# 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_mo_burst101_0ma_a
_audit_block_doi                 10.5517/ccdc.csd.cc25bxfw
_database_code_depnum_ccdc_archive 'CCDC 2006488'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/D0DT01968B 2020
loop_
_audit_author_name
_audit_author_address
'Stefan Burger'
;Technical University of Munich
Germany
;
_audit_update_record             
;
2020-05-28 deposited with the CCDC.	2020-08-04 downloaded from the CCDC.
;
_audit_creation_date             2020-04-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        '6-azaspiro[5.5]undecane cadmium dicyanamide'
_chemical_formula_moiety         'C6 Cd N9, C10 H20 N'
_chemical_formula_sum            'C16 H20 Cd N10'
_chemical_formula_weight         464.82
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z+1/2'

_cell_length_a                   17.1022(9)
_cell_length_b                   10.7274(5)
_cell_length_c                   10.7037(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1963.72(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9910
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.098
_cell_measurement_theta_min      2.241
_shelx_estimated_absorpt_T_max   0.848
_shelx_estimated_absorpt_T_min   0.848
_exptl_absorpt_coefficient_mu    1.135
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7246
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0863 before and 0.0597 after correction. The Ratio of minimum to maximum transmission is 0.9718. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             936
_exptl_crystal_preparation       
'suitable crystal prepared in perfluoroether oil'
_exptl_crystal_recrystallization_method 'mild solution approach'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_unetI/netI     0.0160
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            63288
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.098
_diffrn_reflns_theta_min         2.241
_diffrn_ambient_temperature      100.03
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_special_details          none
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.898
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                4178
_reflns_number_total             4336
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.237
_refine_diff_density_min         -0.420
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.09(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         4336
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0175
_refine_ls_R_factor_gt           0.0153
_refine_ls_restrained_S_all      1.125
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0154P)²+0.5777P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0355
_refine_ls_wR_factor_ref         0.0377
_refine_special_details          none,Twin
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.91(2)
 0.09(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C2(H2A,H2B), C1(H1A,H1B), C5(H5A,H5B), C8(H8A,H8B), C7(H7A,H7B),
 C10(H10A,H10B), C4(H4A,H4B), C3(H3A,H3B), C6(H6A,H6B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.34423(2) 0.73561(2) 0.39008(3) 0.01593(5) Uani 1 1 d . . . . .
N1 N 0.51898(12) 0.25041(18) 0.3764(4) 0.0191(6) Uani 1 1 d . . . . .
N3 N 0.23836(15) 0.4016(2) 0.5486(2) 0.0286(5) Uani 1 1 d . . . . .
C9 C 0.38273(16) 0.1615(3) 0.3990(4) 0.0310(6) Uani 1 1 d . . . . .
H9A H 0.346594 0.098549 0.363725 0.037 Uiso 1 1 calc R . . . .
H9B H 0.357371 0.244126 0.391675 0.037 Uiso 1 1 calc R . . . .
C16 C 0.52649(16) 0.8371(2) 0.4371(3) 0.0206(5) Uani 1 1 d . . . . .
N4 N 0.34393(14) 0.5517(3) 0.5068(2) 0.0257(5) Uani 1 1 d . . . . .
N9 N 0.58966(13) 0.9034(2) 0.4226(3) 0.0365(9) Uani 1 1 d . . . . .
C15 C 0.65411(13) 0.8523(2) 0.3808(5) 0.0246(6) Uani 1 1 d . . . . .
C2 C 0.55105(15) 0.4775(2) 0.4030(4) 0.0253(6) Uani 1 1 d . . . . .
H2A H 0.560505 0.467089 0.493620 0.030 Uiso 1 1 calc R . . . .
H2B H 0.530411 0.562568 0.389071 0.030 Uiso 1 1 calc R . . . .
C12 C 0.29360(17) 0.4835(3) 0.5310(2) 0.0213(5) Uani 1 1 d . . . . .
C1 C 0.49144(16) 0.3832(2) 0.3603(2) 0.0234(6) Uani 1 1 d . . . . .
H1A H 0.479387 0.397924 0.271033 0.028 Uiso 1 1 calc R . . . .
H1B H 0.442579 0.395163 0.408417 0.028 Uiso 1 1 calc R . . . .
C11 C 0.19932(16) 0.3998(2) 0.6532(3) 0.0211(5) Uani 1 1 d . . . . .
N10 N 0.46742(14) 0.7885(2) 0.4545(2) 0.0239(5) Uani 1 1 d . . . . .
C5 C 0.59395(16) 0.2350(3) 0.3026(3) 0.0257(6) Uani 1 1 d . . . . .
H5A H 0.582422 0.245765 0.212587 0.031 Uiso 1 1 calc R . . . .
H5B H 0.614078 0.149354 0.314808 0.031 Uiso 1 1 calc R . . . .
C8 C 0.39692(19) 0.1326(3) 0.5362(3) 0.0342(7) Uani 1 1 d . . . . .
H8A H 0.414124 0.044936 0.545182 0.041 Uiso 1 1 calc R . . . .
H8B H 0.347629 0.143082 0.583499 0.041 Uiso 1 1 calc R . . . .
C7 C 0.4594(2) 0.2195(3) 0.5893(3) 0.0299(7) Uani 1 1 d . . . . .
H7A H 0.438950 0.305786 0.591231 0.036 Uiso 1 1 calc R . . . .
H7B H 0.471547 0.194409 0.676217 0.036 Uiso 1 1 calc R . . . .
C10 C 0.45798(17) 0.1617(3) 0.3238(3) 0.0263(6) Uani 1 1 d . . . . .
H10A H 0.446108 0.185836 0.236597 0.032 Uiso 1 1 calc R . . . .
H10B H 0.479814 0.076232 0.322479 0.032 Uiso 1 1 calc R . . . .
N8 N 0.71296(13) 0.8175(3) 0.3431(3) 0.0311(6) Uani 1 1 d . . . . .
C4 C 0.65668(16) 0.3277(3) 0.3408(3) 0.0287(6) Uani 1 1 d . . . . .
H4A H 0.702785 0.317270 0.285827 0.034 Uiso 1 1 calc R . . . .
H4B H 0.673279 0.309880 0.427567 0.034 Uiso 1 1 calc R . . . .
C3 C 0.62790(19) 0.4622(3) 0.3325(3) 0.0305(6) Uani 1 1 d . . . . .
H3A H 0.667712 0.518759 0.368592 0.037 Uiso 1 1 calc R . . . .
H3B H 0.620312 0.485380 0.243816 0.037 Uiso 1 1 calc R . . . .
C6 C 0.53346(18) 0.2156(3) 0.5117(3) 0.0225(6) Uani 1 1 d . . . . .
H6A H 0.572223 0.273833 0.547902 0.027 Uiso 1 1 calc R . . . .
H6B H 0.555894 0.130576 0.515305 0.027 Uiso 1 1 calc R . . . .
N2 N 0.15985(14) 0.3899(2) 0.7408(2) 0.0237(5) Uani 1 1 d . . . . .
N7 N 0.29155(15) 0.8482(2) 0.5511(2) 0.0279(5) Uani 1 1 d . . . . .
C14 C 0.23797(17) 0.8779(3) 0.6096(3) 0.0234(6) Uani 1 1 d . . . . .
C13 C 0.15085(15) 1.0096(3) 0.7004(3) 0.0191(5) Uani 1 1 d . . . . .
N6 N 0.17649(17) 0.8978(2) 0.6789(3) 0.0343(6) Uani 1 1 d . . . . .
N5 N 0.12007(14) 1.1025(2) 0.7262(2) 0.0198(5) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 N4 2.335(3) . ?
Cd1 N10 2.288(2) . ?
Cd1 N8 2.370(2) 3_465 ?
