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

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

data_exp_9159
_database_code_depnum_ccdc_archive 'CCDC 2021785'
loop_
_audit_author_name
_audit_author_address
'Houting Liu'
;Liaocheng University
China
;
_audit_update_record             
;
2020-08-06 deposited with the CCDC.	2020-09-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10.50 H14 Cd N0 O8'
_chemical_formula_weight         380.62

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd 0.1185 4.6533 '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                   7.7192(3)
_cell_length_b                   18.9505(7)
_cell_length_c                   19.3675(12)
_cell_angle_alpha                90
_cell_angle_beta                 98.008(5)
_cell_angle_gamma                90
_cell_volume                     2805.5(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2176
_cell_measurement_theta_min      4.6180
_cell_measurement_theta_max      71.2900

_exptl_crystal_description       block
_exptl_crystal_colour            white
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.802
_exptl_crystal_F_000             1512
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    12.799
_shelx_estimated_absorpt_T_min   0.309
_shelx_estimated_absorpt_T_max   0.333
_exptl_absorpt_correction_T_min  0.16731
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            4877
_diffrn_reflns_av_unetI/netI     0.0566
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         4.611
_diffrn_reflns_theta_max         67.241
_diffrn_reflns_theta_full        67.241
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total             2498
_reflns_number_gt                2052
_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       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_structure_solution    'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0820P)²+9.8531P] 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         2498
_refine_ls_number_parameters     187
_refine_ls_number_restraints     396
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0541
_refine_ls_wR_factor_ref         0.1546
_refine_ls_wR_factor_gt          0.1446
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.047
_refine_ls_shift/su_max          0.007
_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 -0.22034(5) 0.55178(2) 0.46903(3) 0.0459(2) Uani 1 1 d . U . . .
O1 O 0.0456(7) 0.5772(3) 0.5217(4) 0.0721(17) Uani 1 1 d . U . . .
O2 O 0.3088(7) 0.5562(3) 0.5693(4) 0.0599(15) Uani 1 1 d . U . . .
O3 O -0.3035(14) 0.5264(5) 0.5751(5) 0.113(3) Uani 1 1 d . U . . .
H3A H -0.378090 0.556686 0.584399 0.170 Uiso 1 1 d R U . . .
H3B H -0.348920 0.485457 0.573879 0.170 Uiso 1 1 d R U . . .
O4 O -0.1146(10) 0.5680(4) 0.3637(4) 0.080(2) Uani 1 1 d . U . . .
H4A H -0.174827 0.598060 0.338024 0.120 Uiso 1 1 d R U . . .
H4C H -0.110757 0.529520 0.341474 0.120 Uiso 1 1 d R U . . .
O5 O -0.1718(6) 0.8330(3) 0.5248(3) 0.0526(13) Uani 1 1 d . U . . .
O6 O 0.0026(6) 0.9104(2) 0.5808(3) 0.0532(13) Uani 1 1 d . U . . .
O7 O 0.5551(6) 0.7893(2) 0.6628(3) 0.0408(10) Uani 1 1 d . U . . .
C1 C 0.1834(8) 0.5978(3) 0.5539(4) 0.0365(13) Uani 1 1 d . U . . .
C2 C 0.2087(7) 0.6735(3) 0.5742(3) 0.0299(11) Uani 1 1 d . U . . .
C3 C 0.3725(8) 0.6938(3) 0.6100(3) 0.0330(12) Uani 1 1 d . U . . .
H3 H 0.460093 0.660416 0.621357 0.040 Uiso 1 1 calc R U . . .
C4 C 0.4021(7) 0.7636(3) 0.6279(3) 0.0296(11) Uani 1 1 d . U . . .
C5 C 0.2702(8) 0.8132(3) 0.6109(3) 0.0300(11) Uani 1 1 d . U . . .
H5 H 0.290318 0.860120 0.623562 0.036 Uiso 1 1 calc R U . . .
C6 C 0.1092(7) 0.7936(3) 0.5752(3) 0.0284(11) Uani 1 1 d . U . . .
C7 C 0.0785(7) 0.7232(3) 0.5560(3) 0.0323(12) Uani 1 1 d . U . . .
H7 H -0.028294 0.709766 0.531243 0.039 Uiso 1 1 calc R U . . .
C8 C -0.0282(8) 0.8490(3) 0.5580(4) 0.0378(13) Uani 1 1 d . U . . .
C9 C 0.6964(8) 0.7411(4) 0.6819(4) 0.0403(14) Uani 1 1 d . U . . .
H9A H 0.729276 0.718334 0.640815 0.048 Uiso 1 1 calc R U . . .
H9B H 0.662275 0.705006 0.712908 0.048 Uiso 1 1 calc R U . . .
C10 C 0.8467(8) 0.7837(4) 0.7181(3) 0.0380(14) Uani 1 1 d . U . . .
H10A H 0.805905 0.811624 0.754659 0.046 Uiso 1 1 calc R U . . .
H10B H 0.886558 0.816064 0.684871 0.046 Uiso 1 1 calc R U . . .
C11 C 1.000000 0.7384(5) 0.750000 0.040(2) Uani 1 2 d S TU P . .
H11A H 0.963049 0.708356 0.785750 0.047 Uiso 0.5 1 calc R U P . .
H11B H 1.036949 0.708355 0.714250 0.047 Uiso 0.5 1 calc R U P . .
O8 O 0.126(5) 0.4457(16) 0.2998(15) 0.219(12) Uani 0.503(18) 1 d . U P A 1
H8C H 0.208197 0.444371 0.333801 0.263 Uiso 0.503(18) 1 d R U P A 1
H8D H 0.053437 0.477221 0.308621 0.263 Uiso 0.503(18) 1 d R U P A 1
O8' O 0.325(6) 0.468(2) 0.2334(18) 0.249(14) Uani 0.497(18) 1 d . U P A 2
H8'C H 0.323578 0.478626 0.275993 0.299 Uiso 0.497(18) 1 d R U P A 2
H8'D H 0.278388 0.501598 0.208223 0.299 Uiso 0.497(18) 1 d R U 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
Cd1 O1 2.214(5) . ?
Cd1 O2 2.250(5) 5_566 ?
Cd1 O3 2.288(9) . ?
Cd1 O4 2.321(8) . ?
Cd1 O5 2.346(5) 7_466 ?
Cd1 O6 2.368(5) 7_466 ?
Cd1 C8 2.700(6) 7_466 ?
O1 C1 1.220(8) . ?
O2 C1 1.253(8) . ?
O5 C8 1.239(8) . ?
O6 C8 1.255(8) . ?
O7 C4 1.366(7) . ?
O7 C9 1.431(7) . ?
C1 C2 1.493(8) . ?
C2 C7 1.386(8) . ?
C2 C3 1.408(8) . ?
C3 C4 1.379(8) . ?
C4 C5 1.390(8) . ?
C5 C6 1.386(8) . ?
C6 C7 1.396(9) . ?
C6 C8 1.498(8) . ?
C9 C10 1.505(8) . ?
C10 C11 1.521(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cd1 O2 124.7(2) . 5_566 ?
O1 Cd1 O3 89.4(3) . . ?
O2 Cd1 O3 89.7(3) 5_566 . ?
O1 Cd1 O4 87.7(3) . . ?
O2 Cd1 O4 87.6(3) 5_566 . ?
O3 Cd1 O4 174.0(3) . . ?
O1 Cd1 O5 95.0(2) . 7_466 ?
O2 Cd1 O5 140.33(19) 5_566 7_466 ?
O3 Cd1 O5 90.2(3) . 7_466 ?
O4 Cd1 O5 95.3(2) . 7_466 ?
O1 Cd1 O6 149.7(2) . 7_466 ?
O2 Cd1 O6 85.46(18) 5_566 7_466 ?
O3 Cd1 O6 94.2(3) . 7_466 ?
O4 Cd1 O6 91.0(3) . 7_466 ?
O5 Cd1 O6 54.99(16) 7_466 7_466 ?
O1 Cd1 C8 122.2(2) . 7_466 ?
O2 Cd1 C8 113.1(2) 5_566 7_466 ?
O3 Cd1 C8 92.1(3) . 7_466 ?
O4 Cd1 C8 93.9(3) . 7_466 ?
O5 Cd1 C8 27.29(19) 7_466 7_466 ?
O6 Cd1 C8 27.70(18) 7_466 7_466 ?
C1 O1 Cd1 172.5(6) . . ?
C1 O2 Cd1 107.8(4) . 5_566 ?
C8 O5 Cd1 92.5(4) . 7_466 ?
C8 O6 Cd1 91.0(4) . 7_466 ?
C4 O7 C9 118.4(5) . . ?
O1 C1 O2 120.6(6) . . ?
O1 C1 C2 121.1(6) . . ?
O2 C1 C2 118.3(6) . . ?
C7 C2 C3 120.6(5) . . ?
C7 C2 C1 121.4(5) . . ?
C3 C2 C1 117.9(5) . . ?
C4 C3 C2 119.5(5) . . ?
O7 C4 C3 124.6(5) . . ?
O7 C4 C5 115.5(5) . . ?
C3 C4 C5 119.9(5) . . ?
C6 C5 C4 120.9(5) . . ?
C5 C6 C7 119.7(5) . . ?
C5 C6 C8 118.8(5) . . ?
C7 C6 C8 121.5(5) . . ?
C2 C7 C6 119.4(5) . . ?
O5 C8 O6 121.5(6) . . ?
O5 C8 C6 119.9(6) . . ?
O6 C8 C6 118.5(6) . . ?
O5 C8 Cd1 60.2(3) . 7_466 ?
O6 C8 Cd1 61.3(3) . 7_466 ?
C6 C8 Cd1 178.1(5) . 7_466 ?
O7 C9 C10 106.7(5) . . ?
C9 C10 C11 113.1(6) . . ?
C10 C11 C10 111.3(8) 2_756 . ?

