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

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

data_cvm003_a
_database_code_depnum_ccdc_archive 'CCDC 2247468'
loop_
_audit_author_name
_audit_author_address
'Bruno Donnadieu'
;Mississippi State University
United States of America
;
_audit_update_record             
;
2023-03-08 deposited with the CCDC.	2023-05-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20.98 H18.31 Ge0.33 Ni0.33 P'
_chemical_formula_sum            'C20.98 H18.31 Ge0.33 Ni0.33 P'
_chemical_formula_weight         345.17

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge -1.0885 0.8855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           218
_space_group_name_H-M_alt        'P -4 3 n'
_space_group_name_Hall           'P -4n 2 3'

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

_cell_length_a                   21.7872(3)
_cell_length_b                   21.7872(3)
_cell_length_c                   21.7872(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10342.0(4)
_cell_formula_units_Z            24
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    2807
_cell_measurement_theta_min      4.058
_cell_measurement_theta_max      74.539

_exptl_crystal_description       'prism frag'
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_F_000             4301
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.157
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.083
_exptl_absorpt_coefficient_mu    2.343
_shelx_estimated_absorpt_T_min   0.710
_shelx_estimated_absorpt_T_max   0.829
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.710
_exptl_absorpt_correction_T_max  0.829
_exptl_absorpt_process_details   Sadabs
_diffrn_ambient_temperature      273(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker AXS D8 Venture  '
_diffrn_measurement_method       'profile data from θ/2θ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            189105
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_av_R_equivalents  0.1807
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         4.058
_diffrn_reflns_theta_max         74.539
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3549
_reflns_number_gt                3165
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.845
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
 Few crystals were tested without a significant improvement. 
 All attempts to grow better crystals failed. 
 Disordered solvent: Benzene was the 
 only solvent of crystallization found in the unit cell.
 The relatively high value for Requiv can be explained by 
 data quality and fact it was not possible to measure sample
 below 270K.
;

