# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2021

####################################################################### 
# 
# 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_mo_PS_1_0m
_database_code_depnum_ccdc_archive 'CCDC 1963350'
loop_
_audit_author_name
_audit_author_address
'Raju Mondal'
;Indian Association for the Cultivation of Science
India
;
_audit_update_record             
;
2021-02-10 deposited with the CCDC.	2021-03-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C43 H30 Cu2 N11 O9'
_chemical_formula_weight         971.86

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   7.2638(3)
_cell_length_b                   11.8595(5)
_cell_length_c                   13.0619(6)
_cell_angle_alpha                72.350(2)
_cell_angle_beta                 78.127(2)
_cell_angle_gamma                76.793(2)
_cell_volume                     1032.53(8)
_cell_formula_units_Z            1
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    22068
_cell_measurement_theta_min      3.102
_cell_measurement_theta_max      30.504

_exptl_crystal_description       Block
_exptl_crystal_colour            Blue
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_F_000             495
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    1.102
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.94679
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
'SADABS v.2.03 (Bruker, 2001), wR2(int)=0.0674 before correction'

_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-2 CCD area detector'
_diffrn_measurement_method       '/w scans'
_diffrn_detector_area_resol_mean 8
_diffrn_reflns_number            40752
_diffrn_reflns_av_unetI/netI     0.0181
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.152
_diffrn_reflns_theta_max         30.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total             5994
_reflns_number_gt                5382
_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 APEX-2'
_computing_cell_refinement       'Bruker APEX-2'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_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)+(0.0598P)²+1.0137P] 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     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_extinction_coef       0.014(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         5994
_refine_ls_number_parameters     303
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0392
_refine_ls_wR_factor_ref         0.1122
_refine_ls_wR_factor_gt          0.1097
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_restrained_S_all      1.090
_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
Cu1 Cu -0.500000 1.000000 0.500000 0.01452(10) Uani 1 2 d S . P . .
Cu2 Cu 0.000000 0.500000 0.000000 0.01435(10) Uani 1 2 d S . P . .
O1 O -0.0449(2) 0.68436(14) 0.11940(12) 0.0269(3) Uani 1 1 d . . . . .
O2 O -0.5110(2) 0.76686(14) 0.57280(12) 0.0241(3) Uani 1 1 d . . . . .
O3 O -0.09255(19) 0.49715(12) 0.14998(10) 0.0196(3) Uani 1 1 d . . . . .
O4 O -0.36273(19) 0.87977(12) 0.42430(10) 0.0190(3) Uani 1 1 d . . . . .
N1 N -0.2053(3) 0.33518(16) 0.55192(14) 0.0261(4) Uani 1 1 d . . . . .
N2 N -0.2644(3) 0.32440(19) 0.64934(16) 0.0338(4) Uani 1 1 d . . . . .
N3 N -0.3152(4) 0.3036(2) 0.73892(18) 0.0488(6) Uani 1 1 d . . . . .
C1 C -0.4029(2) 0.77824(17) 0.48521(14) 0.0178(3) Uani 1 1 d . . . . .
C2 C -0.3096(2) 0.66969(16) 0.44505(14) 0.0169(3) Uani 1 1 d . . . . .
C3 C -0.3043(3) 0.55628(17) 0.51858(14) 0.0185(3) Uani 1 1 d . . . . .
H3 H -0.354492 0.548774 0.591335 0.022 Uiso 1 1 calc R U . . .
C4 C -0.2235(3) 0.45418(17) 0.48246(14) 0.0189(3) Uani 1 1 d . . . . .
C5 C -0.1579(3) 0.46553(17) 0.37246(14) 0.0194(3) Uani 1 1 d . . . . .
H5 H -0.110570 0.397184 0.347762 0.023 Uiso 1 1 calc R U . . .
C6 C -0.1632(3) 0.57891(17) 0.29959(14) 0.0177(3) Uani 1 1 d . . . . .
C7 C -0.2349(3) 0.68203(17) 0.33578(14) 0.0182(3) Uani 1 1 d . . . . .
H7 H -0.232779 0.757936 0.287654 0.022 Uiso 1 1 calc R U . . .
C8 C -0.0943(3) 0.59082(17) 0.18046(14) 0.0178(3) Uani 1 1 d . . . . .
N4 N 1.2862(2) 0.03976(14) 0.40686(12) 0.0173(3) Uani 1 1 d . . . . .
N5 N 0.2528(2) 0.40130(15) 0.04382(13) 0.0195(3) Uani 1 1 d . . . . .
C9 C 1.1171(3) 0.10814(16) 0.43190(14) 0.0171(3) Uani 1 1 d . . . . .
H9 H 1.101178 0.139891 0.490737 0.020 Uiso 1 1 calc R U . . .
C10 C 0.9664(3) 0.13336(17) 0.37450(15) 0.0194(3) Uani 1 1 d . . . . .
H10 H 0.853362 0.182652 0.393934 0.023 Uiso 1 1 calc R U . . .
C11 C 0.9832(3) 0.08494(17) 0.28717(15) 0.0206(3) Uani 1 1 d . . . . .
C12 C 1.1581(3) 0.0150(2) 0.26058(17) 0.0277(4) Uani 1 1 d . . . . .
H12 H 1.177171 -0.018167 0.202391 0.033 Uiso 1 1 calc R U . . .
C13 C 1.3041(3) -0.0051(2) 0.32136(17) 0.0261(4) Uani 1 1 d . . . . .
H13 H 1.420172 -0.051784 0.302064 0.031 Uiso 1 1 calc R U . . .
C14 C 0.8182(3) 0.11114(18) 0.22516(17) 0.0233(4) Uani 1 1 d . . . . .
H14A H 0.700650 0.103165 0.275715 0.028 Uiso 1 1 calc R U . . .
H14B H 0.837478 0.053445 0.183163 0.028 Uiso 1 1 calc R U . . .
C15 C 0.8011(3) 0.23928(19) 0.14857(16) 0.0246(4) Uani 1 1 d . . . . .
H15A H 0.825653 0.292567 0.185791 0.029 Uiso 1 1 calc R U . . .
H15B H 0.899090 0.239438 0.085647 0.029 Uiso 1 1 calc R U . . .
C16 C 0.6093(3) 0.28829(19) 0.11035(16) 0.0232(4) Uani 1 1 d . . . . .
C17 C 0.4414(3) 0.2920(2) 0.18402(17) 0.0262(5) Uani 0.9 1 d . . P A 1
H17 H 0.445296 0.256675 0.257749 0.031 Uiso 1 1 calc R U . A 1
C18 C 0.2694(3) 0.3479(2) 0.14799(17) 0.0247(4) Uani 0.9 1 d . . P A 1
H18 H 0.159176 0.348507 0.198936 0.030 Uiso 1 1 calc R U . A 1
C17' C 0.506(3) 0.407(2) 0.1484(19) 0.030(4) Uiso 0.1 1 d . . P A 2
C18' C 0.331(3) 0.454(2) 0.1143(19) 0.031(4) Uiso 0.1 1 d . . P A 2
C19 C 0.4135(3) 0.3916(2) -0.02960(16) 0.0263(4) Uani 1 1 d . . . . .
H19 H 0.404180 0.424130 -0.103080 0.032 Uiso 1 1 calc R U . . .
C20 C 0.5913(3) 0.3350(2) 0.00064(17) 0.0278(4) Uani 1 1 d . . . . .
H20 H 0.697827 0.328407 -0.052086 0.033 Uiso 1 1 calc R U . . .
C2S C 0.8364(9) 0.9335(5) 0.0410(5) 0.0413(11) Uiso 0.5 1 d . . P . .
O1S O 1.0996(9) 0.9048(6) 0.0634(5) 0.0750(15) Uiso 0.5 1 d D . P . .
C1S C 0.5420(14) 1.0414(9) 0.0034(8) 0.075(2) Uiso 0.5 1 d . . P . .
N1S N 0.5822(17) 0.9160(10) 0.0454(9) 0.112(3) Uiso 0.5 1 d . . P . .
C3S C 0.9331(11) 0.9322(14) 0.0452(12) 0.120(5) Uiso 0.5 1 d D . P . .


_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
Cu1 O4 1.9506(12) . ?
Cu1 O4 1.9506(12) 2_476 ?
Cu1 N4 2.0517(15) 2_666 ?
Cu1 N4 2.0517(15) 1_365 ?
Cu2 O3 1.9285(13) . ?
Cu2 O3 1.9285(13) 2_565 ?
Cu2 N5 2.0282(15) 2_565 ?
Cu2 N5 2.0282(15) . ?
O1 C8 1.234(2) . ?
O2 C1 1.237(2) . ?
O3 C8 1.286(2) . ?
O4 C1 1.285(2) . ?
N1 N2 1.234(3) . ?
N1 C4 1.421(3) . ?
N2 N3 1.120(3) . ?
C1 C2 1.502(2) . ?
C2 C3 1.393(3) . ?
C2 C7 1.394(2) . ?
C3 C4 1.393(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.393(2) . ?
C5 C6 1.389(3) . ?
C5 H5 0.9300 . ?
C6 C7 1.396(2) . ?
C6 C8 1.507(2) . ?
C7 H7 0.9300 . ?
N4 C9 1.347(2) . ?
N4 C13 1.347(2) . ?
N5 C18 1.333(3) . ?
N5 C19 1.357(2) . ?
N5 C18' 1.52(2) . ?
C9 C10 1.379(2) . ?
C9 H9 0.9300 . ?
C10 C11 1.398(3) . ?
C10 H10 0.9300 . ?
C11 C12 1.391(3) . ?
C11 C14 1.505(3) . ?
C12 C13 1.389(3) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 C15 1.539(3) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.506(3) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.391(3) . ?
C16 C20 1.393(3) . ?
C16 C17' 1.60(2) . ?
C17 C18 1.377(3) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C17' C18' 1.37(3) . ?
C19 C20 1.388(3) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
C2S C3S 0.712(9) . ?
C2S N1S 1.892(13) . ?
O1S C3S 1.2312(10) . ?
C1S N1S 1.144(14) 2_675 ?
C1S C1S 1.301(18) 2_675 ?
C1S N1S 1.403(14) . ?
C3S C3S 2.00(3) 2_775 ?

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 Cu1 O4 180.00(8) . 2_476 ?
O4 Cu1 N4 90.66(6) . 2_666 ?
O4 Cu1 N4 89.34(6) 2_476 2_666 ?
O4 Cu1 N4 89.34(6) . 1_365 ?
O4 Cu1 N4 90.66(6) 2_476 1_365 ?
N4 Cu1 N4 180.0 2_666 1_365 ?
O3 Cu2 O3 180.0 . 2_565 ?
O3 Cu2 N5 90.76(6) . 2_565 ?
O3 Cu2 N5 89.24(6) 2_565 2_565 ?
O3 Cu2 N5 89.24(6) . . ?
O3 Cu2 N5 90.76(6) 2_565 . ?
N5 Cu2 N5 180.0 2_565 . ?
C8 O3 Cu2 118.31(12) . . ?
C1 O4 Cu1 106.21(11) . . ?
N2 N1 C4 116.70(18) . . ?
N3 N2 N1 173.6(3) . . ?
O2 C1 O4 123.59(17) . . ?
O2 C1 C2 120.03(18) . . ?
O4 C1 C2 116.38(15) . . ?
C3 C2 C7 120.69(16) . . ?
C3 C2 C1 118.64(15) . . ?
C7 C2 C1 120.64(16) . . ?
C2 C3 C4 119.61(16) . . ?
C2 C3 H3 120.2 . . ?
C4 C3 H3 120.2 . . ?
C5 C4 C3 119.96(17) . . ?
C5 C4 N1 116.35(16) . . ?
C3 C4 N1 123.68(17) . . ?
C6 C5 C4 120.05(16) . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C5 C6 C7 120.41(16) . . ?
C5 C6 C8 119.90(16) . . ?
C7 C6 C8 119.69(16) . . ?
C2 C7 C6 119.10(17) . . ?
C2 C7 H7 120.4 . . ?
C6 C7 H7 120.4 . . ?
O1 C8 O3 124.34(16) . . ?
O1 C8 C6 121.13(16) . . ?
O3 C8 C6 114.53(16) . . ?
C9 N4 C13 116.85(16) . . ?
C9 N4 Cu1 120.99(12) . 1_745 ?
C13 N4 Cu1 122.10(12) . 1_745 ?
C18 N5 C19 117.10(17) . . ?
C19 N5 C18' 96.8(9) . . ?
C18 N5 Cu2 120.66(13) . . ?
C19 N5 Cu2 122.15(13) . . ?
C18' N5 Cu2 111.8(9) . . ?
N4 C9 C10 123.18(16) . . ?
N4 C9 H9 118.4 . . ?
C10 C9 H9 118.4 . . ?
C9 C10 C11 120.09(17) . . ?
C9 C10 H10 120.0 . . ?
C11 C10 H10 120.0 . . ?
C12 C11 C10 116.87(17) . . ?
C12 C11 C14 122.90(18) . . ?
C10 C11 C14 120.23(17) . . ?
C13 C12 C11 119.68(18) . . ?
C13 C12 H12 120.2 . . ?
C11 C12 H12 120.2 . . ?
N4 C13 C12 123.31(18) . . ?
N4 C13 H13 118.3 . . ?
C12 C13 H13 118.3 . . ?
C11 C14 C15 110.36(16) . . ?
C11 C14 H14A 109.6 . . ?
C15 C14 H14A 109.6 . . ?
C11 C14 H14B 109.6 . . ?
C15 C14 H14B 109.6 . . ?
H14A C14 H14B 108.1 . . ?
C16 C15 C14 114.15(17) . . ?
C16 C15 H15A 108.7 . . ?
C14 C15 H15A 108.7 . . ?
C16 C15 H15B 108.7 . . ?
C14 C15 H15B 108.7 . . ?
H15A C15 H15B 107.6 . . ?
C17 C16 C20 116.83(18) . . ?
C17 C16 C15 121.07(18) . . ?
C20 C16 C15 122.08(18) . . ?
C20 C16 C17' 97.5(9) . . ?
C15 C16 C17' 111.3(9) . . ?
C18 C17 C16 120.12(19) . . ?
C18 C17 H17 119.9 . . ?
C16 C17 H17 119.9 . . ?
N5 C18 C17 123.4(2) . . ?
N5 C18 H18 118.3 . . ?
C17 C18 H18 118.3 . . ?
C18' C17' C16 113.0(19) . . ?
C17' C18' N5 122(2) . . ?
N5 C19 C20 122.59(18) . . ?
N5 C19 H19 118.7 . . ?
C20 C19 H19 118.7 . . ?
C19 C20 C16 119.66(19) . . ?
C19 C20 H20 120.2 . . ?
C16 C20 H20 120.2 . . ?
C3S C2S N1S 171.8(15) . . ?
N1S C1S C1S 69.7(10) 2_675 2_675 ?
N1S C1S N1S 119.6(10) 2_675 . ?
C1S C1S N1S 49.9(8) 2_675 . ?
C1S N1S C1S 60.4(10) 2_675 . ?
C1S N1S C2S 139.0(10) 2_675 . ?
C1S N1S C2S 86.8(7) . . ?
C2S C3S O1S 167(2) . . ?
C2S C3S C3S 120.3(17) . 2_775 ?
O1S C3S C3S 72.8(7) . 2_775 ?

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
Cu1 O4 C1 O2 0.9(2) . . . . ?
Cu1 O4 C1 C2 -178.74(12) . . . . ?
O2 C1 C2 C3 -17.1(3) . . . . ?
O4 C1 C2 C3 162.61(16) . . . . ?
O2 C1 C2 C7 161.06(18) . . . . ?
O4 C1 C2 C7 -19.2(2) . . . . ?
C7 C2 C3 C4 0.0(3) . . . . ?
C1 C2 C3 C4 178.15(16) . . . . ?
C2 C3 C4 C5 -3.5(3) . . . . ?
C2 C3 C4 N1 177.62(18) . . . . ?
N2 N1 C4 C5 -179.5(2) . . . . ?
N2 N1 C4 C3 -0.5(3) . . . . ?
C3 C4 C5 C6 3.6(3) . . . . ?
N1 C4 C5 C6 -177.37(18) . . . . ?
C4 C5 C6 C7 -0.3(3) . . . . ?
C4 C5 C6 C8 -179.30(17) . . . . ?
C3 C2 C7 C6 3.3(3) . . . . ?
C1 C2 C7 C6 -174.85(16) . . . . ?
C5 C6 C7 C2 -3.1(3) . . . . ?
C8 C6 C7 C2 175.87(16) . . . . ?
Cu2 O3 C8 O1 1.9(2) . . . . ?
Cu2 O3 C8 C6 -178.23(11) . . . . ?
C5 C6 C8 O1 -158.80(19) . . . . ?
C7 C6 C8 O1 22.2(3) . . . . ?
C5 C6 C8 O3 21.3(2) . . . . ?
C7 C6 C8 O3 -157.64(17) . . . . ?
C13 N4 C9 C10 -0.2(3) . . . . ?
Cu1 N4 C9 C10 -177.31(14) 1_745 . . . ?
N4 C9 C10 C11 1.5(3) . . . . ?
C9 C10 C11 C12 -1.9(3) . . . . ?
C9 C10 C11 C14 179.29(18) . . . . ?
C10 C11 C12 C13 1.0(3) . . . . ?
C14 C11 C12 C13 179.8(2) . . . . ?
C9 N4 C13 C12 -0.7(3) . . . . ?
Cu1 N4 C13 C12 176.37(18) 1_745 . . . ?
C11 C12 C13 N4 0.3(4) . . . . ?
C12 C11 C14 C15 -102.4(2) . . . . ?
C10 C11 C14 C15 76.3(2) . . . . ?
C11 C14 C15 C16 -161.54(17) . . . . ?
C14 C15 C16 C17 54.8(3) . . . . ?
C14 C15 C16 C20 -127.1(2) . . . . ?
C14 C15 C16 C17' 118.7(9) . . . . ?
C20 C16 C17 C18 -4.6(4) . . . . ?
C15 C16 C17 C18 173.5(2) . . . . ?
C19 N5 C18 C17 4.7(4) . . . . ?
Cu2 N5 C18 C17 -172.0(2) . . . . ?
C16 C17 C18 N5 -0.5(4) . . . . ?
C20 C16 C17' C18' 50.7(18) . . . . ?
C15 C16 C17' C18' 179.5(15) . . . . ?
C16 C17' C18' N5 -2(3) . . . . ?
C19 N5 C18' C17' -48(2) . . . . ?
Cu2 N5 C18' C17' -176.2(18) . . . . ?
C18 N5 C19 C20 -3.6(3) . . . . ?
C18' N5 C19 C20 51.8(9) . . . . ?
Cu2 N5 C19 C20 173.00(17) . . . . ?
N5 C19 C20 C16 -1.6(4) . . . . ?
C17 C16 C20 C19 5.6(3) . . . . ?
C15 C16 C20 C19 -172.6(2) . . . . ?
C17' C16 C20 C19 -51.6(9) . . . . ?
N1S C1S N1S C1S 0.002(2) 2_675 . . 2_675 ?
N1S C1S N1S C2S 154.3(11) 2_675 . . . ?
C1S C1S N1S C2S 154.3(11) 2_675 . . . ?