_refine_diff_density_max         1.286
_refine_diff_density_min         -0.944
_refine_diff_density_rms         0.148

####################################################################### 
# 
# 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_exp_11435
_database_code_depnum_ccdc_archive 'CCDC 2021786'
loop_
_audit_author_name
_audit_author_address
'Liu Hou-Ting'
;Liaocheng University
China
;
_audit_update_record             
;
2020-09-10 deposited with the CCDC.	2020-09-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C41 H34 Br4 N4 Ni2 O13'
_chemical_formula_weight         1227.78

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   9.7846(6)
_cell_length_b                   15.8653(10)
_cell_length_c                   16.2608(14)
_cell_angle_alpha                65.276(7)
_cell_angle_beta                 83.245(6)
_cell_angle_gamma                73.817(5)
_cell_volume                     2202.0(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2445
_cell_measurement_theta_min      3.1590
_cell_measurement_theta_max      70.7410

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.852
_exptl_crystal_F_000             1216
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    5.910
_shelx_estimated_absorpt_T_min   0.682
_shelx_estimated_absorpt_T_max   0.718
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14227
_diffrn_reflns_av_unetI/netI     0.1036
_diffrn_reflns_av_R_equivalents  0.0621
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.992
_diffrn_reflns_theta_max         67.250
_diffrn_reflns_theta_full        67.250
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             7878
_reflns_number_gt                4531
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0889P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7878
_refine_ls_number_parameters     577
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1229
_refine_ls_R_factor_gt           0.0650
_refine_ls_wR_factor_ref         0.1908
_refine_ls_wR_factor_gt          0.1547
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_restrained_S_all      1.003
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.20432(13) 1.29222(9) 0.47014(9) 0.0331(3) Uani 1 1 d . . . . .
Ni2 Ni 0.05621(13) 1.11669(9) 0.75108(9) 0.0350(3) Uani 1 1 d . . . . .
Br1 Br -0.48646(11) 1.09373(9) 1.04789(8) 0.0648(3) Uani 1 1 d . . . . .
Br2 Br 0.15160(15) 0.65987(8) 1.04758(9) 0.0802(4) Uani 1 1 d . . . . .
Br3 Br 0.87283(10) 1.08201(8) 0.40836(9) 0.0631(3) Uani 1 1 d . . . . .
Br4 Br 0.56876(11) 1.62379(7) 0.35024(8) 0.0535(3) Uani 1 1 d . . . . .
N1 N -0.1273(7) 1.1171(5) 0.8319(5) 0.0401(17) Uani 1 1 d . . . . .
N2 N 0.0845(7) 0.9722(5) 0.8324(5) 0.0358(16) Uani 1 1 d . . . . .
N3 N 0.3104(7) 1.3952(4) 0.4442(5) 0.0353(16) Uani 1 1 d . . . . .
N4 N 0.3993(7) 1.2319(5) 0.4254(5) 0.0358(16) Uani 1 1 d . . . . .
O1 O 0.2514(5) 1.0854(4) 0.6981(4) 0.0433(15) Uani 1 1 d . . . . .
O2 O 0.2953(6) 1.2240(4) 0.5997(4) 0.0425(15) Uani 1 1 d . . . . .
O3 O 0.8006(6) 1.2482(4) 0.5650(4) 0.0458(16) Uani 1 1 d . . . . .
O4 O 0.9692(5) 1.1188(4) 0.6432(4) 0.0394(14) Uani 1 1 d . . . . .
O5 O 0.8536(6) 0.8341(4) 1.1661(4) 0.0431(15) Uani 1 1 d . . . . .
O6 O 0.9777(6) 0.7351(4) 1.2889(4) 0.0362(13) Uani 1 1 d . . . . .
O7 O 1.1157(6) 0.3805(4) 1.3459(4) 0.0400(14) Uani 1 1 d . . . . .
O8 O 0.9224(6) 0.3297(4) 1.3509(4) 0.0510(17) Uani 1 1 d . . . . .
O9 O 0.7160(6) 0.8501(4) 0.7657(5) 0.061(2) Uani 1 1 d . . . . .
O10 O 0.6221(7) 0.6245(5) 1.0972(5) 0.0563(17) Uani 1 1 d . . . . .
O11 O 0.1168(6) 1.1849(4) 0.4802(4) 0.0426(15) Uani 1 1 d . . . . .
H11B H 0.144121 1.131097 0.536834 0.064 Uiso 1 1 d R U . . .
H11C H 0.014962 1.207879 0.477494 0.064 Uiso 1 1 d R U . . .
O12 O 0.0200(5) 1.3493(4) 0.5279(4) 0.0385(14) Uani 1 1 d . . . . .
H12B H 0.028897 1.319502 0.592638 0.058 Uiso 1 1 d R U . . .
H12D H -0.060382 1.337158 0.510336 0.058 Uiso 1 1 d R U . . .
O13 O 0.3097(11) 0.4636(7) 0.2184(6) 0.109(3) Uani 1 1 d . . . . .
H13C H 0.249313 0.440480 0.257256 0.130 Uiso 1 1 d R U . . .
H13B H 0.267943 0.503260 0.168766 0.130 Uiso 1 1 d R U . . .
C1 C -0.2337(9) 1.1923(6) 0.8259(6) 0.046(2) Uani 1 1 d . . . . .
H1 H -0.233643 1.250647 0.777694 0.055 Uiso 1 1 calc R U . . .
C2 C -0.3450(9) 1.1893(6) 0.8871(6) 0.047(2) Uani 1 1 d . . . . .
H2 H -0.418356 1.243611 0.880394 0.056 Uiso 1 1 calc R U . . .
C3 C -0.3424(9) 1.1032(7) 0.9578(6) 0.046(2) Uani 1 1 d . . . . .
C4 C -0.2343(9) 1.0226(6) 0.9681(6) 0.045(2) Uani 1 1 d . . . . .
H4 H -0.232652 0.964471 1.017038 0.054 Uiso 1 1 calc R U . . .
C5 C -0.1277(9) 1.0309(6) 0.9030(6) 0.038(2) Uani 1 1 d . . . . .
