# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_285-6Cd
_database_code_depnum_ccdc_archive 'CCDC 1509058'
_audit_update_record             
;
2017-03-26 deposited with the CCDC.
2017-04-10 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            'C27 H18 Cd N2 O8'
_chemical_formula_weight         610.83

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                   7.9573(8)
_cell_length_b                   10.3708(8)
_cell_length_c                   14.4980(13)
_cell_angle_alpha                90.488(7)
_cell_angle_beta                 96.737(8)
_cell_angle_gamma                100.862(7)
_cell_volume                     1166.30(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6805
_cell_measurement_theta_min      3.416
_cell_measurement_theta_max      25.049

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.739
_exptl_crystal_F_000             612
_exptl_transmission_factor_min   0.772
_exptl_transmission_factor_max   0.811
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.210
_exptl_absorpt_coefficient_mu    0.995
_shelx_estimated_absorpt_T_min   0.782
_shelx_estimated_absorpt_T_max   0.818
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.782
_exptl_absorpt_correction_T_max  0.818
_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            6805
_diffrn_reflns_av_unetI/netI     0.0776
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.416
_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             4129
_reflns_number_gt                3279
_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)+(0.0173P)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         4129
_refine_ls_number_parameters     344
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0425
_refine_ls_wR_factor_ref         0.0799
_refine_ls_wR_factor_gt          0.0691
_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 0.32820(4) 0.52965(3) 0.08166(2) 0.02833(12) Uani 1 1 d . . . . .
N1 N 0.3048(5) 0.7432(3) 0.0305(3) 0.0321(9) Uani 1 1 d . . . . .
N2 N 0.2823(5) 0.6676(3) 0.2083(3) 0.0330(9) Uani 1 1 d . . . . .
O1 O 0.6190(4) 0.6068(3) 0.0469(2) 0.0353(8) Uani 1 1 d . . . . .
O2 O 0.8530(4) 0.5228(3) 0.0713(2) 0.0414(8) Uani 1 1 d . . . . .
O3 O 0.7148(5) 0.6357(3) 0.5376(2) 0.0475(9) Uani 1 1 d . . . . .
H3 H 0.7070 0.6624 0.5900 0.071 Uiso 1 1 calc R U . . .
O4 O 0.7753(5) 0.8506(3) 0.5112(2) 0.0487(10) Uani 1 1 d . . . . .
O5 O 0.8232(4) 0.4188(3) 0.2466(2) 0.0286(7) Uani 1 1 d . . . . .
O6 O 0.4753(4) 0.4001(3) 0.18030(19) 0.0298(7) Uani 1 1 d . . . . .
O7 O 0.3001(4) 0.3255(3) 0.28560(19) 0.0296(7) Uani 1 1 d . . . . .
O8 O 0.1001(4) 0.3761(3) 0.1217(2) 0.0370(8) Uani 1 1 d . . . . .
H1W H 0.1437 0.3618 0.1769 0.044 Uiso 1 1 d R U . . .
H2W H 0.0204 0.4225 0.1200 0.044 Uiso 1 1 d R U . . .
C1 C 0.7476(6) 0.5825(4) 0.0994(3) 0.0285(11) Uani 1 1 d . . . . .
C2 C 0.7644(5) 0.6254(4) 0.1999(3) 0.0258(10) Uani 1 1 d . . . . .
C3 C 0.7344(6) 0.7484(4) 0.2245(3) 0.0363(12) Uani 1 1 d . . . . .
H3A H 0.7134 0.8067 0.1780 0.044 Uiso 1 1 calc R U . . .
C4 C 0.7349(6) 0.7858(4) 0.3157(3) 0.0386(13) Uani 1 1 d . . . . .
H4 H 0.7209 0.8702 0.3307 0.046 Uiso 1 1 calc R U . . .
C5 C 0.7562(6) 0.6977(4) 0.3851(3) 0.0318(11) Uani 1 1 d . . . . .
C6 C 0.7493(6) 0.7374(5) 0.4830(3) 0.0373(12) Uani 1 1 d . . . . .
C7 C 0.7828(5) 0.5737(4) 0.3627(3) 0.0287(11) Uani 1 1 d . . . . .
H7 H 0.7957 0.5137 0.4091 0.034 Uiso 1 1 calc R U . . .
C8 C 0.7903(5) 0.5397(4) 0.2717(3) 0.0264(10) Uani 1 1 d . . . . .
C9 C 0.7561(6) 0.3124(4) 0.2981(3) 0.0272(10) Uani 1 1 d . . . . .
C10 C 0.8734(6) 0.2426(4) 0.3413(3) 0.0344(12) Uani 1 1 d . . . . .
H10 H 0.9901 0.2680 0.3355 0.041 Uiso 1 1 calc R U . . .
C11 C 0.8181(7) 0.1360(4) 0.3927(3) 0.0403(13) Uani 1 1 d . . . . .
H11 H 0.8972 0.0893 0.4219 0.048 Uiso 1 1 calc R U . . .
C12 C 0.6467(6) 0.0984(4) 0.4011(3) 0.0360(12) Uani 1 1 d . . . . .
H12 H 0.6092 0.0266 0.4365 0.043 Uiso 1 1 calc R U . . .
C13 C 0.5295(6) 0.1666(4) 0.3572(3) 0.0305(11) Uani 1 1 d . . . . .
H13 H 0.4133 0.1399 0.3637 0.037 Uiso 1 1 calc R U . . .
C14 C 0.5800(5) 0.2749(4) 0.3031(3) 0.0247(10) Uani 1 1 d . . . . .
C15 C 0.4421(5) 0.3389(4) 0.2528(3) 0.0231(10) Uani 1 1 d . . . . .
C16 C 0.3244(6) 0.7822(4) -0.0556(3) 0.0415(13) Uani 1 1 d . . . . .
H16 H 0.3552 0.7251 -0.0975 0.050 Uiso 1 1 calc R U . . .
C17 C 0.3003(7) 0.9059(5) -0.0848(4) 0.0535(15) Uani 1 1 d . . . . .
H17 H 0.3183 0.9313 -0.1448 0.064 Uiso 1 1 calc R U . . .
C18 C 0.2507(8) 0.9888(5) -0.0254(4) 0.0586(17) Uani 1 1 d . . . . .
H18 H 0.2307 1.0702 -0.0454 0.070 Uiso 1 1 calc R U . . .
C19 C 0.2294(6) 0.9530(4) 0.0656(4) 0.0390(13) Uani 1 1 d . . . . .
C20 C 0.2600(6) 0.8279(4) 0.0907(3) 0.0298(11) Uani 1 1 d . . . . .
C21 C 0.1805(7) 1.0349(5) 0.1329(4) 0.0500(15) Uani 1 1 d . . . . .
H21 H 0.1587 1.1170 0.1160 0.060 Uiso 1 1 calc R U . . .
C22 C 0.1653(6) 0.9971(5) 0.2194(4) 0.0467(14) Uani 1 1 d . . . . .
H22 H 0.1293 1.0517 0.2612 0.056 Uiso 1 1 calc R U . . .
C23 C 0.2037(6) 0.8725(4) 0.2493(3) 0.0371(12) Uani 1 1 d . . . . .
C24 C 0.2477(6) 0.7875(4) 0.1856(3) 0.0279(11) Uani 1 1 d . . . . .
C25 C 0.1998(7) 0.8333(5) 0.3414(4) 0.0472(14) Uani 1 1 d . . . . .
H25 H 0.1704 0.8875 0.3859 0.057 Uiso 1 1 calc R U . . .
C26 C 0.2394(7) 0.7149(5) 0.3650(4) 0.0497(14) Uani 1 1 d . . . . .
H26 H 0.2407 0.6881 0.4261 0.060 Uiso 1 1 calc R U . . .
C27 C 0.2779(7) 0.6346(5) 0.2963(3) 0.0466(14) Uani 1 1 d . . . . .
H27 H 0.3020 0.5530 0.3130 0.056 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 O8 2.311(3) . ?
Cd1 O6 2.335(3) . ?
Cd1 N1 2.375(3) . ?
Cd1 O1 2.415(3) . ?
Cd1 N2 2.421(4) . ?
Cd1 O1 2.452(3) 2_665 ?
Cd1 O2 2.495(3) 2_665 ?
N1 C16 1.333(5) . ?
N1 C20 1.355(5) . ?
N2 C27 1.327(6) . ?
N2 C24 1.359(5) . ?
O1 C1 1.267(5) . ?
O1 Cd1 2.452(3) 2_665 ?
O2 C1 1.235(5) . ?
O2 Cd1 2.495(3) 2_665 ?
O3 C6 1.329(5) . ?
O3 H3 0.8200 . ?
O4 C6 1.212(5) . ?
O5 C8 1.382(5) . ?
O5 C9 1.395(5) . ?
O6 C15 1.261(5) . ?
O7 C15 1.261(5) . ?
O8 H1W 0.8601 . ?
O8 H2W 0.8637 . ?
C1 C2 1.504(6) . ?
C2 C3 1.392(5) . ?
C2 C8 1.397(5) . ?
C3 C4 1.374(6) . ?
C3 H3A 0.9300 . ?
C4 C5 1.382(6) . ?
C4 H4 0.9300 . ?
C5 C7 1.385(6) . ?
C5 C6 1.485(6) . ?
C7 C8 1.373(6) . ?
C7 H7 0.9300 . ?
C9 C10 1.383(6) . ?
C9 C14 1.392(6) . ?
C10 C11 1.371(6) . ?
C10 H10 0.9300 . ?
C11 C12 1.366(6) . ?
C11 H11 0.9300 . ?
C12 C13 1.376(6) . ?
C12 H12 0.9300 . ?
C13 C14 1.399(5) . ?
C13 H13 0.9300 . ?
C14 C15 1.507(5) . ?
C16 C17 1.395(6) . ?
C16 H16 0.9300 . ?
C17 C18 1.353(7) . ?
C17 H17 0.9300 . ?
C18 C19 1.395(7) . ?
C18 H18 0.9300 . ?
C19 C20 1.408(5) . ?
C19 C21 1.423(7) . ?
C20 C24 1.450(6) . ?
C21 C22 1.329(7) . ?
C21 H21 0.9300 . ?
C22 C23 1.441(6) . ?
C22 H22 0.9300 . ?
C23 C24 1.390(6) . ?
C23 C25 1.401(6) . ?
C25 C26 1.361(6) . ?
C25 H25 0.9300 . ?
C26 C27 1.391(6) . ?
C26 H26 0.9300 . ?
C27 H27 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
O8 Cd1 O6 79.46(10) . . ?
O8 Cd1 N1 124.18(11) . . ?
O6 Cd1 N1 147.79(11) . . ?
O8 Cd1 O1 155.39(10) . . ?
O6 Cd1 O1 79.91(10) . . ?
N1 Cd1 O1 80.15(11) . . ?
O8 Cd1 N2 87.32(11) . . ?
O6 Cd1 N2 93.24(11) . . ?
N1 Cd1 N2 68.99(12) . . ?
O1 Cd1 N2 107.12(11) . . ?
O8 Cd1 O1 93.95(10) . 2_665 ?
O6 Cd1 O1 86.73(10) . 2_665 ?
N1 Cd1 O1 110.43(11) . 2_665 ?
O1 Cd1 O1 71.58(11) . 2_665 ?
N2 Cd1 O1 178.69(12) . 2_665 ?
O8 Cd1 O2 78.22(10) . 2_665 ?
O6 Cd1 O2 131.30(10) . 2_665 ?
N1 Cd1 O2 78.76(11) . 2_665 ?
O1 Cd1 O2 106.08(10) . 2_665 ?
N2 Cd1 O2 128.03(11) . 2_665 ?
O1 Cd1 O2 52.63(10) 2_665 2_665 ?
C16 N1 C20 118.1(4) . . ?
C16 N1 Cd1 123.6(3) . . ?
C20 N1 Cd1 118.2(3) . . ?
C27 N2 C24 117.1(4) . . ?
C27 N2 Cd1 126.3(3) . . ?
C24 N2 Cd1 116.4(3) . . ?
C1 O1 Cd1 121.2(3) . . ?
C1 O1 Cd1 92.7(3) . 2_665 ?
Cd1 O1 Cd1 108.42(11) . 2_665 ?
C1 O2 Cd1 91.6(3) . 2_665 ?
C6 O3 H3 109.5 . . ?
C8 O5 C9 116.4(3) . . ?
C15 O6 Cd1 133.8(3) . . ?
Cd1 O8 H1W 98.1 . . ?
Cd1 O8 H2W 100.9 . . ?
H1W O8 H2W 114.1 . . ?
O2 C1 O1 122.5(4) . . ?
O2 C1 C2 120.4(4) . . ?
O1 C1 C2 117.1(4) . . ?
C3 C2 C8 117.2(4) . . ?
C3 C2 C1 120.4(4) . . ?
C8 C2 C1 121.9(4) . . ?
C4 C3 C2 121.6(4) . . ?
C4 C3 H3A 119.2 . . ?
C2 C3 H3A 119.2 . . ?
C3 C4 C5 119.9(4) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 H4 120.1 . . ?
C4 C5 C7 119.8(4) . . ?
C4 C5 C6 119.4(4) . . ?
C7 C5 C6 120.8(4) . . ?
O4 C6 O3 123.1(5) . . ?
O4 C6 C5 123.7(4) . . ?
O3 C6 C5 113.1(4) . . ?
C8 C7 C5 119.7(4) . . ?
C8 C7 H7 120.1 . . ?
C5 C7 H7 120.1 . . ?
C7 C8 O5 121.7(4) . . ?
C7 C8 C2 121.6(4) . . ?
O5 C8 C2 116.6(4) . . ?
C10 C9 C14 121.5(4) . . ?
C10 C9 O5 116.4(4) . . ?
C14 C9 O5 122.1(4) . . ?
C11 C10 C9 120.1(4) . . ?
C11 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?
C12 C11 C10 120.0(4) . . ?
C12 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
C11 C12 C13 120.0(4) . . ?
C11 C12 H12 120.0 . . ?
C13 C12 H12 120.0 . . ?
C12 C13 C14 121.9(4) . . ?
C12 C13 H13 119.0 . . ?
C14 C13 H13 119.0 . . ?
C9 C14 C13 116.4(4) . . ?
C9 C14 C15 125.1(4) . . ?
C13 C14 C15 118.4(4) . . ?
O7 C15 O6 124.5(4) . . ?
O7 C15 C14 117.4(4) . . ?
O6 C15 C14 118.0(4) . . ?
N1 C16 C17 122.2(5) . . ?
N1 C16 H16 118.9 . . ?
C17 C16 H16 118.9 . . ?
C18 C17 C16 119.6(5) . . ?
C18 C17 H17 120.2 . . ?
C16 C17 H17 120.2 . . ?
C17 C18 C19 120.4(5) . . ?
C17 C18 H18 119.8 . . ?
C19 C18 H18 119.8 . . ?
C18 C19 C20 116.7(5) . . ?
C18 C19 C21 124.1(5) . . ?
C20 C19 C21 119.3(5) . . ?
N1 C20 C19 123.0(4) . . ?
N1 C20 C24 117.8(4) . . ?
C19 C20 C24 119.2(4) . . ?
C22 C21 C19 121.7(5) . . ?
C22 C21 H21 119.2 . . ?
C19 C21 H21 119.2 . . ?
C21 C22 C23 120.9(5) . . ?
C21 C22 H22 119.6 . . ?
C23 C22 H22 119.6 . . ?
C24 C23 C25 118.1(4) . . ?
C24 C23 C22 119.6(5) . . ?
C25 C23 C22 122.4(5) . . ?
N2 C24 C23 122.8(4) . . ?
N2 C24 C20 117.9(4) . . ?
C23 C24 C20 119.3(4) . . ?
C26 C25 C23 119.2(5) . . ?
C26 C25 H25 120.4 . . ?
C23 C25 H25 120.4 . . ?
C25 C26 C27 118.9(5) . . ?
C25 C26 H26 120.5 . . ?
C27 C26 H26 120.5 . . ?
N2 C27 C26 123.8(5) . . ?
N2 C27 H27 118.1 . . ?
C26 C27 H27 118.1 . . ?

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
Cd1 O2 C1 O1 -7.9(4) 2_665 . . . ?
Cd1 O2 C1 C2 169.8(3) 2_665 . . . ?
Cd1 O1 C1 O2 121.5(4) . . . . ?
Cd1 O1 C1 O2 8.0(4) 2_665 . . . ?
Cd1 O1 C1 C2 -56.2(4) . . . . ?
Cd1 O1 C1 C2 -169.7(3) 2_665 . . . ?
O2 C1 C2 C3 139.0(4) . . . . ?
O1 C1 C2 C3 -43.2(6) . . . . ?
O2 C1 C2 C8 -48.6(6) . . . . ?
O1 C1 C2 C8 129.2(4) . . . . ?
C8 C2 C3 C4 1.8(7) . . . . ?
C1 C2 C3 C4 174.6(4) . . . . ?
C2 C3 C4 C5 -3.6(7) . . . . ?
C3 C4 C5 C7 2.2(7) . . . . ?
C3 C4 C5 C6 -177.5(4) . . . . ?
C4 C5 C6 O4 -22.1(7) . . . . ?
C7 C5 C6 O4 158.2(5) . . . . ?
C4 C5 C6 O3 159.2(5) . . . . ?
C7 C5 C6 O3 -20.5(6) . . . . ?
C4 C5 C7 C8 0.9(7) . . . . ?
C6 C5 C7 C8 -179.4(4) . . . . ?
C5 C7 C8 O5 177.5(4) . . . . ?
C5 C7 C8 C2 -2.7(7) . . . . ?
C9 O5 C8 C7 34.9(5) . . . . ?
C9 O5 C8 C2 -144.9(4) . . . . ?
C3 C2 C8 C7 1.4(6) . . . . ?
C1 C2 C8 C7 -171.3(4) . . . . ?
C3 C2 C8 O5 -178.8(4) . . . . ?
C1 C2 C8 O5 8.6(6) . . . . ?
C8 O5 C9 C10 -122.6(4) . . . . ?
C8 O5 C9 C14 59.8(5) . . . . ?
C14 C9 C10 C11 -1.9(7) . . . . ?
O5 C9 C10 C11 -179.5(4) . . . . ?
C9 C10 C11 C12 0.2(7) . . . . ?
C10 C11 C12 C13 0.7(7) . . . . ?
C11 C12 C13 C14 0.2(7) . . . . ?
C10 C9 C14 C13 2.6(6) . . . . ?
O5 C9 C14 C13 -179.9(4) . . . . ?
C10 C9 C14 C15 -175.4(4) . . . . ?
O5 C9 C14 C15 2.0(6) . . . . ?
C12 C13 C14 C9 -1.8(6) . . . . ?
C12 C13 C14 C15 176.4(4) . . . . ?
Cd1 O6 C15 O7 6.9(7) . . . . ?
Cd1 O6 C15 C14 -174.3(2) . . . . ?
C9 C14 C15 O7 -157.3(4) . . . . ?
C13 C14 C15 O7 24.6(6) . . . . ?
C9 C14 C15 O6 23.8(6) . . . . ?
C13 C14 C15 O6 -154.2(4) . . . . ?
C20 N1 C16 C17 0.0(7) . . . . ?
Cd1 N1 C16 C17 176.3(4) . . . . ?
N1 C16 C17 C18 -1.9(8) . . . . ?
C16 C17 C18 C19 2.2(9) . . . . ?
C17 C18 C19 C20 -0.7(8) . . . . ?
C17 C18 C19 C21 178.9(5) . . . . ?
C16 N1 C20 C19 1.7(7) . . . . ?
Cd1 N1 C20 C19 -174.9(3) . . . . ?
C16 N1 C20 C24 -176.9(4) . . . . ?
Cd1 N1 C20 C24 6.6(5) . . . . ?
C18 C19 C20 N1 -1.3(7) . . . . ?
C21 C19 C20 N1 179.1(4) . . . . ?
C18 C19 C20 C24 177.2(5) . . . . ?
C21 C19 C20 C24 -2.4(7) . . . . ?
C18 C19 C21 C22 -178.6(5) . . . . ?
C20 C19 C21 C22 0.9(8) . . . . ?
C19 C21 C22 C23 2.2(8) . . . . ?
C21 C22 C23 C24 -3.8(7) . . . . ?
C21 C22 C23 C25 175.8(5) . . . . ?
C27 N2 C24 C23 -2.0(7) . . . . ?
Cd1 N2 C24 C23 174.2(3) . . . . ?
C27 N2 C24 C20 177.1(4) . . . . ?
Cd1 N2 C24 C20 -6.7(5) . . . . ?
C25 C23 C24 N2 1.7(7) . . . . ?
C22 C23 C24 N2 -178.7(4) . . . . ?
C25 C23 C24 C20 -177.4(4) . . . . ?
C22 C23 C24 C20 2.2(7) . . . . ?
N1 C20 C24 N2 0.3(6) . . . . ?
C19 C20 C24 N2 -178.3(4) . . . . ?
N1 C20 C24 C23 179.4(4) . . . . ?
C19 C20 C24 C23 0.8(7) . . . . ?
C24 C23 C25 C26 0.3(7) . . . . ?
C22 C23 C25 C26 -179.3(5) . . . . ?
C23 C25 C26 C27 -1.8(8) . . . . ?
C24 N2 C27 C26 0.3(8) . . . . ?
Cd1 N2 C27 C26 -175.4(4) . . . . ?
C25 C26 C27 N2 1.6(8) . . . . ?

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
O3 H3 O7 0.82 1.81 2.611(4) 163.5 2_666
O8 H1W O7 0.86 1.98 2.812(4) 164.0 .
O8 H2W O2 0.86 1.92 2.743(4) 160.0 1_455

_refine_diff_density_max         0.721
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.102


# start Validation Reply Form
_vrf_PLAT910_I                   
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min) 11 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_277-5Mn2
_database_code_depnum_ccdc_archive 'CCDC 1509063'
_audit_update_record             
;
2017-03-26 deposited with the CCDC.
2017-04-10 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            'C66 H42 Mn3 N6 O16'
_chemical_formula_weight         1339.87

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'
Mn Mn 0.3368 0.7283 '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                   21.8374(9)
_cell_length_b                   10.3384(5)
_cell_length_c                   24.6652(12)
_cell_angle_alpha                90
_cell_angle_beta                 95.758(4)
_cell_angle_gamma                90
_cell_volume                     5540.4(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    10818
_cell_measurement_theta_min      3.378
_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    1.606
_exptl_crystal_F_000             2732
_exptl_transmission_factor_min   0.834
_exptl_transmission_factor_max   0.873
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    0.757
_shelx_estimated_absorpt_T_min   0.828
_shelx_estimated_absorpt_T_max   0.876
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.828
_exptl_absorpt_correction_T_max  0.876
_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            10818
_diffrn_reflns_av_unetI/netI     0.0753
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         3.378
_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             4920
_reflns_number_gt                3337
_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)+(0.0181P)²+6.1555P] 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         4920
_refine_ls_number_parameters     415
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0858
_refine_ls_R_factor_gt           0.0517
_refine_ls_wR_factor_ref         0.1017
_refine_ls_wR_factor_gt          0.0839
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.050
_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
Mn1 Mn 0.41080(2) 0.78982(6) 0.38673(2) 0.03350(17) Uani 1 1 d . . . . .
Mn2 Mn 0.49866(5) 0.94321(10) 0.27055(4) 0.0312(3) Uani 0.5 1 d . . P . .
N1 N 0.46946(13) 0.6086(3) 0.40732(11) 0.0383(8) Uani 1 1 d . . . . .
N2 N 0.34980(13) 0.6351(3) 0.42233(11) 0.0403(8) Uani 1 1 d . . . . .
N3 N 0.45097(14) 1.1167(3) 0.27790(14) 0.0553(10) Uani 1 1 d . . . . .
O1 O 0.42680(11) 0.8269(3) 0.23648(10) 0.0523(8) Uani 1 1 d . . . . .
O2 O 0.38952(10) 0.7203(2) 0.30420(9) 0.0416(6) Uani 1 1 d . . . . .
O3 O 0.19429(11) 0.5173(3) 0.06120(10) 0.0543(8) Uani 1 1 d . . . . .
O4 O 0.17134(10) 0.4029(3) 0.13340(9) 0.0440(7) Uani 1 1 d . . . . .
O5 O 0.36701(10) 0.8046(2) 0.13363(9) 0.0356(6) Uani 1 1 d . . . . .
O6 O 0.47184(14) 0.9576(4) 0.05676(11) 0.0989(14) Uani 1 1 d . . . . .
O7 O 0.50829(10) 0.8931(3) 0.13814(10) 0.0455(7) Uani 1 1 d . . . . .
O8 O 0.41066(11) 0.8769(3) 0.46850(9) 0.0519(8) Uani 1 1 d . . . . .
H1W H 0.3832 0.9344 0.4636 0.062 Uiso 1 1 d R U . . .
H2W H 0.4433 0.9148 0.4765 0.062 Uiso 1 1 d R U . . .
C1 C 0.38968(15) 0.7512(3) 0.25549(14) 0.0317(8) Uani 1 1 d . . . . .
C2 C 0.34196(14) 0.6874(3) 0.21531(13) 0.0303(8) Uani 1 1 d . . . . .
C3 C 0.30617(15) 0.5901(4) 0.23457(14) 0.0394(10) Uani 1 1 d . . . . .
H3 H 0.3115 0.5696 0.2715 0.047 Uiso 1 1 calc R U . . .
C4 C 0.26281(16) 0.5221(4) 0.20111(14) 0.0409(10) Uani 1 1 d . . . . .
H4 H 0.2404 0.4559 0.2153 0.049 Uiso 1 1 calc R U . . .
C5 C 0.25297(15) 0.5533(3) 0.14633(13) 0.0328(9) Uani 1 1 d . . . . .
C6 C 0.20238(15) 0.4854(4) 0.11001(15) 0.0366(9) Uani 1 1 d . . . . .
C7 C 0.28772(15) 0.6505(3) 0.12619(13) 0.0348(9) Uani 1 1 d . . . . .
H7 H 0.2814 0.6718 0.0894 0.042 Uiso 1 1 calc R U . . .
C8 C 0.33173(14) 0.7166(3) 0.15974(13) 0.0299(8) Uani 1 1 d . . . . .
C9 C 0.36541(16) 0.9356(4) 0.14525(13) 0.0320(9) Uani 1 1 d . . . . .
C10 C 0.31691(17) 0.9938(4) 0.16792(14) 0.0427(10) Uani 1 1 d . . . . .
H10 H 0.2845 0.9439 0.1781 0.051 Uiso 1 1 calc R U . . .
C11 C 0.31681(19) 1.1272(4) 0.17549(15) 0.0507(11) Uani 1 1 d . . . . .
H11 H 0.2846 1.1665 0.1913 0.061 Uiso 1 1 calc R U . . .
C12 C 0.36445(18) 1.2010(4) 0.15958(14) 0.0465(10) Uani 1 1 d . . . . .
H12 H 0.3643 1.2903 0.1641 0.056 Uiso 1 1 calc R U . . .
C13 C 0.41233(17) 1.1410(4) 0.13693(14) 0.0397(9) Uani 1 1 d . . . . .
H13 H 0.4443 1.1911 0.1262 0.048 Uiso 1 1 calc R U . . .
C14 C 0.41396(15) 1.0083(3) 0.12977(12) 0.0296(8) Uani 1 1 d . . . . .
C15 C 0.46834(16) 0.9479(4) 0.10512(15) 0.0351(9) Uani 1 1 d . . . . .
C16 C 0.29131(17) 0.6496(4) 0.43150(15) 0.0522(11) Uani 1 1 d . . . . .
H16 H 0.2720 0.7273 0.4214 0.063 Uiso 1 1 calc R U . . .
C17 C 0.2572(2) 0.5556(5) 0.45539(16) 0.0601(13) Uani 1 1 d . . . . .
H17 H 0.2166 0.5713 0.4619 0.072 Uiso 1 1 calc R U . . .
C18 C 0.2843(2) 0.4404(5) 0.46908(16) 0.0603(13) Uani 1 1 d . . . . .
H18 H 0.2617 0.3756 0.4841 0.072 Uiso 1 1 calc R U . . .
C19 C 0.3462(2) 0.4184(4) 0.46078(15) 0.0502(11) Uani 1 1 d . . . . .
C20 C 0.37730(17) 0.5205(4) 0.43729(13) 0.0372(9) Uani 1 1 d . . . . .
C21 C 0.3792(3) 0.3023(4) 0.47531(17) 0.0660(14) Uani 1 1 d . . . . .
H21 H 0.3586 0.2331 0.4894 0.079 Uiso 1 1 calc R U . . .
C22 C 0.4393(2) 0.2911(4) 0.46905(16) 0.0628(13) Uani 1 1 d . . . . .
H22 H 0.4596 0.2145 0.4793 0.075 Uiso 1 1 calc R U . . .
C23 C 0.4726(2) 0.3936(4) 0.44711(14) 0.0460(11) Uani 1 1 d . . . . .
C24 C 0.44159(17) 0.5077(4) 0.42977(13) 0.0361(9) Uani 1 1 d . . . . .
C25 C 0.5355(2) 0.3870(4) 0.44122(16) 0.0552(12) Uani 1 1 d . . . . .
H25 H 0.5581 0.3147 0.4535 0.066 Uiso 1 1 calc R U . . .
C26 C 0.56349(19) 0.4862(4) 0.41751(16) 0.0546(12) Uani 1 1 d . . . . .
H26 H 0.6051 0.4815 0.4125 0.066 Uiso 1 1 calc R U . . .
C27 C 0.52863(18) 0.5968(4) 0.40054(15) 0.0479(11) Uani 1 1 d . . . . .
H27 H 0.5480 0.6641 0.3840 0.057 Uiso 1 1 calc R U . . .
C28 C 0.4029(2) 1.1163(7) 0.3065(2) 0.095(2) Uani 1 1 d . . . . .
H28 H 0.3859 1.0373 0.3149 0.113 Uiso 1 1 calc R U . . .
C29 C 0.3765(2) 1.2296(10) 0.3246(2) 0.112(3) Uani 1 1 d . . . . .
H29 H 0.3429 1.2252 0.3449 0.135 Uiso 1 1 calc R U . . .
C30 C 0.4001(2) 1.3446(7) 0.31258(19) 0.0794(19) Uani 1 1 d . . . . .
H30 H 0.3830 1.4204 0.3247 0.095 Uiso 1 1 calc R U . . .
C31 C 0.45034(17) 1.3504(4) 0.28190(15) 0.0432(10) Uani 1 1 d . . . . .
C32 C 0.47670(18) 1.4679(4) 0.26560(18) 0.0626(14) Uani 1 1 d . . . . .
H32 H 0.4613 1.5463 0.2768 0.075 Uiso 1 1 calc R U . . .
C33 C 0.47384(14) 1.2331(3) 0.26546(13) 0.0332(9) 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
Mn1 O4 2.157(2) 4 ?
Mn1 O2 2.165(2) . ?
Mn1 O7 2.204(3) 2_655 ?
Mn1 O8 2.209(2) . ?
Mn1 N1 2.297(3) . ?
Mn1 N2 2.311(3) . ?
Mn2 Mn2 1.0214(19) 2_655 ?
Mn2 O1 2.045(3) 2_655 ?
Mn2 O1 2.086(3) . ?
Mn2 N3 2.091(4) . ?
Mn2 O7 2.330(3) 2_655 ?
Mn2 N3 2.473(4) 2_655 ?
N1 C27 1.325(4) . ?
N1 C24 1.354(4) . ?
N2 C16 1.328(4) . ?
N2 C20 1.362(4) . ?
N3 C28 1.322(6) . ?
N3 C33 1.350(4) . ?
N3 Mn2 2.473(4) 2_655 ?
O1 C1 1.251(4) . ?
O1 Mn2 2.045(3) 2_655 ?
O2 C1 1.244(4) . ?
O3 C6 1.244(4) . ?
O4 C6 1.264(4) . ?
O4 Mn1 2.157(2) 4_545 ?
O5 C9 1.385(4) . ?
O5 C8 1.391(4) . ?
O6 C15 1.207(4) . ?
O7 C15 1.266(4) . ?
O7 Mn1 2.204(2) 2_655 ?
O7 Mn2 2.330(3) 2_655 ?
O8 H1W 0.8437 . ?
O8 H2W 0.8200 . ?
C1 C2 1.515(4) . ?
C2 C3 1.387(4) . ?
C2 C8 1.399(4) . ?
C3 C4 1.383(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.385(4) . ?
C4 H4 0.9300 . ?
C5 C7 1.381(5) . ?
C5 C6 1.523(4) . ?
C7 C8 1.384(4) . ?
C7 H7 0.9300 . ?
C9 C10 1.384(5) . ?
C9 C14 1.384(5) . ?
C10 C11 1.392(5) . ?
C10 H10 0.9300 . ?
C11 C12 1.378(5) . ?
C11 H11 0.9300 . ?
C12 C13 1.381(5) . ?
C12 H12 0.9300 . ?
C13 C14 1.385(5) . ?
C13 H13 0.9300 . ?
C14 C15 1.521(5) . ?
C16 C17 1.391(5) . ?
C16 H16 0.9300 . ?
C17 C18 1.357(6) . ?
C17 H17 0.9300 . ?
C18 C19 1.405(6) . ?
C18 H18 0.9300 . ?
C19 C20 1.412(5) . ?
C19 C21 1.427(6) . ?
C20 C24 1.440(5) . ?
C21 C22 1.342(6) . ?
C21 H21 0.9300 . ?
C22 C23 1.423(6) . ?
C22 H22 0.9300 . ?
C23 C25 1.397(5) . ?
C23 C24 1.406(5) . ?
C25 C26 1.356(6) . ?
C25 H25 0.9300 . ?
C26 C27 1.414(5) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
C28 C29 1.398(8) . ?
C28 H28 0.9300 . ?
C29 C30 1.341(8) . ?
C29 H29 0.9300 . ?
C30 C31 1.395(6) . ?
C30 H30 0.9300 . ?
C31 C33 1.393(5) . ?
C31 C32 1.420(5) . ?
C32 C32 1.336(8) 2_655 ?
C32 H32 0.9300 . ?
C33 C33 1.436(7) 2_655 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Mn1 O2 82.44(9) 4 . ?
O4 Mn1 O7 110.16(10) 4 2_655 ?
O2 Mn1 O7 90.10(9) . 2_655 ?
O4 Mn1 O8 84.95(9) 4 . ?
O2 Mn1 O8 166.92(9) . . ?
O7 Mn1 O8 97.54(9) 2_655 . ?
O4 Mn1 N1 157.72(11) 4 . ?
O2 Mn1 N1 89.97(10) . . ?
O7 Mn1 N1 90.68(10) 2_655 . ?
O8 Mn1 N1 100.50(10) . . ?
O4 Mn1 N2 87.99(10) 4 . ?
O2 Mn1 N2 92.85(10) . . ?
O7 Mn1 N2 161.84(10) 2_655 . ?
O8 Mn1 N2 83.20(10) . . ?
N1 Mn1 N2 71.42(11) . . ?
Mn2 Mn2 O1 77.90(12) 2_655 2_655 ?
Mn2 Mn2 O1 73.49(11) 2_655 . ?
O1 Mn2 O1 101.53(15) 2_655 . ?
Mn2 Mn2 N3 99.48(11) 2_655 . ?
O1 Mn2 N3 156.83(13) 2_655 . ?
O1 Mn2 N3 99.69(12) . . ?
Mn2 Mn2 O7 167.16(7) 2_655 2_655 ?
O1 Mn2 O7 94.64(10) 2_655 2_655 ?
O1 Mn2 O7 98.17(10) . 2_655 ?
N3 Mn2 O7 91.46(12) . 2_655 ?
Mn2 Mn2 N3 56.48(9) 2_655 2_655 ?
O1 Mn2 N3 89.37(12) 2_655 2_655 ?
O1 Mn2 N3 125.20(11) . 2_655 ?
N3 Mn2 N3 70.70(17) . 2_655 ?
O7 Mn2 N3 134.68(10) 2_655 2_655 ?
C27 N1 C24 117.7(3) . . ?
C27 N1 Mn1 125.2(3) . . ?
C24 N1 Mn1 117.1(2) . . ?
C16 N2 C20 117.3(4) . . ?
C16 N2 Mn1 126.0(3) . . ?
C20 N2 Mn1 116.7(2) . . ?
C28 N3 C33 117.1(5) . . ?
C28 N3 Mn2 118.2(4) . . ?
C33 N3 Mn2 123.1(3) . . ?
C28 N3 Mn2 132.2(4) . 2_655 ?
C33 N3 Mn2 110.1(3) . 2_655 ?
Mn2 N3 Mn2 24.04(6) . 2_655 ?
C1 O1 Mn2 161.9(2) . 2_655 ?
C1 O1 Mn2 134.3(2) . . ?
Mn2 O1 Mn2 28.61(6) 2_655 . ?
C1 O2 Mn1 143.3(2) . . ?
C6 O4 Mn1 137.1(2) . 4_545 ?
C9 O5 C8 121.1(3) . . ?
C15 O7 Mn1 123.9(2) . 2_655 ?
C15 O7 Mn2 114.5(2) . 2_655 ?
Mn1 O7 Mn2 120.55(10) 2_655 2_655 ?
Mn1 O8 H1W 102.8 . . ?
Mn1 O8 H2W 109.5 . . ?
H1W O8 H2W 106.6 . . ?
O2 C1 O1 126.0(3) . . ?
O2 C1 C2 116.8(3) . . ?
O1 C1 C2 117.1(3) . . ?
C3 C2 C8 116.9(3) . . ?
C3 C2 C1 117.8(3) . . ?
C8 C2 C1 125.3(3) . . ?
C4 C3 C2 122.6(3) . . ?
C4 C3 H3 118.7 . . ?
C2 C3 H3 118.7 . . ?
C3 C4 C5 119.6(3) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 H4 120.2 . . ?
C7 C5 C4 118.9(3) . . ?
C7 C5 C6 121.1(3) . . ?
C4 C5 C6 119.9(3) . . ?
O3 C6 O4 126.2(3) . . ?
O3 C6 C5 118.1(3) . . ?
O4 C6 C5 115.7(3) . . ?
C5 C7 C8 121.2(3) . . ?
C5 C7 H7 119.4 . . ?
C8 C7 H7 119.4 . . ?
C7 C8 O5 115.5(3) . . ?
C7 C8 C2 120.8(3) . . ?
O5 C8 C2 123.6(3) . . ?
C10 C9 C14 120.9(4) . . ?
C10 C9 O5 123.0(3) . . ?
C14 C9 O5 116.0(3) . . ?
C9 C10 C11 119.8(4) . . ?
C9 C10 H10 120.1 . . ?
C11 C10 H10 120.1 . . ?
C12 C11 C10 119.9(4) . . ?
C12 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
C11 C12 C13 119.4(4) . . ?
C11 C12 H12 120.3 . . ?
C13 C12 H12 120.3 . . ?
C12 C13 C14 121.8(4) . . ?
C12 C13 H13 119.1 . . ?
C14 C13 H13 119.1 . . ?
C9 C14 C13 118.2(4) . . ?
C9 C14 C15 122.5(3) . . ?
C13 C14 C15 119.3(3) . . ?
O6 C15 O7 124.4(4) . . ?
O6 C15 C14 119.3(3) . . ?
O7 C15 C14 116.2(3) . . ?
N2 C16 C17 123.9(4) . . ?
N2 C16 H16 118.0 . . ?
C17 C16 H16 118.0 . . ?
C18 C17 C16 118.7(4) . . ?
C18 C17 H17 120.7 . . ?
C16 C17 H17 120.7 . . ?
C17 C18 C19 120.5(4) . . ?
C17 C18 H18 119.7 . . ?
C19 C18 H18 119.7 . . ?
C18 C19 C20 116.6(4) . . ?
C18 C19 C21 124.6(4) . . ?
C20 C19 C21 118.7(4) . . ?
N2 C20 C19 123.0(4) . . ?
N2 C20 C24 117.0(3) . . ?
C19 C20 C24 120.0(4) . . ?
C22 C21 C19 121.3(5) . . ?
C22 C21 H21 119.4 . . ?
C19 C21 H21 119.4 . . ?
C21 C22 C23 121.5(4) . . ?
C21 C22 H22 119.2 . . ?
C23 C22 H22 119.2 . . ?
C25 C23 C24 117.3(4) . . ?
C25 C23 C22 123.3(4) . . ?
C24 C23 C22 119.4(4) . . ?
N1 C24 C23 123.3(4) . . ?
N1 C24 C20 117.8(3) . . ?
C23 C24 C20 118.9(4) . . ?
C26 C25 C23 119.9(4) . . ?
C26 C25 H25 120.1 . . ?
C23 C25 H25 120.1 . . ?
C25 C26 C27 119.1(4) . . ?
C25 C26 H26 120.4 . . ?
C27 C26 H26 120.4 . . ?
N1 C27 C26 122.7(4) . . ?
N1 C27 H27 118.7 . . ?
C26 C27 H27 118.7 . . ?
N3 C28 C29 122.9(6) . . ?
N3 C28 H28 118.5 . . ?
C29 C28 H28 118.5 . . ?
C30 C29 C28 119.4(5) . . ?
C30 C29 H29 120.3 . . ?
C28 C29 H29 120.3 . . ?
C29 C30 C31 120.0(5) . . ?
C29 C30 H30 120.0 . . ?
C31 C30 H30 120.0 . . ?
C33 C31 C30 116.9(4) . . ?
C33 C31 C32 119.4(4) . . ?
C30 C31 C32 123.6(5) . . ?
C32 C32 C31 121.1(2) 2_655 . ?
C32 C32 H32 119.4 2_655 . ?
C31 C32 H32 119.4 . . ?
N3 C33 C31 123.7(3) . . ?
N3 C33 C33 116.9(2) . 2_655 ?
C31 C33 C33 119.4(2) . 2_655 ?