Cd1 N2 2.302(2) 4_554 ?
Cd1 N7 2.290(2) . ?
Cd1 N5 2.343(2) 4_544 ?
N1 C1 1.510(3) . ?
N1 C5 1.515(4) . ?
N1 C10 1.520(4) . ?
N1 C6 1.516(5) . ?
N3 C12 1.304(4) . ?
N3 C11 1.304(4) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C8 1.520(6) . ?
C9 C10 1.517(4) . ?
C16 N9 1.302(4) . ?
C16 N10 1.152(4) . ?
N4 C12 1.159(4) . ?
N9 C15 1.310(4) . ?
C15 N8 1.147(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C1 1.507(4) . ?
C2 C3 1.524(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C11 N2 1.160(4) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C4 1.519(4) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C7 1.527(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C6 1.516(4) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C3 1.528(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
N7 C14 1.154(4) . ?
C14 N6 1.305(4) . ?
C13 N6 1.297(4) . ?
C13 N5 1.160(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 Cd1 N8 84.75(9) . 3_465 ?
N4 Cd1 N5 83.46(9) . 4_544 ?
N10 Cd1 N4 92.89(9) . . ?
N10 Cd1 N8 174.66(9) . 3_465 ?
N10 Cd1 N2 93.37(9) . 4_554 ?
N10 Cd1 N7 90.26(9) . . ?
N10 Cd1 N5 97.87(9) . 4_544 ?
N2 Cd1 N4 168.21(9) 4_554 . ?
N2 Cd1 N8 89.81(9) 4_554 3_465 ?
N2 Cd1 N5 85.79(9) 4_554 4_544 ?
N7 Cd1 N4 92.43(9) . . ?
N7 Cd1 N8 85.06(9) . 3_465 ?
N7 Cd1 N2 97.53(9) . 4_554 ?
N7 Cd1 N5 171.05(9) . 4_544 ?
N5 Cd1 N8 86.64(9) 4_544 3_465 ?
C1 N1 C5 107.9(2) . . ?
C1 N1 C10 109.5(2) . . ?
C1 N1 C6 113.1(3) . . ?
C5 N1 C10 108.6(3) . . ?
C5 N1 C6 109.5(2) . . ?
C6 N1 C10 108.2(2) . . ?
C12 N3 C11 120.4(2) . . ?
H9A C9 H9B 107.9 . . ?
C8 C9 H9A 109.2 . . ?
C8 C9 H9B 109.2 . . ?
C10 C9 H9A 109.2 . . ?
C10 C9 H9B 109.2 . . ?
C10 C9 C8 112.1(3) . . ?
N10 C16 N9 173.6(3) . . ?
C12 N4 Cd1 130.9(2) . . ?
C16 N9 C15 120.7(2) . . ?
N8 C15 N9 174.3(3) . . ?
H2A C2 H2B 108.0 . . ?
C1 C2 H2A 109.4 . . ?
C1 C2 H2B 109.4 . . ?
C1 C2 C3 111.2(3) . . ?
C3 C2 H2A 109.4 . . ?
C3 C2 H2B 109.4 . . ?
N4 C12 N3 174.8(3) . . ?
N1 C1 H1A 109.0 . . ?
N1 C1 H1B 109.0 . . ?
C2 C1 N1 112.8(2) . . ?
C2 C1 H1A 109.0 . . ?
C2 C1 H1B 109.0 . . ?
H1A C1 H1B 107.8 . . ?
N2 C11 N3 173.4(3) . . ?
C16 N10 Cd1 150.6(2) . . ?
N1 C5 H5A 109.1 . . ?
N1 C5 H5B 109.1 . . ?
N1 C5 C4 112.7(2) . . ?
H5A C5 H5B 107.8 . . ?
C4 C5 H5A 109.1 . . ?
C4 C5 H5B 109.1 . . ?
C9 C8 H8A 109.6 . . ?
C9 C8 H8B 109.6 . . ?
C9 C8 C7 110.3(3) . . ?
H8A C8 H8B 108.1 . . ?
C7 C8 H8A 109.6 . . ?
C7 C8 H8B 109.6 . . ?
C8 C7 H7A 109.4 . . ?
C8 C7 H7B 109.4 . . ?
H7A C7 H7B 108.0 . . ?
C6 C7 C8 111.3(3) . . ?
C6 C7 H7A 109.4 . . ?
C6 C7 H7B 109.4 . . ?
N1 C10 H10A 109.0 . . ?
N1 C10 H10B 109.0 . . ?
C9 C10 N1 112.7(3) . . ?
C9 C10 H10A 109.0 . . ?
C9 C10 H10B 109.0 . . ?
H10A C10 H10B 107.8 . . ?
C15 N8 Cd1 146.6(3) . 3_565 ?
C5 C4 H4A 109.2 . . ?
C5 C4 H4B 109.2 . . ?
C5 C4 C3 112.0(2) . . ?
H4A C4 H4B 107.9 . . ?
C3 C4 H4A 109.2 . . ?
C3 C4 H4B 109.2 . . ?
C2 C3 C4 110.5(2) . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
C4 C3 H3A 109.5 . . ?
C4 C3 H3B 109.5 . . ?
H3A C3 H3B 108.1 . . ?
N1 C6 C7 112.4(2) . . ?
N1 C6 H6A 109.1 . . ?
N1 C6 H6B 109.1 . . ?
C7 C6 H6A 109.1 . . ?
C7 C6 H6B 109.1 . . ?
H6A C6 H6B 107.9 . . ?
C11 N2 Cd1 130.1(2) . 4_545 ?
C14 N7 Cd1 150.0(2) . . ?
N7 C14 N6 173.4(3) . . ?
N5 C13 N6 171.6(3) . . ?
C13 N6 C14 121.6(3) . . ?
C13 N5 Cd1 125.7(2) . 4 ?

_olex2_exptl_crystal_mounting_method 'on microloop sample holder'
_olex2_submission_original_sample_id C16H20CdN10
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.91(2)
2 0.09(2)

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

data_mo_burst114_0m_a
_audit_block_doi                 10.5517/ccdc.csd.cc25bxgx
_database_code_depnum_ccdc_archive 'CCDC 2006489'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/D0DT01968B 2020
loop_
_audit_author_name
_audit_author_address
'Stefan Burger'
;Technical University of Munich
Germany
;
_audit_update_record             
;
2020-05-28 deposited with the CCDC.	2020-08-04 downloaded from the CCDC.
