# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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_111
_database_code_depnum_ccdc_archive 'CCDC 2291721'
loop_
_audit_author_name
_audit_author_address
'Xin Guo'
;Beijing Institute Of Technology
China
;
_audit_update_record             
;
2023-08-30 deposited with the CCDC.	2023-11-21 downloaded from the CCDC.
;
_audit_creation_date             2022-10-17
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C32 H46 N8 Ni2 O6, 2(Cl), 3(H2 O)'
_chemical_formula_sum            'C32 H52 Cl2 N8 Ni2 O9'
_chemical_formula_weight         881.13
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
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                   10.2398(4)
_cell_length_b                   15.3856(6)
_cell_length_c                   12.1399(4)
_cell_angle_alpha                90
_cell_angle_beta                 102.111(3)
_cell_angle_gamma                90
_cell_volume                     1870.02(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6897
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.5660
_cell_measurement_theta_min      4.2810
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.213
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             924
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0654
_diffrn_reflns_av_unetI/netI     0.0466
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.901
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            25225
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.901
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.664
_diffrn_reflns_theta_min         3.555
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.901
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3927
_reflns_number_total             4760
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         1.770
_refine_diff_density_min         -0.783
_refine_diff_density_rms         0.124
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         4760
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0695
_refine_ls_R_factor_gt           0.0564
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1070P)²+1.6509P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1629
_refine_ls_wR_factor_ref         0.1715
_refine_special_details          SQUEEZE
_olex2_refinement_description    
;
1. Others
 Fixed Sof: O5(0.5) HB(0.5) HC(0.5)
2.a Free rotating group:
 O4(H,HA), O5(HB,HC)
2.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B),
 C14(H14A,H14B), C16(H16A,H16B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7)
2.d X=CH2 refined with riding coordinates:
 N3(H3A,H3B), N4(H4A,H4B)
2.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.40452(4) 0.43212(2) 0.43970(3) 0.02399(15) Uani 1 1 d . . . . .
O1 O 0.5900(2) 0.43751(13) 0.53891(19) 0.0274(4) Uani 1 1 d . . . . .
O2 O 0.4850(2) 0.44172(15) 0.29734(19) 0.0341(5) Uani 1 1 d . . . . .
O3 O 0.3135(2) 0.41808(15) 0.57661(19) 0.0326(5) Uani 1 1 d . . . . .
N1 N 0.4147(3) 0.29612(17) 0.4563(2) 0.0285(5) Uani 1 1 d . . . . .
N2 N 0.2290(3) 0.45099(18) 0.3182(2) 0.0282(5) Uani 1 1 d . . . . .
N3 N 0.4524(4) 0.5137(2) 0.1325(3) 0.0493(8) Uani 1 1 d . . . . .
H3A H 0.533734 0.505841 0.126400 0.059 Uiso 1 1 calc R . . . .
H3B H 0.397959 0.541680 0.081067 0.059 Uiso 1 1 calc R . . . .
N4 N 0.3099(3) 0.3305(2) 0.7239(2) 0.0427(7) Uani 1 1 d . . . . .
H4A H 0.269987 0.368966 0.756277 0.051 Uiso 1 1 calc R . . . .
H4B H 0.330002 0.280838 0.755447 0.051 Uiso 1 1 calc R . . . .
C1 C 1.0227(4) 0.1988(2) 0.5748(4) 0.0438(8) Uani 1 1 d . . . . .
H1A H 1.101969 0.228569 0.565164 0.066 Uiso 1 1 calc GR . . . .
H1B H 1.000710 0.154171 0.518758 0.066 Uiso 1 1 calc GR . . . .
H1C H 1.038031 0.173091 0.648461 0.066 Uiso 1 1 calc GR . . . .
C2 C 0.9087(3) 0.2627(2) 0.5624(3) 0.0344(7) Uani 1 1 d . . . . .
C3 C 0.9294(3) 0.3477(2) 0.6010(3) 0.0342(7) Uani 1 1 d . . . . .
H3 H 1.015615 0.364916 0.634596 0.041 Uiso 1 1 calc R . . . .
C4 C 0.8259(3) 0.4082(2) 0.5914(3) 0.0290(6) Uani 1 1 d . . . . .
C5 C 0.6929(3) 0.38337(19) 0.5419(2) 0.0258(6) Uani 1 1 d . . . . .
C6 C 0.6721(3) 0.2973(2) 0.4996(2) 0.0276(6) Uani 1 1 d . . . . .
C7 C 0.7794(3) 0.2394(2) 0.5125(3) 0.0324(7) Uani 1 1 d . . . . .
H7 H 0.763200 0.182756 0.486390 0.039 Uiso 1 1 calc R . . . .
C8 C 0.5416(3) 0.2650(2) 0.4273(3) 0.0324(6) Uani 1 1 d . . . . .
H8A H 0.540146 0.281339 0.349890 0.039 Uiso 1 1 calc R . . . .
H8B H 0.542019 0.202002 0.430432 0.039 Uiso 1 1 calc R . . . .
C9 C 0.3034(3) 0.2480(2) 0.3825(3) 0.0394(8) Uani 1 1 d . . . . .
H9A H 0.289387 0.193993 0.419540 0.047 Uiso 1 1 calc R . . . .
H9B H 0.330677 0.233269 0.312982 0.047 Uiso 1 1 calc R . . . .
C10 C 0.1706(4) 0.2966(2) 0.3532(3) 0.0396(8) Uani 1 1 d . . . . .
H10A H 0.100552 0.255216 0.323615 0.048 Uiso 1 1 calc R . . . .
H10B H 0.151384 0.320765 0.421837 0.048 Uiso 1 1 calc R . . . .
C11 C 0.1662(4) 0.3687(2) 0.2691(3) 0.0384(7) Uani 1 1 d . . . . .
H11A H 0.211155 0.349420 0.210579 0.046 Uiso 1 1 calc R . . . .
H11B H 0.073708 0.380156 0.233919 0.046 Uiso 1 1 calc R . . . .
C12 C 0.1317(3) 0.5007(2) 0.3690(3) 0.0342(7) Uani 1 1 d . . . . .
H12A H 0.114395 0.468008 0.432723 0.041 Uiso 1 1 calc R . . . .
H12B H 0.048315 0.504538 0.313891 0.041 Uiso 1 1 calc R . . . .
C13 C 0.4110(3) 0.4826(2) 0.2207(3) 0.0322(6) Uani 1 1 d . . . . .
C14 C 0.2683(3) 0.5030(2) 0.2267(3) 0.0343(7) Uani 1 1 d . . . . .
H14A H 0.259818 0.564515 0.241477 0.041 Uiso 1 1 calc R . . . .
H14B H 0.209524 0.489480 0.155172 0.041 Uiso 1 1 calc R . . . .
C15 C 0.3404(3) 0.3477(2) 0.6253(3) 0.0309(6) Uani 1 1 d . . . . .
C16 C 0.4161(3) 0.2788(2) 0.5767(3) 0.0333(7) Uani 1 1 d . . . . .
H16A H 0.507693 0.277110 0.618784 0.040 Uiso 1 1 calc R . . . .
H16B H 0.376082 0.222441 0.583810 0.040 Uiso 1 1 calc R . . . .
Cl1 Cl 0.22270(10) 0.49921(7) 0.89006(8) 0.0503(3) Uani 1 1 d . . . . .
O4 O 0.3335(4) 0.1485(2) 0.7942(3) 0.0607(8) Uani 1 1 d . . . . .
H H 0.296663 0.119915 0.736010 0.091 Uiso 1 1 d G . . . .
HA H 0.297893 0.128870 0.846380 0.091 Uiso 1 1 d G . . . .
O5 O 0.4920(12) 0.0697(6) 0.5011(10) 0.096(3) Uani 0.5 1 d . . P A -1
HB H 0.515466 0.034116 0.455257 0.144 Uiso 0.5 1 d G . P A -1
HC H 0.492000 0.039679 0.559878 0.144 Uiso 0.5 1 d G . P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1 2.022(2) 3_666 ?
Ni1 O1 2.026(2) . ?
Ni1 O2 2.070(2) . ?
Ni1 O3 2.080(2) . ?
Ni1 N1 2.103(3) . ?
Ni1 N2 2.092(3) . ?
O1 C5 1.338(3) . ?
O2 C13 1.241(4) . ?
O3 C15 1.237(4) . ?
N1 C8 1.494(4) . ?
N1 C9 1.490(4) . ?
N1 C16 1.483(4) . ?
N2 C11 1.488(4) . ?
N2 C12 1.489(4) . ?
N2 C14 1.491(4) . ?
N3 H3A 0.8600 . ?
N3 H3B 0.8600 . ?
N3 C13 1.322(4) . ?
N4 H4A 0.8600 . ?
N4 H4B 0.8600 . ?
N4 C15 1.325(4) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C1 C2 1.509(5) . ?
C2 C3 1.390(5) . ?
C2 C7 1.382(5) . ?
C3 H3 0.9300 . ?
C3 C4 1.397(4) . ?
C4 C5 1.421(4) . ?
C4 C12 1.516(4) 3_666 ?
C5 C6 1.420(4) . ?
C6 C7 1.398(4) . ?
C6 C8 1.520(4) . ?
C7 H7 0.9300 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.527(5) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C11 1.501(5) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C14 1.510(5) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.506(5) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
O4 H 0.8499 . ?
O4 HA 0.8501 . ?
O5 HB 0.8502 . ?
O5 HC 0.8498 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni1 O1 83.44(9) 3_666 . ?
O1 Ni1 O2 90.31(9) . . ?
O1 Ni1 O2 91.78(9) 3_666 . ?
O1 Ni1 O3 90.32(9) 3_666 . ?
O1 Ni1 O3 92.89(9) . . ?
O1 Ni1 N1 167.29(10) 3_666 . ?
O1 Ni1 N1 87.83(9) . . ?
O1 Ni1 N2 87.11(9) 3_666 . ?
O1 Ni1 N2 166.61(10) . . ?