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
Mn1 O2 C1 O1 31.5(6) . . . . ?
Mn1 O2 C1 C2 -151.0(3) . . . . ?
Mn2 O1 C1 O2 11.5(11) 2_655 . . . ?
Mn2 O1 C1 O2 -4.4(6) . . . . ?
Mn2 O1 C1 C2 -166.0(7) 2_655 . . . ?
Mn2 O1 C1 C2 178.0(2) . . . . ?
O2 C1 C2 C3 -6.6(5) . . . . ?
O1 C1 C2 C3 171.2(3) . . . . ?
O2 C1 C2 C8 174.8(3) . . . . ?
O1 C1 C2 C8 -7.4(5) . . . . ?
C8 C2 C3 C4 1.0(5) . . . . ?
C1 C2 C3 C4 -177.6(3) . . . . ?
C2 C3 C4 C5 -1.7(6) . . . . ?
C3 C4 C5 C7 1.2(5) . . . . ?
C3 C4 C5 C6 -175.9(3) . . . . ?
Mn1 O4 C6 O3 -7.4(6) 4_545 . . . ?
Mn1 O4 C6 C5 170.8(2) 4_545 . . . ?
C7 C5 C6 O3 1.9(5) . . . . ?
C4 C5 C6 O3 178.9(3) . . . . ?
C7 C5 C6 O4 -176.3(3) . . . . ?
C4 C5 C6 O4 0.6(5) . . . . ?
C4 C5 C7 C8 -0.1(5) . . . . ?
C6 C5 C7 C8 176.9(3) . . . . ?
C5 C7 C8 O5 174.9(3) . . . . ?
C5 C7 C8 C2 -0.5(5) . . . . ?
C9 O5 C8 C7 117.3(3) . . . . ?
C9 O5 C8 C2 -67.5(4) . . . . ?
C3 C2 C8 C7 0.0(5) . . . . ?
C1 C2 C8 C7 178.6(3) . . . . ?
C3 C2 C8 O5 -174.9(3) . . . . ?
C1 C2 C8 O5 3.6(5) . . . . ?
C8 O5 C9 C10 -21.9(4) . . . . ?
C8 O5 C9 C14 161.9(3) . . . . ?
C14 C9 C10 C11 -0.2(5) . . . . ?
O5 C9 C10 C11 -176.2(3) . . . . ?
C9 C10 C11 C12 1.1(5) . . . . ?
C10 C11 C12 C13 -0.9(5) . . . . ?
C11 C12 C13 C14 -0.1(5) . . . . ?
C10 C9 C14 C13 -0.8(5) . . . . ?
O5 C9 C14 C13 175.5(3) . . . . ?
C10 C9 C14 C15 179.5(3) . . . . ?
O5 C9 C14 C15 -4.2(4) . . . . ?
C12 C13 C14 C9 1.0(5) . . . . ?
C12 C13 C14 C15 -179.3(3) . . . . ?
Mn1 O7 C15 O6 -5.2(6) 2_655 . . . ?
Mn2 O7 C15 O6 163.2(4) 2_655 . . . ?
Mn1 O7 C15 C14 176.9(2) 2_655 . . . ?
Mn2 O7 C15 C14 -14.7(4) 2_655 . . . ?
C9 C14 C15 O6 104.2(4) . . . . ?
C13 C14 C15 O6 -75.5(5) . . . . ?
C9 C14 C15 O7 -77.8(4) . . . . ?
C13 C14 C15 O7 102.5(4) . . . . ?
C20 N2 C16 C17 0.2(6) . . . . ?
Mn1 N2 C16 C17 -176.9(3) . . . . ?
N2 C16 C17 C18 -1.7(6) . . . . ?
C16 C17 C18 C19 1.9(6) . . . . ?
C17 C18 C19 C20 -0.7(6) . . . . ?
C17 C18 C19 C21 178.0(4) . . . . ?
C16 N2 C20 C19 1.1(5) . . . . ?
Mn1 N2 C20 C19 178.5(3) . . . . ?
C16 N2 C20 C24 -176.9(3) . . . . ?
Mn1 N2 C20 C24 0.4(4) . . . . ?
C18 C19 C20 N2 -0.9(5) . . . . ?
C21 C19 C20 N2 -179.7(3) . . . . ?
C18 C19 C20 C24 177.1(3) . . . . ?
C21 C19 C20 C24 -1.7(5) . . . . ?
C18 C19 C21 C22 -176.0(4) . . . . ?
C20 C19 C21 C22 2.7(6) . . . . ?
C19 C21 C22 C23 -0.7(6) . . . . ?
C21 C22 C23 C25 178.3(4) . . . . ?
C21 C22 C23 C24 -2.3(6) . . . . ?
C27 N1 C24 C23 1.5(5) . . . . ?
Mn1 N1 C24 C23 -176.5(2) . . . . ?
C27 N1 C24 C20 179.9(3) . . . . ?
Mn1 N1 C24 C20 1.9(4) . . . . ?
C25 C23 C24 N1 1.0(5) . . . . ?
C22 C23 C24 N1 -178.5(3) . . . . ?
C25 C23 C24 C20 -177.4(3) . . . . ?
C22 C23 C24 C20 3.2(5) . . . . ?
N2 C20 C24 N1 -1.6(5) . . . . ?
C19 C20 C24 N1 -179.7(3) . . . . ?
N2 C20 C24 C23 176.9(3) . . . . ?
C19 C20 C24 C23 -1.2(5) . . . . ?
C24 C23 C25 C26 -2.6(5) . . . . ?
C22 C23 C25 C26 176.8(4) . . . . ?
C23 C25 C26 C27 1.9(6) . . . . ?
C24 N1 C27 C26 -2.3(5) . . . . ?
Mn1 N1 C27 C26 175.4(3) . . . . ?
C25 C26 C27 N1 0.7(6) . . . . ?
C33 N3 C28 C29 -1.3(7) . . . . ?
Mn2 N3 C28 C29 164.8(4) . . . . ?
Mn2 N3 C28 C29 -171.0(4) 2_655 . . . ?
N3 C28 C29 C30 0.5(9) . . . . ?
C28 C29 C30 C31 0.4(8) . . . . ?
C29 C30 C31 C33 -0.4(6) . . . . ?
C29 C30 C31 C32 177.6(5) . . . . ?
C33 C31 C32 C32 0.6(7) . . . 2_655 ?
C30 C31 C32 C32 -177.4(5) . . . 2_655 ?
C28 N3 C33 C31 1.3(5) . . . . ?
Mn2 N3 C33 C31 -164.1(3) . . . . ?
Mn2 N3 C33 C31 173.2(3) 2_655 . . . ?
C28 N3 C33 C33 179.8(4) . . . 2_655 ?
Mn2 N3 C33 C33 14.5(5) . . . 2_655 ?
Mn2 N3 C33 C33 -8.3(4) 2_655 . . 2_655 ?
C30 C31 C33 N3 -0.4(5) . . . . ?
C32 C31 C33 N3 -178.5(3) . . . . ?
C30 C31 C33 C33 -179.0(4) . . . 2_655 ?
C32 C31 C33 C33 3.0(6) . . . 2_655 ?

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
O8 H2W O6 0.82 2.15 2.826(4) 140.3 2_655
O8 H1W O3 0.84 1.94 2.750(3) 160.1 4

_refine_diff_density_max         0.333
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.065


# start Validation Reply Form
_vrf_PLAT910_I                   
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min) 11 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_283-15Mn1
_database_code_depnum_ccdc_archive 'CCDC 1509059'
_audit_update_record             
;
2017-03-26 deposited with the CCDC.
2017-04-10 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            'C27 H18 Mn N2 O8'
_chemical_formula_weight         553.37

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'
Mn Mn 0.3368 0.7283 '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'
H H 0.0000 0.0000 '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                   10.3948(10)
_cell_length_b                   7.9986(6)
_cell_length_c                   28.3241(17)
_cell_angle_alpha                90
_cell_angle_beta                 93.650(7)
_cell_angle_gamma                90
_cell_volume                     2350.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    14824
_cell_measurement_theta_min      3.268
_cell_measurement_theta_max      25.048

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_F_000             1132
_exptl_transmission_factor_min   0.846
_exptl_transmission_factor_max   0.867
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.230
_exptl_absorpt_coefficient_mu    0.620
_shelx_estimated_absorpt_T_min   0.851
_shelx_estimated_absorpt_T_max   0.871
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.851
_exptl_absorpt_correction_T_max  0.871
_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            14824
_diffrn_reflns_av_unetI/netI     0.0483
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         3.268
_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             4163
_reflns_number_gt                3263
_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)+(0.0263P)²+2.0850P] 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         4163
_refine_ls_number_parameters     344
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0410
_refine_ls_wR_factor_ref         0.0932
_refine_ls_wR_factor_gt          0.0838
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      1.011
_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
Mn1 Mn 0.43503(4) 0.83104(5) 0.29580(2) 0.02589(13) Uani 1 1 d . . . . .
N1 N 0.3009(2) 0.8097(3) 0.35806(8) 0.0332(6) Uani 1 1 d . . . . .
N2 N 0.2453(2) 0.7155(3) 0.26690(8) 0.0317(6) Uani 1 1 d . . . . .
O1 O 0.52022(18) 0.8177(2) 0.22808(6) 0.0292(4) Uani 1 1 d . . . . .
O2 O 0.63171(19) 0.5795(2) 0.22504(6) 0.0316(5) Uani 1 1 d . . . . .
O3 O 0.8276(2) 0.8285(3) 0.00210(7) 0.0424(5) Uani 1 1 d . . . . .
O4 O 0.6207(2) 0.7736(3) -0.01675(7) 0.0501(6) Uani 1 1 d . . . . .
H4 H 0.6464 0.7644 -0.0434 0.075 Uiso 1 1 calc R U . . .
O5 O 0.40158(17) 0.7787(2) 0.13481(6) 0.0259(4) Uani 1 1 d . . . . .
O6 O 0.33915(19) 0.2691(2) 0.10642(6) 0.0330(5) Uani 1 1 d . . . . .
O7 O 0.41806(19) 0.4531(2) 0.15983(7) 0.0339(5) Uani 1 1 d . . . . .
O8 O 0.5159(2) 0.6051(2) 0.32273(7) 0.0500(6) Uani 1 1 d . . . . .
H8A H 0.5189 0.5148 0.3073 0.060 Uiso 1 1 d R U . . .
H8B H 0.5722 0.6261 0.3435 0.060 Uiso 1 1 d R U . . .
C1 C 0.5886(3) 0.7134(3) 0.20759(9) 0.0245(6) Uani 1 1 d . . . . .
C2 C 0.6223(3) 0.7524(3) 0.15759(9) 0.0243(6) Uani 1 1 d . . . . .
C3 C 0.7500(3) 0.7604(4) 0.14600(10) 0.0325(7) Uani 1 1 d . . . . .
H3 H 0.8154 0.7504 0.1698 0.039 Uiso 1 1 calc R U . . .
C4 C 0.7816(3) 0.7830(4) 0.09984(10) 0.0343(7) Uani 1 1 d . . . . .
H4A H 0.8675 0.7922 0.0928 0.041 Uiso 1 1 calc R U . . .
C5 C 0.6847(3) 0.7918(3) 0.06390(9) 0.0279(6) Uani 1 1 d . . . . .
C6 C 0.7198(3) 0.8016(4) 0.01387(10) 0.0310(7) Uani 1 1 d . . . . .
C7 C 0.5564(3) 0.7861(3) 0.07473(9) 0.0270(6) Uani 1 1 d . . . . .
H7 H 0.4910 0.7924 0.0508 0.032 Uiso 1 1 calc R U . . .
C8 C 0.5268(2) 0.7711(3) 0.12141(9) 0.0224(6) Uani 1 1 d . . . . .
C9 C 0.3023(3) 0.7225(3) 0.10345(9) 0.0238(6) Uani 1 1 d . . . . .
C10 C 0.2276(3) 0.8435(3) 0.08079(10) 0.0292(6) Uani 1 1 d . . . . .
H10 H 0.2512 0.9553 0.0838 0.035 Uiso 1 1 calc R U . . .
C11 C 0.1180(3) 0.8004(4) 0.05370(10) 0.0316(7) Uani 1 1 d . . . . .
H11 H 0.0664 0.8826 0.0390 0.038 Uiso 1 1 calc R U . . .
C12 C 0.0855(3) 0.6332(4) 0.04862(10) 0.0326(7) Uani 1 1 d . . . . .
H12 H 0.0106 0.6026 0.0310 0.039 Uiso 1 1 calc R U . . .
C13 C 0.1644(3) 0.5122(4) 0.06965(9) 0.0292(6) Uani 1 1 d . . . . .
H13 H 0.1441 0.4001 0.0645 0.035 Uiso 1 1 calc R U . . .
C14 C 0.2738(2) 0.5533(3) 0.09843(9) 0.0227(6) Uani 1 1 d . . . . .
C15 C 0.3499(3) 0.4149(3) 0.12327(9) 0.0261(6) Uani 1 1 d . . . . .
C16 C 0.3294(3) 0.8459(4) 0.40315(11) 0.0430(8) Uani 1 1 d . . . . .
H16 H 0.4097 0.8924 0.4114 0.052 Uiso 1 1 calc R U . . .
C17 C 0.2464(4) 0.8183(5) 0.43881(12) 0.0518(9) Uani 1 1 d . . . . .
H17 H 0.2714 0.8437 0.4701 0.062 Uiso 1 1 calc R U . . .
C18 C 0.1274(3) 0.7534(4) 0.42716(11) 0.0468(9) Uani 1 1 d . . . . .
H18 H 0.0701 0.7348 0.4505 0.056 Uiso 1 1 calc R U . . .
C19 C 0.0918(3) 0.7149(4) 0.38008(11) 0.0376(7) Uani 1 1 d . . . . .
C20 C 0.1827(3) 0.7415(3) 0.34673(10) 0.0305(7) Uani 1 1 d . . . . .
C21 C -0.0320(3) 0.6511(4) 0.36498(13) 0.0509(9) Uani 1 1 d . . . . .
H21 H -0.0934 0.6372 0.3871 0.061 Uiso 1 1 calc R U . . .
C22 C -0.0624(3) 0.6105(4) 0.31956(14) 0.0522(9) Uani 1 1 d . . . . .
H22 H -0.1444 0.5705 0.3106 0.063 Uiso 1 1 calc R U . . .
C23 C 0.0311(3) 0.6288(4) 0.28500(11) 0.0387(8) Uani 1 1 d . . . . .
C24 C 0.1528(3) 0.6944(3) 0.29814(10) 0.0297(7) Uani 1 1 d . . . . .
C25 C 0.0054(3) 0.5853(4) 0.23728(12) 0.0496(9) Uani 1 1 d . . . . .
H25 H -0.0749 0.5431 0.2270 0.059 Uiso 1 1 calc R U . . .
C26 C 0.0991(3) 0.6053(5) 0.20631(12) 0.0516(9) Uani 1 1 d . . . . .
H26 H 0.0840 0.5755 0.1747 0.062 Uiso 1 1 calc R U . . .
C27 C 0.2171(3) 0.6706(4) 0.22256(11) 0.0429(8) Uani 1 1 d . . . . .
H27 H 0.2801 0.6837 0.2010 0.051 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
Mn1 O8 2.114(2) . ?
Mn1 O7 2.1493(19) 2_655 ?
Mn1 O1 2.1659(18) . ?
Mn1 O2 2.1742(19) 2_655 ?
Mn1 N2 2.282(2) . ?
Mn1 N1 2.323(2) . ?
N1 C16 1.325(4) . ?
N1 C20 1.364(4) . ?
N2 C27 1.321(4) . ?
N2 C24 1.358(3) . ?
O1 C1 1.261(3) . ?
O2 C1 1.251(3) . ?
O2 Mn1 2.1742(19) 2_645 ?
O3 C6 1.208(3) . ?
O4 C6 1.323(3) . ?
O4 H4 0.8200 . ?
O5 C8 1.380(3) . ?
O5 C9 1.392(3) . ?
O6 C15 1.262(3) . ?
O7 C15 1.254(3) . ?
O7 Mn1 2.1493(19) 2_645 ?
O8 H8A 0.8454 . ?
O8 H8B 0.8200 . ?
C1 C2 1.513(4) . ?
C2 C3 1.388(4) . ?
C2 C8 1.389(4) . ?
C3 C4 1.380(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.387(4) . ?
C4 H4A 0.9300 . ?
C5 C7 1.389(4) . ?
C5 C6 1.488(4) . ?
C7 C8 1.382(4) . ?
C7 H7 0.9300 . ?
C9 C10 1.374(4) . ?
C9 C14 1.391(4) . ?
C10 C11 1.376(4) . ?
C10 H10 0.9300 . ?
C11 C12 1.384(4) . ?
C11 H11 0.9300 . ?
C12 C13 1.379(4) . ?
C12 H12 0.9300 . ?
C13 C14 1.396(4) . ?
C13 H13 0.9300 . ?
C14 C15 1.509(4) . ?
C16 C17 1.388(4) . ?
C16 H16 0.9300 . ?
C17 C18 1.362(5) . ?
C17 H17 0.9300 . ?
C18 C19 1.396(5) . ?
C18 H18 0.9300 . ?
C19 C20 1.394(4) . ?
C19 C21 1.424(5) . ?
C20 C24 1.442(4) . ?
C21 C22 1.345(5) . ?
C21 H21 0.9300 . ?
C22 C23 1.431(4) . ?
C22 H22 0.9300 . ?
C23 C24 1.397(4) . ?
C23 C25 1.405(4) . ?
C25 C26 1.361(4) . ?
C25 H25 0.9300 . ?
C26 C27 1.385(4) . ?
C26 H26 0.9300 . ?
C27 H27 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
O8 Mn1 O7 85.75(8) . 2_655 ?
O8 Mn1 O1 95.84(8) . . ?
O7 Mn1 O1 103.00(7) 2_655 . ?
O8 Mn1 O2 172.58(8) . 2_655 ?
O7 Mn1 O2 86.92(7) 2_655 2_655 ?
O1 Mn1 O2 86.91(7) . 2_655 ?
O8 Mn1 N2 95.61(9) . . ?
O7 Mn1 N2 163.58(8) 2_655 . ?
O1 Mn1 N2 93.16(8) . . ?
O2 Mn1 N2 91.11(8) 2_655 . ?
O8 Mn1 N1 84.68(9) . . ?
O7 Mn1 N1 91.61(8) 2_655 . ?
O1 Mn1 N1 165.39(8) . . ?
O2 Mn1 N1 94.40(8) 2_655 . ?
N2 Mn1 N1 72.28(8) . . ?
C16 N1 C20 117.2(3) . . ?
C16 N1 Mn1 127.4(2) . . ?
C20 N1 Mn1 115.22(18) . . ?
C27 N2 C24 117.5(3) . . ?
C27 N2 Mn1 125.9(2) . . ?
C24 N2 Mn1 116.64(18) . . ?
C1 O1 Mn1 135.59(17) . . ?
C1 O2 Mn1 125.12(17) . 2_645 ?
C6 O4 H4 109.5 . . ?
C8 O5 C9 118.92(19) . . ?
C15 O7 Mn1 135.63(18) . 2_645 ?
Mn1 O8 H8A 124.8 . . ?
Mn1 O8 H8B 109.4 . . ?
H8A O8 H8B 119.8 . . ?
O2 C1 O1 125.6(2) . . ?
O2 C1 C2 116.6(2) . . ?
O1 C1 C2 117.7(2) . . ?
C3 C2 C8 118.0(2) . . ?
C3 C2 C1 120.9(2) . . ?
C8 C2 C1 121.0(2) . . ?
C4 C3 C2 121.3(3) . . ?
C4 C3 H3 119.4 . . ?
C2 C3 H3 119.4 . . ?
C3 C4 C5 119.8(3) . . ?
C3 C4 H4A 120.1 . . ?
C5 C4 H4A 120.1 . . ?
C4 C5 C7 119.9(2) . . ?
C4 C5 C6 119.4(2) . . ?
C7 C5 C6 120.6(3) . . ?
O3 C6 O4 123.1(3) . . ?
O3 C6 C5 124.1(3) . . ?
O4 C6 C5 112.8(2) . . ?
C8 C7 C5 119.3(2) . . ?
C8 C7 H7 120.3 . . ?
C5 C7 H7 120.3 . . ?
O5 C8 C7 122.0(2) . . ?
O5 C8 C2 116.4(2) . . ?
C7 C8 C2 121.6(2) . . ?
C10 C9 C14 121.8(3) . . ?
C10 C9 O5 116.4(2) . . ?
C14 C9 O5 121.6(2) . . ?
C9 C10 C11 120.5(3) . . ?
C9 C10 H10 119.8 . . ?
C11 C10 H10 119.8 . . ?
C10 C11 C12 119.2(3) . . ?
C10 C11 H11 120.4 . . ?
C12 C11 H11 120.4 . . ?
C13 C12 C11 120.0(3) . . ?
C13 C12 H12 120.0 . . ?
C11 C12 H12 120.0 . . ?
C12 C13 C14 121.8(3) . . ?
C12 C13 H13 119.1 . . ?
C14 C13 H13 119.1 . . ?
C9 C14 C13 116.7(2) . . ?
C9 C14 C15 124.3(2) . . ?
C13 C14 C15 118.9(2) . . ?
O7 C15 O6 124.7(3) . . ?
O7 C15 C14 117.3(2) . . ?
O6 C15 C14 118.0(2) . . ?
N1 C16 C17 123.7(3) . . ?
N1 C16 H16 118.1 . . ?
C17 C16 H16 118.1 . . ?
C18 C17 C16 118.8(3) . . ?
C18 C17 H17 120.6 . . ?
C16 C17 H17 120.6 . . ?
C17 C18 C19 119.9(3) . . ?
C17 C18 H18 120.1 . . ?
C19 C18 H18 120.1 . . ?
C20 C19 C18 117.6(3) . . ?
C20 C19 C21 119.3(3) . . ?
C18 C19 C21 123.1(3) . . ?
N1 C20 C19 122.7(3) . . ?
N1 C20 C24 117.7(2) . . ?
C19 C20 C24 119.5(3) . . ?
C22 C21 C19 121.8(3) . . ?
C22 C21 H21 119.1 . . ?
C19 C21 H21 119.1 . . ?
C21 C22 C23 120.1(3) . . ?
C21 C22 H22 120.0 . . ?
C23 C22 H22 120.0 . . ?
C24 C23 C25 117.6(3) . . ?
C24 C23 C22 119.9(3) . . ?
C25 C23 C22 122.5(3) . . ?
N2 C24 C23 122.7(3) . . ?
N2 C24 C20 118.1(3) . . ?
C23 C24 C20 119.3(3) . . ?
C26 C25 C23 119.4(3) . . ?
C26 C25 H25 120.3 . . ?
C23 C25 H25 120.3 . . ?
C25 C26 C27 119.0(3) . . ?
C25 C26 H26 120.5 . . ?
C27 C26 H26 120.5 . . ?
N2 C27 C26 123.9(3) . . ?
N2 C27 H27 118.1 . . ?
C26 C27 H27 118.1 . . ?

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
Mn1 O2 C1 O1 108.9(3) 2_645 . . . ?
Mn1 O2 C1 C2 -71.3(3) 2_645 . . . ?
Mn1 O1 C1 O2 -3.2(4) . . . . ?
Mn1 O1 C1 C2 177.01(17) . . . . ?
O2 C1 C2 C3 -56.7(3) . . . . ?
O1 C1 C2 C3 123.1(3) . . . . ?
O2 C1 C2 C8 119.2(3) . . . . ?
O1 C1 C2 C8 -60.9(3) . . . . ?
C8 C2 C3 C4 -1.2(4) . . . . ?
C1 C2 C3 C4 174.9(3) . . . . ?
C2 C3 C4 C5 -2.4(4) . . . . ?
C3 C4 C5 C7 3.1(4) . . . . ?
C3 C4 C5 C6 -174.8(3) . . . . ?
C4 C5 C6 O3 -12.0(4) . . . . ?
C7 C5 C6 O3 170.1(3) . . . . ?
C4 C5 C6 O4 166.5(3) . . . . ?
C7 C5 C6 O4 -11.5(4) . . . . ?
C4 C5 C7 C8 -0.2(4) . . . . ?
C6 C5 C7 C8 177.7(2) . . . . ?
C9 O5 C8 C7 30.7(3) . . . . ?
C9 O5 C8 C2 -151.2(2) . . . . ?
C5 C7 C8 O5 174.5(2) . . . . ?
C5 C7 C8 C2 -3.5(4) . . . . ?
C3 C2 C8 O5 -173.9(2) . . . . ?
C1 C2 C8 O5 10.0(4) . . . . ?
C3 C2 C8 C7 4.2(4) . . . . ?
C1 C2 C8 C7 -171.9(2) . . . . ?
C8 O5 C9 C10 -105.0(3) . . . . ?
C8 O5 C9 C14 80.3(3) . . . . ?
C14 C9 C10 C11 2.7(4) . . . . ?
O5 C9 C10 C11 -172.0(2) . . . . ?
C9 C10 C11 C12 -1.5(4) . . . . ?
C10 C11 C12 C13 -1.6(4) . . . . ?
C11 C12 C13 C14 3.6(4) . . . . ?
C10 C9 C14 C13 -0.7(4) . . . . ?
O5 C9 C14 C13 173.7(2) . . . . ?
C10 C9 C14 C15 -178.4(2) . . . . ?
O5 C9 C14 C15 -4.0(4) . . . . ?
C12 C13 C14 C9 -2.4(4) . . . . ?
C12 C13 C14 C15 175.4(2) . . . . ?
Mn1 O7 C15 O6 12.1(4) 2_645 . . . ?
Mn1 O7 C15 C14 -169.18(17) 2_645 . . . ?
C9 C14 C15 O7 21.0(4) . . . . ?
C13 C14 C15 O7 -156.6(3) . . . . ?
C9 C14 C15 O6 -160.2(2) . . . . ?
C13 C14 C15 O6 22.2(4) . . . . ?
C20 N1 C16 C17 0.0(5) . . . . ?
Mn1 N1 C16 C17 -175.2(2) . . . . ?
N1 C16 C17 C18 -1.3(5) . . . . ?
C16 C17 C18 C19 0.5(5) . . . . ?
C17 C18 C19 C20 1.5(5) . . . . ?
C17 C18 C19 C21 -178.2(3) . . . . ?
C16 N1 C20 C19 2.2(4) . . . . ?
Mn1 N1 C20 C19 178.0(2) . . . . ?
C16 N1 C20 C24 -177.2(3) . . . . ?
Mn1 N1 C20 C24 -1.4(3) . . . . ?
C18 C19 C20 N1 -3.0(4) . . . . ?
C21 C19 C20 N1 176.8(3) . . . . ?
C18 C19 C20 C24 176.4(3) . . . . ?
C21 C19 C20 C24 -3.8(4) . . . . ?
C20 C19 C21 C22 2.2(5) . . . . ?
C18 C19 C21 C22 -178.0(3) . . . . ?
C19 C21 C22 C23 0.8(5) . . . . ?
C21 C22 C23 C24 -2.2(5) . . . . ?
C21 C22 C23 C25 178.7(3) . . . . ?
C27 N2 C24 C23 -0.3(4) . . . . ?
Mn1 N2 C24 C23 178.5(2) . . . . ?
C27 N2 C24 C20 179.5(3) . . . . ?
Mn1 N2 C24 C20 -1.8(3) . . . . ?
C25 C23 C24 N2 -0.6(4) . . . . ?
C22 C23 C24 N2 -179.7(3) . . . . ?
C25 C23 C24 C20 179.7(3) . . . . ?
C22 C23 C24 C20 0.6(4) . . . . ?
N1 C20 C24 N2 2.1(4) . . . . ?
C19 C20 C24 N2 -177.3(3) . . . . ?
N1 C20 C24 C23 -178.1(3) . . . . ?
C19 C20 C24 C23 2.5(4) . . . . ?
C24 C23 C25 C26 1.2(5) . . . . ?
C22 C23 C25 C26 -179.7(3) . . . . ?
C23 C25 C26 C27 -1.0(5) . . . . ?
C24 N2 C27 C26 0.5(5) . . . . ?
Mn1 N2 C27 C26 -178.1(3) . . . . ?
C25 C26 C27 N2 0.1(6) . . . . ?

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
O4 H4 O6 0.82 1.82 2.622(3) 165.4 3_665
O8 H8A O1 0.85 1.90 2.726(3) 165.6 2_645
O8 H8B O6 0.82 2.00 2.763(3) 154.3 2_655

_refine_diff_density_max         0.262
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.056


# start Validation Reply Form
_vrf_PLAT910_I                   
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min) 8 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_277-4Cd
_database_code_depnum_ccdc_archive 'CCDC 1509368'
_audit_update_record             
;
2017-03-26 deposited with the CCDC.
2017-04-10 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 H23 Cd2 Cl N4 O7'
_chemical_formula_weight         919.86

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'
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/n'
_space_group_name_Hall           '-P 2yn'

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

_cell_length_a                   9.9405(4)
_cell_length_b                   17.5969(7)
_cell_length_c                   19.2671(7)
_cell_angle_alpha                90
_cell_angle_beta                 95.778(4)
_cell_angle_gamma                90
_cell_volume                     3353.1(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    12410
_cell_measurement_theta_min      3.314
_cell_measurement_theta_max      25.048

