?
C13 H13 0.9300 . ?
C14 C15 1.373(7) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C17 1.370(7) . ?
C16 H16 0.9300 . ?
C17 C18 1.395(7) . ?
C17 H17 0.9300 . ?
C18 C19 1.384(7) . ?
C18 C21 1.482(6) . ?
C19 C20 1.379(6) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
C21 C22 1.380(9) . ?
C21 C25 1.388(9) . ?
C22 C23 1.445(11) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 C25 1.367(10) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?

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
O7 Zn1 O5 104.86(15) . 2 ?
O7 Zn1 N1 96.50(15) . . ?
O5 Zn1 N1 96.40(14) 2 . ?
O7 Zn1 O1 94.73(15) . . ?
O5 Zn1 O1 152.06(14) 2 . ?
N1 Zn1 O1 101.02(15) . . ?
O7 Zn1 O2 153.74(14) . . ?
O5 Zn1 O2 99.70(13) 2 . ?
N1 Zn1 O2 89.78(14) . . ?
O1 Zn1 O2 59.02(14) . . ?
O7 Zn1 O6 90.87(14) . 2 ?
O5 Zn1 O6 58.56(12) 2 2 ?
N1 Zn1 O6 154.96(14) . 2 ?
O1 Zn1 O6 102.18(13) . 2 ?
O2 Zn1 O6 94.11(13) . 2 ?
O7 Zn1 C12 98.51(15) . 2 ?
O5 Zn1 C12 29.83(13) 2 2 ?
N1 Zn1 C12 126.23(15) . 2 ?
O1 Zn1 C12 128.52(14) . 2 ?
O2 Zn1 C12 98.17(14) . 2 ?
O6 Zn1 C12 28.74(13) 2 2 ?
C16 N1 C20 117.0(4) . . ?
C16 N1 Zn1 118.7(3) . . ?
C20 N1 Zn1 123.8(3) . . ?
C24 N2 C23 119.1(8) . . ?
C1 O1 Zn1 93.2(3) . . ?
C1 O2 Zn1 85.4(3) . . ?
C5 O3 H1 109.5 . . ?
C12 O5 Zn1 97.8(3) . 2 ?
C12 O6 Zn1 83.5(3) . 2 ?
Zn1 O7 H1W 124.4 . . ?
Zn1 O7 H2W 109.7 . . ?
H1W O7 H2W 124.5 . . ?
H3W O8 H4W 124.2 . . ?
O1 C1 O2 121.2(5) . . ?
O1 C1 C2 120.1(4) . . ?
O2 C1 C2 118.5(5) . . ?
C3 C2 C8 119.8(4) . . ?
C3 C2 C1 115.9(4) . . ?
C8 C2 C1 124.3(4) . . ?
C4 C3 C2 121.9(5) . . ?
C4 C3 H3 119.1 . . ?
C2 C3 H3 119.1 . . ?
C6 C4 C3 118.7(5) . . ?
C6 C4 C5 121.2(6) . . ?
C3 C4 C5 119.9(7) . . ?
O4 C5 O3 122.7(7) . . ?
O4 C5 C4 119.3(8) . . ?
O3 C5 C4 118.0(9) . . ?
C4 C6 C7 120.5(5) . . ?
C4 C6 H6 119.8 . . ?
C7 C6 H6 119.8 . . ?
C6 C7 C8 121.4(5) . . ?
C6 C7 H7A 119.3 . . ?
C8 C7 H7A 119.3 . . ?
C7 C8 C2 117.7(4) . . ?
C7 C8 C9 119.8(4) . . ?
C2 C8 C9 122.5(4) . . ?
C10 C9 C15 118.4(4) . . ?
C10 C9 C8 121.3(4) . . ?
C15 C9 C8 120.4(4) . . ?
C11 C10 C9 121.1(4) . . ?
C11 C10 H10 119.4 . . ?
C9 C10 H10 119.4 . . ?
C10 C11 C13 119.2(4) . . ?
C10 C11 C12 120.1(4) . . ?
C13 C11 C12 120.7(4) . . ?
O6 C12 O5 120.1(4) . . ?
O6 C12 C11 122.6(4) . . ?
O5 C12 C11 117.2(4) . . ?
O6 C12 Zn1 67.8(2) . 2 ?
O5 C12 Zn1 52.4(2) . 2 ?
C11 C12 Zn1 169.3(3) . 2 ?
C14 C13 C11 120.0(4) . . ?
C14 C13 H13 120.0 . . ?
C11 C13 H13 120.0 . . ?
C15 C14 C13 120.9(4) . . ?
C15 C14 H14 119.5 . . ?
C13 C14 H14 119.5 . . ?
C14 C15 C9 120.4(4) . . ?
C14 C15 H15 119.8 . . ?
C9 C15 H15 119.8 . . ?
N1 C16 C17 123.5(5) . . ?
N1 C16 H16 118.2 . . ?
C17 C16 H16 118.2 . . ?
C16 C17 C18 119.4(5) . . ?
C16 C17 H17 120.3 . . ?
C18 C17 H17 120.3 . . ?
C19 C18 C17 117.5(4) . . ?
C19 C18 C21 121.0(5) . . ?
C17 C18 C21 121.4(4) . . ?
C20 C19 C18 119.0(5) . . ?
C20 C19 H19 120.5 . . ?
C18 C19 H19 120.5 . . ?
N1 C20 C19 123.5(4) . . ?
N1 C20 H20 118.2 . . ?
C19 C20 H20 118.2 . . ?
C22 C21 C25 118.5(6) . . ?
C22 C21 C18 120.2(5) . . ?
C25 C21 C18 121.2(5) . . ?
C21 C22 C23 116.8(8) . . ?
C21 C22 H22 121.6 . . ?
C23 C22 H22 121.6 . . ?
N2 C23 C22 121.4(9) . . ?
N2 C23 H23 119.3 . . ?
C22 C23 H23 119.3 . . ?
N2 C24 C25 124.7(10) . . ?
N2 C24 H24 117.6 . . ?
C25 C24 H24 117.6 . . ?
C24 C25 C21 119.5(8) . . ?
C24 C25 H25 120.3 . . ?
C21 C25 H25 120.3 . . ?

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
Zn1 O1 C1 O2 11.5(4) . . . . ?
Zn1 O1 C1 C2 -162.5(3) . . . . ?
Zn1 O2 C1 O1 -10.7(4) . . . . ?
Zn1 O2 C1 C2 163.4(4) . . . . ?
O1 C1 C2 C3 107.3(5) . . . . ?
O2 C1 C2 C3 -66.9(6) . . . . ?
O1 C1 C2 C8 -72.4(6) . . . . ?
O2 C1 C2 C8 113.4(5) . . . . ?
C8 C2 C3 C4 0.5(7) . . . . ?
C1 C2 C3 C4 -179.2(5) . . . . ?
C2 C3 C4 C6 -0.2(8) . . . . ?
C2 C3 C4 C5 -175.7(5) . . . . ?
C6 C4 C5 O4 -178.9(7) . . . . ?
C3 C4 C5 O4 -3.6(10) . . . . ?
C6 C4 C5 O3 -0.3(10) . . . . ?
C3 C4 C5 O3 175.0(6) . . . . ?
C3 C4 C6 C7 0.6(8) . . . . ?
C5 C4 C6 C7 175.9(6) . . . . ?
C4 C6 C7 C8 -1.2(8) . . . . ?
C6 C7 C8 C2 1.4(7) . . . . ?
C6 C7 C8 C9 -176.9(5) . . . . ?
C3 C2 C8 C7 -1.0(7) . . . . ?
C1 C2 C8 C7 178.7(4) . . . . ?
C3 C2 C8 C9 177.2(4) . . . . ?
C1 C2 C8 C9 -3.1(7) . . . . ?
C7 C8 C9 C10 137.8(5) . . . . ?
C2 C8 C9 C10 -40.4(6) . . . . ?
C7 C8 C9 C15 -41.0(6) . . . . ?
C2 C8 C9 C15 140.8(5) . . . . ?
C15 C9 C10 C11 -0.3(6) . . . . ?
C8 C9 C10 C11 -179.2(4) . . . . ?
C9 C10 C11 C13 -1.7(6) . . . . ?
C9 C10 C11 C12 176.0(4) . . . . ?
Zn1 O6 C12 O5 1.0(4) 2 . . . ?
Zn1 O6 C12 C11 -177.4(4) 2 . . . ?
Zn1 O5 C12 O6 -1.2(5) 2 . . . ?
Zn1 O5 C12 C11 177.3(3) 2 . . . ?
C10 C11 C12 O6 12.2(7) . . . . ?
C13 C11 C12 O6 -170.1(5) . . . . ?
C10 C11 C12 O5 -166.3(4) . . . . ?
C13 C11 C12 O5 11.5(6) . . . . ?
C10 C11 C12 Zn1 -154.6(15) . . . 2 ?
C13 C11 C12 Zn1 23.2(19) . . . 2 ?
C10 C11 C13 C14 2.8(7) . . . . ?
C12 C11 C13 C14 -174.9(4) . . . . ?
C11 C13 C14 C15 -1.9(8) . . . . ?
C13 C14 C15 C9 -0.2(8) . . . . ?
C10 C9 C15 C14 1.3(7) . . . . ?
C8 C9 C15 C14 -179.8(4) . . . . ?
C20 N1 C16 C17 0.8(7) . . . . ?
Zn1 N1 C16 C17 -170.8(4) . . . . ?
N1 C16 C17 C18 -0.4(8) . . . . ?
C16 C17 C18 C19 -1.1(7) . . . . ?
C16 C17 C18 C21 176.9(5) . . . . ?
C17 C18 C19 C20 2.1(7) . . . . ?
C21 C18 C19 C20 -175.9(5) . . . . ?
C16 N1 C20 C19 0.2(7) . . . . ?
Zn1 N1 C20 C19 171.4(4) . . . . ?
C18 C19 C20 N1 -1.7(8) . . . . ?
C19 C18 C21 C22 134.7(6) . . . . ?
C17 C18 C21 C22 -43.2(7) . . . . ?
C19 C18 C21 C25 -44.5(7) . . . . ?
C17 C18 C21 C25 137.5(5) . . . . ?
C25 C21 C22 C23 2.1(8) . . . . ?
C18 C21 C22 C23 -177.1(5) . . . . ?
C24 N2 C23 C22 -0.4(14) . . . . ?
C21 C22 C23 N2 -1.7(11) . . . . ?
C23 N2 C24 C25 2.1(14) . . . . ?
N2 C24 C25 C21 -1.5(11) . . . . ?
C22 C21 C25 C24 -0.7(8) . . . . ?
C18 C21 C25 C24 178.5(5) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C20 H20 O7 0.93 2.61 3.441(6) 148.8 2_665
C17 H17 O3 0.93 2.62 3.503(8) 158.1 2_666
O8 H4W O2 0.85 1.97 2.817(6) 177.9 1_655
O8 H3W O6 0.86 2.08 2.816(5) 142.7 1_655
O7 H2W O5 0.82 1.90 2.710(5) 169.2 1_665
O7 H1W O8 0.85 1.83 2.615(5) 153.8 .
O3 H1 N2 0.82 2.04 2.839(9) 164.6 2_676
C20 H20 O7 0.93 2.61 3.441(6) 148.8 2_665
C17 H17 O3 0.93 2.62 3.503(8) 158.1 2_666
O8 H4W O2 0.85 1.97 2.817(6) 177.9 1_655
O8 H3W O6 0.86 2.08 2.816(5) 142.7 1_655
O7 H2W O5 0.82 1.90 2.710(5) 169.2 1_665
O7 H1W O8 0.85 1.83 2.615(5) 153.8 .
O3 H1 N2 0.82 2.04 2.839(9) 164.6 2_676
C20 H20 O7 0.93 2.61 3.441(6) 148.8 2_665
C17 H17 O3 0.93 2.62 3.503(8) 158.1 2_666
O8 H4W O2 0.85 1.97 2.817(6) 177.9 1_655
O8 H3W O6 0.86 2.08 2.816(5) 142.7 1_655
O7 H2W O5 0.82 1.90 2.710(5) 169.2 1_665
O7 H1W O8 0.85 1.83 2.615(5) 153.8 .
O3 H1 N2 0.82 2.04 2.839(9) 164.6 2_676
C20 H20 O7 0.93 2.61 3.441(6) 148.8 2_665
C20 H20 O5 0.93 2.67 3.224(5) 119.2 2
C17 H17 O3 0.93 2.62 3.503(8) 158.1 2_666
O8 H4W O2 0.85 1.97 2.817(6) 177.9 1_655
O8 H3W O6 0.86 2.08 2.816(5) 142.7 1_655
O7 H2W O5 0.82 1.90 2.710(5) 169.2 1_665
O7 H1W O8 0.85 1.83 2.615(5) 153.8 .
C20 H20 O7 0.93 2.61 3.441(6) 148.8 2_665
C20 H20 O5 0.93 2.67 3.224(5) 119.2 2
C17 H17 O3 0.93 2.62 3.503(8) 158.1 2_666
O8 H4W O2 0.85 1.97 2.817(6) 177.9 1_655
O8 H3W O6 0.86 2.08 2.816(5) 142.7 1_655
O7 H2W O5 0.82 1.90 2.710(5) 169.2 1_665
O7 H1W O8 0.85 1.83 2.615(5) 153.8 .
C20 H20 O7 0.93 2.61 3.441(6) 148.8 2_665
C20 H20 O5 0.93 2.67 3.224(5) 119.2 2
C17 H17 O3 0.93 2.62 3.503(8) 158.1 2_666
O8 H4W O2 0.85 1.97 2.817(6) 177.9 1_655
O8 H3W O6 0.86 2.08 2.816(5) 142.7 1_655
O7 H2W O5 0.82 1.90 2.710(5) 169.2 1_665
O7 H1W O8 0.85 1.83 2.615(5) 153.8 .
C20 H20 O7 0.93 2.61 3.441(6) 148.8 2_665
C17 H17 O3 0.93 2.62 3.503(8) 158.1 2_666
O8 H4W O2 0.85 1.97 2.817(6) 177.9 1_655
O8 H3W O6 0.86 2.08 2.816(5) 142.7 1_655
O7 H2W O5 0.82 1.90 2.710(5) 169.2 1_665
O7 H1W O8 0.85 1.83 2.615(5) 153.8 .
O7 H1W O8 0.85 1.83 2.615(5) 153.8 .
O7 H2W O5 0.82 1.90 2.710(5) 169.2 1_665
O8 H3W O6 0.86 2.08 2.816(5) 142.7 1_655
O8 H4W O2 0.85 1.97 2.817(6) 177.9 1_655
C17 H17 O3 0.93 2.62 3.503(8) 158.1 2_666
C20 H20 O5 0.93 2.67 3.224(5) 119.2 2
C20 H20 O7 0.93 2.61 3.441(6) 148.8 2_665
O3 H1 N2 0.82 2.04 2.839(9) 164.6 2_676
O7 H1W O8 0.85 1.83 2.615(5) 153.8 .
O7 H2W O5 0.82 1.90 2.710(5) 169.2 1_665
O8 H3W O6 0.86 2.08 2.816(5) 142.7 1_655
O8 H4W O2 0.85 1.97 2.817(6) 177.9 1_655
C17 H17 O3 0.93 2.62 3.503(8) 158.1 2_666
C20 H20 O7 0.93 2.61 3.441(6) 148.8 2_665
O3 H1 N2 0.82 2.04 2.839(9) 164.6 2_676
O7 H1W O8 0.85 1.83 2.615(5) 153.8 .
O7 H2W O5 0.82 1.90 2.710(5) 169.2 1_665
O8 H3W O6 0.86 2.08 2.816(5) 142.7 1_655
O8 H4W O2 0.85 1.97 2.817(6) 177.9 1_655
C17 H17 O3 0.93 2.62 3.503(8) 158.1 2_666
C20 H20 O5 0.93 2.67 3.224(5) 119.2 2
C20 H20 O7 0.93 2.61 3.441(6) 148.8 2_665
O3 H1 N2 0.82 2.04 2.839(9) 164.6 2_676
O7 H1W O8 0.85 1.83 2.615(5) 153.8 .
O7 H2W O5 0.82 1.90 2.710(5) 169.2 1_665
O8 H3W O6 0.86 2.08 2.816(5) 142.7 1_655
O8 H4W O2 0.85 1.97 2.817(6) 177.9 1_655
C17 H17 O3 0.93 2.62 3.503(8) 158.1 2_666
C20 H20 O7 0.93 2.61 3.441(6) 148.8 2_665
O3 H1 N2 0.82 2.04 2.839(9) 164.6 2_676
O7 H1W O8 0.85 1.83 2.615(5) 153.8 .
O7 H2W O5 0.82 1.90 2.710(5) 169.2 1_665
O8 H3W O6 0.86 2.08 2.816(5) 142.7 1_655
O8 H4W O2 0.85 1.97 2.817(6) 177.9 1_655
C17 H17 O3 0.93 2.62 3.503(8) 158.1 2_666
C20 H20 O5 0.93 2.67 3.224(5) 119.2 2
C20 H20 O7 0.93 2.61 3.441(6) 148.8 2_665
O3 H1 N2 0.82 2.04 2.839(9) 164.6 2_676
O7 H1W O8 0.85 1.83 2.615(5) 153.8 .
O7 H2W O5 0.82 1.90 2.710(5) 169.2 1_665
O8 H3W O6 0.86 2.08 2.816(5) 142.7 1_655
O8 H4W O2 0.85 1.97 2.817(6) 177.9 1_655
C17 H17 O3 0.93 2.62 3.503(8) 158.1 2_666
C20 H20 O7 0.93 2.61 3.441(6) 148.8 2_665
O3 H1 N2 0.82 2.04 2.839(9) 164.6 2_676
O7 H1W O8 0.85 1.83 2.615(5) 153.8 .
O7 H2W O5 0.82 1.90 2.710(5) 169.2 1_665
O8 H3W O6 0.86 2.08 2.816(5) 142.7 1_655
O8 H4W O2 0.85 1.97 2.817(6) 177.9 1_655
C17 H17 O3 0.93 2.62 3.503(8) 158.1 2_666
C20 H20 O5 0.93 2.67 3.224(5) 119.2 2
C20 H20 O7 0.93 2.61 3.441(6) 148.8 2_665
O3 H1 N2 0.82 2.04 2.839(9) 164.6 2_676
O7 H1W O8 0.85 1.83 2.615(5) 153.8 .
O7 H2W O5 0.82 1.90 2.710(5) 169.2 1_665
O8 H3W O6 0.86 2.08 2.816(5) 142.7 1_655
O8 H4W O2 0.85 1.97 2.817(6) 177.9 1_655
C17 H17 O3 0.93 2.62 3.503(8) 158.1 2_666
C20 H20 O7 0.93 2.61 3.441(6) 148.8 2_665