_computing_data_collection       'APEX4 v2021.4-0'
_computing_cell_refinement       'APEX4 v2021.4-0'
_computing_data_reduction        'Saint, APEX4 v2021.4-0.'
_computing_structure_solution    SHELXT
_computing_structure_refinement  SHELXTL-2018/3
_computing_molecular_graphics    'Mercury V.4.2.0,POV-Ray v 3.7'
_computing_publication_material  'APEX4 v2021.4-0'
_refine_special_details          'Refined as a 2-component inversion twin.,Twin'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0664P)²+5.8694P] 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 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.08(6)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         3549
_refine_ls_number_parameters     243
_refine_ls_number_restraints     63
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0520
_refine_ls_wR_factor_ref         0.1337
_refine_ls_wR_factor_gt          0.1269
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_restrained_S_all      1.139
_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
Ge1 Ge 0.25678(3) 0.74322(3) 0.74322(3) 0.0568(4) Uani 1 3 d S T P . .
Ni1 Ni 0.31767(4) 0.68233(4) 0.68233(4) 0.0392(4) Uani 1 3 d S T P . .
P1 P 0.23743(6) 0.62822(7) 0.65543(6) 0.0397(3) Uani 1 1 d . . . . .
C1 C 0.1680(3) 0.7238(4) 0.7363(4) 0.076(2) Uani 1 1 d . . . . .
H1A H 0.144750 0.749668 0.764205 0.091 Uiso 1 1 calc R U . . .
H1B H 0.153967 0.732039 0.694873 0.091 Uiso 1 1 calc R U . . .
C2 C 0.1575(3) 0.6584(4) 0.7516(4) 0.072(2) Uani 1 1 d . . . . .
C3 C 0.1220(4) 0.6428(6) 0.8034(5) 0.106(3) Uani 1 1 d . . . . .
H3 H 0.104238 0.674042 0.826410 0.127 Uiso 1 1 calc R U . . .
C4 C 0.1132(6) 0.5847(8) 0.8207(6) 0.144(5) Uani 1 1 d . . . . .
H4 H 0.090770 0.576723 0.856145 0.173 Uiso 1 1 calc R U . . .
C5 C 0.1366(5) 0.5360(6) 0.7870(5) 0.117(4) Uani 1 1 d . . . . .
H5 H 0.128091 0.495533 0.797748 0.140 Uiso 1 1 calc R U . . .
C6 C 0.1729(4) 0.5497(4) 0.7367(4) 0.075(2) Uani 1 1 d . . . . .
H6 H 0.190592 0.517809 0.714449 0.090 Uiso 1 1 calc R U . . .
C7 C 0.1838(3) 0.6108(3) 0.7184(3) 0.0547(15) Uani 1 1 d . . . . .
C8 C 0.1847(3) 0.6581(3) 0.5961(3) 0.0475(13) Uani 1 1 d D . . . .
C9 C 0.1211(3) 0.6519(4) 0.6001(4) 0.080(2) Uani 1 1 d D . . . .
H9 H 0.103391 0.635305 0.635184 0.097 Uiso 1 1 calc R U . . .
C10 C 0.0850(4) 0.6703(5) 0.5524(5) 0.101(3) Uani 1 1 d D . . . .
H10 H 0.042572 0.667489 0.556297 0.122 Uiso 1 1 calc R U . . .
C11 C 0.1095(5) 0.6931(4) 0.4980(5) 0.093(3) Uani 1 1 d D . . . .
H11 H 0.084509 0.703348 0.464928 0.111 Uiso 1 1 calc R U . . .
C12 C 0.1719(5) 0.7000(4) 0.4951(4) 0.089(3) Uani 1 1 d D . . . .
H12 H 0.189554 0.716967 0.460163 0.107 Uiso 1 1 calc R U . . .
C13 C 0.2090(3) 0.6819(3) 0.5434(3) 0.0608(17) Uani 1 1 d D . . . .
H13 H 0.251289 0.686063 0.539856 0.073 Uiso 1 1 calc R U . . .
C14 C 0.2512(2) 0.5516(2) 0.6210(2) 0.0419(12) Uani 1 1 d . . . . .
C15 C 0.2051(3) 0.5180(3) 0.5932(3) 0.0585(16) Uani 1 1 d . . . . .
H15 H 0.165668 0.534340 0.591311 0.070 Uiso 1 1 calc R U . . .
C16 C 0.2158(4) 0.4614(3) 0.5685(3) 0.0672(19) Uani 1 1 d . . . . .
H16 H 0.183846 0.439972 0.550045 0.081 Uiso 1 1 calc R U . . .
C17 C 0.2726(4) 0.4363(3) 0.5705(4) 0.079(2) Uani 1 1 d . . . . .
H17 H 0.280128 0.397942 0.553471 0.095 Uiso 1 1 calc R U . . .
C18 C 0.3180(4) 0.4681(4) 0.5978(5) 0.094(3) Uani 1 1 d . . . . .
H18 H 0.356857 0.450711 0.600242 0.113 Uiso 1 1 calc R U . . .
C19 C 0.3086(3) 0.5256(3) 0.6221(3) 0.0653(19) Uani 1 1 d . . . . .
H19 H 0.341322 0.546958 0.639427 0.078 Uiso 1 1 calc R U . . .
C1S C 0.5267(15) 0.4553(17) 0.0371(15) 0.145(7) Uani 0.33 1 d D U P A -1
H1S H 0.542595 0.422311 0.059053 0.174 Uiso 0.33 1 calc R U P A -1
C2S C 0.5262(11) 0.5140(19) 0.0623(14) 0.145(7) Uani 0.33 1 d D U P A -1
H2S H 0.541861 0.520926 0.101409 0.174 Uiso 0.33 1 calc R U P A -1
C3S C 0.5026(17) 0.5613(17) 0.0288(19) 0.144(7) Uani 0.33 1 d D U P A -1
H3S H 0.502384 0.600458 0.045854 0.173 Uiso 0.33 1 calc R U P A -1
C4S C 0.4787(18) 0.5534(17) -0.0299(19) 0.144(7) Uani 0.33 1 d D U P A -1
H4S H 0.462757 0.586330 -0.051908 0.173 Uiso 0.33 1 calc R U P A -1
C5S C 0.4794(16) 0.4955(18) -0.0540(14) 0.144(7) Uani 0.33 1 d D U P A -1
H5S H 0.463786 0.488580 -0.093145 0.172 Uiso 0.33 1 calc R U P A -1
C6S C 0.5033(18) 0.4472(17) -0.0205(16) 0.144(7) Uani 0.33 1 d D U P A -1
H6S H 0.503492 0.408078 -0.037665 0.173 Uiso 0.33 1 calc R U P A -1