C6 C -0.0084(8) 0.9507(6) 0.9024(6) 0.0350(19) Uani 1 1 d . . . . .
C7 C 0.0105(9) 0.8575(6) 0.9679(6) 0.042(2) Uani 1 1 d . . . . .
H7 H -0.051173 0.843131 1.016993 0.050 Uiso 1 1 calc R U . . .
C8 C 0.1214(10) 0.7873(6) 0.9587(7) 0.048(2) Uani 1 1 d . . . . .
C9 C 0.2125(10) 0.8086(7) 0.8863(7) 0.050(2) Uani 1 1 d . . . . .
H9 H 0.286981 0.760794 0.879254 0.060 Uiso 1 1 calc R U . . .
C10 C 0.1910(9) 0.9023(6) 0.8246(7) 0.046(2) Uani 1 1 d . . . . .
H10 H 0.252769 0.917348 0.775609 0.055 Uiso 1 1 calc R U . . .
C11 C 0.2529(9) 1.4818(6) 0.4424(6) 0.043(2) Uani 1 1 d . . . . .
H11A H 0.158632 1.495531 0.460805 0.051 Uiso 1 1 calc R U . . .
C12 C 0.3242(9) 1.5538(6) 0.4149(6) 0.045(2) Uani 1 1 d . . . . .
H12A H 0.280388 1.614063 0.414544 0.054 Uiso 1 1 calc R U . . .
C13 C 0.4648(9) 1.5305(6) 0.3878(6) 0.040(2) Uani 1 1 d . . . . .
C14 C 0.5291(9) 1.4403(6) 0.3905(6) 0.041(2) Uani 1 1 d . . . . .
H14 H 0.624188 1.424323 0.374509 0.050 Uiso 1 1 calc R U . . .
C15 C 0.4479(8) 1.3740(6) 0.4177(5) 0.0331(18) Uani 1 1 d . . . . .
C16 C 0.4999(8) 1.2785(6) 0.4160(6) 0.0342(18) Uani 1 1 d . . . . .
C17 C 0.6418(8) 1.2373(6) 0.4078(6) 0.039(2) Uani 1 1 d . . . . .
H17 H 0.710372 1.270227 0.401146 0.047 Uiso 1 1 calc R U . . .
C18 C 0.6795(8) 1.1465(6) 0.4096(6) 0.042(2) Uani 1 1 d . . . . .
C19 C 0.5770(9) 1.0983(6) 0.4176(6) 0.044(2) Uani 1 1 d . . . . .
H19 H 0.600846 1.036485 0.419488 0.053 Uiso 1 1 calc R U . . .
C20 C 0.4375(9) 1.1471(6) 0.4224(6) 0.044(2) Uani 1 1 d . . . . .
H20 H 0.366307 1.118120 0.423719 0.052 Uiso 1 1 calc R U . . .
C21 C 0.3337(8) 1.1378(6) 0.6531(6) 0.0341(18) Uani 1 1 d . . . . .
C22 C 0.4910(8) 1.0915(5) 0.6666(5) 0.0303(17) Uani 1 1 d . . . . .
C23 C 0.5899(7) 1.1466(5) 0.6350(5) 0.0316(18) Uani 1 1 d . . . . .
H23 H 0.559322 1.212969 0.604780 0.038 Uiso 1 1 calc R U . . .
C24 C 0.7335(8) 1.1025(6) 0.6486(5) 0.0333(18) Uani 1 1 d . . . . .
C25 C 0.7803(8) 1.0029(6) 0.6947(6) 0.040(2) Uani 1 1 d . . . . .
H25 H 0.876885 0.973445 0.705180 0.048 Uiso 1 1 calc R U . . .
C26 C 0.6819(8) 0.9485(6) 0.7247(6) 0.040(2) Uani 1 1 d . . . . .
C27 C 0.5392(8) 0.9929(6) 0.7122(6) 0.041(2) Uani 1 1 d . . . . .
H27 H 0.473459 0.956038 0.734746 0.049 Uiso 1 1 calc R U . . .
C28 C 0.8616(9) 0.7985(6) 0.7887(7) 0.053(3) Uani 1 1 d . . . . .
H28A H 0.900807 0.823319 0.823449 0.064 Uiso 1 1 calc R U . . .
H28B H 0.918371 0.804837 0.734369 0.064 Uiso 1 1 calc R U . . .
C29 C 0.8621(12) 0.6958(7) 0.8437(7) 0.063(3) Uani 1 1 d . . . . .
H29A H 0.958492 0.659445 0.863751 0.076 Uiso 1 1 calc R U . . .
H29B H 0.832706 0.670638 0.805538 0.076 Uiso 1 1 calc R U . . .
C30 C 0.7660(14) 0.6811(7) 0.9251(8) 0.075(3) Uani 1 1 d . . . . .
H30A H 0.670587 0.719877 0.904980 0.090 Uiso 1 1 calc R U . . .
H30B H 0.797911 0.704261 0.964121 0.090 Uiso 1 1 calc R U . . .
C31 C 0.7596(14) 0.5782(7) 0.9802(8) 0.071(3) Uani 1 1 d . . . . .
H31A H 0.753571 0.548994 0.939356 0.085 Uiso 1 1 calc R U . . .
H31B H 0.846892 0.542839 1.014672 0.085 Uiso 1 1 calc R U . . .
C32 C 0.6344(12) 0.5697(7) 1.0446(8) 0.064(3) Uani 1 1 d . . . . .
H32A H 0.547690 0.591331 1.010114 0.077 Uiso 1 1 calc R U . . .
H32B H 0.644950 0.502752 1.084963 0.077 Uiso 1 1 calc R U . . .
C33 C 0.7334(9) 0.6030(6) 1.1526(6) 0.041(2) Uani 1 1 d . . . . .
C34 C 0.8065(9) 0.5094(6) 1.2059(6) 0.041(2) Uani 1 1 d . . . . .
H34 H 0.784647 0.457535 1.202511 0.050 Uiso 1 1 calc R U . . .
C35 C 0.9116(8) 0.4947(6) 1.2637(6) 0.0343(19) Uani 1 1 d . . . . .
C36 C 0.9439(8) 0.5723(6) 1.2689(6) 0.038(2) Uani 1 1 d . . . . .
H36 H 1.014839 0.561562 1.308100 0.046 Uiso 1 1 calc R U . . .
C37 C 0.8719(8) 0.6649(6) 1.2166(6) 0.0358(19) Uani 1 1 d . . . . .
C38 C 0.7653(9) 0.6805(6) 1.1569(6) 0.041(2) Uani 1 1 d . . . . .
H38 H 0.716718 0.742683 1.120645 0.049 Uiso 1 1 calc R U . . .
C39 C 0.8394(8) 1.1620(6) 0.6161(6) 0.0350(19) Uani 1 1 d . . . . .
C40 C 0.9029(8) 0.7489(6) 1.2236(6) 0.038(2) Uani 1 1 d . . . . .
C41 C 0.9872(8) 0.3924(6) 1.3258(6) 0.0368(19) 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
Ni1 O7 2.040(6) 1_464 ?
Ni1 N3 2.048(6) . ?
Ni1 O11 2.052(5) . ?
Ni1 N4 2.079(7) . ?
Ni1 O12 2.087(6) . ?
Ni1 O2 2.097(6) . ?
Ni2 O1 2.020(5) . ?
Ni2 O4 2.022(6) 1_455 ?
Ni2 N2 2.068(6) . ?
Ni2 O6 2.097(5) 2_677 ?
Ni2 N1 2.097(7) . ?
Ni2 O5 2.178(6) 2_677 ?
Ni2 C40 2.475(9) 2_677 ?
Br1 C3 1.899(8) . ?
Br2 C8 1.895(8) . ?
Br3 C18 1.885(8) . ?
Br4 C13 1.880(8) . ?
N1 C1 1.324(11) . ?
N1 C5 1.373(10) . ?
N2 C10 1.333(11) . ?
N2 C6 1.357(10) . ?
N3 C11 1.321(10) . ?
N3 C15 1.357(10) . ?
N4 C20 1.312(10) . ?
N4 C16 1.347(10) . ?
O1 C21 1.264(9) . ?
O2 C21 1.250(9) . ?
O3 C39 1.240(10) . ?
O4 C39 1.293(9) . ?
O5 C40 1.272(10) . ?