_refine_diff_density_max         1.054
_refine_diff_density_min         -0.912
_refine_diff_density_rms         0.088


# start Validation Reply Form
_vrf_PLAT910_I                   
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min) 12 Note
RESPONSE: Reduction of beam stop mask did not yield significant improvement.
Most of those missing srtong reflections appeared to be very strong and were
treated as overflows.
;
# end Validation Reply Form

####################################################################### 
# 
# 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_437-6Zn
_database_code_depnum_ccdc_archive 'CCDC 2012746'
_audit_update_record             
;
2020-06-28 deposited with the CCDC.	2021-01-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C60 H46 N6 O16 Zn3'
_chemical_formula_weight         1303.14

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'
Zn Zn 0.2839 1.4301 '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                   12.8194(10)
_cell_length_b                   13.5884(10)
_cell_length_c                   19.4475(15)
_cell_angle_alpha                75.329(7)
_cell_angle_beta                 87.264(6)
_cell_angle_gamma                85.755(6)
_cell_volume                     3266.7(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    22024
_cell_measurement_theta_min      3.232
_cell_measurement_theta_max      25.049

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_F_000             1332
_exptl_transmission_factor_min   0.784
_exptl_transmission_factor_max   0.802
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    1.159
_shelx_estimated_absorpt_T_min   0.793
_shelx_estimated_absorpt_T_max   0.810
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.793
_exptl_absorpt_correction_T_max  0.810
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APE-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22024
_diffrn_reflns_av_unetI/netI     0.1720
_diffrn_reflns_av_R_equivalents  0.0858
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.232
_diffrn_reflns_theta_max         25.049
_diffrn_reflns_theta_full        25.049
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             11536
_reflns_number_gt                5554
_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    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     'w=1/[σ²(Fo²)] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11536
_refine_ls_number_parameters     766
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1494
_refine_ls_R_factor_gt           0.0816
_refine_ls_wR_factor_ref         0.1492
_refine_ls_wR_factor_gt          0.1249
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_restrained_S_all      1.116
_refine_ls_shift/su_max          0.000
_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
Zn1 Zn 0.46323(6) 0.08626(6) 0.17150(4) 0.0381(2) Uani 1 1 d . . . . .
Zn2 Zn 0.74232(7) 0.47218(8) 0.45127(5) 0.0571(3) Uani 1 1 d . . . . .
Zn3 Zn 1.02679(6) 0.70520(6) 0.82709(4) 0.0387(2) Uani 1 1 d . . . . .
N1 N 0.3638(4) 0.1021(4) 0.0861(3) 0.0320(14) Uani 1 1 d . . . . .
N2 N 0.5710(4) 0.1124(4) 0.0812(3) 0.0318(14) Uani 1 1 d . . . . .
N3 N 0.7964(6) 0.6243(6) 0.4277(3) 0.061(2) Uani 1 1 d . . . . .
N4 N 0.9035(5) 0.4451(7) 0.4324(3) 0.065(2) Uani 1 1 d . . . . .
N5 N 1.1300(4) 0.6567(4) 0.9148(3) 0.0351(14) Uani 1 1 d . . . . .
N6 N 0.9217(4) 0.6690(4) 0.9189(3) 0.0355(15) Uani 1 1 d . . . . .
O1 O 0.5005(4) 0.2052(4) 0.2075(3) 0.0544(15) Uani 1 1 d . . . . .
O2 O 0.4430(5) 0.3045(4) 0.1075(4) 0.093(3) Uani 1 1 d . . . . .
O3 O 0.7512(4) 0.3708(4) 0.3394(3) 0.0576(16) Uani 1 1 d . . . . .
O4 O 0.6496(3) 0.4917(4) 0.3697(2) 0.0423(13) Uani 1 1 d . . . . .
O5 O 0.6148(5) 0.9859(5) 0.2462(4) 0.101(2) Uani 1 1 d . . . . .
O6 O 0.4976(4) 0.9284(4) 0.1905(3) 0.0618(16) Uani 1 1 d . . . . .
O7 O 0.8956(4) 0.6750(4) 0.7619(3) 0.0605(16) Uani 1 1 d . . . . .
O8 O 1.0112(4) 0.5518(4) 0.8077(3) 0.0546(15) Uani 1 1 d . . . . .
O9 O 0.7997(4) 0.2642(4) 0.6302(3) 0.0513(15) Uani 1 1 d . . . . .
O10 O 0.7190(4) 0.1212(4) 0.6690(3) 0.0667(18) Uani 1 1 d . . . . .
O11 O 1.0593(5) -0.1183(4) 0.8880(3) 0.092(2) Uani 1 1 d . . . . .
O12 O 0.9832(4) -0.1458(3) 0.7961(3) 0.0477(14) Uani 1 1 d . . . . .
O13 O 0.3382(4) 0.0588(3) 0.2476(2) 0.0545(15) Uani 1 1 d . . . . .
H1W H 0.3850 0.1017 0.2358 0.065 Uiso 1 1 d R U . . .
H2W H 0.3339 -0.0028 0.2630 0.065 Uiso 1 1 d R U . . .
O14 O 0.6482(4) 0.5078(5) 0.5362(3) 0.101(2) Uani 1 1 d . . . . .
H3W H 0.6684 0.4519 0.5261 0.122 Uiso 1 1 d R U . . .
H4W H 0.6896 0.5413 0.5049 0.122 Uiso 1 1 d R U . . .
O15 O 0.7181(4) 0.3221(4) 0.5014(3) 0.0798(19) Uani 1 1 d . . . . .
H5W H 0.7479 0.3068 0.5394 0.096 Uiso 1 1 d R U . . .
H6W H 0.7691 0.3566 0.4820 0.096 Uiso 1 1 d R U . . .
O16 O 1.1533(4) 0.7297(4) 0.7516(3) 0.0622(16) Uani 1 1 d . . . . .
H7W H 1.1606 0.6822 0.7325 0.075 Uiso 1 1 d R U . . .
H8W H 1.1038 0.7667 0.7646 0.075 Uiso 1 1 d R U . . .
C1 C 0.2618(5) 0.0966(5) 0.0912(4) 0.0398(18) Uani 1 1 d . . . . .
H1 H 0.2297 0.0847 0.1361 0.048 Uiso 1 1 calc R U . . .
C2 C 0.1992(6) 0.1077(6) 0.0327(4) 0.047(2) Uani 1 1 d . . . . .
H2 H 0.1273 0.1018 0.0386 0.056 Uiso 1 1 calc R U . . .
C3 C 0.2461(6) 0.1275(6) -0.0334(4) 0.053(2) Uani 1 1 d . . . . .
H3 H 0.2065 0.1382 -0.0737 0.064 Uiso 1 1 calc R U . . .
C4 C 0.3529(6) 0.1315(5) -0.0391(4) 0.043(2) Uani 1 1 d . . . . .
H4 H 0.3867 0.1414 -0.0835 0.052 Uiso 1 1 calc R U . . .
C5 C 0.4103(5) 0.1207(5) 0.0216(4) 0.0313(17) Uani 1 1 d . . . . .
C6 C 0.5260(5) 0.1251(5) 0.0176(4) 0.0343(17) Uani 1 1 d . . . . .
C7 C 0.5860(6) 0.1395(5) -0.0452(4) 0.049(2) Uani 1 1 d . . . . .
H7 H 0.5537 0.1484 -0.0884 0.059 Uiso 1 1 calc R U . . .
C8 C 0.6933(6) 0.1405(6) -0.0435(5) 0.060(2) Uani 1 1 d . . . . .
H8 H 0.7345 0.1501 -0.0850 0.072 Uiso 1 1 calc R U . . .
C9 C 0.7377(6) 0.1270(6) 0.0216(5) 0.060(2) Uani 1 1 d . . . . .
H9 H 0.8099 0.1271 0.0244 0.072 Uiso 1 1 calc R U . . .
C10 C 0.6755(6) 0.1133(5) 0.0827(4) 0.0420(19) Uani 1 1 d . . . . .
H10 H 0.7069 0.1043 0.1262 0.050 Uiso 1 1 calc R U . . .
C11 C 0.4851(5) 0.2899(6) 0.1643(5) 0.044(2) Uani 1 1 d . . . . .
C12 C 0.5241(5) 0.3829(5) 0.1824(4) 0.0333(17) Uani 1 1 d . . . . .
C13 C 0.5806(5) 0.3726(5) 0.2433(4) 0.0368(18) Uani 1 1 d . . . . .
H13A H 0.5917 0.3085 0.2742 0.044 Uiso 1 1 calc R U . . .
C14 C 0.6209(5) 0.4567(5) 0.2589(3) 0.0317(17) Uani 1 1 d . . . . .
C15 C 0.6795(6) 0.4364(6) 0.3274(4) 0.0415(19) Uani 1 1 d . . . . .
C16 C 0.6087(5) 0.5519(5) 0.2122(3) 0.0272(16) Uani 1 1 d . . . . .
C17 C 0.5513(5) 0.5619(5) 0.1519(3) 0.0331(17) Uani 1 1 d . . . . .
H17 H 0.5401 0.6260 0.1209 0.040 Uiso 1 1 calc R U . . .
C18 C 0.5096(5) 0.4775(5) 0.1366(4) 0.0386(19) Uani 1 1 d . . . . .
H18 H 0.4721 0.4857 0.0956 0.046 Uiso 1 1 calc R U . . .
C19 C 0.6599(6) 0.6419(5) 0.2232(4) 0.0394(18) Uani 1 1 d . . . . .
C20 C 0.6001(5) 0.7325(5) 0.2209(3) 0.0311(17) Uani 1 1 d . . . . .
H20 H 0.5286 0.7356 0.2139 0.037 Uiso 1 1 calc R U . . .
C21 C 0.6448(6) 0.8159(5) 0.2286(3) 0.0367(18) Uani 1 1 d . . . . .
C22 C 0.7543(6) 0.8116(5) 0.2380(4) 0.045(2) Uani 1 1 d . . . . .
H22 H 0.7865 0.8684 0.2430 0.054 Uiso 1 1 calc R U . . .
C23 C 0.8105(5) 0.7231(5) 0.2395(4) 0.0412(19) Uani 1 1 d . . . . .
H23 H 0.8824 0.7195 0.2453 0.049 Uiso 1 1 calc R U . . .
C24 C 0.7649(5) 0.6398(5) 0.2328(4) 0.0389(19) Uani 1 1 d . . . . .
H24 H 0.8058 0.5797 0.2348 0.047 Uiso 1 1 calc R U . . .
C25 C 0.7433(8) 0.7116(9) 0.4274(5) 0.086(3) Uani 1 1 d . . . . .
H25 H 0.6724 0.7086 0.4398 0.104 Uiso 1 1 calc R U . . .
C26 C 0.7832(10) 0.8073(9) 0.4105(5) 0.105(4) Uani 1 1 d . . . . .
H26 H 0.7428 0.8675 0.4087 0.126 Uiso 1 1 calc R U . . .
C27 C 0.8904(10) 0.8028(10) 0.3966(6) 0.101(4) Uani 1 1 d . . . . .
H27 H 0.9233 0.8637 0.3873 0.121 Uiso 1 1 calc R U . . .
C28 C 0.9517(8) 0.7171(10) 0.3955(5) 0.083(3) Uani 1 1 d . . . . .
H28 H 1.0228 0.7188 0.3837 0.100 Uiso 1 1 calc R U . . .
C29 C 0.9016(8) 0.6280(9) 0.4130(4) 0.069(3) Uani 1 1 d . . . . .
C30 C 0.9583(7) 0.5289(9) 0.4154(4) 0.066(3) Uani 1 1 d . . . . .
C31 C 1.0670(9) 0.5177(10) 0.4027(5) 0.080(4) Uani 1 1 d . . . . .
H31 H 1.1069 0.5743 0.3929 0.096 Uiso 1 1 calc R U . . .
C32 C 1.1103(9) 0.4299(11) 0.4046(5) 0.092(4) Uani 1 1 d . . . . .
H32 H 1.1821 0.4253 0.3954 0.111 Uiso 1 1 calc R U . . .
C33 C 1.0575(9) 0.3383(9) 0.4196(5) 0.089(3) Uani 1 1 d . . . . .
H33 H 1.0910 0.2751 0.4200 0.107 Uiso 1 1 calc R U . . .
C34 C 0.9470(8) 0.3528(8) 0.4341(5) 0.075(3) Uani 1 1 d . . . . .
H34 H 0.9057 0.2971 0.4446 0.090 Uiso 1 1 calc R U . . .
C35 C 0.7839(5) 0.1850(6) 0.6742(4) 0.0385(18) Uani 1 1 d . . . . .
C36 C 0.8496(5) 0.1543(5) 0.7411(3) 0.0300(16) Uani 1 1 d . . . . .
C37 C 0.8946(5) 0.0541(5) 0.7577(4) 0.0351(17) Uani 1 1 d . . . . .
H37 H 0.8796 0.0105 0.7300 0.042 Uiso 1 1 calc R U . . .
C38 C 0.9613(5) 0.0184(5) 0.8147(4) 0.0406(19) Uani 1 1 d . . . . .
C39 C 0.9820(5) 0.0868(5) 0.8538(4) 0.044(2) Uani 1 1 d . . . . .
H39 H 1.0291 0.0659 0.8904 0.052 Uiso 1 1 calc R U . . .
C40 C 0.9352(5) 0.1851(5) 0.8406(4) 0.0424(19) Uani 1 1 d . . . . .
H40 H 0.9459 0.2261 0.8710 0.051 Uiso 1 1 calc R U . . .
C41 C 0.8714(5) 0.2230(5) 0.7810(4) 0.0331(17) Uani 1 1 d . . . . .
C42 C 0.8280(5) 0.3287(5) 0.7685(3) 0.0319(17) Uani 1 1 d . . . . .
C43 C 0.7247(5) 0.3572(5) 0.7523(4) 0.042(2) Uani 1 1 d . . . . .
H43 H 0.6802 0.3085 0.7474 0.050 Uiso 1 1 calc R U . . .
C44 C 0.6867(6) 0.4578(6) 0.7433(4) 0.051(2) Uani 1 1 d . . . . .
H44 H 0.6171 0.4759 0.7318 0.061 Uiso 1 1 calc R U . . .
C45 C 0.7504(6) 0.5315(6) 0.7511(4) 0.046(2) Uani 1 1 d . . . . .
H45 H 0.7242 0.5987 0.7454 0.055 Uiso 1 1 calc R U . . .
C46 C 0.8541(5) 0.5033(5) 0.7678(3) 0.0307(17) Uani 1 1 d . . . . .
C47 C 0.9247(7) 0.5807(6) 0.7781(4) 0.051(2) Uani 1 1 d . . . . .
C48 C 0.8912(5) 0.4036(5) 0.7769(3) 0.0322(17) Uani 1 1 d . . . . .
H48 H 0.9606 0.3856 0.7889 0.039 Uiso 1 1 calc R U . . .
C49 C 1.2336(6) 0.6524(5) 0.9096(4) 0.049(2) Uani 1 1 d . . . . .
H49 H 1.2658 0.6661 0.8646 0.058 Uiso 1 1 calc R U . . .
C50 C 1.2960(6) 0.6283(5) 0.9688(4) 0.049(2) Uani 1 1 d . . . . .
H50 H 1.3684 0.6276 0.9632 0.059 Uiso 1 1 calc R U . . .
C51 C 1.2518(6) 0.6064(6) 1.0332(4) 0.054(2) Uani 1 1 d . . . . .
H51 H 1.2928 0.5903 1.0731 0.065 Uiso 1 1 calc R U . . .
C52 C 1.1412(5) 0.6077(5) 1.0408(4) 0.0423(19) Uani 1 1 d . . . . .
H52 H 1.1083 0.5919 1.0855 0.051 Uiso 1 1 calc R U . . .
C53 C 1.0837(5) 0.6331(5) 0.9800(4) 0.0347(17) Uani 1 1 d . . . . .
C54 C 0.9687(5) 0.6375(5) 0.9822(4) 0.0327(17) Uani 1 1 d . . . . .
C55 C 0.9118(6) 0.6092(5) 1.0447(4) 0.043(2) Uani 1 1 d . . . . .
H55 H 0.9448 0.5891 1.0881 0.052 Uiso 1 1 calc R U . . .
C56 C 0.8045(6) 0.6113(5) 1.0418(4) 0.045(2) Uani 1 1 d . . . . .
H56 H 0.7645 0.5912 1.0835 0.054 Uiso 1 1 calc R U . . .
C57 C 0.7567(6) 0.6427(5) 0.9784(4) 0.044(2) Uani 1 1 d . . . . .
H57 H 0.6842 0.6450 0.9762 0.053 Uiso 1 1 calc R U . . .
C58 C 0.8171(6) 0.6706(5) 0.9181(4) 0.046(2) Uani 1 1 d . . . . .
H58 H 0.7846 0.6917 0.8746 0.055 Uiso 1 1 calc R U . . .
C59 C 0.5807(7) 0.9153(7) 0.2228(4) 0.059(2) Uani 1 1 d . . . . .
C60 C 1.0066(5) -0.0906(6) 0.8351(4) 0.044(2) 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
Zn1 O1 2.012(5) . ?
Zn1 O6 2.099(5) 1_545 ?
Zn1 N1 2.100(5) . ?
Zn1 O13 2.117(5) . ?
Zn1 N2 2.155(5) . ?
Zn1 H1W 1.6103 . ?
Zn2 O4 1.980(4) . ?
Zn2 O15 2.065(5) . ?
Zn2 N4 2.103(7) . ?
Zn2 O14 2.131(6) . ?
Zn2 N3 2.160(7) . ?
Zn2 H3W 1.6724 . ?
Zn2 H4W 1.6622 . ?
Zn2 H6W 1.5512 . ?
Zn3 O12 2.006(5) 1_565 ?
Zn3 O16 2.122(5) . ?
Zn3 N5 2.147(5) . ?
Zn3 N6 2.160(6) . ?
Zn3 O8 2.235(5) . ?
Zn3 O7 2.275(5) . ?
Zn3 C47 2.597(8) . ?
Zn3 H8W 1.6259 . ?
N1 C1 1.312(7) . ?
N1 C5 1.336(8) . ?
N2 C10 1.343(7) . ?
N2 C6 1.355(7) . ?
N3 C25 1.322(11) . ?
N3 C29 1.367(11) . ?
N4 C34 1.327(10) . ?
N4 C30 1.343(10) . ?
N5 C49 1.325(8) . ?
N5 C53 1.346(8) . ?
N6 C58 1.340(8) . ?
N6 C54 1.351(7) . ?
O1 C11 1.250(8) . ?
O2 C11 1.217(8) . ?
O3 C15 1.220(8) . ?
O4 C15 1.275(8) . ?
O5 C59 1.273(9) . ?
O6 C59 1.242(9) . ?
O6 Zn1 2.099(5) 1_565 ?
O7 C47 1.272(8) . ?
O8 C47 1.263(8) . ?
O9 C35 1.218(8) . ?
O10 C35 1.271(7) . ?
O11 C60 1.220(8) . ?
O12 C60 1.253(8) . ?
O12 Zn3 2.006(5) 1_545 ?
O13 H1W 0.8500 . ?
O13 H2W 0.8200 . ?
O14 H3W 0.8505 . ?
O14 H4W 0.8501 . ?
O15 H5W 0.8200 . ?
O15 H6W 0.8494 . ?
O16 H7W 0.8200 . ?
O16 H8W 0.8500 . ?
C1 C2 1.394(8) . ?
C1 H1 0.9300 . ?
C2 C3 1.364(10) . ?
C2 H2 0.9300 . ?
C3 C4 1.371(9) . ?
C3 H3 0.9300 . ?
C4 C5 1.391(8) . ?
C4 H4 0.9300 . ?
C5 C6 1.486(8) . ?
C6 C7 1.391(9) . ?
C7 C8 1.379(9) . ?
C7 H7 0.9300 . ?
C8 C9 1.377(10) . ?
C8 H8 0.9300 . ?
C9 C10 1.378(10) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 C12 1.518(9) . ?
C12 C18 1.371(9) . ?
C12 C13 1.390(8) . ?
C13 C14 1.393(8) . ?
C13 H13A 0.9300 . ?
C14 C16 1.382(8) . ?
C14 C15 1.515(8) . ?
C16 C17 1.387(7) . ?
C16 C19 1.496(8) . ?
C17 C18 1.402(8) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C19 C24 1.365(8) . ?
C19 C20 1.392(8) . ?
C20 C21 1.352(8) . ?
C20 H20 0.9300 . ?
C21 C22 1.419(9) . ?
C21 C59 1.510(10) . ?
C22 C23 1.350(9) . ?
C22 H22 0.9300 . ?
C23 C24 1.349(8) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 C26 1.388(12) . ?
C25 H25 0.9300 . ?
C26 C27 1.388(13) . ?
C26 H26 0.9300 . ?
C27 C28 1.360(13) . ?
C27 H27 0.9300 . ?
C28 C29 1.370(12) . ?
C28 H28 0.9300 . ?
C29 C30 1.474(12) . ?
C30 C31 1.408(12) . ?
C31 C32 1.270(13) . ?
C31 H31 0.9300 . ?
C32 C33 1.420(13) . ?
C32 H32 0.9300 . ?
C33 C34 1.440(11) . ?
C33 H33 0.9300 . ?
C34 H34 0.9300 . ?
C35 C36 1.533(8) . ?
C36 C37 1.403(8) . ?
C36 C41 1.407(8) . ?
C37 C38 1.398(8) . ?
C37 H37 0.9300 . ?
C38 C39 1.387(9) . ?
C38 C60 1.512(9) . ?
C39 C40 1.390(9) . ?
C39 H39 0.9300 . ?
C40 C41 1.415(8) . ?
C40 H40 0.9300 . ?
C41 C42 1.466(9) . ?
C42 C43 1.380(8) . ?
C42 C48 1.392(8) . ?
C43 C44 1.388(9) . ?
C43 H43 0.9300 . ?
C44 C45 1.379(9) . ?
C44 H44 0.9300 . ?
C45 C46 1.387(8) . ?
C45 H45 0.9300 . ?
C46 C48 1.373(8) . ?
C46 C47 1.493(9) . ?
C48 H48 0.9300 . ?
C49 C50 1.390(9) . ?
C49 H49 0.9300 . ?
C50 C51 1.320(10) . ?
C50 H50 0.9300 . ?
C51 C52 1.418(9) . ?
C51 H51 0.9300 . ?
C52 C53 1.377(8) . ?
C52 H52 0.9300 . ?
C53 C54 1.470(8) . ?
C54 C55 1.371(9) . ?
C55 C56 1.377(8) . ?
C55 H55 0.9300 . ?
C56 C57 1.359(9) . ?
C56 H56 0.9300 . ?
C57 C58 1.360(10) . ?
C57 H57 0.9300 . ?
C58 H58 0.9300 . ?

