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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
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data_310-1Cd
_database_code_depnum_ccdc_archive 'CCDC 1589514'
_audit_update_record             
;
2017-12-06 deposited with the CCDC.
2018-04-30 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            'C15 H17 Cd N O13'
_chemical_formula_weight         531.70

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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

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

_cell_length_a                   8.1880(4)
_cell_length_b                   9.5193(5)
_cell_length_c                   12.5867(8)
_cell_angle_alpha                91.511(5)
_cell_angle_beta                 101.114(5)
_cell_angle_gamma                98.054(4)
_cell_volume                     951.73(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5900
_cell_measurement_theta_min      3.322
_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    1.855
_exptl_crystal_F_000             532
_exptl_transmission_factor_min   0.746
_exptl_transmission_factor_max   0.755
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.240
_exptl_absorpt_coefficient_mu    1.220
_shelx_estimated_absorpt_T_min   0.734
_shelx_estimated_absorpt_T_max   0.758
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.734
_exptl_absorpt_correction_T_max  0.758
_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            5900
_diffrn_reflns_av_unetI/netI     0.0564
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.322
_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             3365
_reflns_number_gt                2836
_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)+(0.0380P)²+1.1692P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3365
_refine_ls_number_parameters     282
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0404
_refine_ls_wR_factor_ref         0.0983
_refine_ls_wR_factor_gt          0.0884
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.32129(4) 0.74127(4) -0.00074(3) 0.03177(14) Uani 1 1 d . . . . .
N1 N -0.0466(5) 0.0512(4) 0.6905(3) 0.0304(9) Uani 1 1 d . . . . .
O1 O 0.3609(4) 0.5614(4) 0.1132(3) 0.0398(9) Uani 1 1 d . . . . .
O2 O 0.1966(4) 0.6885(4) 0.1817(3) 0.0418(9) Uani 1 1 d . . . . .
O3 O 0.2619(5) 0.4798(4) 0.6560(3) 0.0430(9) Uani 1 1 d . . . . .
O4 O 0.1594(5) 0.6452(4) 0.5542(3) 0.0418(10) Uani 1 1 d . . . . .
O5 O 0.1340(4) -0.2264(3) 0.7344(3) 0.0351(8) Uani 1 1 d . . . . .
O6 O 0.3179(4) -0.0951(3) 0.8645(3) 0.0380(8) Uani 1 1 d . . . . .
O7 O -0.0421(5) 0.0085(4) 0.7825(3) 0.0475(10) Uani 1 1 d . . . . .
O8 O -0.1741(4) 0.0732(4) 0.6306(3) 0.0462(10) Uani 1 1 d . . . . .
O9 O 0.6051(4) 0.8292(4) 0.0373(3) 0.0431(9) Uani 1 1 d . . . . .
H1W H 0.6630 0.7615 0.0529 0.065 Uiso 1 1 d R U . . .
H2W H 0.6268 0.8902 0.0914 0.065 Uiso 1 1 d R U . . .
O10 O 0.3644(4) 0.5696(4) -0.1252(3) 0.0405(9) Uani 1 1 d . . . . .
H3W H 0.4675 0.5538 -0.1106 0.061 Uiso 1 1 d R U . . .
H4W H 0.3435 0.5992 -0.1900 0.061 Uiso 1 1 d R U . . .
O11 O 0.3038(5) 0.9483(4) 0.0957(3) 0.0584(11) Uani 1 1 d . . . . .
H5W H 0.2055 0.9444 0.1135 0.088 Uiso 1 1 d R U . . .
H6W H 0.3183 1.0215 0.0566 0.088 Uiso 1 1 d R U . . .
O12 O 0.0492(4) 0.6559(4) -0.0798(3) 0.0533(11) Uani 1 1 d . . . . .
H8W H 0.0214 0.6901 -0.1438 0.080 Uiso 1 1 d R U . . .
H7W H -0.0197 0.6802 -0.0396 0.080 Uiso 1 1 d R U . . .
O13 O 0.8587(5) 0.6713(4) 0.0791(4) 0.0560(11) Uani 1 1 d G . . . .
H10W H 0.9530 0.6873 0.1230 0.084 Uiso 1 1 d G U . . .
H9W H 0.8079 0.5900 0.0891 0.084 Uiso 1 1 d G U . . .
C1 C 0.2799(6) 0.5881(5) 0.1858(4) 0.0300(11) Uani 1 1 d . . . . .
C2 C 0.2846(5) 0.4941(5) 0.2797(4) 0.0251(10) Uani 1 1 d . . . . .
C3 C 0.3290(6) 0.3587(5) 0.2752(4) 0.0282(10) Uani 1 1 d . . . . .
H3 H 0.3584 0.3245 0.2127 0.034 Uiso 1 1 calc R U . . .
C4 C 0.3299(6) 0.2747(5) 0.3627(4) 0.0279(10) Uani 1 1 d . . . . .
H4 H 0.3587 0.1840 0.3576 0.033 Uiso 1 1 calc R U . . .
C5 C 0.2889(5) 0.3217(4) 0.4589(3) 0.0206(9) Uani 1 1 d . . . . .
C6 C 0.2507(5) 0.4612(4) 0.4659(3) 0.0208(9) Uani 1 1 d . . . . .
C7 C 0.2246(5) 0.5273(5) 0.5683(4) 0.0236(10) Uani 1 1 d . . . . .
C8 C 0.2461(5) 0.5433(5) 0.3751(3) 0.0224(9) Uani 1 1 d . . . . .
H8 H 0.2162 0.6337 0.3790 0.027 Uiso 1 1 calc R U . . .
C9 C 0.2775(5) 0.2186(4) 0.5448(3) 0.0216(9) Uani 1 1 d . . . . .
C10 C 0.4115(6) 0.1481(5) 0.5869(4) 0.0293(11) Uani 1 1 d . . . . .
H10 H 0.5133 0.1702 0.5644 0.035 Uiso 1 1 calc R U . . .
C11 C 0.3957(6) 0.0455(5) 0.6619(4) 0.0305(11) Uani 1 1 d . . . . .
H11 H 0.4881 0.0017 0.6901 0.037 Uiso 1 1 calc R U . . .
C12 C 0.2454(6) 0.0068(4) 0.6958(4) 0.0243(10) Uani 1 1 d . . . . .
C13 C 0.2288(6) -0.1150(5) 0.7705(4) 0.0256(10) Uani 1 1 d . . . . .
C14 C 0.1130(5) 0.0787(4) 0.6527(4) 0.0223(9) Uani 1 1 d . . . . .
C15 C 0.1268(5) 0.1817(5) 0.5799(4) 0.0250(10) Uani 1 1 d . . . . .
H15 H 0.0350 0.2274 0.5537 0.030 Uiso 1 1 calc R U . . .
H1 H 0.155(7) 0.690(6) 0.606(5) 0.051(19) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 O12 2.283(3) . ?
Cd1 O1 2.280(3) . ?
Cd1 O9 2.310(3) . ?
Cd1 O11 2.324(4) . ?
Cd1 O6 2.332(3) 1_564 ?
Cd1 O10 2.343(3) . ?
N1 O8 1.212(5) . ?
N1 O7 1.233(5) . ?
N1 C14 1.467(5) . ?
O1 C1 1.268(6) . ?
O2 C1 1.246(6) . ?
O3 C7 1.205(5) . ?
O4 C7 1.311(5) . ?
O5 C13 1.242(5) . ?
O6 C13 1.259(5) . ?
O6 Cd1 2.332(3) 1_546 ?
C1 C2 1.499(6) . ?
C2 C8 1.386(6) . ?
C2 C3 1.390(6) . ?
C3 C4 1.377(6) . ?
C4 C5 1.396(6) . ?
C5 C6 1.411(6) . ?
C5 C9 1.487(6) . ?
C6 C8 1.398(6) . ?
C6 C7 1.484(6) . ?
C9 C15 1.392(6) . ?
C9 C10 1.391(6) . ?
C10 C11 1.387(6) . ?
C11 C12 1.384(6) . ?
C12 C14 1.392(6) . ?
C12 C13 1.520(6) . ?
C14 C15 1.368(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O12 Cd1 O1 96.53(13) . . ?
O12 Cd1 O9 166.44(14) . . ?
O1 Cd1 O9 91.69(13) . . ?
O12 Cd1 O11 104.41(16) . . ?
O1 Cd1 O11 110.54(14) . . ?
O9 Cd1 O11 82.60(14) . . ?
O12 Cd1 O6 87.45(13) . 1_564 ?
O1 Cd1 O6 168.36(13) . 1_564 ?
O9 Cd1 O6 82.50(12) . 1_564 ?
O11 Cd1 O6 78.83(13) . 1_564 ?
O12 Cd1 O10 79.78(14) . . ?
O1 Cd1 O10 81.20(12) . . ?
O9 Cd1 O10 90.90(13) . . ?
O11 Cd1 O10 166.63(12) . . ?
O6 Cd1 O10 88.78(12) 1_564 . ?
O8 N1 O7 123.9(4) . . ?
O8 N1 C14 118.5(4) . . ?
O7 N1 C14 117.6(4) . . ?
C1 O1 Cd1 102.9(3) . . ?
C13 O6 Cd1 125.1(3) . 1_546 ?
O2 C1 O1 122.6(4) . . ?
O2 C1 C2 119.1(4) . . ?
O1 C1 C2 118.3(4) . . ?
C8 C2 C3 118.3(4) . . ?
C8 C2 C1 119.5(4) . . ?
C3 C2 C1 122.2(4) . . ?
C4 C3 C2 120.6(4) . . ?
C3 C4 C5 121.9(4) . . ?
C4 C5 C6 118.0(4) . . ?
C4 C5 C9 117.9(4) . . ?
C6 C5 C9 124.0(4) . . ?
C8 C6 C5 119.1(4) . . ?
C8 C6 C7 118.5(4) . . ?
C5 C6 C7 122.2(4) . . ?
O3 C7 O4 122.9(4) . . ?
O3 C7 C6 124.0(4) . . ?
O4 C7 C6 113.1(4) . . ?
C2 C8 C6 122.1(4) . . ?
C15 C9 C10 117.7(4) . . ?
C15 C9 C5 120.5(4) . . ?
C10 C9 C5 121.6(4) . . ?
C11 C10 C9 121.1(4) . . ?
C10 C11 C12 121.4(4) . . ?
C11 C12 C14 116.5(4) . . ?
C11 C12 C13 119.8(4) . . ?
C14 C12 C13 123.6(4) . . ?
O5 C13 O6 125.1(4) . . ?
O5 C13 C12 118.6(4) . . ?
O6 C13 C12 116.3(4) . . ?
C15 C14 C12 122.9(4) . . ?
C15 C14 N1 117.2(4) . . ?
C12 C14 N1 119.8(4) . . ?
C14 C15 C9 120.3(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
Cd1 O1 C1 O2 3.3(5) . . . . ?
Cd1 O1 C1 C2 -177.0(3) . . . . ?
O2 C1 C2 C8 -20.9(6) . . . . ?
O1 C1 C2 C8 159.4(4) . . . . ?
O2 C1 C2 C3 160.1(4) . . . . ?
O1 C1 C2 C3 -19.6(6) . . . . ?
C8 C2 C3 C4 1.8(6) . . . . ?
C1 C2 C3 C4 -179.2(4) . . . . ?
C2 C3 C4 C5 -0.8(7) . . . . ?
C3 C4 C5 C6 -1.9(6) . . . . ?
C3 C4 C5 C9 174.3(4) . . . . ?
C4 C5 C6 C8 3.6(6) . . . . ?
C9 C5 C6 C8 -172.3(4) . . . . ?
C4 C5 C6 C7 -172.9(4) . . . . ?
C9 C5 C6 C7 11.2(6) . . . . ?
C8 C6 C7 O3 -162.9(4) . . . . ?
C5 C6 C7 O3 13.6(7) . . . . ?
C8 C6 C7 O4 15.8(6) . . . . ?
C5 C6 C7 O4 -167.7(4) . . . . ?
C3 C2 C8 C6 0.0(6) . . . . ?
C1 C2 C8 C6 -179.1(4) . . . . ?
C5 C6 C8 C2 -2.7(6) . . . . ?
C7 C6 C8 C2 173.9(4) . . . . ?
C4 C5 C9 C15 -118.9(5) . . . . ?
C6 C5 C9 C15 57.0(6) . . . . ?
C4 C5 C9 C10 56.3(6) . . . . ?
C6 C5 C9 C10 -127.8(5) . . . . ?
C15 C9 C10 C11 -0.5(7) . . . . ?
C5 C9 C10 C11 -175.8(4) . . . . ?
C9 C10 C11 C12 1.6(7) . . . . ?
C10 C11 C12 C14 -1.6(7) . . . . ?
C10 C11 C12 C13 174.6(4) . . . . ?
Cd1 O6 C13 O5 -2.7(7) 1_546 . . . ?
Cd1 O6 C13 C12 179.5(3) 1_546 . . . ?
C11 C12 C13 O5 -111.7(5) . . . . ?
C14 C12 C13 O5 64.2(6) . . . . ?
C11 C12 C13 O6 66.3(6) . . . . ?
C14 C12 C13 O6 -117.8(5) . . . . ?
C11 C12 C14 C15 0.6(7) . . . . ?
C13 C12 C14 C15 -175.5(4) . . . . ?
C11 C12 C14 N1 -175.6(4) . . . . ?
C13 C12 C14 N1 8.4(7) . . . . ?
O8 N1 C14 C15 28.7(6) . . . . ?
O7 N1 C14 C15 -150.4(4) . . . . ?
O8 N1 C14 C12 -154.9(4) . . . . ?
O7 N1 C14 C12 25.9(6) . . . . ?
C12 C14 C15 C9 0.5(7) . . . . ?
N1 C14 C15 C9 176.7(4) . . . . ?
C10 C9 C15 C14 -0.5(7) . . . . ?
C5 C9 C15 C14 174.9(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
O4 H1 O5 0.78(6) 1.83(6) 2.606(5) 173(6) 1_565
C15 H15 O4 0.93 2.38 3.280(6) 163.9 2_566
O13 H9W O12 0.85 2.77 3.305(6) 122.6 2_665
O13 H9W O10 0.85 2.05 2.869(5) 162.9 2_665
O13 H10W O2 0.85 1.99 2.799(5) 159.3 1_655
O12 H7W O13 0.88 1.95 2.776(6) 157.4 1_455
O12 H8W O5 0.88 2.06 2.784(5) 139.5 1_564
O11 H6W O9 0.87 1.98 2.841(5) 167.6 2_675
O11 H5W O7 0.87 2.13 2.931(5) 153.3 2_566
O10 H4W O5 0.86 2.62 3.221(5) 127.9 1_564
O10 H4W O3 0.86 2.16 2.794(5) 129.8 1_554
O10 H3W O1 0.86 1.90 2.702(5) 153.0 2_665
O9 H2W O6 0.86 1.98 2.724(5) 144.6 2_666
O9 H1W O13 0.86 1.90 2.710(5) 156.9 .
O4 H1 O5 0.78(6) 1.83(6) 2.606(5) 173(6) 1_565
C15 H15 O4 0.93 2.38 3.280(6) 163.9 2_566
O13 H9W O12 0.85 2.77 3.305(6) 122.6 2_665
O13 H9W O10 0.85 2.05 2.869(5) 162.9 2_665
O13 H10W O2 0.85 1.99 2.799(5) 159.3 1_655
O12 H7W O13 0.88 1.95 2.776(6) 157.4 1_455
O12 H8W O5 0.88 2.06 2.784(5) 139.5 1_564
O11 H6W O9 0.87 1.98 2.841(5) 167.6 2_675
O11 H5W O7 0.87 2.13 2.931(5) 153.3 2_566
O10 H4W O5 0.86 2.62 3.221(5) 127.9 1_564
O10 H4W O3 0.86 2.16 2.794(5) 129.8 1_554
O10 H3W O1 0.86 1.90 2.702(5) 153.0 2_665
O9 H2W O6 0.86 1.98 2.724(5) 144.6 2_666
O9 H1W O13 0.86 1.90 2.710(5) 156.9 .
O9 H1W O13 0.86 1.90 2.710(5) 156.9 .
O9 H2W O6 0.86 1.98 2.724(5) 144.6 2_666
O10 H3W O1 0.86 1.90 2.702(5) 153.0 2_665
O10 H4W O3 0.86 2.16 2.794(5) 129.8 1_554
O10 H4W O5 0.86 2.62 3.221(5) 127.9 1_564
O11 H5W O7 0.87 2.13 2.931(5) 153.3 2_566
O11 H6W O9 0.87 1.98 2.841(5) 167.6 2_675
O12 H8W O5 0.88 2.06 2.784(5) 139.5 1_564
O12 H7W O13 0.88 1.95 2.776(6) 157.4 1_455
O13 H10W O2 0.85 1.99 2.799(5) 159.3 1_655
O13 H9W O10 0.85 2.05 2.869(5) 162.9 2_665
C15 H15 O4 0.93 2.38 3.280(6) 163.9 2_566
O4 H1 O5 0.78(6) 1.83(6) 2.606(5) 173(6) 1_565
O9 H1W O13 0.86 1.90 2.710(5) 156.9 .
O9 H2W O6 0.86 1.98 2.724(5) 144.6 2_666
O10 H3W O1 0.86 1.90 2.702(5) 153.0 2_665
O10 H4W O3 0.86 2.16 2.794(5) 129.8 1_554
O10 H4W O5 0.86 2.62 3.221(5) 127.9 1_564
O11 H5W O7 0.87 2.13 2.931(5) 153.3 2_566
O11 H6W O9 0.87 1.98 2.841(5) 167.6 2_675
O12 H8W O5 0.88 2.06 2.784(5) 139.5 1_564
O12 H7W O13 0.88 1.95 2.776(6) 157.4 1_455
O13 H10W O2 0.85 1.99 2.799(5) 159.3 1_655
O13 H9W O10 0.85 2.05 2.869(5) 162.9 2_665
C15 H15 O4 0.93 2.38 3.280(6) 163.9 2_566
O4 H1 O5 0.78(6) 1.83(6) 2.606(5) 173(6) 1_565

_refine_diff_density_max         1.399
_refine_diff_density_min         -0.876
_refine_diff_density_rms         0.102

####################################################################### 
# 
# 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_315-9Cd
_database_code_depnum_ccdc_archive 'CCDC 1589519'
_audit_update_record             
;
2017-12-06 deposited with the CCDC.
2018-04-30 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 Cd3 N6 O17'
_chemical_formula_weight         1324.00

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      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                   13.0611(7)
_cell_length_b                   14.1389(7)
_cell_length_c                   14.3715(7)
_cell_angle_alpha                102.999(4)
_cell_angle_beta                 98.038(4)
_cell_angle_gamma                110.742(5)
_cell_volume                     2347.2(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    14642
_cell_measurement_theta_min      3.344
_cell_measurement_theta_max      25.050

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.873
_exptl_crystal_F_000             1304
_exptl_transmission_factor_min   0.704
_exptl_transmission_factor_max   0.751
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    1.432
_shelx_estimated_absorpt_T_min   0.690
_shelx_estimated_absorpt_T_max   0.763
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.690
_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            14642
_diffrn_reflns_av_unetI/netI     0.0543
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.344
_diffrn_reflns_theta_max         25.050
_diffrn_reflns_theta_full        25.050
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             8300
_reflns_number_gt                6491
_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)+(0.0161P)²+0.8015P] 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         8300
_refine_ls_number_parameters     686
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0339
_refine_ls_wR_factor_ref         0.0662
_refine_ls_wR_factor_gt          0.0577
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_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 0.33802(3) -0.07666(2) 0.21162(2) 0.02735(9) Uani 1 1 d . . . . .
Cd2 Cd 0.37763(3) -0.29938(3) 0.23842(2) 0.03164(9) Uani 1 1 d . . . . .
Cd3 Cd 0.25184(3) 0.18989(3) 0.23567(2) 0.03001(9) Uani 1 1 d . . . . .
N1 N 0.9176(3) -0.2444(3) 0.4585(3) 0.0417(10) Uani 1 1 d . . . . .
N2 N 0.8006(4) 0.4843(3) 0.1379(3) 0.0458(10) Uani 1 1 d . . . . .
N3 N 0.2392(3) -0.4277(3) 0.2793(2) 0.0355(9) Uani 1 1 d . . . . .
N4 N 0.4614(3) -0.3877(3) 0.3137(3) 0.0373(9) Uani 1 1 d . . . . .
N5 N 0.1050(3) 0.2349(3) 0.1751(2) 0.0324(8) Uani 1 1 d . . . . .
N6 N 0.3076(3) 0.2939(3) 0.1313(2) 0.0348(9) Uani 1 1 d . . . . .
O1 O 0.5169(2) -0.0537(2) 0.2039(2) 0.0379(8) Uani 1 1 d . . . . .
O2 O 0.5487(2) -0.1875(2) 0.2415(2) 0.0428(8) Uani 1 1 d . . . . .
O3 O 0.8118(2) -0.0373(2) -0.11233(18) 0.0340(7) Uani 1 1 d . . . . .
O4 O 0.6737(2) 0.0135(2) -0.08114(19) 0.0370(8) Uani 1 1 d . . . . .
O5 O 0.7538(3) -0.2433(2) 0.5996(2) 0.0393(8) Uani 1 1 d . . . . .
O6 O 0.8630(3) -0.0760(2) 0.6838(2) 0.0402(8) Uani 1 1 d . . . . .
O7 O 0.9089(3) -0.3200(3) 0.3919(3) 0.0670(11) Uani 1 1 d . . . . .
O8 O 0.9679(3) -0.2244(3) 0.5435(2) 0.0651(11) Uani 1 1 d . . . . .
O9 O 0.3869(2) 0.0807(2) 0.32548(19) 0.0340(7) Uani 1 1 d . . . . .
O10 O 0.4387(2) 0.2305(2) 0.2855(2) 0.0371(7) Uani 1 1 d . . . . .
O11 O 0.6582(2) 0.1657(2) 0.66771(18) 0.0315(7) Uani 1 1 d . . . . .
O12 O 0.8270(3) 0.1805(3) 0.6424(2) 0.0515(9) Uani 1 1 d . . . . .
O13 O 0.6470(3) 0.3770(3) -0.0662(2) 0.0474(9) Uani 1 1 d . . . . .
O14 O 0.7054(3) 0.2491(2) -0.10660(19) 0.0366(7) Uani 1 1 d . . . . .
O15 O 0.7912(4) 0.5605(3) 0.1892(3) 0.0909(16) Uani 1 1 d . . . . .
O16 O 0.8642(3) 0.4900(3) 0.0835(3) 0.0727(12) Uani 1 1 d . . . . .
O17 O 0.1482(2) -0.1306(3) 0.1929(2) 0.0448(8) Uani 1 1 d . . . . .
H1W H 0.1261 -0.0813 0.1828 0.067 Uiso 1 1 d R U . . .
H2W H 0.1293 -0.1447 0.2458 0.067 Uiso 1 1 d R U . . .
C1 C 0.5748(3) -0.1071(3) 0.2123(3) 0.0272(9) Uani 1 1 d . . . . .
C2 C 0.6822(3) -0.0764(3) 0.1763(3) 0.0252(9) Uani 1 1 d . . . . .
C3 C 0.7818(3) -0.0822(3) 0.2214(3) 0.0263(9) Uani 1 1 d . . . . .
C4 C 0.8683(3) -0.0689(3) 0.1719(3) 0.0326(10) Uani 1 1 d . . . . .
H4 H 0.9350 -0.0718 0.2010 0.039 Uiso 1 1 calc R U . . .
C5 C 0.8574(3) -0.0517(3) 0.0813(3) 0.0300(10) Uani 1 1 d . . . . .
H5 H 0.9149 -0.0464 0.0486 0.036 Uiso 1 1 calc R U . . .
C6 C 0.7612(3) -0.0422(3) 0.0386(3) 0.0238(9) Uani 1 1 d . . . . .
C7 C 0.7476(3) -0.0202(3) -0.0580(3) 0.0267(9) Uani 1 1 d . . . . .
C8 C 0.6753(3) -0.0528(3) 0.0883(3) 0.0260(9) Uani 1 1 d . . . . .
H8 H 0.6116 -0.0438 0.0613 0.031 Uiso 1 1 calc R U . . .
C9 C 0.7996(3) -0.0963(3) 0.3211(3) 0.0286(10) Uani 1 1 d . . . . .
C10 C 0.8502(3) -0.1624(3) 0.3431(3) 0.0323(10) Uani 1 1 d . . . . .
H10 H 0.8755 -0.1984 0.2953 0.039 Uiso 1 1 calc R U . . .
C11 C 0.8630(3) -0.1746(4) 0.4365(3) 0.0315(10) Uani 1 1 d . . . . .
C12 C 0.8250(4) -0.1248(3) 0.5092(3) 0.0314(10) Uani 1 1 d . . . . .
C13 C 0.8158(4) -0.1505(4) 0.6053(3) 0.0340(11) Uani 1 1 d . . . . .
C14 C 0.7786(4) -0.0551(4) 0.4876(3) 0.0425(12) Uani 1 1 d . . . . .
H14 H 0.7554 -0.0175 0.5360 0.051 Uiso 1 1 calc R U . . .
C15 C 0.7668(4) -0.0414(4) 0.3960(3) 0.0383(11) Uani 1 1 d . . . . .
H15 H 0.7360 0.0059 0.3835 0.046 Uiso 1 1 calc R U . . .
C16 C 0.4597(3) 0.1660(3) 0.3246(3) 0.0264(10) Uani 1 1 d . . . . .
C17 C 0.5807(3) 0.1983(3) 0.3784(3) 0.0225(9) Uani 1 1 d . . . . .
C18 C 0.6734(3) 0.2499(3) 0.3417(3) 0.0259(9) Uani 1 1 d . . . . .
C19 C 0.7810(3) 0.2791(4) 0.3987(3) 0.0374(11) Uani 1 1 d . . . . .
H19 H 0.8428 0.3139 0.3760 0.045 Uiso 1 1 calc R U . . .
C20 C 0.7998(4) 0.2588(4) 0.4870(3) 0.0350(11) Uani 1 1 d . . . . .
H20 H 0.8731 0.2790 0.5227 0.042 Uiso 1 1 calc R U . . .
C21 C 0.7082(3) 0.2077(3) 0.5230(3) 0.0264(9) Uani 1 1 d . . . . .
C22 C 0.7347(4) 0.1835(3) 0.6184(3) 0.0304(10) Uani 1 1 d . . . . .
C23 C 0.6002(3) 0.1785(3) 0.4685(3) 0.0267(9) Uani 1 1 d . . . . .
H23 H 0.5391 0.1447 0.4924 0.032 Uiso 1 1 calc R U . . .
C24 C 0.6643(3) 0.2671(3) 0.2427(3) 0.0261(9) Uani 1 1 d . . . . .
C25 C 0.7242(3) 0.3672(3) 0.2341(3) 0.0305(10) Uani 1 1 d . . . . .
H25 H 0.7602 0.4253 0.2899 0.037 Uiso 1 1 calc R U . . .
C26 C 0.7292(3) 0.3788(3) 0.1420(3) 0.0279(9) Uani 1 1 d . . . . .
C27 C 0.6783(3) 0.2952(3) 0.0554(3) 0.0266(9) Uani 1 1 d . . . . .
C28 C 0.6789(3) 0.3103(4) -0.0456(3) 0.0316(10) Uani 1 1 d . . . . .
C29 C 0.6192(3) 0.1973(3) 0.0656(3) 0.0303(10) Uani 1 1 d . . . . .
H29 H 0.5841 0.1393 0.0095 0.036 Uiso 1 1 calc R U . . .
C30 C 0.6102(3) 0.1822(3) 0.1573(3) 0.0301(10) Uani 1 1 d . . . . .
H30 H 0.5679 0.1154 0.1613 0.036 Uiso 1 1 calc R U . . .
C31 C 0.1320(4) -0.4381(4) 0.2698(4) 0.0525(13) Uani 1 1 d . . . . .
H31 H 0.1055 -0.4036 0.2305 0.063 Uiso 1 1 calc R U . . .
C32 C 0.0597(4) -0.4970(4) 0.3152(4) 0.0627(15) Uani 1 1 d . . . . .
H32 H -0.0142 -0.5022 0.3069 0.075 Uiso 1 1 calc R U . . .
C33 C 0.0981(4) -0.5481(4) 0.3731(4) 0.0594(15) Uani 1 1 d . . . . .
H33 H 0.0509 -0.5874 0.4058 0.071 Uiso 1 1 calc R U . . .
C34 C 0.2075(4) -0.5407(4) 0.3825(3) 0.0453(12) Uani 1 1 d . . . . .
H34 H 0.2347 -0.5759 0.4204 0.054 Uiso 1 1 calc R U . . .
C35 C 0.2757(4) -0.4800(3) 0.3345(3) 0.0321(10) Uani 1 1 d . . . . .
C36 C 0.3945(4) -0.4681(3) 0.3415(3) 0.0324(10) Uani 1 1 d . . . . .
C37 C 0.4368(4) -0.5346(3) 0.3748(3) 0.0382(11) Uani 1 1 d . . . . .
H37 H 0.3907 -0.5896 0.3947 0.046 Uiso 1 1 calc R U . . .
C38 C 0.5478(4) -0.5187(4) 0.3784(3) 0.0461(13) Uani 1 1 d . . . . .
H38 H 0.5765 -0.5640 0.3992 0.055 Uiso 1 1 calc R U . . .
C39 C 0.6153(4) -0.4365(4) 0.3513(4) 0.0552(14) Uani 1 1 d . . . . .
H39 H 0.6908 -0.4238 0.3545 0.066 Uiso 1 1 calc R U . . .
C40 C 0.5691(4) -0.3728(4) 0.3191(4) 0.0528(14) Uani 1 1 d . . . . .
H40 H 0.6148 -0.3167 0.3002 0.063 Uiso 1 1 calc R U . . .
C41 C 0.0078(4) 0.2073(4) 0.2021(3) 0.0422(12) Uani 1 1 d . . . . .
H41 H 0.0025 0.1823 0.2566 0.051 Uiso 1 1 calc R U . . .
C42 C -0.0851(4) 0.2148(4) 0.1516(4) 0.0488(13) Uani 1 1 d . . . . .
H42 H -0.1517 0.1966 0.1725 0.059 Uiso 1 1 calc R U . . .
C43 C -0.0786(4) 0.2491(5) 0.0707(4) 0.0632(16) Uani 1 1 d . . . . .
H43 H -0.1416 0.2516 0.0339 0.076 Uiso 1 1 calc R U . . .
C44 C 0.0221(4) 0.2799(5) 0.0444(4) 0.0576(15) Uani 1 1 d . . . . .
H44 H 0.0283 0.3049 -0.0100 0.069 Uiso 1 1 calc R U . . .
C45 C 0.1153(4) 0.2738(3) 0.0985(3) 0.0349(11) Uani 1 1 d . . . . .
C46 C 0.2256(4) 0.3049(4) 0.0734(3) 0.0356(11) Uani 1 1 d . . . . .
C47 C 0.2452(5) 0.3437(5) -0.0050(4) 0.0637(17) Uani 1 1 d . . . . .
H47 H 0.1875 0.3507 -0.0450 0.076 Uiso 1 1 calc R U . . .
C48 C 0.3502(5) 0.3719(5) -0.0237(4) 0.0741(19) Uani 1 1 d . . . . .
H48 H 0.3638 0.3975 -0.0770 0.089 Uiso 1 1 calc R U . . .
C49 C 0.4350(5) 0.3625(4) 0.0356(4) 0.0621(16) Uani 1 1 d . . . . .
H49 H 0.5071 0.3824 0.0246 0.074 Uiso 1 1 calc R U . . .
C50 C 0.4097(4) 0.3227(4) 0.1120(3) 0.0491(14) Uani 1 1 d . . . . .
H50 H 0.4666 0.3154 0.1526 0.059 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 O9 2.258(3) . ?
Cd1 O4 2.260(2) 2_655 ?
Cd1 O1 2.265(3) . ?
Cd1 O17 2.276(3) . ?
Cd1 O11 2.366(2) 2_656 ?
Cd1 O14 2.382(3) 2_655 ?
Cd1 Cd2 3.4607(4) . ?
Cd2 O2 2.221(3) . ?
Cd2 N4 2.274(3) . ?
Cd2 O11 2.295(3) 2_656 ?
Cd2 N3 2.315(3) . ?
Cd2 O13 2.395(3) 2_655 ?
Cd2 O14 2.418(3) 2_655 ?
Cd2 C28 2.721(4) 2_655 ?
Cd3 O3 2.255(3) 2_655 ?
Cd3 O10 2.266(3) . ?
Cd3 O5 2.338(3) 2_656 ?
Cd3 N6 2.341(3) . ?
Cd3 N5 2.343(3) . ?
Cd3 O6 2.408(3) 2_656 ?
Cd3 C13 2.665(4) 2_656 ?
N1 O8 1.221(4) . ?
N1 O7 1.222(4) . ?
N1 C11 1.471(5) . ?
N2 O16 1.213(4) . ?
N2 O15 1.217(5) . ?
N2 C26 1.471(5) . ?
N3 C31 1.339(5) . ?
N3 C35 1.345(5) . ?
N4 C40 1.335(5) . ?
N4 C36 1.347(5) . ?
N5 C41 1.331(5) . ?
N5 C45 1.339(5) . ?
N6 C46 1.339(5) . ?
N6 C50 1.338(5) . ?
O1 C1 1.256(4) . ?
O2 C1 1.250(4) . ?
O3 C7 1.270(4) . ?
O3 Cd3 2.255(3) 2_655 ?
O4 C7 1.256(4) . ?
O4 Cd1 2.260(2) 2_655 ?
O5 C13 1.251(5) . ?
O5 Cd3 2.338(3) 2_656 ?
O6 C13 1.254(5) . ?
O6 Cd3 2.408(3) 2_656 ?
O9 C16 1.248(5) . ?
O10 C16 1.261(4) . ?
O11 C22 1.290(4) . ?
O11 Cd2 2.295(3) 2_656 ?
O11 Cd1 2.366(2) 2_656 ?
O12 C22 1.225(5) . ?
O13 C28 1.232(4) . ?
O13 Cd2 2.395(3) 2_655 ?
O14 C28 1.262(4) . ?
O14 Cd1 2.382(3) 2_655 ?
O14 Cd2 2.418(3) 2_655 ?
O17 H1W 0.8754 . ?
O17 H2W 0.8745 . ?
C1 C2 1.516(5) . ?
C2 C8 1.378(5) . ?
C2 C3 1.408(5) . ?
C3 C4 1.398(5) . ?
C3 C9 1.489(5) . ?
C4 C5 1.375(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.384(5) . ?
C5 H5 0.9300 . ?
C6 C8 1.394(5) . ?
C6 C7 1.490(5) . ?
C8 H8 0.9300 . ?
C9 C10 1.386(5) . ?
C9 C15 1.391(5) . ?
C10 C11 1.386(5) . ?
C10 H10 0.9300 . ?
C11 C12 1.377(5) . ?
C12 C14 1.392(5) . ?
C12 C13 1.516(5) . ?
C13 Cd3 2.665(4) 2_656 ?
C14 C15 1.370(5) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C17 1.514(5) . ?
C17 C23 1.393(5) . ?
C17 C18 1.415(5) . ?
C18 C19 1.390(5) . ?
C18 C24 1.492(5) . ?
C19 C20 1.371(5) . ?
C19 H19 0.9300 . ?
C20 C21 1.396(5) . ?
C20 H20 0.9300 . ?
C21 C23 1.380(5) . ?
C21 C22 1.511(5) . ?
C23 H23 0.9300 . ?
C24 C30 1.393(5) . ?
C24 C25 1.397(5) . ?
C25 C26 1.378(5) . ?
C25 H25 0.9300 . ?
C26 C27 1.392(5) . ?
C27 C29 1.379(5) . ?
C27 C28 1.514(5) . ?
C28 Cd2 2.721(4) 2_655 ?
C29 C30 1.395(5) . ?
C29 H29 0.9300 . ?
C30 H30 0.9300 . ?
C31 C32 1.368(6) . ?
C31 H31 0.9300 . ?
C32 C33 1.371(7) . ?
C32 H32 0.9300 . ?
C33 C34 1.379(6) . ?
C33 H33 0.9300 . ?
C34 C35 1.379(5) . ?
C34 H34 0.9300 . ?
C35 C36 1.487(6) . ?
C36 C37 1.383(5) . ?
C37 C38 1.378(6) . ?
C37 H37 0.9300 . ?
C38 C39 1.361(6) . ?
C38 H38 0.9300 . ?
C39 C40 1.373(6) . ?
C39 H39 0.9300 . ?
C40 H40 0.9300 . ?
C41 C42 1.375(6) . ?
C41 H41 0.9300 . ?
C42 C43 1.358(6) . ?
C42 H42 0.9300 . ?
C43 C44 1.368(7) . ?
C43 H43 0.9300 . ?
C44 C45 1.391(6) . ?
C44 H44 0.9300 . ?
C45 C46 1.471(6) . ?
C46 C47 1.377(6) . ?
C47 C48 1.370(7) . ?
C47 H47 0.9300 . ?
C48 C49 1.363(7) . ?
C48 H48 0.9300 . ?
C49 C50 1.371(6) . ?
C49 H49 0.9300 . ?
C50 H50 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
O9 Cd1 O4 95.06(10) . 2_655 ?
O9 Cd1 O1 95.28(10) . . ?
O4 Cd1 O1 87.86(9) 2_655 . ?
O9 Cd1 O17 96.58(10) . . ?
O4 Cd1 O17 89.77(10) 2_655 . ?
O1 Cd1 O17 168.07(11) . . ?
O9 Cd1 O11 92.74(9) . 2_656 ?
O4 Cd1 O11 172.18(10) 2_655 2_656 ?
O1 Cd1 O11 91.87(9) . 2_656 ?
O17 Cd1 O11 88.88(9) . 2_656 ?
O9 Cd1 O14 173.35(9) . 2_655 ?
O4 Cd1 O14 91.26(10) 2_655 2_655 ?
O1 Cd1 O14 82.89(10) . 2_655 ?
O17 Cd1 O14 85.47(11) . 2_655 ?
O11 Cd1 O14 80.95(9) 2_656 2_655 ?
O9 Cd1 Cd2 129.08(7) . . ?
O4 Cd1 Cd2 131.75(7) 2_655 . ?
O1 Cd1 Cd2 71.67(7) . . ?
O17 Cd1 Cd2 101.57(8) . . ?
O11 Cd1 Cd2 41.28(6) 2_656 . ?
O14 Cd1 Cd2 44.28(6) 2_655 . ?
O2 Cd2 N4 88.03(12) . . ?
O2 Cd2 O11 91.65(10) . 2_656 ?
N4 Cd2 O11 119.47(11) . 2_656 ?
O2 Cd2 N3 158.93(11) . . ?
N4 Cd2 N3 72.09(12) . . ?
O11 Cd2 N3 92.19(11) 2_656 . ?
O2 Cd2 O13 88.38(11) . 2_655 ?
N4 Cd2 O13 104.66(11) . 2_655 ?
O11 Cd2 O13 135.85(9) 2_656 2_655 ?
N3 Cd2 O13 103.06(12) . 2_655 ?
O2 Cd2 O14 90.78(10) . 2_655 ?
N4 Cd2 O14 158.90(11) . 2_655 ?
O11 Cd2 O14 81.62(9) 2_656 2_655 ?
N3 Cd2 O14 110.27(11) . 2_655 ?
O13 Cd2 O14 54.24(9) 2_655 2_655 ?
O2 Cd2 C28 86.43(11) . 2_655 ?
N4 Cd2 C28 131.32(13) . 2_655 ?
O11 Cd2 C28 109.01(11) 2_656 2_655 ?
N3 Cd2 C28 111.77(12) . 2_655 ?
O13 Cd2 C28 26.92(10) 2_655 2_655 ?
O14 Cd2 C28 27.64(10) 2_655 2_655 ?
O2 Cd2 Cd1 76.18(7) . . ?
N4 Cd2 Cd1 154.46(10) . . ?
O11 Cd2 Cd1 42.84(6) 2_656 . ?
N3 Cd2 Cd1 119.55(8) . . ?
O13 Cd2 Cd1 94.96(7) 2_655 . ?
O14 Cd2 Cd1 43.44(7) 2_655 . ?
C28 Cd2 Cd1 68.40(9) 2_655 . ?
O3 Cd3 O10 104.01(10) 2_655 . ?
O3 Cd3 O5 137.57(10) 2_655 2_656 ?
O10 Cd3 O5 89.11(10) . 2_656 ?
O3 Cd3 N6 92.89(11) 2_655 . ?
O10 Cd3 N6 84.30(11) . . ?
O5 Cd3 N6 128.88(12) 2_656 . ?
O3 Cd3 N5 92.81(11) 2_655 . ?
O10 Cd3 N5 150.08(11) . . ?
O5 Cd3 N5 94.98(11) 2_656 . ?
N6 Cd3 N5 70.11(11) . . ?
O3 Cd3 O6 82.25(10) 2_655 2_656 ?
O10 Cd3 O6 113.73(10) . 2_656 ?
O5 Cd3 O6 55.79(10) 2_656 2_656 ?
N6 Cd3 O6 161.96(11) . 2_656 ?
N5 Cd3 O6 92.69(11) . 2_656 ?
O3 Cd3 C13 109.63(13) 2_655 2_656 ?
O10 Cd3 C13 100.28(11) . 2_656 ?
O5 Cd3 C13 27.99(12) 2_656 2_656 ?
N6 Cd3 C13 154.86(13) . 2_656 ?
N5 Cd3 C13 96.98(11) . 2_656 ?
O6 Cd3 C13 28.03(12) 2_656 2_656 ?
O8 N1 O7 123.6(4) . . ?
O8 N1 C11 117.7(4) . . ?
O7 N1 C11 118.7(4) . . ?
O16 N2 O15 124.1(5) . . ?
O16 N2 C26 118.3(4) . . ?
O15 N2 C26 117.6(4) . . ?
C31 N3 C35 117.8(4) . . ?
C31 N3 Cd2 124.7(3) . . ?
C35 N3 Cd2 115.9(3) . . ?
C40 N4 C36 119.1(4) . . ?
C40 N4 Cd2 122.8(3) . . ?
C36 N4 Cd2 117.4(3) . . ?
C41 N5 C45 120.2(4) . . ?
C41 N5 Cd3 122.8(3) . . ?
C45 N5 Cd3 116.1(3) . . ?
C46 N6 C50 118.4(3) . . ?
C46 N6 Cd3 116.6(3) . . ?
C50 N6 Cd3 123.4(3) . . ?
C1 O1 Cd1 134.4(3) . . ?
C1 O2 Cd2 128.2(3) . . ?
C7 O3 Cd3 119.7(3) . 2_655 ?
C7 O4 Cd1 122.8(2) . 2_655 ?
C13 O5 Cd3 90.7(2) . 2_656 ?
C13 O6 Cd3 87.5(3) . 2_656 ?
C16 O9 Cd1 124.5(2) . . ?
C16 O10 Cd3 113.4(3) . . ?
C22 O11 Cd2 122.4(3) . 2_656 ?
C22 O11 Cd1 121.4(2) . 2_656 ?
Cd2 O11 Cd1 95.87(9) 2_656 2_656 ?
C28 O13 Cd2 91.4(2) . 2_655 ?
C28 O14 Cd1 149.5(3) . 2_655 ?
C28 O14 Cd2 89.6(2) . 2_655 ?
Cd1 O14 Cd2 92.28(9) 2_655 2_655 ?
Cd1 O17 H1W 110.9 . . ?
Cd1 O17 H2W 110.4 . . ?
H1W O17 H2W 108.0 . . ?
O2 C1 O1 126.2(4) . . ?
O2 C1 C2 116.8(3) . . ?
O1 C1 C2 116.8(3) . . ?
C8 C2 C3 119.5(3) . . ?
C8 C2 C1 116.3(3) . . ?
C3 C2 C1 123.8(3) . . ?
C4 C3 C2 118.1(3) . . ?
C4 C3 C9 119.5(3) . . ?
C2 C3 C9 122.3(3) . . ?
C5 C4 C3 121.7(4) . . ?
C5 C4 H4 119.2 . . ?
C3 C4 H4 119.2 . . ?
C6 C5 C4 120.2(3) . . ?
C6 C5 H5 119.9 . . ?
C4 C5 H5 119.9 . . ?
C5 C6 C8 118.7(3) . . ?
C5 C6 C7 121.9(3) . . ?
C8 C6 C7 119.4(3) . . ?
O4 C7 O3 123.9(3) . . ?
O4 C7 C6 118.6(3) . . ?
O3 C7 C6 117.6(3) . . ?
C2 C8 C6 121.7(3) . . ?
C2 C8 H8 119.2 . . ?
C6 C8 H8 119.2 . . ?
C10 C9 C15 117.9(3) . . ?
C10 C9 C3 121.9(3) . . ?
C15 C9 C3 120.2(3) . . ?
C11 C10 C9 119.8(4) . . ?
C11 C10 H10 120.1 . . ?
C9 C10 H10 120.1 . . ?
C12 C11 C10 122.4(3) . . ?
C12 C11 N1 118.7(3) . . ?
C10 C11 N1 118.9(3) . . ?
C11 C12 C14 117.3(3) . . ?
C11 C12 C13 124.8(4) . . ?
C14 C12 C13 117.3(3) . . ?
O5 C13 O6 125.0(4) . . ?
O5 C13 C12 116.8(4) . . ?
O6 C13 C12 117.9(4) . . ?
O5 C13 Cd3 61.3(2) . 2_656 ?
O6 C13 Cd3 64.5(2) . 2_656 ?
C12 C13 Cd3 164.8(3) . 2_656 ?
C15 C14 C12 120.8(4) . . ?
C15 C14 H14 119.6 . . ?
C12 C14 H14 119.6 . . ?
C14 C15 C9 121.6(4) . . ?
C14 C15 H15 119.2 . . ?
C9 C15 H15 119.2 . . ?
O9 C16 O10 124.3(4) . . ?
O9 C16 C17 118.7(3) . . ?
O10 C16 C17 116.9(4) . . ?
C23 C17 C18 119.5(4) . . ?
C23 C17 C16 118.1(3) . . ?
C18 C17 C16 122.4(3) . . ?
C19 C18 C17 117.6(3) . . ?
C19 C18 C24 117.4(3) . . ?
C17 C18 C24 124.8(4) . . ?
C20 C19 C18 122.8(4) . . ?
C20 C19 H19 118.6 . . ?
C18 C19 H19 118.6 . . ?
C19 C20 C21 119.6(4) . . ?
C19 C20 H20 120.2 . . ?
C21 C20 H20 120.2 . . ?
C23 C21 C20 119.1(3) . . ?
C23 C21 C22 124.0(4) . . ?
C20 C21 C22 116.9(4) . . ?
O12 C22 O11 124.9(4) . . ?
O12 C22 C21 117.2(3) . . ?
O11 C22 C21 117.9(3) . . ?
C21 C23 C17 121.5(4) . . ?
C21 C23 H23 119.2 . . ?
C17 C23 H23 119.2 . . ?
C30 C24 C25 118.6(3) . . ?
C30 C24 C18 121.1(4) . . ?
C25 C24 C18 119.7(4) . . ?
C26 C25 C24 119.3(4) . . ?
C26 C25 H25 120.3 . . ?
C24 C25 H25 120.3 . . ?
C25 C26 C27 123.4(4) . . ?
C25 C26 N2 116.8(4) . . ?
C27 C26 N2 119.5(3) . . ?
C29 C27 C26 116.2(3) . . ?
C29 C27 C28 120.8(4) . . ?
C26 C27 C28 122.8(4) . . ?
O13 C28 O14 123.2(4) . . ?
O13 C28 C27 118.7(4) . . ?
O14 C28 C27 118.0(4) . . ?
O13 C28 Cd2 61.7(2) . 2_655 ?
O14 C28 Cd2 62.7(2) . 2_655 ?
C27 C28 Cd2 164.8(3) . 2_655 ?
C27 C29 C30 122.2(4) . . ?
C27 C29 H29 118.9 . . ?
C30 C29 H29 118.9 . . ?
C24 C30 C29 120.1(4) . . ?
C24 C30 H30 119.9 . . ?
C29 C30 H30 119.9 . . ?
N3 C31 C32 123.0(5) . . ?
N3 C31 H31 118.5 . . ?
C32 C31 H31 118.5 . . ?
C31 C32 C33 118.8(5) . . ?
C31 C32 H32 120.6 . . ?
C33 C32 H32 120.6 . . ?
C32 C33 C34 119.3(5) . . ?
C32 C33 H33 120.3 . . ?
C34 C33 H33 120.3 . . ?
C35 C34 C33 118.7(4) . . ?
C35 C34 H34 120.7 . . ?
C33 C34 H34 120.7 . . ?
N3 C35 C34 122.2(4) . . ?
N3 C35 C36 116.1(4) . . ?
C34 C35 C36 121.6(4) . . ?
N4 C36 C37 120.4(4) . . ?
N4 C36 C35 116.5(3) . . ?
C37 C36 C35 123.1(4) . . ?
C38 C37 C36 119.4(4) . . ?
C38 C37 H37 120.3 . . ?
C36 C37 H37 120.3 . . ?
C39 C38 C37 119.8(4) . . ?
C39 C38 H38 120.1 . . ?
C37 C38 H38 120.1 . . ?
C38 C39 C40 118.3(5) . . ?
C38 C39 H39 120.9 . . ?
C40 C39 H39 120.9 . . ?
N4 C40 C39 122.9(4) . . ?
N4 C40 H40 118.6 . . ?
C39 C40 H40 118.6 . . ?
N5 C41 C42 121.6(4) . . ?
N5 C41 H41 119.2 . . ?
C42 C41 H41 119.2 . . ?
C43 C42 C41 119.4(5) . . ?
C43 C42 H42 120.3 . . ?
C41 C42 H42 120.3 . . ?
C42 C43 C44 118.9(4) . . ?
C42 C43 H43 120.6 . . ?
C44 C43 H43 120.6 . . ?
C43 C44 C45 120.3(4) . . ?
C43 C44 H44 119.9 . . ?
C45 C44 H44 119.9 . . ?
N5 C45 C44 119.5(4) . . ?
N5 C45 C46 117.6(3) . . ?
C44 C45 C46 122.8(4) . . ?
N6 C46 C47 120.9(4) . . ?
N6 C46 C45 116.5(3) . . ?
C47 C46 C45 122.6(4) . . ?
C48 C47 C46 119.5(5) . . ?
C48 C47 H47 120.2 . . ?
C46 C47 H47 120.2 . . ?
C49 C48 C47 120.2(5) . . ?
C49 C48 H48 119.9 . . ?
C47 C48 H48 119.9 . . ?
C48 C49 C50 117.4(5) . . ?
C48 C49 H49 121.3 . . ?
C50 C49 H49 121.3 . . ?
N6 C50 C49 123.6(4) . . ?
N6 C50 H50 118.2 . . ?
C49 C50 H50 118.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cd2 O2 C1 O1 24.0(6) . . . . ?
Cd2 O2 C1 C2 -150.9(3) . . . . ?
Cd1 O1 C1 O2 -10.1(7) . . . . ?
Cd1 O1 C1 C2 164.7(3) . . . . ?
O2 C1 C2 C8 133.0(4) . . . . ?
O1 C1 C2 C8 -42.4(5) . . . . ?
O2 C1 C2 C3 -39.7(6) . . . . ?
O1 C1 C2 C3 144.9(4) . . . . ?
C8 C2 C3 C4 -3.1(6) . . . . ?
C1 C2 C3 C4 169.4(4) . . . . ?
C8 C2 C3 C9 173.6(4) . . . . ?
C1 C2 C3 C9 -13.9(6) . . . . ?
C2 C3 C4 C5 -0.7(6) . . . . ?
C9 C3 C4 C5 -177.5(4) . . . . ?
C3 C4 C5 C6 3.0(7) . . . . ?
C4 C5 C6 C8 -1.4(6) . . . . ?
C4 C5 C6 C7 178.1(4) . . . . ?
Cd1 O4 C7 O3 -10.9(6) 2_655 . . . ?
Cd1 O4 C7 C6 169.3(3) 2_655 . . . ?
Cd3 O3 C7 O4 -81.6(4) 2_655 . . . ?
Cd3 O3 C7 C6 98.2(4) 2_655 . . . ?
C5 C6 C7 O4 -162.3(4) . . . . ?
C8 C6 C7 O4 17.2(6) . . . . ?
C5 C6 C7 O3 17.8(6) . . . . ?
C8 C6 C7 O3 -162.6(4) . . . . ?
C3 C2 C8 C6 4.8(6) . . . . ?
C1 C2 C8 C6 -168.3(4) . . . . ?
C5 C6 C8 C2 -2.5(6) . . . . ?
C7 C6 C8 C2 177.9(4) . . . . ?
C4 C3 C9 C10 -43.8(6) . . . . ?
C2 C3 C9 C10 139.5(4) . . . . ?
C4 C3 C9 C15 135.2(4) . . . . ?
C2 C3 C9 C15 -41.5(6) . . . . ?
C15 C9 C10 C11 2.2(6) . . . . ?
C3 C9 C10 C11 -178.7(4) . . . . ?
C9 C10 C11 C12 1.4(7) . . . . ?
C9 C10 C11 N1 -179.6(4) . . . . ?
O8 N1 C11 C12 -29.4(6) . . . . ?
O7 N1 C11 C12 149.4(4) . . . . ?
O8 N1 C11 C10 151.5(4) . . . . ?
O7 N1 C11 C10 -29.7(6) . . . . ?
C10 C11 C12 C14 -4.0(7) . . . . ?
N1 C11 C12 C14 176.9(4) . . . . ?
C10 C11 C12 C13 167.7(4) . . . . ?
N1 C11 C12 C13 -11.4(7) . . . . ?
Cd3 O5 C13 O6 11.0(4) 2_656 . . . ?
Cd3 O5 C13 C12 -162.9(3) 2_656 . . . ?
Cd3 O6 C13 O5 -10.7(4) 2_656 . . . ?
Cd3 O6 C13 C12 163.1(3) 2_656 . . . ?
C11 C12 C13 O5 -59.1(6) . . . . ?
C14 C12 C13 O5 112.5(5) . . . . ?
C11 C12 C13 O6 126.6(5) . . . . ?
C14 C12 C13 O6 -61.8(6) . . . . ?
C11 C12 C13 Cd3 -138.2(11) . . . 2_656 ?
C14 C12 C13 Cd3 33.5(15) . . . 2_656 ?
C11 C12 C14 C15 3.1(7) . . . . ?
C13 C12 C14 C15 -169.2(5) . . . . ?
C12 C14 C15 C9 0.4(8) . . . . ?
C10 C9 C15 C14 -3.1(7) . . . . ?
C3 C9 C15 C14 177.8(4) . . . . ?
Cd1 O9 C16 O10 92.8(4) . . . . ?
Cd1 O9 C16 C17 -90.7(4) . . . . ?
Cd3 O10 C16 O9 8.7(5) . . . . ?
Cd3 O10 C16 C17 -167.9(2) . . . . ?
O9 C16 C17 C23 -39.1(5) . . . . ?
O10 C16 C17 C23 137.7(4) . . . . ?
O9 C16 C17 C18 142.5(4) . . . . ?
O10 C16 C17 C18 -40.7(5) . . . . ?
C23 C17 C18 C19 -0.4(6) . . . . ?
C16 C17 C18 C19 177.9(4) . . . . ?
C23 C17 C18 C24 174.2(4) . . . . ?
C16 C17 C18 C24 -7.5(6) . . . . ?
C17 C18 C19 C20 0.8(7) . . . . ?
C24 C18 C19 C20 -174.2(4) . . . . ?
C18 C19 C20 C21 -0.7(7) . . . . ?
C19 C20 C21 C23 0.1(6) . . . . ?
C19 C20 C21 C22 177.4(4) . . . . ?
Cd2 O11 C22 O12 104.0(5) 2_656 . . . ?
Cd1 O11 C22 O12 -17.9(6) 2_656 . . . ?
Cd2 O11 C22 C21 -77.3(4) 2_656 . . . ?
Cd1 O11 C22 C21 160.8(3) 2_656 . . . ?
C23 C21 C22 O12 156.1(4) . . . . ?
C20 C21 C22 O12 -21.0(6) . . . . ?
C23 C21 C22 O11 -22.7(6) . . . . ?
C20 C21 C22 O11 160.1(4) . . . . ?
C20 C21 C23 C17 0.3(6) . . . . ?
C22 C21 C23 C17 -176.8(4) . . . . ?
C18 C17 C23 C21 -0.1(6) . . . . ?
C16 C17 C23 C21 -178.5(4) . . . . ?
C19 C18 C24 C30 117.4(4) . . . . ?
C17 C18 C24 C30 -57.1(5) . . . . ?
C19 C18 C24 C25 -53.5(5) . . . . ?
C17 C18 C24 C25 132.0(4) . . . . ?
C30 C24 C25 C26 -0.9(5) . . . . ?
C18 C24 C25 C26 170.2(3) . . . . ?
C24 C25 C26 C27 -0.7(6) . . . . ?
C24 C25 C26 N2 -175.4(3) . . . . ?
O16 N2 C26 C25 133.8(4) . . . . ?
O15 N2 C26 C25 -46.7(6) . . . . ?
O16 N2 C26 C27 -41.1(6) . . . . ?
O15 N2 C26 C27 138.3(4) . . . . ?
C25 C26 C27 C29 1.0(6) . . . . ?
N2 C26 C27 C29 175.7(3) . . . . ?
C25 C26 C27 C28 176.3(4) . . . . ?
N2 C26 C27 C28 -9.0(6) . . . . ?
Cd2 O13 C28 O14 12.8(4) 2_655 . . . ?
Cd2 O13 C28 C27 -162.7(3) 2_655 . . . ?
Cd1 O14 C28 O13 -106.5(5) 2_655 . . . ?
Cd2 O14 C28 O13 -12.6(4) 2_655 . . . ?
Cd1 O14 C28 C27 68.9(6) 2_655 . . . ?
Cd2 O14 C28 C27 162.8(3) 2_655 . . . ?
Cd1 O14 C28 Cd2 -93.9(5) 2_655 . . 2_655 ?
C29 C27 C28 O13 123.3(4) . . . . ?
C26 C27 C28 O13 -51.8(6) . . . . ?
C29 C27 C28 O14 -52.4(5) . . . . ?
C26 C27 C28 O14 132.5(4) . . . . ?
C29 C27 C28 Cd2 36.2(13) . . . 2_655 ?
C26 C27 C28 Cd2 -138.9(10) . . . 2_655 ?
C26 C27 C29 C30 0.2(6) . . . . ?
C28 C27 C29 C30 -175.2(3) . . . . ?
C25 C24 C30 C29 2.0(5) . . . . ?
C18 C24 C30 C29 -168.9(3) . . . . ?
C27 C29 C30 C24 -1.7(6) . . . . ?
C35 N3 C31 C32 1.5(7) . . . . ?
Cd2 N3 C31 C32 -164.0(4) . . . . ?
N3 C31 C32 C33 -0.1(9) . . . . ?
C31 C32 C33 C34 -1.3(9) . . . . ?
C32 C33 C34 C35 1.2(8) . . . . ?
C31 N3 C35 C34 -1.6(7) . . . . ?
Cd2 N3 C35 C34 165.2(3) . . . . ?
C31 N3 C35 C36 178.9(4) . . . . ?
Cd2 N3 C35 C36 -14.4(5) . . . . ?
C33 C34 C35 N3 0.2(7) . . . . ?
C33 C34 C35 C36 179.8(4) . . . . ?
C40 N4 C36 C37 -0.3(6) . . . . ?
Cd2 N4 C36 C37 170.8(3) . . . . ?
C40 N4 C36 C35 179.6(4) . . . . ?
Cd2 N4 C36 C35 -9.4(5) . . . . ?
N3 C35 C36 N4 15.9(6) . . . . ?
C34 C35 C36 N4 -163.6(4) . . . . ?
N3 C35 C36 C37 -164.2(4) . . . . ?
C34 C35 C36 C37 16.2(7) . . . . ?
N4 C36 C37 C38 -0.7(7) . . . . ?
C35 C36 C37 C38 179.5(4) . . . . ?
C36 C37 C38 C39 1.5(7) . . . . ?
C37 C38 C39 C40 -1.3(8) . . . . ?
C36 N4 C40 C39 0.5(8) . . . . ?
Cd2 N4 C40 C39 -170.1(4) . . . . ?
C38 C39 C40 N4 0.3(8) . . . . ?
C45 N5 C41 C42 1.8(7) . . . . ?
Cd3 N5 C41 C42 -166.3(3) . . . . ?
N5 C41 C42 C43 1.4(8) . . . . ?
C41 C42 C43 C44 -3.0(8) . . . . ?
C42 C43 C44 C45 1.4(9) . . . . ?
C41 N5 C45 C44 -3.4(7) . . . . ?
Cd3 N5 C45 C44 165.5(4) . . . . ?
C41 N5 C45 C46 178.8(4) . . . . ?
Cd3 N5 C45 C46 -12.3(5) . . . . ?
C43 C44 C45 N5 1.9(8) . . . . ?
C43 C44 C45 C46 179.5(5) . . . . ?
C50 N6 C46 C47 0.9(7) . . . . ?
Cd3 N6 C46 C47 -165.4(4) . . . . ?
C50 N6 C46 C45 -179.0(4) . . . . ?
Cd3 N6 C46 C45 14.7(5) . . . . ?
N5 C45 C46 N6 -1.6(6) . . . . ?
C44 C45 C46 N6 -179.3(5) . . . . ?
N5 C45 C46 C47 178.5(5) . . . . ?
C44 C45 C46 C47 0.9(8) . . . . ?
N6 C46 C47 C48 -0.3(8) . . . . ?
C45 C46 C47 C48 179.5(5) . . . . ?
C46 C47 C48 C49 -0.6(10) . . . . ?
C47 C48 C49 C50 1.0(10) . . . . ?
C46 N6 C50 C49 -0.4(8) . . . . ?
Cd3 N6 C50 C49 164.8(4) . . . . ?
C48 C49 C50 N6 -0.5(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
C50 H50 O10 0.93 2.48 3.100(5) 124.5 .
C49 H49 O13 0.93 2.40 3.274(5) 156.0 .
C47 H47 O15 0.93 2.65 3.284(6) 125.9 2_665
C40 H40 O2 0.93 2.53 3.147(5) 124.0 .
C39 H39 O7 0.93 2.61 3.497(7) 159.5 .
C37 H37 O5 0.93 2.47 3.381(5) 164.9 2_646
C34 H34 O5 0.93 2.57 3.326(5) 139.0 2_646
O17 H2W O12 0.87 1.87 2.628(4) 144.6 2_656
O17 H1W O6 0.88 2.53 3.121(4) 125.1 2_656
O17 H1W O3 0.88 2.13 2.789(4) 131.8 2_655

