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

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

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1983778'
loop_
_audit_author_name
_audit_author_address
'Shiro Hikichi'
;Kanagawa University
Japan
;
_audit_update_record             
;
2020-02-13 deposited with the CCDC.	2020-04-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        '[Ni(TOAMe2)(Cl)](BPh4)'
_chemical_name_common            
'[Chloridotris{(4,4-dimethyloxazolin-2-yl)methyl}aminenickel(II)]tetraphenylborate'
_chemical_melting_point          ?
_chemical_formula_moiety         
;C18 H30 Cl N4 Ni O3, C24 H20 B
;
_chemical_formula_sum            'C42 H50 B Cl N4 Ni O3'
_chemical_formula_weight         763.83

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   14.905(7)
_cell_length_b                   24.920(12)
_cell_length_c                   10.988(5)
_cell_angle_alpha                90
_cell_angle_beta                 102.752(4)
_cell_angle_gamma                90
_cell_volume                     3981(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    113(2)
_cell_measurement_reflns_used    9965
_cell_measurement_theta_min      1.4008
_cell_measurement_theta_max      27.3599

_exptl_crystal_description       Platelet
_exptl_crystal_colour            Orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_F_000             1616
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.597
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_correction_T_max  0.9404
_exptl_absorpt_correction_T_min  0.8331
_shelx_estimated_absorpt_T_min   0.796
_shelx_estimated_absorpt_T_max   0.943
_exptl_absorpt_process_details   
;Numerical (Based on real shape of the crystal) absorption
correction was parformed on CrystalClear (Rigaku Inc., 2008)
with NUMABS (Rigaku, 1999) method.
;
_diffrn_special_details          
;
 ?
;

_diffrn_source_power             3.0000
_diffrn_source_voltage           50.0000
_diffrn_source_current           60.0000

_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_detector       CCD
_diffrn_measurement_device       
;
Saturn70 (2x2 bin mode)
;
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measurement_method       dtprofit.ref
_diffrn_reflns_number            9021
_diffrn_number_total             9021
_diffrn_reflns_av_R_equivalents  0.0570
_diffrn_reflns_av_sigmaI/detI    0.1429

_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_measurement_details      
;
scan:
	Number of images: 600
	           Slice: -115.0000 - 65.0000
	     Image width: 0.3000
	        Exp time: 20.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 0.0000
	             XTD: 55.2371
	          2theta: -24.9030
scan:
	Number of images: 600
	           Slice: -115.0000 - 65.0000
	     Image width: 0.3000
	        Exp time: 20.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 90.0000
	             XTD: 55.2371
	          2theta: -24.9030
scan:
	Number of images: 600
	           Slice: -115.0000 - 65.0000
	     Image width: 0.3000
	        Exp time: 20.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 180.0000
	             XTD: 55.2371
	          2theta: -24.9030

;
_diffrn_measurement_device_details 
;
AFC10: Fixed Chi 2 circle
;
_diffrn_orient_matrix_UB_11      -0.0923
_diffrn_orient_matrix_UB_12      0.0133
_diffrn_orient_matrix_UB_13      0.0024
_diffrn_orient_matrix_UB_21      0.0023
_diffrn_orient_matrix_UB_22      0.0088
_diffrn_orient_matrix_UB_23      0.0391
_diffrn_orient_matrix_UB_31      -0.0061
_diffrn_orient_matrix_UB_32      0.0669
_diffrn_orient_matrix_UB_33      -0.0148
_diffrn_orient_matrix_type       d*Trek


_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      113(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  ?

_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.401
_diffrn_reflns_theta_max         27.303
_diffrn_reflns_theta_full        27.303
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measured_fraction_theta_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_point_group_measured_fraction_full 0.980
_reflns_number_total             8791
_reflns_number_gt                6909
_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       'CrystalClear (Rigaku Inc., 2007)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        
'CrystalClear (Rigaku Inc., 2007), SORTAV (Blessing, 1995)'
_computing_structure_solution    'SIR92 (Altomare et al, 1994)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0931P)²+4.5187P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8791
_refine_ls_number_parameters     476
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0667
_refine_ls_wR_factor_ref         0.1957
_refine_ls_wR_factor_gt          0.1871
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_restrained_S_all      1.077
_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 0.23201(3) 0.32542(2) 0.14701(4) 0.01597(14) Uani 1 1 d . . . . .
Cl1 Cl 0.23915(6) 0.26891(3) 0.31742(8) 0.0220(2) Uani 1 1 d . . . . .
N4 N 0.22280(19) 0.37550(11) -0.0288(3) 0.0172(6) Uani 1 1 d . . . . .
O3 O 0.23567(19) 0.48960(10) 0.1883(2) 0.0272(6) Uani 1 1 d . . . . .
N3 N 0.2431(2) 0.39985(12) 0.2217(3) 0.0216(6) Uani 1 1 d . . . . .
O1 O 0.45344(17) 0.32076(10) -0.0193(2) 0.0231(6) Uani 1 1 d . . . . .
O2 O -0.01405(18) 0.32705(11) -0.1157(3) 0.0298(6) Uani 1 1 d . . . . .
N2 N 0.0956(2) 0.31747(11) 0.0616(3) 0.0192(6) Uani 1 1 d . . . . .
N1 N 0.35919(19) 0.31149(11) 0.1149(3) 0.0179(6) Uani 1 1 d . . . . .
C27 C 0.0415(3) 0.01962(16) 0.1815(4) 0.0299(9) Uani 1 1 d . . . . .
H27 H 0.0136 0.0453 0.1211 0.036 Uiso 1 1 calc R U . . .
C28 C 0.0021(3) 0.00811(16) 0.2827(4) 0.0311(9) Uani 1 1 d . . . . .
H28 H -0.0527 0.0257 0.2915 0.037 Uiso 1 1 calc R U . . .
C4 C 0.4395(2) 0.27564(13) 0.1691(3) 0.0188(7) Uani 1 1 d . . . . .
C13 C 0.2068(3) 0.43238(14) 0.0048(4) 0.0245(8) Uani 1 1 d . . . . .
H13A H 0.1416 0.4421 -0.0286 0.029 Uiso 1 1 calc R U . . .
H13B H 0.2457 0.4567 -0.0328 0.029 Uiso 1 1 calc R U . . .
C25 C 0.1676(2) -0.04535(13) 0.2566(3) 0.0207(7) Uani 1 1 d . . . . .
C19 C 0.2543(2) -0.09276(13) 0.0896(3) 0.0212(7) Uani 1 1 d . . . . .
C29 C 0.0442(3) -0.02941(15) 0.3703(4) 0.0296(9) Uani 1 1 d . . . . .
H29 H 0.0179 -0.0379 0.4392 0.036 Uiso 1 1 calc R U . . .
C7 C 0.1411(2) 0.35511(15) -0.1220(3) 0.0221(7) Uani 1 1 d . . . . .
H7A H 0.1601 0.3266 -0.1737 0.026 Uiso 1 1 calc R U . . .
H7B H 0.1127 0.3846 -0.1778 0.026 Uiso 1 1 calc R U . . .
C31 C 0.3546(2) -0.03801(14) 0.2805(3) 0.0203(7) Uani 1 1 d . . . . .
C32 C 0.3529(3) 0.01676(14) 0.2477(3) 0.0217(7) Uani 1 1 d . . . . .
H32 H 0.2954 0.0330 0.2127 0.026 Uiso 1 1 calc R U . . .
C23 C 0.3259(3) -0.11289(15) -0.0874(4) 0.0318(9) Uani 1 1 d . . . . .
H23 H 0.3802 -0.1167 -0.1184 0.038 Uiso 1 1 calc R U . . .
C14 C 0.2299(2) 0.43890(14) 0.1445(3) 0.0206(7) Uani 1 1 d . . . . .
C37 C 0.2738(2) -0.13292(14) 0.3230(3) 0.0209(7) Uani 1 1 d . . . . .
C3 C 0.5071(2) 0.28784(15) 0.0837(3) 0.0220(7) Uani 1 1 d . . . . .
H3A H 0.5613 0.3079 0.1300 0.026 Uiso 1 1 calc R U . . .
H3B H 0.5283 0.2542 0.0512 0.026 Uiso 1 1 calc R U . . .
C26 C 0.1226(2) -0.00693(15) 0.1689(4) 0.0244(8) Uani 1 1 d . . . . .
H26 H 0.1479 0.0013 0.0990 0.029 Uiso 1 1 calc R U . . .
C40 C 0.2821(3) -0.22943(16) 0.4687(4) 0.0319(9) Uani 1 1 d . . . . .
H40 H 0.2844 -0.2612 0.5171 0.038 Uiso 1 1 calc R U . . .
C41 C 0.2525(3) -0.23115(15) 0.3389(4) 0.0294(9) Uani 1 1 d . . . . .
H41 H 0.2352 -0.2644 0.2981 0.035 Uiso 1 1 calc R U . . .
C20 C 0.1689(3) -0.10506(14) 0.0075(4) 0.0252(8) Uani 1 1 d . . . . .
H20 H 0.1143 -0.1033 0.0385 0.030 Uiso 1 1 calc R U . . .
C24 C 0.3323(3) -0.09729(14) 0.0373(4) 0.0254(8) Uani 1 1 d . . . . .
H24 H 0.3912 -0.0895 0.0880 0.030 Uiso 1 1 calc R U . . .
C42 C 0.2485(2) -0.18374(14) 0.2686(4) 0.0231(8) Uani 1 1 d . . . . .
H42 H 0.2277 -0.1859 0.1806 0.028 Uiso 1 1 calc R U . . .
C38 C 0.3040(3) -0.13302(16) 0.4542(4) 0.0269(8) Uani 1 1 d . . . . .
H38 H 0.3222 -0.1000 0.4956 0.032 Uiso 1 1 calc R U . . .
C21 C 0.1619(3) -0.11960(14) -0.1166(4) 0.0291(9) Uani 1 1 d . . . . .
H21 H 0.1033 -0.1274 -0.1681 0.035 Uiso 1 1 calc R U . . .
C5 C 0.4812(3) 0.29122(16) 0.3044(3) 0.0273(8) Uani 1 1 d . . . . .
H5A H 0.4973 0.3294 0.3084 0.041 Uiso 1 1 calc R U . . .
H5B H 0.5366 0.2698 0.3357 0.041 Uiso 1 1 calc R U . . .
H5C H 0.4363 0.2845 0.3557 0.041 Uiso 1 1 calc R U . . .
C2 C 0.3749(2) 0.33167(13) 0.0146(3) 0.0184(7) Uani 1 1 d . . . . .
C33 C 0.4335(3) 0.04845(15) 0.2649(4) 0.0272(8) Uani 1 1 d . . . . .
H33 H 0.4291 0.0852 0.2410 0.033 Uiso 1 1 calc R U . . .
C6 C 0.4076(3) 0.21687(14) 0.1573(4) 0.0264(8) Uani 1 1 d . . . . .
H6A H 0.3639 0.2107 0.2106 0.040 Uiso 1 1 calc R U . . .
H6B H 0.4610 0.1932 0.1835 0.040 Uiso 1 1 calc R U . . .
H6C H 0.3778 0.2092 0.0703 0.040 Uiso 1 1 calc R U . . .
C30 C 0.1256(2) -0.05484(14) 0.3571(4) 0.0236(8) Uani 1 1 d . . . . .
H30 H 0.1538 -0.0797 0.4194 0.028 Uiso 1 1 calc R U . . .
C10 C 0.0123(2) 0.29017(16) 0.0911(4) 0.0266(8) Uani 1 1 d . . . . .
C22 C 0.2405(3) -0.12284(15) -0.1658(4) 0.0325(9) Uani 1 1 d . . . . .
H22 H 0.2358 -0.1317 -0.2510 0.039 Uiso 1 1 calc R U . . .
C8 C 0.0733(2) 0.33321(14) -0.0523(3) 0.0207(7) Uani 1 1 d . . . . .
C16 C 0.2633(3) 0.42279(15) 0.3520(3) 0.0279(8) Uani 1 1 d . . . . .
C1 C 0.3101(2) 0.36866(14) -0.0725(3) 0.0212(7) Uani 1 1 d . . . . .
H1A H 0.3397 0.4041 -0.0753 0.025 Uiso 1 1 calc R U . . .
H1B H 0.2963 0.3535 -0.1578 0.025 Uiso 1 1 calc R U . . .
B1 B 0.2627(3) -0.07717(16) 0.2394(4) 0.0193(8) Uani 1 1 d . . . . .
C15 C 0.2594(3) 0.48424(16) 0.3260(4) 0.0381(11) Uani 1 1 d . . . . .
H15A H 0.2119 0.5015 0.3633 0.046 Uiso 1 1 calc R U . . .
H15B H 0.3196 0.5012 0.3612 0.046 Uiso 1 1 calc R U . . .
C34 C 0.5183(3) 0.02632(17) 0.3162(4) 0.0315(9) Uani 1 1 d . . . . .
H34 H 0.5727 0.0474 0.3274 0.038 Uiso 1 1 calc R U . . .
C11 C -0.0038(3) 0.3093(2) 0.2170(4) 0.0389(10) Uani 1 1 d . . . . .
H11A H 0.0493 0.2997 0.2833 0.058 Uiso 1 1 calc R U . . .
H11B H -0.0592 0.2922 0.2331 0.058 Uiso 1 1 calc R U . . .
H11C H -0.0118 0.3484 0.2151 0.058 Uiso 1 1 calc R U . . .
C12 C 0.0282(3) 0.22927(16) 0.0887(4) 0.0349(10) Uani 1 1 d . . . . .
H12A H 0.0369 0.2187 0.0062 0.052 Uiso 1 1 calc R U . . .
H12B H -0.0253 0.2105 0.1062 0.052 Uiso 1 1 calc R U . . .
H12C H 0.0831 0.2198 0.1522 0.052 Uiso 1 1 calc R U . . .
C39 C 0.3083(3) -0.18006(17) 0.5258(4) 0.0305(9) Uani 1 1 d . . . . .
H39 H 0.3291 -0.1783 0.6139 0.037 Uiso 1 1 calc R U . . .
C35 C 0.5227(3) -0.02769(18) 0.3513(4) 0.0378(10) Uani 1 1 d . . . . .
H35 H 0.5805 -0.0436 0.3869 0.045 Uiso 1 1 calc R U . . .
C17 C 0.1900(4) 0.40455(19) 0.4191(5) 0.0462(12) Uani 1 1 d . . . . .
H17A H 0.1294 0.4161 0.3719 0.069 Uiso 1 1 calc R U . . .
H17B H 0.2019 0.4205 0.5027 0.069 Uiso 1 1 calc R U . . .
H17C H 0.1912 0.3653 0.4261 0.069 Uiso 1 1 calc R U . . .
C18 C 0.3602(3) 0.40578(17) 0.4198(4) 0.0378(10) Uani 1 1 d . . . . .
H18A H 0.3622 0.3667 0.4301 0.057 Uiso 1 1 calc R U . . .
H18B H 0.3758 0.4230 0.5019 0.057 Uiso 1 1 calc R U . . .
H18C H 0.4045 0.4167 0.3707 0.057 Uiso 1 1 calc R U . . .
C36 C 0.4428(3) -0.05817(16) 0.3341(4) 0.0318(9) Uani 1 1 d . . . . .
H36 H 0.4480 -0.0946 0.3600 0.038 Uiso 1 1 calc R U . . .
C9 C -0.0646(3) 0.30810(19) -0.0220(4) 0.0349(10) Uani 1 1 d . . . . .
H9A H -0.1054 0.2776 -0.0549 0.042 Uiso 1 1 calc R U . . .
H9B H -0.1021 0.3373 0.0023 0.042 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 N3 2.020(3) . ?
Ni1 N1 2.033(3) . ?
Ni1 N2 2.052(3) . ?
Ni1 N4 2.279(3) . ?
Ni1 Cl1 2.3264(12) . ?
N4 C1 1.492(4) . ?
N4 C7 1.497(4) . ?
N4 C13 1.497(4) . ?
O3 C14 1.348(4) . ?
O3 C15 1.481(5) . ?
N3 C14 1.277(5) . ?
N3 C16 1.509(5) . ?
O1 C2 1.331(4) . ?
O1 C3 1.481(4) . ?
O2 C8 1.343(4) . ?
O2 C9 1.481(5) . ?
N2 C8 1.284(5) . ?
N2 C10 1.513(4) . ?
N1 C2 1.280(5) . ?
N1 C4 1.507(4) . ?
C27 C28 1.397(6) . ?
C27 C26 1.411(5) . ?
C27 H27 0.9500 . ?
C28 C29 1.388(6) . ?
C28 H28 0.9500 . ?
C4 C5 1.529(5) . ?
C4 C6 1.536(5) . ?
C4 C3 1.551(5) . ?
C13 C14 1.505(5) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C25 C30 1.404(5) . ?
C25 C26 1.418(5) . ?
C25 B1 1.670(5) . ?
C19 C24 1.411(5) . ?
C19 C20 1.422(5) . ?
C19 B1 1.669(5) . ?
C29 C30 1.405(5) . ?
C29 H29 0.9500 . ?
C7 C8 1.499(5) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C31 C36 1.410(5) . ?
C31 C32 1.411(5) . ?
C31 B1 1.662(5) . ?
C32 C33 1.414(5) . ?
C32 H32 0.9500 . ?
C23 C22 1.393(6) . ?
C23 C24 1.407(6) . ?
C23 H23 0.9500 . ?
C37 C38 1.412(5) . ?
C37 C42 1.416(5) . ?
C37 B1 1.654(5) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C26 H26 0.9500 . ?
C40 C39 1.397(6) . ?
C40 C41 1.398(6) . ?
C40 H40 0.9500 . ?
C41 C42 1.405(5) . ?
C41 H41 0.9500 . ?
C20 C21 1.392(5) . ?
C20 H20 0.9500 . ?
C24 H24 0.9500 . ?
C42 H42 0.9500 . ?
C38 C39 1.406(5) . ?
C38 H38 0.9500 . ?
C21 C22 1.397(6) . ?
C21 H21 0.9500 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C2 C1 1.514(5) . ?
C33 C34 1.381(6) . ?
C33 H33 0.9500 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C30 H30 0.9500 . ?
C10 C11 1.532(6) . ?
C10 C12 1.537(6) . ?
C10 C9 1.558(6) . ?
C22 H22 0.9500 . ?
C16 C17 1.517(6) . ?
C16 C18 1.531(6) . ?
C16 C15 1.557(6) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C34 C35 1.398(6) . ?
C34 H34 0.9500 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C39 H39 0.9500 . ?
C35 C36 1.390(6) . ?
C35 H35 0.9500 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C36 H36 0.9500 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Ni1 N1 103.39(12) . . ?
N3 Ni1 N2 104.96(12) . . ?
N1 Ni1 N2 140.50(12) . . ?
N3 Ni1 N4 79.97(12) . . ?
N1 Ni1 N4 80.23(11) . . ?
N2 Ni1 N4 78.28(11) . . ?
N3 Ni1 Cl1 104.10(10) . . ?
N1 Ni1 Cl1 99.07(9) . . ?
N2 Ni1 Cl1 100.05(9) . . ?
N4 Ni1 Cl1 175.91(8) . . ?
C1 N4 C7 112.2(3) . . ?
C1 N4 C13 112.7(3) . . ?
C7 N4 C13 109.9(3) . . ?
C1 N4 Ni1 108.4(2) . . ?
C7 N4 Ni1 106.4(2) . . ?
C13 N4 Ni1 107.0(2) . . ?
C14 O3 C15 105.2(3) . . ?
C14 N3 C16 108.1(3) . . ?
C14 N3 Ni1 116.3(2) . . ?
C16 N3 Ni1 135.6(2) . . ?
C2 O1 C3 105.0(3) . . ?
C8 O2 C9 105.0(3) . . ?
C8 N2 C10 107.3(3) . . ?
C8 N2 Ni1 115.7(2) . . ?
C10 N2 Ni1 136.3(2) . . ?
C2 N1 C4 107.0(3) . . ?
C2 N1 Ni1 116.0(2) . . ?
C4 N1 Ni1 136.2(2) . . ?
C28 C27 C26 120.1(4) . . ?
C28 C27 H27 120.0 . . ?
C26 C27 H27 120.0 . . ?
C29 C28 C27 119.0(4) . . ?
C29 C28 H28 120.5 . . ?
C27 C28 H28 120.5 . . ?
N1 C4 C5 110.5(3) . . ?
N1 C4 C6 109.2(3) . . ?
C5 C4 C6 112.1(3) . . ?
N1 C4 C3 102.1(3) . . ?
C5 C4 C3 111.0(3) . . ?
C6 C4 C3 111.4(3) . . ?
N4 C13 C14 109.9(3) . . ?
N4 C13 H13A 109.7 . . ?
C14 C13 H13A 109.7 . . ?
N4 C13 H13B 109.7 . . ?
C14 C13 H13B 109.7 . . ?
H13A C13 H13B 108.2 . . ?
C30 C25 C26 114.9(3) . . ?
C30 C25 B1 123.1(3) . . ?
C26 C25 B1 122.0(3) . . ?
C24 C19 C20 115.3(3) . . ?
C24 C19 B1 122.1(3) . . ?
C20 C19 B1 122.5(3) . . ?
C28 C29 C30 120.0(4) . . ?
C28 C29 H29 120.0 . . ?
C30 C29 H29 120.0 . . ?
N4 C7 C8 108.2(3) . . ?
N4 C7 H7A 110.1 . . ?
C8 C7 H7A 110.1 . . ?
N4 C7 H7B 110.1 . . ?
C8 C7 H7B 110.1 . . ?
H7A C7 H7B 108.4 . . ?
C36 C31 C32 114.5(3) . . ?
C36 C31 B1 122.8(3) . . ?
C32 C31 B1 122.1(3) . . ?
C31 C32 C33 122.7(3) . . ?
C31 C32 H32 118.7 . . ?
C33 C32 H32 118.7 . . ?
C22 C23 C24 120.5(4) . . ?
C22 C23 H23 119.7 . . ?
C24 C23 H23 119.7 . . ?
N3 C14 O3 119.2(3) . . ?
N3 C14 C13 124.2(3) . . ?
O3 C14 C13 116.6(3) . . ?
C38 C37 C42 115.1(3) . . ?
C38 C37 B1 122.6(3) . . ?
C42 C37 B1 122.2(3) . . ?
O1 C3 C4 104.9(3) . . ?
O1 C3 H3A 110.8 . . ?
C4 C3 H3A 110.8 . . ?
O1 C3 H3B 110.8 . . ?
C4 C3 H3B 110.8 . . ?
H3A C3 H3B 108.8 . . ?
C27 C26 C25 122.5(4) . . ?
C27 C26 H26 118.8 . . ?
C25 C26 H26 118.8 . . ?
C39 C40 C41 118.6(4) . . ?
C39 C40 H40 120.7 . . ?
C41 C40 H40 120.7 . . ?
C40 C41 C42 120.0(4) . . ?
C40 C41 H41 120.0 . . ?
C42 C41 H41 120.0 . . ?
C21 C20 C19 122.7(4) . . ?
C21 C20 H20 118.6 . . ?
C19 C20 H20 118.6 . . ?
C23 C24 C19 122.2(4) . . ?
C23 C24 H24 118.9 . . ?
C19 C24 H24 118.9 . . ?
C41 C42 C37 123.0(4) . . ?
C41 C42 H42 118.5 . . ?
C37 C42 H42 118.5 . . ?
C39 C38 C37 122.5(4) . . ?
C39 C38 H38 118.7 . . ?
C37 C38 H38 118.7 . . ?
C20 C21 C22 120.4(4) . . ?
C20 C21 H21 119.8 . . ?
C22 C21 H21 119.8 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N1 C2 O1 120.0(3) . . ?
N1 C2 C1 124.8(3) . . ?
O1 C2 C1 115.2(3) . . ?
C34 C33 C32 120.4(4) . . ?
C34 C33 H33 119.8 . . ?
C32 C33 H33 119.8 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C25 C30 C29 123.4(4) . . ?
C25 C30 H30 118.3 . . ?
C29 C30 H30 118.3 . . ?
N2 C10 C11 110.7(3) . . ?
N2 C10 C12 107.7(3) . . ?
C11 C10 C12 112.2(4) . . ?
N2 C10 C9 101.2(3) . . ?
C11 C10 C9 113.4(3) . . ?
C12 C10 C9 111.0(3) . . ?
C23 C22 C21 118.7(4) . . ?
C23 C22 H22 120.6 . . ?
C21 C22 H22 120.6 . . ?
N2 C8 O2 119.0(3) . . ?
N2 C8 C7 123.4(3) . . ?
O2 C8 C7 117.5(3) . . ?
N3 C16 C17 109.4(3) . . ?
N3 C16 C18 109.0(3) . . ?
C17 C16 C18 112.6(4) . . ?
N3 C16 C15 101.9(3) . . ?
C17 C16 C15 112.5(4) . . ?
C18 C16 C15 110.8(3) . . ?
N4 C1 C2 110.3(3) . . ?
N4 C1 H1A 109.6 . . ?
C2 C1 H1A 109.6 . . ?
N4 C1 H1B 109.6 . . ?
C2 C1 H1B 109.6 . . ?
H1A C1 H1B 108.1 . . ?
C37 B1 C31 111.5(3) . . ?
C37 B1 C19 109.2(3) . . ?
C31 B1 C19 106.4(3) . . ?
C37 B1 C25 108.6(3) . . ?
C31 B1 C25 111.1(3) . . ?
C19 B1 C25 110.0(3) . . ?
O3 C15 C16 105.5(3) . . ?
O3 C15 H15A 110.6 . . ?
C16 C15 H15A 110.6 . . ?
O3 C15 H15B 110.6 . . ?
C16 C15 H15B 110.6 . . ?
H15A C15 H15B 108.8 . . ?
C33 C34 C35 118.7(4) . . ?
C33 C34 H34 120.7 . . ?
C35 C34 H34 120.7 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C40 C39 C38 120.6(4) . . ?
C40 C39 H39 119.7 . . ?
C38 C39 H39 119.7 . . ?
C36 C35 C34 120.2(4) . . ?
C36 C35 H35 119.9 . . ?
C34 C35 H35 119.9 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C35 C36 C31 123.7(4) . . ?
C35 C36 H36 118.2 . . ?
C31 C36 H36 118.2 . . ?
O2 C9 C10 104.4(3) . . ?
O2 C9 H9A 110.9 . . ?
C10 C9 H9A 110.9 . . ?
O2 C9 H9B 110.9 . . ?
C10 C9 H9B 110.9 . . ?
H9A C9 H9B 108.9 . . ?

