# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_400-2Co
_database_code_depnum_ccdc_archive 'CCDC 1984462'
_audit_update_record             
;
2020-02-17 deposited with the CCDC.	2020-05-11 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            'C44 H31 Co N5 O8'
_chemical_formula_weight         816.67

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                   11.3259(8)
_cell_length_b                   13.2252(9)
_cell_length_c                   14.6526(13)
_cell_angle_alpha                67.349(7)
_cell_angle_beta                 76.175(7)
_cell_angle_gamma                65.591(7)
_cell_volume                     1836.1(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    11783
_cell_measurement_theta_min      3.284
_cell_measurement_theta_max      25.049

_exptl_crystal_description       needle
_exptl_crystal_colour            pink
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_F_000             842
_exptl_transmission_factor_min   0.880
_exptl_transmission_factor_max   0.904
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    0.533
_shelx_estimated_absorpt_T_min   0.869
_shelx_estimated_absorpt_T_max   0.906
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.869
_exptl_absorpt_correction_T_max  0.906
_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            11783
_diffrn_reflns_av_unetI/netI     0.0897
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.284
_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             6511
_reflns_number_gt                4370
_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)+(0.0431P)²+0.0114P] 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         6511
_refine_ls_number_parameters     519
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0946
_refine_ls_R_factor_gt           0.0582
_refine_ls_wR_factor_ref         0.1339
_refine_ls_wR_factor_gt          0.1121
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.79781(5) 0.85638(5) 0.70217(4) 0.03568(18) Uani 1 1 d . . . . .
N1 N 1.0287(3) 1.2466(3) 0.6987(2) 0.0341(8) Uani 1 1 d . . . . .
N2 N 0.7528(3) 0.7213(3) 0.6917(2) 0.0381(8) Uani 1 1 d . . . . .
N3 N 0.6037(3) 0.9490(3) 0.6605(2) 0.0373(8) Uani 1 1 d . . . . .
N4 N 0.9796(3) 0.7397(3) 0.7639(2) 0.0396(8) Uani 1 1 d . . . . .
N5 N 0.7414(3) 0.8211(3) 0.8564(2) 0.0376(8) Uani 1 1 d . . . . .
O1 O 0.8232(2) 0.9989(2) 0.70772(18) 0.0403(7) Uani 1 1 d . . . . .
O2 O 0.8905(2) 1.0923(2) 0.55383(17) 0.0379(7) Uani 1 1 d . . . . .
O3 O 1.4717(3) 0.5920(3) 1.1217(2) 0.0721(11) Uani 1 1 d . . . . .
O4 O 1.4151(3) 0.7243(3) 1.1989(2) 0.0588(10) Uani 1 1 d . . . . .
H4 H 1.4649 0.6698 1.2384 0.088 Uiso 1 1 calc R U . . .
O5 O 0.5582(2) 1.5788(3) 0.32903(18) 0.0545(9) Uani 1 1 d . . . . .
O6 O 0.6922(3) 1.6757(3) 0.2921(2) 0.0659(10) Uani 1 1 d . . . . .
O7 O 0.8708(2) 0.9005(2) 0.54909(17) 0.0461(7) Uani 1 1 d . . . . .
H1W H 0.9483 0.8654 0.5257 0.055 Uiso 1 1 d R U . . .
H2W H 0.8740 0.9664 0.5300 0.055 Uiso 1 1 d R U . . .
O8 O 0.3762(4) 0.4369(4) 0.0789(3) 0.1180(14) Uiso 1 1 d . . . . .
H3W H 0.4217 0.4666 0.0945 0.142 Uiso 1 1 d R U . . .
H4W H 0.4180 0.4290 0.0241 0.142 Uiso 1 1 d R U . . .
C1 C 0.8812(3) 1.0651(3) 0.6468(3) 0.0306(9) Uani 1 1 d . . . . .
C2 C 0.9514(3) 1.1060(3) 0.6931(2) 0.0274(8) Uani 1 1 d . . . . .
C3 C 1.0196(3) 1.0238(3) 0.7730(2) 0.0322(9) Uani 1 1 d . . . . .
H3 H 1.0147 0.9493 0.7987 0.039 Uiso 1 1 calc R U . . .
C4 C 1.0952(3) 1.0504(3) 0.8152(3) 0.0326(9) Uani 1 1 d . . . . .
C5 C 1.0966(3) 1.1637(3) 0.7744(3) 0.0372(10) Uani 1 1 d . . . . .
H5 H 1.1478 1.1831 0.8011 0.045 Uiso 1 1 calc R U . . .
C6 C 0.9563(3) 1.2182(3) 0.6583(2) 0.0286(8) Uani 1 1 d . . . . .
C7 C 1.1733(3) 0.9598(3) 0.8975(3) 0.0373(10) Uani 1 1 d . . . . .
C8 C 1.2380(4) 0.8462(4) 0.8952(3) 0.0541(13) Uani 1 1 d . . . . .
H8 H 1.2323 0.8280 0.8415 0.065 Uiso 1 1 calc R U . . .
C9 C 1.3113(4) 0.7588(4) 0.9714(3) 0.0563(13) Uani 1 1 d . . . . .
H9 H 1.3541 0.6830 0.9684 0.068 Uiso 1 1 calc R U . . .
C10 C 1.3207(3) 0.7848(4) 1.0520(3) 0.0415(11) Uani 1 1 d . . . . .
C11 C 1.4096(4) 0.6903(4) 1.1294(3) 0.0475(12) Uani 1 1 d . . . . .
C12 C 1.2543(3) 0.8971(4) 1.0564(3) 0.0438(11) Uani 1 1 d . . . . .
H12 H 1.2584 0.9146 1.1110 0.053 Uiso 1 1 calc R U . . .
C13 C 1.1814(3) 0.9844(4) 0.9796(3) 0.0414(10) Uani 1 1 d . . . . .
H13 H 1.1375 1.0599 0.9831 0.050 Uiso 1 1 calc R U . . .
C14 C 0.8795(3) 1.3153(3) 0.5773(2) 0.0266(8) Uani 1 1 d . . . . .
C15 C 0.7527(3) 1.3278(3) 0.5719(2) 0.0289(9) Uani 1 1 d . . . . .
H15 H 0.7152 1.2764 0.6198 0.035 Uiso 1 1 calc R U . . .
C16 C 0.6831(3) 1.4167(3) 0.4954(2) 0.0298(9) Uani 1 1 d . . . . .
H16 H 0.5997 1.4228 0.4910 0.036 Uiso 1 1 calc R U . . .
C17 C 0.7347(3) 1.4967(3) 0.4254(2) 0.0296(9) Uani 1 1 d . . . . .
C18 C 0.6568(4) 1.5938(3) 0.3418(3) 0.0362(10) Uani 1 1 d . . . . .
C19 C 0.8587(3) 1.4869(3) 0.4317(2) 0.0347(9) Uani 1 1 d . . . . .
H19 H 0.8936 1.5414 0.3856 0.042 Uiso 1 1 calc R U . . .
C20 C 0.9315(3) 1.3960(3) 0.5064(2) 0.0334(9) Uani 1 1 d . . . . .
H20 H 1.0158 1.3889 0.5093 0.040 Uiso 1 1 calc R U . . .
C21 C 0.8245(4) 0.6092(4) 0.7089(3) 0.0495(11) Uani 1 1 d . . . . .
H21 H 0.9069 0.5823 0.7295 0.059 Uiso 1 1 calc R U . . .
C22 C 0.7842(5) 0.5294(4) 0.6982(3) 0.0600(13) Uani 1 1 d . . . . .
H22 H 0.8385 0.4512 0.7111 0.072 Uiso 1 1 calc R U . . .
C23 C 0.6636(5) 0.5669(5) 0.6685(3) 0.0648(14) Uani 1 1 d . . . . .
H23 H 0.6352 0.5141 0.6609 0.078 Uiso 1 1 calc R U . . .
C24 C 0.5830(4) 0.6843(4) 0.6496(3) 0.0472(11) Uani 1 1 d . . . . .
C25 C 0.6312(4) 0.7597(4) 0.6625(3) 0.0385(10) Uani 1 1 d . . . . .
C26 C 0.4552(5) 0.7320(5) 0.6187(3) 0.0607(14) Uani 1 1 d . . . . .
H26 H 0.4231 0.6833 0.6083 0.073 Uiso 1 1 calc R U . . .
C27 C 0.3802(4) 0.8453(5) 0.6042(3) 0.0596(14) Uani 1 1 d . . . . .
H27 H 0.2973 0.8736 0.5841 0.071 Uiso 1 1 calc R U . . .
C28 C 0.4255(4) 0.9228(4) 0.6191(3) 0.0438(11) Uani 1 1 d . . . . .
C29 C 0.5514(3) 0.8810(4) 0.6466(3) 0.0379(10) Uani 1 1 d . . . . .
C30 C 0.3514(4) 1.0407(4) 0.6070(3) 0.0556(13) Uani 1 1 d . . . . .
H30 H 0.2672 1.0722 0.5885 0.067 Uiso 1 1 calc R U . . .
C31 C 0.4016(4) 1.1105(4) 0.6221(3) 0.0527(12) Uani 1 1 d . . . . .
H31 H 0.3523 1.1890 0.6145 0.063 Uiso 1 1 calc R U . . .
C32 C 0.5287(4) 1.0607(4) 0.6491(3) 0.0489(11) Uani 1 1 d . . . . .
H32 H 0.5626 1.1080 0.6597 0.059 Uiso 1 1 calc R U . . .
C33 C 1.0965(4) 0.6981(4) 0.7191(3) 0.0507(11) Uani 1 1 d . . . . .
H33 H 1.1064 0.7208 0.6501 0.061 Uiso 1 1 calc R U . . .
C34 C 1.2059(4) 0.6215(4) 0.7707(4) 0.0542(12) Uani 1 1 d . . . . .
H34 H 1.2860 0.5935 0.7360 0.065 Uiso 1 1 calc R U . . .
C35 C 1.1955(4) 0.5884(4) 0.8705(4) 0.0561(13) Uani 1 1 d . . . . .
H35 H 1.2681 0.5377 0.9051 0.067 Uiso 1 1 calc R U . . .
C36 C 1.0741(4) 0.6309(4) 0.9218(3) 0.0462(11) Uani 1 1 d . . . . .
C37 C 0.9679(4) 0.7059(3) 0.8656(3) 0.0367(9) Uani 1 1 d . . . . .
C38 C 1.0547(5) 0.6010(4) 1.0277(3) 0.0577(13) Uani 1 1 d . . . . .
H38 H 1.1248 0.5514 1.0653 0.069 Uiso 1 1 calc R U . . .
C39 C 0.9355(5) 0.6443(4) 1.0732(3) 0.0578(13) Uani 1 1 d . . . . .
H39 H 0.9253 0.6239 1.1421 0.069 Uiso 1 1 calc R U . . .
C40 C 0.8245(4) 0.7206(4) 1.0187(3) 0.0440(11) Uani 1 1 d . . . . .
C41 C 0.8404(4) 0.7509(3) 0.9143(3) 0.0381(10) Uani 1 1 d . . . . .
C42 C 0.6997(4) 0.7697(4) 1.0613(3) 0.0548(12) Uani 1 1 d . . . . .
H42 H 0.6841 0.7527 1.1298 0.066 Uiso 1 1 calc R U . . .
C43 C 0.6007(4) 0.8426(4) 1.0028(3) 0.0556(13) Uani 1 1 d . . . . .
H43 H 0.5176 0.8764 1.0308 0.067 Uiso 1 1 calc R U . . .
C44 C 0.6253(4) 0.8659(4) 0.9003(3) 0.0500(12) Uani 1 1 d . . . . .
H44 H 0.5567 0.9152 0.8611 0.060 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O1 2.054(3) . ?
Co1 N5 2.117(3) . ?
Co1 N2 2.117(3) . ?
Co1 N3 2.132(3) . ?
Co1 O7 2.135(2) . ?
Co1 N4 2.151(3) . ?
N1 C5 1.340(4) . ?
N1 C6 1.351(4) . ?
N2 C21 1.317(5) . ?
N2 C25 1.368(4) . ?
N3 C32 1.331(5) . ?
N3 C29 1.356(5) . ?
N4 C33 1.322(5) . ?
N4 C37 1.371(4) . ?
N5 C44 1.319(5) . ?
N5 C41 1.351(4) . ?
O1 C1 1.260(4) . ?
O2 C1 1.258(4) . ?
O3 C11 1.231(6) . ?
O4 C11 1.285(6) . ?
O4 H4 0.8200 . ?
O5 C18 1.278(4) . ?
O6 C18 1.214(4) . ?
O7 H1W 0.8642 . ?
O7 H2W 0.8200 . ?
O8 H3W 0.8733 . ?
O8 H4W 0.8500 . ?
C1 C2 1.510(5) . ?
C2 C3 1.380(4) . ?
C2 C6 1.391(5) . ?
C3 C4 1.382(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.388(5) . ?
C4 C7 1.481(4) . ?
C5 H5 0.9300 . ?
C6 C14 1.488(4) . ?
C7 C8 1.383(6) . ?
C7 C13 1.392(6) . ?
C8 C9 1.388(5) . ?
C8 H8 0.9300 . ?
C9 C10 1.389(6) . ?
C9 H9 0.9300 . ?
C10 C12 1.379(6) . ?
C10 C11 1.508(5) . ?
C12 C13 1.392(4) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 C20 1.392(4) . ?
C14 C15 1.394(4) . ?
C15 C16 1.379(4) . ?
C15 H15 0.9300 . ?
C16 C17 1.379(4) . ?
C16 H16 0.9300 . ?
C17 C19 1.378(4) . ?
C17 C18 1.516(4) . ?
C19 C20 1.387(4) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
C21 C22 1.380(6) . ?
C21 H21 0.9300 . ?
C22 C23 1.363(6) . ?
C22 H22 0.9300 . ?
C23 C24 1.393(6) . ?
C23 H23 0.9300 . ?
C24 C25 1.404(5) . ?
C24 C26 1.428(6) . ?
C25 C29 1.435(6) . ?
C26 C27 1.342(7) . ?
C26 H26 0.9300 . ?
C27 C28 1.422(6) . ?
C27 H27 0.9300 . ?
C28 C29 1.398(5) . ?
C28 C30 1.394(6) . ?
C30 C31 1.369(6) . ?
C30 H30 0.9300 . ?
C31 C32 1.397(5) . ?
C31 H31 0.9300 . ?
C32 H32 0.9300 . ?
C33 C34 1.398(5) . ?
C33 H33 0.9300 . ?
C34 C35 1.346(6) . ?
C34 H34 0.9300 . ?
C35 C36 1.402(6) . ?
C35 H35 0.9300 . ?
C36 C37 1.402(5) . ?
C36 C38 1.431(6) . ?
C37 C41 1.440(5) . ?
C38 C39 1.349(6) . ?
C38 H38 0.9300 . ?
C39 C40 1.431(5) . ?
C39 H39 0.9300 . ?
C40 C42 1.393(6) . ?
C40 C41 1.410(5) . ?
C42 C43 1.361(5) . ?
C42 H42 0.9300 . ?
C43 C44 1.393(5) . ?
C43 H43 0.9300 . ?
C44 H44 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 Co1 N5 85.55(11) . . ?
O1 Co1 N2 174.18(11) . . ?
N5 Co1 N2 95.11(12) . . ?
O1 Co1 N3 95.61(11) . . ?
N5 Co1 N3 94.64(12) . . ?
N2 Co1 N3 78.57(12) . . ?
O1 Co1 O7 88.43(10) . . ?
N5 Co1 O7 172.85(11) . . ?
N2 Co1 O7 91.27(11) . . ?
N3 Co1 O7 89.77(10) . . ?
O1 Co1 N4 91.46(11) . . ?
N5 Co1 N4 78.23(12) . . ?
N2 Co1 N4 94.34(12) . . ?
N3 Co1 N4 169.56(11) . . ?
O7 Co1 N4 98.10(11) . . ?
C5 N1 C6 118.3(3) . . ?
C21 N2 C25 117.7(4) . . ?
C21 N2 Co1 129.2(3) . . ?
C25 N2 Co1 113.1(3) . . ?
C32 N3 C29 117.4(3) . . ?
C32 N3 Co1 129.2(3) . . ?
C29 N3 Co1 113.4(3) . . ?
C33 N4 C37 117.3(3) . . ?
C33 N4 Co1 130.1(3) . . ?
C37 N4 Co1 112.6(2) . . ?
C44 N5 C41 117.8(3) . . ?
C44 N5 Co1 127.6(3) . . ?
C41 N5 Co1 114.4(2) . . ?
C1 O1 Co1 131.4(3) . . ?
C11 O4 H4 109.5 . . ?
Co1 O7 H1W 125.1 . . ?
Co1 O7 H2W 109.5 . . ?
H1W O7 H2W 97.6 . . ?
H3W O8 H4W 100.1 . . ?
O2 C1 O1 125.3(3) . . ?
O2 C1 C2 119.5(3) . . ?
O1 C1 C2 115.0(3) . . ?
C3 C2 C6 118.4(3) . . ?
C3 C2 C1 116.9(3) . . ?
C6 C2 C1 124.6(3) . . ?
C4 C3 C2 121.0(3) . . ?
C4 C3 H3 119.5 . . ?
C2 C3 H3 119.5 . . ?
C3 C4 C5 116.6(3) . . ?
C3 C4 C7 120.6(3) . . ?
C5 C4 C7 122.8(3) . . ?
N1 C5 C4 124.0(3) . . ?
N1 C5 H5 118.0 . . ?
C4 C5 H5 118.0 . . ?
N1 C6 C2 121.7(3) . . ?
N1 C6 C14 115.6(3) . . ?
C2 C6 C14 122.7(3) . . ?
C8 C7 C13 118.2(3) . . ?
C8 C7 C4 119.8(4) . . ?
C13 C7 C4 122.0(4) . . ?
C7 C8 C9 121.4(4) . . ?
C7 C8 H8 119.3 . . ?
C9 C8 H8 119.3 . . ?
C10 C9 C8 120.0(4) . . ?
C10 C9 H9 120.0 . . ?
C8 C9 H9 120.0 . . ?
C12 C10 C9 119.3(3) . . ?
C12 C10 C11 122.1(4) . . ?
C9 C10 C11 118.5(4) . . ?
O3 C11 O4 125.5(4) . . ?
O3 C11 C10 120.8(4) . . ?
O4 C11 C10 113.6(4) . . ?
C10 C12 C13 120.4(4) . . ?
C10 C12 H12 119.8 . . ?
C13 C12 H12 119.8 . . ?
C12 C13 C7 120.7(4) . . ?
C12 C13 H13 119.6 . . ?
C7 C13 H13 119.6 . . ?
C20 C14 C15 118.7(3) . . ?
C20 C14 C6 121.0(3) . . ?
C15 C14 C6 120.2(3) . . ?
C16 C15 C14 119.9(3) . . ?
C16 C15 H15 120.1 . . ?
C14 C15 H15 120.1 . . ?
C15 C16 C17 121.2(3) . . ?
C15 C16 H16 119.4 . . ?
C17 C16 H16 119.4 . . ?
C19 C17 C16 119.3(3) . . ?
C19 C17 C18 120.1(3) . . ?
C16 C17 C18 120.6(3) . . ?
O6 C18 O5 125.7(3) . . ?
O6 C18 C17 119.7(3) . . ?
O5 C18 C17 114.6(3) . . ?
C17 C19 C20 120.2(3) . . ?
C17 C19 H19 119.9 . . ?
C20 C19 H19 119.9 . . ?
C19 C20 C14 120.6(3) . . ?
C19 C20 H20 119.7 . . ?
C14 C20 H20 119.7 . . ?
N2 C21 C22 123.6(4) . . ?
N2 C21 H21 118.2 . . ?
C22 C21 H21 118.2 . . ?
C23 C22 C21 119.2(5) . . ?
C23 C22 H22 120.4 . . ?
C21 C22 H22 120.4 . . ?
C22 C23 C24 119.9(5) . . ?
C22 C23 H23 120.1 . . ?
C24 C23 H23 120.1 . . ?
C23 C24 C25 117.4(4) . . ?
C23 C24 C26 124.1(5) . . ?
C25 C24 C26 118.4(4) . . ?
N2 C25 C24 122.2(4) . . ?
N2 C25 C29 117.8(4) . . ?
C24 C25 C29 120.0(4) . . ?
C27 C26 C24 121.7(4) . . ?
C27 C26 H26 119.2 . . ?
C24 C26 H26 119.2 . . ?
C26 C27 C28 121.0(4) . . ?
C26 C27 H27 119.5 . . ?
C28 C27 H27 119.5 . . ?
C29 C28 C30 116.9(4) . . ?
C29 C28 C27 119.4(4) . . ?
C30 C28 C27 123.7(4) . . ?
N3 C29 C28 123.5(4) . . ?
N3 C29 C25 117.1(3) . . ?
C28 C29 C25 119.4(4) . . ?
C31 C30 C28 120.6(4) . . ?
C31 C30 H30 119.7 . . ?
C28 C30 H30 119.7 . . ?
C30 C31 C32 118.4(4) . . ?
C30 C31 H31 120.8 . . ?
C32 C31 H31 120.8 . . ?
N3 C32 C31 123.3(4) . . ?
N3 C32 H32 118.4 . . ?
C31 C32 H32 118.4 . . ?
N4 C33 C34 123.0(4) . . ?
N4 C33 H33 118.5 . . ?
C34 C33 H33 118.5 . . ?
C35 C34 C33 120.1(4) . . ?
C35 C34 H34 120.0 . . ?
C33 C34 H34 120.0 . . ?
C34 C35 C36 119.3(4) . . ?
C34 C35 H35 120.3 . . ?
C36 C35 H35 120.3 . . ?
C37 C36 C35 117.7(4) . . ?
C37 C36 C38 119.4(4) . . ?
C35 C36 C38 122.9(4) . . ?
N4 C37 C36 122.6(4) . . ?
N4 C37 C41 117.3(3) . . ?
C36 C37 C41 120.1(4) . . ?
C39 C38 C36 120.4(4) . . ?
C39 C38 H38 119.8 . . ?
C36 C38 H38 119.8 . . ?
C38 C39 C40 122.0(4) . . ?
C38 C39 H39 119.0 . . ?
C40 C39 H39 119.0 . . ?
C42 C40 C41 116.5(4) . . ?
C42 C40 C39 124.7(4) . . ?
C41 C40 C39 118.8(4) . . ?
N5 C41 C40 123.3(4) . . ?
N5 C41 C37 117.5(3) . . ?
C40 C41 C37 119.2(3) . . ?
C43 C42 C40 120.1(4) . . ?
C43 C42 H42 119.9 . . ?
C40 C42 H42 119.9 . . ?
C42 C43 C44 119.3(4) . . ?
C42 C43 H43 120.4 . . ?
C44 C43 H43 120.4 . . ?
N5 C44 C43 122.9(4) . . ?
N5 C44 H44 118.5 . . ?
C43 C44 H44 118.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Co1 O1 C1 O2 32.3(5) . . . . ?
Co1 O1 C1 C2 -143.3(3) . . . . ?
O2 C1 C2 C3 -134.1(4) . . . . ?
O1 C1 C2 C3 41.7(4) . . . . ?
O2 C1 C2 C6 43.0(5) . . . . ?
O1 C1 C2 C6 -141.1(4) . . . . ?
C6 C2 C3 C4 -2.4(5) . . . . ?
C1 C2 C3 C4 174.9(3) . . . . ?
C2 C3 C4 C5 1.1(5) . . . . ?
C2 C3 C4 C7 -176.9(3) . . . . ?
C6 N1 C5 C4 -1.3(5) . . . . ?
C3 C4 C5 N1 0.9(6) . . . . ?
C7 C4 C5 N1 178.8(4) . . . . ?
C5 N1 C6 C2 -0.2(5) . . . . ?
C5 N1 C6 C14 177.8(3) . . . . ?
C3 C2 C6 N1 2.0(5) . . . . ?
C1 C2 C6 N1 -175.1(3) . . . . ?
C3 C2 C6 C14 -175.8(3) . . . . ?
C1 C2 C6 C14 7.1(5) . . . . ?
C3 C4 C7 C8 40.1(5) . . . . ?
C5 C4 C7 C8 -137.7(4) . . . . ?
C3 C4 C7 C13 -138.2(4) . . . . ?
C5 C4 C7 C13 44.0(5) . . . . ?
C13 C7 C8 C9 -1.2(6) . . . . ?
C4 C7 C8 C9 -179.5(4) . . . . ?
C7 C8 C9 C10 0.0(7) . . . . ?
C8 C9 C10 C12 1.4(6) . . . . ?
C8 C9 C10 C11 -175.2(4) . . . . ?
C12 C10 C11 O3 -177.1(4) . . . . ?
C9 C10 C11 O3 -0.6(6) . . . . ?
C12 C10 C11 O4 1.0(6) . . . . ?
C9 C10 C11 O4 177.5(4) . . . . ?
C9 C10 C12 C13 -1.7(6) . . . . ?
C11 C10 C12 C13 174.9(3) . . . . ?
C10 C12 C13 C7 0.5(6) . . . . ?
C8 C7 C13 C12 0.9(6) . . . . ?
C4 C7 C13 C12 179.3(3) . . . . ?
N1 C6 C14 C20 39.8(5) . . . . ?
C2 C6 C14 C20 -142.2(4) . . . . ?
N1 C6 C14 C15 -139.3(4) . . . . ?
C2 C6 C14 C15 38.7(5) . . . . ?
C20 C14 C15 C16 2.2(6) . . . . ?
C6 C14 C15 C16 -178.7(3) . . . . ?
C14 C15 C16 C17 -2.3(6) . . . . ?
C15 C16 C17 C19 0.5(6) . . . . ?
C15 C16 C17 C18 180.0(4) . . . . ?
C19 C17 C18 O6 -14.3(6) . . . . ?
C16 C17 C18 O6 166.3(4) . . . . ?
C19 C17 C18 O5 164.1(4) . . . . ?
C16 C17 C18 O5 -15.3(5) . . . . ?
C16 C17 C19 C20 1.4(6) . . . . ?
C18 C17 C19 C20 -178.1(4) . . . . ?
C17 C19 C20 C14 -1.5(6) . . . . ?
C15 C14 C20 C19 -0.3(6) . . . . ?
C6 C14 C20 C19 -179.4(4) . . . . ?
C25 N2 C21 C22 0.7(6) . . . . ?
Co1 N2 C21 C22 -179.2(3) . . . . ?
N2 C21 C22 C23 -0.2(7) . . . . ?
C21 C22 C23 C24 -0.1(7) . . . . ?
C22 C23 C24 C25 -0.1(6) . . . . ?
C22 C23 C24 C26 -179.7(4) . . . . ?
C21 N2 C25 C24 -0.8(5) . . . . ?
Co1 N2 C25 C24 179.1(3) . . . . ?
C21 N2 C25 C29 178.1(3) . . . . ?
Co1 N2 C25 C29 -2.0(4) . . . . ?
C23 C24 C25 N2 0.5(6) . . . . ?
C26 C24 C25 N2 -179.8(3) . . . . ?
C23 C24 C25 C29 -178.4(4) . . . . ?
C26 C24 C25 C29 1.3(6) . . . . ?
C23 C24 C26 C27 178.0(5) . . . . ?
C25 C24 C26 C27 -1.6(7) . . . . ?
C24 C26 C27 C28 0.1(7) . . . . ?
C26 C27 C28 C29 1.8(7) . . . . ?
C26 C27 C28 C30 -178.9(4) . . . . ?
C32 N3 C29 C28 1.5(6) . . . . ?
Co1 N3 C29 C28 180.0(3) . . . . ?
C32 N3 C29 C25 -177.8(3) . . . . ?
Co1 N3 C29 C25 0.6(4) . . . . ?
C30 C28 C29 N3 -0.8(6) . . . . ?
C27 C28 C29 N3 178.6(4) . . . . ?
C30 C28 C29 C25 178.6(4) . . . . ?
C27 C28 C29 C25 -2.0(6) . . . . ?
N2 C25 C29 N3 0.9(5) . . . . ?
C24 C25 C29 N3 179.9(3) . . . . ?
N2 C25 C29 C28 -178.5(3) . . . . ?
C24 C25 C29 C28 0.5(6) . . . . ?
C29 C28 C30 C31 -0.2(6) . . . . ?
C27 C28 C30 C31 -179.6(4) . . . . ?
C28 C30 C31 C32 0.5(6) . . . . ?
C29 N3 C32 C31 -1.3(6) . . . . ?
Co1 N3 C32 C31 -179.5(3) . . . . ?
C30 C31 C32 N3 0.3(6) . . . . ?
C37 N4 C33 C34 0.7(6) . . . . ?
Co1 N4 C33 C34 -179.6(3) . . . . ?
N4 C33 C34 C35 -1.0(7) . . . . ?
C33 C34 C35 C36 0.3(7) . . . . ?
C34 C35 C36 C37 0.8(6) . . . . ?
C34 C35 C36 C38 -179.4(4) . . . . ?
C33 N4 C37 C36 0.4(6) . . . . ?
Co1 N4 C37 C36 -179.3(3) . . . . ?
C33 N4 C37 C41 -179.7(4) . . . . ?
Co1 N4 C37 C41 0.5(4) . . . . ?
C35 C36 C37 N4 -1.2(6) . . . . ?
C38 C36 C37 N4 179.0(4) . . . . ?
C35 C36 C37 C41 179.0(4) . . . . ?
C38 C36 C37 C41 -0.8(6) . . . . ?
C37 C36 C38 C39 0.1(7) . . . . ?
C35 C36 C38 C39 -179.8(4) . . . . ?
C36 C38 C39 C40 0.2(7) . . . . ?
C38 C39 C40 C42 -178.7(5) . . . . ?
C38 C39 C40 C41 0.3(7) . . . . ?
C44 N5 C41 C40 2.1(6) . . . . ?
Co1 N5 C41 C40 177.4(3) . . . . ?
C44 N5 C41 C37 -177.7(4) . . . . ?
Co1 N5 C41 C37 -2.4(4) . . . . ?
C42 C40 C41 N5 -1.7(6) . . . . ?
C39 C40 C41 N5 179.2(4) . . . . ?
C42 C40 C41 C37 178.0(4) . . . . ?
C39 C40 C41 C37 -1.0(6) . . . . ?
N4 C37 C41 N5 1.3(5) . . . . ?
C36 C37 C41 N5 -178.9(4) . . . . ?
N4 C37 C41 C40 -178.5(4) . . . . ?
C36 C37 C41 C40 1.3(6) . . . . ?
C41 C40 C42 C43 0.2(6) . . . . ?
C39 C40 C42 C43 179.2(4) . . . . ?
C40 C42 C43 C44 0.9(7) . . . . ?
C41 N5 C44 C43 -0.9(6) . . . . ?
Co1 N5 C44 C43 -175.5(3) . . . . ?
C42 C43 C44 N5 -0.6(7) . . . . ?