;
_audit_creation_date             2020-05-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        C32H44N20Ni2O2
_chemical_formula_moiety         'C12 H4 N18 Ni2 O2, 2.71(C7.37 H14.75 N0.75)'
_chemical_formula_sum            'C32 H44 N20 Ni2 O2'
_chemical_formula_weight         858.29
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   20.3343(9)
_cell_length_b                   9.9398(5)
_cell_length_c                   20.5387(10)
_cell_angle_alpha                90
_cell_angle_beta                 106.735(2)
_cell_angle_gamma                90
_cell_volume                     3975.4(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9528
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.124
_cell_measurement_theta_min      2.033
_shelx_estimated_absorpt_T_max   0.868
_shelx_estimated_absorpt_T_min   0.601
_exptl_absorpt_coefficient_mu    1.005
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.7116
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0792 before and 0.0692 after correction. The Ratio of minimum to maximum transmission is 0.9545. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear greenish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1792
_exptl_crystal_preparation       'crystal prepared in perfluoroether oil'
_exptl_crystal_recrystallization_method 'mild solution approach'
_exptl_crystal_size_max          0.563
_exptl_crystal_size_mid          0.178
_exptl_crystal_size_min          0.145
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0626
_diffrn_reflns_av_unetI/netI     0.0173
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            185972
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.033
_diffrn_ambient_temperature      100.01
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_special_details          none
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7373
_reflns_number_total             8145
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.692
_refine_diff_density_min         -0.615
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       0.00057(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         8145
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0483
_refine_ls_restrained_S_all      1.085
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+19.5027P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1045
_refine_ls_wR_factor_ref         0.1146
_refine_special_details          none,Twin
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.9406(8)
 0.0594(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C24) = Uanis(C31) = Uanis(C23) = Uanis(C26) = Uanis(C25) = Uanis(C29) =
Uanis(C30) = Uanis(C27) = Uanis(C28) = Uanis(C21) = Uanis(C22) = Uanis(C33) =
Uanis(C37) = Uanis(C35) = Uanis(C36) = Uanis(C39) = Uanis(C40) = Uanis(C38) =
Uanis(C34) = Uanis(C32) = Uanis(C7) = Uanis(C10) = Uanis(C8) = Uanis(C1) =
Uanis(C2) = Uanis(C4) = Uanis(C3) = Uanis(C5) = Uanis(C6) = Uanis(C9) =
Uanis(C14) = Uanis(C13) = Uanis(C17) = Uanis(C20) = Uanis(C11) = Uanis(C16) =
Uanis(C12) = Uanis(C18) = Uanis(C19) = Uanis(C15)
Uanis(N3) = Uanis(N4) = Uanis(N1) = Uanis(N2)
Uanis(N21) = Uanis(N15B) = Uanis(N15A)
4. Others
 Sof(C24)=Sof(H24A)=Sof(H24B)=1-FVAR(1)
 Sof(C23)=Sof(H23A)=Sof(H23B)=FVAR(1)
 Sof(C26)=Sof(H26A)=Sof(H26B)=1-FVAR(2)
 Sof(C25)=Sof(H25A)=Sof(H25B)=FVAR(2)
 Sof(C30)=Sof(H30A)=Sof(H30B)=1-FVAR(3)
 Sof(C29)=Sof(H29A)=Sof(H29B)=FVAR(3)
 Sof(C28)=Sof(H28A)=Sof(H28B)=1-FVAR(4)
 Sof(C27)=Sof(H27A)=Sof(H27B)=FVAR(4)
 Sof(C22)=Sof(H22A)=Sof(H22B)=1-FVAR(5)
 Sof(C21)=Sof(H21A)=Sof(H21B)=FVAR(5)
 Sof(N3)=1-FVAR(6)
 Sof(N4)=FVAR(6)
 Sof(C1)=Sof(H1C)=Sof(H1D)=1-FVAR(7)
 Sof(C2)=Sof(H2C)=Sof(H2D)=FVAR(7)
 Sof(C8)=Sof(H8A)=Sof(H8B)=1-FVAR(8)
 Sof(C7)=Sof(H7A)=Sof(H7B)=FVAR(8)
 Sof(C5)=Sof(H5A)=Sof(H5B)=1-FVAR(9)
 Sof(C6)=Sof(H6A)=Sof(H6B)=FVAR(9)
 Sof(C4)=Sof(H4A)=Sof(H4B)=1-FVAR(10)
 Sof(C3)=Sof(H3A)=Sof(H3B)=FVAR(10)
 Sof(C16)=Sof(H16A)=Sof(H16B)=1-FVAR(11)
 Sof(C15)=Sof(H15A)=Sof(H15B)=FVAR(11)
 Sof(C19)=Sof(H19A)=Sof(H19B)=1-FVAR(12)
 Sof(C20)=Sof(H20A)=Sof(H20B)=FVAR(12)
 Sof(C18)=Sof(H18A)=Sof(H18B)=1-FVAR(13)
 Sof(C17)=Sof(H17A)=Sof(H17B)=FVAR(13)
 Sof(C13)=Sof(H13A)=Sof(H13B)=1-FVAR(14)
 Sof(C14)=Sof(H14A)=Sof(H14B)=FVAR(14)
 Sof(N2)=1-FVAR(15)
 Sof(N1)=FVAR(15)
 Sof(C12)=Sof(H12A)=Sof(H12B)=1-FVAR(16)
 Sof(C11)=Sof(H11A)=Sof(H11B)=FVAR(16)
 Sof(C10)=Sof(H10A)=Sof(H10B)=1-FVAR(17)
 Sof(C9)=Sof(H9A)=Sof(H9B)=FVAR(17)
 Sof(C34)=Sof(H34A)=Sof(H34B)=1-FVAR(18)
 Sof(C33)=Sof(H33A)=Sof(H33B)=FVAR(18)
 Sof(C32)=Sof(H32A)=Sof(H32B)=1-FVAR(19)
 Sof(C31)=Sof(H31A)=Sof(H31B)=FVAR(19)
 Sof(C38)=Sof(H38A)=Sof(H38B)=1-FVAR(20)
 Sof(C37)=Sof(H37A)=Sof(H37B)=FVAR(20)
 Sof(C35)=Sof(H35A)=Sof(H35B)=1-FVAR(21)
 Sof(C36)=Sof(H36A)=Sof(H36B)=FVAR(21)
 Sof(C40)=Sof(H40A)=Sof(H40B)=1-FVAR(22)
 Sof(C39)=Sof(H39A)=Sof(H39B)=FVAR(22)
 Fixed Sof: N15B(0.5) N15A(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C6(H6A,H6B), C12(H12A,H12B), C19(H19A,H19B), C1(H1C,H1D),
 C17(H17A,H17B), C10(H10A,H10B), C23(H23A,H23B), C14(H14A,H14B), C8(H8A,H8B),
 C3(H3A,H3B), C30(H30A,H30B), C27(H27A,H27B), C21(H21A,H21B), C22(H22A,H22B),
 C26(H26A,H26B), C24(H24A,H24B), C28(H28A,H28B), C29(H29A,H29B), C25(H25A,H25B),
  C4(H4A,H4B), C13(H13A,H13B), C20(H20A,H20B), C5(H5A,H5B), C2(H2C,H2D),
 C18(H18A,H18B), C7(H7A,H7B), C16(H16A,H16B), C11(H11A,H11B), C9(H9A,H9B),
 C33(H33A,H33B), C31(H31A,H31B), C39(H39A,H39B), C37(H37A,H37B), C40(H40A,H40B),
  C36(H36A,H36B), C32(H32A,H32B), C38(H38A,H38B), C35(H35A,H35B), C34(H34A,H34B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni2 Ni 0.11011(2) 0.30410(5) 0.63289(2) 0.01697(11) Uani 1 1 d . . . . .
Ni1 Ni 0.37262(2) 0.23168(5) 0.39398(2) 0.01866(12) Uani 1 1 d . . . . .
O1 O 0.41973(14) 0.1201(3) 0.48167(13) 0.0202(5) Uani 1 1 d . . . . .
O2 O 0.01966(14) 0.3999(3) 0.57538(14) 0.0200(5) Uani 1 1 d . . . . .
N16 N 0.07685(17) 0.3264(3) 0.71829(16) 0.0244(7) Uani 1 1 d . . . . .
N20 N 0.34658(16) -0.0058(3) 0.84679(17) 0.0257(7) Uani 1 1 d . . . . .
N13 N 0.14148(16) 0.2887(3) 0.54661(16) 0.0251(7) Uani 1 1 d . . . . .
N22 N 0.20032(17) 0.2208(3) 0.68989(16) 0.0251(7) Uani 1 1 d . . . . .
N17 N 0.01661(17) -0.3096(3) 0.56458(17) 0.0264(7) Uani 1 1 d . . . . .
N11 N 0.28468(16) 0.2499(4) 0.42467(16) 0.0275(7) Uani 1 1 d . . . . .
N14 N -0.03958(16) 0.2915(4) 0.86428(16) 0.0266(7) Uani 1 1 d . . . . .