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 C1 1.986(7) . ?
Ge1 C1 1.986(7) 10_656 ?
Ge1 C1 1.986(7) 7_665 ?
Ge1 Ni1 2.2977(17) . ?
Ni1 P1 2.1884(15) 10_656 ?
Ni1 P1 2.1884(15) 7_665 ?
Ni1 P1 2.1885(15) . ?
P1 C7 1.842(6) . ?
P1 C8 1.847(6) . ?
P1 C14 1.854(5) . ?
C1 C2 1.482(11) . ?
C2 C7 1.388(10) . ?
C2 C3 1.410(11) . ?
C3 C4 1.333(16) . ?
C4 C5 1.389(18) . ?
C5 C6 1.384(11) . ?
C6 C7 1.410(10) . ?
C8 C13 1.367(9) . ?
C8 C9 1.395(9) . ?
C9 C10 1.365(12) . ?
C10 C11 1.392(14) . ?
C11 C12 1.368(14) . ?
C12 C13 1.384(10) . ?
C14 C19 1.375(8) . ?
C14 C15 1.383(9) . ?
C15 C16 1.365(10) . ?
C16 C17 1.354(12) . ?
C17 C18 1.345(12) . ?
C18 C19 1.375(9) . ?
C1S C6S 1.367(11) . ?
C1S C2S 1.392(11) . ?
C2S C3S 1.364(13) . ?
C3S C4S 1.391(15) . ?
C4S C5S 1.367(15) . ?
C5S C6S 1.383(12) . ?

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
C1 Ge1 C1 105.3(3) . 10_656 ?
C1 Ge1 C1 105.3(3) . 7_665 ?
C1 Ge1 C1 105.3(3) 10_656 7_665 ?
C1 Ge1 Ni1 113.3(2) . . ?
C1 Ge1 Ni1 113.3(2) 10_656 . ?
C1 Ge1 Ni1 113.3(2) 7_665 . ?
P1 Ni1 P1 119.998(1) 10_656 7_665 ?
P1 Ni1 P1 119.998(1) 10_656 . ?
P1 Ni1 P1 119.998(1) 7_665 . ?
P1 Ni1 Ge1 90.25(5) 10_656 . ?
P1 Ni1 Ge1 90.25(5) 7_665 . ?
P1 Ni1 Ge1 90.25(5) . . ?
C7 P1 C8 101.5(3) . . ?
C7 P1 C14 102.6(3) . . ?
C8 P1 C14 97.7(3) . . ?
C7 P1 Ni1 114.7(2) . . ?
C8 P1 Ni1 119.6(2) . . ?
C14 P1 Ni1 117.65(18) . . ?
C2 C1 Ge1 109.7(5) . . ?
C7 C2 C3 117.5(8) . . ?
C7 C2 C1 122.6(6) . . ?
C3 C2 C1 119.8(8) . . ?
C4 C3 C2 122.3(9) . . ?
C3 C4 C5 121.5(9) . . ?
C6 C5 C4 117.6(10) . . ?
C5 C6 C7 121.6(9) . . ?
C2 C7 C6 119.3(6) . . ?
C2 C7 P1 119.7(6) . . ?
C6 C7 P1 120.8(5) . . ?
C13 C8 C9 118.1(6) . . ?
C13 C8 P1 118.8(5) . . ?
C9 C8 P1 122.7(5) . . ?
C10 C9 C8 119.9(8) . . ?
C9 C10 C11 122.1(9) . . ?
C12 C11 C10 117.4(8) . . ?
C11 C12 C13 120.9(8) . . ?
C8 C13 C12 121.5(7) . . ?
C19 C14 C15 116.8(6) . . ?
C19 C14 P1 120.7(5) . . ?
C15 C14 P1 122.5(5) . . ?
C16 C15 C14 121.8(7) . . ?
C17 C16 C15 120.6(7) . . ?
C18 C17 C16 118.6(7) . . ?
C17 C18 C19 122.1(8) . . ?
C14 C19 C18 120.2(7) . . ?
C6S C1S C2S 118.6(11) . . ?
C3S C2S C1S 119.1(12) . . ?
C2S C3S C4S 122.6(13) . . ?
C5S C4S C3S 117.6(12) . . ?
C4S C5S C6S 120.3(12) . . ?
C1S C6S C5S 121.8(12) . . ?