_refine_diff_density_max         0.371
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.061

####################################################################### 
# 
# 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_400-12Zn
_database_code_depnum_ccdc_archive 'CCDC 1984466'
_audit_update_record             
;
2020-02-17 deposited with the CCDC.	2020-05-11 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 H58 N6 O22 Zn2'
_chemical_formula_weight         1345.86

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 '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                   9.0097(4)
_cell_length_b                   12.2876(5)
_cell_length_c                   14.0100(7)
_cell_angle_alpha                98.691(4)
_cell_angle_beta                 103.242(4)
_cell_angle_gamma                94.766(3)
_cell_volume                     1481.23(12)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8672
_cell_measurement_theta_min      3.666
_cell_measurement_theta_max      64.992

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_F_000             696
_exptl_transmission_factor_min   0.680
_exptl_transmission_factor_max   0.706
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    1.738
_shelx_estimated_absorpt_T_min   0.671
_shelx_estimated_absorpt_T_max   0.723
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.671
_exptl_absorpt_correction_T_max  0.723
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\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            8672
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_av_R_equivalents  0.0224
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.666
_diffrn_reflns_theta_max         64.992
_diffrn_reflns_theta_full        64.992
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measured_fraction_theta_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_point_group_measured_fraction_full 0.960
_reflns_number_total             4851
_reflns_number_gt                4355
_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)+(0.0580P)²+0.4531P] 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         4851
_refine_ls_number_parameters     407
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0340
_refine_ls_wR_factor_ref         0.1015
_refine_ls_wR_factor_gt          0.0972
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.053
_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 0.64124(3) 0.83656(2) 0.71956(2) 0.02906(11) Uani 1 1 d . . . . .
N1 N 0.6877(2) 0.06513(15) 0.98409(13) 0.0305(4) Uani 1 1 d . . . . .
N2 N 0.6416(2) 1.00147(15) 0.69031(13) 0.0302(4) Uani 1 1 d . . . . .
N3 N 0.4213(2) 0.83200(16) 0.61848(13) 0.0337(4) Uani 1 1 d . . . . .
O1 O 0.63088(19) 0.67806(13) 0.75207(12) 0.0373(4) Uani 1 1 d . . . . .
O2 O 0.4305(2) 0.67392(15) 0.82003(17) 0.0520(5) Uani 1 1 d . . . . .
O3 O 1.13537(16) 0.12995(13) 1.18945(11) 0.0320(3) Uani 1 1 d . . . . .
O4 O 1.0294(2) 0.26086(15) 1.26986(12) 0.0479(5) Uani 1 1 d . . . . .
O5 O 0.8979(2) -0.39550(14) 1.20635(14) 0.0437(4) Uani 1 1 d . . . . .
H5 H 0.8865 -0.4492 1.2335 0.066 Uiso 1 1 calc R U . . .
O6 O 0.8202(2) -0.30693(15) 1.33390(13) 0.0504(5) Uani 1 1 d . . . . .
O7 O 0.73771(19) 0.78407(15) 0.59196(12) 0.0417(4) Uani 1 1 d . . . . .
H1W H 0.8202 0.7672 0.6206 0.050 Uiso 1 1 d R U . . .
H2W H 0.6884 0.7261 0.5589 0.050 Uiso 1 1 d R U . . .
O8 O 0.53023(18) 0.89163(13) 0.83519(11) 0.0363(4) Uani 1 1 d . . . . .
H3W H 0.5854 0.9293 0.8881 0.044 Uiso 1 1 d R U . . .
H4W H 0.4856 0.8378 0.8495 0.044 Uiso 1 1 d R U . . .
O9 O 0.8573(2) 0.43062(15) 0.28328(16) 0.0541(5) Uani 1 1 d . . . . .
H6W H 0.7629 0.3983 0.2591 0.065 Uiso 1 1 d R U . . .
H5W H 0.9224 0.3856 0.2750 0.065 Uiso 1 1 d R U . . .
O10 O 0.6398(3) 0.5914(2) 0.44504(16) 0.0782(7) Uani 1 1 d . . . . .
H7W H 0.6945 0.5977 0.4051 0.094 Uiso 1 1 d R U . . .
H8W H 0.5487 0.5716 0.4178 0.094 Uiso 1 1 d R U . . .
O11 O 0.6751(3) 0.4891(2) 0.61484(18) 0.0834(8) Uani 1 1 d . . . . .
H9W H 0.6622 0.5444 0.6553 0.100 Uiso 1 1 d R U . . .
H10W H 0.6646 0.5197 0.5635 0.100 Uiso 1 1 d R U . . .
C1 C 0.5485(2) 0.63745(18) 0.80327(17) 0.0327(5) Uani 1 1 d . . . . .
C2 C 0.5990(2) 0.53787(18) 0.84671(15) 0.0298(4) Uani 1 1 d . . . . .
C3 C 0.4935(3) 0.46651(19) 0.87295(17) 0.0354(5) Uani 1 1 d . . . . .
H3 H 0.3915 0.4802 0.8630 0.043 Uiso 1 1 calc R U . . .
C4 C 0.5384(3) 0.37568(19) 0.91355(17) 0.0352(5) Uani 1 1 d . . . . .
H4 H 0.4653 0.3266 0.9275 0.042 Uiso 1 1 calc R U . . .
C5 C 0.6906(2) 0.35628(17) 0.93389(14) 0.0274(4) Uani 1 1 d . . . . .
C6 C 0.7976(2) 0.42917(19) 0.90965(17) 0.0338(5) Uani 1 1 d . . . . .
H6 H 0.9007 0.4182 0.9238 0.041 Uiso 1 1 calc R U . . .
C7 C 0.7515(3) 0.51750(19) 0.86484(17) 0.0348(5) Uani 1 1 d . . . . .
H7A H 0.8232 0.5638 0.8466 0.042 Uiso 1 1 calc R U . . .
C8 C 0.7366(2) 0.25991(18) 0.98034(15) 0.0280(4) Uani 1 1 d . . . . .
C9 C 0.6554(2) 0.15445(18) 0.94369(15) 0.0310(5) Uani 1 1 d . . . . .
H9 H 0.5738 0.1460 0.8877 0.037 Uiso 1 1 calc R U . . .
C10 C 0.8044(2) 0.07600(17) 1.06545(15) 0.0267(4) Uani 1 1 d . . . . .
C11 C 0.8956(2) 0.17731(18) 1.10613(15) 0.0267(4) Uani 1 1 d . . . . .
C12 C 1.0306(2) 0.19038(18) 1.19630(15) 0.0286(4) Uani 1 1 d . . . . .
C13 C 0.8597(2) 0.26891(18) 1.06297(15) 0.0294(4) Uani 1 1 d . . . . .
H13 H 0.9186 0.3372 1.0894 0.035 Uiso 1 1 calc R U . . .
C14 C 0.8232(2) -0.02421(18) 1.11258(15) 0.0279(4) Uani 1 1 d . . . . .
C15 C 0.8384(3) -0.12522(19) 1.05846(16) 0.0331(5) Uani 1 1 d . . . . .
H15 H 0.8403 -0.1305 0.9918 0.040 Uiso 1 1 calc R U . . .
C16 C 0.8508(3) -0.21856(18) 1.10332(16) 0.0332(5) Uani 1 1 d . . . . .
H16 H 0.8632 -0.2857 1.0671 0.040 Uiso 1 1 calc R U . . .
C17 C 0.8447(2) -0.21156(18) 1.20261(16) 0.0295(4) Uani 1 1 d . . . . .
C18 C 0.8526(3) -0.30909(19) 1.25433(17) 0.0337(5) Uani 1 1 d . . . . .
C19 C 0.8274(3) -0.11087(19) 1.25577(16) 0.0333(5) Uani 1 1 d . . . . .
H19 H 0.8220 -0.1061 1.3218 0.040 Uiso 1 1 calc R U . . .
C20 C 0.8179(3) -0.01768(19) 1.21199(16) 0.0340(5) Uani 1 1 d . . . . .
H20 H 0.8080 0.0497 1.2488 0.041 Uiso 1 1 calc R U . . .
C21 C 0.7572(3) 1.08348(19) 0.73063(17) 0.0360(5) Uani 1 1 d . . . . .
H21 H 0.8490 1.0663 0.7678 0.043 Uiso 1 1 calc R U . . .
C22 C 0.7452(3) 1.1918(2) 0.7191(2) 0.0437(6) Uani 1 1 d . . . . .
H22 H 0.8272 1.2468 0.7481 0.052 Uiso 1 1 calc R U . . .
C23 C 0.6099(3) 1.2170(2) 0.6640(2) 0.0490(6) Uani 1 1 d . . . . .
H23 H 0.5988 1.2898 0.6556 0.059 Uiso 1 1 calc R U . . .
C24 C 0.4906(3) 1.1338(2) 0.6214(2) 0.0440(6) Uani 1 1 d . . . . .
H24 H 0.3985 1.1497 0.5835 0.053 Uiso 1 1 calc R U . . .
C25 C 0.5096(3) 1.02571(19) 0.63561(15) 0.0312(5) Uani 1 1 d . . . . .
C26 C 0.3869(3) 0.93048(19) 0.59326(15) 0.0315(5) Uani 1 1 d . . . . .
C27 C 0.2457(3) 0.9406(2) 0.53257(17) 0.0446(6) Uani 1 1 d . . . . .
H27 H 0.2245 1.0082 0.5139 0.054 Uiso 1 1 calc R U . . .
C28 C 0.1369(3) 0.8483(3) 0.5003(2) 0.0588(8) Uani 1 1 d . . . . .
H28 H 0.0406 0.8538 0.4607 0.071 Uiso 1 1 calc R U . . .
C29 C 0.1712(3) 0.7486(3) 0.5267(2) 0.0586(8) Uani 1 1 d . . . . .
H29 H 0.0988 0.6859 0.5060 0.070 Uiso 1 1 calc R U . . .
C30 C 0.3156(3) 0.7435(2) 0.58495(19) 0.0465(6) Uani 1 1 d . . . . .
H30 H 0.3402 0.6756 0.6015 0.056 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O1 2.0655(15) . ?
Zn1 O3 2.0913(15) 2_767 ?
Zn1 N2 2.1271(18) . ?
Zn1 N3 2.1465(19) . ?
Zn1 O8 2.1463(15) . ?
Zn1 O7 2.1963(16) . ?
N1 C9 1.332(3) . ?
N1 C10 1.343(3) . ?
N2 C25 1.342(3) . ?
N2 C21 1.343(3) . ?
N3 C30 1.334(3) . ?
N3 C26 1.351(3) . ?
O1 C1 1.267(3) . ?
O2 C1 1.245(3) . ?
O3 C12 1.260(3) . ?
O3 Zn1 2.0913(14) 2_767 ?
O4 C12 1.244(3) . ?
O5 C18 1.314(3) . ?
O5 H5 0.8200 . ?
O6 C18 1.212(3) . ?
O7 H1W 0.8190 . ?
O7 H2W 0.8200 . ?
O8 H3W 0.8373 . ?
O8 H4W 0.8200 . ?
O9 H6W 0.8760 . ?
O9 H5W 0.8532 . ?
O10 H7W 0.8345 . ?
O10 H8W 0.8209 . ?
O11 H9W 0.8500 . ?
O11 H10W 0.8500 . ?
C1 C2 1.505(3) . ?
C2 C3 1.388(3) . ?
C2 C7 1.390(3) . ?
C3 C4 1.376(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.383(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.395(3) . ?
C5 C8 1.479(3) . ?
C6 C7 1.380(3) . ?
C6 H6 0.9300 . ?
C7 H7A 0.9300 . ?
C8 C13 1.391(3) . ?
C8 C9 1.396(3) . ?
C9 H9 0.9300 . ?
C10 C11 1.397(3) . ?
C10 C14 1.487(3) . ?
C11 C13 1.383(3) . ?
C11 C12 1.518(3) . ?
C13 H13 0.9300 . ?
C14 C15 1.388(3) . ?
C14 C20 1.395(3) . ?
C15 C16 1.389(3) . ?
C15 H15 0.9300 . ?
C16 C17 1.395(3) . ?
C16 H16 0.9300 . ?
C17 C19 1.384(3) . ?
C17 C18 1.490(3) . ?
C19 C20 1.378(3) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
C21 C22 1.374(3) . ?
C21 H21 0.9300 . ?
C22 C23 1.372(4) . ?
C22 H22 0.9300 . ?
C23 C24 1.377(4) . ?
C23 H23 0.9300 . ?
C24 C25 1.391(3) . ?
C24 H24 0.9300 . ?
C25 C26 1.489(3) . ?
C26 C27 1.386(3) . ?
C27 C28 1.381(4) . ?
C27 H27 0.9300 . ?
C28 C29 1.372(5) . ?
C28 H28 0.9300 . ?
C29 C30 1.380(4) . ?
C29 H29 0.9300 . ?
C30 H30 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Zn1 O3 88.88(6) . 2_767 ?
O1 Zn1 N2 176.70(6) . . ?
O3 Zn1 N2 92.55(7) 2_767 . ?
O1 Zn1 N3 101.83(7) . . ?
O3 Zn1 N3 169.18(7) 2_767 . ?
N2 Zn1 N3 76.85(7) . . ?
O1 Zn1 O8 90.96(6) . . ?
O3 Zn1 O8 95.55(6) 2_767 . ?
N2 Zn1 O8 85.94(6) . . ?
N3 Zn1 O8 85.94(7) . . ?
O1 Zn1 O7 91.44(6) . . ?
O3 Zn1 O7 88.89(6) 2_767 . ?
N2 Zn1 O7 91.56(7) . . ?
N3 Zn1 O7 89.27(7) . . ?
O8 Zn1 O7 174.99(6) . . ?
C9 N1 C10 118.81(18) . . ?
C25 N2 C21 118.9(2) . . ?
C25 N2 Zn1 116.10(15) . . ?
C21 N2 Zn1 124.68(16) . . ?
C30 N3 C26 118.9(2) . . ?
C30 N3 Zn1 125.71(17) . . ?
C26 N3 Zn1 115.29(15) . . ?
C1 O1 Zn1 127.21(15) . . ?
C12 O3 Zn1 124.21(14) . 2_767 ?
C18 O5 H5 109.5 . . ?
Zn1 O7 H1W 100.4 . . ?
Zn1 O7 H2W 109.5 . . ?
H1W O7 H2W 105.9 . . ?
Zn1 O8 H3W 117.3 . . ?
Zn1 O8 H4W 109.4 . . ?
H3W O8 H4W 107.7 . . ?
H6W O9 H5W 111.3 . . ?
H7W O10 H8W 113.5 . . ?
H9W O11 H10W 97.8 . . ?
O2 C1 O1 124.9(2) . . ?
O2 C1 C2 118.3(2) . . ?
O1 C1 C2 116.83(19) . . ?
C3 C2 C7 118.7(2) . . ?
C3 C2 C1 120.0(2) . . ?
C7 C2 C1 121.30(19) . . ?
C4 C3 C2 120.5(2) . . ?
C4 C3 H3 119.7 . . ?
C2 C3 H3 119.7 . . ?
C3 C4 C5 121.0(2) . . ?
C3 C4 H4 119.5 . . ?
C5 C4 H4 119.5 . . ?
C4 C5 C6 118.5(2) . . ?
C4 C5 C8 119.97(19) . . ?
C6 C5 C8 121.49(19) . . ?
C7 C6 C5 120.5(2) . . ?
C7 C6 H6 119.8 . . ?
C5 C6 H6 119.8 . . ?
C6 C7 C2 120.6(2) . . ?
C6 C7 H7A 119.7 . . ?
C2 C7 H7A 119.7 . . ?
C13 C8 C9 116.41(19) . . ?
C13 C8 C5 122.59(19) . . ?
C9 C8 C5 120.99(19) . . ?
N1 C9 C8 123.94(19) . . ?
N1 C9 H9 118.0 . . ?
C8 C9 H9 118.0 . . ?
N1 C10 C11 121.65(19) . . ?
N1 C10 C14 115.76(18) . . ?
C11 C10 C14 122.47(19) . . ?
C13 C11 C10 118.45(19) . . ?
C13 C11 C12 119.18(19) . . ?
C10 C11 C12 122.37(19) . . ?
O4 C12 O3 125.7(2) . . ?
O4 C12 C11 117.32(19) . . ?
O3 C12 C11 116.99(18) . . ?
C11 C13 C8 120.7(2) . . ?
C11 C13 H13 119.7 . . ?
C8 C13 H13 119.7 . . ?
C15 C14 C20 119.4(2) . . ?
C15 C14 C10 121.37(18) . . ?
C20 C14 C10 119.17(19) . . ?
C16 C15 C14 120.32(19) . . ?
C16 C15 H15 119.8 . . ?
C14 C15 H15 119.8 . . ?
C15 C16 C17 120.0(2) . . ?
C15 C16 H16 120.0 . . ?
C17 C16 H16 120.0 . . ?
C19 C17 C16 119.4(2) . . ?
C19 C17 C18 117.86(19) . . ?
C16 C17 C18 122.7(2) . . ?
O6 C18 O5 124.0(2) . . ?
O6 C18 C17 121.9(2) . . ?
O5 C18 C17 114.10(19) . . ?
C20 C19 C17 120.73(19) . . ?
C20 C19 H19 119.6 . . ?
C17 C19 H19 119.6 . . ?
C19 C20 C14 120.2(2) . . ?
C19 C20 H20 119.9 . . ?
C14 C20 H20 119.9 . . ?
N2 C21 C22 122.6(2) . . ?
N2 C21 H21 118.7 . . ?
C22 C21 H21 118.7 . . ?
C23 C22 C21 118.7(2) . . ?
C23 C22 H22 120.6 . . ?
C21 C22 H22 120.6 . . ?
C22 C23 C24 119.5(2) . . ?
C22 C23 H23 120.3 . . ?
C24 C23 H23 120.3 . . ?
C23 C24 C25 119.2(2) . . ?
C23 C24 H24 120.4 . . ?
C25 C24 H24 120.4 . . ?
N2 C25 C24 121.1(2) . . ?
N2 C25 C26 115.74(19) . . ?
C24 C25 C26 123.1(2) . . ?
N3 C26 C27 121.4(2) . . ?
N3 C26 C25 115.56(19) . . ?
C27 C26 C25 123.1(2) . . ?
C28 C27 C26 118.8(3) . . ?
C28 C27 H27 120.6 . . ?
C26 C27 H27 120.6 . . ?
C29 C28 C27 119.8(3) . . ?
C29 C28 H28 120.1 . . ?
C27 C28 H28 120.1 . . ?
C28 C29 C30 118.4(3) . . ?
C28 C29 H29 120.8 . . ?
C30 C29 H29 120.8 . . ?
N3 C30 C29 122.7(3) . . ?
N3 C30 H30 118.7 . . ?
C29 C30 H30 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 O1 C1 O2 20.9(3) . . . . ?
Zn1 O1 C1 C2 -158.98(15) . . . . ?
O2 C1 C2 C3 22.4(3) . . . . ?
O1 C1 C2 C3 -157.8(2) . . . . ?
O2 C1 C2 C7 -155.2(2) . . . . ?
O1 C1 C2 C7 24.6(3) . . . . ?
C7 C2 C3 C4 -1.8(3) . . . . ?
C1 C2 C3 C4 -179.4(2) . . . . ?
C2 C3 C4 C5 3.3(4) . . . . ?
C3 C4 C5 C6 -1.9(3) . . . . ?
C3 C4 C5 C8 178.2(2) . . . . ?
C4 C5 C6 C7 -1.1(3) . . . . ?
C8 C5 C6 C7 178.9(2) . . . . ?
C5 C6 C7 C2 2.5(4) . . . . ?
C3 C2 C7 C6 -1.1(3) . . . . ?
C1 C2 C7 C6 176.5(2) . . . . ?
C4 C5 C8 C13 -130.8(2) . . . . ?
C6 C5 C8 C13 49.3(3) . . . . ?
C4 C5 C8 C9 48.1(3) . . . . ?
C6 C5 C8 C9 -131.9(2) . . . . ?
C10 N1 C9 C8 0.5(3) . . . . ?
C13 C8 C9 N1 1.2(3) . . . . ?
C5 C8 C9 N1 -177.68(19) . . . . ?
C9 N1 C10 C11 -2.4(3) . . . . ?
C9 N1 C10 C14 173.78(18) . . . . ?
N1 C10 C11 C13 2.5(3) . . . . ?
C14 C10 C11 C13 -173.46(18) . . . . ?
N1 C10 C11 C12 -178.27(19) . . . . ?
C14 C10 C11 C12 5.8(3) . . . . ?
Zn1 O3 C12 O4 -18.7(3) 2_767 . . . ?
Zn1 O3 C12 C11 160.09(13) 2_767 . . . ?
C13 C11 C12 O4 56.2(3) . . . . ?
C10 C11 C12 O4 -123.0(2) . . . . ?
C13 C11 C12 O3 -122.7(2) . . . . ?
C10 C11 C12 O3 58.1(3) . . . . ?
C10 C11 C13 C8 -0.6(3) . . . . ?
C12 C11 C13 C8 -179.89(19) . . . . ?
C9 C8 C13 C11 -1.1(3) . . . . ?
C5 C8 C13 C11 177.77(19) . . . . ?
N1 C10 C14 C15 54.8(3) . . . . ?
C11 C10 C14 C15 -129.0(2) . . . . ?
N1 C10 C14 C20 -122.0(2) . . . . ?
C11 C10 C14 C20 54.2(3) . . . . ?
C20 C14 C15 C16 -1.1(3) . . . . ?
C10 C14 C15 C16 -177.9(2) . . . . ?
C14 C15 C16 C17 1.4(3) . . . . ?
C15 C16 C17 C19 -0.5(3) . . . . ?
C15 C16 C17 C18 178.2(2) . . . . ?
C19 C17 C18 O6 12.0(3) . . . . ?
C16 C17 C18 O6 -166.7(2) . . . . ?
C19 C17 C18 O5 -167.7(2) . . . . ?
C16 C17 C18 O5 13.6(3) . . . . ?
C16 C17 C19 C20 -0.8(3) . . . . ?
C18 C17 C19 C20 -179.5(2) . . . . ?
C17 C19 C20 C14 1.1(4) . . . . ?
C15 C14 C20 C19 -0.2(3) . . . . ?
C10 C14 C20 C19 176.7(2) . . . . ?
C25 N2 C21 C22 0.8(3) . . . . ?
Zn1 N2 C21 C22 -171.94(17) . . . . ?
N2 C21 C22 C23 -0.2(4) . . . . ?
C21 C22 C23 C24 -0.4(4) . . . . ?
C22 C23 C24 C25 0.4(4) . . . . ?
C21 N2 C25 C24 -0.8(3) . . . . ?
Zn1 N2 C25 C24 172.54(17) . . . . ?
C21 N2 C25 C26 179.91(18) . . . . ?
Zn1 N2 C25 C26 -6.7(2) . . . . ?
C23 C24 C25 N2 0.2(4) . . . . ?
C23 C24 C25 C26 179.5(2) . . . . ?
C30 N3 C26 C27 -0.9(3) . . . . ?
Zn1 N3 C26 C27 -176.75(17) . . . . ?
C30 N3 C26 C25 178.6(2) . . . . ?
Zn1 N3 C26 C25 2.7(2) . . . . ?
N2 C25 C26 N3 2.6(3) . . . . ?
C24 C25 C26 N3 -176.7(2) . . . . ?
N2 C25 C26 C27 -177.9(2) . . . . ?
C24 C25 C26 C27 2.8(3) . . . . ?
N3 C26 C27 C28 2.1(3) . . . . ?
C25 C26 C27 C28 -177.3(2) . . . . ?
C26 C27 C28 C29 -1.4(4) . . . . ?
C27 C28 C29 C30 -0.5(4) . . . . ?
C26 N3 C30 C29 -1.1(4) . . . . ?
Zn1 N3 C30 C29 174.3(2) . . . . ?
C28 C29 C30 N3 1.8(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
C21 H21 O3 0.93 2.58 3.144(3) 119.6 2_767
O11 H10W O10 0.85 1.97 2.822(3) 179.6 .
O11 H9W O1 0.85 2.05 2.898(3) 179.7 .
O10 H8W O11 0.82 2.01 2.814(4) 165.0 2_666
O10 H7W O6 0.83 2.07 2.836(3) 151.5 1_564
O9 H5W O4 0.85 1.88 2.710(2) 164.2 1_554
O9 H6W O2 0.88 1.90 2.763(3) 167.7 2_666
O8 H4W O2 0.82 1.99 2.711(2) 146.3 .
O8 H3W N1 0.84 1.98 2.776(2) 157.3 1_565
O7 H2W O10 0.82 2.06 2.823(3) 154.9 .
O7 H1W O4 0.82 1.90 2.666(2) 156.3 2_767
O5 H5 O9 0.82 1.75 2.570(2) 176.1 1_546
C21 H21 O3 0.93 2.58 3.144(3) 119.6 2_767
O11 H10W O10 0.85 1.97 2.822(3) 179.6 .
O11 H9W O1 0.85 2.05 2.898(3) 179.7 .
O10 H8W O11 0.82 2.01 2.814(4) 165.0 2_666
O10 H7W O6 0.83 2.07 2.836(3) 151.5 1_564
O9 H5W O4 0.85 1.88 2.710(2) 164.2 1_554
O9 H6W O2 0.88 1.90 2.763(3) 167.7 2_666
O8 H4W O2 0.82 1.99 2.711(2) 146.3 .
O8 H3W N1 0.84 1.98 2.776(2) 157.3 1_565
O7 H2W O10 0.82 2.06 2.823(3) 154.9 .
O7 H1W O4 0.82 1.90 2.666(2) 156.3 2_767
O5 H5 O9 0.82 1.75 2.570(2) 176.1 1_546
O5 H5 O9 0.82 1.75 2.570(2) 176.1 1_546
O7 H1W O4 0.82 1.90 2.666(2) 156.3 2_767
O7 H2W O10 0.82 2.06 2.823(3) 154.9 .
O8 H3W N1 0.84 1.98 2.776(2) 157.3 1_565
O8 H4W O2 0.82 1.99 2.711(2) 146.3 .
O9 H6W O2 0.88 1.90 2.763(3) 167.7 2_666
O9 H5W O4 0.85 1.88 2.710(2) 164.2 1_554
O10 H7W O6 0.83 2.07 2.836(3) 151.5 1_564
O10 H8W O11 0.82 2.01 2.814(4) 165.0 2_666
O11 H9W O1 0.85 2.05 2.898(3) 179.7 .
O11 H10W O10 0.85 1.97 2.822(3) 179.6 .
C21 H21 O3 0.93 2.58 3.144(3) 119.6 2_767

_refine_diff_density_max         0.680
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.051

####################################################################### 
# 
# 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_406-13Ni
_database_code_depnum_ccdc_archive 'CCDC 1984468'
_audit_update_record             
;
2020-05-08 deposited with the CCDC.	2020-05-11 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            'C88 H66 N8 Ni2 O16'
_chemical_formula_weight         1608.90

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 '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                   6.1632(4)
_cell_length_b                   12.2650(7)
_cell_length_c                   24.6163(17)
_cell_angle_alpha                95.914(5)
_cell_angle_beta                 93.921(5)
_cell_angle_gamma                101.777(5)
_cell_volume                     1804.3(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    11613
_cell_measurement_theta_min      3.626
_cell_measurement_theta_max      64.985