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
C26 C27 C28 C29 0.4(6) . . . . ?
C2 N1 C4 C5 125.7(3) . . . . ?
Ni1 N1 C4 C5 -65.3(4) . . . . ?
C2 N1 C4 C6 -110.6(3) . . . . ?
Ni1 N1 C4 C6 58.4(4) . . . . ?
C2 N1 C4 C3 7.5(3) . . . . ?
Ni1 N1 C4 C3 176.5(3) . . . . ?
C1 N4 C13 C14 -102.6(3) . . . . ?
C7 N4 C13 C14 131.5(3) . . . . ?
Ni1 N4 C13 C14 16.5(3) . . . . ?
C27 C28 C29 C30 0.6(6) . . . . ?
C1 N4 C7 C8 147.1(3) . . . . ?
C13 N4 C7 C8 -86.8(3) . . . . ?
Ni1 N4 C7 C8 28.7(3) . . . . ?
C36 C31 C32 C33 1.3(5) . . . . ?
B1 C31 C32 C33 -169.9(3) . . . . ?
C16 N3 C14 O3 0.0(4) . . . . ?
Ni1 N3 C14 O3 179.6(2) . . . . ?
C16 N3 C14 C13 -179.3(3) . . . . ?
Ni1 N3 C14 C13 0.3(5) . . . . ?
C15 O3 C14 N3 1.0(4) . . . . ?
C15 O3 C14 C13 -179.6(3) . . . . ?
N4 C13 C14 N3 -12.9(5) . . . . ?
N4 C13 C14 O3 167.8(3) . . . . ?
C2 O1 C3 C4 8.1(3) . . . . ?
N1 C4 C3 O1 -9.3(3) . . . . ?
C5 C4 C3 O1 -127.2(3) . . . . ?
C6 C4 C3 O1 107.1(3) . . . . ?
C28 C27 C26 C25 -0.5(6) . . . . ?
C30 C25 C26 C27 -0.2(5) . . . . ?
B1 C25 C26 C27 179.0(3) . . . . ?
C39 C40 C41 C42 -0.8(6) . . . . ?
C24 C19 C20 C21 -1.2(5) . . . . ?
B1 C19 C20 C21 -178.1(3) . . . . ?
C22 C23 C24 C19 2.1(6) . . . . ?
C20 C19 C24 C23 0.0(5) . . . . ?
B1 C19 C24 C23 176.9(3) . . . . ?
C40 C41 C42 C37 0.4(6) . . . . ?
C38 C37 C42 C41 0.1(5) . . . . ?
B1 C37 C42 C41 -176.3(3) . . . . ?
C42 C37 C38 C39 -0.3(5) . . . . ?
B1 C37 C38 C39 176.1(3) . . . . ?
C19 C20 C21 C22 0.2(6) . . . . ?
C4 N1 C2 O1 -2.7(4) . . . . ?
Ni1 N1 C2 O1 -174.3(2) . . . . ?
C4 N1 C2 C1 177.7(3) . . . . ?
Ni1 N1 C2 C1 6.1(4) . . . . ?
C3 O1 C2 N1 -3.7(4) . . . . ?
C3 O1 C2 C1 175.9(3) . . . . ?
C31 C32 C33 C34 -0.4(6) . . . . ?
C26 C25 C30 C29 1.2(5) . . . . ?
B1 C25 C30 C29 -178.1(3) . . . . ?
C28 C29 C30 C25 -1.4(6) . . . . ?
C8 N2 C10 C11 -134.1(3) . . . . ?
Ni1 N2 C10 C11 56.0(5) . . . . ?
C8 N2 C10 C12 102.9(3) . . . . ?
Ni1 N2 C10 C12 -67.0(4) . . . . ?
C8 N2 C10 C9 -13.7(4) . . . . ?
Ni1 N2 C10 C9 176.4(3) . . . . ?
C24 C23 C22 C21 -3.1(6) . . . . ?
C20 C21 C22 C23 2.0(6) . . . . ?
C10 N2 C8 O2 4.9(4) . . . . ?
Ni1 N2 C8 O2 177.2(2) . . . . ?
C10 N2 C8 C7 -171.0(3) . . . . ?
Ni1 N2 C8 C7 1.2(4) . . . . ?
C9 O2 C8 N2 7.0(4) . . . . ?
C9 O2 C8 C7 -176.9(3) . . . . ?
N4 C7 C8 N2 -22.6(5) . . . . ?
N4 C7 C8 O2 161.5(3) . . . . ?
C14 N3 C16 C17 118.4(4) . . . . ?
Ni1 N3 C16 C17 -61.1(5) . . . . ?
C14 N3 C16 C18 -118.1(4) . . . . ?
Ni1 N3 C16 C18 62.4(5) . . . . ?
C14 N3 C16 C15 -0.9(4) . . . . ?
Ni1 N3 C16 C15 179.6(3) . . . . ?
C7 N4 C1 C2 -117.8(3) . . . . ?
C13 N4 C1 C2 117.6(3) . . . . ?
Ni1 N4 C1 C2 -0.6(3) . . . . ?
N1 C2 C1 N4 -3.5(5) . . . . ?
O1 C2 C1 N4 176.9(3) . . . . ?
C38 C37 B1 C31 47.2(4) . . . . ?
C42 C37 B1 C31 -136.6(3) . . . . ?
C38 C37 B1 C19 164.5(3) . . . . ?
C42 C37 B1 C19 -19.3(4) . . . . ?
C38 C37 B1 C25 -75.5(4) . . . . ?
C42 C37 B1 C25 100.7(4) . . . . ?
C36 C31 B1 C37 26.4(5) . . . . ?
C32 C31 B1 C37 -163.1(3) . . . . ?
C36 C31 B1 C19 -92.5(4) . . . . ?
C32 C31 B1 C19 77.9(4) . . . . ?
C36 C31 B1 C25 147.8(4) . . . . ?
C32 C31 B1 C25 -41.8(4) . . . . ?
C24 C19 B1 C37 -89.5(4) . . . . ?
C20 C19 B1 C37 87.2(4) . . . . ?
C24 C19 B1 C31 30.9(4) . . . . ?
C20 C19 B1 C31 -152.3(3) . . . . ?
C24 C19 B1 C25 151.3(3) . . . . ?
C20 C19 B1 C25 -31.9(4) . . . . ?
C30 C25 B1 C37 20.2(4) . . . . ?
C26 C25 B1 C37 -158.9(3) . . . . ?
C30 C25 B1 C31 -102.8(4) . . . . ?
C26 C25 B1 C31 78.1(4) . . . . ?
C30 C25 B1 C19 139.7(3) . . . . ?
C26 C25 B1 C19 -39.5(4) . . . . ?
C14 O3 C15 C16 -1.4(4) . . . . ?
N3 C16 C15 O3 1.4(4) . . . . ?
C17 C16 C15 O3 -115.7(4) . . . . ?
C18 C16 C15 O3 117.3(4) . . . . ?
C32 C33 C34 C35 -0.4(6) . . . . ?
C41 C40 C39 C38 0.6(6) . . . . ?
C37 C38 C39 C40 -0.1(6) . . . . ?
C33 C34 C35 C36 0.2(7) . . . . ?
C34 C35 C36 C31 0.9(7) . . . . ?
C32 C31 C36 C35 -1.5(6) . . . . ?
B1 C31 C36 C35 169.6(4) . . . . ?
C8 O2 C9 C10 -15.0(4) . . . . ?
N2 C10 C9 O2 17.1(4) . . . . ?
C11 C10 C9 O2 135.6(4) . . . . ?
C12 C10 C9 O2 -97.0(4) . . . . ?

_refine_diff_density_max         1.645
_refine_diff_density_min         -0.709
_refine_diff_density_rms         0.097

####################################################################### 
# 
# 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_shelx_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1983782'
loop_
_audit_author_name
_audit_author_address
'Shiro Hikichi'
;Kanagawa University
Japan
;
_audit_update_record             
;
2020-02-13 deposited with the CCDC.	2020-04-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        '[Ni(s-TOABu)(Cl)](BPh4)'
_chemical_name_common            
'[Chloridotris{((S)-4-tert-butyloxazolin-2-yl)methyl}aminenickel(II)]tetraphenylborate'
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H42 Cl N4 Ni O3, C24 H20 B'
_chemical_formula_sum            'C48 H62 B Cl N4 Ni O3'
_chemical_formula_weight         847.98
_chemical_absolute_configuration rmad

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'
Cl Cl 0.1484 0.1585 '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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

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

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

_cell_length_a                   12.0793(6)
_cell_length_b                   13.4525(5)
_cell_length_c                   15.1350(6)
_cell_angle_alpha                90
_cell_angle_beta                 111.020(2)
_cell_angle_gamma                90
_cell_volume                     2295.73(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    5969
_cell_measurement_theta_min      1.4414
_cell_measurement_theta_max      27.4810

_exptl_crystal_description       Block
_exptl_crystal_colour            Red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_F_000             904
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.525
_shelx_estimated_absorpt_T_min   0.818
_shelx_estimated_absorpt_T_max   0.902
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_correction_T_max  0.9121
_exptl_absorpt_correction_T_min  0.8241
_exptl_absorpt_process_details   
;Numerical (Based on real shape of the crystal) absorption
correction was parformed on CrystalClear (Rigaku Inc., 2008)
with NUMABS (Rigaku, 1999) method.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      133(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  ?
_diffrn_reflns_av_unetI/netI     0.0510
_diffrn_reflns_av_R_equivalents  0.0179
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.441

_diffrn_measured_fraction_theta_max 0.978
_diffrn_measured_fraction_theta_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.874
_diffrn_reflns_point_group_measured_fraction_full 0.874
_reflns_number_total             9223
_reflns_number_gt                7510
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.714
_reflns_Friedel_fraction_max     0.761
_reflns_Friedel_fraction_full    0.761

_diffrn_special_details          
;
 ?
;

_diffrn_source_power             3.0000
_diffrn_source_voltage           50.0000
_diffrn_source_current           60.0000

_diffrn_radiation_source         'Rotating Anode'

_diffrn_radiation_detector       CCD
_diffrn_measurement_device       
;
Saturn70 (2x2 bin mode)
;
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measurement_method       dtprofit.ref
_diffrn_reflns_number            20428
_diffrn_number_total             5393
_diffrn_reflns_av_sigmaI/detI    0.0752
_diffrn_reflns_theta_full        27.4810
_diffrn_reflns_theta_max         27.4810
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_measurement_details      
;
scan:
	Number of images: 600
	           Slice: -115.0000 - 65.0000
	     Image width: 0.3000
	        Exp time: 8.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 0.0000
	             XTD: 54.8375
	          2theta: -25.1501
scan:
	Number of images: 600
	           Slice: -115.0000 - 65.0000
	     Image width: 0.3000
	        Exp time: 8.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 90.0000
	             XTD: 54.8375
	          2theta: -25.1501
scan:
	Number of images: 600
	           Slice: -115.0000 - 65.0000
	     Image width: 0.3000
	        Exp time: 8.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 180.0000
	             XTD: 54.8375
	          2theta: -25.1501

;
_diffrn_measurement_device_details 
;
AFC10: Fixed Chi 2 circle
;
_diffrn_orient_matrix_UB_11      -0.0596
_diffrn_orient_matrix_UB_12      -0.0643
_diffrn_orient_matrix_UB_13      -0.0136
_diffrn_orient_matrix_UB_21      -0.0052
_diffrn_orient_matrix_UB_22      -0.0107
_diffrn_orient_matrix_UB_23      0.0734
_diffrn_orient_matrix_UB_31      -0.0658
_diffrn_orient_matrix_UB_32      0.0261
_diffrn_orient_matrix_UB_33      -0.0009
_diffrn_orient_matrix_type       d*Trek


_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       'CrystalClear (Rigaku Inc., 2007)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        
'CrystalClear (Rigaku Inc., 2007), SORTAV (Blessing, 1995)'
_computing_structure_solution    'SIR92 (Altomare et al, 1994)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0155P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2737 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.008(3)
_refine_ls_number_reflns         9223
_refine_ls_number_parameters     532
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0246
_refine_ls_R_factor_gt           0.0214
_refine_ls_wR_factor_ref         0.0443
_refine_ls_wR_factor_gt          0.0438
_refine_ls_goodness_of_fit_ref   0.892
_refine_ls_restrained_S_all      0.892
_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 0.90625(2) 0.57674(2) 0.80449(2) 0.01900(6) Uani 1 1 d . . . . .
Cl1 Cl 0.98885(5) 0.62473(4) 0.95669(3) 0.02834(13) Uani 1 1 d . . . . .
O1 O 0.68966(13) 0.78000(11) 0.62850(10) 0.0315(4) Uani 1 1 d . . . . .
O2 O 1.13343(13) 0.48435(11) 0.67963(10) 0.0331(4) Uani 1 1 d . . . . .
O3 O 0.70775(14) 0.32483(11) 0.73641(11) 0.0365(4) Uani 1 1 d . . . . .
N4 N 0.82943(15) 0.53689(12) 0.65204(11) 0.0211(4) Uani 1 1 d . . . . .
N2 N 1.04046(14) 0.49951(12) 0.78340(12) 0.0204(4) Uani 1 1 d . . . . .
N3 N 0.79268(14) 0.46667(13) 0.80598(12) 0.0239(4) Uani 1 1 d . . . . .
C25 C 0.50542(16) 0.57951(18) 0.20911(13) 0.0231(4) Uani 1 1 d . . . . .
C2 C 0.76024(18) 0.70309(16) 0.66333(15) 0.0216(5) Uani 1 1 d . . . . .
N1 N 0.84499(15) 0.71168(12) 0.74255(11) 0.0203(4) Uani 1 1 d . . . . .
C26 C 0.54933(18) 0.63053(16) 0.14801(14) 0.0267(5) Uani 1 1 d . . . . .
H26 H 0.6317 0.6452 0.1690 0.032 Uiso 1 1 calc R U . . .
C20 C 0.7450(2) 0.42226(17) 0.87488(17) 0.0317(5) Uani 1 1 d . . . . .
H20 H 0.8091 0.4194 0.9388 0.038 Uiso 1 1 calc R U . . .
C10 C 1.03802(19) 0.50845(14) 0.69884(15) 0.0224(5) Uani 1 1 d . . . . .
C43 C 0.63485(19) 0.42471(16) 0.30295(15) 0.0252(5) Uani 1 1 d . . . . .
C15 C 1.0851(2) 0.37233(16) 0.95720(15) 0.0319(6) Uani 1 1 d . . . . .
H15A H 1.0045 0.3956 0.9216 0.048 Uiso 1 1 calc R U . . .
H15B H 1.1261 0.4214 1.0058 0.048 Uiso 1 1 calc R U . . .
H15C H 1.0813 0.3087 0.9875 0.048 Uiso 1 1 calc R U . . .
C3 C 0.7249(2) 0.85410(17) 0.70520(16) 0.0327(6) Uani 1 1 d . . . . .
H3A H 0.6677 0.8558 0.7384 0.039 Uiso 1 1 calc R U . . .
H3B H 0.7303 0.9213 0.6803 0.039 Uiso 1 1 calc R U . . .
C41 C 0.9192(2) 0.65109(19) 0.39604(16) 0.0368(6) Uani 1 1 d . . . . .
H41 H 0.9953 0.6294 0.3991 0.044 Uiso 1 1 calc R U . . .
C29 C 0.30913(18) 0.59100(17) 0.08271(14) 0.0282(5) Uani 1 1 d . . . . .
H29 H 0.2265 0.5772 0.0612 0.034 Uiso 1 1 calc R U . . .
C17 C 0.78671(19) 0.43334(15) 0.64641(15) 0.0247(5) Uani 1 1 d . . . . .
H17A H 0.8474 0.3872 0.6402 0.030 Uiso 1 1 calc R U . . .
H17B H 0.7133 0.4252 0.5903 0.030 Uiso 1 1 calc R U . . .
C34 C 0.3953(2) 0.5453(2) 0.51739(17) 0.0432(7) Uani 1 1 d . . . . .
H34 H 0.3569 0.5484 0.5622 0.052 Uiso 1 1 calc R U . . .
C16 C 1.2800(2) 0.32867(19) 0.94811(18) 0.0490(7) Uani 1 1 d . . . . .
H16A H 1.2796 0.2668 0.9822 0.074 Uiso 1 1 calc R U . . .
H16B H 1.3180 0.3813 0.9936 0.074 Uiso 1 1 calc R U . . .
H16C H 1.3241 0.3185 0.9057 0.074 Uiso 1 1 calc R U . . .
C9 C 0.93118(18) 0.54600(16) 0.62026(13) 0.0264(5) Uani 1 1 d . . . . .
H9A H 0.9426 0.6163 0.6061 0.032 Uiso 1 1 calc R U . . .
H9B H 0.9172 0.5062 0.5622 0.032 Uiso 1 1 calc R U . . .
C31 C 0.51681(18) 0.53807(16) 0.38701(14) 0.0256(5) Uani 1 1 d . . . . .
C1 C 0.73358(18) 0.60865(15) 0.60715(14) 0.0275(5) Uani 1 1 d . . . . .
H1A H 0.6568 0.5811 0.6054 0.033 Uiso 1 1 calc R U . . .
H1B H 0.7280 0.6219 0.5413 0.033 Uiso 1 1 calc R U . . .
C11 C 1.2228(2) 0.45451(19) 0.77074(17) 0.0407(6) Uani 1 1 d . . . . .
H11A H 1.2912 0.5007 0.7895 0.049 Uiso 1 1 calc R U . . .
H11B H 1.2518 0.3864 0.7669 0.049 Uiso 1 1 calc R U . . .
C28 C 0.35692(19) 0.64082(16) 0.02487(15) 0.0292(5) Uani 1 1 d . . . . .
H28 H 0.3076 0.6612 -0.0368 0.035 Uiso 1 1 calc R U . . .
C12 C 1.15837(17) 0.45891(15) 0.84187(15) 0.0250(5) Uani 1 1 d . . . . .
H12 H 1.1997 0.5085 0.8921 0.030 Uiso 1 1 calc R U . . .
C37 C 0.70773(18) 0.61339(16) 0.35479(13) 0.0241(5) Uani 1 1 d . . . . .
C48 C 0.7207(2) 0.37577(18) 0.37835(17) 0.0321(6) Uani 1 1 d . . . . .
H48 H 0.7574 0.4117 0.4355 0.039 Uiso 1 1 calc R U . . .
C4 C 0.84723(19) 0.81792(15) 0.77154(15) 0.0256(5) Uani 1 1 d . . . . .
H4 H 0.8507 0.8212 0.8385 0.031 Uiso 1 1 calc R U . . .
C32 C 0.45103(19) 0.62079(18) 0.39546(16) 0.0352(6) Uani 1 1 d . . . . .
H32 H 0.4463 0.6764 0.3556 0.042 Uiso 1 1 calc R U . . .
C47 C 0.7555(2) 0.27853(18) 0.37473(18) 0.0408(6) Uani 1 1 d . . . . .
H47 H 0.8136 0.2491 0.4285 0.049 Uiso 1 1 calc R U . . .
C13 C 1.15229(19) 0.35886(16) 0.89005(15) 0.0275(5) Uani 1 1 d . . . . .
C5 C 0.9540(2) 0.87432(17) 0.76317(15) 0.0319(6) Uani 1 1 d . . . . .
C27 C 0.47692(19) 0.66066(16) 0.05766(14) 0.0281(5) Uani 1 1 d . . . . .
H27 H 0.5104 0.6951 0.0184 0.034 Uiso 1 1 calc R U . . .
C14 C 1.0909(3) 0.27823(18) 0.81748(17) 0.0448(7) Uani 1 1 d . . . . .
H14A H 1.0923 0.2152 0.8503 0.067 Uiso 1 1 calc R U . . .
H14B H 1.1326 0.2703 0.7731 0.067 Uiso 1 1 calc R U . . .
H14C H 1.0085 0.2977 0.7827 0.067 Uiso 1 1 calc R U . . .
C18 C 0.76279(18) 0.41035(15) 0.73397(16) 0.0247(5) Uani 1 1 d . . . . .
C36 C 0.51418(18) 0.45806(17) 0.44512(14) 0.0279(5) Uani 1 1 d . . . . .
H36 H 0.5547 0.3987 0.4409 0.033 Uiso 1 1 calc R U . . .
C33 C 0.3922(2) 0.6255(2) 0.45950(17) 0.0443(7) Uani 1 1 d . . . . .
H33 H 0.3499 0.6839 0.4633 0.053 Uiso 1 1 calc R U . . .
C38 C 0.6979(2) 0.71106(17) 0.38444(15) 0.0318(5) Uani 1 1 d . . . . .
H38 H 0.6218 0.7342 0.3803 0.038 Uiso 1 1 calc R U . . .
C39 C 0.7943(2) 0.77566(19) 0.41970(16) 0.0377(6) Uani 1 1 d . . . . .
H39 H 0.7828 0.8409 0.4388 0.045 Uiso 1 1 calc R U . . .
C8 C 1.0698(2) 0.8237(2) 0.82491(18) 0.0462(7) Uani 1 1 d . . . . .
H8A H 1.0736 0.8215 0.8907 0.069 Uiso 1 1 calc R U . . .
H8B H 1.1375 0.8614 0.8215 0.069 Uiso 1 1 calc R U . . .
H8C H 1.0721 0.7559 0.8020 0.069 Uiso 1 1 calc R U . . .
C40 C 0.9053(2) 0.74504(19) 0.42678(15) 0.0388(7) Uani 1 1 d . . . . .
H40 H 0.9717 0.7879 0.4525 0.047 Uiso 1 1 calc R U . . .
C22 C 0.6785(2) 0.5895(2) 0.90850(18) 0.0494(7) Uani 1 1 d . . . . .
H22A H 0.6127 0.6272 0.9155 0.074 Uiso 1 1 calc R U . . .
H22B H 0.7022 0.6201 0.8592 0.074 Uiso 1 1 calc R U . . .
H22C H 0.7459 0.5898 0.9687 0.074 Uiso 1 1 calc R U . . .
C6 C 0.9484(2) 0.87674(19) 0.66044(17) 0.0462(7) Uani 1 1 d . . . . .
H6A H 1.0172 0.9128 0.6571 0.069 Uiso 1 1 calc R U . . .
H6B H 0.8754 0.9103 0.6209 0.069 Uiso 1 1 calc R U . . .
H6C H 0.9488 0.8086 0.6377 0.069 Uiso 1 1 calc R U . . .
C30 C 0.38283(18) 0.56111(16) 0.17285(14) 0.0266(5) Uani 1 1 d . . . . .
H30 H 0.3485 0.5267 0.2115 0.032 Uiso 1 1 calc R U . . .
C35 C 0.4549(2) 0.46117(19) 0.50900(16) 0.0359(6) Uani 1 1 d . . . . .
H35 H 0.4558 0.4047 0.5469 0.043 Uiso 1 1 calc R U . . .
C21 C 0.6392(2) 0.48273(19) 0.88070(19) 0.0410(6) Uani 1 1 d . . . . .
C44 C 0.5872(2) 0.36720(18) 0.22119(17) 0.0359(6) Uani 1 1 d . . . . .
H44 H 0.5291 0.3960 0.1670 0.043 Uiso 1 1 calc R U . . .
C45 C 0.6217(2) 0.2692(2) 0.21609(19) 0.0514(8) Uani 1 1 d . . . . .
H45 H 0.5871 0.2327 0.1590 0.062 Uiso 1 1 calc R U . . .
C19 C 0.7149(2) 0.31625(18) 0.83536(17) 0.0405(6) Uani 1 1 d . . . . .
H19A H 0.7777 0.2688 0.8710 0.049 Uiso 1 1 calc R U . . .
H19B H 0.6383 0.2939 0.8385 0.049 Uiso 1 1 calc R U . . .
C42 C 0.82201(17) 0.58763(19) 0.36053(13) 0.0303(5) Uani 1 1 d . . . . .
H42 H 0.8342 0.5236 0.3392 0.036 Uiso 1 1 calc R U . . .
B1 B 0.5917(2) 0.53869(18) 0.31347(16) 0.0242(6) Uani 1 1 d . . . . .
C46 C 0.7056(2) 0.22479(19) 0.2933(2) 0.0513(8) Uani 1 1 d . . . . .
H46 H 0.7285 0.1578 0.2899 0.062 Uiso 1 1 calc R U . . .
C23 C 0.5366(2) 0.4835(2) 0.7857(2) 0.0642(9) Uani 1 1 d . . . . .
H23A H 0.4726 0.5257 0.7901 0.096 Uiso 1 1 calc R U . . .
H23B H 0.5070 0.4156 0.7691 0.096 Uiso 1 1 calc R U . . .
H23C H 0.5641 0.5096 0.7367 0.096 Uiso 1 1 calc R U . . .
C7 C 0.9526(3) 0.98136(18) 0.79832(17) 0.0496(7) Uani 1 1 d . . . . .
H7A H 0.9575 0.9801 0.8644 0.074 Uiso 1 1 calc R U . . .
H7B H 0.8789 1.0142 0.7592 0.074 Uiso 1 1 calc R U . . .
H7C H 1.0205 1.0180 0.7938 0.074 Uiso 1 1 calc R U . . .
C24 C 0.6013(3) 0.4367(2) 0.9575(2) 0.0673(9) Uani 1 1 d . . . . .
H24A H 0.6681 0.4380 1.0180 0.101 Uiso 1 1 calc R U . . .
H24B H 0.5763 0.3678 0.9405 0.101 Uiso 1 1 calc R U . . .
H24C H 0.5350 0.4748 0.9632 0.101 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 N3 2.0241(17) . ?
Ni1 N2 2.0447(17) . ?
Ni1 N1 2.0553(16) . ?
Ni1 N4 2.2218(16) . ?
Ni1 Cl1 2.2517(5) . ?
O1 C2 1.324(2) . ?
O1 C3 1.472(3) . ?
O2 C10 1.326(2) . ?
O2 C11 1.470(3) . ?
O3 C18 1.336(2) . ?
O3 C19 1.473(3) . ?
N4 C1 1.473(2) . ?
N4 C9 1.477(3) . ?
N4 C17 1.477(2) . ?
N2 C10 1.275(2) . ?
N2 C12 1.485(2) . ?
N3 C18 1.269(3) . ?
N3 C20 1.485(3) . ?
C25 C26 1.400(3) . ?
C25 C30 1.404(3) . ?
C25 B1 1.644(3) . ?
C2 N1 1.272(2) . ?
C2 C1 1.498(3) . ?
N1 C4 1.492(3) . ?
C26 C27 1.393(3) . ?
C26 H26 0.9500 . ?
C20 C19 1.539(3) . ?
C20 C21 1.544(3) . ?
C20 H20 1.0000 . ?
C10 C9 1.495(3) . ?
C43 C44 1.396(3) . ?
C43 C48 1.401(3) . ?
C43 B1 1.646(3) . ?
C15 C13 1.522(3) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C3 C4 1.537(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C41 C40 1.378(3) . ?
C41 C42 1.394(3) . ?
C41 H41 0.9500 . ?
C29 C28 1.383(3) . ?
C29 C30 1.394(3) . ?
C29 H29 0.9500 . ?
C17 C18 1.487(3) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C34 C35 1.372(3) . ?
C34 C33 1.381(3) . ?
C34 H34 0.9500 . ?
C16 C13 1.531(3) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C31 C36 1.398(3) . ?
C31 C32 1.400(3) . ?
C31 B1 1.667(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C11 C12 1.540(3) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C28 C27 1.379(3) . ?
C28 H28 0.9500 . ?
C12 C13 1.545(3) . ?
C12 H12 1.0000 . ?
C37 C42 1.395(3) . ?
C37 C38 1.407(3) . ?
C37 B1 1.654(3) . ?
C48 C47 1.381(3) . ?
C48 H48 0.9500 . ?
C4 C5 1.541(3) . ?
C4 H4 1.0000 . ?
C32 C33 1.394(3) . ?
C32 H32 0.9500 . ?
C47 C46 1.369(3) . ?
C47 H47 0.9500 . ?
C13 C14 1.532(3) . ?
C5 C6 1.532(3) . ?
C5 C8 1.534(3) . ?
C5 C7 1.537(3) . ?
C27 H27 0.9500 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C36 C35 1.395(3) . ?
C36 H36 0.9500 . ?
C33 H33 0.9500 . ?
C38 C39 1.396(3) . ?
C38 H38 0.9500 . ?
C39 C40 1.370(3) . ?
C39 H39 0.9500 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C40 H40 0.9500 . ?
C22 C21 1.523(4) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C30 H30 0.9500 . ?
C35 H35 0.9500 . ?
C21 C24 1.525(3) . ?
C21 C23 1.525(4) . ?
C44 C45 1.393(3) . ?
C44 H44 0.9500 . ?
C45 C46 1.378(3) . ?
C45 H45 0.9500 . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C42 H42 0.9500 . ?
C46 H46 0.9500 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Ni1 N2 102.03(7) . . ?
N3 Ni1 N1 121.11(7) . . ?
N2 Ni1 N1 123.61(7) . . ?
N3 Ni1 N4 78.63(7) . . ?
N2 Ni1 N4 76.97(6) . . ?
N1 Ni1 N4 77.96(6) . . ?
N3 Ni1 Cl1 104.58(5) . . ?
N2 Ni1 Cl1 102.72(5) . . ?
N1 Ni1 Cl1 99.69(5) . . ?
N4 Ni1 Cl1 176.74(5) . . ?
C2 O1 C3 104.62(16) . . ?
C10 O2 C11 105.36(16) . . ?
C18 O3 C19 104.31(16) . . ?
C1 N4 C9 113.81(15) . . ?
C1 N4 C17 113.01(16) . . ?
C9 N4 C17 111.95(16) . . ?
C1 N4 Ni1 106.69(12) . . ?
C9 N4 Ni1 103.41(12) . . ?
C17 N4 Ni1 107.13(12) . . ?
C10 N2 C12 107.74(17) . . ?
C10 N2 Ni1 111.99(14) . . ?
C12 N2 Ni1 137.60(13) . . ?
C18 N3 C20 107.47(18) . . ?
C18 N3 Ni1 114.36(15) . . ?
C20 N3 Ni1 137.47(14) . . ?
C26 C25 C30 115.13(18) . . ?
C26 C25 B1 122.61(17) . . ?
C30 C25 B1 122.19(18) . . ?
N1 C2 O1 119.33(19) . . ?
N1 C2 C1 123.26(19) . . ?
O1 C2 C1 117.40(18) . . ?
C2 N1 C4 106.72(17) . . ?
C2 N1 Ni1 112.71(14) . . ?
C4 N1 Ni1 138.25(12) . . ?
C27 C26 C25 122.53(19) . . ?
C27 C26 H26 118.7 . . ?
C25 C26 H26 118.7 . . ?
N3 C20 C19 101.37(17) . . ?
N3 C20 C21 111.43(18) . . ?
C19 C20 C21 115.2(2) . . ?
N3 C20 H20 109.5 . . ?
C19 C20 H20 109.5 . . ?
C21 C20 H20 109.5 . . ?
N2 C10 O2 119.2(2) . . ?
N2 C10 C9 122.21(19) . . ?
O2 C10 C9 118.58(18) . . ?
C44 C43 C48 114.3(2) . . ?
C44 C43 B1 123.9(2) . . ?
C48 C43 B1 121.79(19) . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O1 C3 C4 103.84(16) . . ?
O1 C3 H3A 111.0 . . ?
C4 C3 H3A 111.0 . . ?
O1 C3 H3B 111.0 . . ?
C4 C3 H3B 111.0 . . ?
H3A C3 H3B 109.0 . . ?
C40 C41 C42 120.3(2) . . ?
C40 C41 H41 119.8 . . ?
C42 C41 H41 119.8 . . ?
C28 C29 C30 119.6(2) . . ?
C28 C29 H29 120.2 . . ?
C30 C29 H29 120.2 . . ?
N4 C17 C18 108.68(17) . . ?
N4 C17 H17A 110.0 . . ?
C18 C17 H17A 110.0 . . ?
N4 C17 H17B 110.0 . . ?
C18 C17 H17B 110.0 . . ?
H17A C17 H17B 108.3 . . ?
C35 C34 C33 118.8(2) . . ?
C35 C34 H34 120.6 . . ?
C33 C34 H34 120.6 . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N4 C9 C10 107.14(15) . . ?
N4 C9 H9A 110.3 . . ?
C10 C9 H9A 110.3 . . ?
N4 C9 H9B 110.3 . . ?
C10 C9 H9B 110.3 . . ?
H9A C9 H9B 108.5 . . ?
C36 C31 C32 114.4(2) . . ?
C36 C31 B1 124.36(19) . . ?
C32 C31 B1 121.25(19) . . ?
N4 C1 C2 108.70(15) . . ?
N4 C1 H1A 109.9 . . ?
C2 C1 H1A 109.9 . . ?
N4 C1 H1B 109.9 . . ?
C2 C1 H1B 109.9 . . ?
H1A C1 H1B 108.3 . . ?
O2 C11 C12 105.06(17) . . ?
O2 C11 H11A 110.7 . . ?
C12 C11 H11A 110.7 . . ?
O2 C11 H11B 110.7 . . ?
C12 C11 H11B 110.7 . . ?
H11A C11 H11B 108.8 . . ?
C27 C28 C29 119.3(2) . . ?
C27 C28 H28 120.3 . . ?
C29 C28 H28 120.3 . . ?
N2 C12 C11 102.41(16) . . ?
N2 C12 C13 113.81(17) . . ?
C11 C12 C13 114.72(18) . . ?
N2 C12 H12 108.5 . . ?
C11 C12 H12 108.5 . . ?
C13 C12 H12 108.5 . . ?
C42 C37 C38 114.0(2) . . ?
C42 C37 B1 123.91(19) . . ?
C38 C37 B1 122.03(19) . . ?
C47 C48 C43 124.0(2) . . ?
C47 C48 H48 118.0 . . ?
C43 C48 H48 118.0 . . ?
N1 C4 C3 101.50(16) . . ?
N1 C4 C5 112.01(17) . . ?
C3 C4 C5 115.29(18) . . ?
N1 C4 H4 109.2 . . ?
C3 C4 H4 109.2 . . ?
C5 C4 H4 109.2 . . ?
C33 C32 C31 123.2(2) . . ?
C33 C32 H32 118.4 . . ?
C31 C32 H32 118.4 . . ?
C46 C47 C48 119.6(2) . . ?
C46 C47 H47 120.2 . . ?
C48 C47 H47 120.2 . . ?
C15 C13 C16 108.50(19) . . ?
C15 C13 C14 109.0(2) . . ?
C16 C13 C14 110.6(2) . . ?
C15 C13 C12 109.78(17) . . ?
C16 C13 C12 107.05(19) . . ?
C14 C13 C12 111.78(18) . . ?
C6 C5 C8 109.1(2) . . ?
C6 C5 C7 109.23(19) . . ?
C8 C5 C7 109.0(2) . . ?
C6 C5 C4 111.11(19) . . ?
C8 C5 C4 109.77(18) . . ?
C7 C5 C4 108.6(2) . . ?
C28 C27 C26 120.4(2) . . ?
C28 C27 H27 119.8 . . ?
C26 C27 H27 119.8 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N3 C18 O3 118.8(2) . . ?
N3 C18 C17 123.72(19) . . ?
O3 C18 C17 117.49(18) . . ?
C35 C36 C31 123.1(2) . . ?
C35 C36 H36 118.4 . . ?
C31 C36 H36 118.4 . . ?
C34 C33 C32 120.1(2) . . ?
C34 C33 H33 120.0 . . ?
C32 C33 H33 120.0 . . ?
C39 C38 C37 123.3(2) . . ?
C39 C38 H38 118.4 . . ?
C37 C38 H38 118.4 . . ?
C40 C39 C38 120.1(2) . . ?
C40 C39 H39 119.9 . . ?
C38 C39 H39 119.9 . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C39 C40 C41 118.9(2) . . ?
C39 C40 H40 120.5 . . ?
C41 C40 H40 120.5 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C29 C30 C25 123.0(2) . . ?
C29 C30 H30 118.5 . . ?
C25 C30 H30 118.5 . . ?
C34 C35 C36 120.4(2) . . ?
C34 C35 H35 119.8 . . ?
C36 C35 H35 119.8 . . ?
C22 C21 C24 108.7(2) . . ?
C22 C21 C23 108.8(2) . . ?
C24 C21 C23 110.9(2) . . ?
C22 C21 C20 109.27(19) . . ?
C24 C21 C20 108.1(2) . . ?
C23 C21 C20 111.0(2) . . ?
C45 C44 C43 122.5(2) . . ?
C45 C44 H44 118.8 . . ?
C43 C44 H44 118.8 . . ?
C46 C45 C44 120.5(2) . . ?
C46 C45 H45 119.8 . . ?
C44 C45 H45 119.8 . . ?
O3 C19 C20 104.00(17) . . ?
O3 C19 H19A 111.0 . . ?
C20 C19 H19A 111.0 . . ?
O3 C19 H19B 111.0 . . ?
C20 C19 H19B 111.0 . . ?
H19A C19 H19B 109.0 . . ?
C41 C42 C37 123.3(2) . . ?
C41 C42 H42 118.3 . . ?
C37 C42 H42 118.3 . . ?
C25 B1 C43 109.39(17) . . ?
C25 B1 C37 108.63(17) . . ?
C43 B1 C37 110.34(17) . . ?
C25 B1 C31 109.55(17) . . ?
C43 B1 C31 109.06(17) . . ?
C37 B1 C31 109.86(16) . . ?
C47 C46 C45 119.1(2) . . ?
C47 C46 H46 120.4 . . ?
C45 C46 H46 120.4 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 O1 C2 N1 -7.9(3) . . . . ?
C3 O1 C2 C1 170.78(19) . . . . ?
O1 C2 N1 C4 -5.5(3) . . . . ?
C1 C2 N1 C4 175.86(19) . . . . ?
O1 C2 N1 Ni1 160.44(15) . . . . ?
C1 C2 N1 Ni1 -18.2(3) . . . . ?
C30 C25 C26 C27 -0.2(3) . . . . ?
B1 C25 C26 C27 176.7(2) . . . . ?
C18 N3 C20 C19 15.5(2) . . . . ?
Ni1 N3 C20 C19 -153.90(17) . . . . ?
C18 N3 C20 C21 -107.5(2) . . . . ?
Ni1 N3 C20 C21 83.1(2) . . . . ?
C12 N2 C10 O2 -1.4(2) . . . . ?
Ni1 N2 C10 O2 163.46(14) . . . . ?
C12 N2 C10 C9 179.02(18) . . . . ?
Ni1 N2 C10 C9 -16.1(2) . . . . ?
C11 O2 C10 N2 -1.7(2) . . . . ?
C11 O2 C10 C9 177.83(18) . . . . ?
C2 O1 C3 C4 17.0(2) . . . . ?
C1 N4 C17 C18 -93.3(2) . . . . ?
C9 N4 C17 C18 136.60(17) . . . . ?
Ni1 N4 C17 C18 23.91(19) . . . . ?
C1 N4 C9 C10 153.30(16) . . . . ?
C17 N4 C9 C10 -77.0(2) . . . . ?
Ni1 N4 C9 C10 37.96(16) . . . . ?
N2 C10 C9 N4 -17.9(3) . . . . ?
O2 C10 C9 N4 162.54(17) . . . . ?
C9 N4 C1 C2 -86.7(2) . . . . ?
C17 N4 C1 C2 144.14(17) . . . . ?
Ni1 N4 C1 C2 26.67(19) . . . . ?
N1 C2 C1 N4 -7.8(3) . . . . ?
O1 C2 C1 N4 173.55(17) . . . . ?
C10 O2 C11 C12 3.9(2) . . . . ?
C30 C29 C28 C27 -0.4(3) . . . . ?
C10 N2 C12 C11 3.7(2) . . . . ?
Ni1 N2 C12 C11 -155.27(17) . . . . ?
C10 N2 C12 C13 -120.70(19) . . . . ?
Ni1 N2 C12 C13 80.3(2) . . . . ?
O2 C11 C12 N2 -4.6(2) . . . . ?
O2 C11 C12 C13 119.25(19) . . . . ?
C44 C43 C48 C47 -1.1(4) . . . . ?
B1 C43 C48 C47 176.4(2) . . . . ?
C2 N1 C4 C3 15.6(2) . . . . ?
Ni1 N1 C4 C3 -144.81(17) . . . . ?
C2 N1 C4 C5 -108.0(2) . . . . ?
Ni1 N1 C4 C5 91.7(2) . . . . ?
O1 C3 C4 N1 -19.4(2) . . . . ?
O1 C3 C4 C5 101.9(2) . . . . ?
C36 C31 C32 C33 2.9(3) . . . . ?
B1 C31 C32 C33 -176.6(2) . . . . ?
C43 C48 C47 C46 0.7(4) . . . . ?
N2 C12 C13 C15 -61.6(2) . . . . ?
C11 C12 C13 C15 -179.07(18) . . . . ?
N2 C12 C13 C16 -179.15(18) . . . . ?
C11 C12 C13 C16 63.3(2) . . . . ?
N2 C12 C13 C14 59.5(2) . . . . ?
C11 C12 C13 C14 -58.0(3) . . . . ?
N1 C4 C5 C6 62.3(2) . . . . ?
C3 C4 C5 C6 -53.1(3) . . . . ?
N1 C4 C5 C8 -58.5(2) . . . . ?
C3 C4 C5 C8 -173.86(19) . . . . ?
N1 C4 C5 C7 -177.57(17) . . . . ?
C3 C4 C5 C7 67.0(2) . . . . ?
C29 C28 C27 C26 0.2(3) . . . . ?
C25 C26 C27 C28 0.1(3) . . . . ?
C20 N3 C18 O3 -5.2(3) . . . . ?
Ni1 N3 C18 O3 166.92(14) . . . . ?
C20 N3 C18 C17 175.5(2) . . . . ?
Ni1 N3 C18 C17 -12.3(3) . . . . ?
C19 O3 C18 N3 -8.3(3) . . . . ?
C19 O3 C18 C17 171.01(19) . . . . ?
N4 C17 C18 N3 -9.9(3) . . . . ?
N4 C17 C18 O3 170.84(17) . . . . ?
C32 C31 C36 C35 -2.3(3) . . . . ?
B1 C31 C36 C35 177.14(18) . . . . ?
C35 C34 C33 C32 -1.4(4) . . . . ?
C31 C32 C33 C34 -1.2(4) . . . . ?
C42 C37 C38 C39 -2.2(3) . . . . ?
B1 C37 C38 C39 179.91(19) . . . . ?
C37 C38 C39 C40 0.0(3) . . . . ?
C38 C39 C40 C41 1.9(3) . . . . ?
C42 C41 C40 C39 -1.6(3) . . . . ?
C28 C29 C30 C25 0.3(3) . . . . ?
C26 C25 C30 C29 0.0(3) . . . . ?
B1 C25 C30 C29 -176.9(2) . . . . ?
C33 C34 C35 C36 1.9(3) . . . . ?
C31 C36 C35 C34 0.0(3) . . . . ?
N3 C20 C21 C22 -57.9(3) . . . . ?
C19 C20 C21 C22 -172.7(2) . . . . ?
N3 C20 C21 C24 -176.1(2) . . . . ?
C19 C20 C21 C24 69.2(3) . . . . ?
N3 C20 C21 C23 62.1(3) . . . . ?
C19 C20 C21 C23 -52.7(3) . . . . ?
C48 C43 C44 C45 0.7(4) . . . . ?
B1 C43 C44 C45 -176.8(2) . . . . ?
C43 C44 C45 C46 0.1(4) . . . . ?
C18 O3 C19 C20 17.2(2) . . . . ?
N3 C20 C19 O3 -19.5(2) . . . . ?
C21 C20 C19 O3 100.9(2) . . . . ?
C40 C41 C42 C37 -0.8(3) . . . . ?
C38 C37 C42 C41 2.5(3) . . . . ?
B1 C37 C42 C41 -179.6(2) . . . . ?
C26 C25 B1 C43 -90.4(2) . . . . ?
C30 C25 B1 C43 86.2(2) . . . . ?
C26 C25 B1 C37 30.1(3) . . . . ?
C30 C25 B1 C37 -153.3(2) . . . . ?
C26 C25 B1 C31 150.1(2) . . . . ?
C30 C25 B1 C31 -33.3(3) . . . . ?
C44 C43 B1 C25 -10.7(3) . . . . ?
C48 C43 B1 C25 171.95(19) . . . . ?
C44 C43 B1 C37 -130.1(2) . . . . ?
C48 C43 B1 C37 52.5(3) . . . . ?
C44 C43 B1 C31 109.1(2) . . . . ?
C48 C43 B1 C31 -68.3(3) . . . . ?
C42 C37 B1 C25 -107.5(2) . . . . ?
C38 C37 B1 C25 70.2(2) . . . . ?
C42 C37 B1 C43 12.4(3) . . . . ?
C38 C37 B1 C43 -169.88(18) . . . . ?
C42 C37 B1 C31 132.7(2) . . . . ?
C38 C37 B1 C31 -49.6(3) . . . . ?
C36 C31 B1 C25 132.3(2) . . . . ?
C32 C31 B1 C25 -48.3(3) . . . . ?
C36 C31 B1 C43 12.6(3) . . . . ?
C32 C31 B1 C43 -167.96(18) . . . . ?
C36 C31 B1 C37 -108.4(2) . . . . ?
C32 C31 B1 C37 71.0(2) . . . . ?
C48 C47 C46 C45 0.2(4) . . . . ?
C44 C45 C46 C47 -0.6(4) . . . . ?

