Zintl cluster supported low coordinate Rh(i) centers for catalytic H/D exchange between H2 and D2
Townrow, Oliver P. E.; Duckett, Simon B.; Weller, Andrew S.; Goicoechea, Jose M.; Chemical Science  (2022) –; doi:10.1039/D2SC02552C

data_1567138
_publ_section_title
;
 Zintl cluster supported low coordinate Rh(i) centers for catalytic H/D
 exchange between H2 and D2
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC02552C
_journal_year                    2022
_chemical_formula_moiety
'C37 H94 Ge9 Rh Si12 W, C32 H12 B F24, C4 H10 O'
_chemical_formula_sum            'C73 H116 B F24 Ge9 O Rh Si12 W'
_chemical_formula_weight         2753.61
_chemical_name_systematic
;
 [Ge9{Si(SiMe3)}3RhH(H)2W(Cp)2][B{C6H3(CF3)2}4]*Et2O
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2022-02-28 deposited with the CCDC.	2022-06-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.969(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.9023(5)
_cell_length_b                   13.8042(5)
_cell_length_c                   44.4206(12)
_cell_measurement_reflns_used    18711
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      76.2770
_cell_measurement_theta_min      3.7350
_cell_volume                     10896.4(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.81a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.81a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.81a (Rigaku OD, 2020)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5035
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1242
_diffrn_reflns_av_unetI/netI     0.0838
_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       -20
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            101192
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        66.489
_diffrn_reflns_theta_max         66.489
_diffrn_reflns_theta_min         3.778
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.778
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53652
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.81a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_description       needle
_exptl_crystal_F_000             5432
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.040
_refine_diff_density_max         2.530
_refine_diff_density_min         -1.110
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1312
_refine_ls_number_reflns         19207
_refine_ls_number_restraints     367
_refine_ls_restrained_S_all      1.144
_refine_ls_R_factor_all          0.0910
_refine_ls_R_factor_gt           0.0647
_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/[\s^2^(Fo^2^)+(0.0908P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1656
_refine_ls_wR_factor_ref         0.1838
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13688
_reflns_number_total             19207
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc02552c3.cif
_cod_data_source_block           OT490
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1567138
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.409
_shelx_estimated_absorpt_t_max   0.746
_shelx_res_checksum              5386
_shelx_hkl_checksum              29962