# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1954590'
loop_
_audit_author_name
_audit_author_address
'Jing zhao'
;The Cambridge Crystallographic Data Centre
China
;
_audit_update_record             
;
2019-12-17 deposited with the CCDC.	2020-01-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H28 N4 Ni O8'
_chemical_formula_weight         655.29

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.6799(3)
_cell_length_b                   10.5256(5)
_cell_length_c                   10.9153(5)
_cell_angle_alpha                62.4040(10)
_cell_angle_beta                 89.1580(10)
_cell_angle_gamma                74.8170(10)
_cell_volume                     748.78(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4258
_cell_measurement_theta_min      2.12
_cell_measurement_theta_max      28.25

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            Green
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             340
_exptl_absorpt_coefficient_mu    0.707
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9014
_exptl_absorpt_correction_T_max  0.9263
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5484
_diffrn_reflns_av_R_equivalents  0.0089
_diffrn_reflns_av_sigmaI/netI    0.0152
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.12
_diffrn_reflns_theta_max         28.25
_reflns_number_total             3662
_reflns_number_gt                3489
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2001)'
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT+ (Bruker, 1999)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXTL (1998)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0364P)²+0.3371P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3662
_refine_ls_number_parameters     205
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_gt           0.0274
_refine_ls_wR_factor_ref         0.0753
_refine_ls_wR_factor_gt          0.0745
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_restrained_S_all      1.099
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.5000 0.0000 0.5000 0.01690(7) Uani 1 2 d S . .
O1W O 0.66995(13) -0.03165(11) 0.66594(10) 0.0241(2) Uani 1 1 d . . .
H1WA H 0.7175 0.0278 0.6761 0.029 Uiso 1 1 d R . .
H1WB H 0.6646 -0.0999 0.7467 0.029 Uiso 1 1 d R . .
O1 O 0.69999(13) -0.15759(10) 0.47619(11) 0.0241(2) Uani 1 1 d . . .
N1 N 0.61739(15) 0.16747(12) 0.37012(12) 0.0208(2) Uani 1 1 d . . .
C1 C 0.52298(18) 0.31227(14) 0.29572(14) 0.0210(2) Uani 1 1 d . . .
H1A H 0.3969 0.3377 0.2910 0.025 Uiso 1 1 calc R . .
O2 O 0.53833(14) -0.24006(12) 0.37406(12) 0.0290(2) Uani 1 1 d . . .
N2 N 0.57972(17) 0.69337(13) 0.13834(13) 0.0262(2) Uani 1 1 d . . .
H2A H 0.5786 0.7174 0.2038 0.031 Uiso 1 1 calc R . .
C2 C 0.60300(18) 0.42627(15) 0.22534(14) 0.0225(3) Uani 1 1 d . . .
C3 C 0.7911(2) 0.38616(17) 0.23182(17) 0.0311(3) Uani 1 1 d . . .
H3A H 0.8501 0.4591 0.1859 0.037 Uiso 1 1 calc R . .
C4 C 0.8905(2) 0.23709(18) 0.30691(17) 0.0313(3) Uani 1 1 d . . .
H4A H 1.0166 0.2086 0.3118 0.038 Uiso 1 1 calc R . .
O5 O 0.67106(18) 0.72738(13) -0.06958(12) 0.0362(3) Uani 1 1 d . . .
C5 C 0.79909(19) 0.13158(16) 0.37431(15) 0.0256(3) Uani 1 1 d . . .
H5A H 0.8661 0.0315 0.4247 0.031 Uiso 1 1 calc R . .
C6 C 0.4844(2) 0.58719(15) 0.14738(17) 0.0282(3) Uani 1 1 d . . .
H6A H 0.4434 0.6096 0.0540 0.034 Uiso 1 1 calc R . .
H6B H 0.3778 0.5988 0.1943 0.034 Uiso 1 1 calc R . .
C7 C 0.6691(2) 0.75414(15) 0.02968(15) 0.0251(3) Uani 1 1 d . . .
C8 C 0.77189(19) 0.85556(15) 0.03355(14) 0.0239(3) Uani 1 1 d . . .
C9 C 0.9287(2) 0.85838(16) -0.02853(16) 0.0271(3) Uani 1 1 d . . .
H9A H 0.9679 0.7974 -0.0695 0.033 Uiso 1 1 calc R . .
C10 C 1.0314(2) 0.95326(15) -0.03079(15) 0.0245(3) Uani 1 1 d . . .
C11 C 1.1948(2) 0.95743(17) -0.09326(16) 0.0280(3) Uani 1 1 d . . .
H11A H 1.2375 0.8956 -0.1330 0.034 Uiso 1 1 calc R . .
C12 C 1.2898(2) 1.05144(16) -0.09555(15) 0.0268(3) Uani 1 1 d . . .
H12A H 1.3956 1.0543 -0.1381 0.032 Uiso 1 1 calc R . .
C13 C 0.84689(19) -0.37849(15) 0.46724(15) 0.0238(3) Uani 1 1 d . . .
C14 C 1.0197(2) -0.35945(16) 0.46167(18) 0.0300(3) Uani 1 1 d . . .
H14A H 1.0332 -0.2654 0.4359 0.036 Uiso 1 1 calc R . .
C15 C 1.1727(2) -0.48044(16) 0.49448(18) 0.0302(3) Uani 1 1 d . . .
H15A H 1.2881 -0.4671 0.4909 0.036 Uiso 1 1 calc R . .
C16 C 0.68121(18) -0.24824(14) 0.43556(14) 0.0218(3) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1 2.0570(9) . ?
Ni1 O1 2.0570(9) 2_656 ?
Ni1 O1W 2.0923(10) 2_656 ?
Ni1 O1W 2.0923(10) . ?
Ni1 N1 2.0998(11) . ?
Ni1 N1 2.0998(11) 2_656 ?
O1 C16 1.2625(16) . ?
N1 C1 1.3416(17) . ?
N1 C5 1.3424(17) . ?
C1 C2 1.3878(18) . ?
O2 C16 1.2573(17) . ?
N2 C7 1.3381(19) . ?
N2 C6 1.4557(17) . ?
C2 C3 1.388(2) . ?
C2 C6 1.5172(19) . ?
C3 C4 1.384(2) . ?
C4 C5 1.380(2) . ?
O5 C7 1.2384(18) . ?
C7 C8 1.4994(18) . ?
C8 C9 1.373(2) . ?
C8 C12 1.415(2) 2_775 ?
C9 C10 1.4177(19) . ?
C10 C10 1.417(3) 2_775 ?
C10 C11 1.421(2) . ?
C11 C12 1.367(2) . ?
C12 C8 1.415(2) 2_775 ?
C13 C14 1.389(2) . ?
C13 C15 1.394(2) 2_746 ?
C13 C16 1.5094(17) . ?
C14 C15 1.3917(19) . ?
C15 C13 1.394(2) 2_746 ?

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 180.0 . 2_656 ?
O1 Ni1 O1W 90.93(4) . 2_656 ?
O1 Ni1 O1W 89.07(4) 2_656 2_656 ?
O1 Ni1 O1W 89.07(4) . . ?
O1 Ni1 O1W 90.93(4) 2_656 . ?
O1W Ni1 O1W 180.0 2_656 . ?
O1 Ni1 N1 90.15(4) . . ?
O1 Ni1 N1 89.85(4) 2_656 . ?
O1W Ni1 N1 93.13(4) 2_656 . ?
O1W Ni1 N1 86.87(4) . . ?
O1 Ni1 N1 89.85(4) . 2_656 ?
O1 Ni1 N1 90.15(4) 2_656 2_656 ?
O1W Ni1 N1 86.87(4) 2_656 2_656 ?
O1W Ni1 N1 93.13(4) . 2_656 ?
N1 Ni1 N1 180.00(5) . 2_656 ?
C16 O1 Ni1 128.07(9) . . ?
C1 N1 C5 117.75(11) . . ?
C1 N1 Ni1 123.37(9) . . ?
C5 N1 Ni1 118.37(9) . . ?
N1 C1 C2 123.65(12) . . ?
C7 N2 C6 120.94(13) . . ?
C3 C2 C1 117.42(13) . . ?
C3 C2 C6 122.99(12) . . ?
C1 C2 C6 119.58(12) . . ?
C4 C3 C2 119.68(13) . . ?
C5 C4 C3 118.79(13) . . ?
N1 C5 C4 122.70(13) . . ?
N2 C6 C2 112.42(12) . . ?
O5 C7 N2 122.46(13) . . ?
O5 C7 C8 120.51(13) . . ?
N2 C7 C8 117.02(13) . . ?
C9 C8 C12 120.17(12) . 2_775 ?
C9 C8 C7 117.61(13) . . ?
C12 C8 C7 122.20(13) 2_775 . ?
C8 C9 C10 120.74(13) . . ?
C10 C10 C9 118.90(16) 2_775 . ?
C10 C10 C11 119.22(15) 2_775 . ?
C9 C10 C11 121.88(13) . . ?
C12 C11 C10 120.64(13) . . ?
C11 C12 C8 120.32(13) . 2_775 ?
C14 C13 C15 119.64(12) . 2_746 ?
C14 C13 C16 120.34(12) . . ?
C15 C13 C16 120.00(13) 2_746 . ?
C13 C14 C15 120.33(13) . . ?
C14 C15 C13 120.03(14) . 2_746 ?
O2 C16 O1 125.97(12) . . ?
O2 C16 C13 118.37(12) . . ?
O1 C16 C13 115.65(12) . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        28.25
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         0.565
_refine_diff_density_min         -0.679
_refine_diff_density_rms         0.051
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_4
_database_code_depnum_ccdc_archive 'CCDC 1954593'
loop_
_audit_author_name
_audit_author_address
'Jing zhao'
;The Cambridge Crystallographic Data Centre
China
;
_audit_update_record             
;
2019-12-17 deposited with the CCDC.	2020-01-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H32 N4 Ni O11 S'
_chemical_formula_weight         715.37

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.428(2)
_cell_length_b                   12.410(3)
_cell_length_c                   12.769(3)
_cell_angle_alpha                61.507(2)
_cell_angle_beta                 88.882(4)
_cell_angle_gamma                76.364(4)
_cell_volume                     1537.5(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2414
_cell_measurement_theta_min      1.83
_cell_measurement_theta_max      25.00

