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_1567139
_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 H93 Ge9 Rh Si12 W'
_chemical_formula_sum            'C37 H93 Ge9 Rh Si12 W'
_chemical_formula_weight         1815.26
_chemical_name_systematic
;
 Ge9{Si(SiMe3)}3RhH2W(Cp)2
;
_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                 101.5750(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.27830(10)
_cell_length_b                   25.64300(10)
_cell_length_c                   19.84610(10)
_cell_measurement_reflns_used    123473
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      76.4680
_cell_measurement_theta_min      3.8540
_cell_volume                     7118.64(7)
_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 0.997
_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  0.0545
_diffrn_reflns_av_unetI/netI     0.0172
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            196412
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.490
_diffrn_reflns_theta_min         3.599
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.032
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65893
_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            black
_exptl_crystal_density_diffrn    1.694
_exptl_crystal_description       block
_exptl_crystal_F_000             3560
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.971
_refine_diff_density_min         -0.776
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     668
_refine_ls_number_reflns         14900
_refine_ls_number_restraints     157
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0252
_refine_ls_R_factor_gt           0.0244
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0332P)^2^+7.5677P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0623
_refine_ls_wR_factor_ref         0.0629
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14470
_reflns_number_total             14900
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc02552c3.cif
_cod_data_source_block           OT445
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1567139
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.241
_shelx_estimated_absorpt_t_max   0.405
_shelx_res_checksum              11057
_shelx_hkl_checksum              80862