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_F_000             830
_exptl_transmission_factor_min   0.766
_exptl_transmission_factor_max   0.769
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    1.315
_shelx_estimated_absorpt_T_min   0.743
_shelx_estimated_absorpt_T_max   0.779
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.743
_exptl_absorpt_correction_T_max  0.779
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\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            11613
_diffrn_reflns_av_unetI/netI     0.0988
_diffrn_reflns_av_R_equivalents  0.0802
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         3.626
_diffrn_reflns_theta_max         64.985
_diffrn_reflns_theta_full        64.985
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measured_fraction_theta_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_point_group_measured_fraction_full 0.969
_reflns_number_total             5971
_reflns_number_gt                3865
_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)+(0.0997P)²+0.5903P] 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         5971
_refine_ls_number_parameters     515
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1112
_refine_ls_R_factor_gt           0.0736
_refine_ls_wR_factor_ref         0.2336
_refine_ls_wR_factor_gt          0.1989
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.064
_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 0.84088(13) 0.53164(6) 0.65249(3) 0.0403(3) Uani 1 1 d . . . . .
N1 N 0.3505(7) 0.7957(4) 0.81634(17) 0.0481(10) Uani 1 1 d . . . . .
N2 N 0.8767(7) 0.4298(3) 0.71385(17) 0.0421(10) Uani 1 1 d . . . . .
N3 N 1.0877(8) -0.2397(4) 0.9903(2) 0.0585(12) Uani 1 1 d . . . . .
N4 N 0.7924(7) 0.6443(3) 0.59672(17) 0.0442(10) Uani 1 1 d . . . . .
O1 O 0.8800(6) 0.6761(3) 0.71461(14) 0.0459(8) Uani 1 1 d . . . . .
O2 O 0.5532(5) 0.5655(3) 0.68719(14) 0.0442(8) Uani 1 1 d . . . . .
O3 O -0.0789(6) 1.2405(3) 0.61427(19) 0.0651(12) Uani 1 1 d . . . . .
O4 O 0.2694(7) 1.3125(4) 0.6031(2) 0.0908(18) Uani 1 1 d . . . . .
O5 O 0.5072(7) 0.3520(4) 0.96298(19) 0.0752(14) Uani 1 1 d . . . . .
O6 O 0.8599(7) 0.3921(4) 0.9441(2) 0.0753(14) Uani 1 1 d . . . . .
H6 H 0.8709 0.3422 0.9632 0.113 Uiso 1 1 calc R U . . .
O7 O 1.1510(6) 0.5303(4) 0.62733(16) 0.0605(11) Uani 1 1 d . . . . .
O8 O 0.7033(6) 0.3963(3) 0.59712(14) 0.0467(8) Uani 1 1 d . . . . .
H1W H 0.5640 0.3693 0.5964 0.056 Uiso 1 1 d R U . . .
H2W H 0.7884 0.3529 0.5950 0.056 Uiso 1 1 d R U . . .
C1 C 0.6742(8) 0.6542(4) 0.71454(19) 0.0406(11) Uani 1 1 d . . . . .
C2 C 0.5512(8) 0.7343(4) 0.74382(19) 0.0401(11) Uani 1 1 d . . . . .
C3 C 0.4932(8) 0.8138(4) 0.7134(2) 0.0423(11) Uani 1 1 d . . . . .
H3 H 0.5418 0.8190 0.6786 0.051 Uiso 1 1 calc R U . . .
C4 C 0.3648(8) 0.8858(4) 0.7333(2) 0.0432(11) Uani 1 1 d . . . . .
C5 C 0.2961(9) 0.8704(4) 0.7857(2) 0.0511(13) Uani 1 1 d . . . . .
H5 H 0.2054 0.9161 0.8000 0.061 Uiso 1 1 calc R U . . .
C6 C 0.4786(8) 0.7268(4) 0.7963(2) 0.0445(11) Uani 1 1 d . . . . .
C7 C 0.3010(8) 0.9743(4) 0.7031(2) 0.0423(11) Uani 1 1 d . . . . .
C8 C 0.1071(10) 1.0126(5) 0.7114(2) 0.0556(14) Uani 1 1 d . . . . .
H8A H 0.0127 0.9812 0.7362 0.067 Uiso 1 1 calc R U . . .
C9 C 0.0529(9) 1.0960(4) 0.6835(2) 0.0512(13) Uani 1 1 d . . . . .
H9 H -0.0787 1.1195 0.6895 0.061 Uiso 1 1 calc R U . . .
C10 C 0.1886(8) 1.1457(4) 0.6469(2) 0.0452(12) Uani 1 1 d . . . . .
C11 C 0.1222(9) 1.2410(4) 0.6186(2) 0.0492(13) Uani 1 1 d . . . . .
C12 C 0.3823(9) 1.1089(5) 0.6377(2) 0.0514(13) Uani 1 1 d . . . . .
H12 H 0.4778 1.1427 0.6137 0.062 Uiso 1 1 calc R U . . .
C13 C 0.4341(8) 1.0219(4) 0.6640(2) 0.0465(12) Uani 1 1 d . . . . .
H13 H 0.5594 0.9946 0.6557 0.056 Uiso 1 1 calc R U . . .
C14 C 0.5325(8) 0.6447(4) 0.8326(2) 0.0439(11) Uani 1 1 d . . . . .
C15 C 0.3799(9) 0.6065(5) 0.8699(2) 0.0488(12) Uani 1 1 d . . . . .
H15 H 0.2503 0.6340 0.8715 0.059 Uiso 1 1 calc R U . . .
C16 C 0.4190(10) 0.5282(5) 0.9043(2) 0.0523(13) Uani 1 1 d . . . . .
H16 H 0.3151 0.5030 0.9284 0.063 Uiso 1 1 calc R U . . .
C17 C 0.6125(9) 0.4882(4) 0.9028(2) 0.0482(12) Uani 1 1 d . . . . .
C18 C 0.6533(9) 0.4039(5) 0.9398(2) 0.0533(14) Uani 1 1 d . . . . .
C19 C 0.7673(9) 0.5271(5) 0.8669(2) 0.0510(13) Uani 1 1 d . . . . .
H19 H 0.8988 0.5011 0.8662 0.061 Uiso 1 1 calc R U . . .
C20 C 0.7266(9) 0.6045(5) 0.8321(2) 0.0508(13) Uani 1 1 d . . . . .
H20 H 0.8312 0.6297 0.8082 0.061 Uiso 1 1 calc R U . . .
C21 C 0.7021(9) 0.3555(4) 0.7253(2) 0.0501(13) Uani 1 1 d . . . . .
H21 H 0.5639 0.3543 0.7072 0.060 Uiso 1 1 calc R U . . .
C22 C 0.7156(9) 0.2796(4) 0.7627(2) 0.0482(12) Uani 1 1 d . . . . .
H22 H 0.5880 0.2297 0.7696 0.058 Uiso 1 1 calc R U . . .
C23 C 0.9193(8) 0.2780(4) 0.7901(2) 0.0417(11) Uani 1 1 d . . . . .
C24 C 1.0996(8) 0.3587(4) 0.7792(2) 0.0458(12) Uani 1 1 d . . . . .
H24 H 1.2390 0.3635 0.7974 0.055 Uiso 1 1 calc R U . . .
C25 C 1.0731(8) 0.4314(4) 0.7417(2) 0.0456(12) Uani 1 1 d . . . . .
H25 H 1.1969 0.4843 0.7352 0.055 Uiso 1 1 calc R U . . .
C26 C 0.9445(8) 0.1932(4) 0.8276(2) 0.0443(12) Uani 1 1 d . . . . .
C27 C 0.7872(10) 0.0952(5) 0.8260(3) 0.0655(17) Uani 1 1 d . . . . .
H27 H 0.6581 0.0847 0.8025 0.079 Uiso 1 1 calc R U . . .
C28 C 0.8138(10) 0.0123(5) 0.8578(3) 0.0675(18) Uani 1 1 d . . . . .
H28 H 0.7026 -0.0523 0.8558 0.081 Uiso 1 1 calc R U . . .
C29 C 1.0071(8) 0.0244(4) 0.8933(2) 0.0424(11) Uani 1 1 d . . . . .
C30 C 1.1607(10) 0.1228(5) 0.8957(2) 0.0606(16) Uani 1 1 d . . . . .
H30 H 1.2878 0.1349 0.9200 0.073 Uiso 1 1 calc R U . . .
C31 C 1.1333(10) 0.2040(5) 0.8633(3) 0.0654(18) Uani 1 1 d . . . . .
H31 H 1.2448 0.2685 0.8654 0.078 Uiso 1 1 calc R U . . .
C32 C 1.0331(9) -0.0674(4) 0.9270(2) 0.0464(12) Uani 1 1 d . . . . .
C33 C 0.8554(9) -0.1469(5) 0.9383(2) 0.0519(13) Uani 1 1 d . . . . .
H33 H 0.7118 -0.1444 0.9251 0.062 Uiso 1 1 calc R U . . .
C34 C 0.8897(10) -0.2306(5) 0.9694(2) 0.0583(15) Uani 1 1 d . . . . .
H34 H 0.7662 -0.2836 0.9760 0.070 Uiso 1 1 calc R U . . .
C35 C 1.2579(10) -0.1635(5) 0.9788(3) 0.0655(17) Uani 1 1 d . . . . .
H35 H 1.3996 -0.1687 0.9923 0.079 Uiso 1 1 calc R U . . .
C36 C 1.2410(10) -0.0766(5) 0.9481(2) 0.0567(15) Uani 1 1 d . . . . .
H36 H 1.3676 -0.0254 0.9418 0.068 Uiso 1 1 calc R U . . .
C37 C 0.6066(9) 0.6257(4) 0.5626(2) 0.0520(14) Uani 1 1 d . . . . .
H37 H 0.5198 0.5533 0.5560 0.062 Uiso 1 1 calc R U . . .
C38 C 0.5379(10) 0.7092(4) 0.5367(2) 0.0565(15) Uani 1 1 d . . . . .
H38 H 0.4086 0.6913 0.5129 0.068 Uiso 1 1 calc R U . . .
C39 C 0.6564(9) 0.8177(4) 0.5453(2) 0.0454(12) Uani 1 1 d . . . . .
C40 C 0.8559(9) 0.8357(4) 0.5790(2) 0.0496(13) Uani 1 1 d . . . . .
H40 H 0.9485 0.9067 0.5850 0.059 Uiso 1 1 calc R U . . .
C41 C 0.9151(9) 0.7491(5) 0.6034(2) 0.0496(13) Uani 1 1 d . . . . .
H41 H 1.0480 0.7640 0.6258 0.059 Uiso 1 1 calc R U . . .
C42 C 0.5774(9) 0.9105(4) 0.52192(19) 0.0433(11) Uani 1 1 d . . . . .
C43 C 0.3597(9) 0.8974(4) 0.4996(2) 0.0524(14) Uani 1 1 d . . . . .
H43 H 0.2622 0.8285 0.4990 0.063 Uiso 1 1 calc R U . . .
C44 C 0.7162(9) 1.0160(5) 0.5218(2) 0.0570(15) Uani 1 1 d . . . . .
H44 H 0.8634 1.0282 0.5365 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
Ni1 O8 2.033(3) . ?
Ni1 O7 2.052(4) . ?
Ni1 N2 2.085(4) . ?
Ni1 N4 2.094(4) . ?
Ni1 O2 2.116(3) . ?
Ni1 O1 2.180(4) . ?
N1 C5 1.323(6) . ?
N1 C6 1.349(7) . ?
N2 C21 1.327(7) . ?
N2 C25 1.345(6) . ?
N3 C35 1.322(8) . ?
N3 C34 1.322(7) . ?
N4 C37 1.339(6) . ?
N4 C41 1.340(7) . ?
O1 C1 1.242(6) . ?
O2 C1 1.281(6) . ?
O3 C11 1.235(6) . ?
O4 C11 1.237(7) . ?
O5 C18 1.205(7) . ?
O6 C18 1.309(7) . ?
O6 H6 0.8200 . ?
O8 H1W 0.8527 . ?
O8 H2W 0.8200 . ?
C1 C2 1.515(7) . ?
C2 C3 1.377(6) . ?
C2 C6 1.401(7) . ?
C3 C4 1.376(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.405(7) . ?
C4 C7 1.478(6) . ?
C5 H5 0.9300 . ?
C6 C14 1.486(7) . ?
C7 C8 1.391(7) . ?
C7 C13 1.403(7) . ?
C8 C9 1.372(7) . ?
C8 H8A 0.9300 . ?
C9 C10 1.376(7) . ?
C9 H9 0.9300 . ?
C10 C12 1.384(7) . ?
C10 C11 1.532(6) . ?
C12 C13 1.383(7) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 C20 1.384(7) . ?
C14 C15 1.403(7) . ?
C15 C16 1.391(7) . ?
C15 H15 0.9300 . ?
C16 C17 1.381(8) . ?
C16 H16 0.9300 . ?
C17 C19 1.390(7) . ?
C17 C18 1.494(7) . ?
C19 C20 1.392(7) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
C21 C22 1.387(7) . ?
C21 H21 0.9300 . ?
C22 C23 1.388(6) . ?
C22 H22 0.9300 . ?
C23 C24 1.391(7) . ?
C23 C26 1.483(6) . ?
C24 C25 1.371(6) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
C26 C27 1.377(8) . ?
C26 C31 1.386(7) . ?
C27 C28 1.375(7) . ?
C27 H27 0.9300 . ?
C28 C29 1.400(7) . ?
C28 H28 0.9300 . ?
C29 C30 1.367(7) . ?
C29 C32 1.493(6) . ?
C30 C31 1.366(7) . ?
C30 H30 0.9300 . ?
C31 H31 0.9300 . ?
C32 C33 1.375(7) . ?
C32 C36 1.380(7) . ?
C33 C34 1.383(7) . ?
C33 H33 0.9300 . ?
C34 H34 0.9300 . ?
C35 C36 1.385(7) . ?
C35 H35 0.9300 . ?
C36 H36 0.9300 . ?
C37 C38 1.382(7) . ?
C37 H37 0.9300 . ?
C38 C39 1.369(7) . ?
C38 H38 0.9300 . ?
C39 C40 1.401(7) . ?
C39 C42 1.479(6) . ?
C40 C41 1.371(7) . ?
C40 H40 0.9300 . ?
C41 H41 0.9300 . ?
C42 C43 1.386(7) . ?
C42 C44 1.399(7) . ?
C43 C44 1.381(7) 2_676 ?
C43 H43 0.9300 . ?
C44 C43 1.381(7) 2_676 ?
C44 H44 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O8 Ni1 O7 90.97(17) . . ?
O8 Ni1 N2 91.66(15) . . ?
O7 Ni1 N2 93.63(15) . . ?
O8 Ni1 N4 92.42(15) . . ?
O7 Ni1 N4 90.40(16) . . ?
N2 Ni1 N4 174.22(17) . . ?
O8 Ni1 O2 100.58(14) . . ?
O7 Ni1 O2 168.22(16) . . ?
N2 Ni1 O2 88.37(15) . . ?
N4 Ni1 O2 86.85(15) . . ?
O8 Ni1 O1 162.19(14) . . ?
O7 Ni1 O1 106.63(16) . . ?
N2 Ni1 O1 89.93(15) . . ?
N4 Ni1 O1 84.94(15) . . ?
O2 Ni1 O1 61.73(13) . . ?
C5 N1 C6 118.8(5) . . ?
C21 N2 C25 116.9(4) . . ?
C21 N2 Ni1 119.8(3) . . ?
C25 N2 Ni1 123.2(3) . . ?
C35 N3 C34 115.6(5) . . ?
C37 N4 C41 116.1(4) . . ?
C37 N4 Ni1 121.2(3) . . ?
C41 N4 Ni1 120.5(3) . . ?
C1 O1 Ni1 87.1(3) . . ?
C1 O2 Ni1 88.9(3) . . ?
C18 O6 H6 109.5 . . ?
Ni1 O8 H1W 118.3 . . ?
Ni1 O8 H2W 109.5 . . ?
H1W O8 H2W 118.7 . . ?
O1 C1 O2 121.8(5) . . ?
O1 C1 C2 121.8(4) . . ?
O2 C1 C2 116.2(4) . . ?
C3 C2 C6 119.3(5) . . ?
C3 C2 C1 115.4(4) . . ?
C6 C2 C1 125.1(4) . . ?
C2 C3 C4 121.5(5) . . ?
C2 C3 H3 119.3 . . ?
C4 C3 H3 119.3 . . ?
C3 C4 C5 115.1(4) . . ?
C3 C4 C7 124.0(5) . . ?
C5 C4 C7 120.8(5) . . ?
N1 C5 C4 125.0(5) . . ?
N1 C5 H5 117.5 . . ?
C4 C5 H5 117.5 . . ?
N1 C6 C2 120.2(4) . . ?
N1 C6 C14 116.1(5) . . ?
C2 C6 C14 123.7(5) . . ?
C8 C7 C13 117.3(4) . . ?
C8 C7 C4 122.0(5) . . ?
C13 C7 C4 120.7(4) . . ?
C9 C8 C7 120.9(5) . . ?
C9 C8 H8A 119.5 . . ?
C7 C8 H8A 119.5 . . ?
C8 C9 C10 121.5(5) . . ?
C8 C9 H9 119.2 . . ?
C10 C9 H9 119.2 . . ?
C9 C10 C12 118.7(5) . . ?
C9 C10 C11 118.9(5) . . ?
C12 C10 C11 122.4(5) . . ?
O3 C11 O4 125.3(5) . . ?
O3 C11 C10 115.6(5) . . ?
O4 C11 C10 119.0(5) . . ?
C13 C12 C10 120.2(5) . . ?
C13 C12 H12 119.9 . . ?
C10 C12 H12 119.9 . . ?
C12 C13 C7 121.2(5) . . ?
C12 C13 H13 119.4 . . ?
C7 C13 H13 119.4 . . ?
C20 C14 C15 118.2(5) . . ?
C20 C14 C6 123.4(5) . . ?
C15 C14 C6 118.4(5) . . ?
C16 C15 C14 121.2(5) . . ?
C16 C15 H15 119.4 . . ?
C14 C15 H15 119.4 . . ?
C17 C16 C15 119.8(5) . . ?
C17 C16 H16 120.1 . . ?
C15 C16 H16 120.1 . . ?
C16 C17 C19 119.6(5) . . ?
C16 C17 C18 119.6(5) . . ?
C19 C17 C18 120.8(5) . . ?
O5 C18 O6 124.0(5) . . ?
O5 C18 C17 122.3(5) . . ?
O6 C18 C17 113.7(5) . . ?
C17 C19 C20 120.4(5) . . ?
C17 C19 H19 119.8 . . ?
C20 C19 H19 119.8 . . ?
C14 C20 C19 120.8(5) . . ?
C14 C20 H20 119.6 . . ?
C19 C20 H20 119.6 . . ?
N2 C21 C22 123.2(5) . . ?
N2 C21 H21 118.4 . . ?
C22 C21 H21 118.4 . . ?
C21 C22 C23 120.1(5) . . ?
C21 C22 H22 119.9 . . ?
C23 C22 H22 119.9 . . ?
C22 C23 C24 116.1(4) . . ?
C22 C23 C26 122.0(5) . . ?
C24 C23 C26 121.9(4) . . ?
C25 C24 C23 120.4(4) . . ?
C25 C24 H24 119.8 . . ?
C23 C24 H24 119.8 . . ?
N2 C25 C24 123.2(5) . . ?
N2 C25 H25 118.4 . . ?
C24 C25 H25 118.4 . . ?
C27 C26 C31 116.1(5) . . ?
C27 C26 C23 121.5(4) . . ?
C31 C26 C23 122.3(5) . . ?
C28 C27 C26 122.5(5) . . ?
C28 C27 H27 118.7 . . ?
C26 C27 H27 118.7 . . ?
C27 C28 C29 120.5(6) . . ?
C27 C28 H28 119.8 . . ?
C29 C28 H28 119.8 . . ?
C30 C29 C28 116.9(5) . . ?
C30 C29 C32 123.7(5) . . ?
C28 C29 C32 119.5(5) . . ?
C31 C30 C29 122.0(5) . . ?
C31 C30 H30 119.0 . . ?
C29 C30 H30 119.0 . . ?
C30 C31 C26 122.0(5) . . ?
C30 C31 H31 119.0 . . ?
C26 C31 H31 119.0 . . ?
C33 C32 C36 116.6(5) . . ?
C33 C32 C29 122.7(5) . . ?
C36 C32 C29 120.8(5) . . ?
C32 C33 C34 120.2(5) . . ?
C32 C33 H33 119.9 . . ?
C34 C33 H33 119.9 . . ?
N3 C34 C33 123.8(6) . . ?
N3 C34 H34 118.1 . . ?
C33 C34 H34 118.1 . . ?
N3 C35 C36 124.9(5) . . ?
N3 C35 H35 117.5 . . ?
C36 C35 H35 117.5 . . ?
C32 C36 C35 118.9(6) . . ?
C32 C36 H36 120.6 . . ?
C35 C36 H36 120.6 . . ?
N4 C37 C38 123.0(5) . . ?
N4 C37 H37 118.5 . . ?
C38 C37 H37 118.5 . . ?
C39 C38 C37 121.3(5) . . ?
C39 C38 H38 119.3 . . ?
C37 C38 H38 119.3 . . ?
C38 C39 C40 115.4(4) . . ?
C38 C39 C42 122.6(5) . . ?
C40 C39 C42 122.0(5) . . ?
C41 C40 C39 120.3(5) . . ?
C41 C40 H40 119.9 . . ?
C39 C40 H40 119.9 . . ?
N4 C41 C40 123.7(5) . . ?
N4 C41 H41 118.1 . . ?
C40 C41 H41 118.1 . . ?
C43 C42 C44 116.5(5) . . ?
C43 C42 C39 121.4(5) . . ?
C44 C42 C39 122.1(5) . . ?
C44 C43 C42 121.8(5) 2_676 . ?
C44 C43 H43 119.1 2_676 . ?
C42 C43 H43 119.1 . . ?
C43 C44 C42 121.7(5) 2_676 . ?
C43 C44 H44 119.2 2_676 . ?
C42 C44 H44 119.2 . . ?

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
Ni1 O1 C1 O2 6.4(4) . . . . ?
Ni1 O1 C1 C2 -169.7(4) . . . . ?
Ni1 O2 C1 O1 -6.5(4) . . . . ?
Ni1 O2 C1 C2 169.7(3) . . . . ?
O1 C1 C2 C3 88.0(6) . . . . ?
O2 C1 C2 C3 -88.3(6) . . . . ?
O1 C1 C2 C6 -97.7(6) . . . . ?
O2 C1 C2 C6 86.1(6) . . . . ?
C6 C2 C3 C4 -0.3(8) . . . . ?
C1 C2 C3 C4 174.5(5) . . . . ?
C2 C3 C4 C5 -1.1(8) . . . . ?
C2 C3 C4 C7 178.7(5) . . . . ?
C6 N1 C5 C4 -1.2(9) . . . . ?
C3 C4 C5 N1 1.9(8) . . . . ?
C7 C4 C5 N1 -177.9(5) . . . . ?
C5 N1 C6 C2 -0.3(8) . . . . ?
C5 N1 C6 C14 -179.7(5) . . . . ?
C3 C2 C6 N1 1.0(8) . . . . ?
C1 C2 C6 N1 -173.2(5) . . . . ?
C3 C2 C6 C14 -179.7(5) . . . . ?
C1 C2 C6 C14 6.2(8) . . . . ?
C3 C4 C7 C8 152.4(5) . . . . ?
C5 C4 C7 C8 -27.8(8) . . . . ?
C3 C4 C7 C13 -26.5(8) . . . . ?
C5 C4 C7 C13 153.2(5) . . . . ?
C13 C7 C8 C9 -2.0(8) . . . . ?
C4 C7 C8 C9 179.0(5) . . . . ?
C7 C8 C9 C10 -0.7(9) . . . . ?
C8 C9 C10 C12 1.0(8) . . . . ?
C8 C9 C10 C11 -178.0(5) . . . . ?
C9 C10 C11 O3 -25.6(8) . . . . ?
C12 C10 C11 O3 155.5(5) . . . . ?
C9 C10 C11 O4 152.9(6) . . . . ?
C12 C10 C11 O4 -26.0(8) . . . . ?
C9 C10 C12 C13 1.5(8) . . . . ?
C11 C10 C12 C13 -179.6(5) . . . . ?
C10 C12 C13 C7 -4.3(8) . . . . ?
C8 C7 C13 C12 4.4(8) . . . . ?
C4 C7 C13 C12 -176.5(5) . . . . ?
N1 C6 C14 C20 -150.3(5) . . . . ?
C2 C6 C14 C20 30.4(8) . . . . ?
N1 C6 C14 C15 29.1(7) . . . . ?
C2 C6 C14 C15 -150.2(5) . . . . ?
C20 C14 C15 C16 -1.6(8) . . . . ?
C6 C14 C15 C16 179.0(5) . . . . ?
C14 C15 C16 C17 0.9(8) . . . . ?
C15 C16 C17 C19 0.4(8) . . . . ?
C15 C16 C17 C18 -179.8(5) . . . . ?
C16 C17 C18 O5 15.5(9) . . . . ?
C19 C17 C18 O5 -164.8(6) . . . . ?
C16 C17 C18 O6 -164.9(5) . . . . ?
C19 C17 C18 O6 14.9(8) . . . . ?
C16 C17 C19 C20 -1.0(9) . . . . ?
C18 C17 C19 C20 179.2(5) . . . . ?
C15 C14 C20 C19 1.0(8) . . . . ?
C6 C14 C20 C19 -179.6(5) . . . . ?
C17 C19 C20 C14 0.3(9) . . . . ?
C25 N2 C21 C22 -1.7(8) . . . . ?
Ni1 N2 C21 C22 175.4(4) . . . . ?
N2 C21 C22 C23 -0.6(9) . . . . ?
C21 C22 C23 C24 2.7(8) . . . . ?
C21 C22 C23 C26 -175.6(5) . . . . ?
C22 C23 C24 C25 -2.5(8) . . . . ?
C26 C23 C24 C25 175.8(5) . . . . ?
C21 N2 C25 C24 1.9(8) . . . . ?
Ni1 N2 C25 C24 -175.1(4) . . . . ?
C23 C24 C25 N2 0.2(9) . . . . ?
C22 C23 C26 C27 18.0(9) . . . . ?
C24 C23 C26 C27 -160.2(6) . . . . ?
C22 C23 C26 C31 -166.5(6) . . . . ?
C24 C23 C26 C31 15.3(9) . . . . ?
C31 C26 C27 C28 0.0(11) . . . . ?
C23 C26 C27 C28 175.8(6) . . . . ?
C26 C27 C28 C29 -0.8(12) . . . . ?
C27 C28 C29 C30 2.1(10) . . . . ?
C27 C28 C29 C32 -179.3(6) . . . . ?
C28 C29 C30 C31 -2.9(10) . . . . ?
C32 C29 C30 C31 178.6(6) . . . . ?
C29 C30 C31 C26 2.3(11) . . . . ?
C27 C26 C31 C30 -0.7(10) . . . . ?
C23 C26 C31 C30 -176.5(6) . . . . ?
C30 C29 C32 C33 157.8(6) . . . . ?
C28 C29 C32 C33 -20.6(9) . . . . ?
C30 C29 C32 C36 -22.7(9) . . . . ?
C28 C29 C32 C36 158.9(6) . . . . ?
C36 C32 C33 C34 0.0(9) . . . . ?
C29 C32 C33 C34 179.5(5) . . . . ?
C35 N3 C34 C33 -1.3(10) . . . . ?
C32 C33 C34 N3 0.8(10) . . . . ?
C34 N3 C35 C36 1.3(10) . . . . ?
C33 C32 C36 C35 0.0(9) . . . . ?
C29 C32 C36 C35 -179.5(5) . . . . ?
N3 C35 C36 C32 -0.7(11) . . . . ?
C41 N4 C37 C38 -2.1(9) . . . . ?
Ni1 N4 C37 C38 161.2(5) . . . . ?
N4 C37 C38 C39 -1.0(10) . . . . ?
C37 C38 C39 C40 3.8(9) . . . . ?
C37 C38 C39 C42 -174.6(5) . . . . ?
C38 C39 C40 C41 -3.5(9) . . . . ?
C42 C39 C40 C41 174.9(5) . . . . ?
C37 N4 C41 C40 2.3(9) . . . . ?
Ni1 N4 C41 C40 -161.1(4) . . . . ?
C39 C40 C41 N4 0.5(9) . . . . ?
C38 C39 C42 C43 13.5(9) . . . . ?
C40 C39 C42 C43 -164.8(6) . . . . ?
C38 C39 C42 C44 -167.4(6) . . . . ?
C40 C39 C42 C44 14.4(9) . . . . ?
C44 C42 C43 C44 0.1(10) . . . 2_676 ?
C39 C42 C43 C44 179.3(5) . . . 2_676 ?
C43 C42 C44 C43 -0.1(10) . . . 2_676 ?
C39 C42 C44 C43 -179.3(5) . . . 2_676 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C34 H34 O5 0.93 2.41 3.248(7) 149.2 2_657
C25 H25 O2 0.93 2.63 3.503(6) 156.7 1_655
O8 H2W O3 0.82 1.83 2.602(5) 156.9 1_645
O8 H1W O4 0.85 1.83 2.681(6) 173.8 1_545
O6 H6 N3 0.82 1.83 2.647(6) 175.2 2_757
C34 H34 O5 0.93 2.41 3.248(7) 149.2 2_657
C25 H25 O2 0.93 2.63 3.503(6) 156.7 1_655
O8 H2W O3 0.82 1.83 2.602(5) 156.9 1_645
O8 H1W O4 0.85 1.83 2.681(6) 173.8 1_545
O6 H6 N3 0.82 1.83 2.647(6) 175.2 2_757
O6 H6 N3 0.82 1.83 2.647(6) 175.2 2_757
O8 H1W O4 0.85 1.83 2.681(6) 173.8 1_545
O8 H2W O3 0.82 1.83 2.602(5) 156.9 1_645
C25 H25 O2 0.93 2.63 3.503(6) 156.7 1_655
C34 H34 O5 0.93 2.41 3.248(7) 149.2 2_657
O6 H6 N3 0.82 1.83 2.647(6) 175.2 2_757
O8 H1W O4 0.85 1.83 2.681(6) 173.8 1_545
O8 H2W O3 0.82 1.83 2.602(5) 156.9 1_645
C25 H25 O2 0.93 2.63 3.503(6) 156.7 1_655
C34 H34 O5 0.93 2.41 3.248(7) 149.2 2_657

_refine_diff_density_max         0.895
_refine_diff_density_min         -0.636
_refine_diff_density_rms         0.078

####################################################################### 
# 
# 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_410-11Fe
_database_code_depnum_ccdc_archive 'CCDC 1984469'
_audit_update_record             
;
2020-05-08 deposited with the CCDC.	2020-05-11 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            'C20 H15 Fe N O8'
_chemical_formula_weight         453.18

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'
Fe Fe 0.3463 0.8444 '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                   6.9066(8)
_cell_length_b                   9.3698(8)
_cell_length_c                   14.8244(9)
_cell_angle_alpha                74.751(6)
_cell_angle_beta                 85.796(7)
_cell_angle_gamma                82.493(8)
_cell_volume                     916.87(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5677
_cell_measurement_theta_min      3.529
_cell_measurement_theta_max      25.048