O6 C40 1.269(10) . ?
O7 C41 1.279(9) . ?
O8 C41 1.229(9) . ?
O9 C26 1.373(10) . ?
O9 C28 1.435(10) . ?
O10 C33 1.372(10) . ?
O10 C32 1.429(12) . ?
C1 C2 1.382(12) . ?
C2 C3 1.365(12) . ?
C3 C4 1.375(13) . ?
C4 C5 1.388(11) . ?
C5 C6 1.470(12) . ?
C6 C7 1.389(11) . ?
C7 C8 1.366(12) . ?
C8 C9 1.371(13) . ?
C9 C10 1.374(12) . ?
C11 C12 1.391(11) . ?
C12 C13 1.390(12) . ?
C13 C14 1.377(12) . ?
C14 C15 1.388(10) . ?
C15 C16 1.469(11) . ?
C16 C17 1.377(11) . ?
C17 C18 1.373(12) . ?
C18 C19 1.386(11) . ?
C19 C20 1.380(12) . ?
C21 C22 1.506(10) . ?
C22 C27 1.386(11) . ?
C22 C23 1.395(10) . ?
C23 C24 1.382(10) . ?
C24 C25 1.398(11) . ?
C24 C39 1.499(10) . ?
C25 C26 1.382(11) . ?
C26 C27 1.374(11) . ?
C28 C29 1.494(13) . ?
C29 C30 1.504(15) . ?
C30 C31 1.514(14) . ?
C31 C32 1.512(16) . ?
C33 C38 1.381(12) . ?
C33 C34 1.394(12) . ?
C34 C35 1.381(11) . ?
C35 C36 1.390(11) . ?
C35 C41 1.528(11) . ?
C36 C37 1.377(11) . ?
C37 C38 1.408(12) . ?
C37 C40 1.498(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O7 Ni1 N3 84.3(2) 1_464 . ?
O7 Ni1 O11 92.4(2) 1_464 . ?
N3 Ni1 O11 171.1(3) . . ?
O7 Ni1 N4 97.4(2) 1_464 . ?
N3 Ni1 N4 79.1(3) . . ?
O11 Ni1 N4 93.2(2) . . ?
O7 Ni1 O12 88.3(2) 1_464 . ?
N3 Ni1 O12 98.9(2) . . ?
O11 Ni1 O12 89.2(2) . . ?
N4 Ni1 O12 173.8(3) . . ?
O7 Ni1 O2 169.9(2) 1_464 . ?
N3 Ni1 O2 87.3(2) . . ?
O11 Ni1 O2 96.8(2) . . ?
N4 Ni1 O2 86.4(3) . . ?
O12 Ni1 O2 87.6(2) . . ?
O1 Ni2 O4 89.3(2) . 1_455 ?
O1 Ni2 N2 88.8(2) . . ?
O4 Ni2 N2 97.9(3) 1_455 . ?
O1 Ni2 O6 100.4(2) . 2_677 ?
O4 Ni2 O6 99.0(2) 1_455 2_677 ?
N2 Ni2 O6 160.8(3) . 2_677 ?
O1 Ni2 N1 166.1(3) . . ?
O4 Ni2 N1 97.4(3) 1_455 . ?
N2 Ni2 N1 78.3(3) . . ?
O6 Ni2 N1 90.6(2) 2_677 . ?
O1 Ni2 O5 88.9(2) . 2_677 ?
O4 Ni2 O5 159.9(2) 1_455 2_677 ?
N2 Ni2 O5 102.1(2) . 2_677 ?
O6 Ni2 O5 61.7(2) 2_677 2_677 ?
N1 Ni2 O5 88.9(3) . 2_677 ?
O1 Ni2 C40 94.2(2) . 2_677 ?
O4 Ni2 C40 129.4(3) 1_455 2_677 ?
N2 Ni2 C40 132.6(3) . 2_677 ?
O6 Ni2 C40 30.8(2) 2_677 2_677 ?
N1 Ni2 C40 90.9(3) . 2_677 ?
O5 Ni2 C40 30.9(2) 2_677 2_677 ?
C1 N1 C5 118.0(7) . . ?
C1 N1 Ni2 126.9(6) . . ?
C5 N1 Ni2 114.8(5) . . ?
C10 N2 C6 119.4(7) . . ?
C10 N2 Ni2 124.9(5) . . ?
C6 N2 Ni2 115.5(5) . . ?
C11 N3 C15 118.6(7) . . ?
C11 N3 Ni1 125.6(5) . . ?
C15 N3 Ni1 115.3(5) . . ?
C20 N4 C16 118.8(7) . . ?
C20 N4 Ni1 126.1(5) . . ?
C16 N4 Ni1 113.8(5) . . ?
C21 O1 Ni2 131.6(5) . . ?
C21 O2 Ni1 132.7(6) . . ?
C39 O4 Ni2 125.0(5) . 1_655 ?
C40 O5 Ni2 87.5(5) . 2_677 ?
C40 O6 Ni2 91.3(5) . 2_677 ?
C41 O7 Ni1 124.0(5) . 1_646 ?
C26 O9 C28 119.2(7) . . ?
C33 O10 C32 118.0(8) . . ?
N1 C1 C2 123.9(8) . . ?
C3 C2 C1 117.1(8) . . ?
C2 C3 C4 121.8(8) . . ?
C2 C3 Br1 119.9(7) . . ?
C4 C3 Br1 118.2(7) . . ?
C3 C4 C5 117.8(8) . . ?
N1 C5 C4 121.4(8) . . ?
N1 C5 C6 114.3(7) . . ?
C4 C5 C6 124.3(8) . . ?
N2 C6 C7 120.6(7) . . ?
N2 C6 C5 115.9(7) . . ?
C7 C6 C5 123.4(7) . . ?
C8 C7 C6 118.7(8) . . ?
C7 C8 C9 120.6(8) . . ?
C7 C8 Br2 119.7(7) . . ?
C9 C8 Br2 119.6(7) . . ?
C8 C9 C10 118.4(9) . . ?
N2 C10 C9 122.2(8) . . ?
N3 C11 C12 124.2(8) . . ?
C13 C12 C11 116.1(8) . . ?
C14 C13 C12 121.2(8) . . ?
C14 C13 Br4 120.1(6) . . ?
C12 C13 Br4 118.7(6) . . ?
C13 C14 C15 118.1(8) . . ?
N3 C15 C14 121.6(7) . . ?
N3 C15 C16 114.8(6) . . ?
C14 C15 C16 123.5(7) . . ?
N4 C16 C17 121.5(7) . . ?
N4 C16 C15 115.5(7) . . ?
C17 C16 C15 123.0(7) . . ?
C18 C17 C16 118.3(7) . . ?
C17 C18 C19 120.8(8) . . ?
C17 C18 Br3 120.4(6) . . ?
C19 C18 Br3 118.7(7) . . ?
C20 C19 C18 116.3(8) . . ?
N4 C20 C19 124.0(8) . . ?
O2 C21 O1 125.5(7) . . ?
O2 C21 C22 118.0(7) . . ?
O1 C21 C22 116.5(7) . . ?
C27 C22 C23 119.0(7) . . ?
C27 C22 C21 120.0(7) . . ?
C23 C22 C21 121.0(7) . . ?
C24 C23 C22 119.8(7) . . ?
C23 C24 C25 120.4(7) . . ?
C23 C24 C39 119.7(7) . . ?
C25 C24 C39 119.8(7) . . ?
C26 C25 C24 119.4(7) . . ?
O9 C26 C27 115.7(7) . . ?
O9 C26 C25 124.5(7) . . ?
C27 C26 C25 119.8(8) . . ?
C26 C27 C22 121.4(7) . . ?
O9 C28 C29 106.6(8) . . ?
C28 C29 C30 113.6(9) . . ?
C29 C30 C31 114.9(10) . . ?
C32 C31 C30 113.0(9) . . ?
O10 C32 C31 112.5(9) . . ?
O10 C33 C38 115.7(8) . . ?
O10 C33 C34 123.3(8) . . ?
C38 C33 C34 120.8(8) . . ?
C35 C34 C33 119.2(8) . . ?
C34 C35 C36 120.3(8) . . ?
C34 C35 C41 119.6(7) . . ?
C36 C35 C41 119.9(7) . . ?
C37 C36 C35 120.7(8) . . ?
C36 C37 C38 119.3(8) . . ?
C36 C37 C40 121.1(8) . . ?
C38 C37 C40 119.6(7) . . ?
C33 C38 C37 119.6(8) . . ?
O3 C39 O4 123.5(7) . . ?
O3 C39 C24 119.8(7) . . ?
O4 C39 C24 116.7(7) . . ?
O6 C40 O5 119.4(8) . . ?
O6 C40 C37 119.5(7) . . ?
O5 C40 C37 121.2(8) . . ?
O6 C40 Ni2 57.9(4) . 2_677 ?
O5 C40 Ni2 61.6(4) . 2_677 ?
C37 C40 Ni2 174.8(6) . 2_677 ?
O8 C41 O7 125.9(8) . . ?
O8 C41 C35 118.7(7) . . ?
O7 C41 C35 115.3(7) . . ?