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.822
_exptl_crystal_F_000             1816
_exptl_transmission_factor_min   0.720
_exptl_transmission_factor_max   0.776
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    1.408
_shelx_estimated_absorpt_T_min   0.702
_shelx_estimated_absorpt_T_max   0.786
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.702
_exptl_absorpt_correction_T_max  0.786
_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            12410
_diffrn_reflns_av_unetI/netI     0.0932
_diffrn_reflns_av_R_equivalents  0.0528
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.314
_diffrn_reflns_theta_max         25.048
_diffrn_reflns_theta_full        25.048
_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             5918
_reflns_number_gt                3970
_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)+(0.0275P)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         5918
_refine_ls_number_parameters     478
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0474
_refine_ls_wR_factor_ref         0.1061
_refine_ls_wR_factor_gt          0.0819
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.015
_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 0.55369(5) 0.28319(2) 0.08967(2) 0.03154(15) Uani 1 1 d . . . . .
Cd2 Cd 0.55668(5) 0.15113(3) -0.05433(2) 0.03578(16) Uani 1 1 d . . . . .
Cl1 Cl 0.69179(17) 0.26888(9) -0.01571(9) 0.0451(4) Uani 1 1 d . . . . .
N1 N 0.3268(5) 0.2599(3) 0.1110(3) 0.0373(13) Uani 1 1 d . . . . .
N2 N 0.4048(6) 0.3598(3) 0.0157(3) 0.0432(15) Uani 1 1 d . . . . .
N3 N 0.3965(6) 0.2235(3) -0.1233(3) 0.0382(13) Uani 1 1 d . . . . .
N4 N 0.3396(5) 0.1259(3) -0.0212(3) 0.0361(13) Uani 1 1 d . . . . .
O1 O 0.5950(5) 0.1646(2) 0.1271(2) 0.0407(11) Uani 1 1 d . . . . .
O2 O 0.6471(5) 0.0877(2) 0.0419(2) 0.0505(13) Uani 1 1 d . . . . .
O3 O 0.9462(5) -0.1543(3) 0.3033(3) 0.0587(15) Uani 1 1 d . . . . .
O4 O 0.7712(5) -0.1363(3) 0.3598(2) 0.0648(16) Uani 1 1 d . . . . .
O5 O 0.4864(4) 0.0592(2) 0.2151(2) 0.0368(11) Uani 1 1 d . . . . .
O6 O 0.3224(5) -0.1568(3) 0.1726(3) 0.0663(16) Uani 1 1 d . . . . .
O7 O 0.4029(5) -0.0567(3) 0.1238(2) 0.0553(14) Uani 1 1 d . . . . .
C1 C 0.6374(6) 0.1041(4) 0.1044(3) 0.0335(15) Uani 1 1 d . . . . .
C2 C 0.6854(6) 0.0446(3) 0.1576(3) 0.0296(15) Uani 1 1 d . . . . .
C3 C 0.8090(6) 0.0089(3) 0.1535(3) 0.0321(15) Uani 1 1 d . . . . .
H3 H 0.8603 0.0213 0.1173 0.039 Uiso 1 1 calc R U . . .
C4 C 0.8575(6) -0.0452(3) 0.2025(3) 0.0361(16) Uani 1 1 d . . . . .
H4 H 0.9420 -0.0670 0.1996 0.043 Uiso 1 1 calc R U . . .
C5 C 0.7814(6) -0.0667(3) 0.2554(3) 0.0279(14) Uani 1 1 d . . . . .
C6 C 0.8356(7) -0.1229(3) 0.3092(3) 0.0361(16) Uani 1 1 d . . . . .
C7 C 0.6545(6) -0.0328(3) 0.2581(3) 0.0328(15) Uani 1 1 d . . . . .
H7 H 0.6000 -0.0478 0.2921 0.039 Uiso 1 1 calc R U . . .
C8 C 0.6095(6) 0.0229(3) 0.2106(3) 0.0277(14) Uani 1 1 d . . . . .
C9 C 0.3901(6) 0.0260(4) 0.2536(3) 0.0333(15) Uani 1 1 d . . . . .
C10 C 0.3579(7) 0.0685(4) 0.3103(3) 0.0466(19) Uani 1 1 d . . . . .
H10 H 0.4054 0.1128 0.3227 0.056 Uiso 1 1 calc R U . . .
C11 C 0.2553(8) 0.0450(4) 0.3483(4) 0.059(2) Uani 1 1 d . . . . .
H11 H 0.2317 0.0738 0.3856 0.071 Uiso 1 1 calc R U . . .
C12 C 0.1889(8) -0.0209(4) 0.3306(4) 0.057(2) Uani 1 1 d . . . . .
H12 H 0.1198 -0.0370 0.3563 0.068 Uiso 1 1 calc R U . . .
C13 C 0.2223(7) -0.0643(4) 0.2751(4) 0.0450(18) Uani 1 1 d . . . . .
H13 H 0.1759 -0.1094 0.2643 0.054 Uiso 1 1 calc R U . . .
C14 C 0.3236(6) -0.0417(3) 0.2354(3) 0.0330(15) Uani 1 1 d . . . . .
C15 C 0.3527(7) -0.0889(4) 0.1729(4) 0.0422(17) Uani 1 1 d . . . . .
C16 C 0.2910(8) 0.2131(4) 0.1596(4) 0.052(2) Uani 1 1 d . . . . .
H16 H 0.3566 0.1812 0.1816 0.063 Uiso 1 1 calc R U . . .
C17 C 0.1611(9) 0.2092(5) 0.1796(5) 0.072(3) Uani 1 1 d . . . . .
H17 H 0.1405 0.1762 0.2148 0.087 Uiso 1 1 calc R U . . .
C18 C 0.0640(8) 0.2551(5) 0.1463(5) 0.071(3) Uani 1 1 d . . . . .
H18 H -0.0241 0.2533 0.1585 0.085 Uiso 1 1 calc R U . . .
C19 C 0.0967(7) 0.3042(4) 0.0943(4) 0.0485(19) Uani 1 1 d . . . . .
C20 C 0.2318(7) 0.3049(4) 0.0779(3) 0.0370(16) Uani 1 1 d . . . . .
C21 C 0.0009(8) 0.3540(5) 0.0548(5) 0.071(3) Uani 1 1 d . . . . .
H21 H -0.0886 0.3547 0.0651 0.085 Uiso 1 1 calc R U . . .
C22 C 0.0381(8) 0.3988(5) 0.0044(5) 0.072(3) Uani 1 1 d . . . . .
H22 H -0.0269 0.4279 -0.0216 0.087 Uiso 1 1 calc R U . . .
C23 C 0.1746(8) 0.4031(5) -0.0106(4) 0.055(2) Uani 1 1 d . . . . .
C24 C 0.2717(7) 0.3563(4) 0.0264(3) 0.0391(17) Uani 1 1 d . . . . .
C25 C 0.2195(11) 0.4515(5) -0.0606(4) 0.086(3) Uani 1 1 d . . . . .
H25 H 0.1586 0.4833 -0.0863 0.104 Uiso 1 1 calc R U . . .
C26 C 0.3504(10) 0.4522(5) -0.0718(5) 0.089(3) Uani 1 1 d . . . . .
H26 H 0.3805 0.4839 -0.1057 0.107 Uiso 1 1 calc R U . . .
C27 C 0.4408(9) 0.4053(4) -0.0323(4) 0.068(2) Uani 1 1 d . . . . .
H27 H 0.5313 0.4065 -0.0406 0.081 Uiso 1 1 calc R U . . .
C28 C 0.4264(8) 0.2699(4) -0.1738(4) 0.055(2) Uani 1 1 d . . . . .
H28 H 0.5169 0.2777 -0.1802 0.066 Uiso 1 1 calc R U . . .
C29 C 0.3269(9) 0.3078(4) -0.2181(4) 0.061(2) Uani 1 1 d . . . . .
H29 H 0.3510 0.3404 -0.2528 0.073 Uiso 1 1 calc R U . . .
C30 C 0.1960(9) 0.2956(4) -0.2091(4) 0.058(2) Uani 1 1 d . . . . .
H30 H 0.1286 0.3192 -0.2385 0.070 Uiso 1 1 calc R U . . .
C31 C 0.1608(7) 0.2482(4) -0.1563(4) 0.0443(18) Uani 1 1 d . . . . .
C32 C 0.2663(7) 0.2125(3) -0.1140(3) 0.0356(16) Uani 1 1 d . . . . .
C33 C 0.0226(8) 0.2331(4) -0.1439(4) 0.061(2) Uani 1 1 d . . . . .
H33 H -0.0482 0.2548 -0.1724 0.074 Uiso 1 1 calc R U . . .
C34 C -0.0031(8) 0.1873(5) -0.0907(5) 0.065(2) Uani 1 1 d . . . . .
H34 H -0.0929 0.1794 -0.0829 0.078 Uiso 1 1 calc R U . . .
C35 C 0.0971(7) 0.1510(4) -0.0465(4) 0.0474(19) Uani 1 1 d . . . . .
C36 C 0.2357(7) 0.1622(3) -0.0587(3) 0.0348(16) Uani 1 1 d . . . . .
C37 C 0.0737(8) 0.1000(5) 0.0069(4) 0.063(2) Uani 1 1 d . . . . .
H37 H -0.0143 0.0908 0.0171 0.076 Uiso 1 1 calc R U . . .
C38 C 0.1778(9) 0.0642(4) 0.0437(4) 0.060(2) Uani 1 1 d . . . . .
H38 H 0.1618 0.0307 0.0793 0.072 Uiso 1 1 calc R U . . .
C39 C 0.3109(8) 0.0782(4) 0.0276(4) 0.0507(19) Uani 1 1 d . . . . .
H39 H 0.3816 0.0524 0.0527 0.061 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 2.232(4) . ?
Cd1 O3 2.337(4) 2_655 ?
Cd1 N1 2.369(5) . ?
Cd1 N2 2.369(5) . ?
Cd1 O4 2.376(5) 2_655 ?
Cd1 Cl1 2.5751(16) . ?
Cd1 C6 2.704(6) 2_655 ?
Cd2 O7 2.196(4) 3_655 ?
Cd2 O2 2.269(4) . ?
Cd2 N3 2.345(5) . ?
Cd2 N4 2.353(5) . ?
Cd2 Cl1 2.5396(17) . ?
N1 C16 1.322(8) . ?
N1 C20 1.343(8) . ?
N2 C27 1.302(8) . ?
N2 C24 1.360(8) . ?
N3 C28 1.327(8) . ?
N3 C32 1.338(8) . ?
N4 C39 1.313(7) . ?
N4 C36 1.359(7) . ?
O1 C1 1.241(7) . ?
O2 C1 1.252(7) . ?
O3 C6 1.246(7) . ?
O3 Cd1 2.337(4) 2_645 ?
O4 C6 1.242(7) . ?
O4 Cd1 2.376(5) 2_645 ?
O5 C8 1.391(6) . ?
O5 C9 1.397(7) . ?
O6 C15 1.233(7) . ?
O7 C15 1.249(7) . ?
O7 Cd2 2.196(4) 3_655 ?
C1 C2 1.508(8) . ?
C2 C8 1.383(8) . ?
C2 C3 1.389(8) . ?
C3 C4 1.392(8) . ?
C3 H3 0.9300 . ?
C4 C5 1.382(8) . ?
C4 H4 0.9300 . ?
C5 C7 1.402(8) . ?
C5 C6 1.493(8) . ?
C6 Cd1 2.704(6) 2_645 ?
C7 C8 1.385(8) . ?
C7 H7 0.9300 . ?
C9 C10 1.387(8) . ?
C9 C14 1.391(8) . ?
C10 C11 1.377(9) . ?
C10 H10 0.9300 . ?
C11 C12 1.360(9) . ?
C11 H11 0.9300 . ?
C12 C13 1.382(9) . ?
C12 H12 0.9300 . ?
C13 C14 1.383(8) . ?
C13 H13 0.9300 . ?
C14 C15 1.514(9) . ?
C16 C17 1.386(10) . ?
C16 H16 0.9300 . ?
C17 C18 1.368(11) . ?
C17 H17 0.9300 . ?
C18 C19 1.387(10) . ?
C18 H18 0.9300 . ?
C19 C20 1.410(9) . ?
C19 C21 1.452(10) . ?
C20 C24 1.428(9) . ?
C21 C22 1.333(10) . ?
C21 H21 0.9300 . ?
C22 C23 1.417(10) . ?
C22 H22 0.9300 . ?
C23 C25 1.394(10) . ?
C23 C24 1.407(9) . ?
C25 C26 1.340(11) . ?
C25 H25 0.9300 . ?
C26 C27 1.389(10) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
C28 C29 1.408(10) . ?
C28 H28 0.9300 . ?
C29 C30 1.348(10) . ?
C29 H29 0.9300 . ?
C30 C31 1.387(9) . ?
C30 H30 0.9300 . ?
C31 C32 1.410(9) . ?
C31 C33 1.442(10) . ?
C32 C36 1.441(8) . ?
C33 C34 1.349(10) . ?
C33 H33 0.9300 . ?
C34 C35 1.398(10) . ?
C34 H34 0.9300 . ?
C35 C37 1.402(9) . ?
C35 C36 1.434(9) . ?
C37 C38 1.350(10) . ?
C37 H37 0.9300 . ?
C38 C39 1.411(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 O3 99.84(17) . 2_655 ?
O1 Cd1 N1 85.95(17) . . ?
O3 Cd1 N1 81.06(17) 2_655 . ?
O1 Cd1 N2 144.06(18) . . ?
O3 Cd1 N2 101.98(18) 2_655 . ?
N1 Cd1 N2 69.80(19) . . ?
O1 Cd1 O4 108.79(18) . 2_655 ?
O3 Cd1 O4 54.72(15) 2_655 2_655 ?
N1 Cd1 O4 134.71(17) . 2_655 ?
N2 Cd1 O4 107.1(2) . 2_655 ?
O1 Cd1 Cl1 93.90(11) . . ?
O3 Cd1 Cl1 142.07(12) 2_655 . ?
N1 Cd1 Cl1 135.41(13) . . ?
N2 Cd1 Cl1 86.10(14) . . ?
O4 Cd1 Cl1 87.40(12) 2_655 . ?
O1 Cd1 C6 106.88(17) . 2_655 ?
O3 Cd1 C6 27.40(17) 2_655 2_655 ?
N1 Cd1 C6 107.9(2) . 2_655 ?
N2 Cd1 C6 105.65(18) . 2_655 ?
O4 Cd1 C6 27.34(17) 2_655 2_655 ?
Cl1 Cd1 C6 114.68(16) . 2_655 ?
O7 Cd2 O2 92.53(16) 3_655 . ?
O7 Cd2 N3 102.78(18) 3_655 . ?
O2 Cd2 N3 156.95(18) . . ?
O7 Cd2 N4 104.56(18) 3_655 . ?
O2 Cd2 N4 89.10(17) . . ?
N3 Cd2 N4 70.56(18) . . ?
O7 Cd2 Cl1 132.23(14) 3_655 . ?
O2 Cd2 Cl1 90.43(12) . . ?
N3 Cd2 Cl1 91.82(14) . . ?
N4 Cd2 Cl1 123.16(12) . . ?
Cd2 Cl1 Cd1 90.15(5) . . ?
C16 N1 C20 118.5(6) . . ?
C16 N1 Cd1 124.0(5) . . ?
C20 N1 Cd1 116.8(4) . . ?
C27 N2 C24 118.5(6) . . ?
C27 N2 Cd1 125.3(5) . . ?
C24 N2 Cd1 116.2(4) . . ?
C28 N3 C32 118.6(6) . . ?
C28 N3 Cd2 124.1(5) . . ?
C32 N3 Cd2 117.1(4) . . ?
C39 N4 C36 118.3(6) . . ?
C39 N4 Cd2 125.9(5) . . ?
C36 N4 Cd2 115.8(4) . . ?
C1 O1 Cd1 138.3(4) . . ?
C1 O2 Cd2 127.6(4) . . ?
C6 O3 Cd1 92.9(4) . 2_645 ?
C6 O4 Cd1 91.2(4) . 2_645 ?
C8 O5 C9 119.7(4) . . ?
C15 O7 Cd2 103.3(4) . 3_655 ?
O1 C1 O2 126.7(6) . . ?
O1 C1 C2 116.9(5) . . ?
O2 C1 C2 116.4(5) . . ?
C8 C2 C3 118.0(5) . . ?
C8 C2 C1 122.2(5) . . ?
C3 C2 C1 119.8(5) . . ?
C2 C3 C4 121.2(6) . . ?
C2 C3 H3 119.4 . . ?
C4 C3 H3 119.4 . . ?
C5 C4 C3 120.6(6) . . ?
C5 C4 H4 119.7 . . ?
C3 C4 H4 119.7 . . ?
C4 C5 C7 118.2(5) . . ?
C4 C5 C6 120.5(6) . . ?
C7 C5 C6 121.3(5) . . ?
O4 C6 O3 121.1(6) . . ?
O4 C6 C5 119.5(6) . . ?
O3 C6 C5 119.4(6) . . ?
O4 C6 Cd1 61.4(3) . 2_645 ?
O3 C6 Cd1 59.7(3) . 2_645 ?
C5 C6 Cd1 175.9(4) . 2_645 ?
C8 C7 C5 120.6(6) . . ?
C8 C7 H7 119.7 . . ?
C5 C7 H7 119.7 . . ?
C2 C8 C7 121.3(5) . . ?
C2 C8 O5 118.0(5) . . ?
C7 C8 O5 120.7(5) . . ?
C10 C9 C14 121.2(6) . . ?
C10 C9 O5 114.7(6) . . ?
C14 C9 O5 123.9(6) . . ?
C11 C10 C9 119.9(6) . . ?
C11 C10 H10 120.1 . . ?
C9 C10 H10 120.1 . . ?
C12 C11 C10 119.4(7) . . ?
C12 C11 H11 120.3 . . ?
C10 C11 H11 120.3 . . ?
C11 C12 C13 121.1(7) . . ?
C11 C12 H12 119.5 . . ?
C13 C12 H12 119.5 . . ?
C12 C13 C14 121.0(7) . . ?
C12 C13 H13 119.5 . . ?
C14 C13 H13 119.5 . . ?
C13 C14 C9 117.4(6) . . ?
C13 C14 C15 119.4(6) . . ?
C9 C14 C15 123.1(6) . . ?
O6 C15 O7 123.5(7) . . ?
O6 C15 C14 117.9(7) . . ?
O7 C15 C14 118.5(6) . . ?
N1 C16 C17 123.6(8) . . ?
N1 C16 H16 118.2 . . ?
C17 C16 H16 118.2 . . ?
C18 C17 C16 118.2(8) . . ?
C18 C17 H17 120.9 . . ?
C16 C17 H17 120.9 . . ?
C17 C18 C19 120.1(7) . . ?
C17 C18 H18 120.0 . . ?
C19 C18 H18 120.0 . . ?
C18 C19 C20 117.7(7) . . ?
C18 C19 C21 124.4(8) . . ?
C20 C19 C21 117.9(7) . . ?
N1 C20 C19 121.9(6) . . ?
N1 C20 C24 118.2(6) . . ?
C19 C20 C24 119.9(6) . . ?
C22 C21 C19 121.5(8) . . ?
C22 C21 H21 119.2 . . ?
C19 C21 H21 119.2 . . ?
C21 C22 C23 121.4(8) . . ?
C21 C22 H22 119.3 . . ?
C23 C22 H22 119.3 . . ?
C25 C23 C24 117.1(7) . . ?
C25 C23 C22 123.6(8) . . ?
C24 C23 C22 119.3(8) . . ?
N2 C24 C23 121.7(7) . . ?
N2 C24 C20 118.4(6) . . ?
C23 C24 C20 119.8(7) . . ?
C26 C25 C23 120.1(8) . . ?
C26 C25 H25 119.9 . . ?
C23 C25 H25 119.9 . . ?
C25 C26 C27 119.4(8) . . ?
C25 C26 H26 120.3 . . ?
C27 C26 H26 120.3 . . ?
N2 C27 C26 123.2(8) . . ?
N2 C27 H27 118.4 . . ?
C26 C27 H27 118.4 . . ?
N3 C28 C29 122.7(7) . . ?
N3 C28 H28 118.6 . . ?
C29 C28 H28 118.6 . . ?
C30 C29 C28 118.4(7) . . ?
C30 C29 H29 120.8 . . ?
C28 C29 H29 120.8 . . ?
C29 C30 C31 120.5(7) . . ?
C29 C30 H30 119.7 . . ?
C31 C30 H30 119.7 . . ?
C30 C31 C32 117.7(7) . . ?
C30 C31 C33 123.1(7) . . ?
C32 C31 C33 119.2(7) . . ?
N3 C32 C31 122.0(6) . . ?
N3 C32 C36 117.8(6) . . ?
C31 C32 C36 120.1(6) . . ?
C34 C33 C31 119.5(7) . . ?
C34 C33 H33 120.2 . . ?
C31 C33 H33 120.2 . . ?
C33 C34 C35 123.9(7) . . ?
C33 C34 H34 118.1 . . ?
C35 C34 H34 118.1 . . ?
C34 C35 C37 125.3(8) . . ?
C34 C35 C36 118.4(7) . . ?
C37 C35 C36 116.2(7) . . ?
N4 C36 C35 122.7(6) . . ?
N4 C36 C32 118.5(6) . . ?
C35 C36 C32 118.9(6) . . ?
C38 C37 C35 120.6(8) . . ?
C38 C37 H37 119.7 . . ?
C35 C37 H37 119.7 . . ?
C37 C38 C39 119.3(7) . . ?
C37 C38 H38 120.3 . . ?
C39 C38 H38 120.3 . . ?
N4 C39 C38 123.0(7) . . ?
N4 C39 H39 118.5 . . ?
C38 C39 H39 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 -15.9(11) . . . . ?
Cd1 O1 C1 C2 162.5(4) . . . . ?
Cd2 O2 C1 O1 -12.5(10) . . . . ?
Cd2 O2 C1 C2 169.1(4) . . . . ?
O1 C1 C2 C8 49.0(8) . . . . ?
O2 C1 C2 C8 -132.5(6) . . . . ?
O1 C1 C2 C3 -131.9(6) . . . . ?
O2 C1 C2 C3 46.7(8) . . . . ?
C8 C2 C3 C4 -2.1(9) . . . . ?
C1 C2 C3 C4 178.7(6) . . . . ?
C2 C3 C4 C5 2.2(9) . . . . ?
C3 C4 C5 C7 0.1(9) . . . . ?
C3 C4 C5 C6 -178.0(5) . . . . ?
Cd1 O4 C6 O3 3.0(7) 2_645 . . . ?
Cd1 O4 C6 C5 -175.4(5) 2_645 . . . ?
Cd1 O3 C6 O4 -3.0(7) 2_645 . . . ?
Cd1 O3 C6 C5 175.4(5) 2_645 . . . ?
C4 C5 C6 O4 173.4(6) . . . . ?
C7 C5 C6 O4 -4.7(9) . . . . ?
C4 C5 C6 O3 -5.0(9) . . . . ?
C7 C5 C6 O3 176.9(6) . . . . ?
C4 C5 C7 C8 -2.5(9) . . . . ?
C6 C5 C7 C8 175.6(5) . . . . ?
C3 C2 C8 C7 -0.3(9) . . . . ?
C1 C2 C8 C7 178.8(5) . . . . ?
C3 C2 C8 O5 179.4(5) . . . . ?
C1 C2 C8 O5 -1.5(8) . . . . ?
C5 C7 C8 C2 2.6(9) . . . . ?
C5 C7 C8 O5 -177.0(5) . . . . ?
C9 O5 C8 C2 161.9(5) . . . . ?
C9 O5 C8 C7 -18.4(8) . . . . ?
C8 O5 C9 C10 117.5(6) . . . . ?
C8 O5 C9 C14 -66.6(8) . . . . ?
C14 C9 C10 C11 -2.1(10) . . . . ?
O5 C9 C10 C11 174.0(6) . . . . ?
C9 C10 C11 C12 1.6(11) . . . . ?
C10 C11 C12 C13 -0.3(12) . . . . ?
C11 C12 C13 C14 -0.6(11) . . . . ?
C12 C13 C14 C9 0.1(10) . . . . ?
C12 C13 C14 C15 -177.1(6) . . . . ?
C10 C9 C14 C13 1.3(9) . . . . ?
O5 C9 C14 C13 -174.4(6) . . . . ?
C10 C9 C14 C15 178.3(6) . . . . ?
O5 C9 C14 C15 2.6(9) . . . . ?
Cd2 O7 C15 O6 -7.6(8) 3_655 . . . ?
Cd2 O7 C15 C14 174.2(5) 3_655 . . . ?
C13 C14 C15 O6 -25.0(9) . . . . ?
C9 C14 C15 O6 158.0(6) . . . . ?
C13 C14 C15 O7 153.2(6) . . . . ?
C9 C14 C15 O7 -23.7(9) . . . . ?
C20 N1 C16 C17 -1.5(11) . . . . ?
Cd1 N1 C16 C17 168.8(6) . . . . ?
N1 C16 C17 C18 1.3(13) . . . . ?
C16 C17 C18 C19 -0.4(13) . . . . ?
C17 C18 C19 C20 -0.3(12) . . . . ?
C17 C18 C19 C21 178.7(8) . . . . ?
C16 N1 C20 C19 0.7(9) . . . . ?
Cd1 N1 C20 C19 -170.3(5) . . . . ?
C16 N1 C20 C24 178.8(6) . . . . ?
Cd1 N1 C20 C24 7.8(7) . . . . ?
C18 C19 C20 N1 0.2(10) . . . . ?
C21 C19 C20 N1 -178.9(6) . . . . ?
C18 C19 C20 C24 -177.9(6) . . . . ?
C21 C19 C20 C24 2.9(10) . . . . ?
C18 C19 C21 C22 -178.5(8) . . . . ?
C20 C19 C21 C22 0.5(12) . . . . ?
C19 C21 C22 C23 -3.6(13) . . . . ?
C21 C22 C23 C25 -177.1(8) . . . . ?
C21 C22 C23 C24 3.1(12) . . . . ?
C27 N2 C24 C23 -3.3(10) . . . . ?
Cd1 N2 C24 C23 175.3(5) . . . . ?
C27 N2 C24 C20 178.4(6) . . . . ?
Cd1 N2 C24 C20 -2.9(7) . . . . ?
C25 C23 C24 N2 2.3(11) . . . . ?
C22 C23 C24 N2 -177.8(6) . . . . ?
C25 C23 C24 C20 -179.4(7) . . . . ?
C22 C23 C24 C20 0.4(11) . . . . ?
N1 C20 C24 N2 -3.3(9) . . . . ?
C19 C20 C24 N2 174.9(6) . . . . ?
N1 C20 C24 C23 178.4(6) . . . . ?
C19 C20 C24 C23 -3.4(10) . . . . ?
C24 C23 C25 C26 -0.1(13) . . . . ?
C22 C23 C25 C26 -180.0(9) . . . . ?
C23 C25 C26 C27 -1.1(15) . . . . ?
C24 N2 C27 C26 2.1(12) . . . . ?
Cd1 N2 C27 C26 -176.4(7) . . . . ?
C25 C26 C27 N2 0.1(15) . . . . ?
C32 N3 C28 C29 -0.2(11) . . . . ?
Cd2 N3 C28 C29 174.6(5) . . . . ?
N3 C28 C29 C30 -0.7(12) . . . . ?
C28 C29 C30 C31 1.4(12) . . . . ?
C29 C30 C31 C32 -1.3(11) . . . . ?
C29 C30 C31 C33 179.8(7) . . . . ?
C28 N3 C32 C31 0.3(10) . . . . ?
Cd2 N3 C32 C31 -174.8(5) . . . . ?
C28 N3 C32 C36 -179.8(6) . . . . ?
Cd2 N3 C32 C36 5.1(7) . . . . ?
C30 C31 C32 N3 0.4(10) . . . . ?
C33 C31 C32 N3 179.3(6) . . . . ?
C30 C31 C32 C36 -179.5(6) . . . . ?
C33 C31 C32 C36 -0.6(10) . . . . ?
C30 C31 C33 C34 -178.9(7) . . . . ?
C32 C31 C33 C34 2.3(11) . . . . ?
C31 C33 C34 C35 -1.6(12) . . . . ?
C33 C34 C35 C37 -176.5(7) . . . . ?
C33 C34 C35 C36 -0.7(12) . . . . ?
C39 N4 C36 C35 0.7(9) . . . . ?
Cd2 N4 C36 C35 178.0(5) . . . . ?
C39 N4 C36 C32 -177.8(6) . . . . ?
Cd2 N4 C36 C32 -0.5(7) . . . . ?
C34 C35 C36 N4 -176.1(6) . . . . ?
C37 C35 C36 N4 0.1(10) . . . . ?
C34 C35 C36 C32 2.4(10) . . . . ?
C37 C35 C36 C32 178.5(6) . . . . ?
N3 C32 C36 N4 -3.1(9) . . . . ?
C31 C32 C36 N4 176.8(6) . . . . ?
N3 C32 C36 C35 178.4(6) . . . . ?
C31 C32 C36 C35 -1.7(9) . . . . ?
C34 C35 C37 C38 175.7(7) . . . . ?
C36 C35 C37 C38 -0.2(11) . . . . ?
C35 C37 C38 C39 -0.4(12) . . . . ?
C36 N4 C39 C38 -1.3(10) . . . . ?
Cd2 N4 C39 C38 -178.3(5) . . . . ?
C37 C38 C39 N4 1.2(12) . . . . ?

_refine_diff_density_max         0.769
_refine_diff_density_min         -0.573
_refine_diff_density_rms         0.120


# start Validation Reply Form
_vrf_PLAT910_I                   
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min) 14 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_269-11Cd
_database_code_depnum_ccdc_archive 'CCDC 1509061'
_audit_update_record             
;
2017-03-26 deposited with the CCDC.
2017-04-10 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 Cd3 N2 O14'
_chemical_formula_weight         1093.81

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      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                   14.9155(11)
_cell_length_b                   20.1133(9)
_cell_length_c                   14.3821(7)
_cell_angle_alpha                90
_cell_angle_beta                 105.870(6)
_cell_angle_gamma                90
_cell_volume                     4150.2(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7773
_cell_measurement_theta_min      3.500
_cell_measurement_theta_max      25.049

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.751
_exptl_crystal_F_000             2136
_exptl_transmission_factor_min   0.728
_exptl_transmission_factor_max   0.751
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    1.591
_shelx_estimated_absorpt_T_min   0.711
_shelx_estimated_absorpt_T_max   0.763
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.711
_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            7773
_diffrn_reflns_av_unetI/netI     0.0567
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.500
_diffrn_reflns_theta_max         25.049
_diffrn_reflns_theta_full        25.049
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             3658
_reflns_number_gt                2977
_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)+(0.0169P)²+0.7753P] 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         3658
_refine_ls_number_parameters     267
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0319
_refine_ls_wR_factor_ref         0.0613
_refine_ls_wR_factor_gt          0.0563
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_restrained_S_all      0.990
_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
Cd1 Cd 0.77529(2) 0.21558(2) 0.62518(2) 0.02294(9) Uani 1 1 d . . . . .
Cd2 Cd 1.0000 0.14345(2) 0.7500 0.02221(11) Uani 1 2 d S T P . .
O1 O 0.84550(17) 0.26657(14) 0.50769(17) 0.0321(7) Uani 1 1 d . . . . .
O2 O 0.94663(17) 0.22831(13) 0.63607(17) 0.0290(7) Uani 1 1 d . . . . .
O3 O 1.04661(17) 0.13800(12) 0.54326(17) 0.0245(6) Uani 1 1 d . . . . .
O4 O 1.14100(17) 0.17142(13) 0.72599(17) 0.0267(6) Uani 1 1 d . . . . .
O5 O 1.28873(19) 0.14253(14) 0.77091(18) 0.0360(7) Uani 1 1 d . . . . .
O6 O 1.07453(18) -0.06499(13) 0.35085(17) 0.0305(7) Uani 1 1 d . . . . .
O7 O 1.1974(2) -0.11933(14) 0.44450(18) 0.0366(7) Uani 1 1 d . . . . .
N1 N 0.7556(3) 0.30971(18) 0.7072(2) 0.0363(9) Uani 1 1 d . . . . .
C1 C 0.9266(3) 0.24676(19) 0.5496(3) 0.0229(9) Uani 1 1 d . . . . .
C2 C 0.9990(2) 0.2478(2) 0.4951(3) 0.0244(9) Uani 1 1 d . . . . .
C3 C 1.0041(3) 0.3033(2) 0.4391(3) 0.0478(13) Uani 1 1 d . . . . .
H3 H 0.9608 0.3374 0.4333 0.057 Uiso 1 1 calc R U . . .
C4 C 1.0733(4) 0.3082(3) 0.3919(4) 0.0616(15) Uani 1 1 d . . . . .
H4 H 1.0768 0.3457 0.3552 0.074 Uiso 1 1 calc R U . . .
C5 C 1.1359(3) 0.2582(3) 0.3995(4) 0.0555(14) Uani 1 1 d . . . . .
H5 H 1.1831 0.2623 0.3689 0.067 Uiso 1 1 calc R U . . .
C6 C 1.1311(3) 0.2017(2) 0.4513(3) 0.0405(12) Uani 1 1 d . . . . .
H6 H 1.1739 0.1675 0.4549 0.049 Uiso 1 1 calc R U . . .
C7 C 1.0619(2) 0.19616(19) 0.4983(2) 0.0231(9) Uani 1 1 d . . . . .
C8 C 1.1129(2) 0.08764(18) 0.5549(2) 0.0202(8) Uani 1 1 d . . . . .
C9 C 1.1916(3) 0.08653(19) 0.6348(2) 0.0231(9) Uani 1 1 d . . . . .
C10 C 1.2089(3) 0.1369(2) 0.7150(3) 0.0261(9) Uani 1 1 d . . . . .
C11 C 1.2540(3) 0.0343(2) 0.6420(3) 0.0329(10) Uani 1 1 d . . . . .
H11 H 1.3079 0.0336 0.6932 0.039 Uiso 1 1 calc R U . . .
C12 C 1.2381(3) -0.0164(2) 0.5752(3) 0.0333(10) Uani 1 1 d . . . . .
H12 H 1.2802 -0.0514 0.5823 0.040 Uiso 1 1 calc R U . . .
C13 C 1.1591(3) -0.01512(19) 0.4971(2) 0.0226(9) Uani 1 1 d . . . . .
C14 C 1.1418(3) -0.0716(2) 0.4239(3) 0.0270(9) Uani 1 1 d . . . . .
C15 C 1.0976(2) 0.03764(18) 0.4873(2) 0.0224(9) Uani 1 1 d . . . . .
H15 H 1.0453 0.0393 0.4344 0.027 Uiso 1 1 calc R U . . .
C20 C 0.6777(3) 0.3450(2) 0.6904(4) 0.0540(14) Uani 1 1 d . . . . .
H20 H 0.6275 0.3328 0.6389 0.065 Uiso 1 1 calc R U . . .
C19 C 0.6679(4) 0.3985(3) 0.7450(4) 0.0710(17) Uani 1 1 d . . . . .
H19 H 0.6118 0.4216 0.7311 0.085 Uiso 1 1 calc R U . . .
C18 C 0.7398(5) 0.4176(3) 0.8194(4) 0.0696(18) Uani 1 1 d . . . . .
H18 H 0.7349 0.4547 0.8563 0.084 Uiso 1 1 calc R U . . .
C17 C 0.8182(5) 0.3821(3) 0.8387(4) 0.0802(19) Uani 1 1 d . . . . .
H17 H 0.8681 0.3936 0.8909 0.096 Uiso 1 1 calc R U . . .
C16 C 0.8257(4) 0.3285(3) 0.7818(4) 0.0630(15) Uani 1 1 d . . . . .
H16 H 0.8813 0.3047 0.7958 0.076 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 2.267(3) 5_756 ?
Cd1 O1 2.268(3) 7_656 ?
Cd1 N1 2.292(3) . ?
Cd1 O4 2.338(2) 2_756 ?
Cd1 O1 2.444(2) . ?
Cd1 O5 2.467(2) 2_756 ?
Cd1 O2 2.530(3) . ?
Cd1 C10 2.747(4) 2_756 ?
Cd2 O6 2.224(3) 5_756 ?
Cd2 O6 2.224(3) 6_556 ?
Cd2 O4 2.293(2) . ?
Cd2 O4 2.293(2) 2_756 ?
Cd2 O2 2.349(3) 2_756 ?
Cd2 O2 2.349(3) . ?
O1 C1 1.259(4) . ?
O1 Cd1 2.268(3) 7_656 ?
O2 C1 1.254(4) . ?
O3 C7 1.385(4) . ?
O3 C8 1.394(4) . ?
O4 C10 1.273(4) . ?
O4 Cd1 2.338(2) 2_756 ?
O5 C10 1.247(4) . ?
O5 Cd1 2.467(2) 2_756 ?
O6 C14 1.246(4) . ?
O6 Cd2 2.224(3) 5_756 ?
O7 C14 1.250(4) . ?
O7 Cd1 2.267(3) 5_756 ?
N1 C20 1.326(5) . ?
N1 C16 1.332(6) . ?
C1 C2 1.498(5) . ?
C2 C7 1.391(5) . ?
C2 C3 1.392(5) . ?
C3 C4 1.384(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.357(6) . ?
C4 H4 0.9300 . ?
C5 C6 1.371(6) . ?
C5 H5 0.9300 . ?
C6 C7 1.385(5) . ?
C6 H6 0.9300 . ?
C8 C15 1.373(5) . ?
C8 C9 1.401(5) . ?
C9 C11 1.388(5) . ?
C9 C10 1.503(5) . ?
C10 Cd1 2.748(4) 2_756 ?
C11 C12 1.377(5) . ?
C11 H11 0.9300 . ?
C12 C13 1.388(5) . ?
C12 H12 0.9300 . ?
C13 C15 1.384(5) . ?
C13 C14 1.522(5) . ?
C15 H15 0.9300 . ?
C20 C19 1.363(7) . ?
C20 H20 0.9300 . ?
C19 C18 1.348(7) . ?
C19 H19 0.9300 . ?
C18 C17 1.333(7) . ?
C18 H18 0.9300 . ?
C17 C16 1.377(7) . ?
C17 H17 0.9300 . ?
C16 H16 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 O1 87.71(10) 5_756 7_656 ?
O7 Cd1 N1 175.33(11) 5_756 . ?
O1 Cd1 N1 96.81(11) 7_656 . ?
O7 Cd1 O4 87.98(9) 5_756 2_756 ?
O1 Cd1 O4 159.02(9) 7_656 2_756 ?
N1 Cd1 O4 87.38(11) . 2_756 ?
O7 Cd1 O1 83.69(9) 5_756 . ?
O1 Cd1 O1 75.10(10) 7_656 . ?
N1 Cd1 O1 98.56(11) . . ?
O4 Cd1 O1 124.74(8) 2_756 . ?
O7 Cd1 O5 84.56(10) 5_756 2_756 ?
O1 Cd1 O5 104.77(9) 7_656 2_756 ?
N1 Cd1 O5 93.14(11) . 2_756 ?
O4 Cd1 O5 54.36(9) 2_756 2_756 ?
O1 Cd1 O5 168.24(9) . 2_756 ?
O7 Cd1 O2 79.25(9) 5_756 . ?
O1 Cd1 O2 126.32(8) 7_656 . ?
N1 Cd1 O2 98.87(11) . . ?
O4 Cd1 O2 72.80(8) 2_756 . ?
O1 Cd1 O2 51.96(8) . . ?
O5 Cd1 O2 125.07(8) 2_756 . ?
O7 Cd1 C10 83.88(10) 5_756 2_756 ?
O1 Cd1 C10 131.53(11) 7_656 2_756 ?
N1 Cd1 C10 92.22(11) . 2_756 ?
O4 Cd1 C10 27.50(10) 2_756 2_756 ?
O1 Cd1 C10 149.92(10) . 2_756 ?
O5 Cd1 C10 26.98(10) 2_756 2_756 ?
O2 Cd1 C10 98.76(10) . 2_756 ?
O6 Cd2 O6 89.62(14) 5_756 6_556 ?
O6 Cd2 O4 113.04(9) 5_756 . ?
O6 Cd2 O4 87.53(9) 6_556 . ?
O6 Cd2 O4 87.52(9) 5_756 2_756 ?
O6 Cd2 O4 113.04(9) 6_556 2_756 ?
O4 Cd2 O4 151.59(13) . 2_756 ?
O6 Cd2 O2 169.70(9) 5_756 2_756 ?
O6 Cd2 O2 92.70(9) 6_556 2_756 ?
O4 Cd2 O2 77.11(8) . 2_756 ?
O4 Cd2 O2 82.33(9) 2_756 2_756 ?
O6 Cd2 O2 92.70(9) 5_756 . ?
O6 Cd2 O2 169.70(9) 6_556 . ?
O4 Cd2 O2 82.33(9) . . ?
O4 Cd2 O2 77.11(8) 2_756 . ?
O2 Cd2 O2 86.80(13) 2_756 . ?
C1 O1 Cd1 153.0(2) . 7_656 ?
C1 O1 Cd1 94.2(2) . . ?
Cd1 O1 Cd1 104.90(10) 7_656 . ?
C1 O2 Cd2 148.3(3) . . ?
C1 O2 Cd1 90.3(2) . . ?
Cd2 O2 Cd1 96.52(9) . . ?
C7 O3 C8 117.9(3) . . ?
C10 O4 Cd2 132.8(2) . . ?
C10 O4 Cd1 94.4(2) . 2_756 ?
Cd2 O4 Cd1 103.74(9) . 2_756 ?
C10 O5 Cd1 89.2(2) . 2_756 ?
C14 O6 Cd2 128.2(3) . 5_756 ?
C14 O7 Cd1 137.6(2) . 5_756 ?
C20 N1 C16 116.8(4) . . ?
C20 N1 Cd1 125.3(3) . . ?
C16 N1 Cd1 117.7(3) . . ?
O2 C1 O1 120.4(3) . . ?
O2 C1 C2 120.8(3) . . ?
O1 C1 C2 118.7(3) . . ?
C7 C2 C3 118.3(3) . . ?
C7 C2 C1 123.3(3) . . ?
C3 C2 C1 118.4(4) . . ?
C4 C3 C2 120.5(4) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C5 C4 C3 119.8(4) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C4 C5 C6 121.3(4) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 H5 119.3 . . ?
C5 C6 C7 119.3(4) . . ?
C5 C6 H6 120.4 . . ?
C7 C6 H6 120.4 . . ?
C6 C7 O3 122.4(4) . . ?
C6 C7 C2 120.6(4) . . ?
O3 C7 C2 116.8(3) . . ?
C15 C8 O3 118.2(3) . . ?
C15 C8 C9 120.6(3) . . ?
O3 C8 C9 121.2(3) . . ?
C11 C9 C8 117.8(3) . . ?
C11 C9 C10 118.8(3) . . ?
C8 C9 C10 123.2(3) . . ?
O5 C10 O4 121.5(4) . . ?
O5 C10 C9 119.3(4) . . ?
O4 C10 C9 119.2(3) . . ?
O5 C10 Cd1 63.9(2) . 2_756 ?
O4 C10 Cd1 58.05(18) . 2_756 ?
C9 C10 Cd1 170.9(3) . 2_756 ?
C12 C11 C9 121.7(4) . . ?
C12 C11 H11 119.2 . . ?
C9 C11 H11 119.2 . . ?
C11 C12 C13 119.8(4) . . ?
C11 C12 H12 120.1 . . ?
C13 C12 H12 120.1 . . ?
C15 C13 C12 119.3(4) . . ?
C15 C13 C14 121.3(3) . . ?
C12 C13 C14 119.4(4) . . ?
O6 C14 O7 127.7(4) . . ?
O6 C14 C13 116.7(4) . . ?
O7 C14 C13 115.7(3) . . ?
C8 C15 C13 120.8(3) . . ?
C8 C15 H15 119.6 . . ?
C13 C15 H15 119.6 . . ?
N1 C20 C19 123.0(5) . . ?
N1 C20 H20 118.5 . . ?
C19 C20 H20 118.5 . . ?
C18 C19 C20 119.7(6) . . ?
C18 C19 H19 120.2 . . ?
C20 C19 H19 120.2 . . ?
C17 C18 C19 118.3(5) . . ?
C17 C18 H18 120.8 . . ?
C19 C18 H18 120.8 . . ?
C18 C17 C16 120.4(6) . . ?
C18 C17 H17 119.8 . . ?
C16 C17 H17 119.8 . . ?
N1 C16 C17 121.8(5) . . ?
N1 C16 H16 119.1 . . ?
C17 C16 H16 119.1 . . ?

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 0.000 0.500 -0.013 313 48 ' '
2 0.500 0.000 0.007 313 48 ' '
3 0.000 0.177 0.250 7 1 ' '
4 0.500 0.677 0.250 7 1 ' '
5 0.000 0.823 0.750 7 1 ' '
6 0.500 0.323 0.750 7 1 ' '
_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
Cd2 O2 C1 O1 120.7(4) . . . . ?
Cd1 O2 C1 O1 17.7(4) . . . . ?
Cd2 O2 C1 C2 -61.3(6) . . . . ?
Cd1 O2 C1 C2 -164.3(3) . . . . ?
Cd1 O1 C1 O2 -153.8(4) 7_656 . . . ?
Cd1 O1 C1 O2 -18.4(4) . . . . ?
Cd1 O1 C1 C2 28.2(8) 7_656 . . . ?
Cd1 O1 C1 C2 163.6(3) . . . . ?
O2 C1 C2 C7 44.6(6) . . . . ?
O1 C1 C2 C7 -137.3(4) . . . . ?
O2 C1 C2 C3 -134.8(4) . . . . ?
O1 C1 C2 C3 43.2(6) . . . . ?
C7 C2 C3 C4 -3.3(7) . . . . ?
C1 C2 C3 C4 176.2(4) . . . . ?
C2 C3 C4 C5 0.7(8) . . . . ?
C3 C4 C5 C6 1.5(9) . . . . ?
C4 C5 C6 C7 -1.2(8) . . . . ?
C5 C6 C7 O3 173.0(4) . . . . ?
C5 C6 C7 C2 -1.5(6) . . . . ?
C8 O3 C7 C6 10.8(5) . . . . ?
C8 O3 C7 C2 -174.6(3) . . . . ?
C3 C2 C7 C6 3.6(6) . . . . ?
C1 C2 C7 C6 -175.8(4) . . . . ?
C3 C2 C7 O3 -171.1(4) . . . . ?
C1 C2 C7 O3 9.4(5) . . . . ?
C7 O3 C8 C15 -96.2(4) . . . . ?
C7 O3 C8 C9 86.0(4) . . . . ?
C15 C8 C9 C11 1.4(5) . . . . ?
O3 C8 C9 C11 179.2(3) . . . . ?
C15 C8 C9 C10 -175.4(3) . . . . ?
O3 C8 C9 C10 2.4(5) . . . . ?
Cd1 O5 C10 O4 7.4(4) 2_756 . . . ?
Cd1 O5 C10 C9 -170.3(3) 2_756 . . . ?
Cd2 O4 C10 O5 -121.2(4) . . . . ?
Cd1 O4 C10 O5 -7.8(4) 2_756 . . . ?
Cd2 O4 C10 C9 56.6(5) . . . . ?
Cd1 O4 C10 C9 169.9(3) 2_756 . . . ?
Cd2 O4 C10 Cd1 -113.3(3) . . . 2_756 ?
C11 C9 C10 O5 20.0(5) . . . . ?
C8 C9 C10 O5 -163.2(4) . . . . ?
C11 C9 C10 O4 -157.8(4) . . . . ?
C8 C9 C10 O4 19.0(5) . . . . ?
C8 C9 C11 C12 -2.5(6) . . . . ?
C10 C9 C11 C12 174.5(4) . . . . ?
C9 C11 C12 C13 1.6(6) . . . . ?
C11 C12 C13 C15 0.4(6) . . . . ?
C11 C12 C13 C14 -179.7(3) . . . . ?
Cd2 O6 C14 O7 19.4(6) 5_756 . . . ?
Cd2 O6 C14 C13 -160.7(2) 5_756 . . . ?
Cd1 O7 C14 O6 4.0(7) 5_756 . . . ?
Cd1 O7 C14 C13 -175.8(2) 5_756 . . . ?
C15 C13 C14 O6 6.2(5) . . . . ?
C12 C13 C14 O6 -173.8(4) . . . . ?
C15 C13 C14 O7 -173.9(3) . . . . ?
C12 C13 C14 O7 6.1(5) . . . . ?
O3 C8 C15 C13 -177.4(3) . . . . ?
C9 C8 C15 C13 0.5(5) . . . . ?
C12 C13 C15 C8 -1.4(5) . . . . ?
C14 C13 C15 C8 178.6(3) . . . . ?
C16 N1 C20 C19 0.4(7) . . . . ?
Cd1 N1 C20 C19 176.0(4) . . . . ?
N1 C20 C19 C18 0.7(8) . . . . ?
C20 C19 C18 C17 -1.9(9) . . . . ?
C19 C18 C17 C16 2.0(9) . . . . ?
C20 N1 C16 C17 -0.2(8) . . . . ?
Cd1 N1 C16 C17 -176.2(4) . . . . ?
C18 C17 C16 N1 -1.0(9) . . . . ?