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.634
_exptl_crystal_F_000             460
_exptl_transmission_factor_min   0.804
_exptl_transmission_factor_max   0.832
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.210
_exptl_absorpt_coefficient_mu    0.874
_shelx_estimated_absorpt_T_min   0.811
_shelx_estimated_absorpt_T_max   0.838
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.811
_exptl_absorpt_correction_T_max  0.838
_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            5677
_diffrn_reflns_av_unetI/netI     0.0653
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.529
_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             3236
_reflns_number_gt                2585
_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)+(0.0435P)²+0.3693P] 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         3236
_refine_ls_number_parameters     275
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0418
_refine_ls_wR_factor_ref         0.1093
_refine_ls_wR_factor_gt          0.0967
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.032
_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
Fe1 Fe 0.5000 0.5000 0.5000 0.01396(18) Uani 1 2 d S . P . .
Fe2 Fe 1.0000 0.5000 0.5000 0.01460(18) Uani 1 2 d S . P . .
N1 N 0.2084(5) 0.3910(3) 0.10444(17) 0.0272(7) Uani 1 1 d . . . . .
O1 O 0.1103(3) 0.4312(2) 0.38386(14) 0.0202(5) Uani 1 1 d . . . . .
O2 O 0.4159(3) 0.4961(2) 0.37114(13) 0.0210(5) Uani 1 1 d . . . . .
O3 O 0.3833(3) -0.2869(2) 0.47581(15) 0.0239(5) Uani 1 1 d . . . . .
O4 O 0.0798(3) -0.2973(2) 0.43448(15) 0.0228(5) Uani 1 1 d . . . . .
O5 O 0.2277(4) 1.3436(3) -0.14002(16) 0.0397(7) Uani 1 1 d . . . . .
H5 H 0.2100 1.4208 -0.1817 0.059 Uiso 1 1 calc R U . . .
O6 O 0.2789(5) 1.2406(3) -0.26108(17) 0.0489(8) Uani 1 1 d . . . . .
O7 O 0.7492(3) 0.5622(2) 0.43996(13) 0.0181(5) Uani 1 1 d . . . . .
O8 O 0.2287(4) 0.5961(3) 0.72519(16) 0.0330(6) Uani 1 1 d . . . . .
H1W H 0.1329 0.5885 0.6946 0.040 Uiso 1 1 d R U . . .
H2W H 0.3331 0.5690 0.6970 0.040 Uiso 1 1 d R U . . .
C1 C 0.2682(5) 0.4647(3) 0.3385(2) 0.0162(7) Uani 1 1 d . . . . .
C2 C 0.2716(5) 0.4811(3) 0.2354(2) 0.0165(7) Uani 1 1 d . . . . .
C3 C 0.2361(5) 0.3662(3) 0.1967(2) 0.0175(7) Uani 1 1 d . . . . .
C4 C 0.2215(6) 0.5282(4) 0.0502(2) 0.0266(8) Uani 1 1 d . . . . .
H4 H 0.1975 0.5454 -0.0129 0.032 Uiso 1 1 calc R U . . .
C5 C 0.2681(5) 0.6474(3) 0.0807(2) 0.0214(8) Uani 1 1 d . . . . .
C6 C 0.2931(5) 0.6206(3) 0.1760(2) 0.0195(7) Uani 1 1 d . . . . .
H6 H 0.3244 0.6963 0.2002 0.023 Uiso 1 1 calc R U . . .
C7 C 0.2337(5) 0.2113(3) 0.2564(2) 0.0208(7) Uani 1 1 d . . . . .
C8 C 0.3751(5) 0.1513(4) 0.3227(2) 0.0243(8) Uani 1 1 d . . . . .
H8 H 0.4713 0.2083 0.3292 0.029 Uiso 1 1 calc R U . . .
C9 C 0.3736(5) 0.0088(3) 0.3785(2) 0.0235(8) Uani 1 1 d . . . . .
H9 H 0.4715 -0.0312 0.4209 0.028 Uiso 1 1 calc R U . . .
C10 C 0.2270(5) -0.0757(3) 0.3720(2) 0.0196(7) Uani 1 1 d . . . . .
C11 C 0.2284(5) -0.2306(3) 0.4323(2) 0.0180(7) Uani 1 1 d . . . . .
C12 C 0.0850(6) -0.0170(4) 0.3064(2) 0.0272(8) Uani 1 1 d . . . . .
H12 H -0.0141 -0.0727 0.3018 0.033 Uiso 1 1 calc R U . . .
C13 C 0.0908(6) 0.1245(4) 0.2476(2) 0.0268(8) Uani 1 1 d . . . . .
H13 H -0.0014 0.1617 0.2020 0.032 Uiso 1 1 calc R U . . .
C14 C 0.2777(5) 0.7974(4) 0.0161(2) 0.0216(7) Uani 1 1 d . . . . .
C15 C 0.3206(6) 0.8150(4) -0.0798(2) 0.0269(8) Uani 1 1 d . . . . .
H15 H 0.3524 0.7314 -0.1029 0.032 Uiso 1 1 calc R U . . .
C16 C 0.3161(6) 0.9549(4) -0.1401(2) 0.0279(8) Uani 1 1 d . . . . .
H16 H 0.3422 0.9644 -0.2038 0.033 Uiso 1 1 calc R U . . .
C17 C 0.2735(5) 1.0811(4) -0.1078(2) 0.0241(8) Uani 1 1 d . . . . .
C18 C 0.2606(5) 1.2289(4) -0.1774(2) 0.0283(8) Uani 1 1 d . . . . .
C19 C 0.2392(5) 1.0669(4) -0.0121(2) 0.0264(8) Uani 1 1 d . . . . .
H19 H 0.2153 1.1509 0.0110 0.032 Uiso 1 1 calc R U . . .
C20 C 0.2412(5) 0.9262(4) 0.0478(2) 0.0244(8) Uani 1 1 d . . . . .
H20 H 0.2174 0.9171 0.1115 0.029 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
Fe1 O7 1.964(2) 2_666 ?
Fe1 O7 1.964(2) . ?
Fe1 O3 2.003(2) 2_656 ?
Fe1 O3 2.003(2) 1_565 ?
Fe1 O2 2.048(2) . ?
Fe1 O2 2.048(2) 2_666 ?
Fe2 O7 1.955(2) 2_766 ?
Fe2 O7 1.955(2) . ?
Fe2 O4 2.020(2) 2_656 ?
Fe2 O4 2.020(2) 1_665 ?
Fe2 O1 2.055(2) 1_655 ?
Fe2 O1 2.055(2) 2_666 ?
N1 C4 1.335(4) . ?
N1 C3 1.350(4) . ?
O1 C1 1.269(4) . ?
O1 Fe2 2.055(2) 1_455 ?
O2 C1 1.260(4) . ?
O3 C11 1.270(4) . ?
O3 Fe1 2.003(2) 1_545 ?
O4 C11 1.264(4) . ?
O4 Fe2 2.020(2) 1_445 ?
O5 C18 1.321(4) . ?
O5 H5 0.8200 . ?
O6 C18 1.215(4) . ?
O8 H1W 0.8500 . ?
O8 H2W 0.8500 . ?
C1 C2 1.494(4) . ?
C2 C6 1.390(4) . ?
C2 C3 1.400(4) . ?
C3 C7 1.489(4) . ?
C4 C5 1.392(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.388(4) . ?
C5 C14 1.484(4) . ?
C6 H6 0.9300 . ?
C7 C13 1.392(5) . ?
C7 C8 1.394(5) . ?
C8 C9 1.374(4) . ?
C8 H8 0.9300 . ?
C9 C10 1.388(4) . ?
C9 H9 0.9300 . ?
C10 C12 1.389(5) . ?
C10 C11 1.491(4) . ?
C12 C13 1.385(4) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 C20 1.394(5) . ?
C14 C15 1.401(4) . ?
C15 C16 1.377(4) . ?
C15 H15 0.9300 . ?
C16 C17 1.380(5) . ?
C16 H16 0.9300 . ?
C17 C19 1.394(4) . ?
C17 C18 1.490(4) . ?
C19 C20 1.381(5) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O7 Fe1 O7 180.0 2_666 . ?
O7 Fe1 O3 90.47(9) 2_666 2_656 ?
O7 Fe1 O3 89.53(9) . 2_656 ?
O7 Fe1 O3 89.53(9) 2_666 1_565 ?
O7 Fe1 O3 90.47(9) . 1_565 ?
O3 Fe1 O3 180.00(13) 2_656 1_565 ?
O7 Fe1 O2 91.99(8) 2_666 . ?
O7 Fe1 O2 88.01(8) . . ?
O3 Fe1 O2 90.85(9) 2_656 . ?
O3 Fe1 O2 89.15(9) 1_565 . ?
O7 Fe1 O2 88.01(8) 2_666 2_666 ?
O7 Fe1 O2 91.99(8) . 2_666 ?
O3 Fe1 O2 89.15(9) 2_656 2_666 ?
O3 Fe1 O2 90.85(9) 1_565 2_666 ?
O2 Fe1 O2 180.0 . 2_666 ?
O7 Fe2 O7 180.0 2_766 . ?
O7 Fe2 O4 88.23(9) 2_766 2_656 ?
O7 Fe2 O4 91.77(9) . 2_656 ?
O7 Fe2 O4 91.77(9) 2_766 1_665 ?
O7 Fe2 O4 88.23(9) . 1_665 ?
O4 Fe2 O4 180.0 2_656 1_665 ?
O7 Fe2 O1 91.37(9) 2_766 1_655 ?
O7 Fe2 O1 88.63(9) . 1_655 ?
O4 Fe2 O1 92.65(8) 2_656 1_655 ?
O4 Fe2 O1 87.35(8) 1_665 1_655 ?
O7 Fe2 O1 88.63(9) 2_766 2_666 ?
O7 Fe2 O1 91.37(9) . 2_666 ?
O4 Fe2 O1 87.35(8) 2_656 2_666 ?
O4 Fe2 O1 92.65(8) 1_665 2_666 ?
O1 Fe2 O1 180.0 1_655 2_666 ?
C4 N1 C3 117.9(3) . . ?
C1 O1 Fe2 125.77(19) . 1_455 ?
C1 O2 Fe1 136.5(2) . . ?
C11 O3 Fe1 125.9(2) . 1_545 ?
C11 O4 Fe2 135.9(2) . 1_445 ?
C18 O5 H5 109.5 . . ?
Fe2 O7 Fe1 123.55(10) . . ?
H1W O8 H2W 107.7 . . ?
O2 C1 O1 125.9(3) . . ?
O2 C1 C2 117.3(3) . . ?
O1 C1 C2 116.6(3) . . ?
C6 C2 C3 118.9(3) . . ?
C6 C2 C1 118.1(3) . . ?
C3 C2 C1 122.8(3) . . ?
N1 C3 C2 121.4(3) . . ?
N1 C3 C7 118.0(3) . . ?
C2 C3 C7 120.6(3) . . ?
N1 C4 C5 125.2(3) . . ?
N1 C4 H4 117.4 . . ?
C5 C4 H4 117.4 . . ?
C6 C5 C4 116.2(3) . . ?
C6 C5 C14 121.8(3) . . ?
C4 C5 C14 122.0(3) . . ?
C5 C6 C2 120.3(3) . . ?
C5 C6 H6 119.8 . . ?
C2 C6 H6 119.8 . . ?
C13 C7 C8 118.9(3) . . ?
C13 C7 C3 121.0(3) . . ?
C8 C7 C3 120.1(3) . . ?
C9 C8 C7 120.6(3) . . ?
C9 C8 H8 119.7 . . ?
C7 C8 H8 119.7 . . ?
C8 C9 C10 120.4(3) . . ?
C8 C9 H9 119.8 . . ?
C10 C9 H9 119.8 . . ?
C9 C10 C12 119.5(3) . . ?
C9 C10 C11 119.8(3) . . ?
C12 C10 C11 120.7(3) . . ?
O4 C11 O3 125.0(3) . . ?
O4 C11 C10 118.3(3) . . ?
O3 C11 C10 116.7(3) . . ?
C13 C12 C10 120.1(3) . . ?
C13 C12 H12 120.0 . . ?
C10 C12 H12 120.0 . . ?
C12 C13 C7 120.5(3) . . ?
C12 C13 H13 119.8 . . ?
C7 C13 H13 119.8 . . ?
C20 C14 C15 117.3(3) . . ?
C20 C14 C5 121.6(3) . . ?
C15 C14 C5 121.1(3) . . ?
C16 C15 C14 120.6(3) . . ?
C16 C15 H15 119.7 . . ?
C14 C15 H15 119.7 . . ?
C15 C16 C17 121.1(3) . . ?
C15 C16 H16 119.5 . . ?
C17 C16 H16 119.5 . . ?
C16 C17 C19 119.5(3) . . ?
C16 C17 C18 118.3(3) . . ?
C19 C17 C18 122.2(3) . . ?
O6 C18 O5 123.8(3) . . ?
O6 C18 C17 122.0(3) . . ?
O5 C18 C17 114.2(3) . . ?
C20 C19 C17 119.1(3) . . ?
C20 C19 H19 120.5 . . ?
C17 C19 H19 120.5 . . ?
C19 C20 C14 122.3(3) . . ?
C19 C20 H20 118.8 . . ?
C14 C20 H20 118.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 O2 C1 O1 4.8(5) . . . . ?
Fe1 O2 C1 C2 179.1(2) . . . . ?
Fe2 O1 C1 O2 27.6(4) 1_455 . . . ?
Fe2 O1 C1 C2 -146.7(2) 1_455 . . . ?
O2 C1 C2 C6 -59.1(4) . . . . ?
O1 C1 C2 C6 115.7(3) . . . . ?
O2 C1 C2 C3 126.9(3) . . . . ?
O1 C1 C2 C3 -58.3(4) . . . . ?
C4 N1 C3 C2 1.9(5) . . . . ?
C4 N1 C3 C7 -176.3(3) . . . . ?
C6 C2 C3 N1 -4.9(5) . . . . ?
C1 C2 C3 N1 169.0(3) . . . . ?
C6 C2 C3 C7 173.3(3) . . . . ?
C1 C2 C3 C7 -12.8(5) . . . . ?
C3 N1 C4 C5 2.3(5) . . . . ?
N1 C4 C5 C6 -3.2(6) . . . . ?
N1 C4 C5 C14 -179.3(3) . . . . ?
C4 C5 C6 C2 0.0(5) . . . . ?
C14 C5 C6 C2 176.1(3) . . . . ?
C3 C2 C6 C5 3.8(5) . . . . ?
C1 C2 C6 C5 -170.4(3) . . . . ?
N1 C3 C7 C13 -44.9(5) . . . . ?
C2 C3 C7 C13 136.9(3) . . . . ?
N1 C3 C7 C8 135.5(3) . . . . ?
C2 C3 C7 C8 -42.8(5) . . . . ?
C13 C7 C8 C9 0.0(5) . . . . ?
C3 C7 C8 C9 179.6(3) . . . . ?
C7 C8 C9 C10 -2.3(5) . . . . ?
C8 C9 C10 C12 2.1(5) . . . . ?
C8 C9 C10 C11 179.4(3) . . . . ?
Fe2 O4 C11 O3 2.0(5) 1_445 . . . ?
Fe2 O4 C11 C10 179.8(2) 1_445 . . . ?
Fe1 O3 C11 O4 34.6(4) 1_545 . . . ?
Fe1 O3 C11 C10 -143.3(2) 1_545 . . . ?
C9 C10 C11 O4 170.3(3) . . . . ?
C12 C10 C11 O4 -12.5(4) . . . . ?
C9 C10 C11 O3 -11.7(4) . . . . ?
C12 C10 C11 O3 165.5(3) . . . . ?
C9 C10 C12 C13 0.4(5) . . . . ?
C11 C10 C12 C13 -176.9(3) . . . . ?
C10 C12 C13 C7 -2.7(5) . . . . ?
C8 C7 C13 C12 2.5(5) . . . . ?
C3 C7 C13 C12 -177.1(3) . . . . ?
C6 C5 C14 C20 -23.7(5) . . . . ?
C4 C5 C14 C20 152.2(4) . . . . ?
C6 C5 C14 C15 157.5(3) . . . . ?
C4 C5 C14 C15 -26.6(5) . . . . ?
C20 C14 C15 C16 -3.3(5) . . . . ?
C5 C14 C15 C16 175.5(3) . . . . ?
C14 C15 C16 C17 1.4(6) . . . . ?
C15 C16 C17 C19 1.6(6) . . . . ?
C15 C16 C17 C18 -176.8(3) . . . . ?
C16 C17 C18 O6 2.9(5) . . . . ?
C19 C17 C18 O6 -175.4(4) . . . . ?
C16 C17 C18 O5 -177.2(3) . . . . ?
C19 C17 C18 O5 4.4(5) . . . . ?
C16 C17 C19 C20 -2.5(5) . . . . ?
C18 C17 C19 C20 175.8(3) . . . . ?
C17 C19 C20 C14 0.4(6) . . . . ?
C15 C14 C20 C19 2.4(5) . . . . ?
C5 C14 C20 C19 -176.4(3) . . . . ?

_refine_diff_density_max         0.603
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.078

####################################################################### 
# 
# 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_400-9Co
_database_code_depnum_ccdc_archive 'CCDC 1984465'
_audit_update_record             
;
2020-02-17 deposited with the CCDC.	2020-05-11 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            'C30 H25 Co N3 O9'
_chemical_formula_weight         630.46

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                   6.9985(6)
_cell_length_b                   9.2423(13)
_cell_length_c                   21.235(2)
_cell_angle_alpha                91.236(10)
_cell_angle_beta                 91.092(8)
_cell_angle_gamma                105.276(10)
_cell_volume                     1324.2(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8358
_cell_measurement_theta_min      3.27
_cell_measurement_theta_max      25.049

_exptl_crystal_description       block
_exptl_crystal_colour            pink
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_F_000             650
_exptl_transmission_factor_min   0.837
_exptl_transmission_factor_max   0.855
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.220
_exptl_absorpt_coefficient_mu    0.713
_shelx_estimated_absorpt_T_min   0.842
_shelx_estimated_absorpt_T_max   0.859
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.842
_exptl_absorpt_correction_T_max  0.859
_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            8358
_diffrn_reflns_av_unetI/netI     0.1876
_diffrn_reflns_av_R_equivalents  0.0848
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.270
_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             4682
_reflns_number_gt                2258
_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)+(0.0544P)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         4682
_refine_ls_number_parameters     389
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1730
_refine_ls_R_factor_gt           0.0868
_refine_ls_wR_factor_ref         0.2158
_refine_ls_wR_factor_gt          0.1597
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.022
_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 0.50330(13) 0.69424(12) 0.66031(5) 0.0372(4) Uani 1 1 d . . . . .
N1 N 0.2881(8) 0.4058(7) 0.9216(3) 0.0422(17) Uani 1 1 d . . . . .
N2 N 0.6299(8) 0.7563(7) 0.5731(3) 0.0357(16) Uani 1 1 d . . . . .
N3 N 0.5947(8) 0.5036(7) 0.6291(3) 0.0326(15) Uani 1 1 d . . . . .
O1 O 0.3947(6) 0.5884(6) 0.7401(2) 0.0402(14) Uani 1 1 d . . . . .
O2 O 0.0744(7) 0.5848(6) 0.7365(2) 0.0475(15) Uani 1 1 d . . . . .
O3 O 0.4371(7) -0.1079(6) 0.6857(2) 0.0501(16) Uani 1 1 d . . . . .
O4 O 0.1389(7) -0.1144(6) 0.6451(2) 0.0444(14) Uani 1 1 d . . . . .
O5 O 0.2116(10) 1.1049(8) 1.1739(3) 0.078(2) Uani 1 1 d . . . . .
O6 O 0.2391(9) 1.2628(8) 1.0962(3) 0.0576(17) Uani 1 1 d . . . . .
H6 H 0.2501 1.3238 1.1256 0.086 Uiso 1 1 calc R U . . .
O7 O 0.7751(6) 0.7817(6) 0.7063(2) 0.0426(14) Uani 1 1 d . . . . .
H1W H 0.8821 0.8047 0.6865 0.051 Uiso 1 1 d R U . . .
H2W H 0.7584 0.7896 0.7442 0.051 Uiso 1 1 d R U . . .
O8 O 0.2058(6) 0.6211(6) 0.6161(2) 0.0406(14) Uani 1 1 d . . . . .
H3W H 0.1638 0.6945 0.6098 0.049 Uiso 1 1 d R U . . .
H4W H 0.1235 0.5575 0.6377 0.049 Uiso 1 1 d R U . . .
O9 O 0.2667(7) 0.4629(6) 0.1874(2) 0.0506(15) Uani 1 1 d . . . . .
H5W H 0.3753 0.4431 0.2080 0.061 Uiso 1 1 d R U . . .
H6W H 0.1645 0.4487 0.2098 0.061 Uiso 1 1 d R U . . .
C1 C 0.2268(11) 0.5758(9) 0.7652(3) 0.0359(19) Uani 1 1 d . . . . .
C2 C 0.2241(9) 0.5488(9) 0.8352(3) 0.0325(18) Uani 1 1 d . . . . .
C3 C 0.2106(9) 0.6629(9) 0.8755(4) 0.0359(19) Uani 1 1 d . . . . .
H3 H 0.1816 0.7479 0.8596 0.043 Uiso 1 1 calc R U . . .
C4 C 0.2396(10) 0.6529(9) 0.9400(4) 0.0355(19) Uani 1 1 d . . . . .
C5 C 0.2798(10) 0.5222(9) 0.9589(4) 0.043(2) Uani 1 1 d . . . . .
H5 H 0.3034 0.5141 1.0017 0.052 Uiso 1 1 calc R U . . .
C6 C 0.2537(10) 0.4161(9) 0.8595(3) 0.0321(18) Uani 1 1 d . . . . .
C7 C 0.2516(10) 0.2873(9) 0.8173(4) 0.0360(19) Uani 1 1 d . . . . .
C8 C 0.3916(11) 0.2045(10) 0.8252(4) 0.047(2) Uani 1 1 d . . . . .
H8A H 0.4805 0.2264 0.8594 0.056 Uiso 1 1 calc R U . . .
C9 C 0.3994(11) 0.0898(9) 0.7823(4) 0.044(2) Uani 1 1 d . . . . .
H9 H 0.4970 0.0391 0.7873 0.052 Uiso 1 1 calc R U . . .
C10 C 0.2635(10) 0.0504(8) 0.7326(4) 0.0349(19) Uani 1 1 d . . . . .
C11 C 0.2815(11) -0.0667(9) 0.6852(4) 0.038(2) Uani 1 1 d . . . . .
C12 C 0.1170(10) 0.1268(9) 0.7276(4) 0.039(2) Uani 1 1 d . . . . .
H12 H 0.0192 0.0984 0.6961 0.047 Uiso 1 1 calc R U . . .
C13 C 0.1149(10) 0.2427(8) 0.7684(4) 0.0362(19) Uani 1 1 d . . . . .
H13 H 0.0177 0.2936 0.7629 0.043 Uiso 1 1 calc R U . . .
C14 C 0.2307(10) 0.7780(9) 0.9846(4) 0.038(2) Uani 1 1 d . . . . .
C15 C 0.1977(10) 0.7499(10) 1.0487(4) 0.047(2) Uani 1 1 d . . . . .
H15 H 0.1770 0.6526 1.0629 0.056 Uiso 1 1 calc R U . . .
C16 C 0.1957(11) 0.8642(10) 1.0906(4) 0.049(2) Uani 1 1 d . . . . .
H16 H 0.1760 0.8440 1.1331 0.058 Uiso 1 1 calc R U . . .
C17 C 0.2224(9) 1.0080(9) 1.0707(4) 0.0353(19) Uani 1 1 d . . . . .
C18 C 0.2214(11) 1.1282(11) 1.1185(4) 0.048(2) Uani 1 1 d . . . . .
C19 C 0.2516(10) 1.0400(10) 1.0071(4) 0.043(2) Uani 1 1 d . . . . .
H19 H 0.2669 1.1368 0.9929 0.051 Uiso 1 1 calc R U . . .
C20 C 0.2572(10) 0.9225(9) 0.9657(4) 0.042(2) Uani 1 1 d . . . . .
H20 H 0.2798 0.9430 0.9234 0.050 Uiso 1 1 calc R U . . .
C21 C 0.6466(11) 0.8908(10) 0.5476(4) 0.051(2) Uani 1 1 d . . . . .
H21 H 0.6042 0.9631 0.5704 0.061 Uiso 1 1 calc R U . . .
C22 C 0.7239(11) 0.9256(11) 0.4890(4) 0.057(3) Uani 1 1 d . . . . .
H22 H 0.7371 1.0208 0.4734 0.068 Uiso 1 1 calc R U . . .
C23 C 0.7819(11) 0.8181(11) 0.4537(4) 0.054(2) Uani 1 1 d . . . . .
H23 H 0.8299 0.8380 0.4134 0.064 Uiso 1 1 calc R U . . .
C24 C 0.7665(10) 0.6806(11) 0.4798(4) 0.049(2) Uani 1 1 d . . . . .
H24 H 0.8040 0.6063 0.4569 0.059 Uiso 1 1 calc R U . . .
C25 C 0.6951(10) 0.6518(10) 0.5404(4) 0.041(2) Uani 1 1 d . . . . .
C26 C 0.6859(9) 0.5134(9) 0.5729(4) 0.0328(18) Uani 1 1 d . . . . .
C27 C 0.7659(10) 0.4035(10) 0.5495(4) 0.047(2) Uani 1 1 d . . . . .
H27 H 0.8245 0.4120 0.5103 0.057 Uiso 1 1 calc R U . . .
C28 C 0.7571(10) 0.2798(10) 0.5858(4) 0.052(2) Uani 1 1 d . . . . .
H28 H 0.8126 0.2048 0.5713 0.063 Uiso 1 1 calc R U . . .
C29 C 0.6667(10) 0.2665(10) 0.6432(4) 0.052(2) Uani 1 1 d . . . . .
H29 H 0.6602 0.1840 0.6682 0.062 Uiso 1 1 calc R U . . .
C30 C 0.5855(10) 0.3825(9) 0.6623(4) 0.041(2) Uani 1 1 d . . . . .
H30 H 0.5212 0.3741 0.7005 0.049 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 O1 2.034(5) . ?
Co1 O3 2.064(5) 1_565 ?
Co1 O7 2.076(4) . ?
Co1 N2 2.095(6) . ?
Co1 N3 2.124(6) . ?
Co1 O8 2.197(4) . ?
N1 C5 1.336(9) . ?
N1 C6 1.346(8) . ?
N2 C21 1.344(10) . ?
N2 C25 1.355(9) . ?
N3 C30 1.324(9) . ?
N3 C26 1.358(8) . ?
O1 C1 1.277(7) . ?
O2 C1 1.240(7) . ?
O3 C11 1.244(7) . ?
O3 Co1 2.064(5) 1_545 ?
O4 C11 1.279(8) . ?
O5 C18 1.199(10) . ?
O6 C18 1.316(10) . ?
O6 H6 0.8200 . ?
O7 H1W 0.8450 . ?
O7 H2W 0.8200 . ?
O8 H3W 0.8200 . ?
O8 H4W 0.8544 . ?
O9 H5W 0.9309 . ?
O9 H6W 0.8499 . ?
C1 C2 1.514(10) . ?
C2 C3 1.367(10) . ?
C2 C6 1.404(10) . ?
C3 C4 1.390(9) . ?
C3 H3 0.9300 . ?
C4 C5 1.377(10) . ?
C4 C14 1.493(10) . ?
C5 H5 0.9300 . ?
C6 C7 1.470(10) . ?
C7 C13 1.379(10) . ?
C7 C8 1.403(9) . ?
C8 C9 1.394(10) . ?
C8 H8A 0.9300 . ?
C9 C10 1.385(10) . ?
C9 H9 0.9300 . ?
C10 C12 1.394(9) . ?
C10 C11 1.492(10) . ?
C12 C13 1.366(9) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 C20 1.369(10) . ?
C14 C15 1.403(10) . ?
C15 C16 1.370(10) . ?
C15 H15 0.9300 . ?
C16 C17 1.369(11) . ?
C16 H16 0.9300 . ?
C17 C19 1.397(10) . ?
C17 C18 1.490(11) . ?
C19 C20 1.392(10) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
C21 C22 1.377(11) . ?
C21 H21 0.9300 . ?
C22 C23 1.381(11) . ?
C22 H22 0.9300 . ?
C23 C24 1.376(11) . ?
C23 H23 0.9300 . ?
C24 C25 1.394(10) . ?
C24 H24 0.9300 . ?
C25 C26 1.454(11) . ?
C26 C27 1.372(9) . ?
C27 C28 1.380(11) . ?
C27 H27 0.9300 . ?
C28 C29 1.378(11) . ?
C28 H28 0.9300 . ?
C29 C30 1.395(10) . ?
C29 H29 0.9300 . ?
C30 H30 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Co1 O3 94.2(2) . 1_565 ?
O1 Co1 O7 89.8(2) . . ?
O3 Co1 O7 86.71(19) 1_565 . ?
O1 Co1 N2 166.8(2) . . ?
O3 Co1 N2 99.0(2) 1_565 . ?
O7 Co1 N2 90.9(2) . . ?
O1 Co1 N3 90.7(2) . . ?
O3 Co1 N3 174.4(2) 1_565 . ?
O7 Co1 N3 90.60(19) . . ?
N2 Co1 N3 76.1(2) . . ?
O1 Co1 O8 89.50(19) . . ?
O3 Co1 O8 87.46(18) 1_565 . ?
O7 Co1 O8 174.06(18) . . ?
N2 Co1 O8 91.2(2) . . ?
N3 Co1 O8 95.31(19) . . ?
C5 N1 C6 117.4(7) . . ?
C21 N2 C25 118.8(7) . . ?
C21 N2 Co1 124.1(5) . . ?
C25 N2 Co1 117.0(5) . . ?
C30 N3 C26 117.7(6) . . ?
C30 N3 Co1 125.3(5) . . ?
C26 N3 Co1 116.7(5) . . ?
C1 O1 Co1 129.3(5) . . ?
C11 O3 Co1 133.7(5) . 1_545 ?
C18 O6 H6 109.5 . . ?
Co1 O7 H1W 121.8 . . ?
Co1 O7 H2W 109.5 . . ?
H1W O7 H2W 128.6 . . ?
Co1 O8 H3W 109.4 . . ?
Co1 O8 H4W 113.4 . . ?
H3W O8 H4W 110.1 . . ?
H5W O9 H6W 113.6 . . ?
O2 C1 O1 125.0(7) . . ?
O2 C1 C2 120.5(6) . . ?
O1 C1 C2 114.6(6) . . ?
C3 C2 C6 119.8(7) . . ?
C3 C2 C1 118.4(7) . . ?
C6 C2 C1 121.5(7) . . ?
C2 C3 C4 120.6(7) . . ?
C2 C3 H3 119.7 . . ?
C4 C3 H3 119.7 . . ?
C5 C4 C3 115.2(7) . . ?
C5 C4 C14 123.4(7) . . ?
C3 C4 C14 121.4(7) . . ?
N1 C5 C4 126.4(8) . . ?
N1 C5 H5 116.8 . . ?
C4 C5 H5 116.8 . . ?
N1 C6 C2 120.4(7) . . ?
N1 C6 C7 119.0(7) . . ?
C2 C6 C7 120.6(7) . . ?
C13 C7 C8 116.9(7) . . ?
C13 C7 C6 122.3(6) . . ?
C8 C7 C6 120.9(7) . . ?
C9 C8 C7 120.9(7) . . ?
C9 C8 H8A 119.6 . . ?
C7 C8 H8A 119.6 . . ?
C10 C9 C8 120.8(7) . . ?
C10 C9 H9 119.6 . . ?
C8 C9 H9 119.6 . . ?
C9 C10 C12 117.8(7) . . ?
C9 C10 C11 119.9(6) . . ?
C12 C10 C11 122.3(7) . . ?
O3 C11 O4 124.0(7) . . ?
O3 C11 C10 118.1(7) . . ?
O4 C11 C10 117.8(6) . . ?
C13 C12 C10 121.0(7) . . ?
C13 C12 H12 119.5 . . ?
C10 C12 H12 119.5 . . ?
C12 C13 C7 122.5(7) . . ?
C12 C13 H13 118.8 . . ?
C7 C13 H13 118.8 . . ?
C20 C14 C15 117.7(8) . . ?
C20 C14 C4 122.4(7) . . ?
C15 C14 C4 119.9(8) . . ?
C16 C15 C14 120.7(9) . . ?
C16 C15 H15 119.7 . . ?
C14 C15 H15 119.7 . . ?
C15 C16 C17 120.8(8) . . ?
C15 C16 H16 119.6 . . ?
C17 C16 H16 119.6 . . ?
C16 C17 C19 120.3(8) . . ?
C16 C17 C18 118.4(8) . . ?
C19 C17 C18 121.3(8) . . ?
O5 C18 O6 122.2(9) . . ?
O5 C18 C17 122.2(9) . . ?
O6 C18 C17 115.6(8) . . ?
C20 C19 C17 117.9(8) . . ?
C20 C19 H19 121.1 . . ?
C17 C19 H19 121.1 . . ?
C14 C20 C19 122.7(8) . . ?
C14 C20 H20 118.6 . . ?
C19 C20 H20 118.6 . . ?
N2 C21 C22 122.4(8) . . ?
N2 C21 H21 118.8 . . ?
C22 C21 H21 118.8 . . ?
C21 C22 C23 119.6(9) . . ?
C21 C22 H22 120.2 . . ?
C23 C22 H22 120.2 . . ?
C24 C23 C22 118.1(8) . . ?
C24 C23 H23 121.0 . . ?
C22 C23 H23 121.0 . . ?
C23 C24 C25 120.6(8) . . ?
C23 C24 H24 119.7 . . ?
C25 C24 H24 119.7 . . ?
N2 C25 C24 120.3(8) . . ?
N2 C25 C26 115.6(7) . . ?
C24 C25 C26 124.1(7) . . ?
N3 C26 C27 122.8(8) . . ?
N3 C26 C25 114.2(6) . . ?
C27 C26 C25 123.0(7) . . ?
C26 C27 C28 118.1(8) . . ?
C26 C27 H27 120.9 . . ?
C28 C27 H27 120.9 . . ?
C29 C28 C27 120.6(8) . . ?
C29 C28 H28 119.7 . . ?
C27 C28 H28 119.7 . . ?
C28 C29 C30 117.0(8) . . ?
C28 C29 H29 121.5 . . ?
C30 C29 H29 121.5 . . ?
N3 C30 C29 123.7(7) . . ?
N3 C30 H30 118.2 . . ?
C29 C30 H30 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
Co1 O1 C1 O2 23.8(11) . . . . ?
Co1 O1 C1 C2 -155.8(5) . . . . ?
O2 C1 C2 C3 -71.7(10) . . . . ?
O1 C1 C2 C3 107.9(7) . . . . ?
O2 C1 C2 C6 114.4(8) . . . . ?
O1 C1 C2 C6 -66.0(10) . . . . ?
C6 C2 C3 C4 4.5(10) . . . . ?
C1 C2 C3 C4 -169.5(6) . . . . ?
C2 C3 C4 C5 -0.6(10) . . . . ?
C2 C3 C4 C14 178.4(6) . . . . ?
C6 N1 C5 C4 -0.1(12) . . . . ?
C3 C4 C5 N1 -1.7(12) . . . . ?
C14 C4 C5 N1 179.3(7) . . . . ?
C5 N1 C6 C2 4.3(10) . . . . ?
C5 N1 C6 C7 -176.9(6) . . . . ?
C3 C2 C6 N1 -6.5(11) . . . . ?
C1 C2 C6 N1 167.4(6) . . . . ?
C3 C2 C6 C7 174.7(6) . . . . ?
C1 C2 C6 C7 -11.4(10) . . . . ?
N1 C6 C7 C13 139.4(7) . . . . ?
C2 C6 C7 C13 -41.8(11) . . . . ?
N1 C6 C7 C8 -41.2(10) . . . . ?
C2 C6 C7 C8 137.6(8) . . . . ?
C13 C7 C8 C9 4.5(12) . . . . ?
C6 C7 C8 C9 -175.0(7) . . . . ?
C7 C8 C9 C10 -2.9(12) . . . . ?
C8 C9 C10 C12 -1.4(12) . . . . ?
C8 C9 C10 C11 176.5(7) . . . . ?
Co1 O3 C11 O4 -31.3(12) 1_545 . . . ?
Co1 O3 C11 C10 151.5(6) 1_545 . . . ?
C9 C10 C11 O3 -11.9(11) . . . . ?
C12 C10 C11 O3 165.9(7) . . . . ?
C9 C10 C11 O4 170.7(7) . . . . ?
C12 C10 C11 O4 -11.5(11) . . . . ?
C9 C10 C12 C13 3.9(11) . . . . ?
C11 C10 C12 C13 -174.0(7) . . . . ?
C10 C12 C13 C7 -2.2(12) . . . . ?
C8 C7 C13 C12 -2.0(12) . . . . ?
C6 C7 C13 C12 177.4(7) . . . . ?
C5 C4 C14 C20 157.5(7) . . . . ?
C3 C4 C14 C20 -21.4(10) . . . . ?
C5 C4 C14 C15 -21.3(11) . . . . ?
C3 C4 C14 C15 159.8(7) . . . . ?
C20 C14 C15 C16 -1.1(11) . . . . ?
C4 C14 C15 C16 177.8(6) . . . . ?
C14 C15 C16 C17 1.1(11) . . . . ?
C15 C16 C17 C19 0.2(11) . . . . ?
C15 C16 C17 C18 -179.2(6) . . . . ?
C16 C17 C18 O5 5.2(12) . . . . ?
C19 C17 C18 O5 -174.2(7) . . . . ?
C16 C17 C18 O6 -177.2(7) . . . . ?
C19 C17 C18 O6 3.5(10) . . . . ?
C16 C17 C19 C20 -1.5(10) . . . . ?
C18 C17 C19 C20 177.9(6) . . . . ?
C15 C14 C20 C19 -0.3(11) . . . . ?
C4 C14 C20 C19 -179.1(6) . . . . ?
C17 C19 C20 C14 1.6(11) . . . . ?
C25 N2 C21 C22 1.3(12) . . . . ?
Co1 N2 C21 C22 -177.5(6) . . . . ?
N2 C21 C22 C23 2.0(13) . . . . ?
C21 C22 C23 C24 -2.4(12) . . . . ?
C22 C23 C24 C25 -0.3(12) . . . . ?
C21 N2 C25 C24 -4.0(10) . . . . ?
Co1 N2 C25 C24 174.8(5) . . . . ?
C21 N2 C25 C26 175.6(6) . . . . ?
Co1 N2 C25 C26 -5.6(8) . . . . ?
C23 C24 C25 N2 3.5(11) . . . . ?
C23 C24 C25 C26 -176.0(7) . . . . ?
C30 N3 C26 C27 0.5(10) . . . . ?
Co1 N3 C26 C27 174.8(6) . . . . ?
C30 N3 C26 C25 -178.2(6) . . . . ?
Co1 N3 C26 C25 -3.9(8) . . . . ?
N2 C25 C26 N3 6.2(9) . . . . ?
C24 C25 C26 N3 -174.3(7) . . . . ?
N2 C25 C26 C27 -172.5(7) . . . . ?
C24 C25 C26 C27 7.0(12) . . . . ?
N3 C26 C27 C28 -1.7(11) . . . . ?
C25 C26 C27 C28 176.9(7) . . . . ?
C26 C27 C28 C29 1.2(12) . . . . ?
C27 C28 C29 C30 0.2(12) . . . . ?
C26 N3 C30 C29 1.1(11) . . . . ?
Co1 N3 C30 C29 -172.6(5) . . . . ?
C28 C29 C30 N3 -1.5(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
C30 H30 O1 0.93 2.51 3.070(9) 119.0 .
C24 H24 O8 0.93 2.57 3.466(10) 162.3 2_666
O9 H6W O2 0.85 2.00 2.851(7) 179.4 2_566
O9 H5W O1 0.93 2.02 2.949(7) 174.5 2_666
O8 H4W O2 0.85 2.15 2.731(7) 124.7 .
O8 H3W O4 0.82 1.95 2.669(7) 145.2 1_565
O7 H2W O5 0.82 1.96 2.722(8) 155.1 2_677
O7 H1W O4 0.84 1.99 2.826(7) 172.5 1_665
O6 H6 O9 0.82 1.80 2.617(7) 176.8 1_566
O6 H6 O9 0.82 1.80 2.617(7) 176.8 1_566
O7 H1W O4 0.84 1.99 2.826(7) 172.5 1_665
O7 H2W O5 0.82 1.96 2.722(8) 155.1 2_677
O8 H3W O4 0.82 1.95 2.669(7) 145.2 1_565
O8 H4W O2 0.85 2.15 2.731(7) 124.7 .
O9 H5W O1 0.93 2.02 2.949(7) 174.5 2_666
O9 H6W O2 0.85 2.00 2.851(7) 179.4 2_566
C24 H24 O8 0.93 2.57 3.466(10) 162.3 2_666
C30 H30 O1 0.93 2.51 3.070(9) 119.0 .
O6 H6 O9 0.82 1.80 2.617(7) 176.8 1_566
O7 H1W O4 0.84 1.99 2.826(7) 172.5 1_665
O7 H2W O5 0.82 1.96 2.722(8) 155.1 2_677
O8 H3W O4 0.82 1.95 2.669(7) 145.2 1_565
O8 H4W O2 0.85 2.15 2.731(7) 124.7 .
O9 H5W O1 0.93 2.02 2.949(7) 174.5 2_666
O9 H6W O2 0.85 2.00 2.851(7) 179.4 2_566
C24 H24 O8 0.93 2.57 3.466(10) 162.3 2_666
C30 H30 O1 0.93 2.51 3.070(9) 119.0 .