_refine_diff_density_max         1.093
_refine_diff_density_min         -0.715
_refine_diff_density_rms         0.087

####################################################################### 
# 
# 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_PS220116_0m
_database_code_depnum_ccdc_archive 'CCDC 1963351'
loop_
_audit_author_name
_audit_author_address
'Raju Mondal'
;Indian Association for the Cultivation of Science
India
;
_audit_update_record             
;
2019-11-04 deposited with the CCDC.	2021-03-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H21 Co N6 O4'
_chemical_formula_weight         540.42

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                   10.0002(10)
_cell_length_b                   10.0870(10)
_cell_length_c                   13.5209(14)
_cell_angle_alpha                98.126(4)
_cell_angle_beta                 94.279(4)
_cell_angle_gamma                112.649(3)
_cell_volume                     1233.6(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    1330
_cell_measurement_theta_min      2.279
_cell_measurement_theta_max      3.376

_exptl_crystal_description       Block
_exptl_crystal_colour            Pink
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_F_000             556
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_exptl_absorpt_coefficient_mu    0.741
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.89817
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
'SADABS v.2.03 (Bruker, 2001), wR2(int)=0.0690 before correction'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-2 CCD area detector'
_diffrn_measurement_method       '/w scans'
_diffrn_detector_area_resol_mean 8
_diffrn_reflns_number            16189
_diffrn_reflns_av_unetI/netI     0.1111
_diffrn_reflns_av_R_equivalents  0.0940
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.537
_diffrn_reflns_theta_max         26.401
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             4975
_reflns_number_gt                2965
_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 APEX-2'
_computing_cell_refinement       'Bruker APEX-2'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_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)+(0.0665P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4975
_refine_ls_number_parameters     334
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1254
_refine_ls_R_factor_gt           0.0633
_refine_ls_wR_factor_ref         0.1539
_refine_ls_wR_factor_gt          0.1288
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.015
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.85434(7) 0.69484(7) 0.24422(4) 0.0288(2) Uani 1 1 d . . . . .
O1 O 1.0677(3) 0.8624(4) 0.2768(2) 0.0497(9) Uani 1 1 d . . . . .
O2 O 1.0839(4) 0.6580(5) 0.2297(3) 0.0763(13) Uani 1 1 d . . . . .
O3 O 0.7804(4) 0.8619(4) 0.2833(3) 0.0552(10) Uani 1 1 d . . . . .
O4 O 0.5933(4) 0.6542(5) 0.2362(3) 0.0614(11) Uani 1 1 d . . . . .
N1 N 1.5861(5) 1.2110(5) 0.4472(3) 0.0541(12) Uani 1 1 d . . . . .
N2 N 1.5049(5) 1.2709(5) 0.4767(4) 0.0590(13) Uani 1 1 d . . . . .
N3 N 1.4423(7) 1.3369(6) 0.5073(5) 0.094(2) Uani 1 1 d . . . . .
C1 C 1.1420(6) 0.7871(7) 0.2648(4) 0.0468(13) Uani 1 1 d . . . . .
C2 C 1.3050(5) 0.8612(5) 0.2971(3) 0.0313(10) Uani 1 1 d . . . . .
C3 C 1.3642(5) 0.9995(5) 0.3555(3) 0.0349(11) Uani 1 1 d . . . . .
H3A H 1.3036 1.0466 0.3741 0.042 Uiso 1 1 calc R U . . .
C4 C 1.5137(5) 1.0683(5) 0.3864(3) 0.0356(11) Uani 1 1 d . . . . .
C5 C 1.6043(5) 0.9994(5) 0.3575(3) 0.0384(12) Uani 1 1 d . . . . .
H5A H 1.7048 1.0465 0.3773 0.046 Uiso 1 1 calc R U . . .
C6 C 1.5453(5) 0.8608(5) 0.2994(3) 0.0345(11) Uani 1 1 d . . . . .
C7 C 1.3950(5) 0.7911(5) 0.2698(3) 0.0367(11) Uani 1 1 d . . . . .
H7A H 1.3549 0.6971 0.2317 0.044 Uiso 1 1 calc R U . . .
C8 C 0.6454(7) 0.7852(7) 0.2705(4) 0.0467(13) Uani 1 1 d . . . . .
N4 N 0.8752(4) 0.6754(4) 0.4017(3) 0.0348(9) Uani 1 1 d . . . . .
N5 N 0.8310(4) 0.7143(4) 0.0868(3) 0.0392(10) Uani 1 1 d . . . . .
C9 C 0.8465(5) 0.5534(5) 0.4393(3) 0.0399(12) Uani 1 1 d . . . . .
H9A H 0.8150 0.4652 0.3942 0.048 Uiso 1 1 calc R U . . .
C10 C 0.8607(5) 0.5505(5) 0.5409(3) 0.0408(12) Uani 1 1 d . . . . .
H10A H 0.8388 0.4619 0.5625 0.049 Uiso 1 1 calc R U . . .
C11 C 0.9071(5) 0.6779(6) 0.6104(3) 0.0397(12) Uani 1 1 d . . . . .
C12 C 0.9375(6) 0.8034(6) 0.5724(4) 0.0552(15) Uani 1 1 d . . . . .
H12A H 0.9696 0.8929 0.6162 0.066 Uiso 1 1 calc R U . . .
C13 C 0.9206(6) 0.7981(5) 0.4694(3) 0.0493(14) Uani 1 1 d . . . . .
H13A H 0.9423 0.8855 0.4462 0.059 Uiso 1 1 calc R U . . .
C14 C 0.9197(6) 0.6804(6) 0.7218(3) 0.0533(15) Uani 1 1 d . . . . .
H14A H 1.0150 0.7526 0.7539 0.064 Uiso 1 1 calc R U . . .
H14B H 0.9123 0.5857 0.7344 0.064 Uiso 1 1 calc R U . . .
C15 C 0.8012(6) 0.7167(7) 0.7682(3) 0.0591(16) Uani 1 1 d . . . . .
H15A H 0.8096 0.8119 0.7561 0.071 Uiso 1 1 calc R U . . .
H15B H 0.7061 0.6454 0.7351 0.071 Uiso 1 1 calc R U . . .
C16 C 0.8100(6) 0.7179(6) 0.8789(3) 0.0456(13) Uani 1 1 d . . . . .
C17 C 0.6990(6) 0.6237(6) 0.9198(4) 0.0511(14) Uani 1 1 d . . . . .
H17A H 0.6138 0.5586 0.8783 0.077 Uiso 1 1 calc R U . . .
C18 C 0.7125(6) 0.6248(6) 0.0222(4) 0.0506(14) Uani 1 1 d . . . . .
H18A H 0.6348 0.5595 0.0476 0.076 Uiso 1 1 calc R U . . .
C19 C 0.9386(6) 0.8076(5) 0.0479(3) 0.0441(13) Uani 1 1 d . . . . .
H19A H 1.0226 0.8717 0.0910 0.066 Uiso 1 1 calc R U . . .
C20 C 0.9310(7) 0.8137(6) 0.9458(4) 0.0549(15) Uani 1 1 d . . . . .
H20A H 1.0080 0.8829 0.9223 0.082 Uiso 1 1 calc R U . . .
N4A N 0.7604(4) 0.4628(4) 0.1910(3) 0.0372(9) Uani 1 1 d . . . . .
C9A C 0.8176(6) 0.4034(6) 0.1197(4) 0.0508(14) Uani 1 1 d . . . . .
H9AA H 0.9071 0.4610 0.1023 0.061 Uiso 1 1 calc R U . . .
C10A C 0.7480(7) 0.2598(7) 0.0714(5) 0.0679(18) Uani 1 1 d . . . . .
H10B H 0.7881 0.2251 0.0191 0.081 Uiso 1 1 calc R U . . .
C11A C 0.6215(7) 0.1672(6) 0.0986(5) 0.0619(16) Uani 1 1 d . . . . .
C12A C 0.5627(7) 0.2295(6) 0.1722(4) 0.0566(15) Uani 1 1 d . . . . .
H12B H 0.4749 0.1726 0.1922 0.068 Uiso 1 1 calc R U . . .
C13A C 0.6329(5) 0.3733(5) 0.2154(3) 0.0423(12) Uani 1 1 d . . . . .
H13B H 0.5904 0.4117 0.2643 0.051 Uiso 1 1 calc R U . . .
C14A C 0.5455(8) 0.0083(6) 0.0472(4) 0.077(2) Uani 1 1 d . . . . .
H14C H 0.6185 -0.0306 0.0334 0.116 Uiso 1 1 calc R U . . .
H14D H 0.4850 -0.0474 0.0921 0.116 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 O3 2.105(3) . ?
Co1 O1 2.115(3) . ?
Co1 N4A 2.147(4) . ?
Co1 N5 2.168(4) . ?
Co1 N4 2.168(4) . ?
O1 C1 1.254(6) . ?
O2 C1 1.208(6) . ?
O3 C8 1.254(6) . ?
O4 C8 1.222(6) . ?
N1 N2 1.242(6) . ?
N1 C4 1.430(6) . ?
N2 N3 1.134(6) . ?
C1 C2 1.507(6) . ?
C2 C3 1.380(6) . ?
C2 C7 1.383(6) . ?
C3 C4 1.385(6) . ?
C3 H3A 0.9300 . ?
C4 C5 1.385(6) . ?
C5 C6 1.380(6) . ?
C5 H5A 0.9300 . ?
C6 C7 1.389(6) . ?
C6 C8 1.517(7) 1_655 ?
C7 H7A 0.9300 . ?
C8 C6 1.517(7) 1_455 ?
N4 C13 1.326(6) . ?
N4 C9 1.335(6) . ?
N5 C19 1.328(6) . ?
N5 C18 1.335(6) . ?
C9 C10 1.376(6) . ?
C9 H9A 0.9300 . ?
C10 C11 1.372(6) . ?
C10 H10A 0.9300 . ?
C11 C12 1.368(7) . ?
C11 C14 1.498(6) . ?
C12 C13 1.381(6) . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
C14 C15 1.520(7) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.490(6) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.367(7) . ?
C16 C20 1.380(7) . ?
C17 C18 1.379(6) 1_556 ?
C17 H17A 0.9300 . ?
C18 C17 1.379(6) 1_554 ?
C18 H18A 0.9300 . ?
C19 C20 1.389(6) 1_554 ?
C19 H19A 0.9300 . ?
C20 C19 1.389(6) 1_556 ?
C20 H20A 0.9300 . ?
N4A C9A 1.341(6) . ?
N4A C13A 1.345(6) . ?
C9A C10A 1.377(7) . ?
C9A H9AA 0.9300 . ?
C10A C11A 1.366(8) . ?
C10A H10B 0.9300 . ?
C11A C12A 1.387(8) . ?
C11A C14A 1.515(8) . ?
C12A C13A 1.361(7) . ?
C12A H12B 0.9300 . ?
C13A H13B 0.9300 . ?
C14A C14A 1.461(11) 2_655 ?
C14A H14C 0.9700 . ?
C14A H14D 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Co1 O1 86.02(15) . . ?
O3 Co1 N4A 137.72(15) . . ?
O1 Co1 N4A 136.23(15) . . ?
O3 Co1 N5 90.37(14) . . ?
O1 Co1 N5 93.36(14) . . ?
N4A Co1 N5 86.22(15) . . ?
O3 Co1 N4 89.17(14) . . ?
O1 Co1 N4 87.09(13) . . ?
N4A Co1 N4 93.80(14) . . ?
N5 Co1 N4 179.33(15) . . ?
C1 O1 Co1 100.0(4) . . ?
C8 O3 Co1 98.7(3) . . ?
N2 N1 C4 115.6(4) . . ?
N3 N2 N1 173.6(6) . . ?
O2 C1 O1 120.8(5) . . ?
O2 C1 C2 120.9(5) . . ?
O1 C1 C2 118.3(5) . . ?
C3 C2 C7 120.0(4) . . ?
C3 C2 C1 119.4(4) . . ?
C7 C2 C1 120.6(4) . . ?
C2 C3 C4 120.0(4) . . ?
C2 C3 H3A 120.0 . . ?
C4 C3 H3A 120.0 . . ?
C3 C4 C5 120.1(4) . . ?
C3 C4 N1 124.6(4) . . ?
C5 C4 N1 115.3(4) . . ?
C6 C5 C4 120.0(4) . . ?
C6 C5 H5A 120.0 . . ?
C4 C5 H5A 120.0 . . ?
C5 C6 C7 119.8(4) . . ?
C5 C6 C8 119.5(4) . 1_655 ?
C7 C6 C8 120.8(5) . 1_655 ?
C2 C7 C6 120.2(4) . . ?
C2 C7 H7A 119.9 . . ?
C6 C7 H7A 119.9 . . ?
O4 C8 O3 122.7(5) . . ?
O4 C8 C6 119.8(5) . 1_455 ?
O3 C8 C6 117.5(5) . 1_455 ?
C13 N4 C9 115.5(4) . . ?
C13 N4 Co1 117.0(3) . . ?
C9 N4 Co1 127.5(3) . . ?
C19 N5 C18 116.4(4) . . ?
C19 N5 Co1 121.8(3) . . ?
C18 N5 Co1 121.6(3) . . ?
N4 C9 C10 123.8(4) . . ?
N4 C9 H9A 118.1 . . ?
C10 C9 H9A 118.1 . . ?
C11 C10 C9 120.3(4) . . ?
C11 C10 H10A 119.9 . . ?
C9 C10 H10A 119.9 . . ?
C12 C11 C10 116.2(4) . . ?
C12 C11 C14 121.3(5) . . ?
C10 C11 C14 122.4(5) . . ?
C11 C12 C13 120.3(5) . . ?
C11 C12 H12A 119.8 . . ?
C13 C12 H12A 119.8 . . ?
N4 C13 C12 123.8(5) . . ?
N4 C13 H13A 118.1 . . ?
C12 C13 H13A 118.1 . . ?
C11 C14 C15 111.8(4) . . ?
C11 C14 H14A 109.2 . . ?
C15 C14 H14A 109.2 . . ?
C11 C14 H14B 109.2 . . ?
C15 C14 H14B 109.2 . . ?
H14A C14 H14B 107.9 . . ?
C16 C15 C14 112.9(4) . . ?
C16 C15 H15A 109.0 . . ?
C14 C15 H15A 109.0 . . ?
C16 C15 H15B 109.0 . . ?
C14 C15 H15B 109.0 . . ?
H15A C15 H15B 107.8 . . ?
C17 C16 C20 116.3(4) . . ?
C17 C16 C15 121.9(5) . . ?
C20 C16 C15 121.9(5) . . ?
C16 C17 C18 120.4(5) . 1_556 ?
C16 C17 H17A 119.8 . . ?
C18 C17 H17A 119.8 1_556 . ?
N5 C18 C17 123.6(5) . 1_554 ?
N5 C18 H18A 118.2 . . ?
C17 C18 H18A 118.2 1_554 . ?
N5 C19 C20 122.9(5) . 1_554 ?
N5 C19 H19A 118.6 . . ?
C20 C19 H19A 118.6 1_554 . ?
C16 C20 C19 120.4(5) . 1_556 ?
C16 C20 H20A 119.8 . . ?
C19 C20 H20A 119.8 1_556 . ?
C9A N4A C13A 116.4(4) . . ?
C9A N4A Co1 120.1(3) . . ?
C13A N4A Co1 122.9(3) . . ?
N4A C9A C10A 122.2(5) . . ?
N4A C9A H9AA 118.9 . . ?
C10A C9A H9AA 118.9 . . ?
C11A C10A C9A 121.5(5) . . ?
C11A C10A H10B 119.2 . . ?
C9A C10A H10B 119.2 . . ?
C10A C11A C12A 115.8(5) . . ?
C10A C11A C14A 122.0(6) . . ?
C12A C11A C14A 122.1(6) . . ?
C13A C12A C11A 120.4(5) . . ?
C13A C12A H12B 119.8 . . ?
C11A C12A H12B 119.8 . . ?
N4A C13A C12A 123.5(5) . . ?
N4A C13A H13B 118.3 . . ?
C12A C13A H13B 118.3 . . ?
C14A C14A C11A 111.5(6) 2_655 . ?
C14A C14A H14C 109.3 2_655 . ?
C11A C14A H14C 109.3 . . ?
C14A C14A H14D 109.3 2_655 . ?
C11A C14A H14D 109.3 . . ?
H14C C14A H14D 108.0 . . ?

_refine_diff_density_max         0.655
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.079

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_SA030417_0M
_database_code_depnum_ccdc_archive 'CCDC 1963356'
loop_
_audit_author_name
_audit_author_address
'Raju Mondal'
;Indian Association for the Cultivation of Science
India
;
_audit_update_record             
;
2019-11-04 deposited with the CCDC.	2021-03-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H15 N5 O4 Zn'
_chemical_formula_weight         454.74

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

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

_cell_length_a                   14.5651(8)
_cell_length_b                   15.7498(9)
_cell_length_c                   16.6824(9)
_cell_angle_alpha                90
_cell_angle_beta                 104.2180(14)
_cell_angle_gamma                90
_cell_volume                     3709.7(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    6286
_cell_measurement_theta_min      2.519
_cell_measurement_theta_max      29.879

_exptl_crystal_description       Needle
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.628
_exptl_crystal_F_000             1856
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_exptl_absorpt_coefficient_mu    1.365
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.77831
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
'SADABS v.2.03 (Bruker, 2001), wR2(int)=0.1054 before correction'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-2 CCD area detector'
_diffrn_measurement_method       '/w scans'
_diffrn_detector_area_resol_mean 8
_diffrn_reflns_number            28674
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_av_R_equivalents  0.0509
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.937
_diffrn_reflns_theta_max         30.555
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             5599
_reflns_number_gt                4041
_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 APEX-2'
_computing_cell_refinement       'Bruker APEX-2'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_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)+(0.0515P)²+9.5845P] 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         5599
_refine_ls_number_parameters     271
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0716
_refine_ls_R_factor_gt           0.0466
_refine_ls_wR_factor_ref         0.1226
_refine_ls_wR_factor_gt          0.1090
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.26116(2) 0.25354(2) 0.30870(2) 0.01758(9) Uani 1 1 d . . . . .
O1 O 0.24335(12) 0.29165(12) 0.19476(10) 0.0232(4) Uani 1 1 d . . . . .
O2 O 0.09450(14) 0.24668(13) 0.17656(12) 0.0305(4) Uani 1 1 d . . . . .
O3 O 0.38591(14) 0.26990(13) 0.38881(13) 0.0315(5) Uani 1 1 d . . . . .
O4 O 0.41182(15) 0.16846(16) 0.30651(12) 0.0396(5) Uani 1 1 d . . . . .
N1 N 0.25792(17) 0.39769(16) -0.09294(14) 0.0294(5) Uani 1 1 d . . . . .
N2 N 0.33547(18) 0.41693(16) -0.04750(15) 0.0300(5) Uani 1 1 d . . . . .
N3 N 0.4088(2) 0.4377(2) -0.0139(2) 0.0515(8) Uani 1 1 d . . . . .
C1 C 0.16013(18) 0.27506(16) 0.14998(15) 0.0199(5) Uani 1 1 d . . . . .
C2 C 0.14307(17) 0.29516(15) 0.05919(14) 0.0166(4) Uani 1 1 d . . . . .
C3 C 0.05577(17) 0.27538(16) 0.00662(15) 0.0179(4) Uani 1 1 d . . . . .
H3B H 0.0104 0.2469 0.0270 0.021 Uiso 1 1 calc R U . . .
C4 C 0.03613(17) 0.29820(15) -0.07646(15) 0.0187(5) Uani 1 1 d . . . . .
C5 C 0.10418(18) 0.33911(16) -0.10759(15) 0.0207(5) Uani 1 1 d . . . . .
H5A H 0.0910 0.3547 -0.1630 0.025 Uiso 1 1 calc R U . . .
C6 C 0.19203(17) 0.35670(16) -0.05544(15) 0.0192(5) Uani 1 1 d . . . . .
C7 C 0.21207(17) 0.33530(15) 0.02833(15) 0.0187(5) Uani 1 1 d . . . . .
H7A H 0.2709 0.3478 0.0630 0.022 Uiso 1 1 calc R U . . .
C8 C -0.06109(18) 0.28589(18) -0.13194(16) 0.0237(5) Uani 1 1 d . . . . .
N4 N 0.19274(16) 0.33991(14) 0.36844(14) 0.0232(4) Uani 1 1 d . . . . .
C9 C 0.2371(3) 0.3707(2) 0.44313(19) 0.0460(9) Uani 1 1 d . . . . .
H9A H 0.3005 0.3565 0.4642 0.055 Uiso 1 1 calc R U . . .
C10 C 0.1946(3) 0.4215(2) 0.4899(2) 0.0438(8) Uani 1 1 d . . . . .
H10A H 0.2294 0.4433 0.5399 0.053 Uiso 1 1 calc R U . . .
C11 C 0.0991(2) 0.44003(18) 0.46183(19) 0.0321(6) Uani 1 1 d . . . . .
C12 C 0.0548(2) 0.4108(2) 0.3860(2) 0.0453(9) Uani 1 1 d . . . . .
H12A H -0.0086 0.4238 0.3638 0.054 Uiso 1 1 calc R U . . .
C13 C 0.1040(2) 0.3611(2) 0.3408(2) 0.0468(9) Uani 1 1 d . . . . .
H13A H 0.0719 0.3424 0.2886 0.056 Uiso 1 1 calc R U . . .
C19 C 0.0510(2) 0.49065(19) 0.5181(2) 0.0339(7) Uani 1 1 d . . . . .
H19A H 0.0567 0.4592 0.5691 0.051 Uiso 1 1 calc R U . . .
H19B H 0.0845 0.5439 0.5321 0.051 Uiso 1 1 calc R U . . .
N4A N 0.19768(15) 0.13942(14) 0.31715(13) 0.0209(4) Uani 1 1 d . . . . .
C9A C 0.22591(19) 0.06883(17) 0.28508(17) 0.0249(5) Uani 1 1 d . . . . .
H9AA H 0.2807 0.0710 0.2660 0.030 Uiso 1 1 calc R U . . .
C10A C 0.1770(2) -0.00684(17) 0.27922(18) 0.0279(6) Uani 1 1 d . . . . .
H10B H 0.1993 -0.0543 0.2567 0.033 Uiso 1 1 calc R U . . .
C11A C 0.0949(2) -0.01247(17) 0.30662(17) 0.0261(6) Uani 1 1 d . . . . .
C12A C 0.0675(2) 0.06038(19) 0.34179(18) 0.0290(6) Uani 1 1 d . . . . .
H12B H 0.0148 0.0590 0.3638 0.035 Uiso 1 1 calc R U . . .
C13A C 0.1180(2) 0.13441(18) 0.34413(17) 0.0261(5) Uani 1 1 d . . . . .
H13B H 0.0962 0.1830 0.3652 0.031 Uiso 1 1 calc R U . . .
C19A C 0.0344(2) -0.09101(18) 0.2933(2) 0.0329(6) Uani 1 1 d . . . . .
H19C H -0.0014 -0.0940 0.3351 0.049 Uiso 1 1 calc R U . . .
H19D H 0.0748 -0.1408 0.2991 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
Zn1 O1 1.9489(17) . ?
Zn1 O3 1.990(2) . ?
Zn1 N4A 2.042(2) . ?
Zn1 N4 2.079(2) . ?
O1 C1 1.285(3) . ?
O2 C1 1.232(3) . ?
O3 C8 1.272(4) 8_556 ?
O4 C8 1.236(3) 8_556 ?
N1 N2 1.234(3) . ?
N1 C6 1.423(3) . ?
N2 N3 1.126(4) . ?
C1 C2 1.507(3) . ?
C2 C7 1.389(3) . ?
C2 C3 1.391(3) . ?
C3 C4 1.392(3) . ?
C3 H3B 0.9300 . ?
C4 C5 1.386(3) . ?
C4 C8 1.502(3) . ?
C5 C6 1.387(3) . ?
C5 H5A 0.9300 . ?
C6 C7 1.397(3) . ?
C7 H7A 0.9300 . ?
C8 O4 1.236(3) 8_455 ?
C8 O3 1.272(4) 8_455 ?
N4 C13 1.305(4) . ?
N4 C9 1.345(4) . ?
C9 C10 1.367(4) . ?
C9 H9A 0.9300 . ?
C10 C11 1.386(5) . ?
C10 H10A 0.9300 . ?
C11 C12 1.351(5) . ?
C11 C19 1.527(4) . ?
C12 C13 1.400(4) . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
C19 C19 1.488(6) 5_566 ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
N4A C9A 1.341(3) . ?
N4A C13A 1.347(3) . ?
C9A C10A 1.380(4) . ?
C9A H9AA 0.9300 . ?
C10A C11A 1.384(4) . ?
C10A H10B 0.9300 . ?
C11A C12A 1.391(4) . ?
C11A C19A 1.503(4) . ?
C12A C13A 1.374(4) . ?
C12A H12B 0.9300 . ?
C13A H13B 0.9300 . ?
C19A C19A 1.543(6) 2 ?
C19A H19C 0.9700 . ?
C19A H19D 0.9700 . ?