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            Green
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             744
_exptl_absorpt_coefficient_mu    0.768
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8935
_exptl_absorpt_correction_T_max  0.9203
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8890
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_sigmaI/netI    0.0584
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.83
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5424
_reflns_number_gt                4189
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2001)'
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT+ (Bruker, 1999)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXTL (1998)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0872P)²+1.4363P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5424
_refine_ls_number_parameters     424
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_gt           0.0519
_refine_ls_wR_factor_ref         0.1574
_refine_ls_wR_factor_gt          0.1491
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_restrained_S_all      1.009
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni -0.05384(4) 0.10103(4) 0.27304(4) 0.02347(17) Uani 1 1 d . . .
S1 S 0.35778(12) 0.04131(13) 0.06694(12) 0.0516(4) Uani 1 1 d . . .
O1 O -0.0384(2) -0.0075(3) 0.1926(2) 0.0306(6) Uani 1 1 d . . .
O1W O -0.0701(3) 0.1910(3) 0.3764(2) 0.0345(7) Uani 1 1 d . . .
H1WA H -0.0819 0.1471 0.4490 0.041 Uiso 1 1 d R . .
H1WB H -0.0899 0.2685 0.3592 0.041 Uiso 1 1 d R . .
N1 N 0.0398(3) 0.2317(3) 0.1577(3) 0.0282(8) Uani 1 1 d . . .
C1 C 0.0536(4) -0.0654(4) 0.1654(3) 0.0274(9) Uani 1 1 d . . .
O2 O 0.0507(3) -0.1489(3) 0.1384(3) 0.0397(8) Uani 1 1 d . . .
O2W O -0.1448(3) -0.0241(3) 0.4050(2) 0.0351(7) Uani 1 1 d . . .
H2WA H -0.1841 -0.0454 0.4659 0.042 Uiso 1 1 d R . .
H2WB H -0.1289 -0.0851 0.3894 0.042 Uiso 1 1 d R . .
N2 N -0.2228(3) 0.2103(3) 0.1682(3) 0.0285(8) Uani 1 1 d . . .
C2 C 0.2078(4) -0.0512(4) 0.3730(4) 0.0301(9) Uani 1 1 d . . .
O3W O 0.2445(3) 0.1197(3) -0.2252(3) 0.0544(9) Uani 1 1 d . . .
H3WA H 0.3049 0.0591 -0.2148 0.065 Uiso 1 1 d R . .
H3WB H 0.1837 0.0890 -0.2026 0.065 Uiso 1 1 d R . .
O3 O 0.0978(3) -0.0222(3) 0.3897(2) 0.0346(7) Uani 1 1 d . . .
C3 C 0.2389(4) -0.0225(4) 0.2491(3) 0.0290(9) Uani 1 1 d . . .
N3 N -0.2694(3) 0.3575(3) -0.2147(3) 0.0380(9) Uani 1 1 d . . .
H3A H -0.2055 0.2991 -0.2045 0.046 Uiso 1 1 calc R . .
O4W O 0.4791(3) 0.1773(3) 0.4334(3) 0.0487(9) Uani 1 1 d . . .
H4WA H 0.5528 0.1699 0.4514 0.058 Uiso 1 1 d R . .
H4WB H 0.4444 0.2560 0.3930 0.058 Uiso 1 1 d R . .
N4 N 0.1961(3) 0.3653(3) -0.2229(3) 0.0322(8) Uani 1 1 d . . .
H4B H 0.2350 0.2936 -0.2162 0.039 Uiso 1 1 calc R . .
O4 O 0.2903(3) -0.1031(4) 0.4560(3) 0.0541(10) Uani 1 1 d . . .
C4 C 0.3427(4) 0.0123(4) 0.2107(4) 0.0416(11) Uani 1 1 d . . .
H4A H 0.3988 0.0196 0.2572 0.050 Uiso 1 1 calc R . .
O5 O -0.3574(3) 0.5671(3) -0.3035(3) 0.0460(8) Uani 1 1 d . . .
C5 C 0.2276(4) 0.0002(4) 0.0587(4) 0.0409(11) Uani 1 1 d . . .
H5A H 0.1982 -0.0014 -0.0079 0.049 Uiso 1 1 calc R . .
O5W O 0.3885(3) 0.0141(3) 0.6316(3) 0.0556(9) Uani 1 1 d . . .
H5WA H 0.4193 0.0553 0.5680 0.067 Uiso 1 1 d R . .
H5WB H 0.4129 -0.0642 0.6520 0.067 Uiso 1 1 d R . .
O6 O 0.1949(3) 0.5668(3) -0.2824(3) 0.0488(9) Uani 1 1 d . . .
C6 C 0.1713(4) -0.0304(4) 0.1608(4) 0.0291(9) Uani 1 1 d . . .
C7 C -0.3151(4) 0.2575(4) 0.2127(4) 0.0377(11) Uani 1 1 d . . .
H7A H -0.3026 0.2451 0.2898 0.045 Uiso 1 1 calc R . .
C8 C -0.4270(5) 0.3233(5) 0.1500(4) 0.0559(15) Uani 1 1 d . . .
H8A H -0.4899 0.3524 0.1849 0.067 Uiso 1 1 calc R . .
C9 C -0.4452(4) 0.3458(5) 0.0334(4) 0.0491(13) Uani 1 1 d . . .
H9A H -0.5208 0.3904 -0.0107 0.059 Uiso 1 1 calc R . .
C10 C -0.3510(4) 0.3019(4) -0.0165(4) 0.0311(9) Uani 1 1 d . . .
C11 C -0.2425(4) 0.2326(4) 0.0550(4) 0.0316(9) Uani 1 1 d . . .
H11A H -0.1793 0.1993 0.0233 0.038 Uiso 1 1 calc R . .
C12 C -0.3683(4) 0.3227(4) -0.1438(4) 0.0361(10) Uani 1 1 d . . .
H12A H -0.3792 0.2454 -0.1390 0.043 Uiso 1 1 calc R . .
H12B H -0.4421 0.3889 -0.1850 0.043 Uiso 1 1 calc R . .
C13 C -0.2745(4) 0.4785(4) -0.2960(4) 0.0342(10) Uani 1 1 d . . .
C14 C -0.1759(4) 0.5034(4) -0.3771(4) 0.0359(10) Uani 1 1 d . . .
C15 C -0.1048(4) 0.4131(4) -0.3992(4) 0.0381(11) Uani 1 1 d . . .
H15A H -0.1190 0.3329 -0.3647 0.046 Uiso 1 1 calc R . .
C16 C -0.0093(4) 0.4385(4) -0.4739(4) 0.0350(10) Uani 1 1 d . . .
C17 C 0.0656(5) 0.3450(4) -0.4953(4) 0.0430(12) Uani 1 1 d . . .
H17A H 0.0533 0.2641 -0.4607 0.052 Uiso 1 1 calc R . .
C18 C 0.1566(4) 0.3731(4) -0.5670(4) 0.0400(11) Uani 1 1 d . . .
H18A H 0.2066 0.3102 -0.5794 0.048 Uiso 1 1 calc R . .
C19 C 0.1017(4) 0.2883(4) 0.1951(4) 0.0378(11) Uani 1 1 d . . .
H19A H 0.1021 0.2697 0.2748 0.045 Uiso 1 1 calc R . .
C20 C 0.1651(5) 0.3732(5) 0.1208(4) 0.0471(12) Uani 1 1 d . . .
H20A H 0.2091 0.4086 0.1507 0.057 Uiso 1 1 calc R . .
C21 C 0.1618(4) 0.4044(4) 0.0011(4) 0.0409(11) Uani 1 1 d . . .
H21A H 0.2010 0.4636 -0.0515 0.049 Uiso 1 1 calc R . .
C22 C 0.0995(4) 0.3460(4) -0.0387(3) 0.0287(9) Uani 1 1 d . . .
C23 C 0.0418(4) 0.2615(4) 0.0425(3) 0.0270(9) Uani 1 1 d . . .
H23A H 0.0007 0.2216 0.0154 0.032 Uiso 1 1 calc R . .
C24 C 0.0849(4) 0.3739(4) -0.1677(4) 0.0353(10) Uani 1 1 d . . .
H24A H 0.0439 0.3151 -0.1709 0.042 Uiso 1 1 calc R . .
H24B H 0.0327 0.4587 -0.2151 0.042 Uiso 1 1 calc R . .
C25 C 0.2391(4) 0.4669(4) -0.2840(4) 0.0317(10) Uani 1 1 d . . .
C26 C 0.3437(4) 0.4547(4) -0.3535(4) 0.0307(9) Uani 1 1 d . . .
C27 C 0.4149(4) 0.3345(4) -0.3349(4) 0.0345(10) Uani 1 1 d . . .
H27A H 0.3978 0.2602 -0.2769 0.041 Uiso 1 1 calc R . .
C28 C 0.5081(4) 0.3287(4) -0.4024(4) 0.0365(10) Uani 1 1 d . . .
H28A H 0.5543 0.2502 -0.3901 0.044 Uiso 1 1 calc R . .
C29 C 0.5345(4) 0.4401(4) -0.4901(4) 0.0306(9) Uani 1 1 d . . .
C30 C 0.6298(4) 0.4373(4) -0.5629(4) 0.0336(10) Uani 1 1 d . . .
H30A H 0.6749 0.3595 -0.5530 0.040 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1 2.026(3) . ?
Ni1 O3 2.058(3) . ?
Ni1 O1W 2.079(3) . ?
Ni1 N1 2.104(3) . ?
Ni1 N2 2.120(3) . ?
Ni1 O2W 2.128(3) . ?
S1 C5 1.703(5) . ?
S1 C4 1.707(5) . ?
O1 C1 1.269(5) . ?
N1 C23 1.335(5) . ?
N1 C19 1.336(6) . ?
C1 O2 1.247(5) . ?
C1 C6 1.499(6) . ?
N2 C7 1.335(5) . ?
N2 C11 1.347(5) . ?
C2 O4 1.236(5) . ?
C2 O3 1.267(5) . ?
C2 C3 1.502(5) . ?
C3 C4 1.360(6) . ?
C3 C6 1.433(6) . ?
N3 C13 1.344(6) . ?
N3 C12 1.450(5) . ?
N4 C25 1.333(5) . ?
N4 C24 1.448(5) . ?
O5 C13 1.236(5) . ?
C5 C6 1.368(6) . ?
O6 C25 1.234(5) . ?
C7 C8 1.366(7) . ?
C8 C9 1.388(7) . ?
C9 C10 1.375(6) . ?
C10 C11 1.379(6) . ?
C10 C12 1.528(6) . ?
C13 C14 1.501(6) . ?
C14 C15 1.364(6) . ?
C14 C18 1.420(6) 2_564 ?
C15 C16 1.427(6) . ?
C16 C17 1.407(6) . ?
C16 C16 1.413(9) 2_564 ?
C17 C18 1.367(7) . ?
C18 C14 1.420(6) 2_564 ?
C19 C20 1.384(6) . ?
C20 C21 1.384(6) . ?
C21 C22 1.378(6) . ?
C22 C23 1.369(6) . ?
C22 C24 1.517(5) . ?
C25 C26 1.496(6) . ?
C26 C30 1.357(6) 2_664 ?
C26 C27 1.429(6) . ?
C27 C28 1.368(6) . ?
C28 C29 1.401(6) . ?
C29 C29 1.411(8) 2_664 ?
C29 C30 1.423(6) . ?
C30 C26 1.357(6) 2_664 ?