_refine_diff_density_max         0.687
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.100

####################################################################### 
# 
# 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_401-7Zn
_database_code_depnum_ccdc_archive 'CCDC 1984467'
_audit_update_record             
;
2020-02-17 deposited with the CCDC.	2020-05-11 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            'C26 H17 N5 O6 Zn'
_chemical_formula_weight         560.82

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 '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                   9.1466(7)
_cell_length_b                   9.5909(7)
_cell_length_c                   13.2159(10)
_cell_angle_alpha                84.013(6)
_cell_angle_beta                 78.778(7)
_cell_angle_gamma                77.986(7)
_cell_volume                     1109.82(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6756
_cell_measurement_theta_min      4.724
_cell_measurement_theta_max      65.999

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.678
_exptl_crystal_F_000             572
_exptl_transmission_factor_min   0.630
_exptl_transmission_factor_max   0.665
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    2.041
_shelx_estimated_absorpt_T_min   0.629
_shelx_estimated_absorpt_T_max   0.686
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.629
_exptl_absorpt_correction_T_max  0.686
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\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            6756
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_av_R_equivalents  0.0185
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         4.724
_diffrn_reflns_theta_max         65.999
_diffrn_reflns_theta_full        65.999
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measured_fraction_theta_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_point_group_measured_fraction_full 0.960
_reflns_number_total             3709
_reflns_number_gt                3320
_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)+(0.0415P)²+0.1954P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3709
_refine_ls_number_parameters     344
_refine_ls_number_restraints     55
_refine_ls_R_factor_all          0.0333
_refine_ls_R_factor_gt           0.0286
_refine_ls_wR_factor_ref         0.0760
_refine_ls_wR_factor_gt          0.0724
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.085
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.33063(3) 1.08241(2) 0.48137(2) 0.02530(9) Uani 1 1 d . . . . .
N1 N 0.5691(2) 0.67865(18) 0.88733(13) 0.0344(4) Uani 1 1 d . . . . .
N2 N 0.19332(18) 1.22144(18) 0.38353(13) 0.0299(3) Uani 1 1 d . . . . .
N5 N 0.21693(18) 0.94136(18) 0.43607(12) 0.0286(3) Uani 1 1 d . . . . .
O1 O 0.44622(15) 0.93695(15) 0.58758(10) 0.0291(3) Uani 1 1 d . . . . .
O2 O 0.24319(16) 0.87758(16) 0.68967(12) 0.0360(3) Uani 1 1 d . . . . .
O3 O 0.1846(2) 0.1873(2) 0.72693(15) 0.0555(5) Uani 1 1 d . . . . .
O4 O 0.3079(2) 0.23906(17) 0.56977(13) 0.0519(5) Uani 1 1 d . . . . .
O5 O 0.9767(2) 1.32041(18) 1.05430(15) 0.0531(5) Uani 1 1 d . . . . .
H5 H 1.0201 1.3856 1.0589 0.080 Uiso 1 1 calc R U . . .
O6 O 0.9054(2) 1.46188(19) 0.92053(14) 0.0508(4) Uani 1 1 d . . . . .
C1 C 0.3772(2) 0.88670(18) 0.67393(14) 0.0237(4) Uani 1 1 d . . . . .
C2 C 0.4711(2) 0.84438(19) 0.75774(13) 0.0229(3) Uani 1 1 d . . . . .
C3 C 0.5327(2) 0.94930(19) 0.78839(14) 0.0251(4) Uani 1 1 d . . . . .
H3 H 0.5191 1.0401 0.7549 0.030 Uiso 1 1 calc R U . . .
C4 C 0.6150(2) 0.9207(2) 0.86879(13) 0.0247(4) Uani 1 1 d . . . . .
C5 C 0.6271(3) 0.7822(2) 0.91533(16) 0.0343(4) Uani 1 1 d . . . . .
H5A H 0.6797 0.7605 0.9703 0.041 Uiso 1 1 calc R U . . .
C6 C 0.4934(2) 0.7081(2) 0.80778(14) 0.0251(4) Uani 1 1 d . . . . .
C7 C 0.4410(2) 0.58713(19) 0.77333(14) 0.0259(4) Uani 1 1 d . . . . .
C8 C 0.3769(2) 0.4893(2) 0.84358(14) 0.0301(4) Uani 1 1 d . . . . .
H8 H 0.3726 0.4946 0.9140 0.036 Uiso 1 1 calc R U . . .
C9 C 0.3190(2) 0.3831(2) 0.80949(15) 0.0314(4) Uani 1 1 d . . . . .
H9 H 0.2716 0.3211 0.8574 0.038 Uiso 1 1 calc R U . . .
C10 C 0.3313(2) 0.36891(19) 0.70426(15) 0.0280(4) Uani 1 1 d . . . . .
C11 C 0.2674(2) 0.2546(2) 0.66639(17) 0.0333(4) Uani 1 1 d . . . . .
C12 C 0.4012(2) 0.4628(2) 0.63422(15) 0.0332(4) Uani 1 1 d . . . . .
H12 H 0.4126 0.4526 0.5637 0.040 Uiso 1 1 calc R U . . .
C13 C 0.4543(2) 0.5715(2) 0.66769(15) 0.0324(4) Uani 1 1 d . . . . .
H13 H 0.4993 0.6348 0.6195 0.039 Uiso 1 1 calc R U . . .
C14 C 0.6866(2) 1.0309(2) 0.90048(14) 0.0262(4) Uani 1 1 d . . . . .
C15 C 0.7554(3) 1.0093(2) 0.98800(17) 0.0377(5) Uani 1 1 d . . . . .
H15 H 0.7542 0.9246 1.0292 0.045 Uiso 1 1 calc R U . . .
C16 C 0.8254(3) 1.1120(2) 1.01445(18) 0.0398(5) Uani 1 1 d . . . . .
H16 H 0.8699 1.0962 1.0733 0.048 Uiso 1 1 calc R U . . .
C17 C 0.8292(2) 1.2384(2) 0.95323(16) 0.0320(4) Uani 1 1 d . . . . .
C18 C 0.9077(2) 1.3492(2) 0.97533(17) 0.0349(4) Uani 1 1 d . . . . .
C19 C 0.7568(3) 1.2635(2) 0.86854(18) 0.0420(5) Uani 1 1 d . . . . .
H19 H 0.7548 1.3498 0.8291 0.050 Uiso 1 1 calc R U . . .
C20 C 0.6875(3) 1.1607(2) 0.84250(17) 0.0393(5) Uani 1 1 d . . . . .
H20 H 0.6404 1.1786 0.7849 0.047 Uiso 1 1 calc R U . . .
C21 C 0.1519(3) 1.3624(2) 0.35265(19) 0.0400(4) Uani 1 1 d . U . . .
H21 H 0.1988 1.4353 0.3637 0.048 Uiso 1 1 calc R U . . .
C22 C 0.0312(3) 1.3795(3) 0.30329(19) 0.0428(4) Uani 1 1 d . U . . .
H22 H -0.0189 1.4644 0.2747 0.051 Uiso 1 1 calc R U . . .
N3 N -0.00131(19) 1.2463(2) 0.30438(14) 0.0365(3) Uani 1 1 d . U . . .
H1 H -0.0722 1.2252 0.2781 0.044 Uiso 1 1 calc R U . . .
C23 C 0.0975(2) 1.1550(2) 0.35388(14) 0.0284(3) Uani 1 1 d . U . . .
C24 C 0.1112(2) 1.0031(2) 0.38081(14) 0.0278(3) Uani 1 1 d . U . . .
N4 N 0.03394(19) 0.90778(19) 0.36101(13) 0.0337(3) Uani 1 1 d . U . . .
H2 H -0.0396 0.9249 0.3269 0.040 Uiso 1 1 calc R U . . .
C25 C 0.0934(3) 0.7786(2) 0.40498(17) 0.0386(4) Uani 1 1 d . U . . .
H25 H 0.0624 0.6926 0.4036 0.046 Uiso 1 1 calc R U . . .
C26 C 0.2070(3) 0.7999(2) 0.45120(17) 0.0363(4) Uani 1 1 d . U . . .
H26 H 0.2677 0.7299 0.4871 0.044 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O4 1.9510(15) 1_565 ?
Zn1 O1 2.0455(14) 2_676 ?
Zn1 N5 2.0657(15) . ?
Zn1 O1 2.1422(13) . ?
Zn1 N2 2.1454(16) . ?
N1 C5 1.333(3) . ?
N1 C6 1.343(3) . ?
N2 C23 1.321(2) . ?
N2 C21 1.367(3) . ?
N5 C24 1.329(3) . ?
N5 C26 1.370(3) . ?
O1 C1 1.290(2) . ?
O1 Zn1 2.0455(13) 2_676 ?
O2 C1 1.223(2) . ?
O3 C11 1.221(3) . ?
O4 C11 1.274(3) . ?
O4 Zn1 1.9511(15) 1_545 ?
O5 C18 1.299(3) . ?
O5 H5 0.8200 . ?
O6 C18 1.235(3) . ?
C1 C2 1.503(2) . ?
C2 C3 1.380(2) . ?
C2 C6 1.396(3) . ?
C3 C4 1.391(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.396(3) . ?
C4 C14 1.486(2) . ?
C5 H5A 0.9300 . ?
C6 C7 1.486(2) . ?
C7 C8 1.387(3) . ?
C7 C13 1.399(3) . ?
C8 C9 1.391(3) . ?
C8 H8 0.9300 . ?
C9 C10 1.392(3) . ?
C9 H9 0.9300 . ?
C10 C12 1.382(3) . ?
C10 C11 1.512(2) . ?
C12 C13 1.382(3) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 C20 1.393(3) . ?
C14 C15 1.399(3) . ?
C15 C16 1.387(3) . ?
C15 H15 0.9300 . ?
C16 C17 1.388(3) . ?
C16 H16 0.9300 . ?
C17 C19 1.384(3) . ?
C17 C18 1.481(3) . ?
C19 C20 1.382(3) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
C21 C22 1.361(3) . ?
C21 H21 0.9300 . ?
C22 N3 1.368(3) . ?
C22 H22 0.9300 . ?
N3 C23 1.339(3) . ?
N3 H1 0.8600 . ?
C23 C24 1.449(3) . ?
C24 N4 1.339(3) . ?
N4 C25 1.364(3) . ?
N4 H2 0.8600 . ?
C25 C26 1.361(3) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Zn1 O1 101.37(7) 1_565 2_676 ?
O4 Zn1 N5 143.81(8) 1_565 . ?
O1 Zn1 N5 114.82(6) 2_676 . ?
O4 Zn1 O1 90.72(7) 1_565 . ?
O1 Zn1 O1 77.08(6) 2_676 . ?
N5 Zn1 O1 97.36(6) . . ?
O4 Zn1 N2 89.58(7) 1_565 . ?
O1 Zn1 N2 108.74(6) 2_676 . ?
N5 Zn1 N2 78.96(6) . . ?
O1 Zn1 N2 173.99(6) . . ?
C5 N1 C6 118.14(17) . . ?
C23 N2 C21 105.90(17) . . ?
C23 N2 Zn1 111.28(13) . . ?
C21 N2 Zn1 141.76(14) . . ?
C24 N5 C26 106.21(16) . . ?
C24 N5 Zn1 113.91(13) . . ?
C26 N5 Zn1 139.65(14) . . ?
C1 O1 Zn1 133.91(12) . 2_676 ?
C1 O1 Zn1 123.11(12) . . ?
Zn1 O1 Zn1 102.92(6) 2_676 . ?
C11 O4 Zn1 134.88(15) . 1_545 ?
C18 O5 H5 109.5 . . ?
O2 C1 O1 123.43(17) . . ?
O2 C1 C2 121.01(17) . . ?
O1 C1 C2 115.52(15) . . ?
C3 C2 C6 119.21(16) . . ?
C3 C2 C1 117.09(16) . . ?
C6 C2 C1 123.65(16) . . ?
C2 C3 C4 120.71(17) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 H3 119.6 . . ?
C3 C4 C5 115.42(16) . . ?
C3 C4 C14 121.45(17) . . ?
C5 C4 C14 123.12(17) . . ?
N1 C5 C4 125.22(17) . . ?
N1 C5 H5A 117.4 . . ?
C4 C5 H5A 117.4 . . ?
N1 C6 C2 121.25(16) . . ?
N1 C6 C7 116.65(17) . . ?
C2 C6 C7 122.05(16) . . ?
C8 C7 C13 118.62(17) . . ?
C8 C7 C6 121.60(16) . . ?
C13 C7 C6 119.78(17) . . ?
C7 C8 C9 120.45(17) . . ?
C7 C8 H8 119.8 . . ?
C9 C8 H8 119.8 . . ?
C8 C9 C10 120.57(18) . . ?
C8 C9 H9 119.7 . . ?
C10 C9 H9 119.7 . . ?
C12 C10 C9 118.87(17) . . ?
C12 C10 C11 120.15(18) . . ?
C9 C10 C11 120.98(18) . . ?
O3 C11 O4 125.89(19) . . ?
O3 C11 C10 120.10(19) . . ?
O4 C11 C10 114.00(19) . . ?
C10 C12 C13 120.79(18) . . ?
C10 C12 H12 119.6 . . ?
C13 C12 H12 119.6 . . ?
C12 C13 C7 120.59(18) . . ?
C12 C13 H13 119.7 . . ?
C7 C13 H13 119.7 . . ?
C20 C14 C15 117.57(17) . . ?
C20 C14 C4 120.32(17) . . ?
C15 C14 C4 122.12(18) . . ?
C16 C15 C14 121.1(2) . . ?
C16 C15 H15 119.4 . . ?
C14 C15 H15 119.4 . . ?
C15 C16 C17 120.06(19) . . ?
C15 C16 H16 120.0 . . ?
C17 C16 H16 120.0 . . ?
C19 C17 C16 119.43(18) . . ?
C19 C17 C18 118.18(19) . . ?
C16 C17 C18 122.39(19) . . ?
O6 C18 O5 123.24(19) . . ?
O6 C18 C17 120.5(2) . . ?
O5 C18 C17 116.27(19) . . ?
C20 C19 C17 120.2(2) . . ?
C20 C19 H19 119.9 . . ?
C17 C19 H19 119.9 . . ?
C19 C20 C14 121.57(19) . . ?
C19 C20 H20 119.2 . . ?
C14 C20 H20 119.2 . . ?
C22 C21 N2 109.47(19) . . ?
C22 C21 H21 125.3 . . ?
N2 C21 H21 125.3 . . ?
C21 C22 N3 106.03(19) . . ?
C21 C22 H22 127.0 . . ?
N3 C22 H22 127.0 . . ?
C23 N3 C22 107.43(17) . . ?
C23 N3 H1 126.3 . . ?
C22 N3 H1 126.3 . . ?
N2 C23 N3 111.17(18) . . ?
N2 C23 C24 117.85(17) . . ?
N3 C23 C24 130.95(18) . . ?
N5 C24 N4 110.84(18) . . ?
N5 C24 C23 117.42(16) . . ?
N4 C24 C23 131.73(18) . . ?
C24 N4 C25 107.36(17) . . ?
C24 N4 H2 126.3 . . ?
C25 N4 H2 126.3 . . ?
C26 C25 N4 106.86(18) . . ?
C26 C25 H25 126.6 . . ?
N4 C25 H25 126.6 . . ?
C25 C26 N5 108.7(2) . . ?
C25 C26 H26 125.6 . . ?
N5 C26 H26 125.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Zn1 O1 C1 O2 -159.12(14) 2_676 . . . ?
Zn1 O1 C1 O2 24.3(2) . . . . ?
Zn1 O1 C1 C2 23.3(2) 2_676 . . . ?
Zn1 O1 C1 C2 -153.26(12) . . . . ?
O2 C1 C2 C3 -118.9(2) . . . . ?
O1 C1 C2 C3 58.8(2) . . . . ?
O2 C1 C2 C6 58.6(3) . . . . ?
O1 C1 C2 C6 -123.78(19) . . . . ?
C6 C2 C3 C4 -0.6(3) . . . . ?
C1 C2 C3 C4 176.96(16) . . . . ?
C2 C3 C4 C5 -1.1(3) . . . . ?
C2 C3 C4 C14 177.90(17) . . . . ?
C6 N1 C5 C4 0.3(3) . . . . ?
C3 C4 C5 N1 1.3(3) . . . . ?
C14 C4 C5 N1 -177.7(2) . . . . ?
C5 N1 C6 C2 -2.2(3) . . . . ?
C5 N1 C6 C7 175.27(19) . . . . ?
C3 C2 C6 N1 2.3(3) . . . . ?
C1 C2 C6 N1 -175.09(18) . . . . ?
C3 C2 C6 C7 -174.98(17) . . . . ?
C1 C2 C6 C7 7.6(3) . . . . ?
N1 C6 C7 C8 42.4(3) . . . . ?
C2 C6 C7 C8 -140.2(2) . . . . ?
N1 C6 C7 C13 -138.4(2) . . . . ?
C2 C6 C7 C13 39.0(3) . . . . ?
C13 C7 C8 C9 -3.8(3) . . . . ?
C6 C7 C8 C9 175.38(18) . . . . ?
C7 C8 C9 C10 3.3(3) . . . . ?
C8 C9 C10 C12 -0.4(3) . . . . ?
C8 C9 C10 C11 -179.47(18) . . . . ?
Zn1 O4 C11 O3 -25.9(4) 1_545 . . . ?
Zn1 O4 C11 C10 154.38(17) 1_545 . . . ?
C12 C10 C11 O3 -168.0(2) . . . . ?
C9 C10 C11 O3 11.0(3) . . . . ?
C12 C10 C11 O4 11.7(3) . . . . ?
C9 C10 C11 O4 -169.26(19) . . . . ?
C9 C10 C12 C13 -1.8(3) . . . . ?
C11 C10 C12 C13 177.25(19) . . . . ?
C10 C12 C13 C7 1.2(3) . . . . ?
C8 C7 C13 C12 1.6(3) . . . . ?
C6 C7 C13 C12 -177.61(19) . . . . ?
C3 C4 C14 C20 -7.4(3) . . . . ?
C5 C4 C14 C20 171.5(2) . . . . ?
C3 C4 C14 C15 172.90(19) . . . . ?
C5 C4 C14 C15 -8.2(3) . . . . ?
C20 C14 C15 C16 -1.6(3) . . . . ?
C4 C14 C15 C16 178.1(2) . . . . ?
C14 C15 C16 C17 -0.5(4) . . . . ?
C15 C16 C17 C19 2.9(4) . . . . ?
C15 C16 C17 C18 -177.5(2) . . . . ?
C19 C17 C18 O6 1.5(3) . . . . ?
C16 C17 C18 O6 -178.2(2) . . . . ?
C19 C17 C18 O5 -178.7(2) . . . . ?
C16 C17 C18 O5 1.6(3) . . . . ?
C16 C17 C19 C20 -3.0(4) . . . . ?
C18 C17 C19 C20 177.3(2) . . . . ?
C17 C19 C20 C14 0.8(4) . . . . ?
C15 C14 C20 C19 1.5(4) . . . . ?
C4 C14 C20 C19 -178.2(2) . . . . ?
C23 N2 C21 C22 -0.6(3) . . . . ?
Zn1 N2 C21 C22 -166.83(18) . . . . ?
N2 C21 C22 N3 0.1(3) . . . . ?
C21 C22 N3 C23 0.5(3) . . . . ?
C21 N2 C23 N3 0.9(2) . . . . ?
Zn1 N2 C23 N3 171.81(13) . . . . ?
C21 N2 C23 C24 -177.43(18) . . . . ?
Zn1 N2 C23 C24 -6.5(2) . . . . ?
C22 N3 C23 N2 -0.9(2) . . . . ?
C22 N3 C23 C24 177.2(2) . . . . ?
C26 N5 C24 N4 0.5(2) . . . . ?
Zn1 N5 C24 N4 -175.10(13) . . . . ?
C26 N5 C24 C23 179.96(17) . . . . ?
Zn1 N5 C24 C23 4.3(2) . . . . ?
N2 C23 C24 N5 1.7(3) . . . . ?
N3 C23 C24 N5 -176.2(2) . . . . ?
N2 C23 C24 N4 -179.0(2) . . . . ?
N3 C23 C24 N4 3.1(4) . . . . ?
N5 C24 N4 C25 -0.4(2) . . . . ?
C23 C24 N4 C25 -179.7(2) . . . . ?
C24 N4 C25 C26 0.1(2) . . . . ?
N4 C25 C26 N5 0.2(3) . . . . ?
C24 N5 C26 C25 -0.5(2) . . . . ?
Zn1 N5 C26 C25 173.39(16) . . . . ?

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
N4 H2 O3 0.86 2.13 2.839(2) 139.3 2_566
N4 H2 O2 0.86 2.39 3.052(2) 134.2 2_576
N3 H1 O2 0.86 1.97 2.706(2) 142.4 2_576
O5 H5 O6 0.82 1.80 2.618(2) 173.0 2_787
O5 H5 O6 0.82 1.80 2.618(2) 173.0 2_787
N3 H1 O2 0.86 1.97 2.706(2) 142.4 2_576
N4 H2 O2 0.86 2.39 3.052(2) 134.2 2_576
N4 H2 O3 0.86 2.13 2.839(2) 139.3 2_566

_refine_diff_density_max         0.263
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.051

####################################################################### 
# 
# 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_405-5Zn
_database_code_depnum_ccdc_archive 'CCDC 1984464'
_audit_update_record             
;
2020-02-17 deposited with the CCDC.	2020-05-11 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            'C32 H19 N3 O6 Zn'
_chemical_formula_weight         606.87

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 '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                   17.6863(4)
_cell_length_b                   17.2313(3)
_cell_length_c                   18.2480(3)
_cell_angle_alpha                90
_cell_angle_beta                 108.186(2)
_cell_angle_gamma                90
_cell_volume                     5283.43(18)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    21385
_cell_measurement_theta_min      3.616
_cell_measurement_theta_max      64.999