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 119.73(8) . . ?
O1 Zn1 N4A 112.60(8) . . ?
O3 Zn1 N4A 114.95(9) . . ?
O1 Zn1 N4 107.54(9) . . ?
O3 Zn1 N4 93.41(9) . . ?
N4A Zn1 N4 105.33(9) . . ?
C1 O1 Zn1 112.65(16) . . ?
C8 O3 Zn1 104.05(17) 8_556 . ?
N2 N1 C6 117.1(2) . . ?
N3 N2 N1 172.1(3) . . ?
O2 C1 O1 124.7(2) . . ?
O2 C1 C2 119.1(2) . . ?
O1 C1 C2 116.2(2) . . ?
C7 C2 C3 120.1(2) . . ?
C7 C2 C1 120.8(2) . . ?
C3 C2 C1 119.1(2) . . ?
C2 C3 C4 120.2(2) . . ?
C2 C3 H3B 119.9 . . ?
C4 C3 H3B 119.9 . . ?
C5 C4 C3 120.2(2) . . ?
C5 C4 C8 118.8(2) . . ?
C3 C4 C8 120.8(2) . . ?
C4 C5 C6 119.5(2) . . ?
C4 C5 H5A 120.3 . . ?
C6 C5 H5A 120.3 . . ?
C5 C6 C7 120.9(2) . . ?
C5 C6 N1 115.6(2) . . ?
C7 C6 N1 123.5(2) . . ?
C2 C7 C6 119.2(2) . . ?
C2 C7 H7A 120.4 . . ?
C6 C7 H7A 120.4 . . ?
O4 C8 O3 122.4(2) 8_455 8_455 ?
O4 C8 C4 119.8(3) 8_455 . ?
O3 C8 C4 117.7(2) 8_455 . ?
C13 N4 C9 116.4(3) . . ?
C13 N4 Zn1 123.25(19) . . ?
C9 N4 Zn1 120.10(19) . . ?
N4 C9 C10 123.9(3) . . ?
N4 C9 H9A 118.1 . . ?
C10 C9 H9A 118.1 . . ?
C9 C10 C11 119.3(3) . . ?
C9 C10 H10A 120.4 . . ?
C11 C10 H10A 120.4 . . ?
C12 C11 C10 116.9(3) . . ?
C12 C11 C19 124.6(3) . . ?
C10 C11 C19 118.5(3) . . ?
C11 C12 C13 120.3(3) . . ?
C11 C12 H12A 119.8 . . ?
C13 C12 H12A 119.8 . . ?
N4 C13 C12 123.2(3) . . ?
N4 C13 H13A 118.4 . . ?
C12 C13 H13A 118.4 . . ?
C19 C19 C11 114.6(3) 5_566 . ?
C19 C19 H19A 108.6 5_566 . ?
C11 C19 H19A 108.6 . . ?
C19 C19 H19B 108.6 5_566 . ?
C11 C19 H19B 108.6 . . ?
H19A C19 H19B 107.6 . . ?
C9A N4A C13A 117.3(2) . . ?
C9A N4A Zn1 120.91(18) . . ?
C13A N4A Zn1 121.12(18) . . ?
N4A C9A C10A 122.7(2) . . ?
N4A C9A H9AA 118.6 . . ?
C10A C9A H9AA 118.6 . . ?
C9A C10A C11A 120.3(3) . . ?
C9A C10A H10B 119.8 . . ?
C11A C10A H10B 119.8 . . ?
C10A C11A C12A 116.5(3) . . ?
C10A C11A C19A 121.7(3) . . ?
C12A C11A C19A 121.6(3) . . ?
C13A C12A C11A 120.4(3) . . ?
C13A C12A H12B 119.8 . . ?
C11A C12A H12B 119.8 . . ?
N4A C13A C12A 122.6(3) . . ?
N4A C13A H13B 118.7 . . ?
C12A C13A H13B 118.7 . . ?
C11A C19A C19A 111.2(2) . 2 ?
C11A C19A H19C 109.4 . . ?
C19A C19A H19C 109.4 2 . ?
C11A C19A H19D 109.4 . . ?
C19A C19A H19D 109.4 2 . ?
H19C C19A H19D 108.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Zn1 O1 C1 O2 7.4(3) . . . . ?
Zn1 O1 C1 C2 -174.63(16) . . . . ?
O2 C1 C2 C7 173.3(2) . . . . ?
O1 C1 C2 C7 -4.8(3) . . . . ?
O2 C1 C2 C3 -4.7(4) . . . . ?
O1 C1 C2 C3 177.3(2) . . . . ?
C7 C2 C3 C4 -2.1(4) . . . . ?
C1 C2 C3 C4 175.9(2) . . . . ?
C2 C3 C4 C5 1.4(4) . . . . ?
C2 C3 C4 C8 -173.3(2) . . . . ?
C3 C4 C5 C6 0.3(4) . . . . ?
C8 C4 C5 C6 175.1(2) . . . . ?
C4 C5 C6 C7 -1.3(4) . . . . ?
C4 C5 C6 N1 179.1(2) . . . . ?
N2 N1 C6 C5 177.4(2) . . . . ?
N2 N1 C6 C7 -2.1(4) . . . . ?
C3 C2 C7 C6 1.1(3) . . . . ?
C1 C2 C7 C6 -176.9(2) . . . . ?
C5 C6 C7 C2 0.6(4) . . . . ?
N1 C6 C7 C2 -179.9(2) . . . . ?
C5 C4 C8 O4 -21.0(4) . . . 8_455 ?
C3 C4 C8 O4 153.7(3) . . . 8_455 ?
C5 C4 C8 O3 161.7(2) . . . 8_455 ?
C3 C4 C8 O3 -23.5(4) . . . 8_455 ?
C13 N4 C9 C10 0.1(6) . . . . ?
Zn1 N4 C9 C10 -173.9(3) . . . . ?
N4 C9 C10 C11 3.2(6) . . . . ?
C9 C10 C11 C12 -4.4(5) . . . . ?
C9 C10 C11 C19 174.9(3) . . . . ?
C10 C11 C12 C13 2.7(5) . . . . ?
C19 C11 C12 C13 -176.6(3) . . . . ?
C9 N4 C13 C12 -2.0(6) . . . . ?
Zn1 N4 C13 C12 171.7(3) . . . . ?
C11 C12 C13 N4 0.6(6) . . . . ?
C12 C11 C19 C19 -2.2(5) . . . 5_566 ?
C10 C11 C19 C19 178.5(3) . . . 5_566 ?
C13A N4A C9A C10A -0.1(4) . . . . ?
Zn1 N4A C9A C10A -170.8(2) . . . . ?
N4A C9A C10A C11A 0.3(4) . . . . ?
C9A C10A C11A C12A -1.9(4) . . . . ?
C9A C10A C11A C19A 173.6(3) . . . . ?
C10A C11A C12A C13A 3.5(4) . . . . ?
C19A C11A C12A C13A -172.1(3) . . . . ?
C9A N4A C13A C12A 1.7(4) . . . . ?
Zn1 N4A C13A C12A 172.4(2) . . . . ?
C11A C12A C13A N4A -3.5(4) . . . . ?
C10A C11A C19A C19A -84.0(4) . . . 2 ?
C12A C11A C19A C19A 91.3(4) . . . 2 ?

_refine_diff_density_max         1.309
_refine_diff_density_min         -0.677
_refine_diff_density_rms         0.098

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_MR190417_1_0m
_database_code_depnum_ccdc_archive 'CCDC 1963355'
loop_
_audit_author_name
_audit_author_address
'Raju Mondal'
;Indian Association for the Cultivation of Science
India
;
_audit_update_record             
;
2021-02-10 deposited with the CCDC.	2021-03-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H21 N5 O6 Zn'
_chemical_formula_weight         504.80

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/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                   7.8286(3)
_cell_length_b                   17.0971(7)
_cell_length_c                   16.1032(7)
_cell_angle_alpha                90
_cell_angle_beta                 95.5120(10)
_cell_angle_gamma                90
_cell_volume                     2145.39(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9439
_cell_measurement_theta_min      2.382
_cell_measurement_theta_max      27.132

_exptl_crystal_description       Block
_exptl_crystal_colour            Brown
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_F_000             1040
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.24
_exptl_absorpt_coefficient_mu    1.195
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.73139
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
'SADABS v.2.03 (Bruker, 2001), wR2(int)=0.0963 before correction'

_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-2 CCD area detector'
_diffrn_measurement_method       '/w scans'
_diffrn_detector_area_resol_mean 8
_diffrn_reflns_number            28153
_diffrn_reflns_av_unetI/netI     0.0197
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.382
_diffrn_reflns_theta_max         26.998
_diffrn_reflns_theta_full        25.242
_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             4649
_reflns_number_gt                3854
_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 APEX-2'
_computing_cell_refinement       'Bruker APEX-2'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_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)+(0.0757P)²+1.4301P] 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         4649
_refine_ls_number_parameters     302
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0427
_refine_ls_wR_factor_ref         0.1272
_refine_ls_wR_factor_gt          0.1214
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.054
_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 0.63875(4) 0.15324(2) 0.28912(2) 0.03977(13) Uani 1 1 d . . . . .
O1 O 0.5466(3) 0.22827(15) 0.36545(12) 0.0574(6) Uani 1 1 d . . . . .
O2 O 0.7750(3) 0.19161(14) 0.44534(15) 0.0655(6) Uani 1 1 d . . . . .
O3 O 0.4796(3) 0.15296(11) 0.18899(12) 0.0484(5) Uani 1 1 d . . . . .
O4 O 0.3051(3) 0.07176(16) 0.24525(15) 0.0721(7) Uani 1 1 d . . . . .
N1 N 0.2839(4) 0.4430(2) 0.5390(2) 0.0840(11) Uani 1 1 d . . . . .
N2 N 0.1743(4) 0.4305(3) 0.4807(2) 0.0926(12) Uani 1 1 d . . . . .
N3 N 0.0643(6) 0.4255(4) 0.4310(3) 0.138(2) Uani 1 1 d . . . . .
C1 C 0.6509(4) 0.23506(18) 0.43085(17) 0.0456(6) Uani 1 1 d . . . . .
C2 C 0.6190(3) 0.29967(16) 0.49017(15) 0.0396(5) Uani 1 1 d . . . . .
C3 C 0.4659(4) 0.34030(19) 0.48260(17) 0.0487(7) Uani 1 1 d . . . . .
H3 H 0.382569 0.329358 0.439019 0.058 Uiso 1 1 calc R U . . .
C4 C 0.4376(4) 0.3978(2) 0.54081(18) 0.0534(7) Uani 1 1 d . . . . .
C5 C 0.5589(4) 0.41252(18) 0.60680(18) 0.0494(7) Uani 1 1 d . . . . .
H5 H 0.537458 0.450040 0.646303 0.059 Uiso 1 1 calc R U . . .
C6 C 0.7125(3) 0.37173(15) 0.61455(15) 0.0383(5) Uani 1 1 d . . . . .
C7 C 0.7420(3) 0.31582(15) 0.55582(15) 0.0378(5) Uani 1 1 d . . . . .
H7 H 0.845358 0.288651 0.560284 0.045 Uiso 1 1 calc R U . . .
C8 C 0.3401(4) 0.11488(16) 0.18862(16) 0.0432(6) Uani 1 1 d . . . . .
N4 N 0.7451(3) 0.04598(12) 0.30648(13) 0.0401(5) Uani 1 1 d . . . . .
N5 N 0.8422(3) 0.21355(14) 0.24741(14) 0.0429(5) Uani 1 1 d . . . . .
C9 C 0.8547(4) 0.02815(19) 0.37193(19) 0.0567(8) Uani 1 1 d . . . . .
H9 H 0.857184 0.059302 0.419377 0.068 Uiso 1 1 calc R U . . .
C10 C 0.9649(5) -0.0348(2) 0.3721(2) 0.0670(9) Uani 1 1 d . . . . .
H10 H 1.039858 -0.045195 0.419211 0.080 Uiso 1 1 calc R U . . .
C11 C 0.9648(4) -0.08189(16) 0.3040(2) 0.0539(7) Uani 1 1 d . . . . .
C12 C 0.8463(4) -0.06499(18) 0.2375(2) 0.0543(7) Uani 1 1 d . . . . .
H12 H 0.838631 -0.096627 0.190291 0.065 Uiso 1 1 calc R U . . .
C13 C 0.7394(4) -0.00140(17) 0.24075(18) 0.0505(6) Uani 1 1 d . . . . .
H13 H 0.660080 0.008836 0.195274 0.061 Uiso 1 1 calc R U . . .
C14 C 0.9938(4) 0.2160(2) 0.2930(2) 0.0595(8) Uani 1 1 d . . . . .
H14 H 1.011944 0.182123 0.338209 0.071 Uiso 1 1 calc R U . . .
C15 C 1.1239(4) 0.2656(2) 0.2771(2) 0.0604(8) Uani 1 1 d . . . . .
H15 H 1.227633 0.264670 0.310457 0.073 Uiso 1 1 calc R U . . .
C16 C 1.0990(4) 0.31735(19) 0.2103(2) 0.0552(7) Uani 1 1 d . . . . .
C17 C 0.9463(4) 0.3106(2) 0.1606(2) 0.0606(8) Uani 1 1 d . . . . .
H17 H 0.926723 0.341599 0.113119 0.073 Uiso 1 1 calc R U . . .
C18 C 0.8234(4) 0.25905(18) 0.18018(18) 0.0496(6) Uani 1 1 d . . . . .
H18 H 0.722270 0.255552 0.145051 0.059 Uiso 1 1 calc R U . . .
C19 C 1.0912(5) -0.14731(19) 0.3003(3) 0.0773(12) Uani 1 1 d . . . . .
H19A H 1.075315 -0.183940 0.344922 0.093 Uiso 1 1 calc R U . . .
H19B H 1.066583 -0.174843 0.247867 0.093 Uiso 1 1 calc R U . . .
C20 C 1.2699(5) -0.1225(2) 0.3075(4) 0.0869(14) Uani 1 1 d . . . . .
H20A H 1.298797 -0.103126 0.363746 0.130 Uiso 1 1 calc R U . . .
H20B H 1.279990 -0.078830 0.269794 0.130 Uiso 1 1 calc R U . . .
O1S O 0.2965(7) 0.0888(4) 0.4228(3) 0.1487(18) Uani 1 1 d D . . . .
H1S H 0.293676 0.096099 0.372371 0.223 Uiso 1 1 calc DR U . . .
C1S C 0.4247(14) 0.0524(10) 0.4466(16) 0.408(17) Uani 1 1 d D . . . .
H1S1 H 0.402418 -0.002574 0.439752 0.612 Uiso 1 1 d DR U . . .
H1S2 H 0.449957 0.064075 0.504746 0.612 Uiso 1 1 d DR U . . .
H1S3 H 0.520885 0.066582 0.416998 0.612 Uiso 1 1 d DR U . . .
O1W' O 0.1272(10) 0.2162(5) 0.5027(5) 0.0531(17) Uiso 0.3 1 d . . P A 1
O1W O 0.1491(13) 0.1836(5) 0.4966(5) 0.270(8) Uani 0.7 1 d D . P B 2
H1WA H 0.192500 0.152600 0.464800 0.406 Uiso 1 1 d D U . . .
H1WB H 0.006100 0.198300 0.481000 0.406 Uiso 1 1 d . U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O3 1.9409(19) . ?
Zn1 O1 1.961(2) . ?
Zn1 N4 2.022(2) . ?
Zn1 N5 2.063(2) . ?
O1 C1 1.274(3) . ?
O2 C1 1.227(4) . ?
O3 C8 1.271(3) . ?
O4 C8 1.224(3) . ?
N1 N2 1.229(5) . ?
N1 C4 1.428(4) . ?
N2 N3 1.121(5) . ?
C1 C2 1.497(4) . ?
C2 C3 1.381(4) . ?
C2 C7 1.387(3) . ?
C3 C4 1.390(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.379(4) . ?
C5 C6 1.386(4) . ?
C5 H5 0.9300 . ?
C6 C7 1.379(4) . ?
C6 C8 1.498(3) 4_666 ?
C7 H7 0.9300 . ?
N4 C9 1.329(3) . ?
N4 C13 1.330(4) . ?
N5 C18 1.330(4) . ?
N5 C14 1.335(4) . ?
C9 C10 1.380(4) . ?
C9 H9 0.9300 . ?
C10 C11 1.360(5) . ?
C10 H10 0.9300 . ?
C11 C12 1.379(5) . ?
C11 C19 1.498(4) . ?
C12 C13 1.376(4) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 C15 1.368(5) . ?
C14 H14 0.9300 . ?
C15 C16 1.393(5) . ?
C15 H15 0.9300 . ?
C16 C17 1.378(5) . ?
C16 C20 1.500(5) 2_755 ?
C17 C18 1.364(4) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C19 C20 1.456(5) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
O1S C1S 1.211(15) . ?
O1S H1S 0.8200 . ?
C1S H1S1 0.9600 . ?
C1S H1S2 0.9600 . ?
C1S H1S3 0.9600 . ?
O1W' H1WA 1.3703 . ?
O1W' H1WB 1.0253 . ?
O1W H1WA 0.8322 . ?
O1W H1WB 1.1512 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Zn1 O1 106.08(9) . . ?
O3 Zn1 N4 109.60(8) . . ?
O1 Zn1 N4 132.67(9) . . ?
O3 Zn1 N5 100.66(9) . . ?
O1 Zn1 N5 102.65(10) . . ?
N4 Zn1 N5 100.24(9) . . ?
C1 O1 Zn1 109.43(18) . . ?
C8 O3 Zn1 119.20(18) . . ?
N2 N1 C4 116.5(3) . . ?
N3 N2 N1 172.4(4) . . ?
O2 C1 O1 122.3(3) . . ?
O2 C1 C2 120.2(2) . . ?
O1 C1 C2 117.5(3) . . ?
C3 C2 C7 120.0(2) . . ?
C3 C2 C1 120.8(2) . . ?
C7 C2 C1 119.1(2) . . ?
C2 C3 C4 119.3(3) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C5 C4 C3 120.4(3) . . ?
C5 C4 N1 115.7(3) . . ?
C3 C4 N1 123.9(3) . . ?
C4 C5 C6 120.3(3) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C7 C6 C5 119.2(2) . . ?
C7 C6 C8 120.6(2) . 4_666 ?
C5 C6 C8 120.1(2) . 4_666 ?
C6 C7 C2 120.7(2) . . ?
C6 C7 H7 119.6 . . ?
C2 C7 H7 119.6 . . ?
O4 C8 O3 124.0(3) . . ?
O4 C8 C6 120.3(3) . 4_565 ?
O3 C8 C6 115.6(2) . 4_565 ?
C9 N4 C13 117.5(2) . . ?
C9 N4 Zn1 122.92(19) . . ?
C13 N4 Zn1 117.42(18) . . ?
C18 N5 C14 116.9(3) . . ?
C18 N5 Zn1 121.93(19) . . ?
C14 N5 Zn1 120.6(2) . . ?
N4 C9 C10 122.5(3) . . ?
N4 C9 H9 118.8 . . ?
C10 C9 H9 118.8 . . ?
C11 C10 C9 120.5(3) . . ?
C11 C10 H10 119.7 . . ?
C9 C10 H10 119.7 . . ?
C10 C11 C12 116.8(3) . . ?
C10 C11 C19 121.6(3) . . ?
C12 C11 C19 121.5(3) . . ?
C13 C12 C11 120.1(3) . . ?
C13 C12 H12 119.9 . . ?
C11 C12 H12 119.9 . . ?
N4 C13 C12 122.5(3) . . ?
N4 C13 H13 118.7 . . ?
C12 C13 H13 118.7 . . ?
N5 C14 C15 123.7(3) . . ?
N5 C14 H14 118.2 . . ?
C15 C14 H14 118.2 . . ?
C14 C15 C16 119.2(3) . . ?
C14 C15 H15 120.4 . . ?
C16 C15 H15 120.4 . . ?
C17 C16 C15 116.4(3) . . ?
C17 C16 C20 121.2(3) . 2_755 ?
C15 C16 C20 122.4(3) . 2_755 ?
C18 C17 C16 120.7(3) . . ?
C18 C17 H17 119.6 . . ?
C16 C17 H17 119.6 . . ?
N5 C18 C17 122.8(3) . . ?
N5 C18 H18 118.6 . . ?
C17 C18 H18 118.6 . . ?
C20 C19 C11 114.3(3) . . ?
C20 C19 H19A 108.7 . . ?
C11 C19 H19A 108.7 . . ?
C20 C19 H19B 108.7 . . ?
C11 C19 H19B 108.7 . . ?
H19A C19 H19B 107.6 . . ?
C19 C20 C16 117.0(3) . 2_745 ?
C19 C20 H20A 108.0 . . ?
C16 C20 H20A 108.0 2_745 . ?
C19 C20 H20B 108.0 . . ?
C16 C20 H20B 108.0 2_745 . ?
H20A C20 H20B 107.3 . . ?
C1S O1S H1S 109.5 . . ?
O1S C1S H1S1 109.4 . . ?
O1S C1S H1S2 106.7 . . ?
H1S1 C1S H1S2 109.5 . . ?
O1S C1S H1S3 112.3 . . ?
H1S1 C1S H1S3 109.5 . . ?
H1S2 C1S H1S3 109.5 . . ?
H1WA O1W' H1WB 89.0 . . ?
H1WA O1W H1WB 116.8 . . ?