_refine_diff_density_max         0.650
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.057

####################################################################### 
# 
# 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_cvm004_final
_database_code_depnum_ccdc_archive 'CCDC 2247469'
loop_
_audit_author_name
_audit_author_address
'Bruno Donnadieu'
;Mississippi State University
United States of America
;
_audit_update_record             
;
2023-03-08 deposited with the CCDC.	2023-05-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20.50 H17.50 Ni0.33 P Si0.33'
_chemical_formula_sum            'C20.50 H17.50 Ni0.33 P Si0.33'
_chemical_formula_weight         323.75

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           218
_space_group_name_H-M_alt        'P -4 3 n'
_space_group_name_Hall           'P -4n 2 3'

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

_cell_length_a                   21.7616(2)
_cell_length_b                   21.7616(2)
_cell_length_c                   21.7616(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10305.6(3)
_cell_formula_units_Z            24
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1181
_cell_measurement_theta_min      4.063
_cell_measurement_theta_max      74.785

_exptl_crystal_description       'prism frag'
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_F_000             4068
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.079
_exptl_absorpt_coefficient_mu    1.936
_shelx_estimated_absorpt_T_min   0.747
_shelx_estimated_absorpt_T_max   0.862
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.747
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_process_details   Sadabs
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker AXS D8 Venture  '
_diffrn_measurement_method       'profile data from θ/2θ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            239227
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_av_R_equivalents  0.2016
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         4.063
_diffrn_reflns_theta_max         74.785
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3542
_reflns_number_gt                3087
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.846
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    1.000

_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
 Severalcrystals were tested without a significant improvement. 
 All attempts to grow better crystals failed. 
 Disordered solvent: Benzene was the 
 only solvent of crystallization found in the unit cell.
;