_refine_diff_density_max         2.351
_refine_diff_density_min         -0.652
_refine_diff_density_rms         0.127

####################################################################### 
# 
# 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_exp_9169
_database_code_depnum_ccdc_archive 'CCDC 2021787'
loop_
_audit_author_name
_audit_author_address
'Liu Hou-Ting'
;Liaocheng University
China
;
_audit_update_record             
;
2020-09-10 deposited with the CCDC.	2020-09-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C31 H30 N2 Ni O12'
_chemical_formula_weight         681.28

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   8.3958(8)
_cell_length_b                   12.1818(11)
_cell_length_c                   15.1802(14)
_cell_angle_alpha                102.597(8)
_cell_angle_beta                 95.828(8)
_cell_angle_gamma                94.332(8)
_cell_volume                     1499.7(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1710
_cell_measurement_theta_min      3.0110
_cell_measurement_theta_max      71.1430

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_F_000             708
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    1.542
_shelx_estimated_absorpt_T_min   0.837
_shelx_estimated_absorpt_T_max   0.849
_exptl_absorpt_correction_T_min  0.75349
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9352
_diffrn_reflns_av_unetI/netI     0.1930
_diffrn_reflns_av_R_equivalents  0.1307
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.737
_diffrn_reflns_theta_max         67.233
_diffrn_reflns_theta_full        67.233
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             5328
_reflns_number_gt                3137
_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       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_structure_solution    'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0761P)²+1.8635P] 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         5328
_refine_ls_number_parameters     418
_refine_ls_number_restraints     1110
_refine_ls_R_factor_all          0.1395
_refine_ls_R_factor_gt           0.0721
_refine_ls_wR_factor_ref         0.2108
_refine_ls_wR_factor_gt          0.1714
_refine_ls_goodness_of_fit_ref   0.876
_refine_ls_restrained_S_all      0.805
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 1.500000 0.500000 0.500000 0.0195(3) Uani 1 2 d S U P . .
Ni2 Ni 0.500000 0.000000 0.000000 0.0179(3) Uani 1 2 d S U P . .
N1 N 1.2967(6) 0.4098(4) 0.4232(3) 0.0245(10) Uani 1 1 d . U . . .
N2 N 0.6562(6) 0.0740(4) 0.1218(3) 0.0236(10) Uani 1 1 d . U . . .
O1 O 1.5884(6) 0.0910(4) 0.7694(3) 0.0451(12) Uani 1 1 d . U . . .
H1 H 1.583550 0.062491 0.813381 0.068 Uiso 1 1 calc R U . . .
O2 O 1.6781(8) -0.0714(4) 0.7105(4) 0.0681(18) Uani 1 1 d . U . . .
O3 O 1.7913(6) -0.0265(4) 0.3943(3) 0.0440(11) Uani 1 1 d . U . . .
O4 O 1.5066(5) 0.3793(3) 0.5830(2) 0.0248(8) Uani 1 1 d . U . . .
O5 O 1.6269(5) 0.3600(3) 0.4598(2) 0.0259(8) Uani 1 1 d . U . . .
O7 O 0.3119(4) -0.0247(3) 0.0754(2) 0.0244(8) Uani 1 1 d . U . . .
H7B H 0.228550 -0.055647 0.039401 0.029 Uiso 1 1 d R U . . .
H7D H 0.292340 0.038843 0.106301 0.037 Uiso 1 1 d R U . . .
O8 O 0.4420(4) 0.1558(3) -0.0107(2) 0.0220(8) Uani 1 1 d . U . . .
O9 O 0.2304(5) 0.1795(3) 0.0664(3) 0.0277(9) Uani 1 1 d . U . . .
O10 O 0.1652(5) 0.5995(3) 0.0735(3) 0.0342(10) Uani 1 1 d . U . . .
O11 O 0.4571(6) 0.3735(4) -0.2477(3) 0.0451(12) Uani 1 1 d . U . . .
H11 H 0.484062 0.388520 -0.294505 0.068 Uiso 1 1 calc R U . . .
O12 O 0.4152(8) 0.5531(4) -0.2165(4) 0.0638(17) Uani 1 1 d . U . . .
O13 O 0.0980(6) 0.7966(4) 0.9941(4) 0.0518(14) Uani 1 1 d . . . . .
H13C H -0.001399 0.798521 0.977618 0.062 Uiso 1 1 d R U . . .
H13D H 0.108741 0.738621 1.015989 0.062 Uiso 1 1 d R U . . .
C1 C 1.6414(9) 0.0193(5) 0.7032(4) 0.0359(14) Uani 1 1 d . U . . .
C2 C 1.6546(8) 0.0628(5) 0.6194(4) 0.0289(12) Uani 1 1 d . U . . .
C3 C 1.7159(8) -0.0068(5) 0.5480(4) 0.0314(13) Uani 1 1 d . U . . .
H3 H 1.744768 -0.077633 0.552957 0.038 Uiso 1 1 calc R U . . .
C4 C 1.7333(8) 0.0314(5) 0.4688(4) 0.0301(12) Uani 1 1 d . U . . .
C5 C 1.8443(8) -0.1354(5) 0.3932(4) 0.0353(14) Uani 1 1 d . U . . .
H5A H 1.756057 -0.188597 0.398944 0.042 Uiso 1 1 calc R U . . .
H5B H 1.929419 -0.131320 0.442428 0.042 Uiso 1 1 calc R U . . .
C6 C 1.9051(8) -0.1699(5) 0.3025(4) 0.0353(14) Uani 1 1 d . U . . .
H6A H 1.985229 -0.110799 0.297008 0.042 Uiso 1 1 calc R U . . .
H6B H 1.816326 -0.173943 0.255336 0.042 Uiso 1 1 calc R U . . .
C7 C 1.6912(7) 0.1384(5) 0.4636(4) 0.0292(12) Uani 1 1 d . U . . .
H7A H 1.703724 0.164134 0.411138 0.035 Uiso 1 1 calc R U . . .
C8 C 1.6310(7) 0.2069(4) 0.5352(4) 0.0240(11) Uani 1 1 d . U . . .
C9 C 1.6112(7) 0.1689(4) 0.6143(4) 0.0259(11) Uani 1 1 d . U . . .
H9 H 1.569678 0.214053 0.662521 0.031 Uiso 1 1 calc R U . . .
C10 C 1.5873(6) 0.3210(4) 0.5257(3) 0.0210(11) Uani 1 1 d . U . . .
C11 C 1.3088(7) 0.3574(5) 0.3370(4) 0.0294(12) Uani 1 1 d . U . . .
H11A H 1.406320 0.366439 0.314087 0.035 Uiso 1 1 calc R U . . .
C12 C 1.1538(8) 0.3977(5) 0.4532(4) 0.0362(14) Uani 1 1 d . U . . .
H12 H 1.143408 0.434572 0.512489 0.043 Uiso 1 1 calc R U . . .
C13 C 1.0203(8) 0.3333(5) 0.4010(4) 0.0354(14) Uani 1 1 d . U . . .
H13 H 0.922702 0.328059 0.424576 0.042 Uiso 1 1 calc R U . . .
C14 C 1.0351(7) 0.2765(4) 0.3123(4) 0.0251(11) Uani 1 1 d . U . . .
C15 C 1.1811(7) 0.2901(5) 0.2810(4) 0.0296(12) Uani 1 1 d . U . . .
H15 H 1.194578 0.254143 0.222003 0.036 Uiso 1 1 calc R U . . .