_refine_diff_density_max         0.675
_refine_diff_density_min         -0.888
_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_test_a
_database_code_depnum_ccdc_archive 'CCDC 1963354'
loop_
_audit_author_name
_audit_author_address
'Raju Mondal'
;Indian Association for the Cultivation of Science
India
;
_audit_update_record             
;
2021-02-10 deposited with the CCDC.	2021-03-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C55 H48 Mn2 N13 O10'
_chemical_formula_weight         1160.94

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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   27.0143(15)
_cell_length_b                   10.0527(6)
_cell_length_c                   20.5229(12)
_cell_angle_alpha                90
_cell_angle_beta                 111.043(2)
_cell_angle_gamma                90
_cell_volume                     5201.7(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    16221
_cell_measurement_theta_min      2.296
_cell_measurement_theta_max      32.577

_exptl_crystal_description       Block
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_F_000             2396
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.22
_exptl_absorpt_coefficient_mu    0.560
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.69626
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
'SADABS v.2.03 (Bruker, 2001), wR2(int)=0.1366 before correction'

_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-2 CCD area detector'
_diffrn_measurement_method       '/w scans'
_diffrn_detector_area_resol_mean 8
_diffrn_reflns_number            57048
_diffrn_reflns_av_unetI/netI     0.0580
_diffrn_reflns_av_R_equivalents  0.0777
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.181
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.404
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.404
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.404
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             10146
_reflns_number_gt                7626
_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 APEX-2'
_computing_cell_refinement       'Bruker APEX-2'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0881P)²+38.6114P] 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         10146
_refine_ls_number_parameters     733
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.1095
_refine_ls_R_factor_gt           0.0840
_refine_ls_wR_factor_ref         0.2316
_refine_ls_wR_factor_gt          0.2198
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_restrained_S_all      1.003
_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
Mn01 Mn -0.09027(2) 0.94993(6) 0.27822(3) 0.01517(17) Uani 1 1 d . . . . .
Mn02 Mn 0.41127(2) 1.08390(6) 0.77818(3) 0.01764(18) Uani 1 1 d . . . . .
O1 O -0.10209(12) 0.7934(3) 0.34179(16) 0.0248(7) Uani 1 1 d . . . . .
O2 O -0.08759(13) 0.6792(3) 0.25786(17) 0.0282(7) Uani 1 1 d . . . . .
O3 O -0.11702(13) 0.0842(3) 0.35199(17) 0.0269(7) Uani 1 1 d . . . . .
O4 O -0.09443(12) 0.1752(3) 0.26975(16) 0.0245(7) Uani 1 1 d . . . . .
N1 N -0.17360(18) 0.4837(4) 0.4704(2) 0.0348(10) Uani 1 1 d . . . . .
N2 N -0.1854(2) 0.3873(5) 0.4979(3) 0.0433(12) Uani 1 1 d . . . . .
N3 N -0.1971(3) 0.3096(5) 0.5293(3) 0.074(2) Uani 1 1 d . . . . .
C1 C -0.09966(16) 0.6852(4) 0.3111(2) 0.0193(8) Uani 1 1 d . . . . .
C2 C -0.11366(15) 0.5589(4) 0.3400(2) 0.0164(8) Uani 1 1 d . . . . .
C3 C -0.10607(16) 0.4341(4) 0.3160(2) 0.0165(8) Uani 1 1 d . . . . .
H3 H -0.091637 0.426469 0.280229 0.020 Uiso 1 1 calc R U . . .
C4 C -0.11965(16) 0.3202(4) 0.3445(2) 0.0179(8) Uani 1 1 d . . . . .
C5 C -0.14177(16) 0.3322(4) 0.3962(2) 0.0208(9) Uani 1 1 d . . . . .
H5 H -0.150961 0.254570 0.415736 0.025 Uiso 1 1 calc R U . . .
C6 C -0.15034(18) 0.4567(4) 0.4191(2) 0.0231(9) Uani 1 1 d . . . . .
C7 C -0.13541(17) 0.5703(4) 0.3918(2) 0.0202(9) Uani 1 1 d . . . . .
H7 H -0.140093 0.655638 0.408584 0.024 Uiso 1 1 calc R U . . .
C8 C -0.10987(16) 0.1855(4) 0.3200(2) 0.0207(9) Uani 1 1 d . . . . .
O1A O 0.39075(14) 0.9305(3) 0.8399(2) 0.0349(8) Uani 1 1 d . . . . .
O2A O 0.40568(16) 0.8218(4) 0.7556(2) 0.0508(11) Uani 1 1 d . . . . .
O3A O 0.41490(12) 0.3202(3) 0.77138(15) 0.0236(7) Uani 1 1 d . . . . .
O4A O 0.39691(12) 0.2221(3) 0.85640(16) 0.0244(7) Uani 1 1 d . . . . .
N1A N 0.33321(16) 0.5995(4) 0.9761(2) 0.0311(9) Uani 1 1 d . . . . .
N2A N 0.32745(17) 0.4960(5) 1.0050(2) 0.0345(10) Uani 1 1 d . . . . .
N3A N 0.3206(2) 0.4065(6) 1.0348(3) 0.0535(14) Uani 1 1 d . . . . .
C1A C 0.39449(17) 0.8244(4) 0.8098(3) 0.0259(10) Uani 1 1 d . . . . .
C2A C 0.38442(16) 0.6968(4) 0.8404(2) 0.0192(8) Uani 1 1 d . . . . .
C3A C 0.36356(16) 0.7001(4) 0.8929(2) 0.0197(8) Uani 1 1 d . . . . .
H3A H 0.354993 0.783056 0.908313 0.024 Uiso 1 1 calc R U . . .
C4A C 0.35505(16) 0.5830(4) 0.9231(2) 0.0200(9) Uani 1 1 d . . . . .
C5A C 0.36757(16) 0.4611(4) 0.9009(2) 0.0182(8) Uani 1 1 d . . . . .
H5A H 0.362215 0.380783 0.921874 0.022 Uiso 1 1 calc R U . . .
C6A C 0.38802(15) 0.4580(4) 0.8476(2) 0.0154(8) Uani 1 1 d . . . . .
C7A C 0.39598(15) 0.5750(4) 0.8170(2) 0.0155(8) Uani 1 1 d . . . . .
H7A H 0.409310 0.572024 0.779991 0.019 Uiso 1 1 calc R U . . .
C8A C 0.40117(15) 0.3253(4) 0.8236(2) 0.0192(9) Uani 1 1 d . . . . .
N4 N -0.00346(13) 0.9585(3) 0.35119(17) 0.0176(7) Uani 1 1 d . . . . .
N5 N 0.32619(14) 1.1038(4) 0.70160(19) 0.0233(8) Uani 1 1 d . . . . .
C9 C 0.01064(18) 0.9316(4) 0.4197(2) 0.0244(9) Uani 1 1 d . . . . .
H9 H -0.016085 0.902688 0.436487 0.029 Uiso 1 1 calc R U . . .
C10 C 0.06182(19) 0.9437(5) 0.4669(2) 0.0266(10) Uani 1 1 d . . . . .
H10 H 0.069587 0.923678 0.514768 0.032 Uiso 1 1 calc R U . . .
C11 C 0.10238(17) 0.9855(4) 0.4440(2) 0.0239(9) Uani 1 1 d . . . . .
C12 C 0.08819(18) 1.0124(5) 0.3739(2) 0.0254(9) Uani 1 1 d . . . . .
H12 H 0.114296 1.039482 0.355602 0.030 Uiso 1 1 calc R U . . .
C13 C 0.03614(17) 0.9999(4) 0.3304(2) 0.0247(9) Uani 1 1 d . . . . .
H13 H 0.027407 1.021793 0.282568 0.030 Uiso 1 1 calc R U . . .
C14 C 0.15886(18) 0.9967(5) 0.4933(2) 0.0273(10) Uani 1 1 d . . . . .
H14A H 0.181936 1.011599 0.465812 0.033 Uiso 1 1 calc R U . . .
H14B H 0.169589 0.911507 0.518605 0.033 Uiso 1 1 calc R U . . .
C15 C 0.16776(17) 1.1091(5) 0.5463(2) 0.0258(10) Uani 1 1 d . . . . .
H15A H 0.161196 1.195369 0.521381 0.031 Uiso 1 1 calc R U . . .
H15B H 0.141820 1.100279 0.570022 0.031 Uiso 1 1 calc R U . . .
C16 C 0.22292(17) 1.1093(5) 0.6004(2) 0.0244(9) Uani 1 1 d . . . . .
C17 C 0.25246(19) 1.2247(5) 0.6219(3) 0.0323(11) Uani 1 1 d . . . . .
H17 H 0.237934 1.308096 0.602657 0.039 Uiso 1 1 calc R U . . .
C18 C 0.30277(19) 1.2180(5) 0.6712(3) 0.0341(11) Uani 1 1 d . . . . .
H18 H 0.322238 1.298392 0.684649 0.041 Uiso 1 1 calc R U . . .
C19 C 0.2975(2) 0.9944(5) 0.6810(3) 0.0483(16) Uani 1 1 d . . . . .
H19 H 0.313071 0.912050 0.700674 0.058 Uiso 1 1 calc R U . . .
C20 C 0.2466(2) 0.9924(6) 0.6330(3) 0.0465(15) Uani 1 1 d . . . . .
H20 H 0.227626 0.910881 0.622107 0.056 Uiso 1 1 calc R U . . .
N4A N 0.49784(14) 1.0682(3) 0.84919(18) 0.0204(7) Uani 1 1 d . . . . .
N5A N 0.82663(14) 0.9248(4) 1.19611(19) 0.0229(8) Uani 1 1 d . . . . .
C9A C 0.53786(19) 1.0408(6) 0.8268(2) 0.0322(11) Uani 1 1 d . . . . .
H9A H 0.529578 1.030265 0.778052 0.039 Uiso 1 1 calc R U . . .
C10A C 0.58994(18) 1.0272(5) 0.8701(2) 0.0306(11) Uani 1 1 d . . . . .
H10A H 0.616441 1.009119 0.850889 0.037 Uiso 1 1 calc R U . . .
C11A C 0.60383(17) 1.0399(4) 0.9421(2) 0.0210(9) Uani 1 1 d . . . . .
C12A C 0.56245(17) 1.0661(4) 0.9656(2) 0.0226(9) Uani 1 1 d . . . . .
H12A H 0.569519 1.075302 1.014148 0.027 Uiso 1 1 calc R U . . .
C13A C 0.51138(17) 1.0786(4) 0.9187(2) 0.0194(8) Uani 1 1 d . . . . .
H13A H 0.484054 1.095704 0.936544 0.023 Uiso 1 1 calc R U . . .
C14A C 0.66045(17) 1.0250(4) 0.9902(2) 0.0226(9) Uani 1 1 d . . . . .
H14C H 0.672460 1.109105 1.016166 0.027 Uiso 1 1 calc R U . . .
H14D H 0.682957 1.008181 0.962207 0.027 Uiso 1 1 calc R U . . .
C15A C 0.66774(18) 0.9103(5) 1.0428(3) 0.0292(10) Uani 1 1 d . . . . .
H15C H 0.641859 0.920104 1.066486 0.035 Uiso 1 1 calc R U . . .
H15D H 0.660824 0.824349 1.017527 0.035 Uiso 1 1 calc R U . . .
C16A C 0.72298(17) 0.9104(4) 1.0961(2) 0.0251(9) Uani 1 1 d . . . . .
C17A C 0.76645(19) 0.8668(5) 1.0822(3) 0.0325(11) Uani 1 1 d . . . . .
H17A H 0.761703 0.830902 1.037576 0.039 Uiso 1 1 calc R U . . .
C18A C 0.81671(19) 0.8742(5) 1.1320(2) 0.0300(10) Uani 1 1 d . . . . .
H18A H 0.845645 0.842225 1.120466 0.036 Uiso 1 1 calc R U . . .
C19A C 0.78440(19) 0.9654(5) 1.2099(3) 0.0326(11) Uani 1 1 d . . . . .
H19A H 0.790216 1.000254 1.255034 0.039 Uiso 1 1 calc R U . . .
C20A C 0.73302(19) 0.9602(5) 1.1632(3) 0.0349(11) Uani 1 1 d . . . . .
H20A H 0.704642 0.990114 1.176498 0.042 Uiso 1 1 calc R U . . .
N4B N -0.06014(14) 0.9544(3) 0.18791(17) 0.0185(7) Uani 1 1 d . . . . .
C9B C -0.06192(19) 1.0610(5) 0.1490(2) 0.0260(10) Uani 1 1 d . . . . .
H9B H -0.075900 1.141313 0.159743 0.031 Uiso 1 1 calc R U . . .
C10B C -0.0442(2) 1.0606(5) 0.0932(2) 0.0292(10) Uani 1 1 d . . . . .
H10B H -0.046069 1.139743 0.067150 0.035 Uiso 1 1 calc R U . . .
C11B C -0.02403(17) 0.9459(5) 0.0753(2) 0.0251(10) Uani 1 1 d . . . . .
C12B C -0.02274(18) 0.8340(5) 0.1156(2) 0.0259(10) Uani 1 1 d . . . . .
H12B H -0.010001 0.751840 0.104915 0.031 Uiso 1 1 calc R U . . .
C13B C -0.03990(18) 0.8423(5) 0.1708(2) 0.0257(10) Uani 1 1 d . . . . .
H13B H -0.037422 0.765092 0.198550 0.031 Uiso 1 1 calc R U . . .
C14B C -0.00294(18) 0.9349(5) 0.0160(2) 0.0267(10) Uani 1 1 d . . . . .
H14E H 0.032073 0.890402 0.033905 0.032 Uiso 1 1 calc R U . . .
H14F H -0.027203 0.877425 -0.020857 0.032 Uiso 1 1 calc R U . . .
N4C N 0.43709(13) 1.0716(3) 0.68371(18) 0.0182(7) Uani 1 1 d . . . . .
C9C C 0.44103(18) 0.9595(5) 0.6517(2) 0.0254(10) Uani 1 1 d . . . . .
H9C H 0.430677 0.879094 0.667523 0.031 Uiso 1 1 calc R U . . .
C10C C 0.45920(18) 0.9521(4) 0.5969(2) 0.0241(9) Uani 1 1 d . . . . .
H10C H 0.461211 0.868448 0.576547 0.029 Uiso 1 1 calc R U . . .
C11C C 0.47445(15) 1.0664(4) 0.5718(2) 0.0188(8) Uani 1 1 d . . . . .
C12C C 0.46963(18) 1.1854(4) 0.6043(2) 0.0255(10) Uani 1 1 d . . . . .
H12C H 0.479047 1.267457 0.588885 0.031 Uiso 1 1 calc R U . . .
C13C C 0.45117(19) 1.1834(5) 0.6589(2) 0.0263(10) Uani 1 1 d . . . . .
H13C H 0.448259 1.265564 0.680142 0.032 Uiso 1 1 calc R U . . .
C14C C 0.49681(16) 1.0681(4) 0.5145(2) 0.0180(8) Uani 1 1 d . . . . .
H14G H 0.531953 1.111921 0.532410 0.022 Uiso 1 1 calc R U . . .
H14H H 0.473390 1.123154 0.475659 0.022 Uiso 1 1 calc R U . . .
O1S O -0.2532(2) 0.2814(7) 0.2644(3) 0.0393(17) Uani 0.5 1 d D . P A .
O1S' O -0.2640(4) 0.4980(11) 0.2796(5) 0.133(7) Uani 0.5 1 d D . P A 2
N1S N -0.23398(19) 0.4391(5) 0.2034(3) 0.0483(13) Uani 1 1 d . . . . .
C1S C -0.2521(2) 0.4035(7) 0.2532(4) 0.0532(18) Uani 1 1 d . . . . .
C2S C -0.2155(3) 0.3382(7) 0.1649(4) 0.0642(19) Uani 1 1 d . . . . .
H2S1 H -0.235230 0.347894 0.114696 0.096 Uiso 1 1 calc R U . . .
H2S2 H -0.221551 0.249067 0.179939 0.096 Uiso 1 1 calc R U . . .
H2S3 H -0.177577 0.350661 0.174536 0.096 Uiso 1 1 calc R U . . .
C3S C -0.2292(3) 0.5758(7) 0.1858(5) 0.073(2) Uani 1 1 d . . . . .
H3S1 H -0.248815 0.589501 0.135873 0.109 Uiso 1 1 calc R U . . .
H3S2 H -0.191752 0.597522 0.196766 0.109 Uiso 1 1 calc R U . . .
H3S3 H -0.243919 0.633509 0.212884 0.109 Uiso 1 1 calc R U . . .
O1W O -0.3045(3) 0.3262(7) 0.3681(4) 0.119(3) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn01 O1 2.140(3) . ?
Mn01 O4 2.271(3) 1_565 ?
Mn01 N4B 2.276(3) . ?
Mn01 N5A 2.286(4) 1_454 ?
Mn01 N4 2.286(3) . ?
Mn01 O3 2.328(3) 1_565 ?
Mn01 C8 2.637(4) 1_565 ?
Mn02 O1A 2.190(3) . ?
Mn02 O4A 2.260(3) 1_565 ?
Mn02 N4A 2.274(4) . ?
Mn02 N5 2.280(4) . ?
Mn02 N4C 2.287(3) . ?
Mn02 O3A 2.384(3) 1_565 ?
O1 C1 1.271(5) . ?
O2 C1 1.248(5) . ?
O3 C8 1.264(5) . ?
O4 C8 1.249(5) . ?
N1 N2 1.219(6) . ?
N1 C6 1.433(6) . ?
N2 N3 1.129(6) . ?
C1 C2 1.505(5) . ?
C2 C3 1.390(5) . ?
C2 C7 1.392(6) . ?
C3 C4 1.393(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.398(6) . ?
C4 C8 1.499(5) . ?
C5 C6 1.385(6) . ?
C5 H5 0.9500 . ?
C6 C7 1.394(6) . ?
C7 H7 0.9500 . ?
O1A C1A 1.256(6) . ?
O2A C1A 1.253(6) . ?
O3A C8A 1.255(5) . ?
O4A C8A 1.264(5) . ?
N1A N2A 1.234(6) . ?
N1A C4A 1.421(5) . ?
N2A N3A 1.140(6) . ?
C1A C2A 1.495(6) . ?
C2A C3A 1.384(6) . ?
C2A C7A 1.391(6) . ?
C3A C4A 1.387(6) . ?
C3A H3A 0.9500 . ?
C4A C5A 1.391(6) . ?
C5A C6A 1.391(6) . ?
C5A H5A 0.9500 . ?
C6A C7A 1.387(6) . ?
C6A C8A 1.508(5) . ?
C7A H7A 0.9500 . ?
N4 C9 1.346(5) . ?
N4 C13 1.352(6) . ?
N5 C19 1.324(6) . ?
N5 C18 1.351(6) . ?
C9 C10 1.379(6) . ?
C9 H9 0.9500 . ?
C10 C11 1.402(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.377(6) . ?
C11 C14 1.501(6) . ?
C12 C13 1.374(6) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C15 1.527(6) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.505(6) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.386(7) . ?
C16 C20 1.391(7) . ?
C17 C18 1.374(7) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C20 1.373(7) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
N4A C13A 1.344(5) . ?
N4A C9A 1.346(6) . ?
N5A C19A 1.333(6) . ?
N5A C18A 1.346(6) . ?
C9A C10A 1.375(6) . ?
C9A H9A 0.9500 . ?
C10A C11A 1.394(6) . ?
C10A H10A 0.9500 . ?
C11A C12A 1.392(6) . ?
C11A C14A 1.501(6) . ?
C12A C13A 1.375(6) . ?
C12A H12A 0.9500 . ?
C13A H13A 0.9500 . ?
C14A C15A 1.542(6) . ?
C14A H14C 0.9900 . ?
C14A H14D 0.9900 . ?
C15A C16A 1.501(6) . ?
C15A H15C 0.9900 . ?
C15A H15D 0.9900 . ?
C16A C17A 1.376(7) . ?
C16A C20A 1.397(7) . ?
C17A C18A 1.377(7) . ?
C17A H17A 0.9500 . ?
C18A H18A 0.9500 . ?
C19A C20A 1.375(7) . ?
C19A H19A 0.9500 . ?
C20A H20A 0.9500 . ?
N4B C9B 1.328(6) . ?
N4B C13B 1.353(6) . ?
C9B C10B 1.390(6) . ?
C9B H9B 0.9500 . ?
C10B C11B 1.380(7) . ?
C10B H10B 0.9500 . ?
C11B C12B 1.389(6) . ?
C11B C14B 1.522(6) . ?
C12B C13B 1.373(6) . ?
C12B H12B 0.9500 . ?
C13B H13B 0.9500 . ?
C14B C14B 1.499(9) 3_575 ?
C14B H14E 0.9900 . ?
C14B H14F 0.9900 . ?
N4C C9C 1.328(6) . ?
N4C C13C 1.343(6) . ?
C9C C10C 1.380(6) . ?
C9C H9C 0.9500 . ?
C10C C11C 1.381(6) . ?
C10C H10C 0.9500 . ?
C11C C12C 1.399(6) . ?
C11C C14C 1.502(6) . ?
C12C C13C 1.381(6) . ?
C12C H12C 0.9500 . ?
C13C H13C 0.9500 . ?
C14C C14C 1.527(8) 3_676 ?
C14C H14G 0.9900 . ?
C14C H14H 0.9900 . ?
O1S C1S 1.251(10) . ?
O1S' C1S 1.193(13) . ?
N1S C1S 1.333(9) . ?
N1S C3S 1.438(8) . ?
N1S C2S 1.478(9) . ?
C2S H2S1 0.9800 . ?
C2S H2S2 0.9800 . ?
C2S H2S3 0.9800 . ?
C3S H3S1 0.9800 . ?
C3S H3S2 0.9800 . ?
C3S H3S3 0.9800 . ?
O1W O1W 0.00(2) 1 ?