O2 Ni1 O3 176.35(9) . . ?
O2 Ni1 N1 97.50(10) . . ?
O2 Ni1 N2 80.50(10) . . ?
O3 Ni1 N1 80.89(9) . . ?
O3 Ni1 N2 96.63(10) . . ?
N2 Ni1 N1 102.93(10) . . ?
Ni1 O1 Ni1 96.56(9) 3_666 . ?
C5 O1 Ni1 127.86(19) . 3_666 ?
C5 O1 Ni1 128.70(18) . . ?
C13 O2 Ni1 112.0(2) . . ?
C15 O3 Ni1 112.4(2) . . ?
C8 N1 Ni1 108.93(19) . . ?
C9 N1 Ni1 114.8(2) . . ?
C9 N1 C8 107.0(2) . . ?
C16 N1 Ni1 105.30(18) . . ?
C16 N1 C8 110.2(2) . . ?
C16 N1 C9 110.5(3) . . ?
C11 N2 Ni1 113.6(2) . . ?
C11 N2 C12 109.4(3) . . ?
C11 N2 C14 108.7(3) . . ?
C12 N2 Ni1 109.23(19) . . ?
C12 N2 C14 110.0(3) . . ?
C14 N2 Ni1 105.88(19) . . ?
H3A N3 H3B 120.0 . . ?
C13 N3 H3A 120.0 . . ?
C13 N3 H3B 120.0 . . ?
H4A N4 H4B 120.0 . . ?
C15 N4 H4A 120.0 . . ?
C15 N4 H4B 120.0 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
C3 C2 C1 121.2(3) . . ?
C7 C2 C1 121.6(3) . . ?
C7 C2 C3 117.1(3) . . ?
C2 C3 H3 118.7 . . ?
C2 C3 C4 122.6(3) . . ?
C4 C3 H3 118.7 . . ?
C3 C4 C5 120.0(3) . . ?
C3 C4 C12 115.4(3) . 3_666 ?
C5 C4 C12 124.6(3) . 3_666 ?
O1 C5 C4 121.6(3) . . ?
O1 C5 C6 120.9(3) . . ?
C6 C5 C4 117.5(3) . . ?
C5 C6 C8 124.1(3) . . ?
C7 C6 C5 120.0(3) . . ?
C7 C6 C8 115.6(3) . . ?
C2 C7 C6 122.8(3) . . ?
C2 C7 H7 118.6 . . ?
C6 C7 H7 118.6 . . ?
N1 C8 C6 117.5(2) . . ?
N1 C8 H8A 107.9 . . ?
N1 C8 H8B 107.9 . . ?
C6 C8 H8A 107.9 . . ?
C6 C8 H8B 107.9 . . ?
H8A C8 H8B 107.2 . . ?
N1 C9 H9A 108.4 . . ?
N1 C9 H9B 108.4 . . ?
N1 C9 C10 115.4(3) . . ?
H9A C9 H9B 107.5 . . ?
C10 C9 H9A 108.4 . . ?
C10 C9 H9B 108.4 . . ?
C9 C10 H10A 108.6 . . ?
C9 C10 H10B 108.6 . . ?
H10A C10 H10B 107.6 . . ?
C11 C10 C9 114.7(3) . . ?
C11 C10 H10A 108.6 . . ?
C11 C10 H10B 108.6 . . ?
N2 C11 C10 114.1(3) . . ?
N2 C11 H11A 108.7 . . ?
N2 C11 H11B 108.7 . . ?
C10 C11 H11A 108.7 . . ?
C10 C11 H11B 108.7 . . ?
H11A C11 H11B 107.6 . . ?
N2 C12 C4 115.8(3) . 3_666 ?
N2 C12 H12A 108.3 . . ?
N2 C12 H12B 108.3 . . ?
C4 C12 H12A 108.3 3_666 . ?
C4 C12 H12B 108.3 3_666 . ?
H12A C12 H12B 107.4 . . ?
O2 C13 N3 122.8(3) . . ?
O2 C13 C14 121.0(3) . . ?
N3 C13 C14 116.2(3) . . ?
N2 C14 C13 109.8(3) . . ?
N2 C14 H14A 109.7 . . ?
N2 C14 H14B 109.7 . . ?
C13 C14 H14A 109.7 . . ?
C13 C14 H14B 109.7 . . ?
H14A C14 H14B 108.2 . . ?
O3 C15 N4 122.4(3) . . ?
O3 C15 C16 120.7(3) . . ?
N4 C15 C16 116.9(3) . . ?
N1 C16 C15 111.1(3) . . ?
N1 C16 H16A 109.4 . . ?
N1 C16 H16B 109.4 . . ?
C15 C16 H16A 109.4 . . ?
C15 C16 H16B 109.4 . . ?
H16A C16 H16B 108.0 . . ?
H O4 HA 104.5 . . ?
HB O5 HC 104.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 O1 C5 C4 17.7(4) 3_666 . . . ?
Ni1 O1 C5 C4 161.6(2) . . . . ?
Ni1 O1 C5 C6 -165.0(2) 3_666 . . . ?
Ni1 O1 C5 C6 -21.1(4) . . . . ?
Ni1 O2 C13 N3 164.6(3) . . . . ?
Ni1 O2 C13 C14 -12.6(4) . . . . ?
Ni1 O3 C15 N4 169.6(3) . . . . ?
Ni1 O3 C15 C16 -7.4(4) . . . . ?
Ni1 N1 C8 C6 61.6(3) . . . . ?
Ni1 N1 C9 C10 -29.5(4) . . . . ?
Ni1 N1 C16 C15 30.2(3) . . . . ?
Ni1 N2 C11 C10 39.7(4) . . . . ?
Ni1 N2 C12 C4 63.1(3) . . . 3_666 ?
Ni1 N2 C14 C13 30.0(3) . . . . ?
O1 C5 C6 C7 -174.3(3) . . . . ?
O1 C5 C6 C8 13.3(4) . . . . ?
O2 C13 C14 N2 -12.8(4) . . . . ?
O3 C15 C16 N1 -16.8(4) . . . . ?
N1 C9 C10 C11 73.9(4) . . . . ?
N3 C13 C14 N2 169.8(3) . . . . ?
N4 C15 C16 N1 166.1(3) . . . . ?
C1 C2 C3 C4 -179.6(3) . . . . ?
C1 C2 C7 C6 -179.8(3) . . . . ?
C2 C3 C4 C5 0.9(5) . . . . ?
C2 C3 C4 C12 -176.1(3) . . . 3_666 ?
C3 C2 C7 C6 0.3(5) . . . . ?
C3 C4 C5 O1 174.9(3) . . . . ?
C3 C4 C5 C6 -2.5(4) . . . . ?
C4 C5 C6 C7 3.0(4) . . . . ?
C4 C5 C6 C8 -169.3(3) . . . . ?
C5 C6 C7 C2 -2.0(5) . . . . ?
C5 C6 C8 N1 -39.0(4) . . . . ?
C7 C2 C3 C4 0.3(5) . . . . ?
C7 C6 C8 N1 148.3(3) . . . . ?
C8 N1 C9 C10 -150.5(3) . . . . ?
C8 N1 C16 C15 147.5(3) . . . . ?
C8 C6 C7 C2 171.0(3) . . . . ?
C9 N1 C8 C6 -173.7(3) . . . . ?
C9 N1 C16 C15 -94.4(3) . . . . ?
C9 C10 C11 N2 -80.5(4) . . . . ?
C11 N2 C12 C4 -172.0(3) . . . 3_666 ?
C11 N2 C14 C13 -92.3(3) . . . . ?
C12 N2 C11 C10 -82.6(4) . . . . ?
C12 N2 C14 C13 147.9(3) . . . . ?
C12 C4 C5 O1 -8.5(5) 3_666 . . . ?
C12 C4 C5 C6 174.2(3) 3_666 . . . ?
C14 N2 C11 C10 157.3(3) . . . . ?
C14 N2 C12 C4 -52.7(4) . . . 3_666 ?
C16 N1 C8 C6 -53.5(4) . . . . ?
C16 N1 C9 C10 89.4(4) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT420_111                 
;
PROBLEM: D-H Bond Without Acceptor  O4       --Ha       .     Please Check 
RESPONSE: Because the hydrogen atoms on O4 is stablilized by O-H pi (benzene
ring) interaction.
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1102-ni2-z_sq_sq
_database_code_depnum_ccdc_archive 'CCDC 2291722'
loop_
_audit_author_name
_audit_author_address
'Xin Guo'
;Beijing Institute Of Technology
China
;
_audit_update_record             
;
2023-08-30 deposited with the CCDC.	2023-11-21 downloaded from the CCDC.