_refine_diff_density_max         0.406
_refine_diff_density_min         -0.207
_refine_diff_density_rms         0.032

####################################################################### 
# 
# 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_shelx_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 1983781'
loop_
_audit_author_name
_audit_author_address
'Shiro Hikichi'
;Kanagawa University
Japan
;
_audit_update_record             
;
2020-02-13 deposited with the CCDC.	2020-04-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
'[(Acetato){tris(4,4-dimethyl-2-oxazolylmethyl)amine}nickel(II)]tetraphenylborate'
_chemical_name_common            '[Ni(OAc)(TOAMe2)](BPh4)'
_chemical_melting_point          ?
_chemical_formula_moiety         
;C20 H33 N4 Ni O5, C24 H20 B1
;

_chemical_formula_sum            'C44 H53 B N4 Ni O5'
_chemical_formula_weight         787.42

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 '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'
_chemical_compound_source        'synthesis as described'
_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   11.790(6)
_cell_length_b                   13.799(6)
_cell_length_c                   15.362(7)
_cell_angle_alpha                64.129(15)
_cell_angle_beta                 83.65(2)
_cell_angle_gamma                81.82(2)
_cell_volume                     2222.6(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6100
_cell_measurement_theta_min      1.6492
_cell_measurement_theta_max      27.4514

_exptl_crystal_description       Block
_exptl_crystal_colour            Green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.177
_exptl_crystal_F_000             836
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.550
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.250
_exptl_absorpt_coefficient_mu    0.482
_shelx_estimated_absorpt_T_min   0.777
_shelx_estimated_absorpt_T_max   0.889
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_correction_T_max  0.9008
_exptl_absorpt_correction_T_min  0.8208
_exptl_absorpt_process_details   
;Numerical (Based on real shape of the crystal) absorption
correction was parformed on CrystalClear (Rigaku Inc., 2007)
with FS_ABSCOR method.
;
_exptl_absorpt_special_details   ?


_diffrn_special_details          
;
 ?
;

_diffrn_source_power             3.0000
_diffrn_source_voltage           50.0000
_diffrn_source_current           60.0000

_diffrn_radiation_source         'Rotating Anode'

_diffrn_radiation_detector       CCD
_diffrn_measurement_device       
;
Saturn70 (4x4 bin mode)
;
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            9293
_diffrn_number_total             9293
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_av_sigmaI/detI    0.0769
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_measurement_details      
;
scan:
	Number of images: 600
	           Slice: -110.0000 - 70.0000
	     Image width: 0.3000
	        Exp time: 15.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 0.0000
	             XTD: 45.2014
	          2theta: -20.0548
scan:
	Number of images: 600
	           Slice: -110.0000 - 70.0000
	     Image width: 0.3000
	        Exp time: 15.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 90.0000
	             XTD: 45.2014
	          2theta: -20.0548

;
_diffrn_measurement_device_details 
;
AFC10: Fixed Chi 2 circle
;
_diffrn_orient_matrix_UB_11      0.0797
_diffrn_orient_matrix_UB_12      -0.0068
_diffrn_orient_matrix_UB_13      -0.0312
_diffrn_orient_matrix_UB_21      -0.0209
_diffrn_orient_matrix_UB_22      0.0646
_diffrn_orient_matrix_UB_23      -0.0442
_diffrn_orient_matrix_UB_31      0.0232
_diffrn_orient_matrix_UB_32      0.0146
_diffrn_orient_matrix_UB_33      0.0671
_diffrn_orient_matrix_type       d*Trek


_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ω
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_theta_min         1.649
_diffrn_reflns_theta_max         27.449
_diffrn_reflns_theta_full        27.449
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measured_fraction_theta_full 0.914
_diffrn_reflns_Laue_measured_fraction_max 0.914
_diffrn_reflns_Laue_measured_fraction_full 0.914
_diffrn_reflns_point_group_measured_fraction_max 0.914
_diffrn_reflns_point_group_measured_fraction_full 0.914
_reflns_number_total             9293
_reflns_number_gt                6613
_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       'CrystalClear (Rigaku Inc., 2007)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        
'CrystalClear (Rigaku Inc., 2007), SORTAV (Blessing, 1995)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_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_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0437
_refine_ls_wR_factor_ref         0.1589
_refine_ls_goodness_of_fit_ref   0.725
_refine_ls_restrained_S_all      0.725
_refine_ls_number_reflns         9293
_refine_ls_number_parameters     496
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1532P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.002
_refine_diff_density_max         0.422
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none

loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Ni1 0.29600(2) 0.348737(19) 0.110501(17) 0.04166(12) Uani d . 1 . . Ni
O2 0.29468(14) 0.51904(12) 0.02105(11) 0.0516(4) Uani d . 1 . . O
O31 0.49296(17) 0.29058(17) -0.10610(13) 0.0727(5) Uani d . 1 . . O
O1 0.13886(14) 0.43690(13) 0.07495(13) 0.0584(4) Uani d . 1 . . O
N4 0.47647(15) 0.28888(14) 0.13412(12) 0.0471(4) Uani d . 1 . . N
N1 0.32770(19) 0.38866(17) 0.22623(13) 0.0586(5) Uani d . 1 . . N
N3 0.34079(17) 0.32134(15) -0.01429(12) 0.0490(4) Uani d . 1 . . N
O21 0.35994(18) 0.03655(17) 0.30998(17) 0.1034(9) Uani d . 1 . . O
N2 0.27189(16) 0.19112(15) 0.20358(13) 0.0499(4) Uani d . 1 . . N
C111 0.73369(19) 0.01058(19) 0.32692(16) 0.0522(5) Uani d . 1 . . C
C36 0.5353(2) 0.2868(2) 0.04417(17) 0.0556(5) Uani d . 1 . . C
H36A 0.583 0.2186 0.0599 0.067 Uiso calc R 1 . . H
H36B 0.5844 0.3449 0.0143 0.067 Uiso calc R 1 . . H
O11 0.4692(2) 0.4443(2) 0.27515(16) 0.1037(8) Uani d . 1 . . O
C116 0.6651(2) -0.0045(2) 0.41237(17) 0.0636(6) Uani d . 1 . . C
H116 0.6356 -0.0706 0.4482 0.076 Uiso calc R 1 . . H
C16 0.5228(2) 0.3672(2) 0.16036(18) 0.0635(6) Uani d . 1 . . C
H16A 0.542 0.4304 0.1022 0.076 Uiso calc R 1 . . H
H16B 0.5917 0.3337 0.1957 0.076 Uiso calc R 1 . . H
C131 0.7646(2) -0.0261(2) 0.16790(18) 0.0573(6) Uani d . 1 . . C
C115 0.6404(3) 0.0762(3) 0.44443(19) 0.0759(8) Uani d . 1 . . C
H115 0.593 0.0639 0.5 0.091 Uiso calc R 1 . . H
C132 0.6645(2) -0.0170(2) 0.1242(2) 0.0652(6) Uani d . 1 . . C
H132 0.6015 -0.049 0.1627 0.078 Uiso calc R 1 . . H
C26 0.4794(2) 0.17938(19) 0.21715(17) 0.0606(6) Uani d . 1 . . C
H26A 0.5343 0.1294 0.2011 0.073 Uiso calc R 1 . . H
H26B 0.5051 0.183 0.2734 0.073 Uiso calc R 1 . . H
C15 0.4325(3) 0.3997(2) 0.22195(16) 0.0657(7) Uani d . 1 . . C
C136 0.8549(3) 0.0241(3) 0.1034(2) 0.0780(8) Uani d . 1 . . C
H136 0.9246 0.0203 0.1283 0.094 Uiso calc R 1 . . H
C141 0.6907(2) -0.1854(2) 0.33625(17) 0.0642(7) Uani d . 1 . . C
C112 0.7762(2) 0.1124(2) 0.27896(19) 0.0599(6) Uani d . 1 . . C
H112 0.8213 0.127 0.2219 0.072 Uiso calc R 1 . . H
C35 0.4479(2) 0.29980(18) -0.02527(15) 0.0518(5) Uani d . 1 . . C
C121 0.9057(2) -0.1358(2) 0.3209(2) 0.0622(6) Uani d . 1 . . C
C134 0.7461(4) 0.0868(3) -0.0366(2) 0.0902(10) Uani d . 1 . . C
H134 0.7401 0.1231 -0.1033 0.108 Uiso calc R 1 . . H
C1 0.1871(2) 0.52329(19) 0.02712(17) 0.0554(6) Uani d . 1 . . C
C113 0.7540(2) 0.1918(2) 0.3124(2) 0.0696(7) Uani d . 1 . . C
H113 0.7859 0.257 0.2789 0.084 Uiso calc R 1 . . H
C23 0.1774(2) 0.1187(2) 0.25032(18) 0.0624(6) Uani d . 1 . . C
C33 0.2889(2) 0.3339(2) -0.10435(17) 0.0614(6) Uani d . 1 . . C
C135 0.8441(4) 0.0793(3) 0.0037(2) 0.0935(10) Uani d . 1 . . C
H135 0.9063 0.1117 -0.0359 0.112 Uiso calc R 1 . . H
C146 0.7326(3) -0.2946(2) 0.36491(18) 0.0743(8) Uani d . 1 . . C
H146 0.8112 -0.3127 0.3587 0.089 Uiso calc R 1 . . H
B1 0.7739(2) -0.0849(2) 0.2879(2) 0.0553(6) Uani d . 1 . . B
C126 0.9459(2) -0.1419(2) 0.4061(2) 0.0737(8) Uani d . 1 . . C
H126 0.8987 -0.1089 0.4404 0.088 Uiso calc R 1 . . H
C25 0.3645(2) 0.13777(19) 0.24128(17) 0.0590(6) Uani d . 1 . . C
C114 0.6851(3) 0.1748(3) 0.3951(2) 0.0763(8) Uani d . 1 . . C
H114 0.6688 0.2283 0.4174 0.092 Uiso calc R 1 . . H
C125 1.0494(3) -0.1929(3) 0.4418(3) 0.1021(12) Uani d . 1 . . C
H125 1.0703 -0.1951 0.4993 0.123 Uiso calc R 1 . . H
C133 0.6551(3) 0.0394(3) 0.0232(2) 0.0824(9) Uani d . 1 . . C
H133 0.586 0.0445 -0.0033 0.099 Uiso calc R 1 . . H
C122 0.9830(3) -0.1843(3) 0.2716(3) 0.0914(10) Uani d . 1 . . C
H122 0.9624 -0.1818 0.2139 0.11 Uiso calc R 1 . . H
C34 0.3943(3) 0.3069(3) -0.1614(2) 0.0911(10) Uani d . 1 . . C
H34A 0.3865 0.2418 -0.1687 0.109 Uiso calc R 1 . . H
H34B 0.4026 0.3659 -0.2254 0.109 Uiso calc R 1 . . H
C31 0.2348(3) 0.4507(3) -0.1582(2) 0.0939(11) Uani d . 1 . . C
H31A 0.2924 0.4995 -0.1745 0.141 Uiso calc R 1 . . H
H31B 0.1748 0.4669 -0.1174 0.141 Uiso calc R 1 . . H
H31C 0.2034 0.459 -0.2163 0.141 Uiso calc R 1 . . H
C145 0.6594(4) -0.3784(3) 0.4029(2) 0.0894(10) Uani d . 1 . . C
H145 0.6902 -0.4501 0.4222 0.107 Uiso calc R 1 . . H
C2 0.1152(3) 0.6297(2) -0.0226(3) 0.0896(10) Uani d . 1 . . C
H2A 0.0354 0.6186 -0.01 0.134 Uiso calc R 1 . . H
H2B 0.1334 0.6589 -0.0912 0.134 Uiso calc R 1 . . H
H2C 0.131 0.6796 0.0016 0.134 Uiso calc R 1 . . H
C32 0.1982(3) 0.2553(3) -0.0778(2) 0.0815(9) Uani d . 1 . . C
H32A 0.233 0.1824 -0.0445 0.122 Uiso calc R 1 . . H
H32B 0.1663 0.2634 -0.1357 0.122 Uiso calc R 1 . . H
H32C 0.1384 0.2707 -0.0364 0.122 Uiso calc R 1 . . H
C142 0.5695(3) -0.1653(3) 0.3470(2) 0.0845(9) Uani d . 1 . . C
H142 0.5368 -0.0943 0.329 0.101 Uiso calc R 1 . . H
C144 0.5424(4) -0.3537(4) 0.4113(2) 0.1086(14) Uani d . 1 . . C
H144 0.4943 -0.4087 0.4357 0.13 Uiso calc R 1 . . H
C21 0.0837(4) 0.1710(4) 0.2954(4) 0.144(2) Uani d . 1 . . C
H21A 0.0475 0.2348 0.2455 0.216 Uiso calc R 1 . . H
H21B 0.116 0.1904 0.3395 0.216 Uiso calc R 1 . . H
H21C 0.0279 0.1211 0.3299 0.216 Uiso calc R 1 . . H
C22 0.1272(4) 0.0960(4) 0.1767(3) 0.1203(16) Uani d . 1 . . C
H22A 0.0877 0.1615 0.1313 0.18 Uiso calc R 1 . . H
H22B 0.0742 0.0427 0.2086 0.18 Uiso calc R 1 . . H
H22C 0.1875 0.0693 0.1429 0.18 Uiso calc R 1 . . H
C143 0.4973(4) -0.2487(4) 0.3839(3) 0.1059(13) Uani d . 1 . . C
H143 0.4184 -0.2322 0.3896 0.127 Uiso calc R 1 . . H
C13 0.2691(3) 0.4285(3) 0.2984(2) 0.0876(10) Uani d . 1 . . C
C123 1.0889(3) -0.2356(3) 0.3064(5) 0.1206(17) Uani d . 1 . . C
H123 1.1378 -0.2667 0.2716 0.145 Uiso calc R 1 . . H
C11 0.1705(6) 0.5136(5) 0.2516(5) 0.189(3) Uani d . 1 . . C
H11A 0.1994 0.5722 0.1952 0.283 Uiso calc R 1 . . H
H11B 0.1343 0.5406 0.297 0.283 Uiso calc R 1 . . H
H11C 0.1156 0.4819 0.2332 0.283 Uiso calc R 1 . . H
C124 1.1237(3) -0.2416(3) 0.3925(4) 0.1185(17) Uani d . 1 . . C
H124 1.1946 -0.2771 0.4161 0.142 Uiso calc R 1 . . H
C24 0.2399(3) 0.0184(3) 0.3231(3) 0.162(3) Uani d . 1 . . C
H24A 0.2108 0.0057 0.3883 0.195 Uiso calc R 1 . . H
H24B 0.2301 -0.0441 0.3124 0.195 Uiso calc R 1 . . H
C14 0.3643(5) 0.4801(5) 0.3177(4) 0.155(2) Uani d . 1 . . C
H14A 0.3496 0.5584 0.2875 0.186 Uiso calc R 1 . . H
H14B 0.37 0.4558 0.3867 0.186 Uiso calc R 1 . . H
C12 0.2303(5) 0.3357(4) 0.3861(3) 0.159(3) Uani d . 1 . . C
H12A 0.2951 0.284 0.4132 0.239 Uiso calc R 1 . . H
H12B 0.176 0.3021 0.3691 0.239 Uiso calc R 1 . . H
H12C 0.1948 0.3608 0.4329 0.239 Uiso calc R 1 . . H