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 Mn01 O4 139.98(12) . 1_565 ?
O1 Mn01 N4B 133.31(12) . . ?
O4 Mn01 N4B 86.59(12) 1_565 . ?
O1 Mn01 N5A 92.65(13) . 1_454 ?
O4 Mn01 N5A 92.58(12) 1_565 1_454 ?
N4B Mn01 N5A 86.88(13) . 1_454 ?
O1 Mn01 N4 88.34(12) . . ?
O4 Mn01 N4 91.34(12) 1_565 . ?
N4B Mn01 N4 87.14(12) . . ?
N5A Mn01 N4 172.64(13) 1_454 . ?
O1 Mn01 O3 83.14(11) . 1_565 ?
O4 Mn01 O3 56.87(11) 1_565 1_565 ?
N4B Mn01 O3 143.44(12) . 1_565 ?
N5A Mn01 O3 95.24(12) 1_454 1_565 ?
N4 Mn01 O3 92.12(12) . 1_565 ?
O1 Mn01 C8 111.76(13) . 1_565 ?
O4 Mn01 C8 28.24(12) 1_565 1_565 ?
N4B Mn01 C8 114.82(13) . 1_565 ?
N5A Mn01 C8 94.60(13) 1_454 1_565 ?
N4 Mn01 C8 91.81(12) . 1_565 ?
O3 Mn01 C8 28.63(12) 1_565 1_565 ?
O1A Mn02 O4A 83.00(13) . 1_565 ?
O1A Mn02 N4A 89.77(13) . . ?
O4A Mn02 N4A 89.25(12) 1_565 . ?
O1A Mn02 N5 93.37(13) . . ?
O4A Mn02 N5 92.77(12) 1_565 . ?
N4A Mn02 N5 176.46(13) . . ?
O1A Mn02 N4C 132.09(13) . . ?
O4A Mn02 N4C 144.86(12) 1_565 . ?
N4A Mn02 N4C 89.02(13) . . ?
N5 Mn02 N4C 87.66(12) . . ?
O1A Mn02 O3A 139.45(12) . 1_565 ?
O4A Mn02 O3A 56.63(10) 1_565 1_565 ?
N4A Mn02 O3A 93.00(12) . 1_565 ?
N5 Mn02 O3A 85.69(12) . 1_565 ?
N4C Mn02 O3A 88.42(11) . 1_565 ?
C1 O1 Mn01 106.4(3) . . ?
C8 O3 Mn01 89.4(3) . 1_545 ?
C8 O4 Mn01 92.4(2) . 1_545 ?
N2 N1 C6 116.4(4) . . ?
N3 N2 N1 171.0(6) . . ?
O2 C1 O1 123.5(4) . . ?
O2 C1 C2 119.1(4) . . ?
O1 C1 C2 117.5(4) . . ?
C3 C2 C7 120.1(4) . . ?
C3 C2 C1 122.1(4) . . ?
C7 C2 C1 117.8(4) . . ?
C2 C3 C4 120.0(4) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C3 C4 C5 119.7(4) . . ?
C3 C4 C8 119.8(4) . . ?
C5 C4 C8 120.4(4) . . ?
C6 C5 C4 120.3(4) . . ?
C6 C5 H5 119.9 . . ?
C4 C5 H5 119.9 . . ?
C5 C6 C7 119.8(4) . . ?
C5 C6 N1 126.3(4) . . ?
C7 C6 N1 114.0(4) . . ?
C2 C7 C6 120.1(4) . . ?
C2 C7 H7 119.9 . . ?
C6 C7 H7 119.9 . . ?
O4 C8 O3 121.4(4) . . ?
O4 C8 C4 120.2(4) . . ?
O3 C8 C4 118.5(4) . . ?
O4 C8 Mn01 59.4(2) . 1_545 ?
O3 C8 Mn01 62.0(2) . 1_545 ?
C4 C8 Mn01 178.6(3) . 1_545 ?
C1A O1A Mn02 103.4(3) . . ?
C8A O3A Mn02 87.7(2) . 1_545 ?
C8A O4A Mn02 93.1(2) . 1_545 ?
N2A N1A C4A 115.4(4) . . ?
N3A N2A N1A 174.6(5) . . ?
O2A C1A O1A 122.8(4) . . ?
O2A C1A C2A 119.6(4) . . ?
O1A C1A C2A 117.6(4) . . ?
C3A C2A C7A 119.6(4) . . ?
C3A C2A C1A 119.5(4) . . ?
C7A C2A C1A 120.8(4) . . ?
C2A C3A C4A 120.5(4) . . ?
C2A C3A H3A 119.8 . . ?
C4A C3A H3A 119.8 . . ?
C3A C4A C5A 120.2(4) . . ?
C3A C4A N1A 115.1(4) . . ?
C5A C4A N1A 124.7(4) . . ?
C6A C5A C4A 119.3(4) . . ?
C6A C5A H5A 120.4 . . ?
C4A C5A H5A 120.4 . . ?
C7A C6A C5A 120.5(4) . . ?
C7A C6A C8A 120.6(4) . . ?
C5A C6A C8A 118.9(4) . . ?
C6A C7A C2A 120.0(4) . . ?
C6A C7A H7A 120.0 . . ?
C2A C7A H7A 120.0 . . ?
O3A C8A O4A 122.2(4) . . ?
O3A C8A C6A 119.4(4) . . ?
O4A C8A C6A 118.4(4) . . ?
C9 N4 C13 115.6(4) . . ?
C9 N4 Mn01 121.0(3) . . ?
C13 N4 Mn01 123.2(3) . . ?
C19 N5 C18 115.8(4) . . ?
C19 N5 Mn02 118.5(3) . . ?
C18 N5 Mn02 125.6(3) . . ?
N4 C9 C10 123.5(4) . . ?
N4 C9 H9 118.3 . . ?
C10 C9 H9 118.3 . . ?
C9 C10 C11 119.9(4) . . ?
C9 C10 H10 120.0 . . ?
C11 C10 H10 120.0 . . ?
C12 C11 C10 116.8(4) . . ?
C12 C11 C14 121.5(4) . . ?
C10 C11 C14 121.7(4) . . ?
C13 C12 C11 119.8(4) . . ?
C13 C12 H12 120.1 . . ?
C11 C12 H12 120.1 . . ?
N4 C13 C12 124.4(4) . . ?
N4 C13 H13 117.8 . . ?
C12 C13 H13 117.8 . . ?
C11 C14 C15 113.4(4) . . ?
C11 C14 H14A 108.9 . . ?
C15 C14 H14A 108.9 . . ?
C11 C14 H14B 108.9 . . ?
C15 C14 H14B 108.9 . . ?
H14A C14 H14B 107.7 . . ?
C16 C15 C14 112.8(4) . . ?
C16 C15 H15A 109.0 . . ?
C14 C15 H15A 109.0 . . ?
C16 C15 H15B 109.0 . . ?
C14 C15 H15B 109.0 . . ?
H15A C15 H15B 107.8 . . ?
C17 C16 C20 116.1(4) . . ?
C17 C16 C15 122.7(4) . . ?
C20 C16 C15 121.1(4) . . ?
C18 C17 C16 119.8(5) . . ?
C18 C17 H17 120.1 . . ?
C16 C17 H17 120.1 . . ?
N5 C18 C17 123.9(5) . . ?
N5 C18 H18 118.1 . . ?
C17 C18 H18 118.1 . . ?
N5 C19 C20 124.1(5) . . ?
N5 C19 H19 117.9 . . ?
C20 C19 H19 117.9 . . ?
C19 C20 C16 120.2(5) . . ?
C19 C20 H20 119.9 . . ?
C16 C20 H20 119.9 . . ?
C13A N4A C9A 115.6(4) . . ?
C13A N4A Mn02 120.0(3) . . ?
C9A N4A Mn02 124.3(3) . . ?
C19A N5A C18A 116.0(4) . . ?
C19A N5A Mn01 119.9(3) . 1_656 ?
C18A N5A Mn01 124.1(3) . 1_656 ?
N4A C9A C10A 124.2(4) . . ?
N4A C9A H9A 117.9 . . ?
C10A C9A H9A 117.9 . . ?
C9A C10A C11A 119.9(4) . . ?
C9A C10A H10A 120.0 . . ?
C11A C10A H10A 120.0 . . ?
C12A C11A C10A 116.1(4) . . ?
C12A C11A C14A 123.1(4) . . ?
C10A C11A C14A 120.7(4) . . ?
C13A C12A C11A 120.3(4) . . ?
C13A C12A H12A 119.9 . . ?
C11A C12A H12A 119.9 . . ?
N4A C13A C12A 123.9(4) . . ?
N4A C13A H13A 118.1 . . ?
C12A C13A H13A 118.1 . . ?
C11A C14A C15A 112.3(4) . . ?
C11A C14A H14C 109.1 . . ?
C15A C14A H14C 109.1 . . ?
C11A C14A H14D 109.1 . . ?
C15A C14A H14D 109.1 . . ?
H14C C14A H14D 107.9 . . ?
C16A C15A C14A 110.7(4) . . ?
C16A C15A H15C 109.5 . . ?
C14A C15A H15C 109.5 . . ?
C16A C15A H15D 109.5 . . ?
C14A C15A H15D 109.5 . . ?
H15C C15A H15D 108.1 . . ?
C17A C16A C20A 116.1(4) . . ?
C17A C16A C15A 123.2(4) . . ?
C20A C16A C15A 120.6(4) . . ?
C16A C17A C18A 121.2(5) . . ?
C16A C17A H17A 119.4 . . ?
C18A C17A H17A 119.4 . . ?
N5A C18A C17A 122.9(4) . . ?
N5A C18A H18A 118.6 . . ?
C17A C18A H18A 118.6 . . ?
N5A C19A C20A 124.6(5) . . ?
N5A C19A H19A 117.7 . . ?
C20A C19A H19A 117.7 . . ?
C19A C20A C16A 119.3(5) . . ?
C19A C20A H20A 120.3 . . ?
C16A C20A H20A 120.3 . . ?
C9B N4B C13B 116.6(4) . . ?
C9B N4B Mn01 124.0(3) . . ?
C13B N4B Mn01 119.4(3) . . ?
N4B C9B C10B 123.0(4) . . ?
N4B C9B H9B 118.5 . . ?
C10B C9B H9B 118.5 . . ?
C11B C10B C9B 120.5(4) . . ?
C11B C10B H10B 119.8 . . ?
C9B C10B H10B 119.8 . . ?
C10B C11B C12B 116.5(4) . . ?
C10B C11B C14B 124.8(4) . . ?
C12B C11B C14B 118.7(4) . . ?
C13B C12B C11B 119.9(4) . . ?
C13B C12B H12B 120.1 . . ?
C11B C12B H12B 120.1 . . ?
N4B C13B C12B 123.5(4) . . ?
N4B C13B H13B 118.2 . . ?
C12B C13B H13B 118.2 . . ?
C14B C14B C11B 114.6(5) 3_575 . ?
C14B C14B H14E 108.6 3_575 . ?
C11B C14B H14E 108.6 . . ?
C14B C14B H14F 108.6 3_575 . ?
C11B C14B H14F 108.6 . . ?
H14E C14B H14F 107.6 . . ?
C9C N4C C13C 116.0(4) . . ?
C9C N4C Mn02 124.6(3) . . ?
C13C N4C Mn02 119.3(3) . . ?
N4C C9C C10C 124.3(4) . . ?
N4C C9C H9C 117.9 . . ?
C10C C9C H9C 117.9 . . ?
C9C C10C C11C 120.1(4) . . ?
C9C C10C H10C 120.0 . . ?
C11C C10C H10C 120.0 . . ?
C10C C11C C12C 116.2(4) . . ?
C10C C11C C14C 124.0(4) . . ?
C12C C11C C14C 119.7(4) . . ?
C13C C12C C11C 119.8(4) . . ?
C13C C12C H12C 120.1 . . ?
C11C C12C H12C 120.1 . . ?
N4C C13C C12C 123.6(4) . . ?
N4C C13C H13C 118.2 . . ?
C12C C13C H13C 118.2 . . ?
C11C C14C C14C 115.4(4) . 3_676 ?
C11C C14C H14G 108.4 . . ?
C14C C14C H14G 108.4 3_676 . ?
C11C C14C H14H 108.4 . . ?
C14C C14C H14H 108.4 3_676 . ?
H14G C14C H14H 107.5 . . ?
C1S N1S C3S 122.7(6) . . ?
C1S N1S C2S 120.9(5) . . ?
C3S N1S C2S 116.4(6) . . ?
O1S' C1S O1S 132.2(9) . . ?
O1S' C1S N1S 111.5(7) . . ?
O1S C1S N1S 116.3(6) . . ?
N1S C2S H2S1 109.5 . . ?
N1S C2S H2S2 109.5 . . ?
H2S1 C2S H2S2 109.5 . . ?
N1S C2S H2S3 109.5 . . ?
H2S1 C2S H2S3 109.5 . . ?
H2S2 C2S H2S3 109.5 . . ?
N1S C3S H3S1 109.5 . . ?
N1S C3S H3S2 109.5 . . ?
H3S1 C3S H3S2 109.5 . . ?
N1S C3S H3S3 109.5 . . ?
H3S1 C3S H3S3 109.5 . . ?
H3S2 C3S H3S3 109.5 . . ?

_refine_diff_density_max         1.756
_refine_diff_density_min         -1.235
_refine_diff_density_rms         0.119

####################################################################### 
# 
# 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_PS110317_0m
_database_code_depnum_ccdc_archive 'CCDC 1963353'
loop_
_audit_author_name
_audit_author_address
'Raju Mondal'
;Indian Association for the Cultivation of Science
India
;
_audit_update_record             
;
2021-02-10 deposited with the CCDC.	2021-03-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H19 Cd N8 O8'
_chemical_formula_weight         707.91

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   12.7472(15)
_cell_length_b                   17.173(2)
_cell_length_c                   13.6504(16)
_cell_angle_alpha                90
_cell_angle_beta                 110.216(3)
_cell_angle_gamma                90
_cell_volume                     2804.2(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    5134
_cell_measurement_theta_min      2.227
_cell_measurement_theta_max      27.12

_exptl_crystal_description       Block
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.677
_exptl_crystal_F_000             1420
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_exptl_absorpt_coefficient_mu    0.846
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.89926
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
'SADABS v.2.03 (Bruker, 2001), wR2(int)=0.0714 before correction'