_refine_diff_density_max         0.748
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.091

####################################################################### 
# 
# 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_317-10Cd
_database_code_depnum_ccdc_archive 'CCDC 1589523'
_audit_update_record             
;
2017-12-06 deposited with the CCDC.
2018-04-30 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            'C35 H25 Cd2 N5 O10'
_chemical_formula_weight         900.40

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      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                   10.5051(5)
_cell_length_b                   12.9514(9)
_cell_length_c                   13.7037(9)
_cell_angle_alpha                106.801(6)
_cell_angle_beta                 104.715(5)
_cell_angle_gamma                93.327(5)
_cell_volume                     1708.85(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    11027
_cell_measurement_theta_min      3.636
_cell_measurement_theta_max      25.048

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.750
_exptl_crystal_F_000             892
_exptl_transmission_factor_min   0.757
_exptl_transmission_factor_max   0.780
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    1.311
_shelx_estimated_absorpt_T_min   0.761
_shelx_estimated_absorpt_T_max   0.789
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.761
_exptl_absorpt_correction_T_max  0.789
_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            11027
_diffrn_reflns_av_unetI/netI     0.0754
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.636
_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             6044
_reflns_number_gt                4314
_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)+(0.0343P)²+1.9839P] 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         6044
_refine_ls_number_parameters     469
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_gt           0.0479
_refine_ls_wR_factor_ref         0.1182
_refine_ls_wR_factor_gt          0.0993
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.048
_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 0.31427(4) 0.30439(4) 0.06535(4) 0.03816(15) Uani 1 1 d . . . . .
Cd2 Cd 0.11939(4) 0.45456(4) 0.24854(4) 0.04119(16) Uani 1 1 d . . . . .
N1 N -0.0891(7) -0.0701(5) 0.3269(5) 0.0633(18) Uani 1 1 d . . . . .
N2 N 0.4824(5) 0.2514(5) -0.0188(4) 0.0470(14) Uani 1 1 d . . . . .
N3 N 0.4893(5) 0.4481(4) 0.1192(4) 0.0442(13) Uani 1 1 d . . . . .
N4 N -0.0246(5) 0.5358(4) 0.3443(4) 0.0454(14) Uani 1 1 d . . . . .
N5 N -0.0634(5) 0.3277(5) 0.2201(5) 0.0463(14) Uani 1 1 d . . . . .
O1 O 0.4012(4) 0.2721(4) 0.2192(4) 0.0515(12) Uani 1 1 d . . . . .
O2 O 0.2225(4) 0.3046(4) 0.2757(4) 0.0513(12) Uani 1 1 d . . . . .
O3 O 0.7101(5) 0.4473(5) 0.6159(4) 0.0744(17) Uani 1 1 d . . . . .
O4 O 0.7481(5) 0.3241(6) 0.6991(4) 0.092(2) Uani 1 1 d . . . . .
O5 O -0.1806(4) -0.1272(4) 0.0084(4) 0.0569(13) Uani 1 1 d . . . . .
O6 O -0.1617(4) -0.2271(4) 0.1147(4) 0.0550(13) Uani 1 1 d . . . . .
O7 O -0.2034(6) -0.0544(6) 0.2935(5) 0.096(2) Uani 1 1 d . . . . .
O8 O -0.0537(7) -0.1104(5) 0.3980(5) 0.102(2) Uani 1 1 d . . . . .
O9 O 0.1535(4) 0.4193(3) 0.0855(3) 0.0343(9) Uani 1 1 d . . . . .
H1 H 0.1002 0.4467 0.0542 0.041 Uiso 1 1 d R U . . .
O10 O 0.0248(7) 0.6177(6) 0.1341(7) 0.150(3) Uani 1 1 d . . . . .
H1W H 0.0146 0.6756 0.1198 0.180 Uiso 1 1 d R U . . .
H2W H 0.0193 0.6220 0.1947 0.180 Uiso 1 1 d R U . . .
C1 C 0.3342(6) 0.2747(5) 0.2828(5) 0.0348(14) Uani 1 1 d . . . . .
C2 C 0.3944(5) 0.2383(5) 0.3759(5) 0.0319(13) Uani 1 1 d . . . . .
C3 C 0.5047(5) 0.3046(5) 0.4533(5) 0.0374(15) Uani 1 1 d . . . . .
H3 H 0.5370 0.3687 0.4445 0.045 Uiso 1 1 calc R U . . .
C4 C 0.5680(6) 0.2785(6) 0.5425(5) 0.0445(16) Uani 1 1 d . . . . .
C5 C 0.6854(7) 0.3563(8) 0.6264(6) 0.062(2) Uani 1 1 d . . . . .
C6 C 0.5209(7) 0.1843(6) 0.5544(5) 0.056(2) Uani 1 1 d . . . . .
H6 H 0.5647 0.1641 0.6127 0.067 Uiso 1 1 calc R U . . .
C7 C 0.4081(7) 0.1172(5) 0.4808(6) 0.0546(19) Uani 1 1 d . . . . .
H7 H 0.3761 0.0543 0.4918 0.066 Uiso 1 1 calc R U . . .
C8 C 0.3429(6) 0.1432(5) 0.3912(5) 0.0355(14) Uani 1 1 d . . . . .
C9 C 0.2216(6) 0.0725(4) 0.3148(5) 0.0337(14) Uani 1 1 d . . . . .
C10 C 0.1250(6) 0.0292(5) 0.3525(5) 0.0459(17) Uani 1 1 d . . . . .
H10 H 0.1372 0.0450 0.4252 0.055 Uiso 1 1 calc R U . . .
C11 C 0.0120(6) -0.0368(5) 0.2810(5) 0.0411(15) Uani 1 1 d . . . . .
C12 C -0.0119(6) -0.0642(4) 0.1724(5) 0.0345(14) Uani 1 1 d . . . . .
C13 C -0.1282(6) -0.1442(5) 0.0932(5) 0.0420(16) Uani 1 1 d . . . . .
C14 C 0.0832(6) -0.0207(4) 0.1355(5) 0.0359(14) Uani 1 1 d . . . . .
H14 H 0.0701 -0.0362 0.0628 0.043 Uiso 1 1 calc R U . . .
C15 C 0.1982(6) 0.0462(4) 0.2064(5) 0.0345(14) Uani 1 1 d . . . . .
H15 H 0.2608 0.0736 0.1796 0.041 Uiso 1 1 calc R U . . .
C16 C 0.4714(8) 0.1568(6) -0.0934(6) 0.066(2) Uani 1 1 d . . . . .
H16 H 0.3985 0.1051 -0.1072 0.079 Uiso 1 1 calc R U . . .
C17 C 0.5591(9) 0.1303(8) -0.1509(7) 0.084(3) Uani 1 1 d . . . . .
H17 H 0.5470 0.0623 -0.2019 0.101 Uiso 1 1 calc R U . . .
C18 C 0.6656(9) 0.2064(8) -0.1317(7) 0.077(3) Uani 1 1 d . . . . .
H18 H 0.7279 0.1910 -0.1697 0.092 Uiso 1 1 calc R U . . .
C19 C 0.6799(7) 0.3057(7) -0.0559(6) 0.061(2) Uani 1 1 d . . . . .
H19 H 0.7516 0.3585 -0.0422 0.073 Uiso 1 1 calc R U . . .
C20 C 0.5867(6) 0.3265(6) -0.0001(5) 0.0463(17) Uani 1 1 d . . . . .
C21 C 0.5952(6) 0.4322(5) 0.0818(5) 0.0402(16) Uani 1 1 d . . . . .
C22 C 0.7036(6) 0.5132(6) 0.1184(6) 0.0539(19) Uani 1 1 d . . . . .
H22 H 0.7764 0.5025 0.0917 0.065 Uiso 1 1 calc R U . . .
C23 C 0.7032(7) 0.6098(7) 0.1948(7) 0.063(2) Uani 1 1 d . . . . .
H23 H 0.7760 0.6643 0.2197 0.076 Uiso 1 1 calc R U . . .
C24 C 0.5967(8) 0.6252(6) 0.2335(6) 0.061(2) Uani 1 1 d . . . . .
H24 H 0.5945 0.6897 0.2849 0.074 Uiso 1 1 calc R U . . .
C25 C 0.4920(7) 0.5415(6) 0.1937(6) 0.061(2) Uani 1 1 d . . . . .
H25 H 0.4189 0.5507 0.2203 0.073 Uiso 1 1 calc R U . . .
C26 C 0.0028(8) 0.6375(6) 0.4088(6) 0.064(2) Uani 1 1 d . . . . .
H26 H 0.0713 0.6832 0.4044 0.077 Uiso 1 1 calc R U . . .
C27 C -0.0654(9) 0.6794(7) 0.4828(6) 0.076(3) Uani 1 1 d . . . . .
H27 H -0.0444 0.7514 0.5268 0.091 Uiso 1 1 calc R U . . .
C28 C -0.1652(10) 0.6098(9) 0.4879(7) 0.085(3) Uani 1 1 d . . . . .
H28 H -0.2127 0.6338 0.5370 0.102 Uiso 1 1 calc R U . . .
C29 C -0.1943(8) 0.5063(7) 0.4214(7) 0.069(2) Uani 1 1 d . . . . .
H29 H -0.2626 0.4593 0.4243 0.083 Uiso 1 1 calc R U . . .
C30 C -0.1238(6) 0.4701(6) 0.3498(5) 0.0466(17) Uani 1 1 d . . . . .
C31 C -0.1523(6) 0.3571(6) 0.2744(6) 0.0459(17) Uani 1 1 d . . . . .
C32 C -0.2669(7) 0.2849(7) 0.2566(7) 0.066(2) Uani 1 1 d . . . . .
H32 H -0.3297 0.3059 0.2928 0.079 Uiso 1 1 calc R U . . .
C33 C -0.2842(8) 0.1835(7) 0.1855(8) 0.078(3) Uani 1 1 d . . . . .
H33 H -0.3603 0.1353 0.1723 0.094 Uiso 1 1 calc R U . . .
C34 C -0.1916(7) 0.1514(6) 0.1333(7) 0.066(2) Uani 1 1 d . . . . .
H34 H -0.2021 0.0814 0.0861 0.079 Uiso 1 1 calc R U . . .
C35 C -0.0833(6) 0.2253(6) 0.1527(6) 0.058(2) Uani 1 1 d . . . . .
H35 H -0.0196 0.2039 0.1176 0.070 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 2.243(4) . ?
Cd1 O9 2.331(3) . ?
Cd1 N3 2.347(5) . ?
Cd1 N2 2.375(5) . ?
Cd1 O5 2.413(4) 2 ?
Cd1 O6 2.457(4) 2 ?
Cd2 O3 2.227(5) 2_666 ?
Cd2 O9 2.273(4) . ?
Cd2 N5 2.329(5) . ?
Cd2 N4 2.348(5) . ?
Cd2 O2 2.354(4) . ?
N1 O8 1.222(8) . ?
N1 O7 1.223(8) . ?
N1 C11 1.467(8) . ?
N2 C16 1.326(8) . ?
N2 C20 1.343(8) . ?
N3 C25 1.332(8) . ?
N3 C21 1.341(7) . ?
N4 C26 1.324(8) . ?
N4 C30 1.337(8) . ?
N5 C31 1.342(8) . ?
N5 C35 1.348(8) . ?
O1 C1 1.247(7) . ?
O2 C1 1.246(7) . ?
O3 C5 1.248(9) . ?
O3 Cd2 2.227(5) 2_666 ?
O4 C5 1.241(9) . ?
O5 C13 1.241(7) . ?
O5 Cd1 2.413(4) 2 ?
O6 C13 1.248(7) . ?
O6 Cd1 2.457(4) 2 ?
O9 H1 0.7826 . ?
O10 H1W 0.8345 . ?
O10 H2W 0.8330 . ?
C1 C2 1.491(8) . ?
C2 C3 1.392(8) . ?
C2 C8 1.408(8) . ?
C3 C4 1.380(8) . ?
C3 H3 0.9300 . ?
C4 C6 1.359(9) . ?
C4 C5 1.525(9) . ?
C6 C7 1.393(9) . ?
C6 H6 0.9300 . ?
C7 C8 1.389(8) . ?
C7 H7 0.9300 . ?
C8 C9 1.481(8) . ?
C9 C15 1.377(8) . ?
C9 C10 1.406(8) . ?
C10 C11 1.381(8) . ?
C10 H10 0.9300 . ?
C11 C12 1.379(8) . ?
C12 C14 1.387(8) . ?
C12 C13 1.507(8) . ?
C14 C15 1.396(8) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C17 1.355(11) . ?
C16 H16 0.9300 . ?
C17 C18 1.366(11) . ?
C17 H17 0.9300 . ?
C18 C19 1.372(11) . ?
C18 H18 0.9300 . ?
C19 C20 1.381(9) . ?
C19 H19 0.9300 . ?
C20 C21 1.479(9) . ?
C21 C22 1.384(9) . ?
C22 C23 1.381(10) . ?
C22 H22 0.9300 . ?
C23 C24 1.356(10) . ?
C23 H23 0.9300 . ?
C24 C25 1.378(9) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
C26 C27 1.390(11) . ?
C26 H26 0.9300 . ?
C27 C28 1.371(12) . ?
C27 H27 0.9300 . ?
C28 C29 1.352(12) . ?
C28 H28 0.9300 . ?
C29 C30 1.369(9) . ?
C29 H29 0.9300 . ?
C30 C31 1.489(10) . ?
C31 C32 1.404(9) . ?
C32 C33 1.360(11) . ?
C32 H32 0.9300 . ?
C33 C34 1.363(11) . ?
C33 H33 0.9300 . ?
C34 C35 1.362(9) . ?
C34 H34 0.9300 . ?
C35 H35 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 O9 109.42(15) . . ?
O1 Cd1 N3 87.80(17) . . ?
O9 Cd1 N3 94.06(16) . . ?
O1 Cd1 N2 99.19(17) . . ?
O9 Cd1 N2 146.39(16) . . ?
N3 Cd1 N2 69.24(19) . . ?
O1 Cd1 O5 91.09(16) . 2 ?
O9 Cd1 O5 101.72(15) . 2 ?
N3 Cd1 O5 163.61(18) . 2 ?
N2 Cd1 O5 94.84(18) . 2 ?
O1 Cd1 O6 144.59(16) . 2 ?
O9 Cd1 O6 82.26(15) . 2 ?
N3 Cd1 O6 125.59(17) . 2 ?
N2 Cd1 O6 84.52(17) . 2 ?
O5 Cd1 O6 53.52(15) 2 2 ?
O3 Cd2 O9 115.20(18) 2_666 . ?
O3 Cd2 N5 137.6(2) 2_666 . ?
O9 Cd2 N5 103.68(17) . . ?
O3 Cd2 N4 88.50(19) 2_666 . ?
O9 Cd2 N4 140.94(16) . . ?
N5 Cd2 N4 69.99(19) . . ?
O3 Cd2 O2 84.4(2) 2_666 . ?
O9 Cd2 O2 91.21(15) . . ?
N5 Cd2 O2 78.41(16) . . ?
N4 Cd2 O2 123.14(17) . . ?
O8 N1 O7 123.5(7) . . ?
O8 N1 C11 117.9(7) . . ?
O7 N1 C11 118.6(7) . . ?
C16 N2 C20 117.6(6) . . ?
C16 N2 Cd1 123.8(5) . . ?
C20 N2 Cd1 118.0(5) . . ?
C25 N3 C21 118.9(6) . . ?
C25 N3 Cd1 121.5(5) . . ?
C21 N3 Cd1 119.2(4) . . ?
C26 N4 C30 118.5(6) . . ?
C26 N4 Cd2 122.8(5) . . ?
C30 N4 Cd2 117.4(4) . . ?
C31 N5 C35 118.3(6) . . ?
C31 N5 Cd2 118.6(5) . . ?
C35 N5 Cd2 123.1(4) . . ?
C1 O1 Cd1 120.5(4) . . ?
C1 O2 Cd2 137.8(4) . . ?
C5 O3 Cd2 109.2(5) . 2_666 ?
C13 O5 Cd1 92.4(4) . 2 ?
C13 O6 Cd1 90.2(4) . 2 ?
Cd2 O9 Cd1 111.75(16) . . ?
Cd2 O9 H1 105.2 . . ?
Cd1 O9 H1 142.6 . . ?
H1W O10 H2W 112.7 . . ?
O2 C1 O1 126.3(6) . . ?
O2 C1 C2 117.4(6) . . ?
O1 C1 C2 116.3(5) . . ?
C3 C2 C8 118.7(5) . . ?
C3 C2 C1 117.7(5) . . ?
C8 C2 C1 123.5(5) . . ?
C4 C3 C2 122.3(6) . . ?
C4 C3 H3 118.8 . . ?
C2 C3 H3 118.8 . . ?
C6 C4 C3 118.5(6) . . ?
C6 C4 C5 121.6(7) . . ?
C3 C4 C5 119.9(7) . . ?
O3 C5 O4 125.6(7) . . ?
O3 C5 C4 116.9(7) . . ?
O4 C5 C4 117.5(8) . . ?
C4 C6 C7 121.2(6) . . ?
C4 C6 H6 119.4 . . ?
C7 C6 H6 119.4 . . ?
C8 C7 C6 120.8(6) . . ?
C8 C7 H7 119.6 . . ?
C6 C7 H7 119.6 . . ?
C7 C8 C2 118.4(5) . . ?
C7 C8 C9 120.2(6) . . ?
C2 C8 C9 121.4(5) . . ?
C15 C9 C10 117.5(5) . . ?
C15 C9 C8 122.6(6) . . ?
C10 C9 C8 119.8(6) . . ?
C11 C10 C9 119.7(6) . . ?
C11 C10 H10 120.1 . . ?
C9 C10 H10 120.1 . . ?
C12 C11 C10 123.2(6) . . ?
C12 C11 N1 120.5(6) . . ?
C10 C11 N1 116.1(6) . . ?
C11 C12 C14 116.9(5) . . ?
C11 C12 C13 123.9(6) . . ?
C14 C12 C13 119.0(6) . . ?
O5 C13 O6 123.6(6) . . ?
O5 C13 C12 118.7(6) . . ?
O6 C13 C12 117.6(6) . . ?
C12 C14 C15 120.8(6) . . ?
C12 C14 H14 119.6 . . ?
C15 C14 H14 119.6 . . ?
C9 C15 C14 121.9(6) . . ?
C9 C15 H15 119.1 . . ?
C14 C15 H15 119.1 . . ?
N2 C16 C17 124.6(8) . . ?
N2 C16 H16 117.7 . . ?
C17 C16 H16 117.7 . . ?
C16 C17 C18 118.0(9) . . ?
C16 C17 H17 121.0 . . ?
C18 C17 H17 121.0 . . ?
C17 C18 C19 119.3(8) . . ?
C17 C18 H18 120.4 . . ?
C19 C18 H18 120.4 . . ?
C18 C19 C20 119.4(8) . . ?
C18 C19 H19 120.3 . . ?
C20 C19 H19 120.3 . . ?
N2 C20 C19 121.1(7) . . ?
N2 C20 C21 116.6(6) . . ?
C19 C20 C21 122.2(7) . . ?
N3 C21 C22 120.1(7) . . ?
N3 C21 C20 116.4(6) . . ?
C22 C21 C20 123.5(6) . . ?
C23 C22 C21 119.8(7) . . ?
C23 C22 H22 120.1 . . ?
C21 C22 H22 120.1 . . ?
C24 C23 C22 120.0(7) . . ?
C24 C23 H23 120.0 . . ?
C22 C23 H23 120.0 . . ?
C23 C24 C25 117.4(8) . . ?
C23 C24 H24 121.3 . . ?
C25 C24 H24 121.3 . . ?
N3 C25 C24 123.8(7) . . ?
N3 C25 H25 118.1 . . ?
C24 C25 H25 118.1 . . ?
N4 C26 C27 123.4(8) . . ?
N4 C26 H26 118.3 . . ?
C27 C26 H26 118.3 . . ?
C28 C27 C26 117.0(8) . . ?
C28 C27 H27 121.5 . . ?
C26 C27 H27 121.5 . . ?
C29 C28 C27 119.7(8) . . ?
C29 C28 H28 120.1 . . ?
C27 C28 H28 120.1 . . ?
C28 C29 C30 120.4(8) . . ?
C28 C29 H29 119.8 . . ?
C30 C29 H29 119.8 . . ?
N4 C30 C29 121.0(7) . . ?
N4 C30 C31 116.4(6) . . ?
C29 C30 C31 122.6(7) . . ?
N5 C31 C32 120.6(7) . . ?
N5 C31 C30 116.1(6) . . ?
C32 C31 C30 123.2(7) . . ?
C33 C32 C31 118.7(7) . . ?
C33 C32 H32 120.6 . . ?
C31 C32 H32 120.6 . . ?
C32 C33 C34 121.0(7) . . ?
C32 C33 H33 119.5 . . ?
C34 C33 H33 119.5 . . ?
C35 C34 C33 117.7(8) . . ?
C35 C34 H34 121.2 . . ?
C33 C34 H34 121.2 . . ?
N5 C35 C34 123.6(7) . . ?
N5 C35 H35 118.2 . . ?
C34 C35 H35 118.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cd2 O2 C1 O1 -50.3(10) . . . . ?
Cd2 O2 C1 C2 129.7(5) . . . . ?
Cd1 O1 C1 O2 -7.6(9) . . . . ?
Cd1 O1 C1 C2 172.5(4) . . . . ?
O2 C1 C2 C3 -110.4(6) . . . . ?
O1 C1 C2 C3 69.5(7) . . . . ?
O2 C1 C2 C8 67.2(8) . . . . ?
O1 C1 C2 C8 -112.8(7) . . . . ?
C8 C2 C3 C4 2.2(9) . . . . ?
C1 C2 C3 C4 180.0(6) . . . . ?
C2 C3 C4 C6 0.5(10) . . . . ?
C2 C3 C4 C5 -177.9(6) . . . . ?
Cd2 O3 C5 O4 -1.9(10) 2_666 . . . ?
Cd2 O3 C5 C4 178.0(5) 2_666 . . . ?
C6 C4 C5 O3 -170.5(7) . . . . ?
C3 C4 C5 O3 7.8(10) . . . . ?
C6 C4 C5 O4 9.5(11) . . . . ?
C3 C4 C5 O4 -172.2(6) . . . . ?
C3 C4 C6 C7 -2.6(11) . . . . ?
C5 C4 C6 C7 175.7(7) . . . . ?
C4 C6 C7 C8 2.1(11) . . . . ?
C6 C7 C8 C2 0.7(10) . . . . ?
C6 C7 C8 C9 -178.7(6) . . . . ?
C3 C2 C8 C7 -2.8(9) . . . . ?
C1 C2 C8 C7 179.6(6) . . . . ?
C3 C2 C8 C9 176.7(6) . . . . ?
C1 C2 C8 C9 -1.0(9) . . . . ?
C7 C8 C9 C15 -138.2(7) . . . . ?
C2 C8 C9 C15 42.4(9) . . . . ?
C7 C8 C9 C10 41.6(9) . . . . ?
C2 C8 C9 C10 -137.9(6) . . . . ?
C15 C9 C10 C11 -0.1(9) . . . . ?
C8 C9 C10 C11 -179.9(5) . . . . ?
C9 C10 C11 C12 0.6(10) . . . . ?
C9 C10 C11 N1 -174.5(6) . . . . ?
O8 N1 C11 C12 133.4(7) . . . . ?
O7 N1 C11 C12 -48.0(9) . . . . ?
O8 N1 C11 C10 -51.4(9) . . . . ?
O7 N1 C11 C10 127.2(7) . . . . ?
C10 C11 C12 C14 -1.1(9) . . . . ?
N1 C11 C12 C14 173.8(6) . . . . ?
C10 C11 C12 C13 174.2(6) . . . . ?
N1 C11 C12 C13 -10.9(9) . . . . ?
Cd1 O5 C13 O6 -5.5(7) 2 . . . ?
Cd1 O5 C13 C12 170.5(5) 2 . . . ?
Cd1 O6 C13 O5 5.4(7) 2 . . . ?
Cd1 O6 C13 C12 -170.7(5) 2 . . . ?
C11 C12 C13 O5 144.8(7) . . . . ?
C14 C12 C13 O5 -40.0(9) . . . . ?
C11 C12 C13 O6 -38.9(9) . . . . ?
C14 C12 C13 O6 136.2(6) . . . . ?
C11 C12 C14 C15 1.1(8) . . . . ?
C13 C12 C14 C15 -174.4(5) . . . . ?
C10 C9 C15 C14 0.2(9) . . . . ?
C8 C9 C15 C14 180.0(5) . . . . ?
C12 C14 C15 C9 -0.7(9) . . . . ?
C20 N2 C16 C17 1.0(11) . . . . ?
Cd1 N2 C16 C17 171.9(6) . . . . ?
N2 C16 C17 C18 -0.7(13) . . . . ?
C16 C17 C18 C19 0.0(13) . . . . ?
C17 C18 C19 C20 0.4(12) . . . . ?
C16 N2 C20 C19 -0.6(9) . . . . ?
Cd1 N2 C20 C19 -172.1(5) . . . . ?
C16 N2 C20 C21 178.7(6) . . . . ?
Cd1 N2 C20 C21 7.2(7) . . . . ?
C18 C19 C20 N2 -0.1(10) . . . . ?
C18 C19 C20 C21 -179.3(6) . . . . ?
C25 N3 C21 C22 -1.7(9) . . . . ?
Cd1 N3 C21 C22 -175.3(4) . . . . ?
C25 N3 C21 C20 179.5(6) . . . . ?
Cd1 N3 C21 C20 5.9(7) . . . . ?
N2 C20 C21 N3 -8.6(8) . . . . ?
C19 C20 C21 N3 170.7(6) . . . . ?
N2 C20 C21 C22 172.6(5) . . . . ?
C19 C20 C21 C22 -8.1(9) . . . . ?
N3 C21 C22 C23 1.0(9) . . . . ?
C20 C21 C22 C23 179.7(6) . . . . ?
C21 C22 C23 C24 -0.1(10) . . . . ?
C22 C23 C24 C25 0.1(11) . . . . ?
C21 N3 C25 C24 1.7(11) . . . . ?
Cd1 N3 C25 C24 175.2(6) . . . . ?
C23 C24 C25 N3 -0.8(12) . . . . ?
C30 N4 C26 C27 0.6(10) . . . . ?
Cd2 N4 C26 C27 -165.6(5) . . . . ?
N4 C26 C27 C28 0.5(12) . . . . ?
C26 C27 C28 C29 -1.1(13) . . . . ?
C27 C28 C29 C30 0.7(13) . . . . ?
C26 N4 C30 C29 -1.0(9) . . . . ?
Cd2 N4 C30 C29 166.0(5) . . . . ?
C26 N4 C30 C31 179.0(6) . . . . ?
Cd2 N4 C30 C31 -14.1(7) . . . . ?
C28 C29 C30 N4 0.4(11) . . . . ?
C28 C29 C30 C31 -179.6(7) . . . . ?
C35 N5 C31 C32 -3.6(9) . . . . ?
Cd2 N5 C31 C32 177.3(5) . . . . ?
C35 N5 C31 C30 178.5(6) . . . . ?
Cd2 N5 C31 C30 -0.6(7) . . . . ?
N4 C30 C31 N5 9.8(8) . . . . ?
C29 C30 C31 N5 -170.2(6) . . . . ?
N4 C30 C31 C32 -168.1(6) . . . . ?
C29 C30 C31 C32 11.9(10) . . . . ?
N5 C31 C32 C33 1.8(11) . . . . ?
C30 C31 C32 C33 179.6(7) . . . . ?
C31 C32 C33 C34 1.0(13) . . . . ?
C32 C33 C34 C35 -1.8(13) . . . . ?
C31 N5 C35 C34 2.8(11) . . . . ?
Cd2 N5 C35 C34 -178.1(6) . . . . ?
C33 C34 C35 N5 -0.2(12) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C34 H34 O5 0.93 2.65 3.542(9) 161.1 .
C26 H26 O4 0.93 2.63 3.394(11) 139.5 2_666
O9 H1 O10 0.78 2.45 2.998(9) 128.7 2_565
O9 H1 O10 0.78 2.44 2.957(8) 124.4 .
C34 H34 O5 0.93 2.65 3.542(9) 161.1 .
C26 H26 O4 0.93 2.63 3.394(11) 139.5 2_666
O9 H1 O10 0.78 2.45 2.998(9) 128.7 2_565
O9 H1 O10 0.78 2.44 2.957(8) 124.4 .
O9 H1 O10 0.78 2.45 2.998(9) 128.7 2_565
O9 H1 O10 0.78 2.44 2.957(8) 124.4 .
C34 H34 O5 0.93 2.65 3.542(9) 161.1 .
C26 H26 O4 0.93 2.63 3.394(11) 139.5 2_666
O10 H1W O6 0.83 2.30 2.907(8) 130.3 1_565
O10 H2W O4 0.83 2.45 2.740(9) 101.8 2_666
C34 H34 O5 0.93 2.65 3.542(9) 161.1 .
C26 H26 O4 0.93 2.63 3.394(11) 139.5 2_666
O10 H1W O6 0.83 2.30 2.907(8) 130.3 1_565
O10 H2W O4 0.83 2.45 2.740(9) 101.8 2_666
C26 H26 O4 0.93 2.63 3.394(11) 139.5 2_666
C25 H25 O4 0.93 2.68 3.530(10) 151.7 2_666
O10 H1W O9 0.83 2.79 2.998(9) 96.5 2_565
O10 H1W O6 0.83 2.30 2.907(8) 130.3 1_565
O9 H1 O10 0.78 2.44 2.957(8) 124.4 .
C27 H27 O8 0.93 2.84 3.261(11) 108.6 1_565
C26 H26 O4 0.93 2.63 3.394(11) 139.5 2_666
C26 H26 O3 0.93 2.95 3.333(9) 106.1 2_666
O10 H1W O9 0.83 2.79 2.998(9) 96.5 2_565
O10 H1W O6 0.83 2.30 2.907(8) 130.3 1_565
O10 H1W O6 0.83 2.30 2.907(8) 130.3 1_565
O10 H1W O9 0.83 2.79 2.998(9) 96.5 2_565
C25 H25 O4 0.93 2.68 3.530(10) 151.7 2_666
C26 H26 O4 0.93 2.63 3.394(11) 139.5 2_666
C27 H27 O8 0.93 2.84 3.261(11) 108.6 1_565
O9 H1 O10 0.78 2.44 2.957(8) 124.4 .
O10 H1W O6 0.83 2.30 2.907(8) 130.3 1_565
O10 H1W O9 0.83 2.79 2.998(9) 96.5 2_565
C25 H25 O4 0.93 2.68 3.530(10) 151.7 2_666
C26 H26 O4 0.93 2.63 3.394(11) 139.5 2_666
O9 H1 O10 0.78 2.44 2.957(8) 124.4 .
O10 H2W O4 0.83 2.45 2.740(9) 101.8 2_666
O10 H1W O6 0.83 2.30 2.907(8) 130.3 1_565
C26 H26 O4 0.93 2.63 3.394(11) 139.5 2_666
C34 H34 O5 0.93 2.65 3.542(9) 161.1 .
O9 H1 O10 0.78 2.44 2.957(8) 124.4 .
O9 H1 O10 0.78 2.45 2.998(9) 128.7 2_565
C25 H25 O4 0.93 2.68 3.530(10) 151.7 2_666
C26 H26 O4 0.93 2.63 3.394(11) 139.5 2_666
C34 H34 O5 0.93 2.65 3.542(9) 161.1 .