_refine_diff_density_max         0.496
_refine_diff_density_min         -0.432
_refine_diff_density_rms         0.097


# 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.
;
_vrf_PLAT990_I                   
;
PROBLEM: Deprecated RES file style based 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_286-11Cd
_database_code_depnum_ccdc_archive 'CCDC 1509371'
_audit_update_record             
;
2017-03-26 deposited with the CCDC.
2017-04-10 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            'C42 H26 Cd3 N8 O14'
_chemical_formula_weight         1203.91

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           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

_cell_length_a                   11.6055(5)
_cell_length_b                   14.9903(4)
_cell_length_c                   13.1804(9)
_cell_angle_alpha                90
_cell_angle_beta                 114.102(7)
_cell_angle_gamma                90
_cell_volume                     2093.1(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7626
_cell_measurement_theta_min      3.327
_cell_measurement_theta_max      25.046

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.910
_exptl_crystal_F_000             1180
_exptl_transmission_factor_min   0.657
_exptl_transmission_factor_max   0.683
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.240
_exptl_absorpt_coefficient_mu    1.591
_shelx_estimated_absorpt_T_min   0.673
_shelx_estimated_absorpt_T_max   0.701
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.673
_exptl_absorpt_correction_T_max  0.701
_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            7626
_diffrn_reflns_av_unetI/netI     0.0635
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         3.327
_diffrn_reflns_theta_max         25.046
_diffrn_reflns_theta_full        25.046
_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             3684
_reflns_number_gt                2827
_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)+(0.0239P)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         3684
_refine_ls_number_parameters     304
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0358
_refine_ls_wR_factor_ref         0.0776
_refine_ls_wR_factor_gt          0.0662
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.025
_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
Cd1 Cd -0.14478(3) 0.13064(2) 0.13100(3) 0.02664(12) Uani 1 1 d . . . . .
Cd2 Cd 0.0000 0.0000 0.0000 0.02392(14) Uani 1 2 d S . P . .
O1 O 0.0351(3) 0.1965(2) 0.1554(3) 0.0474(11) Uani 1 1 d . . . . .
O2 O 0.1208(3) 0.12456(19) 0.0529(3) 0.0314(8) Uani 1 1 d . . . . .
O3 O 0.5252(3) 0.50465(19) 0.3353(3) 0.0303(8) Uani 1 1 d . . . . .
O4 O 0.5708(3) 0.4696(2) 0.1948(3) 0.0392(9) Uani 1 1 d . . . . .
O5 O 0.2614(3) 0.49268(18) 0.2380(3) 0.0251(8) Uani 1 1 d . . . . .
O6 O 0.1833(3) 0.4590(2) 0.5219(3) 0.0421(10) Uani 1 1 d . . . . .
O7 O 0.3120(3) 0.42236(19) 0.4426(3) 0.0255(8) Uani 1 1 d . . . . .
N1 N -0.1727(4) 0.2153(3) 0.2651(3) 0.0331(10) Uani 1 1 d . . . . .
N2 N -0.2460(4) 0.2583(3) 0.0402(4) 0.0422(11) Uani 1 1 d . . . . .
N3 N -0.3262(4) 0.3872(3) 0.0553(4) 0.0496(13) Uani 1 1 d . . . . .
H1 H -0.3492 0.4318 0.0837 0.060 Uiso 1 1 calc R U . . .
N4 N -0.2225(4) 0.3470(3) 0.3069(4) 0.0451(12) Uani 1 1 d . . . . .
H2 H -0.2504 0.4009 0.2993 0.054 Uiso 1 1 calc R U . . .
C1 C 0.1166(4) 0.1862(3) 0.1167(4) 0.0279(12) Uani 1 1 d . . . . .
C2 C 0.2192(4) 0.2566(3) 0.1509(4) 0.0249(11) Uani 1 1 d . . . . .
C3 C 0.3388(4) 0.2383(3) 0.1576(4) 0.0271(11) Uani 1 1 d . . . . .
H3 H 0.3583 0.1813 0.1417 0.032 Uiso 1 1 calc R U . . .
C4 C 0.4293(4) 0.3041(3) 0.1878(4) 0.0297(12) Uani 1 1 d . . . . .
H4 H 0.5087 0.2914 0.1899 0.036 Uiso 1 1 calc R U . . .
C5 C 0.4040(4) 0.3899(3) 0.2153(4) 0.0216(11) Uani 1 1 d . . . . .
C6 C 0.5071(4) 0.4589(3) 0.2499(4) 0.0242(11) Uani 1 1 d . . . . .
C7 C 0.2836(4) 0.4069(3) 0.2117(4) 0.0229(11) Uani 1 1 d . . . . .
C8 C 0.1925(4) 0.3411(3) 0.1784(4) 0.0242(11) Uani 1 1 d . . . . .
H8 H 0.1123 0.3536 0.1743 0.029 Uiso 1 1 calc R U . . .
C9 C 0.1432(4) 0.5110(3) 0.2383(4) 0.0246(11) Uani 1 1 d . . . . .
C10 C 0.0567(4) 0.5508(3) 0.1444(4) 0.0371(13) Uani 1 1 d . . . . .
H10 H 0.0767 0.5622 0.0841 0.045 Uiso 1 1 calc R U . . .
C11 C -0.0610(5) 0.5738(4) 0.1403(5) 0.0470(15) Uani 1 1 d . . . . .
H11 H -0.1210 0.5991 0.0759 0.056 Uiso 1 1 calc R U . . .
C12 C -0.0896(5) 0.5597(4) 0.2301(5) 0.0437(15) Uani 1 1 d . . . . .
H12 H -0.1683 0.5759 0.2269 0.052 Uiso 1 1 calc R U . . .
C13 C -0.0019(4) 0.5215(3) 0.3247(5) 0.0322(12) Uani 1 1 d . . . . .
H13 H -0.0220 0.5120 0.3853 0.039 Uiso 1 1 calc R U . . .
C14 C 0.1182(4) 0.4966(3) 0.3316(4) 0.0241(11) Uani 1 1 d . . . . .
C15 C 0.2100(4) 0.4583(3) 0.4384(4) 0.0274(12) Uani 1 1 d . . . . .
C16 C -0.1416(6) 0.2202(4) 0.3765(5) 0.0576(17) Uani 1 1 d . . . . .
H16 H -0.1055 0.1740 0.4266 0.069 Uiso 1 1 calc R U . . .
C17 C -0.1704(7) 0.3012(5) 0.4039(5) 0.071(2) Uani 1 1 d . . . . .
H17 H -0.1574 0.3214 0.4745 0.085 Uiso 1 1 calc R U . . .
C18 C -0.2228(4) 0.2939(3) 0.2253(4) 0.0283(12) Uani 1 1 d . . . . .
C19 C -0.2665(4) 0.3143(3) 0.1085(4) 0.0309(12) Uani 1 1 d . . . . .
C20 C -0.3439(6) 0.3777(4) -0.0530(6) 0.067(2) Uani 1 1 d . . . . .
H20 H -0.3830 0.4182 -0.1103 0.081 Uiso 1 1 calc R U . . .
C21 C -0.2942(6) 0.2989(4) -0.0606(5) 0.0613(19) Uani 1 1 d . . . . .
H21 H -0.2929 0.2754 -0.1254 0.074 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 2.211(3) . ?
Cd1 O3 2.278(3) 2_545 ?
Cd1 N1 2.304(4) . ?
Cd1 N2 2.308(4) . ?
Cd1 O6 2.348(3) 4_565 ?
Cd1 O7 2.455(3) 4_565 ?
Cd1 C15 2.752(5) 4_565 ?
Cd2 O2 2.267(3) . ?
Cd2 O2 2.267(3) 3 ?
Cd2 O3 2.307(3) 4_565 ?
Cd2 O3 2.307(3) 2_545 ?
Cd2 O7 2.311(3) 2_545 ?
Cd2 O7 2.311(3) 4_565 ?
Cd2 Cd1 3.4655(4) 3 ?
O1 C1 1.254(5) . ?
O2 C1 1.263(5) . ?
O3 C6 1.260(5) . ?
O3 Cd1 2.278(3) 2 ?
O3 Cd2 2.307(3) 2 ?
O4 C6 1.240(5) . ?
O5 C7 1.383(5) . ?
O5 C9 1.401(5) . ?
O6 C15 1.260(6) . ?
O6 Cd1 2.348(3) 4_666 ?
O7 C15 1.281(5) . ?
O7 Cd2 2.311(3) 2 ?
O7 Cd1 2.455(3) 4_666 ?
N1 C18 1.323(6) . ?
N1 C16 1.363(7) . ?
N2 C19 1.321(6) . ?
N2 C21 1.357(7) . ?
N3 C19 1.331(6) . ?
N3 C20 1.363(7) . ?
N3 H1 0.8600 . ?
N4 C18 1.337(6) . ?
N4 C17 1.357(7) . ?
N4 H2 0.8600 . ?
C1 C2 1.516(6) . ?
C2 C3 1.382(6) . ?
C2 C8 1.387(6) . ?
C3 C4 1.376(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.399(6) . ?
C4 H4 0.9300 . ?
C5 C7 1.402(6) . ?
C5 C6 1.505(6) . ?
C7 C8 1.379(6) . ?
C8 H8 0.9300 . ?
C9 C10 1.371(6) . ?
C9 C14 1.391(6) . ?
C10 C11 1.389(6) . ?
C10 H10 0.9300 . ?
C11 C12 1.370(7) . ?
C11 H11 0.9300 . ?
C12 C13 1.372(7) . ?
C12 H12 0.9300 . ?
C13 C14 1.409(6) . ?
C13 H13 0.9300 . ?
C14 C15 1.490(7) . ?
C15 Cd1 2.752(5) 4_666 ?
C16 C17 1.347(8) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
C18 C19 1.444(7) . ?
C20 C21 1.336(8) . ?
C20 H20 0.9300 . ?
C21 H21 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 O3 82.98(12) . 2_545 ?
O1 Cd1 N1 93.59(14) . . ?
O3 Cd1 N1 124.94(13) 2_545 . ?
O1 Cd1 N2 87.44(15) . . ?
O3 Cd1 N2 158.34(13) 2_545 . ?
N1 Cd1 N2 74.89(15) . . ?
O1 Cd1 O6 149.39(13) . 4_565 ?
O3 Cd1 O6 86.73(12) 2_545 4_565 ?
N1 Cd1 O6 115.75(13) . 4_565 ?
N2 Cd1 O6 91.83(14) . 4_565 ?
O1 Cd1 O7 94.74(12) . 4_565 ?
O3 Cd1 O7 77.63(11) 2_545 4_565 ?
N1 Cd1 O7 156.80(12) . 4_565 ?
N2 Cd1 O7 83.89(13) . 4_565 ?
O6 Cd1 O7 54.82(11) 4_565 4_565 ?
O1 Cd1 C15 122.48(14) . 4_565 ?
O3 Cd1 C15 82.70(12) 2_545 4_565 ?
N1 Cd1 C15 138.57(14) . 4_565 ?
N2 Cd1 C15 86.19(14) . 4_565 ?
O6 Cd1 C15 27.15(12) 4_565 4_565 ?
O7 Cd1 C15 27.74(11) 4_565 4_565 ?
O2 Cd2 O2 180.0 . 3 ?
O2 Cd2 O3 90.83(11) . 4_565 ?
O2 Cd2 O3 89.17(11) 3 4_565 ?
O2 Cd2 O3 89.17(11) . 2_545 ?
O2 Cd2 O3 90.83(11) 3 2_545 ?
O3 Cd2 O3 180.00(14) 4_565 2_545 ?
O2 Cd2 O7 86.08(10) . 2_545 ?
O2 Cd2 O7 93.92(10) 3 2_545 ?
O3 Cd2 O7 80.05(11) 4_565 2_545 ?
O3 Cd2 O7 99.95(11) 2_545 2_545 ?
O2 Cd2 O7 93.92(10) . 4_565 ?
O2 Cd2 O7 86.08(10) 3 4_565 ?
O3 Cd2 O7 99.95(11) 4_565 4_565 ?
O3 Cd2 O7 80.05(11) 2_545 4_565 ?
O7 Cd2 O7 180.0(2) 2_545 4_565 ?
O2 Cd2 Cd1 104.72(8) . 3 ?
O2 Cd2 Cd1 75.28(8) 3 3 ?
O3 Cd2 Cd1 40.58(7) 4_565 3 ?
O3 Cd2 Cd1 139.42(7) 2_545 3 ?
O7 Cd2 Cd1 45.02(8) 2_545 3 ?
O7 Cd2 Cd1 134.98(8) 4_565 3 ?
C1 O1 Cd1 135.2(3) . . ?
C1 O2 Cd2 128.3(3) . . ?
C6 O3 Cd1 119.4(3) . 2 ?
C6 O3 Cd2 141.7(3) . 2 ?
Cd1 O3 Cd2 98.20(12) 2 2 ?
C7 O5 C9 117.8(3) . . ?
C15 O6 Cd1 94.6(3) . 4_666 ?
C15 O7 Cd2 122.3(3) . 2 ?
C15 O7 Cd1 89.1(3) . 4_666 ?
Cd2 O7 Cd1 93.23(11) 2 4_666 ?
C18 N1 C16 105.0(4) . . ?
C18 N1 Cd1 111.3(3) . . ?
C16 N1 Cd1 142.9(4) . . ?
C19 N2 C21 105.4(4) . . ?
C19 N2 Cd1 111.6(3) . . ?
C21 N2 Cd1 143.0(4) . . ?
C19 N3 C20 106.8(5) . . ?
C19 N3 H1 126.6 . . ?
C20 N3 H1 126.6 . . ?
C18 N4 C17 108.1(5) . . ?
C18 N4 H2 126.0 . . ?
C17 N4 H2 126.0 . . ?
O1 C1 O2 126.9(4) . . ?
O1 C1 C2 115.1(4) . . ?
O2 C1 C2 117.9(4) . . ?
C3 C2 C8 119.4(4) . . ?
C3 C2 C1 121.8(4) . . ?
C8 C2 C1 118.8(4) . . ?
C4 C3 C2 120.3(4) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C3 C4 C5 121.2(4) . . ?
C3 C4 H4 119.4 . . ?
C5 C4 H4 119.4 . . ?
C4 C5 C7 118.0(4) . . ?
C4 C5 C6 119.0(4) . . ?
C7 C5 C6 122.9(4) . . ?
O4 C6 O3 122.1(4) . . ?
O4 C6 C5 120.1(4) . . ?
O3 C6 C5 117.8(4) . . ?
C8 C7 O5 123.2(4) . . ?
C8 C7 C5 120.3(4) . . ?
O5 C7 C5 116.5(4) . . ?
C7 C8 C2 120.8(4) . . ?
C7 C8 H8 119.6 . . ?
C2 C8 H8 119.6 . . ?
C10 C9 C14 121.7(4) . . ?
C10 C9 O5 116.0(4) . . ?
C14 C9 O5 122.0(4) . . ?
C9 C10 C11 119.3(5) . . ?
C9 C10 H10 120.4 . . ?
C11 C10 H10 120.4 . . ?
C12 C11 C10 120.6(5) . . ?
C12 C11 H11 119.7 . . ?
C10 C11 H11 119.7 . . ?
C11 C12 C13 119.9(5) . . ?
C11 C12 H12 120.1 . . ?
C13 C12 H12 120.1 . . ?
C12 C13 C14 121.1(5) . . ?
C12 C13 H13 119.4 . . ?
C14 C13 H13 119.4 . . ?
C9 C14 C13 117.3(4) . . ?
C9 C14 C15 124.6(4) . . ?
C13 C14 C15 118.1(4) . . ?
O6 C15 O7 121.2(5) . . ?
O6 C15 C14 119.1(4) . . ?
O7 C15 C14 119.7(5) . . ?
O6 C15 Cd1 58.3(3) . 4_666 ?
O7 C15 Cd1 63.2(3) . 4_666 ?
C14 C15 Cd1 172.1(3) . 4_666 ?
C17 C16 N1 110.6(6) . . ?
C17 C16 H16 124.7 . . ?
N1 C16 H16 124.7 . . ?
C16 C17 N4 105.5(5) . . ?
C16 C17 H17 127.2 . . ?
N4 C17 H17 127.2 . . ?
N1 C18 N4 110.8(5) . . ?
N1 C18 C19 121.1(4) . . ?
N4 C18 C19 128.0(5) . . ?
N2 C19 N3 111.3(5) . . ?
N2 C19 C18 120.6(4) . . ?
N3 C19 C18 128.1(5) . . ?
C21 C20 N3 106.6(5) . . ?
C21 C20 H20 126.7 . . ?
N3 C20 H20 126.7 . . ?
C20 C21 N2 109.9(6) . . ?
C20 C21 H21 125.1 . . ?
N2 C21 H21 125.1 . . ?

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
Cd1 O1 C1 O2 -6.3(8) . . . . ?
Cd1 O1 C1 C2 173.4(3) . . . . ?
Cd2 O2 C1 O1 -8.2(7) . . . . ?
Cd2 O2 C1 C2 172.2(3) . . . . ?
O1 C1 C2 C3 151.9(5) . . . . ?
O2 C1 C2 C3 -28.4(7) . . . . ?
O1 C1 C2 C8 -26.7(6) . . . . ?
O2 C1 C2 C8 153.0(5) . . . . ?
C8 C2 C3 C4 -2.2(7) . . . . ?
C1 C2 C3 C4 179.3(5) . . . . ?
C2 C3 C4 C5 1.9(8) . . . . ?
C3 C4 C5 C7 0.2(7) . . . . ?
C3 C4 C5 C6 178.8(5) . . . . ?
Cd1 O3 C6 O4 14.1(6) 2 . . . ?
Cd2 O3 C6 O4 -154.4(3) 2 . . . ?
Cd1 O3 C6 C5 -165.5(3) 2 . . . ?
Cd2 O3 C6 C5 26.1(7) 2 . . . ?
C4 C5 C6 O4 47.2(6) . . . . ?
C7 C5 C6 O4 -134.3(5) . . . . ?
C4 C5 C6 O3 -133.2(5) . . . . ?
C7 C5 C6 O3 45.3(7) . . . . ?
C9 O5 C7 C8 4.7(6) . . . . ?
C9 O5 C7 C5 -178.1(4) . . . . ?
C4 C5 C7 C8 -2.0(7) . . . . ?
C6 C5 C7 C8 179.5(4) . . . . ?
C4 C5 C7 O5 -179.2(4) . . . . ?
C6 C5 C7 O5 2.3(7) . . . . ?
O5 C7 C8 C2 178.7(4) . . . . ?
C5 C7 C8 C2 1.7(7) . . . . ?
C3 C2 C8 C7 0.4(7) . . . . ?
C1 C2 C8 C7 179.0(4) . . . . ?
C7 O5 C9 C10 -98.4(5) . . . . ?
C7 O5 C9 C14 86.8(5) . . . . ?
C14 C9 C10 C11 -2.9(7) . . . . ?
O5 C9 C10 C11 -177.7(4) . . . . ?
C9 C10 C11 C12 2.0(8) . . . . ?
C10 C11 C12 C13 -0.7(8) . . . . ?
C11 C12 C13 C14 0.2(8) . . . . ?
C10 C9 C14 C13 2.3(7) . . . . ?
O5 C9 C14 C13 176.9(4) . . . . ?
C10 C9 C14 C15 -176.6(4) . . . . ?
O5 C9 C14 C15 -2.0(7) . . . . ?
C12 C13 C14 C9 -1.0(7) . . . . ?
C12 C13 C14 C15 178.0(5) . . . . ?
Cd1 O6 C15 O7 -5.9(4) 4_666 . . . ?
Cd1 O6 C15 C14 171.3(3) 4_666 . . . ?
Cd2 O7 C15 O6 -87.6(5) 2 . . . ?
Cd1 O7 C15 O6 5.6(4) 4_666 . . . ?
Cd2 O7 C15 C14 95.1(4) 2 . . . ?
Cd1 O7 C15 C14 -171.6(4) 4_666 . . . ?
Cd2 O7 C15 Cd1 -93.3(3) 2 . . 4_666 ?
C9 C14 C15 O6 170.8(4) . . . . ?
C13 C14 C15 O6 -8.1(6) . . . . ?
C9 C14 C15 O7 -11.9(7) . . . . ?
C13 C14 C15 O7 169.2(4) . . . . ?
C18 N1 C16 C17 -1.1(7) . . . . ?
Cd1 N1 C16 C17 166.8(5) . . . . ?
N1 C16 C17 N4 1.0(8) . . . . ?
C18 N4 C17 C16 -0.5(7) . . . . ?
C16 N1 C18 N4 0.8(6) . . . . ?
Cd1 N1 C18 N4 -171.4(3) . . . . ?
C16 N1 C18 C19 179.3(5) . . . . ?
Cd1 N1 C18 C19 7.2(5) . . . . ?
C17 N4 C18 N1 -0.2(6) . . . . ?
C17 N4 C18 C19 -178.7(5) . . . . ?
C21 N2 C19 N3 0.6(6) . . . . ?
Cd1 N2 C19 N3 -179.3(3) . . . . ?
C21 N2 C19 C18 -177.8(5) . . . . ?
Cd1 N2 C19 C18 2.4(6) . . . . ?
C20 N3 C19 N2 -0.5(7) . . . . ?
C20 N3 C19 C18 177.7(5) . . . . ?
N1 C18 C19 N2 -6.9(7) . . . . ?
N4 C18 C19 N2 171.4(5) . . . . ?
N1 C18 C19 N3 175.0(5) . . . . ?
N4 C18 C19 N3 -6.7(9) . . . . ?
C19 N3 C20 C21 0.2(8) . . . . ?
N3 C20 C21 N2 0.2(8) . . . . ?
C19 N2 C21 C20 -0.5(7) . . . . ?
Cd1 N2 C21 C20 179.3(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
N3 H1 O4 0.86 2.11 2.852(6) 144.6 1_455
N4 H2 O4 0.86 2.22 2.902(6) 136.1 1_455

_refine_diff_density_max         0.790
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.113


# start Validation Reply Form
_vrf_PLAT910_I                   
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min) 7 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_278-7Mn1
_database_code_depnum_ccdc_archive 'CCDC 1509062'
_audit_update_record             
;
2017-03-26 deposited with the CCDC.
2017-04-10 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 H30 Mn3 N4 O14'
_chemical_formula_weight         1075.60

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'
Mn Mn 0.3368 0.7283 '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                   12.1882(5)
_cell_length_b                   15.0139(4)
_cell_length_c                   13.2410(6)
_cell_angle_alpha                90
_cell_angle_beta                 114.569(5)
_cell_angle_gamma                90
_cell_volume                     2203.65(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8231
_cell_measurement_theta_min      3.266
_cell_measurement_theta_max      25.049

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_F_000             1090
_exptl_transmission_factor_min   0.801
_exptl_transmission_factor_max   0.839
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    0.925
_shelx_estimated_absorpt_T_min   0.795
_shelx_estimated_absorpt_T_max   0.844
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.795
_exptl_absorpt_correction_T_max  0.844
_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            8231
_diffrn_reflns_av_unetI/netI     0.0600
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         3.266
_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             3892
_reflns_number_gt                2976
_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)+(0.0214P)²+0.2447P] 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         3892
_refine_ls_number_parameters     322
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0399
_refine_ls_wR_factor_ref         0.0821
_refine_ls_wR_factor_gt          0.0715
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_restrained_S_all      1.069
_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
Mn1 Mn 0.24470(4) 0.38233(3) 0.88074(4) 0.02656(14) Uani 1 1 d . . . . .
Mn2 Mn 0.5000 0.5000 1.0000 0.02346(16) Uani 1 2 d S . P . .
N1 N 0.2092(2) 0.25292(16) 0.9500(2) 0.0338(6) Uani 1 1 d . . . . .
N2 N 0.0930(2) 0.31595(15) 0.7436(2) 0.0286(6) Uani 1 1 d . . . . .
O1 O 0.62367(16) 0.57073(12) 0.94055(15) 0.0279(5) Uani 1 1 d . . . . .
O2 O 0.81827(18) 0.54079(14) 1.01150(18) 0.0425(6) Uani 1 1 d . . . . .
O3 O 0.48506(17) 0.50723(11) 0.73287(16) 0.0296(5) Uani 1 1 d . . . . .
O4 O 0.33399(16) 0.49566(12) 0.84739(16) 0.0293(5) Uani 1 1 d . . . . .
O5 O 0.16304(17) 0.54074(13) 0.71247(18) 0.0417(6) Uani 1 1 d . . . . .
O6 O 0.62291(17) 0.80349(12) 0.63877(18) 0.0401(6) Uani 1 1 d . . . . .
O7 O 0.44852(17) 0.87636(12) 0.55186(16) 0.0322(5) Uani 1 1 d . . . . .
C1 C 0.7162(3) 0.53836(18) 0.9319(3) 0.0297(7) Uani 1 1 d . . . . .
C2 C 0.7043(3) 0.49723(17) 0.8245(2) 0.0270(7) Uani 1 1 d . . . . .
C3 C 0.5954(3) 0.48411(17) 0.7322(2) 0.0270(7) Uani 1 1 d . . . . .
C4 C 0.5913(3) 0.4406(2) 0.6388(3) 0.0388(8) Uani 1 1 d . . . . .
H4 H 0.5179 0.4332 0.5777 0.047 Uiso 1 1 calc R U . . .
C5 C 0.6956(3) 0.4081(2) 0.6359(3) 0.0468(9) Uani 1 1 d . . . . .
H5 H 0.6926 0.3780 0.5735 0.056 Uiso 1 1 calc R U . . .
C6 C 0.8042(3) 0.4205(2) 0.7255(3) 0.0454(9) Uani 1 1 d . . . . .
H6 H 0.8748 0.3989 0.7235 0.054 Uiso 1 1 calc R U . . .
C7 C 0.8087(3) 0.46474(19) 0.8183(3) 0.0364(8) Uani 1 1 d . . . . .
H7 H 0.8829 0.4732 0.8781 0.044 Uiso 1 1 calc R U . . .
C8 C 0.4454(2) 0.59429(17) 0.7137(2) 0.0230(6) Uani 1 1 d . . . . .
C9 C 0.3407(2) 0.61337(16) 0.7282(2) 0.0220(6) Uani 1 1 d . . . . .
C10 C 0.2733(3) 0.54606(17) 0.7642(2) 0.0257(7) Uani 1 1 d . . . . .
C11 C 0.2941(2) 0.69942(17) 0.7042(2) 0.0272(7) Uani 1 1 d . . . . .
H11 H 0.2255 0.7140 0.7148 0.033 Uiso 1 1 calc R U . . .
C12 C 0.3477(2) 0.76328(17) 0.6650(2) 0.0280(7) Uani 1 1 d . . . . .
H12 H 0.3143 0.8200 0.6484 0.034 Uiso 1 1 calc R U . . .
C13 C 0.4511(2) 0.74336(17) 0.6501(2) 0.0233(6) Uani 1 1 d . . . . .
C14 C 0.5116(3) 0.81361(18) 0.6094(2) 0.0265(7) Uani 1 1 d . . . . .
C15 C 0.5003(2) 0.65850(17) 0.6753(2) 0.0260(7) Uani 1 1 d . . . . .
H15 H 0.5701 0.6448 0.6663 0.031 Uiso 1 1 calc R U . . .
C16 C 0.2767(3) 0.2228(2) 1.0523(3) 0.0450(9) Uani 1 1 d . . . . .
H16 H 0.3263 0.2629 1.1050 0.054 Uiso 1 1 calc R U . . .
C17 C 0.2763(3) 0.1359(2) 1.0833(3) 0.0462(9) Uani 1 1 d . . . . .
H17 H 0.3249 0.1173 1.1552 0.055 Uiso 1 1 calc R U . . .
C18 C 0.2027(3) 0.0773(2) 1.0060(3) 0.0560(10) Uani 1 1 d . . . . .
H18 H 0.2010 0.0176 1.0244 0.067 Uiso 1 1 calc R U . . .
C19 C 0.1308(3) 0.1069(2) 0.9005(3) 0.0488(9) Uani 1 1 d . . . . .
H19 H 0.0787 0.0679 0.8477 0.059 Uiso 1 1 calc R U . . .
C20 C 0.1372(3) 0.19498(18) 0.8743(3) 0.0305(7) Uani 1 1 d . . . . .
C21 C 0.0675(3) 0.23156(19) 0.7613(3) 0.0337(7) Uani 1 1 d . . . . .
C22 C -0.0190(3) 0.1819(2) 0.6770(3) 0.0618(12) Uani 1 1 d . . . . .
H22 H -0.0371 0.1242 0.6906 0.074 Uiso 1 1 calc R U . . .
C23 C -0.0775(4) 0.2191(3) 0.5732(3) 0.0764(14) Uani 1 1 d . . . . .
H23 H -0.1348 0.1863 0.5160 0.092 Uiso 1 1 calc R U . . .
C24 C -0.0511(3) 0.3051(2) 0.5541(3) 0.0548(10) Uani 1 1 d . . . . .
H24 H -0.0895 0.3314 0.4845 0.066 Uiso 1 1 calc R U . . .
C25 C 0.0343(3) 0.3503(2) 0.6418(3) 0.0369(8) Uani 1 1 d . . . . .
H25 H 0.0523 0.4084 0.6297 0.044 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
Mn1 O6 2.102(2) 2_646 ?
Mn1 O4 2.1620(18) . ?
Mn1 O2 2.206(2) 3_667 ?
Mn1 N2 2.217(2) . ?
Mn1 N1 2.266(2) . ?
Mn1 O1 2.3479(19) 3_667 ?
Mn1 C1 2.610(3) 3_667 ?
Mn2 O7 2.1609(18) 4_576 ?
Mn2 O7 2.1609(18) 2_646 ?
Mn2 O4 2.1867(18) . ?
Mn2 O4 2.1867(18) 3_667 ?
Mn2 O1 2.2374(18) . ?
Mn2 O1 2.2374(18) 3_667 ?
N1 C16 1.338(4) . ?
N1 C20 1.342(3) . ?
N2 C25 1.339(4) . ?
N2 C21 1.348(3) . ?
O1 C1 1.276(3) . ?
O1 Mn1 2.3479(19) 3_667 ?
O2 C1 1.252(3) . ?
O2 Mn1 2.206(2) 3_667 ?
O3 C8 1.380(3) . ?
O3 C3 1.393(3) . ?
O4 C10 1.286(3) . ?
O5 C10 1.231(3) . ?
O6 C14 1.256(3) . ?
O6 Mn1 2.102(2) 2_656 ?
O7 C14 1.254(3) . ?
O7 Mn2 2.1609(18) 2_656 ?
C1 C2 1.501(4) . ?
C1 Mn1 2.610(3) 3_667 ?
C2 C3 1.394(4) . ?
C2 C7 1.397(4) . ?
C3 C4 1.381(4) . ?
C4 C5 1.377(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.374(4) . ?
C5 H5 0.9300 . ?
C6 C7 1.378(4) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 C15 1.385(4) . ?
C8 C9 1.397(4) . ?
C9 C11 1.394(3) . ?
C9 C10 1.501(4) . ?
C11 C12 1.378(4) . ?
C11 H11 0.9300 . ?
C12 C13 1.388(4) . ?
C12 H12 0.9300 . ?
C13 C15 1.388(3) . ?
C13 C14 1.508(4) . ?
C15 H15 0.9300 . ?
C16 C17 1.368(4) . ?
C16 H16 0.9300 . ?
C17 C18 1.366(4) . ?
C17 H17 0.9300 . ?
C18 C19 1.377(4) . ?
C18 H18 0.9300 . ?
C19 C20 1.378(4) . ?
C19 H19 0.9300 . ?
C20 C21 1.485(4) . ?
C21 C22 1.390(4) . ?
C22 C23 1.376(5) . ?
C22 H22 0.9300 . ?
C23 C24 1.379(5) . ?
C23 H23 0.9300 . ?
C24 C25 1.374(4) . ?
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
O6 Mn1 O4 86.60(8) 2_646 . ?
O6 Mn1 O2 149.92(8) 2_646 3_667 ?
O4 Mn1 O2 93.46(8) . 3_667 ?
O6 Mn1 N2 93.87(8) 2_646 . ?
O4 Mn1 N2 120.37(8) . . ?
O2 Mn1 N2 111.65(8) 3_667 . ?
O6 Mn1 N1 81.52(9) 2_646 . ?
O4 Mn1 N1 162.68(8) . . ?
O2 Mn1 N1 90.60(9) 3_667 . ?
N2 Mn1 N1 73.23(9) . . ?
O6 Mn1 O1 93.16(7) 2_646 3_667 ?
O4 Mn1 O1 77.21(7) . 3_667 ?
O2 Mn1 O1 57.78(7) 3_667 3_667 ?
N2 Mn1 O1 161.42(8) . 3_667 ?
N1 Mn1 O1 90.85(8) . 3_667 ?
O6 Mn1 C1 121.84(9) 2_646 3_667 ?
O4 Mn1 C1 85.79(8) . 3_667 ?
O2 Mn1 C1 28.59(8) 3_667 3_667 ?
N2 Mn1 C1 138.05(9) . 3_667 ?
N1 Mn1 C1 89.81(9) . 3_667 ?
O1 Mn1 C1 29.22(7) 3_667 3_667 ?
O7 Mn2 O7 180.0 4_576 2_646 ?
O7 Mn2 O4 92.29(7) 4_576 . ?
O7 Mn2 O4 87.71(7) 2_646 . ?
O7 Mn2 O4 87.71(7) 4_576 3_667 ?
O7 Mn2 O4 92.29(7) 2_646 3_667 ?
O4 Mn2 O4 180.0 . 3_667 ?
O7 Mn2 O1 91.79(7) 4_576 . ?
O7 Mn2 O1 88.21(7) 2_646 . ?
O4 Mn2 O1 100.89(7) . . ?
O4 Mn2 O1 79.11(7) 3_667 . ?
O7 Mn2 O1 88.21(7) 4_576 3_667 ?
O7 Mn2 O1 91.79(7) 2_646 3_667 ?
O4 Mn2 O1 79.11(7) . 3_667 ?
O4 Mn2 O1 100.89(7) 3_667 3_667 ?
O1 Mn2 O1 180.00(8) . 3_667 ?
C16 N1 C20 118.2(3) . . ?
C16 N1 Mn1 124.0(2) . . ?
C20 N1 Mn1 115.4(2) . . ?
C25 N2 C21 118.1(2) . . ?
C25 N2 Mn1 124.5(2) . . ?
C21 N2 Mn1 117.02(19) . . ?
C1 O1 Mn2 126.91(17) . . ?
C1 O1 Mn1 86.86(17) . 3_667 ?
Mn2 O1 Mn1 93.78(7) . 3_667 ?
C1 O2 Mn1 93.92(18) . 3_667 ?
C8 O3 C3 120.0(2) . . ?
C10 O4 Mn1 118.58(17) . . ?
C10 O4 Mn2 139.06(17) . . ?
Mn1 O4 Mn2 100.70(8) . . ?
C14 O6 Mn1 132.83(18) . 2_656 ?
C14 O7 Mn2 130.79(18) . 2_656 ?
O2 C1 O1 121.3(3) . . ?
O2 C1 C2 118.7(3) . . ?
O1 C1 C2 120.0(3) . . ?
O2 C1 Mn1 57.49(15) . 3_667 ?
O1 C1 Mn1 63.91(15) . 3_667 ?
C2 C1 Mn1 174.5(2) . 3_667 ?
C3 C2 C7 117.2(3) . . ?
C3 C2 C1 124.8(3) . . ?
C7 C2 C1 117.9(3) . . ?
C4 C3 O3 116.6(3) . . ?
C4 C3 C2 121.3(3) . . ?
O3 C3 C2 121.9(3) . . ?
C5 C4 C3 120.1(3) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C6 C5 C4 119.8(3) . . ?
C6 C5 H5 120.1 . . ?
C4 C5 H5 120.1 . . ?
C5 C6 C7 120.1(3) . . ?
C5 C6 H6 119.9 . . ?
C7 C6 H6 119.9 . . ?
C6 C7 C2 121.4(3) . . ?
C6 C7 H7 119.3 . . ?
C2 C7 H7 119.3 . . ?
O3 C8 C15 122.8(2) . . ?
O3 C8 C9 116.0(2) . . ?
C15 C8 C9 121.1(2) . . ?
C11 C9 C8 117.9(2) . . ?
C11 C9 C10 118.1(2) . . ?
C8 C9 C10 123.9(2) . . ?
O5 C10 O4 123.0(3) . . ?
O5 C10 C9 118.8(3) . . ?
O4 C10 C9 118.2(2) . . ?
C12 C11 C9 121.2(3) . . ?
C12 C11 H11 119.4 . . ?
C9 C11 H11 119.4 . . ?
C11 C12 C13 120.3(3) . . ?
C11 C12 H12 119.8 . . ?
C13 C12 H12 119.8 . . ?
C12 C13 C15 119.4(2) . . ?
C12 C13 C14 120.5(2) . . ?
C15 C13 C14 120.1(3) . . ?
O7 C14 O6 126.1(3) . . ?
O7 C14 C13 118.4(2) . . ?
O6 C14 C13 115.5(2) . . ?
C8 C15 C13 120.1(3) . . ?
C8 C15 H15 120.0 . . ?
C13 C15 H15 120.0 . . ?
N1 C16 C17 123.3(3) . . ?
N1 C16 H16 118.3 . . ?
C17 C16 H16 118.3 . . ?
C18 C17 C16 118.2(3) . . ?
C18 C17 H17 120.9 . . ?
C16 C17 H17 120.9 . . ?
C17 C18 C19 119.7(3) . . ?
C17 C18 H18 120.2 . . ?
C19 C18 H18 120.2 . . ?
C18 C19 C20 119.1(3) . . ?
C18 C19 H19 120.4 . . ?
C20 C19 H19 120.4 . . ?
N1 C20 C19 121.4(3) . . ?
N1 C20 C21 115.8(3) . . ?
C19 C20 C21 122.7(3) . . ?
N2 C21 C22 121.1(3) . . ?
N2 C21 C20 116.5(2) . . ?
C22 C21 C20 122.4(3) . . ?
C23 C22 C21 119.3(3) . . ?
C23 C22 H22 120.4 . . ?
C21 C22 H22 120.4 . . ?
C22 C23 C24 120.0(3) . . ?
C22 C23 H23 120.0 . . ?
C24 C23 H23 120.0 . . ?
C25 C24 C23 117.4(3) . . ?
C25 C24 H24 121.3 . . ?
C23 C24 H24 121.3 . . ?
N2 C25 C24 124.1(3) . . ?
N2 C25 H25 118.0 . . ?
C24 C25 H25 118.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mn1 O2 C1 O1 -3.9(3) 3_667 . . . ?
Mn1 O2 C1 C2 175.4(2) 3_667 . . . ?
Mn2 O1 C1 O2 -88.7(3) . . . . ?
Mn1 O1 C1 O2 3.7(3) 3_667 . . . ?
Mn2 O1 C1 C2 92.0(3) . . . . ?
Mn1 O1 C1 C2 -175.7(2) 3_667 . . . ?
Mn2 O1 C1 Mn1 -92.37(17) . . . 3_667 ?
O2 C1 C2 C3 175.0(3) . . . . ?
O1 C1 C2 C3 -5.6(4) . . . . ?
O2 C1 C2 C7 -0.9(4) . . . . ?
O1 C1 C2 C7 178.4(3) . . . . ?
C8 O3 C3 C4 -103.4(3) . . . . ?
C8 O3 C3 C2 81.9(3) . . . . ?
C7 C2 C3 C4 0.1(4) . . . . ?
C1 C2 C3 C4 -175.8(3) . . . . ?
C7 C2 C3 O3 174.6(2) . . . . ?
C1 C2 C3 O3 -1.3(4) . . . . ?
O3 C3 C4 C5 -173.9(3) . . . . ?
C2 C3 C4 C5 0.9(4) . . . . ?
C3 C4 C5 C6 -1.1(5) . . . . ?
C4 C5 C6 C7 0.4(5) . . . . ?
C5 C6 C7 C2 0.7(5) . . . . ?
C3 C2 C7 C6 -0.9(4) . . . . ?
C1 C2 C7 C6 175.4(3) . . . . ?
C3 O3 C8 C15 11.1(4) . . . . ?
C3 O3 C8 C9 -173.1(2) . . . . ?
O3 C8 C9 C11 -176.8(2) . . . . ?
C15 C8 C9 C11 -0.8(4) . . . . ?
O3 C8 C9 C10 1.0(4) . . . . ?
C15 C8 C9 C10 177.0(3) . . . . ?
Mn1 O4 C10 O5 10.7(4) . . . . ?
Mn2 O4 C10 O5 -151.2(2) . . . . ?
Mn1 O4 C10 C9 -168.32(18) . . . . ?
Mn2 O4 C10 C9 29.8(4) . . . . ?
C11 C9 C10 O5 45.6(4) . . . . ?
C8 C9 C10 O5 -132.3(3) . . . . ?
C11 C9 C10 O4 -135.3(3) . . . . ?
C8 C9 C10 O4 46.9(4) . . . . ?
C8 C9 C11 C12 1.5(4) . . . . ?
C10 C9 C11 C12 -176.5(3) . . . . ?
C9 C11 C12 C13 -1.0(4) . . . . ?
C11 C12 C13 C15 -0.1(4) . . . . ?
C11 C12 C13 C14 -178.8(3) . . . . ?
Mn2 O7 C14 O6 -10.3(5) 2_656 . . . ?
Mn2 O7 C14 C13 168.59(18) 2_656 . . . ?
Mn1 O6 C14 O7 4.4(5) 2_656 . . . ?
Mn1 O6 C14 C13 -174.53(18) 2_656 . . . ?
C12 C13 C14 O7 -26.1(4) . . . . ?
C15 C13 C14 O7 155.3(3) . . . . ?
C12 C13 C14 O6 153.0(3) . . . . ?
C15 C13 C14 O6 -25.7(4) . . . . ?
O3 C8 C15 C13 175.5(2) . . . . ?
C9 C8 C15 C13 -0.2(4) . . . . ?
C12 C13 C15 C8 0.7(4) . . . . ?
C14 C13 C15 C8 179.4(2) . . . . ?
C20 N1 C16 C17 0.3(5) . . . . ?
Mn1 N1 C16 C17 -161.5(3) . . . . ?
N1 C16 C17 C18 -0.4(5) . . . . ?
C16 C17 C18 C19 -0.6(5) . . . . ?
C17 C18 C19 C20 1.8(5) . . . . ?
C16 N1 C20 C19 0.9(4) . . . . ?
Mn1 N1 C20 C19 164.2(2) . . . . ?
C16 N1 C20 C21 -178.1(3) . . . . ?
Mn1 N1 C20 C21 -14.7(3) . . . . ?
C18 C19 C20 N1 -1.9(5) . . . . ?
C18 C19 C20 C21 177.0(3) . . . . ?
C25 N2 C21 C22 -1.2(4) . . . . ?
Mn1 N2 C21 C22 -174.4(3) . . . . ?
C25 N2 C21 C20 178.2(3) . . . . ?
Mn1 N2 C21 C20 5.0(3) . . . . ?
N1 C20 C21 N2 6.7(4) . . . . ?
C19 C20 C21 N2 -172.2(3) . . . . ?
N1 C20 C21 C22 -173.9(3) . . . . ?
C19 C20 C21 C22 7.1(5) . . . . ?
N2 C21 C22 C23 1.4(6) . . . . ?
C20 C21 C22 C23 -177.9(3) . . . . ?
C21 C22 C23 C24 -0.7(7) . . . . ?
C22 C23 C24 C25 -0.1(6) . . . . ?
C21 N2 C25 C24 0.3(5) . . . . ?
Mn1 N2 C25 C24 173.0(3) . . . . ?
C23 C24 C25 N2 0.3(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
C25 H25 O5 0.93 2.40 3.208(4) 145.9 .
C17 H17 O3 0.93 2.59 3.290(4) 132.7 4_566
C25 H25 O5 0.93 2.40 3.208(4) 145.9 .
C17 H17 O3 0.93 2.59 3.290(4) 132.7 4_566
C17 H17 O3 0.93 2.59 3.290(4) 132.7 4_566
C25 H25 O5 0.93 2.40 3.208(4) 145.9 .
C17 H17 O3 0.93 2.59 3.290(4) 132.7 4_566
C25 H25 O5 0.93 2.40 3.208(4) 145.9 .