_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-2 CCD area detector'
_diffrn_measurement_method       '/w scans'
_diffrn_detector_area_resol_mean 8
_diffrn_reflns_number            38491
_diffrn_reflns_av_unetI/netI     0.0461
_diffrn_reflns_av_R_equivalents  0.0683
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.702
_diffrn_reflns_theta_max         27.019
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6119
_reflns_number_gt                4407
_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 APEX-2'
_computing_cell_refinement       'Bruker APEX-2'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_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)+(0.0346P)²+1.2482P] 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         6119
_refine_ls_number_parameters     406
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0730
_refine_ls_R_factor_gt           0.0461
_refine_ls_wR_factor_ref         0.1073
_refine_ls_wR_factor_gt          0.0990
_refine_ls_goodness_of_fit_ref   1.309
_refine_ls_restrained_S_all      1.462
_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
Cd1 Cd 0.72840(2) 0.11240(2) 0.19628(2) 0.02989(10) Uani 1 1 d . . . . .
O1 O 0.7595(3) -0.03369(17) 0.1837(2) 0.0420(8) Uani 1 1 d . . . . .
O2 O 0.9434(3) -0.04096(19) 0.2216(4) 0.0710(12) Uani 1 1 d . . . . .
O3 O 0.9437(3) 0.10551(19) 0.2478(3) 0.0643(10) Uani 1 1 d . . . . .
O4 O 0.8577(3) 0.21613(19) 0.2377(3) 0.0485(8) Uani 1 1 d . . . . .
N1 N 0.6473(3) -0.3273(2) 0.1226(3) 0.0503(10) Uani 1 1 d . . . . .
N2 N 0.5571(4) -0.2937(3) 0.1005(3) 0.0530(11) Uani 1 1 d . . . . .
N3 N 0.4696(4) -0.2707(3) 0.0785(5) 0.0855(17) Uani 1 1 d . . . . .
C1 C 0.8434(4) -0.0717(3) 0.1981(3) 0.0368(10) Uani 1 1 d . . . . .
C2 C 0.8438(3) -0.1589(2) 0.1911(3) 0.0317(9) Uani 1 1 d . . . . .
C3 C 0.7432(4) -0.1995(3) 0.1597(3) 0.0366(10) Uani 1 1 d . . . . .
H3 H 0.675798 -0.172710 0.142149 0.044 Uiso 1 1 calc R U . . .
C4 C 0.7439(4) -0.2801(3) 0.1546(3) 0.0349(10) Uani 1 1 d . . . . .
C5 C 0.8445(4) -0.3195(3) 0.1825(3) 0.0366(10) Uani 1 1 d . . . . .
H5 H 0.844455 -0.373668 0.180178 0.044 Uiso 1 1 calc R U . . .
C6 C 0.9447(3) -0.2802(2) 0.2135(3) 0.0318(9) Uani 1 1 d . . . . .
C7 C 0.9443(4) -0.1986(2) 0.2169(3) 0.0341(10) Uani 1 1 d . . . . .
H7 H 1.011338 -0.171250 0.236464 0.041 Uiso 1 1 calc R U . . .
C8 C 0.9447(4) 0.1778(3) 0.2557(3) 0.0382(11) Uani 1 1 d . . . . .
O1A O 0.5342(2) 0.08004(18) 0.1514(2) 0.0392(7) Uani 1 1 d . . . . .
O2A O 0.5847(2) 0.20291(18) 0.1810(3) 0.0477(8) Uani 1 1 d . . . . .
O3A O -0.0005(2) 0.09666(18) 0.0005(3) 0.0762(12) Uani 1 1 d D . . . .
H333 H -0.052100 0.058400 -0.028300 0.091 Uiso 1 1 d D U . . .
O4A O 0.1365(3) 0.0117(2) 0.0551(3) 0.0731(12) Uani 1 1 d . . . . .
N1A N 0.2352(4) 0.3570(2) 0.0872(4) 0.0543(11) Uani 1 1 d . . . . .
N2A N 0.1378(4) 0.3799(3) 0.0539(4) 0.0622(12) Uani 1 1 d . . . . .
N3A N 0.0555(5) 0.4100(4) 0.0247(6) 0.113(2) Uani 1 1 d . . . . .
C1A C 0.5115(3) 0.1507(3) 0.1561(3) 0.0333(10) Uani 1 1 d . . . . .
C2A C 0.3914(3) 0.1745(3) 0.1275(3) 0.0326(9) Uani 1 1 d . . . . .
C3A C 0.3084(3) 0.1197(3) 0.1027(3) 0.0351(10) Uani 1 1 d . . . . .
H3A H 0.326842 0.067158 0.106399 0.042 Uiso 1 1 calc R U . . .
C4A C 0.1959(3) 0.1420(3) 0.0717(3) 0.0339(10) Uani 1 1 d . . . . .
C5A C 0.1691(4) 0.2199(3) 0.0657(3) 0.0388(10) Uani 1 1 d . . . . .
H5A H 0.094681 0.235346 0.044395 0.047 Uiso 1 1 calc R U . . .
C6A C 0.2532(4) 0.2752(3) 0.0915(3) 0.0394(11) Uani 1 1 d . . . . .
C7A C 0.3639(4) 0.2527(3) 0.1226(3) 0.0385(10) Uani 1 1 d . . . . .
H7A H 0.420015 0.290144 0.140265 0.046 Uiso 1 1 calc R U . . .
C8A C 0.1081(4) 0.0815(3) 0.0435(4) 0.0433(11) Uani 1 1 d . . . . .
N4 N 0.6992(3) 0.1173(2) 0.0219(3) 0.0336(8) Uani 1 1 d . . . . .
N5 N 0.7410(3) 0.0870(2) 0.3651(3) 0.0355(8) Uani 1 1 d . . . . .
C9 C 0.6123(4) 0.0810(3) -0.0471(3) 0.0409(11) Uani 1 1 d . . . . .
H9 H 0.563931 0.053518 -0.022097 0.049 Uiso 1 1 calc R U . . .
C10 C 0.5904(4) 0.0819(3) -0.1531(3) 0.0425(11) Uani 1 1 d . . . . .
H10 H 0.527876 0.056291 -0.197855 0.051 Uiso 1 1 calc R U . . .
C11 C 0.6609(4) 0.1208(3) -0.1926(3) 0.0375(10) Uani 1 1 d . . . . .
C12 C 0.7493(4) 0.1599(3) -0.1220(3) 0.0423(11) Uani 1 1 d . . . . .
H12 H 0.798159 0.188379 -0.145239 0.051 Uiso 1 1 calc R U . . .
C13 C 0.7651(4) 0.1568(3) -0.0172(3) 0.0388(10) Uani 1 1 d . . . . .
H13 H 0.825295 0.183839 0.028759 0.047 Uiso 1 1 calc R U . . .
C14 C 0.6831(5) 0.0315(3) 0.3876(4) 0.0572(14) Uani 1 1 d . . . . .
H14 H 0.642825 -0.001974 0.334224 0.069 Uiso 1 1 calc R U . . .
C15 C 0.6782(5) 0.0194(3) 0.4861(4) 0.0596(15) Uani 1 1 d . . . . .
H15 H 0.636949 -0.022029 0.497591 0.071 Uiso 1 1 calc R U . . .
C16 C 0.7329(4) 0.0675(3) 0.5658(3) 0.0428(11) Uani 1 1 d . . . . .
C17 C 0.7914(5) 0.1275(4) 0.5422(4) 0.0673(17) Uani 1 1 d . . . . .
H17 H 0.828858 0.163423 0.593311 0.081 Uiso 1 1 calc R U . . .
C18 C 0.7945(5) 0.1344(4) 0.4424(4) 0.0618(16) Uani 1 1 d . . . . .
H18 H 0.836531 0.174619 0.428989 0.074 Uiso 1 1 calc R U . . .
C19 C 0.6477(4) 0.1177(3) -0.3062(3) 0.0472(12) Uani 1 1 d . . . . .
H19A H 0.660582 0.169067 -0.329228 0.071 Uiso 1 1 calc R U . . .
H19B H 0.571708 0.102449 -0.346659 0.071 Uiso 1 1 calc R U . . .
C20 C 0.7292(4) 0.0600(3) 0.6740(3) 0.0528(14) Uani 1 1 d . . . . .
H20A H 0.803379 0.068878 0.724329 0.079 Uiso 1 1 calc R U . . .
H20B H 0.706957 0.007407 0.684026 0.079 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 N4 2.281(3) . ?
Cd1 N5 2.296(3) . ?
Cd1 O2A 2.356(3) . ?
Cd1 O4 2.359(3) . ?
Cd1 O1A 2.401(3) . ?
Cd1 O1 2.555(3) . ?
Cd1 O3 2.590(4) . ?
Cd1 C1A 2.707(4) . ?
O1 C1 1.211(5) . ?
O2 C1 1.313(5) . ?
O3 C8 1.246(5) . ?
O4 C8 1.239(5) . ?
N1 N2 1.229(5) . ?
N1 C4 1.412(5) . ?
N2 N3 1.121(6) . ?
C1 C2 1.500(6) . ?
C2 C7 1.385(5) . ?
C2 C3 1.391(6) . ?
C3 C4 1.386(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.382(6) . ?
C5 C6 1.375(6) . ?
C5 H5 0.9300 . ?
C6 C7 1.403(6) . ?
C6 C8 1.508(6) 2_745 ?
C7 H7 0.9300 . ?
O1A C1A 1.254(5) . ?
O2A C1A 1.254(5) . ?
O3A C8A 1.329(5) . ?
O3A H333 0.9168 . ?
O4A C8A 1.247(6) . ?
N1A N2A 1.230(6) . ?
N1A C6A 1.421(6) . ?
N2A N3A 1.112(7) . ?
C1A C2A 1.500(6) . ?
C2A C3A 1.368(6) . ?
C2A C7A 1.384(6) . ?
C3A C4A 1.401(6) . ?
C3A H3A 0.9300 . ?
C4A C5A 1.376(6) . ?
C4A C8A 1.478(6) . ?
C5A C6A 1.383(6) . ?
C5A H5A 0.9300 . ?
C6A C7A 1.381(6) . ?
C7A H7A 0.9300 . ?
N4 C13 1.327(5) . ?
N4 C9 1.334(5) . ?
N5 C14 1.306(6) . ?
N5 C18 1.321(6) . ?
C9 C10 1.376(6) . ?
C9 H9 0.9300 . ?
C10 C11 1.370(6) . ?
C10 H10 0.9300 . ?
C11 C12 1.378(6) . ?
C11 C19 1.502(6) . ?
C12 C13 1.375(6) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 C15 1.383(6) . ?
C14 H14 0.9300 . ?
C15 C16 1.351(6) . ?
C15 H15 0.9300 . ?
C16 C17 1.375(7) . ?
C16 C20 1.499(6) . ?
C17 C18 1.381(7) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C19 C20 1.526(6) 1_554 ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 Cd1 N5 169.87(13) . . ?
N4 Cd1 O2A 92.39(12) . . ?
N5 Cd1 O2A 89.82(12) . . ?
N4 Cd1 O4 94.08(12) . . ?
N5 Cd1 O4 95.85(12) . . ?
O2A Cd1 O4 88.88(11) . . ?
N4 Cd1 O1A 87.70(11) . . ?
N5 Cd1 O1A 85.45(12) . . ?
O2A Cd1 O1A 55.16(10) . . ?
O4 Cd1 O1A 144.04(11) . . ?
N4 Cd1 O1 86.52(11) . . ?
N5 Cd1 O1 85.54(11) . . ?
O2A Cd1 O1 140.87(10) . . ?
O4 Cd1 O1 130.23(11) . . ?
O1A Cd1 O1 85.73(10) . . ?
N4 Cd1 O3 93.47(13) . . ?
N5 Cd1 O3 91.08(13) . . ?
O2A Cd1 O3 140.60(10) . . ?
O4 Cd1 O3 51.85(11) . . ?
O1A Cd1 O3 163.99(11) . . ?
O1 Cd1 O3 78.41(10) . . ?
N4 Cd1 C1A 89.57(12) . . ?
N5 Cd1 C1A 87.81(12) . . ?
O2A Cd1 C1A 27.57(12) . . ?
O4 Cd1 C1A 116.45(13) . . ?
O1A Cd1 C1A 27.59(11) . . ?
O1 Cd1 C1A 113.32(12) . . ?
O3 Cd1 C1A 168.07(13) . . ?
C1 O1 Cd1 131.9(3) . . ?
C8 O3 Cd1 87.5(3) . . ?
C8 O4 Cd1 98.6(3) . . ?
N2 N1 C4 116.6(4) . . ?
N3 N2 N1 172.5(6) . . ?
O1 C1 O2 123.5(4) . . ?
O1 C1 C2 123.4(4) . . ?
O2 C1 C2 113.1(4) . . ?
C7 C2 C3 120.3(4) . . ?
C7 C2 C1 119.9(4) . . ?
C3 C2 C1 119.8(4) . . ?
C4 C3 C2 119.6(4) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
C5 C4 C3 119.8(4) . . ?
C5 C4 N1 115.5(4) . . ?
C3 C4 N1 124.7(4) . . ?
C6 C5 C4 121.2(4) . . ?
C6 C5 H5 119.4 . . ?
C4 C5 H5 119.4 . . ?
C5 C6 C7 119.2(4) . . ?
C5 C6 C8 122.0(4) . 2_745 ?
C7 C6 C8 118.8(4) . 2_745 ?
C2 C7 C6 119.8(4) . . ?
C2 C7 H7 120.1 . . ?
C6 C7 H7 120.1 . . ?
O4 C8 O3 122.0(4) . . ?
O4 C8 C6 119.2(4) . 2_755 ?
O3 C8 C6 118.7(4) . 2_755 ?
C1A O1A Cd1 89.9(2) . . ?
C1A O2A Cd1 92.0(3) . . ?
C8A O3A H333 122.2 . . ?
N2A N1A C6A 117.4(4) . . ?
N3A N2A N1A 171.0(6) . . ?
O2A C1A O1A 122.9(4) . . ?
O2A C1A C2A 118.2(4) . . ?
O1A C1A C2A 118.9(4) . . ?
O2A C1A Cd1 60.4(2) . . ?
O1A C1A Cd1 62.5(2) . . ?
C2A C1A Cd1 176.3(3) . . ?
C3A C2A C7A 119.5(4) . . ?
C3A C2A C1A 120.6(4) . . ?
C7A C2A C1A 119.8(4) . . ?
C2A C3A C4A 120.7(4) . . ?
C2A C3A H3A 119.7 . . ?
C4A C3A H3A 119.7 . . ?
C5A C4A C3A 119.4(4) . . ?
C5A C4A C8A 121.2(4) . . ?
C3A C4A C8A 119.4(4) . . ?
C4A C5A C6A 119.8(4) . . ?
C4A C5A H5A 120.1 . . ?
C6A C5A H5A 120.1 . . ?
C7A C6A C5A 120.4(4) . . ?
C7A C6A N1A 115.0(4) . . ?
C5A C6A N1A 124.6(4) . . ?
C6A C7A C2A 120.1(4) . . ?
C6A C7A H7A 119.9 . . ?
C2A C7A H7A 119.9 . . ?
O4A C8A O3A 117.1(4) . . ?
O4A C8A C4A 118.9(4) . . ?
O3A C8A C4A 123.9(4) . . ?
C13 N4 C9 116.2(4) . . ?
C13 N4 Cd1 122.7(3) . . ?
C9 N4 Cd1 121.0(3) . . ?
C14 N5 C18 116.1(4) . . ?
C14 N5 Cd1 121.7(3) . . ?
C18 N5 Cd1 121.5(3) . . ?
N4 C9 C10 123.7(4) . . ?
N4 C9 H9 118.2 . . ?
C10 C9 H9 118.2 . . ?
C11 C10 C9 119.8(4) . . ?
C11 C10 H10 120.1 . . ?
C9 C10 H10 120.1 . . ?
C10 C11 C12 116.9(4) . . ?
C10 C11 C19 122.2(4) . . ?
C12 C11 C19 120.8(4) . . ?
C13 C12 C11 119.9(4) . . ?
C13 C12 H12 120.0 . . ?
C11 C12 H12 120.0 . . ?
N4 C13 C12 123.5(4) . . ?
N4 C13 H13 118.2 . . ?
C12 C13 H13 118.2 . . ?
N5 C14 C15 123.8(5) . . ?
N5 C14 H14 118.1 . . ?
C15 C14 H14 118.1 . . ?
C16 C15 C14 120.5(5) . . ?
C16 C15 H15 119.8 . . ?
C14 C15 H15 119.8 . . ?
C15 C16 C17 116.1(4) . . ?
C15 C16 C20 123.9(5) . . ?
C17 C16 C20 120.0(5) . . ?
C16 C17 C18 119.9(5) . . ?
C16 C17 H17 120.1 . . ?
C18 C17 H17 120.1 . . ?
N5 C18 C17 123.5(5) . . ?
N5 C18 H18 118.2 . . ?
C17 C18 H18 118.2 . . ?
C11 C19 C20 111.4(4) . 1_554 ?
C11 C19 H19A 109.3 . . ?
C20 C19 H19A 109.3 1_554 . ?
C11 C19 H19B 109.3 . . ?
C20 C19 H19B 109.3 1_554 . ?
H19A C19 H19B 108.0 . . ?
C16 C20 C19 112.0(4) . 1_556 ?
C16 C20 H20A 109.2 . . ?
C19 C20 H20A 109.2 1_556 . ?
C16 C20 H20B 109.2 . . ?
C19 C20 H20B 109.2 1_556 . ?
H20A C20 H20B 107.9 . . ?

_refine_diff_density_max         2.423
_refine_diff_density_min         -2.048
_refine_diff_density_rms         0.103

####################################################################### 
# 
# 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_mo_PROBHATTRC160519_0m_a
_database_code_depnum_ccdc_archive 'CCDC 1963352'
loop_
_audit_author_name
_audit_author_address
'Raju Mondal'
;Indian Association for the Cultivation of Science
India
;
_audit_update_record             
;
2021-02-10 deposited with the CCDC.	2021-03-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C78 H63 N18 Ni3 O12'
_chemical_formula_weight         1620.59

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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   15.1952(7)
_cell_length_b                   17.0749(9)
_cell_length_c                   17.2622(9)
_cell_angle_alpha                115.355(2)
_cell_angle_beta                 112.7570(10)
_cell_angle_gamma                92.171(2)
_cell_volume                     3619.2(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    10961
_cell_measurement_theta_min      2.392
_cell_measurement_theta_max      30.097

_exptl_crystal_description       Needle
_exptl_crystal_colour            Green
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_F_000             1674
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_exptl_absorpt_coefficient_mu    0.850
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.65884
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
'SADABS v.2.03 (Bruker, 2001), wR2(int)=0.1562 before correction'