_refine_diff_density_max         1.041
_refine_diff_density_min         -0.684
_refine_diff_density_rms         0.105

####################################################################### 
# 
# 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_315-12Zn
_database_code_depnum_ccdc_archive 'CCDC 1589518'
_audit_update_record             
;
2017-12-06 deposited with the CCDC.
2018-04-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C25 H17 N3 O9 Zn'
_chemical_formula_weight         568.78

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           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                   9.8401(7)
_cell_length_b                   28.4620(16)
_cell_length_c                   8.4345(5)
_cell_angle_alpha                90
_cell_angle_beta                 101.113(7)
_cell_angle_gamma                90
_cell_volume                     2317.9(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8498
_cell_measurement_theta_min      3.249
_cell_measurement_theta_max      25.049

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_F_000             1160
_exptl_transmission_factor_min   0.746
_exptl_transmission_factor_max   0.764
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.240
_exptl_absorpt_coefficient_mu    1.123
_shelx_estimated_absorpt_T_min   0.751
_shelx_estimated_absorpt_T_max   0.774
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.751
_exptl_absorpt_correction_T_max  0.774
_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            8498
_diffrn_reflns_av_unetI/netI     0.1403
_diffrn_reflns_av_R_equivalents  0.0696
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.249
_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             4084
_reflns_number_gt                2251
_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)+(0.0101P)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         4084
_refine_ls_number_parameters     347
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1301
_refine_ls_R_factor_gt           0.0614
_refine_ls_wR_factor_ref         0.1127
_refine_ls_wR_factor_gt          0.0806
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.034
_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 0.78645(7) 0.13575(2) 0.49154(7) 0.0394(2) Uani 1 1 d . . . . .
N1 N 0.7323(5) -0.13265(16) 0.5426(5) 0.0372(12) Uani 1 1 d . . . . .
N2 N 0.8728(5) 0.19968(16) 0.5636(5) 0.0375(12) Uani 1 1 d . . . . .
N3 N 0.6517(5) 0.18125(16) 0.3388(5) 0.0411(13) Uani 1 1 d . . . . .
O1 O 0.6611(4) 0.08673(13) 0.5409(4) 0.0369(10) Uani 1 1 d . . . . .
O2 O 0.7033(4) 0.12869(13) 0.7655(4) 0.0472(11) Uani 1 1 d . . . . .
O3 O 0.1229(4) 0.05743(14) 0.9358(4) 0.0445(11) Uani 1 1 d . . . . .
H1 H 0.0611 0.0734 0.9611 0.067 Uiso 1 1 calc R U . . .
O4 O 0.2258(5) 0.12692(16) 0.9371(5) 0.0708(14) Uani 1 1 d . . . . .
O5 O 1.1132(4) -0.10333(14) 0.6731(4) 0.0446(11) Uani 1 1 d . . . . .
O6 O 1.0104(4) -0.09773(13) 0.4183(4) 0.0427(10) Uani 1 1 d . . . . .
O7 O 0.8298(5) -0.15957(14) 0.5620(5) 0.0613(13) Uani 1 1 d . . . . .
O8 O 0.6131(4) -0.14449(14) 0.4916(5) 0.0582(13) Uani 1 1 d . . . . .
C1 C 0.6465(5) 0.09479(19) 0.6845(6) 0.0313(14) Uani 1 1 d . . . . .
C2 C 0.5507(6) 0.06286(19) 0.7526(5) 0.0285(13) Uani 1 1 d . . . . .
C3 C 0.4459(6) 0.08486(19) 0.8142(5) 0.0358(15) Uani 1 1 d . . . . .
H3 H 0.4480 0.1173 0.8277 0.043 Uiso 1 1 calc R U . . .
C4 C 0.3375(6) 0.0590(2) 0.8560(5) 0.0346(15) Uani 1 1 d . . . . .
C5 C 0.2251(7) 0.0849(2) 0.9137(6) 0.0399(16) Uani 1 1 d . . . . .
C6 C 0.3375(6) 0.0108(2) 0.8409(6) 0.0360(14) Uani 1 1 d . . . . .
H6 H 0.2649 -0.0069 0.8660 0.043 Uiso 1 1 calc R U . . .
C7 C 0.4456(6) -0.0112(2) 0.7886(5) 0.0364(15) Uani 1 1 d . . . . .
H7 H 0.4458 -0.0438 0.7832 0.044 Uiso 1 1 calc R U . . .
C8 C 0.5542(6) 0.01330(18) 0.7434(5) 0.0275(13) Uani 1 1 d . . . . .
C9 C 0.6708(6) -0.01304(19) 0.6952(5) 0.0282(13) Uani 1 1 d . . . . .
C10 C 0.6502(6) -0.05778(18) 0.6280(5) 0.0305(14) Uani 1 1 d . . . . .
H10 H 0.5616 -0.0705 0.6056 0.037 Uiso 1 1 calc R U . . .
C11 C 0.7599(6) -0.08321(18) 0.5946(5) 0.0281(13) Uani 1 1 d . . . . .
C12 C 0.8934(6) -0.06541(18) 0.6152(5) 0.0275(13) Uani 1 1 d . . . . .
C13 C 1.0102(6) -0.09049(19) 0.5634(6) 0.0332(14) Uani 1 1 d . . . . .
C14 C 0.9129(6) -0.02083(19) 0.6813(6) 0.0348(14) Uani 1 1 d . . . . .
H14 H 1.0007 -0.0074 0.6969 0.042 Uiso 1 1 calc R U . . .
C15 C 0.8061(6) 0.00423(19) 0.7244(6) 0.0371(15) Uani 1 1 d . . . . .
H15 H 0.8244 0.0333 0.7741 0.044 Uiso 1 1 calc R U . . .
C16 C 0.9898(7) 0.2059(2) 0.6707(6) 0.0516(18) Uani 1 1 d . . . . .
H16 H 1.0352 0.1798 0.7218 0.062 Uiso 1 1 calc R U . . .
O9 O 0.9052(4) 0.09536(16) 0.0141(4) 0.0726(16) Uani 1 1 d DG . . . .
H1W H 0.8380 0.1068 -0.0476 0.087 Uiso 1 1 d DR U . . .
H2W H 0.8908 0.0994 0.1094 0.087 Uiso 1 1 d R U . . .
C17 C 1.0460(7) 0.2499(2) 0.7082(7) 0.060(2) Uani 1 1 d . . . . .
H17 H 1.1271 0.2536 0.7844 0.072 Uiso 1 1 calc R U . . .
C18 C 0.9781(8) 0.2884(2) 0.6290(7) 0.064(2) Uani 1 1 d . . . . .
H18 H 1.0136 0.3185 0.6512 0.077 Uiso 1 1 calc R U . . .
C19 C 0.8576(7) 0.2818(2) 0.5173(7) 0.0562(19) Uani 1 1 d . . . . .
H19 H 0.8114 0.3073 0.4630 0.067 Uiso 1 1 calc R U . . .
C20 C 0.8066(6) 0.23722(19) 0.4867(6) 0.0369(15) Uani 1 1 d . . . . .
C21 C 0.6802(6) 0.2267(2) 0.3656(6) 0.0385(15) Uani 1 1 d . . . . .
C22 C 0.5952(7) 0.2613(2) 0.2810(6) 0.0489(18) Uani 1 1 d . . . . .
H22 H 0.6163 0.2929 0.2989 0.059 Uiso 1 1 calc R U . . .
C23 C 0.4803(7) 0.2480(2) 0.1714(7) 0.059(2) Uani 1 1 d . . . . .
H23 H 0.4213 0.2706 0.1160 0.071 Uiso 1 1 calc R U . . .
C24 C 0.4520(7) 0.2005(2) 0.1433(7) 0.060(2) Uani 1 1 d . . . . .
H24 H 0.3760 0.1906 0.0672 0.072 Uiso 1 1 calc R U . . .
C25 C 0.5398(6) 0.1691(2) 0.2315(7) 0.0525(18) Uani 1 1 d . . . . .
H25 H 0.5205 0.1372 0.2158 0.063 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 O1 1.959(4) . ?
Zn1 N2 2.050(4) . ?
Zn1 O5 2.069(4) 3_756 ?
Zn1 N3 2.106(4) . ?
Zn1 O6 2.271(4) 3_756 ?
Zn1 C13 2.497(6) 3_756 ?
N1 O7 1.214(5) . ?
N1 O8 1.216(5) . ?
N1 C11 1.484(6) . ?
N2 C16 1.331(6) . ?
N2 C20 1.350(6) . ?
N3 C25 1.329(6) . ?
N3 C21 1.335(7) . ?
O1 C1 1.268(5) . ?
O2 C1 1.250(6) . ?
O3 C5 1.315(7) . ?
O3 H1 0.8200 . ?
O4 C5 1.213(7) . ?
O5 C13 1.287(6) . ?
O5 Zn1 2.069(4) 3_756 ?
O6 C13 1.241(5) . ?
O6 Zn1 2.271(4) 3_756 ?
C1 C2 1.501(7) . ?
C2 C3 1.390(7) . ?
C2 C8 1.414(7) . ?
C3 C4 1.396(7) . ?
C3 H3 0.9300 . ?
C4 C6 1.379(7) . ?
C4 C5 1.486(8) . ?
C6 C7 1.378(7) . ?
C6 H6 0.9300 . ?
C7 C8 1.390(7) . ?
C7 H7 0.9300 . ?
C8 C9 1.491(7) . ?
C9 C10 1.392(6) . ?
C9 C15 1.396(7) . ?
C10 C11 1.373(7) . ?
C10 H10 0.9300 . ?
C11 C12 1.387(7) . ?
C12 C14 1.384(6) . ?
C12 C13 1.489(7) . ?
C13 Zn1 2.497(6) 3_756 ?
C14 C15 1.376(7) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C17 1.381(8) . ?
C16 H16 0.9300 . ?
O9 H1W 0.8253 . ?
O9 H2W 0.8501 . ?
C17 C18 1.385(8) . ?
C17 H17 0.9300 . ?
C18 C19 1.378(8) . ?
C18 H18 0.9300 . ?
C19 C20 1.369(7) . ?
C19 H19 0.9300 . ?
C20 C21 1.480(7) . ?
C21 C22 1.394(7) . ?
C22 C23 1.369(8) . ?
C22 H22 0.9300 . ?
C23 C24 1.392(8) . ?
C23 H23 0.9300 . ?
C24 C25 1.361(7) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Zn1 N2 144.17(16) . . ?
O1 Zn1 O5 103.08(16) . 3_756 ?
N2 Zn1 O5 111.77(17) . 3_756 ?
O1 Zn1 N3 102.69(17) . . ?
N2 Zn1 N3 79.15(18) . . ?
O5 Zn1 N3 100.90(16) 3_756 . ?
O1 Zn1 O6 98.00(14) . 3_756 ?
N2 Zn1 O6 92.06(17) . 3_756 ?
O5 Zn1 O6 60.63(12) 3_756 3_756 ?
N3 Zn1 O6 155.14(17) . 3_756 ?
O1 Zn1 C13 103.41(17) . 3_756 ?
N2 Zn1 C13 102.24(19) . 3_756 ?
O5 Zn1 C13 30.97(13) 3_756 3_756 ?
N3 Zn1 C13 129.51(18) . 3_756 ?
O6 Zn1 C13 29.70(13) 3_756 3_756 ?
O7 N1 O8 123.8(5) . . ?
O7 N1 C11 117.6(5) . . ?
O8 N1 C11 118.5(5) . . ?
C16 N2 C20 119.6(5) . . ?
C16 N2 Zn1 125.0(4) . . ?
C20 N2 Zn1 115.2(4) . . ?
C25 N3 C21 119.2(5) . . ?
C25 N3 Zn1 126.7(4) . . ?
C21 N3 Zn1 114.0(4) . . ?
C1 O1 Zn1 105.4(3) . . ?
C5 O3 H1 109.5 . . ?
C13 O5 Zn1 93.2(3) . 3_756 ?
C13 O6 Zn1 85.3(3) . 3_756 ?
O2 C1 O1 122.7(5) . . ?
O2 C1 C2 120.4(5) . . ?
O1 C1 C2 116.8(5) . . ?
C3 C2 C8 119.8(5) . . ?
C3 C2 C1 115.9(5) . . ?
C8 C2 C1 124.0(5) . . ?
C2 C3 C4 121.0(5) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 H3 119.5 . . ?
C6 C4 C3 119.2(6) . . ?
C6 C4 C5 122.4(6) . . ?
C3 C4 C5 118.3(5) . . ?
O4 C5 O3 122.9(6) . . ?
O4 C5 C4 124.1(6) . . ?
O3 C5 C4 113.0(5) . . ?
C7 C6 C4 119.6(6) . . ?
C7 C6 H6 120.2 . . ?
C4 C6 H6 120.2 . . ?
C6 C7 C8 122.9(5) . . ?
C6 C7 H7 118.6 . . ?
C8 C7 H7 118.6 . . ?
C7 C8 C2 117.2(5) . . ?
C7 C8 C9 119.7(5) . . ?
C2 C8 C9 123.0(5) . . ?
C10 C9 C15 116.9(5) . . ?
C10 C9 C8 120.8(5) . . ?
C15 C9 C8 122.2(5) . . ?
C11 C10 C9 120.5(5) . . ?
C11 C10 H10 119.7 . . ?
C9 C10 H10 119.7 . . ?
C10 C11 C12 123.0(5) . . ?
C10 C11 N1 117.0(5) . . ?
C12 C11 N1 119.9(5) . . ?
C11 C12 C14 116.1(5) . . ?
C11 C12 C13 123.7(5) . . ?
C14 C12 C13 120.2(5) . . ?
O6 C13 O5 120.7(5) . . ?
O6 C13 C12 121.1(5) . . ?
O5 C13 C12 118.1(5) . . ?
O6 C13 Zn1 65.0(3) . 3_756 ?
O5 C13 Zn1 55.9(3) . 3_756 ?
C12 C13 Zn1 173.6(4) . 3_756 ?
C15 C14 C12 121.9(5) . . ?
C15 C14 H14 119.1 . . ?
C12 C14 H14 119.1 . . ?
C14 C15 C9 121.5(5) . . ?
C14 C15 H15 119.3 . . ?
C9 C15 H15 119.3 . . ?
N2 C16 C17 122.1(6) . . ?
N2 C16 H16 118.9 . . ?
C17 C16 H16 118.9 . . ?
H1W O9 H2W 106.5 . . ?
C16 C17 C18 118.2(6) . . ?
C16 C17 H17 120.9 . . ?
C18 C17 H17 120.9 . . ?
C19 C18 C17 119.5(6) . . ?
C19 C18 H18 120.3 . . ?
C17 C18 H18 120.3 . . ?
C18 C19 C20 119.5(6) . . ?
C18 C19 H19 120.3 . . ?
C20 C19 H19 120.3 . . ?
N2 C20 C19 121.1(5) . . ?
N2 C20 C21 115.8(5) . . ?
C19 C20 C21 123.0(5) . . ?
N3 C21 C22 120.8(5) . . ?
N3 C21 C20 115.7(5) . . ?
C22 C21 C20 123.5(5) . . ?
C23 C22 C21 119.1(6) . . ?
C23 C22 H22 120.4 . . ?
C21 C22 H22 120.4 . . ?
C22 C23 C24 119.7(6) . . ?
C22 C23 H23 120.1 . . ?
C24 C23 H23 120.1 . . ?
C25 C24 C23 117.4(6) . . ?
C25 C24 H24 121.3 . . ?
C23 C24 H24 121.3 . . ?
N3 C25 C24 123.8(6) . . ?
N3 C25 H25 118.1 . . ?
C24 C25 H25 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
Zn1 O1 C1 O2 1.2(6) . . . . ?
Zn1 O1 C1 C2 178.2(4) . . . . ?
O2 C1 C2 C3 51.2(6) . . . . ?
O1 C1 C2 C3 -125.9(5) . . . . ?
O2 C1 C2 C8 -134.8(5) . . . . ?
O1 C1 C2 C8 48.2(7) . . . . ?
C8 C2 C3 C4 -5.0(7) . . . . ?
C1 C2 C3 C4 169.3(4) . . . . ?
C2 C3 C4 C6 2.2(7) . . . . ?
C2 C3 C4 C5 -177.1(4) . . . . ?
C6 C4 C5 O4 175.6(5) . . . . ?
C3 C4 C5 O4 -5.1(8) . . . . ?
C6 C4 C5 O3 -5.0(7) . . . . ?
C3 C4 C5 O3 174.3(4) . . . . ?
C3 C4 C6 C7 1.5(7) . . . . ?
C5 C4 C6 C7 -179.2(4) . . . . ?
C4 C6 C7 C8 -2.5(7) . . . . ?
C6 C7 C8 C2 -0.1(7) . . . . ?
C6 C7 C8 C9 177.2(4) . . . . ?
C3 C2 C8 C7 3.8(7) . . . . ?
C1 C2 C8 C7 -170.0(4) . . . . ?
C3 C2 C8 C9 -173.4(4) . . . . ?
C1 C2 C8 C9 12.8(7) . . . . ?
C7 C8 C9 C10 27.8(6) . . . . ?
C2 C8 C9 C10 -155.0(4) . . . . ?
C7 C8 C9 C15 -147.8(5) . . . . ?
C2 C8 C9 C15 29.4(7) . . . . ?
C15 C9 C10 C11 0.6(7) . . . . ?
C8 C9 C10 C11 -175.3(4) . . . . ?
C9 C10 C11 C12 -4.2(7) . . . . ?
C9 C10 C11 N1 172.6(4) . . . . ?
O7 N1 C11 C10 -157.0(5) . . . . ?
O8 N1 C11 C10 19.0(7) . . . . ?
O7 N1 C11 C12 19.8(7) . . . . ?
O8 N1 C11 C12 -164.1(5) . . . . ?
C10 C11 C12 C14 3.7(7) . . . . ?
N1 C11 C12 C14 -172.9(4) . . . . ?
C10 C11 C12 C13 -173.2(4) . . . . ?
N1 C11 C12 C13 10.1(7) . . . . ?
Zn1 O6 C13 O5 4.1(5) 3_756 . . . ?
Zn1 O6 C13 C12 -177.9(5) 3_756 . . . ?
Zn1 O5 C13 O6 -4.5(5) 3_756 . . . ?
Zn1 O5 C13 C12 177.4(4) 3_756 . . . ?
C11 C12 C13 O6 66.0(7) . . . . ?
C14 C12 C13 O6 -110.8(6) . . . . ?
C11 C12 C13 O5 -115.9(6) . . . . ?
C14 C12 C13 O5 67.3(7) . . . . ?
C11 C12 C14 C15 0.2(7) . . . . ?
C13 C12 C14 C15 177.3(4) . . . . ?
C12 C14 C15 C9 -3.7(8) . . . . ?
C10 C9 C15 C14 3.2(7) . . . . ?
C8 C9 C15 C14 179.0(4) . . . . ?
C20 N2 C16 C17 0.9(9) . . . . ?
Zn1 N2 C16 C17 176.8(5) . . . . ?
N2 C16 C17 C18 -0.9(10) . . . . ?
C16 C17 C18 C19 0.3(11) . . . . ?
C17 C18 C19 C20 0.3(11) . . . . ?
C16 N2 C20 C19 -0.2(9) . . . . ?
Zn1 N2 C20 C19 -176.5(5) . . . . ?
C16 N2 C20 C21 177.8(5) . . . . ?
Zn1 N2 C20 C21 1.5(6) . . . . ?
C18 C19 C20 N2 -0.4(10) . . . . ?
C18 C19 C20 C21 -178.2(6) . . . . ?
C25 N3 C21 C22 -0.8(9) . . . . ?
Zn1 N3 C21 C22 -176.0(4) . . . . ?
C25 N3 C21 C20 -180.0(5) . . . . ?
Zn1 N3 C21 C20 4.8(7) . . . . ?
N2 C20 C21 N3 -4.3(8) . . . . ?
C19 C20 C21 N3 173.7(6) . . . . ?
N2 C20 C21 C22 176.6(5) . . . . ?
C19 C20 C21 C22 -5.5(10) . . . . ?
N3 C21 C22 C23 1.0(10) . . . . ?
C20 C21 C22 C23 -179.9(6) . . . . ?
C21 C22 C23 C24 -1.6(10) . . . . ?
C22 C23 C24 C25 1.9(11) . . . . ?
C21 N3 C25 C24 1.2(10) . . . . ?
Zn1 N3 C25 C24 175.7(5) . . . . ?
C23 C24 C25 N3 -1.7(11) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C24 H24 O4 0.93 2.46 3.297(8) 149.9 1_554
C22 H22 O2 0.93 2.43 3.318(7) 160.9 4_565
C19 H19 O2 0.93 2.56 3.474(7) 168.5 4_565
O9 H2W O5 0.85 1.85 2.688(5) 170.7 3_756
O9 H1W O2 0.83 1.96 2.764(5) 166.0 1_554
C16 H16 O6 0.93 2.62 3.169(8) 118.6 3_756
C10 H10 O1 0.93 2.34 3.226(6) 158.2 3_656
O3 H1 O9 0.82 1.79 2.596(5) 166.5 1_456
O9 H1W O2 0.83 1.96 2.764(5) 166.0 1_554
C24 H24 O4 0.93 2.46 3.297(8) 149.9 1_554
C22 H22 O2 0.93 2.43 3.318(7) 160.9 4_565
C19 H19 O2 0.93 2.56 3.474(7) 168.5 4_565
O9 H2W O5 0.85 1.85 2.688(5) 170.7 3_756
C16 H16 O6 0.93 2.62 3.169(8) 118.6 3_756
C10 H10 O1 0.93 2.34 3.226(6) 158.2 3_656
O3 H1 O9 0.82 1.79 2.596(5) 166.5 1_456
C24 H24 O4 0.93 2.46 3.297(8) 149.9 1_554
C22 H22 O2 0.93 2.43 3.318(7) 160.9 4_565
C19 H19 O2 0.93 2.56 3.474(7) 168.5 4_565
C16 H16 O6 0.93 2.62 3.169(8) 118.6 3_756
C10 H10 O1 0.93 2.34 3.226(6) 158.2 3_656
C10 H10 O1 0.93 2.34 3.226(6) 158.2 3_656
C16 H16 O6 0.93 2.62 3.169(8) 118.6 3_756
C19 H19 O2 0.93 2.56 3.474(7) 168.5 4_565
C22 H22 O2 0.93 2.43 3.318(7) 160.9 4_565
C24 H24 O4 0.93 2.46 3.297(8) 149.9 1_554

_refine_diff_density_max         0.455
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.091

####################################################################### 
# 
# 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_316-11Cd
_database_code_depnum_ccdc_archive 'CCDC 1589524'
_audit_update_record             
;
2017-12-06 deposited with the CCDC.
2018-04-30 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 H25 Cd2 N5 O10'
_chemical_formula_weight         948.44

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      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                   11.4599(6)
_cell_length_b                   12.1509(8)
_cell_length_c                   13.8435(8)
_cell_angle_alpha                105.284(5)
_cell_angle_beta                 107.683(5)
_cell_angle_gamma                91.786(5)
_cell_volume                     1758.62(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    11317
_cell_measurement_theta_min      3.261
_cell_measurement_theta_max      25.049

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.791
_exptl_crystal_F_000             940
_exptl_transmission_factor_min   0.724
_exptl_transmission_factor_max   0.755
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.220
_exptl_absorpt_coefficient_mu    1.279
_shelx_estimated_absorpt_T_min   0.732
_shelx_estimated_absorpt_T_max   0.766
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.732
_exptl_absorpt_correction_T_max  0.766
_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            11317
_diffrn_reflns_av_unetI/netI     0.0622
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.261
_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             6225
_reflns_number_gt                4668
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     'w=1/[σ²(Fo²)] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6225
_refine_ls_number_parameters     509
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0392
_refine_ls_wR_factor_ref         0.0554
_refine_ls_wR_factor_gt          0.0489
_refine_ls_goodness_of_fit_ref   1.160
_refine_ls_restrained_S_all      1.160
_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 0.36518(3) 0.01803(3) 0.24448(2) 0.03410(10) Uani 1 1 d . . . . .
Cd2 Cd 0.19727(3) 0.20117(3) 0.41785(2) 0.03417(10) Uani 1 1 d . . . . .
H1 H 0.373(3) 0.079(3) 0.430(3) 0.000(12) Uiso 1 1 d . . . . .
N1 N 0.5942(4) 0.5693(4) 0.1806(3) 0.0480(11) Uani 1 1 d . . . . .
N2 N 0.5318(3) 0.1543(3) 0.2728(3) 0.0339(9) Uani 1 1 d . . . . .
N3 N 0.4809(3) -0.0597(3) 0.1336(3) 0.0353(9) Uani 1 1 d . . . . .
N4 N 0.0297(3) 0.0561(3) 0.3685(3) 0.0360(9) Uani 1 1 d . . . . .
N5 N 0.0522(3) 0.2708(3) 0.5030(3) 0.0405(10) Uani 1 1 d . . . . .
O1 O 0.2514(3) 0.1603(3) 0.1840(2) 0.0572(10) Uani 1 1 d . . . . .
O2 O 0.1231(3) 0.2469(3) 0.2664(2) 0.0496(9) Uani 1 1 d . . . . .
O3 O -0.2223(3) 0.2528(3) -0.2083(3) 0.0687(11) Uani 1 1 d . . . . .
O4 O -0.2064(3) 0.1101(3) -0.1337(2) 0.0488(9) Uani 1 1 d . . . . .
O5 O 0.6502(2) 0.7409(3) 0.3910(2) 0.0410(8) Uani 1 1 d . . . . .
O6 O 0.6721(3) 0.6232(3) 0.4915(2) 0.0447(8) Uani 1 1 d . . . . .
O7 O 0.5683(3) 0.6034(4) 0.1036(3) 0.0972(15) Uani 1 1 d . . . . .
O8 O 0.6990(3) 0.5540(4) 0.2275(3) 0.0783(13) Uani 1 1 d . . . . .
O9 O 0.4425(3) -0.1357(3) 0.3322(2) 0.0532(9) Uani 1 1 d . . . . .
H2W H 0.5044 -0.1715 0.3501 0.064 Uiso 1 1 d R U . . .
H1W H 0.3726 -0.1727 0.2931 0.064 Uiso 1 1 d R U . . .
O10 O 0.3333(4) 0.0900(4) 0.3909(3) 0.0483(11) Uani 1 1 d . . . . .
C1 C 0.1698(4) 0.2218(4) 0.1923(3) 0.0342(11) Uani 1 1 d . . . . .
C2 C 0.1168(4) 0.2761(4) 0.1027(3) 0.0298(10) Uani 1 1 d . . . . .
C3 C 0.0068(4) 0.2221(4) 0.0257(3) 0.0334(11) Uani 1 1 d . . . . .
H3 H -0.0320 0.1572 0.0319 0.040 Uiso 1 1 calc R U . . .
C4 C -0.0469(4) 0.2625(4) -0.0607(3) 0.0322(11) Uani 1 1 d . . . . .
C5 C -0.1697(4) 0.2057(4) -0.1416(4) 0.0402(12) Uani 1 1 d . . . . .
C6 C 0.0139(4) 0.3571(4) -0.0696(3) 0.0432(12) Uani 1 1 d . . . . .
H6 H -0.0201 0.3857 -0.1268 0.052 Uiso 1 1 calc R U . . .
C7 C 0.1252(4) 0.4100(4) 0.0057(3) 0.0398(12) Uani 1 1 d . . . . .
H7 H 0.1660 0.4723 -0.0030 0.048 Uiso 1 1 calc R U . . .
C8 C 0.1772(4) 0.3725(4) 0.0934(3) 0.0292(10) Uani 1 1 d . . . . .
C9 C 0.2940(4) 0.4373(3) 0.1744(3) 0.0292(10) Uani 1 1 d . . . . .
C10 C 0.3879(4) 0.4769(4) 0.1432(3) 0.0336(11) Uani 1 1 d . . . . .
H10 H 0.3799 0.4606 0.0718 0.040 Uiso 1 1 calc R U . . .
C11 C 0.4922(4) 0.5403(4) 0.2187(3) 0.0316(11) Uani 1 1 d . . . . .
C12 C 0.5113(4) 0.5702(3) 0.3263(3) 0.0296(10) Uani 1 1 d . . . . .
C13 C 0.6202(4) 0.6502(4) 0.4081(3) 0.0304(10) Uani 1 1 d . . . . .
C14 C 0.4183(4) 0.5288(4) 0.3560(3) 0.0335(11) Uani 1 1 d . . . . .
H14 H 0.4273 0.5457 0.4276 0.040 Uiso 1 1 calc R U . . .
C15 C 0.3125(4) 0.4632(3) 0.2831(3) 0.0333(11) Uani 1 1 d . . . . .
H15 H 0.2525 0.4357 0.3064 0.040 Uiso 1 1 calc R U . . .
C16 C 0.5547(4) 0.2589(4) 0.3377(4) 0.0453(13) Uani 1 1 d . . . . .
H16 H 0.4989 0.2831 0.3733 0.054 Uiso 1 1 calc R U . . .
C17 C 0.6571(5) 0.3354(4) 0.3565(4) 0.0560(14) Uani 1 1 d . . . . .
H17 H 0.6703 0.4084 0.4039 0.067 Uiso 1 1 calc R U . . .
C18 C 0.7376(4) 0.2997(4) 0.3032(4) 0.0534(14) Uani 1 1 d . . . . .
H18 H 0.8067 0.3493 0.3137 0.064 Uiso 1 1 calc R U . . .
C19 C 0.7178(4) 0.1906(5) 0.2334(4) 0.0446(13) Uani 1 1 d . . . . .
C20 C 0.6112(4) 0.1203(4) 0.2193(3) 0.0332(11) Uani 1 1 d . . . . .
C21 C 0.7974(5) 0.1499(5) 0.1727(4) 0.0627(16) Uani 1 1 d . . . . .
H21 H 0.8678 0.1965 0.1812 0.075 Uiso 1 1 calc R U . . .
C22 C 0.7700(5) 0.0441(5) 0.1033(4) 0.0610(16) Uani 1 1 d . . . . .
H22 H 0.8236 0.0187 0.0657 0.073 Uiso 1 1 calc R U . . .
C23 C 0.6631(4) -0.0299(5) 0.0854(3) 0.0433(13) Uani 1 1 d . . . . .
C24 C 0.5835(4) 0.0071(4) 0.1446(3) 0.0337(11) Uani 1 1 d . . . . .
C25 C 0.6289(5) -0.1393(5) 0.0113(4) 0.0567(16) Uani 1 1 d . . . . .
H25 H 0.6777 -0.1670 -0.0304 0.068 Uiso 1 1 calc R U . . .
C26 C 0.5249(5) -0.2049(4) 0.0003(4) 0.0566(15) Uani 1 1 d . . . . .
H26 H 0.5017 -0.2771 -0.0488 0.068 Uiso 1 1 calc R U . . .
C27 C 0.4539(4) -0.1618(4) 0.0639(3) 0.0482(13) Uani 1 1 d . . . . .
H27 H 0.3835 -0.2077 0.0567 0.058 Uiso 1 1 calc R U . . .
C28 C 0.0172(5) -0.0448(4) 0.3007(4) 0.0506(14) Uani 1 1 d . . . . .
H28 H 0.0790 -0.0628 0.2705 0.061 Uiso 1 1 calc R U . . .
C29 C -0.0845(5) -0.1267(4) 0.2715(4) 0.0549(14) Uani 1 1 d . . . . .
H29 H -0.0902 -0.1974 0.2223 0.066 Uiso 1 1 calc R U . . .
C30 C -0.1748(4) -0.1028(4) 0.3152(4) 0.0497(13) Uani 1 1 d . . . . .
H30 H -0.2428 -0.1569 0.2972 0.060 Uiso 1 1 calc R U . . .
C31 C -0.1645(4) 0.0048(4) 0.3882(3) 0.0385(12) Uani 1 1 d . . . . .
C32 C -0.0603(4) 0.0833(4) 0.4122(3) 0.0302(10) Uani 1 1 d . . . . .
C33 C -0.2547(4) 0.0367(5) 0.4388(4) 0.0499(14) Uani 1 1 d . . . . .
H33 H -0.3248 -0.0146 0.4217 0.060 Uiso 1 1 calc R U . . .
C34 C -0.2406(4) 0.1391(5) 0.5105(4) 0.0491(14) Uani 1 1 d . . . . .
H34 H -0.2993 0.1570 0.5443 0.059 Uiso 1 1 calc R U . . .
C35 C -0.1353(4) 0.2213(4) 0.5356(3) 0.0442(13) Uani 1 1 d . . . . .
C36 C -0.0476(4) 0.1945(4) 0.4857(3) 0.0339(11) Uani 1 1 d . . . . .
C37 C -0.1181(5) 0.3285(5) 0.6089(4) 0.0610(16) Uani 1 1 d . . . . .
H37 H -0.1735 0.3473 0.6461 0.073 Uiso 1 1 calc R U . . .
C38 C -0.0203(5) 0.4059(5) 0.6264(4) 0.0730(18) Uani 1 1 d . . . . .
H38 H -0.0089 0.4786 0.6739 0.088 Uiso 1 1 calc R U . . .
C39 C 0.0633(5) 0.3728(4) 0.5706(4) 0.0566(15) Uani 1 1 d . . . . .
H39 H 0.1299 0.4259 0.5821 0.068 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 O10 2.132(4) . ?
Cd1 O4 2.226(3) 2 ?
Cd1 N2 2.355(3) . ?
Cd1 N3 2.357(3) . ?
Cd1 O1 2.373(3) . ?
Cd1 O9 2.529(3) . ?
Cd2 O10 2.148(4) . ?
Cd2 O2 2.233(3) . ?
Cd2 O6 2.370(3) 2_666 ?
Cd2 N4 2.370(4) . ?
Cd2 N5 2.371(3) . ?
Cd2 O5 2.585(3) 2_666 ?
N1 O7 1.203(4) . ?
N1 O8 1.225(4) . ?
N1 C11 1.489(5) . ?
N2 C16 1.314(5) . ?
N2 C20 1.348(4) . ?
N3 C27 1.316(5) . ?
N3 C24 1.354(5) . ?
N4 C28 1.306(5) . ?
N4 C32 1.354(4) . ?
N5 C39 1.317(5) . ?
N5 C36 1.370(5) . ?
O1 C1 1.228(5) . ?
O2 C1 1.270(4) . ?
O3 C5 1.227(5) . ?
O4 C5 1.266(5) . ?
O4 Cd1 2.226(3) 2 ?
O5 C13 1.245(5) . ?
O5 Cd2 2.585(3) 2_666 ?
O6 C13 1.260(4) . ?
O6 Cd2 2.370(3) 2_666 ?
O9 H2W 0.8500 . ?
O9 H1W 0.8500 . ?
O10 H1 0.64(3) . ?
C1 C2 1.530(5) . ?
C2 C3 1.386(5) . ?
C2 C8 1.396(5) . ?
C3 C4 1.390(5) . ?
C3 H3 0.9300 . ?
C4 C6 1.378(6) . ?
C4 C5 1.512(5) . ?
C6 C7 1.383(5) . ?
C6 H6 0.9300 . ?
C7 C8 1.381(5) . ?
C7 H7 0.9300 . ?
C8 C9 1.492(5) . ?
C9 C10 1.392(5) . ?
C9 C15 1.400(5) . ?
C10 C11 1.369(5) . ?
C10 H10 0.9300 . ?
C11 C12 1.381(5) . ?
C12 C14 1.378(5) . ?
C12 C13 1.507(5) . ?
C14 C15 1.378(5) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C17 1.389(6) . ?
C16 H16 0.9300 . ?
C17 C18 1.362(6) . ?
C17 H17 0.9300 . ?
C18 C19 1.384(6) . ?
C18 H18 0.9300 . ?
C19 C20 1.401(6) . ?
C19 C21 1.434(6) . ?
C20 C24 1.444(6) . ?
C21 C22 1.347(6) . ?
C21 H21 0.9300 . ?
C22 C23 1.414(7) . ?
C22 H22 0.9300 . ?
C23 C25 1.406(6) . ?
C23 C24 1.411(5) . ?
C25 C26 1.358(6) . ?
C25 H25 0.9300 . ?
C26 C27 1.389(5) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
C28 C29 1.393(6) . ?
C28 H28 0.9300 . ?
C29 C30 1.353(5) . ?
C29 H29 0.9300 . ?
C30 C31 1.402(6) . ?
C30 H30 0.9300 . ?
C31 C32 1.402(6) . ?
C31 C33 1.425(5) . ?
C32 C36 1.433(6) . ?
C33 C34 1.342(6) . ?
C33 H33 0.9300 . ?
C34 C35 1.436(6) . ?
C34 H34 0.9300 . ?
C35 C36 1.386(5) . ?
C35 C37 1.389(6) . ?
C37 C38 1.360(7) . ?
C37 H37 0.9300 . ?
C38 C39 1.410(6) . ?
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
O10 Cd1 O4 110.21(13) . 2 ?
O10 Cd1 N2 96.81(14) . . ?
O4 Cd1 N2 149.75(11) 2 . ?
O10 Cd1 N3 156.19(13) . . ?
O4 Cd1 N3 88.03(12) 2 . ?
N2 Cd1 N3 70.49(12) . . ?
O10 Cd1 O1 86.30(12) . . ?
O4 Cd1 O1 86.91(12) 2 . ?
N2 Cd1 O1 81.38(12) . . ?
N3 Cd1 O1 110.60(11) . . ?
O10 Cd1 O9 81.83(12) . . ?
O4 Cd1 O9 87.98(11) 2 . ?
N2 Cd1 O9 109.70(11) . . ?
N3 Cd1 O9 83.73(10) . . ?
O1 Cd1 O9 164.59(10) . . ?
O10 Cd2 O2 103.92(12) . . ?
O10 Cd2 O6 99.32(13) . 2_666 ?
O2 Cd2 O6 94.48(11) . 2_666 ?
O10 Cd2 N4 97.51(14) . . ?
O2 Cd2 N4 92.16(11) . . ?
O6 Cd2 N4 159.84(11) 2_666 . ?
O10 Cd2 N5 152.80(14) . . ?
O2 Cd2 N5 100.82(12) . . ?
O6 Cd2 N5 89.78(12) 2_666 . ?
N4 Cd2 N5 70.27(13) . . ?
O10 Cd2 O5 81.89(12) . 2_666 ?
O2 Cd2 O5 147.24(11) . 2_666 ?
O6 Cd2 O5 52.86(9) 2_666 2_666 ?
N4 Cd2 O5 119.38(10) . 2_666 ?
N5 Cd2 O5 83.43(11) . 2_666 ?
O7 N1 O8 123.8(4) . . ?
O7 N1 C11 117.9(4) . . ?
O8 N1 C11 118.3(4) . . ?
C16 N2 C20 117.9(4) . . ?
C16 N2 Cd1 125.4(3) . . ?
C20 N2 Cd1 116.7(3) . . ?
C27 N3 C24 118.4(4) . . ?
C27 N3 Cd1 125.2(3) . . ?
C24 N3 Cd1 116.3(3) . . ?
C28 N4 C32 118.9(4) . . ?
C28 N4 Cd2 124.7(3) . . ?
C32 N4 Cd2 116.4(3) . . ?
C39 N5 C36 117.5(4) . . ?
C39 N5 Cd2 125.9(3) . . ?
C36 N5 Cd2 116.4(3) . . ?
C1 O1 Cd1 146.0(3) . . ?
C1 O2 Cd2 123.5(3) . . ?
C5 O4 Cd1 128.6(3) . 2 ?
C13 O5 Cd2 86.6(2) . 2_666 ?
C13 O6 Cd2 96.2(3) . 2_666 ?
Cd1 O9 H2W 143.5 . . ?
Cd1 O9 H1W 83.5 . . ?
H2W O9 H1W 120.2 . . ?
Cd1 O10 Cd2 127.03(17) . . ?
Cd1 O10 H1 113(4) . . ?
Cd2 O10 H1 120(4) . . ?
O1 C1 O2 128.3(4) . . ?
O1 C1 C2 116.7(4) . . ?
O2 C1 C2 115.0(4) . . ?
C3 C2 C8 119.8(4) . . ?
C3 C2 C1 117.1(4) . . ?
C8 C2 C1 123.0(4) . . ?
C2 C3 C4 121.6(4) . . ?
C2 C3 H3 119.2 . . ?
C4 C3 H3 119.2 . . ?
C6 C4 C3 118.1(4) . . ?
C6 C4 C5 120.9(4) . . ?
C3 C4 C5 121.0(4) . . ?
O3 C5 O4 126.5(5) . . ?
O3 C5 C4 119.0(5) . . ?
O4 C5 C4 114.5(4) . . ?
C4 C6 C7 120.7(4) . . ?
C4 C6 H6 119.7 . . ?
C7 C6 H6 119.7 . . ?
C8 C7 C6 121.5(4) . . ?
C8 C7 H7 119.2 . . ?
C6 C7 H7 119.2 . . ?
C7 C8 C2 118.2(4) . . ?
C7 C8 C9 118.7(4) . . ?
C2 C8 C9 123.0(4) . . ?
C10 C9 C15 117.7(4) . . ?
C10 C9 C8 120.3(4) . . ?
C15 C9 C8 122.1(4) . . ?
C11 C10 C9 119.2(4) . . ?
C11 C10 H10 120.4 . . ?
C9 C10 H10 120.4 . . ?
C10 C11 C12 124.4(4) . . ?
C10 C11 N1 116.4(4) . . ?
C12 C11 N1 119.0(4) . . ?
C14 C12 C11 115.6(4) . . ?
C14 C12 C13 120.2(4) . . ?
C11 C12 C13 124.0(4) . . ?
O5 C13 O6 124.1(4) . . ?
O5 C13 C12 118.0(4) . . ?
O6 C13 C12 117.8(4) . . ?
C15 C14 C12 122.2(4) . . ?
C15 C14 H14 118.9 . . ?
C12 C14 H14 118.9 . . ?
C14 C15 C9 120.8(4) . . ?
C14 C15 H15 119.6 . . ?
C9 C15 H15 119.6 . . ?
N2 C16 C17 124.0(4) . . ?
N2 C16 H16 118.0 . . ?
C17 C16 H16 118.0 . . ?
C18 C17 C16 117.6(5) . . ?
C18 C17 H17 121.2 . . ?
C16 C17 H17 121.2 . . ?
C17 C18 C19 120.8(5) . . ?
C17 C18 H18 119.6 . . ?
C19 C18 H18 119.6 . . ?
C18 C19 C20 117.1(4) . . ?
C18 C19 C21 123.1(5) . . ?
C20 C19 C21 119.6(5) . . ?
N2 C20 C19 122.5(4) . . ?
N2 C20 C24 118.0(4) . . ?
C19 C20 C24 119.5(4) . . ?
C22 C21 C19 120.0(5) . . ?
C22 C21 H21 120.0 . . ?
C19 C21 H21 120.0 . . ?
C21 C22 C23 122.7(5) . . ?
C21 C22 H22 118.7 . . ?
C23 C22 H22 118.7 . . ?
C25 C23 C24 116.6(5) . . ?
C25 C23 C22 124.6(5) . . ?
C24 C23 C22 118.8(5) . . ?
N3 C24 C23 122.4(4) . . ?
N3 C24 C20 118.3(4) . . ?
C23 C24 C20 119.4(4) . . ?
C26 C25 C23 120.4(4) . . ?
C26 C25 H25 119.8 . . ?
C23 C25 H25 119.8 . . ?
C25 C26 C27 118.7(5) . . ?
C25 C26 H26 120.6 . . ?
C27 C26 H26 120.6 . . ?
N3 C27 C26 123.5(5) . . ?
N3 C27 H27 118.3 . . ?
C26 C27 H27 118.3 . . ?
N4 C28 C29 123.0(4) . . ?
N4 C28 H28 118.5 . . ?
C29 C28 H28 118.5 . . ?
C30 C29 C28 119.5(5) . . ?
C30 C29 H29 120.3 . . ?
C28 C29 H29 120.3 . . ?
C29 C30 C31 119.0(5) . . ?
C29 C30 H30 120.5 . . ?
C31 C30 H30 120.5 . . ?
C30 C31 C32 118.1(4) . . ?
C30 C31 C33 122.7(5) . . ?
C32 C31 C33 119.2(4) . . ?
N4 C32 C31 121.5(4) . . ?
N4 C32 C36 119.0(4) . . ?
C31 C32 C36 119.5(4) . . ?
C34 C33 C31 121.4(5) . . ?
C34 C33 H33 119.3 . . ?
C31 C33 H33 119.3 . . ?
C33 C34 C35 120.4(4) . . ?
C33 C34 H34 119.8 . . ?
C35 C34 H34 119.8 . . ?
C36 C35 C37 118.2(5) . . ?
C36 C35 C34 119.8(4) . . ?
C37 C35 C34 122.0(4) . . ?
N5 C36 C35 122.5(4) . . ?
N5 C36 C32 117.8(4) . . ?
C35 C36 C32 119.7(4) . . ?
C38 C37 C35 120.0(5) . . ?
C38 C37 H37 120.0 . . ?
C35 C37 H37 120.0 . . ?
C37 C38 C39 118.2(5) . . ?
C37 C38 H38 120.9 . . ?
C39 C38 H38 120.9 . . ?
N5 C39 C38 123.5(5) . . ?
N5 C39 H39 118.3 . . ?
C38 C39 H39 118.3 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cd1 O1 C1 O2 16.5(9) . . . . ?
Cd1 O1 C1 C2 -163.8(4) . . . . ?
Cd2 O2 C1 O1 8.3(6) . . . . ?
Cd2 O2 C1 C2 -171.4(3) . . . . ?
O1 C1 C2 C3 98.4(5) . . . . ?
O2 C1 C2 C3 -81.8(5) . . . . ?
O1 C1 C2 C8 -78.3(5) . . . . ?
O2 C1 C2 C8 101.4(5) . . . . ?
C8 C2 C3 C4 -1.1(6) . . . . ?
C1 C2 C3 C4 -177.9(4) . . . . ?
C2 C3 C4 C6 1.6(6) . . . . ?
C2 C3 C4 C5 -177.3(4) . . . . ?
Cd1 O4 C5 O3 7.6(7) 2 . . . ?
Cd1 O4 C5 C4 -170.8(2) 2 . . . ?
C6 C4 C5 O3 -8.9(7) . . . . ?
C3 C4 C5 O3 170.0(4) . . . . ?
C6 C4 C5 O4 169.7(4) . . . . ?
C3 C4 C5 O4 -11.5(6) . . . . ?
C3 C4 C6 C7 -0.1(6) . . . . ?
C5 C4 C6 C7 178.8(4) . . . . ?
C4 C6 C7 C8 -2.0(7) . . . . ?
C6 C7 C8 C2 2.5(6) . . . . ?
C6 C7 C8 C9 -176.8(4) . . . . ?
C3 C2 C8 C7 -0.9(6) . . . . ?
C1 C2 C8 C7 175.7(4) . . . . ?
C3 C2 C8 C9 178.3(3) . . . . ?
C1 C2 C8 C9 -5.0(6) . . . . ?
C7 C8 C9 C10 -41.7(6) . . . . ?
C2 C8 C9 C10 139.1(4) . . . . ?
C7 C8 C9 C15 136.6(4) . . . . ?
C2 C8 C9 C15 -42.6(6) . . . . ?
C15 C9 C10 C11 -1.1(6) . . . . ?
C8 C9 C10 C11 177.3(4) . . . . ?
C9 C10 C11 C12 -1.0(7) . . . . ?
C9 C10 C11 N1 173.7(4) . . . . ?
O7 N1 C11 C10 45.2(6) . . . . ?
O8 N1 C11 C10 -132.7(5) . . . . ?
O7 N1 C11 C12 -139.8(5) . . . . ?
O8 N1 C11 C12 42.3(6) . . . . ?
C10 C11 C12 C14 1.9(6) . . . . ?
N1 C11 C12 C14 -172.6(4) . . . . ?
C10 C11 C12 C13 -173.3(4) . . . . ?
N1 C11 C12 C13 12.1(6) . . . . ?
Cd2 O5 C13 O6 -5.0(4) 2_666 . . . ?
Cd2 O5 C13 C12 172.0(3) 2_666 . . . ?
Cd2 O6 C13 O5 5.5(4) 2_666 . . . ?
Cd2 O6 C13 C12 -171.5(3) 2_666 . . . ?
C14 C12 C13 O5 -129.9(4) . . . . ?
C11 C12 C13 O5 45.1(6) . . . . ?
C14 C12 C13 O6 47.3(6) . . . . ?
C11 C12 C13 O6 -137.7(4) . . . . ?
C11 C12 C14 C15 -0.8(6) . . . . ?
C13 C12 C14 C15 174.6(4) . . . . ?
C12 C14 C15 C9 -1.1(6) . . . . ?
C10 C9 C15 C14 2.1(6) . . . . ?
C8 C9 C15 C14 -176.2(4) . . . . ?
C20 N2 C16 C17 -1.6(7) . . . . ?
Cd1 N2 C16 C17 176.7(3) . . . . ?
N2 C16 C17 C18 0.8(8) . . . . ?
C16 C17 C18 C19 -0.5(8) . . . . ?
C17 C18 C19 C20 1.0(7) . . . . ?
C17 C18 C19 C21 178.0(5) . . . . ?
C16 N2 C20 C19 2.1(6) . . . . ?
Cd1 N2 C20 C19 -176.4(3) . . . . ?
C16 N2 C20 C24 -177.5(4) . . . . ?
Cd1 N2 C20 C24 4.0(5) . . . . ?
C18 C19 C20 N2 -1.8(7) . . . . ?
C21 C19 C20 N2 -179.0(4) . . . . ?
C18 C19 C20 C24 177.8(4) . . . . ?
C21 C19 C20 C24 0.6(7) . . . . ?
C18 C19 C21 C22 -177.6(5) . . . . ?
C20 C19 C21 C22 -0.6(8) . . . . ?
C19 C21 C22 C23 1.2(9) . . . . ?
C21 C22 C23 C25 177.8(5) . . . . ?
C21 C22 C23 C24 -1.8(8) . . . . ?
C27 N3 C24 C23 -1.2(7) . . . . ?
Cd1 N3 C24 C23 178.3(3) . . . . ?
C27 N3 C24 C20 178.5(4) . . . . ?
Cd1 N3 C24 C20 -2.1(5) . . . . ?
C25 C23 C24 N3 1.8(7) . . . . ?
C22 C23 C24 N3 -178.5(4) . . . . ?
C25 C23 C24 C20 -177.9(4) . . . . ?
C22 C23 C24 C20 1.8(7) . . . . ?
N2 C20 C24 N3 -1.3(6) . . . . ?
C19 C20 C24 N3 179.1(4) . . . . ?
N2 C20 C24 C23 178.3(4) . . . . ?
C19 C20 C24 C23 -1.3(6) . . . . ?
C24 C23 C25 C26 -1.0(7) . . . . ?
C22 C23 C25 C26 179.4(5) . . . . ?
C23 C25 C26 C27 -0.3(8) . . . . ?
C24 N3 C27 C26 -0.3(7) . . . . ?
Cd1 N3 C27 C26 -179.6(3) . . . . ?
C25 C26 C27 N3 1.0(8) . . . . ?
C32 N4 C28 C29 -0.4(7) . . . . ?
Cd2 N4 C28 C29 -178.2(4) . . . . ?
N4 C28 C29 C30 -0.6(8) . . . . ?
C28 C29 C30 C31 0.7(7) . . . . ?
C29 C30 C31 C32 0.2(7) . . . . ?
C29 C30 C31 C33 -179.3(4) . . . . ?
C28 N4 C32 C31 1.4(6) . . . . ?
Cd2 N4 C32 C31 179.4(3) . . . . ?
C28 N4 C32 C36 -179.3(4) . . . . ?
Cd2 N4 C32 C36 -1.3(5) . . . . ?
C30 C31 C32 N4 -1.3(6) . . . . ?
C33 C31 C32 N4 178.2(4) . . . . ?
C30 C31 C32 C36 179.3(4) . . . . ?
C33 C31 C32 C36 -1.1(6) . . . . ?
C30 C31 C33 C34 178.1(5) . . . . ?
C32 C31 C33 C34 -1.5(7) . . . . ?
C31 C33 C34 C35 2.2(7) . . . . ?
C33 C34 C35 C36 -0.3(7) . . . . ?
C33 C34 C35 C37 179.6(5) . . . . ?
C39 N5 C36 C35 0.4(7) . . . . ?
Cd2 N5 C36 C35 175.8(3) . . . . ?
C39 N5 C36 C32 -180.0(4) . . . . ?
Cd2 N5 C36 C32 -4.6(5) . . . . ?
C37 C35 C36 N5 -2.5(7) . . . . ?
C34 C35 C36 N5 177.3(4) . . . . ?
C37 C35 C36 C32 177.9(4) . . . . ?
C34 C35 C36 C32 -2.2(7) . . . . ?
N4 C32 C36 N5 4.0(6) . . . . ?
C31 C32 C36 N5 -176.7(4) . . . . ?
N4 C32 C36 C35 -176.4(4) . . . . ?
C31 C32 C36 C35 2.9(6) . . . . ?
C36 C35 C37 C38 3.1(8) . . . . ?
C34 C35 C37 C38 -176.7(5) . . . . ?
C35 C37 C38 C39 -1.7(9) . . . . ?
C36 N5 C39 C38 1.1(8) . . . . ?
Cd2 N5 C39 C38 -173.8(4) . . . . ?
C37 C38 C39 N5 -0.5(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
C17 H17 O6 0.93 2.57 3.475(6) 165.0 .
C10 H10 O7 0.93 2.60 3.490(5) 160.7 2_665
O9 H1W O3 0.85 1.83 2.682(4) 179.8 2
O9 H2W O5 0.85 2.03 2.875(4) 179.1 1_545
C17 H17 O6 0.93 2.57 3.475(6) 165.0 .
C10 H10 O7 0.93 2.60 3.490(5) 160.7 2_665
O9 H2W O5 0.85 2.03 2.875(4) 179.1 1_545
C10 H10 O7 0.93 2.60 3.490(5) 160.7 2_665
O9 H2W O5 0.85 2.03 2.875(4) 179.1 1_545
C17 H17 O6 0.93 2.57 3.475(6) 165.0 .
C17 H17 O6 0.93 2.57 3.475(6) 165.0 .
O9 H2W O5 0.85 2.03 2.875(4) 179.1 1_545
C10 H10 O7 0.93 2.60 3.490(5) 160.7 2_665
C17 H17 O6 0.93 2.57 3.475(6) 165.0 .
O9 H2W O5 0.85 2.03 2.875(4) 179.1 1_545
C10 H10 O7 0.93 2.60 3.490(5) 160.7 2_665
C17 H17 O6 0.93 2.57 3.475(6) 165.0 .
O9 H2W O5 0.85 2.03 2.875(4) 179.1 1_545
C10 H10 O7 0.93 2.60 3.490(5) 160.7 2_665