_computing_data_collection       'APEX4 v2021.4-0'
_computing_cell_refinement       'APEX4 v2021.4-0'
_computing_data_reduction        'Saint, APEX4 v2021.4-0.'
_computing_structure_solution    SHELXT
_computing_structure_refinement  SHELXTL-2018/3
_computing_molecular_graphics    'Mercury V.4.2.0,POV-Ray v 3.7'
_computing_publication_material  'APEX4 v2021.4-0'
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0887P)²+1.1679P] 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     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.00020(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.08(6)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3542
_refine_ls_number_parameters     208
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0519
_refine_ls_wR_factor_ref         0.1432
_refine_ls_wR_factor_gt          0.1353
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_restrained_S_all      1.110
_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 0.68285(3) 0.31715(3) 0.31715(3) 0.0423(3) Uani 1 3 d S T P . .
P1 P 0.65516(6) 0.37129(6) 0.23756(6) 0.0430(3) Uani 1 1 d . . . . .
Si1 Si 0.74244(6) 0.25756(6) 0.25756(6) 0.0573(6) Uani 1 3 d S T P . .
C1 C 0.7357(3) 0.2744(3) 0.1722(3) 0.0739(19) Uani 1 1 d . . . . .
H1A H 0.763651 0.247015 0.149062 0.089 Uiso 1 1 calc R U . . .
H1B H 0.693123 0.266014 0.158418 0.089 Uiso 1 1 calc R U . . .
C2 C 0.7515(3) 0.3396(3) 0.1590(3) 0.0716(16) Uani 1 1 d D . . . .
C3 C 0.8022(4) 0.3542(5) 0.1220(4) 0.108(3) Uani 1 1 d D . . . .
H3 H 0.825343 0.321648 0.104329 0.129 Uiso 1 1 calc R U . . .
C4 C 0.8195(5) 0.4128(6) 0.1104(5) 0.142(4) Uani 1 1 d D . . . .
H4 H 0.854899 0.420400 0.086031 0.170 Uiso 1 1 calc R U . . .
C5 C 0.7866(5) 0.4614(5) 0.1334(4) 0.114(3) Uani 1 1 d D . . . .
H5 H 0.798186 0.502402 0.124113 0.137 Uiso 1 1 calc R U . . .
C6 C 0.7353(3) 0.4494(3) 0.1708(3) 0.0760(18) Uani 1 1 d D . . . .
H6 H 0.712347 0.482616 0.187472 0.091 Uiso 1 1 calc R U . . .
C7 C 0.7182(2) 0.3890(3) 0.1837(3) 0.0551(12) Uani 1 1 d D . . . .
C8 C 0.5953(2) 0.3412(2) 0.1854(2) 0.0517(11) Uani 1 1 d . . . . .
C9 C 0.5985(4) 0.3475(4) 0.1214(3) 0.086(2) Uani 1 1 d . . . . .
H9 H 0.634232 0.364708 0.103139 0.103 Uiso 1 1 calc R U . . .
C10 C 0.5504(5) 0.3289(5) 0.0849(4) 0.110(3) Uani 1 1 d . . . . .
H10 H 0.553631 0.331993 0.041428 0.132 Uiso 1 1 calc R U . . .
C11 C 0.4975(4) 0.3058(4) 0.1109(4) 0.098(3) Uani 1 1 d . . . . .
H11 H 0.463692 0.294546 0.085712 0.118 Uiso 1 1 calc R U . . .
C12 C 0.4939(3) 0.2992(3) 0.1729(4) 0.088(2) Uani 1 1 d . . . . .
H12 H 0.457978 0.282156 0.190948 0.105 Uiso 1 1 calc R U . . .
C13 C 0.5428(3) 0.3172(3) 0.2102(3) 0.0659(15) Uani 1 1 d . . . . .
H13 H 0.539501 0.312708 0.253483 0.079 Uiso 1 1 calc R U . . .
C14 C 0.6208(2) 0.4486(2) 0.2513(2) 0.0462(11) Uani 1 1 d . . . . .
C15 C 0.5934(3) 0.4814(3) 0.2052(3) 0.0615(14) Uani 1 1 d . . . . .
H15 H 0.591917 0.464419 0.165018 0.074 Uiso 1 1 calc R U . . .
C16 C 0.5679(3) 0.5382(3) 0.2156(3) 0.0690(16) Uani 1 1 d . . . . .
H16 H 0.548934 0.559940 0.182911 0.083 Uiso 1 1 calc R U . . .
C17 C 0.5700(3) 0.5630(3) 0.2724(4) 0.081(2) Uani 1 1 d . . . . .
H17 H 0.552596 0.602334 0.280149 0.097 Uiso 1 1 calc R U . . .
C18 C 0.5969(4) 0.5314(3) 0.3176(4) 0.097(3) Uani 1 1 d . . . . .
H18 H 0.599096 0.549313 0.357311 0.117 Uiso 1 1 calc R U . . .
C19 C 0.6216(3) 0.4740(3) 0.3089(3) 0.0678(16) Uani 1 1 d . . . . .
H19 H 0.638977 0.452198 0.342444 0.081 Uiso 1 1 calc R U . . .
C1S C 0.5146(14) 0.4668(10) 1.0579(12) 0.107(5) Uiso 0.25 1 d D U P A -1
H1S H 0.522359 0.450689 1.097740 0.129 Uiso 0.25 1 calc R U P A -1
C2S C 0.5627(13) 0.4842(11) 1.0186(14) 0.107(5) Uiso 0.25 1 d D U P A -1
H2S H 0.603812 0.479791 1.032475 0.129 Uiso 0.25 1 calc R U P A -1
C3S C 0.5525(15) 0.5072(12) 0.9617(13) 0.107(5) Uiso 0.25 1 d D U P A -1
H3S H 0.586565 0.518384 0.936720 0.129 Uiso 0.25 1 calc R U P A -1
C4S C 0.4941(16) 0.5145(12) 0.9394(11) 0.107(5) Uiso 0.25 1 d D U P A -1
H4S H 0.487414 0.530694 0.899438 0.129 Uiso 0.25 1 calc R U P A -1
C5S C 0.4443(14) 0.4977(14) 0.9768(13) 0.107(5) Uiso 0.25 1 d D U P A -1
H5S H 0.403406 0.502451 0.962178 0.129 Uiso 0.25 1 calc R U P A -1
C6S C 0.4547(13) 0.4741(12) 1.0356(13) 0.107(5) Uiso 0.25 1 d D U P A -1
H6S H 0.420797 0.462906 1.060731 0.129 Uiso 0.25 1 calc R U P A -1