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 O3 90.19(12) . . ?
O1 Ni1 O1W 172.49(11) . . ?
O3 Ni1 O1W 85.62(12) . . ?
O1 Ni1 N1 98.50(12) . . ?
O3 Ni1 N1 94.44(12) . . ?
O1W Ni1 N1 88.05(12) . . ?
O1 Ni1 N2 88.55(12) . . ?
O3 Ni1 N2 172.30(12) . . ?
O1W Ni1 N2 94.77(12) . . ?
N1 Ni1 N2 93.26(13) . . ?
O1 Ni1 O2W 88.05(11) . . ?
O3 Ni1 O2W 83.20(11) . . ?
O1W Ni1 O2W 85.28(11) . . ?
N1 Ni1 O2W 173.07(12) . . ?
N2 Ni1 O2W 89.16(12) . . ?
C5 S1 C4 91.8(2) . . ?
C1 O1 Ni1 131.4(3) . . ?
C23 N1 C19 116.3(4) . . ?
C23 N1 Ni1 121.4(3) . . ?
C19 N1 Ni1 122.3(3) . . ?
O2 C1 O1 123.0(4) . . ?
O2 C1 C6 117.4(4) . . ?
O1 C1 C6 119.6(3) . . ?
C7 N2 C11 117.2(4) . . ?
C7 N2 Ni1 121.2(3) . . ?
C11 N2 Ni1 121.6(3) . . ?
O4 C2 O3 121.8(4) . . ?
O4 C2 C3 119.0(4) . . ?
O3 C2 C3 119.1(4) . . ?
C2 O3 Ni1 131.9(3) . . ?
C4 C3 C6 112.3(4) . . ?
C4 C3 C2 120.6(4) . . ?
C6 C3 C2 127.1(4) . . ?
C13 N3 C12 122.0(4) . . ?
C25 N4 C24 121.1(4) . . ?
C3 C4 S1 112.1(4) . . ?
C6 C5 S1 112.4(4) . . ?
C5 C6 C3 111.4(4) . . ?
C5 C6 C1 118.4(4) . . ?
C3 C6 C1 130.2(3) . . ?
N2 C7 C8 123.0(4) . . ?
C7 C8 C9 118.9(4) . . ?
C10 C9 C8 119.6(4) . . ?
C9 C10 C11 117.4(4) . . ?
C9 C10 C12 121.1(4) . . ?
C11 C10 C12 121.5(4) . . ?
N2 C11 C10 123.9(4) . . ?
N3 C12 C10 114.8(4) . . ?
O5 C13 N3 121.2(4) . . ?
O5 C13 C14 120.6(4) . . ?
N3 C13 C14 118.1(4) . . ?
C15 C14 C18 119.0(4) . 2_564 ?
C15 C14 C13 122.9(4) . . ?
C18 C14 C13 118.1(4) 2_564 . ?
C14 C15 C16 121.6(4) . . ?
C17 C16 C16 120.2(5) . 2_564 ?
C17 C16 C15 121.9(4) . . ?
C16 C16 C15 117.9(5) 2_564 . ?
C18 C17 C16 120.0(4) . . ?
C17 C18 C14 121.1(4) . 2_564 ?
N1 C19 C20 123.1(4) . . ?
C19 C20 C21 118.8(4) . . ?
C22 C21 C20 118.8(4) . . ?
C23 C22 C21 117.8(4) . . ?
C23 C22 C24 117.6(4) . . ?
C21 C22 C24 124.6(4) . . ?
N1 C23 C22 125.2(4) . . ?
N4 C24 C22 115.6(4) . . ?
O6 C25 N4 121.1(4) . . ?
O6 C25 C26 121.3(4) . . ?
N4 C25 C26 117.6(4) . . ?
C30 C26 C27 119.7(4) 2_664 . ?
C30 C26 C25 118.0(4) 2_664 . ?
C27 C26 C25 122.3(4) . . ?
C28 C27 C26 120.0(4) . . ?
C27 C28 C29 120.4(4) . . ?
C28 C29 C29 120.6(5) . 2_664 ?
C28 C29 C30 121.7(4) . . ?
C29 C29 C30 117.7(5) 2_664 . ?
C26 C30 C29 121.6(4) 2_664 . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.663
_refine_diff_density_min         -0.665
_refine_diff_density_rms         0.084
####################################################################### 
# 
# 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_5
_database_code_depnum_ccdc_archive 'CCDC 1954594'
loop_
_audit_author_name
_audit_author_address
'Jing zhao'
;The Cambridge Crystallographic Data Centre
China
;
_audit_update_record             
;
2019-12-17 deposited with the CCDC.	2020-01-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C60 H54 N8 Ni2 O17 S2'
_chemical_formula_weight         1340.65

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'C 2/c'

loop_
_symmetry_equiv_pos_as_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                   34.360(7)
_cell_length_b                   9.0513(16)
_cell_length_c                   19.787(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.545(7)
_cell_angle_gamma                90.00
_cell_volume                     5867.5(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3594
_cell_measurement_theta_min      1.24
_cell_measurement_theta_max      24.99