_refine_diff_density_max         0.750
_refine_diff_density_min         -0.661
_refine_diff_density_rms         0.093

####################################################################### 
# 
# 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_310-9Zn2
_database_code_depnum_ccdc_archive 'CCDC 1589515'
_audit_update_record             
;
2017-12-06 deposited with the CCDC.
2018-04-30 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            'C54 H34 N6 O18 Zn2'
_chemical_formula_weight         1185.61

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

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

_cell_length_a                   9.0806(10)
_cell_length_b                   10.0170(9)
_cell_length_c                   14.9919(13)
_cell_angle_alpha                98.323(8)
_cell_angle_beta                 93.031(8)
_cell_angle_gamma                115.650(10)
_cell_volume                     1206.1(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7484
_cell_measurement_theta_min      3.680
_cell_measurement_theta_max      25.046

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_F_000             604
_exptl_transmission_factor_min   0.780
_exptl_transmission_factor_max   0.805
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    1.083
_shelx_estimated_absorpt_T_min   0.789
_shelx_estimated_absorpt_T_max   0.812
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_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            7484
_diffrn_reflns_av_unetI/netI     0.0942
_diffrn_reflns_av_R_equivalents  0.0463
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.680
_diffrn_reflns_theta_max         25.046
_diffrn_reflns_theta_full        25.046
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             4258
_reflns_number_gt                2967
_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)+(0.0179P)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         4258
_refine_ls_number_parameters     365
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0882
_refine_ls_R_factor_gt           0.0555
_refine_ls_wR_factor_ref         0.0976
_refine_ls_wR_factor_gt          0.0824
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.054
_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 0.76082(6) 0.50645(5) 0.26471(3) 0.03708(17) Uani 1 1 d . . . . .
N1 N 0.6224(5) 0.0286(4) -0.2568(3) 0.0470(11) Uani 1 1 d . . . . .
N2 N 0.7209(4) 0.6376(4) 0.3721(2) 0.0377(9) Uani 1 1 d . . . . .
N3 N 0.7892(4) 0.4017(3) 0.3666(2) 0.0339(9) Uani 1 1 d . . . . .
O1 O 0.6088(4) 0.2470(3) 0.12813(19) 0.0450(8) Uani 1 1 d . . . . .
O2 O 0.5520(4) 0.4303(3) 0.18950(19) 0.0458(8) Uani 1 1 d . . . . .
O3 O -0.0746(4) 0.1825(3) 0.1704(2) 0.0457(8) Uani 1 1 d . . . . .
O4 O -0.1889(4) 0.1781(4) 0.0342(2) 0.0493(8) Uani 1 1 d . . . . .
H4 H -0.2545 0.1955 0.0634 0.074 Uiso 1 1 calc R U . . .
O5 O 1.0597(4) 0.4407(3) -0.1933(2) 0.0564(9) Uani 1 1 d . . . . .
O6 O 0.9267(4) 0.2192(3) -0.2822(2) 0.0583(10) Uani 1 1 d . . . . .
O7 O 0.6807(5) -0.0527(4) -0.2368(2) 0.0793(13) Uani 1 1 d . . . . .
O8 O 0.5460(5) 0.0107(5) -0.3289(3) 0.1109(17) Uani 1 1 d . . . . .
O9 O 0.9728(6) 0.0226(4) 0.3087(3) 0.0787(12) Uani 1 1 d G . . . .
H2W H 1.0098 0.0800 0.2704 0.118 Uiso 1 1 d G U . . .
H1W H 1.0092 -0.0430 0.3031 0.118 Uiso 1 1 d G U . . .
C1 C 0.5223(5) 0.3138(5) 0.1306(3) 0.0328(10) Uani 1 1 d . . . . .
C2 C 0.3707(5) 0.2632(4) 0.0642(3) 0.0255(9) Uani 1 1 d . . . . .
C3 C 0.2250(5) 0.2453(4) 0.1002(3) 0.0285(9) Uani 1 1 d . . . . .
H3 H 0.2274 0.2651 0.1630 0.034 Uiso 1 1 calc R U . . .
C4 C 0.0798(5) 0.1995(4) 0.0458(3) 0.0258(9) Uani 1 1 d . . . . .
C5 C -0.0686(5) 0.1854(4) 0.0902(3) 0.0313(10) Uani 1 1 d . . . . .
C6 C 0.0773(5) 0.1734(4) -0.0476(3) 0.0297(10) Uani 1 1 d . . . . .
H6 H -0.0202 0.1447 -0.0854 0.036 Uiso 1 1 calc R U . . .
C7 C 0.2179(5) 0.1898(4) -0.0850(3) 0.0295(10) Uani 1 1 d . . . . .
H7 H 0.2140 0.1712 -0.1479 0.035 Uiso 1 1 calc R U . . .
C8 C 0.3660(5) 0.2337(4) -0.0305(3) 0.0265(9) Uani 1 1 d . . . . .
C9 C 0.5151(5) 0.2524(4) -0.0752(3) 0.0257(9) Uani 1 1 d . . . . .
C10 C 0.5073(5) 0.1389(4) -0.1431(3) 0.0311(10) Uani 1 1 d . . . . .
H10 H 0.4107 0.0494 -0.1590 0.037 Uiso 1 1 calc R U . . .
C11 C 0.6425(5) 0.1585(4) -0.1871(3) 0.0269(9) Uani 1 1 d . . . . .
C12 C 0.7902(5) 0.2891(4) -0.1678(3) 0.0273(9) Uani 1 1 d . . . . .
C13 C 0.9364(5) 0.3157(5) -0.2188(3) 0.0327(10) Uani 1 1 d . . . . .
C14 C 0.7955(5) 0.4015(4) -0.0988(3) 0.0328(10) Uani 1 1 d . . . . .
H14 H 0.8921 0.4910 -0.0831 0.039 Uiso 1 1 calc R U . . .
C15 C 0.6632(5) 0.3845(4) -0.0536(3) 0.0305(10) Uani 1 1 d . . . . .
H15 H 0.6720 0.4620 -0.0078 0.037 Uiso 1 1 calc R U . . .
C16 C 0.6816(6) 0.7502(5) 0.3728(3) 0.0533(14) Uani 1 1 d . . . . .
H16 H 0.6754 0.7839 0.3187 0.064 Uiso 1 1 calc R U . . .
C17 C 0.6489(6) 0.8205(5) 0.4512(4) 0.0627(16) Uani 1 1 d . . . . .
H17 H 0.6211 0.8992 0.4491 0.075 Uiso 1 1 calc R U . . .
C18 C 0.6582(6) 0.7728(5) 0.5305(4) 0.0587(15) Uani 1 1 d . . . . .
H18 H 0.6375 0.8193 0.5833 0.070 Uiso 1 1 calc R U . . .
C19 C 0.6990(5) 0.6531(5) 0.5328(3) 0.0442(12) Uani 1 1 d . . . . .
C20 C 0.7279(5) 0.5882(4) 0.4512(3) 0.0324(10) Uani 1 1 d . . . . .
C21 C 0.7097(6) 0.5938(6) 0.6135(3) 0.0586(15) Uani 1 1 d . . . . .
H21 H 0.6895 0.6358 0.6681 0.070 Uiso 1 1 calc R U . . .
C22 C 0.7484(6) 0.4786(6) 0.6105(3) 0.0566(14) Uani 1 1 d . . . . .
H22 H 0.7560 0.4432 0.6638 0.068 Uiso 1 1 calc R U . . .
C23 C 0.7784(5) 0.4080(5) 0.5281(3) 0.0407(11) Uani 1 1 d . . . . .
C24 C 0.7663(5) 0.4631(4) 0.4484(3) 0.0329(10) Uani 1 1 d . . . . .
C25 C 0.8187(6) 0.2882(5) 0.5208(3) 0.0518(13) Uani 1 1 d . . . . .
H25 H 0.8278 0.2487 0.5721 0.062 Uiso 1 1 calc R U . . .
C26 C 0.8449(6) 0.2282(5) 0.4393(3) 0.0505(13) Uani 1 1 d . . . . .
H26 H 0.8739 0.1493 0.4347 0.061 Uiso 1 1 calc R U . . .
C27 C 0.8274(5) 0.2872(5) 0.3628(3) 0.0435(12) Uani 1 1 d . . . . .
H27 H 0.8432 0.2448 0.3070 0.052 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 1.919(3) 2_765 ?
Zn1 O2 1.929(3) . ?
Zn1 N3 2.039(3) . ?
Zn1 N2 2.076(3) . ?
N1 O8 1.199(5) . ?
N1 O7 1.208(5) . ?
N1 C11 1.483(5) . ?
N2 C16 1.321(5) . ?
N2 C20 1.358(5) . ?
N3 C27 1.328(5) . ?
N3 C24 1.359(4) . ?
O1 C1 1.232(4) . ?
O2 C1 1.272(4) . ?
O3 C5 1.210(4) . ?
O4 C5 1.311(5) . ?
O4 H4 0.8200 . ?
O5 C13 1.253(5) . ?
O5 Zn1 1.919(3) 2_765 ?
O6 C13 1.223(4) . ?
O9 H2W 0.8501 . ?
O9 H1W 0.8500 . ?
C1 C2 1.499(5) . ?
C2 C8 1.402(5) . ?
C2 C3 1.404(5) . ?
C3 C4 1.367(5) . ?
C3 H3 0.9300 . ?
C4 C6 1.385(5) . ?
C4 C5 1.495(5) . ?
C6 C7 1.376(5) . ?
C6 H6 0.9300 . ?
C7 C8 1.392(5) . ?
C7 H7 0.9300 . ?
C8 C9 1.493(5) . ?
C9 C10 1.387(5) . ?
C9 C15 1.398(5) . ?
C10 C11 1.377(5) . ?
C10 H10 0.9300 . ?
C11 C12 1.387(5) . ?
C12 C14 1.397(5) . ?
C12 C13 1.510(5) . ?
C14 C15 1.369(5) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C17 1.394(6) . ?
C16 H16 0.9300 . ?
C17 C18 1.356(7) . ?
C17 H17 0.9300 . ?
C18 C19 1.404(6) . ?
C18 H18 0.9300 . ?
C19 C20 1.393(5) . ?
C19 C21 1.439(6) . ?
C20 C24 1.435(5) . ?
C21 C22 1.340(6) . ?
C21 H21 0.9300 . ?
C22 C23 1.432(6) . ?
C22 H22 0.9300 . ?
C23 C25 1.390(6) . ?
C23 C24 1.404(5) . ?
C25 C26 1.361(6) . ?
C25 H25 0.9300 . ?
C26 C27 1.396(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
O5 Zn1 O2 111.51(14) 2_765 . ?
O5 Zn1 N3 112.30(14) 2_765 . ?
O2 Zn1 N3 120.90(13) . . ?
O5 Zn1 N2 129.61(13) 2_765 . ?
O2 Zn1 N2 99.19(13) . . ?
N3 Zn1 N2 81.36(14) . . ?
O8 N1 O7 124.8(4) . . ?
O8 N1 C11 116.9(4) . . ?
O7 N1 C11 118.3(4) . . ?
C16 N2 C20 118.1(4) . . ?
C16 N2 Zn1 130.3(3) . . ?
C20 N2 Zn1 111.4(3) . . ?
C27 N3 C24 118.3(4) . . ?
C27 N3 Zn1 129.2(3) . . ?
C24 N3 Zn1 112.5(3) . . ?
C1 O2 Zn1 113.0(3) . . ?
C5 O4 H4 109.5 . . ?
C13 O5 Zn1 118.1(3) . 2_765 ?
H2W O9 H1W 109.5 . . ?
O1 C1 O2 123.5(4) . . ?
O1 C1 C2 122.5(4) . . ?
O2 C1 C2 114.0(4) . . ?
C8 C2 C3 118.6(4) . . ?
C8 C2 C1 124.2(4) . . ?
C3 C2 C1 117.1(3) . . ?
C4 C3 C2 121.9(4) . . ?
C4 C3 H3 119.0 . . ?
C2 C3 H3 119.0 . . ?
C3 C4 C6 119.0(4) . . ?
C3 C4 C5 118.2(4) . . ?
C6 C4 C5 122.8(4) . . ?
O3 C5 O4 124.0(4) . . ?
O3 C5 C4 122.5(4) . . ?
O4 C5 C4 113.5(4) . . ?
C7 C6 C4 120.4(4) . . ?
C7 C6 H6 119.8 . . ?
C4 C6 H6 119.8 . . ?
C6 C7 C8 121.2(4) . . ?
C6 C7 H7 119.4 . . ?
C8 C7 H7 119.4 . . ?
C7 C8 C2 118.8(4) . . ?
C7 C8 C9 118.7(4) . . ?
C2 C8 C9 122.5(4) . . ?
C10 C9 C15 117.9(3) . . ?
C10 C9 C8 119.9(3) . . ?
C15 C9 C8 122.1(3) . . ?
C11 C10 C9 120.0(4) . . ?
C11 C10 H10 120.0 . . ?
C9 C10 H10 120.0 . . ?
C10 C11 C12 123.3(3) . . ?
C10 C11 N1 115.6(3) . . ?
C12 C11 N1 121.1(3) . . ?
C11 C12 C14 115.7(3) . . ?
C11 C12 C13 123.9(3) . . ?
C14 C12 C13 120.4(4) . . ?
O6 C13 O5 124.7(4) . . ?
O6 C13 C12 119.6(4) . . ?
O5 C13 C12 115.7(4) . . ?
C15 C14 C12 122.2(4) . . ?
C15 C14 H14 118.9 . . ?
C12 C14 H14 118.9 . . ?
C14 C15 C9 120.9(4) . . ?
C14 C15 H15 119.5 . . ?
C9 C15 H15 119.5 . . ?
N2 C16 C17 122.7(5) . . ?
N2 C16 H16 118.6 . . ?
C17 C16 H16 118.6 . . ?
C18 C17 C16 119.2(5) . . ?
C18 C17 H17 120.4 . . ?
C16 C17 H17 120.4 . . ?
C17 C18 C19 120.0(4) . . ?
C17 C18 H18 120.0 . . ?
C19 C18 H18 120.0 . . ?
C20 C19 C18 117.1(4) . . ?
C20 C19 C21 119.1(4) . . ?
C18 C19 C21 123.8(4) . . ?
N2 C20 C19 122.9(4) . . ?
N2 C20 C24 117.3(3) . . ?
C19 C20 C24 119.8(4) . . ?
C22 C21 C19 120.6(4) . . ?
C22 C21 H21 119.7 . . ?
C19 C21 H21 119.7 . . ?
C21 C22 C23 122.2(4) . . ?
C21 C22 H22 118.9 . . ?
C23 C22 H22 118.9 . . ?
C25 C23 C24 117.2(4) . . ?
C25 C23 C22 124.8(4) . . ?
C24 C23 C22 118.0(4) . . ?
N3 C24 C23 122.4(4) . . ?
N3 C24 C20 117.4(4) . . ?
C23 C24 C20 120.3(4) . . ?
C26 C25 C23 120.7(4) . . ?
C26 C25 H25 119.7 . . ?
C23 C25 H25 119.7 . . ?
C25 C26 C27 118.7(4) . . ?
C25 C26 H26 120.6 . . ?
C27 C26 H26 120.6 . . ?
N3 C27 C26 122.7(4) . . ?
N3 C27 H27 118.7 . . ?
C26 C27 H27 118.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Zn1 O2 C1 O1 7.5(5) . . . . ?
Zn1 O2 C1 C2 -173.1(2) . . . . ?
O1 C1 C2 C8 -51.6(6) . . . . ?
O2 C1 C2 C8 129.0(4) . . . . ?
O1 C1 C2 C3 128.6(4) . . . . ?
O2 C1 C2 C3 -50.8(5) . . . . ?
C8 C2 C3 C4 0.3(5) . . . . ?
C1 C2 C3 C4 -179.9(3) . . . . ?
C2 C3 C4 C6 -1.5(6) . . . . ?
C2 C3 C4 C5 -179.2(3) . . . . ?
C3 C4 C5 O3 -15.5(6) . . . . ?
C6 C4 C5 O3 167.0(3) . . . . ?
C3 C4 C5 O4 163.9(3) . . . . ?
C6 C4 C5 O4 -13.6(5) . . . . ?
C3 C4 C6 C7 1.6(5) . . . . ?
C5 C4 C6 C7 179.2(3) . . . . ?
C4 C6 C7 C8 -0.5(6) . . . . ?
C6 C7 C8 C2 -0.8(6) . . . . ?
C6 C7 C8 C9 -178.8(3) . . . . ?
C3 C2 C8 C7 0.9(5) . . . . ?
C1 C2 C8 C7 -178.9(3) . . . . ?
C3 C2 C8 C9 178.8(3) . . . . ?
C1 C2 C8 C9 -1.0(6) . . . . ?
C7 C8 C9 C10 -50.2(5) . . . . ?
C2 C8 C9 C10 131.9(4) . . . . ?
C7 C8 C9 C15 127.2(4) . . . . ?
C2 C8 C9 C15 -50.8(5) . . . . ?
C15 C9 C10 C11 -0.2(6) . . . . ?
C8 C9 C10 C11 177.2(4) . . . . ?
C9 C10 C11 C12 -0.6(6) . . . . ?
C9 C10 C11 N1 178.4(4) . . . . ?
O8 N1 C11 C10 77.6(5) . . . . ?
O7 N1 C11 C10 -101.0(5) . . . . ?
O8 N1 C11 C12 -103.3(5) . . . . ?
O7 N1 C11 C12 78.1(5) . . . . ?
C10 C11 C12 C14 0.9(6) . . . . ?
N1 C11 C12 C14 -178.1(4) . . . . ?
C10 C11 C12 C13 -176.5(4) . . . . ?
N1 C11 C12 C13 4.5(6) . . . . ?
Zn1 O5 C13 O6 5.8(6) 2_765 . . . ?
Zn1 O5 C13 C12 -172.0(3) 2_765 . . . ?
C11 C12 C13 O6 1.2(6) . . . . ?
C14 C12 C13 O6 -176.1(4) . . . . ?
C11 C12 C13 O5 179.1(4) . . . . ?
C14 C12 C13 O5 1.8(6) . . . . ?
C11 C12 C14 C15 -0.4(6) . . . . ?
C13 C12 C14 C15 177.1(4) . . . . ?
C12 C14 C15 C9 -0.3(6) . . . . ?
C10 C9 C15 C14 0.7(6) . . . . ?
C8 C9 C15 C14 -176.7(4) . . . . ?
C20 N2 C16 C17 0.7(6) . . . . ?
Zn1 N2 C16 C17 175.8(3) . . . . ?
N2 C16 C17 C18 0.3(8) . . . . ?
C16 C17 C18 C19 -0.5(8) . . . . ?
C17 C18 C19 C20 -0.2(7) . . . . ?
C17 C18 C19 C21 -179.2(5) . . . . ?
C16 N2 C20 C19 -1.5(6) . . . . ?
Zn1 N2 C20 C19 -177.5(3) . . . . ?
C16 N2 C20 C24 178.3(4) . . . . ?
Zn1 N2 C20 C24 2.3(4) . . . . ?
C18 C19 C20 N2 1.3(6) . . . . ?
C21 C19 C20 N2 -179.7(4) . . . . ?
C18 C19 C20 C24 -178.5(4) . . . . ?
C21 C19 C20 C24 0.5(6) . . . . ?
C20 C19 C21 C22 0.6(7) . . . . ?
C18 C19 C21 C22 179.6(5) . . . . ?
C19 C21 C22 C23 -0.9(8) . . . . ?
C21 C22 C23 C25 -179.9(5) . . . . ?
C21 C22 C23 C24 0.0(7) . . . . ?
C27 N3 C24 C23 -1.3(6) . . . . ?
Zn1 N3 C24 C23 179.5(3) . . . . ?
C27 N3 C24 C20 178.9(4) . . . . ?
Zn1 N3 C24 C20 -0.3(4) . . . . ?
C25 C23 C24 N3 1.3(6) . . . . ?
C22 C23 C24 N3 -178.6(4) . . . . ?
C25 C23 C24 C20 -178.9(4) . . . . ?
C22 C23 C24 C20 1.2(6) . . . . ?
N2 C20 C24 N3 -1.4(5) . . . . ?
C19 C20 C24 N3 178.4(4) . . . . ?
N2 C20 C24 C23 178.8(4) . . . . ?
C19 C20 C24 C23 -1.4(6) . . . . ?
C24 C23 C25 C26 0.0(6) . . . . ?
C22 C23 C25 C26 179.9(5) . . . . ?
C23 C25 C26 C27 -1.2(7) . . . . ?
C24 N3 C27 C26 0.0(6) . . . . ?
Zn1 N3 C27 C26 179.1(3) . . . . ?
C25 C26 C27 N3 1.3(7) . . . . ?

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
C27 H27 O3 0.93 2.31 3.228(5) 169.2 1_655
C26 H26 O9 0.93 2.54 3.251(6) 133.4 .
O9 H1W O6 0.85 2.07 2.921(5) 173.9 2_755
O9 H2W O3 0.85 2.21 2.919(5) 140.4 1_655
O4 H4 O1 0.82 1.81 2.632(4) 176.3 1_455

_refine_diff_density_max         0.399
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.075

####################################################################### 
# 
# 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_334-9Ni
_database_code_depnum_ccdc_archive 'CCDC 1589517'
_audit_update_record             
;
2017-12-06 deposited with the CCDC.
2018-04-30 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 H37 N5 Ni O15'
_chemical_formula_weight         874.44

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           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                   13.4082(8)
_cell_length_b                   14.3932(7)
_cell_length_c                   20.3585(12)
_cell_angle_alpha                90
_cell_angle_beta                 103.230(6)
_cell_angle_gamma                90
_cell_volume                     3824.7(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    14678
_cell_measurement_theta_min      3.229
_cell_measurement_theta_max      25.049

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_F_000             1816
_exptl_transmission_factor_min   0.863
_exptl_transmission_factor_max   0.878
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.220
_exptl_absorpt_coefficient_mu    0.589
_shelx_estimated_absorpt_T_min   0.867
_shelx_estimated_absorpt_T_max   0.881
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.867
_exptl_absorpt_correction_T_max  0.881
_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            14678
_diffrn_reflns_av_unetI/netI     0.1298
_diffrn_reflns_av_R_equivalents  0.0806
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.229
_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             6767
_reflns_number_gt                3373
_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)+(0.0298P)²+1.8194P] 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         6767
_refine_ls_number_parameters     545
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1497
_refine_ls_R_factor_gt           0.0700
_refine_ls_wR_factor_ref         0.1601
_refine_ls_wR_factor_gt          0.1187
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_restrained_S_all      1.016
_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 0.47307(5) 0.78434(5) 0.66989(4) 0.0422(2) Uani 1 1 d . . . . .
N1 N 0.5959(5) 0.9380(5) 0.9766(3) 0.0728(17) Uani 1 1 d . . . . .
N2 N 0.3291(4) 0.8011(3) 0.6064(2) 0.0485(12) Uani 1 1 d . . . . .
N3 N 0.3815(4) 0.7848(3) 0.7407(2) 0.0418(11) Uani 1 1 d . . . . .
N4 N 0.6042(3) 0.7527(3) 0.7417(2) 0.0449(12) Uani 1 1 d . . . . .
N5 N 0.4701(3) 0.6402(3) 0.6626(2) 0.0401(11) Uani 1 1 d . . . . .
O1 O 0.5138(3) 0.9232(2) 0.67794(18) 0.0448(10) Uani 1 1 d . . . . .
O2 O 0.4804(3) 1.0426(3) 0.6076(2) 0.0628(12) Uani 1 1 d . . . . .
O3 O 0.0796(3) 1.0452(4) 0.5568(2) 0.0841(16) Uani 1 1 d . . . . .
O4 O 0.0110(3) 1.0365(4) 0.6457(2) 0.0802(14) Uani 1 1 d . . . . .
H1 H -0.0405 1.0214 0.6175 0.120 Uiso 1 1 calc R U . . .
O5 O 0.8205(4) 0.9414(5) 0.9492(3) 0.114(2) Uani 1 1 d . . . . .
O6 O 0.8213(4) 1.0927(5) 0.9658(3) 0.130(3) Uani 1 1 d . . . . .
O7 O 0.6601(4) 0.9629(4) 1.0250(2) 0.108(2) Uani 1 1 d . . . . .
O8 O 0.5323(5) 0.8793(4) 0.9793(3) 0.111(2) Uani 1 1 d . . . . .
O9 O 0.5504(3) 0.7835(2) 0.59241(19) 0.0650(12) Uani 1 1 d . . . . .
H2W H 0.5414 0.8354 0.5714 0.078 Uiso 1 1 d R U . . .
H1W H 0.5267 0.7397 0.5649 0.078 Uiso 1 1 d R U . . .
O10 O 0.4519(4) 0.2332(3) 0.6084(3) 0.134(2) Uani 1 1 d . . . . .
H3W H 0.4665 0.2548 0.5754 0.161 Uiso 1 1 d R U . . .
H4W H 0.4600 0.1747 0.6078 0.161 Uiso 1 1 d R U . . .
O11 O 0.1504(4) 0.0257(4) 0.4397(2) 0.1069(18) Uani 1 1 d . . . . .
H6W H 0.1373 0.0586 0.4590 0.128 Uiso 1 1 d R U . . .
H5W H 0.2094 0.0638 0.4372 0.128 Uiso 1 1 d R U . . .
O12 O 0.6184(4) 0.9622(5) 0.5390(3) 0.152(3) Uani 1 1 d . . . . .
H7W H 0.5764 0.9854 0.5600 0.182 Uiso 1 1 d R U . . .
H8W H 0.6341 1.0218 0.5315 0.182 Uiso 1 1 d R U . . .
O14 O 0.9922(3) 0.8427(2) 0.98999(19) 0.0596(11) Uani 1 1 d . . . . .
H11W H 0.9365 0.8728 0.9750 0.072 Uiso 1 1 d R U . . .
H12W H 1.0493 0.8712 0.9962 0.072 Uiso 1 1 d R U . . .
C1 C 0.4637(4) 0.9945(4) 0.6548(3) 0.0407(14) Uani 1 1 d . . . . .
C2 C 0.3740(4) 1.0209(3) 0.6849(3) 0.0356(13) Uani 1 1 d . . . . .
C3 C 0.2786(4) 1.0283(3) 0.6417(3) 0.0417(14) Uani 1 1 d . . . . .
H3 H 0.2733 1.0263 0.5953 0.050 Uiso 1 1 calc R U . . .
C4 C 0.1903(4) 1.0385(3) 0.6658(3) 0.0412(14) Uani 1 1 d . . . . .
C5 C 0.0893(5) 1.0409(4) 0.6172(3) 0.0539(16) Uani 1 1 d . . . . .
C6 C 0.1999(4) 1.0450(4) 0.7351(3) 0.0458(15) Uani 1 1 d . . . . .
H6 H 0.1416 1.0507 0.7522 0.055 Uiso 1 1 calc R U . . .
C7 C 0.2942(4) 1.0430(3) 0.7783(3) 0.0452(15) Uani 1 1 d . . . . .
H7 H 0.2993 1.0502 0.8243 0.054 Uiso 1 1 calc R U . . .
C8 C 0.3828(4) 1.0305(3) 0.7546(3) 0.0357(13) Uani 1 1 d . . . . .
C9 C 0.4839(4) 1.0302(4) 0.8040(3) 0.0435(14) Uani 1 1 d . . . . .
C10 C 0.5699(4) 1.0755(4) 0.7914(3) 0.0492(15) Uani 1 1 d . . . . .
H10 H 0.5641 1.1074 0.7510 0.059 Uiso 1 1 calc R U . . .
C11 C 0.6629(5) 1.0741(4) 0.8373(3) 0.0586(17) Uani 1 1 d . . . . .
H11 H 0.7185 1.1053 0.8275 0.070 Uiso 1 1 calc R U . . .
C12 C 0.6748(5) 1.0269(4) 0.8977(3) 0.0560(17) Uani 1 1 d . . . . .
C13 C 0.7834(6) 1.0208(7) 0.9429(4) 0.080(2) Uani 1 1 d . . . . .
C14 C 0.5893(5) 0.9848(4) 0.9108(3) 0.0499(15) Uani 1 1 d . . . . .
C15 C 0.4959(4) 0.9858(4) 0.8657(3) 0.0431(14) Uani 1 1 d . . . . .
H15 H 0.4402 0.9563 0.8766 0.052 Uiso 1 1 calc R U . . .
C16 C 0.3037(6) 0.8104(4) 0.5401(3) 0.075(2) Uani 1 1 d . . . . .
H16 H 0.3557 0.8129 0.5168 0.090 Uiso 1 1 calc R U . . .
C17 C 0.2023(7) 0.8165(5) 0.5035(4) 0.090(3) Uani 1 1 d . . . . .
H17 H 0.1878 0.8242 0.4569 0.108 Uiso 1 1 calc R U . . .
O13 O 0.7729(6) 0.8037(5) 0.6164(5) 0.245(4) Uani 1 1 d G . . . .
H10W H 0.7617 0.7765 0.6510 0.294 Uiso 1 1 d R U . . .
H9W H 0.7452 0.7732 0.5812 0.294 Uiso 1 1 d R U . . .
O15 O 0.2873(9) 0.7646(7) 1.0042(5) 0.288(5) Uani 1 1 d . . . . .
H13W H 0.2709 0.7097 0.9807 0.345 Uiso 1 1 d R U . . .
H14W H 0.3358 0.8239 1.0048 0.345 Uiso 1 1 d R U . . .
C18 C 0.1242(6) 0.8112(5) 0.5363(5) 0.090(3) Uani 1 1 d . . . . .
H18 H 0.0564 0.8147 0.5123 0.108 Uiso 1 1 calc R U . . .
C19 C 0.1481(6) 0.8004(4) 0.6067(4) 0.070(2) Uani 1 1 d . . . . .
C20 C 0.2515(5) 0.7968(4) 0.6393(3) 0.0511(16) Uani 1 1 d . . . . .
C21 C 0.0724(6) 0.7932(5) 0.6457(5) 0.089(3) Uani 1 1 d . . . . .
H21 H 0.0034 0.7927 0.6239 0.106 Uiso 1 1 calc R U . . .
C22 C 0.0990(6) 0.7871(5) 0.7131(5) 0.086(3) Uani 1 1 d . . . . .
H22 H 0.0482 0.7847 0.7375 0.103 Uiso 1 1 calc R U . . .
C23 C 0.2036(5) 0.7843(4) 0.7479(4) 0.0623(19) Uani 1 1 d . . . . .
C24 C 0.2795(5) 0.7880(3) 0.7110(3) 0.0480(15) Uani 1 1 d . . . . .
C25 C 0.2365(6) 0.7790(4) 0.8184(4) 0.074(2) Uani 1 1 d . . . . .
H25 H 0.1885 0.7780 0.8449 0.089 Uiso 1 1 calc R U . . .
C26 C 0.3376(6) 0.7754(4) 0.8479(4) 0.0634(18) Uani 1 1 d . . . . .
H26 H 0.3595 0.7710 0.8946 0.076 Uiso 1 1 calc R U . . .
C27 C 0.4093(5) 0.7782(4) 0.8069(3) 0.0555(16) Uani 1 1 d . . . . .
H27 H 0.4788 0.7754 0.8274 0.067 Uiso 1 1 calc R U . . .
C28 C 0.6683(5) 0.8086(4) 0.7826(3) 0.0562(17) Uani 1 1 d . . . . .
H28 H 0.6552 0.8721 0.7797 0.067 Uiso 1 1 calc R U . . .
C29 C 0.7535(5) 0.7779(5) 0.8294(3) 0.0653(19) Uani 1 1 d . . . . .
H29 H 0.7969 0.8200 0.8566 0.078 Uiso 1 1 calc R U . . .
C30 C 0.7731(5) 0.6843(5) 0.8353(3) 0.0651(19) Uani 1 1 d . . . . .
H30 H 0.8308 0.6625 0.8659 0.078 Uiso 1 1 calc R U . . .
C31 C 0.7059(4) 0.6223(4) 0.7948(3) 0.0495(15) Uani 1 1 d . . . . .
C32 C 0.6222(4) 0.6598(4) 0.7480(3) 0.0409(14) Uani 1 1 d . . . . .
C33 C 0.7192(5) 0.5234(5) 0.7978(3) 0.0612(18) Uani 1 1 d . . . . .
H33 H 0.7751 0.4979 0.8281 0.073 Uiso 1 1 calc R U . . .
C34 C 0.6524(5) 0.4676(4) 0.7579(3) 0.0618(18) Uani 1 1 d . . . . .
H34 H 0.6624 0.4037 0.7613 0.074 Uiso 1 1 calc R U . . .
C35 C 0.5661(5) 0.5032(4) 0.7101(3) 0.0515(16) Uani 1 1 d . . . . .
C36 C 0.5500(4) 0.5993(4) 0.7058(3) 0.0396(14) Uani 1 1 d . . . . .
C37 C 0.4932(5) 0.4482(4) 0.6657(3) 0.0571(17) Uani 1 1 d . . . . .
H37 H 0.5001 0.3839 0.6666 0.069 Uiso 1 1 calc R U . . .
C38 C 0.4134(5) 0.4881(4) 0.6218(3) 0.0584(17) Uani 1 1 d . . . . .
H38 H 0.3656 0.4520 0.5923 0.070 Uiso 1 1 calc R U . . .
C39 C 0.4047(4) 0.5849(4) 0.6219(3) 0.0472(15) Uani 1 1 d . . . . .
H39 H 0.3498 0.6121 0.5918 0.057 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N4 2.064(4) . ?
Ni1 O1 2.068(3) . ?
Ni1 N5 2.080(4) . ?
Ni1 N2 2.078(5) . ?
Ni1 O9 2.076(4) . ?
Ni1 N3 2.098(4) . ?
N1 O7 1.206(6) . ?
N1 O8 1.210(6) . ?
N1 C14 1.483(8) . ?
N2 C16 1.320(7) . ?
N2 C20 1.361(7) . ?
N3 C27 1.317(7) . ?
N3 C24 1.364(6) . ?
N4 C28 1.323(6) . ?
N4 C32 1.359(6) . ?
N5 C39 1.324(6) . ?
N5 C36 1.356(6) . ?
O1 C1 1.258(6) . ?
O2 C1 1.246(6) . ?
O3 C5 1.207(7) . ?
O4 C5 1.312(7) . ?
O5 C13 1.240(9) . ?
O6 C13 1.199(9) . ?
C1 C2 1.517(7) . ?
C2 C3 1.381(7) . ?
C2 C8 1.404(7) . ?
C3 C4 1.389(7) . ?
C4 C6 1.390(7) . ?
C4 C5 1.484(7) . ?
C6 C7 1.365(7) . ?
C7 C8 1.391(7) . ?
C8 C9 1.491(7) . ?
C9 C15 1.385(7) . ?
C9 C10 1.399(7) . ?
C10 C11 1.377(7) . ?
C11 C12 1.381(8) . ?
C12 C14 1.375(8) . ?
C12 C13 1.537(9) . ?
C14 C15 1.374(7) . ?
C16 C17 1.396(9) . ?
C17 C18 1.366(10) . ?
C18 C19 1.405(10) . ?
C19 C20 1.394(8) . ?
C19 C21 1.428(10) . ?
C20 C24 1.429(8) . ?
C21 C22 1.340(10) . ?
C22 C23 1.420(9) . ?
C23 C25 1.404(9) . ?
C23 C24 1.397(8) . ?
C25 C26 1.352(8) . ?
C26 C27 1.410(8) . ?
C28 C29 1.382(8) . ?
C29 C30 1.372(8) . ?
C30 C31 1.396(8) . ?
C31 C32 1.403(7) . ?
C31 C33 1.434(7) . ?
C32 C36 1.433(7) . ?
C33 C34 1.332(8) . ?
C34 C35 1.427(8) . ?
C35 C36 1.399(7) . ?
C35 C37 1.412(8) . ?
C37 C38 1.355(7) . ?
C38 C39 1.399(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 Ni1 O1 89.46(16) . . ?
N4 Ni1 N5 80.20(18) . . ?
O1 Ni1 N5 165.92(16) . . ?
N4 Ni1 N2 170.51(18) . . ?
O1 Ni1 N2 97.35(16) . . ?
N5 Ni1 N2 94.10(17) . . ?
N4 Ni1 O9 92.57(17) . . ?
O1 Ni1 O9 84.09(14) . . ?
N5 Ni1 O9 86.84(15) . . ?
N2 Ni1 O9 94.71(18) . . ?
N4 Ni1 N3 92.94(18) . . ?
O1 Ni1 N3 97.34(15) . . ?
N5 Ni1 N3 92.74(16) . . ?
N2 Ni1 N3 79.67(19) . . ?
O9 Ni1 N3 174.32(18) . . ?
O7 N1 O8 123.3(7) . . ?
O7 N1 C14 119.2(7) . . ?
O8 N1 C14 117.4(6) . . ?
C16 N2 C20 117.4(6) . . ?
C16 N2 Ni1 129.3(5) . . ?
C20 N2 Ni1 113.2(4) . . ?
C27 N3 C24 118.5(5) . . ?
C27 N3 Ni1 129.1(4) . . ?
C24 N3 Ni1 112.4(4) . . ?
C28 N4 C32 117.6(5) . . ?
C28 N4 Ni1 129.5(4) . . ?
C32 N4 Ni1 112.8(4) . . ?
C39 N5 C36 117.2(5) . . ?
C39 N5 Ni1 130.0(4) . . ?
C36 N5 Ni1 112.8(3) . . ?
C1 O1 Ni1 130.5(3) . . ?
O2 C1 O1 124.5(5) . . ?
O2 C1 C2 118.1(5) . . ?
O1 C1 C2 117.3(5) . . ?
C3 C2 C8 119.2(5) . . ?
C3 C2 C1 117.8(5) . . ?
C8 C2 C1 122.8(5) . . ?
C2 C3 C4 121.5(5) . . ?
C3 C4 C6 118.5(5) . . ?
C3 C4 C5 119.2(5) . . ?
C6 C4 C5 122.3(5) . . ?
O3 C5 O4 122.8(6) . . ?
O3 C5 C4 123.4(6) . . ?
O4 C5 C4 113.8(6) . . ?
C7 C6 C4 120.6(5) . . ?
C6 C7 C8 121.2(5) . . ?
C7 C8 C2 118.8(5) . . ?
C7 C8 C9 118.9(5) . . ?
C2 C8 C9 122.3(5) . . ?
C15 C9 C10 116.8(5) . . ?
C15 C9 C8 120.8(5) . . ?
C10 C9 C8 122.4(5) . . ?
C11 C10 C9 121.7(6) . . ?
C12 C11 C10 120.8(6) . . ?
C11 C12 C14 117.3(6) . . ?
C11 C12 C13 117.4(6) . . ?
C14 C12 C13 125.1(6) . . ?
O6 C13 O5 129.1(8) . . ?
O6 C13 C12 116.2(8) . . ?
O5 C13 C12 114.7(8) . . ?
C15 C14 C12 122.5(6) . . ?
C15 C14 N1 117.7(6) . . ?
C12 C14 N1 119.7(6) . . ?
C14 C15 C9 120.7(5) . . ?
N2 C16 C17 122.9(7) . . ?
C18 C17 C16 119.9(8) . . ?
C17 C18 C19 118.9(8) . . ?
C20 C19 C18 117.3(8) . . ?
C20 C19 C21 119.3(7) . . ?
C18 C19 C21 123.4(8) . . ?
N2 C20 C19 123.6(7) . . ?
N2 C20 C24 117.2(6) . . ?
C19 C20 C24 119.3(7) . . ?
C22 C21 C19 121.2(8) . . ?
C21 C22 C23 120.9(8) . . ?
C25 C23 C24 117.0(7) . . ?
C25 C23 C22 123.7(7) . . ?
C24 C23 C22 119.3(7) . . ?
N3 C24 C23 122.7(6) . . ?
N3 C24 C20 117.3(5) . . ?
C23 C24 C20 120.0(7) . . ?
C26 C25 C23 120.4(7) . . ?
C25 C26 C27 119.1(7) . . ?
N3 C27 C26 122.4(6) . . ?
N4 C28 C29 123.7(6) . . ?
C30 C29 C28 119.0(6) . . ?
C29 C30 C31 119.5(6) . . ?
C30 C31 C32 117.5(6) . . ?
C30 C31 C33 123.6(6) . . ?
C32 C31 C33 118.9(6) . . ?
N4 C32 C31 122.6(5) . . ?
N4 C32 C36 117.4(5) . . ?
C31 C32 C36 119.9(5) . . ?
C34 C33 C31 120.9(6) . . ?
C33 C34 C35 121.8(6) . . ?
C36 C35 C37 116.2(5) . . ?
C36 C35 C34 119.1(6) . . ?
C37 C35 C34 124.7(6) . . ?
N5 C36 C35 123.8(5) . . ?
N5 C36 C32 116.8(5) . . ?
C35 C36 C32 119.4(5) . . ?
C38 C37 C35 120.7(6) . . ?
C37 C38 C39 118.4(6) . . ?
N5 C39 C38 123.7(5) . . ?