_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-2 CCD area detector'
_diffrn_measurement_method       '/w scans'
_diffrn_detector_area_resol_mean 8
_diffrn_reflns_number            51754
_diffrn_reflns_av_unetI/netI     0.1379
_diffrn_reflns_av_R_equivalents  0.1034
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.257
_diffrn_reflns_theta_max         30.122
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.181
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.181
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.181
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             21005
_reflns_number_gt                11321
_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 APEX-2'
_computing_cell_refinement       'Bruker APEX-2'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         21005
_refine_ls_number_parameters     1001
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1517
_refine_ls_R_factor_gt           0.0796
_refine_ls_wR_factor_ref         0.2474
_refine_ls_wR_factor_gt          0.1878
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_restrained_S_all      1.091
_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 1.43399(3) 0.27742(3) 0.71275(3) 0.02276(11) Uani 1 1 d . . . . .
Ni2 Ni 1.10288(3) 0.62324(3) 0.37953(3) 0.02585(11) Uani 1 1 d . . . . .
Ni3 Ni 0.23361(3) 0.07678(3) -0.04024(3) 0.02677(12) Uani 1 1 d . . . . .
O1 O 0.41710(16) -0.31524(15) 0.18014(17) 0.0301(5) Uani 1 1 d . . . . .
O2 O 0.51797(17) -0.18903(15) 0.23043(16) 0.0299(5) Uani 1 1 d . . . . .
O3 O 0.23757(18) -0.03374(16) -0.02510(17) 0.0350(6) Uani 1 1 d . . . . .
O4 O 0.3986(2) -0.0143(2) 0.0586(2) 0.0600(8) Uani 1 1 d . . . . .
N1 N 0.0751(2) -0.2788(2) 0.0006(3) 0.0497(9) Uani 1 1 d . . . . .
N2 N 0.0612(3) -0.3305(3) 0.0298(3) 0.0557(10) Uani 1 1 d . . . . .
N3 N 0.0403(3) -0.3789(3) 0.0519(4) 0.0819(14) Uani 1 1 d . . . . .
C1 C 0.4337(2) -0.2422(2) 0.1795(2) 0.0280(7) Uani 1 1 d . . . . .
C2 C 0.3498(2) -0.2173(2) 0.1206(2) 0.0295(7) Uani 1 1 d . . . . .
C3 C 0.2535(3) -0.2611(2) 0.0883(2) 0.0340(8) Uani 1 1 d . . . . .
H3 H 0.241504 -0.307205 0.102479 0.041 Uiso 1 1 calc R U . . .
C4 C 0.1760(3) -0.2377(2) 0.0358(3) 0.0367(8) Uani 1 1 d . . . . .
C5 C 0.1942(3) -0.1693(2) 0.0150(3) 0.0379(8) Uani 1 1 d . . . . .
H5 H 0.140424 -0.153087 -0.021049 0.045 Uiso 1 1 calc R U . . .
C6 C 0.2887(3) -0.1258(2) 0.0463(2) 0.0319(8) Uani 1 1 d . . . . .
C7 C 0.3671(3) -0.1494(2) 0.1004(2) 0.0323(8) Uani 1 1 d . . . . .
H7 H 0.432759 -0.118795 0.123634 0.039 Uiso 1 1 calc R U . . .
C8 C 0.3122(3) -0.0501(3) 0.0262(3) 0.0355(8) Uani 1 1 d . . . . .
O1A O 0.08004(16) 0.03602(15) -0.13736(17) 0.0304(5) Uani 1 1 d . . . . .
O2A O 0.16587(16) 0.16865(16) -0.08945(17) 0.0335(5) Uani 1 1 d . . . . .
O3A O -0.16156(17) 0.24805(16) -0.40161(17) 0.0337(5) Uani 1 1 d . . . . .
O4A O -0.01317(18) 0.32464(17) -0.28730(18) 0.0361(6) Uani 1 1 d . . . . .
N1A N -0.2797(2) 0.0494(2) -0.2992(2) 0.0429(8) Uani 1 1 d . . . . .
N2A N -0.2817(2) -0.0015(2) -0.2649(2) 0.0399(7) Uani 1 1 d . . . . .
N3A N -0.2937(2) -0.0492(2) -0.2392(3) 0.0511(9) Uani 1 1 d . . . . .
C1A C 0.0856(2) 0.1104(2) -0.1363(3) 0.0303(7) Uani 1 1 d . . . . .
C2A C -0.0062(2) 0.1281(2) -0.1945(2) 0.0295(7) Uani 1 1 d . . . . .
C3A C -0.0969(2) 0.0806(2) -0.2180(2) 0.0320(7) Uani 1 1 d . . . . .
H3A H -0.100015 0.038613 -0.196142 0.038 Uiso 1 1 calc R U . . .
C4A C -0.1829(2) 0.0941(2) -0.2730(3) 0.0313(7) Uani 1 1 d . . . . .
C5A C -0.1783(3) 0.1520(2) -0.3090(3) 0.0327(8) Uani 1 1 d . . . . .
H5A H -0.237388 0.159657 -0.348714 0.039 Uiso 1 1 calc R U . . .
C6A C -0.0878(2) 0.1992(2) -0.2872(2) 0.0296(7) Uani 1 1 d . . . . .
C7A C -0.0011(2) 0.1886(2) -0.2280(2) 0.0294(7) Uani 1 1 d . . . . .
H7A H 0.060950 0.222375 -0.210562 0.035 Uiso 1 1 calc R U . . .
C8A C -0.0867(3) 0.2607(2) -0.3283(3) 0.0311(7) Uani 1 1 d . . . . .
O1B O 1.3224(2) 0.7020(2) 0.5335(3) 0.0669(9) Uani 1 1 d . . . . .
O2B O 1.19864(18) 0.58548(17) 0.46893(18) 0.0386(6) Uani 1 1 d . . . . .
O3B O 1.44066(17) 0.38200(15) 0.68926(17) 0.0305(5) Uani 1 1 d . . . . .
O4B O 1.28981(18) 0.40772(18) 0.6523(2) 0.0465(7) Uani 1 1 d . . . . .
N1B N 1.6300(2) 0.5894(2) 0.6458(2) 0.0451(8) Uani 1 1 d . . . . .
N2B N 1.6552(2) 0.6397(2) 0.6192(2) 0.0431(8) Uani 1 1 d . . . . .
N3B N 1.6902(3) 0.6849(3) 0.6007(3) 0.0575(10) Uani 1 1 d . . . . .
C1B C 1.2884(3) 0.6256(3) 0.5160(3) 0.0387(9) Uani 1 1 d . . . . .
C2B C 1.3603(3) 0.5788(2) 0.5570(3) 0.0340(8) Uani 1 1 d . . . . .
C3B C 1.4579(3) 0.6045(2) 0.5775(3) 0.0353(8) Uani 1 1 d . . . . .
H3B H 1.477040 0.647157 0.561805 0.042 Uiso 1 1 calc R U . . .
C4B C 1.5278(2) 0.5671(2) 0.6214(3) 0.0333(8) Uani 1 1 d . . . . .
C5B C 1.5004(3) 0.5055(2) 0.6452(3) 0.0342(8) Uani 1 1 d . . . . .
H5B H 1.548151 0.479585 0.674003 0.041 Uiso 1 1 calc R U . . .
C6B C 1.4034(2) 0.4815(2) 0.6271(2) 0.0292(7) Uani 1 1 d . . . . .
C7B C 1.3324(3) 0.5169(2) 0.5803(2) 0.0312(7) Uani 1 1 d . . . . .
H7B H 1.265227 0.498382 0.564523 0.037 Uiso 1 1 calc R U . . .
C8B C 1.3732(2) 0.4183(2) 0.6573(3) 0.0313(7) Uani 1 1 d . . . . .
N4 N 0.2728(2) 0.0236(2) -0.1531(2) 0.0337(7) Uani 1 1 d . . . . .
N5 N 0.52022(19) -0.21067(18) -0.60314(19) 0.0263(6) Uani 1 1 d . . . . .
C9 C 0.3468(3) -0.0156(3) -0.1460(3) 0.0466(10) Uani 1 1 d . . . . .
H9 H 0.380283 -0.020772 -0.089803 0.056 Uiso 1 1 calc R U . . .
C10 C 0.3777(3) -0.0495(3) -0.2174(3) 0.0547(12) Uani 1 1 d . . . . .
H10 H 0.431301 -0.077142 -0.209447 0.066 Uiso 1 1 calc R U . . .
C11 C 0.3300(3) -0.0430(3) -0.3010(3) 0.0468(10) Uani 1 1 d . . . . .
C12 C 0.2568(3) 0.0020(3) -0.3047(3) 0.0525(11) Uani 1 1 d . . . . .
H12 H 0.225191 0.012042 -0.357863 0.063 Uiso 1 1 calc R U . . .
C13 C 0.2289(3) 0.0325(3) -0.2326(3) 0.0478(10) Uani 1 1 d . . . . .
H13 H 0.176229 0.061277 -0.238626 0.057 Uiso 1 1 calc R U . . .
C14 C 0.4672(3) -0.1503(3) -0.5998(3) 0.0393(9) Uani 1 1 d . . . . .
H14 H 0.443394 -0.138343 -0.652291 0.047 Uiso 1 1 calc R U . . .
C15 C 0.4446(3) -0.1037(3) -0.5248(3) 0.0519(11) Uani 1 1 d . . . . .
H15 H 0.406668 -0.060989 -0.526313 0.062 Uiso 1 1 calc R U . . .
C16 C 0.4783(3) -0.1202(3) -0.4462(3) 0.0493(11) Uani 1 1 d . . . . .
C17 C 0.5318(3) -0.1839(3) -0.4517(3) 0.0469(10) Uani 1 1 d . . . . .
H17 H 0.555275 -0.199009 -0.401556 0.056 Uiso 1 1 calc R U . . .
C18 C 0.5515(3) -0.2256(2) -0.5280(3) 0.0414(9) Uani 1 1 d . . . . .
H18 H 0.590108 -0.268078 -0.527965 0.050 Uiso 1 1 calc R U . . .
C19 C 0.3557(3) -0.0821(4) -0.3836(3) 0.0651(14) Uani 1 1 d . . . . .
H19A H 0.324809 -0.147056 -0.421075 0.078 Uiso 1 1 calc R U . . .
H19B H 0.325215 -0.055820 -0.425789 0.078 Uiso 1 1 calc R U . . .
C20 C 0.4567(3) -0.0702(4) -0.3612(3) 0.0748(17) Uani 1 1 d . . . . .
H20A H 0.489312 -0.089923 -0.313144 0.090 Uiso 1 1 calc R U . . .
H20B H 0.486369 -0.005595 -0.331212 0.090 Uiso 1 1 calc R U . . .
N4A N 0.81470(19) 0.87011(18) 0.93421(19) 0.0277(6) Uani 1 1 d . . . . .
N5A N 1.0474(2) 0.68512(18) 0.4782(2) 0.0297(6) Uani 1 1 d . . . . .
C9A C 0.8749(2) 0.9256(2) 0.9293(2) 0.0312(7) Uani 1 1 d . . . . .
H9A H 0.884707 0.988155 0.966857 0.037 Uiso 1 1 calc R U . . .
C10A C 0.9228(3) 0.8973(2) 0.8732(3) 0.0338(8) Uani 1 1 d . . . . .
H10A H 0.964612 0.939726 0.872748 0.041 Uiso 1 1 calc R U . . .
C11A C 0.9102(3) 0.8063(2) 0.8169(3) 0.0327(8) Uani 1 1 d . . . . .
C12A C 0.8472(3) 0.7486(2) 0.8213(3) 0.0361(8) Uani 1 1 d . . . . .
H12A H 0.834933 0.685819 0.783306 0.043 Uiso 1 1 calc R U . . .
C13A C 0.8027(3) 0.7826(2) 0.8806(3) 0.0335(8) Uani 1 1 d . . . . .
H13A H 0.761450 0.741769 0.883481 0.040 Uiso 1 1 calc R U . . .
C14A C 1.1092(3) 0.7542(2) 0.5639(3) 0.0384(9) Uani 1 1 d . . . . .
H14A H 1.175465 0.772360 0.576914 0.046 Uiso 1 1 calc R U . . .
C15A C 1.0789(3) 0.8001(2) 0.6342(3) 0.0399(9) Uani 1 1 d . . . . .
H15A H 1.124216 0.849368 0.693463 0.048 Uiso 1 1 calc R U . . .
C16A C 0.9832(3) 0.7742(2) 0.6183(3) 0.0369(8) Uani 1 1 d . . . . .
C17A C 0.9206(3) 0.7027(3) 0.5301(3) 0.0373(8) Uani 1 1 d . . . . .
H17A H 0.854476 0.682068 0.515791 0.045 Uiso 1 1 calc R U . . .
C18A C 0.9547(3) 0.6616(2) 0.4630(3) 0.0333(8) Uani 1 1 d . . . . .
H18A H 0.909824 0.613696 0.402334 0.040 Uiso 1 1 calc R U . . .
C19A C 0.9488(3) 0.8205(3) 0.6938(3) 0.0439(10) Uani 1 1 d . . . . .
H19C H 0.879281 0.822044 0.662943 0.053 Uiso 1 1 calc R U . . .
H19D H 0.988819 0.882887 0.737199 0.053 Uiso 1 1 calc R U . . .
C20A C 0.9586(3) 0.7713(3) 0.7514(3) 0.0421(9) Uani 1 1 d . . . . .
H20C H 0.927923 0.706779 0.706809 0.051 Uiso 1 1 calc R U . . .
H20D H 1.029171 0.778080 0.790057 0.051 Uiso 1 1 calc R U . . .
N4B N 1.3919(2) 0.34198(17) 0.82215(19) 0.0261(6) Uani 1 1 d . . . . .
N5B N 1.1683(2) 0.56879(18) 1.2866(2) 0.0280(6) Uani 1 1 d . . . . .
C9B C 1.3417(3) 0.2946(2) 0.8434(3) 0.0349(8) Uani 1 1 d . . . . .
H9B H 1.335531 0.231858 0.815593 0.042 Uiso 1 1 calc R U . . .
C10B C 1.2987(3) 0.3318(2) 0.9035(3) 0.0374(8) Uani 1 1 d . . . . .
H10B H 1.261781 0.294726 0.914249 0.045 Uiso 1 1 calc R U . . .
C11B C 1.3094(3) 0.4237(3) 0.9483(3) 0.0356(8) Uani 1 1 d . . . . .
C12B C 1.3656(3) 0.4733(2) 0.9298(3) 0.0363(8) Uani 1 1 d . . . . .
H12B H 1.377537 0.536658 0.960806 0.044 Uiso 1 1 calc R U . . .
C13B C 1.4038(3) 0.4309(2) 0.8666(2) 0.0338(8) Uani 1 1 d . . . . .
H13B H 1.440362 0.466296 0.853949 0.041 Uiso 1 1 calc R U . . .
C14B C 1.2522(2) 0.6182(2) 1.3044(3) 0.0333(8) Uani 1 1 d . . . . .
H14B H 1.278406 0.676942 1.357370 0.040 Uiso 1 1 calc R U . . .
C15B C 1.3015(2) 0.5872(2) 1.2492(3) 0.0352(8) Uani 1 1 d . . . . .
H15B H 1.360198 0.624642 1.264701 0.042 Uiso 1 1 calc R U . . .
C16B C 1.2666(3) 0.5025(2) 1.1718(3) 0.0334(8) Uani 1 1 d . . . . .
C17B C 1.1805(3) 0.4510(3) 1.1547(3) 0.0382(9) Uani 1 1 d . . . . .
H17B H 1.153422 0.391544 1.103167 0.046 Uiso 1 1 calc R U . . .
C18B C 1.1359(3) 0.4867(2) 1.2127(3) 0.0363(8) Uani 1 1 d . . . . .
H18B H 1.077517 0.450238 1.199180 0.044 Uiso 1 1 calc R U . . .
C19B C 1.3174(3) 0.4659(3) 1.1092(3) 0.0416(9) Uani 1 1 d . . . . .
H19E H 1.320261 0.404047 1.096735 0.050 Uiso 1 1 calc R U . . .
H19F H 1.385811 0.502552 1.142990 0.050 Uiso 1 1 calc R U . . .
C20B C 1.2639(3) 0.4662(3) 1.0146(3) 0.0428(9) Uani 1 1 d . . . . .
H20E H 1.194218 0.433404 0.983332 0.051 Uiso 1 1 calc R U . . .
H20F H 1.265323 0.528571 1.027075 0.051 Uiso 1 1 calc R U . . .
N4C N 0.9939(2) 0.50757(19) 0.3120(2) 0.0334(7) Uani 1 1 d . . . . .
N5C N 0.3726(2) 0.1632(2) 0.0489(2) 0.0331(7) Uani 1 1 d . . . . .
C9C C 0.9186(3) 0.4846(3) 0.2267(3) 0.0390(9) Uani 1 1 d . . . . .
H9C H 0.921525 0.516884 0.194242 0.047 Uiso 1 1 calc R U . . .
C10C C 0.8375(3) 0.4160(3) 0.1846(3) 0.0455(10) Uani 1 1 d . . . . .
H10C H 0.785951 0.401541 0.123820 0.055 Uiso 1 1 calc R U . . .
C11C C 0.8303(3) 0.3682(3) 0.2299(3) 0.0466(10) Uani 1 1 d . . . . .
C12C C 0.9076(3) 0.3922(3) 0.3178(3) 0.0503(11) Uani 1 1 d . . . . .
H12C H 0.905578 0.361667 0.352180 0.060 Uiso 1 1 calc R U . . .
C13C C 0.9883(3) 0.4612(2) 0.3559(3) 0.0372(8) Uani 1 1 d . . . . .
H13C H 1.041653 0.475838 0.415772 0.045 Uiso 1 1 calc R U . . .
C14C C 0.4112(3) 0.2037(3) 0.0136(3) 0.0501(10) Uani 1 1 d . . . . .
H14C H 0.372863 0.193227 -0.049817 0.060 Uiso 1 1 calc R U . . .
C15C C 0.5042(4) 0.2597(3) 0.0655(4) 0.0660(14) Uani 1 1 d . . . . .
H15C H 0.528690 0.286354 0.037212 0.079 Uiso 1 1 calc R U . . .
C16C C 0.5619(3) 0.2774(3) 0.1581(4) 0.0623(14) Uani 1 1 d . . . . .
C17C C 0.5210(3) 0.2377(3) 0.1955(3) 0.0581(13) Uani 1 1 d . . . . .
H17C H 0.556929 0.248642 0.259487 0.070 Uiso 1 1 calc R U . . .
C18C C 0.4275(3) 0.1823(3) 0.1390(3) 0.0444(9) Uani 1 1 d . . . . .
H18C H 0.400725 0.156098 0.166304 0.053 Uiso 1 1 calc R U . . .
C19C C 0.7372(3) 0.2966(3) 0.1852(3) 0.0581(12) Uani 1 1 d . . . . .
H19G H 0.709809 0.266618 0.114545 0.070 Uiso 1 1 calc R U . . .
H19H H 0.752720 0.251036 0.206175 0.070 Uiso 1 1 calc R U . . .
C20C C 0.6641(4) 0.3380(3) 0.2149(4) 0.104(3) Uani 1 1 d . . . . .
H20G H 0.661462 0.392634 0.208077 0.125 Uiso 1 1 calc R U . . .
H20H H 0.686317 0.356255 0.283537 0.125 Uiso 1 1 calc R U . . .
N4D N 1.2883(2) 0.20074(18) 0.6176(2) 0.0291(6) Uani 1 1 d . . . . .
C9D C 1.2117(2) 0.2294(2) 0.6290(3) 0.0337(8) Uani 1 1 d . . . . .
H9D H 1.221528 0.290821 0.671121 0.040 Uiso 1 1 calc R U . . .
C10D C 1.1190(3) 0.1745(2) 0.5828(3) 0.0396(9) Uani 1 1 d . . . . .
H10D H 1.067522 0.197565 0.595807 0.048 Uiso 1 1 calc R U . . .
C11D C 1.1007(3) 0.0855(3) 0.5173(3) 0.0382(8) Uani 1 1 d . . . . .
C12D C 1.1784(3) 0.0570(3) 0.5017(3) 0.0451(10) Uani 1 1 d . . . . .
H12D H 1.168996 -0.002803 0.455576 0.054 Uiso 1 1 calc R U . . .
C13D C 1.2701(3) 0.1151(2) 0.5528(3) 0.0409(9) Uani 1 1 d . . . . .
H13D H 1.322989 0.093310 0.541659 0.049 Uiso 1 1 calc R U . . .
C19D C 1.0022(3) 0.0227(3) 0.4704(3) 0.0495(10) Uani 1 1 d . . . . .
H19I H 0.989481 -0.023557 0.405479 0.074 Uiso 1 1 calc R U . . .
H19J H 0.950337 0.056077 0.463729 0.074 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O3B 2.000(2) . ?
Ni1 N4B 2.096(3) . ?
Ni1 N4D 2.107(3) . ?
Ni1 O2 2.138(2) 2_756 ?
Ni1 O1 2.141(2) 2_756 ?
Ni1 N5 2.144(3) 2_755 ?
Ni1 C1 2.454(3) 2_756 ?
Ni2 O2B 2.025(3) . ?
Ni2 N4C 2.071(3) . ?
Ni2 N5A 2.089(3) . ?
Ni2 N5B 2.111(3) 1_554 ?
Ni2 O3A 2.154(2) 2_665 ?
Ni2 O4A 2.193(2) 2_665 ?
Ni2 C8A 2.477(3) 2_665 ?
Ni3 O3 2.013(2) . ?
Ni3 N5C 2.076(3) . ?
Ni3 N4A 2.093(3) 2_666 ?
Ni3 N4 2.097(3) . ?
Ni3 O1A 2.143(2) . ?
Ni3 O2A 2.197(2) . ?
Ni3 C1A 2.483(3) . ?
O1 C1 1.269(4) . ?
O2 C1 1.262(4) . ?
O3 C8 1.268(4) . ?
O4 C8 1.220(4) . ?
N1 N2 1.235(5) . ?
N1 C4 1.429(5) . ?
N2 N3 1.130(5) . ?
C1 C2 1.500(5) . ?
C2 C7 1.388(5) . ?
C2 C3 1.392(5) . ?
C3 C4 1.374(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.408(5) . ?
C5 C6 1.372(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.397(5) . ?
C6 C8 1.537(5) . ?
C7 H7 0.9500 . ?
O1A C1A 1.262(4) . ?
O2A C1A 1.260(4) . ?
O3A C8A 1.255(4) . ?
O4A C8A 1.254(4) . ?
N1A N2A 1.248(4) . ?
N1A C4A 1.434(4) . ?
N2A N3A 1.120(4) . ?
C1A C2A 1.501(5) . ?
C2A C3A 1.386(5) . ?
C2A C7A 1.396(4) . ?
C3A C4A 1.382(5) . ?
C3A H3A 0.9500 . ?
C4A C5A 1.387(5) . ?
C5A C6A 1.392(5) . ?
C5A H5A 0.9500 . ?
C6A C7A 1.395(5) . ?
C6A C8A 1.502(5) . ?
C7A H7A 0.9500 . ?
O1B C1B 1.245(4) . ?
O2B C1B 1.258(4) . ?
O3B C8B 1.282(4) . ?
O4B C8B 1.237(4) . ?
N1B N2B 1.243(4) . ?
N1B C4B 1.429(4) . ?
N2B N3B 1.136(4) . ?
C1B C2B 1.512(5) . ?
C2B C7B 1.386(5) . ?
C2B C3B 1.390(5) . ?
C3B C4B 1.396(5) . ?
C3B H3B 0.9500 . ?
C4B C5B 1.386(5) . ?
C5B C6B 1.389(5) . ?
C5B H5B 0.9500 . ?
C6B C7B 1.406(5) . ?
C6B C8B 1.508(4) . ?
C7B H7B 0.9500 . ?
N4 C9 1.322(4) . ?
N4 C13 1.353(5) . ?
N5 C14 1.328(4) . ?
N5 C18 1.336(4) . ?
C9 C10 1.390(5) . ?
C9 H9 0.9500 . ?
C10 C11 1.397(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.373(5) . ?
C11 C19 1.505(5) . ?
C12 C13 1.367(5) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C15 1.382(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.408(6) . ?
C15 H15 0.9500 . ?
C16 C17 1.375(6) . ?
C16 C20 1.521(5) . ?
C17 C18 1.361(5) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C20 1.414(6) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
N4A C13A 1.337(4) . ?
N4A C9A 1.344(4) . ?
N5A C18A 1.339(4) . ?
N5A C14A 1.345(5) . ?
C9A C10A 1.368(4) . ?
C9A H9A 0.9500 . ?
C10A C11A 1.391(5) . ?
C10A H10A 0.9500 . ?
C11A C12A 1.393(5) . ?
C11A C20A 1.508(4) . ?
C12A C13A 1.378(4) . ?
C12A H12A 0.9500 . ?
C13A H13A 0.9500 . ?
C14A C15A 1.393(5) . ?
C14A H14A 0.9500 . ?
C15A C16A 1.388(5) . ?
C15A H15A 0.9500 . ?
C16A C17A 1.383(5) . ?
C16A C19A 1.507(5) . ?
C17A C18A 1.377(4) . ?
C17A H17A 0.9500 . ?
C18A H18A 0.9500 . ?
C19A C20A 1.526(5) . ?
C19A H19C 0.9900 . ?
C19A H19D 0.9900 . ?
C20A H20C 0.9900 . ?
C20A H20D 0.9900 . ?
N4B C9B 1.341(4) . ?
N4B C13B 1.342(4) . ?
N5B C18B 1.328(4) . ?
N5B C14B 1.350(4) . ?
C9B C10B 1.378(4) . ?
C9B H9B 0.9500 . ?
C10B C11B 1.391(5) . ?
C10B H10B 0.9500 . ?
C11B C12B 1.391(5) . ?
C11B C20B 1.502(4) . ?
C12B C13B 1.378(4) . ?
C12B H12B 0.9500 . ?
C13B H13B 0.9500 . ?
C14B C15B 1.378(4) . ?
C14B H14B 0.9500 . ?
C15B C16B 1.377(5) . ?
C15B H15B 0.9500 . ?
C16B C17B 1.401(5) . ?
C16B C19B 1.503(4) . ?
C17B C18B 1.367(5) . ?
C17B H17B 0.9500 . ?
C18B H18B 0.9500 . ?
C19B C20B 1.519(5) . ?
C19B H19E 0.9900 . ?
C19B H19F 0.9900 . ?
C20B H20E 0.9900 . ?
C20B H20F 0.9900 . ?
N4C C13C 1.330(4) . ?
N4C C9C 1.340(5) . ?
N5C C18C 1.329(5) . ?
N5C C14C 1.340(4) . ?
C9C C10C 1.374(5) . ?
C9C H9C 0.9500 . ?
C10C C11C 1.377(6) . ?
C10C H10C 0.9500 . ?
C11C C12C 1.380(6) . ?
C11C C19C 1.519(5) . ?
C12C C13C 1.388(5) . ?
C12C H12C 0.9500 . ?
C13C H13C 0.9500 . ?
C14C C15C 1.378(6) . ?
C14C H14C 0.9500 . ?
C15C C16C 1.378(7) . ?
C15C H15C 0.9500 . ?
C16C C17C 1.383(6) . ?
C16C C20C 1.508(6) . ?
C17C C18C 1.378(5) . ?
C17C H17C 0.9500 . ?
C18C H18C 0.9500 . ?
C19C C20C 1.479(6) . ?
C19C H19G 0.9900 . ?
C19C H19H 0.9900 . ?
C20C H20G 0.9900 . ?
C20C H20H 0.9900 . ?
N4D C9D 1.331(4) . ?
N4D C13D 1.340(4) . ?
C9D C10D 1.374(5) . ?
C9D H9D 0.9500 . ?
C10D C11D 1.385(5) . ?
C10D H10D 0.9500 . ?
C11D C12D 1.371(5) . ?
C11D C19D 1.497(5) . ?
C12D C13D 1.377(5) . ?
C12D H12D 0.9500 . ?
C13D H13D 0.9500 . ?
C19D C19D 1.541(7) 2_756 ?
C19D H19I 0.9900 . ?
C19D H19J 0.9900 . ?