#==============================================================================

# MOLECULAR GEOMETRY

_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni1 N2 . 2.0561(19) ?
Ni1 O1 . 2.0526(19) ?
Ni1 N3 . 2.1092(19) ?
Ni1 O2 . 2.1418(17) ?
Ni1 N1 . 2.1597(19) ?
Ni1 N4 . 2.180(2) ?
Ni1 C1 . 2.425(3) ?
O2 C1 . 1.256(3) ?
O31 C35 . 1.346(3) ?
O31 C34 . 1.451(4) ?
O1 C1 . 1.273(3) ?
N4 C16 . 1.492(3) ?
N4 C36 . 1.486(3) ?
N4 C26 . 1.491(3) ?
N1 C15 . 1.257(3) ?
N1 C13 . 1.504(3) ?
N3 C35 . 1.266(3) ?
N3 C33 . 1.505(3) ?
O21 C25 . 1.338(3) ?
O21 C24 . 1.449(4) ?
N2 C25 . 1.268(3) ?
N2 C23 . 1.507(3) ?
C111 C112 . 1.409(3) ?
C111 C116 . 1.412(3) ?
C111 B1 . 1.664(4) ?
C36 C35 . 1.502(3) ?
C36 H36A . 0.97 ?
C36 H36B . 0.97 ?
O11 C15 . 1.352(3) ?
O11 C14 . 1.460(5) ?
C116 C115 . 1.387(4) ?
C116 H116 . 0.93 ?
C16 C15 . 1.497(4) ?
C16 H16A . 0.97 ?
C16 H16B . 0.97 ?
C131 C136 . 1.404(4) ?
C131 C132 . 1.385(4) ?
C131 B1 . 1.669(4) ?
C115 C114 . 1.386(4) ?
C115 H115 . 0.93 ?
C132 C133 . 1.409(4) ?
C132 H132 . 0.93 ?
C26 C25 . 1.493(4) ?
C26 H26A . 0.97 ?
C26 H26B . 0.97 ?
C136 C135 . 1.394(4) ?
C136 H136 . 0.93 ?
C141 C146 . 1.402(4) ?
C141 C142 . 1.422(4) ?
C141 B1 . 1.662(3) ?
C112 C113 . 1.383(4) ?
C112 H112 . 0.93 ?
C121 C122 . 1.403(4) ?
C121 C126 . 1.405(4) ?
C121 B1 . 1.649(4) ?
C134 C135 . 1.339(5) ?
C134 C133 . 1.372(5) ?
C134 H134 . 0.93 ?
C1 C2 . 1.507(4) ?
C113 C114 . 1.377(4) ?
C113 H113 . 0.93 ?
C23 C24 . 1.501(4) ?
C23 C22 . 1.496(4) ?
C23 C21 . 1.503(5) ?
C33 C32 . 1.527(4) ?
C33 C31 . 1.533(4) ?
C33 C34 . 1.538(4) ?
C135 H135 . 0.93 ?
C146 C145 . 1.416(4) ?
C146 H146 . 0.93 ?
C126 C125 . 1.361(5) ?
C126 H126 . 0.93 ?
C114 H114 . 0.93 ?
C125 C124 . 1.387(6) ?
C125 H125 . 0.93 ?
C133 H133 . 0.93 ?
C122 C123 . 1.382(6) ?
C122 H122 . 0.93 ?
C34 H34A . 0.97 ?
C34 H34B . 0.97 ?
C31 H31A . 0.96 ?
C31 H31B . 0.96 ?
C31 H31C . 0.96 ?
C145 C144 . 1.378(6) ?
C145 H145 . 0.93 ?
C2 H2A . 0.96 ?
C2 H2B . 0.96 ?
C2 H2C . 0.96 ?
C32 H32A . 0.96 ?
C32 H32B . 0.96 ?
C32 H32C . 0.96 ?
C142 C143 . 1.405(4) ?
C142 H142 . 0.93 ?
C144 C143 . 1.363(6) ?
C144 H144 . 0.93 ?
C21 H21A . 0.96 ?
C21 H21B . 0.96 ?
C21 H21C . 0.96 ?
C22 H22A . 0.96 ?
C22 H22B . 0.96 ?
C22 H22C . 0.96 ?
C143 H143 . 0.93 ?
C13 C12 . 1.479(5) ?
C13 C11 . 1.518(7) ?
C13 C14 . 1.530(5) ?
C123 C124 . 1.393(7) ?
C123 H123 . 0.93 ?
C11 H11A . 0.96 ?
C11 H11B . 0.96 ?
C11 H11C . 0.96 ?
C124 H124 . 0.93 ?
C24 H24A . 0.97 ?
C24 H24B . 0.97 ?
C14 H14A . 0.97 ?
C14 H14B . 0.97 ?
C12 H12A . 0.96 ?
C12 H12B . 0.96 ?
C12 H12C . 0.96 ?

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
N2 Ni1 O1 109.01(8) . . ?
N2 Ni1 N3 96.49(8) . . ?
O1 Ni1 N3 100.21(8) . . ?
N2 Ni1 O2 171.10(7) . . ?
O1 Ni1 O2 62.81(7) . . ?
N3 Ni1 O2 88.75(7) . . ?
N2 Ni1 N1 93.10(8) . . ?
O1 Ni1 N1 98.41(8) . . ?
N3 Ni1 N1 154.96(8) . . ?
O2 Ni1 N1 85.01(8) . . ?
N2 Ni1 N4 82.94(7) . . ?
O1 Ni1 N4 167.78(7) . . ?
N3 Ni1 N4 80.42(7) . . ?
O2 Ni1 N4 105.10(7) . . ?
N1 Ni1 N4 77.88(8) . . ?
N2 Ni1 C1 140.54(8) . . ?
O1 Ni1 C1 31.67(7) . . ?
N3 Ni1 C1 95.49(8) . . ?
O2 Ni1 C1 31.14(7) . . ?
N1 Ni1 C1 91.61(9) . . ?
N4 Ni1 C1 136.20(8) . . ?
C1 O2 Ni1 86.98(13) . . ?
C35 O31 C34 104.3(2) . . ?
C1 O1 Ni1 90.51(15) . . ?
C16 N4 C36 111.55(18) . . ?
C16 N4 C26 111.01(18) . . ?
C36 N4 C26 112.7(2) . . ?
C16 N4 Ni1 104.64(15) . . ?
C36 N4 Ni1 109.93(13) . . ?
C26 N4 Ni1 106.56(14) . . ?
C15 N1 C13 106.8(2) . . ?
C15 N1 Ni1 108.81(15) . . ?
C13 N1 Ni1 142.9(2) . . ?
C35 N3 C33 106.76(19) . . ?
C35 N3 Ni1 112.26(14) . . ?
C33 N3 Ni1 140.25(16) . . ?
C25 O21 C24 105.5(2) . . ?
C25 N2 C23 107.40(19) . . ?
C25 N2 Ni1 111.51(15) . . ?
C23 N2 Ni1 140.74(15) . . ?
C112 C111 C116 114.7(2) . . ?
C112 C111 B1 120.5(2) . . ?
C116 C111 B1 124.6(2) . . ?
N4 C36 C35 109.83(19) . . ?
N4 C36 H36A 109.7 . . ?
C35 C36 H36A 109.7 . . ?
N4 C36 H36B 109.7 . . ?
C35 C36 H36B 109.7 . . ?
H36A C36 H36B 108.2 . . ?
C15 O11 C14 104.6(3) . . ?
C115 C116 C111 122.0(3) . . ?
C115 C116 H116 119 . . ?
C111 C116 H116 119 . . ?
N4 C16 C15 107.99(19) . . ?
N4 C16 H16A 110.1 . . ?
C15 C16 H16A 110.1 . . ?
N4 C16 H16B 110.1 . . ?
C15 C16 H16B 110.1 . . ?
H16A C16 H16B 108.4 . . ?
C136 C131 C132 114.6(3) . . ?
C136 C131 B1 122.9(2) . . ?
C132 C131 B1 122.4(2) . . ?
C116 C115 C114 121.1(3) . . ?
C116 C115 H115 119.4 . . ?
C114 C115 H115 119.4 . . ?
C133 C132 C131 122.1(3) . . ?
C133 C132 H132 119 . . ?
C131 C132 H132 119 . . ?
C25 C26 N4 111.83(19) . . ?
C25 C26 H26A 109.3 . . ?
N4 C26 H26A 109.3 . . ?
C25 C26 H26B 109.3 . . ?
N4 C26 H26B 109.3 . . ?
H26A C26 H26B 107.9 . . ?
N1 C15 O11 119.5(3) . . ?
N1 C15 C16 124.5(2) . . ?
O11 C15 C16 116.0(2) . . ?
C131 C136 C135 122.6(3) . . ?
C131 C136 H136 118.7 . . ?
C135 C136 H136 118.7 . . ?
C146 C141 C142 114.9(3) . . ?
C146 C141 B1 123.4(3) . . ?
C142 C141 B1 121.6(3) . . ?
C113 C112 C111 123.3(2) . . ?
C113 C112 H112 118.4 . . ?
C111 C112 H112 118.4 . . ?
N3 C35 O31 120.3(2) . . ?
N3 C35 C36 125.50(19) . . ?
O31 C35 C36 114.2(2) . . ?
C122 C121 C126 114.7(3) . . ?
C122 C121 B1 123.2(3) . . ?
C126 C121 B1 121.9(2) . . ?
C135 C134 C133 118.3(3) . . ?
C135 C134 H134 120.9 . . ?
C133 C134 H134 120.9 . . ?
O2 C1 O1 119.7(2) . . ?
O2 C1 C2 120.4(2) . . ?
O1 C1 C2 119.9(2) . . ?
O2 C1 Ni1 61.88(12) . . ?
O1 C1 Ni1 57.82(12) . . ?
C2 C1 Ni1 177.7(2) . . ?
C114 C113 C112 120.3(3) . . ?
C114 C113 H113 119.8 . . ?
C112 C113 H113 119.8 . . ?
N2 C23 C24 102.2(2) . . ?
N2 C23 C22 110.3(2) . . ?
C24 C23 C22 111.4(4) . . ?
N2 C23 C21 110.7(2) . . ?
C24 C23 C21 113.3(4) . . ?
C22 C23 C21 108.8(3) . . ?
N3 C33 C32 110.1(2) . . ?
N3 C33 C31 109.64(19) . . ?
C32 C33 C31 110.1(3) . . ?
N3 C33 C34 101.9(2) . . ?
C32 C33 C34 112.7(2) . . ?
C31 C33 C34 112.0(3) . . ?
C134 C135 C136 121.5(3) . . ?
C134 C135 H135 119.2 . . ?
C136 C135 H135 119.2 . . ?
C141 C146 C145 122.3(4) . . ?
C141 C146 H146 118.9 . . ?
C145 C146 H146 118.9 . . ?
C111 B1 C121 107.71(19) . . ?
C111 B1 C131 107.1(2) . . ?
C121 B1 C131 112.7(2) . . ?
C111 B1 C141 112.3(2) . . ?
C121 B1 C141 107.9(2) . . ?
C131 B1 C141 109.15(19) . . ?
C125 C126 C121 124.2(3) . . ?
C125 C126 H126 117.9 . . ?
C121 C126 H126 117.9 . . ?
N2 C25 O21 118.2(2) . . ?
N2 C25 C26 125.4(2) . . ?
O21 C25 C26 116.4(2) . . ?
C113 C114 C115 118.5(3) . . ?
C113 C114 H114 120.7 . . ?
C115 C114 H114 120.7 . . ?
C126 C125 C124 120.1(4) . . ?
C126 C125 H125 119.9 . . ?
C124 C125 H125 119.9 . . ?
C134 C133 C132 121.0(3) . . ?
C134 C133 H133 119.5 . . ?
C132 C133 H133 119.5 . . ?
C121 C122 C123 121.9(4) . . ?
C121 C122 H122 119.1 . . ?
C123 C122 H122 119.1 . . ?
O31 C34 C33 106.5(2) . . ?
O31 C34 H34A 110.4 . . ?
C33 C34 H34A 110.4 . . ?
O31 C34 H34B 110.4 . . ?
C33 C34 H34B 110.4 . . ?
H34A C34 H34B 108.6 . . ?
C33 C31 H31A 109.5 . . ?
C33 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C33 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C144 C145 C146 120.1(4) . . ?
C144 C145 H145 120 . . ?
C146 C145 H145 120 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C33 C32 H32A 109.5 . . ?
C33 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C33 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C143 C142 C141 122.4(4) . . ?
C143 C142 H142 118.8 . . ?
C141 C142 H142 118.8 . . ?
C145 C144 C143 119.9(3) . . ?
C145 C144 H144 120 . . ?
C143 C144 H144 120 . . ?
C23 C21 H21A 109.5 . . ?
C23 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C23 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 C22 H22A 109.5 . . ?
C23 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C23 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C144 C143 C142 120.3(4) . . ?
C144 C143 H143 119.8 . . ?
C142 C143 H143 119.8 . . ?
C12 C13 N1 109.4(3) . . ?
C12 C13 C11 112.2(5) . . ?
N1 C13 C11 109.3(3) . . ?
C12 C13 C14 112.6(4) . . ?
N1 C13 C14 102.4(3) . . ?
C11 C13 C14 110.4(4) . . ?
C124 C123 C122 121.3(4) . . ?
C124 C123 H123 119.4 . . ?
C122 C123 H123 119.4 . . ?
C13 C11 H11A 109.5 . . ?
C13 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C13 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C125 C124 C123 117.9(4) . . ?
C125 C124 H124 121.1 . . ?
C123 C124 H124 121.1 . . ?
O21 C24 C23 106.6(2) . . ?
O21 C24 H24A 110.4 . . ?
C23 C24 H24A 110.4 . . ?
O21 C24 H24B 110.4 . . ?
C23 C24 H24B 110.4 . . ?
H24A C24 H24B 108.6 . . ?
O11 C14 C13 105.1(3) . . ?
O11 C14 H14A 110.7 . . ?
C13 C14 H14A 110.7 . . ?
O11 C14 H14B 110.7 . . ?
C13 C14 H14B 110.7 . . ?
H14A C14 H14B 108.8 . . ?
C13 C12 H12A 109.5 . . ?
C13 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C13 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 Ni1 O2 C1 -23.4(4) . . . . ?
O1 Ni1 O2 C1 0.63(13) . . . . ?
N3 Ni1 O2 C1 102.78(14) . . . . ?
N1 Ni1 O2 C1 -101.49(14) . . . . ?
N4 Ni1 O2 C1 -177.49(13) . . . . ?
N2 Ni1 O1 C1 175.56(14) . . . . ?
N3 Ni1 O1 C1 -83.87(15) . . . . ?
O2 Ni1 O1 C1 -0.62(13) . . . . ?
N1 Ni1 O1 C1 79.31(15) . . . . ?
N4 Ni1 O1 C1 8.0(4) . . . . ?
N2 Ni1 N4 C16 -129.46(14) . . . . ?
O1 Ni1 N4 C16 38.7(4) . . . . ?
N3 Ni1 N4 C16 132.70(14) . . . . ?
O2 Ni1 N4 C16 46.63(14) . . . . ?
N1 Ni1 N4 C16 -34.74(14) . . . . ?
C1 Ni1 N4 C16 44.75(18) . . . . ?
N2 Ni1 N4 C36 110.64(15) . . . . ?
O1 Ni1 N4 C36 -81.2(4) . . . . ?
N3 Ni1 N4 C36 12.80(14) . . . . ?
O2 Ni1 N4 C36 -73.27(15) . . . . ?
N1 Ni1 N4 C36 -154.64(15) . . . . ?
C1 Ni1 N4 C36 -75.15(18) . . . . ?
N2 Ni1 N4 C26 -11.80(15) . . . . ?
O1 Ni1 N4 C26 156.4(3) . . . . ?
N3 Ni1 N4 C26 -109.64(16) . . . . ?
O2 Ni1 N4 C26 164.29(14) . . . . ?
N1 Ni1 N4 C26 82.92(16) . . . . ?
C1 Ni1 N4 C26 162.41(15) . . . . ?
N2 Ni1 N1 C15 108.23(19) . . . . ?
O1 Ni1 N1 C15 -142.03(18) . . . . ?
N3 Ni1 N1 C15 -4.3(3) . . . . ?
O2 Ni1 N1 C15 -80.50(18) . . . . ?
N4 Ni1 N1 C15 26.14(18) . . . . ?
C1 Ni1 N1 C15 -110.96(19) . . . . ?
N2 Ni1 N1 C13 -88.2(3) . . . . ?
O1 Ni1 N1 C13 21.5(3) . . . . ?
N3 Ni1 N1 C13 159.2(3) . . . . ?
O2 Ni1 N1 C13 83.0(3) . . . . ?
N4 Ni1 N1 C13 -170.3(3) . . . . ?
C1 Ni1 N1 C13 52.6(3) . . . . ?
N2 Ni1 N3 C35 -90.99(16) . . . . ?
O1 Ni1 N3 C35 158.30(15) . . . . ?
O2 Ni1 N3 C35 96.23(16) . . . . ?
N1 Ni1 N3 C35 20.9(3) . . . . ?
N4 Ni1 N3 C35 -9.31(15) . . . . ?
C1 Ni1 N3 C35 126.67(16) . . . . ?
N2 Ni1 N3 C33 100.6(2) . . . . ?
O1 Ni1 N3 C33 -10.1(2) . . . . ?
O2 Ni1 N3 C33 -72.1(2) . . . . ?
N1 Ni1 N3 C33 -147.5(2) . . . . ?
N4 Ni1 N3 C33 -177.7(2) . . . . ?
C1 Ni1 N3 C33 -41.7(2) . . . . ?
O1 Ni1 N2 C25 -168.33(18) . . . . ?
N3 Ni1 N2 C25 88.50(19) . . . . ?
O2 Ni1 N2 C25 -145.8(4) . . . . ?
N1 Ni1 N2 C25 -68.33(19) . . . . ?
N4 Ni1 N2 C25 9.04(18) . . . . ?
C1 Ni1 N2 C25 -164.66(17) . . . . ?
O1 Ni1 N2 C23 3.7(3) . . . . ?
N3 Ni1 N2 C23 -99.4(2) . . . . ?
O2 Ni1 N2 C23 26.3(5) . . . . ?
N1 Ni1 N2 C23 103.7(3) . . . . ?
N4 Ni1 N2 C23 -178.9(3) . . . . ?
C1 Ni1 N2 C23 7.4(3) . . . . ?
C16 N4 C36 C35 -129.4(2) . . . . ?
C26 N4 C36 C35 104.9(2) . . . . ?
Ni1 N4 C36 C35 -13.8(2) . . . . ?
C112 C111 C116 C115 1.2(4) . . . . ?
B1 C111 C116 C115 175.8(2) . . . . ?
C36 N4 C16 C15 156.5(2) . . . . ?
C26 N4 C16 C15 -76.9(2) . . . . ?
Ni1 N4 C16 C15 37.7(2) . . . . ?
C111 C116 C115 C114 -1.9(4) . . . . ?
C136 C131 C132 C133 -0.7(4) . . . . ?
B1 C131 C132 C133 175.5(2) . . . . ?
C16 N4 C26 C25 125.9(2) . . . . ?
C36 N4 C26 C25 -108.1(2) . . . . ?
Ni1 N4 C26 C25 12.5(3) . . . . ?
C13 N1 C15 O11 -2.0(3) . . . . ?
Ni1 N1 C15 O11 167.7(2) . . . . ?
C13 N1 C15 C16 178.4(3) . . . . ?
Ni1 N1 C15 C16 -11.8(3) . . . . ?
C14 O11 C15 N1 -6.4(4) . . . . ?
C14 O11 C15 C16 173.1(3) . . . . ?
N4 C16 C15 N1 -19.0(3) . . . . ?
N4 C16 C15 O11 161.5(2) . . . . ?
C132 C131 C136 C135 0.5(4) . . . . ?
B1 C131 C136 C135 -175.6(3) . . . . ?
C116 C111 C112 C113 0.6(4) . . . . ?
B1 C111 C112 C113 -174.3(2) . . . . ?
C33 N3 C35 O31 -1.2(3) . . . . ?
Ni1 N3 C35 O31 -173.43(17) . . . . ?
C33 N3 C35 C36 176.3(2) . . . . ?
Ni1 N3 C35 C36 4.1(3) . . . . ?
C34 O31 C35 N3 -1.7(3) . . . . ?
C34 O31 C35 C36 -179.5(2) . . . . ?
N4 C36 C35 N3 7.2(3) . . . . ?
N4 C36 C35 O31 -175.16(19) . . . . ?
Ni1 O2 C1 O1 -1.0(2) . . . . ?
Ni1 O2 C1 C2 179.6(3) . . . . ?
Ni1 O1 C1 O2 1.1(2) . . . . ?
Ni1 O1 C1 C2 -179.5(2) . . . . ?
N2 Ni1 C1 O2 174.45(11) . . . . ?
O1 Ni1 C1 O2 -178.9(2) . . . . ?
N3 Ni1 C1 O2 -78.37(13) . . . . ?
N1 Ni1 C1 O2 77.59(14) . . . . ?
N4 Ni1 C1 O2 3.50(19) . . . . ?
N2 Ni1 C1 O1 -6.6(2) . . . . ?
N3 Ni1 C1 O1 100.56(14) . . . . ?
O2 Ni1 C1 O1 178.9(2) . . . . ?
N1 Ni1 C1 O1 -103.47(15) . . . . ?
N4 Ni1 C1 O1 -177.56(12) . . . . ?
N2 Ni1 C1 C2 4(6) . . . . ?
O1 Ni1 C1 C2 11(5) . . . . ?
N3 Ni1 C1 C2 111(5) . . . . ?
O2 Ni1 C1 C2 -170(6) . . . . ?
N1 Ni1 C1 C2 -93(5) . . . . ?
N4 Ni1 C1 C2 -167(5) . . . . ?
C111 C112 C113 C114 -1.7(4) . . . . ?
C25 N2 C23 C24 2.3(4) . . . . ?
Ni1 N2 C23 C24 -169.9(3) . . . . ?
C25 N2 C23 C22 -116.2(3) . . . . ?
Ni1 N2 C23 C22 71.5(4) . . . . ?
C25 N2 C23 C21 123.3(3) . . . . ?
Ni1 N2 C23 C21 -49.0(4) . . . . ?
C35 N3 C33 C32 123.2(2) . . . . ?
Ni1 N3 C33 C32 -68.1(3) . . . . ?
C35 N3 C33 C31 -115.6(3) . . . . ?
Ni1 N3 C33 C31 53.2(3) . . . . ?
C35 N3 C33 C34 3.3(3) . . . . ?
Ni1 N3 C33 C34 172.0(2) . . . . ?
C133 C134 C135 C136 0.7(5) . . . . ?
C131 C136 C135 C134 -0.6(5) . . . . ?
C142 C141 C146 C145 -0.8(4) . . . . ?
B1 C141 C146 C145 -177.8(2) . . . . ?
C112 C111 B1 C121 75.6(3) . . . . ?
C116 C111 B1 C121 -98.7(3) . . . . ?
C112 C111 B1 C131 -45.9(3) . . . . ?
C116 C111 B1 C131 139.8(2) . . . . ?
C112 C111 B1 C141 -165.7(2) . . . . ?
C116 C111 B1 C141 20.0(3) . . . . ?
C122 C121 B1 C111 -154.0(3) . . . . ?
C126 C121 B1 C111 31.4(3) . . . . ?
C122 C121 B1 C131 -36.1(3) . . . . ?
C126 C121 B1 C131 149.4(2) . . . . ?
C122 C121 B1 C141 84.5(3) . . . . ?
C126 C121 B1 C141 -90.0(3) . . . . ?
C136 C131 B1 C111 87.7(3) . . . . ?
C132 C131 B1 C111 -88.1(3) . . . . ?
C136 C131 B1 C121 -30.6(3) . . . . ?
C132 C131 B1 C121 153.6(2) . . . . ?
C136 C131 B1 C141 -150.5(3) . . . . ?
C132 C131 B1 C141 33.7(3) . . . . ?
C146 C141 B1 C111 -141.3(2) . . . . ?
C142 C141 B1 C111 41.9(3) . . . . ?
C146 C141 B1 C121 -22.7(3) . . . . ?
C142 C141 B1 C121 160.5(2) . . . . ?
C146 C141 B1 C131 100.1(3) . . . . ?
C142 C141 B1 C131 -76.7(3) . . . . ?
C122 C121 C126 C125 -2.0(4) . . . . ?
B1 C121 C126 C125 173.0(3) . . . . ?
C23 N2 C25 O21 -0.6(3) . . . . ?
Ni1 N2 C25 O21 174.2(2) . . . . ?
C23 N2 C25 C26 -179.0(3) . . . . ?
Ni1 N2 C25 C26 -4.3(3) . . . . ?
C24 O21 C25 N2 -1.5(5) . . . . ?
C24 O21 C25 C26 177.0(4) . . . . ?
N4 C26 C25 N2 -6.5(4) . . . . ?
N4 C26 C25 O21 175.0(2) . . . . ?
C112 C113 C114 C115 1.1(4) . . . . ?
C116 C115 C114 C113 0.7(4) . . . . ?
C121 C126 C125 C124 1.2(5) . . . . ?
C135 C134 C133 C132 -0.8(5) . . . . ?
C131 C132 C133 C134 0.8(4) . . . . ?
C126 C121 C122 C123 1.3(4) . . . . ?
B1 C121 C122 C123 -173.6(3) . . . . ?
C35 O31 C34 C33 3.7(3) . . . . ?
N3 C33 C34 O31 -4.2(3) . . . . ?
C32 C33 C34 O31 -122.2(3) . . . . ?
C31 C33 C34 O31 112.9(3) . . . . ?
C141 C146 C145 C144 1.1(4) . . . . ?
C146 C141 C142 C143 0.2(4) . . . . ?
B1 C141 C142 C143 177.2(3) . . . . ?
C146 C145 C144 C143 -0.6(5) . . . . ?
C145 C144 C143 C142 0.0(5) . . . . ?
C141 C142 C143 C144 0.2(5) . . . . ?
C15 N1 C13 C12 -110.6(4) . . . . ?
Ni1 N1 C13 C12 85.7(5) . . . . ?
C15 N1 C13 C11 126.1(4) . . . . ?
Ni1 N1 C13 C11 -37.6(5) . . . . ?
C15 N1 C13 C14 9.1(4) . . . . ?
Ni1 N1 C13 C14 -154.7(3) . . . . ?
C121 C122 C123 C124 0.1(6) . . . . ?
C126 C125 C124 C123 0.3(6) . . . . ?
C122 C123 C124 C125 -1.0(6) . . . . ?
C25 O21 C24 C23 2.9(5) . . . . ?
N2 C23 C24 O21 -3.1(5) . . . . ?
C22 C23 C24 O21 114.6(4) . . . . ?
C21 C23 C24 O21 -122.3(4) . . . . ?
C15 O11 C14 C13 11.5(5) . . . . ?
C12 C13 C14 O11 105.0(4) . . . . ?
N1 C13 C14 O11 -12.4(5) . . . . ?
C11 C13 C14 O11 -128.7(4) . . . . ?


