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_7121758
_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            'C34 H56 Cl2 O2 P2 Rh2'
_chemical_formula_weight         835.44
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2018-04-17 deposited with the CCDC.
2018-05-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
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_cell_length_c                   29.4358(13)
_cell_measurement_reflns_used    9917
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.86
_cell_measurement_theta_min      2.31
_cell_volume                     7164.5(6)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
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_computing_data_reduction        'SAINT (Bruker, 2013)'
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_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_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0529
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_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       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            68470
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
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_diffrn_reflns_theta_max         27.996
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_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.69
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_description       prism
_exptl_crystal_F_000             3440
_exptl_crystal_size_max          0.331
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_exptl_crystal_size_min          0.130
_refine_diff_density_max         1.170
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_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         8637
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0327
_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^)+(0.0352P)^2^+9.6888P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0744
_refine_ls_wR_factor_ref         0.0826
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6882
_reflns_number_total             8637
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc03913e2.cif
_cod_data_source_block           ax1481absn
_cod_depositor_comments
'Adding full bibliography for 7121756--7121760.cif.'
_cod_database_code               7121758
_shelx_estimated_absorpt_t_min   0.694
_shelx_estimated_absorpt_t_max   0.861
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_shelx_res_checksum              34727