;
_audit_creation_date             2022-11-04
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C32 H46 N8 Ni2 O6, 2(C2 H3 O2), H2 O, 2(C H4 O)'
_chemical_formula_sum            'C38 H62 N8 Ni2 O13'
_chemical_formula_weight         956.37
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   15.3815(5)
_cell_length_b                   18.3733(4)
_cell_length_c                   16.7250(5)
_cell_angle_alpha                90
_cell_angle_beta                 111.493(3)
_cell_angle_gamma                90
_cell_volume                     4398.0(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    16515
_cell_measurement_temperature    99.85(10)
_cell_measurement_theta_max      30.0230
_cell_measurement_theta_min      4.0320
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.927
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56452
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2024
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0253
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.911
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            28956
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.911
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.739
_diffrn_reflns_theta_min         3.584
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -63.00   5.10   0.30   12.00    --    0.10 -82.00  30.00  227
  2  ω    -40.00  29.90   0.30   12.00    --    0.10 -82.00 120.00  233
  3  ω    -62.00  -8.90   0.30   12.00    --    0.10 -57.00  30.00  177
  4  ω     36.00  89.10   0.30   12.00    --    0.10  38.00  90.00  177
  5  ω    -49.00 -22.90   0.30   12.00    --    0.10 -82.00-180.00   87
  6  ω    -65.00 -40.70   0.30   12.00    --    0.10 -77.00-120.00   81
  7  ω     45.00  78.00   0.30   12.00    --    0.10  38.00 120.00  110
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5261
_reflns_number_total             5711
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_refine_diff_density_max         0.608
_refine_diff_density_min         -0.678
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         5711
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0350
_refine_ls_restrained_S_all      1.060
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0335P)²+9.7242P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0865
_refine_ls_wR_factor_ref         0.0882
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Others
 Sof(H9BC)=Sof(H9BD)=Sof(H12C)=Sof(H12D)=Sof(C10)=Sof(H10A)=Sof(H10B)=1-FVAR(1)
 Sof(H9AA)=Sof(H9AB)=Sof(H12A)=Sof(H12B)=Sof(C11)=Sof(H11A)=Sof(H11B)=FVAR(1)
 Fixed Sof: O8(0.5) H8C(0.5) H8D(0.5) O7(0.5) H7A(0.5) O6(0.5) H6(0.5)
 C20(0.5) H20A(0.5) H20B(0.5) H20C(0.5) C21(0.5) H21A(0.5) H21B(0.5) H21C(0.5)
3.a Free rotating group:
 O8(H8C,H8D)
3.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C14(H14A,H14B), C8(H8A,H8B), C9(H9AA,H9AB), C9(H9BC,H9BD),
 C17(H17A,H17B), C12(H12A,H12B), C12(H12C,H12D), C11(H11A,H11B), C10(H10A,H10B)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7)
3.d X=CH2 refined with riding coordinates:
 N4(H4A,H4B), N3(H3A,H3B)
3.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C)
3.f Idealised tetrahedral OH refined as rotating group:
 O7(H7A), O6(H6)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.57981(2) -0.03961(2) 1.06691(2) 0.01456(7) Uani 1 1 d . . . . .
O1 O 0.55819(8) 0.05323(6) 0.99859(7) 0.0158(2) Uani 1 1 d . . . . .
O2 O 0.55023(8) 0.00533(7) 1.17080(7) 0.0184(2) Uani 1 1 d . . . . .
O3 O 0.37376(9) 0.09423(7) 1.02114(8) 0.0259(3) Uani 1 1 d . . . . .
N2 N 0.41604(12) 0.14607(9) 0.88808(9) 0.0265(3) Uani 1 1 d . . . . .
N1 N 0.71230(10) -0.00035(11) 1.14087(9) 0.0299(4) Uani 1 1 d . . . . .
N4 N 0.62520(11) 0.06233(9) 1.29764(9) 0.0248(3) Uani 1 1 d . . . . .
H4A H 0.581196 0.050965 1.317382 0.030 Uiso 1 1 calc R U . . .
H4B H 0.674119 0.087630 1.329717 0.030 Uiso 1 1 calc R U . . .
N3 N 0.34464(16) 0.20935(11) 1.05430(11) 0.0439(5) Uani 1 1 d . . . . .
H3A H 0.311682 0.194202 1.084379 0.053 Uiso 1 1 calc R U . . .
H3B H 0.352816 0.256256 1.049055 0.053 Uiso 1 1 calc R U . . .
C15 C 0.38181(15) 0.16172(11) 1.01707(11) 0.0313(4) Uani 1 1 d . . . . .
C5 C 0.61960(12) 0.09041(10) 0.97476(10) 0.0212(3) Uani 1 1 d . . . . .
C13 C 0.48885(15) 0.15588(10) 0.85056(12) 0.0282(4) Uani 1 1 d . . . . .
H13A H 0.483524 0.206058 0.827689 0.034 Uiso 1 1 calc R U . . .
H13B H 0.474655 0.122290 0.801108 0.034 Uiso 1 1 calc R U . . .
C14 C 0.43772(18) 0.19124(10) 0.96643(12) 0.0342(5) Uani 1 1 d . . . . .
H14A H 0.420726 0.242642 0.950512 0.041 Uiso 1 1 calc R U . . .
H14B H 0.505356 0.188909 1.001348 0.041 Uiso 1 1 calc R U . . .
C16 C 0.61781(12) 0.04141(10) 1.21991(10) 0.0209(3) Uani 1 1 d . . . . .
C6 C 0.71705(13) 0.08112(13) 1.01805(11) 0.0326(5) Uani 1 1 d . . . . .
C8 C 0.76207(13) 0.02237(17) 1.08346(12) 0.0421(6) Uani 1 1 d . . . . .
H8A H 0.770245 -0.021243 1.052166 0.051 Uiso 1 1 calc R U . . .
H8B H 0.825226 0.039335 1.120099 0.051 Uiso 1 1 calc R U . . .
C3 C 0.65503(19) 0.18576(12) 0.88999(13) 0.0390(5) Uani 1 1 d . . . . .
H3 H 0.633284 0.221987 0.846663 0.047 Uiso 1 1 calc R U . . .
C4 C 0.58915(15) 0.14369(10) 0.90895(11) 0.0262(4) Uani 1 1 d . . . . .
C7 C 0.77935(16) 0.12479(16) 0.99535(13) 0.0474(7) Uani 1 1 d . . . . .
H7 H 0.844518 0.118181 1.025284 0.057 Uiso 1 1 calc R U . . .
C2 C 0.75018(19) 0.17693(15) 0.93147(15) 0.0489(7) Uani 1 1 d . . . . .
C9 C 0.77204(14) -0.05417(17) 1.20463(13) 0.0491(7) Uani 1 1 d . . . . .
H9AA H 0.758300 -0.050317 1.257857 0.059 Uiso 0.754(6) 1 calc R U P A 1
H9AB H 0.838331 -0.040481 1.219224 0.059 Uiso 0.754(6) 1 calc R U P A 1
H9BC H 0.808617 -0.081141 1.176378 0.059 Uiso 0.246(6) 1 calc R U P A 2
H9BD H 0.817286 -0.026181 1.252422 0.059 Uiso 0.246(6) 1 calc R U P A 2
C17 C 0.69521(13) 0.06232(13) 1.18812(11) 0.0304(4) Uani 1 1 d . . . . .
H17A H 0.676234 0.105250 1.149856 0.036 Uiso 1 1 calc R U . . .
H17B H 0.752818 0.074697 1.237338 0.036 Uiso 1 1 calc R U . . .
C12 C 0.32443(18) 0.16888(14) 0.82219(13) 0.0450(6) Uani 1 1 d . . . . .
H12A H 0.317981 0.222076 0.827645 0.054 Uiso 0.754(6) 1 calc R U P A 1
H12B H 0.326861 0.159834 0.764699 0.054 Uiso 0.754(6) 1 calc R U P A 1
H12C H 0.335812 0.206631 0.784936 0.054 Uiso 0.246(6) 1 calc R U P A 2
H12D H 0.285700 0.190986 0.851758 0.054 Uiso 0.246(6) 1 calc R U P A 2
C1 C 0.8194(3) 0.22381(19) 0.90946(19) 0.0743(12) Uani 1 1 d . . . . .
H1A H 0.793374 0.236515 0.848323 0.111 Uiso 1 1 calc R U . . .
H1B H 0.877885 0.196838 0.921810 0.111 Uiso 1 1 calc R U . . .
H1C H 0.831811 0.268379 0.944030 0.111 Uiso 1 1 calc R U . . .
O4 O 0.78926(10) -0.14320(9) 0.88942(8) 0.0349(3) Uani 1 1 d . . . . .
O5 O 0.87960(13) -0.14350(11) 1.02849(9) 0.0506(5) Uani 1 1 d . . . . .
C19 C 0.84931(14) -0.11442(15) 0.95487(12) 0.0379(5) Uani 1 1 d . . . . .
C18 C 0.8836(2) -0.0400(3) 0.94333(18) 0.0888(15) Uani 1 1 d . . . . .
H18A H 0.920505 -0.043373 0.906583 0.133 Uiso 1 1 calc R U . . .
H18B H 0.922529 -0.020241 0.999498 0.133 Uiso 1 1 calc R U . . .
H18C H 0.829989 -0.007748 0.916389 0.133 Uiso 1 1 calc R U . . .
C11 C 0.7597(2) -0.1342(2) 1.17501(17) 0.0510(12) Uani 0.754(6) 1 d . . P A 1
H11A H 0.758273 -0.136598 1.115389 0.061 Uiso 0.754(6) 1 calc R U P A 1
H11B H 0.814819 -0.162276 1.211840 0.061 Uiso 0.754(6) 1 calc R U P A 1
C10 C 0.7338(5) -0.1016(5) 1.2381(5) 0.033(2) Uani 0.246(6) 1 d . . P A 2
H10A H 0.690651 -0.075416 1.259800 0.039 Uiso 0.246(6) 1 calc R U P A 2
H10B H 0.783636 -0.122972 1.288577 0.039 Uiso 0.246(6) 1 calc R U P A 2
O8 O 0.9954(2) -0.06044(17) 1.17615(18) 0.0317(6) Uani 0.5 1 d G . P B -2
H8C H 0.996785 -0.094396 1.212828 0.048 Uiso 0.5 1 d G U P B -2
H8D H 0.971788 -0.081541 1.126238 0.048 Uiso 0.5 1 d G U P B -2
O7 O 1.0030(14) 0.0655(3) 1.2437(13) 0.093(3) Uani 0.5 1 d . . P C -1
H7A H 0.980753 0.029899 1.261369 0.139 Uiso 0.5 1 calc R U P C -1
O6 O 1.0026(3) -0.1531(2) 1.1916(2) 0.0487(9) Uani 0.5 1 d . . P D -1
H6 H 0.966998 -0.149074 1.139978 0.073 Uiso 0.5 1 calc R U P D -1
C20 C 1.0104(4) -0.2276(3) 1.2158(3) 0.0575(15) Uani 0.5 1 d . . P D -1
H20A H 1.025405 -0.256506 1.173248 0.086 Uiso 0.5 1 calc R U P D -1
H20B H 0.951017 -0.244407 1.218376 0.086 Uiso 0.5 1 calc R U P D -1
H20C H 1.060114 -0.233417 1.272294 0.086 Uiso 0.5 1 calc R U P D -1
C21 C 0.9798(4) 0.1276(3) 1.2735(4) 0.0589(16) Uani 0.5 1 d . . P C -1
H21A H 0.973932 0.166943 1.232246 0.088 Uiso 0.5 1 calc R U P C -1
H21B H 1.028466 0.140107 1.328780 0.088 Uiso 0.5 1 calc R U P C -1
H21C H 0.920105 0.121125 1.281195 0.088 Uiso 0.5 1 calc R U P C -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1 2.0119(11) . ?