_refine_diff_density_max         0.270
_refine_diff_density_min         -0.266
_refine_diff_density_rms         0.063


# start Validation Reply Form
_vrf_PLAT910_I                   
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min) 7 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_282-12Zn1
_database_code_depnum_ccdc_archive 'CCDC 1509367'
_audit_update_record             
;
2017-03-26 deposited with the CCDC.
2017-04-10 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            'C66 H46 N6 O17 Zn3'
_chemical_formula_weight         1391.20

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                   17.3969(10)
_cell_length_b                   22.9035(12)
_cell_length_c                   14.6548(9)
_cell_angle_alpha                90
_cell_angle_beta                 99.242(5)
_cell_angle_gamma                90
_cell_volume                     5763.4(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    10479
_cell_measurement_theta_min      3.332
_cell_measurement_theta_max      25.049

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_F_000             2840
_exptl_transmission_factor_min   0.716
_exptl_transmission_factor_max   0.738
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.230
_exptl_absorpt_coefficient_mu    1.321
_shelx_estimated_absorpt_T_min   0.725
_shelx_estimated_absorpt_T_max   0.751
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.725
_exptl_absorpt_correction_T_max  0.751
_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            10479
_diffrn_reflns_av_unetI/netI     0.1196
_diffrn_reflns_av_R_equivalents  0.0696
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.332
_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             5100
_reflns_number_gt                3080
_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)+(0.0372P)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         5100
_refine_ls_number_parameters     416
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1167
_refine_ls_R_factor_gt           0.0638
_refine_ls_wR_factor_ref         0.1390
_refine_ls_wR_factor_gt          0.1092
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      1.011
_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 0.05591(4) 0.32390(3) 0.02330(4) 0.0342(2) Uani 1 1 d . . . . .
Zn2 Zn 0.5000 0.48287(4) 0.2500 0.0398(3) Uani 1 2 d S T P . .
N1 N 0.0642(3) 0.23288(19) 0.0340(3) 0.0370(12) Uani 1 1 d . . . . .
N2 N 0.1371(3) 0.30766(19) -0.0630(3) 0.0350(11) Uani 1 1 d . . . . .
N3 N 0.4448(3) 0.4123(2) 0.3036(3) 0.0428(12) Uani 1 1 d . . . . .
O1 O 0.0812(2) 0.34998(16) 0.1533(2) 0.0396(10) Uani 1 1 d . . . . .
O2 O 0.1193(2) 0.42080(17) 0.0694(3) 0.0485(11) Uani 1 1 d . . . . .
O3 O 0.2366(2) 0.48731(15) 0.1778(3) 0.0356(9) Uani 1 1 d . . . . .
O4 O 0.0997(3) 0.70175(19) -0.0159(3) 0.0587(13) Uani 1 1 d . . . . .
O5 O 0.0327(2) 0.63793(17) 0.0525(3) 0.0493(11) Uani 1 1 d . . . . .
O6 O 0.4045(2) 0.54148(19) 0.2705(3) 0.0618(13) Uani 1 1 d . . . . .
O7 O 0.4167(2) 0.51094(18) 0.1329(3) 0.0551(12) Uani 1 1 d . . . . .
O8 O 0.1261(4) 0.7315(2) 0.8047(4) 0.120(3) Uani 1 1 d . . . . .
H1W H 0.1131 0.7077 0.7604 0.144 Uiso 1 1 d R U . . .
H2W H 0.1185 0.7228 0.8589 0.144 Uiso 1 1 d R U . . .
O9 O 0.0000 0.5900(14) 0.2500 0.69(3) Uani 1 2 d S T P . .
H3W H -0.0087 0.6021 0.3022 0.829 Uiso 1 1 d R U . . .
H4W H 0.0087 0.6021 0.1978 0.829 Uiso 1 1 d R U . . .
C1 C 0.1113(3) 0.4012(2) 0.1453(4) 0.0341(14) Uani 1 1 d . . . . .
C2 C 0.1338(3) 0.4341(2) 0.2347(4) 0.0304(13) Uani 1 1 d . . . . .
C3 C 0.0947(3) 0.4238(2) 0.3081(4) 0.0399(15) Uani 1 1 d . . . . .
H3 H 0.0576 0.3942 0.3027 0.048 Uiso 1 1 calc R U . . .
C4 C 0.1084(4) 0.4552(3) 0.3881(4) 0.0503(17) Uani 1 1 d . . . . .
H4 H 0.0776 0.4496 0.4336 0.060 Uiso 1 1 calc R U . . .
C5 C 0.1684(4) 0.4953(3) 0.4011(4) 0.0536(18) Uani 1 1 d . . . . .
H5 H 0.1805 0.5151 0.4570 0.064 Uiso 1 1 calc R U . . .
C6 C 0.2105(4) 0.5059(2) 0.3302(4) 0.0450(16) Uani 1 1 d . . . . .
H6 H 0.2513 0.5326 0.3385 0.054 Uiso 1 1 calc R U . . .
C7 C 0.1916(3) 0.4766(2) 0.2469(4) 0.0326(13) Uani 1 1 d . . . . .
C8 C 0.2359(3) 0.5451(2) 0.1471(3) 0.0269(12) Uani 1 1 d . . . . .
C9 C 0.1673(3) 0.5736(2) 0.1153(3) 0.0322(13) Uani 1 1 d . . . . .
H9 H 0.1197 0.5557 0.1179 0.039 Uiso 1 1 calc R U . . .
C10 C 0.1699(3) 0.6293(2) 0.0795(3) 0.0314(13) Uani 1 1 d . . . . .
C11 C 0.0958(4) 0.6589(3) 0.0356(4) 0.0393(15) Uani 1 1 d . . . . .
C12 C 0.2411(3) 0.6565(2) 0.0804(4) 0.0395(15) Uani 1 1 d . . . . .
H12 H 0.2427 0.6942 0.0573 0.047 Uiso 1 1 calc R U . . .
C13 C 0.3095(3) 0.6286(2) 0.1149(4) 0.0419(16) Uani 1 1 d . . . . .
H13 H 0.3569 0.6476 0.1166 0.050 Uiso 1 1 calc R U . . .
C14 C 0.3072(3) 0.5716(2) 0.1472(4) 0.0317(13) Uani 1 1 d . . . . .
C15 C 0.3814(3) 0.5385(2) 0.1863(5) 0.0382(15) Uani 1 1 d . . . . .
C16 C 0.0278(4) 0.1974(3) 0.0833(5) 0.0581(19) Uani 1 1 d . . . . .
H16 H -0.0047 0.2128 0.1218 0.070 Uiso 1 1 calc R U . . .
C17 C 0.0370(4) 0.1368(3) 0.0787(6) 0.075(2) Uani 1 1 d . . . . .
H17 H 0.0099 0.1124 0.1131 0.090 Uiso 1 1 calc R U . . .
C18 C 0.0854(4) 0.1135(3) 0.0244(6) 0.074(2) Uani 1 1 d . . . . .
H18 H 0.0919 0.0732 0.0221 0.089 Uiso 1 1 calc R U . . .
C19 C 0.1252(4) 0.1497(3) -0.0278(5) 0.0494(17) Uani 1 1 d . . . . .
C20 C 0.1123(3) 0.2100(2) -0.0200(4) 0.0358(14) Uani 1 1 d . . . . .
C21 C 0.1779(4) 0.1310(3) -0.0883(5) 0.063(2) Uani 1 1 d . . . . .
H21 H 0.1857 0.0911 -0.0949 0.075 Uiso 1 1 calc R U . . .
C22 C 0.2165(4) 0.1681(3) -0.1359(5) 0.063(2) Uani 1 1 d . . . . .
H22 H 0.2511 0.1541 -0.1729 0.076 Uiso 1 1 calc R U . . .
C23 C 0.2035(3) 0.2293(3) -0.1288(4) 0.0424(16) Uani 1 1 d . . . . .
C24 C 0.1528(3) 0.2497(2) -0.0716(4) 0.0331(14) Uani 1 1 d . . . . .
C25 C 0.2398(4) 0.2701(3) -0.1785(4) 0.060(2) Uani 1 1 d . . . . .
H25 H 0.2745 0.2582 -0.2169 0.072 Uiso 1 1 calc R U . . .
C26 C 0.2231(4) 0.3282(3) -0.1696(5) 0.064(2) Uani 1 1 d . . . . .
H26 H 0.2464 0.3562 -0.2022 0.076 Uiso 1 1 calc R U . . .
C27 C 0.1715(4) 0.3449(3) -0.1118(4) 0.0508(17) Uani 1 1 d . . . . .
H27 H 0.1605 0.3844 -0.1072 0.061 Uiso 1 1 calc R U . . .
C28 C 0.3882(4) 0.4139(3) 0.3543(5) 0.063(2) Uani 1 1 d . . . . .
H28 H 0.3704 0.4500 0.3715 0.075 Uiso 1 1 calc R U . . .
C29 C 0.3545(5) 0.3629(4) 0.3829(5) 0.077(2) Uani 1 1 d . . . . .
H29 H 0.3140 0.3649 0.4173 0.093 Uiso 1 1 calc R U . . .
C30 C 0.3817(5) 0.3110(4) 0.3596(5) 0.078(3) Uani 1 1 d . . . . .
H30 H 0.3603 0.2770 0.3797 0.094 Uiso 1 1 calc R U . . .
C31 C 0.4413(4) 0.3061(3) 0.3062(5) 0.059(2) Uani 1 1 d . . . . .
C32 C 0.4702(3) 0.3595(3) 0.2793(4) 0.0405(15) Uani 1 1 d . . . . .
C33 C 0.4723(4) 0.2528(3) 0.2770(5) 0.070(3) Uani 1 1 d . . . . .
H33 H 0.4537 0.2175 0.2957 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 O5 1.956(4) 5_565 ?
Zn1 O1 1.977(4) . ?
Zn1 N2 2.075(4) . ?
Zn1 N1 2.094(4) . ?
Zn2 N3 2.096(5) 2_655 ?
Zn2 N3 2.096(5) . ?
Zn2 O7 2.158(4) 2_655 ?
Zn2 O7 2.158(4) . ?
Zn2 O6 2.194(4) 2_655 ?
Zn2 O6 2.194(4) . ?
Zn2 C15 2.476(6) 2_655 ?
N1 C16 1.317(7) . ?
N1 C20 1.345(6) . ?
N2 C27 1.317(7) . ?
N2 C24 1.365(6) . ?
N3 C28 1.325(7) . ?
N3 C32 1.355(7) . ?
O1 C1 1.299(6) . ?
O2 C1 1.228(6) . ?
O3 C7 1.397(6) . ?
O3 C8 1.398(6) . ?
O4 C11 1.246(7) . ?
O5 C11 1.259(7) . ?
O5 Zn1 1.956(4) 5_565 ?
O6 C15 1.236(7) . ?
O7 C15 1.242(6) . ?
O8 H1W 0.8490 . ?
O8 H2W 0.8506 . ?
O9 H3W 0.8502 . ?
O9 H4W 0.8502 . ?
C1 C2 1.507(7) . ?
C2 C3 1.382(7) . ?
C2 C7 1.391(7) . ?
C3 C4 1.364(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.381(8) . ?
C4 H4 0.9300 . ?
C5 C6 1.384(8) . ?
C5 H5 0.9300 . ?
C6 C7 1.386(7) . ?
C6 H6 0.9300 . ?
C8 C9 1.375(7) . ?
C8 C14 1.381(6) . ?
C9 C10 1.383(7) . ?
C9 H9 0.9300 . ?
C10 C12 1.385(7) . ?
C10 C11 1.506(7) . ?
C12 C13 1.373(7) . ?
C12 H12 0.9300 . ?
C13 C14 1.392(7) . ?
C13 H13 0.9300 . ?
C14 C15 1.527(7) . ?
C16 C17 1.400(9) . ?
C16 H16 0.9300 . ?
C17 C18 1.358(10) . ?
C17 H17 0.9300 . ?
C18 C19 1.387(9) . ?
C18 H18 0.9300 . ?
C19 C20 1.408(7) . ?
C19 C21 1.439(9) . ?
C20 C24 1.438(7) . ?
C21 C22 1.346(9) . ?
C21 H21 0.9300 . ?
C22 C23 1.424(8) . ?
C22 H22 0.9300 . ?
C23 C24 1.392(7) . ?
C23 C25 1.398(8) . ?
C25 C26 1.373(9) . ?
C25 H25 0.9300 . ?
C26 C27 1.383(8) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
C28 C29 1.403(9) . ?
C28 H28 0.9300 . ?
C29 C30 1.344(10) . ?
C29 H29 0.9300 . ?
C30 C31 1.400(10) . ?
C30 H30 0.9300 . ?
C31 C32 1.404(8) . ?
C31 C33 1.427(9) . ?
C32 C32 1.447(11) 2_655 ?
C33 C33 1.341(14) 2_655 ?
C33 H33 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
O5 Zn1 O1 116.43(16) 5_565 . ?
O5 Zn1 N2 106.61(18) 5_565 . ?
O1 Zn1 N2 124.99(16) . . ?
O5 Zn1 N1 121.75(17) 5_565 . ?
O1 Zn1 N1 103.12(16) . . ?
N2 Zn1 N1 79.70(18) . . ?
N3 Zn2 N3 79.1(3) 2_655 . ?
N3 Zn2 O7 103.78(17) 2_655 2_655 ?
N3 Zn2 O7 102.77(18) . 2_655 ?
N3 Zn2 O7 102.77(18) 2_655 . ?
N3 Zn2 O7 103.78(17) . . ?
O7 Zn2 O7 145.3(2) 2_655 . ?
N3 Zn2 O6 91.02(18) 2_655 2_655 ?
N3 Zn2 O6 157.78(17) . 2_655 ?
O7 Zn2 O6 60.00(15) 2_655 2_655 ?
O7 Zn2 O6 97.78(16) . 2_655 ?
N3 Zn2 O6 157.78(17) 2_655 . ?
N3 Zn2 O6 91.02(18) . . ?
O7 Zn2 O6 97.78(16) 2_655 . ?
O7 Zn2 O6 60.00(15) . . ?
O6 Zn2 O6 104.5(2) 2_655 . ?
N3 Zn2 C15 97.68(18) 2_655 2_655 ?
N3 Zn2 C15 131.3(2) . 2_655 ?
O7 Zn2 C15 30.11(16) 2_655 2_655 ?
O7 Zn2 C15 123.96(18) . 2_655 ?
O6 Zn2 C15 29.92(16) 2_655 2_655 ?
O6 Zn2 C15 103.72(16) . 2_655 ?
C16 N1 C20 118.8(5) . . ?
C16 N1 Zn1 128.5(4) . . ?
C20 N1 Zn1 112.7(4) . . ?
C27 N2 C24 117.7(5) . . ?
C27 N2 Zn1 128.9(4) . . ?
C24 N2 Zn1 113.4(4) . . ?
C28 N3 C32 118.4(5) . . ?
C28 N3 Zn2 128.0(5) . . ?
C32 N3 Zn2 113.6(4) . . ?
C1 O1 Zn1 102.5(3) . . ?
C7 O3 C8 115.0(4) . . ?
C11 O5 Zn1 110.5(4) . 5_565 ?
C15 O6 Zn2 87.8(4) . . ?
C15 O7 Zn2 89.2(4) . . ?
H1W O8 H2W 120.2 . . ?
H3W O9 H4W 142.1 . . ?
O2 C1 O1 121.2(5) . . ?
O2 C1 C2 123.7(5) . . ?
O1 C1 C2 115.2(5) . . ?
C3 C2 C7 117.2(5) . . ?
C3 C2 C1 120.0(5) . . ?
C7 C2 C1 122.8(5) . . ?
C4 C3 C2 122.6(5) . . ?
C4 C3 H3 118.7 . . ?
C2 C3 H3 118.7 . . ?
C3 C4 C5 119.6(6) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 H4 120.2 . . ?
C4 C5 C6 119.4(6) . . ?
C4 C5 H5 120.3 . . ?
C6 C5 H5 120.3 . . ?
C5 C6 C7 119.9(6) . . ?
C5 C6 H6 120.0 . . ?
C7 C6 H6 120.0 . . ?
C6 C7 C2 121.0(5) . . ?
C6 C7 O3 118.2(5) . . ?
C2 C7 O3 120.6(5) . . ?
C9 C8 C14 121.6(5) . . ?
C9 C8 O3 121.4(5) . . ?
C14 C8 O3 117.0(4) . . ?
C8 C9 C10 119.1(5) . . ?
C8 C9 H9 120.4 . . ?
C10 C9 H9 120.4 . . ?
C9 C10 C12 119.6(5) . . ?
C9 C10 C11 119.9(5) . . ?
C12 C10 C11 120.4(5) . . ?
O4 C11 O5 123.7(6) . . ?
O4 C11 C10 119.1(6) . . ?
O5 C11 C10 117.2(5) . . ?
C13 C12 C10 121.1(5) . . ?
C13 C12 H12 119.5 . . ?
C10 C12 H12 119.5 . . ?
C12 C13 C14 119.4(5) . . ?
C12 C13 H13 120.3 . . ?
C14 C13 H13 120.3 . . ?
C8 C14 C13 119.1(5) . . ?
C8 C14 C15 119.2(5) . . ?
C13 C14 C15 121.7(5) . . ?
O6 C15 O7 122.9(6) . . ?
O6 C15 C14 117.8(5) . . ?
O7 C15 C14 119.3(6) . . ?
N1 C16 C17 121.2(7) . . ?
N1 C16 H16 119.4 . . ?
C17 C16 H16 119.4 . . ?
C18 C17 C16 120.3(7) . . ?
C18 C17 H17 119.9 . . ?
C16 C17 H17 119.9 . . ?
C17 C18 C19 120.0(7) . . ?
C17 C18 H18 120.0 . . ?
C19 C18 H18 120.0 . . ?
C18 C19 C20 116.2(6) . . ?
C18 C19 C21 125.8(7) . . ?
C20 C19 C21 118.0(6) . . ?
N1 C20 C19 123.5(6) . . ?
N1 C20 C24 117.8(5) . . ?
C19 C20 C24 118.6(6) . . ?
C22 C21 C19 123.4(6) . . ?
C22 C21 H21 118.3 . . ?
C19 C21 H21 118.3 . . ?
C21 C22 C23 119.1(6) . . ?
C21 C22 H22 120.5 . . ?
C23 C22 H22 120.5 . . ?
C24 C23 C25 118.1(6) . . ?
C24 C23 C22 119.9(6) . . ?
C25 C23 C22 122.0(6) . . ?
N2 C24 C23 122.6(6) . . ?
N2 C24 C20 116.3(5) . . ?
C23 C24 C20 121.0(5) . . ?
C26 C25 C23 118.7(6) . . ?
C26 C25 H25 120.7 . . ?
C23 C25 H25 120.7 . . ?
C25 C26 C27 119.6(7) . . ?
C25 C26 H26 120.2 . . ?
C27 C26 H26 120.2 . . ?
N2 C27 C26 123.4(6) . . ?
N2 C27 H27 118.3 . . ?
C26 C27 H27 118.3 . . ?
N3 C28 C29 121.9(7) . . ?
N3 C28 H28 119.0 . . ?
C29 C28 H28 119.0 . . ?
C30 C29 C28 118.7(7) . . ?
C30 C29 H29 120.7 . . ?
C28 C29 H29 120.7 . . ?
C29 C30 C31 122.4(7) . . ?
C29 C30 H30 118.8 . . ?
C31 C30 H30 118.8 . . ?
C30 C31 C32 114.8(7) . . ?
C30 C31 C33 125.8(7) . . ?
C32 C31 C33 119.4(7) . . ?
N3 C32 C31 123.8(6) . . ?
N3 C32 C32 116.8(3) . 2_655 ?
C31 C32 C32 119.3(4) . 2_655 ?
C33 C33 C31 121.2(4) 2_655 . ?
C33 C33 H33 119.4 2_655 . ?
C31 C33 H33 119.4 . . ?

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 -1.7(6) . . . . ?
Zn1 O1 C1 C2 177.5(4) . . . . ?
O2 C1 C2 C3 151.3(5) . . . . ?
O1 C1 C2 C3 -27.8(7) . . . . ?
O2 C1 C2 C7 -26.7(8) . . . . ?
O1 C1 C2 C7 154.2(5) . . . . ?
C7 C2 C3 C4 3.1(9) . . . . ?
C1 C2 C3 C4 -174.9(5) . . . . ?
C2 C3 C4 C5 -6.3(10) . . . . ?
C3 C4 C5 C6 4.3(10) . . . . ?
C4 C5 C6 C7 0.6(9) . . . . ?
C5 C6 C7 C2 -3.7(9) . . . . ?
C5 C6 C7 O3 -178.4(5) . . . . ?
C3 C2 C7 C6 1.9(8) . . . . ?
C1 C2 C7 C6 179.9(5) . . . . ?
C3 C2 C7 O3 176.5(5) . . . . ?
C1 C2 C7 O3 -5.5(8) . . . . ?
C8 O3 C7 C6 -61.1(6) . . . . ?
C8 O3 C7 C2 124.1(5) . . . . ?
C7 O3 C8 C9 -54.6(6) . . . . ?
C7 O3 C8 C14 127.6(5) . . . . ?
C14 C8 C9 C10 2.4(8) . . . . ?
O3 C8 C9 C10 -175.3(4) . . . . ?
C8 C9 C10 C12 -3.2(8) . . . . ?
C8 C9 C10 C11 173.8(5) . . . . ?
Zn1 O5 C11 O4 6.4(7) 5_565 . . . ?
Zn1 O5 C11 C10 -172.7(3) 5_565 . . . ?
C9 C10 C11 O4 -162.4(5) . . . . ?
C12 C10 C11 O4 14.6(8) . . . . ?
C9 C10 C11 O5 16.6(8) . . . . ?
C12 C10 C11 O5 -166.3(5) . . . . ?
C9 C10 C12 C13 1.2(8) . . . . ?
C11 C10 C12 C13 -175.8(5) . . . . ?
C10 C12 C13 C14 1.7(9) . . . . ?
C9 C8 C14 C13 0.5(8) . . . . ?
O3 C8 C14 C13 178.3(5) . . . . ?
C9 C8 C14 C15 178.0(5) . . . . ?
O3 C8 C14 C15 -4.2(7) . . . . ?
C12 C13 C14 C8 -2.5(8) . . . . ?
C12 C13 C14 C15 -179.9(5) . . . . ?
Zn2 O6 C15 O7 -3.0(6) . . . . ?
Zn2 O6 C15 C14 178.6(4) . . . . ?
Zn2 O7 C15 O6 3.0(6) . . . . ?
Zn2 O7 C15 C14 -178.6(4) . . . . ?
C8 C14 C15 O6 -86.0(7) . . . . ?
C13 C14 C15 O6 91.5(7) . . . . ?
C8 C14 C15 O7 95.5(6) . . . . ?
C13 C14 C15 O7 -87.0(7) . . . . ?
C20 N1 C16 C17 -1.4(9) . . . . ?
Zn1 N1 C16 C17 176.6(5) . . . . ?
N1 C16 C17 C18 1.4(11) . . . . ?
C16 C17 C18 C19 -0.8(12) . . . . ?
C17 C18 C19 C20 0.3(10) . . . . ?
C17 C18 C19 C21 -179.8(7) . . . . ?
C16 N1 C20 C19 0.9(8) . . . . ?
Zn1 N1 C20 C19 -177.4(4) . . . . ?
C16 N1 C20 C24 -178.6(5) . . . . ?
Zn1 N1 C20 C24 3.1(6) . . . . ?
C18 C19 C20 N1 -0.3(9) . . . . ?
C21 C19 C20 N1 179.8(5) . . . . ?
C18 C19 C20 C24 179.2(5) . . . . ?
C21 C19 C20 C24 -0.7(8) . . . . ?
C18 C19 C21 C22 -178.4(7) . . . . ?
C20 C19 C21 C22 1.5(10) . . . . ?
C19 C21 C22 C23 -1.9(11) . . . . ?
C21 C22 C23 C24 1.4(9) . . . . ?
C21 C22 C23 C25 -178.0(6) . . . . ?
C27 N2 C24 C23 0.5(8) . . . . ?
Zn1 N2 C24 C23 177.7(4) . . . . ?
C27 N2 C24 C20 -177.9(5) . . . . ?
Zn1 N2 C24 C20 -0.7(6) . . . . ?
C25 C23 C24 N2 0.4(8) . . . . ?
C22 C23 C24 N2 -179.0(5) . . . . ?
C25 C23 C24 C20 178.7(5) . . . . ?
C22 C23 C24 C20 -0.7(8) . . . . ?
N1 C20 C24 N2 -1.6(7) . . . . ?
C19 C20 C24 N2 178.8(5) . . . . ?
N1 C20 C24 C23 180.0(5) . . . . ?
C19 C20 C24 C23 0.4(8) . . . . ?
C24 C23 C25 C26 -0.8(9) . . . . ?
C22 C23 C25 C26 178.7(6) . . . . ?
C23 C25 C26 C27 0.3(10) . . . . ?
C24 N2 C27 C26 -1.1(9) . . . . ?
Zn1 N2 C27 C26 -177.7(5) . . . . ?
C25 C26 C27 N2 0.7(10) . . . . ?
C32 N3 C28 C29 -0.1(10) . . . . ?
Zn2 N3 C28 C29 177.6(5) . . . . ?
N3 C28 C29 C30 1.5(12) . . . . ?
C28 C29 C30 C31 -1.5(12) . . . . ?
C29 C30 C31 C32 0.2(11) . . . . ?
C29 C30 C31 C33 -178.6(7) . . . . ?
C28 N3 C32 C31 -1.3(9) . . . . ?
Zn2 N3 C32 C31 -179.4(4) . . . . ?
C28 N3 C32 C32 177.5(6) . . . 2_655 ?
Zn2 N3 C32 C32 -0.5(8) . . . 2_655 ?
C30 C31 C32 N3 1.3(9) . . . . ?
C33 C31 C32 N3 -179.8(6) . . . . ?
C30 C31 C32 C32 -177.5(6) . . . 2_655 ?
C33 C31 C32 C32 1.4(10) . . . 2_655 ?
C30 C31 C33 C33 177.6(8) . . . 2_655 ?
C32 C31 C33 C33 -1.1(12) . . . 2_655 ?

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
O8 H1W O1 0.85 2.06 2.908(6) 179.6 6_566
O8 H2W O4 0.85 1.97 2.824(7) 179.1 1_556

_refine_diff_density_max         0.544
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.087


# 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_282-3Cd
_database_code_depnum_ccdc_archive 'CCDC 1509370'
_audit_update_record             
;
2017-03-26 deposited with the CCDC.
2017-04-10 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            'C66 H42 Cd3 N6 O16'
_chemical_formula_weight         1512.25

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           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                   22.5877(5)
_cell_length_b                   10.2617(2)
_cell_length_c                   24.0631(5)
_cell_angle_alpha                90
_cell_angle_beta                 95.087(2)
_cell_angle_gamma                90
_cell_volume                     5555.6(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9327
_cell_measurement_theta_min      3.365
_cell_measurement_theta_max      25.044

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.808
_exptl_crystal_F_000             3008
_exptl_transmission_factor_min   0.718
_exptl_transmission_factor_max   0.737
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.250
_exptl_absorpt_coefficient_mu    1.221
_shelx_estimated_absorpt_T_min   0.726
_shelx_estimated_absorpt_T_max   0.750
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.726
_exptl_absorpt_correction_T_max  0.750
_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            9327
_diffrn_reflns_av_unetI/netI     0.0498
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.365
_diffrn_reflns_theta_max         25.044
_diffrn_reflns_theta_full        25.044
_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             4915
_reflns_number_gt                3930
_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)+(0.0143P)²+6.8253P] 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         4915
_refine_ls_number_parameters     411
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0330
_refine_ls_wR_factor_ref         0.0655
_refine_ls_wR_factor_gt          0.0571
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.004
_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 1.0000 0.45725(4) 0.2500 0.02824(11) Uani 1 2 d S T P . .
Cd2 Cd 1.08262(2) 0.31700(3) 0.10884(2) 0.02906(9) Uani 1 1 d . . . . .
N1 N 1.02531(14) 0.1251(3) 0.09373(13) 0.0376(8) Uani 1 1 d . . . . .
N2 N 1.14118(15) 0.1484(4) 0.07422(13) 0.0404(9) Uani 1 1 d . . . . .
N3 N 1.05146(13) 0.6440(3) 0.22484(13) 0.0330(8) Uani 1 1 d . . . . .
O1 O 1.00687(10) 0.4182(3) 0.15025(10) 0.0361(7) Uani 1 1 d . . . . .
O2 O 0.97311(12) 0.4418(3) 0.06219(11) 0.0525(8) Uani 1 1 d . . . . .
O3 O 0.86330(10) 0.3209(3) 0.12895(11) 0.0341(6) Uani 1 1 d . . . . .
O4 O 0.66713(12) -0.0663(3) 0.13009(11) 0.0484(8) Uani 1 1 d . . . . .
O5 O 0.69452(11) 0.0376(3) 0.05529(11) 0.0473(8) Uani 1 1 d . . . . .
O6 O 0.88315(12) 0.2367(3) 0.30292(12) 0.0504(8) Uani 1 1 d . . . . .
O7 O 0.92135(13) 0.3357(3) 0.23274(13) 0.0637(10) Uani 1 1 d . . . . .
O8 O 1.09434(11) 0.4019(3) 0.01991(11) 0.0470(8) Uani 1 1 d . . . . .
H2W H 1.0741 0.4470 -0.0046 0.056 Uiso 1 1 d R U . . .
H1W H 1.1257 0.4438 0.0309 0.056 Uiso 1 1 d R U . . .
C1 C 0.96770(15) 0.4564(4) 0.11242(16) 0.0286(9) Uani 1 1 d . . . . .
C2 C 0.91336(15) 0.5217(4) 0.13098(14) 0.0259(8) Uani 1 1 d . . . . .
C3 C 0.91330(17) 0.6551(4) 0.13959(15) 0.0335(9) Uani 1 1 d . . . . .
H3 H 0.9468 0.7033 0.1331 0.040 Uiso 1 1 calc R U . . .
C4 C 0.86434(18) 0.7179(4) 0.15767(17) 0.0423(11) Uani 1 1 d . . . . .
H4 H 0.8649 0.8078 0.1627 0.051 Uiso 1 1 calc R U . . .
C5 C 0.81483(19) 0.6473(5) 0.16822(18) 0.0474(12) Uani 1 1 d . . . . .
H5 H 0.7820 0.6893 0.1807 0.057 Uiso 1 1 calc R U . . .
C6 C 0.81378(16) 0.5138(4) 0.16032(16) 0.0371(10) Uani 1 1 d . . . . .
H6 H 0.7804 0.4660 0.1677 0.045 Uiso 1 1 calc R U . . .
C7 C 0.86233(15) 0.4520(4) 0.14154(15) 0.0288(9) Uani 1 1 d . . . . .
C8 C 0.82748(14) 0.2347(4) 0.15618(15) 0.0286(9) Uani 1 1 d . . . . .
C9 C 0.78430(15) 0.1710(4) 0.12187(15) 0.0320(9) Uani 1 1 d . . . . .
H9 H 0.7789 0.1930 0.0843 0.038 Uiso 1 1 calc R U . . .
C10 C 0.74909(15) 0.0753(4) 0.14261(16) 0.0314(9) Uani 1 1 d . . . . .
C11 C 0.69985(16) 0.0105(4) 0.10550(17) 0.0330(9) Uani 1 1 d . . . . .
C12 C 0.75781(16) 0.0444(4) 0.19912(16) 0.0382(10) Uani 1 1 d . . . . .
H12 H 0.7350 -0.0201 0.2140 0.046 Uiso 1 1 calc R U . . .
C13 C 0.80050(15) 0.1101(4) 0.23286(16) 0.0343(10) Uani 1 1 d . . . . .
H13 H 0.8054 0.0895 0.2706 0.041 Uiso 1 1 calc R U . . .
C14 C 0.83654(15) 0.2059(4) 0.21273(15) 0.0293(9) Uani 1 1 d . . . . .
C15 C 0.88380(16) 0.2669(4) 0.25326(17) 0.0312(9) Uani 1 1 d . . . . .
C16 C 0.96813(19) 0.1139(5) 0.10238(18) 0.0500(12) Uani 1 1 d . . . . .
H16 H 0.9499 0.1827 0.1193 0.060 Uiso 1 1 calc R U . . .
C17 C 0.9344(2) 0.0036(5) 0.0872(2) 0.0624(14) Uani 1 1 d . . . . .
H17 H 0.8942 0.0002 0.0929 0.075 Uiso 1 1 calc R U . . .
C18 C 0.9610(3) -0.0981(5) 0.0641(2) 0.0663(16) Uani 1 1 d . . . . .
H18 H 0.9387 -0.1711 0.0526 0.080 Uiso 1 1 calc R U . . .
C19 C 1.0219(3) -0.0947(4) 0.05736(17) 0.0538(13) Uani 1 1 d . . . . .
C20 C 1.0521(2) 0.0211(4) 0.07210(16) 0.0409(11) Uani 1 1 d . . . . .
C21 C 1.0532(3) -0.2008(5) 0.0355(2) 0.0779(19) Uani 1 1 d . . . . .
H21 H 1.0331 -0.2779 0.0260 0.093 Uiso 1 1 calc R U . . .
C22 C 1.1113(3) -0.1909(5) 0.0286(2) 0.081(2) Uani 1 1 d . . . . .
H22 H 1.1311 -0.2625 0.0155 0.097 Uiso 1 1 calc R U . . .
C23 C 1.1433(3) -0.0739(5) 0.04070(18) 0.0586(14) Uani 1 1 d . . . . .
C24 C 1.1141(2) 0.0333(4) 0.06259(16) 0.0456(12) Uani 1 1 d . . . . .
C25 C 1.2028(3) -0.0552(6) 0.03052(19) 0.0715(18) Uani 1 1 d . . . . .
H25 H 1.2240 -0.1234 0.0163 0.086 Uiso 1 1 calc R U . . .
C26 C 1.2300(2) 0.0609(7) 0.0411(2) 0.0719(17) Uani 1 1 d . . . . .
H26 H 1.2693 0.0736 0.0337 0.086 Uiso 1 1 calc R U . . .
C27 C 1.1976(2) 0.1608(5) 0.06334(18) 0.0562(13) Uani 1 1 d . . . . .
H27 H 1.2164 0.2403 0.0709 0.067 Uiso 1 1 calc R U . . .
C28 C 1.10097(18) 0.6442(5) 0.19927(18) 0.0475(11) Uani 1 1 d . . . . .
H28 H 1.1187 0.5648 0.1923 0.057 Uiso 1 1 calc R U . . .
C29 C 1.1277(2) 0.7588(5) 0.18236(19) 0.0551(13) Uani 1 1 d . . . . .
H29 H 1.1622 0.7549 0.1640 0.066 Uiso 1 1 calc R U . . .
C30 C 1.10297(19) 0.8756(5) 0.19286(17) 0.0467(12) Uani 1 1 d . . . . .
H30 H 1.1202 0.9523 0.1815 0.056 Uiso 1 1 calc R U . . .
C31 C 1.05100(18) 0.8802(4) 0.22113(16) 0.0394(10) Uani 1 1 d . . . . .
C32 C 1.02406(18) 0.9979(4) 0.23555(19) 0.0510(13) Uani 1 1 d . . . . .
H32 H 1.0399 1.0768 0.2249 0.061 Uiso 1 1 calc R U . . .
C33 C 1.02696(15) 0.7606(4) 0.23594(15) 0.0308(9) 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
Cd1 O7 2.180(3) . ?
Cd1 O7 2.180(3) 2_755 ?
Cd1 N3 2.349(3) . ?
Cd1 N3 2.349(3) 2_755 ?
Cd1 O1 2.452(2) . ?
Cd1 O1 2.452(2) 2_755 ?
Cd2 O4 2.273(3) 3 ?
Cd2 O1 2.302(2) . ?
Cd2 O6 2.344(3) 2_755 ?
Cd2 O8 2.347(3) . ?
Cd2 N1 2.367(3) . ?
Cd2 N2 2.373(3) . ?
N1 C16 1.331(5) . ?
N1 C20 1.354(5) . ?
N2 C27 1.329(5) . ?
N2 C24 1.348(5) . ?
N3 C28 1.323(5) . ?
N3 C33 1.354(5) . ?
O1 C1 1.274(4) . ?
O2 C1 1.235(4) . ?
O3 C7 1.379(4) . ?
O3 C8 1.401(4) . ?
O4 C11 1.263(4) . ?
O4 Cd2 2.273(3) 3_445 ?
O5 C11 1.235(4) . ?
O6 C15 1.236(4) . ?
O6 Cd2 2.344(3) 2_755 ?
O7 C15 1.239(5) . ?
O8 H2W 0.8504 . ?
O8 H1W 0.8501 . ?
C1 C2 1.501(5) . ?
C2 C3 1.384(5) . ?
C2 C7 1.399(5) . ?
C3 C4 1.384(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.375(6) . ?
C4 H4 0.9300 . ?
C5 C6 1.382(6) . ?
C5 H5 0.9300 . ?
C6 C7 1.377(5) . ?
C6 H6 0.9300 . ?
C8 C9 1.384(5) . ?
C8 C14 1.390(5) . ?
C9 C10 1.385(5) . ?
C9 H9 0.9300 . ?
C10 C12 1.393(5) . ?
C10 C11 1.517(5) . ?
C12 C13 1.380(5) . ?
C12 H12 0.9300 . ?
C13 C14 1.390(5) . ?
C13 H13 0.9300 . ?
C14 C15 1.516(5) . ?
C16 C17 1.395(6) . ?
C16 H16 0.9300 . ?
C17 C18 1.348(7) . ?
C17 H17 0.9300 . ?
C18 C19 1.401(7) . ?
C18 H18 0.9300 . ?
C19 C20 1.401(6) . ?
C19 C21 1.423(7) . ?
C20 C24 1.443(6) . ?
C21 C22 1.342(7) . ?
C21 H21 0.9300 . ?
C22 C23 1.417(7) . ?
C22 H22 0.9300 . ?
C23 C25 1.402(7) . ?
C23 C24 1.408(6) . ?
C25 C26 1.354(7) . ?
C25 H25 0.9300 . ?
C26 C27 1.395(6) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
C28 C29 1.399(6) . ?
C28 H28 0.9300 . ?
C29 C30 1.356(6) . ?
C29 H29 0.9300 . ?
C30 C31 1.409(6) . ?
C30 H30 0.9300 . ?
C31 C33 1.401(5) . ?
C31 C32 1.410(5) . ?
C32 C32 1.341(9) 2_755 ?
C32 H32 0.9300 . ?
C33 C33 1.445(7) 2_755 ?