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            Green
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2776
_exptl_absorpt_coefficient_mu    0.793
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8903
_exptl_absorpt_correction_T_max  0.9178
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16495
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_av_sigmaI/netI    0.0413
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.24
_diffrn_reflns_theta_max         25.15
_reflns_number_total             5214
_reflns_number_gt                4041
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2001)'
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT+ (Bruker, 1999)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXTL (1998)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0429P)²+6.6618P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5214
_refine_ls_number_parameters     402
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0363
_refine_ls_wR_factor_ref         0.0963
_refine_ls_wR_factor_gt          0.0842
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.029
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.126957(11) 0.76937(4) 0.296158(17) 0.02606(12) Uani 1 1 d . . .
S1 S 0.12205(2) 1.10019(8) 0.54407(4) 0.03168(19) Uani 1 1 d . . .
O1 O 0.13347(6) 0.8220(2) 0.39976(9) 0.0318(5) Uani 1 1 d . . .
O1W O 0.07278(6) 0.8919(2) 0.26518(10) 0.0370(5) Uani 1 1 d . . .
H1WA H 0.0449 0.8428 0.2591 0.044 Uiso 1 1 d R . .
H1WB H 0.0701 0.9410 0.2926 0.044 Uiso 1 1 d R . .
N1 N 0.18457(7) 0.6649(3) 0.33083(12) 0.0302(6) Uani 1 1 d . . .
C1 C 0.12063(9) 0.9345(3) 0.42479(15) 0.0297(7) Uani 1 1 d . . .
O2 O 0.10049(8) 1.0382(2) 0.39003(11) 0.0507(6) Uani 1 1 d . . .
N2 N 0.25795(8) 0.4529(3) 0.21053(12) 0.0364(6) Uani 1 1 d . . .
H2A H 0.2833 0.4728 0.2170 0.044 Uiso 1 1 d R . .
C2 C 0.13070(8) 0.9401(3) 0.50408(14) 0.0267(6) Uani 1 1 d . . .
O2W O 0.11057(8) 0.5334(3) 0.08457(12) 0.0523(6) Uani 1 1 d . . .
H2WA H 0.1133 0.6189 0.1132 0.063 Uiso 1 1 d R . .
H2WB H 0.1351 0.4948 0.0946 0.063 Uiso 1 1 d R . .
O3 O 0.15162(6) 1.0426(2) 0.75093(10) 0.0339(5) Uani 1 1 d . . .
N3 N 0.09809(7) 0.5706(3) 0.29878(12) 0.0309(6) Uani 1 1 d . . .
C3 C 0.14497(9) 0.8308(3) 0.55221(15) 0.0324(7) Uani 1 1 d . . .
H3A H 0.1514 0.7365 0.5402 0.039 Uiso 1 1 calc R . .
O3W O 0.0000 0.7321(4) 0.2500 0.0494(8) Uani 1 2 d S . .
H3WA H 0.0016 0.6765 0.2194 0.059 Uiso 1 1 d R . .
O4 O 0.12353(6) 1.2332(2) 0.68568(10) 0.0328(5) Uani 1 1 d . . .
N4 N 0.04355(8) 0.4970(3) 0.45854(13) 0.0348(6) Uani 1 1 d . . .
H4B H 0.0586 0.5079 0.5017 0.042 Uiso 1 1 d R . .
C4 C 0.14905(9) 0.8756(3) 0.62223(14) 0.0329(7) Uani 1 1 d . . .
H4A H 0.1582 0.8135 0.6613 0.039 Uiso 1 1 calc R . .
O5 O -0.00830(7) 0.5802(2) 0.36781(11) 0.0478(6) Uani 1 1 d . . .
C5 C 0.13816(9) 1.0199(3) 0.62672(14) 0.0268(6) Uani 1 1 d . . .
O6 O 0.19388(7) 0.4573(3) 0.13662(11) 0.0485(6) Uani 1 1 d . . .
C6 C 0.13788(8) 1.1037(3) 0.69111(14) 0.0278(6) Uani 1 1 d . . .
C7 C 0.20944(10) 0.6880(4) 0.39606(16) 0.0401(8) Uani 1 1 d . . .
H7A H 0.2018 0.7569 0.4246 0.048 Uiso 1 1 calc R . .
C8 C 0.24573(10) 0.6149(4) 0.42300(17) 0.0497(9) Uani 1 1 d . . .
H8A H 0.2620 0.6340 0.4690 0.060 Uiso 1 1 calc R . .
C9 C 0.25804(10) 0.5131(4) 0.38183(16) 0.0390(8) Uani 1 1 d . . .
H9A H 0.2827 0.4633 0.3995 0.047 Uiso 1 1 calc R . .
C10 C 0.19681(9) 0.5646(3) 0.29115(15) 0.0328(7) Uani 1 1 d . . .
H10A H 0.1798 0.5469 0.2455 0.039 Uiso 1 1 calc R . .
C11 C 0.23314(9) 0.4862(3) 0.31400(15) 0.0293(7) Uani 1 1 d . . .
C12 C 0.24570(10) 0.3783(3) 0.26606(15) 0.0360(7) Uani 1 1 d . . .
H12A H 0.2682 0.3187 0.2942 0.043 Uiso 1 1 calc R . .
H12B H 0.2231 0.3126 0.2445 0.043 Uiso 1 1 calc R . .
C13 C 0.23020(11) 0.4910(3) 0.14947(16) 0.0367(7) Uani 1 1 d . . .
C14 C 0.24582(11) 0.5822(4) 0.09886(16) 0.0417(8) Uani 1 1 d . . .
C15 C 0.28803(11) 0.6151(4) 0.11078(17) 0.0478(9) Uani 1 1 d . . .
H15A H 0.3074 0.5752 0.1500 0.057 Uiso 1 1 calc R . .
C16 C 0.30028(11) 0.7049(4) 0.06516(17) 0.0514(9) Uani 1 1 d . . .
H16A H 0.3278 0.7254 0.0729 0.062 Uiso 1 1 calc R . .
C17 C 0.27094(10) 0.7647(4) 0.00730(17) 0.0424(8) Uani 1 1 d . . .
C18 C 0.21698(12) 0.6385(4) 0.04201(17) 0.0482(9) Uani 1 1 d . . .
H18A H 0.1896 0.6157 0.0344 0.058 Uiso 1 1 calc R . .
C19 C 0.09100(11) 0.4757(4) 0.24485(17) 0.0471(9) Uani 1 1 d . . .
H19A H 0.0995 0.5003 0.2059 0.056 Uiso 1 1 calc R . .
C20 C 0.07160(14) 0.3427(4) 0.24476(19) 0.0611(11) Uani 1 1 d . . .
H20A H 0.0678 0.2779 0.2068 0.073 Uiso 1 1 calc R . .
C21 C 0.05796(11) 0.3062(3) 0.30089(17) 0.0461(9) Uani 1 1 d . . .
H21A H 0.0447 0.2169 0.3013 0.055 Uiso 1 1 calc R . .
C22 C 0.06416(9) 0.4035(3) 0.35688(15) 0.0304(7) Uani 1 1 d . . .
C23 C 0.08487(9) 0.5330(3) 0.35360(15) 0.0324(7) Uani 1 1 d . . .
H23A H 0.0899 0.5978 0.3917 0.039 Uiso 1 1 calc R . .
C24 C 0.04839(11) 0.3675(3) 0.41849(17) 0.0413(8) Uani 1 1 d . . .
H24A H 0.0222 0.3181 0.4007 0.050 Uiso 1 1 calc R . .
H24B H 0.0672 0.2996 0.4500 0.050 Uiso 1 1 calc R . .
C25 C 0.01553(10) 0.5993(3) 0.42815(16) 0.0352(7) Uani 1 1 d . . .
C26 C 0.01473(9) 0.7398(3) 0.46782(15) 0.0311(7) Uani 1 1 d . . .
C27 C 0.03944(9) 0.7639(3) 0.53888(15) 0.0346(7) Uani 1 1 d . . .
H27A H 0.0566 0.6894 0.5633 0.042 Uiso 1 1 calc R . .
C28 C 0.03804(9) 0.8957(3) 0.57108(15) 0.0363(7) Uani 1 1 d . . .
H28A H 0.0542 0.9097 0.6176 0.044 Uiso 1 1 calc R . .
C29 C 0.01248(9) 1.0118(3) 0.53533(14) 0.0301(7) Uani 1 1 d . . .
C30 C -0.01077(9) 0.8500(3) 0.43275(15) 0.0341(7) Uani 1 1 d . . .
H30A H -0.0274 0.8332 0.3867 0.041 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1 2.0502(18) . ?
Ni1 N3 2.062(2) . ?
Ni1 O1W 2.094(2) . ?
Ni1 N1 2.113(2) . ?
Ni1 O4 2.1536(19) 6_575 ?
Ni1 O3 2.208(2) 6_575 ?
Ni1 C6 2.500(3) 6_575 ?
S1 C2 1.719(3) . ?
S1 C5 1.721(3) . ?
O1 C1 1.268(3) . ?
O1W H1WA 1.0307 . ?
O1W H1WB 0.7290 . ?
N1 C7 1.332(4) . ?
N1 C10 1.347(4) . ?
C1 O2 1.243(3) . ?
C1 C2 1.502(4) . ?
N2 C13 1.339(4) . ?
N2 C12 1.455(4) . ?
N2 H2A 0.8600 . ?
C2 C3 1.358(4) . ?
O2W H2WA 0.9467 . ?
O2W H2WB 0.8784 . ?
O3 C6 1.262(3) . ?
O3 Ni1 2.208(2) 6_576 ?
N3 C19 1.334(4) . ?
N3 C23 1.340(4) . ?
C3 C4 1.409(4) . ?
C3 H3A 0.9300 . ?
O3W H3WA 0.8029 . ?
O4 C6 1.264(3) . ?
O4 Ni1 2.1536(19) 6_576 ?
N4 C25 1.341(4) . ?
N4 C24 1.452(4) . ?
N4 H4B 0.8600 . ?
C4 C5 1.370(4) . ?
C4 H4A 0.9300 . ?
O5 C25 1.240(4) . ?
C5 C6 1.485(4) . ?
O6 C13 1.234(4) . ?
C6 Ni1 2.500(3) 6_576 ?
C7 C8 1.369(4) . ?
C7 H7A 0.9300 . ?
C8 C9 1.379(4) . ?
C8 H8A 0.9300 . ?
C9 C11 1.378(4) . ?
C9 H9A 0.9300 . ?
C10 C11 1.388(4) . ?
C10 H10A 0.9300 . ?
C11 C12 1.512(4) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C14 1.515(4) . ?
C14 C18 1.355(5) . ?
C14 C15 1.429(5) . ?
C15 C16 1.372(5) . ?
C15 H15A 0.9300 . ?
C16 C17 1.387(5) . ?
C16 H16A 0.9300 . ?
C17 C17 1.405(7) 7_565 ?
C17 C18 1.461(5) 7_565 ?
C18 C17 1.461(5) 7_565 ?
C18 H18A 0.9300 . ?
C19 C20 1.376(5) . ?
C19 H19A 0.9300 . ?
C20 C21 1.370(5) . ?
C20 H20A 0.9300 . ?
C21 C22 1.381(4) . ?
C21 H21A 0.9300 . ?
C22 C23 1.383(4) . ?
C22 C24 1.511(4) . ?
C23 H23A 0.9300 . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 C26 1.499(4) . ?
C26 C30 1.370(4) . ?
C26 C27 1.423(4) . ?
C27 C28 1.360(4) . ?
C27 H27A 0.9300 . ?
C28 C29 1.415(4) . ?
C28 H28A 0.9300 . ?
C29 C30 1.411(4) 5_576 ?
C29 C29 1.419(6) 5_576 ?
C30 C29 1.411(4) 5_576 ?
C30 H30A 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni1 N3 94.93(9) . . ?
O1 Ni1 O1W 89.37(8) . . ?
N3 Ni1 O1W 94.45(9) . . ?
O1 Ni1 N1 88.30(8) . . ?
N3 Ni1 N1 90.68(9) . . ?
O1W Ni1 N1 174.53(9) . . ?
O1 Ni1 O4 166.81(8) . 6_575 ?
N3 Ni1 O4 97.84(8) . 6_575 ?
O1W Ni1 O4 86.38(8) . 6_575 ?
N1 Ni1 O4 94.82(8) . 6_575 ?
O1 Ni1 O3 106.65(8) . 6_575 ?
N3 Ni1 O3 158.28(8) . 6_575 ?
O1W Ni1 O3 83.63(8) . 6_575 ?
N1 Ni1 O3 92.31(8) . 6_575 ?
O4 Ni1 O3 60.47(7) 6_575 6_575 ?
O1 Ni1 C6 136.54(9) . 6_575 ?
N3 Ni1 C6 128.00(9) . 6_575 ?
O1W Ni1 C6 81.73(8) . 6_575 ?
N1 Ni1 C6 96.60(9) . 6_575 ?
O4 Ni1 C6 30.37(8) 6_575 6_575 ?
O3 Ni1 C6 30.29(8) 6_575 6_575 ?
C2 S1 C5 91.78(13) . . ?
C1 O1 Ni1 129.14(18) . . ?
Ni1 O1W H1WA 121.3 . . ?
Ni1 O1W H1WB 114.0 . . ?
H1WA O1W H1WB 91.6 . . ?
C7 N1 C10 116.7(3) . . ?
C7 N1 Ni1 120.6(2) . . ?
C10 N1 Ni1 122.59(19) . . ?
O2 C1 O1 126.2(3) . . ?
O2 C1 C2 117.8(2) . . ?
O1 C1 C2 115.9(3) . . ?
C13 N2 C12 120.8(3) . . ?
C13 N2 H2A 119.6 . . ?
C12 N2 H2A 119.6 . . ?
C3 C2 C1 128.9(3) . . ?
C3 C2 S1 111.5(2) . . ?
C1 C2 S1 119.5(2) . . ?
H2WA O2W H2WB 105.9 . . ?
C6 O3 Ni1 87.80(16) . 6_576 ?
C19 N3 C23 117.3(3) . . ?
C19 N3 Ni1 121.0(2) . . ?
C23 N3 Ni1 121.68(19) . . ?
C2 C3 C4 112.8(3) . . ?
C2 C3 H3A 123.6 . . ?
C4 C3 H3A 123.6 . . ?
C6 O4 Ni1 90.17(15) . 6_576 ?
C25 N4 C24 119.8(3) . . ?
C25 N4 H4B 120.1 . . ?
C24 N4 H4B 120.1 . . ?
C5 C4 C3 112.9(3) . . ?
C5 C4 H4A 123.5 . . ?
C3 C4 H4A 123.5 . . ?
C4 C5 C6 128.0(3) . . ?
C4 C5 S1 110.9(2) . . ?
C6 C5 S1 121.1(2) . . ?
O3 C6 O4 120.8(2) . . ?
O3 C6 C5 118.9(3) . . ?
O4 C6 C5 120.2(2) . . ?
O3 C6 Ni1 61.91(14) . 6_576 ?
O4 C6 Ni1 59.46(14) . 6_576 ?
C5 C6 Ni1 171.6(2) . 6_576 ?
N1 C7 C8 123.0(3) . . ?
N1 C7 H7A 118.5 . . ?
C8 C7 H7A 118.5 . . ?
C7 C8 C9 119.9(3) . . ?
C7 C8 H8A 120.1 . . ?
C9 C8 H8A 120.1 . . ?
C11 C9 C8 118.9(3) . . ?
C11 C9 H9A 120.6 . . ?
C8 C9 H9A 120.6 . . ?
N1 C10 C11 124.2(3) . . ?
N1 C10 H10A 117.9 . . ?
C11 C10 H10A 117.9 . . ?
C9 C11 C10 117.4(3) . . ?
C9 C11 C12 120.9(3) . . ?
C10 C11 C12 121.6(3) . . ?
N2 C12 C11 112.1(2) . . ?
N2 C12 H12A 109.2 . . ?
C11 C12 H12A 109.2 . . ?
N2 C12 H12B 109.2 . . ?
C11 C12 H12B 109.2 . . ?
H12A C12 H12B 107.9 . . ?
O6 C13 N2 121.5(3) . . ?
O6 C13 C14 122.4(3) . . ?
N2 C13 C14 116.0(3) . . ?
C18 C14 C15 120.7(3) . . ?
C18 C14 C13 115.9(3) . . ?
C15 C14 C13 123.3(3) . . ?
C16 C15 C14 120.8(3) . . ?
C16 C15 H15A 119.6 . . ?
C14 C15 H15A 119.6 . . ?
C15 C16 C17 118.9(3) . . ?
C15 C16 H16A 120.5 . . ?
C17 C16 H16A 120.5 . . ?
C16 C17 C17 122.7(4) . 7_565 ?
C16 C17 C18 120.2(3) . 7_565 ?
C17 C17 C18 117.1(4) 7_565 7_565 ?
C14 C18 C17 119.7(3) . 7_565 ?
C14 C18 H18A 120.1 . . ?
C17 C18 H18A 120.1 7_565 . ?
N3 C19 C20 122.4(3) . . ?
N3 C19 H19A 118.8 . . ?
C20 C19 H19A 118.8 . . ?
C21 C20 C19 119.6(3) . . ?
C21 C20 H20A 120.2 . . ?
C19 C20 H20A 120.2 . . ?
C20 C21 C22 119.3(3) . . ?
C20 C21 H21A 120.4 . . ?
C22 C21 H21A 120.4 . . ?
C21 C22 C23 117.4(3) . . ?
C21 C22 C24 120.3(3) . . ?
C23 C22 C24 122.4(3) . . ?
N3 C23 C22 124.0(3) . . ?
N3 C23 H23A 118.0 . . ?
C22 C23 H23A 118.0 . . ?
N4 C24 C22 113.2(2) . . ?
N4 C24 H24A 108.9 . . ?
C22 C24 H24A 108.9 . . ?
N4 C24 H24B 108.9 . . ?
C22 C24 H24B 108.9 . . ?
H24A C24 H24B 107.7 . . ?
O5 C25 N4 120.8(3) . . ?
O5 C25 C26 120.8(3) . . ?
N4 C25 C26 118.4(3) . . ?
C30 C26 C27 119.3(3) . . ?
C30 C26 C25 117.5(3) . . ?
C27 C26 C25 123.2(3) . . ?
C28 C27 C26 120.2(3) . . ?
C28 C27 H27A 119.9 . . ?
C26 C27 H27A 119.9 . . ?
C27 C28 C29 121.4(3) . . ?
C27 C28 H28A 119.3 . . ?
C29 C28 H28A 119.3 . . ?
C30 C29 C28 122.6(3) 5_576 . ?
C30 C29 C29 118.7(3) 5_576 5_576 ?
C28 C29 C29 118.7(3) . 5_576 ?
C26 C30 C29 121.7(3) . 5_576 ?
C26 C30 H30A 119.2 . . ?
C29 C30 H30A 119.2 5_576 . ?