_refine_diff_density_max         0.411
_refine_diff_density_min         -0.365
_refine_diff_density_rms         0.067

####################################################################### 
# 
# 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_334-6Co
_database_code_depnum_ccdc_archive 'CCDC 1589521'
_audit_update_record             
;
2017-12-06 deposited with the CCDC.
2018-04-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C60 H76 Co3 N8 O36'
_chemical_formula_weight         1662.07

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'
Co Co 0.3494 0.9721 '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                   11.7676(6)
_cell_length_b                   12.7588(7)
_cell_length_c                   14.2231(7)
_cell_angle_alpha                104.592(5)
_cell_angle_beta                 109.891(5)
_cell_angle_gamma                104.632(5)
_cell_volume                     1803.99(18)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    11272
_cell_measurement_theta_min      3.281
_cell_measurement_theta_max      25.047

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_F_000             861
_exptl_transmission_factor_min   0.804
_exptl_transmission_factor_max   0.829
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.240
_exptl_absorpt_coefficient_mu    0.781
_shelx_estimated_absorpt_T_min   0.811
_shelx_estimated_absorpt_T_max   0.835
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.811
_exptl_absorpt_correction_T_max  0.835
_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            11272
_diffrn_reflns_av_unetI/netI     0.0695
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.281
_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             6358
_reflns_number_gt                4798
_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)+(0.0633P)²+4.3420P] 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         6358
_refine_ls_number_parameters     484
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0818
_refine_ls_R_factor_gt           0.0601
_refine_ls_wR_factor_ref         0.1656
_refine_ls_wR_factor_gt          0.1467
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.030
_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
Co1 Co 0.21636(6) 0.76763(5) 0.28912(5) 0.02126(18) Uani 1 1 d . . . . .
Co2 Co 0.5000 0.5000 0.0000 0.0377(3) Uani 1 2 d S . P . .
N1 N 0.1514(5) 1.1172(4) 0.0978(4) 0.0432(12) Uani 1 1 d . . . . .
N2 N 0.3238(4) 0.8859(3) 0.2338(3) 0.0270(9) Uani 1 1 d . . . . .
N3 N 0.7902(4) 1.2613(4) 0.1341(4) 0.0428(11) Uani 1 1 d . . . . .
N4 N 0.1272(4) 0.6550(3) 0.3592(3) 0.0297(9) Uani 1 1 d . . . . .
O1 O -0.0855(3) 0.7698(3) 0.1729(3) 0.0320(8) Uani 1 1 d . . . . .
O2 O 0.1085(3) 0.8717(3) 0.3132(2) 0.0253(7) Uani 1 1 d . . . . .
O3 O -0.4222(3) 0.7552(3) 0.3182(3) 0.0304(8) Uani 1 1 d . . . . .
O4 O -0.4021(3) 0.9170(3) 0.4391(3) 0.0325(8) Uani 1 1 d . . . . .
O5 O 0.3473(4) 1.3187(4) 0.1731(3) 0.0497(10) Uani 1 1 d . . . . .
O6 O 0.4853(4) 1.3887(4) 0.3468(3) 0.0626(13) Uani 1 1 d . . . . .
O7 O 0.2126(6) 1.0617(5) 0.0717(4) 0.0775(15) Uani 1 1 d . . . . .
O8 O 0.0706(5) 1.1395(5) 0.0361(3) 0.0694(14) Uani 1 1 d . . . . .
O9 O 0.3646(3) 0.8621(3) 0.4441(2) 0.0271(7) Uani 1 1 d . . . . .
H1W H 0.4354 0.8772 0.4418 0.032 Uiso 1 1 d R U . . .
H2W H 0.3764 0.9310 0.4805 0.032 Uiso 1 1 d R U . . .
O10 O 0.0644(3) 0.6581(3) 0.1352(2) 0.0290(7) Uani 1 1 d . . . . .
H3W H 0.0052 0.6829 0.1226 0.035 Uiso 1 1 d R U . . .
H4W H 0.0622 0.6397 0.0727 0.035 Uiso 1 1 d R U . . .
O11 O 0.3241(3) 0.6639(3) 0.2713(3) 0.0331(8) Uani 1 1 d . . . . .
H5W H 0.2781 0.6033 0.2186 0.040 Uiso 1 1 d R U . . .
H6W H 0.4043 0.6929 0.2861 0.040 Uiso 1 1 d R U . . .
O12 O 0.5161(4) 0.4486(3) 0.1249(3) 0.0517(10) Uani 1 1 d . . . . .
H7W H 0.5727 0.5013 0.1809 0.062 Uiso 1 1 d R U . . .
H8W H 0.4618 0.4069 0.1404 0.062 Uiso 1 1 d R U . . .
O13 O 0.7083(4) 0.5480(3) 0.0518(3) 0.0502(10) Uani 1 1 d . . . . .
H9W H 0.6521 0.5183 0.0724 0.060 Uiso 1 1 d R U . . .
H10W H 0.7694 0.6133 0.0971 0.060 Uiso 1 1 d R U . . .
O14 O 0.5275(4) 0.6668(3) 0.0953(3) 0.0511(10) Uani 1 1 d . . . . .
H11W H 0.5763 0.7166 0.0852 0.061 Uiso 1 1 d R U . . .
H12W H 0.5432 0.6934 0.1601 0.061 Uiso 1 1 d R U . . .
O15 O 0.6952(4) 0.8108(4) 0.0544(3) 0.0525(11) Uani 1 1 d . . . . .
H13W H 0.7209 0.8486 0.0185 0.063 Uiso 1 1 d R U . . .
H14W H 0.7611 0.7982 0.0903 0.063 Uiso 1 1 d R U . . .
O16 O 0.7968(4) 0.5520(3) 0.8913(3) 0.0503(10) Uani 1 1 d . . . . .
H15W H 0.7706 0.5500 0.9394 0.060 Uiso 1 1 d R U . . .
H16W H 0.7527 0.5915 0.8708 0.060 Uiso 1 1 d R U . . .
O17 O 0.3464(4) 0.4318(3) 0.6639(3) 0.0479(10) Uani 1 1 d . . . . .
H17W H 0.3697 0.3750 0.6697 0.057 Uiso 1 1 d R U . . .
H18W H 0.3978 0.4892 0.6599 0.057 Uiso 1 1 d R U . . .
O18 O 0.0576(4) 0.5997(3) 0.9329(3) 0.0474(10) Uani 1 1 d . . . . .
H19W H 0.1036 0.6423 0.9133 0.057 Uiso 1 1 d R U . . .
H20W H 0.0228 0.5262 0.9137 0.057 Uiso 1 1 d R U . . .
C1 C -0.0100(4) 0.8515(4) 0.2626(4) 0.0220(9) Uani 1 1 d . . . . .
C2 C -0.0702(4) 0.9244(4) 0.3149(3) 0.0209(9) Uani 1 1 d . . . . .
C3 C -0.1810(4) 0.8672(4) 0.3234(4) 0.0239(10) Uani 1 1 d . . . . .
H3 H -0.2169 0.7861 0.2942 0.029 Uiso 1 1 calc R U . . .
C4 C -0.2401(4) 0.9271(4) 0.3741(3) 0.0228(10) Uani 1 1 d . . . . .
C5 C -0.3634(4) 0.8621(4) 0.3781(3) 0.0218(9) Uani 1 1 d . . . . .
C6 C -0.1847(5) 1.0481(4) 0.4185(4) 0.0303(11) Uani 1 1 d . . . . .
H6 H -0.2209 1.0899 0.4553 0.036 Uiso 1 1 calc R U . . .
C7 C -0.0763(5) 1.1068(4) 0.4084(4) 0.0309(11) Uani 1 1 d . . . . .
H7 H -0.0412 1.1879 0.4376 0.037 Uiso 1 1 calc R U . . .
C8 C -0.0184(4) 1.0469(4) 0.3552(3) 0.0245(10) Uani 1 1 d . . . . .
C9 C 0.0880(4) 1.1152(4) 0.3360(4) 0.0241(10) Uani 1 1 d . . . . .
C10 C 0.0777(5) 1.0853(4) 0.2308(4) 0.0289(10) Uani 1 1 d . . . . .
H10A H 0.0091 1.0203 0.1749 0.035 Uiso 1 1 calc R U . . .
C11 C 0.1716(5) 1.1546(4) 0.2124(4) 0.0291(11) Uani 1 1 d . . . . .
C12 C 0.2768(5) 1.2508(4) 0.2913(4) 0.0318(11) Uani 1 1 d . . . . .
C13 C 0.3791(5) 1.3268(5) 0.2698(5) 0.0395(13) Uani 1 1 d . . . . .
C14 C 0.2853(5) 1.2783(5) 0.3952(4) 0.0383(12) Uani 1 1 d . . . . .
H14A H 0.3553 1.3422 0.4513 0.046 Uiso 1 1 calc R U . . .
C15 C 0.1911(5) 1.2117(4) 0.4162(4) 0.0338(12) Uani 1 1 d . . . . .
H15 H 0.1978 1.2328 0.4860 0.041 Uiso 1 1 calc R U . . .
C16 C 0.3622(5) 0.8466(4) 0.1578(4) 0.0314(11) Uani 1 1 d . . . . .
H16 H 0.3256 0.7671 0.1167 0.038 Uiso 1 1 calc R U . . .
C17 C 0.4528(5) 0.9175(4) 0.1372(4) 0.0324(11) Uani 1 1 d . . . . .
H17 H 0.4759 0.8855 0.0834 0.039 Uiso 1 1 calc R U . . .
C18 C 0.5088(5) 1.0350(4) 0.1959(4) 0.0295(11) Uani 1 1 d . . . . .
C19 C 0.4691(5) 1.0777(4) 0.2751(4) 0.0306(11) Uani 1 1 d . . . . .
H19 H 0.5042 1.1569 0.3170 0.037 Uiso 1 1 calc R U . . .
C20 C 0.3778(5) 1.0011(4) 0.2901(4) 0.0315(11) Uani 1 1 d . . . . .
H20 H 0.3518 1.0311 0.3425 0.038 Uiso 1 1 calc R U . . .
C21 C 0.6085(5) 1.1148(4) 0.1768(4) 0.0301(11) Uani 1 1 d . . . . .
C22 C 0.6967(5) 1.0781(5) 0.1464(4) 0.0398(13) Uani 1 1 d . . . . .
H22 H 0.6967 1.0037 0.1398 0.048 Uiso 1 1 calc R U . . .
C23 C 0.7846(5) 1.1535(5) 0.1262(5) 0.0458(14) Uani 1 1 d . . . . .
H23 H 0.8429 1.1275 0.1059 0.055 Uiso 1 1 calc R U . . .
C24 C 0.7059(6) 1.2954(5) 0.1634(5) 0.0501(15) Uani 1 1 d . . . . .
H24 H 0.7084 1.3704 0.1697 0.060 Uiso 1 1 calc R U . . .
C25 C 0.6147(6) 1.2267(5) 0.1850(5) 0.0449(14) Uani 1 1 d . . . . .
H25 H 0.5576 1.2553 0.2049 0.054 Uiso 1 1 calc R U . . .
C26 C 0.2015(5) 0.6239(6) 0.4322(5) 0.0522(17) Uani 1 1 d . . . . .
H26 H 0.2891 0.6448 0.4469 0.063 Uiso 1 1 calc R U . . .
C27 C 0.1562(5) 0.5625(6) 0.4877(5) 0.0562(18) Uani 1 1 d . . . . .
H27 H 0.2125 0.5416 0.5367 0.067 Uiso 1 1 calc R U . . .
C28 C 0.0263(5) 0.5318(4) 0.4701(4) 0.0314(11) Uani 1 1 d . . . . .
C29 C -0.0500(5) 0.5648(4) 0.3951(4) 0.0352(12) Uani 1 1 d . . . . .
H29 H -0.1374 0.5473 0.3802 0.042 Uiso 1 1 calc R U . . .
C30 C 0.0028(5) 0.6236(5) 0.3418(4) 0.0362(12) Uani 1 1 d . . . . .
H30 H -0.0523 0.6427 0.2902 0.043 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
Co1 O11 2.079(3) . ?
Co1 O9 2.083(3) . ?
Co1 O2 2.100(3) . ?
Co1 O10 2.115(3) . ?
Co1 N2 2.193(4) . ?
Co1 N4 2.197(4) . ?
Co2 O12 2.011(4) . ?
Co2 O12 2.011(4) 2_665 ?
Co2 O14 2.091(4) . ?
Co2 O14 2.091(4) 2_665 ?
Co2 O13 2.171(4) 2_665 ?
Co2 O13 2.171(4) . ?
Co2 H9W 1.6530 . ?
N1 O8 1.205(6) . ?
N1 O7 1.210(6) . ?
N1 C11 1.492(6) . ?
N2 C16 1.340(6) . ?
N2 C20 1.340(6) . ?
N3 C24 1.325(7) . ?
N3 C23 1.334(7) . ?
N4 C26 1.329(6) . ?
N4 C30 1.332(6) . ?
O1 C1 1.263(5) . ?
O2 C1 1.254(5) . ?
O3 C5 1.265(5) . ?
O4 C5 1.255(5) . ?
O5 C13 1.264(6) . ?
O6 C13 1.233(7) . ?
O9 H1W 0.8200 . ?
O9 H2W 0.8495 . ?
O10 H3W 0.8200 . ?
O10 H4W 0.8503 . ?
O11 H5W 0.8200 . ?
O11 H6W 0.8489 . ?
O12 H7W 0.8200 . ?
O12 H8W 0.8500 . ?
O13 H9W 0.8537 . ?
O13 H10W 0.8589 . ?
O14 H11W 0.8200 . ?
O14 H12W 0.8332 . ?
O15 H13W 0.8608 . ?
O15 H14W 0.8501 . ?
O16 H15W 0.8443 . ?
O16 H16W 0.8431 . ?
O17 H17W 0.8499 . ?
O17 H18W 0.8520 . ?
O18 H19W 0.8349 . ?
O18 H20W 0.8500 . ?
C1 C2 1.504(6) . ?
C2 C3 1.386(6) . ?
C2 C8 1.404(6) . ?
C3 C4 1.385(6) . ?
C3 H3 0.9300 . ?
C4 C6 1.388(6) . ?
C4 C5 1.506(6) . ?
C6 C7 1.380(6) . ?
C6 H6 0.9300 . ?
C7 C8 1.394(6) . ?
C7 H7 0.9300 . ?
C8 C9 1.485(6) . ?
C9 C15 1.373(7) . ?
C9 C10 1.401(6) . ?
C10 C11 1.375(6) . ?
C10 H10A 0.9300 . ?
C11 C12 1.376(7) . ?
C12 C14 1.392(7) . ?
C12 C13 1.515(7) . ?
C14 C15 1.385(7) . ?
C14 H14A 0.9300 . ?
C15 H15 0.9300 . ?
C16 C17 1.379(6) . ?
C16 H16 0.9300 . ?
C17 C18 1.369(7) . ?
C17 H17 0.9300 . ?
C18 C19 1.400(6) . ?
C18 C21 1.497(6) . ?
C19 C20 1.373(6) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
C21 C25 1.385(7) . ?
C21 C22 1.388(7) . ?
C22 C23 1.386(7) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 C25 1.379(7) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
C26 C27 1.381(7) . ?
C26 H26 0.9300 . ?
C27 C28 1.394(7) . ?
C27 H27 0.9300 . ?
C28 C29 1.374(7) . ?
C28 C28 1.488(8) 2_566 ?
C29 C30 1.376(6) . ?
C29 H29 0.9300 . ?
C30 H30 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O11 Co1 O9 86.47(13) . . ?
O11 Co1 O2 177.64(12) . . ?
O9 Co1 O2 91.97(12) . . ?
O11 Co1 O10 90.54(13) . . ?
O9 Co1 O10 174.81(12) . . ?
O2 Co1 O10 90.88(12) . . ?
O11 Co1 N2 89.65(13) . . ?
O9 Co1 N2 88.01(13) . . ?
O2 Co1 N2 92.07(13) . . ?
O10 Co1 N2 96.22(13) . . ?
O11 Co1 N4 88.13(14) . . ?
O9 Co1 N4 86.52(13) . . ?
O2 Co1 N4 90.01(13) . . ?
O10 Co1 N4 89.15(14) . . ?
N2 Co1 N4 174.21(15) . . ?
O12 Co2 O12 180.0 . 2_665 ?
O12 Co2 O14 89.81(16) . . ?
O12 Co2 O14 90.18(16) 2_665 . ?
O12 Co2 O14 90.18(16) . 2_665 ?
O12 Co2 O14 89.82(16) 2_665 2_665 ?
O14 Co2 O14 180.0 . 2_665 ?
O12 Co2 O13 90.88(16) . 2_665 ?
O12 Co2 O13 89.12(16) 2_665 2_665 ?
O14 Co2 O13 88.88(15) . 2_665 ?
O14 Co2 O13 91.12(15) 2_665 2_665 ?
O12 Co2 O13 89.12(16) . . ?
O12 Co2 O13 90.88(16) 2_665 . ?
O14 Co2 O13 91.12(15) . . ?
O14 Co2 O13 88.88(15) 2_665 . ?
O13 Co2 O13 180.0(2) 2_665 . ?
O12 Co2 H9W 68.5 . . ?
O12 Co2 H9W 111.5 2_665 . ?
O14 Co2 H9W 91.4 . . ?
O14 Co2 H9W 88.6 2_665 . ?
O13 Co2 H9W 159.4 2_665 . ?
O13 Co2 H9W 20.6 . . ?
O8 N1 O7 124.1(5) . . ?
O8 N1 C11 117.7(5) . . ?
O7 N1 C11 118.1(5) . . ?
C16 N2 C20 116.1(4) . . ?
C16 N2 Co1 121.8(3) . . ?
C20 N2 Co1 120.5(3) . . ?
C24 N3 C23 116.6(4) . . ?
C26 N4 C30 115.5(4) . . ?
C26 N4 Co1 119.8(3) . . ?
C30 N4 Co1 124.3(3) . . ?
C1 O2 Co1 129.7(3) . . ?
Co1 O9 H1W 109.6 . . ?
Co1 O9 H2W 122.7 . . ?
H1W O9 H2W 97.2 . . ?
Co1 O10 H3W 109.4 . . ?
Co1 O10 H4W 131.9 . . ?
H3W O10 H4W 97.2 . . ?
Co1 O11 H5W 109.6 . . ?
Co1 O11 H6W 122.0 . . ?
H5W O11 H6W 118.3 . . ?
Co2 O12 H7W 109.6 . . ?
Co2 O12 H8W 133.9 . . ?
H7W O12 H8W 108.2 . . ?
Co2 O13 H9W 43.0 . . ?
Co2 O13 H10W 128.0 . . ?
H9W O13 H10W 116.0 . . ?
Co2 O14 H11W 110.2 . . ?
Co2 O14 H12W 129.5 . . ?
H11W O14 H12W 106.7 . . ?
H13W O15 H14W 104.8 . . ?
H15W O16 H16W 91.2 . . ?
H17W O17 H18W 118.6 . . ?
H19W O18 H20W 133.5 . . ?
O2 C1 O1 124.9(4) . . ?
O2 C1 C2 118.2(4) . . ?
O1 C1 C2 116.8(4) . . ?
C3 C2 C8 119.2(4) . . ?
C3 C2 C1 118.0(4) . . ?
C8 C2 C1 122.8(4) . . ?
C4 C3 C2 122.0(4) . . ?
C4 C3 H3 119.0 . . ?
C2 C3 H3 119.0 . . ?
C3 C4 C6 118.4(4) . . ?
C3 C4 C5 120.5(4) . . ?
C6 C4 C5 121.1(4) . . ?
O4 C5 O3 124.2(4) . . ?
O4 C5 C4 118.4(4) . . ?
O3 C5 C4 117.4(4) . . ?
C7 C6 C4 120.5(4) . . ?
C7 C6 H6 119.8 . . ?
C4 C6 H6 119.8 . . ?
C6 C7 C8 121.3(4) . . ?
C6 C7 H7 119.4 . . ?
C8 C7 H7 119.4 . . ?
C7 C8 C2 118.5(4) . . ?
C7 C8 C9 118.4(4) . . ?
C2 C8 C9 122.9(4) . . ?
C15 C9 C10 118.9(4) . . ?
C15 C9 C8 122.1(4) . . ?
C10 C9 C8 118.7(4) . . ?
C11 C10 C9 118.3(4) . . ?
C11 C10 H10A 120.8 . . ?
C9 C10 H10A 120.8 . . ?
C10 C11 C12 124.0(4) . . ?
C10 C11 N1 114.5(4) . . ?
C12 C11 N1 121.4(4) . . ?
C11 C12 C14 116.5(4) . . ?
C11 C12 C13 123.5(4) . . ?
C14 C12 C13 119.9(5) . . ?
O6 C13 O5 126.3(5) . . ?
O6 C13 C12 117.5(5) . . ?
O5 C13 C12 116.2(5) . . ?
C15 C14 C12 120.9(5) . . ?
C15 C14 H14A 119.5 . . ?
C12 C14 H14A 119.5 . . ?
C9 C15 C14 121.2(4) . . ?
C9 C15 H15 119.4 . . ?
C14 C15 H15 119.4 . . ?
N2 C16 C17 123.6(5) . . ?
N2 C16 H16 118.2 . . ?
C17 C16 H16 118.2 . . ?
C18 C17 C16 119.9(5) . . ?
C18 C17 H17 120.0 . . ?
C16 C17 H17 120.0 . . ?
C17 C18 C19 117.2(4) . . ?
C17 C18 C21 121.6(4) . . ?
C19 C18 C21 121.2(4) . . ?
C20 C19 C18 119.1(5) . . ?
C20 C19 H19 120.4 . . ?
C18 C19 H19 120.4 . . ?
N2 C20 C19 123.9(4) . . ?
N2 C20 H20 118.0 . . ?
C19 C20 H20 118.0 . . ?
C25 C21 C22 117.0(4) . . ?
C25 C21 C18 121.8(4) . . ?
C22 C21 C18 121.2(4) . . ?
C23 C22 C21 119.3(5) . . ?
C23 C22 H22 120.3 . . ?
C21 C22 H22 120.3 . . ?
N3 C23 C22 123.6(5) . . ?
N3 C23 H23 118.2 . . ?
C22 C23 H23 118.2 . . ?
N3 C24 C25 124.1(5) . . ?
N3 C24 H24 118.0 . . ?
C25 C24 H24 118.0 . . ?
C24 C25 C21 119.5(5) . . ?
C24 C25 H25 120.3 . . ?
C21 C25 H25 120.3 . . ?
N4 C26 C27 123.9(5) . . ?
N4 C26 H26 118.1 . . ?
C27 C26 H26 118.1 . . ?
C26 C27 C28 120.0(5) . . ?
C26 C27 H27 120.0 . . ?
C28 C27 H27 120.0 . . ?
C29 C28 C27 116.0(4) . . ?
C29 C28 C28 122.0(5) . 2_566 ?
C27 C28 C28 122.0(6) . 2_566 ?
C28 C29 C30 120.1(4) . . ?
C28 C29 H29 120.0 . . ?
C30 C29 H29 120.0 . . ?
N4 C30 C29 124.5(5) . . ?
N4 C30 H30 117.7 . . ?
C29 C30 H30 117.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Co1 O2 C1 O1 -13.0(6) . . . . ?
Co1 O2 C1 C2 162.8(3) . . . . ?
O2 C1 C2 C3 -126.6(4) . . . . ?
O1 C1 C2 C3 49.6(6) . . . . ?
O2 C1 C2 C8 53.1(6) . . . . ?
O1 C1 C2 C8 -130.7(5) . . . . ?
C8 C2 C3 C4 -2.4(7) . . . . ?
C1 C2 C3 C4 177.4(4) . . . . ?
C2 C3 C4 C6 -0.8(7) . . . . ?
C2 C3 C4 C5 177.6(4) . . . . ?
C3 C4 C5 O4 168.6(4) . . . . ?
C6 C4 C5 O4 -13.1(7) . . . . ?
C3 C4 C5 O3 -12.2(6) . . . . ?
C6 C4 C5 O3 166.1(4) . . . . ?
C3 C4 C6 C7 2.4(7) . . . . ?
C5 C4 C6 C7 -175.9(4) . . . . ?
C4 C6 C7 C8 -1.0(8) . . . . ?
C6 C7 C8 C2 -2.1(7) . . . . ?
C6 C7 C8 C9 172.9(4) . . . . ?
C3 C2 C8 C7 3.8(7) . . . . ?
C1 C2 C8 C7 -175.9(4) . . . . ?
C3 C2 C8 C9 -171.0(4) . . . . ?
C1 C2 C8 C9 9.3(7) . . . . ?
C7 C8 C9 C15 48.9(7) . . . . ?
C2 C8 C9 C15 -136.3(5) . . . . ?
C7 C8 C9 C10 -126.3(5) . . . . ?
C2 C8 C9 C10 48.5(6) . . . . ?
C15 C9 C10 C11 -0.3(7) . . . . ?
C8 C9 C10 C11 175.0(4) . . . . ?
C9 C10 C11 C12 1.2(7) . . . . ?
C9 C10 C11 N1 -179.0(4) . . . . ?
O8 N1 C11 C10 77.2(6) . . . . ?
O7 N1 C11 C10 -99.4(6) . . . . ?
O8 N1 C11 C12 -103.1(6) . . . . ?
O7 N1 C11 C12 80.3(6) . . . . ?
C10 C11 C12 C14 -0.8(8) . . . . ?
N1 C11 C12 C14 179.5(5) . . . . ?
C10 C11 C12 C13 -179.6(5) . . . . ?
N1 C11 C12 C13 0.7(8) . . . . ?
C11 C12 C13 O6 -160.1(5) . . . . ?
C14 C12 C13 O6 21.2(8) . . . . ?
C11 C12 C13 O5 18.7(8) . . . . ?
C14 C12 C13 O5 -160.0(5) . . . . ?
C11 C12 C14 C15 -0.5(8) . . . . ?
C13 C12 C14 C15 178.3(5) . . . . ?
C10 C9 C15 C14 -1.0(8) . . . . ?
C8 C9 C15 C14 -176.2(5) . . . . ?
C12 C14 C15 C9 1.5(8) . . . . ?
C20 N2 C16 C17 0.8(7) . . . . ?
Co1 N2 C16 C17 -165.3(4) . . . . ?
N2 C16 C17 C18 0.0(8) . . . . ?
C16 C17 C18 C19 -0.5(7) . . . . ?
C16 C17 C18 C21 179.4(5) . . . . ?
C17 C18 C19 C20 0.2(7) . . . . ?
C21 C18 C19 C20 -179.7(4) . . . . ?
C16 N2 C20 C19 -1.1(7) . . . . ?
Co1 N2 C20 C19 165.2(4) . . . . ?
C18 C19 C20 N2 0.7(8) . . . . ?
C17 C18 C21 C25 143.7(5) . . . . ?
C19 C18 C21 C25 -36.4(7) . . . . ?
C17 C18 C21 C22 -34.2(7) . . . . ?
C19 C18 C21 C22 145.7(5) . . . . ?
C25 C21 C22 C23 -0.1(8) . . . . ?
C18 C21 C22 C23 177.9(5) . . . . ?
C24 N3 C23 C22 0.1(9) . . . . ?
C21 C22 C23 N3 0.1(9) . . . . ?
C23 N3 C24 C25 -0.3(9) . . . . ?
N3 C24 C25 C21 0.3(10) . . . . ?
C22 C21 C25 C24 -0.1(8) . . . . ?
C18 C21 C25 C24 -178.1(5) . . . . ?
C30 N4 C26 C27 0.4(9) . . . . ?
Co1 N4 C26 C27 173.9(6) . . . . ?
N4 C26 C27 C28 -1.5(11) . . . . ?
C26 C27 C28 C29 0.9(10) . . . . ?
C26 C27 C28 C28 -178.4(7) . . . 2_566 ?
C27 C28 C29 C30 0.5(8) . . . . ?
C28 C28 C29 C30 179.9(6) 2_566 . . . ?
C26 N4 C30 C29 1.2(8) . . . . ?
Co1 N4 C30 C29 -172.0(4) . . . . ?
C28 C29 C30 N4 -1.7(9) . . . . ?

_refine_diff_density_max         0.457
_refine_diff_density_min         -1.363
_refine_diff_density_rms         0.092

####################################################################### 
# 
# 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_334-1Zn
_database_code_depnum_ccdc_archive 'CCDC 1589520'
_audit_update_record             
;
2017-12-06 deposited with the CCDC.
2018-04-30 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 N8 O22 Zn3'
_chemical_formula_weight         1499.22

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           5
_space_group_name_H-M_alt        'C 2'
_space_group_name_Hall           'C 2y'

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

_cell_length_a                   11.2162(4)
_cell_length_b                   23.1617(10)
_cell_length_c                   14.1043(7)
_cell_angle_alpha                90
_cell_angle_beta                 109.037(5)
_cell_angle_gamma                90
_cell_volume                     3463.7(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6223
_cell_measurement_theta_min      3.264
_cell_measurement_theta_max      25.050

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_F_000             1528
_exptl_transmission_factor_min   0.732
_exptl_transmission_factor_max   0.766
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.240
_exptl_absorpt_coefficient_mu    1.111
_shelx_estimated_absorpt_T_min   0.739
_shelx_estimated_absorpt_T_max   0.776
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.739
_exptl_absorpt_correction_T_max  0.776
_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            6223
_diffrn_reflns_av_unetI/netI     0.0760
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.264
_diffrn_reflns_theta_max         25.050
_diffrn_reflns_theta_full        25.050
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.725
_diffrn_reflns_point_group_measured_fraction_full 0.724
_reflns_number_total             4454
_reflns_number_gt                3421
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.415
_reflns_Friedel_fraction_max     0.437
_reflns_Friedel_fraction_full    0.437

_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)+(0.1060P)²+6.2749P] 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_abs_structure_details 
;
 Flack x determined using 797 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.047(16)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         4454
_refine_ls_number_parameters     447
_refine_ls_number_restraints     114
_refine_ls_R_factor_all          0.0800
_refine_ls_R_factor_gt           0.0599
_refine_ls_wR_factor_ref         0.1717
_refine_ls_wR_factor_gt          0.1512
_refine_ls_goodness_of_fit_ref   0.889
_refine_ls_restrained_S_all      0.914
_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 0.84512(10) 0.27676(6) 0.70067(8) 0.0476(3) Uani 1 1 d . . . . .
Zn2 Zn 0.0000 0.47885(7) 0.5000 0.0502(5) Uani 1 2 d S T P . .
N1 N 0.7267(13) 0.1933(6) 1.0642(8) 0.085(4) Uani 1 1 d . . . . .
N2 N 0.8347(9) 0.2316(6) 0.5696(8) 0.070(3) Uani 1 1 d . . . . .
N3 N 0.8350(8) 0.1885(4) 0.7430(7) 0.054(2) Uani 1 1 d . . . . .
N4 N 0.0002(9) 0.5493(5) 0.5954(8) 0.066(3) Uani 1 1 d . . . . .
O1 O 0.6770(7) 0.3003(3) 0.7046(5) 0.0519(18) Uani 1 1 d . . . . .
O2 O 0.6431(8) 0.3863(4) 0.6292(7) 0.081(3) Uani 1 1 d . . . . .
O3 O 0.1819(7) 0.4458(3) 0.5330(6) 0.0562(19) Uani 1 1 d . . . . .
O4 O 0.0746(7) 0.4186(4) 0.6297(7) 0.070(2) Uani 1 1 d . . . . .
O5 O 1.0415(9) 0.3009(5) 1.1648(7) 0.099(3) Uani 1 1 d . . . . .
O6 O 0.9164(8) 0.2495(6) 1.2183(7) 0.117(5) Uani 1 1 d . . . . .
O7 O 0.8166(15) 0.1629(6) 1.0690(11) 0.138(6) Uani 1 1 d . . . . .
O8 O 0.6438(10) 0.1836(6) 1.0983(11) 0.132(5) Uani 1 1 d . . . . .
O9 O 0.8734(9) 0.3535(5) 0.6330(10) 0.121(5) Uani 1 1 d . . . . .
H9A H 0.9363 0.3738 0.6327 0.145 Uiso 1 1 d R U . . .
H9B H 0.8008 0.3640 0.6329 0.145 Uiso 1 1 d R U . . .
O10 O 0.0612(19) 0.4369(8) 0.1676(11) 0.182(7) Uani 1 1 d D . . . .
H10A H 0.0553 0.4003 0.1663 0.219 Uiso 1 1 d R U . . .
H10B H 0.0635 0.4158 0.2187 0.219 Uiso 1 1 d DR U . . .
O11 O 0.696(3) 0.4941(9) 0.7131(17) 0.269(13) Uani 1 1 d . . . . .
H11A H 0.7642 0.4775 0.7467 0.322 Uiso 1 1 d R U . . .
H11B H 0.6785 0.4607 0.6872 0.322 Uiso 1 1 d R U . . .
C1 C 0.6176(9) 0.3470(5) 0.6807(7) 0.051(3) Uani 1 1 d . . . . .
C2 C 0.5047(8) 0.3558(4) 0.7137(7) 0.039(2) Uani 1 1 d . . . . .
C3 C 0.3970(9) 0.3808(4) 0.6484(7) 0.042(2) Uani 1 1 d . . . . .
H3 H 0.3966 0.3927 0.5854 0.051 Uiso 1 1 calc R U . . .
C4 C 0.2890(9) 0.3883(5) 0.6755(8) 0.048(2) Uani 1 1 d . . . . .
C5 C 0.1759(10) 0.4194(4) 0.6078(9) 0.050(3) Uani 1 1 d . . . . .
C6 C 0.2878(10) 0.3667(7) 0.7663(9) 0.069(4) Uani 1 1 d . . . . .
H6 H 0.2141 0.3681 0.7828 0.083 Uiso 1 1 calc R U . . .
C7 C 0.3945(10) 0.3433(6) 0.8322(8) 0.067(4) Uani 1 1 d . . . . .
H7 H 0.3934 0.3316 0.8950 0.081 Uiso 1 1 calc R U . . .
C8 C 0.5067(10) 0.3362(5) 0.8082(7) 0.053(3) Uani 1 1 d . . . . .
C9 C 0.6210(9) 0.3167(5) 0.8890(7) 0.050(3) Uani 1 1 d . . . . .
C10 C 0.6215(10) 0.2643(5) 0.9382(7) 0.050(3) Uani 1 1 d . . . . .
H10 H 0.5529 0.2393 0.9179 0.060 Uiso 1 1 calc R U . . .
C11 C 0.7276(10) 0.2509(5) 1.0182(7) 0.055(3) Uani 1 1 d . . . . .
C12 C 0.8303(9) 0.2863(6) 1.0568(7) 0.052(3) Uani 1 1 d . . . . .
C13 C 0.9370(11) 0.2766(8) 1.1538(7) 0.070(3) Uani 1 1 d . . . . .
C14 C 0.8263(10) 0.3380(6) 1.0034(7) 0.060(3) Uani 1 1 d . . . . .
H14 H 0.8947 0.3631 1.0231 0.073 Uiso 1 1 calc R U . . .
C15 C 0.7231(10) 0.3519(6) 0.9228(8) 0.056(3) Uani 1 1 d . . . . .
H15 H 0.7230 0.3867 0.8899 0.067 Uiso 1 1 calc R U . . .
C16 C 0.8313(14) 0.2536(8) 0.4807(11) 0.096(5) Uani 1 1 d . U . . .
H16 H 0.8302 0.2935 0.4721 0.115 Uiso 1 1 calc R U . . .
C17 C 0.8295(18) 0.2165(11) 0.3990(15) 0.113(4) Uani 1 1 d . U . . .
H17 H 0.8258 0.2326 0.3376 0.136 Uiso 1 1 calc R U . . .
C18 C 0.8327(19) 0.1651(11) 0.4087(15) 0.113(4) Uani 1 1 d . U . . .
H18 H 0.8339 0.1427 0.3543 0.136 Uiso 1 1 calc R U . . .
C19 C 0.8348(15) 0.1377(9) 0.4935(14) 0.098(4) Uani 1 1 d . U . . .
C20 C 0.8362(10) 0.1742(6) 0.5757(10) 0.064(4) Uani 1 1 d . . . . .
C21 C 0.8406(14) 0.0755(9) 0.5235(15) 0.098(4) Uani 1 1 d . U . . .
H21 H 0.8360 0.0489 0.4730 0.118 Uiso 1 1 calc R U . . .
C22 C 0.8506(16) 0.0552(9) 0.6051(15) 0.104(3) Uani 1 1 d . U . . .
H22 H 0.8609 0.0155 0.6144 0.124 Uiso 1 1 calc R U . . .
C23 C 0.8470(16) 0.0907(8) 0.6882(16) 0.103(3) Uani 1 1 d . U . . .
C24 C 0.8408(10) 0.1507(6) 0.6735(11) 0.068(4) Uani 1 1 d . . . . .
C25 C 0.8521(16) 0.0734(9) 0.7816(16) 0.105(3) Uani 1 1 d . U . . .
H25 H 0.8587 0.0340 0.7953 0.126 Uiso 1 1 calc R U . . .
C26 C 0.848(2) 0.1086(10) 0.8542(17) 0.127(7) Uani 1 1 d . U . . .
H26 H 0.8489 0.0945 0.9161 0.152 Uiso 1 1 calc R U . . .
C27 C 0.8431(14) 0.1686(7) 0.8340(12) 0.088(4) Uani 1 1 d . U . . .
H27 H 0.8455 0.1946 0.8848 0.105 Uiso 1 1 calc R U . . .
C28 C 0.0002(15) 0.5458(10) 0.6904(11) 0.106(6) Uani 1 1 d . . . . .
H28 H -0.0004 0.5107 0.7225 0.127 Uiso 1 1 calc R U . . .
C29 C 0.001(2) 0.6027(14) 0.7401(13) 0.142(10) Uani 1 1 d . . . . .
H29 H 0.0052 0.6043 0.8069 0.170 Uiso 1 1 calc R U . . .
C30 C -0.003(2) 0.6457(12) 0.694(2) 0.131(8) Uani 1 1 d . U . . .
H30 H -0.0119 0.6792 0.7276 0.158 Uiso 1 1 calc R U . . .
C31 C 0.0028(13) 0.6541(7) 0.6033(15) 0.091(4) Uani 1 1 d . U . . .
C32 C 0.0010(11) 0.6012(5) 0.5499(9) 0.061(3) Uani 1 1 d . U . . .
C33 C 0.0012(16) 0.7058(7) 0.5409(12) 0.097(5) Uani 1 1 d . 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 1.989(9) 2_757 ?
Zn1 O1 1.982(7) . ?
Zn1 O9 2.089(10) . ?
Zn1 N2 2.093(11) . ?
Zn1 N3 2.143(10) . ?
Zn2 O3 2.084(7) 2_556 ?
Zn2 O3 2.084(7) . ?
Zn2 N4 2.114(10) 2_556 ?
Zn2 N4 2.114(10) . ?
Zn2 O4 2.235(8) 2_556 ?
Zn2 O4 2.235(8) . ?
Zn2 C5 2.478(11) 2_556 ?
N1 O8 1.200(13) . ?
N1 O7 1.214(15) . ?
N1 C11 1.485(16) . ?
N2 C20 1.333(18) . ?
N2 C16 1.343(17) . ?
N3 C27 1.338(16) . ?
N3 C24 1.332(15) . ?
N4 C28 1.342(17) . ?
N4 C32 1.363(17) . ?
O1 C1 1.256(13) . ?
O2 C1 1.255(13) . ?
O3 C5 1.241(13) . ?
O4 C5 1.270(12) . ?
O5 C13 1.264(16) . ?
O5 Zn1 1.989(9) 2_757 ?
O6 C13 1.188(15) . ?
O9 H9A 0.8500 . ?
O9 H9B 0.8501 . ?
O10 H10A 0.8503 . ?
O10 H10B 0.8638 . ?
O11 H11A 0.8499 . ?
O11 H11B 0.8503 . ?
C1 C2 1.498(13) . ?
C2 C8 1.403(13) . ?
C2 C3 1.384(13) . ?
C3 C4 1.395(13) . ?
C3 H3 0.9300 . ?
C4 C6 1.379(15) . ?
C4 C5 1.500(14) . ?
C6 C7 1.365(15) . ?
C6 H6 0.9300 . ?
C7 C8 1.414(14) . ?
C7 H7 0.9300 . ?
C8 C9 1.481(14) . ?
C9 C15 1.359(15) . ?
C9 C10 1.399(15) . ?
C10 C11 1.381(14) . ?
C10 H10 0.9300 . ?
C11 C12 1.374(16) . ?
C12 C14 1.408(17) . ?
C12 C13 1.512(14) . ?
C14 C15 1.370(14) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C17 1.43(2) . ?
C16 H16 0.9300 . ?
C17 C18 1.20(3) . ?
C17 H17 0.9300 . ?
C18 C19 1.35(3) . ?
C18 H18 0.9300 . ?
C19 C20 1.431(19) . ?
C19 C21 1.50(3) . ?
C20 C24 1.47(2) . ?
C21 C22 1.21(2) . ?
C21 H21 0.9300 . ?
C22 C23 1.44(2) . ?
C22 H22 0.9300 . ?
C23 C25 1.36(2) . ?
C23 C24 1.40(2) . ?
C25 C26 1.32(3) . ?
C25 H25 0.9300 . ?
C26 C27 1.42(2) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
C28 C29 1.49(3) . ?
C28 H28 0.9300 . ?
C29 C30 1.18(3) . ?
C29 H29 0.9300 . ?
C30 C31 1.32(3) . ?
C30 H30 0.9300 . ?
C31 C32 1.436(19) . ?
C31 C33 1.48(2) . ?
C32 C32 1.40(3) 2_556 ?
C33 C33 1.15(3) 2_556 ?