Ni1 O1 2.0159(11) 5_657 ?
Ni1 O2 2.1184(11) . ?
Ni1 O3 2.1109(12) 5_657 ?
Ni1 N2 2.0885(16) 5_657 ?
Ni1 N1 2.0872(15) . ?
O1 C5 1.3393(19) . ?
O2 C16 1.253(2) . ?
O3 C15 1.251(3) . ?
N2 C13 1.482(2) . ?
N2 C14 1.482(2) . ?
N2 C12 1.496(3) . ?
N1 C8 1.490(2) . ?
N1 C9 1.497(3) . ?
N1 C17 1.474(3) . ?
N4 H4A 0.8800 . ?
N4 H4B 0.8800 . ?
N4 C16 1.320(2) . ?
N3 H3A 0.8800 . ?
N3 H3B 0.8800 . ?
N3 C15 1.319(2) . ?
C15 C14 1.512(3) . ?
C5 C6 1.416(3) . ?
C5 C4 1.418(3) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C4 1.510(3) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C16 C17 1.520(2) . ?
C6 C8 1.512(3) . ?
C6 C7 1.405(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C3 H3 0.9500 . ?
C3 C4 1.400(3) . ?
C3 C2 1.380(4) . ?
C7 H7 0.9500 . ?
C7 C2 1.382(4) . ?
C2 C1 1.516(3) . ?
C9 H9AA 0.9900 . ?
C9 H9AB 0.9900 . ?
C9 H9BC 0.9900 . ?
C9 H9BD 0.9900 . ?
C9 C11 1.542(5) . ?
C9 C10 1.289(9) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 H12C 0.9900 . ?
C12 H12D 0.9900 . ?
C12 C11 1.459(5) 5_657 ?
C12 C10 1.638(10) 5_657 ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
O4 C19 1.261(3) . ?
O5 C19 1.264(3) . ?
C19 C18 1.504(4) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
O8 H8C 0.8697 . ?
O8 H8D 0.8699 . ?
O7 H7A 0.8400 . ?
O7 C21 1.345(16) . ?
O6 H6 0.8400 . ?
O6 C20 1.419(7) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni1 O1 82.80(5) . 5_657 ?
O1 Ni1 O2 95.44(5) . . ?
O1 Ni1 O2 89.68(4) 5_657 . ?
O1 Ni1 O3 91.98(5) . 5_657 ?
O1 Ni1 O3 96.88(5) 5_657 5_657 ?
O1 Ni1 N2 167.35(6) . 5_657 ?
O1 Ni1 N2 88.09(6) 5_657 5_657 ?
O1 Ni1 N1 88.05(6) . . ?
O1 Ni1 N1 165.92(6) 5_657 . ?
O3 Ni1 O2 170.66(5) 5_657 . ?
N2 Ni1 O2 93.26(5) 5_657 . ?
N2 Ni1 O3 80.37(5) 5_657 5_657 ?
N1 Ni1 O2 80.54(5) . . ?
N1 Ni1 O3 94.09(6) . 5_657 ?
N1 Ni1 N2 102.46(7) . 5_657 ?
Ni1 O1 Ni1 97.20(5) . 5_657 ?
C5 O1 Ni1 128.22(10) . 5_657 ?
C5 O1 Ni1 127.85(11) . . ?
C16 O2 Ni1 111.60(10) . . ?
C15 O3 Ni1 111.59(11) . 5_657 ?
C13 N2 Ni1 109.78(11) . 5_657 ?
C13 N2 C14 110.26(17) . . ?
C13 N2 C12 107.95(14) . . ?
C14 N2 Ni1 103.79(10) . 5_657 ?
C14 N2 C12 109.91(15) . . ?
C12 N2 Ni1 115.09(15) . 5_657 ?
C8 N1 Ni1 109.60(11) . . ?
C8 N1 C9 108.53(16) . . ?
C9 N1 Ni1 113.90(16) . . ?
C17 N1 Ni1 105.10(10) . . ?
C17 N1 C8 111.18(19) . . ?
C17 N1 C9 108.52(16) . . ?
H4A N4 H4B 120.0 . . ?
C16 N4 H4A 120.0 . . ?
C16 N4 H4B 120.0 . . ?
H3A N3 H3B 120.0 . . ?
C15 N3 H3A 120.0 . . ?
C15 N3 H3B 120.0 . . ?
O3 C15 N3 124.3(2) . . ?
O3 C15 C14 118.31(15) . . ?
N3 C15 C14 117.41(19) . . ?
O1 C5 C6 121.08(16) . . ?
O1 C5 C4 120.97(16) . . ?
C6 C5 C4 117.83(16) . . ?
N2 C13 H13A 108.0 . . ?
N2 C13 H13B 108.0 . . ?
N2 C13 C4 117.37(14) . . ?
H13A C13 H13B 107.2 . . ?
C4 C13 H13A 108.0 . . ?
C4 C13 H13B 108.0 . . ?
N2 C14 C15 107.73(18) . . ?
N2 C14 H14A 110.2 . . ?
N2 C14 H14B 110.2 . . ?
C15 C14 H14A 110.2 . . ?
C15 C14 H14B 110.2 . . ?
H14A C14 H14B 108.5 . . ?
O2 C16 N4 123.44(16) . . ?
O2 C16 C17 118.19(14) . . ?
N4 C16 C17 118.37(15) . . ?
C5 C6 C8 125.07(17) . . ?
C7 C6 C5 119.5(2) . . ?
C7 C6 C8 115.24(19) . . ?
N1 C8 C6 117.32(17) . . ?
N1 C8 H8A 108.0 . . ?
N1 C8 H8B 108.0 . . ?
C6 C8 H8A 108.0 . . ?
C6 C8 H8B 108.0 . . ?
H8A C8 H8B 107.2 . . ?
C4 C3 H3 118.5 . . ?
C2 C3 H3 118.5 . . ?
C2 C3 C4 122.9(2) . . ?
C5 C4 C13 124.96(16) . . ?
C3 C4 C5 119.7(2) . . ?
C3 C4 C13 115.11(18) . . ?
C6 C7 H7 118.5 . . ?
C2 C7 C6 123.0(2) . . ?
C2 C7 H7 118.5 . . ?
C3 C2 C7 117.01(18) . . ?
C3 C2 C1 121.4(3) . . ?
C7 C2 C1 121.6(3) . . ?
N1 C9 H9AA 108.4 . . ?
N1 C9 H9AB 108.4 . . ?
N1 C9 H9BC 107.4 . . ?
N1 C9 H9BD 107.4 . . ?
N1 C9 C11 115.49(19) . . ?
H9AA C9 H9AB 107.5 . . ?
H9BC C9 H9BD 106.9 . . ?
C11 C9 H9AA 108.4 . . ?
C11 C9 H9AB 108.4 . . ?
C10 C9 N1 119.8(3) . . ?
C10 C9 H9BC 107.4 . . ?
C10 C9 H9BD 107.4 . . ?
N1 C17 C16 107.85(16) . . ?
N1 C17 H17A 110.1 . . ?
N1 C17 H17B 110.1 . . ?
C16 C17 H17A 110.1 . . ?
C16 C17 H17B 110.1 . . ?
H17A C17 H17B 108.4 . . ?
N2 C12 H12A 107.9 . . ?
N2 C12 H12B 107.9 . . ?
N2 C12 H12C 108.9 . . ?
N2 C12 H12D 108.9 . . ?
N2 C12 C10 113.4(3) . 5_657 ?
H12A C12 H12B 107.2 . . ?
H12C C12 H12D 107.7 . . ?
C11 C12 N2 117.50(19) 5_657 . ?
C11 C12 H12A 107.9 5_657 . ?
C11 C12 H12B 107.9 5_657 . ?
C11 C12 C10 53.1(3) 5_657 5_657 ?
C10 C12 H12C 108.9 5_657 . ?
C10 C12 H12D 108.9 5_657 . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O4 C19 O5 124.0(3) . . ?
O4 C19 C18 116.7(2) . . ?
O5 C19 C18 119.2(2) . . ?
C19 C18 H18A 109.5 . . ?
C19 C18 H18B 109.5 . . ?
C19 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C9 C11 H11A 108.7 . . ?
C9 C11 H11B 108.7 . . ?
C12 C11 C9 114.3(2) 5_657 . ?
C12 C11 H11A 108.7 5_657 . ?
C12 C11 H11B 108.7 5_657 . ?
H11A C11 H11B 107.6 . . ?
C9 C10 C12 118.4(5) . 5_657 ?
C9 C10 H10A 107.7 . . ?
C9 C10 H10B 107.7 . . ?
C12 C10 H10A 107.7 5_657 . ?
C12 C10 H10B 107.7 5_657 . ?
H10A C10 H10B 107.1 . . ?
H8C O8 H8D 104.5 . . ?
C21 O7 H7A 109.5 . . ?
C20 O6 H6 109.5 . . ?
O6 C20 H20A 109.5 . . ?
O6 C20 H20B 109.5 . . ?
O6 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O7 C21 H21A 109.5 . . ?
O7 C21 H21B 109.5 . . ?
O7 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 O1 C5 C6 -20.5(2) . . . . ?
Ni1 O1 C5 C6 -165.04(13) 5_657 . . . ?
Ni1 O1 C5 C4 19.0(2) 5_657 . . . ?
Ni1 O1 C5 C4 163.49(12) . . . . ?
Ni1 O2 C16 N4 -165.64(15) . . . . ?
Ni1 O2 C16 C17 14.5(2) . . . . ?