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
N3 Ni1 O1 C1 -122.0(2) . . . . ?
O1W Ni1 O1 C1 -27.6(2) . . . . ?
N1 Ni1 O1 C1 147.4(2) . . . . ?
O4 Ni1 O1 C1 43.5(5) 6_575 . . . ?
O3 Ni1 O1 C1 55.5(3) 6_575 . . . ?
C6 Ni1 O1 C1 49.6(3) 6_575 . . . ?
O1 Ni1 N1 C7 -14.0(2) . . . . ?
N3 Ni1 N1 C7 -109.0(2) . . . . ?
O1W Ni1 N1 C7 50.7(9) . . . . ?
O4 Ni1 N1 C7 153.1(2) 6_575 . . . ?
O3 Ni1 N1 C7 92.6(2) 6_575 . . . ?
C6 Ni1 N1 C7 122.6(2) 6_575 . . . ?
O1 Ni1 N1 C10 161.0(2) . . . . ?
N3 Ni1 N1 C10 66.1(2) . . . . ?
O1W Ni1 N1 C10 -134.3(8) . . . . ?
O4 Ni1 N1 C10 -31.9(2) 6_575 . . . ?
O3 Ni1 N1 C10 -92.4(2) 6_575 . . . ?
C6 Ni1 N1 C10 -62.3(2) 6_575 . . . ?
Ni1 O1 C1 O2 0.7(5) . . . . ?
Ni1 O1 C1 C2 -179.90(18) . . . . ?
O2 C1 C2 C3 166.0(3) . . . . ?
O1 C1 C2 C3 -13.4(5) . . . . ?
O2 C1 C2 S1 -11.0(4) . . . . ?
O1 C1 C2 S1 169.6(2) . . . . ?
C5 S1 C2 C3 0.4(2) . . . . ?
C5 S1 C2 C1 177.9(2) . . . . ?
O1 Ni1 N3 C19 -171.1(3) . . . . ?
O1W Ni1 N3 C19 99.1(3) . . . . ?
N1 Ni1 N3 C19 -82.8(3) . . . . ?
O4 Ni1 N3 C19 12.2(3) 6_575 . . . ?
O3 Ni1 N3 C19 15.2(4) 6_575 . . . ?
C6 Ni1 N3 C19 16.1(3) 6_575 . . . ?
O1 Ni1 N3 C23 10.4(2) . . . . ?
O1W Ni1 N3 C23 -79.3(2) . . . . ?
N1 Ni1 N3 C23 98.8(2) . . . . ?
O4 Ni1 N3 C23 -166.3(2) 6_575 . . . ?
O3 Ni1 N3 C23 -163.2(2) 6_575 . . . ?
C6 Ni1 N3 C23 -162.3(2) 6_575 . . . ?
C1 C2 C3 C4 -177.2(3) . . . . ?
S1 C2 C3 C4 0.1(3) . . . . ?
C2 C3 C4 C5 -0.7(4) . . . . ?
C3 C4 C5 C6 178.9(3) . . . . ?
C3 C4 C5 S1 0.9(3) . . . . ?
C2 S1 C5 C4 -0.8(2) . . . . ?
C2 S1 C5 C6 -178.9(2) . . . . ?
Ni1 O3 C6 O4 8.5(3) 6_576 . . . ?
Ni1 O3 C6 C5 -170.5(2) 6_576 . . . ?
Ni1 O4 C6 O3 -8.7(3) 6_576 . . . ?
Ni1 O4 C6 C5 170.2(2) 6_576 . . . ?
C4 C5 C6 O3 5.3(5) . . . . ?
S1 C5 C6 O3 -176.9(2) . . . . ?
C4 C5 C6 O4 -173.7(3) . . . . ?
S1 C5 C6 O4 4.1(4) . . . . ?
C4 C5 C6 Ni1 -88.2(14) . . . 6_576 ?
S1 C5 C6 Ni1 89.6(14) . . . 6_576 ?
C10 N1 C7 C8 -0.2(5) . . . . ?
Ni1 N1 C7 C8 175.0(3) . . . . ?
N1 C7 C8 C9 0.5(6) . . . . ?
C7 C8 C9 C11 -0.4(5) . . . . ?
C7 N1 C10 C11 -0.1(4) . . . . ?
Ni1 N1 C10 C11 -175.3(2) . . . . ?
C8 C9 C11 C10 0.1(4) . . . . ?
C8 C9 C11 C12 178.5(3) . . . . ?
N1 C10 C11 C9 0.2(4) . . . . ?
N1 C10 C11 C12 -178.2(3) . . . . ?
C13 N2 C12 C11 -86.2(3) . . . . ?
C9 C11 C12 N2 -106.4(3) . . . . ?
C10 C11 C12 N2 71.9(4) . . . . ?
C12 N2 C13 O6 -4.1(4) . . . . ?
C12 N2 C13 C14 173.8(2) . . . . ?
O6 C13 C14 C18 6.9(4) . . . . ?
N2 C13 C14 C18 -170.9(3) . . . . ?
O6 C13 C14 C15 -176.2(3) . . . . ?
N2 C13 C14 C15 6.0(4) . . . . ?
C18 C14 C15 C16 0.3(5) . . . . ?
C13 C14 C15 C16 -176.4(3) . . . . ?
C14 C15 C16 C17 0.6(5) . . . . ?
C15 C16 C17 C17 -1.1(6) . . . 7_565 ?
C15 C16 C17 C18 179.6(3) . . . 7_565 ?
C15 C14 C18 C17 -0.7(5) . . . 7_565 ?
C13 C14 C18 C17 176.3(3) . . . 7_565 ?
C23 N3 C19 C20 -1.1(5) . . . . ?
Ni1 N3 C19 C20 -179.6(3) . . . . ?
N3 C19 C20 C21 1.7(6) . . . . ?
C19 C20 C21 C22 -0.4(6) . . . . ?
C20 C21 C22 C23 -1.3(5) . . . . ?
C20 C21 C22 C24 178.4(3) . . . . ?
C19 N3 C23 C22 -0.8(5) . . . . ?
Ni1 N3 C23 C22 177.7(2) . . . . ?
C21 C22 C23 N3 2.0(5) . . . . ?
C24 C22 C23 N3 -177.7(3) . . . . ?
C25 N4 C24 C22 66.1(4) . . . . ?
C21 C22 C24 N4 -158.5(3) . . . . ?
C23 C22 C24 N4 21.1(4) . . . . ?
C24 N4 C25 O5 5.0(4) . . . . ?
C24 N4 C25 C26 -172.8(2) . . . . ?
O5 C25 C26 C30 -5.3(4) . . . . ?
N4 C25 C26 C30 172.5(3) . . . . ?
O5 C25 C26 C27 175.7(3) . . . . ?
N4 C25 C26 C27 -6.5(4) . . . . ?
C30 C26 C27 C28 -0.8(4) . . . . ?
C25 C26 C27 C28 178.2(3) . . . . ?
C26 C27 C28 C29 -0.4(5) . . . . ?
C27 C28 C29 C30 -179.3(3) . . . 5_576 ?
C27 C28 C29 C29 0.8(5) . . . 5_576 ?
C27 C26 C30 C29 1.5(4) . . . 5_576 ?
C25 C26 C30 C29 -177.5(3) . . . 5_576 ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.15
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.690
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.064
####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1954591'
loop_
_audit_author_name
_audit_author_address
'Jing zhao'
;The Cambridge Crystallographic Data Centre
China
;
_audit_update_record             
;
2019-12-17 deposited with the CCDC.	2020-01-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C34 H32 N4 Ni O8'
_chemical_formula_weight         683.35