N19 N 0.05925(17) 0.1225(3) 0.61092(17) 0.0250(7) Uani 1 1 d . . . . .
N10 N 0.32526(18) 0.3338(4) 0.30613(18) 0.0329(8) Uani 1 1 d . . . . .
N12 N 0.16874(17) 0.2637(5) 0.43868(17) 0.0339(9) Uani 1 1 d . . . . .
N8 N 0.16653(18) 0.5537(4) 0.15272(17) 0.0310(8) Uani 1 1 d . . . . .
N5 N 0.43351(18) 0.8366(3) 0.47184(18) 0.0298(8) Uani 1 1 d . . . . .
N6 N 0.4019(2) 0.6157(3) 0.5077(2) 0.0333(8) Uani 1 1 d . . . . .
N18 N -0.01480(18) -0.0749(3) 0.57901(19) 0.0301(8) Uani 1 1 d . . . . .
N21 N 0.31711(17) 0.1790(4) 0.76432(17) 0.0275(6) Uani 1 1 d . . . . .
C52 C 0.02823(19) 0.0254(4) 0.59567(18) 0.0197(7) Uani 1 1 d . . . . .
N15B N 0.0544(5) 0.3895(8) 0.8252(5) 0.0275(6) Uani 0.5 1 d . . P A 2
N1 N 0.5202(6) 0.6141(17) 0.3066(5) 0.0269(11) Uani 0.75(6) 1 d . . P B 1
C46 C 0.15750(18) 0.2769(4) 0.49787(18) 0.0208(7) Uani 1 1 d . . . . .
N7 N 0.40972(18) 0.4042(3) 0.44883(17) 0.0271(7) Uani 1 1 d . . . . .
N9 N 0.2456(2) 0.3665(4) 0.19221(19) 0.0446(10) Uani 1 1 d . . . . .
C48 C 0.2534(2) 0.1965(4) 0.72574(19) 0.0230(8) Uani 1 1 d . . . . .
C51 C 0.00525(19) -0.1976(4) 0.57173(18) 0.0212(7) Uani 1 1 d . . . . .
C47 C 0.32984(18) 0.0789(4) 0.80693(19) 0.0212(7) Uani 1 1 d . . . . .
C42 C 0.4067(2) 0.5064(4) 0.4738(2) 0.0237(8) Uani 1 1 d . . . . .
C45 C 0.2320(2) 0.2573(4) 0.43460(18) 0.0250(8) Uani 1 1 d . . . . .
C50 C 0.06592(19) 0.3451(4) 0.76935(19) 0.0252(8) Uani 1 1 d . . . . .
C41 C 0.41972(19) 0.7308(4) 0.4864(2) 0.0241(8) Uani 1 1 d . . . . .
C44 C 0.2867(2) 0.3551(4) 0.2538(2) 0.0302(9) Uani 1 1 d . . . . .
C49 C 0.0050(2) 0.3270(4) 0.84517(19) 0.0258(8) Uani 1 1 d . . . . .
C43 C 0.2050(2) 0.4694(4) 0.1744(2) 0.0287(9) Uani 1 1 d . . . . .
N4 N 0.1875(4) 0.8012(9) 0.4999(4) 0.0269(11) Uani 0.519(9) 1 d . . P C 1
C15 C 0.4582(7) 0.8082(11) 0.2325(5) 0.0356(3) Uani 0.66(4) 1 d . . P B 1
H15A H 0.473356 0.876709 0.268750 0.043 Uiso 0.66(4) 1 calc R . P B 1
H15B H 0.453157 0.853029 0.188314 0.043 Uiso 0.66(4) 1 calc R . P B 1
C6 C 0.6384(3) 0.5245(7) 0.3151(4) 0.0356(3) Uani 0.748(9) 1 d . . P B 1
H6A H 0.642505 0.577306 0.275586 0.043 Uiso 0.748(9) 1 calc R . P B 1
H6B H 0.664740 0.440060 0.317136 0.043 Uiso 0.748(9) 1 calc R . P B 1
C12 C 0.5134(3) 0.6977(6) 0.2431(3) 0.0356(3) Uani 0.787(7) 1 d . . P B 1
H12A H 0.501724 0.637427 0.202970 0.043 Uiso 0.787(7) 1 calc R . P B 1
H12B H 0.558180 0.740128 0.246062 0.043 Uiso 0.787(7) 1 calc R . P B 1
C19 C 0.3895(4) 0.7524(12) 0.2338(4) 0.0356(3) Uani 0.642(15) 1 d . . P B 1
H19A H 0.356685 0.827347 0.230839 0.043 Uiso 0.642(15) 1 calc R . P B 1
H19B H 0.371171 0.693287 0.193882 0.043 Uiso 0.642(15) 1 calc R . P B 1
C1 C 0.5499(3) 0.6929(8) 0.3711(3) 0.0356(3) Uani 0.761(12) 1 d . . P B 1
H1C H 0.545768 0.639077 0.410327 0.043 Uiso 0.761(12) 1 calc R . P B 1
H1D H 0.523017 0.776528 0.369440 0.043 Uiso 0.761(12) 1 calc R . P B 1
C17 C 0.3959(3) 0.6748(6) 0.2969(3) 0.0356(3) Uani 0.785(8) 1 d . . P B 1
H17A H 0.350748 0.635728 0.295620 0.043 Uiso 0.785(8) 1 calc R . P B 1
H17B H 0.410017 0.735854 0.336622 0.043 Uiso 0.785(8) 1 calc R . P B 1
C10 C 0.6682(3) 0.6054(7) 0.3806(3) 0.0356(3) Uani 0.736(9) 1 d . . P B 1
H10A H 0.669532 0.548252 0.420412 0.043 Uiso 0.736(9) 1 calc R . P B 1
H10B H 0.715759 0.633009 0.383741 0.043 Uiso 0.736(9) 1 calc R . P B 1
C23 C 0.1757(5) 0.8387(10) 0.5669(5) 0.0356(3) Uani 0.519(9) 1 d . . P C 1
H23A H 0.152479 0.763184 0.582759 0.043 Uiso 0.519(9) 1 calc R . P C 1
H23B H 0.144837 0.917837 0.560136 0.043 Uiso 0.519(9) 1 calc R . P C 1
C14 C 0.4484(3) 0.5628(7) 0.3048(3) 0.0356(3) Uani 0.762(9) 1 d . . P B 1
H14A H 0.432420 0.499044 0.266442 0.043 Uiso 0.762(9) 1 calc R . P B 1
H14B H 0.451566 0.513023 0.347325 0.043 Uiso 0.762(9) 1 calc R . P B 1
C8 C 0.6251(3) 0.7289(7) 0.3815(3) 0.0356(3) Uani 0.743(9) 1 d . . P B 1
H8A H 0.628668 0.791318 0.345166 0.043 Uiso 0.743(9) 1 calc R . P B 1
H8B H 0.643071 0.775620 0.425655 0.043 Uiso 0.743(9) 1 calc R . P B 1
C3 C 0.5637(3) 0.4921(6) 0.3067(3) 0.0356(3) Uani 0.750(8) 1 d . . P B 1
H3A H 0.544874 0.443014 0.263367 0.043 Uiso 0.750(8) 1 calc R . P B 1
H3B H 0.560726 0.431752 0.344069 0.043 Uiso 0.750(8) 1 calc R . P B 1
C30 C 0.2815(6) 0.9852(10) 0.5995(5) 0.0356(3) Uani 0.542(13) 1 d . . P C 1
H30A H 0.254963 1.069950 0.594978 0.043 Uiso 0.542(13) 1 calc R . P C 1
H30B H 0.326549 0.999026 0.633665 0.043 Uiso 0.542(13) 1 calc R . P C 1
C27 C 0.2915(4) 0.9461(8) 0.5315(4) 0.0356(3) Uani 0.591(9) 1 d . . P C 1
H27A H 0.315029 1.020989 0.515473 0.043 Uiso 0.591(9) 1 calc R . P C 1
H27B H 0.322256 0.866828 0.538359 0.043 Uiso 0.591(9) 1 calc R . P C 1
C21 C 0.2273(4) 0.9139(9) 0.4773(5) 0.0356(3) Uani 0.533(8) 1 d . . P C 1
H21A H 0.238721 0.885882 0.435616 0.043 Uiso 0.533(8) 1 calc R . P C 1
H21B H 0.198130 0.995320 0.466459 0.043 Uiso 0.533(8) 1 calc R . P C 1