# start Validation Reply Form
_vrf_PLAT029_shelx               
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.914 Why?  
RESPONSE: ...Due to low quality of the crystal.
;
# end Validation Reply Form

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

data_shelx_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 1983780'
loop_
_audit_author_name
_audit_author_address
'Shiro Hikichi'
;Kanagawa University
Japan
;
_audit_update_record             
;
2020-02-13 deposited with the CCDC.	2020-04-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        '[Ni(TOAMe2)(NO3)](BPh4)2CH2Cl2'
_chemical_name_common            
'[nitratotris{(4,4-dimethyloxazolin-2-yl)methyl}aminenickel(II)]tetraphenylborate bisdichloromethane'
_chemical_melting_point          ?
_chemical_formula_moiety         
;C18 H30 N5 Ni O6, C24 H20 B, 2(C H2 Cl2)
;
_chemical_formula_sum            'C44 H54 B Cl4 N5 Ni O6'
_chemical_formula_weight         960.24

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'
Cl Cl 0.1484 0.1585 '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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

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

_cell_length_a                   14.544(5)
_cell_length_b                   11.405(4)
_cell_length_c                   28.205(10)
_cell_angle_alpha                90
_cell_angle_beta                 102.024(4)
_cell_angle_gamma                90
_cell_volume                     4576(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    113(2)
_cell_measurement_reflns_used    11986
_cell_measurement_theta_min      1.4677
_cell_measurement_theta_max      27.4853

_exptl_crystal_description       Block
_exptl_crystal_colour            Green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_F_000             2008
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    0.710
_shelx_estimated_absorpt_T_min   0.842
_shelx_estimated_absorpt_T_max   0.901
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_correction_T_max  0.9138
_exptl_absorpt_correction_T_min  0.8353
_exptl_absorpt_process_details   
;Numerical (Based on real shape of the crystal) absorption
correction was parformed on CrystalClear (Rigaku Inc., 2007)
with FS_ABSCOR method.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      113(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ω
_diffrn_reflns_number            41331
_diffrn_reflns_av_unetI/netI     0.0853
_diffrn_reflns_av_R_equivalents  0.0803
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         2.312
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_full        27.484
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             10430
_reflns_number_gt                7617
_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.
;

_diffrn_special_details          
;
 ?
;
_diffrn_source_power             3.0000
_diffrn_source_voltage           50.0000
_diffrn_source_current           60.0000
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_detector       CCD
_diffrn_measurement_device       
;
Saturn70 (2x2 bin mode)
;
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_measurement_details      
;
scan:
	Number of images: 600
	           Slice: -115.0000 - 65.0000
	     Image width: 0.3000
	        Exp time: 10.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 0.0000
	             XTD: 54.9879
	          2theta: -25.1512
scan:
	Number of images: 600
	           Slice: -115.0000 - 65.0000
	     Image width: 0.3000
	        Exp time: 10.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 90.0000
	             XTD: 54.9879
	          2theta: -25.1512
scan:
	Number of images: 600
	           Slice: -115.0000 - 65.0000
	     Image width: 0.3000
	        Exp time: 10.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 180.0000
	             XTD: 54.9879
	          2theta: -25.1512

;
_diffrn_measurement_device_details 
;
AFC10: Fixed Chi 2 circle
;
_diffrn_orient_matrix_UB_11      0.0317
_diffrn_orient_matrix_UB_12      -0.0611
_diffrn_orient_matrix_UB_13      0.0144
_diffrn_orient_matrix_UB_21      -0.0781
_diffrn_orient_matrix_UB_22      -0.0374
_diffrn_orient_matrix_UB_23      0.0135
_diffrn_orient_matrix_UB_31      0.0018
_diffrn_orient_matrix_UB_32      -0.0155
_diffrn_orient_matrix_UB_33      -0.0327
_diffrn_orient_matrix_type       d*Trek


_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        
'CrystalClear (Rigaku Inc., 2007), SORTAV (Blessing, 1995)'
_computing_structure_solution    'SIR92 (Altomare et al, 1994)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'

_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)+(0.1043P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10430
_refine_ls_number_parameters     565
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0807
_refine_ls_R_factor_gt           0.0661
_refine_ls_wR_factor_ref         0.1974
_refine_ls_wR_factor_gt          0.1825
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.64405(3) 0.28451(3) 0.31671(2) 0.01689(14) Uani 1 1 d . . . . .
Cl1 Cl 0.35513(8) 0.51559(12) 0.27451(4) 0.0607(4) Uani 1 1 d . . . . .
Cl2 Cl 0.28261(9) 0.73853(12) 0.30189(5) 0.0670(4) Uani 1 1 d . . . . .
Cl3 Cl 0.55561(9) 0.84098(15) 0.21639(5) 0.0707(4) Uani 1 1 d D . . . .
O2 O 0.89119(15) 0.39945(19) 0.40056(8) 0.0230(5) Uani 1 1 d . . . . .
O5 O 0.74421(16) 0.18597(19) 0.27561(8) 0.0234(5) Uani 1 1 d . . . . .
O3 O 0.47413(16) 0.4261(2) 0.39988(8) 0.0289(5) Uani 1 1 d . . . . .
N4 N 0.65891(17) 0.4749(2) 0.33202(9) 0.0168(5) Uani 1 1 d . . . . .
O6 O 0.72107(18) -0.00360(19) 0.26945(8) 0.0314(6) Uani 1 1 d . . . . .
Cl4 Cl 0.35659(12) 0.8827(3) 0.20339(8) 0.1390(10) Uani 1 1 d D . . . .
O1 O 0.52762(17) 0.5107(2) 0.20627(8) 0.0298(6) Uani 1 1 d . . . . .
N1 N 0.57652(18) 0.3493(2) 0.25033(9) 0.0199(5) Uani 1 1 d . . . . .
O4 O 0.63263(16) 0.10760(19) 0.30482(8) 0.0247(5) Uani 1 1 d . . . . .
N2 N 0.76234(18) 0.2900(2) 0.37215(9) 0.0181(5) Uani 1 1 d . . . . .
N3 N 0.54112(19) 0.3039(2) 0.35503(9) 0.0213(6) Uani 1 1 d . . . . .
C4 C 0.5371(2) 0.3047(3) 0.19963(11) 0.0259(7) Uani 1 1 d . . . . .
C24 C 0.2802(2) 0.6663(3) 0.08059(12) 0.0248(7) Uani 1 1 d . . . . .
H24 H 0.3074 0.7389 0.0927 0.030 Uiso 1 1 calc R U . . .
N5 N 0.70034(19) 0.0942(2) 0.28267(9) 0.0223(6) Uani 1 1 d . . . . .
C41 C 0.1315(2) 0.6875(3) -0.14605(12) 0.0243(7) Uani 1 1 d . . . . .
H41 H 0.1522 0.6744 -0.1754 0.029 Uiso 1 1 calc R U . . .
C42 C 0.1966(2) 0.7150(2) -0.10345(11) 0.0189(6) Uani 1 1 d . . . . .
H42 H 0.2612 0.7201 -0.1048 0.023 Uiso 1 1 calc R U . . .
C13 C 0.6137(2) 0.4956(3) 0.37406(11) 0.0210(7) Uani 1 1 d . . . . .
H13A H 0.5842 0.5742 0.3713 0.025 Uiso 1 1 calc R U . . .
H13B H 0.6618 0.4928 0.4046 0.025 Uiso 1 1 calc R U . . .
C32 C 0.3007(2) 0.9432(3) 0.05110(11) 0.0232(7) Uani 1 1 d . . . . .
H32 H 0.3589 0.9032 0.0609 0.028 Uiso 1 1 calc R U . . .
C37 C 0.1710(2) 0.7352(2) -0.05923(11) 0.0168(6) Uani 1 1 d . . . . .
C19 C 0.2404(2) 0.6573(3) 0.03098(11) 0.0187(6) Uani 1 1 d . . . . .
C26 C 0.4032(2) 0.6513(3) -0.02164(11) 0.0196(6) Uani 1 1 d . . . . .
H26 H 0.3769 0.5813 -0.0119 0.024 Uiso 1 1 calc R U . . .
C38 C 0.0745(2) 0.7245(3) -0.05955(12) 0.0214(7) Uani 1 1 d . . . . .
H38 H 0.0534 0.7359 -0.0302 0.026 Uiso 1 1 calc R U . . .
C25 C 0.3542(2) 0.7574(3) -0.02049(10) 0.0170(6) Uani 1 1 d . . . . .
C28 C 0.5307(2) 0.7457(3) -0.05046(10) 0.0189(6) Uani 1 1 d . . . . .
H28 H 0.5890 0.7418 -0.0605 0.023 Uiso 1 1 calc R U . . .
C7 C 0.7616(2) 0.4945(3) 0.34558(11) 0.0198(6) Uani 1 1 d . . . . .
H7A H 0.7754 0.5655 0.3660 0.024 Uiso 1 1 calc R U . . .
H7B H 0.7877 0.5055 0.3162 0.024 Uiso 1 1 calc R U . . .
C30 C 0.3991(2) 0.8577(3) -0.03492(11) 0.0201(6) Uani 1 1 d . . . . .
H30 H 0.3693 0.9318 -0.0348 0.024 Uiso 1 1 calc R U . . .
C31 C 0.2308(2) 0.8928(3) 0.01448(11) 0.0178(6) Uani 1 1 d . . . . .
C22 C 0.2421(2) 0.4662(3) 0.09754(13) 0.0286(8) Uani 1 1 d . . . . .
H22 H 0.2431 0.4031 0.1197 0.034 Uiso 1 1 calc R U . . .
C8 C 0.8045(2) 0.3887(3) 0.37310(10) 0.0186(6) Uani 1 1 d . . . . .
C29 C 0.4848(2) 0.8521(3) -0.04919(11) 0.0214(6) Uani 1 1 d . . . . .
H29 H 0.5124 0.9220 -0.0582 0.026 Uiso 1 1 calc R U . . .
C16 C 0.4649(2) 0.2307(3) 0.36839(12) 0.0256(7) Uani 1 1 d . . . . .
C15 C 0.4116(3) 0.3243(3) 0.39233(14) 0.0333(8) Uani 1 1 d . . . . .
H15A H 0.3508 0.3443 0.3708 0.040 Uiso 1 1 calc R U . . .
H15B H 0.3996 0.2953 0.4236 0.040 Uiso 1 1 calc R U . . .
C9 C 0.9167(2) 0.2807(3) 0.41876(13) 0.0273(8) Uani 1 1 d . . . . .
H9A H 0.9434 0.2821 0.4540 0.033 Uiso 1 1 calc R U . . .
H9B H 0.9633 0.2456 0.4019 0.033 Uiso 1 1 calc R U . . .
C35 C 0.1352(2) 1.0661(3) 0.02282(12) 0.0267(7) Uani 1 1 d . . . . .
H35 H 0.0780 1.1078 0.0124 0.032 Uiso 1 1 calc R U . . .
C23 C 0.2817(2) 0.5742(3) 0.11286(12) 0.0290(8) Uani 1 1 d . . . . .
H23 H 0.3104 0.5852 0.1460 0.035 Uiso 1 1 calc R U . . .
C14 C 0.5405(2) 0.4035(3) 0.37493(11) 0.0207(6) Uani 1 1 d . . . . .
C6 C 0.6220(3) 0.2817(3) 0.17530(13) 0.0369(9) Uani 1 1 d . . . . .
H6A H 0.5990 0.2554 0.1418 0.055 Uiso 1 1 calc R U . . .
H6B H 0.6624 0.2210 0.1934 0.055 Uiso 1 1 calc R U . . .
H6C H 0.6582 0.3542 0.1753 0.055 Uiso 1 1 calc R U . . .
C27 C 0.4890(2) 0.6445(3) -0.03655(11) 0.0212(7) Uani 1 1 d . . . . .
H27 H 0.5191 0.5708 -0.0372 0.025 Uiso 1 1 calc R U . . .
C40 C 0.0369(2) 0.6795(3) -0.14530(12) 0.0269(7) Uani 1 1 d . . . . .
H40 H -0.0080 0.6619 -0.1740 0.032 Uiso 1 1 calc R U . . .
C1 C 0.6114(2) 0.5423(3) 0.28824(11) 0.0219(7) Uani 1 1 d . . . . .
H1A H 0.5607 0.5912 0.2964 0.026 Uiso 1 1 calc R U . . .
H1B H 0.6574 0.5950 0.2777 0.026 Uiso 1 1 calc R U . . .
C36 C 0.1488(2) 0.9591(3) 0.00133(11) 0.0214(7) Uani 1 1 d . . . . .
H36 H 0.0998 0.9299 -0.0235 0.026 Uiso 1 1 calc R U . . .
C20 C 0.2005(2) 0.5476(3) 0.01646(12) 0.0260(7) Uani 1 1 d . . . . .
H20 H 0.1717 0.5364 -0.0167 0.031 Uiso 1 1 calc R U . . .
C33 C 0.2879(2) 1.0491(3) 0.07348(12) 0.0258(7) Uani 1 1 d . . . . .
H33 H 0.3363 1.0786 0.0986 0.031 Uiso 1 1 calc R U . . .
C10 C 0.8236(2) 0.2112(3) 0.40773(12) 0.0237(7) Uani 1 1 d . . . . .
C39 C 0.0086(2) 0.6977(3) -0.10176(13) 0.0282(8) Uani 1 1 d . . . . .
H39 H -0.0561 0.6919 -0.1007 0.034 Uiso 1 1 calc R U . . .
C11 C 0.7782(3) 0.2024(3) 0.45169(13) 0.0324(8) Uani 1 1 d . . . . .
H11A H 0.7746 0.2806 0.4655 0.049 Uiso 1 1 calc R U . . .
H11B H 0.8162 0.1511 0.4760 0.049 Uiso 1 1 calc R U . . .
H11C H 0.7148 0.1698 0.4417 0.049 Uiso 1 1 calc R U . . .
C34 C 0.2050(3) 1.1118(3) 0.05934(13) 0.0294(8) Uani 1 1 d . . . . .
H34 H 0.1962 1.1844 0.0743 0.035 Uiso 1 1 calc R U . . .
C2 C 0.5713(2) 0.4608(3) 0.24827(11) 0.0229(7) Uani 1 1 d . . . . .
C17 C 0.5078(3) 0.1365(3) 0.40415(14) 0.0360(9) Uani 1 1 d . . . . .
H17A H 0.5471 0.0848 0.3890 0.054 Uiso 1 1 calc R U . . .
H17B H 0.4575 0.0905 0.4136 0.054 Uiso 1 1 calc R U . . .
H17C H 0.5463 0.1732 0.4329 0.054 Uiso 1 1 calc R U . . .
C21 C 0.2010(3) 0.4536(3) 0.04865(13) 0.0328(8) Uani 1 1 d . . . . .
H21 H 0.1732 0.3810 0.0370 0.039 Uiso 1 1 calc R U . . .
C18 C 0.4052(3) 0.1770(4) 0.32292(14) 0.0413(10) Uani 1 1 d . . . . .
H18A H 0.3804 0.2394 0.2999 0.062 Uiso 1 1 calc R U . . .
H18B H 0.3529 0.1334 0.3314 0.062 Uiso 1 1 calc R U . . .
H18C H 0.4439 0.1237 0.3081 0.062 Uiso 1 1 calc R U . . .
C5 C 0.4790(3) 0.1945(4) 0.19976(15) 0.0482(11) Uani 1 1 d . . . . .
H5A H 0.4243 0.2119 0.2138 0.072 Uiso 1 1 calc R U . . .
H5B H 0.5173 0.1339 0.2191 0.072 Uiso 1 1 calc R U . . .
H5C H 0.4577 0.1664 0.1664 0.072 Uiso 1 1 calc R U . . .
C3 C 0.4851(3) 0.4109(4) 0.17715(14) 0.0419(10) Uani 1 1 d . . . . .
H3A H 0.4916 0.4197 0.1431 0.050 Uiso 1 1 calc R U . . .
H3B H 0.4175 0.4047 0.1778 0.050 Uiso 1 1 calc R U . . .
C12 C 0.8362(3) 0.0911(3) 0.38594(13) 0.0376(9) Uani 1 1 d . . . . .
H12A H 0.7754 0.0509 0.3780 0.056 Uiso 1 1 calc R U . . .
H12B H 0.8804 0.0443 0.4094 0.056 Uiso 1 1 calc R U . . .
H12C H 0.8609 0.1012 0.3564 0.056 Uiso 1 1 calc R U . . .
B1 B 0.2489(2) 0.7628(3) -0.00825(12) 0.0159(7) Uani 1 1 d . . . . .
C43 C 0.3271(4) 0.6020(4) 0.32151(17) 0.0605(13) Uani 1 1 d . . . . .
H43A H 0.2803 0.5598 0.3360 0.073 Uiso 1 1 calc R U . . .
H43B H 0.3844 0.6126 0.3471 0.073 Uiso 1 1 calc R U . . .
C44 C 0.4467(4) 0.8212(9) 0.1786(3) 0.076(3) Uani 0.7 1 d D U P A 1
H44A H 0.4348 0.7363 0.1732 0.091 Uiso 0.7 1 calc R U P A 1
H44B H 0.4466 0.8581 0.1468 0.091 Uiso 0.7 1 calc R U P A 1
C45 C 0.4457(6) 0.7780(10) 0.2022(7) 0.080(5) Uani 0.3 1 d D U P A 2
H45A H 0.4415 0.7148 0.2257 0.096 Uiso 0.3 1 calc R U P A 2
H45B H 0.4361 0.7425 0.1695 0.096 Uiso 0.3 1 calc 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
Ni1 N3 2.033(3) . ?
Ni1 O4 2.046(2) . ?
Ni1 N1 2.061(3) . ?
Ni1 N2 2.071(3) . ?
Ni1 N4 2.215(3) . ?
Ni1 O5 2.331(2) . ?
Cl1 C43 1.766(4) . ?
Cl2 C43 1.732(5) . ?
Cl3 C45 1.721(9) . ?
Cl3 C44 1.730(6) . ?
O2 C8 1.341(4) . ?
O2 C9 1.468(4) . ?
O5 N5 1.263(3) . ?
O3 C14 1.333(4) . ?
O3 C15 1.463(4) . ?
N4 C7 1.479(4) . ?
N4 C13 1.490(4) . ?
N4 C1 1.496(4) . ?
O6 N5 1.233(3) . ?
Cl4 C44 1.756(7) . ?
Cl4 C45 1.768(10) . ?
O1 C2 1.348(4) . ?
O1 C3 1.463(4) . ?
N1 C2 1.275(4) . ?
N1 C4 1.513(4) . ?
O4 N5 1.281(3) . ?
N2 C8 1.279(4) . ?
N2 C10 1.496(4) . ?
N3 C14 1.268(4) . ?
N3 C16 1.497(4) . ?
C4 C3 1.497(5) . ?
C4 C5 1.516(5) . ?
C4 C6 1.554(5) . ?
C24 C23 1.387(5) . ?
C24 C19 1.402(4) . ?
C24 H24 0.9500 . ?
C41 C40 1.383(5) . ?
C41 C42 1.402(4) . ?
C41 H41 0.9500 . ?
C42 C37 1.393(4) . ?
C42 H42 0.9500 . ?
C13 C14 1.500(4) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C32 C33 1.394(4) . ?
C32 C31 1.412(4) . ?
C32 H32 0.9500 . ?
C37 C38 1.408(4) . ?
C37 B1 1.665(4) . ?
C19 C20 1.405(4) . ?
C19 B1 1.656(4) . ?
C26 C27 1.400(4) . ?
C26 C25 1.408(4) . ?
C26 H26 0.9500 . ?
C38 C39 1.398(5) . ?
C38 H38 0.9500 . ?
C25 C30 1.419(4) . ?
C25 B1 1.639(4) . ?
C28 C29 1.390(4) . ?
C28 C27 1.397(4) . ?
C28 H28 0.9500 . ?
C7 C8 1.499(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C30 C29 1.389(4) . ?
C30 H30 0.9500 . ?
C31 C36 1.395(4) . ?
C31 B1 1.659(4) . ?
C22 C23 1.391(5) . ?
C22 C21 1.391(5) . ?
C22 H22 0.9500 . ?
C29 H29 0.9500 . ?
C16 C17 1.516(5) . ?
C16 C18 1.519(5) . ?
C16 C15 1.554(5) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C9 C10 1.544(5) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C35 C34 1.388(5) . ?
C35 C36 1.395(4) . ?
C35 H35 0.9500 . ?
C23 H23 0.9500 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C27 H27 0.9500 . ?
C40 C39 1.389(5) . ?
C40 H40 0.9500 . ?
C1 C2 1.484(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C36 H36 0.9500 . ?
C20 C21 1.403(4) . ?
C20 H20 0.9500 . ?
C33 C34 1.387(5) . ?
C33 H33 0.9500 . ?
C10 C11 1.524(5) . ?
C10 C12 1.527(5) . ?
C39 H39 0.9500 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C34 H34 0.9500 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C21 H21 0.9500 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Ni1 O4 98.66(9) . . ?
N3 Ni1 N1 100.35(11) . . ?
O4 Ni1 N1 101.38(10) . . ?
N3 Ni1 N2 100.56(11) . . ?
O4 Ni1 N2 100.37(9) . . ?
N1 Ni1 N2 147.00(10) . . ?
N3 Ni1 N4 80.94(10) . . ?
O4 Ni1 N4 178.14(9) . . ?
N1 Ni1 N4 80.48(10) . . ?
N2 Ni1 N4 77.94(9) . . ?
N3 Ni1 O5 157.32(9) . . ?
O4 Ni1 O5 58.73(8) . . ?
N1 Ni1 O5 87.13(9) . . ?
N2 Ni1 O5 83.29(9) . . ?
N4 Ni1 O5 121.59(8) . . ?
C8 O2 C9 104.8(2) . . ?
N5 O5 Ni1 86.13(16) . . ?
C14 O3 C15 105.5(2) . . ?
C7 N4 C13 111.1(2) . . ?
C7 N4 C1 113.8(2) . . ?
C13 N4 C1 111.8(2) . . ?
C7 N4 Ni1 104.52(17) . . ?
C13 N4 Ni1 105.64(17) . . ?
C1 N4 Ni1 109.49(18) . . ?
C2 O1 C3 103.4(3) . . ?
C2 N1 C4 106.6(3) . . ?
C2 N1 Ni1 114.3(2) . . ?
C4 N1 Ni1 138.8(2) . . ?
N5 O4 Ni1 98.81(17) . . ?
C8 N2 C10 107.4(3) . . ?
C8 N2 Ni1 111.2(2) . . ?
C10 N2 Ni1 140.66(19) . . ?
C14 N3 C16 108.3(3) . . ?
C14 N3 Ni1 114.0(2) . . ?
C16 N3 Ni1 137.7(2) . . ?
C3 C4 N1 100.8(3) . . ?
C3 C4 C5 116.0(3) . . ?
N1 C4 C5 112.2(3) . . ?
C3 C4 C6 109.1(3) . . ?
N1 C4 C6 107.1(3) . . ?
C5 C4 C6 110.9(3) . . ?
C23 C24 C19 123.1(3) . . ?
C23 C24 H24 118.4 . . ?
C19 C24 H24 118.4 . . ?
O6 N5 O5 122.6(3) . . ?
O6 N5 O4 121.1(3) . . ?
O5 N5 O4 116.3(2) . . ?
C40 C41 C42 119.9(3) . . ?
C40 C41 H41 120.0 . . ?
C42 C41 H41 120.0 . . ?
C37 C42 C41 123.0(3) . . ?
C37 C42 H42 118.5 . . ?
C41 C42 H42 118.5 . . ?
N4 C13 C14 109.5(2) . . ?
N4 C13 H13A 109.8 . . ?
C14 C13 H13A 109.8 . . ?
N4 C13 H13B 109.8 . . ?
C14 C13 H13B 109.8 . . ?
H13A C13 H13B 108.2 . . ?
C33 C32 C31 122.7(3) . . ?
C33 C32 H32 118.7 . . ?
C31 C32 H32 118.7 . . ?
C42 C37 C38 115.6(3) . . ?
C42 C37 B1 123.0(3) . . ?
C38 C37 B1 121.3(3) . . ?
C24 C19 C20 114.6(3) . . ?
C24 C19 B1 122.8(3) . . ?
C20 C19 B1 122.4(3) . . ?
C27 C26 C25 122.8(3) . . ?
C27 C26 H26 118.6 . . ?
C25 C26 H26 118.6 . . ?
C39 C38 C37 122.0(3) . . ?
C39 C38 H38 119.0 . . ?
C37 C38 H38 119.0 . . ?
C26 C25 C30 114.9(3) . . ?
C26 C25 B1 122.5(3) . . ?
C30 C25 B1 122.4(3) . . ?
C29 C28 C27 118.4(3) . . ?
C29 C28 H28 120.8 . . ?
C27 C28 H28 120.8 . . ?
N4 C7 C8 107.5(2) . . ?
N4 C7 H7A 110.2 . . ?
C8 C7 H7A 110.2 . . ?
N4 C7 H7B 110.2 . . ?
C8 C7 H7B 110.2 . . ?
H7A C7 H7B 108.5 . . ?
C29 C30 C25 122.8(3) . . ?
C29 C30 H30 118.6 . . ?
C25 C30 H30 118.6 . . ?
C36 C31 C32 114.8(3) . . ?
C36 C31 B1 125.3(3) . . ?
C32 C31 B1 119.9(3) . . ?
C23 C22 C21 117.6(3) . . ?
C23 C22 H22 121.2 . . ?
C21 C22 H22 121.2 . . ?
N2 C8 O2 118.8(3) . . ?
N2 C8 C7 123.5(3) . . ?
O2 C8 C7 117.7(3) . . ?
C30 C29 C28 120.8(3) . . ?
C30 C29 H29 119.6 . . ?
C28 C29 H29 119.6 . . ?
N3 C16 C17 109.8(3) . . ?
N3 C16 C18 109.5(3) . . ?
C17 C16 C18 111.1(3) . . ?
N3 C16 C15 100.9(3) . . ?
C17 C16 C15 111.8(3) . . ?
C18 C16 C15 113.3(3) . . ?
O3 C15 C16 104.9(3) . . ?
O3 C15 H15A 110.8 . . ?
C16 C15 H15A 110.8 . . ?
O3 C15 H15B 110.8 . . ?
C16 C15 H15B 110.8 . . ?
H15A C15 H15B 108.8 . . ?
O2 C9 C10 104.8(2) . . ?
O2 C9 H9A 110.8 . . ?
C10 C9 H9A 110.8 . . ?
O2 C9 H9B 110.8 . . ?
C10 C9 H9B 110.8 . . ?
H9A C9 H9B 108.9 . . ?
C34 C35 C36 120.2(3) . . ?
C34 C35 H35 119.9 . . ?
C36 C35 H35 119.9 . . ?
C24 C23 C22 121.2(3) . . ?
C24 C23 H23 119.4 . . ?
C22 C23 H23 119.4 . . ?
N3 C14 O3 118.7(3) . . ?
N3 C14 C13 123.4(3) . . ?
O3 C14 C13 117.9(3) . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C28 C27 C26 120.3(3) . . ?
C28 C27 H27 119.8 . . ?
C26 C27 H27 119.8 . . ?
C41 C40 C39 118.8(3) . . ?
C41 C40 H40 120.6 . . ?
C39 C40 H40 120.6 . . ?
C2 C1 N4 110.2(2) . . ?
C2 C1 H1A 109.6 . . ?
N4 C1 H1A 109.6 . . ?
C2 C1 H1B 109.6 . . ?
N4 C1 H1B 109.6 . . ?
H1A C1 H1B 108.1 . . ?
C31 C36 C35 123.3(3) . . ?
C31 C36 H36 118.3 . . ?
C35 C36 H36 118.3 . . ?
C21 C20 C19 123.1(3) . . ?
C21 C20 H20 118.5 . . ?
C19 C20 H20 118.5 . . ?
C34 C33 C32 120.5(3) . . ?
C34 C33 H33 119.8 . . ?
C32 C33 H33 119.8 . . ?
N2 C10 C11 106.7(3) . . ?
N2 C10 C12 111.9(3) . . ?
C11 C10 C12 112.2(3) . . ?
N2 C10 C9 101.6(2) . . ?
C11 C10 C9 112.3(3) . . ?
C12 C10 C9 111.6(3) . . ?
C40 C39 C38 120.6(3) . . ?
C40 C39 H39 119.7 . . ?
C38 C39 H39 119.7 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C33 C34 C35 118.5(3) . . ?
C33 C34 H34 120.7 . . ?
C35 C34 H34 120.7 . . ?
N1 C2 O1 118.3(3) . . ?
N1 C2 C1 125.5(3) . . ?
O1 C2 C1 116.2(3) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C22 C21 C20 120.4(3) . . ?
C22 C21 H21 119.8 . . ?
C20 C21 H21 119.8 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O1 C3 C4 105.9(3) . . ?
O1 C3 H3A 110.6 . . ?
C4 C3 H3A 110.6 . . ?
O1 C3 H3B 110.6 . . ?
C4 C3 H3B 110.6 . . ?
H3A C3 H3B 108.7 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C25 B1 C19 108.4(2) . . ?
C25 B1 C31 110.2(2) . . ?
C19 B1 C31 110.6(2) . . ?
C25 B1 C37 108.0(2) . . ?
C19 B1 C37 107.9(2) . . ?
C31 B1 C37 111.6(2) . . ?
Cl2 C43 Cl1 113.0(3) . . ?
Cl2 C43 H43A 109.0 . . ?
Cl1 C43 H43A 109.0 . . ?
Cl2 C43 H43B 109.0 . . ?
Cl1 C43 H43B 109.0 . . ?
H43A C43 H43B 107.8 . . ?
Cl3 C44 Cl4 111.5(4) . . ?
Cl3 C44 H44A 109.3 . . ?
Cl4 C44 H44A 109.3 . . ?
Cl3 C44 H44B 109.3 . . ?
Cl4 C44 H44B 109.3 . . ?
H44A C44 H44B 108.0 . . ?
Cl3 C45 Cl4 111.3(6) . . ?
Cl3 C45 H45A 109.4 . . ?
Cl4 C45 H45A 109.4 . . ?
Cl3 C45 H45B 109.4 . . ?
Cl4 C45 H45B 109.4 . . ?
H45A C45 H45B 108.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 N1 C4 C3 -17.2(4) . . . . ?
Ni1 N1 C4 C3 170.1(3) . . . . ?
C2 N1 C4 C5 -141.3(3) . . . . ?
Ni1 N1 C4 C5 46.0(5) . . . . ?
C2 N1 C4 C6 96.8(3) . . . . ?
Ni1 N1 C4 C6 -75.9(4) . . . . ?
Ni1 O5 N5 O6 -178.2(3) . . . . ?
Ni1 O5 N5 O4 1.4(2) . . . . ?
Ni1 O4 N5 O6 178.0(2) . . . . ?
Ni1 O4 N5 O5 -1.6(3) . . . . ?
C40 C41 C42 C37 0.0(5) . . . . ?
C7 N4 C13 C14 -139.0(3) . . . . ?
C1 N4 C13 C14 92.8(3) . . . . ?
Ni1 N4 C13 C14 -26.2(3) . . . . ?
C41 C42 C37 C38 0.9(4) . . . . ?
C41 C42 C37 B1 177.6(3) . . . . ?
C23 C24 C19 C20 1.0(5) . . . . ?
C23 C24 C19 B1 -173.3(3) . . . . ?
C42 C37 C38 C39 -1.2(4) . . . . ?
B1 C37 C38 C39 -178.0(3) . . . . ?
C27 C26 C25 C30 -0.9(4) . . . . ?
C27 C26 C25 B1 173.7(3) . . . . ?
C13 N4 C7 C8 77.8(3) . . . . ?
C1 N4 C7 C8 -155.0(2) . . . . ?
Ni1 N4 C7 C8 -35.6(2) . . . . ?
C26 C25 C30 C29 0.1(4) . . . . ?
B1 C25 C30 C29 -174.5(3) . . . . ?
C33 C32 C31 C36 1.9(4) . . . . ?
C33 C32 C31 B1 -176.5(3) . . . . ?
C10 N2 C8 O2 4.7(4) . . . . ?
Ni1 N2 C8 O2 -167.6(2) . . . . ?
C10 N2 C8 C7 -174.4(3) . . . . ?
Ni1 N2 C8 C7 13.3(4) . . . . ?
C9 O2 C8 N2 6.0(4) . . . . ?
C9 O2 C8 C7 -174.8(3) . . . . ?
N4 C7 C8 N2 17.6(4) . . . . ?
N4 C7 C8 O2 -161.5(2) . . . . ?
C25 C30 C29 C28 0.7(5) . . . . ?
C27 C28 C29 C30 -0.7(4) . . . . ?
C14 N3 C16 C17 -107.9(3) . . . . ?
Ni1 N3 C16 C17 69.6(4) . . . . ?
C14 N3 C16 C18 129.9(3) . . . . ?
Ni1 N3 C16 C18 -52.6(4) . . . . ?
C14 N3 C16 C15 10.2(4) . . . . ?
Ni1 N3 C16 C15 -172.2(3) . . . . ?
C14 O3 C15 C16 11.5(4) . . . . ?
N3 C16 C15 O3 -12.9(3) . . . . ?
C17 C16 C15 O3 103.8(3) . . . . ?
C18 C16 C15 O3 -129.9(3) . . . . ?
C8 O2 C9 C10 -13.4(3) . . . . ?
C19 C24 C23 C22 -0.8(5) . . . . ?
C21 C22 C23 C24 0.1(5) . . . . ?
C16 N3 C14 O3 -3.5(4) . . . . ?
Ni1 N3 C14 O3 178.3(2) . . . . ?
C16 N3 C14 C13 173.2(3) . . . . ?
Ni1 N3 C14 C13 -5.0(4) . . . . ?
C15 O3 C14 N3 -5.5(4) . . . . ?
C15 O3 C14 C13 177.5(3) . . . . ?
N4 C13 C14 N3 23.2(4) . . . . ?
N4 C13 C14 O3 -160.0(3) . . . . ?
C29 C28 C27 C26 -0.1(4) . . . . ?
C25 C26 C27 C28 1.0(5) . . . . ?
C42 C41 C40 C39 -0.8(5) . . . . ?
C7 N4 C1 C2 115.4(3) . . . . ?
C13 N4 C1 C2 -117.9(3) . . . . ?
Ni1 N4 C1 C2 -1.2(3) . . . . ?
C32 C31 C36 C35 -1.0(4) . . . . ?
B1 C31 C36 C35 177.3(3) . . . . ?
C34 C35 C36 C31 -0.1(5) . . . . ?
C24 C19 C20 C21 -0.7(5) . . . . ?
B1 C19 C20 C21 173.6(3) . . . . ?
C31 C32 C33 C34 -1.7(5) . . . . ?
C8 N2 C10 C11 105.3(3) . . . . ?
Ni1 N2 C10 C11 -86.0(4) . . . . ?
C8 N2 C10 C12 -131.6(3) . . . . ?
Ni1 N2 C10 C12 37.0(5) . . . . ?
C8 N2 C10 C9 -12.5(3) . . . . ?
Ni1 N2 C10 C9 156.2(3) . . . . ?
O2 C9 C10 N2 15.5(3) . . . . ?
O2 C9 C10 C11 -98.1(3) . . . . ?
O2 C9 C10 C12 134.9(3) . . . . ?
C41 C40 C39 C38 0.5(5) . . . . ?
C37 C38 C39 C40 0.6(5) . . . . ?
C32 C33 C34 C35 0.5(5) . . . . ?
C36 C35 C34 C33 0.4(5) . . . . ?
C4 N1 C2 O1 5.7(4) . . . . ?
Ni1 N1 C2 O1 -179.5(2) . . . . ?
C4 N1 C2 C1 -172.9(3) . . . . ?
Ni1 N1 C2 C1 1.9(4) . . . . ?
C3 O1 C2 N1 8.9(4) . . . . ?
C3 O1 C2 C1 -172.3(3) . . . . ?
N4 C1 C2 N1 -0.4(4) . . . . ?
N4 C1 C2 O1 -179.0(3) . . . . ?
C23 C22 C21 C20 0.2(5) . . . . ?
C19 C20 C21 C22 0.2(5) . . . . ?
C2 O1 C3 C4 -19.6(4) . . . . ?
N1 C4 C3 O1 22.1(4) . . . . ?
C5 C4 C3 O1 143.5(3) . . . . ?
C6 C4 C3 O1 -90.5(3) . . . . ?
C26 C25 B1 C19 33.2(4) . . . . ?
C30 C25 B1 C19 -152.6(3) . . . . ?
C26 C25 B1 C31 154.4(3) . . . . ?
C30 C25 B1 C31 -31.4(4) . . . . ?
C26 C25 B1 C37 -83.5(3) . . . . ?
C30 C25 B1 C37 90.8(3) . . . . ?
C24 C19 B1 C25 77.9(3) . . . . ?
C20 C19 B1 C25 -96.0(3) . . . . ?
C24 C19 B1 C31 -43.1(4) . . . . ?
C20 C19 B1 C31 143.1(3) . . . . ?
C24 C19 B1 C37 -165.4(3) . . . . ?
C20 C19 B1 C37 20.7(4) . . . . ?
C36 C31 B1 C25 135.7(3) . . . . ?
C32 C31 B1 C25 -46.0(4) . . . . ?
C36 C31 B1 C19 -104.4(3) . . . . ?
C32 C31 B1 C19 73.8(3) . . . . ?
C36 C31 B1 C37 15.8(4) . . . . ?
C32 C31 B1 C37 -166.0(3) . . . . ?
C42 C37 B1 C25 -1.6(4) . . . . ?
C38 C37 B1 C25 174.9(3) . . . . ?
C42 C37 B1 C19 -118.6(3) . . . . ?
C38 C37 B1 C19 57.9(3) . . . . ?
C42 C37 B1 C31 119.7(3) . . . . ?
C38 C37 B1 C31 -63.8(3) . . . . ?