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   16.5083(7)
_cell_length_b                   9.8738(4)
_cell_length_c                   19.9446(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.5950(10)
_cell_angle_gamma                90.00
_cell_volume                     3098.9(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5220
_cell_measurement_theta_min      2.14
_cell_measurement_theta_max      25.00

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            GREEN
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1424
_exptl_absorpt_coefficient_mu    0.687
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9040
_exptl_absorpt_correction_T_max  0.9283
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            20344
_diffrn_reflns_av_R_equivalents  0.0272
_diffrn_reflns_av_sigmaI/netI    0.0305
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.14
_diffrn_reflns_theta_max         26.99
_reflns_number_total             6740
_reflns_number_gt                5017
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2001)'
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT+ (Bruker, 1999)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXTL (1998)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0619P)²+1.1567P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6740
_refine_ls_number_parameters     428
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0419
_refine_ls_wR_factor_ref         0.1206
_refine_ls_wR_factor_gt          0.1077
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.017
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.752381(17) 0.08039(3) 0.759174(15) 0.03465(11) Uani 1 1 d . . .
O1 O 0.79280(11) 0.09212(15) 0.86639(8) 0.0424(4) Uani 1 1 d . . .
N1 N 0.84336(12) -0.07036(19) 0.76673(10) 0.0365(4) Uani 1 1 d . . .
O1W O 0.66689(10) 0.24147(17) 0.75637(9) 0.0474(4) Uani 1 1 d . . .
H1WA H 0.6754 0.3088 0.7328 0.057 Uiso 1 1 d R . .
H1WB H 0.6924 0.2724 0.7970 0.057 Uiso 1 1 d R . .
C1 C 0.79674(16) 0.1926(2) 0.90512(12) 0.0417(6) Uani 1 1 d . . .
O2W O 0.84387(10) 0.22826(17) 0.75398(10) 0.0495(4) Uani 1 1 d . . .
H2WA H 0.8246 0.2310 0.7094 0.059 Uiso 1 1 d R . .
H2WB H 0.8329 0.3054 0.7680 0.059 Uiso 1 1 d R . .
N2 N 0.66017(11) -0.06401(19) 0.76145(10) 0.0359(4) Uani 1 1 d . . .
O2 O 0.75573(15) 0.3010(2) 0.88659(10) 0.0715(6) Uani 1 1 d . . .
C2 C 0.85341(17) 0.1796(3) 0.98112(13) 0.0494(6) Uani 1 1 d . . .
H2A H 0.8741 0.2688 0.9984 0.059 Uiso 1 1 calc R . .
H2B H 0.8193 0.1464 1.0096 0.059 Uiso 1 1 calc R . .
O3 O 0.70758(11) 0.07091(17) 0.65144(9) 0.0473(4) Uani 1 1 d . . .
N3 N 0.71304(13) -0.4000(2) 0.90492(11) 0.0477(5) Uani 1 1 d . . .
H3A H 0.7307 -0.4637 0.8834 0.057 Uiso 1 1 calc R . .
C3 C 0.92860(16) 0.0864(2) 0.99077(11) 0.0393(5) Uani 1 1 d . . .
N4 N 0.77873(13) -0.4025(2) 0.62840(11) 0.0449(5) Uani 1 1 d . . .
H4B H 0.7629 -0.3675 0.5870 0.054 Uiso 1 1 calc R . .
C4 C 0.92437(16) -0.0507(2) 1.00431(13) 0.0446(6) Uani 1 1 d . . .
H4A H 0.8739 -0.0871 1.0078 0.053 Uiso 1 1 calc R . .
O4 O 0.77694(17) 0.2370(3) 0.61928(11) 0.0921(9) Uani 1 1 d . . .
O5 O 0.74614(10) -0.25676(17) 0.99701(10) 0.0558(5) Uani 1 1 d . . .
C5 C 0.99384(17) -0.1342(3) 1.01264(13) 0.0460(6) Uani 1 1 d . . .
H5A H 0.9884 -0.2259 1.0208 0.055 Uiso 1 1 calc R . .
O6 O 0.73891(12) -0.51143(19) 0.71282(10) 0.0592(5) Uani 1 1 d . . .
C6 C 0.72052(17) 0.1487(3) 0.60666(13) 0.0456(6) Uani 1 1 d . . .
C7 C 0.66422(19) 0.1373(3) 0.53053(14) 0.0525(7) Uani 1 1 d . . .
H7A H 0.6813 0.1738 0.4940 0.063 Uiso 1 1 calc R . .
H7B H 0.696(2) 0.074(3) 0.5115(19) 0.095(12) Uiso 1 1 d . . .
C8 C 0.58040(17) 0.0654(2) 0.51614(12) 0.0433(6) Uani 1 1 d . . .
C9 C 0.57331(18) -0.0708(2) 0.53047(14) 0.0497(6) Uani 1 1 d . . .
H9A H 0.6223 -0.1208 0.5510 0.060 Uiso 1 1 calc R . .
C10 C 0.49537(18) -0.1337(3) 0.51505(13) 0.0486(6) Uani 1 1 d . . .
H10A H 0.4933 -0.2250 0.5259 0.058 Uiso 1 1 calc R . .
C11 C 0.58635(15) -0.0678(3) 0.70928(13) 0.0426(6) Uani 1 1 d . . .
H11A H 0.5772 -0.0058 0.6726 0.051 Uiso 1 1 calc R . .
C12 C 0.52392(16) -0.1605(3) 0.70846(14) 0.0514(7) Uani 1 1 d . . .
H12A H 0.4732 -0.1605 0.6718 0.062 Uiso 1 1 calc R . .
C13 C 0.53682(15) -0.2531(3) 0.76190(14) 0.0475(6) Uani 1 1 d . . .
H13A H 0.4948 -0.3158 0.7620 0.057 Uiso 1 1 calc R . .
C14 C 0.61276(14) -0.2524(2) 0.81563(12) 0.0390(5) Uani 1 1 d . . .
C15 C 0.67217(14) -0.1557(2) 0.81306(12) 0.0382(5) Uani 1 1 d . . .
H15A H 0.7234 -0.1542 0.8491 0.046 Uiso 1 1 calc R . .
C16 C 0.62642(16) -0.3515(3) 0.87591(15) 0.0558(7) Uani 1 1 d . . .
H16A H 0.6094 -0.3084 0.9132 0.067 Uiso 1 1 calc R . .
H16B H 0.5894 -0.4288 0.8598 0.067 Uiso 1 1 calc R . .
C17 C 0.76590(15) -0.3493(2) 0.96355(13) 0.0421(6) Uani 1 1 d . . .
C18 C 0.85291(15) -0.4098(2) 0.98730(13) 0.0404(5) Uani 1 1 d . . .
C19 C 0.89562(16) -0.4424(2) 0.94042(13) 0.0421(6) Uani 1 1 d . . .
H19A H 0.8686 -0.4319 0.8925 0.050 Uiso 1 1 calc R . .
C20 C 0.97975(15) -0.4915(2) 0.96318(12) 0.0383(5) Uani 1 1 d . . .
C21 C 1.02595(17) -0.5245(2) 0.91606(13) 0.0456(6) Uani 1 1 d . . .
H21A H 1.0007 -0.5130 0.8680 0.055 Uiso 1 1 calc R . .
C22 C 1.10683(16) -0.5730(2) 0.94005(14) 0.0450(6) Uani 1 1 d . . .
H22A H 1.1358 -0.5950 0.9082 0.054 Uiso 1 1 calc R . .
C23 C 0.91958(15) -0.0666(3) 0.81653(13) 0.0437(6) Uani 1 1 d . . .
H23A H 0.9310 0.0035 0.8492 0.052 Uiso 1 1 calc R . .
C24 C 0.98082(15) -0.1627(3) 0.82066(13) 0.0473(6) Uani 1 1 d . . .
H24A H 1.0330 -0.1570 0.8554 0.057 Uiso 1 1 calc R . .
C25 C 0.96471(15) -0.2677(2) 0.77311(13) 0.0427(6) Uani 1 1 d . . .
H25A H 1.0062 -0.3324 0.7747 0.051 Uiso 1 1 calc R . .
C26 C 0.88550(14) -0.2759(2) 0.72272(12) 0.0366(5) Uani 1 1 d . . .
C27 C 0.82769(14) -0.1746(2) 0.72165(12) 0.0364(5) Uani 1 1 d . . .
H27A H 0.7748 -0.1789 0.6877 0.044 Uiso 1 1 calc R . .
C28 C 0.86669(16) -0.3919(3) 0.67063(14) 0.0486(6) Uani 1 1 d . . .
H28A H 0.9015 -0.3814 0.6395 0.058 Uiso 1 1 calc R . .
H28B H 0.8833 -0.4760 0.6963 0.058 Uiso 1 1 calc R . .
C29 C 0.72165(17) -0.4656(2) 0.65263(14) 0.0454(6) Uani 1 1 d . . .
C30 C 0.63327(16) -0.4778(2) 0.60263(13) 0.0429(6) Uani 1 1 d . . .
C31 C 0.61727(16) -0.4784(2) 0.53118(13) 0.0431(6) Uani 1 1 d . . .
H31A H 0.6622 -0.4693 0.5125 0.052 Uiso 1 1 calc R . .
C32 C 0.53410(16) -0.4927(2) 0.48536(13) 0.0405(5) Uani 1 1 d . . .
C33 C 0.51598(17) -0.4945(3) 0.41140(13) 0.0485(6) Uani 1 1 d . . .
H33A H 0.5601 -0.4868 0.3916 0.058 Uiso 1 1 calc R . .
C34 C 0.43450(17) -0.5073(3) 0.36879(14) 0.0493(6) Uani 1 1 d . . .
H34A H 0.4235 -0.5061 0.3202 0.059 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1 2.0417(16) . ?
Ni1 O3 2.0523(17) . ?
Ni1 N1 2.0875(19) . ?
Ni1 N2 2.0962(19) . ?
Ni1 O1W 2.1158(16) . ?
Ni1 O2W 2.1255(17) . ?
O1 C1 1.247(3) . ?
N1 C27 1.339(3) . ?
N1 C23 1.347(3) . ?
C1 O2 1.260(3) . ?
C1 C2 1.527(3) . ?
N2 C15 1.340(3) . ?
N2 C11 1.342(3) . ?
C2 C3 1.510(4) . ?
O3 C6 1.245(3) . ?
N3 C17 1.328(3) . ?
N3 C16 1.452(3) . ?
C3 C5 1.385(4) 3_757 ?
C3 C4 1.387(3) . ?
N4 C29 1.336(3) . ?
N4 C28 1.445(3) . ?
C4 C5 1.381(4) . ?
O4 C6 1.245(3) . ?
O5 C17 1.232(3) . ?
C5 C3 1.385(4) 3_757 ?
O6 C29 1.233(3) . ?
C6 C7 1.526(4) . ?
C7 C8 1.503(4) . ?
C8 C9 1.387(3) . ?
C8 C10 1.391(4) 3_656 ?
C9 C10 1.377(4) . ?
C10 C8 1.391(4) 3_656 ?
C11 C12 1.375(4) . ?
C12 C13 1.371(4) . ?
C13 C14 1.381(3) . ?
C14 C15 1.381(3) . ?
C14 C16 1.513(3) . ?
C17 C18 1.494(3) . ?
C18 C19 1.369(4) . ?
C18 C22 1.410(3) 3_747 ?
C19 C20 1.410(3) . ?
C20 C21 1.416(3) . ?
C20 C20 1.428(4) 3_747 ?
C21 C22 1.362(3) . ?
C22 C18 1.410(3) 3_747 ?
C23 C24 1.371(4) . ?
C24 C25 1.376(4) . ?
C25 C26 1.390(3) . ?
C26 C27 1.378(3) . ?
C26 C28 1.515(3) . ?
C29 C30 1.503(3) . ?
C30 C31 1.368(3) . ?
C30 C34 1.409(4) 3_646 ?
C31 C32 1.408(3) . ?
C32 C33 1.414(3) . ?
C32 C32 1.423(5) 3_646 ?
C33 C34 1.362(4) . ?
C34 C30 1.409(4) 3_646 ?