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 P1 2.1796(13) . ?
Ni1 P1 2.1797(13) 7_665 ?
Ni1 P1 2.1797(13) 10_656 ?
Ni1 Si1 2.246(2) . ?
P1 C7 1.845(5) . ?
P1 C8 1.847(5) . ?
P1 C14 1.864(5) . ?
Si1 C1 1.899(7) 7_665 ?
Si1 C1 1.899(7) 10_656 ?
Si1 C1 1.899(7) . ?
C1 C2 1.487(10) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C7 1.403(8) . ?
C2 C3 1.404(9) . ?
C3 C4 1.353(14) . ?
C3 H3 0.9500 . ?
C4 C5 1.371(15) . ?
C4 H4 0.9500 . ?
C5 C6 1.405(10) . ?
C5 H5 0.9500 . ?
C6 C7 1.396(9) . ?
C6 H6 0.9500 . ?
C8 C13 1.368(8) . ?
C8 C9 1.401(8) . ?
C9 C10 1.377(10) . ?
C9 H9 0.9500 . ?
C10 C11 1.378(13) . ?
C10 H10 0.9500 . ?
C11 C12 1.359(12) . ?
C11 H11 0.9500 . ?
C12 C13 1.393(9) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C15 1.368(8) . ?
C14 C19 1.371(7) . ?
C15 C16 1.374(9) . ?
C15 H15 0.9500 . ?
C16 C17 1.350(10) . ?
C16 H16 0.9500 . ?
C17 C18 1.335(10) . ?
C17 H17 0.9500 . ?
C18 C19 1.371(8) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C1S C6S 1.400(11) . ?
C1S C2S 1.403(11) . ?
C1S H1S 0.9500 . ?
C2S C3S 1.354(15) . ?
C2S H2S 0.9500 . ?
C3S C4S 1.370(17) . ?
C3S H3S 0.9500 . ?
C4S C5S 1.405(12) . ?
C4S H4S 0.9500 . ?
C5S C6S 1.397(11) . ?
C5S H5S 0.9500 . ?
C6S H6S 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
P1 Ni1 P1 119.985(2) . 7_665 ?
P1 Ni1 P1 119.982(2) . 10_656 ?
P1 Ni1 P1 119.983(2) 7_665 10_656 ?
P1 Ni1 Si1 90.74(4) . . ?
P1 Ni1 Si1 90.74(4) 7_665 . ?
P1 Ni1 Si1 90.74(4) 10_656 . ?
C7 P1 C8 102.0(2) . . ?
C7 P1 C14 102.2(2) . . ?
C8 P1 C14 97.8(2) . . ?
C7 P1 Ni1 114.4(2) . . ?
C8 P1 Ni1 119.42(18) . . ?
C14 P1 Ni1 118.11(16) . . ?
C1 Si1 C1 104.5(2) 7_665 10_656 ?
C1 Si1 C1 104.5(2) 7_665 . ?
C1 Si1 C1 104.5(2) 10_656 . ?
C1 Si1 Ni1 114.1(2) 7_665 . ?
C1 Si1 Ni1 114.1(2) 10_656 . ?
C1 Si1 Ni1 114.1(2) . . ?
C2 C1 Si1 110.8(5) . . ?
C2 C1 H1A 109.5 . . ?
Si1 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
Si1 C1 H1B 109.5 . . ?