_refine_diff_density_max         1.826
_refine_diff_density_min         -1.399
_refine_diff_density_rms         0.097

####################################################################### 
# 
# 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_shelx_CCDC4
_database_code_depnum_ccdc_archive 'CCDC 1983779'
loop_
_audit_author_name
_audit_author_address
'Shiro Hikichi'
;Kanagawa University
Japan
;
_audit_update_record             
;
2020-02-13 deposited with the CCDC.	2020-04-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        '[Ni(mCBA)(TOAMe2)(OH2)](BPh4)'
_chemical_name_common            
'[(3-chlorobenzoato)aquatris{(4,4-dimethyloxazolin-2-yl)methyl}aminenickel(II)]tetraphenylborate'
_chemical_melting_point          ?
_chemical_formula_moiety         ' C25 H36 Cl N4 Ni O6, C24 H20 B '
_chemical_formula_sum            'C49 H56 B Cl N4 Ni O6  '
_chemical_formula_weight         901.93

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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_H-M_alt        'F d d 2'
_space_group_name_Hall           'F 2 -2d'

_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'
'-x+1/4, y+1/4, z+1/4'
'x+1/4, -y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x+1/4, y+3/4, z+3/4'
'x+1/4, -y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'-x+3/4, y+1/4, z+3/4'
'x+3/4, -y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+3/4, y+3/4, z+1/4'
'x+3/4, -y+3/4, z+1/4'

_cell_length_a                   63.3792(17)
_cell_length_b                   58.8576(15)
_cell_length_c                   9.7929(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     36530.9(15)
_cell_formula_units_Z            32
_cell_measurement_temperature    113(2)
_cell_measurement_reflns_used    21176
_cell_measurement_theta_min      1.5258
_cell_measurement_theta_max      27.4815

_exptl_crystal_description       needle
_exptl_crystal_colour            Green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_F_000             15232
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.537
_shelx_estimated_absorpt_T_min   0.775
_shelx_estimated_absorpt_T_max   0.948
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_correction_T_max  0.9524
_exptl_absorpt_correction_T_min  0.8348
_exptl_absorpt_process_details   
;Numerical (Based on real shape of the crystal) absorption
correction was parformed on CrystalClear (Rigaku Inc., 2007)
with FS_ABSCOR method.
;
_exptl_absorpt_special_details   ?


_diffrn_special_details          
;
 ?
;

_diffrn_source_power             3.0000
_diffrn_source_voltage           50.0000
_diffrn_source_current           60.0000
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_detector       CCD
_diffrn_measurement_device       
;
Saturn70 (2x2 bin mode)
;
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_theta_full        27.4815
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_measurement_details      
;
scan:
	Number of images: 600
	           Slice: -115.0000 - 65.0000
	     Image width: 0.3000
	        Exp time: 30.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 0.0000
	             XTD: 54.8475
	          2theta: -25.1967
scan:
	Number of images: 600
	           Slice: -115.0000 - 65.0000
	     Image width: 0.3000
	        Exp time: 30.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 90.0000
	             XTD: 54.8475
	          2theta: -25.1967
scan:
	Number of images: 600
	           Slice: -115.0000 - 65.0000
	     Image width: 0.3000
	        Exp time: 30.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 180.0000
	             XTD: 54.8475
	          2theta: -25.1967

;
_diffrn_measurement_device_details 
;
AFC10: Fixed Chi 2 circle
;
_diffrn_orient_matrix_UB_11      -0.0962
_diffrn_orient_matrix_UB_12      -0.0338
_diffrn_orient_matrix_UB_13      -0.0062
_diffrn_orient_matrix_UB_21      0.0057
_diffrn_orient_matrix_UB_22      -0.0159
_diffrn_orient_matrix_UB_23      -0.0014
_diffrn_orient_matrix_UB_31      -0.0005
_diffrn_orient_matrix_UB_32      -0.0016
_diffrn_orient_matrix_UB_33      0.0157
_diffrn_orient_matrix_type       d*Trek


_diffrn_ambient_temperature      113(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ω
_diffrn_reflns_number            83891
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_limit_h_min       -80
_diffrn_reflns_limit_h_max       82
_diffrn_reflns_limit_k_min       -76
_diffrn_reflns_limit_k_max       76
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.526
_diffrn_reflns_theta_max         27.481
_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 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             20846
_reflns_number_gt                19997
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.882
_reflns_Friedel_fraction_max     0.991
_reflns_Friedel_fraction_full    0.991