Ni1 O3 C15 N3 168.55(17) 5_657 . . . ?
Ni1 O3 C15 C14 -11.5(2) 5_657 . . . ?
Ni1 N2 C13 C4 -60.09(18) 5_657 . . . ?
Ni1 N2 C14 C15 -44.29(17) 5_657 . . . ?
Ni1 N2 C12 C11 28.5(3) 5_657 . . 5_657 ?
Ni1 N2 C12 C10 -30.6(3) 5_657 . . 5_657 ?
Ni1 N1 C8 C6 59.5(2) . . . . ?
Ni1 N1 C9 C11 35.4(2) . . . . ?
Ni1 N1 C9 C10 -31.0(5) . . . . ?
Ni1 N1 C17 C16 42.32(16) . . . . ?
O1 C5 C6 C8 10.2(3) . . . . ?
O1 C5 C6 C7 -175.45(17) . . . . ?
O1 C5 C4 C13 -10.2(3) . . . . ?
O1 C5 C4 C3 174.97(15) . . . . ?
O2 C16 C17 N1 -40.1(2) . . . . ?
O3 C15 C14 N2 39.6(2) . . . . ?
N2 C13 C4 C5 35.8(2) . . . . ?
N2 C13 C4 C3 -149.10(16) . . . . ?
N1 C9 C11 C12 -76.9(3) . . . 5_657 ?
N1 C9 C10 C12 72.3(6) . . . 5_657 ?
N4 C16 C17 N1 140.05(17) . . . . ?
N3 C15 C14 N2 -140.48(19) . . . . ?
C5 C6 C8 N1 -34.7(3) . . . . ?
C5 C6 C7 C2 -0.5(3) . . . . ?
C13 N2 C14 C15 -161.82(15) . . . . ?
C13 N2 C12 C11 151.5(2) . . . 5_657 ?
C13 N2 C12 C10 92.4(3) . . . 5_657 ?
C14 N2 C13 C4 53.7(2) . . . . ?
C14 N2 C12 C11 -88.2(3) . . . 5_657 ?
C14 N2 C12 C10 -147.3(3) . . . 5_657 ?
C6 C5 C4 C13 173.73(16) . . . . ?
C6 C5 C4 C3 -1.1(2) . . . . ?
C6 C7 C2 C3 0.8(3) . . . . ?
C6 C7 C2 C1 179.2(2) . . . . ?
C8 N1 C9 C11 -87.0(2) . . . . ?
C8 N1 C9 C10 -153.4(5) . . . . ?
C8 N1 C17 C16 160.82(14) . . . . ?
C8 C6 C7 C2 174.4(2) . . . . ?
C4 C5 C6 C8 -173.74(18) . . . . ?
C4 C5 C6 C7 0.6(3) . . . . ?
C4 C3 C2 C7 -1.3(3) . . . . ?
C4 C3 C2 C1 -179.69(19) . . . . ?
C7 C6 C8 N1 150.71(19) . . . . ?
C2 C3 C4 C5 1.5(3) . . . . ?
C2 C3 C4 C13 -173.82(17) . . . . ?
C9 N1 C8 C6 -175.6(2) . . . . ?
C9 N1 C17 C16 -79.89(19) . . . . ?
C17 N1 C8 C6 -56.3(2) . . . . ?
C17 N1 C9 C11 152.07(19) . . . . ?
C17 N1 C9 C10 85.7(5) . . . . ?
C12 N2 C13 C4 173.74(17) . . . . ?
C12 N2 C14 C15 79.30(19) . . . . ?

_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
# start Validation Reply Form
_vrf_PLAT910_1102-ni2-z_sq_sq    
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         11 Note  
RESPONSE: The missing FCF reflections below theta(min) were caused by the
high beamstop theta(min) limit set.
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1122-ga-93-exp_1589_sq
_database_code_depnum_ccdc_archive 'CCDC 2291723'
loop_
_audit_author_name
_audit_author_address
'Xin Guo'
;Beijing Institute Of Technology
China
;
_audit_update_record             
;
2023-08-30 deposited with the CCDC.	2023-11-21 downloaded from the CCDC.
;
_audit_creation_date             2023-02-08
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C32 H44 Ga N8 Ni O6, Br, C H4 O'
_chemical_formula_sum            'C33 H48 Br Ga N8 Ni O7'
_chemical_formula_weight         877.13
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga 0.2307 1.6083 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   29.4737(12)
_cell_length_b                   14.7532(5)
_cell_length_c                   20.5922(8)
_cell_angle_alpha                90
_cell_angle_beta                 103.741(4)
_cell_angle_gamma                90
_cell_volume                     8697.9(6)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    15592
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.4240
_cell_measurement_theta_min      3.7260
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.020
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71947
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3616
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.913
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            58238
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.913
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.621
_diffrn_reflns_theta_min         3.525
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.913
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     15.00  41.00   0.50   68.00    --    0.10  59.00-142.00   52
  2  ω    -28.00  -2.00   0.50   68.00    --    0.10 -59.00  77.00   52
  3  ω    -27.00   6.00   0.50   68.00    --    0.10 -82.00  60.00   66
  4  ω    -77.00 -50.00   0.50   68.00    --    0.10 -38.00 -60.00   54
  5  ω    -26.00   1.00   0.50   68.00    --    0.10 -82.00  30.00   54
  6  ω    -16.00  78.00   0.50   68.00    --    0.10  38.00-180.00  188
  7  ω    -13.00  65.00   0.50   68.00    --    0.10  38.00  90.00  156
  8  ω      6.00  31.00   0.50   68.00    --    0.10 -82.00-150.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8612
_reflns_number_total             11178
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_refine_diff_density_max         0.756
_refine_diff_density_min         -1.107
_refine_diff_density_rms         0.086
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         11178
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0462
_refine_ls_restrained_S_all      1.021
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0557P)²+29.5569P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1180
_refine_ls_wR_factor_ref         0.1254
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Others
 Sof(Br2)=1-FVAR(1)
 Sof(Br1)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C12(H12A,H12B), C11(H11A,H11B), C10(H10A,H10B), C28(H28A,
 H28B), C9(H9A,H9B), C8(H8A,H8B), C20(H20A,H20B), C25(H25A,H25B), C24(H24A,
 H24B), C32(H32A,H32B), C23(H23A,H23B), C21(H21A,H21B), C22(H22A,H22B)
3.b Aromatic/amide H refined with riding coordinates:
 N8(H8), N5(H5), C7(H7), C14(H14), C17(H17), C3(H3)
3.c X=CH2 refined with riding coordinates:
 N7(H7A,H7B), N6(H6A,H6B)
3.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C16(H16A,H16B,H16C), C33(H33A,H33B,H33C)
3.e Idealised tetrahedral OH refined as rotating group:
 O7(H7C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ga1 Ga 0.30833(2) 0.62191(2) 0.68277(2) 0.02054(8) Uani 1 1 d . . . . .
Ni1 Ni 0.37311(2) 0.77447(2) 0.74940(2) 0.02650(10) Uani 1 1 d . . . . .
O1 O 0.36347(7) 0.63951(13) 0.75940(10) 0.0228(4) Uani 1 1 d . . . . .
O2 O 0.31596(7) 0.75526(13) 0.67151(10) 0.0244(4) Uani 1 1 d . . . . .
O3 O 0.33591(7) 0.79545(14) 0.82101(11) 0.0283(4) Uani 1 1 d . . . . .
O4 O 0.41260(8) 0.75992(14) 0.67918(12) 0.0328(5) Uani 1 1 d . . . . .
O5 O 0.19509(8) 0.68323(16) 0.75546(11) 0.0342(5) Uani 1 1 d . . . . .
O6 O 0.39604(8) 0.49527(15) 0.58803(11) 0.0329(5) Uani 1 1 d . . . . .
N8 N 0.26751(8) 0.64098(15) 0.74495(11) 0.0198(4) Uani 1 1 d . . . . .
H8 H 0.279505 0.640403 0.788377 0.024 Uiso 1 1 calc R U . . .
N5 N 0.34689(8) 0.59804(15) 0.61918(11) 0.0230(5) Uani 1 1 d . . . . .
H5 H 0.353185 0.642114 0.593882 0.028 Uiso 1 1 calc R U . . .
N4 N 0.31097(8) 0.47700(15) 0.68846(11) 0.0228(5) Uani 1 1 d . . . . .
N3 N 0.24124(9) 0.61826(16) 0.61328(11) 0.0238(5) Uani 1 1 d . . . . .
N7 N 0.33510(9) 0.74554(17) 0.92379(14) 0.0309(5) Uani 1 1 d . . . . .
H7A H 0.305257 0.758424 0.918084 0.037 Uiso 1 1 calc R U . . .
H7B H 0.350710 0.721737 0.961720 0.037 Uiso 1 1 calc R U . . .
C30 C 0.36326(10) 0.51668(19) 0.61435(13) 0.0247(6) Uani 1 1 d . . . . .
N2 N 0.37356(10) 0.90900(18) 0.72046(16) 0.0390(7) Uani 1 1 d . . . . .
N1 N 0.42799(9) 0.76542(19) 0.83466(14) 0.0345(6) Uani 1 1 d . . . . .
N6 N 0.41516(10) 0.8172(2) 0.57901(15) 0.0396(6) Uani 1 1 d . . . . .
H6A H 0.427129 0.767039 0.567094 0.047 Uiso 1 1 calc R U . . .
H6B H 0.409599 0.863641 0.551403 0.047 Uiso 1 1 calc R U . . .
C27 C 0.22332(10) 0.65428(19) 0.72217(14) 0.0249(6) Uani 1 1 d . . . . .
C5 C 0.39830(10) 0.5775(2) 0.77932(13) 0.0234(5) Uani 1 1 d . . . . .
C29 C 0.33759(11) 0.44121(18) 0.64131(14) 0.0268(6) Uani 1 1 d . . . . .
H29A H 0.315858 0.410679 0.603588 0.032 Uiso 1 1 calc R U . . .