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 O3 177.97(7) . . ?
O1 Ni1 N1 87.97(7) . . ?
O3 Ni1 N1 93.83(7) . . ?
O1 Ni1 N2 91.46(7) . . ?
O3 Ni1 N2 87.56(7) . . ?
N1 Ni1 N2 91.42(8) . . ?
O1 Ni1 O1W 89.38(7) . . ?
O3 Ni1 O1W 88.87(7) . . ?
N1 Ni1 O1W 175.99(7) . . ?
N2 Ni1 O1W 91.66(7) . . ?
O1 Ni1 O2W 90.01(7) . . ?
O3 Ni1 O2W 90.96(7) . . ?
N1 Ni1 O2W 89.25(7) . . ?
N2 Ni1 O2W 178.41(7) . . ?
O1W Ni1 O2W 87.74(7) . . ?
C1 O1 Ni1 129.29(15) . . ?
C27 N1 C23 117.6(2) . . ?
C27 N1 Ni1 120.71(15) . . ?
C23 N1 Ni1 121.65(16) . . ?
O1 C1 O2 124.8(2) . . ?
O1 C1 C2 116.7(2) . . ?
O2 C1 C2 118.4(2) . . ?
C15 N2 C11 117.7(2) . . ?
C15 N2 Ni1 122.45(15) . . ?
C11 N2 Ni1 119.81(16) . . ?
C3 C2 C1 114.3(2) . . ?
C6 O3 Ni1 129.60(16) . . ?
C17 N3 C16 122.2(2) . . ?
C5 C3 C4 116.3(2) 3_757 . ?
C5 C3 C2 121.5(2) 3_757 . ?
C4 C3 C2 122.1(2) . . ?
C29 N4 C28 121.1(2) . . ?
C5 C4 C3 121.1(2) . . ?
C4 C5 C3 122.5(2) . 3_757 ?
O3 C6 O4 124.6(2) . . ?
O3 C6 C7 118.9(2) . . ?
O4 C6 C7 116.5(2) . . ?
C8 C7 C6 118.3(2) . . ?
C9 C8 C10 116.2(3) . 3_656 ?
C9 C8 C7 123.3(3) . . ?
C10 C8 C7 120.5(2) 3_656 . ?
C10 C9 C8 121.5(3) . . ?
C9 C10 C8 122.3(2) . 3_656 ?
N2 C11 C12 122.0(2) . . ?
C13 C12 C11 119.7(2) . . ?
C12 C13 C14 119.4(2) . . ?
C15 C14 C13 117.6(2) . . ?
C15 C14 C16 122.7(2) . . ?
C13 C14 C16 119.7(2) . . ?
N2 C15 C14 123.6(2) . . ?
N3 C16 C14 115.0(2) . . ?
O5 C17 N3 123.1(2) . . ?
O5 C17 C18 120.7(2) . . ?
N3 C17 C18 116.2(2) . . ?
C19 C18 C22 119.6(2) . 3_747 ?
C19 C18 C17 121.5(2) . . ?
C22 C18 C17 118.9(2) 3_747 . ?
C18 C19 C20 121.4(2) . . ?
C19 C20 C21 122.8(2) . . ?
C19 C20 C20 118.8(3) . 3_747 ?
C21 C20 C20 118.5(3) . 3_747 ?
C22 C21 C20 121.0(2) . . ?
C21 C22 C18 120.7(2) . 3_747 ?
N1 C23 C24 122.2(2) . . ?
C23 C24 C25 119.7(2) . . ?
C24 C25 C26 119.1(2) . . ?
C27 C26 C25 117.7(2) . . ?
C27 C26 C28 122.8(2) . . ?
C25 C26 C28 119.5(2) . . ?
N1 C27 C26 123.7(2) . . ?
N4 C28 C26 114.6(2) . . ?
O6 C29 N4 122.9(2) . . ?
O6 C29 C30 120.6(2) . . ?
N4 C29 C30 116.5(2) . . ?
C31 C30 C34 119.6(2) . 3_646 ?
C31 C30 C29 122.3(2) . . ?
C34 C30 C29 118.1(2) 3_646 . ?
C30 C31 C32 121.3(2) . . ?
C31 C32 C33 122.4(2) . . ?
C31 C32 C32 118.7(3) . 3_646 ?
C33 C32 C32 118.9(3) . 3_646 ?
C34 C33 C32 120.6(3) . . ?
C33 C34 C30 120.8(2) . 3_646 ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        26.99
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.578
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.059
####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1954592'
loop_
_audit_author_name
_audit_author_address
'Jing zhao'
;The Cambridge Crystallographic Data Centre
China
;
_audit_update_record             
;
2019-12-17 deposited with the CCDC.	2020-01-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H28 N4 Ni O9'
_chemical_formula_sum            'C32 H28 N4 Ni O9'
_chemical_formula_weight         671.27

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           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                   21.551(2)
_cell_length_b                   7.2511(7)
_cell_length_c                   20.8300(18)
_cell_angle_alpha                90
_cell_angle_beta                 117.421(1)
_cell_angle_gamma                90
_cell_volume                     2889.4(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4555
_cell_measurement_theta_min      2.13
_cell_measurement_theta_max      25.00