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 Zn1 O6 139.8(2) . 1_545 ?
O1 Zn1 N1 122.8(2) . . ?
O6 Zn1 N1 97.3(2) 1_545 . ?
O1 Zn1 O13 90.20(19) . . ?
O6 Zn1 O13 89.39(19) 1_545 . ?
N1 Zn1 O13 92.7(2) . . ?
O1 Zn1 N2 96.2(2) . . ?
O6 Zn1 N2 90.48(19) 1_545 . ?
N1 Zn1 N2 77.6(2) . . ?
O13 Zn1 N2 170.24(19) . . ?
O1 Zn1 H1W 68.9 . . ?
O6 Zn1 H1W 105.7 1_545 . ?
N1 Zn1 H1W 103.8 . . ?
O13 Zn1 H1W 21.3 . . ?
N2 Zn1 H1W 163.3 . . ?
O4 Zn2 O15 99.74(19) . . ?
O4 Zn2 N4 117.3(2) . . ?
O15 Zn2 N4 94.6(3) . . ?
O4 Zn2 O14 106.7(2) . . ?
O15 Zn2 O14 85.4(2) . . ?
N4 Zn2 O14 135.2(2) . . ?
O4 Zn2 N3 98.1(2) . . ?
O15 Zn2 N3 162.1(2) . . ?
N4 Zn2 N3 78.2(3) . . ?
O14 Zn2 N3 88.3(3) . . ?
O4 Zn2 H3W 108.5 . . ?
O15 Zn2 H3W 63.5 . . ?
N4 Zn2 H3W 132.1 . . ?
O14 Zn2 H3W 21.9 . . ?
N3 Zn2 H3W 109.2 . . ?
O4 Zn2 H4W 107.9 . . ?
O15 Zn2 H4W 106.3 . . ?
N4 Zn2 H4W 125.5 . . ?
O14 Zn2 H4W 21.7 . . ?
N3 Zn2 H4W 66.6 . . ?
H3W Zn2 H4W 43.2 . . ?
O4 Zn2 H6W 109.4 . . ?
O15 Zn2 H6W 21.8 . . ?
N4 Zn2 H6W 72.9 . . ?
O14 Zn2 H6W 100.9 . . ?
N3 Zn2 H6W 146.8 . . ?
H3W Zn2 H6W 79.8 . . ?
H4W Zn2 H6W 119.1 . . ?
O12 Zn3 O16 89.07(19) 1_565 . ?
O12 Zn3 N5 117.4(2) 1_565 . ?
O16 Zn3 N5 92.5(2) . . ?
O12 Zn3 N6 96.9(2) 1_565 . ?
O16 Zn3 N6 168.74(19) . . ?
N5 Zn3 N6 76.3(2) . . ?
O12 Zn3 O8 145.30(19) 1_565 . ?
O16 Zn3 O8 89.89(19) . . ?
N5 Zn3 O8 97.3(2) . . ?
N6 Zn3 O8 90.6(2) . . ?
O12 Zn3 O7 88.34(19) 1_565 . ?
O16 Zn3 O7 102.30(19) . . ?
N5 Zn3 O7 150.7(2) . . ?
N6 Zn3 O7 87.5(2) . . ?
O8 Zn3 O7 58.09(17) . . ?
O12 Zn3 C47 117.6(2) 1_565 . ?
O16 Zn3 C47 100.0(2) . . ?
N5 Zn3 C47 123.5(2) . . ?
N6 Zn3 C47 85.8(2) . . ?
O8 Zn3 C47 29.09(19) . . ?
O7 Zn3 C47 29.3(2) . . ?
O12 Zn3 H8W 67.7 1_565 . ?
O16 Zn3 H8W 21.4 . . ?
N5 Zn3 H8W 101.8 . . ?
N6 Zn3 H8W 161.9 . . ?
O8 Zn3 H8W 107.5 . . ?
O7 Zn3 H8W 100.9 . . ?
C47 Zn3 H8W 109.4 . . ?
C1 N1 C5 118.6(6) . . ?
C1 N1 Zn1 125.7(5) . . ?
C5 N1 Zn1 115.7(4) . . ?
C10 N2 C6 118.6(6) . . ?
C10 N2 Zn1 126.7(5) . . ?
C6 N2 Zn1 114.6(4) . . ?
C25 N3 C29 116.9(9) . . ?
C25 N3 Zn2 129.4(8) . . ?
C29 N3 Zn2 113.7(7) . . ?
C34 N4 C30 122.5(10) . . ?
C34 N4 Zn2 122.5(7) . . ?
C30 N4 Zn2 114.9(8) . . ?
C49 N5 C53 118.6(6) . . ?
C49 N5 Zn3 125.3(5) . . ?
C53 N5 Zn3 116.1(5) . . ?
C58 N6 C54 118.5(6) . . ?
C58 N6 Zn3 126.2(5) . . ?
C54 N6 Zn3 115.2(4) . . ?
C11 O1 Zn1 114.2(5) . . ?
C15 O4 Zn2 113.0(4) . . ?
C59 O6 Zn1 102.9(5) . 1_565 ?
C47 O7 Zn3 89.5(5) . . ?
C47 O8 Zn3 91.6(5) . . ?
C60 O12 Zn3 117.3(5) . 1_545 ?
Zn1 O13 H1W 43.5 . . ?
Zn1 O13 H2W 109.3 . . ?
H1W O13 H2W 139.1 . . ?
Zn2 O14 H3W 47.1 . . ?
Zn2 O14 H4W 46.3 . . ?
H3W O14 H4W 92.3 . . ?
Zn2 O15 H5W 108.9 . . ?
Zn2 O15 H6W 42.7 . . ?
H5W O15 H6W 90.0 . . ?
Zn3 O16 H7W 109.5 . . ?
Zn3 O16 H8W 44.3 . . ?
H7W O16 H8W 138.3 . . ?
N1 C1 C2 123.5(7) . . ?
N1 C1 H1 118.3 . . ?
C2 C1 H1 118.3 . . ?
C3 C2 C1 118.2(7) . . ?
C3 C2 H2 120.9 . . ?
C1 C2 H2 120.9 . . ?
C4 C3 C2 118.7(7) . . ?
C4 C3 H3 120.6 . . ?
C2 C3 H3 120.6 . . ?
C3 C4 C5 119.9(7) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 H4 120.1 . . ?
N1 C5 C4 121.0(6) . . ?
N1 C5 C6 117.3(6) . . ?
C4 C5 C6 121.6(7) . . ?
N2 C6 C7 121.2(6) . . ?
N2 C6 C5 114.7(6) . . ?
C7 C6 C5 124.0(6) . . ?
C8 C7 C6 119.9(7) . . ?
C8 C7 H7 120.0 . . ?
C6 C7 H7 120.0 . . ?
C9 C8 C7 118.1(8) . . ?
C9 C8 H8 121.0 . . ?
C7 C8 H8 121.0 . . ?
C8 C9 C10 120.2(7) . . ?
C8 C9 H9 119.9 . . ?
C10 C9 H9 119.9 . . ?
N2 C10 C9 121.9(7) . . ?
N2 C10 H10 119.0 . . ?
C9 C10 H10 119.0 . . ?
O2 C11 O1 125.4(7) . . ?
O2 C11 C12 116.4(8) . . ?
O1 C11 C12 118.1(7) . . ?
C18 C12 C13 118.9(6) . . ?
C18 C12 C11 120.4(6) . . ?
C13 C12 C11 120.6(7) . . ?
C12 C13 C14 121.1(7) . . ?
C12 C13 H13A 119.4 . . ?
C14 C13 H13A 119.4 . . ?
C16 C14 C13 120.2(6) . . ?
C16 C14 C15 123.4(6) . . ?
C13 C14 C15 116.4(6) . . ?
O3 C15 O4 123.7(7) . . ?
O3 C15 C14 120.1(7) . . ?
O4 C15 C14 116.2(6) . . ?
C14 C16 C17 118.4(6) . . ?
C14 C16 C19 121.9(6) . . ?
C17 C16 C19 119.7(6) . . ?
C16 C17 C18 121.3(6) . . ?
C16 C17 H17 119.3 . . ?
C18 C17 H17 119.3 . . ?
C12 C18 C17 120.0(6) . . ?
C12 C18 H18 120.0 . . ?
C17 C18 H18 120.0 . . ?
C24 C19 C20 118.3(7) . . ?
C24 C19 C16 122.1(6) . . ?
C20 C19 C16 119.6(6) . . ?
C21 C20 C19 120.9(7) . . ?
C21 C20 H20 119.6 . . ?
C19 C20 H20 119.6 . . ?
C20 C21 C22 119.6(7) . . ?
C20 C21 C59 120.7(7) . . ?
C22 C21 C59 119.6(7) . . ?
C23 C22 C21 118.4(7) . . ?
C23 C22 H22 120.8 . . ?
C21 C22 H22 120.8 . . ?
C24 C23 C22 121.6(7) . . ?
C24 C23 H23 119.2 . . ?
C22 C23 H23 119.2 . . ?
C23 C24 C19 121.3(7) . . ?
C23 C24 H24 119.4 . . ?
C19 C24 H24 119.4 . . ?
N3 C25 C26 126.3(11) . . ?
N3 C25 H25 116.9 . . ?
C26 C25 H25 116.9 . . ?
C25 C26 C27 112.3(12) . . ?
C25 C26 H26 123.9 . . ?
C27 C26 H26 123.9 . . ?
C28 C27 C26 125.7(12) . . ?
C28 C27 H27 117.1 . . ?
C26 C27 H27 117.1 . . ?
C27 C28 C29 115.5(11) . . ?
C27 C28 H28 122.2 . . ?
C29 C28 H28 122.2 . . ?
N3 C29 C28 123.2(11) . . ?
N3 C29 C30 115.2(9) . . ?
C28 C29 C30 121.6(11) . . ?
N4 C30 C31 118.7(11) . . ?
N4 C30 C29 118.1(9) . . ?
C31 C30 C29 123.2(10) . . ?
C32 C31 C30 119.7(13) . . ?
C32 C31 H31 120.2 . . ?
C30 C31 H31 120.2 . . ?
C31 C32 C33 125.1(13) . . ?
C31 C32 H32 117.5 . . ?
C33 C32 H32 117.5 . . ?
C32 C33 C34 113.4(11) . . ?
C32 C33 H33 123.3 . . ?
C34 C33 H33 123.3 . . ?
N4 C34 C33 120.5(10) . . ?
N4 C34 H34 119.8 . . ?
C33 C34 H34 119.8 . . ?
O9 C35 O10 125.6(7) . . ?
O9 C35 C36 119.1(6) . . ?
O10 C35 C36 115.2(7) . . ?
C37 C36 C41 120.9(6) . . ?
C37 C36 C35 115.8(6) . . ?
C41 C36 C35 123.2(6) . . ?
C38 C37 C36 121.6(6) . . ?
C38 C37 H37 119.2 . . ?
C36 C37 H37 119.2 . . ?
C39 C38 C37 117.0(7) . . ?
C39 C38 C60 120.8(6) . . ?
C37 C38 C60 122.1(6) . . ?
C38 C39 C40 122.8(7) . . ?
C38 C39 H39 118.6 . . ?
C40 C39 H39 118.6 . . ?
C39 C40 C41 120.2(7) . . ?
C39 C40 H40 119.9 . . ?
C41 C40 H40 119.9 . . ?
C36 C41 C40 117.3(7) . . ?
C36 C41 C42 125.1(6) . . ?
C40 C41 C42 117.5(6) . . ?
C43 C42 C48 117.8(6) . . ?
C43 C42 C41 122.9(6) . . ?
C48 C42 C41 119.2(6) . . ?
C44 C43 C42 120.5(6) . . ?
C44 C43 H43 119.7 . . ?
C42 C43 H43 119.7 . . ?
C43 C44 C45 121.1(7) . . ?
C43 C44 H44 119.4 . . ?
C45 C44 H44 119.4 . . ?
C46 C45 C44 118.7(7) . . ?
C46 C45 H45 120.7 . . ?
C44 C45 H45 120.7 . . ?
C48 C46 C45 120.0(6) . . ?
C48 C46 C47 119.9(6) . . ?
C45 C46 C47 120.1(7) . . ?
O8 C47 O7 119.5(7) . . ?
O8 C47 C46 119.7(7) . . ?
O7 C47 C46 120.6(7) . . ?
O8 C47 Zn3 59.4(4) . . ?
O7 C47 Zn3 61.1(4) . . ?
C46 C47 Zn3 165.9(5) . . ?
C46 C48 C42 121.9(6) . . ?
C46 C48 H48 119.0 . . ?
C42 C48 H48 119.0 . . ?
N5 C49 C50 122.5(7) . . ?
N5 C49 H49 118.8 . . ?
C50 C49 H49 118.8 . . ?
C51 C50 C49 119.6(8) . . ?
C51 C50 H50 120.2 . . ?
C49 C50 H50 120.2 . . ?
C50 C51 C52 119.4(7) . . ?
C50 C51 H51 120.3 . . ?
C52 C51 H51 120.3 . . ?
C53 C52 C51 118.1(7) . . ?
C53 C52 H52 120.9 . . ?
C51 C52 H52 120.9 . . ?
N5 C53 C52 121.7(6) . . ?
N5 C53 C54 115.9(6) . . ?
C52 C53 C54 122.4(7) . . ?
N6 C54 C55 121.5(6) . . ?
N6 C54 C53 116.4(6) . . ?
C55 C54 C53 122.0(6) . . ?
C54 C55 C56 118.4(6) . . ?
C54 C55 H55 120.8 . . ?
C56 C55 H55 120.8 . . ?
C57 C56 C55 120.4(7) . . ?
C57 C56 H56 119.8 . . ?
C55 C56 H56 119.8 . . ?
C56 C57 C58 118.6(7) . . ?
C56 C57 H57 120.7 . . ?
C58 C57 H57 120.7 . . ?
N6 C58 C57 122.6(7) . . ?
N6 C58 H58 118.7 . . ?
C57 C58 H58 118.7 . . ?
O6 C59 O5 121.2(9) . . ?
O6 C59 C21 118.0(8) . . ?
O5 C59 C21 120.7(8) . . ?
O11 C60 O12 125.7(7) . . ?
O11 C60 C38 118.7(7) . . ?
O12 C60 C38 115.6(6) . . ?