H29B H 0.360450 0.395681 0.664477 0.032 Uiso 1 1 calc R U . . .
C6 C 0.38659(10) 0.4853(2) 0.77696(14) 0.0255(6) Uani 1 1 d . . . . .
C19 C 0.28184(10) 0.81605(18) 0.64728(14) 0.0241(6) Uani 1 1 d . . . . .
C12 C 0.24054(11) 0.69688(19) 0.56679(14) 0.0261(6) Uani 1 1 d . . . . .
H12A H 0.211722 0.693106 0.530561 0.031 Uiso 1 1 calc R U . . .
H12B H 0.267418 0.690918 0.545976 0.031 Uiso 1 1 calc R U . . .
C11 C 0.23586(11) 0.53478(19) 0.57089(14) 0.0277(6) Uani 1 1 d . . . . .
H11A H 0.262727 0.531046 0.549887 0.033 Uiso 1 1 calc R U . . .
H11B H 0.207272 0.541212 0.534513 0.033 Uiso 1 1 calc R U . . .
C10 C 0.23276(11) 0.4461(2) 0.60740(15) 0.0308(6) Uani 1 1 d . . . . .
H10A H 0.240741 0.396065 0.580027 0.037 Uiso 1 1 calc R U . . .
H10B H 0.199849 0.437288 0.609579 0.037 Uiso 1 1 calc R U . . .
C28 C 0.20362(10) 0.6285(2) 0.64921(14) 0.0269(6) Uani 1 1 d . . . . .
H28A H 0.186196 0.570750 0.647015 0.032 Uiso 1 1 calc R U . . .
H28B H 0.181507 0.675879 0.627101 0.032 Uiso 1 1 calc R U . . .
C9 C 0.26344(10) 0.43668(19) 0.67821(15) 0.0277(6) Uani 1 1 d . . . . .
H9A H 0.247236 0.465765 0.709710 0.033 Uiso 1 1 calc R U . . .
H9B H 0.266762 0.371460 0.689653 0.033 Uiso 1 1 calc R U . . .
C18 C 0.28599(11) 0.90763(19) 0.66672(14) 0.0281(6) Uani 1 1 d . . . . .
C8 C 0.33631(10) 0.45599(19) 0.75916(14) 0.0255(6) Uani 1 1 d . . . . .
H8A H 0.334925 0.389808 0.766384 0.031 Uiso 1 1 calc R U . . .
H8B H 0.319827 0.486109 0.789893 0.031 Uiso 1 1 calc R U . . .
C7 C 0.42137(11) 0.4198(2) 0.79535(15) 0.0316(6) Uani 1 1 d . . . . .
H7 H 0.413023 0.357482 0.792450 0.038 Uiso 1 1 calc R U . . .
C26 C 0.35620(10) 0.76173(19) 0.87600(15) 0.0271(6) Uani 1 1 d . . . . .
C4 C 0.44486(10) 0.6032(2) 0.80612(14) 0.0280(6) Uani 1 1 d . . . . .
C14 C 0.20630(13) 0.8501(2) 0.57411(14) 0.0333(7) Uani 1 1 d . . . . .
H14 H 0.179026 0.829661 0.543002 0.040 Uiso 1 1 calc R U . . .
C31 C 0.40561(11) 0.8229(2) 0.63783(18) 0.0336(7) Uani 1 1 d . . . . .
C13 C 0.24252(11) 0.78900(19) 0.59855(13) 0.0262(6) Uani 1 1 d . . . . .
C17 C 0.24994(13) 0.9675(2) 0.63931(15) 0.0354(7) Uani 1 1 d . . . . .
H17 H 0.253342 1.029586 0.651886 0.043 Uiso 1 1 calc R U . . .
C20 C 0.32643(12) 0.9474(2) 0.71803(18) 0.0350(7) Uani 1 1 d . . . . .
H20A H 0.327511 1.013347 0.709505 0.042 Uiso 1 1 calc R U . . .
H20B H 0.319918 0.939841 0.762716 0.042 Uiso 1 1 calc R U . . .
C2 C 0.46797(11) 0.4439(2) 0.81782(16) 0.0361(7) Uani 1 1 d . . . . .
C25 C 0.40731(11) 0.7327(3) 0.88899(16) 0.0357(7) Uani 1 1 d . . . . .
H25A H 0.424898 0.757962 0.932205 0.043 Uiso 1 1 calc R U . . .
H25B H 0.409451 0.665817 0.891689 0.043 Uiso 1 1 calc R U . . .
C24 C 0.46222(11) 0.6995(2) 0.81904(18) 0.0350(7) Uani 1 1 d . . . . .
H24A H 0.490185 0.698974 0.856815 0.042 Uiso 1 1 calc R U . . .
H24B H 0.472151 0.721364 0.779117 0.042 Uiso 1 1 calc R U . . .
C15 C 0.20941(14) 0.9403(2) 0.59451(15) 0.0389(8) Uani 1 1 d . . . . .
C3 C 0.47883(11) 0.5354(2) 0.82411(15) 0.0333(7) Uani 1 1 d . . . . .
H3 H 0.510449 0.552794 0.841232 0.040 Uiso 1 1 calc R U . . .
C32 C 0.38402(15) 0.9115(2) 0.6537(2) 0.0523(11) Uani 1 1 d . . . . .
H32A H 0.405860 0.961974 0.652151 0.063 Uiso 1 1 calc R U . . .
H32B H 0.354839 0.923031 0.619406 0.063 Uiso 1 1 calc R U . . .
C1 C 0.50544(13) 0.3726(3) 0.8377(2) 0.0488(9) Uani 1 1 d . . . . .
H1A H 0.532838 0.389959 0.821391 0.073 Uiso 1 1 calc R U . . .
H1B H 0.493511 0.314193 0.818197 0.073 Uiso 1 1 calc R U . . .
H1C H 0.514282 0.367285 0.886568 0.073 Uiso 1 1 calc R U . . .
C23 C 0.45228(13) 0.8533(3) 0.8555(2) 0.0545(11) Uani 1 1 d . . . . .
H23A H 0.436266 0.884041 0.886541 0.065 Uiso 1 1 calc R U . . .
H23B H 0.484579 0.839982 0.880709 0.065 Uiso 1 1 calc R U . . .
C16 C 0.17033(18) 1.0074(3) 0.56821(19) 0.0631(14) Uani 1 1 d . . . . .
H16A H 0.179303 1.047509 0.535424 0.095 Uiso 1 1 calc R U . . .
H16B H 0.164627 1.043637 0.605372 0.095 Uiso 1 1 calc R U . . .
H16C H 0.141829 0.974438 0.546856 0.095 Uiso 1 1 calc R U . . .
C21 C 0.40875(14) 0.9639(3) 0.7729(3) 0.0634(13) Uani 1 1 d . . . . .
H21A H 0.415354 1.021474 0.752148 0.076 Uiso 1 1 calc R U . . .
H21B H 0.394072 0.979459 0.809979 0.076 Uiso 1 1 calc R U . . .
C22 C 0.45453(15) 0.9164(3) 0.8016(2) 0.0583(11) Uani 1 1 d . . . . .
H22A H 0.464063 0.882770 0.765451 0.070 Uiso 1 1 calc R U . . .
H22B H 0.478817 0.962500 0.818917 0.070 Uiso 1 1 calc R U . . .
Br1 Br 0.39271(2) 1.00330(8) 0.47786(6) 0.0524(4) Uani 0.843(5) 1 d . . P A 1
O7 O 0.43455(10) 0.63998(18) 0.53765(13) 0.0474(6) Uani 1 1 d . . . . .
H7C H 0.423223 0.593236 0.550950 0.071 Uiso 1 1 calc R U . . .
C33 C 0.4633(3) 0.6154(4) 0.4967(3) 0.093(2) Uani 1 1 d . . . . .
H33A H 0.444219 0.595937 0.453203 0.139 Uiso 1 1 calc R U . . .
H33B H 0.483581 0.565443 0.517254 0.139 Uiso 1 1 calc R U . . .
H33C H 0.482513 0.667393 0.490389 0.139 Uiso 1 1 calc R U . . .
Br2 Br 0.39721(19) 0.9646(7) 0.4523(4) 0.0912(18) Uani 0.157(5) 1 d . . P A 2


_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
Ga1 O1 1.995(2) . ?
Ga1 O2 1.9999(19) . ?
Ga1 N8 1.974(2) . ?
Ga1 N5 1.959(2) . ?
Ga1 N4 2.141(2) . ?
Ga1 N3 2.149(2) . ?
Ni1 O1 2.029(2) . ?
Ni1 O2 2.051(2) . ?
Ni1 O3 2.059(2) . ?
Ni1 O4 2.071(2) . ?
Ni1 N2 2.073(3) . ?
Ni1 N1 2.090(3) . ?
O1 C5 1.364(3) . ?
O2 C19 1.351(3) . ?
O3 C26 1.251(4) . ?
O4 C31 1.244(4) . ?
O5 C27 1.271(4) . ?
O6 C30 1.255(3) . ?
N8 H8 0.8800 . ?
N8 C27 1.290(4) . ?
N5 H5 0.8800 . ?
N5 C30 1.306(4) . ?
N4 C29 1.483(3) . ?
N4 C9 1.490(4) . ?
N4 C8 1.502(3) . ?
N3 C12 1.501(3) . ?
N3 C11 1.496(4) . ?
N3 C28 1.479(4) . ?
N7 H7A 0.8800 . ?
N7 H7B 0.8800 . ?
N7 C26 1.305(4) . ?
C30 C29 1.523(4) . ?
N2 C20 1.490(4) . ?
N2 C32 1.478(5) . ?
N2 C21 1.538(5) . ?
N1 C25 1.476(4) . ?
N1 C24 1.491(4) . ?
N1 C23 1.494(4) . ?
N6 H6A 0.8800 . ?
N6 H6B 0.8800 . ?
N6 C31 1.310(4) . ?
C27 C28 1.525(4) . ?
C5 C6 1.401(4) . ?