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_F_000             2480
_exptl_transmission_factor_min   0.679
_exptl_transmission_factor_max   0.681
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.220
_exptl_absorpt_coefficient_mu    1.745
_shelx_estimated_absorpt_T_min   0.670
_shelx_estimated_absorpt_T_max   0.700
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.670
_exptl_absorpt_correction_T_max  0.700
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\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            21385
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.616
_diffrn_reflns_theta_max         64.999
_diffrn_reflns_theta_full        64.999
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measured_fraction_theta_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_point_group_measured_fraction_full 0.980
_reflns_number_total             8814
_reflns_number_gt                6899
_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)+(0.0878P)²+1.8603P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8814
_refine_ls_number_parameters     759
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0486
_refine_ls_wR_factor_ref         0.1515
_refine_ls_wR_factor_gt          0.1338
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_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 0.33708(3) 0.07669(2) 0.06511(2) 0.03641(14) Uani 1 1 d . . . . .
Zn2 Zn 0.33927(3) 0.11495(2) 0.56520(2) 0.03809(14) Uani 1 1 d . . . . .
N1 N 0.40345(15) 0.41373(14) -0.02641(13) 0.0337(5) Uani 1 1 d . . . . .
N2 N 0.38235(16) -0.22164(14) 0.46845(13) 0.0343(5) Uani 1 1 d . . . . .
N3 N 0.24303(16) -0.00070(15) 0.01219(16) 0.0415(6) Uani 1 1 d . . . . .
N4 N 0.37029(16) 0.03773(16) -0.03083(15) 0.0397(6) Uani 1 1 d . . . . .
N5 N 0.37241(17) 0.14601(16) 0.46641(15) 0.0415(6) Uani 1 1 d . . . . .
N6 N 0.25144(17) 0.19766(15) 0.51277(18) 0.0481(7) Uani 1 1 d . . . . .
O1 O 0.30978(18) 0.18819(14) 0.03830(16) 0.0589(7) Uani 1 1 d . . . . .
O2 O 0.4401(2) 0.17820(16) 0.07941(19) 0.0838(11) Uani 1 1 d . . . . .
O3 O 0.43502(16) 0.60599(15) 0.42584(13) 0.0533(6) Uani 1 1 d . . . . .
O4 O 0.38774(19) 0.70124(14) 0.34154(14) 0.0576(7) Uani 1 1 d . . . . .
H4 H 0.3921 0.7263 0.3809 0.086 Uiso 1 1 calc R U . . .
O5 O 0.3212(2) 0.12050(15) -0.32633(15) 0.0633(8) Uani 1 1 d . . . . .
O6 O 0.41395(15) 0.19340(16) -0.34538(13) 0.0539(6) Uani 1 1 d . . . . .
O7 O 0.39892(14) 0.00583(15) 0.15660(13) 0.0464(6) Uani 1 1 d . . . . .
O8 O 0.30247(18) 0.07649(15) 0.17136(14) 0.0559(7) Uani 1 1 d . . . . .
O9 O 0.27702(14) 0.00652(13) 0.52476(14) 0.0465(5) Uani 1 1 d . . . . .
O10 O 0.40617(15) 0.00860(13) 0.57438(15) 0.0520(6) Uani 1 1 d . . . . .
O11 O 0.39035(19) -0.50658(14) 0.84504(14) 0.0576(7) Uani 1 1 d . . . . .
H11 H 0.3954 -0.5305 0.8852 0.086 Uiso 1 1 calc R U . . .
O12 O 0.41228(16) -0.40378(14) 0.92356(13) 0.0505(6) Uani 1 1 d . . . . .
C1 C 0.3784(3) 0.21637(19) 0.05428(18) 0.0495(9) Uani 1 1 d . . . . .
C2 C 0.38538(19) 0.30352(17) 0.04443(17) 0.0356(6) Uani 1 1 d . . . . .
C3 C 0.38789(19) 0.35081(17) 0.10605(17) 0.0366(6) Uani 1 1 d . . . . .
H3 H 0.3818 0.3292 0.1506 0.044 Uiso 1 1 calc R U . . .
C4 C 0.39941(17) 0.43040(16) 0.10263(16) 0.0314(6) Uani 1 1 d . . . . .
C5 C 0.40657(19) 0.45841(16) 0.03343(16) 0.0351(6) Uani 1 1 d . . . . .
H5 H 0.4139 0.5114 0.0291 0.042 Uiso 1 1 calc R U . . .
C6 C 0.39396(18) 0.33634(16) -0.02218(17) 0.0333(6) Uani 1 1 d . . . . .
C7 C 0.39212(18) 0.29149(15) -0.09196(15) 0.0315(6) Uani 1 1 d . . . . .
C8 C 0.3319(2) 0.23741(18) -0.12341(17) 0.0391(7) Uani 1 1 d . . . . .
H8 H 0.2942 0.2276 -0.0987 0.047 Uiso 1 1 calc R U . . .
C9 C 0.3275(2) 0.19834(18) -0.19048(17) 0.0420(7) Uani 1 1 d . . . . .
H9 H 0.2864 0.1632 -0.2110 0.050 Uiso 1 1 calc R U . . .
C10 C 0.38370(19) 0.21079(17) -0.22772(17) 0.0365(6) Uani 1 1 d . . . . .
C11 C 0.3732(2) 0.1722(2) -0.30424(18) 0.0459(8) Uani 1 1 d . . . . .
C12 C 0.44445(19) 0.2639(2) -0.19627(18) 0.0419(7) Uani 1 1 d . . . . .
H12 H 0.4828 0.2727 -0.2205 0.050 Uiso 1 1 calc R U . . .
C13 C 0.44839(18) 0.30363(19) -0.12971(17) 0.0389(7) Uani 1 1 d . . . . .
H13 H 0.4893 0.3391 -0.1097 0.047 Uiso 1 1 calc R U . . .
C14 C 0.40445(17) 0.48301(17) 0.16846(16) 0.0321(6) Uani 1 1 d . . . . .
C15 C 0.4345(2) 0.45623(18) 0.24421(17) 0.0396(7) Uani 1 1 d . . . . .
H15 H 0.4523 0.4053 0.2535 0.048 Uiso 1 1 calc R U . . .
C16 C 0.4379(2) 0.50467(19) 0.30547(18) 0.0416(7) Uani 1 1 d . . . . .
H16 H 0.4584 0.4863 0.3557 0.050 Uiso 1 1 calc R U . . .
C17 C 0.41084(18) 0.58105(17) 0.29233(17) 0.0345(6) Uani 1 1 d . . . . .
C18 C 0.41305(19) 0.63022(19) 0.36013(18) 0.0385(7) Uani 1 1 d . . . . .
C19 C 0.38162(19) 0.60782(17) 0.21724(18) 0.0375(7) Uani 1 1 d . . . . .
H19 H 0.3639 0.6588 0.2079 0.045 Uiso 1 1 calc R U . . .
C20 C 0.37850(18) 0.55957(17) 0.15622(17) 0.0353(6) Uani 1 1 d . . . . .
H20 H 0.3588 0.5784 0.1061 0.042 Uiso 1 1 calc R U . . .
C21 C 0.35385(19) 0.02536(18) 0.19520(17) 0.0378(7) Uani 1 1 d . . . . .
C22 C 0.36044(18) -0.01671(16) 0.26881(16) 0.0318(6) Uani 1 1 d . . . . .
C23 C 0.42170(17) -0.06816(17) 0.30116(16) 0.0326(6) Uani 1 1 d . . . . .
H23 H 0.4620 -0.0747 0.2789 0.039 Uiso 1 1 calc R U . . .
C24 C 0.42356(18) -0.10995(16) 0.36628(16) 0.0324(6) Uani 1 1 d . . . . .
H24 H 0.4648 -0.1448 0.3874 0.039 Uiso 1 1 calc R U . . .
C25 C 0.36388(17) -0.10006(15) 0.40058(15) 0.0284(6) Uani 1 1 d . . . . .
C26 C 0.30229(18) -0.04782(17) 0.36757(16) 0.0345(6) Uani 1 1 d . . . . .
H26 H 0.2623 -0.0405 0.3900 0.041 Uiso 1 1 calc R U . . .
C27 C 0.30027(19) -0.00735(18) 0.30241(17) 0.0367(6) Uani 1 1 d . . . . .
H27 H 0.2585 0.0266 0.2804 0.044 Uiso 1 1 calc R U . . .
C28 C 0.36487(17) -0.14566(16) 0.46986(16) 0.0304(6) Uani 1 1 d . . . . .
C29 C 0.34969(17) -0.11313(16) 0.53393(16) 0.0302(6) Uani 1 1 d . . . . .
C30 C 0.34216(19) -0.02652(17) 0.54400(16) 0.0342(6) Uani 1 1 d . . . . .
C31 C 0.35185(18) -0.16054(16) 0.59570(16) 0.0340(6) Uani 1 1 d . . . . .
H31 H 0.3405 -0.1399 0.6382 0.041 Uiso 1 1 calc R U . . .
C32 C 0.37078(19) -0.23864(16) 0.59488(17) 0.0348(6) Uani 1 1 d . . . . .
C33 C 0.38556(19) -0.26596(16) 0.52894(17) 0.0367(6) Uani 1 1 d . . . . .
H33 H 0.3984 -0.3181 0.5271 0.044 Uiso 1 1 calc R U . . .
C34 C 0.37894(18) -0.28938(17) 0.66233(17) 0.0346(6) Uani 1 1 d . . . . .
C35 C 0.3569(2) -0.36704(18) 0.65289(17) 0.0382(7) Uani 1 1 d . . . . .
H35 H 0.3378 -0.3878 0.6035 0.046 Uiso 1 1 calc R U . . .
C36 C 0.3631(2) -0.41398(17) 0.71627(18) 0.0400(7) Uani 1 1 d . . . . .
H36 H 0.3486 -0.4660 0.7090 0.048 Uiso 1 1 calc R U . . .
C37 C 0.39058(19) -0.38401(18) 0.79002(18) 0.0366(6) Uani 1 1 d . . . . .
C38 C 0.3981(2) -0.43216(18) 0.85977(18) 0.0392(7) Uani 1 1 d . . . . .
C39 C 0.4131(2) -0.30645(18) 0.80030(17) 0.0396(7) Uani 1 1 d . . . . .
H39 H 0.4319 -0.2857 0.8497 0.048 Uiso 1 1 calc R U . . .
C40 C 0.4076(2) -0.26021(17) 0.73701(17) 0.0397(7) Uani 1 1 d . . . . .
H40 H 0.4234 -0.2086 0.7445 0.048 Uiso 1 1 calc R U . . .
C41 C 0.1817(2) -0.0200(2) 0.0351(3) 0.0608(10) Uani 1 1 d . . . . .
H41 H 0.1754 0.0041 0.0785 0.073 Uiso 1 1 calc R U . . .
C42 C 0.1254(3) -0.0760(3) -0.0043(4) 0.0818(15) Uani 1 1 d . . . . .
H42 H 0.0825 -0.0881 0.0129 0.098 Uiso 1 1 calc R U . . .
C43 C 0.1338(3) -0.1118(3) -0.0668(3) 0.0850(17) Uani 1 1 d . . . . .
H43 H 0.0971 -0.1492 -0.0924 0.102 Uiso 1 1 calc R U . . .
C44 C 0.1977(3) -0.0928(2) -0.0932(3) 0.0670(12) Uani 1 1 d . . . . .
C45 C 0.2514(2) -0.03662(18) -0.0509(2) 0.0461(8) Uani 1 1 d . . . . .
C46 C 0.2110(4) -0.1255(3) -0.1602(3) 0.096(2) Uani 1 1 d . . . . .
H46 H 0.1758 -0.1627 -0.1886 0.115 Uiso 1 1 calc R U . . .
C47 C 0.2717(4) -0.1044(3) -0.1827(3) 0.0971(19) Uani 1 1 d . . . . .
H47 H 0.2777 -0.1267 -0.2269 0.117 Uiso 1 1 calc R U . . .
C48 C 0.3290(3) -0.0480(3) -0.1415(2) 0.0710(13) Uani 1 1 d . . . . .
C49 C 0.3189(2) -0.01513(19) -0.07428(19) 0.0448(8) Uani 1 1 d . . . . .
C50 C 0.3953(4) -0.0220(4) -0.1626(3) 0.0875(17) Uani 1 1 d . . . . .
H50 H 0.4044 -0.0416 -0.2066 0.105 Uiso 1 1 calc R U . . .
C51 C 0.4451(3) 0.0310(3) -0.1190(3) 0.0783(14) Uani 1 1 d . . . . .
H51 H 0.4886 0.0482 -0.1328 0.094 Uiso 1 1 calc R U . . .
C52 C 0.4315(2) 0.0602(2) -0.0530(2) 0.0546(9) Uani 1 1 d . . . . .
H52 H 0.4666 0.0968 -0.0234 0.066 Uiso 1 1 calc R U . . .
C53 C 0.4303(2) 0.1158(2) 0.4426(2) 0.0528(9) Uani 1 1 d . . . . .
H53 H 0.4638 0.0790 0.4735 0.063 Uiso 1 1 calc R U . . .
C54 C 0.4429(3) 0.1370(3) 0.3737(3) 0.0737(13) Uani 1 1 d . . . . .
H54 H 0.4827 0.1136 0.3582 0.088 Uiso 1 1 calc R U . . .
C55 C 0.3957(4) 0.1926(4) 0.3296(3) 0.0849(17) Uani 1 1 d . . . . .
H55 H 0.4040 0.2084 0.2840 0.102 Uiso 1 1 calc R U . . .
C56 C 0.3346(3) 0.2261(3) 0.3525(2) 0.0743(14) Uani 1 1 d . . . . .
C57 C 0.3244(2) 0.1998(2) 0.4222(2) 0.0493(8) Uani 1 1 d . . . . .
C58 C 0.2807(5) 0.2840(4) 0.3110(4) 0.118(3) Uani 1 1 d . . . . .
H58 H 0.2873 0.3036 0.2658 0.142 Uiso 1 1 calc R U . . .
C59 C 0.2208(5) 0.3117(4) 0.3341(4) 0.120(3) Uani 1 1 d . . . . .
H59 H 0.1866 0.3487 0.3042 0.144 Uiso 1 1 calc R U . . .
C60 C 0.2090(3) 0.2852(2) 0.4036(3) 0.0782(16) Uani 1 1 d . . . . .
C61 C 0.2605(2) 0.22818(19) 0.4474(2) 0.0547(10) Uani 1 1 d . . . . .
C62 C 0.1475(3) 0.3102(3) 0.4307(4) 0.112(3) Uani 1 1 d . . . . .
H62 H 0.1127 0.3485 0.4041 0.134 Uiso 1 1 calc R U . . .
C63 C 0.1382(3) 0.2794(3) 0.4948(4) 0.097(2) Uani 1 1 d . . . . .
H63 H 0.0963 0.2954 0.5118 0.116 Uiso 1 1 calc R U . . .
C64 C 0.1923(2) 0.2226(2) 0.5364(3) 0.0688(12) Uani 1 1 d . . . . .
H64 H 0.1861 0.2023 0.5814 0.083 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O1 2.004(3) . ?
Zn1 O7 2.082(2) . ?
Zn1 N3 2.115(3) . ?
Zn1 N4 2.122(3) . ?
Zn1 O8 2.208(2) . ?
Zn1 O2 2.480(4) . ?
Zn2 O5 2.103(3) 1_556 ?
Zn2 N6 2.105(3) . ?
Zn2 N5 2.131(3) . ?
Zn2 O10 2.159(2) . ?
Zn2 O9 2.177(2) . ?
Zn2 O6 2.211(3) 1_556 ?
Zn2 C11 2.474(3) 1_556 ?
N1 C5 1.323(4) . ?
N1 C6 1.349(4) . ?
N2 C33 1.329(4) . ?
N2 C28 1.347(4) . ?
N3 C41 1.321(5) . ?
N3 C45 1.355(5) . ?
N4 C52 1.325(5) . ?
N4 C49 1.355(5) . ?
N5 C53 1.337(5) . ?
N5 C57 1.343(5) . ?
N6 C64 1.322(5) . ?
N6 C61 1.358(5) . ?
O1 C1 1.254(5) . ?
O2 C1 1.233(5) . ?
O3 C18 1.213(4) . ?
O4 C18 1.311(4) . ?
O4 H4 0.8200 . ?
O5 C11 1.254(5) . ?
O5 Zn2 2.103(3) 1_554 ?
O6 C11 1.246(4) . ?
O6 Zn2 2.211(3) 1_554 ?
O7 C21 1.263(4) . ?
O8 C21 1.243(4) . ?
O9 C30 1.234(4) . ?
O10 C30 1.250(4) . ?
O11 C38 1.309(4) . ?
O11 H11 0.8200 . ?
O12 C38 1.214(4) . ?
C1 C2 1.522(4) . ?
C2 C3 1.378(4) . ?
C2 C6 1.391(4) . ?
C3 C4 1.391(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.394(4) . ?
C4 C14 1.485(4) . ?
C5 H5 0.9300 . ?
C6 C7 1.481(4) . ?
C7 C13 1.392(4) . ?
C7 C8 1.396(4) . ?
C8 C9 1.378(4) . ?
C8 H8 0.9300 . ?
C9 C10 1.384(5) . ?
C9 H9 0.9300 . ?
C10 C12 1.392(5) . ?
C10 C11 1.504(4) . ?
C11 Zn2 2.473(3) 1_554 ?
C12 C13 1.377(4) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 C20 1.392(4) . ?
C14 C15 1.395(4) . ?
C15 C16 1.381(4) . ?
C15 H15 0.9300 . ?
C16 C17 1.395(4) . ?
C16 H16 0.9300 . ?
C17 C19 1.384(4) . ?
C17 C18 1.490(4) . ?
C19 C20 1.377(4) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
C21 C22 1.498(4) . ?
C22 C23 1.382(4) . ?
C22 C27 1.393(4) . ?
C23 C24 1.381(4) . ?
C23 H23 0.9300 . ?
C24 C25 1.396(4) . ?
C24 H24 0.9300 . ?
C25 C26 1.396(4) . ?
C25 C28 1.484(4) . ?
C26 C27 1.369(4) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
C28 C29 1.396(4) . ?
C29 C31 1.383(4) . ?
C29 C30 1.515(4) . ?
C31 C32 1.388(4) . ?
C31 H31 0.9300 . ?
C32 C33 1.391(4) . ?
C32 C34 1.480(4) . ?
C33 H33 0.9300 . ?
C34 C40 1.391(4) . ?
C34 C35 1.389(4) . ?
C35 C36 1.387(4) . ?
C35 H35 0.9300 . ?
C36 C37 1.381(4) . ?
C36 H36 0.9300 . ?
C37 C39 1.391(4) . ?
C37 C38 1.490(4) . ?
C39 C40 1.381(4) . ?
C39 H39 0.9300 . ?
C40 H40 0.9300 . ?
C41 C42 1.412(6) . ?
C41 H41 0.9300 . ?
C42 C43 1.345(8) . ?
C42 H42 0.9300 . ?
C43 C44 1.399(7) . ?
C43 H43 0.9300 . ?
C44 C45 1.407(5) . ?
C44 C46 1.432(8) . ?
C45 C49 1.436(5) . ?
C46 C47 1.314(9) . ?
C46 H46 0.9300 . ?
C47 C48 1.435(8) . ?
C47 H47 0.9300 . ?
C48 C49 1.412(5) . ?
C48 C50 1.417(8) . ?
C50 C51 1.345(8) . ?
C50 H50 0.9300 . ?
C51 C52 1.394(6) . ?
C51 H51 0.9300 . ?
C52 H52 0.9300 . ?
C53 C54 1.391(5) . ?
C53 H53 0.9300 . ?
C54 C55 1.357(8) . ?
C54 H54 0.9300 . ?
C55 C56 1.399(8) . ?
C55 H55 0.9300 . ?
C56 C57 1.414(6) . ?
C56 C58 1.423(8) . ?
C57 C61 1.432(6) . ?
C58 C59 1.345(10) . ?
C58 H58 0.9300 . ?
C59 C60 1.424(9) . ?
C59 H59 0.9300 . ?
C60 C62 1.396(9) . ?
C60 C61 1.407(5) . ?
C62 C63 1.340(9) . ?
C62 H62 0.9300 . ?
C63 C64 1.413(7) . ?
C63 H63 0.9300 . ?
C64 H64 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 O7 141.65(11) . . ?
O1 Zn1 N3 113.43(11) . . ?
O7 Zn1 N3 97.92(10) . . ?
O1 Zn1 N4 102.09(10) . . ?
O7 Zn1 N4 105.35(10) . . ?
N3 Zn1 N4 78.74(11) . . ?
O1 Zn1 O8 95.98(9) . . ?
O7 Zn1 O8 61.00(9) . . ?
N3 Zn1 O8 90.34(11) . . ?
N4 Zn1 O8 161.46(10) . . ?
O1 Zn1 O2 57.48(11) . . ?
O7 Zn1 O2 98.31(10) . . ?
N3 Zn1 O2 160.03(11) . . ?
N4 Zn1 O2 85.79(12) . . ?
O8 Zn1 O2 107.72(12) . . ?
O5 Zn2 N6 95.14(12) 1_556 . ?
O5 Zn2 N5 161.36(10) 1_556 . ?
N6 Zn2 N5 78.71(12) . . ?
O5 Zn2 O10 101.90(11) 1_556 . ?
N6 Zn2 O10 156.72(11) . . ?
N5 Zn2 O10 89.43(11) . . ?
O5 Zn2 O9 98.56(10) 1_556 . ?
N6 Zn2 O9 101.75(10) . . ?
N5 Zn2 O9 99.92(10) . . ?
O10 Zn2 O9 60.32(9) . . ?
O5 Zn2 O6 60.60(10) 1_556 1_556 ?
N6 Zn2 O6 96.17(10) . 1_556 ?
N5 Zn2 O6 102.24(10) . 1_556 ?
O10 Zn2 O6 105.96(9) . 1_556 ?
O9 Zn2 O6 153.79(10) . 1_556 ?
O5 Zn2 C11 30.45(12) 1_556 1_556 ?
N6 Zn2 C11 95.18(11) . 1_556 ?
N5 Zn2 C11 131.80(12) . 1_556 ?
O10 Zn2 C11 107.56(10) . 1_556 ?
O9 Zn2 C11 127.88(11) . 1_556 ?
O6 Zn2 C11 30.20(11) 1_556 1_556 ?
C5 N1 C6 120.1(2) . . ?
C33 N2 C28 119.6(2) . . ?
C41 N3 C45 118.2(3) . . ?
C41 N3 Zn1 128.3(3) . . ?
C45 N3 Zn1 113.4(2) . . ?
C52 N4 C49 118.7(3) . . ?
C52 N4 Zn1 128.4(3) . . ?
C49 N4 Zn1 112.8(2) . . ?
C53 N5 C57 118.6(3) . . ?
C53 N5 Zn2 128.2(2) . . ?
C57 N5 Zn2 113.1(2) . . ?
C64 N6 C61 118.9(4) . . ?
C64 N6 Zn2 128.2(3) . . ?
C61 N6 Zn2 112.9(2) . . ?
C1 O1 Zn1 99.9(2) . . ?
C1 O2 Zn1 78.6(2) . . ?
C18 O4 H4 109.5 . . ?
C11 O5 Zn2 91.3(2) . 1_554 ?
C11 O6 Zn2 86.6(2) . 1_554 ?
C21 O7 Zn1 91.49(19) . . ?
C21 O8 Zn1 86.32(19) . . ?
C30 O9 Zn2 88.34(19) . . ?
C30 O10 Zn2 88.74(19) . . ?
C38 O11 H11 109.5 . . ?
O2 C1 O1 124.0(3) . . ?
O2 C1 C2 118.4(4) . . ?
O1 C1 C2 117.6(3) . . ?
C3 C2 C6 119.2(3) . . ?
C3 C2 C1 118.1(3) . . ?
C6 C2 C1 122.6(3) . . ?
C2 C3 C4 121.0(3) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 H3 119.5 . . ?
C3 C4 C5 116.0(3) . . ?
C3 C4 C14 122.6(3) . . ?
C5 C4 C14 121.5(3) . . ?
N1 C5 C4 123.6(3) . . ?
N1 C5 H5 118.2 . . ?
C4 C5 H5 118.2 . . ?
N1 C6 C2 120.1(3) . . ?
N1 C6 C7 115.9(2) . . ?
C2 C6 C7 124.0(3) . . ?
C13 C7 C8 117.9(3) . . ?
C13 C7 C6 121.3(3) . . ?
C8 C7 C6 120.7(3) . . ?
C9 C8 C7 121.0(3) . . ?
C9 C8 H8 119.5 . . ?
C7 C8 H8 119.5 . . ?
C8 C9 C10 120.7(3) . . ?
C8 C9 H9 119.7 . . ?
C10 C9 H9 119.7 . . ?
C9 C10 C12 118.6(3) . . ?
C9 C10 C11 119.2(3) . . ?
C12 C10 C11 121.9(3) . . ?
O6 C11 O5 121.2(3) . . ?
O6 C11 C10 120.2(3) . . ?
O5 C11 C10 118.5(3) . . ?
O6 C11 Zn2 63.17(18) . 1_554 ?
O5 C11 Zn2 58.22(17) . 1_554 ?
C10 C11 Zn2 173.1(2) . 1_554 ?
C13 C12 C10 120.7(3) . . ?
C13 C12 H12 119.6 . . ?
C10 C12 H12 119.6 . . ?
C12 C13 C7 121.0(3) . . ?
C12 C13 H13 119.5 . . ?
C7 C13 H13 119.5 . . ?
C20 C14 C15 118.5(3) . . ?
C20 C14 C4 121.0(3) . . ?
C15 C14 C4 120.5(3) . . ?
C16 C15 C14 120.6(3) . . ?
C16 C15 H15 119.7 . . ?
C14 C15 H15 119.7 . . ?
C15 C16 C17 120.3(3) . . ?
C15 C16 H16 119.8 . . ?
C17 C16 H16 119.8 . . ?
C19 C17 C16 119.1(3) . . ?
C19 C17 C18 122.5(3) . . ?
C16 C17 C18 118.4(3) . . ?
O3 C18 O4 123.7(3) . . ?
O3 C18 C17 122.8(3) . . ?
O4 C18 C17 113.4(3) . . ?
C20 C19 C17 120.5(3) . . ?
C20 C19 H19 119.7 . . ?
C17 C19 H19 119.7 . . ?
C19 C20 C14 121.0(3) . . ?
C19 C20 H20 119.5 . . ?
C14 C20 H20 119.5 . . ?
O8 C21 O7 120.9(3) . . ?
O8 C21 C22 120.0(3) . . ?
O7 C21 C22 119.0(3) . . ?
C23 C22 C27 119.4(3) . . ?
C23 C22 C21 121.6(3) . . ?
C27 C22 C21 118.8(3) . . ?
C24 C23 C22 120.5(3) . . ?
C24 C23 H23 119.8 . . ?
C22 C23 H23 119.8 . . ?
C23 C24 C25 120.3(3) . . ?
C23 C24 H24 119.9 . . ?
C25 C24 H24 119.9 . . ?
C24 C25 C26 118.9(3) . . ?
C24 C25 C28 120.5(3) . . ?
C26 C25 C28 120.6(2) . . ?
C27 C26 C25 120.6(3) . . ?
C27 C26 H26 119.7 . . ?
C25 C26 H26 119.7 . . ?
C26 C27 C22 120.4(3) . . ?
C26 C27 H27 119.8 . . ?
C22 C27 H27 119.8 . . ?
N2 C28 C29 120.8(3) . . ?
N2 C28 C25 116.1(2) . . ?
C29 C28 C25 123.1(2) . . ?
C31 C29 C28 118.8(3) . . ?
C31 C29 C30 117.7(2) . . ?
C28 C29 C30 123.0(2) . . ?
O9 C30 O10 122.6(3) . . ?
O9 C30 C29 122.0(3) . . ?
O10 C30 C29 115.4(3) . . ?
C29 C31 C32 120.6(3) . . ?
C29 C31 H31 119.7 . . ?
C32 C31 H31 119.7 . . ?
C31 C32 C33 116.7(3) . . ?
C31 C32 C34 121.7(3) . . ?
C33 C32 C34 121.6(3) . . ?
N2 C33 C32 123.6(3) . . ?
N2 C33 H33 118.2 . . ?
C32 C33 H33 118.2 . . ?
C40 C34 C35 118.2(3) . . ?
C40 C34 C32 120.8(3) . . ?
C35 C34 C32 121.0(3) . . ?
C36 C35 C34 120.8(3) . . ?
C36 C35 H35 119.6 . . ?
C34 C35 H35 119.6 . . ?
C37 C36 C35 120.5(3) . . ?
C37 C36 H36 119.8 . . ?
C35 C36 H36 119.8 . . ?
C36 C37 C39 119.3(3) . . ?
C36 C37 C38 122.3(3) . . ?
C39 C37 C38 118.3(3) . . ?
O12 C38 O11 124.7(3) . . ?
O12 C38 C37 122.1(3) . . ?
O11 C38 C37 113.2(3) . . ?
C40 C39 C37 120.0(3) . . ?
C40 C39 H39 120.0 . . ?
C37 C39 H39 120.0 . . ?
C39 C40 C34 121.3(3) . . ?
C39 C40 H40 119.4 . . ?
C34 C40 H40 119.4 . . ?
N3 C41 C42 121.9(4) . . ?
N3 C41 H41 119.0 . . ?
C42 C41 H41 119.0 . . ?
C43 C42 C41 120.0(5) . . ?
C43 C42 H42 120.0 . . ?
C41 C42 H42 120.0 . . ?
C42 C43 C44 119.9(4) . . ?
C42 C43 H43 120.0 . . ?
C44 C43 H43 120.0 . . ?
C43 C44 C45 116.9(4) . . ?
C43 C44 C46 124.7(5) . . ?
C45 C44 C46 118.5(5) . . ?
N3 C45 C44 123.1(4) . . ?
N3 C45 C49 117.2(3) . . ?
C44 C45 C49 119.7(4) . . ?
C47 C46 C44 121.7(5) . . ?
C47 C46 H46 119.1 . . ?
C44 C46 H46 119.1 . . ?
C46 C47 C48 122.4(5) . . ?
C46 C47 H47 118.8 . . ?
C48 C47 H47 118.8 . . ?
C49 C48 C50 116.7(4) . . ?
C49 C48 C47 117.9(5) . . ?
C50 C48 C47 125.5(5) . . ?
N4 C49 C48 122.4(4) . . ?
N4 C49 C45 117.9(3) . . ?
C48 C49 C45 119.8(4) . . ?
C51 C50 C48 119.9(4) . . ?
C51 C50 H50 120.0 . . ?
C48 C50 H50 120.0 . . ?
C50 C51 C52 120.0(5) . . ?
C50 C51 H51 120.0 . . ?
C52 C51 H51 120.0 . . ?
N4 C52 C51 122.4(4) . . ?
N4 C52 H52 118.8 . . ?
C51 C52 H52 118.8 . . ?
N5 C53 C54 123.1(4) . . ?
N5 C53 H53 118.4 . . ?
C54 C53 H53 118.4 . . ?
C55 C54 C53 118.6(5) . . ?
C55 C54 H54 120.7 . . ?
C53 C54 H54 120.7 . . ?
C54 C55 C56 120.3(4) . . ?
C54 C55 H55 119.9 . . ?
C56 C55 H55 119.9 . . ?
C55 C56 C57 117.6(4) . . ?
C55 C56 C58 125.5(5) . . ?
C57 C56 C58 116.8(6) . . ?
N5 C57 C56 121.8(4) . . ?
N5 C57 C61 117.2(3) . . ?
C56 C57 C61 121.0(4) . . ?
C59 C58 C56 122.9(6) . . ?
C59 C58 H58 118.5 . . ?
C56 C58 H58 118.5 . . ?
C58 C59 C60 121.0(5) . . ?
C58 C59 H59 119.5 . . ?
C60 C59 H59 119.5 . . ?
C62 C60 C61 116.9(5) . . ?
C62 C60 C59 124.4(5) . . ?
C61 C60 C59 118.7(6) . . ?
N6 C61 C60 122.4(4) . . ?
N6 C61 C57 118.1(3) . . ?
C60 C61 C57 119.5(4) . . ?
C63 C62 C60 120.6(5) . . ?
C63 C62 H62 119.7 . . ?
C60 C62 H62 119.7 . . ?
C62 C63 C64 119.7(5) . . ?
C62 C63 H63 120.1 . . ?
C64 C63 H63 120.1 . . ?
N6 C64 C63 121.5(5) . . ?
N6 C64 H64 119.3 . . ?
C63 C64 H64 119.3 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Zn1 O2 C1 O1 0.2(3) . . . . ?
Zn1 O2 C1 C2 178.0(3) . . . . ?
Zn1 O1 C1 O2 -0.2(4) . . . . ?
Zn1 O1 C1 C2 -178.0(2) . . . . ?
O2 C1 C2 C3 -89.2(4) . . . . ?
O1 C1 C2 C3 88.8(4) . . . . ?
O2 C1 C2 C6 87.0(4) . . . . ?
O1 C1 C2 C6 -95.1(4) . . . . ?
C6 C2 C3 C4 -0.5(5) . . . . ?
C1 C2 C3 C4 175.8(3) . . . . ?
C2 C3 C4 C5 1.1(5) . . . . ?
C2 C3 C4 C14 -178.5(3) . . . . ?
C6 N1 C5 C4 -0.9(5) . . . . ?
C3 C4 C5 N1 -0.4(5) . . . . ?
C14 C4 C5 N1 179.1(3) . . . . ?
C5 N1 C6 C2 1.6(5) . . . . ?
C5 N1 C6 C7 -179.3(3) . . . . ?
C3 C2 C6 N1 -1.0(5) . . . . ?
C1 C2 C6 N1 -177.0(3) . . . . ?
C3 C2 C6 C7 -179.9(3) . . . . ?
C1 C2 C6 C7 4.0(5) . . . . ?
N1 C6 C7 C13 46.9(4) . . . . ?
C2 C6 C7 C13 -134.1(3) . . . . ?
N1 C6 C7 C8 -130.8(3) . . . . ?
C2 C6 C7 C8 48.1(4) . . . . ?
C13 C7 C8 C9 -1.2(5) . . . . ?
C6 C7 C8 C9 176.7(3) . . . . ?
C7 C8 C9 C10 1.1(5) . . . . ?
C8 C9 C10 C12 -0.4(5) . . . . ?
C8 C9 C10 C11 -174.9(3) . . . . ?
Zn2 O6 C11 O5 4.7(3) 1_554 . . . ?
Zn2 O6 C11 C10 -173.1(3) 1_554 . . . ?
Zn2 O5 C11 O6 -4.9(3) 1_554 . . . ?
Zn2 O5 C11 C10 172.9(2) 1_554 . . . ?
C9 C10 C11 O6 166.6(3) . . . . ?
C12 C10 C11 O6 -7.7(5) . . . . ?
C9 C10 C11 O5 -11.2(5) . . . . ?
C12 C10 C11 O5 174.5(3) . . . . ?
C9 C10 C12 C13 -0.3(5) . . . . ?
C11 C10 C12 C13 174.0(3) . . . . ?
C10 C12 C13 C7 0.3(5) . . . . ?
C8 C7 C13 C12 0.4(5) . . . . ?
C6 C7 C13 C12 -177.4(3) . . . . ?
C3 C4 C14 C20 -149.0(3) . . . . ?
C5 C4 C14 C20 31.4(4) . . . . ?
C3 C4 C14 C15 30.2(4) . . . . ?
C5 C4 C14 C15 -149.4(3) . . . . ?
C20 C14 C15 C16 0.3(5) . . . . ?
C4 C14 C15 C16 -178.9(3) . . . . ?
C14 C15 C16 C17 0.4(5) . . . . ?
C15 C16 C17 C19 -0.9(5) . . . . ?
C15 C16 C17 C18 177.8(3) . . . . ?
C19 C17 C18 O3 176.3(3) . . . . ?
C16 C17 C18 O3 -2.3(5) . . . . ?
C19 C17 C18 O4 -2.5(4) . . . . ?
C16 C17 C18 O4 178.8(3) . . . . ?
C16 C17 C19 C20 0.7(5) . . . . ?
C18 C17 C19 C20 -178.0(3) . . . . ?
C17 C19 C20 C14 0.1(5) . . . . ?
C15 C14 C20 C19 -0.6(5) . . . . ?
C4 C14 C20 C19 178.6(3) . . . . ?
Zn1 O8 C21 O7 5.4(3) . . . . ?
Zn1 O8 C21 C22 -171.7(3) . . . . ?
Zn1 O7 C21 O8 -5.8(3) . . . . ?
Zn1 O7 C21 C22 171.4(2) . . . . ?
O8 C21 C22 C23 -173.3(3) . . . . ?
O7 C21 C22 C23 9.5(4) . . . . ?
O8 C21 C22 C27 11.0(5) . . . . ?
O7 C21 C22 C27 -166.2(3) . . . . ?
C27 C22 C23 C24 -0.1(4) . . . . ?
C21 C22 C23 C24 -175.8(3) . . . . ?
C22 C23 C24 C25 -0.6(4) . . . . ?
C23 C24 C25 C26 0.5(4) . . . . ?
C23 C24 C25 C28 179.1(3) . . . . ?
C24 C25 C26 C27 0.4(4) . . . . ?
C28 C25 C26 C27 -178.2(3) . . . . ?
C25 C26 C27 C22 -1.1(5) . . . . ?
C23 C22 C27 C26 1.0(5) . . . . ?
C21 C22 C27 C26 176.8(3) . . . . ?
C33 N2 C28 C29 -0.3(4) . . . . ?
C33 N2 C28 C25 179.0(3) . . . . ?
C24 C25 C28 N2 -43.5(4) . . . . ?
C26 C25 C28 N2 135.0(3) . . . . ?
C24 C25 C28 C29 135.8(3) . . . . ?
C26 C25 C28 C29 -45.7(4) . . . . ?
N2 C28 C29 C31 -0.9(4) . . . . ?
C25 C28 C29 C31 179.9(3) . . . . ?
N2 C28 C29 C30 170.4(3) . . . . ?
C25 C28 C29 C30 -8.9(4) . . . . ?
Zn2 O9 C30 O10 0.8(3) . . . . ?
Zn2 O9 C30 C29 179.4(2) . . . . ?
Zn2 O10 C30 O9 -0.8(3) . . . . ?
Zn2 O10 C30 C29 -179.5(2) . . . . ?
C31 C29 C30 O9 -93.4(4) . . . . ?
C28 C29 C30 O9 95.2(4) . . . . ?
C31 C29 C30 O10 85.3(4) . . . . ?
C28 C29 C30 O10 -86.1(4) . . . . ?
C28 C29 C31 C32 1.6(5) . . . . ?
C30 C29 C31 C32 -170.1(3) . . . . ?
C29 C31 C32 C33 -1.2(5) . . . . ?
C29 C31 C32 C34 175.7(3) . . . . ?
C28 N2 C33 C32 0.8(5) . . . . ?
C31 C32 C33 N2 0.0(5) . . . . ?
C34 C32 C33 N2 -177.0(3) . . . . ?
C31 C32 C34 C40 -32.8(5) . . . . ?
C33 C32 C34 C40 144.0(3) . . . . ?
C31 C32 C34 C35 146.1(3) . . . . ?
C33 C32 C34 C35 -37.1(5) . . . . ?
C40 C34 C35 C36 0.3(5) . . . . ?
C32 C34 C35 C36 -178.6(3) . . . . ?
C34 C35 C36 C37 0.7(5) . . . . ?
C35 C36 C37 C39 -0.9(5) . . . . ?
C35 C36 C37 C38 179.9(3) . . . . ?
C36 C37 C38 O12 -170.2(3) . . . . ?
C39 C37 C38 O12 10.5(5) . . . . ?
C36 C37 C38 O11 11.8(5) . . . . ?
C39 C37 C38 O11 -167.4(3) . . . . ?
C36 C37 C39 C40 0.2(5) . . . . ?
C38 C37 C39 C40 179.5(3) . . . . ?
C37 C39 C40 C34 0.7(5) . . . . ?
C35 C34 C40 C39 -1.0(5) . . . . ?
C32 C34 C40 C39 177.9(3) . . . . ?
C45 N3 C41 C42 -0.4(6) . . . . ?
Zn1 N3 C41 C42 -176.6(3) . . . . ?
N3 C41 C42 C43 0.6(7) . . . . ?
C41 C42 C43 C44 -0.8(8) . . . . ?
C42 C43 C44 C45 0.9(7) . . . . ?
C42 C43 C44 C46 -178.0(5) . . . . ?
C41 N3 C45 C44 0.5(5) . . . . ?
Zn1 N3 C45 C44 177.3(3) . . . . ?
C41 N3 C45 C49 -179.5(3) . . . . ?
Zn1 N3 C45 C49 -2.7(4) . . . . ?
C43 C44 C45 N3 -0.8(6) . . . . ?
C46 C44 C45 N3 178.2(4) . . . . ?
C43 C44 C45 C49 179.2(4) . . . . ?
C46 C44 C45 C49 -1.8(6) . . . . ?
C43 C44 C46 C47 179.0(6) . . . . ?
C45 C44 C46 C47 0.1(8) . . . . ?
C44 C46 C47 C48 0.7(10) . . . . ?
C46 C47 C48 C49 0.3(9) . . . . ?
C46 C47 C48 C50 -179.4(6) . . . . ?
C52 N4 C49 C48 1.1(5) . . . . ?
Zn1 N4 C49 C48 179.2(3) . . . . ?
C52 N4 C49 C45 -177.8(3) . . . . ?
Zn1 N4 C49 C45 0.3(4) . . . . ?
C50 C48 C49 N4 -1.1(6) . . . . ?
C47 C48 C49 N4 179.1(4) . . . . ?
C50 C48 C49 C45 177.8(4) . . . . ?
C47 C48 C49 C45 -2.0(6) . . . . ?
N3 C45 C49 N4 1.7(4) . . . . ?
C44 C45 C49 N4 -178.3(3) . . . . ?
N3 C45 C49 C48 -177.2(3) . . . . ?
C44 C45 C49 C48 2.8(5) . . . . ?
C49 C48 C50 C51 0.5(7) . . . . ?
C47 C48 C50 C51 -179.8(5) . . . . ?
C48 C50 C51 C52 0.1(8) . . . . ?
C49 N4 C52 C51 -0.5(5) . . . . ?
Zn1 N4 C52 C51 -178.2(3) . . . . ?
C50 C51 C52 N4 -0.1(7) . . . . ?
C57 N5 C53 C54 -0.6(5) . . . . ?
Zn2 N5 C53 C54 175.1(3) . . . . ?
N5 C53 C54 C55 2.0(6) . . . . ?
C53 C54 C55 C56 -1.6(7) . . . . ?
C54 C55 C56 C57 -0.1(7) . . . . ?
C54 C55 C56 C58 -179.3(5) . . . . ?
C53 N5 C57 C56 -1.3(5) . . . . ?
Zn2 N5 C57 C56 -177.6(3) . . . . ?
C53 N5 C57 C61 177.0(3) . . . . ?
Zn2 N5 C57 C61 0.7(4) . . . . ?
C55 C56 C57 N5 1.6(6) . . . . ?
C58 C56 C57 N5 -179.1(4) . . . . ?
C55 C56 C57 C61 -176.6(4) . . . . ?
C58 C56 C57 C61 2.6(6) . . . . ?
C55 C56 C58 C59 177.0(6) . . . . ?
C57 C56 C58 C59 -2.2(9) . . . . ?
C56 C58 C59 C60 1.5(11) . . . . ?
C58 C59 C60 C62 -178.9(6) . . . . ?
C58 C59 C60 C61 -1.1(9) . . . . ?
C64 N6 C61 C60 -0.3(5) . . . . ?
Zn2 N6 C61 C60 -179.2(3) . . . . ?
C64 N6 C61 C57 -179.3(3) . . . . ?
Zn2 N6 C61 C57 1.8(4) . . . . ?
C62 C60 C61 N6 0.5(6) . . . . ?
C59 C60 C61 N6 -177.4(4) . . . . ?
C62 C60 C61 C57 179.5(4) . . . . ?
C59 C60 C61 C57 1.6(6) . . . . ?
N5 C57 C61 N6 -1.7(5) . . . . ?
C56 C57 C61 N6 176.6(3) . . . . ?
N5 C57 C61 C60 179.3(3) . . . . ?
C56 C57 C61 C60 -2.4(5) . . . . ?
C61 C60 C62 C63 -1.2(8) . . . . ?
C59 C60 C62 C63 176.6(5) . . . . ?
C60 C62 C63 C64 1.6(8) . . . . ?
C61 N6 C64 C63 0.7(6) . . . . ?
Zn2 N6 C64 C63 179.4(3) . . . . ?
C62 C63 C64 N6 -1.4(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
C64 H64 O12 0.93 2.51 3.089(5) 120.9 2_556
C53 H53 O10 0.93 2.66 3.166(5) 115.0 .
C52 H52 O2 0.93 2.50 3.124(5) 124.6 .
C51 H51 O7 0.93 2.36 3.109(5) 137.9 3_655
C42 H42 O3 0.93 2.62 3.248(5) 125.8 4_565
C41 H41 O3 0.93 2.61 3.225(5) 124.1 2_545
C33 H33 O3 0.93 2.51 3.194(4) 130.8 1_545
C5 H5 O12 0.93 2.41 3.130(4) 134.2 1_564
O11 H11 N1 0.82 1.85 2.665(3) 177.9 1_546
O4 H4 N2 0.82 1.89 2.698(3) 169.3 1_565