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 O7 110.22(18) . 2_755 ?
O7 Cd1 N3 146.23(10) . . ?
O7 Cd1 N3 95.88(12) 2_755 . ?
O7 Cd1 N3 95.88(12) . 2_755 ?
O7 Cd1 N3 146.23(10) 2_755 2_755 ?
N3 Cd1 N3 70.61(15) . 2_755 ?
O7 Cd1 O1 80.86(11) . . ?
O7 Cd1 O1 88.38(10) 2_755 . ?
N3 Cd1 O1 78.78(10) . . ?
N3 Cd1 O1 117.49(9) 2_755 . ?
O7 Cd1 O1 88.38(10) . 2_755 ?
O7 Cd1 O1 80.86(11) 2_755 2_755 ?
N3 Cd1 O1 117.49(9) . 2_755 ?
N3 Cd1 O1 78.78(10) 2_755 2_755 ?
O1 Cd1 O1 161.17(13) . 2_755 ?
O4 Cd2 O1 107.86(10) 3 . ?
O4 Cd2 O6 77.20(10) 3 2_755 ?
O1 Cd2 O6 87.97(9) . 2_755 ?
O4 Cd2 O8 81.33(9) 3 . ?
O1 Cd2 O8 112.06(9) . . ?
O6 Cd2 O8 154.37(9) 2_755 . ?
O4 Cd2 N1 155.48(11) 3 . ?
O1 Cd2 N1 91.38(11) . . ?
O6 Cd2 N1 88.77(11) 2_755 . ?
O8 Cd2 N1 105.85(10) . . ?
O4 Cd2 N2 88.84(11) 3 . ?
O1 Cd2 N2 159.94(11) . . ?
O6 Cd2 N2 84.97(11) 2_755 . ?
O8 Cd2 N2 80.74(11) . . ?
N1 Cd2 N2 69.75(12) . . ?
C16 N1 C20 117.7(4) . . ?
C16 N1 Cd2 125.0(3) . . ?
C20 N1 Cd2 117.2(3) . . ?
C27 N2 C24 117.9(4) . . ?
C27 N2 Cd2 125.0(3) . . ?
C24 N2 Cd2 117.1(3) . . ?
C28 N3 C33 117.9(4) . . ?
C28 N3 Cd1 125.4(3) . . ?
C33 N3 Cd1 116.7(2) . . ?
C1 O1 Cd2 109.0(2) . . ?
C1 O1 Cd1 123.3(2) . . ?
Cd2 O1 Cd1 127.70(10) . . ?
C7 O3 C8 119.5(3) . . ?
C11 O4 Cd2 137.6(3) . 3_445 ?
C15 O6 Cd2 139.1(3) . 2_755 ?
C15 O7 Cd1 145.6(3) . . ?
Cd2 O8 H2W 137.4 . . ?
Cd2 O8 H1W 93.6 . . ?
H2W O8 H1W 108.8 . . ?
O2 C1 O1 122.6(4) . . ?
O2 C1 C2 120.0(3) . . ?
O1 C1 C2 117.4(3) . . ?
C3 C2 C7 117.8(3) . . ?
C3 C2 C1 119.8(3) . . ?
C7 C2 C1 122.3(3) . . ?
C4 C3 C2 121.3(4) . . ?
C4 C3 H3 119.3 . . ?
C2 C3 H3 119.3 . . ?
C5 C4 C3 119.9(4) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C4 C5 C6 120.1(4) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C7 C6 C5 119.8(4) . . ?
C7 C6 H6 120.1 . . ?
C5 C6 H6 120.1 . . ?
C6 C7 O3 123.4(3) . . ?
C6 C7 C2 121.1(4) . . ?
O3 C7 C2 115.4(3) . . ?
C9 C8 C14 121.3(3) . . ?
C9 C8 O3 115.1(3) . . ?
C14 C8 O3 123.4(3) . . ?
C8 C9 C10 121.1(3) . . ?
C8 C9 H9 119.4 . . ?
C10 C9 H9 119.4 . . ?
C9 C10 C12 118.5(3) . . ?
C9 C10 C11 120.9(3) . . ?
C12 C10 C11 120.5(3) . . ?
O5 C11 O4 126.0(3) . . ?
O5 C11 C10 118.7(3) . . ?
O4 C11 C10 115.3(3) . . ?
C13 C12 C10 119.6(4) . . ?
C13 C12 H12 120.2 . . ?
C10 C12 H12 120.2 . . ?
C12 C13 C14 122.7(4) . . ?
C12 C13 H13 118.6 . . ?
C14 C13 H13 118.6 . . ?
C8 C14 C13 116.8(3) . . ?
C8 C14 C15 125.2(3) . . ?
C13 C14 C15 117.9(3) . . ?
O6 C15 O7 126.6(4) . . ?
O6 C15 C14 116.8(4) . . ?
O7 C15 C14 116.5(4) . . ?
N1 C16 C17 123.0(5) . . ?
N1 C16 H16 118.5 . . ?
C17 C16 H16 118.5 . . ?
C18 C17 C16 118.9(5) . . ?
C18 C17 H17 120.6 . . ?
C16 C17 H17 120.6 . . ?
C17 C18 C19 120.5(5) . . ?
C17 C18 H18 119.8 . . ?
C19 C18 H18 119.8 . . ?
C18 C19 C20 117.0(5) . . ?
C18 C19 C21 123.3(5) . . ?
C20 C19 C21 119.7(5) . . ?
N1 C20 C19 122.8(4) . . ?
N1 C20 C24 117.8(4) . . ?
C19 C20 C24 119.4(4) . . ?
C22 C21 C19 120.7(5) . . ?
C22 C21 H21 119.6 . . ?
C19 C21 H21 119.6 . . ?
C21 C22 C23 121.7(6) . . ?
C21 C22 H22 119.2 . . ?
C23 C22 H22 119.2 . . ?
C25 C23 C24 116.5(5) . . ?
C25 C23 C22 124.0(5) . . ?
C24 C23 C22 119.4(5) . . ?
N2 C24 C23 122.9(5) . . ?
N2 C24 C20 118.1(4) . . ?
C23 C24 C20 119.0(5) . . ?
C26 C25 C23 121.0(5) . . ?
C26 C25 H25 119.5 . . ?
C23 C25 H25 119.5 . . ?
C25 C26 C27 118.3(5) . . ?
C25 C26 H26 120.9 . . ?
C27 C26 H26 120.9 . . ?
N2 C27 C26 123.4(5) . . ?
N2 C27 H27 118.3 . . ?
C26 C27 H27 118.3 . . ?
N3 C28 C29 122.7(4) . . ?
N3 C28 H28 118.6 . . ?
C29 C28 H28 118.6 . . ?
C30 C29 C28 119.6(4) . . ?
C30 C29 H29 120.2 . . ?
C28 C29 H29 120.2 . . ?
C29 C30 C31 119.7(4) . . ?
C29 C30 H30 120.2 . . ?
C31 C30 H30 120.2 . . ?
C33 C31 C30 116.9(4) . . ?
C33 C31 C32 120.2(4) . . ?
C30 C31 C32 123.0(4) . . ?
C32 C32 C31 121.0(3) 2_755 . ?
C32 C32 H32 119.5 2_755 . ?
C31 C32 H32 119.5 . . ?
N3 C33 C31 123.3(4) . . ?
N3 C33 C33 117.9(2) . 2_755 ?
C31 C33 C33 118.7(2) . 2_755 ?

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
Cd2 O1 C1 O2 -1.9(5) . . . . ?
Cd1 O1 C1 O2 176.3(3) . . . . ?
Cd2 O1 C1 C2 178.2(2) . . . . ?
Cd1 O1 C1 C2 -3.6(4) . . . . ?
O2 C1 C2 C3 -91.5(5) . . . . ?
O1 C1 C2 C3 88.5(4) . . . . ?
O2 C1 C2 C7 90.2(4) . . . . ?
O1 C1 C2 C7 -89.8(4) . . . . ?
C7 C2 C3 C4 -0.4(5) . . . . ?
C1 C2 C3 C4 -178.8(3) . . . . ?
C2 C3 C4 C5 1.0(6) . . . . ?
C3 C4 C5 C6 -0.6(6) . . . . ?
C4 C5 C6 C7 -0.4(6) . . . . ?
C5 C6 C7 O3 -175.4(3) . . . . ?
C5 C6 C7 C2 0.9(6) . . . . ?
C8 O3 C7 C6 -27.8(5) . . . . ?
C8 O3 C7 C2 155.7(3) . . . . ?
C3 C2 C7 C6 -0.5(5) . . . . ?
C1 C2 C7 C6 177.8(3) . . . . ?
C3 C2 C7 O3 176.1(3) . . . . ?
C1 C2 C7 O3 -5.6(5) . . . . ?
C7 O3 C8 C9 117.0(4) . . . . ?
C7 O3 C8 C14 -67.7(5) . . . . ?
C14 C8 C9 C10 -0.8(6) . . . . ?
O3 C8 C9 C10 174.6(3) . . . . ?
C8 C9 C10 C12 0.3(6) . . . . ?
C8 C9 C10 C11 177.0(3) . . . . ?
Cd2 O4 C11 O5 -5.8(7) 3_445 . . . ?
Cd2 O4 C11 C10 173.1(3) 3_445 . . . ?
C9 C10 C11 O5 5.4(6) . . . . ?
C12 C10 C11 O5 -178.0(4) . . . . ?
C9 C10 C11 O4 -173.6(4) . . . . ?
C12 C10 C11 O4 3.0(6) . . . . ?
C9 C10 C12 C13 0.6(6) . . . . ?
C11 C10 C12 C13 -176.1(3) . . . . ?
C10 C12 C13 C14 -1.1(6) . . . . ?
C9 C8 C14 C13 0.4(6) . . . . ?
O3 C8 C14 C13 -174.7(3) . . . . ?
C9 C8 C14 C15 178.0(3) . . . . ?
O3 C8 C14 C15 2.9(6) . . . . ?
C12 C13 C14 C8 0.6(6) . . . . ?
C12 C13 C14 C15 -177.2(4) . . . . ?
Cd2 O6 C15 O7 26.1(7) 2_755 . . . ?
Cd2 O6 C15 C14 -158.7(3) 2_755 . . . ?
Cd1 O7 C15 O6 -5.1(8) . . . . ?
Cd1 O7 C15 C14 179.7(4) . . . . ?
C8 C14 C15 O6 175.3(4) . . . . ?
C13 C14 C15 O6 -7.1(5) . . . . ?
C8 C14 C15 O7 -9.0(6) . . . . ?
C13 C14 C15 O7 168.5(4) . . . . ?
C20 N1 C16 C17 -3.8(6) . . . . ?
Cd2 N1 C16 C17 172.8(3) . . . . ?
N1 C16 C17 C18 1.9(7) . . . . ?
C16 C17 C18 C19 2.2(7) . . . . ?
C17 C18 C19 C20 -4.1(6) . . . . ?
C17 C18 C19 C21 177.2(5) . . . . ?
C16 N1 C20 C19 1.7(6) . . . . ?
Cd2 N1 C20 C19 -175.1(3) . . . . ?
C16 N1 C20 C24 179.9(3) . . . . ?
Cd2 N1 C20 C24 3.0(4) . . . . ?
C18 C19 C20 N1 2.1(6) . . . . ?
C21 C19 C20 N1 -179.1(4) . . . . ?
C18 C19 C20 C24 -176.0(4) . . . . ?
C21 C19 C20 C24 2.8(6) . . . . ?
C18 C19 C21 C22 178.2(5) . . . . ?
C20 C19 C21 C22 -0.4(7) . . . . ?
C19 C21 C22 C23 -2.2(8) . . . . ?
C21 C22 C23 C25 -175.3(5) . . . . ?
C21 C22 C23 C24 2.4(8) . . . . ?
C27 N2 C24 C23 1.4(6) . . . . ?
Cd2 N2 C24 C23 178.6(3) . . . . ?
C27 N2 C24 C20 -177.4(4) . . . . ?
Cd2 N2 C24 C20 -0.2(5) . . . . ?
C25 C23 C24 N2 -0.9(6) . . . . ?
C22 C23 C24 N2 -178.8(4) . . . . ?
C25 C23 C24 C20 177.9(4) . . . . ?
C22 C23 C24 C20 0.0(6) . . . . ?
N1 C20 C24 N2 -1.9(5) . . . . ?
C19 C20 C24 N2 176.3(4) . . . . ?
N1 C20 C24 C23 179.3(4) . . . . ?
C19 C20 C24 C23 -2.5(6) . . . . ?
C24 C23 C25 C26 -0.4(7) . . . . ?
C22 C23 C25 C26 177.4(5) . . . . ?
C23 C25 C26 C27 1.1(7) . . . . ?
C24 N2 C27 C26 -0.6(6) . . . . ?
Cd2 N2 C27 C26 -177.6(3) . . . . ?
C25 C26 C27 N2 -0.6(7) . . . . ?
C33 N3 C28 C29 -1.6(6) . . . . ?
Cd1 N3 C28 C29 176.1(3) . . . . ?
N3 C28 C29 C30 0.9(7) . . . . ?
C28 C29 C30 C31 0.6(7) . . . . ?
C29 C30 C31 C33 -1.3(6) . . . . ?
C29 C30 C31 C32 177.4(4) . . . . ?
C33 C31 C32 C32 1.3(8) . . . 2_755 ?
C30 C31 C32 C32 -177.3(5) . . . 2_755 ?
C28 N3 C33 C31 0.8(6) . . . . ?
Cd1 N3 C33 C31 -177.0(3) . . . . ?
C28 N3 C33 C33 -179.8(4) . . . 2_755 ?
Cd1 N3 C33 C33 2.4(5) . . . 2_755 ?
C30 C31 C33 N3 0.6(6) . . . . ?
C32 C31 C33 N3 -178.1(4) . . . . ?
C30 C31 C33 C33 -178.8(4) . . . 2_755 ?
C32 C31 C33 C33 2.5(6) . . . 2_755 ?

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
O8 H1W O5 0.85 1.88 2.728(4) 179.6 3
O8 H2W O2 0.85 2.02 2.875(4) 178.6 5_765

_refine_diff_density_max         0.683
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.084


# start Validation Reply Form
_vrf_PLAT910_I                   
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min) 10 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_277-6Ni1
_database_code_depnum_ccdc_archive 'CCDC 1509373'
_audit_update_record             
;
2017-03-26 deposited with the CCDC.
2017-04-10 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            'C81 H58 N9 Ni3 O17'
_chemical_formula_weight         1605.49

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      monoclinic
_space_group_IT_number           11
_space_group_name_H-M_alt        'P 21/m'
_space_group_name_Hall           '-P 2yb'

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

_cell_length_a                   9.5810(3)
_cell_length_b                   41.4136(15)
_cell_length_c                   9.8344(4)
_cell_angle_alpha                90
_cell_angle_beta                 98.146(4)
_cell_angle_gamma                90
_cell_volume                     3862.7(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    13736
_cell_measurement_theta_min      3.265
_cell_measurement_theta_max      25.050

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_F_000             1654
_exptl_transmission_factor_min   0.813
_exptl_transmission_factor_max   0.859
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    0.798
_shelx_estimated_absorpt_T_min   0.819
_shelx_estimated_absorpt_T_max   0.863
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.819
_exptl_absorpt_correction_T_max  0.863
_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            13736
_diffrn_reflns_av_unetI/netI     0.0775
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.265
_diffrn_reflns_theta_max         25.050
_diffrn_reflns_theta_full        25.050
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             6929
_reflns_number_gt                4812
_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)+(0.0619P)²+0.1136P] 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         6929
_refine_ls_number_parameters     502
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0816
_refine_ls_R_factor_gt           0.0556
_refine_ls_wR_factor_ref         0.1537
_refine_ls_wR_factor_gt          0.1345
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.039
_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
Ni1 Ni 0.11362(5) 0.06792(2) 0.35841(5) 0.03859(18) Uani 1 1 d . . . . .
Ni2 Ni -0.02383(7) 0.2500 1.17266(7) 0.0366(2) Uani 1 2 d S T P . .
N1 N 0.2778(3) 0.04478(8) 0.4851(3) 0.0411(8) Uani 1 1 d . . . . .
N2 N 0.2825(3) 0.09836(8) 0.3326(3) 0.0428(8) Uani 1 1 d . . . . .
N3 N 0.1429(3) 0.03794(8) 0.1911(3) 0.0447(8) Uani 1 1 d . . . . .
N4 N -0.0573(3) 0.21750(8) 1.3309(3) 0.0396(8) Uani 1 1 d . . . . .
N5 N -0.2372(5) 0.2500 1.0939(5) 0.0438(12) Uani 1 2 d S T P . .
O1 O 0.0933(3) 0.09727(7) 0.5228(3) 0.0490(7) Uani 1 1 d . . . . .
O2 O -0.0032(3) 0.06432(7) 0.6645(3) 0.0540(8) Uani 1 1 d . . . . .
O3 O 0.0012(3) 0.21226(6) 1.0380(3) 0.0411(7) Uani 1 1 d . . . . .
O4 O 0.2295(3) 0.20040(8) 1.0962(4) 0.0729(11) Uani 1 1 d . . . . .
O5 O -0.0818(3) 0.14327(7) 1.0425(3) 0.0531(8) Uani 1 1 d . . . . .
O6 O -0.0382(3) 0.09408(7) 1.2288(3) 0.0494(7) Uani 1 1 d . . . . .
O7 O -0.2219(3) 0.06236(8) 1.2455(3) 0.0615(9) Uani 1 1 d . . . . .
O8 O -0.0315(3) 0.03580(6) 0.4205(3) 0.0459(7) Uani 1 1 d . . . . .
H1W H -0.0946 0.0445 0.3626 0.055 Uiso 1 1 d R U . . .
H2W H -0.0227 0.0449 0.4986 0.055 Uiso 1 1 d R U . . .
O9 O 0.1897(4) 0.2500 1.2542(4) 0.0494(10) Uani 1 2 d S T P . .
H3W H 0.2028 0.2340 1.2031 0.059 Uiso 0.5 1 d R U P . .
C1 C 0.0539(4) 0.09010(10) 0.6365(4) 0.0394(9) Uani 1 1 d . . . . .
C2 C 0.0770(4) 0.11664(10) 0.7430(4) 0.0397(9) Uani 1 1 d . . . . .
C3 C 0.1746(4) 0.14101(10) 0.7361(4) 0.0485(11) Uani 1 1 d . . . . .
H3 H 0.2321 0.1409 0.6674 0.058 Uiso 1 1 calc R U . . .
C4 C 0.1855(4) 0.16552(10) 0.8327(4) 0.0479(11) Uani 1 1 d . . . . .
H4 H 0.2545 0.1812 0.8304 0.057 Uiso 1 1 calc R U . . .
C5 C 0.0979(4) 0.16753(9) 0.9326(4) 0.0373(9) Uani 1 1 d . . . . .
C6 C 0.1109(4) 0.19592(9) 1.0306(4) 0.0377(9) Uani 1 1 d . . . . .
C7 C 0.0005(4) 0.14271(10) 0.9376(4) 0.0386(9) Uani 1 1 d . . . . .
C8 C -0.0079(4) 0.11724(9) 0.8464(4) 0.0402(10) Uani 1 1 d . . . . .
H8 H -0.0706 0.1004 0.8542 0.048 Uiso 1 1 calc R U . . .
C9 C -0.2155(4) 0.12999(10) 1.0118(4) 0.0459(10) Uani 1 1 d . . . . .
C10 C -0.3076(5) 0.14466(12) 0.9076(5) 0.0638(13) Uani 1 1 d . . . . .
H10 H -0.2771 0.1619 0.8590 0.077 Uiso 1 1 calc R U . . .
C11 C -0.4443(5) 0.13349(14) 0.8766(5) 0.0749(16) Uani 1 1 d . . . . .
H11 H -0.5065 0.1434 0.8080 0.090 Uiso 1 1 calc R U . . .
C12 C -0.4880(5) 0.10767(15) 0.9472(5) 0.0789(17) Uani 1 1 d . . . . .
H12A H -0.5790 0.0996 0.9252 0.095 Uiso 1 1 calc R U . . .
C13 C -0.3962(4) 0.09376(12) 1.0507(5) 0.0642(14) Uani 1 1 d . . . . .
H13 H -0.4281 0.0768 1.1002 0.077 Uiso 1 1 calc R U . . .
C14 C -0.2573(4) 0.10402(10) 1.0842(4) 0.0422(10) Uani 1 1 d . . . . .
C15 C -0.1647(4) 0.08556(10) 1.1951(4) 0.0418(10) Uani 1 1 d . . . . .
C16 C 0.2724(4) 0.01858(10) 0.5600(4) 0.0456(10) Uani 1 1 d . . . . .
H16 H 0.1879 0.0072 0.5525 0.055 Uiso 1 1 calc R U . . .
C17 C 0.3869(4) 0.00696(11) 0.6502(4) 0.0549(12) Uani 1 1 d . . . . .
H17 H 0.3793 -0.0119 0.6999 0.066 Uiso 1 1 calc R U . . .
C18 C 0.5090(5) 0.02371(12) 0.6639(5) 0.0594(13) Uani 1 1 d . . . . .
H18 H 0.5863 0.0165 0.7243 0.071 Uiso 1 1 calc R U . . .
C19 C 0.5198(4) 0.05187(11) 0.5876(4) 0.0514(11) Uani 1 1 d . . . . .
C20 C 0.4011(4) 0.06157(10) 0.4977(4) 0.0408(10) Uani 1 1 d . . . . .
C21 C 0.6448(5) 0.07133(13) 0.5939(5) 0.0684(15) Uani 1 1 d . . . . .
H21 H 0.7254 0.0652 0.6522 0.082 Uiso 1 1 calc R U . . .
C22 C 0.6480(5) 0.09790(14) 0.5183(5) 0.0735(15) Uani 1 1 d . . . . .
H22 H 0.7311 0.1097 0.5242 0.088 Uiso 1 1 calc R U . . .
C23 C 0.5263(4) 0.10869(12) 0.4281(5) 0.0580(12) Uani 1 1 d . . . . .
C24 C 0.4024(4) 0.09018(10) 0.4173(4) 0.0441(10) Uani 1 1 d . . . . .
C25 C 0.5211(5) 0.13684(14) 0.3499(6) 0.0809(17) Uani 1 1 d . . . . .
H25 H 0.6006 0.1499 0.3544 0.097 Uiso 1 1 calc R U . . .
C26 C 0.4001(5) 0.14549(12) 0.2667(6) 0.0742(16) Uani 1 1 d . . . . .
H26 H 0.3964 0.1641 0.2136 0.089 Uiso 1 1 calc R U . . .
C27 C 0.2819(5) 0.12547(11) 0.2640(5) 0.0566(12) Uani 1 1 d . . . . .
H27 H 0.1985 0.1318 0.2105 0.068 Uiso 1 1 calc R U . . .
C28 C 0.1830(5) 0.05023(13) 0.0771(5) 0.0687(14) Uani 1 1 d . . . . .
H28 H 0.1905 0.0725 0.0702 0.082 Uiso 1 1 calc R U . . .
C29 C 0.2136(6) 0.03159(16) -0.0303(6) 0.0864(18) Uani 1 1 d . . . . .
H29 H 0.2420 0.0410 -0.1077 0.104 Uiso 1 1 calc R U . . .
C30 C 0.2014(5) -0.00133(15) -0.0206(6) 0.0774(16) Uani 1 1 d . . . . .
H30 H 0.2234 -0.0146 -0.0908 0.093 Uiso 1 1 calc R U . . .
C31 C 0.1567(5) -0.01432(12) 0.0930(5) 0.0652(14) Uani 1 1 d . . . . .
H31 H 0.1456 -0.0365 0.1009 0.078 Uiso 1 1 calc R U . . .
C32 C 0.1281(4) 0.00634(10) 0.1967(4) 0.0495(11) Uani 1 1 d . . . . .
H32 H 0.0970 -0.0025 0.2739 0.059 Uiso 1 1 calc R U . . .
C33 C -0.0540(4) 0.18576(10) 1.3305(4) 0.0475(10) Uani 1 1 d . . . . .
H33 H -0.0405 0.1754 1.2495 0.057 Uiso 1 1 calc R U . . .
C34 C -0.0697(4) 0.16674(11) 1.4443(5) 0.0542(11) Uani 1 1 d . . . . .
H34 H -0.0669 0.1443 1.4393 0.065 Uiso 1 1 calc R U . . .
C35 C -0.0892(5) 0.18201(11) 1.5636(4) 0.0551(12) Uani 1 1 d . . . . .
H35 H -0.1010 0.1698 1.6406 0.066 Uiso 1 1 calc R U . . .
C36 C -0.0915(4) 0.21560(11) 1.5707(4) 0.0465(10) Uani 1 1 d . . . . .
C37 C -0.1040(5) 0.23381(10) 1.6931(4) 0.0605(12) Uani 1 1 d . . . . .
H37 H -0.1122 0.2229 1.7741 0.073 Uiso 1 1 calc R U . . .
C38 C -0.0751(4) 0.23270(9) 1.4495(4) 0.0388(9) Uani 1 1 d . . . . .
C39 C -0.3102(4) 0.22254(12) 1.0729(5) 0.0588(12) Uani 1 1 d . . . . .
H39 H -0.2617 0.2031 1.0844 0.071 Uiso 1 1 calc R U . . .
C40 C -0.4560(5) 0.22181(14) 1.0345(6) 0.0747(16) Uani 1 1 d . . . . .
H40 H -0.5034 0.2022 1.0222 0.090 Uiso 1 1 calc R U . . .
C41 C -0.5275(7) 0.2500 1.0153(8) 0.076(2) Uani 1 2 d S T P . .
H41 H -0.6247 0.2500 0.9892 0.091 Uiso 1 2 calc R U P . .

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 0.439 0.250 0.557 219 16 ' '
2 0.560 0.750 0.443 220 16 ' '
_platon_squeeze_details          
;
;

_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 O1 2.054(3) . ?
Ni1 O8 2.078(3) . ?
Ni1 N2 2.095(3) . ?
Ni1 O6 2.095(3) 1_554 ?
Ni1 N1 2.095(3) . ?
Ni1 N3 2.112(3) . ?
Ni2 N5 2.081(4) . ?
Ni2 O3 2.084(3) 4_565 ?
Ni2 O3 2.084(3) . ?
Ni2 O9 2.089(3) . ?
Ni2 N4 2.116(3) 4_565 ?
Ni2 N4 2.116(3) . ?
N1 C16 1.317(5) . ?
N1 C20 1.361(5) . ?
N2 C27 1.310(5) . ?
N2 C24 1.363(5) . ?
N3 C32 1.318(5) . ?
N3 C28 1.336(6) . ?
N4 C33 1.315(5) . ?
N4 C38 1.357(5) . ?
N5 C39 1.336(5) . ?
N5 C39 1.336(5) 4_565 ?
O1 C1 1.265(5) . ?
O2 C1 1.248(4) . ?
O3 C6 1.261(4) . ?
O4 C6 1.238(4) . ?
O5 C7 1.384(4) . ?
O5 C9 1.387(4) . ?
O6 C15 1.261(4) . ?
O6 Ni1 2.095(3) 1_556 ?
O7 C15 1.243(5) . ?
O8 H1W 0.8501 . ?
O8 H2W 0.8497 . ?
O9 H3W 0.8501 . ?
C1 C2 1.513(5) . ?
C2 C3 1.385(5) . ?
C2 C8 1.389(5) . ?
C3 C4 1.384(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.383(5) . ?
C4 H4 0.9300 . ?
C5 C7 1.394(5) . ?
C5 C6 1.514(5) . ?
C7 C8 1.380(5) . ?
C8 H8 0.9300 . ?
C9 C14 1.380(5) . ?
C9 C10 1.394(6) . ?
C10 C11 1.381(6) . ?
C10 H10 0.9300 . ?
C11 C12 1.372(7) . ?
C11 H11 0.9300 . ?
C12 C13 1.373(6) . ?
C12 H12A 0.9300 . ?
C13 C14 1.391(5) . ?
C13 H13 0.9300 . ?
C14 C15 1.512(5) . ?
C16 C17 1.395(5) . ?
C16 H16 0.9300 . ?
C17 C18 1.351(6) . ?
C17 H17 0.9300 . ?
C18 C19 1.399(6) . ?
C18 H18 0.9300 . ?
C19 C20 1.397(5) . ?
C19 C21 1.437(6) . ?
C20 C24 1.426(6) . ?
C21 C22 1.330(7) . ?
C21 H21 0.9300 . ?
C22 C23 1.432(6) . ?
C22 H22 0.9300 . ?
C23 C25 1.393(7) . ?
C23 C24 1.404(5) . ?
C25 C26 1.369(6) . ?
C25 H25 0.9300 . ?
C26 C27 1.401(6) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
C28 C29 1.373(7) . ?
C28 H28 0.9300 . ?
C29 C30 1.373(7) . ?
C29 H29 0.9300 . ?
C30 C31 1.363(7) . ?
C30 H30 0.9300 . ?
C31 C32 1.387(6) . ?
C31 H31 0.9300 . ?
C32 H32 0.9300 . ?
C33 C34 1.394(6) . ?
C33 H33 0.9300 . ?
C34 C35 1.369(6) . ?
C34 H34 0.9300 . ?
C35 C36 1.393(6) . ?
C35 H35 0.9300 . ?
C36 C38 1.414(5) . ?
C36 C37 1.440(6) . ?
C37 C37 1.341(9) 4_565 ?
C37 H37 0.9300 . ?
C38 C38 1.433(7) 4_565 ?
C39 C40 1.395(6) . ?
C39 H39 0.9300 . ?
C40 C41 1.353(6) . ?
C40 H40 0.9300 . ?
C41 C40 1.353(6) 4_565 ?
C41 H41 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 Ni1 O8 90.33(11) . . ?
O1 Ni1 N2 84.27(12) . . ?
O8 Ni1 N2 168.98(11) . . ?
O1 Ni1 O6 92.18(11) . 1_554 ?
O8 Ni1 O6 94.24(10) . 1_554 ?
N2 Ni1 O6 95.56(11) . 1_554 ?
O1 Ni1 N1 87.10(11) . . ?
O8 Ni1 N1 90.56(11) . . ?
N2 Ni1 N1 79.60(13) . . ?
O6 Ni1 N1 175.15(12) 1_554 . ?
O1 Ni1 N3 177.83(12) . . ?
O8 Ni1 N3 91.18(12) . . ?
N2 Ni1 N3 93.97(13) . . ?
O6 Ni1 N3 89.27(12) 1_554 . ?
N1 Ni1 N3 91.33(12) . . ?
N5 Ni2 O3 87.66(11) . 4_565 ?
N5 Ni2 O3 87.66(11) . . ?
O3 Ni2 O3 97.17(15) 4_565 . ?
N5 Ni2 O9 179.28(17) . . ?
O3 Ni2 O9 92.81(10) 4_565 . ?
O3 Ni2 O9 92.81(10) . . ?
N5 Ni2 N4 91.75(13) . 4_565 ?
O3 Ni2 N4 91.92(11) 4_565 4_565 ?
O3 Ni2 N4 170.86(12) . 4_565 ?
O9 Ni2 N4 87.70(12) . 4_565 ?
N5 Ni2 N4 91.75(13) . . ?
O3 Ni2 N4 170.86(12) 4_565 . ?
O3 Ni2 N4 91.92(11) . . ?
O9 Ni2 N4 87.70(12) . . ?
N4 Ni2 N4 78.98(18) 4_565 . ?
C16 N1 C20 118.2(3) . . ?
C16 N1 Ni1 128.6(3) . . ?
C20 N1 Ni1 112.9(3) . . ?
C27 N2 C24 118.0(4) . . ?
C27 N2 Ni1 129.1(3) . . ?
C24 N2 Ni1 112.0(3) . . ?
C32 N3 C28 117.3(4) . . ?
C32 N3 Ni1 121.6(3) . . ?
C28 N3 Ni1 121.0(3) . . ?
C33 N4 C38 118.2(3) . . ?
C33 N4 Ni2 128.8(3) . . ?
C38 N4 Ni2 112.8(2) . . ?
C39 N5 C39 116.7(5) . 4_565 ?
C39 N5 Ni2 121.5(2) . . ?
C39 N5 Ni2 121.5(2) 4_565 . ?
C1 O1 Ni1 129.1(3) . . ?
C6 O3 Ni2 127.7(2) . . ?
C7 O5 C9 115.9(3) . . ?
C15 O6 Ni1 125.0(3) . 1_556 ?
Ni1 O8 H1W 88.4 . . ?
Ni1 O8 H2W 89.8 . . ?
H1W O8 H2W 112.7 . . ?
Ni2 O9 H3W 89.5 . . ?
O2 C1 O1 126.2(4) . . ?
O2 C1 C2 119.6(4) . . ?
O1 C1 C2 114.1(4) . . ?
C3 C2 C8 119.5(4) . . ?
C3 C2 C1 121.9(4) . . ?
C8 C2 C1 118.5(4) . . ?
C4 C3 C2 119.1(4) . . ?
C4 C3 H3 120.5 . . ?
C2 C3 H3 120.5 . . ?
C5 C4 C3 122.6(4) . . ?
C5 C4 H4 118.7 . . ?
C3 C4 H4 118.7 . . ?
C4 C5 C7 117.2(4) . . ?
C4 C5 C6 119.7(4) . . ?
C7 C5 C6 123.1(4) . . ?
O4 C6 O3 126.9(4) . . ?
O4 C6 C5 115.8(3) . . ?
O3 C6 C5 117.3(3) . . ?
C8 C7 O5 120.7(4) . . ?
C8 C7 C5 121.2(4) . . ?
O5 C7 C5 118.0(3) . . ?
C7 C8 C2 120.2(4) . . ?
C7 C8 H8 119.9 . . ?
C2 C8 H8 119.9 . . ?
C14 C9 O5 121.6(4) . . ?
C14 C9 C10 121.3(4) . . ?
O5 C9 C10 117.1(4) . . ?
C11 C10 C9 119.9(4) . . ?
C11 C10 H10 120.1 . . ?
C9 C10 H10 120.1 . . ?
C12 C11 C10 119.8(4) . . ?
C12 C11 H11 120.1 . . ?
C10 C11 H11 120.1 . . ?
C11 C12 C13 119.5(5) . . ?
C11 C12 H12A 120.3 . . ?
C13 C12 H12A 120.3 . . ?
C12 C13 C14 122.6(5) . . ?
C12 C13 H13 118.7 . . ?
C14 C13 H13 118.7 . . ?
C9 C14 C13 116.9(4) . . ?
C9 C14 C15 125.6(3) . . ?
C13 C14 C15 117.4(4) . . ?
O7 C15 O6 125.0(4) . . ?
O7 C15 C14 115.5(3) . . ?
O6 C15 C14 119.5(4) . . ?
N1 C16 C17 123.4(4) . . ?
N1 C16 H16 118.3 . . ?
C17 C16 H16 118.3 . . ?
C18 C17 C16 118.6(4) . . ?
C18 C17 H17 120.7 . . ?
C16 C17 H17 120.7 . . ?
C17 C18 C19 120.2(4) . . ?
C17 C18 H18 119.9 . . ?
C19 C18 H18 119.9 . . ?
C20 C19 C18 117.6(4) . . ?
C20 C19 C21 117.7(4) . . ?
C18 C19 C21 124.6(4) . . ?
N1 C20 C19 122.0(4) . . ?
N1 C20 C24 116.8(3) . . ?
C19 C20 C24 121.3(4) . . ?
C22 C21 C19 121.6(4) . . ?
C22 C21 H21 119.2 . . ?
C19 C21 H21 119.2 . . ?
C21 C22 C23 121.5(5) . . ?
C21 C22 H22 119.2 . . ?
C23 C22 H22 119.2 . . ?
C25 C23 C24 116.8(4) . . ?
C25 C23 C22 124.4(4) . . ?
C24 C23 C22 118.8(4) . . ?
N2 C24 C23 122.7(4) . . ?
N2 C24 C20 118.2(3) . . ?
C23 C24 C20 119.1(4) . . ?
C26 C25 C23 120.7(5) . . ?
C26 C25 H25 119.7 . . ?
C23 C25 H25 119.7 . . ?
C25 C26 C27 118.1(5) . . ?
C25 C26 H26 121.0 . . ?
C27 C26 H26 121.0 . . ?
N2 C27 C26 123.6(4) . . ?
N2 C27 H27 118.2 . . ?
C26 C27 H27 118.2 . . ?
N3 C28 C29 123.3(5) . . ?
N3 C28 H28 118.3 . . ?
C29 C28 H28 118.3 . . ?
C28 C29 C30 118.4(5) . . ?
C28 C29 H29 120.8 . . ?
C30 C29 H29 120.8 . . ?
C31 C30 C29 119.3(5) . . ?
C31 C30 H30 120.4 . . ?
C29 C30 H30 120.4 . . ?
C30 C31 C32 118.5(5) . . ?
C30 C31 H31 120.8 . . ?
C32 C31 H31 120.8 . . ?
N3 C32 C31 123.2(5) . . ?
N3 C32 H32 118.4 . . ?
C31 C32 H32 118.4 . . ?
N4 C33 C34 123.8(4) . . ?
N4 C33 H33 118.1 . . ?
C34 C33 H33 118.1 . . ?
C35 C34 C33 118.1(4) . . ?
C35 C34 H34 121.0 . . ?
C33 C34 H34 121.0 . . ?
C34 C35 C36 120.6(4) . . ?
C34 C35 H35 119.7 . . ?
C36 C35 H35 119.7 . . ?
C35 C36 C38 117.0(4) . . ?
C35 C36 C37 124.7(4) . . ?
C38 C36 C37 118.3(4) . . ?
C37 C37 C36 121.6(2) 4_565 . ?
C37 C37 H37 119.2 4_565 . ?
C36 C37 H37 119.2 . . ?
N4 C38 C36 122.3(4) . . ?
N4 C38 C38 117.6(2) . 4_565 ?
C36 C38 C38 120.1(2) . 4_565 ?
N5 C39 C40 122.9(5) . . ?
N5 C39 H39 118.6 . . ?
C40 C39 H39 118.6 . . ?
C41 C40 C39 119.1(5) . . ?
C41 C40 H40 120.4 . . ?
C39 C40 H40 120.4 . . ?
C40 C41 C40 119.2(6) . 4_565 ?
C40 C41 H41 120.4 . . ?
C40 C41 H41 120.4 4_565 . ?

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 -12.5(6) . . . . ?
Ni1 O1 C1 C2 169.4(2) . . . . ?
O2 C1 C2 C3 160.0(4) . . . . ?
O1 C1 C2 C3 -21.7(5) . . . . ?
O2 C1 C2 C8 -23.3(5) . . . . ?
O1 C1 C2 C8 154.9(3) . . . . ?
C8 C2 C3 C4 0.0(6) . . . . ?
C1 C2 C3 C4 176.7(4) . . . . ?
C2 C3 C4 C5 -3.2(6) . . . . ?
C3 C4 C5 C7 3.2(6) . . . . ?
C3 C4 C5 C6 -176.9(4) . . . . ?
Ni2 O3 C6 O4 -5.2(6) . . . . ?
Ni2 O3 C6 C5 174.2(2) . . . . ?
C4 C5 C6 O4 -55.6(5) . . . . ?
C7 C5 C6 O4 124.2(4) . . . . ?
C4 C5 C6 O3 124.9(4) . . . . ?
C7 C5 C6 O3 -55.3(5) . . . . ?
C9 O5 C7 C8 -34.9(5) . . . . ?
C9 O5 C7 C5 149.1(3) . . . . ?
C4 C5 C7 C8 -0.1(5) . . . . ?
C6 C5 C7 C8 -179.9(3) . . . . ?
C4 C5 C7 O5 175.9(3) . . . . ?
C6 C5 C7 O5 -3.9(5) . . . . ?
O5 C7 C8 C2 -178.9(3) . . . . ?
C5 C7 C8 C2 -3.0(5) . . . . ?
C3 C2 C8 C7 3.0(6) . . . . ?
C1 C2 C8 C7 -173.8(3) . . . . ?
C7 O5 C9 C14 119.7(4) . . . . ?
C7 O5 C9 C10 -62.3(5) . . . . ?
C14 C9 C10 C11 1.0(7) . . . . ?
O5 C9 C10 C11 -177.0(4) . . . . ?
C9 C10 C11 C12 -1.0(8) . . . . ?
C10 C11 C12 C13 1.7(9) . . . . ?
C11 C12 C13 C14 -2.5(9) . . . . ?
O5 C9 C14 C13 176.3(4) . . . . ?
C10 C9 C14 C13 -1.6(6) . . . . ?
O5 C9 C14 C15 -4.6(6) . . . . ?
C10 C9 C14 C15 177.5(4) . . . . ?
C12 C13 C14 C9 2.4(7) . . . . ?
C12 C13 C14 C15 -176.8(5) . . . . ?
Ni1 O6 C15 O7 8.5(6) 1_556 . . . ?
Ni1 O6 C15 C14 -170.8(3) 1_556 . . . ?
C9 C14 C15 O7 -178.3(4) . . . . ?
C13 C14 C15 O7 0.8(6) . . . . ?
C9 C14 C15 O6 1.0(6) . . . . ?
C13 C14 C15 O6 -179.9(4) . . . . ?
C20 N1 C16 C17 -0.8(6) . . . . ?
Ni1 N1 C16 C17 -174.1(3) . . . . ?
N1 C16 C17 C18 1.4(7) . . . . ?
C16 C17 C18 C19 -0.7(7) . . . . ?
C17 C18 C19 C20 -0.4(7) . . . . ?
C17 C18 C19 C21 -179.7(4) . . . . ?
C16 N1 C20 C19 -0.4(6) . . . . ?
Ni1 N1 C20 C19 173.9(3) . . . . ?
C16 N1 C20 C24 -178.7(4) . . . . ?
Ni1 N1 C20 C24 -4.4(4) . . . . ?
C18 C19 C20 N1 1.0(6) . . . . ?
C21 C19 C20 N1 -179.7(4) . . . . ?
C18 C19 C20 C24 179.2(4) . . . . ?
C21 C19 C20 C24 -1.4(6) . . . . ?
C20 C19 C21 C22 0.7(7) . . . . ?
C18 C19 C21 C22 180.0(5) . . . . ?
C19 C21 C22 C23 0.8(9) . . . . ?
C21 C22 C23 C25 177.7(5) . . . . ?
C21 C22 C23 C24 -1.6(8) . . . . ?
C27 N2 C24 C23 -3.4(6) . . . . ?
Ni1 N2 C24 C23 -174.1(3) . . . . ?
C27 N2 C24 C20 176.7(4) . . . . ?
Ni1 N2 C24 C20 6.0(5) . . . . ?
C25 C23 C24 N2 1.7(7) . . . . ?
C22 C23 C24 N2 -179.0(4) . . . . ?
C25 C23 C24 C20 -178.5(4) . . . . ?
C22 C23 C24 C20 0.9(7) . . . . ?
N1 C20 C24 N2 -1.1(6) . . . . ?
C19 C20 C24 N2 -179.5(4) . . . . ?
N1 C20 C24 C23 179.0(4) . . . . ?
C19 C20 C24 C23 0.6(6) . . . . ?
C24 C23 C25 C26 -0.3(8) . . . . ?
C22 C23 C25 C26 -179.6(5) . . . . ?
C23 C25 C26 C27 0.8(9) . . . . ?
C24 N2 C27 C26 3.9(7) . . . . ?
Ni1 N2 C27 C26 172.8(4) . . . . ?
C25 C26 C27 N2 -2.6(8) . . . . ?
C32 N3 C28 C29 -2.3(7) . . . . ?
Ni1 N3 C28 C29 175.0(4) . . . . ?
N3 C28 C29 C30 0.5(9) . . . . ?
C28 C29 C30 C31 1.4(8) . . . . ?
C29 C30 C31 C32 -1.4(7) . . . . ?
C28 N3 C32 C31 2.2(6) . . . . ?
Ni1 N3 C32 C31 -175.0(3) . . . . ?
C30 C31 C32 N3 -0.4(7) . . . . ?
C38 N4 C33 C34 0.9(6) . . . . ?
Ni2 N4 C33 C34 176.1(3) . . . . ?
N4 C33 C34 C35 -0.2(6) . . . . ?
C33 C34 C35 C36 -0.8(6) . . . . ?
C34 C35 C36 C38 0.9(6) . . . . ?
C34 C35 C36 C37 -176.6(4) . . . . ?
C35 C36 C37 C37 179.2(3) . . . 4_565 ?
C38 C36 C37 C37 1.7(4) . . . 4_565 ?
C33 N4 C38 C36 -0.6(5) . . . . ?
Ni2 N4 C38 C36 -176.6(3) . . . . ?
C33 N4 C38 C38 178.5(3) . . . 4_565 ?
Ni2 N4 C38 C38 2.6(2) . . . 4_565 ?
C35 C36 C38 N4 -0.2(6) . . . . ?
C37 C36 C38 N4 177.5(3) . . . . ?
C35 C36 C38 C38 -179.4(3) . . . 4_565 ?
C37 C36 C38 C38 -1.7(4) . . . 4_565 ?
C39 N5 C39 C40 -1.7(9) 4_565 . . . ?
Ni2 N5 C39 C40 172.9(4) . . . . ?
N5 C39 C40 C41 1.1(9) . . . . ?
C39 C40 C41 C40 -0.3(12) . . . 4_565 ?