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 102.4(4) 2_757 . ?
O5 Zn1 O9 93.0(5) 2_757 . ?
O1 Zn1 O9 93.8(3) . . ?
O5 Zn1 N2 144.8(4) 2_757 . ?
O1 Zn1 N2 112.5(3) . . ?
O9 Zn1 N2 89.7(6) . . ?
O5 Zn1 N3 94.5(4) 2_757 . ?
O1 Zn1 N3 96.7(3) . . ?
O9 Zn1 N3 165.5(4) . . ?
N2 Zn1 N3 77.1(4) . . ?
O3 Zn2 O3 137.0(4) 2_556 . ?
O3 Zn2 N4 110.1(3) 2_556 2_556 ?
O3 Zn2 N4 102.9(3) . 2_556 ?
O3 Zn2 N4 102.9(3) 2_556 . ?
O3 Zn2 N4 110.1(3) . . ?
N4 Zn2 N4 79.0(6) 2_556 . ?
O3 Zn2 O4 60.7(3) 2_556 2_556 ?
O3 Zn2 O4 91.8(3) . 2_556 ?
N4 Zn2 O4 92.2(4) 2_556 2_556 ?
N4 Zn2 O4 157.7(3) . 2_556 ?
O3 Zn2 O4 91.8(3) 2_556 . ?
O3 Zn2 O4 60.7(3) . . ?
N4 Zn2 O4 157.7(3) 2_556 . ?
N4 Zn2 O4 92.2(4) . . ?
O4 Zn2 O4 102.7(5) 2_556 . ?
O3 Zn2 C5 30.0(3) 2_556 2_556 ?
O3 Zn2 C5 117.3(3) . 2_556 ?
N4 Zn2 C5 101.7(4) 2_556 2_556 ?
N4 Zn2 C5 130.9(3) . 2_556 ?
O4 Zn2 C5 30.7(3) 2_556 2_556 ?
O4 Zn2 C5 99.6(3) . 2_556 ?
O8 N1 O7 127.4(13) . . ?
O8 N1 C11 117.4(12) . . ?
O7 N1 C11 115.0(12) . . ?
C20 N2 C16 115.8(13) . . ?
C20 N2 Zn1 116.5(9) . . ?
C16 N2 Zn1 127.7(12) . . ?
C27 N3 C24 118.4(13) . . ?
C27 N3 Zn1 127.1(10) . . ?
C24 N3 Zn1 113.6(9) . . ?
C28 N4 C32 121.7(13) . . ?
C28 N4 Zn2 126.0(12) . . ?
C32 N4 Zn2 112.3(8) . . ?
C1 O1 Zn1 131.0(6) . . ?
C5 O3 Zn2 92.8(6) . . ?
C5 O4 Zn2 85.3(6) . . ?
C13 O5 Zn1 105.7(8) . 2_757 ?
Zn1 O9 H9A 136.4 . . ?
Zn1 O9 H9B 87.6 . . ?
H9A O9 H9B 129.5 . . ?
H10A O10 H10B 55.6 . . ?
H11A O11 H11B 82.4 . . ?
O1 C1 O2 125.4(10) . . ?
O1 C1 C2 117.5(9) . . ?
O2 C1 C2 117.1(10) . . ?
C8 C2 C3 120.5(8) . . ?
C8 C2 C1 119.9(8) . . ?
C3 C2 C1 119.5(8) . . ?
C2 C3 C4 121.2(8) . . ?
C2 C3 H3 119.4 . . ?
C4 C3 H3 119.4 . . ?
C6 C4 C3 118.7(9) . . ?
C6 C4 C5 120.2(9) . . ?
C3 C4 C5 121.1(9) . . ?
O3 C5 O4 121.0(10) . . ?
O3 C5 C4 120.6(9) . . ?
O4 C5 C4 118.4(10) . . ?
C7 C6 C4 120.3(9) . . ?
C7 C6 H6 119.9 . . ?
C4 C6 H6 119.9 . . ?
C6 C7 C8 122.3(9) . . ?
C6 C7 H7 118.9 . . ?
C8 C7 H7 118.9 . . ?
C2 C8 C7 116.8(9) . . ?
C2 C8 C9 124.8(9) . . ?
C7 C8 C9 117.8(8) . . ?
C15 C9 C10 118.7(10) . . ?
C15 C9 C8 120.4(10) . . ?
C10 C9 C8 120.6(10) . . ?
C11 C10 C9 117.6(11) . . ?
C11 C10 H10 121.2 . . ?
C9 C10 H10 121.2 . . ?
C12 C11 C10 125.3(10) . . ?
C12 C11 N1 119.2(10) . . ?
C10 C11 N1 115.5(11) . . ?
C11 C12 C14 114.8(9) . . ?
C11 C12 C13 125.7(12) . . ?
C14 C12 C13 119.3(12) . . ?
O6 C13 O5 123.0(11) . . ?
O6 C13 C12 118.5(12) . . ?
O5 C13 C12 118.2(11) . . ?
C15 C14 C12 121.0(12) . . ?
C15 C14 H14 119.5 . . ?
C12 C14 H14 119.5 . . ?
C9 C15 C14 122.5(12) . . ?
C9 C15 H15 118.7 . . ?
C14 C15 H15 118.7 . . ?
N2 C16 C17 120.8(18) . . ?
N2 C16 H16 119.6 . . ?
C17 C16 H16 119.6 . . ?
C18 C17 C16 121(2) . . ?
C18 C17 H17 119.6 . . ?
C16 C17 H17 119.6 . . ?
C17 C18 C19 124(2) . . ?
C17 C18 H18 117.9 . . ?
C19 C18 H18 117.9 . . ?
C18 C19 C20 115.6(19) . . ?
C18 C19 C21 133.8(18) . . ?
C20 C19 C21 110.6(17) . . ?
N2 C20 C19 122.8(15) . . ?
N2 C20 C24 115.2(10) . . ?
C19 C20 C24 122.0(15) . . ?
C22 C21 C19 128.5(18) . . ?
C22 C21 H21 115.7 . . ?
C19 C21 H21 115.7 . . ?
C21 C22 C23 122(2) . . ?
C21 C22 H22 118.9 . . ?
C23 C22 H22 118.9 . . ?
C25 C23 C24 114.8(17) . . ?
C25 C23 C22 128.0(19) . . ?
C24 C23 C22 117.2(18) . . ?
N3 C24 C23 123.6(15) . . ?
N3 C24 C20 117.0(13) . . ?
C23 C24 C20 119.4(13) . . ?
C23 C25 C26 125(2) . . ?
C23 C25 H25 117.7 . . ?
C26 C25 H25 117.7 . . ?
C25 C26 C27 117.4(19) . . ?
C25 C26 H26 121.3 . . ?
C27 C26 H26 121.3 . . ?
N3 C27 C26 121.1(17) . . ?
N3 C27 H27 119.5 . . ?
C26 C27 H27 119.5 . . ?
N4 C28 C29 114.3(19) . . ?
N4 C28 H28 122.8 . . ?
C29 C28 H28 122.8 . . ?
C30 C29 C28 120(2) . . ?
C30 C29 H29 120.1 . . ?
C28 C29 H29 120.2 . . ?
C29 C30 C31 131(3) . . ?
C29 C30 H30 114.6 . . ?
C31 C30 H30 114.6 . . ?
C30 C31 C32 112.7(19) . . ?
C30 C31 C33 134.6(18) . . ?
C32 C31 C33 112.5(15) . . ?
N4 C32 C32 118.2(7) . 2_556 ?
N4 C32 C31 120.5(13) . . ?
C32 C32 C31 121.3(10) 2_556 . ?
C33 C33 C31 126.2(9) 2_556 . ?

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 -0.007 0.006 0.000 221 19 ' '
2 -0.013 0.506 0.000 221 19 ' '
3 0.000 0.973 0.500 9 1 ' '
4 0.500 0.473 0.500 9 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
Zn1 O1 C1 O2 15.2(17) . . . . ?
Zn1 O1 C1 C2 -166.7(6) . . . . ?
O1 C1 C2 C8 37.9(15) . . . . ?
O2 C1 C2 C8 -143.8(11) . . . . ?
O1 C1 C2 C3 -138.9(10) . . . . ?
O2 C1 C2 C3 39.4(15) . . . . ?
C8 C2 C3 C4 1.5(16) . . . . ?
C1 C2 C3 C4 178.3(10) . . . . ?
C2 C3 C4 C6 -4.5(17) . . . . ?
C2 C3 C4 C5 175.2(9) . . . . ?
Zn2 O3 C5 O4 4.6(11) . . . . ?
Zn2 O3 C5 C4 -174.7(8) . . . . ?
Zn2 O4 C5 O3 -4.3(10) . . . . ?
Zn2 O4 C5 C4 175.1(8) . . . . ?
C6 C4 C5 O3 170.0(12) . . . . ?
C3 C4 C5 O3 -9.7(16) . . . . ?
C6 C4 C5 O4 -9.4(16) . . . . ?
C3 C4 C5 O4 171.0(10) . . . . ?
C3 C4 C6 C7 6(2) . . . . ?
C5 C4 C6 C7 -173.6(13) . . . . ?
C4 C6 C7 C8 -5(2) . . . . ?
C3 C2 C8 C7 0.1(17) . . . . ?
C1 C2 C8 C7 -176.7(12) . . . . ?
C3 C2 C8 C9 -170.8(11) . . . . ?
C1 C2 C8 C9 12.4(18) . . . . ?
C6 C7 C8 C2 2(2) . . . . ?
C6 C7 C8 C9 173.1(13) . . . . ?
C2 C8 C9 C15 55.6(17) . . . . ?
C7 C8 C9 C15 -115.2(13) . . . . ?
C2 C8 C9 C10 -130.5(11) . . . . ?
C7 C8 C9 C10 58.7(16) . . . . ?
C15 C9 C10 C11 -0.9(14) . . . . ?
C8 C9 C10 C11 -174.8(9) . . . . ?
C9 C10 C11 C12 3.6(15) . . . . ?
C9 C10 C11 N1 -176.5(9) . . . . ?
O8 N1 C11 C12 120.1(14) . . . . ?
O7 N1 C11 C12 -54.8(17) . . . . ?
O8 N1 C11 C10 -59.9(16) . . . . ?
O7 N1 C11 C10 125.3(14) . . . . ?
C10 C11 C12 C14 -4.8(15) . . . . ?
N1 C11 C12 C14 175.3(9) . . . . ?
C10 C11 C12 C13 169.5(10) . . . . ?
N1 C11 C12 C13 -10.4(16) . . . . ?
Zn1 O5 C13 O6 5(2) 2_757 . . . ?
Zn1 O5 C13 C12 -179.4(10) 2_757 . . . ?
C11 C12 C13 O6 -27(2) . . . . ?
C14 C12 C13 O6 147.4(15) . . . . ?
C11 C12 C13 O5 157.9(13) . . . . ?
C14 C12 C13 O5 -28.1(18) . . . . ?
C11 C12 C14 C15 3.4(15) . . . . ?
C13 C12 C14 C15 -171.2(10) . . . . ?
C10 C9 C15 C14 -0.2(16) . . . . ?
C8 C9 C15 C14 173.7(10) . . . . ?
C12 C14 C15 C9 -1.1(17) . . . . ?
C20 N2 C16 C17 0(2) . . . . ?
Zn1 N2 C16 C17 177.3(11) . . . . ?
N2 C16 C17 C18 -1(3) . . . . ?
C16 C17 C18 C19 2(4) . . . . ?
C17 C18 C19 C20 -2(3) . . . . ?
C17 C18 C19 C21 -179(2) . . . . ?
C16 N2 C20 C19 0.2(19) . . . . ?
Zn1 N2 C20 C19 -177.4(10) . . . . ?
C16 N2 C20 C24 179.6(10) . . . . ?
Zn1 N2 C20 C24 2.0(14) . . . . ?
C18 C19 C20 N2 0(2) . . . . ?
C21 C19 C20 N2 178.5(13) . . . . ?
C18 C19 C20 C24 -178.9(13) . . . . ?
C21 C19 C20 C24 -0.9(19) . . . . ?
C18 C19 C21 C22 175(2) . . . . ?
C20 C19 C21 C22 -3(3) . . . . ?
C19 C21 C22 C23 6(3) . . . . ?
C21 C22 C23 C25 177.2(19) . . . . ?
C21 C22 C23 C24 -5(3) . . . . ?
C27 N3 C24 C23 4.2(18) . . . . ?
Zn1 N3 C24 C23 174.2(11) . . . . ?
C27 N3 C24 C20 -177.8(10) . . . . ?
Zn1 N3 C24 C20 -7.8(12) . . . . ?
C25 C23 C24 N3 -3(2) . . . . ?
C22 C23 C24 N3 178.9(13) . . . . ?
C25 C23 C24 C20 179.4(13) . . . . ?
C22 C23 C24 C20 1(2) . . . . ?
N2 C20 C24 N3 4.1(15) . . . . ?
C19 C20 C24 N3 -176.5(11) . . . . ?
N2 C20 C24 C23 -177.9(12) . . . . ?
C19 C20 C24 C23 1.5(19) . . . . ?
C24 C23 C25 C26 2(3) . . . . ?
C22 C23 C25 C26 -180.0(19) . . . . ?
C23 C25 C26 C27 -2(3) . . . . ?
C24 N3 C27 C26 -5(2) . . . . ?
Zn1 N3 C27 C26 -173.2(13) . . . . ?
C25 C26 C27 N3 4(3) . . . . ?
C32 N4 C28 C29 0.0(19) . . . . ?
Zn2 N4 C28 C29 179.6(11) . . . . ?
N4 C28 C29 C30 3(3) . . . . ?
C28 C29 C30 C31 -7(5) . . . . ?
C29 C30 C31 C32 7(4) . . . . ?
C29 C30 C31 C33 -178(3) . . . . ?
C28 N4 C32 C32 -179.1(14) . . . 2_556 ?
Zn2 N4 C32 C32 1.3(17) . . . 2_556 ?
C28 N4 C32 C31 0.5(18) . . . . ?
Zn2 N4 C32 C31 -179.2(10) . . . . ?
C30 C31 C32 N4 -3(2) . . . . ?
C33 C31 C32 N4 -179.0(12) . . . . ?
C30 C31 C32 C32 176.2(17) . . . 2_556 ?
C33 C31 C32 C32 1(2) . . . 2_556 ?
C30 C31 C33 C33 -174(3) . . . 2_556 ?
C32 C31 C33 C33 0(3) . . . 2_556 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C28 H28 O10 0.93 2.55 3.43(3) 158.2 2_556
C17 H17 O6 0.93 2.27 3.11(2) 149.9 1_554
C16 H16 O9 0.93 2.57 3.09(2) 115.5 .
C10 H10 O8 0.93 2.50 3.408(17) 164.9 2_657
O11 H11B O2 0.85 1.89 2.74(2) 178.8 .
O11 H11A O10 0.85 2.15 3.00(3) 179.0 2_656
O10 H10B O9 0.86 2.45 3.29(2) 165.4 2_656
O10 H10A O5 0.85 2.31 3.16(2) 179.2 1_454
O9 H9B O2 0.85 1.83 2.677(12) 178.5 .
O9 H9B O1 0.85 2.46 2.973(11) 119.7 .
O9 H9A O4 0.85 1.88 2.727(12) 179.0 1_655
C28 H28 O10 0.93 2.55 3.43(3) 158.2 2_556
C17 H17 O6 0.93 2.27 3.11(2) 149.9 1_554
C16 H16 O9 0.93 2.57 3.09(2) 115.5 .
C10 H10 O8 0.93 2.50 3.408(17) 164.9 2_657
O11 H11B O2 0.85 1.89 2.74(2) 178.8 .
O11 H11A O10 0.85 2.15 3.00(3) 179.0 2_656
O10 H10B O9 0.86 2.45 3.29(2) 165.4 2_656
O10 H10A O5 0.85 2.31 3.16(2) 179.2 1_454
O9 H9B O2 0.85 1.83 2.677(12) 178.5 .
O9 H9B O1 0.85 2.46 2.973(11) 119.7 .
O9 H9A O4 0.85 1.88 2.727(12) 179.0 1_655
O9 H9A O4 0.85 1.88 2.727(12) 179.0 1_655
O9 H9B O1 0.85 2.46 2.973(11) 119.7 .
O9 H9B O2 0.85 1.83 2.677(12) 178.5 .
O10 H10A O5 0.85 2.31 3.16(2) 179.2 1_454
O10 H10B O9 0.86 2.45 3.29(2) 165.4 2_656
O11 H11A O10 0.85 2.15 3.00(3) 179.0 2_656
O11 H11B O2 0.85 1.89 2.74(2) 178.8 .
C10 H10 O8 0.93 2.50 3.408(17) 164.9 2_657
C16 H16 O9 0.93 2.57 3.09(2) 115.5 .
C17 H17 O6 0.93 2.27 3.11(2) 149.9 1_554
C28 H28 O10 0.93 2.55 3.43(3) 158.2 2_556
O9 H9A O4 0.85 1.88 2.727(12) 179.0 1_655
O9 H9B O1 0.85 2.46 2.973(11) 119.7 .
O9 H9B O2 0.85 1.83 2.677(12) 178.5 .
O10 H10A O5 0.85 2.31 3.16(2) 179.2 1_454
O10 H10B O9 0.86 2.45 3.29(2) 165.4 2_656
O11 H11A O10 0.85 2.15 3.00(3) 179.0 2_656
O11 H11B O2 0.85 1.89 2.74(2) 178.8 .
C10 H10 O8 0.93 2.50 3.408(17) 164.9 2_657
C16 H16 O9 0.93 2.57 3.09(2) 115.5 .
C17 H17 O6 0.93 2.27 3.11(2) 149.9 1_554
C28 H28 O10 0.93 2.55 3.43(3) 158.2 2_556

_refine_diff_density_max         0.426
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.073

####################################################################### 
# 
# 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_323-4Zn
_database_code_depnum_ccdc_archive 'CCDC 1589525'
_audit_update_record             
;
2017-12-06 deposited with the CCDC.
2018-04-30 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            'C35 H25 N5 O10 Zn2'
_chemical_formula_weight         806.34

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           13
_space_group_name_H-M_alt        'P 2/c'
_space_group_name_Hall           '-P 2yc'

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

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

_cell_length_a                   13.6373(9)
_cell_length_b                   15.8049(11)
_cell_length_c                   16.0311(13)
_cell_angle_alpha                90
_cell_angle_beta                 108.194(8)
_cell_angle_gamma                90
_cell_volume                     3282.5(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    11673
_cell_measurement_theta_min      3.395
_cell_measurement_theta_max      25.050

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_F_000             1640
_exptl_transmission_factor_min   0.727
_exptl_transmission_factor_max   0.771
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.170
_exptl_absorpt_coefficient_mu    1.531
_shelx_estimated_absorpt_T_min   0.701
_shelx_estimated_absorpt_T_max   0.781
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.701
_exptl_absorpt_correction_T_max  0.781
_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            11673
_diffrn_reflns_av_unetI/netI     0.1339
_diffrn_reflns_av_R_equivalents  0.0788
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.395
_diffrn_reflns_theta_max         25.050
_diffrn_reflns_theta_full        25.050
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             5824
_reflns_number_gt                3510
_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)+(0.0660P)²+1.9294P] 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         5824
_refine_ls_number_parameters     469
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1285
_refine_ls_R_factor_gt           0.0751
_refine_ls_wR_factor_ref         0.2019
_refine_ls_wR_factor_gt          0.1551
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.062
_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 0.95089(6) 0.29888(6) 0.32759(5) 0.0247(3) Uani 1 1 d . . . . .
Zn2 Zn 0.83004(6) 0.21354(5) 0.09967(5) 0.0237(3) Uani 1 1 d . . . . .
N1 N 1.1519(6) 0.9452(5) 0.4703(5) 0.0451(19) Uani 1 1 d . . . . .
N2 N 0.8093(5) 0.2730(4) 0.3470(4) 0.0287(15) Uani 1 1 d . . . . .
N3 N 0.3187(5) 0.2196(4) 0.4001(4) 0.0317(16) Uani 1 1 d . . . . .
N4 N 0.4744(9) 0.5072(7) 0.1251(10) 0.137(5) Uani 1 1 d . . . . .
N5 N 0.4844(10) 0.9543(7) 0.1257(8) 0.108(4) Uani 1 1 d . . . . .
O1 O 0.9279(4) 0.4292(3) 0.3222(3) 0.0319(13) Uani 1 1 d . . . . .
O2 O 0.8225(4) 0.4466(3) 0.1865(3) 0.0390(14) Uani 1 1 d . . . . .
O3 O 0.8394(4) 0.7533(3) 0.4849(3) 0.0286(12) Uani 1 1 d . . . . .
O4 O 0.9890(4) 0.6845(3) 0.5348(3) 0.0343(13) Uani 1 1 d . . . . .
O5 O 1.1297(4) 1.0957(3) 0.3806(3) 0.0366(14) Uani 1 1 d . . . . .
O6 O 0.9689(4) 1.1489(4) 0.3474(4) 0.0443(16) Uani 1 1 d . . . . .
O7 O 1.1607(5) 0.9939(5) 0.5300(4) 0.061(2) Uani 1 1 d . . . . .
O8 O 1.2230(5) 0.9063(5) 0.4582(5) 0.081(2) Uani 1 1 d . . . . .
O9 O 0.9056(3) 0.2927(3) 0.1882(3) 0.0218(11) Uani 1 1 d . . . . .
H1 H 0.8793 0.3416 0.1875 0.026 Uiso 1 1 d R U . . .
O10 O 0.8627(6) 0.4926(6) 0.5311(5) 0.107(3) Uani 1 1 d . . . . .
H1W H 0.8505 0.5100 0.5770 0.129 Uiso 1 1 d R U . . .
H2W H 0.8937 0.5394 0.5317 0.129 Uiso 1 1 d R U . . .
C1 C 0.8740(5) 0.4754(5) 0.2593(5) 0.0241(17) Uani 1 1 d . . . . .
C2 C 0.8717(5) 0.5678(5) 0.2781(5) 0.0252(17) Uani 1 1 d . . . . .
C3 C 0.8937(5) 0.5956(5) 0.3634(5) 0.0272(18) Uani 1 1 d . . . . .
H3 H 0.9057 0.5563 0.4087 0.033 Uiso 1 1 calc R U . . .
C4 C 0.8981(5) 0.6821(5) 0.3827(4) 0.0196(16) Uani 1 1 d . . . . .
C5 C 0.9110(6) 0.7087(4) 0.4756(5) 0.0225(16) Uani 1 1 d . . . . .
C6 C 0.8889(5) 0.7413(5) 0.3152(5) 0.0233(17) Uani 1 1 d . . . . .
C7 C 0.8640(6) 0.7123(5) 0.2302(5) 0.0302(18) Uani 1 1 d . . . . .
H7 H 0.8533 0.7511 0.1847 0.036 Uiso 1 1 calc R U . . .
C8 C 0.8544(6) 0.6265(5) 0.2108(5) 0.0298(18) Uani 1 1 d . . . . .
H8A H 0.8365 0.6085 0.1527 0.036 Uiso 1 1 calc R U . . .
C9 C 0.9197(6) 0.8306(5) 0.3355(5) 0.0266(18) Uani 1 1 d . . . . .
C10 C 1.0129(6) 0.8498(5) 0.3952(5) 0.0306(18) Uani 1 1 d . . . . .
H10 H 1.0529 0.8069 0.4288 0.037 Uiso 1 1 calc R U . . .
C11 C 1.0486(5) 0.9323(5) 0.4065(5) 0.0258(17) Uani 1 1 d . . . . .
C12 C 0.9910(6) 1.0000(5) 0.3582(5) 0.0294(18) Uani 1 1 d . . . . .
C13 C 1.0322(6) 1.0885(5) 0.3634(5) 0.0276(18) Uani 1 1 d . . . . .
C14 C 0.8957(6) 0.9795(5) 0.2989(5) 0.0311(19) Uani 1 1 d . . . . .
H14 H 0.8545 1.0223 0.2661 0.037 Uiso 1 1 calc R U . . .
C15 C 0.8609(6) 0.8971(5) 0.2876(5) 0.0287(18) Uani 1 1 d . . . . .
H15 H 0.7967 0.8855 0.2471 0.034 Uiso 1 1 calc R U . . .
C16 C 0.7552(6) 0.2022(5) 0.3237(5) 0.036(2) Uani 1 1 d . . . . .
H16 H 0.7829 0.1602 0.2973 0.043 Uiso 1 1 calc R U . . .
C17 C 0.6618(7) 0.1864(6) 0.3356(6) 0.045(2) Uani 1 1 d . . . . .
H17 H 0.6286 0.1350 0.3180 0.054 Uiso 1 1 calc R U . . .
C18 C 0.6169(6) 0.2474(6) 0.3741(6) 0.037(2) Uani 1 1 d . . . . .
C19 C 0.6752(6) 0.3192(6) 0.4017(6) 0.053(3) Uani 1 1 d . . . . .
H19 H 0.6500 0.3615 0.4299 0.064 Uiso 1 1 calc R U . . .
C20 C 0.7707(7) 0.3308(6) 0.3890(6) 0.050(3) Uani 1 1 d . . . . .
H20 H 0.8083 0.3796 0.4101 0.060 Uiso 1 1 calc R U . . .
C21 C 0.5149(6) 0.2355(6) 0.3852(5) 0.038(2) Uani 1 1 d . . . . .
C22 C 0.4758(6) 0.1582(5) 0.3986(5) 0.035(2) Uani 1 1 d . . . . .
H22 H 0.5154 0.1096 0.4030 0.042 Uiso 1 1 calc R U . . .
C23 C 0.3785(6) 0.1532(5) 0.4056(6) 0.038(2) Uani 1 1 d . . . . .
H23 H 0.3535 0.1003 0.4146 0.046 Uiso 1 1 calc R U . . .
C24 C 0.3552(6) 0.2962(5) 0.3877(6) 0.039(2) Uani 1 1 d . . . . .
H24 H 0.3136 0.3436 0.3842 0.047 Uiso 1 1 calc R U . . .
C25 C 0.4526(6) 0.3063(5) 0.3801(6) 0.044(2) Uani 1 1 d . . . . .
H25 H 0.4763 0.3598 0.3717 0.052 Uiso 1 1 calc R U . . .
C26 C 0.5673(10) 0.6370(8) 0.1483(10) 0.105(5) Uani 1 1 d . . . . .
H26 H 0.6314 0.6633 0.1622 0.126 Uiso 1 1 calc R U . . .
C27 C 0.5608(11) 0.5498(10) 0.1469(12) 0.133(6) Uani 1 1 d . . . . .
H27 H 0.6222 0.5192 0.1626 0.159 Uiso 1 1 calc R U . . .
C28 C 0.3904(10) 0.5540(8) 0.1056(10) 0.111(5) Uani 1 1 d . . . . .
H28 H 0.3271 0.5262 0.0896 0.133 Uiso 1 1 calc R U . . .
C29 C 0.3894(9) 0.6401(8) 0.1072(8) 0.084(4) Uani 1 1 d . . . . .
H29 H 0.3271 0.6693 0.0931 0.100 Uiso 1 1 calc R U . . .
C30 C 0.4814(8) 0.6835(7) 0.1298(7) 0.062(3) Uani 1 1 d . . . . .
C31 C 0.4830(7) 0.7777(7) 0.1304(6) 0.053(3) Uani 1 1 d . . . . .
C32 C 0.4006(8) 0.8256(8) 0.1341(7) 0.067(3) Uani 1 1 d . . . . .
H32 H 0.3412 0.7987 0.1373 0.081 Uiso 1 1 calc R U . . .
C33 C 0.4035(10) 0.9108(9) 0.1332(8) 0.085(4) Uani 1 1 d . . . . .
H33 H 0.3467 0.9406 0.1380 0.101 Uiso 1 1 calc R U . . .
C34 C 0.5630(11) 0.9082(11) 0.1208(10) 0.110(5) Uani 1 1 d . . . . .
H34 H 0.6209 0.9365 0.1163 0.131 Uiso 1 1 calc R U . . .
C35 C 0.5655(9) 0.8218(9) 0.1220(7) 0.081(4) Uani 1 1 d . . . . .
H35 H 0.6231 0.7931 0.1171 0.097 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O9 2.053(4) 2_755 ?
Zn1 O1 2.080(5) . ?
Zn1 N2 2.090(6) . ?
Zn1 O4 2.116(5) 3_766 ?
Zn1 O9 2.127(4) . ?
Zn1 O6 2.393(6) 1_545 ?
Zn1 Zn2 3.1511(12) 2_755 ?
Zn2 O9 1.931(5) . ?
Zn2 O5 1.940(5) 2_745 ?
Zn2 O3 1.955(5) 4_565 ?
Zn2 N3 2.032(6) 2_655 ?
Zn2 Zn1 3.1511(12) 2_755 ?
N1 O7 1.205(9) . ?
N1 O8 1.213(9) . ?
N1 C11 1.473(10) . ?
N2 C16 1.328(9) . ?
N2 C20 1.336(9) . ?
N3 C23 1.315(9) . ?
N3 C24 1.348(10) . ?
N3 Zn2 2.032(6) 2_655 ?
N4 C27 1.307(16) . ?
N4 C28 1.317(15) . ?
N5 C34 1.319(17) . ?
N5 C33 1.337(15) . ?
O1 C1 1.277(9) . ?
O2 C1 1.245(8) . ?
O3 C5 1.250(8) . ?
O3 Zn2 1.955(5) 4_566 ?
O4 C5 1.245(9) . ?
O4 Zn1 2.116(5) 3_766 ?
O5 C13 1.277(8) . ?
O5 Zn2 1.940(5) 2_765 ?
O6 C13 1.259(9) . ?
O6 Zn1 2.393(6) 1_565 ?
O9 Zn1 2.053(4) 2_755 ?
O9 H1 0.8500 . ?
O10 H1W 0.8501 . ?
O10 H2W 0.8499 . ?
C1 C2 1.493(10) . ?
C2 C3 1.377(9) . ?
C2 C8 1.386(10) . ?
C3 C4 1.400(9) . ?
C3 H3 0.9300 . ?
C4 C6 1.406(10) . ?
C4 C5 1.504(9) . ?
C6 C7 1.376(10) . ?
C6 C9 1.479(9) . ?
C7 C8 1.388(10) . ?
C7 H7 0.9300 . ?
C8 H8A 0.9300 . ?
C9 C10 1.366(10) . ?
C9 C15 1.397(10) . ?
C10 C11 1.383(10) . ?
C10 H10 0.9300 . ?
C11 C12 1.408(10) . ?
C12 C14 1.388(11) . ?
C12 C13 1.500(10) . ?
C14 C15 1.380(10) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C17 1.369(10) . ?
C16 H16 0.9300 . ?
C17 C18 1.387(11) . ?
C17 H17 0.9300 . ?
C18 C19 1.377(12) . ?
C18 C21 1.468(10) . ?
C19 C20 1.391(10) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
C21 C22 1.376(11) . ?
C21 C25 1.392(11) . ?
C22 C23 1.368(10) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 C25 1.381(10) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
C26 C30 1.336(14) . ?
C26 C27 1.381(17) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
C28 C29 1.361(15) . ?
C28 H28 0.9300 . ?
C29 C30 1.376(14) . ?
C29 H29 0.9300 . ?
C30 C31 1.489(14) . ?
C31 C35 1.365(14) . ?
C31 C32 1.372(14) . ?
C32 C33 1.347(15) . ?
C32 H32 0.9300 . ?
C33 H33 0.9300 . ?
C34 C35 1.366(18) . ?
C34 H34 0.9300 . ?
C35 H35 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
O9 Zn1 O1 100.31(19) 2_755 . ?
O9 Zn1 N2 165.9(2) 2_755 . ?
O1 Zn1 N2 93.8(2) . . ?
O9 Zn1 O4 93.48(18) 2_755 3_766 ?
O1 Zn1 O4 85.7(2) . 3_766 ?
N2 Zn1 O4 86.8(2) . 3_766 ?
O9 Zn1 O9 81.01(19) 2_755 . ?
O1 Zn1 O9 90.65(18) . . ?
N2 Zn1 O9 99.7(2) . . ?
O4 Zn1 O9 172.74(19) 3_766 . ?
O9 Zn1 O6 84.67(17) 2_755 1_545 ?
O1 Zn1 O6 173.36(18) . 1_545 ?
N2 Zn1 O6 81.2(2) . 1_545 ?
O4 Zn1 O6 89.7(2) 3_766 1_545 ?
O9 Zn1 O6 94.48(19) . 1_545 ?
O9 Zn1 Zn2 36.38(12) 2_755 2_755 ?
O1 Zn1 Zn2 123.50(15) . 2_755 ?
N2 Zn1 Zn2 132.42(18) . 2_755 ?
O4 Zn1 Zn2 69.75(14) 3_766 2_755 ?
O9 Zn1 Zn2 107.46(12) . 2_755 ?
O6 Zn1 Zn2 58.74(13) 1_545 2_755 ?
O9 Zn2 O5 116.4(2) . 2_745 ?
O9 Zn2 O3 110.0(2) . 4_565 ?
O5 Zn2 O3 108.2(2) 2_745 4_565 ?
O9 Zn2 N3 105.8(2) . 2_655 ?
O5 Zn2 N3 106.1(2) 2_745 2_655 ?
O3 Zn2 N3 110.3(2) 4_565 2_655 ?
O9 Zn2 Zn1 39.10(13) . 2_755 ?
O5 Zn2 Zn1 99.42(16) 2_745 2_755 ?
O3 Zn2 Zn1 84.31(15) 4_565 2_755 ?
N3 Zn2 Zn1 144.20(19) 2_655 2_755 ?
O7 N1 O8 124.3(8) . . ?
O7 N1 C11 118.5(8) . . ?
O8 N1 C11 117.2(7) . . ?
C16 N2 C20 116.5(6) . . ?
C16 N2 Zn1 125.5(5) . . ?
C20 N2 Zn1 118.0(5) . . ?
C23 N3 C24 118.5(7) . . ?
C23 N3 Zn2 124.1(5) . 2_655 ?
C24 N3 Zn2 117.2(5) . 2_655 ?
C27 N4 C28 114.8(12) . . ?
C34 N5 C33 115.5(12) . . ?
C1 O1 Zn1 129.9(5) . . ?
C5 O3 Zn2 123.1(5) . 4_566 ?
C5 O4 Zn1 135.8(5) . 3_766 ?
C13 O5 Zn2 110.1(5) . 2_765 ?
C13 O6 Zn1 144.4(5) . 1_565 ?
Zn2 O9 Zn1 104.52(19) . 2_755 ?
Zn2 O9 Zn1 135.7(2) . . ?
Zn1 O9 Zn1 98.74(19) 2_755 . ?
Zn2 O9 H1 116.9 . . ?
Zn1 O9 H1 111.7 2_755 . ?
Zn1 O9 H1 87.5 . . ?
H1W O10 H2W 86.7 . . ?
O2 C1 O1 123.2(7) . . ?
O2 C1 C2 120.4(7) . . ?
O1 C1 C2 116.4(7) . . ?
C3 C2 C8 119.4(7) . . ?
C3 C2 C1 120.0(7) . . ?
C8 C2 C1 120.4(7) . . ?
C2 C3 C4 120.9(7) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 H3 119.6 . . ?
C3 C4 C6 119.5(6) . . ?
C3 C4 C5 118.5(6) . . ?
C6 C4 C5 122.1(6) . . ?
O4 C5 O3 126.7(7) . . ?
O4 C5 C4 118.4(6) . . ?
O3 C5 C4 114.9(6) . . ?
C7 C6 C4 118.4(7) . . ?
C7 C6 C9 120.0(6) . . ?
C4 C6 C9 121.0(6) . . ?
C6 C7 C8 121.6(7) . . ?
C6 C7 H7 119.2 . . ?
C8 C7 H7 119.2 . . ?
C2 C8 C7 119.8(7) . . ?
C2 C8 H8A 120.1 . . ?
C7 C8 H8A 120.1 . . ?
C10 C9 C15 117.8(7) . . ?
C10 C9 C6 120.3(7) . . ?
C15 C9 C6 121.5(7) . . ?
C9 C10 C11 121.0(7) . . ?
C9 C10 H10 119.5 . . ?
C11 C10 H10 119.5 . . ?
C10 C11 C12 122.0(7) . . ?
C10 C11 N1 116.3(7) . . ?
C12 C11 N1 121.6(7) . . ?
C14 C12 C11 116.2(7) . . ?
C14 C12 C13 120.6(8) . . ?
C11 C12 C13 122.9(7) . . ?
O6 C13 O5 125.4(7) . . ?
O6 C13 C12 118.4(7) . . ?
O5 C13 C12 116.2(7) . . ?
C15 C14 C12 121.3(8) . . ?
C15 C14 H14 119.3 . . ?
C12 C14 H14 119.3 . . ?
C14 C15 C9 121.6(7) . . ?
C14 C15 H15 119.2 . . ?
C9 C15 H15 119.2 . . ?
N2 C16 C17 125.1(8) . . ?
N2 C16 H16 117.5 . . ?
C17 C16 H16 117.5 . . ?
C16 C17 C18 119.6(9) . . ?
C16 C17 H17 120.2 . . ?
C18 C17 H17 120.2 . . ?
C19 C18 C17 115.2(7) . . ?
C19 C18 C21 122.8(8) . . ?
C17 C18 C21 122.1(8) . . ?
C18 C19 C20 122.3(8) . . ?
C18 C19 H19 118.9 . . ?
C20 C19 H19 118.9 . . ?
N2 C20 C19 121.2(8) . . ?
N2 C20 H20 119.4 . . ?
C19 C20 H20 119.4 . . ?
C22 C21 C25 117.6(7) . . ?
C22 C21 C18 124.2(8) . . ?
C25 C21 C18 118.3(8) . . ?
C23 C22 C21 119.9(8) . . ?
C23 C22 H22 120.1 . . ?
C21 C22 H22 120.1 . . ?
N3 C23 C22 123.0(8) . . ?
N3 C23 H23 118.5 . . ?
C22 C23 H23 118.5 . . ?
N3 C24 C25 121.8(8) . . ?
N3 C24 H24 119.1 . . ?
C25 C24 H24 119.1 . . ?
C24 C25 C21 119.3(8) . . ?
C24 C25 H25 120.4 . . ?
C21 C25 H25 120.4 . . ?
C30 C26 C27 119.9(12) . . ?
C30 C26 H26 120.1 . . ?
C27 C26 H26 120.1 . . ?
N4 C27 C26 124.5(12) . . ?
N4 C27 H27 117.8 . . ?
C26 C27 H27 117.8 . . ?
N4 C28 C29 124.8(12) . . ?
N4 C28 H28 117.6 . . ?
C29 C28 H28 117.6 . . ?
C28 C29 C30 119.4(11) . . ?
C28 C29 H29 120.3 . . ?
C30 C29 H29 120.3 . . ?
C26 C30 C29 116.6(11) . . ?
C26 C30 C31 122.6(10) . . ?
C29 C30 C31 120.7(10) . . ?
C35 C31 C32 115.8(11) . . ?
C35 C31 C30 121.3(10) . . ?
C32 C31 C30 122.8(10) . . ?
C33 C32 C31 121.6(11) . . ?
C33 C32 H32 119.2 . . ?
C31 C32 H32 119.2 . . ?
N5 C33 C32 122.9(12) . . ?
N5 C33 H33 118.6 . . ?
C32 C33 H33 118.6 . . ?
N5 C34 C35 124.7(13) . . ?
N5 C34 H34 117.7 . . ?
C35 C34 H34 117.7 . . ?
C34 C35 C31 119.5(12) . . ?
C34 C35 H35 120.2 . . ?
C31 C35 H35 120.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Zn1 O1 C1 O2 0.8(10) . . . . ?
Zn1 O1 C1 C2 178.4(4) . . . . ?
O2 C1 C2 C3 155.2(7) . . . . ?
O1 C1 C2 C3 -22.3(9) . . . . ?
O2 C1 C2 C8 -29.2(10) . . . . ?
O1 C1 C2 C8 153.2(7) . . . . ?
C8 C2 C3 C4 0.4(11) . . . . ?
C1 C2 C3 C4 176.0(6) . . . . ?
C2 C3 C4 C6 -5.6(10) . . . . ?
C2 C3 C4 C5 173.4(6) . . . . ?
Zn1 O4 C5 O3 -1.5(12) 3_766 . . . ?
Zn1 O4 C5 C4 179.3(5) 3_766 . . . ?
Zn2 O3 C5 O4 -5.8(10) 4_566 . . . ?
Zn2 O3 C5 C4 173.5(4) 4_566 . . . ?
C3 C4 C5 O4 59.6(9) . . . . ?
C6 C4 C5 O4 -121.4(8) . . . . ?
C3 C4 C5 O3 -119.7(7) . . . . ?
C6 C4 C5 O3 59.3(9) . . . . ?
C3 C4 C6 C7 7.3(10) . . . . ?
C5 C4 C6 C7 -171.7(6) . . . . ?
C3 C4 C6 C9 -164.0(7) . . . . ?
C5 C4 C6 C9 17.0(10) . . . . ?
C4 C6 C7 C8 -4.1(11) . . . . ?
C9 C6 C7 C8 167.2(7) . . . . ?
C3 C2 C8 C7 2.9(11) . . . . ?
C1 C2 C8 C7 -172.7(7) . . . . ?
C6 C7 C8 C2 -1.0(12) . . . . ?
C7 C6 C9 C10 -122.7(8) . . . . ?
C4 C6 C9 C10 48.4(10) . . . . ?
C7 C6 C9 C15 49.8(10) . . . . ?
C4 C6 C9 C15 -139.1(7) . . . . ?
C15 C9 C10 C11 -1.3(10) . . . . ?
C6 C9 C10 C11 171.5(6) . . . . ?
C9 C10 C11 C12 0.6(11) . . . . ?
C9 C10 C11 N1 -177.7(7) . . . . ?
O7 N1 C11 C10 -123.8(8) . . . . ?
O8 N1 C11 C10 57.0(10) . . . . ?
O7 N1 C11 C12 57.8(11) . . . . ?
O8 N1 C11 C12 -121.3(9) . . . . ?
C10 C11 C12 C14 0.5(10) . . . . ?
N1 C11 C12 C14 178.7(7) . . . . ?
C10 C11 C12 C13 -174.3(6) . . . . ?
N1 C11 C12 C13 3.9(10) . . . . ?
Zn1 O6 C13 O5 3.4(13) 1_565 . . . ?
Zn1 O6 C13 C12 -173.5(5) 1_565 . . . ?
Zn2 O5 C13 O6 10.7(9) 2_765 . . . ?
Zn2 O5 C13 C12 -172.3(5) 2_765 . . . ?
C14 C12 C13 O6 32.1(10) . . . . ?
C11 C12 C13 O6 -153.3(7) . . . . ?
C14 C12 C13 O5 -145.2(7) . . . . ?
C11 C12 C13 O5 29.5(10) . . . . ?
C11 C12 C14 C15 -0.9(10) . . . . ?
C13 C12 C14 C15 174.1(6) . . . . ?
C12 C14 C15 C9 0.2(11) . . . . ?
C10 C9 C15 C14 0.9(10) . . . . ?
C6 C9 C15 C14 -171.8(6) . . . . ?
C20 N2 C16 C17 3.4(13) . . . . ?
Zn1 N2 C16 C17 -179.1(6) . . . . ?
N2 C16 C17 C18 0.5(14) . . . . ?
C16 C17 C18 C19 -3.2(13) . . . . ?
C16 C17 C18 C21 177.3(8) . . . . ?
C17 C18 C19 C20 2.2(14) . . . . ?
C21 C18 C19 C20 -178.4(9) . . . . ?
C16 N2 C20 C19 -4.4(13) . . . . ?
Zn1 N2 C20 C19 177.9(7) . . . . ?
C18 C19 C20 N2 1.7(15) . . . . ?
C19 C18 C21 C22 -148.0(9) . . . . ?
C17 C18 C21 C22 31.3(13) . . . . ?
C19 C18 C21 C25 33.3(13) . . . . ?
C17 C18 C21 C25 -147.3(9) . . . . ?
C25 C21 C22 C23 0.6(13) . . . . ?
C18 C21 C22 C23 -178.0(8) . . . . ?
C24 N3 C23 C22 -0.5(12) . . . . ?
Zn2 N3 C23 C22 174.9(6) 2_655 . . . ?
C21 C22 C23 N3 -0.1(13) . . . . ?
C23 N3 C24 C25 0.4(12) . . . . ?
Zn2 N3 C24 C25 -175.2(7) 2_655 . . . ?
N3 C24 C25 C21 0.1(13) . . . . ?
C22 C21 C25 C24 -0.6(13) . . . . ?
C18 C21 C25 C24 178.1(8) . . . . ?
C28 N4 C27 C26 -2(3) . . . . ?
C30 C26 C27 N4 3(3) . . . . ?
C27 N4 C28 C29 0(3) . . . . ?
N4 C28 C29 C30 1(2) . . . . ?
C27 C26 C30 C29 -2(2) . . . . ?
C27 C26 C30 C31 179.8(13) . . . . ?
C28 C29 C30 C26 0.6(19) . . . . ?
C28 C29 C30 C31 178.8(12) . . . . ?
C26 C30 C31 C35 21.3(16) . . . . ?
C29 C30 C31 C35 -156.8(11) . . . . ?
C26 C30 C31 C32 -162.7(12) . . . . ?
C29 C30 C31 C32 19.3(15) . . . . ?
C35 C31 C32 C33 -2.7(15) . . . . ?
C30 C31 C32 C33 -179.0(10) . . . . ?
C34 N5 C33 C32 -1.2(19) . . . . ?
C31 C32 C33 N5 2.3(19) . . . . ?
C33 N5 C34 C35 1(2) . . . . ?
N5 C34 C35 C31 -1(2) . . . . ?
C32 C31 C35 C34 2.2(16) . . . . ?
C30 C31 C35 C34 178.5(10) . . . . ?