_refine_diff_density_max         1.018
_refine_diff_density_min         -0.496
_refine_diff_density_rms         0.069

####################################################################### 
# 
# 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_403-7Ni
_database_code_depnum_ccdc_archive 'CCDC 1984463'
_audit_update_record             
;
2020-04-30 deposited with the CCDC.	2020-05-11 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            'C44 H31 N5 Ni O8'
_chemical_formula_weight         816.45

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 '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                   11.3784(7)
_cell_length_b                   13.1996(8)
_cell_length_c                   14.5453(9)
_cell_angle_alpha                67.404(6)
_cell_angle_beta                 76.097(5)
_cell_angle_gamma                65.856(6)
_cell_volume                     1831.5(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    11344
_cell_measurement_theta_min      3.877
_cell_measurement_theta_max      64.995

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_F_000             844
_exptl_transmission_factor_min   0.746
_exptl_transmission_factor_max   0.749
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.220
_exptl_absorpt_coefficient_mu    1.314
_shelx_estimated_absorpt_T_min   0.726
_shelx_estimated_absorpt_T_max   0.761
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.726
_exptl_absorpt_correction_T_max  0.761
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\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            11344
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.877
_diffrn_reflns_theta_max         64.995
_diffrn_reflns_theta_full        64.995
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measured_fraction_theta_full 0.961
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_Laue_measured_fraction_full 0.961
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_point_group_measured_fraction_full 0.961
_reflns_number_total             5990
_reflns_number_gt                4684
_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)+(0.0503P)²+0.2505P] 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         5990
_refine_ls_number_parameters     527
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0388
_refine_ls_wR_factor_ref         0.1054
_refine_ls_wR_factor_gt          0.0940
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.018
_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 0.79599(4) 0.85974(3) 0.70051(3) 0.03329(12) Uani 1 1 d . . . . .
N1 N 1.02846(19) 1.24788(16) 0.69943(15) 0.0356(5) Uani 1 1 d . . . . .
N2 N 0.7567(2) 0.72396(17) 0.69126(15) 0.0377(5) Uani 1 1 d . . . . .
N3 N 0.60810(19) 0.95041(17) 0.65973(15) 0.0367(5) Uani 1 1 d . . . . .
N4 N 0.97464(19) 0.74934(17) 0.75757(15) 0.0375(5) Uani 1 1 d . . . . .
N5 N 0.73867(19) 0.82473(17) 0.85264(15) 0.0374(5) Uani 1 1 d . . . . .
O1 O 0.82106(16) 1.00124(14) 0.70798(12) 0.0374(4) Uani 1 1 d . . . . .
O2 O 0.89229(16) 1.09263(14) 0.55325(11) 0.0374(4) Uani 1 1 d . . . . .
O3 O 1.4728(2) 0.59005(17) 1.11855(16) 0.0633(6) Uani 1 1 d . . . . .
O4 O 1.41738(18) 0.71920(17) 1.19884(13) 0.0525(5) Uani 1 1 d . . . . .
O5 O 0.56002(17) 1.57331(17) 0.32824(13) 0.0508(5) Uani 1 1 d . . . . .
O6 O 0.6901(2) 1.67519(17) 0.29147(15) 0.0649(6) Uani 1 1 d . . . . .
O7 O 0.86489(17) 0.90486(15) 0.54721(12) 0.0402(4) Uani 1 1 d . . . . .
H2W H 0.8759 0.9676 0.5294 0.048 Uiso 1 1 d R U . . .
H1W H 0.9284 0.8457 0.5372 0.048 Uiso 1 1 d R U . . .
O8 O 0.3686(3) 0.4377(2) 0.0751(2) 0.0900(8) Uani 1 1 d . . . . .
H3W H 0.4144 0.4685 0.0903 0.108 Uiso 1 1 d R U . . .
H4W H 0.4212 0.4136 0.0261 0.108 Uiso 1 1 d R U . . .
C1 C 0.8813(2) 1.06583(18) 0.64665(16) 0.0290(5) Uani 1 1 d . . . . .
C2 C 0.9514(2) 1.10668(19) 0.69326(16) 0.0285(5) Uani 1 1 d . . . . .
C3 C 0.9562(2) 1.21969(19) 0.65894(16) 0.0290(5) Uani 1 1 d . . . . .
C4 C 1.0968(2) 1.1647(2) 0.77421(18) 0.0363(5) Uani 1 1 d . . . . .
H5 H 1.1486 1.1841 0.8005 0.044 Uiso 1 1 calc R U . . .
C5 C 1.0957(2) 1.05061(19) 0.81550(17) 0.0327(5) Uani 1 1 d . . . . .
C6 C 1.0199(2) 1.02385(19) 0.77284(17) 0.0328(5) Uani 1 1 d . . . . .
H6 H 1.0153 0.9492 0.7982 0.039 Uiso 1 1 calc R U . . .
C7 C 1.1738(2) 0.9597(2) 0.89781(18) 0.0357(5) Uani 1 1 d . . . . .
C8 C 1.2387(3) 0.8465(2) 0.8933(2) 0.0487(7) Uani 1 1 d . . . . .
H8 H 1.2326 0.8293 0.8387 0.058 Uiso 1 1 calc R U . . .
C9 C 1.3122(3) 0.7592(2) 0.9686(2) 0.0514(7) Uani 1 1 d . . . . .
H9 H 1.3552 0.6841 0.9640 0.062 Uiso 1 1 calc R U . . .
C10 C 1.3224(2) 0.7824(2) 1.05064(18) 0.0395(6) Uani 1 1 d . . . . .
C11 C 1.4110(2) 0.6878(2) 1.12819(19) 0.0422(6) Uani 1 1 d . . . . .
C12 C 1.2560(2) 0.8949(2) 1.05703(18) 0.0410(6) Uani 1 1 d . . . . .
H12 H 1.2610 0.9114 1.1124 0.049 Uiso 1 1 calc R U . . .
C13 C 1.1823(2) 0.9827(2) 0.98121(18) 0.0392(6) Uani 1 1 d . . . . .
H13 H 1.1383 1.0575 0.9862 0.047 Uiso 1 1 calc R U . . .
C14 C 0.8791(2) 1.31594(18) 0.57832(16) 0.0283(5) Uani 1 1 d . . . . .
C15 C 0.9303(2) 1.3975(2) 0.50613(17) 0.0346(5) Uani 1 1 d . . . . .
H15 H 1.0141 1.3912 0.5083 0.042 Uiso 1 1 calc R U . . .
C16 C 0.8573(2) 1.4876(2) 0.43120(17) 0.0361(5) Uani 1 1 d . . . . .
H16 H 0.8914 1.5428 0.3847 0.043 Uiso 1 1 calc R U . . .
C17 C 0.7339(2) 1.49581(19) 0.42534(16) 0.0312(5) Uani 1 1 d . . . . .
C18 C 0.6566(2) 1.5915(2) 0.34156(16) 0.0361(5) Uani 1 1 d . . . . .
C19 C 0.6823(2) 1.41516(19) 0.49740(16) 0.0312(5) Uani 1 1 d . . . . .
H19 H 0.5994 1.4204 0.4939 0.037 Uiso 1 1 calc R U . . .
C20 C 0.7524(2) 1.32792(18) 0.57361(16) 0.0299(5) Uani 1 1 d . . . . .
H20 H 0.7154 1.2763 0.6225 0.036 Uiso 1 1 calc R U . . .
C21 C 0.5336(3) 1.0612(2) 0.6488(2) 0.0449(6) Uani 1 1 d . . . . .
H21 H 0.5672 1.1095 0.6584 0.054 Uiso 1 1 calc R U . . .
C22 C 0.4066(3) 1.1087(3) 0.6236(2) 0.0518(7) Uani 1 1 d . . . . .
H22 H 0.3571 1.1869 0.6171 0.062 Uiso 1 1 calc R U . . .
C23 C 0.3559(3) 1.0397(3) 0.6086(2) 0.0534(7) Uani 1 1 d . . . . .
H23 H 0.2719 1.0707 0.5909 0.064 Uiso 1 1 calc R U . . .
C24 C 0.4306(3) 0.9219(3) 0.62007(19) 0.0452(6) Uani 1 1 d . . . . .
C25 C 0.5568(2) 0.8804(2) 0.64682(17) 0.0359(5) Uani 1 1 d . . . . .
C26 C 0.3863(3) 0.8419(3) 0.6062(2) 0.0593(8) Uani 1 1 d . . . . .
H26 H 0.3036 0.8686 0.5872 0.071 Uiso 1 1 calc R U . . .
C27 C 0.4622(3) 0.7289(3) 0.6203(2) 0.0611(8) Uani 1 1 d . . . . .
H27 H 0.4311 0.6794 0.6100 0.073 Uiso 1 1 calc R U . . .
C28 C 0.5892(3) 0.6832(3) 0.6506(2) 0.0484(7) Uani 1 1 d . . . . .
C29 C 0.6369(3) 0.7593(2) 0.66314(17) 0.0392(6) Uani 1 1 d . . . . .
C30 C 0.6707(4) 0.5651(3) 0.6703(2) 0.0615(9) Uani 1 1 d . . . . .
H30 H 0.6432 0.5113 0.6632 0.074 Uiso 1 1 calc R U . . .
C31 C 0.7898(3) 0.5297(3) 0.6998(2) 0.0597(8) Uani 1 1 d . . . . .
H31 H 0.8445 0.4517 0.7131 0.072 Uiso 1 1 calc R U . . .
C32 C 0.8293(3) 0.6118(2) 0.7098(2) 0.0488(7) Uani 1 1 d . . . . .
H32 H 0.9107 0.5862 0.7307 0.059 Uiso 1 1 calc R U . . .
C33 C 0.6227(3) 0.8679(2) 0.8976(2) 0.0467(6) Uani 1 1 d . . . . .
H33 H 0.5541 0.9162 0.8587 0.056 Uiso 1 1 calc R U . . .
C34 C 0.5995(3) 0.8441(3) 1.0006(2) 0.0526(7) Uani 1 1 d . . . . .
H34 H 0.5173 0.8784 1.0292 0.063 Uiso 1 1 calc R U . . .
C35 C 0.6969(3) 0.7706(3) 1.0596(2) 0.0541(7) Uani 1 1 d . . . . .
H35 H 0.6812 0.7519 1.1288 0.065 Uiso 1 1 calc R U . . .
C36 C 0.8224(3) 0.7230(2) 1.01453(19) 0.0443(6) Uani 1 1 d . . . . .
C37 C 0.8382(2) 0.7545(2) 0.91011(18) 0.0372(5) Uani 1 1 d . . . . .
C38 C 0.9321(3) 0.6466(3) 1.0697(2) 0.0571(8) Uani 1 1 d . . . . .
H38 H 0.9215 0.6251 1.1391 0.069 Uiso 1 1 calc R U . . .
C39 C 1.0502(3) 0.6052(3) 1.0230(2) 0.0554(7) Uani 1 1 d . . . . .
H39 H 1.1198 0.5553 1.0606 0.066 Uiso 1 1 calc R U . . .
C40 C 1.0699(3) 0.6374(2) 0.9155(2) 0.0451(6) Uani 1 1 d . . . . .
C41 C 0.9643(2) 0.7128(2) 0.85933(18) 0.0360(5) Uani 1 1 d . . . . .
C42 C 1.1902(3) 0.5970(2) 0.8625(2) 0.0528(7) Uani 1 1 d . . . . .
H42 H 1.2626 0.5460 0.8966 0.063 Uiso 1 1 calc R U . . .
C43 C 1.2003(3) 0.6331(2) 0.7605(2) 0.0504(7) Uani 1 1 d . . . . .
H43 H 1.2796 0.6063 0.7248 0.060 Uiso 1 1 calc R U . . .
C44 C 1.0917(3) 0.7100(2) 0.7101(2) 0.0463(6) Uani 1 1 d . . . . .
H44 H 1.1008 0.7351 0.6405 0.056 Uiso 1 1 calc R U . . .
H4 H 1.476(4) 0.657(3) 1.255(3) 0.117(15) 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
Ni1 O1 2.0465(16) . ?
Ni1 N2 2.074(2) . ?
Ni1 N5 2.074(2) . ?
Ni1 N3 2.080(2) . ?
Ni1 N4 2.098(2) . ?
Ni1 O7 2.1125(17) . ?
N1 C4 1.336(3) . ?
N1 C3 1.346(3) . ?
N2 C32 1.322(3) . ?
N2 C29 1.358(3) . ?
N3 C21 1.325(3) . ?
N3 C25 1.363(3) . ?
N4 C44 1.337(3) . ?
N4 C41 1.361(3) . ?
N5 C33 1.323(3) . ?
N5 C37 1.357(3) . ?
O1 C1 1.262(3) . ?
O2 C1 1.254(3) . ?
O3 C11 1.237(3) . ?
O4 C11 1.273(3) . ?
O4 H4 1.04(4) . ?
O5 C18 1.287(3) . ?
O6 C18 1.220(3) . ?
O7 H2W 0.8200 . ?
O7 H1W 0.8535 . ?
O8 H3W 0.8853 . ?
O8 H4W 0.8839 . ?
C1 C2 1.510(3) . ?
C2 C6 1.381(3) . ?
C2 C3 1.399(3) . ?
C3 C14 1.482(3) . ?
C4 C5 1.394(3) . ?
C4 H5 0.9300 . ?
C5 C6 1.389(3) . ?
C5 C7 1.482(3) . ?
C6 H6 0.9300 . ?
C7 C8 1.390(4) . ?
C7 C13 1.391(3) . ?
C8 C9 1.382(3) . ?
C8 H8 0.9300 . ?
C9 C10 1.381(4) . ?
C9 H9 0.9300 . ?
C10 C12 1.393(4) . ?
C10 C11 1.511(3) . ?
C12 C13 1.389(3) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 C15 1.397(3) . ?
C14 C20 1.400(3) . ?
C15 C16 1.387(3) . ?
C15 H15 0.9300 . ?
C16 C17 1.385(3) . ?
C16 H16 0.9300 . ?
C17 C19 1.390(3) . ?
C17 C18 1.509(3) . ?
C19 C20 1.372(3) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
C21 C22 1.397(4) . ?
C21 H21 0.9300 . ?
C22 C23 1.362(4) . ?
C22 H22 0.9300 . ?
C23 C24 1.399(4) . ?
C23 H23 0.9300 . ?
C24 C25 1.405(3) . ?
C24 C26 1.434(4) . ?
C25 C29 1.436(4) . ?
C26 C27 1.344(5) . ?
C26 H26 0.9300 . ?
C27 C28 1.427(4) . ?
C27 H27 0.9300 . ?
C28 C29 1.404(3) . ?
C28 C30 1.406(4) . ?
C30 C31 1.359(4) . ?
C30 H30 0.9300 . ?
C31 C32 1.395(4) . ?
C31 H31 0.9300 . ?
C32 H32 0.9300 . ?
C33 C34 1.389(4) . ?
C33 H33 0.9300 . ?
C34 C35 1.357(4) . ?
C34 H34 0.9300 . ?
C35 C36 1.413(4) . ?
C35 H35 0.9300 . ?
C36 C37 1.399(3) . ?
C36 C38 1.431(4) . ?
C37 C41 1.437(3) . ?
C38 C39 1.346(4) . ?
C38 H38 0.9300 . ?
C39 C40 1.441(4) . ?
C39 H39 0.9300 . ?
C40 C42 1.401(4) . ?
C40 C41 1.404(3) . ?
C42 C43 1.364(4) . ?
C42 H42 0.9300 . ?
C43 C44 1.390(4) . ?
C43 H43 0.9300 . ?
C44 H44 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni1 N2 175.84(8) . . ?
O1 Ni1 N5 85.38(7) . . ?
N2 Ni1 N5 94.42(8) . . ?
O1 Ni1 N3 95.46(7) . . ?
N2 Ni1 N3 80.41(8) . . ?
N5 Ni1 N3 94.08(8) . . ?
O1 Ni1 N4 90.32(7) . . ?
N2 Ni1 N4 93.74(8) . . ?
N5 Ni1 N4 80.04(8) . . ?
N3 Ni1 N4 171.42(8) . . ?
O1 Ni1 O7 89.28(7) . . ?
N2 Ni1 O7 91.08(7) . . ?
N5 Ni1 O7 174.16(7) . . ?
N3 Ni1 O7 88.76(7) . . ?
N4 Ni1 O7 97.67(8) . . ?
C4 N1 C3 118.3(2) . . ?
C32 N2 C29 117.6(2) . . ?
C32 N2 Ni1 129.6(2) . . ?
C29 N2 Ni1 112.72(16) . . ?
C21 N3 C25 117.9(2) . . ?
C21 N3 Ni1 129.67(18) . . ?
C25 N3 Ni1 112.38(16) . . ?
C44 N4 C41 117.5(2) . . ?
C44 N4 Ni1 130.28(18) . . ?
C41 N4 Ni1 112.17(16) . . ?
C33 N5 C37 118.2(2) . . ?
C33 N5 Ni1 128.46(18) . . ?
C37 N5 Ni1 113.17(16) . . ?
C1 O1 Ni1 130.18(15) . . ?
C11 O4 H4 118(2) . . ?
Ni1 O7 H2W 109.6 . . ?
Ni1 O7 H1W 108.5 . . ?
H2W O7 H1W 118.2 . . ?
H3W O8 H4W 100.2 . . ?
O2 C1 O1 125.8(2) . . ?
O2 C1 C2 119.0(2) . . ?
O1 C1 C2 115.13(19) . . ?
C6 C2 C3 118.4(2) . . ?
C6 C2 C1 116.68(19) . . ?
C3 C2 C1 124.82(19) . . ?
N1 C3 C2 121.73(19) . . ?
N1 C3 C14 116.23(19) . . ?
C2 C3 C14 122.0(2) . . ?
N1 C4 C5 124.3(2) . . ?
N1 C4 H5 117.8 . . ?
C5 C4 H5 117.8 . . ?
C6 C5 C4 116.3(2) . . ?
C6 C5 C7 120.6(2) . . ?
C4 C5 C7 123.1(2) . . ?
C2 C6 C5 120.9(2) . . ?
C2 C6 H6 119.6 . . ?
C5 C6 H6 119.6 . . ?
C8 C7 C13 118.4(2) . . ?
C8 C7 C5 119.2(2) . . ?
C13 C7 C5 122.4(2) . . ?
C9 C8 C7 121.0(2) . . ?
C9 C8 H8 119.5 . . ?
C7 C8 H8 119.5 . . ?
C10 C9 C8 120.6(3) . . ?
C10 C9 H9 119.7 . . ?
C8 C9 H9 119.7 . . ?
C9 C10 C12 119.0(2) . . ?
C9 C10 C11 119.5(2) . . ?
C12 C10 C11 121.4(2) . . ?
O3 C11 O4 125.2(2) . . ?
O3 C11 C10 120.1(2) . . ?
O4 C11 C10 114.7(2) . . ?
C13 C12 C10 120.3(2) . . ?
C13 C12 H12 119.8 . . ?
C10 C12 H12 119.8 . . ?
C12 C13 C7 120.7(2) . . ?
C12 C13 H13 119.7 . . ?
C7 C13 H13 119.7 . . ?
C15 C14 C20 118.50(19) . . ?
C15 C14 C3 120.9(2) . . ?
C20 C14 C3 120.6(2) . . ?
C16 C15 C14 120.6(2) . . ?
C16 C15 H15 119.7 . . ?
C14 C15 H15 119.7 . . ?
C17 C16 C15 120.3(2) . . ?
C17 C16 H16 119.9 . . ?
C15 C16 H16 119.9 . . ?
C16 C17 C19 119.3(2) . . ?
C16 C17 C18 120.1(2) . . ?
C19 C17 C18 120.6(2) . . ?
O6 C18 O5 125.7(2) . . ?
O6 C18 C17 119.9(2) . . ?
O5 C18 C17 114.3(2) . . ?
C20 C19 C17 120.8(2) . . ?
C20 C19 H19 119.6 . . ?
C17 C19 H19 119.6 . . ?
C19 C20 C14 120.5(2) . . ?
C19 C20 H20 119.7 . . ?
C14 C20 H20 119.7 . . ?
N3 C21 C22 122.8(3) . . ?
N3 C21 H21 118.6 . . ?
C22 C21 H21 118.6 . . ?
C23 C22 C21 119.4(3) . . ?
C23 C22 H22 120.3 . . ?
C21 C22 H22 120.3 . . ?
C22 C23 C24 119.7(3) . . ?
C22 C23 H23 120.1 . . ?
C24 C23 H23 120.1 . . ?
C23 C24 C25 117.4(2) . . ?
C23 C24 C26 124.1(3) . . ?
C25 C24 C26 118.6(3) . . ?
N3 C25 C24 122.7(2) . . ?
N3 C25 C29 117.2(2) . . ?
C24 C25 C29 120.1(2) . . ?
C27 C26 C24 121.2(3) . . ?
C27 C26 H26 119.4 . . ?
C24 C26 H26 119.4 . . ?
C26 C27 C28 121.6(3) . . ?
C26 C27 H27 119.2 . . ?
C28 C27 H27 119.2 . . ?
C29 C28 C30 117.0(3) . . ?
C29 C28 C27 118.9(3) . . ?
C30 C28 C27 124.1(3) . . ?
N2 C29 C28 123.1(3) . . ?
N2 C29 C25 117.3(2) . . ?
C28 C29 C25 119.7(3) . . ?
C31 C30 C28 119.7(3) . . ?
C31 C30 H30 120.1 . . ?
C28 C30 H30 120.1 . . ?
C30 C31 C32 119.3(3) . . ?
C30 C31 H31 120.4 . . ?
C32 C31 H31 120.4 . . ?
N2 C32 C31 123.3(3) . . ?
N2 C32 H32 118.4 . . ?
C31 C32 H32 118.4 . . ?
N5 C33 C34 122.6(3) . . ?
N5 C33 H33 118.7 . . ?
C34 C33 H33 118.7 . . ?
C35 C34 C33 120.0(3) . . ?
C35 C34 H34 120.0 . . ?
C33 C34 H34 120.0 . . ?
C34 C35 C36 119.2(3) . . ?
C34 C35 H35 120.4 . . ?
C36 C35 H35 120.4 . . ?
C37 C36 C35 117.1(3) . . ?
C37 C36 C38 119.3(3) . . ?
C35 C36 C38 123.6(3) . . ?
N5 C37 C36 122.9(2) . . ?
N5 C37 C41 117.2(2) . . ?
C36 C37 C41 119.9(2) . . ?
C39 C38 C36 121.3(3) . . ?
C39 C38 H38 119.4 . . ?
C36 C38 H38 119.4 . . ?
C38 C39 C40 120.7(3) . . ?
C38 C39 H39 119.6 . . ?
C40 C39 H39 119.6 . . ?
C42 C40 C41 117.2(3) . . ?
C42 C40 C39 123.5(3) . . ?
C41 C40 C39 119.3(3) . . ?
N4 C41 C40 123.2(2) . . ?
N4 C41 C37 117.4(2) . . ?
C40 C41 C37 119.5(2) . . ?
C43 C42 C40 119.6(3) . . ?
C43 C42 H42 120.2 . . ?
C40 C42 H42 120.2 . . ?
C42 C43 C44 119.8(3) . . ?
C42 C43 H43 120.1 . . ?
C44 C43 H43 120.1 . . ?
N4 C44 C43 122.7(3) . . ?
N4 C44 H44 118.7 . . ?
C43 C44 H44 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
Ni1 O1 C1 O2 33.1(3) . . . . ?
Ni1 O1 C1 C2 -143.16(16) . . . . ?
O2 C1 C2 C6 -132.8(2) . . . . ?
O1 C1 C2 C6 43.7(3) . . . . ?
O2 C1 C2 C3 44.2(3) . . . . ?
O1 C1 C2 C3 -139.3(2) . . . . ?
C4 N1 C3 C2 0.1(4) . . . . ?
C4 N1 C3 C14 178.2(2) . . . . ?
C6 C2 C3 N1 2.0(3) . . . . ?
C1 C2 C3 N1 -175.0(2) . . . . ?
C6 C2 C3 C14 -176.0(2) . . . . ?
C1 C2 C3 C14 7.0(4) . . . . ?
C3 N1 C4 C5 -1.9(4) . . . . ?
N1 C4 C5 C6 1.6(4) . . . . ?
N1 C4 C5 C7 179.3(2) . . . . ?
C3 C2 C6 C5 -2.4(4) . . . . ?
C1 C2 C6 C5 174.9(2) . . . . ?
C4 C5 C6 C2 0.7(4) . . . . ?
C7 C5 C6 C2 -177.2(2) . . . . ?
C6 C5 C7 C8 40.7(4) . . . . ?
C4 C5 C7 C8 -137.0(3) . . . . ?
C6 C5 C7 C13 -137.8(3) . . . . ?
C4 C5 C7 C13 44.5(4) . . . . ?
C13 C7 C8 C9 -1.3(4) . . . . ?
C5 C7 C8 C9 -179.8(3) . . . . ?
C7 C8 C9 C10 0.3(5) . . . . ?
C8 C9 C10 C12 0.9(5) . . . . ?
C8 C9 C10 C11 -175.6(3) . . . . ?
C9 C10 C11 O3 -0.7(4) . . . . ?
C12 C10 C11 O3 -177.1(3) . . . . ?
C9 C10 C11 O4 177.4(3) . . . . ?
C12 C10 C11 O4 1.1(4) . . . . ?
C9 C10 C12 C13 -1.0(4) . . . . ?
C11 C10 C12 C13 175.4(2) . . . . ?
C10 C12 C13 C7 -0.1(4) . . . . ?
C8 C7 C13 C12 1.2(4) . . . . ?
C5 C7 C13 C12 179.7(2) . . . . ?
N1 C3 C14 C15 40.1(3) . . . . ?
C2 C3 C14 C15 -141.7(2) . . . . ?
N1 C3 C14 C20 -139.1(2) . . . . ?
C2 C3 C14 C20 39.0(3) . . . . ?
C20 C14 C15 C16 -0.5(3) . . . . ?
C3 C14 C15 C16 -179.7(2) . . . . ?
C14 C15 C16 C17 -1.9(4) . . . . ?
C15 C16 C17 C19 2.2(4) . . . . ?
C15 C16 C17 C18 -177.8(2) . . . . ?
C16 C17 C18 O6 -15.1(4) . . . . ?
C19 C17 C18 O6 164.8(2) . . . . ?
C16 C17 C18 O5 162.9(2) . . . . ?
C19 C17 C18 O5 -17.2(3) . . . . ?
C16 C17 C19 C20 -0.2(3) . . . . ?
C18 C17 C19 C20 179.9(2) . . . . ?
C17 C19 C20 C14 -2.2(3) . . . . ?
C15 C14 C20 C19 2.5(3) . . . . ?
C3 C14 C20 C19 -178.2(2) . . . . ?
C25 N3 C21 C22 -0.9(4) . . . . ?
Ni1 N3 C21 C22 -178.0(2) . . . . ?
N3 C21 C22 C23 -0.4(4) . . . . ?
C21 C22 C23 C24 0.9(4) . . . . ?
C22 C23 C24 C25 -0.1(4) . . . . ?
C22 C23 C24 C26 179.9(3) . . . . ?
C21 N3 C25 C24 1.7(4) . . . . ?
Ni1 N3 C25 C24 179.39(19) . . . . ?
C21 N3 C25 C29 -177.4(2) . . . . ?
Ni1 N3 C25 C29 0.3(3) . . . . ?
C23 C24 C25 N3 -1.3(4) . . . . ?
C26 C24 C25 N3 178.7(2) . . . . ?
C23 C24 C25 C29 177.8(2) . . . . ?
C26 C24 C25 C29 -2.2(4) . . . . ?
C23 C24 C26 C27 -178.7(3) . . . . ?
C25 C24 C26 C27 1.3(4) . . . . ?
C24 C26 C27 C28 0.7(5) . . . . ?
C26 C27 C28 C29 -1.9(4) . . . . ?
C26 C27 C28 C30 177.4(3) . . . . ?
C32 N2 C29 C28 -1.7(4) . . . . ?
Ni1 N2 C29 C28 179.21(19) . . . . ?
C32 N2 C29 C25 177.7(2) . . . . ?
Ni1 N2 C29 C25 -1.4(3) . . . . ?
C30 C28 C29 N2 1.1(4) . . . . ?
C27 C28 C29 N2 -179.6(2) . . . . ?
C30 C28 C29 C25 -178.3(2) . . . . ?
C27 C28 C29 C25 1.0(4) . . . . ?
N3 C25 C29 N2 0.7(3) . . . . ?
C24 C25 C29 N2 -178.4(2) . . . . ?
N3 C25 C29 C28 -179.8(2) . . . . ?
C24 C25 C29 C28 1.0(4) . . . . ?
C29 C28 C30 C31 -0.1(4) . . . . ?
C27 C28 C30 C31 -179.4(3) . . . . ?
C28 C30 C31 C32 -0.1(4) . . . . ?
C29 N2 C32 C31 1.5(4) . . . . ?
Ni1 N2 C32 C31 -179.7(2) . . . . ?
C30 C31 C32 N2 -0.6(4) . . . . ?
C37 N5 C33 C34 0.0(4) . . . . ?
Ni1 N5 C33 C34 -174.8(2) . . . . ?
N5 C33 C34 C35 -2.3(4) . . . . ?
C33 C34 C35 C36 2.5(4) . . . . ?
C34 C35 C36 C37 -0.5(4) . . . . ?
C34 C35 C36 C38 178.8(3) . . . . ?
C33 N5 C37 C36 2.2(4) . . . . ?
Ni1 N5 C37 C36 177.74(19) . . . . ?
C33 N5 C37 C41 -177.3(2) . . . . ?
Ni1 N5 C37 C41 -1.8(3) . . . . ?
C35 C36 C37 N5 -2.0(4) . . . . ?
C38 C36 C37 N5 178.8(2) . . . . ?
C35 C36 C37 C41 177.6(2) . . . . ?
C38 C36 C37 C41 -1.7(4) . . . . ?
C37 C36 C38 C39 0.4(4) . . . . ?
C35 C36 C38 C39 -178.8(3) . . . . ?
C36 C38 C39 C40 0.4(5) . . . . ?
C38 C39 C40 C42 -179.8(3) . . . . ?
C38 C39 C40 C41 0.0(4) . . . . ?
C44 N4 C41 C40 0.5(4) . . . . ?
Ni1 N4 C41 C40 179.42(19) . . . . ?
C44 N4 C41 C37 -179.5(2) . . . . ?
Ni1 N4 C41 C37 -0.6(3) . . . . ?
C42 C40 C41 N4 -1.5(4) . . . . ?
C39 C40 C41 N4 178.8(2) . . . . ?
C42 C40 C41 C37 178.5(2) . . . . ?
C39 C40 C41 C37 -1.2(4) . . . . ?
N5 C37 C41 N4 1.7(3) . . . . ?
C36 C37 C41 N4 -177.9(2) . . . . ?
N5 C37 C41 C40 -178.4(2) . . . . ?
C36 C37 C41 C40 2.1(4) . . . . ?
C41 C40 C42 C43 1.0(4) . . . . ?
C39 C40 C42 C43 -179.3(3) . . . . ?
C40 C42 C43 C44 0.5(4) . . . . ?
C41 N4 C44 C43 1.0(4) . . . . ?
Ni1 N4 C44 C43 -177.7(2) . . . . ?
C42 C43 C44 N4 -1.5(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 H4 O5 1.04(4) 1.41(4) 2.452(2) 177(4) 1_646
C43 H43 O5 0.93 2.59 3.385(3) 143.1 2_776
C31 H31 N1 0.93 2.70 3.600(4) 164.3 1_545
C22 H22 O6 0.93 2.47 3.218(4) 137.8 2_686
O8 H4W O3 0.88 2.17 3.022(4) 162.8 2_766
O8 H3W O3 0.89 2.17 3.023(4) 162.4 1_454
O7 H2W O2 0.82 1.90 2.657(2) 153.4 .
O7 H2W O2 0.82 1.90 2.657(2) 153.4 .
O8 H3W O3 0.89 2.17 3.023(4) 162.4 1_454
O8 H4W O3 0.88 2.17 3.022(4) 162.8 2_766
C22 H22 O6 0.93 2.47 3.218(4) 137.8 2_686
C31 H31 N1 0.93 2.70 3.600(4) 164.3 1_545
C43 H43 O5 0.93 2.59 3.385(3) 143.1 2_776
O4 H4 O5 1.04(4) 1.41(4) 2.452(2) 177(4) 1_646
O7 H2W O2 0.82 1.90 2.657(2) 153.4 .
O8 H3W O3 0.89 2.17 3.023(4) 162.4 1_454
O8 H4W O3 0.88 2.17 3.022(4) 162.8 2_766
C22 H22 O6 0.93 2.47 3.218(4) 137.8 2_686
C31 H31 N1 0.93 2.70 3.600(4) 164.3 1_545
C43 H43 O5 0.93 2.59 3.385(3) 143.1 2_776
O4 H4 O5 1.04(4) 1.41(4) 2.452(2) 177(4) 1_646