C16 C 0.9014(7) 0.2023(5) 0.2523(4) 0.0256(11) Uani 1 1 d . U . . .
C17 C 0.9276(8) 0.1005(5) 0.1963(4) 0.0304(12) Uani 1 1 d . U . . .
H17 H 1.027928 0.073316 0.200998 0.036 Uiso 1 1 calc R U . . .
C18 C 0.8043(7) 0.0398(4) 0.1335(4) 0.0287(12) Uani 1 1 d . U . . .
H18 H 0.824444 -0.028531 0.097316 0.034 Uiso 1 1 calc R U . . .
C19 C 0.7458(7) 0.2347(5) 0.2447(4) 0.0295(12) Uani 1 1 d . U . . .
H19 H 0.719922 0.299589 0.283326 0.035 Uiso 1 1 calc R U . . .
C20 C 0.6297(7) 0.1687(5) 0.1784(4) 0.0279(12) Uani 1 1 d . U . . .
H20 H 0.527112 0.192391 0.173555 0.034 Uiso 1 1 calc R U . . .
C21 C 0.3308(7) 0.2109(4) 0.0189(3) 0.0205(11) Uani 1 1 d . U . . .
C22 C 0.3776(7) 0.3414(4) -0.0850(3) 0.0225(11) Uani 1 1 d . U . . .
H22 H 0.428117 0.285503 -0.120512 0.027 Uiso 1 1 calc R U . . .
C23 C 0.3186(7) 0.3238(4) -0.0066(3) 0.0209(11) Uani 1 1 d . U . . .
C24 C 0.3606(7) 0.4441(5) -0.1100(4) 0.0248(11) Uani 1 1 d . U . . .
C25 C 0.4120(8) 0.4639(5) -0.1962(4) 0.0316(13) Uani 1 1 d . U . . .
C26 C 0.2900(7) 0.5275(4) -0.0545(4) 0.0270(12) Uani 1 1 d . U . . .
H26 H 0.280649 0.596296 -0.070656 0.032 Uiso 1 1 calc R U . . .
C27 C 0.2438(7) 0.4073(4) 0.0478(4) 0.0244(11) Uani 1 1 d . U . . .
H27 H 0.201552 0.393876 0.099262 0.029 Uiso 1 1 calc R U . . .
C28 C 0.2331(7) 0.5109(4) 0.0242(4) 0.0256(11) Uani 1 1 d . U . . .
C29 C 0.1138(8) 0.5924(5) 0.1590(4) 0.0317(13) Uani 1 1 d . U . . .
H29A H 0.203360 0.581589 0.200866 0.038 Uiso 1 1 calc R U . . .
H29B H 0.030916 0.530005 0.151584 0.038 Uiso 1 1 calc R U . . .
C30 C 0.0485(8) 0.7035(5) 0.1937(4) 0.0347(14) Uani 1 1 d . U . . .
H30A H -0.035155 0.713815 0.148044 0.042 Uiso 1 1 calc R U . . .
H30B H 0.134313 0.763611 0.199698 0.042 Uiso 1 1 calc R U . . .
C31 C -0.0206(8) 0.7177(5) 0.2841(4) 0.0334(14) Uani 1 1 d . U . . .
H31A H 0.063907 0.717352 0.332547 0.040 Uiso 1 1 calc R U . . .
H31B H -0.102014 0.655739 0.281357 0.040 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 N1 2.058(4) 2_866 ?
Ni1 N1 2.058(4) . ?
Ni1 O5 2.090(4) 2_866 ?
Ni1 O5 2.090(4) . ?
Ni1 O4 2.136(3) 2_866 ?
Ni1 O4 2.136(3) . ?
Ni1 C10 2.449(5) 2_866 ?
Ni2 O8 2.031(3) . ?
Ni2 O8 2.031(3) 2_655 ?
Ni2 O7 2.084(4) 2_655 ?
Ni2 O7 2.084(4) . ?
Ni2 N2 2.133(4) 2_655 ?
Ni2 N2 2.133(4) . ?
N1 C12 1.336(8) . ?
N1 C11 1.341(7) . ?
N2 C20 1.329(7) . ?
N2 C18 1.348(7) . ?
O1 C1 1.317(8) . ?
O1 H1 0.8200 . ?
O2 C1 1.194(8) . ?
O3 C4 1.353(7) . ?
O3 C5 1.428(7) . ?
O4 C10 1.283(6) . ?
O5 C10 1.260(6) . ?
O7 H7B 0.8500 . ?
O7 H7D 0.8500 . ?
O8 C21 1.254(6) . ?
O9 C21 1.255(6) . ?
O10 C28 1.370(6) . ?
O10 C29 1.428(7) . ?
O11 C25 1.310(7) . ?
O11 H11 0.8200 . ?
O12 C25 1.191(7) . ?
O13 H13C 0.8500 . ?
O13 H13D 0.8499 . ?
C1 C2 1.493(8) . ?
C2 C3 1.391(8) . ?
C2 C9 1.385(8) . ?
C3 C4 1.398(8) . ?
C3 H3 0.9300 . ?
C4 C7 1.392(8) . ?
C5 C6 1.503(8) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 C31 1.530(8) 1_745 ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.383(8) . ?
C7 H7A 0.9300 . ?
C8 C9 1.398(7) . ?
C8 C10 1.497(7) . ?
C9 H9 0.9300 . ?
C11 C15 1.386(8) . ?
C11 H11A 0.9300 . ?
C12 C13 1.383(8) . ?
C12 H12 0.9300 . ?
C13 C14 1.397(8) . ?
C13 H13 0.9300 . ?
C14 C15 1.370(8) . ?
C14 C16 1.478(8) . ?
C15 H15 0.9300 . ?
C16 C17 1.389(8) . ?
C16 C19 1.394(8) . ?
C17 C18 1.379(8) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C19 C20 1.392(8) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
C21 C23 1.516(7) . ?
C22 C23 1.386(7) . ?
C22 C24 1.397(7) . ?
C22 H22 0.9300 . ?
C23 C27 1.396(7) . ?
C24 C26 1.381(8) . ?
C24 C25 1.482(7) . ?
C26 C28 1.380(8) . ?
C26 H26 0.9300 . ?
C27 C28 1.391(7) . ?
C27 H27 0.9300 . ?
C29 C30 1.507(7) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 C31 1.524(8) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C31 H31A 0.9700 . ?
C31 H31B 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
N1 Ni1 N1 180.0 2_866 . ?
N1 Ni1 O5 88.97(16) 2_866 2_866 ?
N1 Ni1 O5 91.03(16) . 2_866 ?
N1 Ni1 O5 91.03(16) 2_866 . ?
N1 Ni1 O5 88.97(16) . . ?
O5 Ni1 O5 180.00(12) 2_866 . ?
N1 Ni1 O4 89.74(16) 2_866 2_866 ?
N1 Ni1 O4 90.26(16) . 2_866 ?
O5 Ni1 O4 62.49(14) 2_866 2_866 ?
O5 Ni1 O4 117.51(14) . 2_866 ?
N1 Ni1 O4 90.26(16) 2_866 . ?
N1 Ni1 O4 89.74(16) . . ?
O5 Ni1 O4 117.51(14) 2_866 . ?
O5 Ni1 O4 62.49(14) . . ?
O4 Ni1 O4 180.0(2) 2_866 . ?
N1 Ni1 C10 88.13(17) 2_866 2_866 ?
N1 Ni1 C10 91.87(17) . 2_866 ?
O5 Ni1 C10 30.97(16) 2_866 2_866 ?
O5 Ni1 C10 149.03(16) . 2_866 ?
O4 Ni1 C10 31.56(15) 2_866 2_866 ?
O4 Ni1 C10 148.44(15) . 2_866 ?
O8 Ni2 O8 180.0 . 2_655 ?
O8 Ni2 O7 86.93(14) . 2_655 ?
O8 Ni2 O7 93.07(14) 2_655 2_655 ?
O8 Ni2 O7 93.07(14) . . ?
O8 Ni2 O7 86.93(14) 2_655 . ?
O7 Ni2 O7 180.0 2_655 . ?
O8 Ni2 N2 89.97(15) . 2_655 ?
O8 Ni2 N2 90.03(15) 2_655 2_655 ?
O7 Ni2 N2 90.64(16) 2_655 2_655 ?
O7 Ni2 N2 89.36(16) . 2_655 ?
O8 Ni2 N2 90.03(15) . . ?
O8 Ni2 N2 89.97(15) 2_655 . ?
O7 Ni2 N2 89.36(16) 2_655 . ?
O7 Ni2 N2 90.64(16) . . ?
N2 Ni2 N2 180.0 2_655 . ?
C12 N1 C11 117.4(5) . . ?
C12 N1 Ni1 124.8(4) . . ?
C11 N1 Ni1 117.8(4) . . ?
C20 N2 C18 116.2(5) . . ?
C20 N2 Ni2 122.8(4) . . ?
C18 N2 Ni2 119.5(4) . . ?
C1 O1 H1 109.5 . . ?
C4 O3 C5 120.0(5) . . ?
C10 O4 Ni1 87.8(3) . . ?
C10 O5 Ni1 90.4(3) . . ?
Ni2 O7 H7B 109.2 . . ?
Ni2 O7 H7D 109.2 . . ?
H7B O7 H7D 109.6 . . ?
C21 O8 Ni2 130.6(3) . . ?
C28 O10 C29 119.8(4) . . ?
C25 O11 H11 109.5 . . ?
H13C O13 H13D 108.6 . . ?
O2 C1 O1 122.9(6) . . ?
O2 C1 C2 123.2(6) . . ?
O1 C1 C2 113.9(5) . . ?
C3 C2 C9 121.9(5) . . ?
C3 C2 C1 116.9(5) . . ?
C9 C2 C1 121.1(5) . . ?
C2 C3 C4 118.9(5) . . ?
C2 C3 H3 120.6 . . ?