_refine_diff_density_max         2.535
_refine_diff_density_min         -0.847
_refine_diff_density_rms         0.134

####################################################################### 
# 
# 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_317-15Ni
_database_code_depnum_ccdc_archive 'CCDC 1589522'
_audit_update_record             
;
2017-12-06 deposited with the CCDC.
2018-04-30 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            'C55 H40 N7 Ni3 O20'
_chemical_formula_weight         1295.07

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      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                   13.4144(9)
_cell_length_b                   16.2982(14)
_cell_length_c                   17.8894(13)
_cell_angle_alpha                113.460(8)
_cell_angle_beta                 104.921(6)
_cell_angle_gamma                96.805(6)
_cell_volume                     3357.4(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    22407
_cell_measurement_theta_min      3.242
_cell_measurement_theta_max      25.050

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_F_000             1326
_exptl_transmission_factor_min   0.823
_exptl_transmission_factor_max   0.865
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.160
_exptl_absorpt_coefficient_mu    0.903
_shelx_estimated_absorpt_T_min   0.819
_shelx_estimated_absorpt_T_max   0.869
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.819
_exptl_absorpt_correction_T_max  0.869
_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            22407
_diffrn_reflns_av_unetI/netI     0.2136
_diffrn_reflns_av_R_equivalents  0.0980
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.242
_diffrn_reflns_theta_max         25.050
_diffrn_reflns_theta_full        25.050
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             11909
_reflns_number_gt                5372
_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)+(0.0569P)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         11909
_refine_ls_number_parameters     766
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.1455
_refine_ls_R_factor_gt           0.0764
_refine_ls_wR_factor_ref         0.2026
_refine_ls_wR_factor_gt          0.1659
_refine_ls_goodness_of_fit_ref   0.895
_refine_ls_restrained_S_all      0.900
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.41022(7) 0.76422(5) 0.29674(5) 0.0254(3) Uani 1 1 d . . . . .
Ni2 Ni 0.61827(7) 0.76728(6) 0.23822(5) 0.0275(3) Uani 1 1 d . . . . .
Ni3 Ni 1.16683(7) 0.78735(6) 0.69436(6) 0.0299(3) Uani 1 1 d . . . . .
N1 N 0.3557(7) 1.0374(5) -0.0329(5) 0.062(2) Uani 1 1 d . . . . .
N2 N 0.8721(6) 0.6227(7) 0.4586(5) 0.070(3) Uani 1 1 d . . . . .
N3 N 0.7536(4) 0.8487(4) 0.3444(4) 0.0347(16) Uani 1 1 d . . . . .
N4 N 1.0799(4) 0.8875(4) 0.7081(4) 0.0341(16) Uani 1 1 d . . . . .
N5 N 0.7179(4) 1.1721(4) 0.7025(3) 0.0303(16) Uani 1 1 d . . . . .
N6 N 1.0515(5) 0.6959(4) 0.7040(4) 0.0361(16) Uani 1 1 d . . . . .
N7 N 0.6792(5) 0.3492(4) 0.7003(4) 0.0368(16) Uani 1 1 d . . . . .
O1 O 0.5977(4) 0.9603(3) 0.2425(3) 0.0414(14) Uani 1 1 d . . . . .
O2 O 0.5241(3) 0.8624(3) 0.2813(3) 0.0247(11) Uani 1 1 d . . . . .
O3 O 0.3923(4) 1.2222(4) 0.5388(3) 0.0624(19) Uani 1 1 d . . . . .
O4 O 0.5274(3) 1.1611(3) 0.5706(3) 0.0265(11) Uani 1 1 d . . . . .
O5 O 0.2387(4) 0.8529(3) -0.1734(3) 0.0362(13) Uani 1 1 d . . . . .
O6 O 0.3514(7) 0.7695(5) -0.1525(4) 0.122(4) Uani 1 1 d . . . . .
O7 O 0.3127(10) 1.0960(7) -0.0164(6) 0.172(5) Uani 1 1 d . . . . .
O8 O 0.4002(5) 1.0245(5) -0.0832(4) 0.079(2) Uani 1 1 d . . . . .
O9 O 0.6922(3) 0.6618(3) 0.2001(3) 0.0291(12) Uani 1 1 d . . . . .
O10 O 0.5769(4) 0.5503(3) 0.2004(3) 0.0468(16) Uani 1 1 d . . . . .
O11 O 0.5044(3) 0.3133(3) -0.1253(3) 0.0299(12) Uani 1 1 d . . . . .
O12 O 0.6478(3) 0.2982(3) -0.1662(3) 0.0276(12) Uani 1 1 d . . . . .
O13 O 1.1724(5) 0.7989(4) 0.5091(3) 0.0609(18) Uani 1 1 d . . . . .
O14 O 1.0847(4) 0.7200(3) 0.5594(3) 0.0366(13) Uani 1 1 d . . . . .
O15 O 0.8390(5) 0.6892(6) 0.4942(4) 0.104(3) Uani 1 1 d . . . . .
O16 O 0.8695(8) 0.5513(6) 0.4669(6) 0.126(4) Uani 1 1 d . . . . .
O17 O 0.6814(4) 0.8238(3) 0.1696(3) 0.0453(15) Uani 1 1 d . . . . .
H1W H 0.6454 0.7962 0.1182 0.054 Uiso 1 1 d R U . . .
H2W H 0.6545 0.8679 0.1932 0.054 Uiso 1 1 d R U . . .
O18 O 0.5430(3) 0.7082(3) 0.2999(3) 0.0314(12) Uani 1 1 d . . . . .
H3W H 0.5537 0.6576 0.2679 0.038 Uiso 1 1 d R U . . .
H4W H 0.5647 0.7321 0.3548 0.038 Uiso 1 1 d R U . . .
O19 O 1.2849(4) 0.8579(3) 0.6734(3) 0.0459(15) Uani 1 1 d . . . . .
H5W H 1.2484 0.8388 0.6206 0.055 Uiso 1 1 d R U . . .
H6W H 1.3208 0.9138 0.6992 0.055 Uiso 1 1 d R U . . .
O20 O 1.2550(4) 0.6861(3) 0.6783(3) 0.0494(15) Uani 1 1 d . . . . .
H7W H 1.3045 0.7018 0.7232 0.059 Uiso 1 1 d R U . . .
H8W H 1.2063 0.6959 0.6442 0.059 Uiso 1 1 d R U . . .
C1 C 0.5325(5) 0.9378(5) 0.2722(4) 0.0255(17) Uani 1 1 d . . . . .
C2 C 0.4672(5) 1.0020(4) 0.3017(4) 0.0279(18) Uani 1 1 d . . . . .
C3 C 0.4839(6) 1.0494(4) 0.3911(4) 0.0338(19) Uani 1 1 d . . . . .
H3 H 0.5279 1.0329 0.4294 0.041 Uiso 1 1 calc R U . . .
C4 C 0.4349(6) 1.1211(4) 0.4226(4) 0.034(2) Uani 1 1 d . . . . .
C5 C 0.4522(6) 1.1709(5) 0.5187(4) 0.0322(19) Uani 1 1 d . . . . .
C6 C 0.3669(6) 1.1420(4) 0.3642(4) 0.0340(19) Uani 1 1 d . . . . .
H6 H 0.3338 1.1894 0.3844 0.041 Uiso 1 1 calc R U . . .
C7 C 0.3473(6) 1.0948(5) 0.2779(4) 0.037(2) Uani 1 1 d . . . . .
H7 H 0.2996 1.1093 0.2399 0.045 Uiso 1 1 calc R U . . .
C8 C 0.3977(5) 1.0248(5) 0.2449(4) 0.0319(19) Uani 1 1 d . . . . .
C9 C 0.3771(5) 0.9780(5) 0.1504(4) 0.0322(18) Uani 1 1 d . . . . .
C10 C 0.3735(6) 1.0277(6) 0.1023(5) 0.048(2) Uani 1 1 d . . . . .
H10 H 0.3823 1.0914 0.1286 0.058 Uiso 1 1 calc R U . . .
C11 C 0.3562(6) 0.9800(6) 0.0135(5) 0.044(2) Uani 1 1 d . . . . .
C12 C 0.3399(6) 0.8875(6) -0.0300(5) 0.045(2) Uani 1 1 d . . . . .
C13 C 0.3093(7) 0.8328(6) -0.1259(5) 0.059(3) Uani 1 1 d . . . . .
C14 C 0.3463(6) 0.8399(5) 0.0186(5) 0.048(2) Uani 1 1 d . . . . .
H14 H 0.3391 0.7765 -0.0083 0.058 Uiso 1 1 calc R U . . .
C15 C 0.3631(6) 0.8833(5) 0.1066(5) 0.047(2) Uani 1 1 d . . . . .
H15 H 0.3651 0.8482 0.1369 0.057 Uiso 1 1 calc R U . . .
C16 C 0.6524(6) 0.5789(5) 0.1799(4) 0.036(2) Uani 1 1 d . . . . .
C17 C 0.6970(5) 0.5085(4) 0.1225(4) 0.0298(18) Uani 1 1 d . . . . .
C18 C 0.6351(5) 0.4476(4) 0.0402(4) 0.0320(19) Uani 1 1 d . . . . .
H18 H 0.5624 0.4439 0.0239 0.038 Uiso 1 1 calc R U . . .
C19 C 0.6737(5) 0.3912(4) -0.0201(4) 0.0266(18) Uani 1 1 d . . . . .
C20 C 0.6028(5) 0.3290(4) -0.1120(4) 0.0203(15) Uani 1 1 d . . . . .
C21 C 0.7797(5) 0.3934(5) 0.0051(5) 0.038(2) Uani 1 1 d . . . . .
H21 H 0.8076 0.3557 -0.0346 0.045 Uiso 1 1 calc R U . . .
C22 C 0.8461(5) 0.4514(5) 0.0892(4) 0.038(2) Uani 1 1 d . . . . .
H22 H 0.9177 0.4511 0.1056 0.046 Uiso 1 1 calc R U . . .
C23 C 0.8067(5) 0.5100(5) 0.1491(4) 0.035(2) Uani 1 1 d . . . . .
C24 C 0.8778(5) 0.5715(5) 0.2401(4) 0.0323(19) Uani 1 1 d . . . . .
C25 C 0.8495(6) 0.5724(5) 0.3088(4) 0.039(2) Uani 1 1 d . . . . .
H25 H 0.7844 0.5360 0.2994 0.047 Uiso 1 1 calc R U . . .
C26 C 0.9171(6) 0.6265(5) 0.3904(5) 0.039(2) Uani 1 1 d . . . . .
C27 C 1.0174(5) 0.6826(4) 0.4104(4) 0.034(2) Uani 1 1 d . . . . .
C28 C 1.0970(6) 0.7409(5) 0.5010(5) 0.0325(19) Uani 1 1 d . . . . .
C29 C 1.0453(6) 0.6804(5) 0.3399(5) 0.041(2) Uani 1 1 d . . . . .
H29 H 1.1112 0.7154 0.3490 0.049 Uiso 1 1 calc R U . . .
C30 C 0.9760(6) 0.6266(5) 0.2564(5) 0.044(2) Uani 1 1 d . . . . .
H30 H 0.9954 0.6272 0.2103 0.053 Uiso 1 1 calc R U . . .
C31 C 0.7667(6) 0.9390(5) 0.3915(6) 0.081(4) Uani 1 1 d . . . . .
H31 H 0.7078 0.9632 0.3823 0.097 Uiso 1 1 calc R U . . .
C32 C 0.8592(6) 0.9979(5) 0.4515(6) 0.066(3) Uani 1 1 d . . . . .
H32 H 0.8609 1.0596 0.4825 0.080 Uiso 1 1 calc R U . . .
C33 C 0.9479(5) 0.9697(4) 0.4674(4) 0.0296(18) Uani 1 1 d . U . . .
C34 C 0.9381(7) 0.8784(5) 0.4189(6) 0.083(4) Uani 1 1 d . U . . .
H34 H 0.9972 0.8544 0.4274 0.099 Uiso 1 1 calc R U . . .
C35 C 0.8408(7) 0.8196(5) 0.3565(6) 0.073(3) Uani 1 1 d . U . . .
H35 H 0.8380 0.7582 0.3227 0.087 Uiso 1 1 calc R U . . .
C36 C 1.1139(6) 0.9780(4) 0.7562(5) 0.040(2) Uani 1 1 d . . . . .
H36 H 1.1852 1.0011 0.7910 0.048 Uiso 1 1 calc R U . . .
C37 C 1.0531(6) 1.0410(5) 0.7593(5) 0.042(2) Uani 1 1 d . . . . .
H37 H 1.0828 1.1037 0.7953 0.051 Uiso 1 1 calc R U . . .
C38 C 0.9473(5) 1.0090(5) 0.7079(5) 0.0332(19) Uani 1 1 d . . . . .
C39 C 0.9093(6) 0.9138(5) 0.6553(6) 0.056(3) Uani 1 1 d . . . . .
H39 H 0.8385 0.8887 0.6197 0.067 Uiso 1 1 calc R U . . .
C40 C 0.9779(6) 0.8583(5) 0.6571(6) 0.055(3) Uani 1 1 d . . . . .
H40 H 0.9516 0.7955 0.6200 0.066 Uiso 1 1 calc R U . . .
C41 C 0.8751(5) 1.0713(5) 0.7065(5) 0.0338(19) Uani 1 1 d . . . . .
C42 C 0.8837(6) 1.1514(5) 0.7761(5) 0.049(2) Uani 1 1 d . . . . .
H42 H 0.9427 1.1741 0.8261 0.059 Uiso 1 1 calc R U . . .
C43 C 0.8059(6) 1.1984(5) 0.7726(5) 0.053(3) Uani 1 1 d . . . . .
H43 H 0.8139 1.2520 0.8217 0.063 Uiso 1 1 calc R U . . .
C44 C 0.7134(6) 1.0988(5) 0.6337(5) 0.046(2) Uani 1 1 d . . . . .
H44 H 0.6568 1.0811 0.5832 0.055 Uiso 1 1 calc R U . . .
C45 C 0.7880(6) 1.0452(5) 0.6312(5) 0.045(2) Uani 1 1 d . . . . .
H45 H 0.7800 0.9934 0.5805 0.054 Uiso 1 1 calc R U . . .
C46 C 1.0095(8) 0.7184(6) 0.7634(6) 0.079(4) Uani 1 1 d . . . . .
H46 H 1.0315 0.7793 0.8061 0.094 Uiso 1 1 calc R U . . .
C47 C 0.9324(8) 0.6569(6) 0.7677(6) 0.080(4) Uani 1 1 d . . . . .
H47 H 0.9056 0.6764 0.8133 0.096 Uiso 1 1 calc R U . . .
C48 C 0.8952(6) 0.5649(5) 0.7027(5) 0.042(2) Uani 1 1 d . . . . .
C49 C 0.9442(6) 0.5431(5) 0.6394(5) 0.042(2) Uani 1 1 d . . . . .
H49 H 0.9252 0.4831 0.5955 0.051 Uiso 1 1 calc R U . . .
C50 C 1.0200(6) 0.6092(5) 0.6412(5) 0.044(2) Uani 1 1 d . . . . .
H50 H 1.0502 0.5931 0.5976 0.053 Uiso 1 1 calc R U . . .
C51 C 0.8158(6) 0.4943(5) 0.7023(5) 0.044(2) Uani 1 1 d . . . . .
C52 C 0.8084(7) 0.4941(6) 0.7765(6) 0.067(3) Uani 1 1 d . . . . .
H52 H 0.8504 0.5431 0.8292 0.081 Uiso 1 1 calc R U . . .
C53 C 0.7394(7) 0.4223(5) 0.7760(6) 0.067(3) Uani 1 1 d . . . . .
H53 H 0.7348 0.4249 0.8278 0.081 Uiso 1 1 calc R U . . .
C54 C 0.6860(6) 0.3499(5) 0.6287(5) 0.046(2) Uani 1 1 d . . . . .
H54 H 0.6443 0.2999 0.5766 0.055 Uiso 1 1 calc R U . . .
C55 C 0.7513(6) 0.4200(6) 0.6254(6) 0.054(2) Uani 1 1 d . . . . .
H55 H 0.7517 0.4173 0.5725 0.065 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O12 2.019(4) 2_665 ?
Ni1 O4 2.061(4) 2_676 ?
Ni1 O18 2.094(4) . ?
Ni1 N7 2.107(6) 2_666 ?
Ni1 N5 2.111(5) 2_676 ?
Ni1 O2 2.227(5) . ?
Ni2 O11 2.044(4) 2_665 ?
Ni2 O9 2.056(4) . ?
Ni2 N3 2.076(5) . ?
Ni2 O17 2.080(5) . ?
Ni2 O18 2.087(5) . ?
Ni2 O2 2.147(4) . ?
Ni3 O19 2.046(5) . ?
Ni3 O5 2.058(5) 1_656 ?
Ni3 N4 2.089(6) . ?
Ni3 N6 2.106(6) . ?
Ni3 O20 2.114(5) . ?
Ni3 O14 2.117(5) . ?
Ni3 H8W 1.6357 . ?
N1 O7 1.151(9) . ?
N1 O8 1.168(9) . ?
N1 C11 1.475(11) . ?
N2 O15 1.220(10) . ?
N2 O16 1.229(11) . ?
N2 C26 1.513(11) . ?
N3 C35 1.312(9) . ?
N3 C31 1.335(8) . ?
N4 C36 1.324(7) . ?
N4 C40 1.337(8) . ?
N5 C44 1.311(7) . ?
N5 C43 1.357(9) . ?
N5 Ni1 2.111(5) 2_676 ?
N6 C46 1.277(10) . ?
N6 C50 1.337(8) . ?
N7 C54 1.312(10) . ?
N7 C53 1.353(9) . ?
N7 Ni1 2.108(6) 2_666 ?
O1 C1 1.225(8) . ?
O2 C1 1.299(8) . ?
O3 C5 1.242(8) . ?
O4 C5 1.256(8) . ?
O4 Ni1 2.062(4) 2_676 ?
O5 C13 1.269(10) . ?
O5 Ni3 2.058(5) 1_454 ?
O6 C13 1.223(9) . ?
O9 C16 1.257(8) . ?
O10 C16 1.263(9) . ?
O11 C20 1.255(7) . ?
O11 Ni2 2.044(4) 2_665 ?
O12 C20 1.242(7) . ?
O12 Ni1 2.019(4) 2_665 ?
O13 C28 1.236(8) . ?
O14 C28 1.262(9) . ?
O17 H1W 0.8200 . ?
O17 H2W 0.8499 . ?
O18 H3W 0.8501 . ?
O18 H4W 0.8501 . ?
O19 H5W 0.8501 . ?
O19 H6W 0.8501 . ?
O20 H7W 0.8200 . ?
O20 H8W 0.8499 . ?
C1 C2 1.468(9) . ?
C2 C8 1.391(10) . ?
C2 C3 1.412(9) . ?
C3 C4 1.402(9) . ?
C3 H3 0.9300 . ?
C4 C6 1.381(10) . ?
C4 C5 1.520(9) . ?
C6 C7 1.358(9) . ?
C6 H6 0.9300 . ?
C7 C8 1.399(9) . ?
C7 H7 0.9300 . ?
C8 C9 1.483(9) . ?
C9 C15 1.387(9) . ?
C9 C10 1.395(11) . ?
C10 C11 1.403(10) . ?
C10 H10 0.9300 . ?
C11 C12 1.353(10) . ?
C12 C14 1.370(11) . ?
C12 C13 1.496(10) . ?
C14 C15 1.387(10) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C17 1.507(9) . ?
C17 C18 1.361(8) . ?
C17 C23 1.419(9) . ?
C18 C19 1.375(8) . ?
C18 H18 0.9300 . ?
C19 C21 1.367(9) . ?
C19 C20 1.509(8) . ?
C21 C22 1.389(9) . ?
C21 H21 0.9300 . ?
C22 C23 1.391(9) . ?
C22 H22 0.9300 . ?
C23 C24 1.496(8) . ?
C24 C25 1.373(10) . ?
C24 C30 1.393(10) . ?
C25 C26 1.355(9) . ?
C25 H25 0.9300 . ?
C26 C27 1.404(10) . ?
C27 C29 1.395(10) . ?
C27 C28 1.521(9) . ?
C29 C30 1.383(9) . ?
C29 H29 0.9300 . ?
C30 H30 0.9300 . ?
C31 C32 1.351(9) . ?
C31 H31 0.9300 . ?
C32 C33 1.329(9) . ?
C32 H32 0.9300 . ?
C33 C34 1.361(9) . ?
C33 C33 1.485(12) 2_776 ?
C34 C35 1.404(10) . ?
C34 H34 0.9300 . ?
C35 H35 0.9300 . ?
C36 C37 1.379(9) . ?
C36 H36 0.9300 . ?
C37 C38 1.380(9) . ?
C37 H37 0.9300 . ?
C38 C39 1.398(9) . ?
C38 C41 1.486(9) . ?
C39 C40 1.368(10) . ?
C39 H39 0.9300 . ?
C40 H40 0.9300 . ?
C41 C42 1.365(9) . ?
C41 C45 1.406(9) . ?
C42 C43 1.369(10) . ?
C42 H42 0.9300 . ?
C43 H43 0.9300 . ?
C44 C45 1.401(10) . ?
C44 H44 0.9300 . ?
C45 H45 0.9300 . ?
C46 C47 1.392(11) . ?
C46 H46 0.9300 . ?
C47 C48 1.409(9) . ?
C47 H47 0.9300 . ?
C48 C49 1.399(10) . ?
C48 C51 1.469(10) . ?
C49 C50 1.375(10) . ?
C49 H49 0.9300 . ?
C50 H50 0.9300 . ?
C51 C52 1.359(12) . ?
C51 C55 1.386(10) . ?
C52 C53 1.398(12) . ?
C52 H52 0.9300 . ?
C53 H53 0.9300 . ?
C54 C55 1.386(10) . ?
C54 H54 0.9300 . ?
C55 H55 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
O12 Ni1 O4 174.88(19) 2_665 2_676 ?
O12 Ni1 O18 92.77(17) 2_665 . ?
O4 Ni1 O18 88.90(17) 2_676 . ?
O12 Ni1 N7 90.4(2) 2_665 2_666 ?
O4 Ni1 N7 94.4(2) 2_676 2_666 ?
O18 Ni1 N7 91.7(2) . 2_666 ?
O12 Ni1 N5 88.9(2) 2_665 2_676 ?
O4 Ni1 N5 89.19(19) 2_676 2_676 ?
O18 Ni1 N5 176.89(18) . 2_676 ?
N7 Ni1 N5 90.9(2) 2_666 2_676 ?
O12 Ni1 O2 84.92(17) 2_665 . ?
O4 Ni1 O2 90.74(17) 2_676 . ?
O18 Ni1 O2 77.14(17) . . ?
N7 Ni1 O2 167.66(19) 2_666 . ?
N5 Ni1 O2 100.4(2) 2_676 . ?
O11 Ni2 O9 85.77(17) 2_665 . ?
O11 Ni2 N3 173.5(2) 2_665 . ?
O9 Ni2 N3 90.9(2) . . ?
O11 Ni2 O17 87.19(19) 2_665 . ?
O9 Ni2 O17 89.6(2) . . ?
N3 Ni2 O17 87.2(2) . . ?
O11 Ni2 O18 88.72(18) 2_665 . ?
O9 Ni2 O18 92.08(19) . . ?
N3 Ni2 O18 97.0(2) . . ?
O17 Ni2 O18 175.46(19) . . ?
O11 Ni2 O2 91.15(16) 2_665 . ?
O9 Ni2 O2 170.74(19) . . ?
N3 Ni2 O2 92.96(19) . . ?
O17 Ni2 O2 98.98(19) . . ?
O18 Ni2 O2 79.11(18) . . ?
O19 Ni3 O5 93.5(2) . 1_656 ?
O19 Ni3 N4 93.9(2) . . ?
O5 Ni3 N4 87.7(2) 1_656 . ?
O19 Ni3 N6 171.0(2) . . ?
O5 Ni3 N6 91.1(2) 1_656 . ?
N4 Ni3 N6 94.0(2) . . ?
O19 Ni3 O20 85.4(2) . . ?
O5 Ni3 O20 93.10(19) 1_656 . ?
N4 Ni3 O20 178.9(2) . . ?
N6 Ni3 O20 86.6(2) . . ?
O19 Ni3 O14 89.05(19) . . ?
O5 Ni3 O14 176.8(2) 1_656 . ?
N4 Ni3 O14 90.2(2) . . ?
N6 Ni3 O14 86.7(2) . . ?
O20 Ni3 O14 88.99(19) . . ?
O19 Ni3 H8W 85.3 . . ?
O5 Ni3 H8W 114.9 1_656 . ?
N4 Ni3 H8W 157.4 . . ?
N6 Ni3 H8W 85.7 . . ?
O20 Ni3 H8W 21.8 . . ?
O14 Ni3 H8W 67.2 . . ?
O7 N1 O8 121.5(11) . . ?
O7 N1 C11 118.1(9) . . ?
O8 N1 C11 120.4(9) . . ?
O15 N2 O16 129.6(11) . . ?
O15 N2 C26 115.0(9) . . ?
O16 N2 C26 115.3(10) . . ?
C35 N3 C31 114.8(6) . . ?
C35 N3 Ni2 120.8(5) . . ?
C31 N3 Ni2 122.5(5) . . ?
C36 N4 C40 114.6(6) . . ?
C36 N4 Ni3 128.7(5) . . ?
C40 N4 Ni3 116.5(4) . . ?
C44 N5 C43 115.2(6) . . ?
C44 N5 Ni1 120.8(5) . 2_676 ?
C43 N5 Ni1 123.8(4) . 2_676 ?
C46 N6 C50 119.3(7) . . ?
C46 N6 Ni3 124.7(5) . . ?
C50 N6 Ni3 116.1(5) . . ?
C54 N7 C53 117.7(7) . . ?
C54 N7 Ni1 123.3(5) . 2_666 ?
C53 N7 Ni1 118.8(6) . 2_666 ?
C1 O2 Ni2 121.3(4) . . ?
C1 O2 Ni1 141.1(4) . . ?
Ni2 O2 Ni1 94.98(18) . . ?
C5 O4 Ni1 128.4(4) . 2_676 ?
C13 O5 Ni3 129.2(5) . 1_454 ?
C16 O9 Ni2 124.7(4) . . ?
C20 O11 Ni2 129.0(4) . 2_665 ?
C20 O12 Ni1 130.8(4) . 2_665 ?
C28 O14 Ni3 129.7(4) . . ?
Ni2 O17 H1W 109.5 . . ?
Ni2 O17 H2W 83.3 . . ?
H1W O17 H2W 107.6 . . ?
Ni2 O18 Ni1 100.9(2) . . ?
Ni2 O18 H3W 86.4 . . ?
Ni1 O18 H3W 133.9 . . ?
Ni2 O18 H4W 119.5 . . ?
Ni1 O18 H4W 91.9 . . ?
H3W O18 H4W 123.9 . . ?
Ni3 O19 H5W 92.4 . . ?
Ni3 O19 H6W 132.9 . . ?
H5W O19 H6W 115.3 . . ?
Ni3 O20 H7W 109.8 . . ?
Ni3 O20 H8W 45.6 . . ?
H7W O20 H8W 153.7 . . ?
O1 C1 O2 121.8(6) . . ?
O1 C1 C2 117.5(7) . . ?
O2 C1 C2 120.6(6) . . ?
C8 C2 C3 119.0(6) . . ?
C8 C2 C1 121.4(6) . . ?
C3 C2 C1 119.2(6) . . ?
C4 C3 C2 120.5(7) . . ?
C4 C3 H3 119.7 . . ?
C2 C3 H3 119.7 . . ?
C6 C4 C3 118.7(6) . . ?
C6 C4 C5 121.1(6) . . ?
C3 C4 C5 120.2(7) . . ?
O3 C5 O4 125.8(6) . . ?
O3 C5 C4 115.4(7) . . ?
O4 C5 C4 118.7(6) . . ?
C7 C6 C4 121.3(7) . . ?
C7 C6 H6 119.3 . . ?
C4 C6 H6 119.3 . . ?
C6 C7 C8 121.2(7) . . ?
C6 C7 H7 119.4 . . ?
C8 C7 H7 119.4 . . ?
C2 C8 C7 119.2(6) . . ?
C2 C8 C9 121.7(6) . . ?
C7 C8 C9 119.1(7) . . ?
C15 C9 C10 117.2(7) . . ?
C15 C9 C8 121.5(7) . . ?
C10 C9 C8 121.3(7) . . ?
C9 C10 C11 118.8(7) . . ?
C9 C10 H10 120.6 . . ?
C11 C10 H10 120.6 . . ?
C12 C11 C10 124.2(9) . . ?
C12 C11 N1 120.0(7) . . ?
C10 C11 N1 115.8(7) . . ?
C11 C12 C14 116.2(7) . . ?
C11 C12 C13 125.9(9) . . ?
C14 C12 C13 117.8(8) . . ?
O6 C13 O5 124.8(7) . . ?
O6 C13 C12 117.3(8) . . ?
O5 C13 C12 117.8(7) . . ?
C12 C14 C15 122.1(7) . . ?
C12 C14 H14 119.0 . . ?
C15 C14 H14 119.0 . . ?
C14 C15 C9 121.4(8) . . ?
C14 C15 H15 119.3 . . ?
C9 C15 H15 119.3 . . ?
O9 C16 O10 126.0(7) . . ?
O9 C16 C17 115.7(7) . . ?
O10 C16 C17 118.2(6) . . ?
C18 C17 C23 118.1(6) . . ?
C18 C17 C16 120.5(6) . . ?
C23 C17 C16 121.1(5) . . ?
C17 C18 C19 123.8(6) . . ?
C17 C18 H18 118.1 . . ?
C19 C18 H18 118.1 . . ?
C21 C19 C18 118.1(6) . . ?
C21 C19 C20 120.2(6) . . ?
C18 C19 C20 121.7(6) . . ?
O12 C20 O11 127.0(6) . . ?
O12 C20 C19 116.7(5) . . ?
O11 C20 C19 116.3(5) . . ?
C19 C21 C22 120.7(6) . . ?
C19 C21 H21 119.6 . . ?
C22 C21 H21 119.6 . . ?
C21 C22 C23 120.7(6) . . ?
C21 C22 H22 119.6 . . ?
C23 C22 H22 119.6 . . ?
C22 C23 C17 118.5(6) . . ?
C22 C23 C24 120.8(6) . . ?
C17 C23 C24 120.8(6) . . ?
C25 C24 C30 118.7(6) . . ?
C25 C24 C23 120.9(6) . . ?
C30 C24 C23 120.3(7) . . ?
C26 C25 C24 119.5(7) . . ?
C26 C25 H25 120.3 . . ?
C24 C25 H25 120.3 . . ?
C25 C26 C27 124.1(8) . . ?
C25 C26 N2 112.8(7) . . ?
C27 C26 N2 123.1(6) . . ?
C29 C27 C26 115.7(6) . . ?
C29 C27 C28 118.9(7) . . ?
C26 C27 C28 125.3(7) . . ?
O13 C28 O14 126.1(7) . . ?
O13 C28 C27 117.0(7) . . ?
O14 C28 C27 116.6(7) . . ?
C30 C29 C27 120.6(7) . . ?
C30 C29 H29 119.7 . . ?
C27 C29 H29 119.7 . . ?
C29 C30 C24 121.3(8) . . ?
C29 C30 H30 119.3 . . ?
C24 C30 H30 119.3 . . ?
N3 C31 C32 124.8(8) . . ?
N3 C31 H31 117.6 . . ?
C32 C31 H31 117.6 . . ?
C33 C32 C31 121.6(7) . . ?
C33 C32 H32 119.2 . . ?
C31 C32 H32 119.2 . . ?
C32 C33 C34 115.1(7) . . ?
C32 C33 C33 124.6(7) . 2_776 ?
C34 C33 C33 120.3(8) . 2_776 ?
C33 C34 C35 121.6(7) . . ?
C33 C34 H34 119.2 . . ?
C35 C34 H34 119.2 . . ?
N3 C35 C34 121.9(7) . . ?
N3 C35 H35 119.1 . . ?
C34 C35 H35 119.1 . . ?
N4 C36 C37 125.8(7) . . ?
N4 C36 H36 117.1 . . ?
C37 C36 H36 117.1 . . ?
C38 C37 C36 118.5(7) . . ?
C38 C37 H37 120.7 . . ?
C36 C37 H37 120.7 . . ?
C37 C38 C39 117.0(7) . . ?
C37 C38 C41 122.7(6) . . ?
C39 C38 C41 120.3(6) . . ?
C40 C39 C38 119.0(7) . . ?
C40 C39 H39 120.5 . . ?
C38 C39 H39 120.5 . . ?
N4 C40 C39 124.9(7) . . ?
N4 C40 H40 117.5 . . ?
C39 C40 H40 117.5 . . ?
C42 C41 C45 116.5(7) . . ?
C42 C41 C38 124.1(7) . . ?
C45 C41 C38 119.3(6) . . ?
C41 C42 C43 120.3(7) . . ?
C41 C42 H42 119.9 . . ?
C43 C42 H42 119.9 . . ?
N5 C43 C42 124.5(7) . . ?
N5 C43 H43 117.8 . . ?
C42 C43 H43 117.8 . . ?
N5 C44 C45 124.5(7) . . ?
N5 C44 H44 117.7 . . ?
C45 C44 H44 117.7 . . ?
C44 C45 C41 118.8(6) . . ?
C44 C45 H45 120.6 . . ?
C41 C45 H45 120.6 . . ?
N6 C46 C47 123.6(8) . . ?
N6 C46 H46 118.2 . . ?
C47 C46 H46 118.2 . . ?
C46 C47 C48 119.6(8) . . ?
C46 C47 H47 120.2 . . ?
C48 C47 H47 120.2 . . ?
C49 C48 C47 114.9(7) . . ?
C49 C48 C51 121.3(7) . . ?
C47 C48 C51 123.8(8) . . ?
C50 C49 C48 120.9(7) . . ?
C50 C49 H49 119.5 . . ?
C48 C49 H49 119.5 . . ?
N6 C50 C49 121.7(8) . . ?
N6 C50 H50 119.1 . . ?
C49 C50 H50 119.1 . . ?
C52 C51 C55 116.9(8) . . ?
C52 C51 C48 122.1(7) . . ?
C55 C51 C48 120.8(8) . . ?
C51 C52 C53 121.9(8) . . ?
C51 C52 H52 119.0 . . ?
C53 C52 H52 119.0 . . ?
N7 C53 C52 120.2(9) . . ?
N7 C53 H53 119.9 . . ?
C52 C53 H53 119.9 . . ?
N7 C54 C55 124.5(7) . . ?
N7 C54 H54 117.8 . . ?
C55 C54 H54 117.8 . . ?
C51 C55 C54 118.7(9) . . ?
C51 C55 H55 120.6 . . ?
C54 C55 H55 120.6 . . ?