_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       'CrystalClear (Rigaku Inc., 2007)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        
'CrystalClear (Rigaku Inc., 2007), SORTAV (Blessing, 1995)'
_computing_structure_solution    'SHELXS (Sheldrick, 2002)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0311P)²+0.0454P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 8191 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.010(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         20846
_refine_ls_number_parameters     1145
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0370
_refine_ls_wR_factor_ref         0.0770
_refine_ls_wR_factor_gt          0.0757
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_restrained_S_all      1.152
_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 0.75867(2) 0.15116(2) 0.18538(4) 0.01658(8) Uani 1 1 d . . . . .
Ni2 Ni 0.64702(2) 0.02375(2) 0.18631(4) 0.02001(8) Uani 1 1 d . . . . .
Cl1 Cl 0.77872(2) 0.25649(2) 0.71159(9) 0.0431(2) Uani 1 1 d . . . . .
Cl2 Cl 0.62190(2) 0.12505(2) -0.35805(10) 0.0532(3) Uani 1 1 d . . . . .
O2 O 0.69893(3) 0.12787(4) 0.2837(2) 0.0288(5) Uani 1 1 d . . . . .
O10 O 0.64716(3) 0.05513(3) 0.1021(2) 0.0248(5) Uani 1 1 d . . . . .
O4 O 0.76863(3) 0.18150(3) 0.2568(2) 0.0225(4) Uani 1 1 d . . . . .
O6 O 0.76149(4) 0.13535(4) 0.3848(2) 0.0235(5) Uani 1 1 d . . . . .
O3 O 0.73955(3) 0.15829(3) -0.2161(2) 0.0213(4) Uani 1 1 d . . . . .
O1 O 0.80084(3) 0.10227(3) 0.0577(2) 0.0265(5) Uani 1 1 d . . . . .
O5 O 0.77456(4) 0.17504(3) 0.4798(2) 0.0265(5) Uani 1 1 d . . . . .
O12 O 0.63481(4) 0.00904(4) 0.0037(2) 0.0269(5) Uani 1 1 d . . . . .
O8 O 0.68503(4) -0.03025(3) 0.0642(2) 0.0300(5) Uani 1 1 d . . . . .
O7 O 0.59088(4) 0.00364(4) 0.3630(3) 0.0354(6) Uani 1 1 d . . . . .
N2 N 0.78701(4) 0.13512(4) 0.1349(2) 0.0195(5) Uani 1 1 d . . . . .
O11 O 0.64266(4) 0.04786(4) -0.1201(2) 0.0305(5) Uani 1 1 d . . . . .
O9 O 0.67649(4) 0.02364(4) 0.5619(2) 0.0329(5) Uani 1 1 d . . . . .
N3 N 0.72650(4) 0.15120(4) 0.2423(2) 0.0187(5) Uani 1 1 d . . . . .
C20 C 0.77580(4) 0.21306(5) 0.3982(3) 0.0202(6) Uani 1 1 d . . . . .
N4 N 0.75327(4) 0.16523(4) -0.0079(2) 0.0183(5) Uani 1 1 d . . . . .
N7 N 0.67472(4) 0.00561(4) 0.1108(2) 0.0217(5) Uani 1 1 d . . . . .
C9 C 0.69125(5) 0.15063(5) 0.3207(4) 0.0282(7) Uani 1 1 d . . . . .
H9A H 0.6850 0.1506 0.4133 0.034 Uiso 1 1 calc R U . . .
H9B H 0.6805 0.1560 0.2546 0.034 Uiso 1 1 calc R U . . .
N8 N 0.66069(4) 0.03510(4) 0.3683(3) 0.0221(5) Uani 1 1 d . . . . .
C98 C 0.25311(5) 0.03061(5) 0.2309(3) 0.0281(7) Uani 1 1 d . . . . .
H98 H 0.2432 0.0313 0.1581 0.034 Uiso 1 1 calc R U . . .
C44 C 0.64296(4) 0.20289(5) 0.1912(3) 0.0233(6) Uani 1 1 d . . . . .
C21 C 0.77559(5) 0.22207(5) 0.5291(3) 0.0215(6) Uani 1 1 d . . . . .
H21 H 0.7738 0.2124 0.6059 0.026 Uiso 1 1 calc R U . . .
C87 C 0.28000(4) 0.09286(5) 0.1988(3) 0.0216(6) Uani 1 1 d . . . . .
N1 N 0.74583(4) 0.12114(4) 0.0803(2) 0.0178(5) Uani 1 1 d . . . . .
N5 N 0.64697(4) -0.00805(4) 0.3036(3) 0.0222(5) Uani 1 1 d . . . . .
C39 C 0.66480(5) 0.17179(5) -0.0125(3) 0.0265(7) Uani 1 1 d . . . . .
H39 H 0.6574 0.1658 0.0639 0.032 Uiso 1 1 calc R U . . .
C17 C 0.74493(5) 0.20608(5) -0.0206(3) 0.0289(7) Uani 1 1 d . . . . .
H17A H 0.7298 0.2029 -0.0275 0.043 Uiso 1 1 calc R U . . .
H17B H 0.7481 0.2203 -0.0689 0.043 Uiso 1 1 calc R U . . .
H17C H 0.7489 0.2076 0.0758 0.043 Uiso 1 1 calc R U . . .
C69 C 0.63828(5) 0.08570(5) -0.0421(3) 0.0249(7) Uani 1 1 d . . . . .
N6 N 0.61592(4) 0.02471(4) 0.2613(3) 0.0242(5) Uani 1 1 d . . . . .
C70 C 0.63320(5) 0.09325(5) -0.1735(3) 0.0266(7) Uani 1 1 d . . . . .
H70 H 0.6333 0.0830 -0.2483 0.032 Uiso 1 1 calc R U . . .
C35 C 0.58102(5) 0.19321(5) -0.1591(3) 0.0259(7) Uani 1 1 d . . . . .
H35 H 0.5677 0.1891 -0.1964 0.031 Uiso 1 1 calc R U . . .
C66 C 0.64932(5) 0.07272(5) 0.4530(4) 0.0325(7) Uani 1 1 d . . . . .
H66A H 0.6432 0.0767 0.3642 0.049 Uiso 1 1 calc R U . . .
H66B H 0.6541 0.0866 0.4991 0.049 Uiso 1 1 calc R U . . .
H66C H 0.6386 0.0652 0.5091 0.049 Uiso 1 1 calc R U . . .
C59 C 0.69332(5) 0.00833(5) 0.0166(3) 0.0245(7) Uani 1 1 d . . . . .
C71 C 0.62798(5) 0.11574(6) -0.1933(4) 0.0326(8) Uani 1 1 d . . . . .
C49 C 0.63080(5) 0.18412(5) 0.2349(3) 0.0289(7) Uani 1 1 d . . . . .
H49 H 0.6211 0.1774 0.1727 0.035 Uiso 1 1 calc R U . . .
C92 C 0.27641(5) 0.11643(5) 0.1982(3) 0.0224(6) Uani 1 1 d . . . . .
H92 H 0.2623 0.1218 0.1941 0.027 Uiso 1 1 calc R U . . .
C81 C 0.23736(4) 0.08352(5) 0.2146(3) 0.0194(6) Uani 1 1 d . . . . .
C36 C 0.58221(5) 0.20589(5) -0.0400(3) 0.0275(7) Uani 1 1 d . . . . .
H36 H 0.5697 0.2108 0.0039 0.033 Uiso 1 1 calc R U . . .
C94 C 0.27911(5) 0.04776(5) 0.3706(3) 0.0264(7) Uani 1 1 d . . . . .
H94 H 0.2873 0.0605 0.3975 0.032 Uiso 1 1 calc R U . . .
C93 C 0.26516(5) 0.05023(5) 0.2613(3) 0.0231(6) Uani 1 1 d . . . . .
C37 C 0.60179(5) 0.21142(5) 0.0152(3) 0.0248(7) Uani 1 1 d . . . . .
H37 H 0.6022 0.2202 0.0966 0.030 Uiso 1 1 calc R U . . .
C38 C 0.66179(4) 0.19459(5) -0.0475(3) 0.0223(6) Uani 1 1 d . . . . .
C45 C 0.65596(5) 0.21235(6) 0.2917(3) 0.0282(7) Uani 1 1 d . . . . .
H45 H 0.6638 0.2256 0.2701 0.034 Uiso 1 1 calc R U . . .
C86 C 0.22685(5) 0.09969(5) 0.1335(3) 0.0230(6) Uani 1 1 d . . . . .
H86 H 0.2341 0.1059 0.0572 0.028 Uiso 1 1 calc R U . . .
C14 C 0.74348(4) 0.15172(5) -0.0865(3) 0.0175(6) Uani 1 1 d . . . . .
C10 C 0.71115(5) 0.16586(5) 0.3162(3) 0.0227(6) Uani 1 1 d . . . . .
C83 C 0.20501(5) 0.08258(5) 0.3537(3) 0.0273(7) Uani 1 1 d . . . . .
H83 H 0.1976 0.0765 0.4296 0.033 Uiso 1 1 calc R U . . .
C15 C 0.74882(5) 0.18089(5) -0.2289(3) 0.0236(6) Uani 1 1 d . . . . .
H15A H 0.7380 0.1921 -0.2576 0.028 Uiso 1 1 calc R U . . .
H15B H 0.7604 0.1808 -0.2968 0.028 Uiso 1 1 calc R U . . .
C34 C 0.59959(5) 0.18656(5) -0.2229(3) 0.0236(6) Uani 1 1 d . . . . .
H34 H 0.5990 0.1781 -0.3055 0.028 Uiso 1 1 calc R U . . .
C77 C 0.24247(6) 0.05228(6) -0.1885(4) 0.0354(8) Uani 1 1 d . . . . .
H77 H 0.2298 0.0462 -0.2260 0.042 Uiso 1 1 calc R U . . .
C40 C 0.67819(5) 0.15744(6) -0.0854(4) 0.0327(8) Uani 1 1 d . . . . .
H40 H 0.6796 0.1420 -0.0588 0.039 Uiso 1 1 calc R U . . .
C32 C 0.62098(4) 0.20462(5) -0.0439(3) 0.0187(6) Uani 1 1 d . . . . .
C25 C 0.77842(6) 0.22742(5) 0.2876(3) 0.0310(8) Uani 1 1 d . . . . .
H25 H 0.7785 0.2213 0.1978 0.037 Uiso 1 1 calc R U . . .
C2 C 0.78410(4) 0.11558(5) 0.0817(3) 0.0205(6) Uani 1 1 d . . . . .
C16 C 0.75737(5) 0.18666(5) -0.0845(3) 0.0211(6) Uani 1 1 d . . . . .
C58 C 0.70210(5) -0.01598(5) 0.0110(4) 0.0300(7) Uani 1 1 d . . . . .
H58A H 0.7057 -0.0203 -0.0839 0.036 Uiso 1 1 calc R U . . .
H58B H 0.7149 -0.0174 0.0683 0.036 Uiso 1 1 calc R U . . .
C46 C 0.65782(5) 0.20311(6) 0.4225(3) 0.0336(8) Uani 1 1 d . . . . .
H46 H 0.6672 0.2099 0.4866 0.040 Uiso 1 1 calc R U . . .
C7 C 0.73004(5) 0.11152(5) 0.1759(3) 0.0223(6) Uani 1 1 d . . . . .
H7A H 0.7371 0.1027 0.2488 0.027 Uiso 1 1 calc R U . . .
H7B H 0.7201 0.1014 0.1268 0.027 Uiso 1 1 calc R U . . .
C61 C 0.68575(5) 0.01640(6) -0.1229(3) 0.0295(7) Uani 1 1 d . . . . .
H61A H 0.6758 0.0053 -0.1605 0.044 Uiso 1 1 calc R U . . .
H61B H 0.6979 0.0179 -0.1845 0.044 Uiso 1 1 calc R U . . .
H61C H 0.6788 0.0312 -0.1133 0.044 Uiso 1 1 calc R U . . .
C3 C 0.81920(5) 0.11611(5) 0.0911(4) 0.0302(7) Uani 1 1 d . . . . .
H3A H 0.8268 0.1206 0.0072 0.036 Uiso 1 1 calc R U . . .
H3B H 0.8290 0.1077 0.1513 0.036 Uiso 1 1 calc R U . . .
C85 C 0.20636(5) 0.10695(5) 0.1600(3) 0.0271(7) Uani 1 1 d . . . . .
H85 H 0.1999 0.1178 0.1016 0.033 Uiso 1 1 calc R U . . .
C68 C 0.64330(5) 0.06089(5) -0.0196(3) 0.0252(7) Uani 1 1 d . . . . .
C22 C 0.77796(5) 0.24529(5) 0.5472(3) 0.0260(7) Uani 1 1 d . . . . .
C1 C 0.76321(5) 0.10524(5) 0.0488(3) 0.0219(6) Uani 1 1 d . . . . .
H1A H 0.7628 0.1012 -0.0493 0.026 Uiso 1 1 calc R U . . .
H1B H 0.7614 0.0911 0.1024 0.026 Uiso 1 1 calc R U . . .
C65 C 0.66794(5) 0.05676(5) 0.4319(3) 0.0251(6) Uani 1 1 d . . . . .
C8 C 0.71859(5) 0.13143(5) 0.2353(3) 0.0215(6) Uani 1 1 d . . . . .
C82 C 0.22557(5) 0.07531(5) 0.3271(3) 0.0226(6) Uani 1 1 d . . . . .
H82 H 0.2319 0.0645 0.3864 0.027 Uiso 1 1 calc R U . . .
C84 C 0.19532(5) 0.09851(5) 0.2709(4) 0.0281(7) Uani 1 1 d . . . . .
H84 H 0.1814 0.1036 0.2898 0.034 Uiso 1 1 calc R U . . .
C91 C 0.29272(5) 0.13224(5) 0.2032(3) 0.0283(7) Uani 1 1 d . . . . .
H91 H 0.2895 0.1480 0.2019 0.034 Uiso 1 1 calc R U . . .
C76 C 0.24288(5) 0.05927(5) -0.0531(3) 0.0282(7) Uani 1 1 d . . . . .
H76 H 0.2303 0.0581 -0.0008 0.034 Uiso 1 1 calc R U . . .
C43 C 0.67327(5) 0.20228(6) -0.1609(3) 0.0311(7) Uani 1 1 d . . . . .
H43 H 0.6717 0.2176 -0.1893 0.037 Uiso 1 1 calc R U . . .
C57 C 0.67168(5) -0.01559(5) 0.1247(3) 0.0247(7) Uani 1 1 d . . . . .
C4 C 0.81018(5) 0.13719(5) 0.1655(3) 0.0249(6) Uani 1 1 d . . . . .
C80 C 0.27856(5) 0.07013(5) -0.0759(3) 0.0266(7) Uani 1 1 d . . . . .
H80 H 0.2912 0.0764 -0.0397 0.032 Uiso 1 1 calc R U . . .
C30 C 0.64260(6) 0.27651(6) -0.0593(4) 0.0362(8) Uani 1 1 d . . . . .
H30 H 0.6326 0.2875 -0.0894 0.043 Uiso 1 1 calc R U . . .
C72 C 0.62701(6) 0.13103(6) -0.0859(4) 0.0399(9) Uani 1 1 d . . . . .
H72 H 0.6229 0.1464 -0.1008 0.048 Uiso 1 1 calc R U . . .
C56 C 0.65408(5) -0.02549(5) 0.2046(3) 0.0264(7) Uani 1 1 d . . . . .
H56A H 0.6589 -0.0393 0.2534 0.032 Uiso 1 1 calc R U . . .
H56B H 0.6423 -0.0298 0.1431 0.032 Uiso 1 1 calc R U . . .
C53 C 0.59613(5) 0.03821(6) 0.2408(4) 0.0309(7) Uani 1 1 d . . . . .
C18 C 0.78081(5) 0.19174(5) -0.0859(3) 0.0273(7) Uani 1 1 d . . . . .
H18A H 0.7859 0.1932 0.0081 0.041 Uiso 1 1 calc R U . . .
H18B H 0.7833 0.2060 -0.1350 0.041 Uiso 1 1 calc R U . . .
H18C H 0.7883 0.1793 -0.1317 0.041 Uiso 1 1 calc R U . . .
C12 C 0.70764(5) 0.18771(5) 0.2371(4) 0.0304(7) Uani 1 1 d . . . . .
H12A H 0.7208 0.1965 0.2349 0.046 Uiso 1 1 calc R U . . .
H12B H 0.6966 0.1967 0.2818 0.046 Uiso 1 1 calc R U . . .
H12C H 0.7033 0.1841 0.1436 0.046 Uiso 1 1 calc R U . . .
C33 C 0.61907(5) 0.19228(5) -0.1659(3) 0.0210(6) Uani 1 1 d . . . . .
H33 H 0.6316 0.1876 -0.2117 0.025 Uiso 1 1 calc R U . . .
C19 C 0.77290(4) 0.18780(5) 0.3781(3) 0.0197(6) Uani 1 1 d . . . . .
C74 C 0.63788(6) 0.10106(5) 0.0658(4) 0.0352(8) Uani 1 1 d . . . . .
H74 H 0.6415 0.0962 0.1551 0.042 Uiso 1 1 calc R U . . .
C95 C 0.28154(5) 0.02728(5) 0.4425(4) 0.0328(7) Uani 1 1 d . . . . .
H95 H 0.2915 0.0263 0.5150 0.039 Uiso 1 1 calc R U . . .
C23 C 0.78058(5) 0.25966(5) 0.4379(4) 0.0333(7) Uani 1 1 d . . . . .
H23 H 0.7821 0.2755 0.4518 0.040 Uiso 1 1 calc R U . . .
C26 C 0.65009(5) 0.23723(5) 0.0079(3) 0.0216(6) Uani 1 1 d . . . . .
C29 C 0.66355(6) 0.28277(6) -0.0381(4) 0.0421(9) Uani 1 1 d . . . . .
H29 H 0.6680 0.2979 -0.0546 0.051 Uiso 1 1 calc R U . . .
C75 C 0.26102(5) 0.06798(5) 0.0099(3) 0.0214(6) Uani 1 1 d . . . . .
B2 B 0.26107(5) 0.07400(5) 0.1755(4) 0.0216(7) Uani 1 1 d . . . . .
C31 C 0.63623(5) 0.25415(5) -0.0365(3) 0.0252(7) Uani 1 1 d . . . . .
H31 H 0.6219 0.2503 -0.0517 0.030 Uiso 1 1 calc R U . . .
C90 C 0.31356(5) 0.12523(6) 0.2100(4) 0.0323(8) Uani 1 1 d . . . . .
H90 H 0.3247 0.1360 0.2148 0.039 Uiso 1 1 calc R U . . .
B1 B 0.64377(5) 0.21040(6) 0.0288(3) 0.0198(7) Uani 1 1 d . . . . .
C27 C 0.67106(5) 0.24462(6) 0.0290(3) 0.0316(8) Uani 1 1 d . . . . .
H27 H 0.6812 0.2338 0.0596 0.038 Uiso 1 1 calc R U . . .
C6 C 0.81904(5) 0.15911(6) 0.1076(4) 0.0354(8) Uani 1 1 d . . . . .
H6A H 0.8171 0.1593 0.0083 0.053 Uiso 1 1 calc R U . . .
H6B H 0.8341 0.1602 0.1293 0.053 Uiso 1 1 calc R U . . .
H6C H 0.8116 0.1721 0.1480 0.053 Uiso 1 1 calc R U . . .
C51 C 0.61097(5) 0.00665(5) 0.3248(3) 0.0260(7) Uani 1 1 d . . . . .
C48 C 0.63248(6) 0.17505(6) 0.3657(4) 0.0362(8) Uani 1 1 d . . . . .
H48 H 0.6241 0.1624 0.3906 0.043 Uiso 1 1 calc R U . . .
C97 C 0.25510(6) 0.01044(5) 0.3026(4) 0.0353(8) Uani 1 1 d . . . . .
H97 H 0.2465 -0.0022 0.2793 0.042 Uiso 1 1 calc R U . . .
C60 C 0.70912(5) 0.02481(5) 0.0773(4) 0.0310(7) Uani 1 1 d . . . . .
H60A H 0.7030 0.0401 0.0796 0.046 Uiso 1 1 calc R U . . .
H60B H 0.7219 0.0250 0.0213 0.046 Uiso 1 1 calc R U . . .
H60C H 0.7127 0.0200 0.1704 0.046 Uiso 1 1 calc R U . . .
C55 C 0.59863(6) 0.06236(6) 0.2918(5) 0.0476(10) Uani 1 1 d . . . . .
H55A H 0.6021 0.0622 0.3893 0.071 Uiso 1 1 calc R U . . .
H55B H 0.5854 0.0707 0.2780 0.071 Uiso 1 1 calc R U . . .
H55C H 0.6100 0.0699 0.2411 0.071 Uiso 1 1 calc R U . . .
C78 C 0.26018(6) 0.05404(5) -0.2684(3) 0.0336(8) Uani 1 1 d . . . . .
H78 H 0.2600 0.0489 -0.3605 0.040 Uiso 1 1 calc R U . . .
C41 C 0.68942(5) 0.16561(6) -0.1965(4) 0.0364(8) Uani 1 1 d . . . . .
H41 H 0.6986 0.1560 -0.2465 0.044 Uiso 1 1 calc R U . . .
C73 C 0.63215(7) 0.12344(6) 0.0437(4) 0.0438(9) Uani 1 1 d . . . . .
H73 H 0.6317 0.1337 0.1184 0.053 Uiso 1 1 calc R U . . .
C54 C 0.59025(6) 0.03769(7) 0.0904(4) 0.0429(9) Uani 1 1 d . . . . .
H54A H 0.6016 0.0445 0.0365 0.064 Uiso 1 1 calc R U . . .
H54B H 0.5772 0.0463 0.0764 0.064 Uiso 1 1 calc R U . . .
H54C H 0.5881 0.0219 0.0615 0.064 Uiso 1 1 calc R U . . .
C50 C 0.62553(5) -0.01242(5) 0.3574(3) 0.0273(7) Uani 1 1 d . . . . .
H50A H 0.6262 -0.0145 0.4576 0.033 Uiso 1 1 calc R U . . .
H50B H 0.6200 -0.0266 0.3171 0.033 Uiso 1 1 calc R U . . .
C11 C 0.71949(5) 0.17045(6) 0.4592(3) 0.0325(8) Uani 1 1 d . . . . .
H11A H 0.7220 0.1560 0.5061 0.049 Uiso 1 1 calc R U . . .
H11B H 0.7091 0.1794 0.5104 0.049 Uiso 1 1 calc R U . . .
H11C H 0.7328 0.1789 0.4531 0.049 Uiso 1 1 calc R U . . .
C88 C 0.30145(5) 0.08646(5) 0.2044(3) 0.0284(7) Uani 1 1 d . . . . .
H88 H 0.3049 0.0707 0.2046 0.034 Uiso 1 1 calc R U . . .
C13 C 0.73510(4) 0.12924(5) -0.0463(3) 0.0185(6) Uani 1 1 d . . . . .
H13A H 0.7374 0.1182 -0.1211 0.022 Uiso 1 1 calc R U . . .
H13B H 0.7197 0.1304 -0.0300 0.022 Uiso 1 1 calc R U . . .
C63 C 0.66622(5) 0.01894(5) 0.4456(3) 0.0237(6) Uani 1 1 d . . . . .
C24 C 0.78096(7) 0.25060(6) 0.3062(4) 0.0405(9) Uani 1 1 d . . . . .
H24 H 0.7829 0.2603 0.2297 0.049 Uiso 1 1 calc R U . . .
C28 C 0.67760(6) 0.26663(7) 0.0074(4) 0.0425(9) Uani 1 1 d . . . . .
H28 H 0.6919 0.2707 0.0240 0.051 Uiso 1 1 calc R U . . .
C79 C 0.27826(6) 0.06336(6) -0.2127(3) 0.0332(8) Uani 1 1 d . . . . .
H79 H 0.2905 0.0652 -0.2675 0.040 Uiso 1 1 calc R U . . .
C96 C 0.26964(6) 0.00858(6) 0.4085(4) 0.0365(8) Uani 1 1 d . . . . .
H96 H 0.2713 -0.0053 0.4564 0.044 Uiso 1 1 calc R U . . .
C64 C 0.67702(6) 0.04849(5) 0.5699(3) 0.0315(7) Uani 1 1 d . . . . .
H64A H 0.6917 0.0540 0.5824 0.038 Uiso 1 1 calc R U . . .
H64B H 0.6683 0.0540 0.6469 0.038 Uiso 1 1 calc R U . . .
C89 C 0.31776(5) 0.10214(6) 0.2096(4) 0.0330(8) Uani 1 1 d . . . . .
H89 H 0.3320 0.0970 0.2130 0.040 Uiso 1 1 calc R U . . .
C52 C 0.58029(6) 0.02468(7) 0.3285(4) 0.0445(10) Uani 1 1 d . . . . .
H52A H 0.5766 0.0332 0.4122 0.053 Uiso 1 1 calc R U . . .
H52B H 0.5672 0.0216 0.2764 0.053 Uiso 1 1 calc R U . . .
C67 C 0.68456(6) 0.06750(6) 0.3412(4) 0.0353(8) Uani 1 1 d . . . . .
H67A H 0.6964 0.0569 0.3295 0.053 Uiso 1 1 calc R U . . .
H67B H 0.6897 0.0815 0.3836 0.053 Uiso 1 1 calc R U . . .
H67C H 0.6784 0.0710 0.2519 0.053 Uiso 1 1 calc R U . . .
C62 C 0.66272(5) -0.00563(5) 0.4149(3) 0.0263(7) Uani 1 1 d . . . . .
H62A H 0.6762 -0.0127 0.3869 0.032 Uiso 1 1 calc R U . . .
H62B H 0.6576 -0.0135 0.4979 0.032 Uiso 1 1 calc R U . . .
C5 C 0.81347(6) 0.13564(7) 0.3201(4) 0.0377(8) Uani 1 1 d . . . . .
H5A H 0.8059 0.1481 0.3650 0.057 Uiso 1 1 calc R U . . .
H5B H 0.8286 0.1368 0.3408 0.057 Uiso 1 1 calc R U . . .
H5C H 0.8081 0.1211 0.3533 0.057 Uiso 1 1 calc R U . . .
C42 C 0.68688(6) 0.18819(6) -0.2329(4) 0.0380(9) Uani 1 1 d . . . . .
H42 H 0.6946 0.1941 -0.3082 0.046 Uiso 1 1 calc R U . . .
C47 C 0.64626(6) 0.18434(6) 0.4594(3) 0.0386(9) Uani 1 1 d . . . . .
H47 H 0.6477 0.1779 0.5478 0.046 Uiso 1 1 calc R U . . .
H51A H 0.6359(6) 0.0197(7) -0.047(5) 0.044(12) Uiso 1 1 d . . . . .
H2A H 0.7664(6) 0.1483(7) 0.434(5) 0.060(13) Uiso 1 1 d . . . . .
H2B H 0.7697(6) 0.1247(7) 0.401(4) 0.046(12) Uiso 1 1 d . . . . .
H51B H 0.6230(8) 0.0027(8) -0.020(5) 0.072(16) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O4 2.019(2) . ?
Ni1 N2 2.088(2) . ?
Ni1 N4 2.095(2) . ?
Ni1 N3 2.114(2) . ?
Ni1 O6 2.171(2) . ?
Ni1 N1 2.200(2) . ?
Ni2 O10 2.023(2) . ?
Ni2 N8 2.091(2) . ?
Ni2 N6 2.104(3) . ?
Ni2 O12 2.132(2) . ?
Ni2 N7 2.184(2) . ?
Ni2 N5 2.196(2) . ?
Cl1 C22 1.741(3) . ?
Cl2 C71 1.747(4) . ?
O2 C8 1.349(3) . ?
O2 C9 1.471(4) . ?
O10 C68 1.263(4) . ?
O4 C19 1.273(3) . ?
O6 H2A 0.95(5) . ?
O6 H2B 0.83(4) . ?
O3 C14 1.350(3) . ?
O3 C15 1.459(3) . ?
O1 C2 1.340(3) . ?
O1 C3 1.458(4) . ?
O5 C19 1.252(4) . ?
O12 H51A 0.80(4) . ?
O12 H51B 0.87(5) . ?
O8 C57 1.346(4) . ?
O8 C58 1.466(4) . ?
O7 C51 1.338(4) . ?
O7 C52 1.448(4) . ?
N2 C2 1.276(4) . ?
N2 C4 1.503(4) . ?
O11 C68 1.248(4) . ?
O9 C63 1.341(4) . ?
O9 C64 1.465(4) . ?
N3 C8 1.269(4) . ?
N3 C10 1.488(4) . ?
C20 C25 1.384(4) . ?
C20 C21 1.387(4) . ?
C20 C19 1.511(4) . ?
N4 C14 1.268(4) . ?
N4 C16 1.490(4) . ?
N7 C57 1.270(4) . ?
N7 C59 1.506(4) . ?
C9 C10 1.548(4) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
N8 C63 1.265(4) . ?
N8 C65 1.492(4) . ?
C98 C97 1.385(5) . ?
C98 C93 1.416(4) . ?
C98 H98 0.9500 . ?
C44 C45 1.399(4) . ?
C44 C49 1.414(4) . ?
C44 B1 1.651(5) . ?
C21 C22 1.386(4) . ?
C21 H21 0.9500 . ?
C87 C92 1.406(4) . ?
C87 C88 1.412(4) . ?
C87 B2 1.650(4) . ?
N1 C1 1.478(4) . ?
N1 C7 1.483(4) . ?
N1 C13 1.493(4) . ?
N5 C50 1.479(4) . ?
N5 C56 1.483(4) . ?
N5 C62 1.485(4) . ?
C39 C40 1.394(4) . ?
C39 C38 1.398(4) . ?
C39 H39 0.9500 . ?
C17 C16 1.523(4) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C69 C74 1.391(5) . ?
C69 C70 1.399(4) . ?
C69 C68 1.511(4) . ?
N6 C51 1.271(4) . ?
N6 C53 1.498(4) . ?
C70 C71 1.378(4) . ?
C70 H70 0.9500 . ?
C35 C36 1.386(4) . ?
C35 C34 1.389(4) . ?
C35 H35 0.9500 . ?
C66 C65 1.523(4) . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 0.9800 . ?
C59 C60 1.516(4) . ?
C59 C61 1.523(4) . ?
C59 C58 1.536(4) . ?
C71 C72 1.386(5) . ?
C49 C48 1.391(5) . ?
C49 H49 0.9500 . ?
C92 C91 1.392(4) . ?
C92 H92 0.9500 . ?
C81 C86 1.407(4) . ?
C81 C82 1.416(4) . ?
C81 B2 1.649(4) . ?
C36 C37 1.392(4) . ?
C36 H36 0.9500 . ?
C94 C93 1.396(4) . ?
C94 C95 1.404(4) . ?
C94 H94 0.9500 . ?
C93 B2 1.653(5) . ?
C37 C32 1.406(4) . ?
C37 H37 0.9500 . ?
C38 C43 1.403(4) . ?
C38 B1 1.652(4) . ?
C45 C46 1.397(5) . ?
C45 H45 0.9500 . ?
C86 C85 1.391(4) . ?
C86 H86 0.9500 . ?
C14 C13 1.479(4) . ?
C10 C12 1.518(4) . ?
C10 C11 1.521(4) . ?
C83 C84 1.383(5) . ?
C83 C82 1.396(4) . ?
C83 H83 0.9500 . ?
C15 C16 1.552(4) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C34 C33 1.396(4) . ?
C34 H34 0.9500 . ?
C77 C78 1.372(5) . ?
C77 C76 1.388(5) . ?
C77 H77 0.9500 . ?
C40 C41 1.387(5) . ?
C40 H40 0.9500 . ?
C32 C33 1.403(4) . ?
C32 B1 1.646(4) . ?
C25 C24 1.386(4) . ?
C25 H25 0.9500 . ?
C2 C1 1.492(4) . ?
C16 C18 1.515(4) . ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
C46 C47 1.374(5) . ?
C46 H46 0.9500 . ?
C7 C8 1.496(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C61 H61A 0.9800 . ?
C61 H61B 0.9800 . ?
C61 H61C 0.9800 . ?
C3 C4 1.548(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C85 C84 1.384(5) . ?
C85 H85 0.9500 . ?
C22 C23 1.374(5) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C65 C67 1.516(5) . ?
C65 C64 1.547(5) . ?
C82 H82 0.9500 . ?
C84 H84 0.9500 . ?
C91 C90 1.385(5) . ?
C91 H91 0.9500 . ?
C76 C75 1.402(4) . ?
C76 H76 0.9500 . ?
C43 C42 1.389(4) . ?
C43 H43 0.9500 . ?
C57 C56 1.482(5) . ?
C4 C6 1.517(4) . ?
C4 C5 1.531(5) . ?
C80 C79 1.398(5) . ?
C80 C75 1.399(4) . ?
C80 H80 0.9500 . ?
C30 C29 1.393(5) . ?
C30 C31 1.395(4) . ?
C30 H30 0.9500 . ?
C72 C73 1.384(6) . ?
C72 H72 0.9500 . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C53 C55 1.515(5) . ?
C53 C54 1.519(5) . ?
C53 C52 1.543(5) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C33 H33 0.9500 . ?
C74 C73 1.383(5) . ?
C74 H74 0.9500 . ?
C95 C96 1.375(5) . ?
C95 H95 0.9500 . ?
C23 C24 1.396(5) . ?
C23 H23 0.9500 . ?
C26 C31 1.397(4) . ?
C26 C27 1.414(4) . ?
C26 B1 1.642(4) . ?
C29 C28 1.376(6) . ?
C29 H29 0.9500 . ?
C75 B2 1.660(5) . ?
C31 H31 0.9500 . ?
C90 C89 1.385(5) . ?
C90 H90 0.9500 . ?
C27 C28 1.376(5) . ?
C27 H27 0.9500 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C51 C50 1.488(4) . ?
C48 C47 1.380(5) . ?
C48 H48 0.9500 . ?
C97 C96 1.393(5) . ?
C97 H97 0.9500 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C78 C79 1.383(5) . ?
C78 H78 0.9500 . ?
C41 C42 1.385(5) . ?
C41 H41 0.9500 . ?
C73 H73 0.9500 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C88 C89 1.387(4) . ?
C88 H88 0.9500 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C63 C62 1.494(4) . ?
C24 H24 0.9500 . ?
C28 H28 0.9500 . ?
C79 H79 0.9500 . ?
C96 H96 0.9500 . ?
C64 H64A 0.9900 . ?
C64 H64B 0.9900 . ?
C89 H89 0.9500 . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C67 H67A 0.9800 . ?