C5 C4 1.404(4) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C6 C8 1.503(4) . ?
C6 C7 1.394(4) . ?
C19 C18 1.406(4) . ?
C19 C13 1.399(4) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C13 1.503(4) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C10 1.523(4) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C9 1.529(4) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C18 C17 1.394(4) . ?
C18 C20 1.511(5) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C7 H7 0.9500 . ?
C7 C2 1.387(5) . ?
C26 C25 1.527(4) . ?
C4 C24 1.512(5) . ?
C4 C3 1.401(4) . ?
C14 H14 0.9500 . ?
C14 C13 1.396(4) . ?
C14 C15 1.393(5) . ?
C31 C32 1.523(5) . ?
C17 H17 0.9500 . ?
C17 C15 1.384(5) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C2 C3 1.386(5) . ?
C2 C1 1.510(4) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C15 C16 1.518(5) . ?
C3 H3 0.9500 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C22 1.461(7) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.511(6) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
O7 H7C 0.8400 . ?
O7 C33 1.379(5) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?

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 Ga1 O2 82.58(8) . . ?
O1 Ga1 N4 94.27(8) . . ?
O1 Ga1 N3 167.94(8) . . ?
O2 Ga1 N4 170.00(8) . . ?
O2 Ga1 N3 93.35(8) . . ?
N8 Ga1 O1 88.62(8) . . ?
N8 Ga1 O2 92.16(8) . . ?
N8 Ga1 N4 97.27(9) . . ?
N8 Ga1 N3 80.17(9) . . ?
N5 Ga1 O1 93.39(9) . . ?
N5 Ga1 O2 90.01(9) . . ?
N5 Ga1 N8 177.22(10) . . ?
N5 Ga1 N4 80.67(9) . . ?
N5 Ga1 N3 97.97(10) . . ?
N4 Ga1 N3 91.55(9) . . ?
O1 Ni1 O2 80.50(8) . . ?
O1 Ni1 O3 87.91(8) . . ?
O1 Ni1 O4 94.86(8) . . ?
O1 Ni1 N2 168.35(11) . . ?
O1 Ni1 N1 87.20(9) . . ?
O2 Ni1 O3 95.89(8) . . ?
O2 Ni1 O4 86.16(8) . . ?
O2 Ni1 N2 88.14(11) . . ?
O2 Ni1 N1 167.46(10) . . ?
O3 Ni1 O4 176.80(9) . . ?
O3 Ni1 N2 95.90(10) . . ?
O3 Ni1 N1 81.11(9) . . ?
O4 Ni1 N2 81.69(10) . . ?
O4 Ni1 N1 97.40(10) . . ?
N2 Ni1 N1 104.25(12) . . ?
Ga1 O1 Ni1 98.91(8) . . ?
C5 O1 Ga1 124.34(17) . . ?
C5 O1 Ni1 125.15(17) . . ?
Ga1 O2 Ni1 98.01(8) . . ?
C19 O2 Ga1 126.97(18) . . ?
C19 O2 Ni1 126.72(18) . . ?
C26 O3 Ni1 111.53(18) . . ?
C31 O4 Ni1 111.80(19) . . ?
Ga1 N8 H8 119.9 . . ?
C27 N8 Ga1 120.25(19) . . ?
C27 N8 H8 119.9 . . ?
Ga1 N5 H5 120.0 . . ?
C30 N5 Ga1 119.97(19) . . ?
C30 N5 H5 120.0 . . ?
C29 N4 Ga1 109.73(16) . . ?
C29 N4 C9 113.0(2) . . ?
C29 N4 C8 110.0(2) . . ?
C9 N4 Ga1 111.72(17) . . ?
C9 N4 C8 106.8(2) . . ?
C8 N4 Ga1 105.20(16) . . ?
C12 N3 Ga1 106.04(17) . . ?
C11 N3 Ga1 111.25(18) . . ?
C11 N3 C12 106.3(2) . . ?
C28 N3 Ga1 110.17(17) . . ?
C28 N3 C12 110.0(2) . . ?
C28 N3 C11 112.8(2) . . ?
H7A N7 H7B 120.0 . . ?
C26 N7 H7A 120.0 . . ?
C26 N7 H7B 120.0 . . ?
O6 C30 N5 126.9(3) . . ?
O6 C30 C29 118.3(3) . . ?
N5 C30 C29 114.8(2) . . ?
C20 N2 Ni1 107.72(18) . . ?
C20 N2 C21 106.9(3) . . ?
C32 N2 Ni1 107.9(2) . . ?
C32 N2 C20 111.0(3) . . ?
C32 N2 C21 112.6(3) . . ?
C21 N2 Ni1 110.6(3) . . ?
C25 N1 Ni1 106.32(18) . . ?
C25 N1 C24 111.9(3) . . ?
C25 N1 C23 108.8(3) . . ?
C24 N1 Ni1 106.8(2) . . ?
C24 N1 C23 109.0(3) . . ?
C23 N1 Ni1 114.1(3) . . ?
H6A N6 H6B 120.0 . . ?
C31 N6 H6A 120.0 . . ?
C31 N6 H6B 120.0 . . ?
O5 C27 N8 126.1(3) . . ?
O5 C27 C28 118.1(3) . . ?
N8 C27 C28 115.8(2) . . ?
O1 C5 C6 118.6(2) . . ?
O1 C5 C4 122.2(3) . . ?
C6 C5 C4 119.0(3) . . ?
N4 C29 C30 111.4(2) . . ?
N4 C29 H29A 109.4 . . ?
N4 C29 H29B 109.4 . . ?
C30 C29 H29A 109.4 . . ?
C30 C29 H29B 109.4 . . ?
H29A C29 H29B 108.0 . . ?
C5 C6 C8 120.5(2) . . ?
C7 C6 C5 120.3(3) . . ?
C7 C6 C8 119.1(3) . . ?
O2 C19 C18 121.7(3) . . ?
O2 C19 C13 119.5(2) . . ?
C13 C19 C18 118.7(3) . . ?
N3 C12 H12A 108.4 . . ?
N3 C12 H12B 108.4 . . ?
N3 C12 C13 115.3(2) . . ?
H12A C12 H12B 107.5 . . ?
C13 C12 H12A 108.4 . . ?
C13 C12 H12B 108.4 . . ?
N3 C11 H11A 108.4 . . ?
N3 C11 H11B 108.4 . . ?
N3 C11 C10 115.5(2) . . ?
H11A C11 H11B 107.5 . . ?
C10 C11 H11A 108.4 . . ?
C10 C11 H11B 108.4 . . ?
C11 C10 H10A 108.0 . . ?
C11 C10 H10B 108.0 . . ?
C11 C10 C9 117.2(2) . . ?
H10A C10 H10B 107.2 . . ?
C9 C10 H10A 108.0 . . ?
C9 C10 H10B 108.0 . . ?
N3 C28 C27 111.3(2) . . ?
N3 C28 H28A 109.4 . . ?
N3 C28 H28B 109.4 . . ?
C27 C28 H28A 109.4 . . ?
C27 C28 H28B 109.4 . . ?
H28A C28 H28B 108.0 . . ?
N4 C9 C10 115.0(2) . . ?
N4 C9 H9A 108.5 . . ?
N4 C9 H9B 108.5 . . ?
C10 C9 H9A 108.5 . . ?
C10 C9 H9B 108.5 . . ?
H9A C9 H9B 107.5 . . ?
C19 C18 C20 125.0(3) . . ?
C17 C18 C19 119.2(3) . . ?
C17 C18 C20 115.8(3) . . ?
N4 C8 C6 114.3(2) . . ?
N4 C8 H8A 108.7 . . ?
N4 C8 H8B 108.7 . . ?
C6 C8 H8A 108.7 . . ?
C6 C8 H8B 108.7 . . ?
H8A C8 H8B 107.6 . . ?
C6 C7 H7 119.4 . . ?
C2 C7 C6 121.2(3) . . ?
C2 C7 H7 119.4 . . ?
O3 C26 N7 123.0(3) . . ?
O3 C26 C25 120.6(3) . . ?
N7 C26 C25 116.3(3) . . ?
C5 C4 C24 125.5(3) . . ?
C3 C4 C5 118.8(3) . . ?
C3 C4 C24 115.7(3) . . ?
C13 C14 H14 119.4 . . ?
C15 C14 H14 119.4 . . ?
C15 C14 C13 121.2(3) . . ?
O4 C31 N6 123.3(3) . . ?
O4 C31 C32 120.2(3) . . ?
N6 C31 C32 116.5(3) . . ?
C19 C13 C12 120.7(3) . . ?
C14 C13 C19 120.4(3) . . ?
C14 C13 C12 118.6(3) . . ?
C18 C17 H17 118.7 . . ?
C15 C17 C18 122.7(3) . . ?
C15 C17 H17 118.7 . . ?
N2 C20 C18 116.7(3) . . ?
N2 C20 H20A 108.1 . . ?
N2 C20 H20B 108.1 . . ?
C18 C20 H20A 108.1 . . ?
C18 C20 H20B 108.1 . . ?
H20A C20 H20B 107.3 . . ?
C7 C2 C1 120.9(3) . . ?
C3 C2 C7 118.0(3) . . ?
C3 C2 C1 121.0(3) . . ?
N1 C25 C26 110.1(3) . . ?
N1 C25 H25A 109.6 . . ?
N1 C25 H25B 109.6 . . ?
C26 C25 H25A 109.6 . . ?
C26 C25 H25B 109.6 . . ?
H25A C25 H25B 108.2 . . ?
N1 C24 C4 115.7(2) . . ?
N1 C24 H24A 108.4 . . ?
N1 C24 H24B 108.4 . . ?
C4 C24 H24A 108.4 . . ?
C4 C24 H24B 108.4 . . ?
H24A C24 H24B 107.4 . . ?
C14 C15 C16 121.7(4) . . ?
C17 C15 C14 117.6(3) . . ?
C17 C15 C16 120.7(3) . . ?
C4 C3 H3 118.8 . . ?
C2 C3 C4 122.4(3) . . ?