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.013 -0.014 -0.013 967 218 ' '
_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
Ni2 O2 C1 O1 -3.5(9) . . . . ?
Ni1 O2 C1 O1 -160.0(5) . . . . ?
Ni2 O2 C1 C2 179.8(4) . . . . ?
Ni1 O2 C1 C2 23.3(10) . . . . ?
O1 C1 C2 C8 62.2(9) . . . . ?
O2 C1 C2 C8 -120.9(8) . . . . ?
O1 C1 C2 C3 -110.5(8) . . . . ?
O2 C1 C2 C3 66.4(8) . . . . ?
C8 C2 C3 C4 -2.6(10) . . . . ?
C1 C2 C3 C4 170.2(6) . . . . ?
C2 C3 C4 C6 2.4(11) . . . . ?
C2 C3 C4 C5 179.2(6) . . . . ?
Ni1 O4 C5 O3 -8.5(12) 2_676 . . . ?
Ni1 O4 C5 C4 167.5(4) 2_676 . . . ?
C6 C4 C5 O3 8.2(11) . . . . ?
C3 C4 C5 O3 -168.5(7) . . . . ?
C6 C4 C5 O4 -168.2(7) . . . . ?
C3 C4 C5 O4 15.1(10) . . . . ?
C3 C4 C6 C7 -0.1(12) . . . . ?
C5 C4 C6 C7 -176.9(7) . . . . ?
C4 C6 C7 C8 -1.8(12) . . . . ?
C3 C2 C8 C7 0.7(11) . . . . ?
C1 C2 C8 C7 -172.0(6) . . . . ?
C3 C2 C8 C9 179.7(6) . . . . ?
C1 C2 C8 C9 6.9(11) . . . . ?
C6 C7 C8 C2 1.5(11) . . . . ?
C6 C7 C8 C9 -177.5(7) . . . . ?
C2 C8 C9 C15 42.1(11) . . . . ?
C7 C8 C9 C15 -139.0(8) . . . . ?
C2 C8 C9 C10 -136.4(8) . . . . ?
C7 C8 C9 C10 42.5(10) . . . . ?
C15 C9 C10 C11 -0.1(11) . . . . ?
C8 C9 C10 C11 178.5(7) . . . . ?
C9 C10 C11 C12 1.8(13) . . . . ?
C9 C10 C11 N1 -178.7(7) . . . . ?
O7 N1 C11 C12 137.8(11) . . . . ?
O8 N1 C11 C12 -44.0(12) . . . . ?
O7 N1 C11 C10 -41.7(13) . . . . ?
O8 N1 C11 C10 136.5(9) . . . . ?
C10 C11 C12 C14 -3.2(13) . . . . ?
N1 C11 C12 C14 177.2(8) . . . . ?
C10 C11 C12 C13 172.8(8) . . . . ?
N1 C11 C12 C13 -6.8(13) . . . . ?
Ni3 O5 C13 O6 2.8(16) 1_454 . . . ?
Ni3 O5 C13 C12 -174.1(5) 1_454 . . . ?
C11 C12 C13 O6 140.1(10) . . . . ?
C14 C12 C13 O6 -43.9(14) . . . . ?
C11 C12 C13 O5 -42.7(14) . . . . ?
C14 C12 C13 O5 133.2(9) . . . . ?
C11 C12 C14 C15 3.1(13) . . . . ?
C13 C12 C14 C15 -173.2(7) . . . . ?
C12 C14 C15 C9 -1.7(13) . . . . ?
C10 C9 C15 C14 0.0(11) . . . . ?
C8 C9 C15 C14 -178.5(7) . . . . ?
Ni2 O9 C16 O10 -20.0(11) . . . . ?
Ni2 O9 C16 C17 157.0(5) . . . . ?
O9 C16 C17 C18 -113.5(8) . . . . ?
O10 C16 C17 C18 63.7(11) . . . . ?
O9 C16 C17 C23 59.8(10) . . . . ?
O10 C16 C17 C23 -123.0(8) . . . . ?
C23 C17 C18 C19 -3.9(12) . . . . ?
C16 C17 C18 C19 169.6(7) . . . . ?
C17 C18 C19 C21 3.0(12) . . . . ?
C17 C18 C19 C20 -176.3(7) . . . . ?
Ni1 O12 C20 O11 14.6(11) 2_665 . . . ?
Ni1 O12 C20 C19 -166.0(4) 2_665 . . . ?
Ni2 O11 C20 O12 0.2(11) 2_665 . . . ?
Ni2 O11 C20 C19 -179.2(4) 2_665 . . . ?
C21 C19 C20 O12 -16.3(10) . . . . ?
C18 C19 C20 O12 163.0(7) . . . . ?
C21 C19 C20 O11 163.1(7) . . . . ?
C18 C19 C20 O11 -17.6(10) . . . . ?
C18 C19 C21 C22 -0.3(12) . . . . ?
C20 C19 C21 C22 179.1(7) . . . . ?
C19 C21 C22 C23 -1.4(13) . . . . ?
C21 C22 C23 C17 0.5(12) . . . . ?
C21 C22 C23 C24 179.1(8) . . . . ?
C18 C17 C23 C22 2.0(12) . . . . ?
C16 C17 C23 C22 -171.4(7) . . . . ?
C18 C17 C23 C24 -176.6(7) . . . . ?
C16 C17 C23 C24 10.0(12) . . . . ?
C22 C23 C24 C25 -128.3(9) . . . . ?
C17 C23 C24 C25 50.2(11) . . . . ?
C22 C23 C24 C30 49.3(11) . . . . ?
C17 C23 C24 C30 -132.2(8) . . . . ?
C30 C24 C25 C26 0.2(12) . . . . ?
C23 C24 C25 C26 177.8(7) . . . . ?
C24 C25 C26 C27 -0.8(13) . . . . ?
C24 C25 C26 N2 177.5(8) . . . . ?
O15 N2 C26 C25 -102.9(9) . . . . ?
O16 N2 C26 C25 73.8(11) . . . . ?
O15 N2 C26 C27 75.4(11) . . . . ?
O16 N2 C26 C27 -107.9(10) . . . . ?
C25 C26 C27 C29 0.2(12) . . . . ?
N2 C26 C27 C29 -177.8(8) . . . . ?
C25 C26 C27 C28 -177.2(7) . . . . ?
N2 C26 C27 C28 4.7(13) . . . . ?
Ni3 O14 C28 O13 12.0(11) . . . . ?
Ni3 O14 C28 C27 -174.5(4) . . . . ?
C29 C27 C28 O13 15.5(10) . . . . ?
C26 C27 C28 O13 -167.1(7) . . . . ?
C29 C27 C28 O14 -158.6(7) . . . . ?
C26 C27 C28 O14 18.8(11) . . . . ?
C26 C27 C29 C30 0.9(11) . . . . ?
C28 C27 C29 C30 178.6(6) . . . . ?
C27 C29 C30 C24 -1.6(11) . . . . ?
C25 C24 C30 C29 1.0(11) . . . . ?
C23 C24 C30 C29 -176.6(7) . . . . ?
C35 N3 C31 C32 -3.9(16) . . . . ?
Ni2 N3 C31 C32 -168.4(9) . . . . ?
N3 C31 C32 C33 1.7(18) . . . . ?
C31 C32 C33 C34 0.1(16) . . . . ?
C31 C32 C33 C33 -179.6(11) . . . 2_776 ?
C32 C33 C34 C35 0.6(16) . . . . ?
C33 C33 C34 C35 -179.7(11) 2_776 . . . ?
C31 N3 C35 C34 4.4(15) . . . . ?
Ni2 N3 C35 C34 169.2(8) . . . . ?
C33 C34 C35 N3 -3.1(18) . . . . ?
C40 N4 C36 C37 2.2(12) . . . . ?
Ni3 N4 C36 C37 176.7(6) . . . . ?
N4 C36 C37 C38 -0.5(13) . . . . ?
C36 C37 C38 C39 -0.4(12) . . . . ?
C36 C37 C38 C41 -180.0(7) . . . . ?
C37 C38 C39 C40 -0.4(13) . . . . ?
C41 C38 C39 C40 179.2(8) . . . . ?
C36 N4 C40 C39 -3.1(14) . . . . ?
Ni3 N4 C40 C39 -178.4(8) . . . . ?
C38 C39 C40 N4 2.4(15) . . . . ?
C37 C38 C41 C42 -31.8(13) . . . . ?
C39 C38 C41 C42 148.6(9) . . . . ?
C37 C38 C41 C45 152.2(8) . . . . ?
C39 C38 C41 C45 -27.4(12) . . . . ?
C45 C41 C42 C43 4.7(13) . . . . ?
C38 C41 C42 C43 -171.4(8) . . . . ?
C44 N5 C43 C42 -3.4(13) . . . . ?
Ni1 N5 C43 C42 172.1(7) 2_676 . . . ?
C41 C42 C43 N5 -1.2(15) . . . . ?
C43 N5 C44 C45 4.4(12) . . . . ?
Ni1 N5 C44 C45 -171.2(6) 2_676 . . . ?
N5 C44 C45 C41 -0.9(13) . . . . ?
C42 C41 C45 C44 -3.8(12) . . . . ?
C38 C41 C45 C44 172.5(7) . . . . ?
C50 N6 C46 C47 0.9(17) . . . . ?
Ni3 N6 C46 C47 179.2(9) . . . . ?
N6 C46 C47 C48 -1.7(19) . . . . ?
C46 C47 C48 C49 2.2(15) . . . . ?
C46 C47 C48 C51 178.7(10) . . . . ?
C47 C48 C49 C50 -2.1(13) . . . . ?
C51 C48 C49 C50 -178.7(8) . . . . ?
C46 N6 C50 C49 -0.7(13) . . . . ?
Ni3 N6 C50 C49 -179.1(6) . . . . ?
C48 C49 C50 N6 1.4(13) . . . . ?
C49 C48 C51 C52 144.1(9) . . . . ?
C47 C48 C51 C52 -32.2(14) . . . . ?
C49 C48 C51 C55 -30.1(13) . . . . ?
C47 C48 C51 C55 153.6(9) . . . . ?
C55 C51 C52 C53 0.2(14) . . . . ?
C48 C51 C52 C53 -174.1(8) . . . . ?
C54 N7 C53 C52 -2.0(13) . . . . ?
Ni1 N7 C53 C52 173.0(7) 2_666 . . . ?
C51 C52 C53 N7 1.6(15) . . . . ?
C53 N7 C54 C55 0.5(13) . . . . ?
Ni1 N7 C54 C55 -174.2(6) 2_666 . . . ?
C52 C51 C55 C54 -1.6(12) . . . . ?
C48 C51 C55 C54 172.8(8) . . . . ?
N7 C54 C55 C51 1.3(13) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C54 H54 O4 0.93 2.54 3.137(9) 122.0 1_545
C53 H53 O12 0.93 2.30 2.898(11) 121.4 1_556
C50 H50 O14 0.93 2.45 2.923(10) 111.3 .
C44 H44 O4 0.93 2.31 2.932(9) 123.9 .
C43 H43 O12 0.93 2.47 2.989(9) 115.5 1_566
C40 H40 O15 0.93 2.21 3.025(10) 146.2 .
C40 H40 O14 0.93 2.52 3.017(9) 114.0 .
C35 H35 O9 0.93 2.33 2.932(8) 122.2 .
C32 H32 O13 0.93 2.35 3.205(10) 152.1 2_776
C31 H31 O2 0.93 2.53 3.132(9) 122.4 .
C31 H31 O1 0.93 2.53 3.190(11) 127.7 .
O20 H7W O6 0.82 1.93 2.641(8) 144.7 1_656
O19 H6W O1 0.85 1.92 2.765(6) 179.7 2_776
O19 H5W O14 0.85 2.42 2.920(6) 118.5 .
O19 H5W O13 0.85 1.79 2.639(7) 179.6 .
O18 H4W O4 0.85 2.42 2.910(6) 117.6 2_676
O18 H4W O3 0.85 1.65 2.497(6) 179.3 2_676
O18 H3W O10 0.85 1.80 2.654(6) 179.7 .
O18 H3W O9 0.85 2.48 2.982(6) 119.0 .
O17 H2W O2 0.85 2.65 3.214(6) 124.5 .
O17 H2W O1 0.85 1.79 2.635(6) 179.8 .
C54 H54 O4 0.93 2.54 3.137(9) 122.0 1_545
C53 H53 O12 0.93 2.30 2.898(11) 121.4 1_556
C50 H50 O14 0.93 2.45 2.923(10) 111.3 .
C44 H44 O4 0.93 2.31 2.932(9) 123.9 .
C43 H43 O12 0.93 2.47 2.989(9) 115.5 1_566
C40 H40 O15 0.93 2.21 3.025(10) 146.2 .
C40 H40 O14 0.93 2.52 3.017(9) 114.0 .
C35 H35 O9 0.93 2.33 2.932(8) 122.2 .
C32 H32 O13 0.93 2.35 3.205(10) 152.1 2_776
C31 H31 O2 0.93 2.53 3.132(9) 122.4 .
C31 H31 O1 0.93 2.53 3.190(11) 127.7 .
O20 H7W O6 0.82 1.93 2.641(8) 144.7 1_656
O19 H6W O1 0.85 1.92 2.765(6) 179.7 2_776
O19 H5W O14 0.85 2.42 2.920(6) 118.5 .
O19 H5W O13 0.85 1.79 2.639(7) 179.6 .
O18 H4W O4 0.85 2.42 2.910(6) 117.6 2_676
O18 H4W O3 0.85 1.65 2.497(6) 179.3 2_676
O18 H3W O10 0.85 1.80 2.654(6) 179.7 .
O18 H3W O9 0.85 2.48 2.982(6) 119.0 .
O17 H2W O2 0.85 2.65 3.214(6) 124.5 .
O17 H2W O1 0.85 1.79 2.635(6) 179.8 .
C54 H54 O4 0.93 2.54 3.137(9) 122.0 1_545
C53 H53 O12 0.93 2.30 2.898(11) 121.4 1_556
C50 H50 O14 0.93 2.45 2.923(10) 111.3 .
C44 H44 O4 0.93 2.31 2.932(9) 123.9 .
C43 H43 O12 0.93 2.47 2.989(9) 115.5 1_566
C40 H40 O15 0.93 2.21 3.025(10) 146.2 .
C40 H40 O14 0.93 2.52 3.017(9) 114.0 .
C35 H35 O9 0.93 2.33 2.932(8) 122.2 .
C32 H32 O13 0.93 2.35 3.205(10) 152.1 2_776
C31 H31 O2 0.93 2.53 3.132(9) 122.4 .
C31 H31 O1 0.93 2.53 3.190(11) 127.7 .
O20 H7W O6 0.82 1.93 2.641(8) 144.7 1_656
O19 H6W O1 0.85 1.92 2.765(6) 179.7 2_776
O19 H5W O14 0.85 2.42 2.920(6) 118.5 .
O19 H5W O13 0.85 1.79 2.639(7) 179.6 .
O18 H4W O4 0.85 2.42 2.910(6) 117.6 2_676
O18 H4W O3 0.85 1.65 2.497(6) 179.3 2_676
O18 H3W O10 0.85 1.80 2.654(6) 179.7 .
O18 H3W O9 0.85 2.48 2.982(6) 119.0 .
O17 H2W O2 0.85 2.65 3.214(6) 124.5 .
O17 H2W O1 0.85 1.79 2.635(6) 179.8 .
O17 H2W O1 0.85 1.79 2.635(6) 179.8 .
O17 H2W O2 0.85 2.65 3.214(6) 124.5 .
O18 H3W O9 0.85 2.48 2.982(6) 119.0 .
O18 H3W O10 0.85 1.80 2.654(6) 179.7 .
O18 H4W O3 0.85 1.65 2.497(6) 179.3 2_676
O18 H4W O4 0.85 2.42 2.910(6) 117.6 2_676
O19 H5W O13 0.85 1.79 2.639(7) 179.6 .
O19 H5W O14 0.85 2.42 2.920(6) 118.5 .
O19 H6W O1 0.85 1.92 2.765(6) 179.7 2_776
O20 H7W O6 0.82 1.93 2.641(8) 144.7 1_656
C31 H31 O1 0.93 2.53 3.190(11) 127.7 .
C31 H31 O2 0.93 2.53 3.132(9) 122.4 .
C32 H32 O13 0.93 2.35 3.205(10) 152.1 2_776
C35 H35 O9 0.93 2.33 2.932(8) 122.2 .
C40 H40 O14 0.93 2.52 3.017(9) 114.0 .
C40 H40 O15 0.93 2.21 3.025(10) 146.2 .
C43 H43 O12 0.93 2.47 2.989(9) 115.5 1_566
C44 H44 O4 0.93 2.31 2.932(9) 123.9 .
C50 H50 O14 0.93 2.45 2.923(10) 111.3 .
C53 H53 O12 0.93 2.30 2.898(11) 121.4 1_556
C54 H54 O4 0.93 2.54 3.137(9) 122.0 1_545
O17 H2W O1 0.85 1.79 2.635(6) 179.8 .
O17 H2W O2 0.85 2.65 3.214(6) 124.5 .
O18 H3W O9 0.85 2.48 2.982(6) 119.0 .
O18 H3W O10 0.85 1.80 2.654(6) 179.7 .
O18 H4W O3 0.85 1.65 2.497(6) 179.3 2_676
O18 H4W O4 0.85 2.42 2.910(6) 117.6 2_676
O19 H5W O13 0.85 1.79 2.639(7) 179.6 .
O19 H5W O14 0.85 2.42 2.920(6) 118.5 .
O19 H6W O1 0.85 1.92 2.765(6) 179.7 2_776
O20 H7W O6 0.82 1.93 2.641(8) 144.7 1_656
C31 H31 O1 0.93 2.53 3.190(11) 127.7 .
C31 H31 O2 0.93 2.53 3.132(9) 122.4 .
C32 H32 O13 0.93 2.35 3.205(10) 152.1 2_776
C35 H35 O9 0.93 2.33 2.932(8) 122.2 .
C40 H40 O14 0.93 2.52 3.017(9) 114.0 .
C40 H40 O15 0.93 2.21 3.025(10) 146.2 .
C43 H43 O12 0.93 2.47 2.989(9) 115.5 1_566
C44 H44 O4 0.93 2.31 2.932(9) 123.9 .
C50 H50 O14 0.93 2.45 2.923(10) 111.3 .
C53 H53 O12 0.93 2.30 2.898(11) 121.4 1_556
C54 H54 O4 0.93 2.54 3.137(9) 122.0 1_545

_refine_diff_density_max         0.876
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.106

####################################################################### 
# 
# 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_307-14zn1
_database_code_depnum_ccdc_archive 'CCDC 1589516'
_audit_update_record             
;
2017-12-06 deposited with the CCDC.
2018-04-30 downloaded from the CCDC.
;
_audit_creation_date             2017-12-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C39 H25 N5 O9 Zn, 4.5(H2 O)'
_chemical_formula_sum            'C39 H34 N5 O13.50 Zn'
_chemical_formula_weight         854.08
_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'
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'

_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           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
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                   27.788(2)
_cell_length_b                   14.0450(7)
_cell_length_c                   21.0840(13)
_cell_angle_alpha                90
_cell_angle_beta                 109.680(8)
_cell_angle_gamma                90
_cell_volume                     7748.1(10)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    1358
_cell_measurement_temperature    288.89(19)
_cell_measurement_theta_max      19.8000
_cell_measurement_theta_min      3.5890
_shelx_estimated_absorpt_T_max   0.865
_shelx_estimated_absorpt_T_min   0.843
_exptl_absorpt_coefficient_mu    0.709
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60886
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             3528
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1319
_diffrn_reflns_av_unetI/netI     0.1638
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            23571
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.214
_diffrn_reflns_theta_max         25.049
_diffrn_reflns_theta_min         3.286
_diffrn_ambient_temperature      288.89(19)
_diffrn_detector_area_resol_mean 16.0733
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega -101.00  -72.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.5055  178.0000    0.0000 29

#__ type_ start__ end____ width___ exp.time_
  2 omega  -20.00   25.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.5055  -99.0000 -150.0000 45

#__ type_ start__ end____ width___ exp.time_
  3 omega  -88.00  -62.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.5055  178.0000   60.0000 26

#__ type_ start__ end____ width___ exp.time_
  4 omega   -1.00   27.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       22.6305   57.0000   90.0000 28

#__ type_ start__ end____ width___ exp.time_
  5 omega   46.00   72.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       22.6305  178.0000    0.0000 26

#__ type_ start__ end____ width___ exp.time_
  6 omega  -48.00   29.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       22.6305  -57.0000 -180.0000 77

#__ type_ start__ end____ width___ exp.time_
  7 omega  -14.00   98.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       22.6305   19.0000  150.0000 112

#__ type_ start__ end____ width___ exp.time_
  8 omega  -15.00   46.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       22.6305  -57.0000  -60.0000 61
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0135886000
_diffrn_orient_matrix_UB_12      -0.0091572000
_diffrn_orient_matrix_UB_13      -0.0224389000
_diffrn_orient_matrix_UB_21      -0.0229269000
_diffrn_orient_matrix_UB_22      -0.0156070000
_diffrn_orient_matrix_UB_23      -0.0248119000
_diffrn_orient_matrix_UB_31      -0.0049545000
_diffrn_orient_matrix_UB_32      0.0471265000
_diffrn_orient_matrix_UB_33      -0.0125920000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3032
_reflns_number_total             6877
_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 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         1.196
_refine_diff_density_min         -0.571
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     526
_refine_ls_number_reflns         6877
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1826
_refine_ls_R_factor_gt           0.0857
_refine_ls_restrained_S_all      0.975
_refine_ls_shift/su_max          0.040
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0868P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1900
_refine_ls_wR_factor_ref         0.2341
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H) groups, H15 of C15, H28 of C28, H16 of C16, H18 of C18, H10 of C10,
   H21 of C21, H11 of C11, H27 of C27, H29 of C29, {H9A,H9B} of O9, H30 of C30,
  H22 of C22, H7 of C7, H33 of C33, H34 of C34, H3A of C3, H6 of C6, H25 of C25,
   H17 of C17, H26 of C26, H38 of C38, H37 of C37
 At 1.2 times of:
  {H12A,H12B} of O12, {H10A,H10B} of O10, {H13A,H13B} of O13, {H14A,H14B} of
  O14, H39 of C39, {H15A,H15B} of O15
2. Others
 Fixed Sof: H13A(0.5) H13B(0.5) H14A(0.5) H14B(0.5)
3.a Riding coordinates:
 O10(H10A,H10B), O11(H11A), O12(H12A,H12B), O13(H13A,H13B), O14(H14A,H14B),
 O15(H15A,H15B)
3.b Rotating group:
 O9(H9A,H9B)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3A), C6(H6), C7(H7), C10(H10), C11(H11), C15(H15), C16(H16), C17(H17),
 C18(H18), C21(H21), C22(H22), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29),
  C30(H30), C33(H33), C34(H34), C37(H37), C38(H38), C39(H39)
3.d Tetrahedral OH refined with riding coordinates:
 O3(H3)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.38854(3) 0.02193(6) 0.31297(4) 0.0465(3) Uani 1 1 d . . . . .
N1 N 0.3170(3) 0.2195(6) 0.5513(4) 0.070(2) Uani 1 1 d . . . . .
N2 N 0.3442(3) 0.0330(4) 0.2083(3) 0.0544(17) Uani 1 1 d . . . . .
N3 N 0.3109(2) 0.0254(4) 0.3139(3) 0.0432(15) Uani 1 1 d . . . . .
N4 N 0.4175(2) -0.0083(4) 0.4172(3) 0.0498(16) Uani 1 1 d . . . . .
N5 N 0.3977(2) -0.1307(4) 0.3155(3) 0.0458(15) Uani 1 1 d . . . . .
O1 O 0.40898(18) 0.1625(3) 0.3312(2) 0.0443(12) Uani 1 1 d . . . . .
O2 O 0.4232(2) 0.2791(4) 0.2689(3) 0.0699(17) Uani 1 1 d . . . . .
O3 O 0.1841(2) 0.2747(4) 0.0882(2) 0.0633(15) Uani 1 1 d . . . . .
H3 H 0.1716 0.2778 0.0471 0.095 Uiso 1 1 calc R . . . .
O4 O 0.2551(2) 0.2965(4) 0.0668(3) 0.0725(17) Uani 1 1 d . . . . .
O5 O 0.4413(4) 0.3689(6) 0.6316(3) 0.144(4) Uani 1 1 d . . . . .
O6 O 0.4338(3) 0.2140(5) 0.6364(3) 0.083(2) Uani 1 1 d . . . . .
O7 O 0.2853(3) 0.1550(5) 0.5303(4) 0.103(3) Uani 1 1 d . . . . .
O8 O 0.3238(3) 0.2602(5) 0.6043(3) 0.100(2) Uani 1 1 d . . . . .
O10 O 0.3463(2) 0.2728(5) 0.0382(3) 0.103(2) Uani 1 1 d . . . . .
H10A H 0.3196 0.2949 0.0439 0.124 Uiso 1 1 d R . . . .
H10B H 0.3785 0.2536 0.0554 0.124 Uiso 1 1 d R . . . .
O11 O 0.5000 0.5610(5) 0.2500 0.062(2) Uani 1 2 d S T P . .
H11A H 0.4844 0.5939 0.2140 0.20(6) Uiso 1 1 d R . . . .
O12 O 0.3840(8) 0.4531(11) 0.0820(9) 0.419(14) Uani 1 1 d . . . . .
H12A H 0.4009 0.5039 0.0959 0.503 Uiso 1 1 d R . . . .
H12B H 0.3828 0.4077 0.0688 0.503 Uiso 1 1 d R . . . .
O13 O 0.5000 0.1732(6) 0.2500 0.166(6) Uani 1 2 d S T P . .
H13A H 0.4760 0.2057 0.2559 0.199 Uiso 0.5 1 d R . . . .
H13B H 0.5240 0.2057 0.2441 0.199 Uiso 0.5 1 d R . . . .
O14 O 0.5000 0.1381(4) 0.7500 0.0438(17) Uani 1 2 d S T P . .
H14A H 0.4791 0.1618 0.7142 0.053 Uiso 0.5 1 d R . . . .
H14B H 0.5209 0.1618 0.7858 0.053 Uiso 0.5 1 d R . . . .
O9 O 0.46061(18) 0.0155(3) 0.2945(3) 0.0581(14) Uani 1 1 d . . . . .
H9A H 0.4598 0.0479 0.2570 0.087 Uiso 1 1 d GR . . . .
H9B H 0.4693 -0.0451 0.2885 0.087 Uiso 1 1 d GR . . . .
C1 C 0.3954(3) 0.2335(6) 0.2926(4) 0.0445(19) Uani 1 1 d . . . . .
C2 C 0.3403(3) 0.2649(4) 0.2730(3) 0.0354(17) Uani 1 1 d . . . . .
C3 C 0.3125(3) 0.2708(4) 0.2040(3) 0.0384(17) Uani 1 1 d . . . . .
H3A H 0.3300 0.2673 0.1734 0.058 Uiso 1 1 calc R . . . .
C4 C 0.2600(3) 0.2817(4) 0.1799(3) 0.0393(17) Uani 1 1 d . . . . .
C5 C 0.2337(3) 0.2861(5) 0.1064(4) 0.0463(19) Uani 1 1 d . . . . .
C6 C 0.2343(3) 0.2867(4) 0.2253(3) 0.0432(18) Uani 1 1 d . . . . .
H6 H 0.1988 0.2901 0.2097 0.065 Uiso 1 1 calc R . . . .
C7 C 0.2606(3) 0.2868(4) 0.2940(3) 0.0398(17) Uani 1 1 d . . . . .
H7 H 0.2425 0.2940 0.3237 0.060 Uiso 1 1 calc R . . . .
C8 C 0.3134(3) 0.2763(4) 0.3196(3) 0.0326(16) Uani 1 1 d . . . . .
C9 C 0.3413(3) 0.2809(4) 0.3937(3) 0.0381(17) Uani 1 1 d . . . . .
C10 C 0.3881(3) 0.3248(5) 0.4192(4) 0.0467(19) Uani 1 1 d . . . . .
H10 H 0.4026 0.3520 0.3897 0.070 Uiso 1 1 calc R . . . .
C11 C 0.4138(3) 0.3294(5) 0.4870(4) 0.056(2) Uani 1 1 d . . . . .
H11 H 0.4457 0.3583 0.5025 0.084 Uiso 1 1 calc R . . . .
C12 C 0.3930(3) 0.2913(5) 0.5334(4) 0.052(2) Uani 1 1 d . . . . .
C13 C 0.4259(4) 0.2876(9) 0.6083(5) 0.074(3) Uani 1 1 d . . . . .
C14 C 0.3455(3) 0.2532(5) 0.5077(4) 0.052(2) Uani 1 1 d . . . . .
C15 C 0.3185(3) 0.2455(5) 0.4383(3) 0.0411(17) Uani 1 1 d . . . . .
H15 H 0.2863 0.2176 0.4227 0.062 Uiso 1 1 calc R . . . .
C16 C 0.2941(3) 0.0233(5) 0.3658(4) 0.051(2) Uani 1 1 d . . . . .
H16 H 0.3180 0.0197 0.4090 0.077 Uiso 1 1 calc R . . . .
C17 C 0.2407(4) 0.0264(5) 0.3584(5) 0.068(2) Uani 1 1 d . . . . .
H17 H 0.2306 0.0277 0.3962 0.102 Uiso 1 1 calc R . . . .
C18 C 0.2052(3) 0.0273(5) 0.2960(5) 0.067(3) Uani 1 1 d . . . . .
H18 H 0.1706 0.0273 0.2905 0.100 Uiso 1 1 calc R . . . .
C19 C 0.2217(3) 0.0283(5) 0.2390(5) 0.057(2) Uani 1 1 d . . . . .
C20 C 0.2755(3) 0.0289(4) 0.2512(4) 0.0419(18) Uani 1 1 d . . . . .
C21 C 0.1872(4) 0.0293(5) 0.1724(5) 0.068(3) Uani 1 1 d . . . . .
H21 H 0.1523 0.0258 0.1650 0.102 Uiso 1 1 calc R . . . .
C22 C 0.2034(4) 0.0350(6) 0.1204(6) 0.081(3) Uani 1 1 d . . . . .
H22 H 0.1795 0.0358 0.0771 0.121 Uiso 1 1 calc R . . . .
C23 C 0.2575(4) 0.0401(5) 0.1288(4) 0.059(2) Uani 1 1 d . . . . .
C24 C 0.2936(3) 0.0338(5) 0.1952(4) 0.0470(19) Uani 1 1 d . . . . .
C25 C 0.2786(5) 0.0491(6) 0.0775(5) 0.080(3) Uani 1 1 d . . . . .
H25 H 0.2568 0.0525 0.0330 0.121 Uiso 1 1 calc R . . . .
C26 C 0.3294(5) 0.0530(6) 0.0907(5) 0.085(3) Uani 1 1 d . . . . .
H26 H 0.3428 0.0622 0.0562 0.128 Uiso 1 1 calc R . . . .
C27 C 0.3610(4) 0.0433(5) 0.1560(4) 0.069(3) Uani 1 1 d . . . . .
H27 H 0.3961 0.0438 0.1647 0.103 Uiso 1 1 calc R . . . .
C28 C 0.4265(3) 0.0547(6) 0.4679(4) 0.059(2) Uani 1 1 d . . . . .
H28 H 0.4201 0.1189 0.4576 0.088 Uiso 1 1 calc R . . . .
C29 C 0.4458(3) 0.0265(7) 0.5372(4) 0.074(3) Uani 1 1 d . . . . .
H29 H 0.4513 0.0707 0.5718 0.111 Uiso 1 1 calc R . . . .
C30 C 0.4555(3) -0.0677(8) 0.5501(5) 0.077(3) Uani 1 1 d . . . . .
H30 H 0.4691 -0.0877 0.5947 0.115 Uiso 1 1 calc R . . . .
C31 C 0.4460(3) -0.1361(7) 0.4987(4) 0.059(2) Uani 1 1 d . . . . .
C32 C 0.4273(3) -0.1021(6) 0.4328(4) 0.049(2) Uani 1 1 d . . . . .
C33 C 0.4564(3) -0.2354(7) 0.5100(5) 0.077(3) Uani 1 1 d . . . . .
H33 H 0.4695 -0.2588 0.5538 0.115 Uiso 1 1 calc R . . . .
C34 C 0.4471(4) -0.2945(7) 0.4578(6) 0.081(3) Uani 1 1 d . . . . .
H34 H 0.4529 -0.3592 0.4662 0.122 Uiso 1 1 calc R . . . .
C35 C 0.4289(3) -0.2630(6) 0.3904(5) 0.058(2) Uani 1 1 d . . . . .
C36 C 0.4176(3) -0.1665(5) 0.3778(4) 0.0447(18) Uani 1 1 d . . . . .
C37 C 0.4207(4) -0.3219(6) 0.3339(6) 0.076(3) Uani 1 1 d . . . . .
H37 H 0.4286 -0.3863 0.3403 0.114 Uiso 1 1 calc R . . . .
C38 C 0.4012(4) -0.2871(6) 0.2696(5) 0.075(3) Uani 1 1 d . . . . .
H38 H 0.3962 -0.3256 0.2320 0.113 Uiso 1 1 calc R . . . .
C39 C 0.3895(3) -0.1899(6) 0.2639(4) 0.059(2) Uani 1 1 d . . . . .
H39 H 0.3748 -0.1649 0.2208 0.070 Uiso 1 1 calc R . . . .
O15 O 0.4172(7) 0.4632(12) 0.2583(9) 0.358(9) Uiso 1 1 d . . . . .
H15A H 0.4208 0.4051 0.2702 0.430 Uiso 1 1 d R . . . .
H15B H 0.4075 0.4604 0.2156 0.430 Uiso 1 1 d R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 N2 2.140(6) . ?
Zn1 N3 2.165(6) . ?
Zn1 N4 2.113(6) . ?
Zn1 N5 2.157(6) . ?
Zn1 O1 2.055(4) . ?
Zn1 O9 2.167(5) . ?
N1 O7 1.236(9) . ?
N1 O8 1.210(8) . ?
N1 C14 1.480(10) . ?
N2 C24 1.339(9) . ?
N2 C27 1.342(10) . ?
N3 C16 1.327(9) . ?
N3 C20 1.356(9) . ?
N4 C28 1.345(9) . ?
N4 C32 1.364(8) . ?
N5 C36 1.340(8) . ?
N5 C39 1.327(9) . ?
O1 C1 1.261(8) . ?
O2 C1 1.232(8) . ?
O3 C5 1.309(8) . ?
O4 C5 1.186(8) . ?
O5 C13 1.260(11) . ?
O6 C13 1.175(10) . ?
C1 C2 1.510(9) . ?
C2 C3 1.400(9) . ?
C2 C8 1.431(9) . ?
C3 C4 1.384(9) . ?
C4 C5 1.475(10) . ?
C4 C6 1.376(9) . ?
C6 C7 1.385(9) . ?
C7 C8 1.392(9) . ?
C8 C9 1.493(9) . ?
C9 C10 1.375(9) . ?
C9 C15 1.390(9) . ?
C10 C11 1.367(9) . ?
C11 C12 1.400(10) . ?
C12 C13 1.535(11) . ?
C12 C14 1.357(10) . ?
C14 C15 1.405(9) . ?
C16 C17 1.441(11) . ?
C17 C18 1.351(11) . ?
C18 C19 1.424(12) . ?
C19 C20 1.428(10) . ?
C19 C21 1.408(11) . ?
C20 C24 1.432(10) . ?
C21 C22 1.321(13) . ?
C22 C23 1.458(13) . ?
C23 C24 1.425(10) . ?
C23 C25 1.397(13) . ?
C25 C26 1.347(13) . ?
C26 C27 1.367(11) . ?
C28 C29 1.432(11) . ?
C29 C30 1.361(11) . ?
C30 C31 1.405(11) . ?
C31 C32 1.394(10) . ?
C31 C33 1.428(11) . ?
C32 C36 1.422(10) . ?
C33 C34 1.332(11) . ?
C34 C35 1.410(12) . ?
C35 C36 1.396(9) . ?
C35 C37 1.405(11) . ?
C37 C38 1.370(12) . ?
C38 C39 1.399(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Zn1 N3 77.2(2) . . ?
N2 Zn1 N5 96.9(2) . . ?
N2 Zn1 O9 93.7(2) . . ?
N3 Zn1 O9 170.7(2) . . ?
N4 Zn1 N2 166.4(2) . . ?
N4 Zn1 N3 91.5(2) . . ?
N4 Zn1 N5 77.0(2) . . ?
N4 Zn1 O9 97.3(2) . . ?
N5 Zn1 N3 97.6(2) . . ?
N5 Zn1 O9 81.6(2) . . ?
O1 Zn1 N2 98.6(2) . . ?
O1 Zn1 N3 100.95(19) . . ?
O1 Zn1 N4 90.8(2) . . ?
O1 Zn1 N5 158.0(2) . . ?
O1 Zn1 O9 81.94(18) . . ?
O7 N1 C14 118.5(8) . . ?
O8 N1 O7 123.3(8) . . ?
O8 N1 C14 118.1(9) . . ?
C24 N2 Zn1 114.4(5) . . ?
C24 N2 C27 117.5(7) . . ?
C27 N2 Zn1 128.1(6) . . ?
C16 N3 Zn1 129.3(5) . . ?
C16 N3 C20 117.7(7) . . ?
C20 N3 Zn1 113.0(5) . . ?
C28 N4 Zn1 126.8(5) . . ?
C28 N4 C32 118.4(7) . . ?
C32 N4 Zn1 114.8(5) . . ?
C36 N5 Zn1 113.8(5) . . ?
C39 N5 Zn1 128.0(5) . . ?
C39 N5 C36 118.0(7) . . ?
C1 O1 Zn1 129.4(5) . . ?
O1 C1 C2 117.6(7) . . ?
O2 C1 O1 125.4(7) . . ?
O2 C1 C2 117.0(7) . . ?
C3 C2 C1 117.1(6) . . ?
C3 C2 C8 118.3(6) . . ?
C8 C2 C1 124.1(6) . . ?
C4 C3 C2 122.2(7) . . ?
C3 C4 C5 118.6(7) . . ?
C6 C4 C3 118.7(7) . . ?
C6 C4 C5 122.7(7) . . ?
O3 C5 C4 113.8(7) . . ?
O4 C5 O3 122.4(7) . . ?
O4 C5 C4 123.8(8) . . ?
C7 C6 C4 121.0(7) . . ?
C6 C7 C8 121.4(7) . . ?
C2 C8 C9 121.2(6) . . ?
C7 C8 C2 118.2(6) . . ?
C7 C8 C9 120.6(6) . . ?
C10 C9 C8 121.1(7) . . ?
C15 C9 C8 120.0(6) . . ?
C15 C9 C10 118.8(7) . . ?
C11 C10 C9 121.5(7) . . ?
C10 C11 C12 121.3(7) . . ?
C11 C12 C13 119.3(8) . . ?
C14 C12 C11 116.5(7) . . ?
C14 C12 C13 124.0(8) . . ?
O5 C13 C12 112.1(9) . . ?
O6 C13 O5 128.3(9) . . ?
O6 C13 C12 119.6(9) . . ?
C12 C14 N1 122.0(7) . . ?
C12 C14 C15 123.6(7) . . ?
C15 C14 N1 114.4(7) . . ?
C9 C15 C14 118.2(7) . . ?
N3 C16 C17 123.0(8) . . ?
C18 C17 C16 119.6(9) . . ?
C17 C18 C19 119.0(9) . . ?
C18 C19 C20 117.5(8) . . ?
C21 C19 C18 122.4(9) . . ?
C21 C19 C20 120.0(9) . . ?
N3 C20 C19 123.1(7) . . ?
N3 C20 C24 117.6(7) . . ?
C24 C20 C19 119.2(8) . . ?
C22 C21 C19 121.3(10) . . ?
C21 C22 C23 121.9(9) . . ?
C24 C23 C22 118.1(9) . . ?
C25 C23 C22 126.5(10) . . ?
C25 C23 C24 115.4(9) . . ?
N2 C24 C20 117.8(7) . . ?
N2 C24 C23 123.0(8) . . ?
C23 C24 C20 119.2(8) . . ?
C26 C25 C23 121.8(9) . . ?
C25 C26 C27 118.5(10) . . ?
C26 C27 N2 123.8(10) . . ?
N4 C28 C29 122.3(8) . . ?
C30 C29 C28 117.0(8) . . ?
C29 C30 C31 122.5(8) . . ?
C30 C31 C33 124.3(9) . . ?
C32 C31 C30 116.5(8) . . ?
C32 C31 C33 119.2(8) . . ?
N4 C32 C31 123.2(8) . . ?
N4 C32 C36 116.8(7) . . ?
C31 C32 C36 120.0(7) . . ?
C34 C33 C31 119.9(9) . . ?
C33 C34 C35 122.8(9) . . ?
C36 C35 C34 118.5(9) . . ?
C36 C35 C37 116.7(8) . . ?
C37 C35 C34 124.8(9) . . ?
N5 C36 C32 117.6(7) . . ?
N5 C36 C35 122.9(7) . . ?
C35 C36 C32 119.6(7) . . ?
C38 C37 C35 121.8(8) . . ?
C37 C38 C39 115.9(9) . . ?
N5 C39 C38 124.7(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 O10 0.82 1.84 2.597(7) 153.2 7
O10 H10A O4 0.85 2.01 2.816(9) 158.7 .

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Zn1 N2 C24 C20 0.9(8) . . . . ?
Zn1 N2 C24 C23 -179.6(5) . . . . ?
Zn1 N2 C27 C26 -177.6(6) . . . . ?
Zn1 N3 C16 C17 179.9(5) . . . . ?
Zn1 N3 C20 C19 177.7(5) . . . . ?
Zn1 N3 C20 C24 -2.6(7) . . . . ?
Zn1 N4 C28 C29 179.3(6) . . . . ?
Zn1 N4 C32 C31 -179.4(6) . . . . ?
Zn1 N4 C32 C36 0.8(8) . . . . ?
Zn1 N5 C36 C32 3.2(8) . . . . ?
Zn1 N5 C36 C35 -176.8(5) . . . . ?
Zn1 N5 C39 C38 173.1(6) . . . . ?
Zn1 O1 C1 O2 -111.2(8) . . . . ?
Zn1 O1 C1 C2 68.2(8) . . . . ?
N1 C14 C15 C9 176.2(6) . . . . ?
N3 C16 C17 C18 3.0(11) . . . . ?
N3 C20 C24 N2 1.2(9) . . . . ?
N3 C20 C24 C23 -178.4(6) . . . . ?
N4 C28 C29 C30 1.1(12) . . . . ?
N4 C32 C36 N5 -2.7(10) . . . . ?
N4 C32 C36 C35 177.2(7) . . . . ?
O1 C1 C2 C3 -124.5(7) . . . . ?
O1 C1 C2 C8 46.8(9) . . . . ?
O2 C1 C2 C3 54.9(9) . . . . ?
O2 C1 C2 C8 -133.7(7) . . . . ?
O7 N1 C14 C12 -152.2(8) . . . . ?
O7 N1 C14 C15 30.2(11) . . . . ?
O8 N1 C14 C12 31.9(11) . . . . ?
O8 N1 C14 C15 -145.7(7) . . . . ?
C1 C2 C3 C4 168.0(6) . . . . ?
C1 C2 C8 C7 -167.3(6) . . . . ?
C1 C2 C8 C9 15.1(9) . . . . ?
C2 C3 C4 C5 -179.2(6) . . . . ?
C2 C3 C4 C6 -0.1(9) . . . . ?
C2 C8 C9 C10 36.0(9) . . . . ?
C2 C8 C9 C15 -148.0(6) . . . . ?
C3 C2 C8 C7 3.9(8) . . . . ?
C3 C2 C8 C9 -173.6(5) . . . . ?
C3 C4 C5 O3 165.3(6) . . . . ?
C3 C4 C5 O4 -12.9(11) . . . . ?
C3 C4 C6 C7 4.0(10) . . . . ?
C4 C6 C7 C8 -3.8(10) . . . . ?
C5 C4 C6 C7 -177.0(6) . . . . ?
C6 C4 C5 O3 -13.7(10) . . . . ?
C6 C4 C5 O4 168.0(7) . . . . ?
C6 C7 C8 C2 -0.3(9) . . . . ?
C6 C7 C8 C9 177.3(6) . . . . ?
C7 C8 C9 C10 -141.6(6) . . . . ?
C7 C8 C9 C15 34.5(9) . . . . ?
C8 C2 C3 C4 -3.8(9) . . . . ?
C8 C9 C10 C11 179.9(6) . . . . ?
C8 C9 C15 C14 -178.6(6) . . . . ?
C9 C10 C11 C12 -1.4(11) . . . . ?
C10 C9 C15 C14 -2.4(10) . . . . ?
C10 C11 C12 C13 172.8(7) . . . . ?
C10 C11 C12 C14 -2.4(11) . . . . ?
C11 C12 C13 O5 58.4(12) . . . . ?
C11 C12 C13 O6 -121.4(10) . . . . ?
C11 C12 C14 N1 -173.6(7) . . . . ?
C11 C12 C14 C15 3.8(11) . . . . ?
C12 C14 C15 C9 -1.5(11) . . . . ?
C13 C12 C14 N1 11.4(12) . . . . ?
C13 C12 C14 C15 -171.2(8) . . . . ?
C14 C12 C13 O5 -126.8(10) . . . . ?
C14 C12 C13 O6 53.4(13) . . . . ?
C15 C9 C10 C11 3.8(10) . . . . ?
C16 N3 C20 C19 -1.4(9) . . . . ?
C16 N3 C20 C24 178.3(6) . . . . ?
C16 C17 C18 C19 -2.0(11) . . . . ?
C17 C18 C19 C20 -0.4(11) . . . . ?
C17 C18 C19 C21 -180.0(7) . . . . ?
C18 C19 C20 N3 2.2(10) . . . . ?
C18 C19 C20 C24 -177.5(6) . . . . ?
C18 C19 C21 C22 176.6(8) . . . . ?
C19 C20 C24 N2 -179.1(6) . . . . ?
C19 C20 C24 C23 1.4(10) . . . . ?
C19 C21 C22 C23 0.4(13) . . . . ?
C20 N3 C16 C17 -1.2(10) . . . . ?
C20 C19 C21 C22 -3.0(12) . . . . ?
C21 C19 C20 N3 -178.2(6) . . . . ?
C21 C19 C20 C24 2.1(10) . . . . ?
C21 C22 C23 C24 3.1(12) . . . . ?
C21 C22 C23 C25 -178.0(8) . . . . ?
C22 C23 C24 N2 176.6(6) . . . . ?
C22 C23 C24 C20 -3.9(10) . . . . ?
C22 C23 C25 C26 -179.9(8) . . . . ?
C23 C25 C26 C27 3.2(14) . . . . ?
C24 N2 C27 C26 -1.0(12) . . . . ?
C24 C23 C25 C26 -1.0(12) . . . . ?
C25 C23 C24 N2 -2.4(11) . . . . ?
C25 C23 C24 C20 177.1(6) . . . . ?
C25 C26 C27 N2 -2.2(13) . . . . ?
C27 N2 C24 C20 -176.1(6) . . . . ?
C27 N2 C24 C23 3.4(10) . . . . ?
C28 N4 C32 C31 0.4(11) . . . . ?
C28 N4 C32 C36 -179.5(6) . . . . ?
C28 C29 C30 C31 -2.0(13) . . . . ?
C29 C30 C31 C32 2.0(13) . . . . ?
C29 C30 C31 C33 179.1(8) . . . . ?
C30 C31 C32 N4 -1.1(11) . . . . ?
C30 C31 C32 C36 178.8(7) . . . . ?
C30 C31 C33 C34 -178.4(9) . . . . ?
C31 C32 C36 N5 177.4(7) . . . . ?
C31 C32 C36 C35 -2.6(11) . . . . ?
C31 C33 C34 C35 2.4(14) . . . . ?
C32 N4 C28 C29 -0.4(11) . . . . ?
C32 C31 C33 C34 -1.3(12) . . . . ?
C33 C31 C32 N4 -178.4(7) . . . . ?
C33 C31 C32 C36 1.5(11) . . . . ?
C33 C34 C35 C36 -3.5(13) . . . . ?
C33 C34 C35 C37 177.2(9) . . . . ?
C34 C35 C36 N5 -176.5(7) . . . . ?
C34 C35 C36 C32 3.5(11) . . . . ?
C34 C35 C37 C38 177.7(9) . . . . ?
C35 C37 C38 C39 -0.9(13) . . . . ?
C36 N5 C39 C38 -1.7(11) . . . . ?
C36 C35 C37 C38 -1.6(13) . . . . ?
C37 C35 C36 N5 2.8(11) . . . . ?
C37 C35 C36 C32 -177.1(7) . . . . ?
C37 C38 C39 N5 2.8(13) . . . . ?
C39 N5 C36 C32 178.7(6) . . . . ?
C39 N5 C36 C35 -1.2(10) . . . . ?

_olex2_date_sample_data_collection 2017-03-18
_olex2_submission_special_instructions 'No special instructions were received'