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
O3B Ni1 N4B 93.42(10) . . ?
O3B Ni1 N4D 103.67(11) . . ?
N4B Ni1 N4D 90.31(10) . . ?
O3B Ni1 O2 159.22(10) . 2_756 ?
N4B Ni1 O2 88.44(9) . 2_756 ?
N4D Ni1 O2 97.01(10) . 2_756 ?
O3B Ni1 O1 97.27(9) . 2_756 ?
N4B Ni1 O1 88.88(10) . 2_756 ?
N4D Ni1 O1 159.06(10) . 2_756 ?
O2 Ni1 O1 62.05(9) 2_756 2_756 ?
O3B Ni1 N5 87.43(10) . 2_755 ?
N4B Ni1 N5 178.62(10) . 2_755 ?
N4D Ni1 N5 90.54(10) . 2_755 ?
O2 Ni1 N5 90.38(9) 2_756 2_755 ?
O1 Ni1 N5 89.94(9) 2_756 2_755 ?
O3B Ni1 C1 128.31(11) . 2_756 ?
N4B Ni1 C1 89.26(11) . 2_756 ?
N4D Ni1 C1 127.95(11) . 2_756 ?
O2 Ni1 C1 30.95(10) 2_756 2_756 ?
O1 Ni1 C1 31.12(9) 2_756 2_756 ?
N5 Ni1 C1 89.36(11) 2_755 2_756 ?
O2B Ni2 N4C 93.28(11) . . ?
O2B Ni2 N5A 90.57(10) . . ?
N4C Ni2 N5A 89.91(11) . . ?
O2B Ni2 N5B 88.31(10) . 1_554 ?
N4C Ni2 N5B 94.27(10) . 1_554 ?
N5A Ni2 N5B 175.72(11) . 1_554 ?
O2B Ni2 O3A 113.28(10) . 2_665 ?
N4C Ni2 O3A 153.43(11) . 2_665 ?
N5A Ni2 O3A 89.80(10) . 2_665 ?
N5B Ni2 O3A 86.86(9) 1_554 2_665 ?
O2B Ni2 O4A 173.64(10) . 2_665 ?
N4C Ni2 O4A 92.85(11) . 2_665 ?
N5A Ni2 O4A 91.11(10) . 2_665 ?
N5B Ni2 O4A 89.58(10) 1_554 2_665 ?
O3A Ni2 O4A 60.60(9) 2_665 2_665 ?
O2B Ni2 C8A 143.35(11) . 2_665 ?
N4C Ni2 C8A 123.12(12) . 2_665 ?
N5A Ni2 C8A 93.34(10) . 2_665 ?
N5B Ni2 C8A 85.12(10) 1_554 2_665 ?
O3A Ni2 C8A 30.45(10) 2_665 2_665 ?
O4A Ni2 C8A 30.39(10) 2_665 2_665 ?
O3 Ni3 N5C 107.84(11) . . ?
O3 Ni3 N4A 88.94(10) . 2_666 ?
N5C Ni3 N4A 93.16(11) . 2_666 ?
O3 Ni3 N4 92.74(11) . . ?
N5C Ni3 N4 89.66(11) . . ?
N4A Ni3 N4 176.10(11) 2_666 . ?
O3 Ni3 O1A 95.76(9) . . ?
N5C Ni3 O1A 156.23(10) . . ?
N4A Ni3 O1A 84.28(10) 2_666 . ?
N4 Ni3 O1A 92.05(10) . . ?
O3 Ni3 O2A 156.60(10) . . ?
N5C Ni3 O2A 95.31(10) . . ?
N4A Ni3 O2A 86.38(10) 2_666 . ?
N4 Ni3 O2A 90.69(10) . . ?
O1A Ni3 O2A 60.97(8) . . ?
O3 Ni3 C1A 126.21(11) . . ?
N5C Ni3 C1A 125.72(11) . . ?
N4A Ni3 C1A 83.98(11) 2_666 . ?
N4 Ni3 C1A 92.19(11) . . ?
O1A Ni3 C1A 30.53(9) . . ?
O2A Ni3 C1A 30.45(9) . . ?
C1 O1 Ni1 88.1(2) . 2_756 ?
C1 O2 Ni1 88.47(19) . 2_756 ?
C8 O3 Ni3 126.6(2) . . ?
N2 N1 C4 115.1(3) . . ?
N3 N2 N1 174.2(5) . . ?
O2 C1 O1 121.3(3) . . ?
O2 C1 C2 119.9(3) . . ?
O1 C1 C2 118.7(3) . . ?
O2 C1 Ni1 60.58(17) . 2_756 ?
O1 C1 Ni1 60.73(17) . 2_756 ?
C2 C1 Ni1 174.8(2) . 2_756 ?
C7 C2 C3 119.8(3) . . ?
C7 C2 C1 120.7(3) . . ?
C3 C2 C1 119.5(3) . . ?
C4 C3 C2 120.1(3) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C3 C4 C5 119.8(3) . . ?
C3 C4 N1 123.6(3) . . ?
C5 C4 N1 116.6(3) . . ?
C6 C5 C4 120.7(3) . . ?
C6 C5 H5 119.7 . . ?
C4 C5 H5 119.7 . . ?
C5 C6 C7 119.1(3) . . ?
C5 C6 C8 122.5(3) . . ?
C7 C6 C8 118.4(3) . . ?
C2 C7 C6 120.6(3) . . ?
C2 C7 H7 119.7 . . ?
C6 C7 H7 119.7 . . ?
O4 C8 O3 127.4(4) . . ?
O4 C8 C6 117.7(3) . . ?
O3 C8 C6 114.8(3) . . ?
C1A O1A Ni3 89.8(2) . . ?
C1A O2A Ni3 87.43(19) . . ?
C8A O3A Ni2 89.1(2) . 2_665 ?
C8A O4A Ni2 87.4(2) . 2_665 ?
N2A N1A C4A 114.7(3) . . ?
N3A N2A N1A 172.9(4) . . ?
O2A C1A O1A 121.7(3) . . ?
O2A C1A C2A 119.9(3) . . ?
O1A C1A C2A 118.4(3) . . ?
O2A C1A Ni3 62.12(18) . . ?
O1A C1A Ni3 59.63(17) . . ?
C2A C1A Ni3 177.9(2) . . ?
C3A C2A C7A 120.1(3) . . ?
C3A C2A C1A 119.0(3) . . ?
C7A C2A C1A 120.9(3) . . ?
C4A C3A C2A 120.4(3) . . ?
C4A C3A H3A 119.8 . . ?
C2A C3A H3A 119.8 . . ?
C3A C4A C5A 119.7(3) . . ?
C3A C4A N1A 124.2(3) . . ?
C5A C4A N1A 116.0(3) . . ?
C4A C5A C6A 120.5(3) . . ?
C4A C5A H5A 119.8 . . ?
C6A C5A H5A 119.8 . . ?
C5A C6A C7A 119.7(3) . . ?
C5A C6A C8A 118.5(3) . . ?
C7A C6A C8A 121.8(3) . . ?
C6A C7A C2A 119.5(3) . . ?
C6A C7A H7A 120.3 . . ?
C2A C7A H7A 120.3 . . ?
O4A C8A O3A 121.9(3) . . ?
O4A C8A C6A 119.7(3) . . ?
O3A C8A C6A 118.4(3) . . ?
O4A C8A Ni2 62.21(18) . 2_665 ?
O3A C8A Ni2 60.42(18) . 2_665 ?
C6A C8A Ni2 169.0(2) . 2_665 ?
C1B O2B Ni2 120.4(2) . . ?
C8B O3B Ni1 131.0(2) . . ?
N2B N1B C4B 117.0(3) . . ?
N3B N2B N1B 171.2(4) . . ?
O1B C1B O2B 125.1(3) . . ?
O1B C1B C2B 117.2(3) . . ?
O2B C1B C2B 117.7(3) . . ?
C7B C2B C3B 120.3(3) . . ?
C7B C2B C1B 121.7(3) . . ?
C3B C2B C1B 117.9(3) . . ?
C2B C3B C4B 119.6(3) . . ?
C2B C3B H3B 120.2 . . ?
C4B C3B H3B 120.2 . . ?
C5B C4B C3B 120.4(3) . . ?
C5B C4B N1B 115.8(3) . . ?
C3B C4B N1B 123.8(3) . . ?
C4B C5B C6B 120.2(3) . . ?
C4B C5B H5B 119.9 . . ?
C6B C5B H5B 119.9 . . ?
C5B C6B C7B 119.4(3) . . ?
C5B C6B C8B 121.0(3) . . ?
C7B C6B C8B 119.6(3) . . ?
C2B C7B C6B 120.1(3) . . ?
C2B C7B H7B 120.0 . . ?
C6B C7B H7B 120.0 . . ?
O4B C8B O3B 126.0(3) . . ?
O4B C8B C6B 119.4(3) . . ?
O3B C8B C6B 114.5(3) . . ?
C9 N4 C13 117.1(3) . . ?
C9 N4 Ni3 120.4(3) . . ?
C13 N4 Ni3 122.4(2) . . ?
C14 N5 C18 115.8(3) . . ?
C14 N5 Ni1 125.3(2) . 2_755 ?
C18 N5 Ni1 118.8(2) . 2_755 ?
N4 C9 C10 122.7(4) . . ?
N4 C9 H9 118.7 . . ?
C10 C9 H9 118.7 . . ?
C9 C10 C11 120.1(4) . . ?
C9 C10 H10 120.0 . . ?
C11 C10 H10 120.0 . . ?
C12 C11 C10 116.3(3) . . ?
C12 C11 C19 120.4(4) . . ?
C10 C11 C19 123.3(4) . . ?
C13 C12 C11 120.6(4) . . ?
C13 C12 H12 119.7 . . ?
C11 C12 H12 119.7 . . ?
N4 C13 C12 123.1(4) . . ?
N4 C13 H13 118.5 . . ?
C12 C13 H13 118.5 . . ?
N5 C14 C15 124.1(4) . . ?
N5 C14 H14 118.0 . . ?
C15 C14 H14 118.0 . . ?
C14 C15 C16 119.4(4) . . ?
C14 C15 H15 120.3 . . ?
C16 C15 H15 120.3 . . ?
C17 C16 C15 115.6(3) . . ?
C17 C16 C20 122.7(4) . . ?
C15 C16 C20 121.7(4) . . ?
C18 C17 C16 120.8(4) . . ?
C18 C17 H17 119.6 . . ?
C16 C17 H17 119.6 . . ?
N5 C18 C17 124.3(4) . . ?
N5 C18 H18 117.8 . . ?
C17 C18 H18 117.8 . . ?
C20 C19 C11 117.1(4) . . ?
C20 C19 H19A 108.0 . . ?
C11 C19 H19A 108.0 . . ?
C20 C19 H19B 108.0 . . ?
C11 C19 H19B 108.0 . . ?
H19A C19 H19B 107.3 . . ?
C19 C20 C16 114.8(4) . . ?
C19 C20 H20A 108.6 . . ?
C16 C20 H20A 108.6 . . ?
C19 C20 H20B 108.6 . . ?
C16 C20 H20B 108.6 . . ?
H20A C20 H20B 107.6 . . ?
C13A N4A C9A 116.6(3) . . ?
C13A N4A Ni3 123.7(2) . 2_666 ?
C9A N4A Ni3 118.8(2) . 2_666 ?
C18A N5A C14A 117.0(3) . . ?
C18A N5A Ni2 125.2(2) . . ?
C14A N5A Ni2 117.8(2) . . ?
N4A C9A C10A 123.8(3) . . ?
N4A C9A H9A 118.1 . . ?
C10A C9A H9A 118.1 . . ?
C9A C10A C11A 119.9(3) . . ?
C9A C10A H10A 120.0 . . ?
C11A C10A H10A 120.0 . . ?
C10A C11A C12A 116.5(3) . . ?
C10A C11A C20A 122.2(3) . . ?
C12A C11A C20A 121.3(3) . . ?
C13A C12A C11A 120.0(3) . . ?
C13A C12A H12A 120.0 . . ?
C11A C12A H12A 120.0 . . ?
N4A C13A C12A 123.3(3) . . ?
N4A C13A H13A 118.4 . . ?
C12A C13A H13A 118.4 . . ?
N5A C14A C15A 122.0(3) . . ?
N5A C14A H14A 119.0 . . ?
C15A C14A H14A 119.0 . . ?
C16A C15A C14A 120.5(3) . . ?
C16A C15A H15A 119.8 . . ?
C14A C15A H15A 119.8 . . ?
C17A C16A C15A 116.9(3) . . ?
C17A C16A C19A 121.2(3) . . ?
C15A C16A C19A 121.9(4) . . ?
C18A C17A C16A 119.7(3) . . ?
C18A C17A H17A 120.2 . . ?
C16A C17A H17A 120.2 . . ?
N5A C18A C17A 123.9(3) . . ?
N5A C18A H18A 118.0 . . ?
C17A C18A H18A 118.0 . . ?
C16A C19A C20A 110.2(3) . . ?
C16A C19A H19C 109.6 . . ?
C20A C19A H19C 109.6 . . ?
C16A C19A H19D 109.6 . . ?
C20A C19A H19D 109.6 . . ?
H19C C19A H19D 108.1 . . ?
C11A C20A C19A 111.9(3) . . ?
C11A C20A H20C 109.2 . . ?
C19A C20A H20C 109.2 . . ?
C11A C20A H20D 109.2 . . ?
C19A C20A H20D 109.2 . . ?
H20C C20A H20D 107.9 . . ?
C9B N4B C13B 116.7(3) . . ?
C9B N4B Ni1 120.6(2) . . ?
C13B N4B Ni1 122.3(2) . . ?
C18B N5B C14B 116.0(3) . . ?
C18B N5B Ni2 125.0(2) . 1_556 ?
C14B N5B Ni2 118.9(2) . 1_556 ?
N4B C9B C10B 123.6(3) . . ?
N4B C9B H9B 118.2 . . ?
C10B C9B H9B 118.2 . . ?
C9B C10B C11B 119.7(3) . . ?
C9B C10B H10B 120.1 . . ?
C11B C10B H10B 120.1 . . ?
C12B C11B C10B 116.6(3) . . ?
C12B C11B C20B 122.5(3) . . ?
C10B C11B C20B 120.9(3) . . ?
C13B C12B C11B 120.2(3) . . ?
C13B C12B H12B 119.9 . . ?
C11B C12B H12B 119.9 . . ?
N4B C13B C12B 123.1(3) . . ?
N4B C13B H13B 118.5 . . ?
C12B C13B H13B 118.5 . . ?
N5B C14B C15B 122.9(3) . . ?
N5B C14B H14B 118.6 . . ?
C15B C14B H14B 118.6 . . ?
C16B C15B C14B 120.8(3) . . ?
C16B C15B H15B 119.6 . . ?
C14B C15B H15B 119.6 . . ?
C15B C16B C17B 116.1(3) . . ?
C15B C16B C19B 122.7(3) . . ?
C17B C16B C19B 121.2(3) . . ?
C18B C17B C16B 119.6(3) . . ?
C18B C17B H17B 120.2 . . ?
C16B C17B H17B 120.2 . . ?
N5B C18B C17B 124.6(3) . . ?
N5B C18B H18B 117.7 . . ?
C17B C18B H18B 117.7 . . ?
C16B C19B C20B 111.2(3) . . ?
C16B C19B H19E 109.4 . . ?
C20B C19B H19E 109.4 . . ?
C16B C19B H19F 109.4 . . ?
C20B C19B H19F 109.4 . . ?
H19E C19B H19F 108.0 . . ?
C11B C20B C19B 112.0(3) . . ?
C11B C20B H20E 109.2 . . ?
C19B C20B H20E 109.2 . . ?
C11B C20B H20F 109.2 . . ?
C19B C20B H20F 109.2 . . ?
H20E C20B H20F 107.9 . . ?
C13C N4C C9C 117.7(3) . . ?
C13C N4C Ni2 122.0(3) . . ?
C9C N4C Ni2 119.7(3) . . ?
C18C N5C C14C 116.4(3) . . ?
C18C N5C Ni3 125.4(2) . . ?
C14C N5C Ni3 118.2(3) . . ?
N4C C9C C10C 122.4(4) . . ?
N4C C9C H9C 118.8 . . ?
C10C C9C H9C 118.8 . . ?
C9C C10C C11C 120.5(4) . . ?
C9C C10C H10C 119.8 . . ?
C11C C10C H10C 119.8 . . ?
C10C C11C C12C 117.1(4) . . ?
C10C C11C C19C 119.7(4) . . ?
C12C C11C C19C 123.1(4) . . ?
C11C C12C C13C 119.8(4) . . ?
C11C C12C H12C 120.1 . . ?
C13C C12C H12C 120.1 . . ?
N4C C13C C12C 122.6(4) . . ?
N4C C13C H13C 118.7 . . ?
C12C C13C H13C 118.7 . . ?
N5C C14C C15C 122.8(5) . . ?
N5C C14C H14C 118.6 . . ?
C15C C14C H14C 118.6 . . ?
C14C C15C C16C 120.5(4) . . ?
C14C C15C H15C 119.8 . . ?
C16C C15C H15C 119.8 . . ?
C15C C16C C17C 116.7(4) . . ?
C15C C16C C20C 120.7(5) . . ?
C17C C16C C20C 122.6(5) . . ?
C18C C17C C16C 119.4(5) . . ?
C18C C17C H17C 120.3 . . ?
C16C C17C H17C 120.3 . . ?
N5C C18C C17C 124.1(4) . . ?
N5C C18C H18C 117.9 . . ?
C17C C18C H18C 117.9 . . ?
C20C C19C C11C 109.5(4) . . ?
C20C C19C H19G 109.8 . . ?
C11C C19C H19G 109.8 . . ?
C20C C19C H19H 109.8 . . ?
C11C C19C H19H 109.8 . . ?
H19G C19C H19H 108.2 . . ?
C19C C20C C16C 113.8(4) . . ?
C19C C20C H20G 108.8 . . ?
C16C C20C H20G 108.8 . . ?
C19C C20C H20H 108.8 . . ?
C16C C20C H20H 108.8 . . ?
H20G C20C H20H 107.7 . . ?
C9D N4D C13D 116.6(3) . . ?
C9D N4D Ni1 121.9(2) . . ?
C13D N4D Ni1 120.6(2) . . ?
N4D C9D C10D 123.2(3) . . ?
N4D C9D H9D 118.4 . . ?
C10D C9D H9D 118.4 . . ?
C9D C10D C11D 120.1(3) . . ?
C9D C10D H10D 120.0 . . ?
C11D C10D H10D 120.0 . . ?
C12D C11D C10D 116.7(3) . . ?
C12D C11D C19D 121.9(4) . . ?
C10D C11D C19D 121.3(4) . . ?
C11D C12D C13D 120.1(4) . . ?
C11D C12D H12D 119.9 . . ?
C13D C12D H12D 119.9 . . ?
N4D C13D C12D 123.2(3) . . ?
N4D C13D H13D 118.4 . . ?
C12D C13D H13D 118.4 . . ?
C11D C19D C19D 111.1(4) . 2_756 ?
C11D C19D H19I 109.4 . . ?
C19D C19D H19I 109.4 2_756 . ?
C11D C19D H19J 109.4 . . ?
C19D C19D H19J 109.4 2_756 . ?
H19I C19D H19J 108.0 . . ?

_refine_diff_density_max         2.298
_refine_diff_density_min         -1.395
_refine_diff_density_rms         0.130