H1A C1 H1B 108.1 . . ?
C7 C2 C3 116.9(7) . . ?
C7 C2 C1 122.5(5) . . ?
C3 C2 C1 120.6(7) . . ?
C4 C3 C2 122.6(8) . . ?
C4 C3 H3 118.7 . . ?
C2 C3 H3 118.7 . . ?
C3 C4 C5 120.9(8) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 H4 119.6 . . ?
C4 C5 C6 118.9(9) . . ?
C4 C5 H5 120.5 . . ?
C6 C5 H5 120.5 . . ?
C7 C6 C5 120.1(7) . . ?
C7 C6 H6 119.9 . . ?
C5 C6 H6 119.9 . . ?
C6 C7 C2 120.5(5) . . ?
C6 C7 P1 121.5(5) . . ?
C2 C7 P1 117.8(5) . . ?
C13 C8 C9 118.0(6) . . ?
C13 C8 P1 118.9(4) . . ?
C9 C8 P1 122.7(5) . . ?
C10 C9 C8 120.5(8) . . ?
C10 C9 H9 119.7 . . ?
C8 C9 H9 119.7 . . ?
C9 C10 C11 120.3(8) . . ?
C9 C10 H10 119.9 . . ?
C11 C10 H10 119.9 . . ?
C12 C11 C10 119.7(7) . . ?
C12 C11 H11 120.2 . . ?
C10 C11 H11 120.2 . . ?
C11 C12 C13 120.3(8) . . ?
C11 C12 H12 119.9 . . ?
C13 C12 H12 119.9 . . ?
C8 C13 C12 121.1(7) . . ?
C8 C13 H13 119.4 . . ?
C12 C13 H13 119.4 . . ?
C15 C14 C19 117.7(5) . . ?
C15 C14 P1 121.9(4) . . ?
C19 C14 P1 120.4(4) . . ?
C14 C15 C16 121.7(6) . . ?
C14 C15 H15 119.2 . . ?
C16 C15 H15 119.2 . . ?
C17 C16 C15 119.9(6) . . ?
C17 C16 H16 120.1 . . ?
C15 C16 H16 120.1 . . ?
C18 C17 C16 118.8(6) . . ?
C18 C17 H17 120.6 . . ?
C16 C17 H17 120.6 . . ?
C17 C18 C19 122.7(7) . . ?
C17 C18 H18 118.7 . . ?
C19 C18 H18 118.7 . . ?
C14 C19 C18 119.3(6) . . ?
C14 C19 H19 120.4 . . ?
C18 C19 H19 120.4 . . ?
C6S C1S C2S 116.9(11) . . ?
C6S C1S H1S 121.6 . . ?
C2S C1S H1S 121.6 . . ?
C3S C2S C1S 122.4(12) . . ?
C3S C2S H2S 118.8 . . ?
C1S C2S H2S 118.8 . . ?
C2S C3S C4S 121.1(12) . . ?
C2S C3S H3S 119.4 . . ?
C4S C3S H3S 119.4 . . ?
C3S C4S C5S 118.8(12) . . ?
C3S C4S H4S 120.6 . . ?
C5S C4S H4S 120.6 . . ?
C6S C5S C4S 120.0(11) . . ?
C6S C5S H5S 120.0 . . ?
C4S C5S H5S 120.0 . . ?
C5S C6S C1S 120.7(10) . . ?
C5S C6S H6S 119.6 . . ?
C1S C6S H6S 119.6 . . ?

_refine_diff_density_max         0.559
_refine_diff_density_min         -0.272
_refine_diff_density_rms         0.051