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_F_000             1392
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    0.737
_shelx_estimated_absorpt_T_min   0.897
_shelx_estimated_absorpt_T_max   0.923
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.895
_exptl_absorpt_correction_T_max  0.923
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8203
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_av_R_equivalents  0.0208
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.129
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_full        25.242
_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             2650
_reflns_number_gt                2573
_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       'SMART (Bruker, 2001)'
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT+ (Bruker, 1999)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXTL (1998)'
_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)+(0.0059P)²+60.3216P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_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         2650
_refine_ls_number_parameters     211
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0729
_refine_ls_R_factor_gt           0.0715
_refine_ls_wR_factor_ref         0.1723
_refine_ls_wR_factor_gt          0.1717
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.051
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.0000 1.0000 0.5000 0.0267(3) Uani 1 2 d S . P . .
O1W O -0.0759(2) 0.7996(6) 0.4847(2) 0.0319(9) Uani 1 1 d . . . . .
H1A H -0.1175 0.8208 0.4461 0.038 Uiso 1 1 d R U . . .
H1B H -0.0806 0.8204 0.5249 0.038 Uiso 1 1 d R U . . .
O1 O 0.0281(2) 0.8560(6) 0.43040(19) 0.0328(10) Uani 1 1 d . . . . .
O2 O 0.0696(3) 1.0876(8) 0.3897(3) 0.0611(17) Uani 1 1 d . . . . .
O3 O 0.0000 0.3518(9) 0.2500 0.074(3) Uani 1 2 d S T P . .
H3A H 0.0302 0.2966 0.2916 0.089 Uiso 0.5 1 d R U P . .
O4 O 0.2905(2) 0.6936(6) 0.8669(2) 0.0346(10) Uani 1 1 d . . . . .
N1 N 0.0677(2) 0.8461(7) 0.5883(2) 0.0274(10) Uani 1 1 d . . . . .
N2 N 0.1856(2) 0.8006(7) 0.8477(2) 0.0281(10) Uani 1 1 d . . . . .
H2 H 0.1540 0.8035 0.8620 0.034 Uiso 1 1 calc R U . . .
C1 C 0.0712(3) 0.6634(9) 0.5831(3) 0.0351(14) Uani 1 1 d . . . . .
H1 H 0.0472 0.6091 0.5378 0.042 Uiso 1 1 calc R U . . .
C2 C 0.1085(4) 0.5516(9) 0.6417(3) 0.0413(16) Uani 1 1 d . . . . .
H2A H 0.1097 0.4247 0.6361 0.050 Uiso 1 1 calc R U . . .
C3 C 0.1441(4) 0.6320(9) 0.7088(3) 0.0407(15) Uani 1 1 d . . . . .
H3 H 0.1694 0.5588 0.7492 0.049 Uiso 1 1 calc R U . . .
C4 C 0.1423(3) 0.8212(7) 0.7164(3) 0.0233(11) Uani 1 1 d . . . . .
C5 C 0.1039(3) 0.9202(8) 0.6544(3) 0.0238(11) Uani 1 1 d . . . . .
H5 H 0.1028 1.0477 0.6584 0.029 Uiso 1 1 calc R U . . .
C6 C 0.1790(3) 0.9183(8) 0.7887(3) 0.0290(12) Uani 1 1 d . . . . .
H6A H 0.2252 0.9566 0.7968 0.035 Uiso 1 1 calc R U . . .
H6B H 0.1529 1.0281 0.7878 0.035 Uiso 1 1 calc R U . . .
C7 C 0.2403(3) 0.6875(8) 0.8801(3) 0.0264(12) Uani 1 1 d . . . . .
C8 C 0.2363(3) 0.5431(7) 0.9292(3) 0.0244(12) Uani 1 1 d . . . . .
C9 C 0.2757(3) 0.3883(8) 0.9410(3) 0.0306(13) Uani 1 1 d . . . . .
H9 H 0.3056 0.3788 0.9201 0.037 Uiso 1 1 calc R U . . .
C10 C 0.2727(3) 0.2422(8) 0.9838(3) 0.0276(12) Uani 1 1 d . . . . .
C11 C 0.3128(3) 0.0779(9) 0.9966(3) 0.0387(15) Uani 1 1 d . . . . .
H11 H 0.3426 0.0644 0.9759 0.046 Uiso 1 1 calc R U . . .
C12 C 0.3084(3) -0.0584(8) 1.0384(3) 0.0311(13) Uani 1 1 d . . . . .
H12 H 0.3353 -0.1643 1.0460 0.037 Uiso 1 1 calc R U . . .
C13 C 0.0421(3) 0.9327(9) 0.3840(3) 0.0339(14) Uani 1 1 d . . . . .
C14 C 0.0215(3) 0.8255(8) 0.3147(3) 0.0249(12) Uani 1 1 d . . . . .
C15 C 0.0000 0.9185(11) 0.2500 0.0264(17) Uani 1 2 d S T P . .
H15 H 0.0000 1.0468 0.2500 0.032 Uiso 1 2 calc R U P . .
C16 C 0.0202(3) 0.6351(8) 0.3143(3) 0.0343(14) Uani 1 1 d . . . . .
H16 H 0.0328 0.5704 0.3571 0.041 Uiso 1 1 calc R U . . .
C17 C 0.0000 0.5413(11) 0.2500 0.037(2) Uani 1 2 d S TU 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
Ni1 N1 2.070(5) 5_576 ?
Ni1 N1 2.070(5) . ?
Ni1 O1 2.090(4) . ?
Ni1 O1 2.090(4) 5_576 ?
Ni1 O1W 2.100(4) . ?
Ni1 O1W 2.100(4) 5_576 ?
O1W H1A 0.8999 . ?
O1W H1B 0.8992 . ?
O1 C13 1.268(7) . ?
O2 C13 1.249(8) . ?
O3 C17 1.374(10) . ?
O3 H3A 0.9024 . ?
O4 C7 1.236(6) . ?
N1 C1 1.334(8) . ?
N1 C5 1.343(7) . ?
N2 C7 1.336(7) . ?
N2 C6 1.449(7) . ?
N2 H2 0.8600 . ?
C1 C2 1.374(9) . ?
C1 H1 0.9300 . ?
C2 C3 1.376(9) . ?
C2 H2A 0.9300 . ?
C3 C4 1.384(8) . ?
C3 H3 0.9300 . ?
C4 C5 1.373(7) . ?
C4 C6 1.514(7) . ?
C5 H5 0.9300 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.493(7) . ?
C8 C9 1.360(8) . ?
C8 C12 1.413(7) 7_557 ?
C9 C10 1.406(8) . ?
C9 H9 0.9300 . ?
C10 C11 1.422(8) . ?
C10 C10 1.426(10) 7_557 ?
C11 C12 1.349(8) . ?
C11 H11 0.9300 . ?
C12 C8 1.413(7) 7_557 ?
C12 H12 0.9300 . ?
C13 C14 1.515(7) . ?
C14 C16 1.381(8) . ?
C14 C15 1.381(6) . ?
C15 C14 1.381(6) 2 ?
C15 H15 0.9300 . ?
C16 C17 1.382(7) . ?
C16 H16 0.9300 . ?
C17 C16 1.382(7) 2 ?

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 5_576 . ?
N1 Ni1 O1 87.95(16) 5_576 . ?
N1 Ni1 O1 92.05(16) . . ?
N1 Ni1 O1 92.05(16) 5_576 5_576 ?
N1 Ni1 O1 87.95(16) . 5_576 ?
O1 Ni1 O1 180.0 . 5_576 ?
N1 Ni1 O1W 93.26(17) 5_576 . ?
N1 Ni1 O1W 86.74(17) . . ?
O1 Ni1 O1W 90.20(16) . . ?
O1 Ni1 O1W 89.80(16) 5_576 . ?
N1 Ni1 O1W 86.74(17) 5_576 5_576 ?
N1 Ni1 O1W 93.26(17) . 5_576 ?
O1 Ni1 O1W 89.80(16) . 5_576 ?
O1 Ni1 O1W 90.20(16) 5_576 5_576 ?
O1W Ni1 O1W 180.0 . 5_576 ?
Ni1 O1W H1A 113.7 . . ?
Ni1 O1W H1B 98.9 . . ?
H1A O1W H1B 108.2 . . ?
C13 O1 Ni1 123.9(4) . . ?
C17 O3 H3A 116.3 . . ?
C1 N1 C5 116.9(5) . . ?
C1 N1 Ni1 120.5(4) . . ?
C5 N1 Ni1 122.3(4) . . ?
C7 N2 C6 120.6(5) . . ?
C7 N2 H2 119.7 . . ?
C6 N2 H2 119.7 . . ?
N1 C1 C2 123.1(6) . . ?
N1 C1 H1 118.4 . . ?
C2 C1 H1 118.4 . . ?
C1 C2 C3 118.4(6) . . ?
C1 C2 H2A 120.8 . . ?
C3 C2 H2A 120.8 . . ?
C2 C3 C4 120.3(6) . . ?
C2 C3 H3 119.8 . . ?
C4 C3 H3 119.8 . . ?
C5 C4 C3 116.5(5) . . ?
C5 C4 C6 120.4(5) . . ?
C3 C4 C6 123.1(5) . . ?
N1 C5 C4 124.7(5) . . ?
N1 C5 H5 117.6 . . ?
C4 C5 H5 117.6 . . ?
N2 C6 C4 111.8(5) . . ?
N2 C6 H6A 109.2 . . ?
C4 C6 H6A 109.2 . . ?
N2 C6 H6B 109.2 . . ?
C4 C6 H6B 109.2 . . ?
H6A C6 H6B 107.9 . . ?
O4 C7 N2 121.7(5) . . ?
O4 C7 C8 120.7(5) . . ?
N2 C7 C8 117.5(5) . . ?
C9 C8 C12 119.0(5) . 7_557 ?
C9 C8 C7 118.4(5) . . ?
C12 C8 C7 122.6(5) 7_557 . ?
C8 C9 C10 122.0(5) . . ?
C8 C9 H9 119.0 . . ?
C10 C9 H9 119.0 . . ?
C9 C10 C11 123.3(5) . . ?
C9 C10 C10 118.8(7) . 7_557 ?
C11 C10 C10 117.9(6) . 7_557 ?
C12 C11 C10 121.2(5) . . ?
C12 C11 H11 119.4 . . ?
C10 C11 H11 119.4 . . ?
C11 C12 C8 121.1(5) . 7_557 ?
C11 C12 H12 119.5 . . ?
C8 C12 H12 119.5 7_557 . ?
O2 C13 O1 126.2(6) . . ?
O2 C13 C14 118.1(5) . . ?
O1 C13 C14 115.7(5) . . ?
C16 C14 C15 119.1(5) . . ?
C16 C14 C13 121.0(5) . . ?
C15 C14 C13 119.9(5) . . ?
C14 C15 C14 121.6(7) 2 . ?
C14 C15 H15 119.2 2 . ?
C14 C15 H15 119.2 . . ?
C14 C16 C17 119.6(6) . . ?
C14 C16 H16 120.2 . . ?
C17 C16 H16 120.2 . . ?
O3 C17 C16 119.5(4) . 2 ?
O3 C17 C16 119.5(4) . . ?
C16 C17 C16 121.1(8) 2 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 N1 C1 C2 1.0(9) . . . . ?
Ni1 N1 C1 C2 -171.8(5) . . . . ?
N1 C1 C2 C3 -0.1(10) . . . . ?
C1 C2 C3 C4 -0.4(10) . . . . ?
C2 C3 C4 C5 -0.1(9) . . . . ?
C2 C3 C4 C6 178.8(6) . . . . ?
C1 N1 C5 C4 -1.5(8) . . . . ?
Ni1 N1 C5 C4 171.1(4) . . . . ?
C3 C4 C5 N1 1.1(8) . . . . ?
C6 C4 C5 N1 -177.8(5) . . . . ?
C7 N2 C6 C4 87.3(6) . . . . ?
C5 C4 C6 N2 150.9(5) . . . . ?
C3 C4 C6 N2 -28.0(8) . . . . ?
C6 N2 C7 O4 8.2(8) . . . . ?
C6 N2 C7 C8 -167.4(5) . . . . ?
O4 C7 C8 C9 -20.1(8) . . . . ?
N2 C7 C8 C9 155.6(5) . . . . ?
O4 C7 C8 C12 162.3(6) . . . 7_557 ?
N2 C7 C8 C12 -22.1(8) . . . 7_557 ?
C12 C8 C9 C10 0.7(9) 7_557 . . . ?
C7 C8 C9 C10 -177.1(5) . . . . ?
C8 C9 C10 C11 179.5(6) . . . . ?
C8 C9 C10 C10 -0.5(10) . . . 7_557 ?
C9 C10 C11 C12 179.7(6) . . . . ?
C10 C10 C11 C12 -0.4(11) 7_557 . . . ?
C10 C11 C12 C8 0.1(10) . . . 7_557 ?
Ni1 O1 C13 O2 31.8(9) . . . . ?
Ni1 O1 C13 C14 -146.5(4) . . . . ?
O2 C13 C14 C16 151.5(6) . . . . ?
O1 C13 C14 C16 -30.0(8) . . . . ?
O2 C13 C14 C15 -32.0(8) . . . . ?
O1 C13 C14 C15 146.5(5) . . . . ?
C16 C14 C15 C14 -1.2(4) . . . 2 ?
C13 C14 C15 C14 -177.8(5) . . . 2 ?
C15 C14 C16 C17 2.4(8) . . . . ?
C13 C14 C16 C17 179.0(4) . . . . ?
C14 C16 C17 O3 178.8(4) . . . . ?
C14 C16 C17 C16 -1.2(4) . . . 2 ?

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
N2 H2 O2 0.86 2.29 3.111(6) 161 6_576
O1W H1A O4 0.90 1.91 2.793(5) 167 8_465
O1W H1B O2 0.90 1.81 2.684(6) 163 5_576
O3 H3A O2 0.90 2.37 3.219(7) 158 1_545

_refine_diff_density_max         0.391
_refine_diff_density_min         -0.648
_refine_diff_density_rms         0.093