C22 C 0.2519(5) 0.8230(10) 0.4766(5) 0.0356(3) Uani 0.467(8) 1 d . . P C 2
H22A H 0.252807 0.832964 0.428891 0.043 Uiso 0.467(8) 1 calc R . P C 2
H22B H 0.293266 0.771966 0.501615 0.043 Uiso 0.467(8) 1 calc R . P C 2
C26 C 0.2427(5) 0.8716(9) 0.6217(5) 0.0356(3) Uani 0.513(9) 1 d . . P C 1
H26A H 0.232240 0.897709 0.664167 0.043 Uiso 0.513(9) 1 calc R . P C 1
H26B H 0.272083 0.790326 0.631338 0.043 Uiso 0.513(9) 1 calc R . P C 1
C24 C 0.1878(5) 0.7327(10) 0.5525(5) 0.0356(3) Uani 0.481(9) 1 d . . P C 2
H24A H 0.144915 0.687092 0.553721 0.043 Uiso 0.481(9) 1 calc R . P C 2
H24B H 0.226926 0.675982 0.577540 0.043 Uiso 0.481(9) 1 calc R . P C 2
N3 N 0.1887(4) 0.7465(9) 0.4782(4) 0.0269(11) Uani 0.481(9) 1 d . . P C 2
C28 C 0.2531(7) 0.9610(12) 0.5084(6) 0.0356(3) Uani 0.409(9) 1 d . . P C 2
H28A H 0.212256 1.012541 0.482543 0.043 Uiso 0.409(9) 1 calc R . P C 2
H28B H 0.294465 1.010242 0.505555 0.043 Uiso 0.409(9) 1 calc R . P C 2
C29 C 0.2534(7) 0.9519(12) 0.5836(6) 0.0356(3) Uani 0.458(13) 1 d . . P C 2
H29A H 0.296672 0.909838 0.611066 0.043 Uiso 0.458(13) 1 calc R . P C 2
H29B H 0.250192 1.043029 0.601818 0.043 Uiso 0.458(13) 1 calc R . P C 2
C25 C 0.1924(5) 0.8673(11) 0.5873(5) 0.0356(3) Uani 0.487(9) 1 d . . P C 2
H25A H 0.195134 0.852484 0.635657 0.043 Uiso 0.487(9) 1 calc R . P C 2
H25B H 0.149698 0.918341 0.566277 0.043 Uiso 0.487(9) 1 calc R . P C 2
C4 C 0.5282(9) 0.535(2) 0.2687(10) 0.0356(3) Uani 0.250(8) 1 d . . P B 2
H4A H 0.514685 0.447249 0.283683 0.043 Uiso 0.250(8) 1 calc R . P B 2
H4B H 0.500430 0.549535 0.221032 0.043 Uiso 0.250(8) 1 calc R . P B 2
C13 C 0.4401(10) 0.637(2) 0.3201(10) 0.0356(3) Uani 0.238(9) 1 d . . P B 2
H13A H 0.436465 0.698755 0.356873 0.043 Uiso 0.238(9) 1 calc R . P B 2
H13B H 0.431173 0.544678 0.333117 0.043 Uiso 0.238(9) 1 calc R . P B 2
C20 C 0.3994(7) 0.811(2) 0.2363(7) 0.0356(3) Uani 0.358(15) 1 d . . P B 2
H20A H 0.390517 0.873442 0.270131 0.043 Uiso 0.358(15) 1 calc R . P B 2
H20B H 0.367776 0.834009 0.191257 0.043 Uiso 0.358(15) 1 calc R . P B 2
C5 C 0.6032(9) 0.530(2) 0.2714(9) 0.0356(3) Uani 0.252(9) 1 d . . P B 2
H5A H 0.614662 0.610877 0.249096 0.043 Uiso 0.252(9) 1 calc R . P B 2
H5B H 0.610914 0.450268 0.245417 0.043 Uiso 0.252(9) 1 calc R . P B 2
C2 C 0.5597(10) 0.631(3) 0.3838(10) 0.0356(3) Uani 0.239(12) 1 d . . P B 2
H2C H 0.549771 0.704581 0.412211 0.043 Uiso 0.239(12) 1 calc R . P B 2
H2D H 0.549864 0.544868 0.403165 0.043 Uiso 0.239(12) 1 calc R . P B 2
C18 C 0.3854(11) 0.676(2) 0.2534(12) 0.0356(3) Uani 0.215(8) 1 d . . P B 2
H18A H 0.387465 0.613463 0.216521 0.043 Uiso 0.215(8) 1 calc R . P B 2
H18B H 0.338936 0.670948 0.259482 0.043 Uiso 0.215(8) 1 calc R . P B 2
C7 C 0.6347(10) 0.636(2) 0.3878(9) 0.0356(3) Uani 0.257(9) 1 d . . P B 2
H7A H 0.662803 0.623899 0.435583 0.043 Uiso 0.257(9) 1 calc R . P B 2
H7B H 0.646018 0.723973 0.371616 0.043 Uiso 0.257(9) 1 calc R . P B 2
C16 C 0.4747(13) 0.829(2) 0.2341(9) 0.0356(3) Uani 0.34(4) 1 d . . P B 2
H16A H 0.481148 0.775698 0.195681 0.043 Uiso 0.34(4) 1 calc R . P B 2
H16B H 0.481735 0.924811 0.224760 0.043 Uiso 0.34(4) 1 calc R . P B 2
N2 N 0.5123(16) 0.645(4) 0.3127(16) 0.0269(11) Uani 0.25(6) 1 d . . P B 2
C11 C 0.5235(11) 0.792(2) 0.2914(11) 0.0356(3) Uani 0.213(7) 1 d . . P B 2
H11A H 0.522474 0.854571 0.328716 0.043 Uiso 0.213(7) 1 calc R . P B 2
H11B H 0.569318 0.799537 0.283769 0.043 Uiso 0.213(7) 1 calc R . P B 2
C9 C 0.6510(10) 0.521(2) 0.3430(10) 0.0356(3) Uani 0.264(9) 1 d . . P B 2
H9A H 0.699199 0.529516 0.341848 0.043 Uiso 0.264(9) 1 calc R . P B 2
H9B H 0.645714 0.432770 0.363054 0.043 Uiso 0.264(9) 1 calc R . P B 2
C33 C 0.1208(6) 0.8025(13) 0.4344(11) 0.0356(3) Uani 0.52(5) 1 d . . P C 2
H33A H 0.082847 0.749122 0.442441 0.043 Uiso 0.52(5) 1 calc R . P C 2
H33B H 0.115846 0.896258 0.448479 0.043 Uiso 0.52(5) 1 calc R . P C 2
C31 C 0.2238(4) 0.6665(9) 0.5037(4) 0.0356(3) Uani 0.529(8) 1 d . . P C 1
H31A H 0.271227 0.675165 0.534037 0.043 Uiso 0.529(8) 1 calc R . P C 1
H31B H 0.199635 0.599136 0.524010 0.043 Uiso 0.529(8) 1 calc R . P C 1
C39 C 0.1556(5) 0.6092(9) 0.3842(5) 0.0356(3) Uani 0.515(8) 1 d . . P C 1
H39A H 0.160539 0.587084 0.338879 0.043 Uiso 0.515(8) 1 calc R . P C 1
H39B H 0.128795 0.536424 0.397490 0.043 Uiso 0.515(8) 1 calc R . P C 1
C37 C 0.2263(5) 0.6174(10) 0.4356(4) 0.0356(3) Uani 0.514(8) 1 d . . P C 1
H37A H 0.247708 0.527112 0.440861 0.043 Uiso 0.514(8) 1 calc R . P C 1
H37B H 0.255493 0.678732 0.417995 0.043 Uiso 0.514(8) 1 calc R . P C 1
C40 C 0.1215(5) 0.6614(10) 0.3359(5) 0.0356(3) Uani 0.485(8) 1 d . . P C 2
H40A H 0.119466 0.663710 0.287122 0.043 Uiso 0.485(8) 1 calc R . P C 2
H40B H 0.082920 0.605403 0.340667 0.043 Uiso 0.485(8) 1 calc R . P C 2
C36 C 0.1175(5) 0.7405(12) 0.3803(5) 0.0356(3) Uani 0.489(11) 1 d . . P C 1
H36A H 0.069376 0.728171 0.352139 0.043 Uiso 0.489(11) 1 calc R . P C 1