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.023 0.000 0.500 670 134 ' '
_platon_squeeze_details          
;
;
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
C5 N1 C1 C2 0.9(10) . . . . ?
Zn1 N1 C1 C2 180.0(5) . . . . ?
N1 C1 C2 C3 -1.5(11) . . . . ?
C1 C2 C3 C4 2.6(11) . . . . ?
C2 C3 C4 C5 -3.3(11) . . . . ?
C1 N1 C5 C4 -1.6(9) . . . . ?
Zn1 N1 C5 C4 179.2(5) . . . . ?
C1 N1 C5 C6 -179.2(6) . . . . ?
Zn1 N1 C5 C6 1.6(7) . . . . ?
C3 C4 C5 N1 2.8(10) . . . . ?
C3 C4 C5 C6 -179.6(6) . . . . ?
C10 N2 C6 C7 -0.5(10) . . . . ?
Zn1 N2 C6 C7 -178.0(5) . . . . ?
C10 N2 C6 C5 178.6(6) . . . . ?
Zn1 N2 C6 C5 1.1(7) . . . . ?
N1 C5 C6 N2 -1.8(9) . . . . ?
C4 C5 C6 N2 -179.4(6) . . . . ?
N1 C5 C6 C7 177.2(6) . . . . ?
C4 C5 C6 C7 -0.4(10) . . . . ?
N2 C6 C7 C8 0.3(11) . . . . ?
C5 C6 C7 C8 -178.7(6) . . . . ?
C6 C7 C8 C9 0.0(11) . . . . ?
C7 C8 C9 C10 -0.2(12) . . . . ?
C6 N2 C10 C9 0.3(10) . . . . ?
Zn1 N2 C10 C9 177.5(5) . . . . ?
C8 C9 C10 N2 0.0(12) . . . . ?
Zn1 O1 C11 O2 6.3(11) . . . . ?
Zn1 O1 C11 C12 -172.0(5) . . . . ?
O2 C11 C12 C18 1.2(11) . . . . ?
O1 C11 C12 C18 179.7(6) . . . . ?
O2 C11 C12 C13 -174.7(7) . . . . ?
O1 C11 C12 C13 3.7(10) . . . . ?
C18 C12 C13 C14 1.0(10) . . . . ?
C11 C12 C13 C14 177.0(6) . . . . ?
C12 C13 C14 C16 -2.5(10) . . . . ?
C12 C13 C14 C15 178.9(6) . . . . ?
Zn2 O4 C15 O3 7.1(10) . . . . ?
Zn2 O4 C15 C14 -172.4(4) . . . . ?
C16 C14 C15 O3 -125.4(8) . . . . ?
C13 C14 C15 O3 53.1(10) . . . . ?
C16 C14 C15 O4 54.2(9) . . . . ?
C13 C14 C15 O4 -127.3(7) . . . . ?
C13 C14 C16 C17 3.2(10) . . . . ?
C15 C14 C16 C17 -178.4(6) . . . . ?
C13 C14 C16 C19 -173.7(6) . . . . ?
C15 C14 C16 C19 4.7(10) . . . . ?
C14 C16 C17 C18 -2.4(10) . . . . ?
C19 C16 C17 C18 174.6(6) . . . . ?
C13 C12 C18 C17 -0.2(10) . . . . ?
C11 C12 C18 C17 -176.3(6) . . . . ?
C16 C17 C18 C12 1.0(10) . . . . ?
C14 C16 C19 C24 53.3(10) . . . . ?
C17 C16 C19 C24 -123.5(7) . . . . ?
C14 C16 C19 C20 -129.2(7) . . . . ?
C17 C16 C19 C20 53.9(9) . . . . ?
C24 C19 C20 C21 -0.5(10) . . . . ?
C16 C19 C20 C21 -178.1(6) . . . . ?
C19 C20 C21 C22 1.0(10) . . . . ?
C19 C20 C21 C59 177.3(6) . . . . ?
C20 C21 C22 C23 -0.5(11) . . . . ?
C59 C21 C22 C23 -176.8(7) . . . . ?
C21 C22 C23 C24 -0.5(11) . . . . ?
C22 C23 C24 C19 1.0(12) . . . . ?
C20 C19 C24 C23 -0.5(11) . . . . ?
C16 C19 C24 C23 177.0(6) . . . . ?
C29 N3 C25 C26 3.2(14) . . . . ?
Zn2 N3 C25 C26 -178.9(7) . . . . ?
N3 C25 C26 C27 -3.2(15) . . . . ?
C25 C26 C27 C28 3.2(17) . . . . ?
C26 C27 C28 C29 -3.1(17) . . . . ?
C25 N3 C29 C28 -2.9(12) . . . . ?
Zn2 N3 C29 C28 178.8(7) . . . . ?
C25 N3 C29 C30 178.7(8) . . . . ?
Zn2 N3 C29 C30 0.4(9) . . . . ?
C27 C28 C29 N3 2.9(14) . . . . ?
C27 C28 C29 C30 -178.9(9) . . . . ?
C34 N4 C30 C31 -3.6(12) . . . . ?
Zn2 N4 C30 C31 179.3(6) . . . . ?
C34 N4 C30 C29 178.1(7) . . . . ?
Zn2 N4 C30 C29 1.0(9) . . . . ?
N3 C29 C30 N4 -1.0(11) . . . . ?
C28 C29 C30 N4 -179.4(7) . . . . ?
N3 C29 C30 C31 -179.2(7) . . . . ?
C28 C29 C30 C31 2.4(13) . . . . ?
N4 C30 C31 C32 2.9(13) . . . . ?
C29 C30 C31 C32 -179.0(9) . . . . ?
C30 C31 C32 C33 -0.6(17) . . . . ?
C31 C32 C33 C34 -0.9(15) . . . . ?
C30 N4 C34 C33 2.1(13) . . . . ?
Zn2 N4 C34 C33 178.9(5) . . . . ?
C32 C33 C34 N4 0.2(12) . . . . ?
O9 C35 C36 C37 -130.6(7) . . . . ?
O10 C35 C36 C37 46.8(9) . . . . ?
O9 C35 C36 C41 44.5(10) . . . . ?
O10 C35 C36 C41 -138.0(7) . . . . ?
C41 C36 C37 C38 0.9(10) . . . . ?
C35 C36 C37 C38 176.1(6) . . . . ?
C36 C37 C38 C39 -0.7(10) . . . . ?
C36 C37 C38 C60 177.3(7) . . . . ?
C37 C38 C39 C40 3.5(11) . . . . ?
C60 C38 C39 C40 -174.6(7) . . . . ?
C38 C39 C40 C41 -6.4(11) . . . . ?
C37 C36 C41 C40 -3.6(10) . . . . ?
C35 C36 C41 C40 -178.5(6) . . . . ?
C37 C36 C41 C42 -179.5(6) . . . . ?
C35 C36 C41 C42 5.6(11) . . . . ?
C39 C40 C41 C36 6.2(10) . . . . ?
C39 C40 C41 C42 -177.6(7) . . . . ?
C36 C41 C42 C43 41.7(10) . . . . ?
C40 C41 C42 C43 -134.2(7) . . . . ?
C36 C41 C42 C48 -142.0(7) . . . . ?
C40 C41 C42 C48 42.1(9) . . . . ?
C48 C42 C43 C44 1.4(11) . . . . ?
C41 C42 C43 C44 177.8(7) . . . . ?
C42 C43 C44 C45 -0.9(12) . . . . ?
C43 C44 C45 C46 0.5(12) . . . . ?
C44 C45 C46 C48 -0.6(11) . . . . ?
C44 C45 C46 C47 -178.8(7) . . . . ?
Zn3 O8 C47 O7 11.3(7) . . . . ?
Zn3 O8 C47 C46 -163.7(6) . . . . ?
Zn3 O7 C47 O8 -11.1(7) . . . . ?
Zn3 O7 C47 C46 163.9(6) . . . . ?
C48 C46 C47 O8 -13.3(11) . . . . ?
C45 C46 C47 O8 164.9(7) . . . . ?
C48 C46 C47 O7 171.7(7) . . . . ?
C45 C46 C47 O7 -10.1(11) . . . . ?
C48 C46 C47 Zn3 -95(2) . . . . ?
C45 C46 C47 Zn3 83(2) . . . . ?
C45 C46 C48 C42 1.2(10) . . . . ?
C47 C46 C48 C42 179.4(6) . . . . ?
C43 C42 C48 C46 -1.6(10) . . . . ?
C41 C42 C48 C46 -178.1(6) . . . . ?
C53 N5 C49 C50 -2.5(10) . . . . ?
Zn3 N5 C49 C50 174.6(5) . . . . ?
N5 C49 C50 C51 1.5(12) . . . . ?
C49 C50 C51 C52 0.1(12) . . . . ?
C50 C51 C52 C53 -0.7(11) . . . . ?
C49 N5 C53 C52 1.9(10) . . . . ?
Zn3 N5 C53 C52 -175.5(5) . . . . ?
C49 N5 C53 C54 -179.0(6) . . . . ?
Zn3 N5 C53 C54 3.6(8) . . . . ?
C51 C52 C53 N5 -0.4(10) . . . . ?
C51 C52 C53 C54 -179.4(6) . . . . ?
C58 N6 C54 C55 -1.0(10) . . . . ?
Zn3 N6 C54 C55 -178.1(5) . . . . ?
C58 N6 C54 C53 177.6(6) . . . . ?
Zn3 N6 C54 C53 0.4(7) . . . . ?
N5 C53 C54 N6 -2.7(9) . . . . ?
C52 C53 C54 N6 176.4(6) . . . . ?
N5 C53 C54 C55 175.9(6) . . . . ?
C52 C53 C54 C55 -5.1(11) . . . . ?
N6 C54 C55 C56 1.4(10) . . . . ?
C53 C54 C55 C56 -177.1(6) . . . . ?
C54 C55 C56 C57 -1.3(11) . . . . ?
C55 C56 C57 C58 0.8(11) . . . . ?
C54 N6 C58 C57 0.5(10) . . . . ?
Zn3 N6 C58 C57 177.3(5) . . . . ?
C56 C57 C58 N6 -0.4(11) . . . . ?
Zn1 O6 C59 O5 11.2(10) 1_565 . . . ?
Zn1 O6 C59 C21 -164.0(6) 1_565 . . . ?
C20 C21 C59 O6 -21.5(11) . . . . ?
C22 C21 C59 O6 154.8(7) . . . . ?
C20 C21 C59 O5 163.3(8) . . . . ?
C22 C21 C59 O5 -20.5(11) . . . . ?
Zn3 O12 C60 O11 4.9(11) 1_545 . . . ?
Zn3 O12 C60 C38 -173.0(4) 1_545 . . . ?
C39 C38 C60 O11 2.2(11) . . . . ?
C37 C38 C60 O11 -175.8(7) . . . . ?
C39 C38 C60 O12 -179.8(7) . . . . ?
C37 C38 C60 O12 2.2(10) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C58 H58 O7 0.93 2.60 3.141(9) 117.2 .
C57 H57 O2 0.93 2.30 3.064(9) 138.7 2_666
C55 H55 O8 0.93 2.47 3.282(8) 146.6 2_767
C49 H49 O16 0.93 2.61 3.180(9) 120.1 .
C34 H34 O15 0.93 2.63 3.168(12) 117.2 .
C31 H31 O9 0.93 2.51 3.434(13) 174.8 2_766
C28 H28 O9 0.93 2.30 3.221(12) 170.4 2_766
C9 H9 O11 0.93 2.42 3.187(9) 139.6 2_756
C7 H7 O6 0.93 2.60 3.426(9) 148.8 2_665
C1 H1 O13 0.93 2.57 3.147(8) 120.8 .
O16 H7W O3 0.82 2.00 2.695(7) 142.5 2_766
O15 H5W O9 0.82 1.85 2.667(6) 172.7 .
O13 H2W O10 0.82 1.95 2.700(6) 152.2 2_656

_refine_diff_density_max         1.116
_refine_diff_density_min         -0.773
_refine_diff_density_rms         0.099


# start Validation Reply Form
_vrf_PLAT910_I                   
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min) 23 Note
RESPONSE: Reduction of beam stop mask did not yield significant improvement.
Most of those missing srtong reflections appeared to be very strong and were
treated as overflows.
;
_vrf_PLAT990_I                   
;
PROBLEM: Deprecated .res/.hkl Input Style SQUEEZE Job ... ! Note
RESPONSE: Due to the disordered solvent water molecules.
;
# end Validation Reply Form

####################################################################### 
# 
# 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_435-13Ni
_database_code_depnum_ccdc_archive 'CCDC 2012742'
_audit_update_record             
;
2020-06-28 deposited with the CCDC.	2021-01-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C25 H24 N2 Ni O10'
_chemical_formula_weight         571.17

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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_H-M_alt        'P b c n'
_space_group_name_Hall           '-P 2n 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+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   11.8020(10)
_cell_length_b                   11.5305(9)
_cell_length_c                   35.723(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4861.3(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    16027
_cell_measurement_theta_min      3.362
_cell_measurement_theta_max      25.049

