#------------------------------------------------------------------------------
#$Date: 2023-05-31 01:58:20 +0300 (Wed, 31 May 2023) $
#$Revision: 284077 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/32/7713203.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7713203
loop_
_publ_author_name
'Barrios-Vargas, Luz Jimena'
'Abeynayake, Niroshani Samitri'
'Secrist, Carlee'
'Le, Nghia'
'Webster, Charles Edwin'
'Donnadieu, Bruno'
'Kaphan, David M.'
'Roy, Amitava'
'Ibarra, Ilich A.'
'Montiel-Palma, Virginia'
_publ_section_title
;
 Homogeneous versus MOF-supported catalysis: A direct comparison of
 catalytic hydroboration at Ni tripodal P3E (E = Si, Ge) complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01328F
_journal_year                    2023
_chemical_absolute_configuration ad
_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
_space_group_crystal_system      cubic
_space_group_IT_number           218
_space_group_name_Hall           'P -4n 2 3'
_space_group_name_H-M_alt        'P -4 3 n'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-03-08 deposited with the CCDC.	2023-05-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            24
_cell_length_a                   21.7872(3)
_cell_length_b                   21.7872(3)
_cell_length_c                   21.7872(3)
_cell_measurement_reflns_used    2807
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      74.539
_cell_measurement_theta_min      4.058
_cell_volume                     10342.0(2)
_computing_cell_refinement       'APEX4 v2021.4-0'
_computing_data_collection       'APEX4 v2021.4-0'
_computing_data_reduction        'Saint, APEX4 v2021.4-0.'
_computing_molecular_graphics    'Mercury V.4.2.0,POV-Ray v 3.7'
_computing_publication_material  'APEX4 v2021.4-0'
_computing_structure_refinement  SHELXTL-2018/3
_computing_structure_solution    SHELXT
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker AXS D8 Venture  '
_diffrn_measurement_method       'profile data from θ/2θ scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1807
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            189105
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.539
_diffrn_reflns_theta_min         4.058
_exptl_absorpt_coefficient_mu    2.343
_exptl_absorpt_correction_T_max  0.829
_exptl_absorpt_correction_T_min  0.710
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_description       'prism frag'
_exptl_crystal_F_000             4301
_exptl_crystal_size_max          0.157
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.083
_refine_diff_density_max         0.650
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.08(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         3549
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0520
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0664P)²+5.8694P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1269
_refine_ls_wR_factor_ref         0.1337
_reflns_Friedel_coverage         0.845
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                3165
_reflns_number_total             3549
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3dt01328f2.cif
_cod_data_source_block           cvm003_a
_cod_original_cell_volume        10342.0(4)
_cod_database_code               7713203
_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.
;
_shelx_estimated_absorpt_t_min   0.710
_shelx_estimated_absorpt_t_max   0.829
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'
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
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'
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) . . ?
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) . ?