H36B H 0.138976 0.808888 0.357936 0.043 Uiso 0.489(11) 1 calc R . P C 1
C32 C 0.1942(5) 0.6042(10) 0.4527(5) 0.0356(3) Uani 0.471(8) 1 d . . P C 2
H32A H 0.157280 0.548229 0.461348 0.043 Uiso 0.471(8) 1 calc R . P C 2
H32B H 0.238764 0.564958 0.478704 0.043 Uiso 0.471(8) 1 calc R . P C 2
C38 C 0.1884(5) 0.5997(10) 0.3761(5) 0.0356(3) Uani 0.486(8) 1 d . . P C 2
H38A H 0.227144 0.649772 0.367475 0.043 Uiso 0.486(8) 1 calc R . P C 2
H38B H 0.190833 0.505262 0.361666 0.043 Uiso 0.486(8) 1 calc R . P C 2
C35 C 0.1145(5) 0.8009(11) 0.3600(5) 0.0356(3) Uani 0.511(11) 1 d . . P C 2
H35A H 0.069231 0.837915 0.334428 0.043 Uiso 0.511(11) 1 calc R . P C 2
H35B H 0.150509 0.858880 0.351079 0.043 Uiso 0.511(11) 1 calc R . P C 2
C34 C 0.1180(6) 0.7913(15) 0.4511(12) 0.0356(3) Uani 0.48(5) 1 d . . P C 1
H34A H 0.096089 0.881205 0.446276 0.043 Uiso 0.48(5) 1 calc R . P C 1
H34B H 0.089869 0.729811 0.470055 0.043 Uiso 0.48(5) 1 calc R . P C 1
H1A H 0.416(2) 0.038(5) 0.471(2) 0.033(13) Uiso 1 1 d . . . . .
H2A H 0.011(2) 0.381(5) 0.534(2) 0.031(13) Uiso 1 1 d . . . . .
H1B H 0.464(2) 0.142(5) 0.496(2) 0.031(13) Uiso 1 1 d . . . . .
N15A N 0.0642(5) 0.3521(8) 0.8337(5) 0.0275(6) Uani 0.5 1 d . . P A 1
H2B H 0.024(3) 0.473(6) 0.578(3) 0.053(19) 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
Ni2 O2 2.106(3) . ?
Ni2 N16 2.066(3) . ?
Ni2 N20 2.076(3) 2_556 ?
Ni2 N13 2.055(3) . ?
Ni2 N22 2.045(3) . ?
Ni2 N19 2.065(3) . ?
Ni1 O1 2.097(3) . ?
Ni1 N11 2.068(3) . ?
Ni1 N14 2.059(3) 4_665 ?
Ni1 N10 2.052(3) . ?
Ni1 N8 2.060(4) 2_545 ?
Ni1 N7 2.071(3) . ?
O1 H1A 0.85(5) . ?
O1 H1B 0.89(5) . ?
O2 H2A 0.85(5) . ?
O2 H2B 0.73(6) . ?
N16 C50 1.148(5) . ?
N20 C47 1.155(5) . ?
N13 C46 1.144(5) . ?
N22 C48 1.143(5) . ?
N17 C51 1.155(5) . ?
N11 C45 1.148(5) . ?
N14 C49 1.142(5) . ?
N19 C52 1.146(5) . ?
N10 C44 1.154(5) . ?
N12 C46 1.307(5) . ?
N12 C45 1.315(5) . ?
N8 C43 1.145(5) . ?
N5 C41 1.150(5) . ?
N6 C42 1.310(5) . ?
N6 C41 1.312(5) . ?
N18 C52 1.306(5) . ?
N18 C51 1.308(5) . ?
N21 C48 1.322(5) . ?
N21 C47 1.301(5) . ?
N15B C50 1.313(10) . ?
N15B C49 1.342(10) . ?
N1 C12 1.520(10) . ?
N1 C1 1.507(15) . ?
N1 C14 1.535(11) . ?
N1 C3 1.50(2) . ?
N7 C42 1.148(5) . ?
N9 C44 1.304(6) . ?
N9 C43 1.300(6) . ?
C50 N15A 1.333(10) . ?
C49 N15A 1.317(10) . ?
N4 C23 1.512(12) . ?
N4 C21 1.529(11) . ?
N4 C31 1.519(12) . ?
N4 C34 1.483(15) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C12 1.540(11) . ?
C15 C19 1.511(17) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 C10 1.533(9) . ?
C6 C3 1.515(8) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C17 1.482(10) . ?
C1 H1C 0.9900 . ?
C1 H1D 0.9900 . ?
C1 C8 1.525(8) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C14 1.519(9) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C8 1.511(9) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C26 1.532(13) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C27 1.520(11) . ?
C30 C26 1.521(13) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C21 1.487(12) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 N3 1.501(12) . ?
C22 C28 1.517(16) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C24 N3 1.536(12) . ?
C24 C25 1.507(14) . ?
N3 C33 1.521(14) . ?
N3 C32 1.523(14) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 C29 1.544(15) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C25 1.519(16) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C5 1.51(2) . ?
C4 N2 1.51(5) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C18 1.54(3) . ?
C13 N2 1.52(4) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C18 1.43(3) . ?
C20 C16 1.55(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C9 1.51(3) . ?
C2 H2C 0.9900 . ?
C2 H2D 0.9900 . ?
C2 C7 1.50(3) . ?
C2 N2 1.51(3) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C9 1.56(3) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 C11 1.35(3) . ?
N2 C11 1.56(4) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C35 1.49(2) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C37 1.497(12) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C39 C37 1.521(12) . ?
C39 C36 1.508(14) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C40 C38 1.504(13) . ?
C40 C35 1.494(14) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C36 C34 1.54(2) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C38 1.545(13) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C34 H34A 0.9900 . ?
C34 H34B 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
N16 Ni2 O2 88.92(12) . . ?
N16 Ni2 N20 87.44(13) . 2_556 ?
N20 Ni2 O2 87.28(12) 2_556 . ?
N13 Ni2 O2 89.30(12) . . ?
N13 Ni2 N16 177.85(14) . . ?
N13 Ni2 N20 91.26(14) . 2_556 ?
N13 Ni2 N19 90.40(13) . . ?
N22 Ni2 O2 176.97(13) . . ?
N22 Ni2 N16 90.93(13) . . ?
N22 Ni2 N20 89.69(13) . 2_556 ?
N22 Ni2 N13 90.78(13) . . ?
N22 Ni2 N19 94.68(13) . . ?