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_F_000             2368
_exptl_transmission_factor_min   0.820
_exptl_transmission_factor_max   0.834
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.210
_exptl_absorpt_coefficient_mu    0.862
_shelx_estimated_absorpt_T_min   0.826
_shelx_estimated_absorpt_T_max   0.840
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.826
_exptl_absorpt_correction_T_max  0.840
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APE-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16027
_diffrn_reflns_av_unetI/netI     0.1476
_diffrn_reflns_av_R_equivalents  0.1330
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_theta_min         3.362
_diffrn_reflns_theta_max         25.049
_diffrn_reflns_theta_full        25.049
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4295
_reflns_number_gt                2289
_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    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     'w=1/[σ²(Fo²)] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4295
_refine_ls_number_parameters     344
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1354
_refine_ls_R_factor_gt           0.0621
_refine_ls_wR_factor_ref         0.1051
_refine_ls_wR_factor_gt          0.0794
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_restrained_S_all      0.980
_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
Ni1 Ni 0.61238(6) 0.12610(5) 0.68976(2) 0.02116(19) Uani 1 1 d . . . . .
N1 N 0.6049(4) 0.2565(3) 0.64964(12) 0.0256(11) Uani 1 1 d . . . . .
N2 N 0.5818(5) 0.7295(4) 0.52236(15) 0.0495(16) Uani 1 1 d . . . . .
O1 O 0.5647(3) 0.0063(3) 0.65045(10) 0.0264(9) Uani 1 1 d . . . . .
O2 O 0.4527(3) -0.1024(3) 0.68671(10) 0.0332(10) Uani 1 1 d . . . . .
O3 O 0.7188(3) -0.3881(3) 0.67956(10) 0.0257(9) Uani 1 1 d . . . . .
O4 O 0.6611(3) -0.5238(3) 0.71992(11) 0.0325(10) Uani 1 1 d . . . . .
O5 O 0.4238(4) 0.1110(4) 0.52984(12) 0.0582(14) Uani 1 1 d . . . . .
H5 H 0.4145 0.1579 0.5129 0.087 Uiso 1 1 calc R U . . .
O6 O 0.2680(4) 0.0314(4) 0.50568(13) 0.0670(16) Uani 1 1 d . . . . .
O7 O 0.6205(3) 0.0023(2) 0.73173(9) 0.0278(9) Uani 1 1 d . . . . .
H1W H 0.5828 -0.0537 0.7226 0.033 Uiso 1 1 d R U . . .
H2W H 0.6864 -0.0182 0.7347 0.033 Uiso 1 1 d R U . . .
O8 O 0.6474(3) 0.2491(2) 0.73245(9) 0.0302(10) Uani 1 1 d . . . . .
H3W H 0.6454 0.3147 0.7236 0.036 Uiso 1 1 d R U . . .
H4W H 0.7054 0.2475 0.7413 0.036 Uiso 1 1 d R U . . .
O9 O 0.4410(3) 0.1450(3) 0.70272(9) 0.0291(9) Uani 1 1 d . . . . .
H5W H 0.4272 0.1874 0.7216 0.035 Uiso 1 1 d R U . . .
H6W H 0.4167 0.0841 0.7114 0.035 Uiso 1 1 d R U . . .
O10 O 0.8627(3) 0.2454(3) 0.76012(11) 0.0536(13) Uani 1 1 d . . . . .
H7W H 0.8869 0.2806 0.7792 0.064 Uiso 1 1 d R U . . .
H8W H 0.8765 0.1785 0.7503 0.064 Uiso 1 1 d R U . . .
C1 C 0.4883(5) -0.0692(4) 0.65545(15) 0.0234(13) Uani 1 1 d . . . . .
C2 C 0.4284(4) -0.1112(4) 0.62010(15) 0.0238(13) Uani 1 1 d . . . . .
C3 C 0.4189(5) -0.0330(4) 0.59079(15) 0.0273(14) Uani 1 1 d . . . . .
H3 H 0.4589 0.0363 0.5920 0.033 Uiso 1 1 calc R U . . .
C4 C 0.3519(5) -0.0547(4) 0.55978(16) 0.0309(15) Uani 1 1 d . . . . .
C5 C 0.3434(6) 0.0328(5) 0.52862(18) 0.0395(17) Uani 1 1 d . . . . .
C6 C 0.2917(5) -0.1572(4) 0.55784(16) 0.0373(16) Uani 1 1 d . . . . .
H6 H 0.2423 -0.1706 0.5380 0.045 Uiso 1 1 calc R U . . .
C7 C 0.3053(5) -0.2394(4) 0.58545(15) 0.0311(15) Uani 1 1 d . . . . .
H7A H 0.2678 -0.3100 0.5831 0.037 Uiso 1 1 calc R U . . .
C8 C 0.3727(5) -0.2204(4) 0.61645(15) 0.0234(13) Uani 1 1 d . . . . .
C9 C 0.3932(4) -0.3180(4) 0.64311(15) 0.0221(13) Uani 1 1 d . . . . .
C10 C 0.5012(5) -0.3408(4) 0.65630(14) 0.0226(13) Uani 1 1 d . . . . .
H10 H 0.5607 -0.2938 0.6485 0.027 Uiso 1 1 calc R U . . .
C11 C 0.5239(5) -0.4310(4) 0.68073(14) 0.0224(13) Uani 1 1 d . . . . .
C12 C 0.6431(5) -0.4503(4) 0.69453(15) 0.0229(13) Uani 1 1 d . . . . .
C13 C 0.4367(5) -0.5043(4) 0.69176(17) 0.0337(15) Uani 1 1 d . . . . .
H13 H 0.4515 -0.5651 0.7081 0.040 Uiso 1 1 calc R U . . .
C14 C 0.3287(5) -0.4871(4) 0.67854(16) 0.0351(16) Uani 1 1 d . . . . .
H14 H 0.2703 -0.5364 0.6857 0.042 Uiso 1 1 calc R U . . .
C15 C 0.3075(5) -0.3940(4) 0.65404(16) 0.0331(15) Uani 1 1 d . . . . .
H15 H 0.2345 -0.3830 0.6449 0.040 Uiso 1 1 calc R U . . .
C16 C 0.6954(5) 0.3229(4) 0.64253(15) 0.0298(15) Uani 1 1 d . . . . .
H16 H 0.7619 0.3086 0.6557 0.036 Uiso 1 1 calc R U . . .
C17 C 0.6947(5) 0.4114(4) 0.61664(15) 0.0275(14) Uani 1 1 d . . . . .
H17 H 0.7607 0.4534 0.6122 0.033 Uiso 1 1 calc R U . . .
C18 C 0.5969(5) 0.4387(4) 0.59709(15) 0.0255(14) Uani 1 1 d . . . . .
C19 C 0.5031(5) 0.3678(4) 0.60365(16) 0.0374(16) Uani 1 1 d . . . . .
H19 H 0.4359 0.3800 0.5906 0.045 Uiso 1 1 calc R U . . .
C20 C 0.5110(5) 0.2788(4) 0.62988(16) 0.0345(16) Uani 1 1 d . . . . .
H20 H 0.4477 0.2324 0.6339 0.041 Uiso 1 1 calc R U . . .
C21 C 0.5904(5) 0.5395(4) 0.57108(16) 0.0313(15) Uani 1 1 d . . . . .
C22 C 0.6746(6) 0.6231(5) 0.57107(17) 0.053(2) Uani 1 1 d . . . . .
H22 H 0.7363 0.6172 0.5872 0.064 Uiso 1 1 calc R U . . .
C23 C 0.6652(7) 0.7163(5) 0.5465(2) 0.061(2) Uani 1 1 d . . . . .
H23 H 0.7214 0.7728 0.5471 0.073 Uiso 1 1 calc R U . . .
C24 C 0.5006(6) 0.6501(5) 0.52288(18) 0.0464(18) Uani 1 1 d . . . . .
H24 H 0.4398 0.6586 0.5065 0.056 Uiso 1 1 calc R U . . .
C25 C 0.5020(6) 0.5550(5) 0.54664(16) 0.0392(17) Uani 1 1 d . . . . .
H25 H 0.4429 0.5017 0.5460 0.047 Uiso 1 1 calc R U . . .


_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
Ni1 O3 2.032(3) 8_765 ?
Ni1 O1 2.049(3) . ?
Ni1 O7 2.072(3) . ?
Ni1 N1 2.079(4) . ?
Ni1 O9 2.086(3) . ?
Ni1 O8 2.123(3) . ?
N1 C16 1.339(6) . ?
N1 C20 1.339(6) . ?
N2 C23 1.316(8) . ?
N2 C24 1.326(7) . ?
O1 C1 1.266(6) . ?
O2 C1 1.253(6) . ?
O3 C12 1.264(6) . ?
O3 Ni1 2.032(3) 8_755 ?
O4 C12 1.259(6) . ?
O5 C5 1.310(7) . ?
O5 H5 0.8200 . ?
O6 C5 1.209(7) . ?
O7 H1W 0.8491 . ?
O7 H2W 0.8200 . ?
O8 H3W 0.8200 . ?
O8 H4W 0.7542 . ?
O9 H5W 0.8484 . ?
O9 H6W 0.8200 . ?
O10 H7W 0.8446 . ?
O10 H8W 0.8624 . ?
C1 C2 1.526(7) . ?
C2 C3 1.386(6) . ?
C2 C8 1.427(7) . ?
C3 C4 1.383(7) . ?
C3 H3 0.9300 . ?
C4 C6 1.381(7) . ?
C4 C5 1.505(7) . ?
C6 C7 1.377(6) . ?
C6 H6 0.9300 . ?
C7 C8 1.381(7) . ?
C7 H7A 0.9300 . ?
C8 C9 1.493(6) . ?
C9 C10 1.385(7) . ?
C9 C15 1.394(7) . ?
C10 C11 1.383(6) . ?
C10 H10 0.9300 . ?
C11 C13 1.388(7) . ?
C11 C12 1.507(7) . ?
C13 C14 1.373(7) . ?
C13 H13 0.9300 . ?
C14 C15 1.407(7) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C17 1.378(6) . ?
C16 H16 0.9300 . ?
C17 C18 1.385(7) . ?
C17 H17 0.9300 . ?
C18 C19 1.396(7) . ?
C18 C21 1.490(7) . ?
C19 C20 1.393(6) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
C21 C25 1.372(7) . ?
C21 C22 1.385(8) . ?
C22 C23 1.393(7) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 C25 1.387(7) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Ni1 O1 95.28(14) 8_765 . ?
O3 Ni1 O7 91.65(13) 8_765 . ?
O1 Ni1 O7 92.53(13) . . ?
O3 Ni1 N1 88.65(16) 8_765 . ?
O1 Ni1 N1 90.20(15) . . ?
O7 Ni1 N1 177.21(15) . . ?
O3 Ni1 O9 177.14(14) 8_765 . ?
O1 Ni1 O9 87.49(14) . . ?
O7 Ni1 O9 87.48(13) . . ?
N1 Ni1 O9 92.08(15) . . ?
O3 Ni1 O8 89.52(14) 8_765 . ?
O1 Ni1 O8 175.04(14) . . ?
O7 Ni1 O8 86.06(12) . . ?
N1 Ni1 O8 91.18(14) . . ?
O9 Ni1 O8 87.70(13) . . ?
C16 N1 C20 116.8(5) . . ?
C16 N1 Ni1 120.7(4) . . ?
C20 N1 Ni1 122.5(4) . . ?
C23 N2 C24 116.9(6) . . ?
C1 O1 Ni1 124.2(3) . . ?
C12 O3 Ni1 131.5(3) . 8_755 ?
C5 O5 H5 109.5 . . ?
Ni1 O7 H1W 102.8 . . ?
Ni1 O7 H2W 109.6 . . ?
H1W O7 H2W 109.1 . . ?
Ni1 O8 H3W 109.5 . . ?
Ni1 O8 H4W 117.5 . . ?
H3W O8 H4W 102.1 . . ?
Ni1 O9 H5W 114.9 . . ?
Ni1 O9 H6W 109.5 . . ?
H5W O9 H6W 97.2 . . ?
H7W O10 H8W 134.0 . . ?
O2 C1 O1 125.1(5) . . ?
O2 C1 C2 119.0(5) . . ?
O1 C1 C2 115.5(5) . . ?
C3 C2 C8 117.9(5) . . ?
C3 C2 C1 117.2(5) . . ?
C8 C2 C1 124.7(5) . . ?
C4 C3 C2 122.3(5) . . ?
C4 C3 H3 118.9 . . ?
C2 C3 H3 118.9 . . ?
C6 C4 C3 119.3(5) . . ?
C6 C4 C5 120.1(6) . . ?
C3 C4 C5 120.6(5) . . ?
O6 C5 O5 124.4(6) . . ?
O6 C5 C4 122.8(6) . . ?
O5 C5 C4 112.8(6) . . ?
C7 C6 C4 119.6(6) . . ?
C7 C6 H6 120.2 . . ?
C4 C6 H6 120.2 . . ?
C6 C7 C8 122.2(5) . . ?
C6 C7 H7A 118.9 . . ?
C8 C7 H7A 118.9 . . ?
C7 C8 C2 118.6(5) . . ?
C7 C8 C9 119.0(5) . . ?
C2 C8 C9 122.1(5) . . ?
C10 C9 C15 116.9(5) . . ?
C10 C9 C8 120.6(5) . . ?
C15 C9 C8 122.3(5) . . ?
C11 C10 C9 122.4(5) . . ?
C11 C10 H10 118.8 . . ?
C9 C10 H10 118.8 . . ?
C10 C11 C13 119.6(5) . . ?
C10 C11 C12 119.8(5) . . ?
C13 C11 C12 120.6(5) . . ?
O4 C12 O3 124.5(5) . . ?
O4 C12 C11 119.5(5) . . ?
O3 C12 C11 116.0(5) . . ?
C14 C13 C11 120.1(5) . . ?
C14 C13 H13 119.9 . . ?
C11 C13 H13 119.9 . . ?
C13 C14 C15 119.3(5) . . ?
C13 C14 H14 120.4 . . ?
C15 C14 H14 120.4 . . ?
C9 C15 C14 121.6(5) . . ?
C9 C15 H15 119.2 . . ?
C14 C15 H15 119.2 . . ?
N1 C16 C17 123.1(5) . . ?
N1 C16 H16 118.4 . . ?
C17 C16 H16 118.4 . . ?
C16 C17 C18 120.8(5) . . ?
C16 C17 H17 119.6 . . ?
C18 C17 H17 119.6 . . ?
C17 C18 C19 116.3(5) . . ?
C17 C18 C21 122.3(5) . . ?
C19 C18 C21 121.3(5) . . ?
C20 C19 C18 119.4(5) . . ?
C20 C19 H19 120.3 . . ?
C18 C19 H19 120.3 . . ?
N1 C20 C19 123.5(5) . . ?
N1 C20 H20 118.3 . . ?
C19 C20 H20 118.3 . . ?
C25 C21 C22 117.0(5) . . ?
C25 C21 C18 122.5(5) . . ?
C22 C21 C18 120.4(6) . . ?
C21 C22 C23 118.7(6) . . ?
C21 C22 H22 120.7 . . ?
C23 C22 H22 120.7 . . ?
N2 C23 C22 124.2(7) . . ?
N2 C23 H23 117.9 . . ?
C22 C23 H23 117.9 . . ?
N2 C24 C25 123.1(6) . . ?
N2 C24 H24 118.5 . . ?
C25 C24 H24 118.5 . . ?
C21 C25 C24 120.1(6) . . ?
C21 C25 H25 119.9 . . ?
C24 C25 H25 119.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 O1 C1 O2 -19.9(7) . . . . ?
Ni1 O1 C1 C2 153.2(3) . . . . ?
O2 C1 C2 C3 143.3(5) . . . . ?
O1 C1 C2 C3 -30.3(7) . . . . ?
O2 C1 C2 C8 -30.6(8) . . . . ?
O1 C1 C2 C8 155.8(5) . . . . ?
C8 C2 C3 C4 4.3(8) . . . . ?
C1 C2 C3 C4 -169.9(5) . . . . ?
C2 C3 C4 C6 0.4(9) . . . . ?
C2 C3 C4 C5 179.6(5) . . . . ?
C6 C4 C5 O6 17.0(10) . . . . ?
C3 C4 C5 O6 -162.3(6) . . . . ?
C6 C4 C5 O5 -164.8(5) . . . . ?
C3 C4 C5 O5 16.0(8) . . . . ?
C3 C4 C6 C7 -4.5(9) . . . . ?
C5 C4 C6 C7 176.3(5) . . . . ?
C4 C6 C7 C8 3.8(9) . . . . ?
C6 C7 C8 C2 1.0(9) . . . . ?
C6 C7 C8 C9 -173.5(5) . . . . ?
C3 C2 C8 C7 -5.0(8) . . . . ?
C1 C2 C8 C7 168.8(5) . . . . ?
C3 C2 C8 C9 169.4(5) . . . . ?
C1 C2 C8 C9 -16.8(8) . . . . ?
C7 C8 C9 C10 134.4(6) . . . . ?
C2 C8 C9 C10 -39.9(8) . . . . ?
C7 C8 C9 C15 -41.6(8) . . . . ?
C2 C8 C9 C15 144.1(5) . . . . ?
C15 C9 C10 C11 -3.2(8) . . . . ?
C8 C9 C10 C11 -179.4(5) . . . . ?
C9 C10 C11 C13 2.1(8) . . . . ?
C9 C10 C11 C12 -179.1(5) . . . . ?
Ni1 O3 C12 O4 -2.6(8) 8_755 . . . ?
Ni1 O3 C12 C11 176.3(3) 8_755 . . . ?
C10 C11 C12 O4 172.0(5) . . . . ?
C13 C11 C12 O4 -9.2(8) . . . . ?
C10 C11 C12 O3 -7.0(7) . . . . ?
C13 C11 C12 O3 171.8(5) . . . . ?
C10 C11 C13 C14 -0.1(8) . . . . ?
C12 C11 C13 C14 -178.9(5) . . . . ?
C11 C13 C14 C15 -0.6(9) . . . . ?
C10 C9 C15 C14 2.5(8) . . . . ?
C8 C9 C15 C14 178.6(5) . . . . ?
C13 C14 C15 C9 -0.7(9) . . . . ?
C20 N1 C16 C17 0.7(8) . . . . ?
Ni1 N1 C16 C17 -179.1(4) . . . . ?
N1 C16 C17 C18 2.0(8) . . . . ?
C16 C17 C18 C19 -3.5(8) . . . . ?
C16 C17 C18 C21 175.2(5) . . . . ?
C17 C18 C19 C20 2.5(8) . . . . ?
C21 C18 C19 C20 -176.2(5) . . . . ?
C16 N1 C20 C19 -1.7(8) . . . . ?
Ni1 N1 C20 C19 178.1(4) . . . . ?
C18 C19 C20 N1 0.1(9) . . . . ?
C17 C18 C21 C25 167.8(6) . . . . ?
C19 C18 C21 C25 -13.6(9) . . . . ?
C17 C18 C21 C22 -12.9(8) . . . . ?
C19 C18 C21 C22 165.7(6) . . . . ?
C25 C21 C22 C23 -0.4(9) . . . . ?
C18 C21 C22 C23 -179.7(6) . . . . ?
C24 N2 C23 C22 2.4(11) . . . . ?
C21 C22 C23 N2 -1.4(11) . . . . ?
C23 N2 C24 C25 -1.6(10) . . . . ?
C22 C21 C25 C24 1.1(9) . . . . ?
C18 C21 C25 C24 -179.6(5) . . . . ?
N2 C24 C25 C21 -0.1(10) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O5 H5 N2 0.82 1.81 2.620(6) 170.1 5_666
O7 H1W O2 0.85 2.08 2.822(5) 146.1 .
O7 H2W O4 0.82 1.88 2.629(5) 152.2 8_765
O8 H3W O4 0.82 1.88 2.662(4) 160.0 1_565
O8 H4W O10 0.75 1.97 2.726(5) 175.0 .
O9 H5W O8 0.85 1.99 2.810(5) 160.7 3_656
O9 H6W O2 0.82 2.36 2.912(4) 125.1 .
O9 H6W O7 0.82 2.28 2.952(5) 139.4 3_656
O10 H7W O2 0.84 1.98 2.796(5) 163.7 6_667
O10 H8W O4 0.86 2.61 3.431(5) 159.3 8_765
C16 H16 O3 0.93 2.43 2.949(6) 114.9 8_765
C17 H17 O1 0.93 2.55 3.273(7) 135.3 8_765
O5 H5 N2 0.82 1.81 2.620(6) 170.1 5_666
O7 H1W O2 0.85 2.08 2.822(5) 146.1 .
O7 H2W O4 0.82 1.88 2.629(5) 152.2 8_765
O8 H3W O4 0.82 1.88 2.662(4) 160.0 1_565
O8 H4W O10 0.75 1.97 2.726(5) 175.0 .
O9 H5W O8 0.85 1.99 2.810(5) 160.7 3_656
O9 H6W O2 0.82 2.36 2.912(4) 125.1 .
O9 H6W O7 0.82 2.28 2.952(5) 139.4 3_656
O10 H7W O2 0.84 1.98 2.796(5) 163.7 6_667
O10 H8W O4 0.86 2.61 3.431(5) 159.3 8_765
C16 H16 O3 0.93 2.43 2.949(6) 114.9 8_765
C17 H17 O1 0.93 2.55 3.273(7) 135.3 8_765
C20 H20 O9 0.93 2.66 3.136(6) 112.6 .