C67 H67B 0.9800 . ?
C67 H67C 0.9800 . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C42 H42 0.9500 . ?
C47 H47 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Ni1 N2 102.30(9) . . ?
O4 Ni1 N4 90.85(9) . . ?
N2 Ni1 N4 96.06(9) . . ?
O4 Ni1 N3 102.06(9) . . ?
N2 Ni1 N3 153.19(9) . . ?
N4 Ni1 N3 94.61(9) . . ?
O4 Ni1 O6 92.39(9) . . ?
N2 Ni1 O6 87.02(9) . . ?
N4 Ni1 O6 174.97(9) . . ?
N3 Ni1 O6 80.94(9) . . ?
O4 Ni1 N1 171.01(9) . . ?
N2 Ni1 N1 81.05(9) . . ?
N4 Ni1 N1 80.46(9) . . ?
N3 Ni1 N1 76.57(9) . . ?
O6 Ni1 N1 96.14(9) . . ?
O10 Ni2 N8 93.10(9) . . ?
O10 Ni2 N6 97.01(9) . . ?
N8 Ni2 N6 94.72(10) . . ?
O10 Ni2 O12 91.74(9) . . ?
N8 Ni2 O12 174.17(9) . . ?
N6 Ni2 O12 87.91(10) . . ?
O10 Ni2 N7 107.74(9) . . ?
N8 Ni2 N7 96.40(9) . . ?
N6 Ni2 N7 152.17(10) . . ?
O12 Ni2 N7 79.01(9) . . ?
O10 Ni2 N5 172.52(9) . . ?
N8 Ni2 N5 80.03(9) . . ?
N6 Ni2 N5 80.73(10) . . ?
O12 Ni2 N5 95.29(9) . . ?
N7 Ni2 N5 76.21(9) . . ?
C8 O2 C9 104.5(2) . . ?
C68 O10 Ni2 129.0(2) . . ?
C19 O4 Ni1 130.34(19) . . ?
Ni1 O6 H2A 98(3) . . ?
Ni1 O6 H2B 123(3) . . ?
H2A O6 H2B 108(4) . . ?
C14 O3 C15 105.5(2) . . ?
C2 O1 C3 105.5(2) . . ?
Ni2 O12 H51A 100(3) . . ?
Ni2 O12 H51B 136(3) . . ?
H51A O12 H51B 104(4) . . ?
C57 O8 C58 104.6(2) . . ?
C51 O7 C52 105.2(2) . . ?
C2 N2 C4 107.2(2) . . ?
C2 N2 Ni1 112.31(19) . . ?
C4 N2 Ni1 139.13(19) . . ?
C63 O9 C64 105.2(2) . . ?
C8 N3 C10 107.4(2) . . ?
C8 N3 Ni1 111.45(19) . . ?
C10 N3 Ni1 139.43(18) . . ?
C25 C20 C21 119.4(3) . . ?
C25 C20 C19 120.8(3) . . ?
C21 C20 C19 119.7(3) . . ?
C14 N4 C16 108.1(2) . . ?
C14 N4 Ni1 112.34(19) . . ?
C16 N4 Ni1 139.54(18) . . ?
C57 N7 C59 106.8(2) . . ?
C57 N7 Ni2 108.8(2) . . ?
C59 N7 Ni2 141.73(18) . . ?
O2 C9 C10 104.5(2) . . ?
O2 C9 H9A 110.8 . . ?
C10 C9 H9A 110.8 . . ?
O2 C9 H9B 110.8 . . ?
C10 C9 H9B 110.8 . . ?
H9A C9 H9B 108.9 . . ?
C63 N8 C65 107.9(2) . . ?
C63 N8 Ni2 112.6(2) . . ?
C65 N8 Ni2 139.18(19) . . ?
C97 C98 C93 122.9(3) . . ?
C97 C98 H98 118.6 . . ?
C93 C98 H98 118.6 . . ?
C45 C44 C49 114.8(3) . . ?
C45 C44 B1 123.5(3) . . ?
C49 C44 B1 121.2(3) . . ?
C22 C21 C20 119.6(3) . . ?
C22 C21 H21 120.2 . . ?
C20 C21 H21 120.2 . . ?
C92 C87 C88 114.8(3) . . ?
C92 C87 B2 123.1(2) . . ?
C88 C87 B2 121.7(3) . . ?
C1 N1 C7 113.1(2) . . ?
C1 N1 C13 111.6(2) . . ?
C7 N1 C13 109.8(2) . . ?
C1 N1 Ni1 109.30(17) . . ?
C7 N1 Ni1 105.12(17) . . ?
C13 N1 Ni1 107.51(16) . . ?
C50 N5 C56 113.1(2) . . ?
C50 N5 C62 111.9(2) . . ?
C56 N5 C62 110.0(2) . . ?
C50 N5 Ni2 109.61(18) . . ?
C56 N5 Ni2 104.32(18) . . ?
C62 N5 Ni2 107.54(17) . . ?
C40 C39 C38 122.6(3) . . ?
C40 C39 H39 118.7 . . ?
C38 C39 H39 118.7 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C74 C69 C70 119.2(3) . . ?
C74 C69 C68 121.4(3) . . ?
C70 C69 C68 119.3(3) . . ?
C51 N6 C53 107.6(3) . . ?
C51 N6 Ni2 112.3(2) . . ?
C53 N6 Ni2 138.7(2) . . ?
C71 C70 C69 119.3(3) . . ?
C71 C70 H70 120.3 . . ?
C69 C70 H70 120.3 . . ?
C36 C35 C34 119.0(3) . . ?
C36 C35 H35 120.5 . . ?
C34 C35 H35 120.5 . . ?
C65 C66 H66A 109.5 . . ?
C65 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
C65 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
N7 C59 C60 110.1(2) . . ?
N7 C59 C61 109.7(2) . . ?
C60 C59 C61 111.1(3) . . ?
N7 C59 C58 101.9(2) . . ?
C60 C59 C58 111.8(3) . . ?
C61 C59 C58 111.9(3) . . ?
C70 C71 C72 121.9(3) . . ?
C70 C71 Cl2 119.0(3) . . ?
C72 C71 Cl2 119.2(3) . . ?
C48 C49 C44 122.5(3) . . ?
C48 C49 H49 118.8 . . ?
C44 C49 H49 118.8 . . ?
C91 C92 C87 122.6(3) . . ?
C91 C92 H92 118.7 . . ?
C87 C92 H92 118.7 . . ?
C86 C81 C82 114.9(3) . . ?
C86 C81 B2 122.0(3) . . ?
C82 C81 B2 123.0(3) . . ?
C35 C36 C37 120.1(3) . . ?
C35 C36 H36 120.0 . . ?
C37 C36 H36 120.0 . . ?
C93 C94 C95 122.9(3) . . ?
C93 C94 H94 118.5 . . ?
C95 C94 H94 118.5 . . ?
C94 C93 C98 114.7(3) . . ?
C94 C93 B2 125.3(3) . . ?
C98 C93 B2 119.9(3) . . ?
C36 C37 C32 123.0(3) . . ?
C36 C37 H37 118.5 . . ?
C32 C37 H37 118.5 . . ?
C39 C38 C43 115.6(3) . . ?
C39 C38 B1 121.6(3) . . ?
C43 C38 B1 122.4(3) . . ?
C46 C45 C44 122.7(3) . . ?
C46 C45 H45 118.7 . . ?
C44 C45 H45 118.7 . . ?
C85 C86 C81 123.0(3) . . ?
C85 C86 H86 118.5 . . ?
C81 C86 H86 118.5 . . ?
N4 C14 O3 118.7(3) . . ?
N4 C14 C13 125.1(3) . . ?
O3 C14 C13 116.1(2) . . ?
N3 C10 C12 109.8(2) . . ?
N3 C10 C11 108.9(2) . . ?
C12 C10 C11 111.7(3) . . ?
N3 C10 C9 102.2(2) . . ?
C12 C10 C9 112.7(3) . . ?
C11 C10 C9 111.1(3) . . ?
C84 C83 C82 120.8(3) . . ?
C84 C83 H83 119.6 . . ?
C82 C83 H83 119.6 . . ?
O3 C15 C16 105.2(2) . . ?
O3 C15 H15A 110.7 . . ?
C16 C15 H15A 110.7 . . ?
O3 C15 H15B 110.7 . . ?
C16 C15 H15B 110.7 . . ?
H15A C15 H15B 108.8 . . ?
C35 C34 C33 120.1(3) . . ?
C35 C34 H34 120.0 . . ?
C33 C34 H34 120.0 . . ?
C78 C77 C76 120.5(3) . . ?
C78 C77 H77 119.8 . . ?
C76 C77 H77 119.8 . . ?
C41 C40 C39 120.3(3) . . ?
C41 C40 H40 119.9 . . ?
C39 C40 H40 119.9 . . ?
C33 C32 C37 115.0(3) . . ?
C33 C32 B1 123.5(2) . . ?
C37 C32 B1 121.5(3) . . ?
C20 C25 C24 120.8(3) . . ?
C20 C25 H25 119.6 . . ?
C24 C25 H25 119.6 . . ?
N2 C2 O1 118.9(3) . . ?
N2 C2 C1 125.7(3) . . ?
O1 C2 C1 115.2(2) . . ?
N4 C16 C18 110.0(2) . . ?
N4 C16 C17 109.8(2) . . ?
C18 C16 C17 111.3(3) . . ?
N4 C16 C15 102.2(2) . . ?
C18 C16 C15 112.2(2) . . ?
C17 C16 C15 111.0(2) . . ?
O8 C58 C59 104.7(2) . . ?
O8 C58 H58A 110.8 . . ?
C59 C58 H58A 110.8 . . ?
O8 C58 H58B 110.8 . . ?
C59 C58 H58B 110.8 . . ?
H58A C58 H58B 108.9 . . ?
C47 C46 C45 120.6(3) . . ?
C47 C46 H46 119.7 . . ?
C45 C46 H46 119.7 . . ?
N1 C7 C8 105.9(2) . . ?
N1 C7 H7A 110.6 . . ?
C8 C7 H7A 110.6 . . ?
N1 C7 H7B 110.6 . . ?
C8 C7 H7B 110.6 . . ?
H7A C7 H7B 108.7 . . ?
C59 C61 H61A 109.5 . . ?
C59 C61 H61B 109.5 . . ?
H61A C61 H61B 109.5 . . ?
C59 C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
O1 C3 C4 105.0(2) . . ?
O1 C3 H3A 110.8 . . ?
C4 C3 H3A 110.8 . . ?
O1 C3 H3B 110.8 . . ?
C4 C3 H3B 110.8 . . ?
H3A C3 H3B 108.8 . . ?
C84 C85 C86 120.5(3) . . ?
C84 C85 H85 119.7 . . ?
C86 C85 H85 119.7 . . ?
O11 C68 O10 125.8(3) . . ?
O11 C68 C69 118.2(3) . . ?
O10 C68 C69 116.0(3) . . ?
C23 C22 C21 121.4(3) . . ?
C23 C22 Cl1 118.9(2) . . ?
C21 C22 Cl1 119.6(2) . . ?
N1 C1 C2 111.0(2) . . ?
N1 C1 H1A 109.4 . . ?
C2 C1 H1A 109.4 . . ?
N1 C1 H1B 109.4 . . ?
C2 C1 H1B 109.4 . . ?
H1A C1 H1B 108.0 . . ?
N8 C65 C67 109.0(3) . . ?
N8 C65 C66 110.2(2) . . ?
C67 C65 C66 111.1(3) . . ?
N8 C65 C64 102.2(2) . . ?
C67 C65 C64 112.6(3) . . ?
C66 C65 C64 111.4(3) . . ?
N3 C8 O2 119.2(3) . . ?
N3 C8 C7 123.2(3) . . ?
O2 C8 C7 117.6(2) . . ?
C83 C82 C81 122.2(3) . . ?
C83 C82 H82 118.9 . . ?
C81 C82 H82 118.9 . . ?
C83 C84 C85 118.6(3) . . ?
C83 C84 H84 120.7 . . ?
C85 C84 H84 120.7 . . ?
C90 C91 C92 120.7(3) . . ?
C90 C91 H91 119.6 . . ?
C92 C91 H91 119.6 . . ?
C77 C76 C75 123.0(3) . . ?
C77 C76 H76 118.5 . . ?
C75 C76 H76 118.5 . . ?
C42 C43 C38 122.1(3) . . ?
C42 C43 H43 118.9 . . ?
C38 C43 H43 118.9 . . ?
N7 C57 O8 119.2(3) . . ?
N7 C57 C56 123.9(3) . . ?
O8 C57 C56 116.9(3) . . ?
N2 C4 C6 110.9(2) . . ?
N2 C4 C5 109.0(3) . . ?
C6 C4 C5 111.7(3) . . ?
N2 C4 C3 101.7(2) . . ?
C6 C4 C3 111.7(3) . . ?
C5 C4 C3 111.5(3) . . ?
C79 C80 C75 122.6(3) . . ?
C79 C80 H80 118.7 . . ?
C75 C80 H80 118.7 . . ?
C29 C30 C31 120.1(3) . . ?
C29 C30 H30 119.9 . . ?
C31 C30 H30 119.9 . . ?
C73 C72 C71 118.4(3) . . ?
C73 C72 H72 120.8 . . ?
C71 C72 H72 120.8 . . ?
C57 C56 N5 107.6(2) . . ?
C57 C56 H56A 110.2 . . ?
N5 C56 H56A 110.2 . . ?
C57 C56 H56B 110.2 . . ?
N5 C56 H56B 110.2 . . ?
H56A C56 H56B 108.5 . . ?
N6 C53 C55 111.5(3) . . ?
N6 C53 C54 108.9(3) . . ?
C55 C53 C54 111.3(3) . . ?
N6 C53 C52 101.3(3) . . ?
C55 C53 C52 111.6(3) . . ?
C54 C53 C52 111.7(3) . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C34 C33 C32 122.8(3) . . ?
C34 C33 H33 118.6 . . ?
C32 C33 H33 118.6 . . ?
O5 C19 O4 125.8(3) . . ?
O5 C19 C20 118.4(3) . . ?
O4 C19 C20 115.8(3) . . ?
C73 C74 C69 120.3(3) . . ?
C73 C74 H74 119.8 . . ?
C69 C74 H74 119.8 . . ?
C96 C95 C94 120.4(3) . . ?
C96 C95 H95 119.8 . . ?
C94 C95 H95 119.8 . . ?
C22 C23 C24 119.1(3) . . ?
C22 C23 H23 120.4 . . ?
C24 C23 H23 120.4 . . ?
C31 C26 C27 114.6(3) . . ?
C31 C26 B1 124.8(3) . . ?
C27 C26 B1 120.5(3) . . ?
C28 C29 C30 118.8(3) . . ?
C28 C29 H29 120.6 . . ?
C30 C29 H29 120.6 . . ?
C80 C75 C76 114.8(3) . . ?
C80 C75 B2 124.5(3) . . ?
C76 C75 B2 120.6(3) . . ?
C81 B2 C87 113.7(2) . . ?
C81 B2 C93 108.2(2) . . ?
C87 B2 C93 112.7(2) . . ?
C81 B2 C75 107.3(2) . . ?
C87 B2 C75 106.3(2) . . ?
C93 B2 C75 108.4(2) . . ?
C30 C31 C26 122.7(3) . . ?
C30 C31 H31 118.6 . . ?
C26 C31 H31 118.6 . . ?
C89 C90 C91 118.4(3) . . ?
C89 C90 H90 120.8 . . ?
C91 C90 H90 120.8 . . ?
C26 B1 C32 111.0(2) . . ?
C26 B1 C44 112.7(2) . . ?
C32 B1 C44 109.5(2) . . ?
C26 B1 C38 108.4(2) . . ?
C32 B1 C38 107.1(2) . . ?
C44 B1 C38 107.8(2) . . ?
C28 C27 C26 123.4(3) . . ?
C28 C27 H27 118.3 . . ?
C26 C27 H27 118.3 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N6 C51 O7 118.8(3) . . ?
N6 C51 C50 125.6(3) . . ?
O7 C51 C50 115.5(3) . . ?
C47 C48 C49 120.6(3) . . ?
C47 C48 H48 119.7 . . ?
C49 C48 H48 119.7 . . ?
C98 C97 C96 120.4(3) . . ?
C98 C97 H97 119.8 . . ?
C96 C97 H97 119.8 . . ?
C59 C60 H60A 109.5 . . ?
C59 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C59 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C53 C55 H55A 109.5 . . ?
C53 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C53 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C77 C78 C79 118.9(3) . . ?
C77 C78 H78 120.6 . . ?
C79 C78 H78 120.6 . . ?
C42 C41 C40 118.3(3) . . ?
C42 C41 H41 120.8 . . ?
C40 C41 H41 120.8 . . ?
C74 C73 C72 120.8(4) . . ?
C74 C73 H73 119.6 . . ?
C72 C73 H73 119.6 . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
N5 C50 C51 111.3(2) . . ?
N5 C50 H50A 109.4 . . ?
C51 C50 H50A 109.4 . . ?
N5 C50 H50B 109.4 . . ?
C51 C50 H50B 109.4 . . ?
H50A C50 H50B 108.0 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C89 C88 C87 122.8(3) . . ?
C89 C88 H88 118.6 . . ?
C87 C88 H88 118.6 . . ?
C14 C13 N1 110.0(2) . . ?
C14 C13 H13A 109.7 . . ?
N1 C13 H13A 109.7 . . ?
C14 C13 H13B 109.7 . . ?
N1 C13 H13B 109.7 . . ?
H13A C13 H13B 108.2 . . ?
N8 C63 O9 119.2(3) . . ?
N8 C63 C62 124.5(3) . . ?
O9 C63 C62 116.3(3) . . ?
C25 C24 C23 119.7(3) . . ?
C25 C24 H24 120.1 . . ?
C23 C24 H24 120.1 . . ?
C27 C28 C29 120.3(3) . . ?
C27 C28 H28 119.9 . . ?
C29 C28 H28 119.9 . . ?
C78 C79 C80 120.2(3) . . ?
C78 C79 H79 119.9 . . ?
C80 C79 H79 119.9 . . ?
C95 C96 C97 118.7(3) . . ?
C95 C96 H96 120.6 . . ?
C97 C96 H96 120.6 . . ?
O9 C64 C65 105.0(2) . . ?
O9 C64 H64A 110.7 . . ?
C65 C64 H64A 110.7 . . ?
O9 C64 H64B 110.7 . . ?
C65 C64 H64B 110.7 . . ?
H64A C64 H64B 108.8 . . ?
C90 C89 C88 120.7(3) . . ?
C90 C89 H89 119.7 . . ?
C88 C89 H89 119.7 . . ?
O7 C52 C53 105.6(3) . . ?
O7 C52 H52A 110.6 . . ?
C53 C52 H52A 110.6 . . ?
O7 C52 H52B 110.6 . . ?
C53 C52 H52B 110.6 . . ?
H52A C52 H52B 108.7 . . ?
C65 C67 H67A 109.5 . . ?
C65 C67 H67B 109.5 . . ?
H67A C67 H67B 109.5 . . ?
C65 C67 H67C 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
N5 C62 C63 109.9(2) . . ?
N5 C62 H62A 109.7 . . ?
C63 C62 H62A 109.7 . . ?
N5 C62 H62B 109.7 . . ?
C63 C62 H62B 109.7 . . ?
H62A C62 H62B 108.2 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C41 C42 C43 121.0(3) . . ?
C41 C42 H42 119.5 . . ?
C43 C42 H42 119.5 . . ?
C46 C47 C48 118.8(3) . . ?
C46 C47 H47 120.6 . . ?
C48 C47 H47 120.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C8 O2 C9 C10 -12.4(3) . . . . ?
C25 C20 C21 C22 0.1(4) . . . . ?
C19 C20 C21 C22 -179.1(3) . . . . ?
C74 C69 C70 C71 0.2(5) . . . . ?
C68 C69 C70 C71 178.0(3) . . . . ?
C57 N7 C59 C60 -130.8(3) . . . . ?
Ni2 N7 C59 C60 71.4(4) . . . . ?
C57 N7 C59 C61 106.6(3) . . . . ?
Ni2 N7 C59 C61 -51.1(4) . . . . ?
C57 N7 C59 C58 -12.1(3) . . . . ?
Ni2 N7 C59 C58 -169.8(2) . . . . ?
C69 C70 C71 C72 -1.9(5) . . . . ?
C69 C70 C71 Cl2 179.4(2) . . . . ?
C45 C44 C49 C48 -3.2(4) . . . . ?
B1 C44 C49 C48 169.0(3) . . . . ?
C88 C87 C92 C91 -0.3(4) . . . . ?
B2 C87 C92 C91 -172.9(3) . . . . ?
C34 C35 C36 C37 -1.2(5) . . . . ?
C95 C94 C93 C98 1.8(4) . . . . ?
C95 C94 C93 B2 178.1(3) . . . . ?
C97 C98 C93 C94 -0.7(4) . . . . ?
C97 C98 C93 B2 -177.2(3) . . . . ?
C35 C36 C37 C32 -0.3(5) . . . . ?
C40 C39 C38 C43 -0.4(4) . . . . ?
C40 C39 C38 B1 172.6(3) . . . . ?
C49 C44 C45 C46 3.9(4) . . . . ?
B1 C44 C45 C46 -168.1(3) . . . . ?
C82 C81 C86 C85 -0.7(4) . . . . ?
B2 C81 C86 C85 176.1(3) . . . . ?
C16 N4 C14 O3 2.3(3) . . . . ?
Ni1 N4 C14 O3 -177.80(19) . . . . ?
C16 N4 C14 C13 -175.3(3) . . . . ?
Ni1 N4 C14 C13 4.7(4) . . . . ?
C15 O3 C14 N4 0.8(3) . . . . ?
C15 O3 C14 C13 178.6(2) . . . . ?
C8 N3 C10 C12 -131.1(3) . . . . ?
Ni1 N3 C10 C12 65.9(4) . . . . ?
C8 N3 C10 C11 106.3(3) . . . . ?
Ni1 N3 C10 C11 -56.7(4) . . . . ?
C8 N3 C10 C9 -11.3(3) . . . . ?
Ni1 N3 C10 C9 -174.3(2) . . . . ?
O2 C9 C10 N3 14.2(3) . . . . ?
O2 C9 C10 C12 132.0(3) . . . . ?
O2 C9 C10 C11 -101.7(3) . . . . ?
C14 O3 C15 C16 -3.3(3) . . . . ?
C36 C35 C34 C33 1.2(4) . . . . ?
C38 C39 C40 C41 0.8(5) . . . . ?
C36 C37 C32 C33 1.8(4) . . . . ?
C36 C37 C32 B1 -176.8(3) . . . . ?
C21 C20 C25 C24 0.4(5) . . . . ?
C19 C20 C25 C24 179.6(3) . . . . ?
C4 N2 C2 O1 -3.5(4) . . . . ?
Ni1 N2 C2 O1 -172.8(2) . . . . ?
C4 N2 C2 C1 173.1(3) . . . . ?
Ni1 N2 C2 C1 3.7(4) . . . . ?
C3 O1 C2 N2 -5.5(4) . . . . ?
C3 O1 C2 C1 177.6(3) . . . . ?
C14 N4 C16 C18 -123.4(3) . . . . ?
Ni1 N4 C16 C18 56.7(4) . . . . ?
C14 N4 C16 C17 113.8(3) . . . . ?
Ni1 N4 C16 C17 -66.1(4) . . . . ?
C14 N4 C16 C15 -4.0(3) . . . . ?
Ni1 N4 C16 C15 176.1(2) . . . . ?
O3 C15 C16 N4 4.4(3) . . . . ?
O3 C15 C16 C18 122.2(3) . . . . ?
O3 C15 C16 C17 -112.6(3) . . . . ?
C57 O8 C58 C59 -14.8(3) . . . . ?
N7 C59 C58 O8 16.1(3) . . . . ?
C60 C59 C58 O8 133.7(3) . . . . ?
C61 C59 C58 O8 -101.0(3) . . . . ?
C44 C45 C46 C47 -1.8(5) . . . . ?
C1 N1 C7 C8 160.0(2) . . . . ?
C13 N1 C7 C8 -74.6(3) . . . . ?
Ni1 N1 C7 C8 40.8(2) . . . . ?
C2 O1 C3 C4 11.5(3) . . . . ?
C81 C86 C85 C84 0.7(5) . . . . ?
Ni2 O10 C68 O11 -15.4(5) . . . . ?
Ni2 O10 C68 C69 162.28(19) . . . . ?
C74 C69 C68 O11 177.5(3) . . . . ?
C70 C69 C68 O11 -0.2(4) . . . . ?
C74 C69 C68 O10 -0.4(4) . . . . ?
C70 C69 C68 O10 -178.0(3) . . . . ?
C20 C21 C22 C23 -0.2(5) . . . . ?
C20 C21 C22 Cl1 -177.5(2) . . . . ?
C7 N1 C1 C2 -123.8(3) . . . . ?
C13 N1 C1 C2 111.8(3) . . . . ?
Ni1 N1 C1 C2 -7.0(3) . . . . ?
N2 C2 C1 N1 2.6(4) . . . . ?
O1 C2 C1 N1 179.3(2) . . . . ?
C63 N8 C65 C67 114.4(3) . . . . ?
Ni2 N8 C65 C67 -58.3(4) . . . . ?
C63 N8 C65 C66 -123.4(3) . . . . ?
Ni2 N8 C65 C66 63.9(4) . . . . ?
C63 N8 C65 C64 -5.0(3) . . . . ?
Ni2 N8 C65 C64 -177.6(2) . . . . ?
C10 N3 C8 O2 3.9(4) . . . . ?
Ni1 N3 C8 O2 172.1(2) . . . . ?
C10 N3 C8 C7 -175.9(3) . . . . ?
Ni1 N3 C8 C7 -7.7(4) . . . . ?
C9 O2 C8 N3 6.0(4) . . . . ?
C9 O2 C8 C7 -174.2(3) . . . . ?
N1 C7 C8 N3 -24.4(4) . . . . ?
N1 C7 C8 O2 155.8(2) . . . . ?
C84 C83 C82 C81 -0.8(5) . . . . ?
C86 C81 C82 C83 0.8(4) . . . . ?
B2 C81 C82 C83 -176.0(3) . . . . ?
C82 C83 C84 C85 0.7(5) . . . . ?
C86 C85 C84 C83 -0.6(4) . . . . ?
C87 C92 C91 C90 -0.4(5) . . . . ?
C78 C77 C76 C75 -1.2(5) . . . . ?
C39 C38 C43 C42 -0.5(5) . . . . ?
B1 C38 C43 C42 -173.5(3) . . . . ?
C59 N7 C57 O8 3.2(4) . . . . ?
Ni2 N7 C57 O8 168.8(2) . . . . ?
C59 N7 C57 C56 -176.9(3) . . . . ?
Ni2 N7 C57 C56 -11.2(4) . . . . ?
C58 O8 C57 N7 7.9(4) . . . . ?
C58 O8 C57 C56 -172.1(3) . . . . ?
C2 N2 C4 C6 129.0(3) . . . . ?
Ni1 N2 C4 C6 -66.1(4) . . . . ?
C2 N2 C4 C5 -107.7(3) . . . . ?
Ni1 N2 C4 C5 57.2(4) . . . . ?
C2 N2 C4 C3 10.2(3) . . . . ?
Ni1 N2 C4 C3 175.0(2) . . . . ?
O1 C3 C4 N2 -13.0(3) . . . . ?
O1 C3 C4 C6 -131.2(3) . . . . ?
O1 C3 C4 C5 103.0(3) . . . . ?
C70 C71 C72 C73 2.2(6) . . . . ?
Cl2 C71 C72 C73 -179.1(3) . . . . ?
N7 C57 C56 N5 -22.3(4) . . . . ?
O8 C57 C56 N5 157.7(2) . . . . ?
C50 N5 C56 C57 160.9(2) . . . . ?
C62 N5 C56 C57 -73.2(3) . . . . ?
Ni2 N5 C56 C57 41.9(3) . . . . ?
C51 N6 C53 C55 127.4(3) . . . . ?
Ni2 N6 C53 C55 -67.7(4) . . . . ?
C51 N6 C53 C54 -109.4(3) . . . . ?
Ni2 N6 C53 C54 55.6(4) . . . . ?
C51 N6 C53 C52 8.5(4) . . . . ?
Ni2 N6 C53 C52 173.4(3) . . . . ?
C35 C34 C33 C32 0.4(4) . . . . ?
C37 C32 C33 C34 -1.8(4) . . . . ?
B1 C32 C33 C34 176.8(3) . . . . ?
Ni1 O4 C19 O5 10.7(4) . . . . ?
Ni1 O4 C19 C20 -168.31(18) . . . . ?
C25 C20 C19 O5 166.8(3) . . . . ?
C21 C20 C19 O5 -14.0(4) . . . . ?
C25 C20 C19 O4 -14.2(4) . . . . ?
C21 C20 C19 O4 165.1(3) . . . . ?
C70 C69 C74 C73 1.1(5) . . . . ?
C68 C69 C74 C73 -176.6(3) . . . . ?
C93 C94 C95 C96 -1.3(5) . . . . ?
C21 C22 C23 C24 -0.3(5) . . . . ?
Cl1 C22 C23 C24 177.1(3) . . . . ?
C31 C30 C29 C28 -0.9(5) . . . . ?
C79 C80 C75 C76 -2.2(4) . . . . ?
C79 C80 C75 B2 175.4(3) . . . . ?
C77 C76 C75 C80 2.9(5) . . . . ?
C77 C76 C75 B2 -174.8(3) . . . . ?
C86 C81 B2 C87 71.5(4) . . . . ?
C82 C81 B2 C87 -111.9(3) . . . . ?
C86 C81 B2 C93 -162.5(3) . . . . ?
C82 C81 B2 C93 14.1(4) . . . . ?
C86 C81 B2 C75 -45.7(3) . . . . ?
C82 C81 B2 C75 130.9(3) . . . . ?
C92 C87 B2 C81 -24.0(4) . . . . ?
C88 C87 B2 C81 163.8(3) . . . . ?
C92 C87 B2 C93 -147.6(3) . . . . ?
C88 C87 B2 C93 40.2(4) . . . . ?
C92 C87 B2 C75 93.8(3) . . . . ?
C88 C87 B2 C75 -78.4(3) . . . . ?
C94 C93 B2 C81 -109.1(3) . . . . ?
C98 C93 B2 C81 67.0(3) . . . . ?
C94 C93 B2 C87 17.5(4) . . . . ?
C98 C93 B2 C87 -166.5(3) . . . . ?
C94 C93 B2 C75 134.8(3) . . . . ?
C98 C93 B2 C75 -49.1(4) . . . . ?
C80 C75 B2 C81 147.6(3) . . . . ?
C76 C75 B2 C81 -35.0(4) . . . . ?
C80 C75 B2 C87 25.6(4) . . . . ?
C76 C75 B2 C87 -157.0(3) . . . . ?
C80 C75 B2 C93 -95.7(3) . . . . ?
C76 C75 B2 C93 81.7(3) . . . . ?
C29 C30 C31 C26 0.1(5) . . . . ?
C27 C26 C31 C30 0.5(4) . . . . ?
B1 C26 C31 C30 -176.7(3) . . . . ?
C92 C91 C90 C89 0.9(5) . . . . ?
C31 C26 B1 C32 13.9(4) . . . . ?
C27 C26 B1 C32 -163.1(3) . . . . ?
C31 C26 B1 C44 -109.3(3) . . . . ?
C27 C26 B1 C44 73.6(3) . . . . ?
C31 C26 B1 C38 131.4(3) . . . . ?
C27 C26 B1 C38 -45.7(4) . . . . ?
C33 C32 B1 C26 106.0(3) . . . . ?
C37 C32 B1 C26 -75.5(3) . . . . ?
C33 C32 B1 C44 -129.0(3) . . . . ?
C37 C32 B1 C44 49.5(4) . . . . ?
C33 C32 B1 C38 -12.3(4) . . . . ?
C37 C32 B1 C38 166.2(3) . . . . ?
C45 C44 B1 C26 -32.1(4) . . . . ?
C49 C44 B1 C26 156.3(3) . . . . ?
C45 C44 B1 C32 -156.2(3) . . . . ?
C49 C44 B1 C32 32.2(4) . . . . ?
C45 C44 B1 C38 87.6(3) . . . . ?
C49 C44 B1 C38 -84.0(3) . . . . ?
C39 C38 B1 C26 159.1(3) . . . . ?
C43 C38 B1 C26 -28.4(4) . . . . ?
C39 C38 B1 C32 -81.0(3) . . . . ?
C43 C38 B1 C32 91.6(3) . . . . ?
C39 C38 B1 C44 36.8(4) . . . . ?
C43 C38 B1 C44 -150.6(3) . . . . ?
C31 C26 C27 C28 -0.3(5) . . . . ?
B1 C26 C27 C28 177.0(3) . . . . ?
C53 N6 C51 O7 -2.2(4) . . . . ?
Ni2 N6 C51 O7 -171.6(2) . . . . ?
C53 N6 C51 C50 175.2(3) . . . . ?
Ni2 N6 C51 C50 5.9(4) . . . . ?
C52 O7 C51 N6 -5.7(4) . . . . ?
C52 O7 C51 C50 176.6(3) . . . . ?
C44 C49 C48 C47 0.4(5) . . . . ?
C93 C98 C97 C96 -1.0(5) . . . . ?
C76 C77 C78 C79 -1.4(5) . . . . ?
C39 C40 C41 C42 -0.3(5) . . . . ?
C69 C74 C73 C72 -0.8(6) . . . . ?
C71 C72 C73 C74 -0.8(6) . . . . ?
C56 N5 C50 C51 -120.0(3) . . . . ?
C62 N5 C50 C51 115.1(3) . . . . ?
Ni2 N5 C50 C51 -4.1(3) . . . . ?
N6 C51 C50 N5 -1.1(4) . . . . ?
O7 C51 C50 N5 176.5(3) . . . . ?
C92 C87 C88 C89 0.4(5) . . . . ?
B2 C87 C88 C89 173.1(3) . . . . ?
N4 C14 C13 N1 -19.6(4) . . . . ?
O3 C14 C13 N1 162.8(2) . . . . ?
C1 N1 C13 C14 -97.7(3) . . . . ?
C7 N1 C13 C14 136.0(2) . . . . ?
Ni1 N1 C13 C14 22.2(2) . . . . ?
C65 N8 C63 O9 0.8(4) . . . . ?
Ni2 N8 C63 O9 175.6(2) . . . . ?
C65 N8 C63 C62 -177.2(3) . . . . ?
Ni2 N8 C63 C62 -2.4(4) . . . . ?
C64 O9 C63 N8 4.0(4) . . . . ?
C64 O9 C63 C62 -177.8(3) . . . . ?
C20 C25 C24 C23 -0.9(6) . . . . ?
C22 C23 C24 C25 0.8(6) . . . . ?
C26 C27 C28 C29 -0.5(6) . . . . ?
C30 C29 C28 C27 1.1(6) . . . . ?
C77 C78 C79 C80 2.1(5) . . . . ?
C75 C80 C79 C78 -0.2(5) . . . . ?
C94 C95 C96 C97 -0.5(5) . . . . ?
C98 C97 C96 C95 1.6(5) . . . . ?
C63 O9 C64 C65 -6.7(3) . . . . ?
N8 C65 C64 O9 7.0(3) . . . . ?
C67 C65 C64 O9 -109.8(3) . . . . ?
C66 C65 C64 O9 124.6(3) . . . . ?
C91 C90 C89 C88 -0.8(5) . . . . ?
C87 C88 C89 C90 0.2(6) . . . . ?
C51 O7 C52 C53 10.6(4) . . . . ?
N6 C53 C52 O7 -11.4(4) . . . . ?
C55 C53 C52 O7 -130.2(3) . . . . ?
C54 C53 C52 O7 104.4(3) . . . . ?
C50 N5 C62 C63 -97.0(3) . . . . ?
C56 N5 C62 C63 136.5(3) . . . . ?
Ni2 N5 C62 C63 23.4(3) . . . . ?
N8 C63 C62 N5 -15.7(4) . . . . ?
O9 C63 C62 N5 166.2(3) . . . . ?
C40 C41 C42 C43 -0.6(5) . . . . ?
C38 C43 C42 C41 1.1(5) . . . . ?
C45 C46 C47 C48 -1.2(5) . . . . ?
C49 C48 C47 C46 1.9(5) . . . . ?

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
C61 H61C O11 0.98 2.49 3.300(4) 139.6 .
C15 H15B O5 0.99 2.39 3.304(4) 153.3 1_554
O12 H51A O11 0.80(4) 1.85(4) 2.634(3) 163(4) .
O6 H2A O5 0.95(5) 1.72(4) 2.648(3) 164(4) .

_refine_diff_density_max         0.272
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.043