_refine_diff_density_max         0.268
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.046

####################################################################### 
# 
# 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_403-13Mn
_database_code_depnum_ccdc_archive 'CCDC 1984470'
_audit_update_record             
;
2020-05-08 deposited with the CCDC.	2020-05-11 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 H44 Mn3 N6 O16'
_chemical_formula_weight         1269.83

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_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                   9.4017(13)
_cell_length_b                   10.8041(18)
_cell_length_c                   14.5350(16)
_cell_angle_alpha                105.013(12)
_cell_angle_beta                 99.708(11)
_cell_angle_gamma                107.961(14)
_cell_volume                     1306.0(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7377
_cell_measurement_theta_min      4.561
_cell_measurement_theta_max      64.993

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_F_000             645
_exptl_transmission_factor_min   0.238
_exptl_transmission_factor_max   0.245
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.220
_exptl_absorpt_coefficient_mu    6.518
_shelx_estimated_absorpt_T_min   0.293
_shelx_estimated_absorpt_T_max   0.328
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.293
_exptl_absorpt_correction_T_max  0.328
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\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            7377
_diffrn_reflns_av_unetI/netI     0.0695
_diffrn_reflns_av_R_equivalents  0.0591
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         4.561
_diffrn_reflns_theta_max         64.993
_diffrn_reflns_theta_full        64.993
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measured_fraction_theta_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_point_group_measured_fraction_full 0.960
_reflns_number_total             4266
_reflns_number_gt                3493
_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)+(0.1710P)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         4266
_refine_ls_number_parameters     385
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0926
_refine_ls_R_factor_gt           0.0826
_refine_ls_wR_factor_ref         0.2285
_refine_ls_wR_factor_gt          0.2070
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_restrained_S_all      1.001
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 1.07687(8) 0.97802(7) 0.26891(5) 0.0307(3) Uani 1 1 d . . . . .
Mn2 Mn 1.0000 1.0000 0.0000 0.0300(3) Uani 1 2 d S . P . .
N1 N -0.0439(5) 0.4912(4) 0.1618(3) 0.0371(9) Uani 1 1 d . . . . .
N2 N 1.1161(5) 0.8361(4) 0.3540(3) 0.0366(9) Uani 1 1 d . . . . .
N3 N 0.8933(5) 0.9407(4) 0.3514(3) 0.0363(9) Uani 1 1 d . . . . .
O1 O 0.9179(4) 0.8069(3) 0.1381(3) 0.0368(8) Uani 1 1 d . . . . .
O2 O 0.7965(4) 0.8586(4) 0.0171(3) 0.0409(8) Uani 1 1 d . . . . .
O3 O 0.0645(4) 0.0980(3) 0.1618(3) 0.0378(8) Uani 1 1 d . . . . .
O4 O 0.0320(4) 0.1995(4) 0.3033(3) 0.0463(9) Uani 1 1 d . . . . .
O5 O -0.7076(4) -0.0260(3) 0.2186(3) 0.0368(8) Uani 1 1 d . . . . .
O6 O -0.6707(4) 0.1603(4) 0.3411(3) 0.0424(8) Uani 1 1 d . . . . .
O7 O 1.1291(4) 0.8652(4) 0.0273(3) 0.0383(8) Uani 1 1 d . . . . .
O8 O 0.3374(7) 0.4314(6) 0.4398(5) 0.0921(18) Uani 1 1 d . . . . .
H2W H 0.4153 0.4879 0.4371 0.110 Uiso 1 1 d R U . . .
H1W H 0.3376 0.3540 0.4069 0.110 Uiso 1 1 d R U . . .
C1 C 0.7954(5) 0.8015(5) 0.0819(4) 0.0321(10) Uani 1 1 d . . . . .
C2 C 0.6425(5) 0.7228(4) 0.0932(3) 0.0287(9) Uani 1 1 d . . . . .
C3 C 0.6377(6) 0.6474(5) 0.1584(4) 0.0406(11) Uani 1 1 d . . . . .
H3 H 0.7290 0.6439 0.1921 0.049 Uiso 1 1 calc R U . . .
C4 C 0.4978(6) 0.5783(5) 0.1728(4) 0.0414(12) Uani 1 1 d . . . . .
H4 H 0.4960 0.5284 0.2163 0.050 Uiso 1 1 calc R U . . .
C5 C 0.3595(5) 0.5815(4) 0.1239(3) 0.0306(9) Uani 1 1 d . . . . .
C6 C 0.3639(5) 0.6530(5) 0.0566(4) 0.0367(11) Uani 1 1 d . . . . .
H6 H 0.2721 0.6530 0.0208 0.044 Uiso 1 1 calc R U . . .
C7 C 0.5049(6) 0.7242(5) 0.0430(4) 0.0378(11) Uani 1 1 d . . . . .
H7 H 0.5068 0.7737 -0.0008 0.045 Uiso 1 1 calc R U . . .
C8 C 0.2103(5) 0.5060(4) 0.1416(4) 0.0312(10) Uani 1 1 d . . . . .
C9 C 0.1921(5) 0.3867(4) 0.1653(3) 0.0305(9) Uani 1 1 d . . . . .
H9 H 0.2696 0.3501 0.1653 0.037 Uiso 1 1 calc R U . . .
C10 C 0.0565(5) 0.3217(4) 0.1891(3) 0.0276(9) Uani 1 1 d . . . . .
C11 C 0.0479(5) 0.1986(5) 0.2191(4) 0.0331(10) Uani 1 1 d . . . . .
C12 C -0.0597(5) 0.3763(5) 0.1859(3) 0.0315(10) Uani 1 1 d . . . . .
C13 C 0.0884(6) 0.5519(5) 0.1412(4) 0.0379(11) Uani 1 1 d . . . . .
H13 H 0.0992 0.6317 0.1252 0.045 Uiso 1 1 calc R U . . .
C14 C -0.2100(5) 0.3062(5) 0.2046(4) 0.0314(10) Uani 1 1 d . . . . .
C15 C -0.2924(5) 0.1666(5) 0.1580(4) 0.0350(10) Uani 1 1 d . . . . .
H15 H -0.2551 0.1164 0.1125 0.042 Uiso 1 1 calc R U . . .
C16 C -0.4288(5) 0.1003(5) 0.1774(4) 0.0335(10) Uani 1 1 d . . . . .
H16 H -0.4846 0.0069 0.1435 0.040 Uiso 1 1 calc R U . . .
C17 C -0.4828(5) 0.1739(5) 0.2480(3) 0.0310(9) Uani 1 1 d . . . . .
C18 C -0.6283(5) 0.0977(5) 0.2712(3) 0.0339(10) Uani 1 1 d . . . . .
C19 C -0.4019(6) 0.3131(5) 0.2938(4) 0.0395(11) Uani 1 1 d . . . . .
H19 H -0.4371 0.3631 0.3408 0.047 Uiso 1 1 calc R U . . .
C20 C -0.2686(6) 0.3795(5) 0.2705(4) 0.0416(12) Uani 1 1 d . . . . .
H20 H -0.2180 0.4745 0.2996 0.050 Uiso 1 1 calc R U . . .
C21 C 1.2294(7) 0.7868(6) 0.3523(4) 0.0453(12) Uani 1 1 d . . . . .
H21 H 1.3000 0.8143 0.3170 0.054 Uiso 1 1 calc R U . . .
C22 C 1.2456(8) 0.6956(7) 0.4014(5) 0.0579(16) Uani 1 1 d . . . . .
H22 H 1.3230 0.6595 0.3967 0.070 Uiso 1 1 calc R U . . .
C23 C 1.1454(9) 0.6593(7) 0.4573(5) 0.0626(17) Uani 1 1 d . . . . .
H23 H 1.1563 0.6006 0.4925 0.075 Uiso 1 1 calc R U . . .
C24 C 1.0296(7) 0.7106(6) 0.4604(4) 0.0502(14) Uani 1 1 d . . . . .
H24 H 0.9609 0.6873 0.4978 0.060 Uiso 1 1 calc R U . . .
C25 C 1.0155(6) 0.7983(5) 0.4068(4) 0.0361(11) Uani 1 1 d . . . . .
C26 C 0.8902(6) 0.8531(5) 0.4029(4) 0.0358(10) Uani 1 1 d . . . . .
C27 C 0.7750(7) 0.8206(7) 0.4516(4) 0.0549(15) Uani 1 1 d . . . . .
H27 H 0.7746 0.7618 0.4884 0.066 Uiso 1 1 calc R U . . .
C28 C 0.6621(7) 0.8766(8) 0.4445(5) 0.0589(17) Uani 1 1 d . . . . .
H28 H 0.5853 0.8568 0.4772 0.071 Uiso 1 1 calc R U . . .
C29 C 0.6636(7) 0.9618(7) 0.3889(5) 0.0550(15) Uani 1 1 d . . . . .
H29 H 0.5871 0.9991 0.3820 0.066 Uiso 1 1 calc R U . . .
C30 C 0.7813(6) 0.9905(6) 0.3438(4) 0.0467(13) Uani 1 1 d . . . . .
H30 H 0.7822 1.0479 0.3058 0.056 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 O1 2.187(4) . ?
Mn1 N3 2.258(4) . ?
Mn1 O5 2.276(3) 1_765 ?
Mn1 O3 2.280(3) 1_665 ?
Mn1 N2 2.280(4) . ?
Mn1 O6 2.412(4) 1_765 ?
Mn1 O4 2.495(4) 1_665 ?
Mn2 O2 2.147(3) . ?
Mn2 O2 2.147(3) 2_775 ?
Mn2 O3 2.202(3) 2_665 ?
Mn2 O3 2.202(3) 1_665 ?
Mn2 O7 2.231(3) . ?
Mn2 O7 2.231(3) 2_775 ?
N1 C13 1.339(6) . ?
N1 C12 1.347(6) . ?
N2 C21 1.331(7) . ?
N2 C25 1.348(7) . ?
N3 C30 1.324(7) . ?
N3 C26 1.346(6) . ?
O1 C1 1.271(6) . ?
O2 C1 1.252(6) . ?
O3 C11 1.257(6) . ?
O3 Mn2 2.202(3) 1_445 ?
O3 Mn1 2.280(3) 1_445 ?
O4 C11 1.256(6) . ?
O4 Mn1 2.495(4) 1_445 ?
O5 C18 1.261(6) . ?
O5 Mn1 2.276(3) 1_345 ?
O6 C18 1.263(6) . ?
O6 Mn1 2.412(4) 1_345 ?
O8 H2W 0.8109 . ?
O8 H1W 0.8501 . ?
C1 C2 1.489(6) . ?
C2 C7 1.381(7) . ?
C2 C3 1.397(6) . ?
C3 C4 1.379(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.388(7) . ?
C4 H4 0.9300 . ?
C5 C6 1.393(7) . ?
C5 C8 1.491(6) . ?
C6 C7 1.389(7) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 C9 1.387(6) . ?
C8 C13 1.382(7) . ?
C9 C10 1.401(6) . ?
C9 H9 0.9300 . ?
C10 C12 1.393(6) . ?
C10 C11 1.486(6) . ?
C12 C14 1.490(6) . ?
C13 H13 0.9300 . ?
C14 C15 1.380(7) . ?
C14 C20 1.380(7) . ?
C15 C16 1.377(7) . ?
C15 H15 0.9300 . ?
C16 C17 1.395(7) . ?
C16 H16 0.9300 . ?
C17 C19 1.374(7) . ?
C17 C18 1.505(6) . ?
C19 C20 1.384(7) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
C21 C22 1.387(8) . ?
C21 H21 0.9300 . ?
C22 C23 1.377(10) . ?
C22 H22 0.9300 . ?
C23 C24 1.368(9) . ?
C23 H23 0.9300 . ?
C24 C25 1.394(7) . ?
C24 H24 0.9300 . ?
C25 C26 1.472(7) . ?
C26 C27 1.397(8) . ?
C27 C28 1.377(9) . ?
C27 H27 0.9300 . ?
C28 C29 1.372(9) . ?
C28 H28 0.9300 . ?
C29 C30 1.375(8) . ?
C29 H29 0.9300 . ?
C30 H30 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Mn1 N3 90.01(14) . . ?
O1 Mn1 O5 93.80(13) . 1_765 ?
N3 Mn1 O5 159.48(14) . 1_765 ?
O1 Mn1 O3 81.55(12) . 1_665 ?
N3 Mn1 O3 119.18(15) . 1_665 ?
O5 Mn1 O3 81.34(13) 1_765 1_665 ?
O1 Mn1 N2 93.43(14) . . ?
N3 Mn1 N2 72.05(15) . . ?
O5 Mn1 N2 87.59(14) 1_765 . ?
O3 Mn1 N2 167.47(15) 1_665 . ?
O1 Mn1 O6 146.98(13) . 1_765 ?
N3 Mn1 O6 122.99(14) . 1_765 ?
O5 Mn1 O6 55.90(12) 1_765 1_765 ?
O3 Mn1 O6 81.10(12) 1_665 1_765 ?
N2 Mn1 O6 97.56(14) . 1_765 ?
O1 Mn1 O4 116.95(13) . 1_665 ?
N3 Mn1 O4 78.49(13) . 1_665 ?
O5 Mn1 O4 117.12(12) 1_765 1_665 ?
O3 Mn1 O4 54.27(12) 1_665 1_665 ?
N2 Mn1 O4 137.42(14) . 1_665 ?
O6 Mn1 O4 73.50(13) 1_765 1_665 ?
O2 Mn2 O2 180.00(19) . 2_775 ?
O2 Mn2 O3 93.77(13) . 2_665 ?
O2 Mn2 O3 86.23(13) 2_775 2_665 ?
O2 Mn2 O3 86.23(13) . 1_665 ?
O2 Mn2 O3 93.77(13) 2_775 1_665 ?
O3 Mn2 O3 180.00(9) 2_665 1_665 ?
O2 Mn2 O7 89.50(13) . . ?
O2 Mn2 O7 90.50(13) 2_775 . ?
O3 Mn2 O7 93.03(12) 2_665 . ?
O3 Mn2 O7 86.97(12) 1_665 . ?
O2 Mn2 O7 90.50(13) . 2_775 ?
O2 Mn2 O7 89.50(13) 2_775 2_775 ?
O3 Mn2 O7 86.97(12) 2_665 2_775 ?
O3 Mn2 O7 93.03(12) 1_665 2_775 ?
O7 Mn2 O7 180.0 . 2_775 ?
C13 N1 C12 117.6(4) . . ?
C21 N2 C25 119.0(4) . . ?
C21 N2 Mn1 123.7(4) . . ?
C25 N2 Mn1 117.3(3) . . ?
C30 N3 C26 119.0(4) . . ?
C30 N3 Mn1 122.9(3) . . ?
C26 N3 Mn1 117.8(3) . . ?
C1 O1 Mn1 127.8(3) . . ?
C1 O2 Mn2 125.0(3) . . ?
C11 O3 Mn2 134.8(3) . 1_445 ?
C11 O3 Mn1 97.3(3) . 1_445 ?
Mn2 O3 Mn1 122.82(14) 1_445 1_445 ?
C11 O4 Mn1 87.3(3) . 1_445 ?
C18 O5 Mn1 93.2(3) . 1_345 ?
C18 O6 Mn1 87.0(3) . 1_345 ?
H2W O8 H1W 104.7 . . ?
O2 C1 O1 123.4(4) . . ?
O2 C1 C2 118.2(4) . . ?
O1 C1 C2 118.4(4) . . ?
C7 C2 C3 118.8(4) . . ?
C7 C2 C1 122.0(4) . . ?
C3 C2 C1 119.2(4) . . ?
C4 C3 C2 120.0(4) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C3 C4 C5 121.5(4) . . ?
C3 C4 H4 119.3 . . ?
C5 C4 H4 119.3 . . ?
C4 C5 C6 118.4(4) . . ?
C4 C5 C8 120.1(4) . . ?
C6 C5 C8 121.5(4) . . ?
C7 C6 C5 120.2(4) . . ?
C7 C6 H6 119.9 . . ?
C5 C6 H6 119.9 . . ?
C2 C7 C6 121.1(4) . . ?
C2 C7 H7 119.5 . . ?
C6 C7 H7 119.5 . . ?
C9 C8 C13 116.5(4) . . ?
C9 C8 C5 119.7(4) . . ?
C13 C8 C5 123.7(4) . . ?
C8 C9 C10 119.7(4) . . ?
C8 C9 H9 120.2 . . ?
C10 C9 H9 120.2 . . ?
C12 C10 C9 119.1(4) . . ?
C12 C10 C11 123.8(4) . . ?
C9 C10 C11 117.0(4) . . ?
O4 C11 O3 120.9(4) . . ?
O4 C11 C10 119.6(4) . . ?
O3 C11 C10 119.4(4) . . ?
N1 C12 C10 121.6(4) . . ?
N1 C12 C14 117.2(4) . . ?
C10 C12 C14 121.2(4) . . ?
N1 C13 C8 125.5(4) . . ?
N1 C13 H13 117.3 . . ?
C8 C13 H13 117.3 . . ?
C15 C14 C20 118.5(4) . . ?
C15 C14 C12 121.1(4) . . ?
C20 C14 C12 120.4(4) . . ?
C16 C15 C14 121.4(4) . . ?
C16 C15 H15 119.3 . . ?
C14 C15 H15 119.3 . . ?
C15 C16 C17 119.7(4) . . ?
C15 C16 H16 120.1 . . ?
C17 C16 H16 120.1 . . ?
C19 C17 C16 119.0(4) . . ?
C19 C17 C18 122.3(4) . . ?
C16 C17 C18 118.7(4) . . ?
O6 C18 O5 121.4(4) . . ?
O6 C18 C17 119.3(4) . . ?
O5 C18 C17 119.3(4) . . ?
C17 C19 C20 120.6(5) . . ?
C17 C19 H19 119.7 . . ?
C20 C19 H19 119.7 . . ?
C14 C20 C19 120.6(5) . . ?
C14 C20 H20 119.7 . . ?
C19 C20 H20 119.7 . . ?
N2 C21 C22 122.1(6) . . ?
N2 C21 H21 118.9 . . ?
C22 C21 H21 118.9 . . ?
C23 C22 C21 119.1(6) . . ?
C23 C22 H22 120.5 . . ?
C21 C22 H22 120.5 . . ?
C24 C23 C22 119.2(5) . . ?
C24 C23 H23 120.4 . . ?
C22 C23 H23 120.4 . . ?
C23 C24 C25 119.3(6) . . ?
C23 C24 H24 120.3 . . ?
C25 C24 H24 120.3 . . ?
N2 C25 C24 121.3(5) . . ?
N2 C25 C26 116.1(4) . . ?
C24 C25 C26 122.6(5) . . ?
N3 C26 C27 120.6(5) . . ?
N3 C26 C25 116.6(4) . . ?
C27 C26 C25 122.8(5) . . ?
C28 C27 C26 119.2(5) . . ?
C28 C27 H27 120.4 . . ?
C26 C27 H27 120.4 . . ?
C27 C28 C29 119.5(5) . . ?
C27 C28 H28 120.2 . . ?
C29 C28 H28 120.2 . . ?
C30 C29 C28 118.1(6) . . ?
C30 C29 H29 120.9 . . ?
C28 C29 H29 120.9 . . ?
N3 C30 C29 123.5(5) . . ?
N3 C30 H30 118.2 . . ?
C29 C30 H30 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
Mn2 O2 C1 O1 -9.3(7) . . . . ?
Mn2 O2 C1 C2 171.0(3) . . . . ?
Mn1 O1 C1 O2 77.9(6) . . . . ?
Mn1 O1 C1 C2 -102.4(4) . . . . ?
O2 C1 C2 C7 -7.6(7) . . . . ?
O1 C1 C2 C7 172.8(5) . . . . ?
O2 C1 C2 C3 173.9(5) . . . . ?
O1 C1 C2 C3 -5.7(7) . . . . ?
C7 C2 C3 C4 -1.1(8) . . . . ?
C1 C2 C3 C4 177.4(5) . . . . ?
C2 C3 C4 C5 -0.1(9) . . . . ?
C3 C4 C5 C6 2.1(8) . . . . ?
C3 C4 C5 C8 -179.7(5) . . . . ?
C4 C5 C6 C7 -2.9(8) . . . . ?
C8 C5 C6 C7 179.0(5) . . . . ?
C3 C2 C7 C6 0.3(8) . . . . ?
C1 C2 C7 C6 -178.2(5) . . . . ?
C5 C6 C7 C2 1.8(8) . . . . ?
C4 C5 C8 C9 -30.5(7) . . . . ?
C6 C5 C8 C9 147.6(5) . . . . ?
C4 C5 C8 C13 145.8(5) . . . . ?
C6 C5 C8 C13 -36.1(8) . . . . ?
C13 C8 C9 C10 -1.3(7) . . . . ?
C5 C8 C9 C10 175.2(4) . . . . ?
C8 C9 C10 C12 1.7(7) . . . . ?
C8 C9 C10 C11 -176.7(4) . . . . ?
Mn1 O4 C11 O3 4.8(4) 1_445 . . . ?
Mn1 O4 C11 C10 -171.6(4) 1_445 . . . ?
Mn2 O3 C11 O4 148.5(4) 1_445 . . . ?
Mn1 O3 C11 O4 -5.3(5) 1_445 . . . ?
Mn2 O3 C11 C10 -35.1(6) 1_445 . . . ?
Mn1 O3 C11 C10 171.1(3) 1_445 . . . ?
C12 C10 C11 O4 -58.5(7) . . . . ?
C9 C10 C11 O4 119.9(5) . . . . ?
C12 C10 C11 O3 125.1(5) . . . . ?
C9 C10 C11 O3 -56.6(6) . . . . ?
C13 N1 C12 C10 -0.2(7) . . . . ?
C13 N1 C12 C14 -177.5(5) . . . . ?
C9 C10 C12 N1 -0.9(7) . . . . ?
C11 C10 C12 N1 177.4(5) . . . . ?
C9 C10 C12 C14 176.2(4) . . . . ?
C11 C10 C12 C14 -5.4(7) . . . . ?
C12 N1 C13 C8 0.6(8) . . . . ?
C9 C8 C13 N1 0.2(8) . . . . ?
C5 C8 C13 N1 -176.2(5) . . . . ?
N1 C12 C14 C15 129.1(5) . . . . ?
C10 C12 C14 C15 -48.2(7) . . . . ?
N1 C12 C14 C20 -52.0(6) . . . . ?
C10 C12 C14 C20 130.7(5) . . . . ?
C20 C14 C15 C16 -1.1(7) . . . . ?
C12 C14 C15 C16 177.8(4) . . . . ?
C14 C15 C16 C17 -2.3(7) . . . . ?
C15 C16 C17 C19 2.9(7) . . . . ?
C15 C16 C17 C18 -177.3(4) . . . . ?
Mn1 O6 C18 O5 -15.6(4) 1_345 . . . ?
Mn1 O6 C18 C17 162.4(4) 1_345 . . . ?
Mn1 O5 C18 O6 16.6(5) 1_345 . . . ?
Mn1 O5 C18 C17 -161.5(3) 1_345 . . . ?
C19 C17 C18 O6 -6.5(7) . . . . ?
C16 C17 C18 O6 173.7(4) . . . . ?
C19 C17 C18 O5 171.5(5) . . . . ?
C16 C17 C18 O5 -8.2(6) . . . . ?
C16 C17 C19 C20 -0.2(8) . . . . ?
C18 C17 C19 C20 -180.0(5) . . . . ?
C15 C14 C20 C19 3.9(8) . . . . ?
C12 C14 C20 C19 -175.1(5) . . . . ?
C17 C19 C20 C14 -3.2(8) . . . . ?
C25 N2 C21 C22 1.3(9) . . . . ?
Mn1 N2 C21 C22 -177.0(5) . . . . ?
N2 C21 C22 C23 -2.8(10) . . . . ?
C21 C22 C23 C24 2.0(11) . . . . ?
C22 C23 C24 C25 0.1(10) . . . . ?
C21 N2 C25 C24 1.0(8) . . . . ?
Mn1 N2 C25 C24 179.4(4) . . . . ?
C21 N2 C25 C26 -178.1(5) . . . . ?
Mn1 N2 C25 C26 0.3(6) . . . . ?
C23 C24 C25 N2 -1.7(9) . . . . ?
C23 C24 C25 C26 177.4(6) . . . . ?
C30 N3 C26 C27 -3.2(8) . . . . ?
Mn1 N3 C26 C27 -176.9(4) . . . . ?
C30 N3 C26 C25 178.5(5) . . . . ?
Mn1 N3 C26 C25 4.7(6) . . . . ?
N2 C25 C26 N3 -3.3(7) . . . . ?
C24 C25 C26 N3 177.6(5) . . . . ?
N2 C25 C26 C27 178.4(5) . . . . ?
C24 C25 C26 C27 -0.7(8) . . . . ?
N3 C26 C27 C28 1.6(9) . . . . ?
C25 C26 C27 C28 179.8(6) . . . . ?
C26 C27 C28 C29 0.8(10) . . . . ?
C27 C28 C29 C30 -1.4(10) . . . . ?
C26 N3 C30 C29 2.6(9) . . . . ?
Mn1 N3 C30 C29 176.0(5) . . . . ?
C28 C29 C30 N3 -0.3(10) . . . . ?

_refine_diff_density_max         1.068
_refine_diff_density_min         -1.345
_refine_diff_density_rms         0.156