_refine_diff_density_max         0.673
_refine_diff_density_min         -0.500
_refine_diff_density_rms         0.095


# start Validation Reply Form
_vrf_PLAT420_I                   
;
PROBLEM: D-H Without Acceptor O10--H8W Please Check
RESPONSE: No suitable acceptors were found.
;
# end Validation Reply Form

####################################################################### 
# 
# 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_437-14Zn
_database_code_depnum_ccdc_archive 'CCDC 2012749'
_audit_update_record             
;
2020-06-28 deposited with the CCDC.	2021-01-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H24 N2 O12 Zn3'
_chemical_formula_weight         920.72

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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/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'
'-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                   21.176(3)
_cell_length_b                   9.9222(18)
_cell_length_c                   17.4194(19)
_cell_angle_alpha                90
_cell_angle_beta                 95.754(12)
_cell_angle_gamma                90
_cell_volume                     3641.6(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6894
_cell_measurement_theta_min      3.337
_cell_measurement_theta_max      25.047

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_F_000             1856
_exptl_transmission_factor_min   0.633
_exptl_transmission_factor_max   0.666
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    2.030
_shelx_estimated_absorpt_T_min   0.652
_shelx_estimated_absorpt_T_max   0.687
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.652
_exptl_absorpt_correction_T_max  0.687
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APE-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6894
_diffrn_reflns_av_unetI/netI     0.1151
_diffrn_reflns_av_R_equivalents  0.0692
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.337
_diffrn_reflns_theta_max         25.047
_diffrn_reflns_theta_full        25.047
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3209
_reflns_number_gt                2017
_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    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0335P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3209
_refine_ls_number_parameters     259
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0992
_refine_ls_R_factor_gt           0.0546
_refine_ls_wR_factor_ref         0.1268
_refine_ls_wR_factor_gt          0.1008
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_restrained_S_all      1.012
_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
Zn1 Zn 0.90595(3) 0.74952(7) 1.03513(3) 0.0290(2) Uani 1 1 d . . . . .
Zn2 Zn 1.0000 1.0000 1.0000 0.0275(3) Uani 1 2 d S . P . .
N1 N 0.8253(2) 0.6458(5) 1.0476(3) 0.0357(14) Uani 1 1 d . . . . .
O1 O 0.89636(18) 0.7416(4) 0.9210(2) 0.0310(10) Uani 1 1 d . . . . .
O2 O 0.9657(2) 0.9031(4) 0.9021(2) 0.0360(11) Uani 1 1 d . . . . .
O3 O 0.91542(18) 1.0458(4) 0.55323(19) 0.0285(10) Uani 1 1 d . . . . .
O4 O 0.9024(3) 1.1554(5) 0.6600(2) 0.0581(15) Uani 1 1 d . . . . .
O5 O 0.9525(2) 0.1719(4) 0.9469(2) 0.0449(12) Uani 1 1 d . . . . .
O6 O 1.0171(2) 0.3459(5) 0.9300(2) 0.0435(12) Uani 1 1 d . . . . .
C1 C 0.9265(3) 0.8159(6) 0.8787(3) 0.0253(14) Uani 1 1 d . . . . .
C2 C 0.9126(3) 0.8038(6) 0.7924(3) 0.0238(14) Uani 1 1 d . . . . .
C3 C 0.9187(3) 0.9187(6) 0.7489(3) 0.0273(15) Uani 1 1 d . . . . .
H3 H 0.9312 0.9986 0.7739 0.033 Uiso 1 1 calc R U . . .
C4 C 0.9067(3) 0.9186(6) 0.6693(3) 0.0255(14) Uani 1 1 d . . . . .
C5 C 0.9092(3) 1.0480(7) 0.6275(3) 0.0318(16) Uani 1 1 d . . . . .
C6 C 0.8914(3) 0.8000(7) 0.6324(3) 0.0336(16) Uani 1 1 d . . . . .
H6 H 0.8865 0.7971 0.5788 0.040 Uiso 1 1 calc R U . . .
C7 C 0.8832(3) 0.6844(7) 0.6742(3) 0.0349(16) Uani 1 1 d . . . . .
H7 H 0.8713 0.6050 0.6482 0.042 Uiso 1 1 calc R U . . .
C8 C 0.8925(3) 0.6838(6) 0.7555(3) 0.0258(14) Uani 1 1 d . . . . .
C9 C 0.8794(3) 0.5538(6) 0.7942(3) 0.0271(15) Uani 1 1 d . . . . .
C10 C 0.9260(3) 0.4845(6) 0.8402(3) 0.0321(16) Uani 1 1 d . . . . .
H10 H 0.9663 0.5216 0.8495 0.039 Uiso 1 1 calc R U . . .
C11 C 0.9132(3) 0.3602(7) 0.8726(3) 0.0309(15) Uani 1 1 d . . . . .
C12 C 0.9649(3) 0.2848(7) 0.9210(3) 0.0353(17) Uani 1 1 d . . . . .
C13 C 0.8534(3) 0.3062(7) 0.8592(3) 0.0451(19) Uani 1 1 d . . . . .
H13 H 0.8452 0.2219 0.8792 0.054 Uiso 1 1 calc R U . . .
C14 C 0.8051(4) 0.3753(8) 0.8162(4) 0.055(2) Uani 1 1 d . . . . .
H14 H 0.7643 0.3398 0.8092 0.065 Uiso 1 1 calc R U . . .
C15 C 0.8188(3) 0.4989(7) 0.7838(3) 0.0423(17) Uani 1 1 d . . . . .
H15 H 0.7867 0.5456 0.7547 0.051 Uiso 1 1 calc R U . . .
C16 C 0.8029(3) 0.5615(8) 0.9937(4) 0.053(2) Uani 1 1 d . . . . .
H16 H 0.8262 0.5472 0.9520 0.063 Uiso 1 1 calc R U . . .
C17 C 0.7464(4) 0.4927(9) 0.9955(4) 0.066(2) Uani 1 1 d . . . . .
H17 H 0.7325 0.4333 0.9560 0.079 Uiso 1 1 calc R U . . .
C18 C 0.7116(4) 0.5126(9) 1.0551(5) 0.062(3) Uani 1 1 d . . . . .
H18 H 0.6729 0.4690 1.0568 0.075 Uiso 1 1 calc R U . . .
C19 C 0.7340(3) 0.5976(9) 1.1128(4) 0.062(3) Uani 1 1 d . . . . .
H19 H 0.7113 0.6108 1.1552 0.074 Uiso 1 1 calc R U . . .
C20 C 0.7909(3) 0.6641(8) 1.1077(4) 0.049(2) Uani 1 1 d . . . . .
H20 H 0.8058 0.7231 1.1469 0.059 Uiso 1 1 calc R U . . .


_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
Zn1 O6 1.929(4) 5_767 ?
Zn1 O1 1.980(4) . ?
Zn1 N1 2.024(5) . ?
Zn1 O3 2.062(4) 6_576 ?
Zn1 O4 2.379(4) 6_576 ?
Zn1 C5 2.571(6) 6_576 ?
Zn2 O2 2.027(4) 5_777 ?
Zn2 O2 2.027(4) . ?
Zn2 O5 2.142(4) 5_767 ?
Zn2 O5 2.142(4) 1_565 ?
Zn2 O3 2.146(4) 2_756 ?
Zn2 O3 2.146(4) 6_576 ?
N1 C16 1.312(8) . ?
N1 C20 1.346(7) . ?
O1 C1 1.259(6) . ?
O2 C1 1.240(7) . ?
O3 C5 1.314(6) . ?
O3 Zn1 2.062(4) 6_575 ?
O3 Zn2 2.146(4) 2_756 ?
O4 C5 1.222(7) . ?
O4 Zn1 2.379(4) 6_575 ?
O5 C12 1.245(7) . ?
O5 Zn2 2.142(4) 1_545 ?
O6 C12 1.258(7) . ?
O6 Zn1 1.929(4) 5_767 ?
C1 C2 1.507(7) . ?
C2 C3 1.383(8) . ?
C2 C8 1.399(8) . ?
C3 C4 1.384(7) . ?
C3 H3 0.9300 . ?
C4 C6 1.365(8) . ?
C4 C5 1.479(8) . ?
C5 Zn1 2.571(6) 6_575 ?
C6 C7 1.379(8) . ?
C6 H6 0.9300 . ?
C7 C8 1.411(7) . ?
C7 H7 0.9300 . ?
C8 C9 1.494(8) . ?
C9 C15 1.388(8) . ?
C9 C10 1.389(8) . ?
C10 C11 1.394(8) . ?
C10 H10 0.9300 . ?
C11 C13 1.373(8) . ?
C11 C12 1.511(8) . ?
C13 C14 1.387(9) . ?
C13 H13 0.9300 . ?
C14 C15 1.393(9) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C17 1.381(9) . ?
C16 H16 0.9300 . ?
C17 C18 1.347(10) . ?
C17 H17 0.9300 . ?
C18 C19 1.360(10) . ?
C18 H18 0.9300 . ?
C19 C20 1.385(9) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?