N19 Ni2 O2 88.35(12) . . ?
N19 Ni2 N16 90.77(13) . . ?
N19 Ni2 N20 175.31(13) . 2_556 ?
N11 Ni1 O1 90.33(12) . . ?
N11 Ni1 N7 88.47(14) . . ?
N14 Ni1 O1 88.55(12) 4_665 . ?
N14 Ni1 N11 178.52(15) 4_665 . ?
N14 Ni1 N8 91.01(14) 4_665 2_545 ?
N14 Ni1 N7 92.45(14) 4_665 . ?
N10 Ni1 O1 177.71(14) . . ?
N10 Ni1 N11 89.81(14) . . ?
N10 Ni1 N14 91.28(13) . 4_665 ?
N10 Ni1 N8 89.70(15) . 2_545 ?
N10 Ni1 N7 94.25(15) . . ?
N8 Ni1 O1 88.02(13) 2_545 . ?
N8 Ni1 N11 87.99(14) 2_545 . ?
N8 Ni1 N7 174.68(14) 2_545 . ?
N7 Ni1 O1 88.03(12) . . ?
Ni1 O1 H1A 108(3) . . ?
Ni1 O1 H1B 109(3) . . ?
H1A O1 H1B 109(4) . . ?
Ni2 O2 H2A 111(3) . . ?
Ni2 O2 H2B 109(5) . . ?
H2A O2 H2B 106(5) . . ?
C50 N16 Ni2 171.9(3) . . ?
C47 N20 Ni2 145.8(3) . 2_546 ?
C46 N13 Ni2 177.8(3) . . ?
C48 N22 Ni2 168.1(3) . . ?
C45 N11 Ni1 172.7(3) . . ?
C49 N14 Ni1 167.9(4) . 4_566 ?
C52 N19 Ni2 176.0(3) . . ?
C44 N10 Ni1 158.6(4) . . ?
C46 N12 C45 120.0(3) . . ?
C43 N8 Ni1 159.8(4) . 2 ?
C42 N6 C41 118.3(3) . . ?
C52 N18 C51 122.3(4) . . ?
C47 N21 C48 118.4(3) . . ?
N19 C52 N18 171.6(4) . . ?
C50 N15B C49 116.6(7) . . ?
C12 N1 C14 108.0(7) . . ?
C1 N1 C12 112.7(10) . . ?
C1 N1 C14 109.4(10) . . ?
C3 N1 C12 110.5(10) . . ?
C3 N1 C1 109.4(7) . . ?
C3 N1 C14 106.7(9) . . ?
N13 C46 N12 173.8(4) . . ?
C42 N7 Ni1 156.7(3) . . ?
C43 N9 C44 121.3(4) . . ?
N22 C48 N21 174.1(4) . . ?
N17 C51 N18 173.5(4) . . ?
N20 C47 N21 174.3(4) . . ?
N7 C42 N6 173.7(4) . . ?
N11 C45 N12 173.6(4) . . ?
N16 C50 N15B 169.6(6) . . ?
N16 C50 N15A 168.7(5) . . ?
N5 C41 N6 174.4(4) . . ?
N10 C44 N9 173.5(5) . . ?
N14 C49 N15B 170.3(6) . . ?
N14 C49 N15A 167.9(5) . . ?
N8 C43 N9 173.2(5) . . ?
C23 N4 C21 109.4(8) . . ?
C23 N4 C31 111.8(7) . . ?
C31 N4 C21 111.8(7) . . ?
C34 N4 C23 105.1(10) . . ?
C34 N4 C21 109.2(11) . . ?
C34 N4 C31 109.3(8) . . ?
H15A C15 H15B 107.9 . . ?
C12 C15 H15A 109.2 . . ?
C12 C15 H15B 109.2 . . ?
C19 C15 H15A 109.2 . . ?
C19 C15 H15B 109.2 . . ?
C19 C15 C12 112.1(9) . . ?
H6A C6 H6B 108.2 . . ?
C10 C6 H6A 109.7 . . ?
C10 C6 H6B 109.7 . . ?
C3 C6 H6A 109.7 . . ?
C3 C6 H6B 109.7 . . ?
C3 C6 C10 109.9(5) . . ?
N1 C12 C15 113.1(9) . . ?
N1 C12 H12A 109.0 . . ?
N1 C12 H12B 109.0 . . ?
C15 C12 H12A 109.0 . . ?
C15 C12 H12B 109.0 . . ?
H12A C12 H12B 107.8 . . ?
C15 C19 H19A 109.5 . . ?
C15 C19 H19B 109.5 . . ?
H19A C19 H19B 108.0 . . ?
C17 C19 C15 110.9(6) . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
N1 C1 H1C 109.2 . . ?
N1 C1 H1D 109.2 . . ?
N1 C1 C8 112.2(6) . . ?
H1C C1 H1D 107.9 . . ?
C8 C1 H1C 109.2 . . ?
C8 C1 H1D 109.2 . . ?
C19 C17 H17A 109.5 . . ?
C19 C17 H17B 109.5 . . ?
C19 C17 C14 110.9(6) . . ?
H17A C17 H17B 108.1 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
C6 C10 H10A 109.5 . . ?
C6 C10 H10B 109.5 . . ?
H10A C10 H10B 108.1 . . ?
C8 C10 C6 110.7(5) . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
N4 C23 H23A 109.1 . . ?
N4 C23 H23B 109.1 . . ?
N4 C23 C26 112.3(7) . . ?
H23A C23 H23B 107.9 . . ?
C26 C23 H23A 109.1 . . ?
C26 C23 H23B 109.1 . . ?
N1 C14 H14A 109.0 . . ?
N1 C14 H14B 109.0 . . ?
C17 C14 N1 113.1(8) . . ?
C17 C14 H14A 109.0 . . ?
C17 C14 H14B 109.0 . . ?
H14A C14 H14B 107.8 . . ?
C1 C8 H8A 109.3 . . ?
C1 C8 H8B 109.3 . . ?
C10 C8 C1 111.7(6) . . ?
C10 C8 H8A 109.3 . . ?
C10 C8 H8B 109.3 . . ?
H8A C8 H8B 107.9 . . ?
N1 C3 C6 113.6(6) . . ?
N1 C3 H3A 108.8 . . ?
N1 C3 H3B 108.8 . . ?
C6 C3 H3A 108.8 . . ?
C6 C3 H3B 108.8 . . ?
H3A C3 H3B 107.7 . . ?
H30A C30 H30B 108.5 . . ?
C27 C30 H30A 110.2 . . ?
C27 C30 H30B 110.2 . . ?
C27 C30 C26 107.7(8) . . ?
C26 C30 H30A 110.2 . . ?
C26 C30 H30B 110.2 . . ?
C30 C27 H27A 108.5 . . ?
C30 C27 H27B 108.5 . . ?
H27A C27 H27B 107.5 . . ?
C21 C27 C30 114.9(8) . . ?
C21 C27 H27A 108.5 . . ?
C21 C27 H27B 108.5 . . ?
N4 C21 H21A 109.4 . . ?
N4 C21 H21B 109.4 . . ?
C27 C21 N4 111.0(7) . . ?
C27 C21 H21A 109.4 . . ?
C27 C21 H21B 109.4 . . ?
H21A C21 H21B 108.0 . . ?
H22A C22 H22B 108.1 . . ?
N3 C22 H22A 109.5 . . ?
N3 C22 H22B 109.5 . . ?
N3 C22 C28 110.8(9) . . ?
C28 C22 H22A 109.5 . . ?
C28 C22 H22B 109.5 . . ?
C23 C26 H26A 109.3 . . ?
C23 C26 H26B 109.3 . . ?
C30 C26 C23 111.5(8) . . ?
C30 C26 H26A 109.3 . . ?
