Synthesis of Rh(iii) thiophosphinito pincer hydrido complexes by base-free C-H bond activation at room temperature.
Vlahopoulou, G.; Möller, S; Haak, J.; Hasche, P.; Drexler, H.-J.; Heller, D.; Beweries, T.; Chemical communications (Cambridge, England) 54 (2018) 6292–6295; doi:10.1039/c8cc03913e

data_7121757
_publ_section_title
;
 Synthesis of Rh(iii) thiophosphinito pincer hydrido complexes by
 base-free C-H bond activation at room temperature.
;
_journal_issue                   49
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              6292
_journal_page_last               6295
_journal_paper_doi               10.1039/c8cc03913e
_journal_volume                  54
_journal_year                    2018
_chemical_formula_sum            'C76 H70 Cl6 P4 Rh4 S4'
_chemical_formula_weight         1859.78
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2018-01-12 deposited with the CCDC.
2018-05-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.9850(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0429(3)
_cell_length_b                   13.0157(3)
_cell_length_c                   45.0034(12)
_cell_measurement_reflns_used    9892
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      70.12
_cell_measurement_theta_min      3.67
_cell_volume                     7053.1(3)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.846
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_type           CuK\a
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_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_unetI/netI     0.0414
_diffrn_reflns_Laue_measured_fraction_full 0.846
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            38252
_diffrn_reflns_point_group_measured_fraction_full 0.846
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         61.165
_diffrn_reflns_theta_min         1.964
_diffrn_source                   microfocus
_exptl_absorpt_coefficient_mu    11.848
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.4753
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.751
_exptl_crystal_description       prism
_exptl_crystal_F_000             3728
_exptl_crystal_size_max          0.195
_exptl_crystal_size_mid          0.132
_exptl_crystal_size_min          0.115
_refine_diff_density_max         1.179
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     847
_refine_ls_number_reflns         10806
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0398
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0503P)^2^+14.0513P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0990
_refine_ls_wR_factor_ref         0.1040
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9315
_reflns_number_total             10806
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc03913e2.cif
_cod_data_source_block           ax1402abs1
_cod_depositor_comments
'Adding full bibliography for 7121756--7121760.cif.'
_cod_database_code               7121757
_shelxl_version_number           2014-3
_shelx_res_checksum              13627