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
O6 Zn1 O1 107.19(17) 5_767 . ?
O6 Zn1 N1 114.3(2) 5_767 . ?
O1 Zn1 N1 94.89(18) . . ?
O6 Zn1 O3 111.67(18) 5_767 6_576 ?
O1 Zn1 O3 101.02(16) . 6_576 ?
N1 Zn1 O3 123.67(19) . 6_576 ?
O6 Zn1 O4 90.55(18) 5_767 6_576 ?
O1 Zn1 O4 157.59(17) . 6_576 ?
N1 Zn1 O4 89.93(19) . 6_576 ?
O3 Zn1 O4 58.75(15) 6_576 6_576 ?
O6 Zn1 C5 102.56(19) 5_767 6_576 ?
O1 Zn1 C5 130.78(19) . 6_576 ?
N1 Zn1 C5 107.4(2) . 6_576 ?
O3 Zn1 C5 30.51(16) 6_576 6_576 ?
O4 Zn1 C5 28.25(15) 6_576 6_576 ?
O2 Zn2 O2 180.0 5_777 . ?
O2 Zn2 O5 84.32(17) 5_777 5_767 ?
O2 Zn2 O5 95.68(17) . 5_767 ?
O2 Zn2 O5 95.68(17) 5_777 1_565 ?
O2 Zn2 O5 84.32(17) . 1_565 ?
O5 Zn2 O5 180.0(2) 5_767 1_565 ?
O2 Zn2 O3 91.07(15) 5_777 2_756 ?
O2 Zn2 O3 88.93(14) . 2_756 ?
O5 Zn2 O3 88.79(16) 5_767 2_756 ?
O5 Zn2 O3 91.21(16) 1_565 2_756 ?
O2 Zn2 O3 88.93(14) 5_777 6_576 ?
O2 Zn2 O3 91.07(15) . 6_576 ?
O5 Zn2 O3 91.21(16) 5_767 6_576 ?
O5 Zn2 O3 88.79(16) 1_565 6_576 ?
O3 Zn2 O3 180.0 2_756 6_576 ?
C16 N1 C20 117.3(6) . . ?
C16 N1 Zn1 119.8(4) . . ?
C20 N1 Zn1 122.9(5) . . ?
C1 O1 Zn1 123.9(4) . . ?
C1 O2 Zn2 141.2(4) . . ?
C5 O3 Zn1 96.7(4) . 6_575 ?
C5 O3 Zn2 126.8(4) . 2_756 ?
Zn1 O3 Zn2 102.41(16) 6_575 2_756 ?
C5 O4 Zn1 84.6(4) . 6_575 ?
C12 O5 Zn2 140.0(5) . 1_545 ?
C12 O6 Zn1 120.4(4) . 5_767 ?
O2 C1 O1 125.3(5) . . ?
O2 C1 C2 116.2(5) . . ?
O1 C1 C2 118.5(5) . . ?
C3 C2 C8 119.4(5) . . ?
C3 C2 C1 117.5(5) . . ?
C8 C2 C1 123.1(5) . . ?
C4 C3 C2 122.1(6) . . ?
C4 C3 H3 118.9 . . ?
C2 C3 H3 118.9 . . ?
C6 C4 C3 118.9(6) . . ?
C6 C4 C5 122.4(5) . . ?
C3 C4 C5 118.7(6) . . ?
O4 C5 O3 119.9(6) . . ?
O4 C5 C4 121.2(5) . . ?
O3 C5 C4 118.8(6) . . ?
O4 C5 Zn1 67.1(4) . 6_575 ?
O3 C5 Zn1 52.8(3) . 6_575 ?
C4 C5 Zn1 170.5(5) . 6_575 ?
C4 C6 C7 120.4(5) . . ?
C4 C6 H6 119.8 . . ?
C7 C6 H6 119.8 . . ?
C6 C7 C8 121.4(6) . . ?
C6 C7 H7 119.3 . . ?
C8 C7 H7 119.3 . . ?
C2 C8 C7 117.6(6) . . ?
C2 C8 C9 126.1(5) . . ?
C7 C8 C9 116.3(6) . . ?
C15 C9 C10 118.3(6) . . ?
C15 C9 C8 119.4(5) . . ?
C10 C9 C8 122.3(6) . . ?
C9 C10 C11 121.1(6) . . ?
C9 C10 H10 119.5 . . ?
C11 C10 H10 119.5 . . ?
C13 C11 C10 119.3(6) . . ?
C13 C11 C12 120.4(6) . . ?
C10 C11 C12 120.4(6) . . ?
O5 C12 O6 127.1(6) . . ?
O5 C12 C11 118.8(6) . . ?
O6 C12 C11 114.1(6) . . ?
C11 C13 C14 121.2(6) . . ?
C11 C13 H13 119.4 . . ?
C14 C13 H13 119.4 . . ?
C13 C14 C15 118.8(7) . . ?
C13 C14 H14 120.6 . . ?
C15 C14 H14 120.6 . . ?
C9 C15 C14 121.4(6) . . ?
C9 C15 H15 119.3 . . ?
C14 C15 H15 119.3 . . ?
N1 C16 C17 123.5(7) . . ?
N1 C16 H16 118.3 . . ?
C17 C16 H16 118.3 . . ?
C18 C17 C16 119.1(8) . . ?
C18 C17 H17 120.4 . . ?
C16 C17 H17 120.4 . . ?
C17 C18 C19 118.9(7) . . ?
C17 C18 H18 120.5 . . ?
C19 C18 H18 120.5 . . ?
C18 C19 C20 119.3(7) . . ?
C18 C19 H19 120.3 . . ?
C20 C19 H19 120.3 . . ?
N1 C20 C19 121.8(7) . . ?
N1 C20 H20 119.1 . . ?
C19 C20 H20 119.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Zn2 O2 C1 O1 -9.0(11) . . . . ?
Zn2 O2 C1 C2 168.2(4) . . . . ?
Zn1 O1 C1 O2 -0.2(9) . . . . ?
Zn1 O1 C1 C2 -177.3(4) . . . . ?
O2 C1 C2 C3 -29.2(8) . . . . ?
O1 C1 C2 C3 148.3(6) . . . . ?
O2 C1 C2 C8 152.6(6) . . . . ?
O1 C1 C2 C8 -29.9(8) . . . . ?
C8 C2 C3 C4 -1.4(9) . . . . ?
C1 C2 C3 C4 -179.7(5) . . . . ?
C2 C3 C4 C6 -3.2(9) . . . . ?
C2 C3 C4 C5 175.1(5) . . . . ?
Zn1 O4 C5 O3 1.5(6) 6_575 . . . ?
Zn1 O4 C5 C4 -174.7(6) 6_575 . . . ?
Zn1 O3 C5 O4 -1.8(7) 6_575 . . . ?
Zn2 O3 C5 O4 109.2(6) 2_756 . . . ?
Zn1 O3 C5 C4 174.5(5) 6_575 . . . ?
Zn2 O3 C5 C4 -74.5(7) 2_756 . . . ?
Zn2 O3 C5 Zn1 111.0(4) 2_756 . . 6_575 ?
C6 C4 C5 O4 156.0(7) . . . . ?
C3 C4 C5 O4 -22.3(9) . . . . ?
C6 C4 C5 O3 -20.3(9) . . . . ?
C3 C4 C5 O3 161.5(5) . . . . ?
C3 C4 C6 C7 5.0(9) . . . . ?
C5 C4 C6 C7 -173.2(6) . . . . ?
C4 C6 C7 C8 -2.3(10) . . . . ?
C3 C2 C8 C7 4.0(8) . . . . ?
C1 C2 C8 C7 -177.8(5) . . . . ?
C3 C2 C8 C9 -175.6(6) . . . . ?
C1 C2 C8 C9 2.6(9) . . . . ?
C6 C7 C8 C2 -2.3(9) . . . . ?
C6 C7 C8 C9 177.4(6) . . . . ?
C2 C8 C9 C15 118.7(7) . . . . ?
C7 C8 C9 C15 -60.9(8) . . . . ?
C2 C8 C9 C10 -61.6(8) . . . . ?
C7 C8 C9 C10 118.7(6) . . . . ?
C15 C9 C10 C11 2.7(8) . . . . ?
C8 C9 C10 C11 -176.9(5) . . . . ?
C9 C10 C11 C13 -0.5(9) . . . . ?
C9 C10 C11 C12 178.6(5) . . . . ?
Zn2 O5 C12 O6 -12.5(11) 1_545 . . . ?
Zn2 O5 C12 C11 167.0(4) 1_545 . . . ?
Zn1 O6 C12 O5 16.3(9) 5_767 . . . ?
Zn1 O6 C12 C11 -163.2(3) 5_767 . . . ?
C13 C11 C12 O5 1.5(9) . . . . ?
C10 C11 C12 O5 -177.5(6) . . . . ?
C13 C11 C12 O6 -178.9(6) . . . . ?
C10 C11 C12 O6 2.0(8) . . . . ?
C10 C11 C13 C14 -2.3(10) . . . . ?
C12 C11 C13 C14 178.6(6) . . . . ?
C11 C13 C14 C15 2.7(11) . . . . ?
C10 C9 C15 C14 -2.2(10) . . . . ?
C8 C9 C15 C14 177.4(6) . . . . ?
C13 C14 C15 C9 -0.4(11) . . . . ?
C20 N1 C16 C17 0.5(10) . . . . ?
Zn1 N1 C16 C17 -176.1(6) . . . . ?
N1 C16 C17 C18 0.5(12) . . . . ?
C16 C17 C18 C19 -1.6(12) . . . . ?
C17 C18 C19 C20 1.8(11) . . . . ?
C16 N1 C20 C19 -0.3(10) . . . . ?
Zn1 N1 C20 C19 176.3(5) . . . . ?
C18 C19 C20 N1 -0.9(11) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C20 H20 O4 0.93 2.36 3.029(9) 128.1 6_576
C16 H16 O1 0.93 2.53 3.037(8) 114.9 .
C16 H16 O1 0.93 2.53 3.037(8) 114.9 .
C20 H20 O4 0.93 2.36 3.029(9) 128.1 6_576

_refine_diff_density_max         1.232
_refine_diff_density_min         -0.508
_refine_diff_density_rms         0.115

####################################################################### 
# 
# 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_437-10Cd
_database_code_depnum_ccdc_archive 'CCDC 2012747'
_audit_update_record             
;
2020-06-28 deposited with the CCDC.	2021-01-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C60 H46 Cd3 N6 O16'
_chemical_formula_weight         1444.23

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'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 2/c'
_space_group_name_Hall           '-P 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, -y, -z'
'x, -y, z-1/2'

_cell_length_a                   14.9487(6)
_cell_length_b                   9.2003(3)
_cell_length_c                   20.4618(9)
_cell_angle_alpha                90
_cell_angle_beta                 96.401(4)
_cell_angle_gamma                90
_cell_volume                     2796.62(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    10097
_cell_measurement_theta_min      3.378
_cell_measurement_theta_max      25.048

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_F_000             1440
_exptl_transmission_factor_min   0.765
_exptl_transmission_factor_max   0.805
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    1.208
_shelx_estimated_absorpt_T_min   0.769
_shelx_estimated_absorpt_T_max   0.812
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.769
_exptl_absorpt_correction_T_max  0.812
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APE-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10097
_diffrn_reflns_av_unetI/netI     0.0925
_diffrn_reflns_av_R_equivalents  0.0519
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.378
_diffrn_reflns_theta_max         25.048
_diffrn_reflns_theta_full        25.048
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             4934
_reflns_number_gt                3517
_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    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0342P)²+0.2355P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4934
_refine_ls_number_parameters     384
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0795
_refine_ls_R_factor_gt           0.0504
_refine_ls_wR_factor_ref         0.1204
_refine_ls_wR_factor_gt          0.0992
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_restrained_S_all      1.074
_refine_ls_shift/su_max          0.000
_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
Cd1 Cd 0.01379(3) 0.77759(5) 0.33305(2) 0.02736(16) Uani 1 1 d . . . . .
Cd2 Cd 0.5000 0.51575(7) 0.2500 0.0384(2) Uani 1 2 d S T P . .
N1 N 0.1115(3) 0.6948(6) 0.4229(3) 0.0325(13) Uani 1 1 d . . . . .
N2 N -0.0481(3) 0.8240(6) 0.4321(3) 0.0343(13) Uani 1 1 d . . . . .
N3 N 0.4402(4) 0.3176(6) 0.1965(3) 0.0488(16) Uani 1 1 d . . . . .
O1 O 0.1222(2) 0.9317(4) 0.3130(2) 0.0292(10) Uani 1 1 d . . . . .
O2 O 0.0795(3) 0.9688(4) 0.2057(2) 0.0349(11) Uani 1 1 d . . . . .
O3 O 0.0205(3) 1.4989(5) 0.1649(2) 0.0409(12) Uani 1 1 d . . . . .
O4 O 0.0985(3) 1.6553(4) 0.2305(3) 0.0462(13) Uani 1 1 d . . . . .
O5 O 0.4695(3) 0.6269(5) 0.3529(3) 0.0542(14) Uani 1 1 d . . . . .
O6 O 0.3949(3) 0.6929(5) 0.2599(3) 0.0451(13) Uani 1 1 d . . . . .
O7 O 0.2591(3) 0.7342(6) 0.1602(3) 0.083(2) Uani 1 1 d . . . . .
H1W H 0.3016 0.7220 0.1909 0.099 Uiso 1 1 d R U . . .
H2W H 0.2137 0.7126 0.1798 0.099 Uiso 1 1 d R U . . .
O8 O 0.6307(5) 0.7073(9) 0.4417(4) 0.133(3) Uani 1 1 d . . . . .
H3W H 0.6645 0.7145 0.4111 0.159 Uiso 1 1 d R U . . .
H4W H 0.5840 0.6839 0.4164 0.159 Uiso 1 1 d R U . . .
C1 C 0.1196(4) 1.0034(6) 0.2612(3) 0.0216(13) Uani 1 1 d . . . . .
C2 C 0.1654(4) 1.1509(6) 0.2645(3) 0.0214(13) Uani 1 1 d . . . . .
C3 C 0.2462(4) 1.1828(6) 0.3038(3) 0.0239(14) Uani 1 1 d . . . . .
C4 C 0.2764(4) 1.3271(7) 0.3058(3) 0.0320(16) Uani 1 1 d . . . . .
H4 H 0.3321 1.3489 0.3286 0.038 Uiso 1 1 calc R U . . .
C5 C 0.2253(4) 1.4388(7) 0.2745(3) 0.0333(16) Uani 1 1 d . . . . .
H5 H 0.2459 1.5341 0.2782 0.040 Uiso 1 1 calc R U . . .
C6 C 0.1431(4) 1.4076(6) 0.2375(3) 0.0249(14) Uani 1 1 d . . . . .
C7 C 0.0828(4) 1.5268(7) 0.2078(3) 0.0313(16) Uani 1 1 d . . . . .
C8 C 0.1157(4) 1.2633(6) 0.2312(3) 0.0259(14) Uani 1 1 d . . . . .
H8 H 0.0633 1.2407 0.2042 0.031 Uiso 1 1 calc R U . . .
C9 C 0.3022(3) 1.0725(6) 0.3430(3) 0.0255(14) Uani 1 1 d . . . . .
C10 C 0.3265(4) 0.9421(6) 0.3160(3) 0.0272(15) Uani 1 1 d . . . . .
H10 H 0.3049 0.9193 0.2728 0.033 Uiso 1 1 calc R U . . .
C11 C 0.3833(4) 0.8442(7) 0.3531(3) 0.0306(15) Uani 1 1 d . . . . .
C12 C 0.4166(4) 0.7120(7) 0.3209(4) 0.0333(16) Uani 1 1 d . . . . .
C13 C 0.4124(4) 0.8752(8) 0.4187(4) 0.0410(18) Uani 1 1 d . . . . .
H13 H 0.4478 0.8086 0.4441 0.049 Uiso 1 1 calc R U . . .
C14 C 0.3889(4) 1.0040(8) 0.4457(3) 0.0434(19) Uani 1 1 d . . . . .
H14 H 0.4090 1.0252 0.4893 0.052 Uiso 1 1 calc R U . . .
C15 C 0.3350(4) 1.1035(8) 0.4081(3) 0.0392(17) Uani 1 1 d . . . . .
H15 H 0.3207 1.1916 0.4266 0.047 Uiso 1 1 calc R U . . .
C16 C 0.1900(5) 0.6307(9) 0.4159(4) 0.054(2) Uani 1 1 d . . . . .
H16 H 0.2163 0.6464 0.3774 0.065 Uiso 1 1 calc R U . . .
C17 C 0.2338(5) 0.5411(10) 0.4641(5) 0.066(3) Uani 1 1 d . . . . .
H17 H 0.2883 0.4971 0.4582 0.079 Uiso 1 1 calc R U . . .
C18 C 0.1939(6) 0.5199(9) 0.5207(5) 0.071(3) Uani 1 1 d . . . . .
H18 H 0.2213 0.4594 0.5534 0.085 Uiso 1 1 calc R U . . .
C19 C 0.1156(5) 0.5858(8) 0.5293(4) 0.054(2) Uani 1 1 d . . . . .
H19 H 0.0887 0.5716 0.5676 0.065 Uiso 1 1 calc R U . . .
C20 C 0.0758(4) 0.6757(7) 0.4794(3) 0.0365(16) Uani 1 1 d . . . . .
C21 C -0.0069(4) 0.7605(8) 0.4868(3) 0.0383(17) Uani 1 1 d . . . . .
C22 C -0.0400(5) 0.7820(10) 0.5474(4) 0.057(2) Uani 1 1 d . . . . .
H22 H -0.0122 0.7363 0.5849 0.068 Uiso 1 1 calc R U . . .
C23 C -0.1133(5) 0.8704(11) 0.5519(4) 0.068(3) Uani 1 1 d . . . . .
H23 H -0.1345 0.8856 0.5924 0.082 Uiso 1 1 calc R U . . .
C24 C -0.1551(5) 0.9366(9) 0.4962(4) 0.059(2) Uani 1 1 d . . . . .
H24 H -0.2050 0.9963 0.4978 0.070 Uiso 1 1 calc R U . . .
C25 C -0.1191(4) 0.9096(8) 0.4375(4) 0.0462(19) Uani 1 1 d . . . . .
H25 H -0.1463 0.9540 0.3995 0.055 Uiso 1 1 calc R U . . .
C26 C 0.4670(4) 0.1873(7) 0.2200(4) 0.0384(17) Uani 1 1 d . . . . .
C27 C 0.4337(5) 0.0605(8) 0.1893(4) 0.049(2) Uani 1 1 d . . . . .
H27 H 0.4537 -0.0294 0.2058 0.059 Uiso 1 1 calc R U . . .
C28 C 0.3715(6) 0.0673(9) 0.1350(5) 0.075(3) Uani 1 1 d . . . . .
H28 H 0.3478 -0.0170 0.1149 0.090 Uiso 1 1 calc R U . . .
C29 C 0.3449(7) 0.2033(9) 0.1107(5) 0.093(4) Uani 1 1 d . . . . .
H29 H 0.3041 0.2124 0.0732 0.112 Uiso 1 1 calc R U . . .
C30 C 0.3806(6) 0.3249(9) 0.1437(5) 0.081(3) Uani 1 1 d . . . . .
H30 H 0.3618 0.4161 0.1281 0.097 Uiso 1 1 calc R U . . .


_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
Cd1 O1 2.226(4) . ?
Cd1 O4 2.300(4) 2_545 ?
Cd1 O2 2.328(4) 2 ?
Cd1 N1 2.344(5) . ?
Cd1 N2 2.359(5) . ?
Cd1 O3 2.616(4) 2_545 ?
Cd1 Cd1 3.3776(9) 2 ?
Cd2 N3 2.259(6) 2_655 ?
Cd2 N3 2.259(6) . ?
Cd2 O6 2.289(4) . ?
Cd2 O6 2.289(4) 2_655 ?
Cd2 O5 2.429(5) 2_655 ?
Cd2 O5 2.429(5) . ?
Cd2 C12 2.706(6) 2_655 ?
N1 C16 1.335(8) . ?
N1 C20 1.339(8) . ?
N2 C25 1.336(8) . ?
N2 C21 1.350(8) . ?
N3 C30 1.323(10) . ?
N3 C26 1.336(8) . ?
O1 C1 1.247(7) . ?
O2 C1 1.264(7) . ?
O2 Cd1 2.328(4) 2 ?
O3 C7 1.232(8) . ?
O3 Cd1 2.616(4) 2_565 ?
O4 C7 1.282(7) . ?
O4 Cd1 2.300(4) 2_565 ?
O5 C12 1.245(7) . ?
O6 C12 1.268(8) . ?
O7 H1W 0.8500 . ?
O7 H2W 0.8500 . ?
O8 H3W 0.8499 . ?
O8 H4W 0.8501 . ?
C1 C2 1.518(7) . ?
C2 C3 1.405(8) . ?
C2 C8 1.405(8) . ?
C3 C4 1.401(8) . ?
C3 C9 1.493(8) . ?
C4 C5 1.393(8) . ?
C4 H4 0.9300 . ?
C5 C6 1.400(8) . ?
C5 H5 0.9300 . ?
C6 C8 1.391(7) . ?
C6 C7 1.504(8) . ?
C8 H8 0.9300 . ?
C9 C10 1.386(8) . ?
C9 C15 1.396(9) . ?
C10 C11 1.402(8) . ?
C10 H10 0.9300 . ?
C11 C13 1.393(9) . ?
C11 C12 1.495(8) . ?
C13 C14 1.370(9) . ?
C13 H13 0.9300 . ?
C14 C15 1.393(8) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C17 1.392(10) . ?
C16 H16 0.9300 . ?
C17 C18 1.375(11) . ?
C17 H17 0.9300 . ?
C18 C19 1.347(10) . ?
C18 H18 0.9300 . ?
C19 C20 1.394(9) . ?
C19 H19 0.9300 . ?
C20 C21 1.484(9) . ?
C21 C22 1.400(9) . ?
C22 C23 1.376(10) . ?
C22 H22 0.9300 . ?
C23 C24 1.379(11) . ?
C23 H23 0.9300 . ?
C24 C25 1.393(10) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
C26 C27 1.391(9) . ?
C26 C26 1.486(14) 2_655 ?
C27 C28 1.368(10) . ?
C27 H27 0.9300 . ?
C28 C29 1.388(11) . ?
C28 H28 0.9300 . ?
C29 C30 1.383(11) . ?
C29 H29 0.9300 . ?
C30 H30 0.9300 . ?