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
O9 H3W O4 0.85 1.79 2.636(4) 179.7 .
O8 H2W O2 0.85 1.80 2.654(4) 179.7 .
O8 H1W O7 0.85 1.72 2.571(4) 179.8 1_554

_refine_diff_density_max         0.407
_refine_diff_density_min         -0.276
_refine_diff_density_rms         0.065


# start Validation Reply Form
_vrf_PLAT910_I                   
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min) 20 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 file style based 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_286-9Zn1
_database_code_depnum_ccdc_archive 'CCDC 1509372'
_audit_update_record             
;
2017-03-26 deposited with the CCDC.
2017-04-10 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            'C21 H12 N4 O7 Zn2'
_chemical_formula_weight         563.09

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           ?
_space_group_name_H-M_alt        I2/c
_space_group_name_Hall           ?

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

_cell_length_a                   18.7994(7)
_cell_length_b                   13.0415(8)
_cell_length_c                   16.9882(10)
_cell_angle_alpha                90
_cell_angle_beta                 93.823(5)
_cell_angle_gamma                90
_cell_volume                     4155.8(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    12731
_cell_measurement_theta_min      3.346
_cell_measurement_theta_max      25.047

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.800
_exptl_crystal_F_000             2256
_exptl_transmission_factor_min   0.521
_exptl_transmission_factor_max   0.609
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.210
_exptl_absorpt_coefficient_mu    2.363
_shelx_estimated_absorpt_T_min   0.557
_shelx_estimated_absorpt_T_max   0.637
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.557
_exptl_absorpt_correction_T_max  0.637
_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            12731
_diffrn_reflns_av_unetI/netI     0.0655
_diffrn_reflns_av_R_equivalents  0.0630
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.346
_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             3694
_reflns_number_gt                2461
_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)+(0.0393P)²+22.8148P] 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         3694
_refine_ls_number_parameters     307
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0795
_refine_ls_R_factor_gt           0.0502
_refine_ls_wR_factor_ref         0.1311
_refine_ls_wR_factor_gt          0.1140
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.015
_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 0.23639(3) 0.25006(5) 1.08597(4) 0.0275(2) Uani 1 1 d . . . . .
Zn2 Zn 0.05224(3) 0.24985(5) 1.08527(4) 0.0278(2) Uani 1 1 d . . . . .
O1 O 0.17696(19) 0.3137(3) 0.9968(2) 0.0390(11) Uani 1 1 d . . . . .
O2 O 0.06001(19) 0.3385(3) 0.9926(2) 0.0379(10) Uani 1 1 d . . . . .
O3 O 0.20087(18) 0.6514(3) 0.6738(2) 0.0383(10) Uani 1 1 d . . . . .
O4 O 0.08316(19) 0.6678(3) 0.6767(2) 0.0385(10) Uani 1 1 d . . . . .
O5 O 0.25560(18) 0.4834(3) 0.7523(2) 0.0330(9) Uani 1 1 d . . . . .
O6 O 0.4059(2) 0.6135(3) 0.9184(3) 0.0505(12) Uani 1 1 d . . . . .
O7 O 0.2957(2) 0.6223(3) 0.8656(3) 0.0428(11) Uani 1 1 d . . . . .
N1 N 0.2983(2) 0.1604(4) 1.0000(3) 0.0368(12) Uani 1 1 d . . . . .
N2 N 0.3355(2) 0.3027(4) 1.1115(3) 0.0335(12) Uani 1 1 d . . . . .
N3 N 0.4074(2) 0.1340(4) 0.9641(3) 0.0349(12) Uani 1 1 d . . . . .
H3 H 0.4529 0.1391 0.9628 0.042 Uiso 1 1 calc R U . . .
N4 N 0.4524(2) 0.2925(4) 1.0972(3) 0.0371(13) Uani 1 1 d . . . . .
C1 C 0.1221(3) 0.3540(4) 0.9681(3) 0.0275(13) Uani 1 1 d . . . . .
C2 C 0.1266(3) 0.4245(4) 0.8992(3) 0.0254(12) Uani 1 1 d . . . . .
C3 C 0.0715(3) 0.4903(4) 0.8749(3) 0.0295(13) Uani 1 1 d . . . . .
H2 H 0.0295 0.4902 0.9008 0.035 Uiso 1 1 calc R U . . .
C4 C 0.0791(3) 0.5564(4) 0.8119(3) 0.0295(13) Uani 1 1 d . . . . .
H4 H 0.0419 0.6007 0.7969 0.035 Uiso 1 1 calc R U . . .
C5 C 0.1406(2) 0.5586(4) 0.7706(3) 0.0225(12) Uani 1 1 d . . . . .
C6 C 0.1436(3) 0.6319(4) 0.7018(3) 0.0255(12) Uani 1 1 d . . . . .
C7 C 0.1957(3) 0.4900(4) 0.7954(3) 0.0263(13) Uani 1 1 d . . . . .
C8 C 0.1890(2) 0.4254(4) 0.8586(3) 0.0270(13) Uani 1 1 d . . . . .
H8 H 0.2265 0.3818 0.8745 0.032 Uiso 1 1 calc R U . . .
C9 C 0.3150(3) 0.4288(5) 0.7850(4) 0.0342(14) Uani 1 1 d . . . . .
C10 C 0.3297(3) 0.3353(5) 0.7514(4) 0.0488(18) Uani 1 1 d . . . . .
H10 H 0.2989 0.3088 0.7113 0.059 Uiso 1 1 calc R U . . .
C11 C 0.3896(4) 0.2816(6) 0.7768(5) 0.060(2) Uani 1 1 d . . . . .
H11 H 0.3987 0.2177 0.7553 0.073 Uiso 1 1 calc R U . . .
C12 C 0.4356(4) 0.3225(6) 0.8337(5) 0.055(2) Uani 1 1 d . . . . .
H12 H 0.4763 0.2861 0.8508 0.066 Uiso 1 1 calc R U . . .
C13 C 0.4229(3) 0.4161(5) 0.8658(4) 0.0484(18) Uani 1 1 d . . . . .
H13 H 0.4560 0.4434 0.9032 0.058 Uiso 1 1 calc R U . . .
C14 C 0.3616(3) 0.4715(5) 0.8440(4) 0.0325(14) Uani 1 1 d . . . . .
C15 C 0.3518(3) 0.5764(5) 0.8787(4) 0.0377(15) Uani 1 1 d . . . . .
C16 C 0.2973(3) 0.0891(6) 0.9404(4) 0.0514(18) Uani 1 1 d . . . . .
H16 H 0.2564 0.0571 0.9185 0.062 Uiso 1 1 calc R U . . .
C17 C 0.3641(3) 0.0718(5) 0.9179(4) 0.0440(16) Uani 1 1 d . . . . .
H17 H 0.3776 0.0269 0.8790 0.053 Uiso 1 1 calc R U . . .
C18 C 0.3664(3) 0.1859(4) 1.0122(3) 0.0257(12) Uani 1 1 d . . . . .
C19 C 0.3872(2) 0.2588(4) 1.0731(3) 0.0231(12) Uani 1 1 d . . . . .
C20 C 0.4399(3) 0.3625(6) 1.1557(4) 0.056(2) Uani 1 1 d . . . . .
H20 H 0.4745 0.4002 1.1846 0.068 Uiso 1 1 calc R U . . .
C21 C 0.3677(3) 0.3672(6) 1.1642(4) 0.051(2) Uani 1 1 d . . . . .
H21 H 0.3452 0.4078 1.2000 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
Zn1 O7 1.971(4) 4_546 ?
Zn1 O1 2.002(4) . ?
Zn1 N2 2.005(4) . ?
Zn1 O3 2.111(4) 6_566 ?
Zn1 N1 2.255(5) . ?
Zn2 O4 1.945(4) 6_566 ?
Zn2 O6 1.947(4) 4_546 ?
Zn2 O2 1.967(4) . ?
Zn2 N4 1.981(4) 8_455 ?
O1 C1 1.228(6) . ?
O2 C1 1.281(6) . ?
O3 C6 1.233(6) . ?
O3 Zn1 2.111(4) 6_565 ?
O4 C6 1.276(6) . ?
O4 Zn2 1.945(4) 6_565 ?
O5 C7 1.386(6) . ?
O5 C9 1.406(6) . ?
O6 C15 1.277(7) . ?
O6 Zn2 1.947(4) 4_556 ?
O7 C15 1.221(7) . ?
O7 Zn1 1.971(4) 4_556 ?
N1 C18 1.326(6) . ?
N1 C16 1.374(8) . ?
N2 C19 1.336(6) . ?
N2 C21 1.342(7) . ?
N3 C18 1.342(7) . ?
N3 C17 1.360(7) . ?
N3 H3 0.8600 . ?
N4 C19 1.339(6) . ?
N4 C20 1.381(8) . ?
N4 Zn2 1.981(4) 8 ?
C1 C2 1.495(7) . ?
C2 C3 1.387(7) . ?
C2 C8 1.401(7) . ?
C3 C4 1.389(7) . ?
C3 H2 0.9300 . ?
C4 C5 1.393(7) . ?
C4 H4 0.9300 . ?
C5 C7 1.410(7) . ?
C5 C6 1.513(7) . ?
C7 C8 1.377(7) . ?
C8 H8 0.9300 . ?
C9 C10 1.383(9) . ?
C9 C14 1.402(8) . ?
C10 C11 1.370(9) . ?
C10 H10 0.9300 . ?
C11 C12 1.363(10) . ?
C11 H11 0.9300 . ?
C12 C13 1.366(9) . ?
C12 H12 0.9300 . ?
C13 C14 1.388(8) . ?
C13 H13 0.9300 . ?
C14 C15 1.507(8) . ?
C16 C17 1.356(8) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
C18 C19 1.439(7) . ?
C20 C21 1.376(8) . ?
C20 H20 0.9300 . ?
C21 H21 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 O1 119.73(17) 4_546 . ?
O7 Zn1 N2 120.30(19) 4_546 . ?
O1 Zn1 N2 119.05(19) . . ?
O7 Zn1 O3 95.72(18) 4_546 6_566 ?
O1 Zn1 O3 95.48(17) . 6_566 ?
N2 Zn1 O3 88.37(17) . 6_566 ?
O7 Zn1 N1 91.01(18) 4_546 . ?
O1 Zn1 N1 90.63(17) . . ?
N2 Zn1 N1 78.78(17) . . ?
O3 Zn1 N1 167.15(15) 6_566 . ?
O4 Zn2 O6 115.50(19) 6_566 4_546 ?
O4 Zn2 O2 106.28(19) 6_566 . ?
O6 Zn2 O2 117.33(19) 4_546 . ?
O4 Zn2 N4 107.88(19) 6_566 8_455 ?
O6 Zn2 N4 97.8(2) 4_546 8_455 ?
O2 Zn2 N4 111.57(18) . 8_455 ?
C1 O1 Zn1 152.7(4) . . ?
C1 O2 Zn2 118.1(4) . . ?
C6 O3 Zn1 136.4(4) . 6_565 ?
C6 O4 Zn2 133.0(3) . 6_565 ?
C7 O5 C9 118.3(4) . . ?
C15 O6 Zn2 129.6(4) . 4_556 ?
C15 O7 Zn1 128.5(4) . 4_556 ?
C18 N1 C16 104.6(5) . . ?
C18 N1 Zn1 107.6(4) . . ?
C16 N1 Zn1 147.8(4) . . ?
C19 N2 C21 106.4(4) . . ?
C19 N2 Zn1 116.4(4) . . ?
C21 N2 Zn1 136.9(4) . . ?
C18 N3 C17 107.9(5) . . ?
C18 N3 H3 126.0 . . ?
C17 N3 H3 126.0 . . ?
C19 N4 C20 104.0(4) . . ?
C19 N4 Zn2 136.9(4) . 8 ?
C20 N4 Zn2 117.8(4) . 8 ?
O1 C1 O2 124.2(5) . . ?
O1 C1 C2 118.9(5) . . ?
O2 C1 C2 116.8(5) . . ?
C3 C2 C8 118.8(5) . . ?
C3 C2 C1 122.3(5) . . ?
C8 C2 C1 118.9(5) . . ?
C2 C3 C4 120.0(5) . . ?
C2 C3 H2 120.0 . . ?
C4 C3 H2 120.0 . . ?
C3 C4 C5 122.2(5) . . ?
C3 C4 H4 118.9 . . ?
C5 C4 H4 118.9 . . ?
C4 C5 C7 117.0(5) . . ?
C4 C5 C6 118.4(5) . . ?
C7 C5 C6 124.6(4) . . ?
O3 C6 O4 125.2(5) . . ?
O3 C6 C5 120.4(5) . . ?
O4 C6 C5 114.4(4) . . ?
C8 C7 O5 119.5(5) . . ?
C8 C7 C5 121.2(5) . . ?
O5 C7 C5 119.2(5) . . ?
C7 C8 C2 120.8(5) . . ?
C7 C8 H8 119.6 . . ?
C2 C8 H8 119.6 . . ?
C10 C9 C14 120.8(6) . . ?
C10 C9 O5 117.3(6) . . ?
C14 C9 O5 121.6(5) . . ?
C11 C10 C9 120.2(7) . . ?
C11 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?
C12 C11 C10 119.5(7) . . ?
C12 C11 H11 120.2 . . ?
C10 C11 H11 120.2 . . ?
C11 C12 C13 120.9(6) . . ?
C11 C12 H12 119.5 . . ?
C13 C12 H12 119.5 . . ?
C12 C13 C14 121.5(6) . . ?
C12 C13 H13 119.3 . . ?
C14 C13 H13 119.3 . . ?
C13 C14 C9 117.0(6) . . ?
C13 C14 C15 119.2(6) . . ?
C9 C14 C15 123.6(5) . . ?
O7 C15 O6 124.0(6) . . ?
O7 C15 C14 120.0(5) . . ?
O6 C15 C14 115.9(5) . . ?
C17 C16 N1 110.6(5) . . ?
C17 C16 H16 124.7 . . ?
N1 C16 H16 124.7 . . ?
C16 C17 N3 105.5(5) . . ?
C16 C17 H17 127.2 . . ?
N3 C17 H17 127.2 . . ?
N1 C18 N3 111.4(5) . . ?
N1 C18 C19 119.5(5) . . ?
N3 C18 C19 129.1(5) . . ?
N2 C19 N4 113.0(5) . . ?
N2 C19 C18 117.5(4) . . ?
N4 C19 C18 129.5(5) . . ?
C21 C20 N4 108.7(5) . . ?
C21 C20 H20 125.7 . . ?
N4 C20 H20 125.7 . . ?
N2 C21 C20 107.9(5) . . ?
N2 C21 H21 126.0 . . ?
C20 C21 H21 126.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Zn1 O1 C1 O2 -27.4(13) . . . . ?
Zn1 O1 C1 C2 153.7(7) . . . . ?
Zn2 O2 C1 O1 3.1(8) . . . . ?
Zn2 O2 C1 C2 -178.0(4) . . . . ?
O1 C1 C2 C3 -165.0(6) . . . . ?
O2 C1 C2 C3 16.0(8) . . . . ?
O1 C1 C2 C8 13.9(8) . . . . ?
O2 C1 C2 C8 -165.0(5) . . . . ?
C8 C2 C3 C4 -0.8(8) . . . . ?
C1 C2 C3 C4 178.2(5) . . . . ?
C2 C3 C4 C5 0.9(9) . . . . ?
C3 C4 C5 C7 0.1(8) . . . . ?
C3 C4 C5 C6 178.9(5) . . . . ?
Zn1 O3 C6 O4 5.6(9) 6_565 . . . ?
Zn1 O3 C6 C5 -175.7(4) 6_565 . . . ?
Zn2 O4 C6 O3 6.9(9) 6_565 . . . ?
Zn2 O4 C6 C5 -171.8(4) 6_565 . . . ?
C4 C5 C6 O3 165.5(5) . . . . ?
C7 C5 C6 O3 -15.7(8) . . . . ?
C4 C5 C6 O4 -15.7(7) . . . . ?
C7 C5 C6 O4 163.0(5) . . . . ?
C9 O5 C7 C8 -14.9(7) . . . . ?
C9 O5 C7 C5 168.9(5) . . . . ?
C4 C5 C7 C8 -1.2(8) . . . . ?
C6 C5 C7 C8 -180.0(5) . . . . ?
C4 C5 C7 O5 174.9(5) . . . . ?
C6 C5 C7 O5 -3.8(8) . . . . ?
O5 C7 C8 C2 -174.8(5) . . . . ?
C5 C7 C8 C2 1.3(8) . . . . ?
C3 C2 C8 C7 -0.3(8) . . . . ?
C1 C2 C8 C7 -179.3(5) . . . . ?
C7 O5 C9 C10 108.5(6) . . . . ?
C7 O5 C9 C14 -77.8(7) . . . . ?
C14 C9 C10 C11 1.7(10) . . . . ?
O5 C9 C10 C11 175.4(6) . . . . ?
C9 C10 C11 C12 -2.1(11) . . . . ?
C10 C11 C12 C13 0.2(12) . . . . ?
C11 C12 C13 C14 2.3(11) . . . . ?
C12 C13 C14 C9 -2.6(10) . . . . ?
C12 C13 C14 C15 -177.3(6) . . . . ?
C10 C9 C14 C13 0.6(9) . . . . ?
O5 C9 C14 C13 -172.8(5) . . . . ?
C10 C9 C14 C15 175.1(6) . . . . ?
O5 C9 C14 C15 1.7(9) . . . . ?
Zn1 O7 C15 O6 -12.2(9) 4_556 . . . ?
Zn1 O7 C15 C14 170.9(4) 4_556 . . . ?
Zn2 O6 C15 O7 -43.4(9) 4_556 . . . ?
Zn2 O6 C15 C14 133.6(5) 4_556 . . . ?
C13 C14 C15 O7 -173.6(6) . . . . ?
C9 C14 C15 O7 12.0(9) . . . . ?
C13 C14 C15 O6 9.2(9) . . . . ?
C9 C14 C15 O6 -165.1(6) . . . . ?
C18 N1 C16 C17 0.5(8) . . . . ?
Zn1 N1 C16 C17 -178.2(6) . . . . ?
N1 C16 C17 N3 -0.3(8) . . . . ?
C18 N3 C17 C16 0.0(7) . . . . ?
C16 N1 C18 N3 -0.5(7) . . . . ?
Zn1 N1 C18 N3 178.7(4) . . . . ?
C16 N1 C18 C19 -178.6(5) . . . . ?
Zn1 N1 C18 C19 0.6(6) . . . . ?
C17 N3 C18 N1 0.3(7) . . . . ?
C17 N3 C18 C19 178.2(6) . . . . ?
C21 N2 C19 N4 -0.9(7) . . . . ?
Zn1 N2 C19 N4 -175.5(4) . . . . ?
C21 N2 C19 C18 -179.6(5) . . . . ?
Zn1 N2 C19 C18 5.8(7) . . . . ?
C20 N4 C19 N2 0.4(7) . . . . ?
Zn2 N4 C19 N2 166.2(5) 8 . . . ?
C20 N4 C19 C18 178.9(6) . . . . ?
Zn2 N4 C19 C18 -15.3(10) 8 . . . ?
N1 C18 C19 N2 -4.2(8) . . . . ?
N3 C18 C19 N2 178.1(6) . . . . ?
N1 C18 C19 N4 177.3(6) . . . . ?
N3 C18 C19 N4 -0.4(10) . . . . ?
C19 N4 C20 C21 0.2(8) . . . . ?
Zn2 N4 C20 C21 -168.9(5) 8 . . . ?
C19 N2 C21 C20 1.0(8) . . . . ?
Zn1 N2 C21 C20 173.9(5) . . . . ?
N4 C20 C21 N2 -0.8(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
N3 H3 O2 0.86 2.06 2.900(6) 163.9 8

_refine_diff_density_max         0.661
_refine_diff_density_min         -0.769
_refine_diff_density_rms         0.100


# start Validation Reply Form
_vrf_PLAT910_I                   
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min) 10 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_280-5cd
_database_code_depnum_ccdc_archive 'CCDC 1509060'
_audit_update_record             
;
2017-03-26 deposited with the CCDC.
2017-04-10 downloaded from the CCDC.
;
_audit_creation_date             2017-03-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H23 Cd3 Cl O18, H2 O'
_chemical_formula_sum            'C30 H25 Cd3 Cl O19'
_chemical_formula_weight         1062.15
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   10.8678(6)
_cell_length_b                   14.2781(9)
_cell_length_c                   14.5680(6)
_cell_angle_alpha                109.047(5)
_cell_angle_beta                 103.976(4)
_cell_angle_gamma                90.040(5)
_cell_volume                     2065.7(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4542
_cell_measurement_temperature    294.2(3)
_cell_measurement_theta_max      27.4710
_cell_measurement_theta_min      3.4890
_shelx_estimated_absorpt_T_max   0.732
_shelx_estimated_absorpt_T_min   0.653
_exptl_absorpt_coefficient_mu    1.665
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91273
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.708
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1036
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   1.000
_exptl_transmission_factor_min   0.913
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_av_unetI/netI     0.0588
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12646
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.050
_diffrn_reflns_theta_max         25.050
_diffrn_reflns_theta_min         3.416
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      294.2(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0733
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -20.00   24.40   1.2000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.0420  -99.0000  -30.0000 37

#__ type_ start__ end____ width___ exp.time_
  2 omega   71.00  105.80   1.2000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       27.1670  178.0000  -30.0000 29

#__ type_ start__ end____ width___ exp.time_
  3 omega   -2.00  101.20   1.2000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       27.1670   57.0000   90.0000 86

#__ type_ start__ end____ width___ exp.time_
  4 omega   36.00  115.20   1.2000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       27.1670  178.0000 -120.0000 66

#__ type_ start__ end____ width___ exp.time_
  5 omega  -27.00   60.60   1.2000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       27.1670  -19.0000  150.0000 73

#__ type_ start__ end____ width___ exp.time_
  6 omega   -6.00   96.00   1.2000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       27.1670   38.0000    0.0000 85
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0567045000
_diffrn_orient_matrix_UB_12      0.0092017000
_diffrn_orient_matrix_UB_13      0.0162258000
_diffrn_orient_matrix_UB_21      0.0197318000
_diffrn_orient_matrix_UB_22      0.0515883000
_diffrn_orient_matrix_UB_23      0.0208817000
_diffrn_orient_matrix_UB_31      -0.0308719000
_diffrn_orient_matrix_UB_32      0.0060719000
_diffrn_orient_matrix_UB_33      -0.0462548000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6085
_reflns_number_total             7277
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         2.152
_refine_diff_density_min         -1.412
_refine_diff_density_rms         0.182
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         7277
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0839
_refine_ls_R_factor_gt           0.0731
_refine_ls_restrained_S_all      1.140
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0333P)²+41.2759P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1765
_refine_ls_wR_factor_ref         0.1812
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H) groups, All O(H,H) groups
2.a Riding coordinates:
 O9(H9), O15(H15A,H15B), O16(H16A,H16B), O17(H17A,H17B), O18(H18A,H18B),
 O19(H19A,H19B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9A), C12(H12), C13(H13), C18(H18),
 C19(H19), C20(H20), C21(H21), C24(H24), C27(H27), C28(H28)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.73917(7) 0.94017(6) 0.20493(6) 0.0315(2) Uani 1 1 d . . . . .
Cd2 Cd 0.65211(8) 1.19621(6) 0.18841(6) 0.0296(2) Uani 1 1 d . . . . .
Cd3 Cd 0.90603(8) 1.17921(6) 0.45351(6) 0.0320(2) Uani 1 1 d . . . . .
Cl1 Cl 0.7985(3) 1.2948(2) 0.3596(2) 0.0506(8) Uani 1 1 d . . . . .
O1 O 0.6843(7) 0.8127(6) 0.0622(6) 0.0389(19) Uani 1 1 d . . . . .
O2 O 0.6746(8) 0.6691(7) -0.0591(7) 0.058(3) Uani 1 1 d . . . . .
O3 O 0.9375(7) 0.8800(5) 0.1594(6) 0.0345(18) Uani 1 1 d . . . . .
O4 O 1.2033(8) 0.8247(6) -0.0967(6) 0.044(2) Uani 1 1 d . . . . .
O5 O 1.2582(8) 0.9779(7) -0.0841(7) 0.047(2) Uani 1 1 d . . . . .
O6 O 0.9054(7) 1.0490(6) 0.3031(5) 0.0324(17) Uani 1 1 d . . . . .
O7 O 1.0608(8) 1.1648(6) 0.3549(6) 0.045(2) Uani 1 1 d . . . . .
O8 O 0.7620(7) 0.8294(6) 0.2866(6) 0.041(2) Uani 1 1 d . . . . .
O9 O 0.7520(8) 0.6864(7) 0.3105(8) 0.061(3) Uani 1 1 d . . . . .
H9 H 0.7201 0.6325 0.2816 0.073 Uiso 1 1 d R . . . .
O10 O 0.5198(8) 0.8852(5) 0.2240(6) 0.0380(19) Uani 1 1 d . . . . .
O11 O 0.6173(7) 1.0636(6) 0.2398(6) 0.0348(18) Uani 1 1 d . . . . .
O12 O 0.4879(9) 1.1788(6) 0.2768(7) 0.049(2) Uani 1 1 d . . . . .
O13 O 0.2511(10) 0.7948(9) 0.4317(9) 0.069(3) Uani 1 1 d . . . . .
O14 O 0.2248(10) 0.9391(9) 0.5368(8) 0.066(3) Uani 1 1 d . . . . .
O15 O 0.5663(8) 1.3369(6) 0.1695(7) 0.050(2) Uani 1 1 d . . . . .
H15A H 0.4906 1.3353 0.1350 0.060 Uiso 1 1 d R . . . .
H15B H 0.6230 1.3267 0.2160 0.060 Uiso 1 1 d R . . . .
O16 O 0.5006(8) 1.1133(7) 0.0396(7) 0.053(2) Uani 1 1 d . . . . .
H16A H 0.4410 1.1371 0.0665 0.063 Uiso 1 1 d R . . . .
H16B H 0.5700 1.0870 0.0520 0.063 Uiso 1 1 d R . . . .
O17 O 1.0561(10) 1.1039(7) 0.5438(7) 0.067(3) Uani 1 1 d . . . . .
H17A H 0.9760 1.0913 0.5205 0.081 Uiso 1 1 d R . . . .
H17B H 1.1148 1.1252 0.5979 0.081 Uiso 1 1 d R . . . .
O18 O 1.0116(11) 1.3172(7) 0.5831(9) 0.086(4) Uani 1 1 d . . . . .
H18A H 1.0859 1.3166 0.6162 0.103 Uiso 1 1 d R . . . .
H18B H 0.9587 1.3117 0.5277 0.103 Uiso 1 1 d R . . . .
O19 O 0.9526(17) 1.3532(12) 0.1677(18) 0.179(10) Uani 1 1 d . . . . .
H19A H 0.9040 1.2996 0.1440 0.215 Uiso 1 1 d R . . . .
H19B H 0.9935 1.3482 0.2236 0.215 Uiso 1 1 d R . . . .
C1 C 0.7285(11) 0.7307(9) 0.0222(9) 0.037(3) Uani 1 1 d . . . . .
C2 C 0.8560(11) 0.7089(8) 0.0776(9) 0.034(2) Uani 1 1 d . . . . .
C3 C 0.8732(12) 0.6093(9) 0.0653(11) 0.047(3) Uani 1 1 d . . . . .
H3 H 0.8098 0.5602 0.0220 0.057 Uiso 1 1 calc R . . . .
C4 C 0.9859(14) 0.5831(10) 0.1180(11) 0.051(3) Uani 1 1 d . . . . .
H4 H 0.9955 0.5167 0.1116 0.061 Uiso 1 1 calc R . . . .
C5 C 1.0820(12) 0.6545(10) 0.1789(11) 0.049(3) Uani 1 1 d . . . . .
H5 H 1.1579 0.6363 0.2114 0.059 Uiso 1 1 calc R . . . .
C6 C 1.0661(11) 0.7534(9) 0.1920(9) 0.040(3) Uani 1 1 d . . . . .
H6 H 1.1302 0.8025 0.2340 0.049 Uiso 1 1 calc R . . . .
C7 C 0.9525(10) 0.7782(8) 0.1414(8) 0.030(2) Uani 1 1 d . . . . .
C8 C 1.0259(9) 0.9375(7) 0.1421(8) 0.025(2) Uani 1 1 d . . . . .
C9 C 1.0747(10) 0.8980(8) 0.0597(8) 0.030(2) Uani 1 1 d . . . . .
H9A H 1.0537 0.8317 0.0193 0.036 Uiso 1 1 calc R . . . .
C10 C 1.1553(10) 0.9583(8) 0.0380(8) 0.028(2) Uani 1 1 d . . . . .
C11 C 1.2083(11) 0.9170(9) -0.0547(8) 0.034(3) Uani 1 1 d . . . . .
C12 C 1.1868(11) 1.0563(8) 0.0969(9) 0.035(3) Uani 1 1 d . . . . .
H12 H 1.2404 1.0963 0.0813 0.042 Uiso 1 1 calc R . . . .
C13 C 1.1387(10) 1.0946(8) 0.1786(9) 0.035(3) Uani 1 1 d . . . . .
H13 H 1.1611 1.1608 0.2189 0.042 Uiso 1 1 calc R . . . .
C14 C 1.0564(9) 1.0366(8) 0.2031(8) 0.027(2) Uani 1 1 d . . . . .
C15 C 1.0055(10) 1.0860(9) 0.2918(9) 0.034(3) Uani 1 1 d . . . . .
C16 C 0.7049(11) 0.7476(9) 0.2712(9) 0.038(3) Uani 1 1 d . . . . .
C17 C 0.5756(10) 0.7168(8) 0.1988(8) 0.032(2) Uani 1 1 d . . . . .
C18 C 0.5370(13) 0.6164(9) 0.1475(11) 0.051(3) Uani 1 1 d . . . . .
H18 H 0.5914 0.5697 0.1614 0.061 Uiso 1 1 calc R . . . .
C19 C 0.4226(12) 0.5828(10) 0.0775(9) 0.047(3) Uani 1 1 d . . . . .
H19 H 0.4023 0.5153 0.0422 0.057 Uiso 1 1 calc R . . . .
C20 C 0.3380(13) 0.6514(11) 0.0605(11) 0.060(4) Uani 1 1 d . . . . .
H20 H 0.2585 0.6296 0.0156 0.072 Uiso 1 1 calc R . . . .
C21 C 0.3703(11) 0.7503(10) 0.1088(11) 0.048(3) Uani 1 1 d . . . . .
H21 H 0.3139 0.7958 0.0949 0.058 Uiso 1 1 calc R . . . .
C22 C 0.4884(10) 0.7846(8) 0.1796(8) 0.030(2) Uani 1 1 d . . . . .
C23 C 0.4581(10) 0.9369(8) 0.2979(8) 0.028(2) Uani 1 1 d . . . . .
C24 C 0.3957(11) 0.8873(9) 0.3430(10) 0.040(3) Uani 1 1 d . . . . .
H24 H 0.3925 0.8183 0.3235 0.048 Uiso 1 1 calc R . . . .
C25 C 0.3384(10) 0.9391(9) 0.4164(8) 0.035(3) Uani 1 1 d . . . . .
C26 C 0.2696(12) 0.8859(14) 0.4661(11) 0.055(4) Uani 1 1 d . . . . .
C27 C 0.3423(12) 1.0418(11) 0.4450(9) 0.048(3) Uani 1 1 d . . . . .
H27 H 0.3044 1.0781 0.4948 0.057 Uiso 1 1 calc R . . . .
C28 C 0.4029(13) 1.0881(9) 0.3982(9) 0.044(3) Uani 1 1 d . . . . .
H28 H 0.4046 1.1570 0.4167 0.053 Uiso 1 1 calc R . . . .
C29 C 0.4614(10) 1.0389(8) 0.3256(8) 0.028(2) Uani 1 1 d . . . . .
C30 C 0.5259(10) 1.0973(8) 0.2771(8) 0.029(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
Cd1 O1 2.218(8) . ?
Cd1 O3 2.479(7) . ?
Cd1 O5 2.416(8) 2_775 ?
Cd1 O6 2.241(7) . ?
Cd1 O8 2.250(8) . ?
Cd1 O10 2.614(8) . ?
Cd1 O11 2.206(7) . ?
Cd2 Cl1 2.554(3) . ?
Cd2 O4 2.258(7) 2_775 ?
Cd2 O11 2.312(7) . ?
Cd2 O12 2.495(8) . ?
Cd2 O15 2.285(8) . ?
Cd2 H15B 1.8191 . ?
Cd2 O16 2.326(8) . ?
Cd2 H16B 2.0724 . ?
Cd3 Cl1 2.581(3) . ?
Cd3 O6 2.365(7) . ?
Cd3 O7 2.430(8) . ?
Cd3 O13 2.612(11) 2_676 ?
Cd3 O14 2.268(10) 2_676 ?
Cd3 O17 2.331(9) . ?
Cd3 H17A 1.8834 . ?
Cd3 O18 2.299(10) . ?
Cd3 H18B 1.8542 . ?
O1 C1 1.278(14) . ?
O2 C1 1.226(14) . ?
O3 C7 1.407(12) . ?
O3 C8 1.382(12) . ?
O4 Cd2 2.258(7) 2_775 ?
O4 C11 1.255(14) . ?
O5 Cd1 2.416(8) 2_775 ?
O5 C11 1.259(14) . ?
O6 C15 1.277(13) . ?
O7 C15 1.237(14) . ?
O8 C16 1.250(13) . ?
O9 H9 0.7793 . ?
O9 C16 1.241(14) . ?
O10 C22 1.373(13) . ?
O10 C23 1.409(12) . ?
O11 C30 1.266(13) . ?
O12 C30 1.235(13) . ?
O13 Cd3 2.612(10) 2_676 ?
O13 C26 1.228(19) . ?
O14 Cd3 2.268(10) 2_676 ?
O14 C26 1.267(18) . ?
O15 H15A 0.8501 . ?
O15 H15B 0.8493 . ?
O16 H16A 0.8518 . ?
O16 H16B 0.8496 . ?
O17 H17A 0.8502 . ?
O17 H17B 0.8495 . ?
O18 H18A 0.8355 . ?
O18 H18B 0.8499 . ?
O19 H19A 0.8506 . ?
O19 H19B 0.8542 . ?
C1 C2 1.515(16) . ?
C2 C3 1.391(15) . ?
C2 C7 1.368(15) . ?
C3 H3 0.9300 . ?
C3 C4 1.402(18) . ?
C4 H4 0.9300 . ?
C4 C5 1.371(19) . ?
C5 H5 0.9300 . ?
C5 C6 1.379(17) . ?
C6 H6 0.9300 . ?
C6 C7 1.387(15) . ?
C8 C9 1.381(14) . ?
C8 C14 1.392(14) . ?
C9 H9A 0.9300 . ?
C9 C10 1.385(15) . ?
C10 C11 1.535(14) . ?
C10 C12 1.374(15) . ?
C12 H12 0.9300 . ?
C12 C13 1.366(15) . ?
C13 H13 0.9300 . ?
C13 C14 1.400(15) . ?
C14 C15 1.492(15) . ?
C16 C17 1.503(15) . ?
C17 C18 1.392(16) . ?
C17 C22 1.401(15) . ?
C18 H18 0.9300 . ?
C18 C19 1.372(18) . ?
C19 H19 0.9300 . ?
C19 C20 1.385(19) . ?
C20 H20 0.9300 . ?
C20 C21 1.358(19) . ?
C21 H21 0.9300 . ?
C21 C22 1.408(16) . ?
C23 C24 1.383(15) . ?
C23 C29 1.377(15) . ?
C24 H24 0.9300 . ?
C24 C25 1.372(17) . ?
C25 C26 1.510(17) . ?
C25 C27 1.385(18) . ?
C27 H27 0.9300 . ?
C27 C28 1.359(17) . ?
C28 H28 0.9300 . ?
C28 C29 1.363(15) . ?
C29 C30 1.519(15) . ?