C4 C3 H3 120.6 . . ?
O3 C4 C7 115.0(5) . . ?
O3 C4 C3 125.5(5) . . ?
C7 C4 C3 119.4(5) . . ?
O3 C5 C6 104.4(5) . . ?
O3 C5 H5A 110.9 . . ?
C6 C5 H5A 110.9 . . ?
O3 C5 H5B 110.9 . . ?
C6 C5 H5B 110.9 . . ?
H5A C5 H5B 108.9 . . ?
C5 C6 C31 116.2(5) . 1_745 ?
C5 C6 H6A 108.2 . . ?
C31 C6 H6A 108.2 1_745 . ?
C5 C6 H6B 108.2 . . ?
C31 C6 H6B 108.2 1_745 . ?
H6A C6 H6B 107.4 . . ?
C8 C7 C4 121.1(5) . . ?
C8 C7 H7A 119.5 . . ?
C4 C7 H7A 119.5 . . ?
C7 C8 C9 120.0(5) . . ?
C7 C8 C10 118.7(5) . . ?
C9 C8 C10 121.3(5) . . ?
C2 C9 C8 118.7(5) . . ?
C2 C9 H9 120.7 . . ?
C8 C9 H9 120.7 . . ?
O5 C10 O4 119.1(5) . . ?
O5 C10 C8 120.1(5) . . ?
O4 C10 C8 120.7(5) . . ?
N1 C11 C15 122.3(6) . . ?
N1 C11 H11A 118.8 . . ?
C15 C11 H11A 118.8 . . ?
N1 C12 C13 123.6(5) . . ?
N1 C12 H12 118.2 . . ?
C13 C12 H12 118.2 . . ?
C12 C13 C14 118.7(6) . . ?
C12 C13 H13 120.7 . . ?
C14 C13 H13 120.7 . . ?
C15 C14 C13 117.7(5) . . ?
C15 C14 C16 119.5(5) . . ?
C13 C14 C16 122.8(5) . . ?
C14 C15 C11 120.3(5) . . ?
C14 C15 H15 119.8 . . ?
C11 C15 H15 119.8 . . ?
C17 C16 C19 116.9(5) . . ?
C17 C16 C14 121.4(5) . . ?
C19 C16 C14 121.6(5) . . ?
C18 C17 C16 119.8(6) . . ?
C18 C17 H17 120.1 . . ?
C16 C17 H17 120.1 . . ?
N2 C18 C17 123.7(5) . . ?
N2 C18 H18 118.1 . . ?
C17 C18 H18 118.1 . . ?
C20 C19 C16 119.1(5) . . ?
C20 C19 H19 120.5 . . ?
C16 C19 H19 120.5 . . ?
N2 C20 C19 124.2(6) . . ?
N2 C20 H20 117.9 . . ?
C19 C20 H20 117.9 . . ?
O8 C21 O9 125.3(5) . . ?
O8 C21 C23 116.1(5) . . ?
O9 C21 C23 118.5(5) . . ?
C23 C22 C24 119.3(5) . . ?
C23 C22 H22 120.3 . . ?
C24 C22 H22 120.3 . . ?
C22 C23 C27 121.0(5) . . ?
C22 C23 C21 119.6(5) . . ?
C27 C23 C21 119.4(5) . . ?
C26 C24 C22 119.3(5) . . ?
C26 C24 C25 119.4(5) . . ?
C22 C24 C25 121.2(5) . . ?
O12 C25 O11 123.0(5) . . ?
O12 C25 C24 123.8(6) . . ?
O11 C25 C24 113.1(5) . . ?
C28 C26 C24 121.5(5) . . ?
C28 C26 H26 119.2 . . ?
C24 C26 H26 119.2 . . ?
C28 C27 C23 119.2(5) . . ?
C28 C27 H27 120.4 . . ?
C23 C27 H27 120.4 . . ?
O10 C28 C26 116.2(5) . . ?
O10 C28 C27 124.2(5) . . ?
C26 C28 C27 119.6(5) . . ?
O10 C29 C30 105.2(5) . . ?
O10 C29 H29A 110.7 . . ?
C30 C29 H29A 110.7 . . ?
O10 C29 H29B 110.7 . . ?
C30 C29 H29B 110.7 . . ?
H29A C29 H29B 108.8 . . ?
C29 C30 C31 116.4(5) . . ?
C29 C30 H30A 108.2 . . ?
C31 C30 H30A 108.2 . . ?
C29 C30 H30B 108.2 . . ?
C31 C30 H30B 108.2 . . ?
H30A C30 H30B 107.3 . . ?
C30 C31 C6 108.3(5) . 1_365 ?
C30 C31 H31A 110.0 . . ?
C6 C31 H31A 110.0 1_365 . ?
C30 C31 H31B 110.0 . . ?
C6 C31 H31B 110.0 1_365 . ?
H31A C31 H31B 108.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 C1 C2 C3 -1.2(11) . . . . ?
O1 C1 C2 C3 177.5(6) . . . . ?
O2 C1 C2 C9 -179.7(7) . . . . ?
O1 C1 C2 C9 -0.9(10) . . . . ?
C9 C2 C3 C4 -0.3(10) . . . . ?
C1 C2 C3 C4 -178.8(6) . . . . ?
C5 O3 C4 C7 177.6(6) . . . . ?
C5 O3 C4 C3 -1.5(10) . . . . ?
C2 C3 C4 O3 179.9(6) . . . . ?
C2 C3 C4 C7 0.8(10) . . . . ?
C4 O3 C5 C6 -177.8(6) . . . . ?
O3 C5 C6 C31 176.7(5) . . . 1_745 ?
O3 C4 C7 C8 -179.7(6) . . . . ?
C3 C4 C7 C8 -0.6(10) . . . . ?
C4 C7 C8 C9 -0.2(9) . . . . ?
C4 C7 C8 C10 -179.9(5) . . . . ?
C3 C2 C9 C8 -0.5(9) . . . . ?
C1 C2 C9 C8 177.9(6) . . . . ?
C7 C8 C9 C2 0.7(9) . . . . ?
C10 C8 C9 C2 -179.6(5) . . . . ?
Ni1 O5 C10 O4 -3.7(5) . . . . ?
Ni1 O5 C10 C8 174.9(4) . . . . ?
Ni1 O4 C10 O5 3.6(5) . . . . ?
Ni1 O4 C10 C8 -175.0(4) . . . . ?
C7 C8 C10 O5 -10.4(8) . . . . ?
C9 C8 C10 O5 169.9(5) . . . . ?
C7 C8 C10 O4 168.2(5) . . . . ?
C9 C8 C10 O4 -11.5(8) . . . . ?
C12 N1 C11 C15 -1.9(9) . . . . ?
Ni1 N1 C11 C15 176.9(4) . . . . ?
C11 N1 C12 C13 1.0(9) . . . . ?
Ni1 N1 C12 C13 -177.7(5) . . . . ?
N1 C12 C13 C14 0.8(10) . . . . ?
C12 C13 C14 C15 -1.6(9) . . . . ?
C12 C13 C14 C16 177.6(5) . . . . ?
C13 C14 C15 C11 0.8(9) . . . . ?
C16 C14 C15 C11 -178.5(5) . . . . ?
N1 C11 C15 C14 1.1(9) . . . . ?
C15 C14 C16 C17 39.8(8) . . . . ?
C13 C14 C16 C17 -139.4(6) . . . . ?
C15 C14 C16 C19 -135.6(6) . . . . ?
C13 C14 C16 C19 45.2(8) . . . . ?
C19 C16 C17 C18 3.3(9) . . . . ?
C14 C16 C17 C18 -172.3(5) . . . . ?
C20 N2 C18 C17 -3.8(8) . . . . ?
Ni2 N2 C18 C17 162.3(5) . . . . ?
C16 C17 C18 N2 0.8(9) . . . . ?
C17 C16 C19 C20 -4.2(8) . . . . ?
C14 C16 C19 C20 171.4(5) . . . . ?
C18 N2 C20 C19 2.8(8) . . . . ?
Ni2 N2 C20 C19 -162.9(4) . . . . ?
C16 C19 C20 N2 1.2(9) . . . . ?
Ni2 O8 C21 O9 2.6(8) . . . . ?
Ni2 O8 C21 C23 -176.9(3) . . . . ?
C24 C22 C23 C27 -0.5(8) . . . . ?
C24 C22 C23 C21 177.6(5) . . . . ?
O8 C21 C23 C22 25.7(7) . . . . ?
O9 C21 C23 C22 -153.8(5) . . . . ?
O8 C21 C23 C27 -156.2(5) . . . . ?
O9 C21 C23 C27 24.4(7) . . . . ?
C23 C22 C24 C26 2.2(8) . . . . ?
C23 C22 C24 C25 -175.9(5) . . . . ?
C26 C24 C25 O12 9.8(10) . . . . ?
C22 C24 C25 O12 -172.2(7) . . . . ?
C26 C24 C25 O11 -171.5(6) . . . . ?
C22 C24 C25 O11 6.5(9) . . . . ?
C22 C24 C26 C28 -1.3(9) . . . . ?
C25 C24 C26 C28 176.8(6) . . . . ?
C22 C23 C27 C28 -2.0(8) . . . . ?
C21 C23 C27 C28 179.9(5) . . . . ?
C29 O10 C28 C26 -175.6(5) . . . . ?
C29 O10 C28 C27 6.0(9) . . . . ?
C24 C26 C28 O10 -179.8(5) . . . . ?
C24 C26 C28 C27 -1.3(9) . . . . ?
C23 C27 C28 O10 -178.7(5) . . . . ?
C23 C27 C28 C26 2.9(9) . . . . ?
C28 O10 C29 C30 179.3(5) . . . . ?
O10 C29 C30 C31 178.1(5) . . . . ?
C29 C30 C31 C6 -174.5(6) . . . 1_365 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O13 H13D O10 0.85 2.13 2.977(6) 173.3 1_556 yes
O13 H13C O9 0.85 2.03 2.873(6) 173.1 2_566 yes
O11 H11 O4 0.82 1.87 2.659(5) 161.8 1_454 yes
O7 H7D O9 0.85 2.02 2.657(5) 130.7 . yes
O7 H7B O13 0.85 1.98 2.697(6) 141.3 1_544 yes
O1 H1 O7 0.82 1.98 2.727(5) 150.5 2_756 yes