C30 C26 H26B 109.3 . . ?
H26A C26 H26B 108.0 . . ?
H24A C24 H24B 107.9 . . ?
N3 C24 H24A 109.2 . . ?
N3 C24 H24B 109.2 . . ?
C25 C24 H24A 109.2 . . ?
C25 C24 H24B 109.2 . . ?
C25 C24 N3 112.0(8) . . ?
C22 N3 C24 108.8(8) . . ?
C22 N3 C33 115.9(10) . . ?
C22 N3 C32 108.4(8) . . ?
C33 N3 C24 110.6(11) . . ?
C33 N3 C32 106.2(8) . . ?
C32 N3 C24 106.4(7) . . ?
C22 C28 H28A 109.2 . . ?
C22 C28 H28B 109.2 . . ?
C22 C28 C29 111.9(9) . . ?
H28A C28 H28B 107.9 . . ?
C29 C28 H28A 109.2 . . ?
C29 C28 H28B 109.2 . . ?
C28 C29 H29A 110.0 . . ?
C28 C29 H29B 110.0 . . ?
H29A C29 H29B 108.4 . . ?
C25 C29 C28 108.3(11) . . ?
C25 C29 H29A 110.0 . . ?
C25 C29 H29B 110.0 . . ?
C24 C25 C29 114.0(9) . . ?
C24 C25 H25A 108.8 . . ?
C24 C25 H25B 108.8 . . ?
C29 C25 H25A 108.8 . . ?
C29 C25 H25B 108.8 . . ?
H25A C25 H25B 107.6 . . ?
H4A C4 H4B 107.8 . . ?
C5 C4 H4A 109.0 . . ?
C5 C4 H4B 109.0 . . ?
C5 C4 N2 113.0(18) . . ?
N2 C4 H4A 109.0 . . ?
N2 C4 H4B 109.0 . . ?
H13A C13 H13B 108.0 . . ?
C18 C13 H13A 109.3 . . ?
C18 C13 H13B 109.3 . . ?
N2 C13 H13A 109.3 . . ?
N2 C13 H13B 109.3 . . ?
N2 C13 C18 111.5(18) . . ?
H20A C20 H20B 107.8 . . ?
C18 C20 H20A 109.1 . . ?
C18 C20 H20B 109.1 . . ?
C18 C20 C16 112.6(15) . . ?
C16 C20 H20A 109.1 . . ?
C16 C20 H20B 109.1 . . ?
C4 C5 H5A 108.9 . . ?
C4 C5 H5B 108.9 . . ?
C4 C5 C9 113.5(15) . . ?
H5A C5 H5B 107.7 . . ?
C9 C5 H5A 108.9 . . ?
C9 C5 H5B 108.9 . . ?
H2C C2 H2D 107.7 . . ?
C7 C2 H2C 108.8 . . ?
C7 C2 H2D 108.8 . . ?
C7 C2 N2 114(2) . . ?
N2 C2 H2C 108.8 . . ?
N2 C2 H2D 108.8 . . ?
C13 C18 H18A 110.1 . . ?
C13 C18 H18B 110.1 . . ?
C20 C18 C13 107.9(17) . . ?
C20 C18 H18A 110.1 . . ?
C20 C18 H18B 110.1 . . ?
H18A C18 H18B 108.4 . . ?
C2 C7 H7A 109.8 . . ?
C2 C7 H7B 109.8 . . ?
C2 C7 C9 109.4(16) . . ?
H7A C7 H7B 108.2 . . ?
C9 C7 H7A 109.8 . . ?
C9 C7 H7B 109.8 . . ?
C20 C16 H16A 108.5 . . ?
C20 C16 H16B 108.5 . . ?
H16A C16 H16B 107.5 . . ?
C11 C16 C20 115.2(18) . . ?
C11 C16 H16A 108.5 . . ?
C11 C16 H16B 108.5 . . ?
C4 N2 C13 114(2) . . ?
C4 N2 C11 116(2) . . ?
C13 N2 C11 107(3) . . ?
C2 N2 C4 109(3) . . ?
C2 N2 C13 105(2) . . ?
C2 N2 C11 105(2) . . ?
C16 C11 N2 111(2) . . ?
C16 C11 H11A 109.3 . . ?
C16 C11 H11B 109.3 . . ?
N2 C11 H11A 109.3 . . ?
N2 C11 H11B 109.3 . . ?
H11A C11 H11B 108.0 . . ?
C5 C9 C7 110.3(16) . . ?
C5 C9 H9A 109.6 . . ?
C5 C9 H9B 109.6 . . ?
C7 C9 H9A 109.6 . . ?
C7 C9 H9B 109.6 . . ?
H9A C9 H9B 108.1 . . ?
N3 C33 H33A 108.9 . . ?
N3 C33 H33B 108.9 . . ?
H33A C33 H33B 107.7 . . ?
C35 C33 N3 113.5(12) . . ?
C35 C33 H33A 108.9 . . ?
C35 C33 H33B 108.9 . . ?
N4 C31 H31A 109.1 . . ?
N4 C31 H31B 109.1 . . ?
H31A C31 H31B 107.8 . . ?
C37 C31 N4 112.6(7) . . ?
C37 C31 H31A 109.1 . . ?
C37 C31 H31B 109.1 . . ?
H39A C39 H39B 108.0 . . ?
C37 C39 H39A 109.4 . . ?
C37 C39 H39B 109.4 . . ?
C36 C39 H39A 109.4 . . ?
C36 C39 H39B 109.4 . . ?
C36 C39 C37 111.1(8) . . ?
C31 C37 C39 112.7(8) . . ?
C31 C37 H37A 109.0 . . ?
C31 C37 H37B 109.0 . . ?
C39 C37 H37A 109.0 . . ?
C39 C37 H37B 109.0 . . ?
H37A C37 H37B 107.8 . . ?
H40A C40 H40B 108.1 . . ?
C38 C40 H40A 109.5 . . ?
C38 C40 H40B 109.5 . . ?
C35 C40 H40A 109.5 . . ?
C35 C40 H40B 109.5 . . ?
C35 C40 C38 110.7(8) . . ?
C39 C36 H36A 109.3 . . ?
C39 C36 H36B 109.3 . . ?
C39 C36 C34 111.8(10) . . ?
H36A C36 H36B 107.9 . . ?
C34 C36 H36A 109.3 . . ?
C34 C36 H36B 109.3 . . ?
N3 C32 H32A 109.1 . . ?
N3 C32 H32B 109.1 . . ?
N3 C32 C38 112.7(8) . . ?
H32A C32 H32B 107.8 . . ?
C38 C32 H32A 109.1 . . ?
C38 C32 H32B 109.1 . . ?
C40 C38 C32 109.9(8) . . ?
C40 C38 H38A 109.7 . . ?
C40 C38 H38B 109.7 . . ?
C32 C38 H38A 109.7 . . ?
C32 C38 H38B 109.7 . . ?
H38A C38 H38B 108.2 . . ?
C33 C35 H35A 109.4 . . ?
C33 C35 H35B 109.4 . . ?
C40 C35 C33 111.2(9) . . ?
C40 C35 H35A 109.4 . . ?
C40 C35 H35B 109.4 . . ?
H35A C35 H35B 108.0 . . ?
N4 C34 C36 114.0(12) . . ?
N4 C34 H34A 108.8 . . ?
N4 C34 H34B 108.8 . . ?
C36 C34 H34A 108.8 . . ?
C36 C34 H34B 108.8 . . ?
H34A C34 H34B 107.7 . . ?
C49 N15A C50 117.0(7) . . ?

_olex2_exptl_crystal_mounting_method 
'crystal mounted on microloop sample holder'
_olex2_submission_original_sample_id C32H44N20Ni2O2
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.9406(8)
2 0.0594(8)