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 O3 72.3(3) . . ?
O1 Cd1 O5 79.0(3) . 2_775 ?
O1 Cd1 O6 140.9(3) . . ?
O1 Cd1 O8 87.9(3) . . ?
O1 Cd1 O10 82.6(3) . . ?
O3 Cd1 O10 144.4(2) . . ?
O5 Cd1 O3 81.3(3) 2_775 . ?
O5 Cd1 O10 118.8(3) 2_775 . ?
O6 Cd1 O3 70.1(3) . . ?
O6 Cd1 O5 85.2(3) . 2_775 ?
O6 Cd1 O8 98.9(3) . . ?
O6 Cd1 O10 135.8(2) . . ?
O8 Cd1 O3 84.7(3) . . ?
O8 Cd1 O5 163.1(3) . 2_775 ?
O8 Cd1 O10 69.2(3) . . ?
O11 Cd1 O1 121.7(3) . . ?
O11 Cd1 O3 148.5(3) . . ?
O11 Cd1 O5 74.9(3) . 2_775 ?
O11 Cd1 O6 87.4(3) . . ?
O11 Cd1 O8 121.4(3) . . ?
O11 Cd1 O10 66.8(2) . . ?
Cl1 Cd2 H15B 71.8 . . ?
Cl1 Cd2 H16B 163.9 . . ?
O4 Cd2 Cl1 98.3(2) 2_775 . ?
O4 Cd2 O11 114.8(3) 2_775 . ?
O4 Cd2 O12 167.5(3) 2_775 . ?
O4 Cd2 O15 101.7(3) 2_775 . ?
O4 Cd2 H15B 104.0 2_775 . ?
O4 Cd2 O16 87.5(3) 2_775 . ?
O4 Cd2 H16B 73.7 2_775 . ?
O11 Cd2 Cl1 92.5(2) . . ?
O11 Cd2 O12 53.8(3) . . ?
O11 Cd2 H15B 140.0 . . ?
O11 Cd2 O16 86.9(3) . . ?
O11 Cd2 H16B 78.8 . . ?
O12 Cd2 Cl1 88.1(2) . . ?
O12 Cd2 H15B 88.2 . . ?
O12 Cd2 H16B 97.4 . . ?
O15 Cd2 Cl1 91.8(2) . . ?
O15 Cd2 O11 142.2(3) . . ?
O15 Cd2 O12 88.8(3) . . ?
O15 Cd2 H15B 20.1 . . ?
O15 Cd2 O16 84.9(3) . . ?
O15 Cd2 H16B 103.4 . . ?
H15B Cd2 H16B 123.4 . . ?
O16 Cd2 Cl1 173.8(3) . . ?
O16 Cd2 O12 86.7(3) . . ?
O16 Cd2 H15B 104.9 . . ?
O16 Cd2 H16B 21.3 . . ?
Cl1 Cd3 O13 94.3(3) . 2_676 ?
Cl1 Cd3 H17A 177.0 . . ?
Cl1 Cd3 H18B 68.8 . . ?
O6 Cd3 Cl1 93.1(2) . . ?
O6 Cd3 O7 53.9(2) . . ?
O6 Cd3 O13 129.9(3) . 2_676 ?
O6 Cd3 H17A 86.3 . . ?
O6 Cd3 H18B 144.6 . . ?
O7 Cd3 Cl1 85.5(2) . . ?
O7 Cd3 O13 176.2(3) . 2_676 ?
O7 Cd3 H17A 96.5 . . ?
O7 Cd3 H18B 93.3 . . ?
O13 Cd3 H17A 83.9 2_676 . ?
O13 Cd3 H18B 83.0 2_676 . ?
O14 Cd3 Cl1 116.1(3) 2_676 . ?
O14 Cd3 O6 79.7(3) 2_676 . ?
O14 Cd3 O7 130.5(3) 2_676 . ?
O14 Cd3 O13 52.9(4) 2_676 2_676 ?
O14 Cd3 O17 80.7(4) 2_676 . ?
O14 Cd3 H17A 60.8 2_676 . ?
O14 Cd3 O18 126.9(4) 2_676 . ?
O14 Cd3 H18B 135.3 2_676 . ?
O17 Cd3 Cl1 163.2(3) . . ?
O17 Cd3 O6 90.0(3) . . ?
O17 Cd3 O7 83.0(4) . . ?
O17 Cd3 O13 96.4(4) . 2_676 ?
O17 Cd3 H17A 19.9 . . ?
O17 Cd3 H18B 99.6 . . ?
H17A Cd3 H18B 113.2 . . ?
O18 Cd3 Cl1 89.0(3) . . ?
O18 Cd3 O6 148.6(4) . . ?
O18 Cd3 O7 95.2(4) . . ?
O18 Cd3 O13 81.0(4) . 2_676 ?
O18 Cd3 O17 79.9(3) . . ?
O18 Cd3 H17A 93.1 . . ?
O18 Cd3 H18B 20.2 . . ?
Cd2 Cl1 Cd3 111.67(12) . . ?
C1 O1 Cd1 137.0(7) . . ?
C7 O3 Cd1 116.4(6) . . ?
C8 O3 Cd1 124.2(6) . . ?
C8 O3 C7 119.2(8) . . ?
C11 O4 Cd2 104.5(7) . 2_775 ?
C11 O5 Cd1 151.8(8) . 2_775 ?
Cd1 O6 Cd3 125.7(3) . . ?
C15 O6 Cd1 136.7(7) . . ?
C15 O6 Cd3 94.3(6) . . ?
C15 O7 Cd3 92.3(7) . . ?
C16 O8 Cd1 134.1(7) . . ?
C16 O9 H9 113.0 . . ?
C22 O10 Cd1 112.5(6) . . ?
C22 O10 C23 117.2(8) . . ?
C23 O10 Cd1 126.5(6) . . ?
Cd1 O11 Cd2 116.6(3) . . ?
C30 O11 Cd1 147.1(7) . . ?
C30 O11 Cd2 96.3(6) . . ?
C30 O12 Cd2 88.5(7) . . ?
C26 O13 Cd3 84.0(9) . 2_676 ?
C26 O14 Cd3 99.2(10) . 2_676 ?
Cd2 O15 H15A 121.7 . . ?
Cd2 O15 H15B 47.3 . . ?
H15A O15 H15B 154.8 . . ?
Cd2 O16 H16A 90.6 . . ?
Cd2 O16 H16B 62.3 . . ?
H16A O16 H16B 140.8 . . ?
Cd3 O17 H17A 48.8 . . ?
Cd3 O17 H17B 134.3 . . ?
H17A O17 H17B 143.4 . . ?
Cd3 O18 H18A 121.8 . . ?
Cd3 O18 H18B 48.9 . . ?
H18A O18 H18B 150.5 . . ?
H19A O19 H19B 99.8 . . ?
O1 C1 C2 118.1(10) . . ?
O2 C1 O1 123.9(11) . . ?
O2 C1 C2 118.0(11) . . ?
C3 C2 C1 116.4(11) . . ?
C7 C2 C1 125.8(10) . . ?
C7 C2 C3 117.7(11) . . ?
C2 C3 H3 120.0 . . ?
C2 C3 C4 120.1(12) . . ?
C4 C3 H3 120.0 . . ?
C3 C4 H4 119.8 . . ?
C5 C4 C3 120.4(11) . . ?
C5 C4 H4 119.8 . . ?
C4 C5 H5 120.0 . . ?
C4 C5 C6 120.0(11) . . ?
C6 C5 H5 120.0 . . ?
C5 C6 H6 120.7 . . ?
C5 C6 C7 118.6(11) . . ?
C7 C6 H6 120.7 . . ?
C2 C7 O3 119.8(10) . . ?
C2 C7 C6 123.0(10) . . ?
C6 C7 O3 117.2(10) . . ?
O3 C8 C14 119.5(9) . . ?
C9 C8 O3 119.3(9) . . ?
C9 C8 C14 121.0(9) . . ?
C8 C9 H9A 120.4 . . ?
C8 C9 C10 119.2(10) . . ?
C10 C9 H9A 120.4 . . ?
C9 C10 C11 120.3(10) . . ?
C12 C10 C9 121.0(10) . . ?
C12 C10 C11 118.7(10) . . ?
O4 C11 O5 122.5(10) . . ?
O4 C11 C10 119.2(10) . . ?
O5 C11 C10 118.3(10) . . ?
C10 C12 H12 120.3 . . ?
C13 C12 C10 119.4(10) . . ?
C13 C12 H12 120.3 . . ?
C12 C13 H13 119.3 . . ?
C12 C13 C14 121.5(10) . . ?
C14 C13 H13 119.3 . . ?
C8 C14 C13 117.9(9) . . ?
C8 C14 C15 124.5(9) . . ?
C13 C14 C15 117.5(10) . . ?
O6 C15 C14 121.3(10) . . ?
O7 C15 O6 119.6(10) . . ?
O7 C15 C14 119.2(10) . . ?
O8 C16 C17 120.4(10) . . ?
O9 C16 O8 122.9(11) . . ?
O9 C16 C17 116.6(10) . . ?
C18 C17 C16 120.0(11) . . ?
C18 C17 C22 116.6(10) . . ?
C22 C17 C16 123.4(10) . . ?
C17 C18 H18 118.4 . . ?
C19 C18 C17 123.3(12) . . ?
C19 C18 H18 118.4 . . ?
C18 C19 H19 120.6 . . ?
C18 C19 C20 118.7(12) . . ?
C20 C19 H19 120.6 . . ?
C19 C20 H20 119.8 . . ?
C21 C20 C19 120.5(12) . . ?
C21 C20 H20 119.8 . . ?
C20 C21 H21 119.7 . . ?
C20 C21 C22 120.5(12) . . ?
C22 C21 H21 119.7 . . ?
O10 C22 C17 120.8(9) . . ?
O10 C22 C21 118.9(10) . . ?
C17 C22 C21 120.2(10) . . ?
C24 C23 O10 121.3(10) . . ?
C29 C23 O10 118.7(9) . . ?
C29 C23 C24 119.9(10) . . ?
C23 C24 H24 119.7 . . ?
C25 C24 C23 120.5(11) . . ?
C25 C24 H24 119.7 . . ?
C24 C25 C26 121.1(12) . . ?
C24 C25 C27 119.7(11) . . ?
C27 C25 C26 119.2(12) . . ?
O13 C26 O14 123.3(14) . . ?
O13 C26 C25 119.2(14) . . ?
O14 C26 C25 117.3(15) . . ?
C25 C27 H27 120.9 . . ?
C28 C27 C25 118.3(11) . . ?
C28 C27 H27 120.9 . . ?
C27 C28 H28 118.3 . . ?
C27 C28 C29 123.4(12) . . ?
C29 C28 H28 118.3 . . ?
C23 C29 C30 122.3(9) . . ?
C28 C29 C23 118.1(10) . . ?
C28 C29 C30 119.6(10) . . ?
O11 C30 C29 120.5(9) . . ?
O12 C30 O11 121.4(10) . . ?
O12 C30 C29 118.0(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
O15 H15A O2 0.85 1.86 2.706(12) 179.6 2_675
O15 H15B Cl1 0.85 2.63 3.481(9) 179.9 .
O16 H16B O5 0.85 2.10 2.953(12) 179.5 2_775
O17 H17A O14 0.85 2.13 2.979(14) 179.5 2_676
O17 H17B O8 0.85 1.80 2.651(12) 179.4 2_776
O18 H18B Cl1 0.85 2.58 3.427(11) 179.9 .

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
Cd1 O1 C1 O2 176.7(9) . . . . ?
Cd1 O1 C1 C2 -4.5(17) . . . . ?
Cd1 O3 C7 C2 49.8(12) . . . . ?
Cd1 O3 C7 C6 -128.9(9) . . . . ?
Cd1 O3 C8 C9 -134.6(8) . . . . ?
Cd1 O3 C8 C14 40.2(12) . . . . ?
Cd1 O5 C11 O4 69(2) 2_775 . . . ?
Cd1 O5 C11 C10 -112.3(16) 2_775 . . . ?
Cd1 O6 C15 O7 159.7(8) . . . . ?
Cd1 O6 C15 C14 -19.4(17) . . . . ?
Cd1 O8 C16 O9 160.6(10) . . . . ?
Cd1 O8 C16 C17 -16.4(18) . . . . ?
Cd1 O10 C22 C17 49.6(12) . . . . ?
Cd1 O10 C22 C21 -125.9(10) . . . . ?
Cd1 O10 C23 C24 -139.7(9) . . . . ?
Cd1 O10 C23 C29 39.9(13) . . . . ?
Cd1 O11 C30 O12 -178.4(9) . . . . ?
Cd1 O11 C30 C29 3(2) . . . . ?
Cd2 O4 C11 O5 17.1(13) 2_775 . . . ?
Cd2 O4 C11 C10 -161.2(8) 2_775 . . . ?
Cd2 O11 C30 O12 -0.8(12) . . . . ?
Cd2 O11 C30 C29 -179.5(8) . . . . ?
Cd2 O12 C30 O11 0.7(11) . . . . ?
Cd2 O12 C30 C29 179.5(9) . . . . ?
Cd3 O6 C15 O7 0.7(12) . . . . ?
Cd3 O6 C15 C14 -178.4(9) . . . . ?
Cd3 O7 C15 O6 -0.7(11) . . . . ?
Cd3 O7 C15 C14 178.4(9) . . . . ?
Cd3 O13 C26 O14 7.6(13) 2_676 . . . ?
Cd3 O13 C26 C25 -166.4(11) 2_676 . . . ?
Cd3 O14 C26 O13 -8.9(15) 2_676 . . . ?
Cd3 O14 C26 C25 165.3(9) 2_676 . . . ?
O1 C1 C2 C3 148.3(12) . . . . ?
O1 C1 C2 C7 -28.7(17) . . . . ?
O2 C1 C2 C3 -32.7(17) . . . . ?
O2 C1 C2 C7 150.2(12) . . . . ?
O3 C8 C9 C10 174.8(9) . . . . ?
O3 C8 C14 C13 -175.1(9) . . . . ?
O3 C8 C14 C15 3.6(15) . . . . ?
O8 C16 C17 C18 151.1(13) . . . . ?
O8 C16 C17 C22 -29.5(18) . . . . ?
O9 C16 C17 C18 -26.2(18) . . . . ?
O9 C16 C17 C22 153.3(12) . . . . ?
O10 C23 C24 C25 178.6(10) . . . . ?
O10 C23 C29 C28 -179.1(10) . . . . ?
O10 C23 C29 C30 1.8(15) . . . . ?
C1 C2 C3 C4 -176.7(12) . . . . ?
C1 C2 C7 O3 -0.4(17) . . . . ?
C1 C2 C7 C6 178.2(11) . . . . ?
C2 C3 C4 C5 -3(2) . . . . ?
C3 C2 C7 O3 -177.5(10) . . . . ?
C3 C2 C7 C6 1.2(18) . . . . ?
C3 C4 C5 C6 3(2) . . . . ?
C4 C5 C6 C7 -1(2) . . . . ?
C5 C6 C7 O3 177.7(11) . . . . ?
C5 C6 C7 C2 -1.0(18) . . . . ?
C7 O3 C8 C9 39.0(14) . . . . ?
C7 O3 C8 C14 -146.2(10) . . . . ?
C7 C2 C3 C4 0.6(19) . . . . ?
C8 O3 C7 C2 -124.3(11) . . . . ?
C8 O3 C7 C6 56.9(14) . . . . ?
C8 C9 C10 C11 -178.5(9) . . . . ?
C8 C9 C10 C12 -0.1(16) . . . . ?
C8 C14 C15 O6 -18.7(17) . . . . ?
C8 C14 C15 O7 162.2(11) . . . . ?
C9 C8 C14 C13 -0.4(15) . . . . ?
C9 C8 C14 C15 178.3(10) . . . . ?
C9 C10 C11 O4 -16.5(15) . . . . ?
C9 C10 C11 O5 165.2(10) . . . . ?
C9 C10 C12 C13 0.5(17) . . . . ?
C10 C12 C13 C14 -0.8(17) . . . . ?
C11 C10 C12 C13 178.9(10) . . . . ?
C12 C10 C11 O4 165.1(10) . . . . ?
C12 C10 C11 O5 -13.2(15) . . . . ?
C12 C13 C14 C8 0.8(16) . . . . ?
C12 C13 C14 C15 -178.0(10) . . . . ?
C13 C14 C15 O6 160.0(10) . . . . ?
C13 C14 C15 O7 -19.1(16) . . . . ?
C14 C8 C9 C10 0.1(15) . . . . ?
C16 C17 C18 C19 -177.4(13) . . . . ?
C16 C17 C22 O10 2.9(16) . . . . ?
C16 C17 C22 C21 178.3(11) . . . . ?
C17 C18 C19 C20 -4(2) . . . . ?
C18 C17 C22 O10 -177.7(11) . . . . ?
C18 C17 C22 C21 -2.2(17) . . . . ?
C18 C19 C20 C21 3(2) . . . . ?
C19 C20 C21 C22 -2(2) . . . . ?
C20 C21 C22 O10 177.4(12) . . . . ?
C20 C21 C22 C17 2(2) . . . . ?
C22 O10 C23 C24 16.7(15) . . . . ?
C22 O10 C23 C29 -163.7(10) . . . . ?
C22 C17 C18 C19 3(2) . . . . ?
C23 O10 C22 C17 -110.0(11) . . . . ?
C23 O10 C22 C21 74.5(13) . . . . ?
C23 C24 C25 C26 179.8(11) . . . . ?
C23 C24 C25 C27 0.5(18) . . . . ?
C23 C29 C30 O11 -27.2(16) . . . . ?
C23 C29 C30 O12 154.0(11) . . . . ?
C24 C23 C29 C28 0.5(17) . . . . ?
C24 C23 C29 C30 -178.6(10) . . . . ?
C24 C25 C26 O13 -9.1(18) . . . . ?
C24 C25 C26 O14 176.4(12) . . . . ?
C24 C25 C27 C28 0.4(18) . . . . ?
C25 C27 C28 C29 -1(2) . . . . ?
C26 C25 C27 C28 -179.0(12) . . . . ?
C27 C25 C26 O13 170.2(12) . . . . ?
C27 C25 C26 O14 -4.2(17) . . . . ?
C27 C28 C29 C23 0.4(19) . . . . ?
C27 C28 C29 C30 179.5(12) . . . . ?
C28 C29 C30 O11 153.6(11) . . . . ?
C28 C29 C30 O12 -25.1(16) . . . . ?
C29 C23 C24 C25 -1.0(17) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.144 0.500 0.500 454.7 0.0 ?


_olex2_date_sample_data_collection 2016-06-08
_olex2_submission_special_instructions 'No special instructions were received'

# start Validation Reply Form
_vrf_PLAT420_I                   
;
PROBLEM: D-H Without Acceptor O19 -- H19B ... Please Check
RESPONSE: Due to the disordered solvent water molecules.
;
_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.
;
_vrf_PLAT930_I                   
;
PROBLEM: Check Twin Law ( 0 1 0)[ 1 5 2] Estimated BASF 0.12
RESPONSE: Deu to twin crystal.
;
# 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_282-1cd
_database_code_depnum_ccdc_archive 'CCDC 1509369'
_audit_update_record             
;
2017-03-26 deposited with the CCDC.
2017-04-10 downloaded from the CCDC.
;
_audit_creation_date             2017-03-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(C108 H68 Cd6 N8 O32)'
_chemical_formula_sum            'C54 H34 Cd3 N4 O16'
_chemical_formula_weight         1332.05
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

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

_cell_length_a                   11.6968(4)
_cell_length_b                   16.3288(3)
_cell_length_c                   13.0831(5)
_cell_angle_alpha                90
_cell_angle_beta                 115.442(4)
_cell_angle_gamma                90
_cell_volume                     2256.46(14)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3322
_cell_measurement_temperature    292.80(10)
_cell_measurement_theta_max      27.7960
_cell_measurement_theta_min      3.6620
_shelx_estimated_absorpt_T_max   0.797
_shelx_estimated_absorpt_T_min   0.681
_exptl_absorpt_coefficient_mu    1.487
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91545
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.961
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1316
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_exptl_transmission_factor_max   0.78
_exptl_transmission_factor_min   0.72
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_unetI/netI     0.0589
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7363
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.049
_diffrn_reflns_theta_max         25.049
_diffrn_reflns_theta_min         3.385
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      292.80(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0733
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -39.00   28.20   1.2000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       27.0108  -57.0000 -120.0000 56

#__ type_ start__ end____ width___ exp.time_
  2 omega  -22.00  104.00   1.2000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       27.0108   19.0000   60.0000 105

#__ type_ start__ end____ width___ exp.time_
  3 omega   -6.00   42.00   1.2000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       27.0108   57.0000 -150.0000 40
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0134063000
_diffrn_orient_matrix_UB_12      -0.0293272000
_diffrn_orient_matrix_UB_13      -0.0436844000
_diffrn_orient_matrix_UB_21      -0.0656344000
_diffrn_orient_matrix_UB_22      0.0041228000
_diffrn_orient_matrix_UB_23      -0.0152525000
_diffrn_orient_matrix_UB_31      -0.0037717000
_diffrn_orient_matrix_UB_32      0.0317825000
_diffrn_orient_matrix_UB_33      -0.0383236000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3299
_reflns_number_total             3974
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.598
_refine_diff_density_min         -0.570
_refine_diff_density_rms         0.106
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         3974
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0356
_refine_ls_restrained_S_all      0.997
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0307P)²+0.2985P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0721
_refine_ls_wR_factor_ref         0.0806
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O8(H8A,H8B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C12(H12), C13(H13), C16(H16),
 C17(H17), C18(H18), C21(H21), C22(H22), C25(H25), C26(H26), C27(H27)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.29847(3) 0.41680(2) 1.03610(3) 0.01999(11) Uani 1 1 d . . . . .
Cd2 Cd 0.0000 0.5000 1.0000 0.02802(14) Uani 1 2 d S T P . .
N1 N 0.4206(3) 0.32819(19) 0.9833(3) 0.0235(8) Uani 1 1 d . . . . .
N2 N 0.2950(3) 0.2853(2) 1.1115(3) 0.0243(8) Uani 1 1 d . . . . .
O1 O 0.3614(3) -0.05389(19) 0.7487(3) 0.0384(8) Uani 1 1 d . . . . .
O2 O 0.2046(3) 0.03116(15) 0.6466(2) 0.0211(7) Uani 1 1 d . . . . .
O3 O 0.0540(3) 0.07094(15) 0.7389(3) 0.0248(7) Uani 1 1 d . . . . .
O4 O 0.1206(3) 0.34815(17) 0.9011(3) 0.0336(8) Uani 1 1 d . . . . .
O5 O -0.0419(3) 0.37323(17) 0.9439(3) 0.0328(8) Uani 1 1 d . . . . .
O8 O 0.4911(3) 0.45033(18) 1.1859(3) 0.0346(8) Uani 1 1 d . . . . .
H8A H 0.4832 0.4918 1.2275 0.052 Uiso 1 1 d GR . . . .
H8B H 0.5485 0.4658 1.1614 0.052 Uiso 1 1 d GR . . . .
C1 C 0.2581(4) -0.0210(2) 0.7265(4) 0.0214(10) Uani 1 1 d . . . . .
C2 C 0.1929(4) -0.0431(2) 0.7993(3) 0.0187(9) Uani 1 1 d . . . . .
C3 C 0.2357(4) -0.1119(2) 0.8691(4) 0.0249(10) Uani 1 1 d . . . . .
H3 H 0.3029 -0.1419 0.8683 0.030 Uiso 1 1 calc R . . . .
C4 C 0.1817(5) -0.1366(3) 0.9390(4) 0.0319(11) Uani 1 1 d . . . . .
H4 H 0.2112 -0.1832 0.9836 0.038 Uiso 1 1 calc R . . . .
C5 C 0.0841(5) -0.0921(3) 0.9424(4) 0.0315(11) Uani 1 1 d . . . . .
H5 H 0.0469 -0.1088 0.9891 0.038 Uiso 1 1 calc R . . . .
C6 C 0.0406(4) -0.0221(3) 0.8766(4) 0.0265(10) Uani 1 1 d . . . . .
H6 H -0.0244 0.0087 0.8805 0.032 Uiso 1 1 calc R . . . .
C7 C 0.0938(4) 0.0016(2) 0.8058(3) 0.0183(9) Uani 1 1 d . . . . .
C8 C -0.0263(4) 0.1254(2) 0.7582(3) 0.0183(9) Uani 1 1 d . . . . .
C9 C 0.0280(4) 0.1937(2) 0.8220(4) 0.0216(9) Uani 1 1 d . . . . .
H9 H 0.1151 0.2010 0.8513 0.026 Uiso 1 1 calc R . . . .
C10 C -0.0450(4) 0.2520(2) 0.8432(3) 0.0194(9) Uani 1 1 d . . . . .
C11 C 0.0173(4) 0.3305(2) 0.9016(4) 0.0242(10) Uani 1 1 d . . . . .
C12 C -0.1734(4) 0.2384(2) 0.8036(4) 0.0225(10) Uani 1 1 d . . . . .
H12 H -0.2231 0.2750 0.8213 0.027 Uiso 1 1 calc R . . . .
C13 C -0.2280(4) 0.1704(2) 0.7378(4) 0.0230(10) Uani 1 1 d . . . . .
H13 H -0.3148 0.1624 0.7112 0.028 Uiso 1 1 calc R . . . .
C14 C -0.1573(4) 0.1133(2) 0.7098(4) 0.0199(9) Uani 1 1 d . . . . .
C16 C 0.4856(4) 0.3479(3) 0.9263(4) 0.0292(11) Uani 1 1 d . . . . .
H16 H 0.4992 0.4031 0.9184 0.035 Uiso 1 1 calc R . . . .
C17 C 0.5354(5) 0.2912(3) 0.8772(4) 0.0381(12) Uani 1 1 d . . . . .
H17 H 0.5824 0.3080 0.8389 0.046 Uiso 1 1 calc R . . . .
C18 C 0.5136(5) 0.2107(3) 0.8866(4) 0.0351(12) Uani 1 1 d . . . . .
H18 H 0.5424 0.1718 0.8512 0.042 Uiso 1 1 calc R . . . .
C19 C 0.4480(4) 0.1855(3) 0.9492(4) 0.0260(10) Uani 1 1 d . . . . .
C20 C 0.4041(4) 0.2467(2) 0.9982(4) 0.0234(10) Uani 1 1 d . . . . .
C21 C 0.4224(5) 0.1024(3) 0.9642(4) 0.0348(12) Uani 1 1 d . . . . .
H21 H 0.4481 0.0617 0.9290 0.042 Uiso 1 1 calc R . . . .
C22 C 0.3626(4) 0.0809(2) 1.0272(4) 0.0322(12) Uani 1 1 d . . . . .
H22 H 0.3493 0.0257 1.0359 0.039 Uiso 1 1 calc R . . . .
C23 C 0.3186(4) 0.1414(2) 1.0818(4) 0.0270(10) Uani 1 1 d . . . . .
C24 C 0.3387(4) 0.2251(2) 1.0658(4) 0.0212(10) Uani 1 1 d . . . . .
C25 C 0.2551(5) 0.1232(3) 1.1472(4) 0.0342(12) Uani 1 1 d . . . . .
H25 H 0.2428 0.0688 1.1609 0.041 Uiso 1 1 calc R . . . .
C26 C 0.2102(5) 0.1842(3) 1.1922(4) 0.0381(12) Uani 1 1 d . . . . .
H26 H 0.1665 0.1721 1.2352 0.046 Uiso 1 1 calc R . . . .
C27 C 0.2323(4) 0.2646(3) 1.1711(4) 0.0309(11) Uani 1 1 d . . . . .
H27 H 0.2013 0.3063 1.2006 0.037 Uiso 1 1 calc R . . . .
O6 O 0.1708(3) 0.52232(18) 0.9350(3) 0.0359(8) Uani 1 1 d . . . . .
C15 C 0.2203(4) 0.5456(2) 0.8720(4) 0.0209(9) Uani 1 1 d . . . . .
O7 O 0.3193(3) 0.51399(18) 0.8772(3) 0.0392(9) 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
Cd1 N1 2.336(3) . ?
Cd1 N2 2.371(3) . ?
Cd1 O2 2.320(3) 4_566 ?
Cd1 O4 2.356(3) . ?
Cd1 O8 2.328(3) . ?
Cd1 O6 2.292(3) . ?
Cd2 O2 2.392(3) 4_566 ?
Cd2 O2 2.392(3) 2_556 ?
Cd2 O5 2.181(3) 3_567 ?
Cd2 O5 2.181(3) . ?
Cd2 O6 2.512(3) . ?
Cd2 O6 2.512(3) 3_567 ?
N1 C16 1.313(5) . ?
N1 C20 1.370(5) . ?
N2 C24 1.360(5) . ?
N2 C27 1.323(5) . ?
O1 C1 1.238(5) . ?
O2 Cd1 2.320(3) 4_565 ?
O2 Cd2 2.392(3) 2_546 ?
O2 C1 1.284(5) . ?
O3 C7 1.384(4) . ?
O3 C8 1.393(4) . ?
O4 C11 1.245(5) . ?
O5 C11 1.264(5) . ?
O8 H8A 0.8978 . ?
O8 H8B 0.8954 . ?
C1 C2 1.497(6) . ?
C2 C3 1.397(5) . ?
C2 C7 1.403(5) . ?
C3 H3 0.9300 . ?
C3 C4 1.377(6) . ?
C4 H4 0.9300 . ?
C4 C5 1.370(6) . ?
C5 H5 0.9300 . ?
C5 C6 1.389(6) . ?
C6 H6 0.9300 . ?
C6 C7 1.375(6) . ?
C8 C9 1.375(5) . ?
C8 C14 1.397(6) . ?
C9 H9 0.9300 . ?
C9 C10 1.383(5) . ?
C10 C11 1.511(5) . ?
C10 C12 1.380(6) . ?
C12 H12 0.9300 . ?
C12 C13 1.382(5) . ?
C13 H13 0.9300 . ?
C13 C14 1.396(5) . ?
C14 C15 1.495(5) 2_546 ?
C16 H16 0.9300 . ?
C16 C17 1.390(6) . ?
C17 H17 0.9300 . ?
C17 C18 1.353(6) . ?
C18 H18 0.9300 . ?
C18 C19 1.404(6) . ?
C19 C20 1.400(6) . ?
C19 C21 1.420(6) . ?
C20 C24 1.440(6) . ?
C21 H21 0.9300 . ?
C21 C22 1.337(7) . ?
C22 H22 0.9300 . ?
C22 C23 1.437(6) . ?
C23 C24 1.418(5) . ?
C23 C25 1.385(6) . ?
C25 H25 0.9300 . ?
C25 C26 1.371(6) . ?
C26 H26 0.9300 . ?
C26 C27 1.389(6) . ?
C27 H27 0.9300 . ?
O6 C15 1.252(5) . ?
C15 C14 1.495(5) 2_556 ?
C15 O7 1.242(5) . ?

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
N1 Cd1 N2 71.60(12) . . ?
N1 Cd1 O4 86.50(11) . . ?
O2 Cd1 N1 157.55(11) 4_566 . ?
O2 Cd1 N2 88.55(11) 4_566 . ?
O2 Cd1 O4 98.02(10) 4_566 . ?
O2 Cd1 O8 86.30(11) 4_566 . ?
O4 Cd1 N2 73.36(12) . . ?
O8 Cd1 N1 84.31(12) . . ?
O8 Cd1 N2 92.64(11) . . ?
O8 Cd1 O4 165.15(11) . . ?
O6 Cd1 N1 128.65(11) . . ?
O6 Cd1 N2 142.92(12) . . ?
O6 Cd1 O2 73.67(10) . 4_566 ?
O6 Cd1 O4 77.18(12) . . ?
O6 Cd1 O8 117.65(11) . . ?
O2 Cd2 O2 180.0 4_566 2_556 ?
O2 Cd2 O6 68.61(10) 4_566 . ?
O2 Cd2 O6 111.39(10) 4_566 3_567 ?
O2 Cd2 O6 111.39(10) 2_556 . ?
O2 Cd2 O6 68.61(10) 2_556 3_567 ?
O5 Cd2 O2 94.05(11) . 4_566 ?
O5 Cd2 O2 85.95(11) . 2_556 ?
O5 Cd2 O2 85.95(11) 3_567 4_566 ?
O5 Cd2 O2 94.05(10) 3_567 2_556 ?
O5 Cd2 O5 180.0 3_567 . ?
O5 Cd2 O6 96.89(11) 3_567 3_567 ?
O5 Cd2 O6 83.12(11) 3_567 . ?
O5 Cd2 O6 83.12(11) . 3_567 ?
O5 Cd2 O6 96.88(11) . . ?
O6 Cd2 O6 180.0 . 3_567 ?
C16 N1 Cd1 126.4(3) . . ?
C16 N1 C20 118.0(4) . . ?
C20 N1 Cd1 114.7(3) . . ?
C24 N2 Cd1 113.2(3) . . ?
C27 N2 Cd1 126.2(3) . . ?
C27 N2 C24 118.9(4) . . ?
Cd1 O2 Cd2 99.00(10) 4_565 2_546 ?
C1 O2 Cd1 123.7(3) . 4_565 ?
C1 O2 Cd2 118.8(2) . 2_546 ?
C7 O3 C8 118.5(3) . . ?
C11 O4 Cd1 130.7(3) . . ?
C11 O5 Cd2 125.8(3) . . ?
Cd1 O8 H8A 111.9 . . ?
Cd1 O8 H8B 111.6 . . ?
H8A O8 H8B 107.0 . . ?
O1 C1 O2 124.3(4) . . ?
O1 C1 C2 117.3(4) . . ?
O2 C1 C2 118.3(4) . . ?
C3 C2 C1 118.2(4) . . ?
C3 C2 C7 116.9(4) . . ?
C7 C2 C1 124.9(4) . . ?
C2 C3 H3 118.9 . . ?
C4 C3 C2 122.1(4) . . ?
C4 C3 H3 118.9 . . ?
C3 C4 H4 120.2 . . ?
C5 C4 C3 119.5(4) . . ?
C5 C4 H4 120.2 . . ?
C4 C5 H5 119.8 . . ?
C4 C5 C6 120.3(4) . . ?
C6 C5 H5 119.8 . . ?
C5 C6 H6 120.1 . . ?
C7 C6 C5 119.8(4) . . ?
C7 C6 H6 120.1 . . ?
O3 C7 C2 116.7(3) . . ?
C6 C7 O3 122.0(4) . . ?
C6 C7 C2 121.3(4) . . ?
O3 C8 C14 121.4(4) . . ?
C9 C8 O3 117.2(4) . . ?
C9 C8 C14 121.3(4) . . ?
C8 C9 H9 119.5 . . ?
C8 C9 C10 121.1(4) . . ?
C10 C9 H9 119.5 . . ?
C9 C10 C11 118.7(4) . . ?
C12 C10 C9 118.7(4) . . ?
C12 C10 C11 122.4(4) . . ?
O4 C11 O5 126.2(4) . . ?
O4 C11 C10 116.8(4) . . ?
O5 C11 C10 117.0(4) . . ?
C10 C12 H12 120.0 . . ?
C10 C12 C13 120.0(4) . . ?
C13 C12 H12 120.0 . . ?
C12 C13 H13 118.9 . . ?
C12 C13 C14 122.2(4) . . ?
C14 C13 H13 118.9 . . ?
C8 C14 C15 122.4(4) . 2_546 ?
C13 C14 C8 116.4(4) . . ?
C13 C14 C15 121.1(4) . 2_546 ?
N1 C16 H16 118.0 . . ?
N1 C16 C17 124.0(4) . . ?
C17 C16 H16 118.0 . . ?
C16 C17 H17 120.9 . . ?
C18 C17 C16 118.1(4) . . ?
C18 C17 H17 120.9 . . ?
C17 C18 H18 119.7 . . ?
C17 C18 C19 120.6(4) . . ?
C19 C18 H18 119.7 . . ?
C18 C19 C21 124.2(4) . . ?
C20 C19 C18 117.2(4) . . ?
C20 C19 C21 118.6(4) . . ?
N1 C20 C19 121.8(4) . . ?
N1 C20 C24 118.0(4) . . ?
C19 C20 C24 120.1(4) . . ?
C19 C21 H21 118.9 . . ?
C22 C21 C19 122.2(4) . . ?
C22 C21 H21 118.9 . . ?
C21 C22 H22 119.3 . . ?
C21 C22 C23 121.3(4) . . ?
C23 C22 H22 119.3 . . ?
C24 C23 C22 118.1(4) . . ?
C25 C23 C22 124.2(4) . . ?
C25 C23 C24 117.7(4) . . ?
N2 C24 C20 119.5(3) . . ?
N2 C24 C23 121.0(4) . . ?
C23 C24 C20 119.5(4) . . ?
C23 C25 H25 119.5 . . ?
C26 C25 C23 121.1(4) . . ?
C26 C25 H25 119.5 . . ?
C25 C26 H26 121.2 . . ?
C25 C26 C27 117.6(4) . . ?
C27 C26 H26 121.2 . . ?
N2 C27 C26 123.8(4) . . ?
N2 C27 H27 118.1 . . ?
C26 C27 H27 118.1 . . ?
Cd1 O6 Cd2 96.39(10) . . ?
C15 O6 Cd1 103.7(3) . . ?
C15 O6 Cd2 158.0(3) . . ?
O6 C15 C14 118.0(4) . 2_556 ?
O7 C15 C14 120.5(4) . 2_556 ?
O7 C15 O6 121.4(4) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O8 H8A O1 0.90 1.86 2.628(4) 141.7 4_566
O8 H8B O7 0.90 1.85 2.741(5) 172.1 3_667

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 N1 C16 C17 -166.3(4) . . . . ?
Cd1 N1 C20 C19 166.0(3) . . . . ?
Cd1 N1 C20 C24 -13.6(5) . . . . ?
Cd1 N2 C24 C20 12.4(5) . . . . ?
Cd1 N2 C24 C23 -166.2(3) . . . . ?
Cd1 N2 C27 C26 165.2(4) . . . . ?
Cd1 O2 C1 O1 -5.4(6) 4_565 . . . ?
Cd1 O2 C1 C2 173.8(2) 4_565 . . . ?
Cd1 O4 C11 O5 34.9(6) . . . . ?
Cd1 O4 C11 C10 -147.1(3) . . . . ?
Cd1 O6 C15 C14 178.0(3) . . . 2_556 ?
Cd1 O6 C15 O7 -2.4(5) . . . . ?
Cd2 O2 C1 O1 120.1(4) 2_546 . . . ?
Cd2 O2 C1 C2 -60.7(4) 2_546 . . . ?
Cd2 O5 C11 O4 12.2(6) . . . . ?
Cd2 O5 C11 C10 -165.8(3) . . . . ?
Cd2 O6 C15 C14 22.9(10) . . . 2_556 ?
Cd2 O6 C15 O7 -157.5(5) . . . . ?
N1 C16 C17 C18 1.3(8) . . . . ?
N1 C20 C24 N2 0.6(6) . . . . ?
N1 C20 C24 C23 179.2(4) . . . . ?
O1 C1 C2 C3 -14.5(6) . . . . ?
O1 C1 C2 C7 163.3(4) . . . . ?
O2 C1 C2 C3 166.3(4) . . . . ?
O2 C1 C2 C7 -15.9(6) . . . . ?
O3 C8 C9 C10 178.5(4) . . . . ?
O3 C8 C14 C13 178.1(4) . . . . ?
O3 C8 C14 C15 -4.7(6) . . . 2_546 ?
C1 C2 C3 C4 179.8(4) . . . . ?
C1 C2 C7 O3 0.4(6) . . . . ?
C1 C2 C7 C6 -178.7(4) . . . . ?
C2 C3 C4 C5 -1.2(7) . . . . ?
C3 C2 C7 O3 178.2(3) . . . . ?
C3 C2 C7 C6 -0.8(6) . . . . ?
C3 C4 C5 C6 -0.5(7) . . . . ?
C4 C5 C6 C7 1.5(7) . . . . ?
C5 C6 C7 O3 -179.7(4) . . . . ?
C5 C6 C7 C2 -0.8(6) . . . . ?
C7 O3 C8 C9 98.9(4) . . . . ?
C7 O3 C8 C14 -84.5(5) . . . . ?
C7 C2 C3 C4 1.8(6) . . . . ?
C8 O3 C7 C2 -167.9(4) . . . . ?
C8 O3 C7 C6 11.1(6) . . . . ?
C8 C9 C10 C11 -172.7(4) . . . . ?
C8 C9 C10 C12 3.0(6) . . . . ?
C9 C8 C14 C13 -5.4(6) . . . . ?
C9 C8 C14 C15 171.8(4) . . . 2_546 ?
C9 C10 C11 O4 18.2(6) . . . . ?
C9 C10 C11 O5 -163.5(4) . . . . ?
C9 C10 C12 C13 -4.2(6) . . . . ?
C10 C12 C13 C14 0.5(6) . . . . ?
C11 C10 C12 C13 171.4(4) . . . . ?
C12 C10 C11 O4 -157.3(4) . . . . ?
C12 C10 C11 O5 20.9(6) . . . . ?
C12 C13 C14 C8 4.2(6) . . . . ?
C12 C13 C14 C15 -173.0(4) . . . 2_546 ?
C14 C8 C9 C10 1.9(6) . . . . ?
C16 N1 C20 C19 -3.7(6) . . . . ?
C16 N1 C20 C24 176.7(4) . . . . ?
C16 C17 C18 C19 -3.2(8) . . . . ?
C17 C18 C19 C20 1.6(7) . . . . ?
C17 C18 C19 C21 -179.3(5) . . . . ?
C18 C19 C20 N1 1.9(6) . . . . ?
C18 C19 C20 C24 -178.5(4) . . . . ?
C18 C19 C21 C22 178.1(5) . . . . ?
C19 C20 C24 N2 -179.1(4) . . . . ?
C19 C20 C24 C23 -0.4(6) . . . . ?
C19 C21 C22 C23 1.2(7) . . . . ?
C20 N1 C16 C17 2.1(7) . . . . ?
C20 C19 C21 C22 -2.9(7) . . . . ?
C21 C19 C20 N1 -177.2(4) . . . . ?
C21 C19 C20 C24 2.4(6) . . . . ?
C21 C22 C23 C24 0.8(7) . . . . ?
C21 C22 C23 C25 179.4(5) . . . . ?
C22 C23 C24 N2 177.4(4) . . . . ?
C22 C23 C24 C20 -1.2(6) . . . . ?
C22 C23 C25 C26 -176.7(5) . . . . ?
C23 C25 C26 C27 -1.0(7) . . . . ?
C24 N2 C27 C26 1.4(7) . . . . ?
C24 C23 C25 C26 1.9(7) . . . . ?
C25 C23 C24 N2 -1.2(6) . . . . ?
C25 C23 C24 C20 -179.9(4) . . . . ?
C25 C26 C27 N2 -0.7(8) . . . . ?
C27 N2 C24 C20 178.3(4) . . . . ?
C27 N2 C24 C23 -0.3(6) . . . . ?

_olex2_date_sample_data_collection 2016-06-09
_olex2_submission_special_instructions 'No special instructions were received'

# start Validation Reply Form
_vrf_PLAT910_I                   
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min) 10 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