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 Cd1 O4 135.12(17) . 2_545 ?
O1 Cd1 O2 82.93(15) . 2 ?
O4 Cd1 O2 78.78(14) 2_545 2 ?
O1 Cd1 N1 87.01(16) . . ?
O4 Cd1 N1 129.51(17) 2_545 . ?
O2 Cd1 N1 144.09(17) 2 . ?
O1 Cd1 N2 113.97(17) . . ?
O4 Cd1 N2 104.04(18) 2_545 . ?
O2 Cd1 N2 83.04(17) 2 . ?
N1 Cd1 N2 69.82(18) . . ?
O1 Cd1 O3 140.81(14) . 2_545 ?
O4 Cd1 O3 52.94(14) 2_545 2_545 ?
O2 Cd1 O3 129.42(14) 2 2_545 ?
N1 Cd1 O3 77.02(16) . 2_545 ?
N2 Cd1 O3 93.88(17) . 2_545 ?
O1 Cd1 Cd1 79.90(11) . 2 ?
O4 Cd1 Cd1 55.37(13) 2_545 2 ?
O2 Cd1 Cd1 69.86(11) 2 2 ?
N1 Cd1 Cd1 141.68(13) . 2 ?
N2 Cd1 Cd1 148.09(13) . 2 ?
O3 Cd1 Cd1 90.78(10) 2_545 2 ?
N3 Cd2 N3 72.4(3) 2_655 . ?
N3 Cd2 O6 140.4(2) 2_655 . ?
N3 Cd2 O6 112.27(19) . . ?
N3 Cd2 O6 112.27(19) 2_655 2_655 ?
N3 Cd2 O6 140.4(2) . 2_655 ?
O6 Cd2 O6 89.1(2) . 2_655 ?
N3 Cd2 O5 131.1(2) 2_655 2_655 ?
N3 Cd2 O5 91.3(2) . 2_655 ?
O6 Cd2 O5 88.49(18) . 2_655 ?
O6 Cd2 O5 55.01(17) 2_655 2_655 ?
N3 Cd2 O5 91.3(2) 2_655 . ?
N3 Cd2 O5 131.1(2) . . ?
O6 Cd2 O5 55.01(17) . . ?
O6 Cd2 O5 88.49(18) 2_655 . ?
O5 Cd2 O5 130.2(2) 2_655 . ?
N3 Cd2 C12 128.1(2) 2_655 2_655 ?
N3 Cd2 C12 117.4(2) . 2_655 ?
O6 Cd2 C12 86.21(17) . 2_655 ?
O6 Cd2 C12 27.84(18) 2_655 2_655 ?
O5 Cd2 C12 27.37(17) 2_655 2_655 ?
O5 Cd2 C12 109.04(19) . 2_655 ?
C16 N1 C20 118.3(6) . . ?
C16 N1 Cd1 122.5(5) . . ?
C20 N1 Cd1 116.5(4) . . ?
C25 N2 C21 118.7(6) . . ?
C25 N2 Cd1 124.7(5) . . ?
C21 N2 Cd1 116.6(4) . . ?
C30 N3 C26 119.2(7) . . ?
C30 N3 Cd2 123.2(5) . . ?
C26 N3 Cd2 117.6(5) . . ?
C1 O1 Cd1 122.6(4) . . ?
C1 O2 Cd1 134.7(4) . 2 ?
C7 O3 Cd1 85.3(4) . 2_565 ?
C7 O4 Cd1 98.8(4) . 2_565 ?
C12 O5 Cd2 88.8(4) . . ?
C12 O6 Cd2 94.7(4) . . ?
H1W O7 H2W 100.9 . . ?
H3W O8 H4W 94.9 . . ?
O1 C1 O2 126.7(5) . . ?
O1 C1 C2 117.7(5) . . ?
O2 C1 C2 115.6(5) . . ?
C3 C2 C8 119.9(5) . . ?
C3 C2 C1 124.5(5) . . ?
C8 C2 C1 115.2(5) . . ?
C4 C3 C2 117.9(6) . . ?
C4 C3 C9 118.0(5) . . ?
C2 C3 C9 124.1(5) . . ?
C5 C4 C3 121.8(6) . . ?
C5 C4 H4 119.1 . . ?
C3 C4 H4 119.1 . . ?
C4 C5 C6 120.1(6) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C8 C6 C5 118.5(5) . . ?
C8 C6 C7 120.1(5) . . ?
C5 C6 C7 121.3(5) . . ?
O3 C7 O4 122.9(6) . . ?
O3 C7 C6 120.4(6) . . ?
O4 C7 C6 116.6(6) . . ?
C6 C8 C2 121.6(5) . . ?
C6 C8 H8 119.2 . . ?
C2 C8 H8 119.2 . . ?
C10 C9 C15 118.6(6) . . ?
C10 C9 C3 122.0(6) . . ?
C15 C9 C3 119.4(6) . . ?
C9 C10 C11 120.6(6) . . ?
C9 C10 H10 119.7 . . ?
C11 C10 H10 119.7 . . ?
C13 C11 C10 119.7(6) . . ?
C13 C11 C12 120.5(6) . . ?
C10 C11 C12 119.7(6) . . ?
O5 C12 O6 120.6(6) . . ?
O5 C12 C11 120.2(6) . . ?
O6 C12 C11 119.0(6) . . ?
C14 C13 C11 119.9(6) . . ?
C14 C13 H13 120.0 . . ?
C11 C13 H13 120.0 . . ?
C13 C14 C15 120.3(6) . . ?
C13 C14 H14 119.9 . . ?
C15 C14 H14 119.9 . . ?
C14 C15 C9 120.8(6) . . ?
C14 C15 H15 119.6 . . ?
C9 C15 H15 119.6 . . ?
N1 C16 C17 122.4(7) . . ?
N1 C16 H16 118.8 . . ?
C17 C16 H16 118.8 . . ?
C18 C17 C16 117.9(8) . . ?
C18 C17 H17 121.1 . . ?
C16 C17 H17 121.1 . . ?
C19 C18 C17 120.7(8) . . ?
C19 C18 H18 119.7 . . ?
C17 C18 H18 119.7 . . ?
C18 C19 C20 118.6(7) . . ?
C18 C19 H19 120.7 . . ?
C20 C19 H19 120.7 . . ?
N1 C20 C19 122.1(7) . . ?
N1 C20 C21 115.9(6) . . ?
C19 C20 C21 122.0(7) . . ?
N2 C21 C22 120.0(7) . . ?
N2 C21 C20 116.9(6) . . ?
C22 C21 C20 123.1(7) . . ?
C23 C22 C21 120.3(8) . . ?
C23 C22 H22 119.8 . . ?
C21 C22 H22 119.8 . . ?
C22 C23 C24 119.8(7) . . ?
C22 C23 H23 120.1 . . ?
C24 C23 H23 120.1 . . ?
C23 C24 C25 116.8(8) . . ?
C23 C24 H24 121.6 . . ?
C25 C24 H24 121.6 . . ?
N2 C25 C24 124.2(8) . . ?
N2 C25 H25 117.9 . . ?
C24 C25 H25 117.9 . . ?
N3 C26 C27 120.8(7) . . ?
N3 C26 C26 116.2(4) . 2_655 ?
C27 C26 C26 123.0(4) . 2_655 ?
C28 C27 C26 120.4(7) . . ?
C28 C27 H27 119.8 . . ?
C26 C27 H27 119.8 . . ?
C27 C28 C29 118.2(8) . . ?
C27 C28 H28 120.9 . . ?
C29 C28 H28 120.9 . . ?
C30 C29 C28 118.4(8) . . ?
C30 C29 H29 120.8 . . ?
C28 C29 H29 120.8 . . ?
N3 C30 C29 123.0(8) . . ?
N3 C30 H30 118.5 . . ?
C29 C30 H30 118.5 . . ?

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
Cd1 O1 C1 O2 -27.3(8) . . . . ?
Cd1 O1 C1 C2 149.8(4) . . . . ?
Cd1 O2 C1 O1 4.1(9) 2 . . . ?
Cd1 O2 C1 C2 -173.0(3) 2 . . . ?
O1 C1 C2 C3 37.0(8) . . . . ?
O2 C1 C2 C3 -145.6(6) . . . . ?
O1 C1 C2 C8 -135.4(5) . . . . ?
O2 C1 C2 C8 42.0(7) . . . . ?
C8 C2 C3 C4 -2.7(9) . . . . ?
C1 C2 C3 C4 -174.9(5) . . . . ?
C8 C2 C3 C9 177.7(5) . . . . ?
C1 C2 C3 C9 5.6(9) . . . . ?
C2 C3 C4 C5 5.1(9) . . . . ?
C9 C3 C4 C5 -175.3(6) . . . . ?
C3 C4 C5 C6 -2.7(10) . . . . ?
C4 C5 C6 C8 -2.1(9) . . . . ?
C4 C5 C6 C7 174.9(6) . . . . ?
Cd1 O3 C7 O4 1.1(6) 2_565 . . . ?
Cd1 O3 C7 C6 179.3(5) 2_565 . . . ?
Cd1 O4 C7 O3 -1.3(7) 2_565 . . . ?
Cd1 O4 C7 C6 -179.6(4) 2_565 . . . ?
C8 C6 C7 O3 -17.8(9) . . . . ?
C5 C6 C7 O3 165.3(6) . . . . ?
C8 C6 C7 O4 160.5(6) . . . . ?
C5 C6 C7 O4 -16.4(9) . . . . ?
C5 C6 C8 C2 4.4(9) . . . . ?
C7 C6 C8 C2 -172.6(5) . . . . ?
C3 C2 C8 C6 -2.0(9) . . . . ?
C1 C2 C8 C6 170.8(6) . . . . ?
C4 C3 C9 C10 -130.4(6) . . . . ?
C2 C3 C9 C10 49.2(8) . . . . ?
C4 C3 C9 C15 46.5(8) . . . . ?
C2 C3 C9 C15 -133.9(6) . . . . ?
C15 C9 C10 C11 -0.5(8) . . . . ?
C3 C9 C10 C11 176.4(5) . . . . ?
C9 C10 C11 C13 2.8(9) . . . . ?
C9 C10 C11 C12 -173.4(5) . . . . ?
Cd2 O5 C12 O6 9.2(6) . . . . ?
Cd2 O5 C12 C11 -166.2(5) . . . . ?
Cd2 O6 C12 O5 -9.8(7) . . . . ?
Cd2 O6 C12 C11 165.7(5) . . . . ?
C13 C11 C12 O5 1.4(9) . . . . ?
C10 C11 C12 O5 177.6(6) . . . . ?
C13 C11 C12 O6 -174.1(6) . . . . ?
C10 C11 C12 O6 2.1(9) . . . . ?
C10 C11 C13 C14 -3.0(9) . . . . ?
C12 C11 C13 C14 173.2(6) . . . . ?
C11 C13 C14 C15 0.8(10) . . . . ?
C13 C14 C15 C9 1.6(10) . . . . ?
C10 C9 C15 C14 -1.7(9) . . . . ?
C3 C9 C15 C14 -178.7(5) . . . . ?
C20 N1 C16 C17 2.4(11) . . . . ?
Cd1 N1 C16 C17 -158.7(6) . . . . ?
N1 C16 C17 C18 -0.3(13) . . . . ?
C16 C17 C18 C19 -1.0(14) . . . . ?
C17 C18 C19 C20 0.1(13) . . . . ?
C16 N1 C20 C19 -3.3(10) . . . . ?
Cd1 N1 C20 C19 158.9(5) . . . . ?
C16 N1 C20 C21 174.5(6) . . . . ?
Cd1 N1 C20 C21 -23.4(7) . . . . ?
C18 C19 C20 N1 2.1(11) . . . . ?
C18 C19 C20 C21 -175.6(7) . . . . ?
C25 N2 C21 C22 1.5(10) . . . . ?
Cd1 N2 C21 C22 -179.6(5) . . . . ?
C25 N2 C21 C20 -175.4(6) . . . . ?
Cd1 N2 C21 C20 3.5(8) . . . . ?
N1 C20 C21 N2 13.2(9) . . . . ?
C19 C20 C21 N2 -169.0(6) . . . . ?
N1 C20 C21 C22 -163.7(7) . . . . ?
C19 C20 C21 C22 14.1(11) . . . . ?
N2 C21 C22 C23 -1.5(12) . . . . ?
C20 C21 C22 C23 175.3(7) . . . . ?
C21 C22 C23 C24 0.9(13) . . . . ?
C22 C23 C24 C25 -0.4(13) . . . . ?
C21 N2 C25 C24 -1.1(11) . . . . ?
Cd1 N2 C25 C24 -179.9(6) . . . . ?
C23 C24 C25 N2 0.5(12) . . . . ?
C30 N3 C26 C27 0.6(12) . . . . ?
Cd2 N3 C26 C27 -179.5(5) . . . . ?
C30 N3 C26 C26 -179.1(8) . . . 2_655 ?
Cd2 N3 C26 C26 0.9(10) . . . 2_655 ?
N3 C26 C27 C28 -1.0(11) . . . . ?
C26 C26 C27 C28 178.6(8) 2_655 . . . ?
C26 C27 C28 C29 1.6(14) . . . . ?
C27 C28 C29 C30 -1.8(16) . . . . ?
C26 N3 C30 C29 -0.8(15) . . . . ?
Cd2 N3 C30 C29 179.2(8) . . . . ?
C28 C29 C30 N3 1.4(18) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C25 H25 O2 0.93 2.48 3.102(9) 124.7 2
C19 H19 O3 0.93 2.43 3.349(9) 172.6 4_576
O8 H4W O5 0.85 2.10 2.947(9) 179.3 .
O8 H3W O7 0.85 1.96 2.808(10) 178.9 2_655
O7 H2W O4 0.85 2.17 3.022(7) 179.3 1_545
O7 H1W O6 0.85 1.89 2.739(7) 179.2 .
C25 H25 O2 0.93 2.48 3.102(9) 124.7 2
C19 H19 O3 0.93 2.43 3.349(9) 172.6 4_576
O8 H4W O5 0.85 2.10 2.947(9) 179.3 .
O8 H3W O7 0.85 1.96 2.808(10) 178.9 2_655
O7 H2W O4 0.85 2.17 3.022(7) 179.3 1_545
O7 H1W O6 0.85 1.89 2.739(7) 179.2 .
C25 H25 O2 0.93 2.48 3.102(9) 124.7 2
C19 H19 O3 0.93 2.43 3.349(9) 172.6 4_576
O8 H4W O5 0.85 2.10 2.947(9) 179.3 .
O8 H3W O7 0.85 1.96 2.808(10) 178.9 2_655
O7 H2W O4 0.85 2.17 3.022(7) 179.3 1_545
O7 H1W O6 0.85 1.89 2.739(7) 179.2 .
O7 H1W O6 0.85 1.89 2.739(7) 179.2 .
O7 H2W O4 0.85 2.17 3.022(7) 179.3 1_545
O8 H3W O7 0.85 1.96 2.808(10) 178.9 2_655
O8 H4W O5 0.85 2.10 2.947(9) 179.3 .
C19 H19 O3 0.93 2.43 3.349(9) 172.6 4_576
C25 H25 O2 0.93 2.48 3.102(9) 124.7 2
O7 H1W O6 0.85 1.89 2.739(7) 179.2 .
O7 H2W O4 0.85 2.17 3.022(7) 179.3 1_545
O8 H3W O7 0.85 1.96 2.808(10) 178.9 2_655
O8 H4W O5 0.85 2.10 2.947(9) 179.3 .
C19 H19 O3 0.93 2.43 3.349(9) 172.6 4_576
C25 H25 O2 0.93 2.48 3.102(9) 124.7 2

_refine_diff_density_max         0.814
_refine_diff_density_min         -0.680
_refine_diff_density_rms         0.123


# start Validation Reply Form
_vrf_PLAT910_I                   
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min) 13 Note
RESPONSE: Reduction of beam stop mask did not yield significant improvement.
Most of those missing srtong reflections appeared to be very strong and were
treated as overflows.
;
# end Validation Reply Form