C2 C3 H3 118.8 . . ?
N2 C32 C31 111.6(3) . . ?
N2 C32 H32A 109.3 . . ?
N2 C32 H32B 109.3 . . ?
C31 C32 H32A 109.3 . . ?
C31 C32 H32B 109.3 . . ?
H32A C32 H32B 108.0 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C23 H23A 108.3 . . ?
N1 C23 H23B 108.3 . . ?
H23A C23 H23B 107.4 . . ?
C22 C23 N1 116.1(4) . . ?
C22 C23 H23A 108.3 . . ?
C22 C23 H23B 108.3 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N2 C21 H21A 108.5 . . ?
N2 C21 H21B 108.5 . . ?
H21A C21 H21B 107.5 . . ?
C22 C21 N2 114.9(3) . . ?
C22 C21 H21A 108.5 . . ?
C22 C21 H21B 108.5 . . ?
C23 C22 C21 113.3(4) . . ?
C23 C22 H22A 108.9 . . ?
C23 C22 H22B 108.9 . . ?
C21 C22 H22A 108.9 . . ?
C21 C22 H22B 108.9 . . ?
H22A C22 H22B 107.7 . . ?
C33 O7 H7C 109.5 . . ?
O7 C33 H33A 109.5 . . ?
O7 C33 H33B 109.5 . . ?
O7 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ga1 O1 C5 C6 -37.9(3) . . . . ?
Ga1 O1 C5 C4 146.4(2) . . . . ?
Ga1 O2 C19 C18 152.1(2) . . . . ?
Ga1 O2 C19 C13 -31.9(3) . . . . ?
Ga1 N8 C27 O5 -166.5(2) . . . . ?
Ga1 N8 C27 C28 16.4(3) . . . . ?
Ga1 N5 C30 O6 -162.9(2) . . . . ?
Ga1 N5 C30 C29 20.0(3) . . . . ?
Ga1 N4 C29 C30 11.8(3) . . . . ?
Ga1 N4 C9 C10 68.8(3) . . . . ?
Ga1 N4 C8 C6 -65.8(2) . . . . ?
Ga1 N3 C12 C13 -65.1(3) . . . . ?
Ga1 N3 C11 C10 68.4(3) . . . . ?
Ga1 N3 C28 C27 9.6(3) . . . . ?
Ni1 O1 C5 C6 -173.16(18) . . . . ?
Ni1 O1 C5 C4 11.1(3) . . . . ?
Ni1 O2 C19 C18 10.9(3) . . . . ?
Ni1 O2 C19 C13 -173.05(18) . . . . ?
Ni1 O3 C26 N7 -162.2(2) . . . . ?
Ni1 O3 C26 C25 14.7(3) . . . . ?
Ni1 O4 C31 N6 -159.7(3) . . . . ?
Ni1 O4 C31 C32 19.0(4) . . . . ?
Ni1 N2 C20 C18 -64.5(3) . . . . ?
Ni1 N2 C32 C31 -17.9(4) . . . . ?
Ni1 N2 C21 C22 41.2(4) . . . . ?
Ni1 N1 C25 C26 -28.0(3) . . . . ?
Ni1 N1 C24 C4 -64.3(3) . . . . ?
Ni1 N1 C23 C22 -32.4(4) . . . . ?
O1 C5 C6 C8 -5.8(4) . . . . ?
O1 C5 C6 C7 178.4(2) . . . . ?
O1 C5 C4 C24 2.6(4) . . . . ?
O1 C5 C4 C3 -178.6(2) . . . . ?
O2 C19 C18 C17 179.1(2) . . . . ?
O2 C19 C18 C20 -3.3(4) . . . . ?
O2 C19 C13 C12 -7.7(4) . . . . ?
O2 C19 C13 C14 178.3(2) . . . . ?
O3 C26 C25 N1 10.0(4) . . . . ?
O4 C31 C32 N2 -0.4(5) . . . . ?
O5 C27 C28 N3 165.9(2) . . . . ?
O6 C30 C29 N4 162.2(2) . . . . ?
N8 C27 C28 N3 -16.7(3) . . . . ?
N5 C30 C29 N4 -20.4(4) . . . . ?
N3 C12 C13 C19 64.2(4) . . . . ?
N3 C12 C13 C14 -121.7(3) . . . . ?
N3 C11 C10 C9 -37.7(4) . . . . ?
N7 C26 C25 N1 -173.0(3) . . . . ?
N2 C21 C22 C23 -82.1(5) . . . . ?
N1 C23 C22 C21 75.5(4) . . . . ?
N6 C31 C32 N2 178.4(3) . . . . ?
C5 C6 C8 N4 66.4(3) . . . . ?
C5 C6 C7 C2 1.6(4) . . . . ?
C5 C4 C24 N1 29.4(4) . . . . ?
C5 C4 C3 C2 -1.5(4) . . . . ?
C29 N4 C9 C10 -55.5(3) . . . . ?
C29 N4 C8 C6 52.3(3) . . . . ?
C6 C5 C4 C24 -173.1(3) . . . . ?
C6 C5 C4 C3 5.7(4) . . . . ?
C6 C7 C2 C3 2.6(5) . . . . ?
C6 C7 C2 C1 179.9(3) . . . . ?
C19 C18 C17 C15 1.5(4) . . . . ?
C19 C18 C20 N2 35.4(4) . . . . ?
C12 N3 C11 C10 -176.6(3) . . . . ?
C12 N3 C28 C27 -107.0(3) . . . . ?
C11 N3 C12 C13 176.4(3) . . . . ?
C11 N3 C28 C27 134.5(2) . . . . ?
C11 C10 C9 N4 -38.5(4) . . . . ?
C28 N3 C12 C13 54.0(3) . . . . ?
C28 N3 C11 C10 -56.0(3) . . . . ?
C9 N4 C29 C30 137.3(2) . . . . ?
C9 N4 C8 C6 175.3(2) . . . . ?
C18 C19 C13 C12 168.5(2) . . . . ?
C18 C19 C13 C14 -5.5(4) . . . . ?
C18 C17 C15 C14 -3.3(5) . . . . ?
C18 C17 C15 C16 177.5(3) . . . . ?
C8 N4 C29 C30 -103.5(3) . . . . ?
C8 N4 C9 C10 -176.7(2) . . . . ?
C8 C6 C7 C2 -174.3(3) . . . . ?
C7 C6 C8 N4 -117.7(3) . . . . ?
C7 C2 C3 C4 -2.6(5) . . . . ?
C4 C5 C6 C8 170.1(2) . . . . ?
C4 C5 C6 C7 -5.7(4) . . . . ?
C13 C19 C18 C17 3.0(4) . . . . ?
C13 C19 C18 C20 -179.4(3) . . . . ?
C13 C14 C15 C17 0.7(5) . . . . ?
C13 C14 C15 C16 179.9(3) . . . . ?
C17 C18 C20 N2 -146.9(3) . . . . ?
C20 N2 C32 C31 -135.7(3) . . . . ?
C20 N2 C21 C22 158.2(4) . . . . ?
C20 C18 C17 C15 -176.4(3) . . . . ?
C25 N1 C24 C4 51.7(4) . . . . ?
C25 N1 C23 C22 -150.9(3) . . . . ?
C24 N1 C25 C26 -144.2(3) . . . . ?
C24 N1 C23 C22 86.8(4) . . . . ?
C24 C4 C3 C2 177.3(3) . . . . ?
C15 C14 C13 C19 3.7(4) . . . . ?
C15 C14 C13 C12 -170.4(3) . . . . ?
C3 C4 C24 N1 -149.3(3) . . . . ?
C32 N2 C20 C18 53.4(4) . . . . ?
C32 N2 C21 C22 -79.7(5) . . . . ?
C1 C2 C3 C4 -179.9(3) . . . . ?
C23 N1 C25 C26 95.3(3) . . . . ?
C23 N1 C24 C4 172.0(3) . . . . ?
C21 N2 C20 C18 176.6(3) . . . . ?
C21 N2 C32 C31 104.5(4) . . . . ?

_platon_squeeze_details          ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.486 -0.012 0.001 1956 662 ' '

_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
# start Validation Reply Form
_vrf_PLAT910_1122-ga-93-exp_1589_sq 
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         22 Note  
RESPONSE: The missing FCF reflections below theta(min) were caused
by the high beamstop theta(min) limit set.
;
_vrf_PLAT053_1122-ga-93-exp_1589_sq 
;
PROBLEM: Minimum Crystal Dimension Missing (or Error) ...     Please Check 
RESPONSE: ...
;
_vrf_PLAT054_1122-ga-93-exp_1589_sq 
;
PROBLEM: Medium  Crystal Dimension Missing (or Error) ...     Please Check 
RESPONSE: ...
;
_vrf_PLAT055_1122-ga-93-exp_1589_sq 
;
PROBLEM: Maximum Crystal Dimension Missing (or Error) ...     Please Check 
RESPONSE: ...
;
_vrf_PLAT230_1122-ga-93-exp_1589_sq 
;
PROBLEM: Hirshfeld Test Diff for    N8       --C27      .        5.2 s.u.  
RESPONSE: ...
;
_vrf_PLAT241_1122-ga-93-exp_1589_sq 
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of        C32 Check 
RESPONSE: ...
;
_vrf_PLAT420_1122-ga-93-exp_1589_sq 
;
PROBLEM: D-H Bond Without Acceptor  N5       --H5       .     Please Check 
RESPONSE: ...
;
_vrf_PLAT911_1122-ga-93-exp_1589_sq 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600          3 Report
RESPONSE: ...
;
_vrf_PLAT976_1122-ga-93-exp_1589_sq 
;
PROBLEM: Check Calcd Resid. Dens.  1.10Ang From N5      .      -0.47 eA-3  
RESPONSE: ...
;
_vrf_PLAT977_1122-ga-93-exp_1589_sq 
;
PROBLEM: Check Negative Difference Density on H5        .      -0.37 eA-3  
RESPONSE: ...
;
# end Validation Reply Form