_refine_diff_density_max         0.751
_refine_diff_density_min         -0.593
_refine_diff_density_rms         0.100

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

data_exp_10853
_database_code_depnum_ccdc_archive 'CCDC 2021788'
loop_
_audit_author_name
_audit_author_address
'Houting Liu'
;Liaocheng University
China
;
_audit_update_record             
;
2020-08-06 deposited with the CCDC.	2020-09-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C15.50 H15 Cd0 Co0.50 N O6'
_chemical_formula_weight         340.75

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd 0.1185 4.6533 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co -2.3653 3.6143 '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                   14.8925(19)
_cell_length_b                   11.1228(13)
_cell_length_c                   18.0572(18)
_cell_angle_alpha                90
_cell_angle_beta                 91.812(10)
_cell_angle_gamma                90
_cell_volume                     2989.6(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1423
_cell_measurement_theta_min      4.8900
_cell_measurement_theta_max      70.5620

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_F_000             1412
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    5.111
_shelx_estimated_absorpt_T_min   0.579
_shelx_estimated_absorpt_T_max   0.603
_exptl_absorpt_correction_T_min  0.27488
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            4923
_diffrn_reflns_av_unetI/netI     0.0581
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         4.901
_diffrn_reflns_theta_max         67.249
_diffrn_reflns_theta_full        67.249
_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             2680
_reflns_number_gt                2146
_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       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXL-2018/3 '
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0530P)²+1.2484P] 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     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.00053(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2680
_refine_ls_number_parameters     212
_refine_ls_number_restraints     546
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0464
_refine_ls_wR_factor_ref         0.1188
_refine_ls_wR_factor_gt          0.1090
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      0.946
_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 0.750000 0.250000 0.500000 0.0240(2) Uani 1 2 d S U P . .
N1 N 0.85712(17) 0.2441(2) 0.58780(14) 0.0294(6) Uani 1 1 d . U . . .
O1 O 0.66017(14) 0.1929(2) 0.58359(11) 0.0348(5) Uani 1 1 d . U . . .
H1C H 0.677826 0.125616 0.600918 0.052 Uiso 1 1 d R U . . .
H1D H 0.660366 0.244787 0.618188 0.052 Uiso 1 1 d R U . . .
O2 O 0.71808(15) 0.42619(19) 0.52103(11) 0.0322(5) Uani 1 1 d . U . . .
O3 O 0.67607(17) 0.4220(2) 0.63892(11) 0.0427(6) Uani 1 1 d . U . . .
O4 O 0.75289(19) 0.8350(2) 0.74236(12) 0.0485(7) Uani 1 1 d . U . . .
H4 H 0.772339 0.884527 0.772436 0.073 Uiso 1 1 calc R U . . .
O5 O 0.69140(18) 0.9970(2) 0.68868(11) 0.0446(6) Uani 1 1 d . U . . .
O6 O 0.58813(15) 0.83296(19) 0.43983(11) 0.0360(6) Uani 1 1 d . U . . .
C1 C 0.8690(2) 0.1443(3) 0.62819(17) 0.0348(8) Uani 1 1 d . U . . .
H1A H 0.838039 0.075570 0.613036 0.042 Uiso 1 1 calc R U . . .
C2 C 0.9241(2) 0.1364(3) 0.69074(17) 0.0342(8) Uani 1 1 d . U . . .
H2 H 0.929984 0.063958 0.716103 0.041 Uiso 1 1 calc R U . . .
C3 C 0.9709(2) 0.2378(3) 0.71576(16) 0.0287(7) Uani 1 1 d . U . . .
C4 C 0.9602(2) 0.3416(3) 0.67295(18) 0.0354(8) Uani 1 1 d . U . . .
H4A H 0.991172 0.411418 0.686195 0.043 Uiso 1 1 calc R U . . .
C5 C 0.9033(2) 0.3405(3) 0.61055(18) 0.0348(8) Uani 1 1 d . U . . .
H5 H 0.897099 0.410915 0.583122 0.042 Uiso 1 1 calc R U . . .
C6 C 0.6911(2) 0.4756(3) 0.57923(15) 0.0278(7) Uani 1 1 d . U . . .
C7 C 0.67394(19) 0.6087(3) 0.57501(15) 0.0253(6) Uani 1 1 d . U . . .
C8 C 0.6956(2) 0.6832(3) 0.63414(15) 0.0269(7) Uani 1 1 d . U . . .
H8 H 0.718402 0.651229 0.678468 0.032 Uiso 1 1 calc R U . . .
C9 C 0.68290(19) 0.8067(3) 0.62654(15) 0.0257(7) Uani 1 1 d . U . . .
C10 C 0.7083(2) 0.8909(3) 0.68817(16) 0.0301(7) Uani 1 1 d . U . . .
C11 C 0.6459(2) 0.8545(3) 0.56121(15) 0.0271(7) Uani 1 1 d . U . . .
H11 H 0.636382 0.936881 0.557000 0.033 Uiso 1 1 calc R U . . .
C12 C 0.6233(2) 0.7790(3) 0.50239(16) 0.0276(7) Uani 1 1 d . U . . .
C13 C 0.6380(2) 0.6562(3) 0.50911(15) 0.0289(7) Uani 1 1 d . U . . .
H13 H 0.623792 0.605426 0.469509 0.035 Uiso 1 1 calc R U . . .
C14 C 0.5632(2) 0.7548(3) 0.37989(16) 0.0307(7) Uani 1 1 d . U . . .
H14A H 0.515177 0.701685 0.394317 0.037 Uiso 1 1 calc R U . . .
H14B H 0.614177 0.706052 0.366442 0.037 Uiso 1 1 calc R U . . .
C15 C 0.5324(2) 0.8312(3) 0.31523(15) 0.0299(7) Uani 1 1 d . U . . .
H15A H 0.581654 0.881659 0.300006 0.036 Uiso 1 1 calc R U . . .
H15B H 0.483964 0.883219 0.330176 0.036 Uiso 1 1 calc R U . . .
C16 C 0.500000 0.7535(4) 0.250000 0.0329(10) Uani 1 2 d S TU P . .
H16A H 0.451301 0.702288 0.265396 0.039 Uiso 0.5 1 calc R U P . .
H16B H 0.548699 0.702287 0.234605 0.039 Uiso 0.5 1 calc R U 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
Co1 O2 2.055(2) 7_656 ?
Co1 O2 2.055(2) . ?
Co1 O1 2.144(2) . ?
Co1 O1 2.144(2) 7_656 ?
Co1 N1 2.214(2) 7_656 ?
Co1 N1 2.214(2) . ?
N1 C5 1.332(4) . ?
N1 C1 1.336(4) . ?
O2 C6 1.262(3) . ?
O3 C6 1.258(3) . ?
O4 C10 1.321(4) . ?
O5 C10 1.207(4) . ?
O6 C12 1.369(3) . ?
O6 C14 1.428(3) . ?
C1 C2 1.377(4) . ?
C2 C3 1.393(4) . ?
C3 C4 1.396(4) . ?
C3 C3 1.487(5) 2_756 ?
C4 C5 1.389(4) . ?
C6 C7 1.504(4) . ?
C7 C8 1.382(4) . ?
C7 C13 1.393(4) . ?
C8 C9 1.393(4) . ?
C9 C11 1.392(4) . ?
C9 C10 1.494(4) . ?
C11 C12 1.387(4) . ?
C12 C13 1.389(4) . ?
C14 C15 1.504(4) . ?
C15 C16 1.527(4) . ?

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
O2 Co1 O2 180.00(11) 7_656 . ?
O2 Co1 O1 90.06(9) 7_656 . ?
O2 Co1 O1 89.94(9) . . ?
O2 Co1 O1 89.94(9) 7_656 7_656 ?
O2 Co1 O1 90.06(9) . 7_656 ?
O1 Co1 O1 180.0 . 7_656 ?
O2 Co1 N1 93.54(9) 7_656 7_656 ?
O2 Co1 N1 86.46(9) . 7_656 ?
O1 Co1 N1 93.52(9) . 7_656 ?
O1 Co1 N1 86.48(9) 7_656 7_656 ?
O2 Co1 N1 86.46(9) 7_656 . ?
O2 Co1 N1 93.54(9) . . ?
O1 Co1 N1 86.48(9) . . ?
O1 Co1 N1 93.52(9) 7_656 . ?
N1 Co1 N1 180.0 7_656 . ?
C5 N1 C1 116.2(3) . . ?
C5 N1 Co1 123.4(2) . . ?
C1 N1 Co1 119.7(2) . . ?
C6 O2 Co1 130.6(2) . . ?
C12 O6 C14 116.3(2) . . ?
N1 C1 C2 124.5(3) . . ?
C1 C2 C3 119.6(3) . . ?
C2 C3 C4 116.3(3) . . ?
C2 C3 C3 122.8(2) . 2_756 ?
C4 C3 C3 120.91(19) . 2_756 ?
C5 C4 C3 119.8(3) . . ?
N1 C5 C4 123.6(3) . . ?
O3 C6 O2 125.3(3) . . ?
O3 C6 C7 118.3(3) . . ?
O2 C6 C7 116.4(3) . . ?
C8 C7 C13 120.5(3) . . ?
C8 C7 C6 121.0(3) . . ?
C13 C7 C6 118.5(3) . . ?
C7 C8 C9 119.2(3) . . ?
C11 C9 C8 120.6(3) . . ?
C11 C9 C10 118.4(3) . . ?
C8 C9 C10 121.0(3) . . ?
O5 C10 O4 123.7(3) . . ?
O5 C10 C9 124.8(3) . . ?
O4 C10 C9 111.5(3) . . ?
C12 C11 C9 119.9(3) . . ?
O6 C12 C11 116.4(3) . . ?
O6 C12 C13 123.9(3) . . ?
C11 C12 C13 119.7(3) . . ?
C12 C13 C7 120.2(3) . . ?
O6 C14 C15 108.1(2) . . ?
C14 C15 C16 111.1(3) . . ?
C15 C16 C15 111.1(4) . 2_655 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C1 H1A O2 0.93 2.54 3.056(4) 115.6 7_656 yes
O4 H4 O3 0.82 1.80 2.551(3) 151.1 4_656 yes
O1 H1D O3 0.85 2.02 2.745(3) 142.8 . yes
O1 H1C O5 0.85 2.14 2.917(3) 151.9 1_545 yes
C1 H1A O2 0.93 2.54 3.056(4) 115.6 7_656 yes
O4 H4 O3 0.82 1.80 2.551(3) 151.1 4_656 yes
O1 H1D O3 0.85 2.02 2.745(3) 142.8 . yes
O1 H1C O5 0.85 2.14 2.917(3) 151.9 1_545 yes
O1 H1C O5 0.85 2.14 2.917(3) 151.9 1_545 yes
O1 H1D O3 0.85 2.02 2.745(3) 142.8 . yes
O4 H4 O3 0.82 1.80 2.551(3) 151.1 4_656 yes
C1 H1A O2 0.93 2.54 3.056(4) 115.6 7_656 yes
O1 H1C O5 0.85 2.14 2.917(3) 151.9 1_545 yes
O1 H1D O3 0.85 2.02 2.745(3) 142.8 . yes
O4 H4 O3 0.82 1.80 2.551(3) 151.1 4_656 yes
C1 H1A O2 0.93 2.54 3.056(4) 115.6 7_656 yes
O1 H1C O5 0.85 2.14 2.917(3) 151.9 1_545 yes
O1 H1D O3 0.85 2.02 2.745(3) 142.8 . yes
O4 H4 O3 0.82 1.80 2.551(3) 151.1 4_656 yes
C1 H1A O2 0.93 2.54 3.056(4) 115.6 7_656 yes
O1 H1C O5 0.85 2.14 2.917(3) 151.9 1_545 yes
O1 H1D O3 0.85 2.02 2.745(3) 142.8 . yes
O4 H4 O3 0.82 1.80 2.551(3) 151.1 4_656 yes
C1 H1A O2 0.93 2.54 3.056(4) 115.6 7_656 yes

_refine_diff_density_max         0.465
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.060

