Synthesis and X-ray Crystal Structure of a Cationic Homoleptic (SPS)2Rh(III) Complex and EPR Study of Its Reduction Process
Marjolaine Doux; Nicolas Mézailles; Louis Ricard; Pascal Le Floch; Prashant Adkine; Théo Berclaz; Michel Geoffroy; Inorganic Chemistry 44 (2005) 1147–1152; doi:10.1021/ic049046+

data_4327315
_publ_contact_author_address
;
Laboratoire DCPH
Ecole Polytechnique
Route de Saclay
F91128 Palaiseau
France
;
_publ_contact_author_email       louis.ricard@polytechnique.fr
_publ_contact_author_fax         330169333990
_publ_contact_author_name        'Louis Ricard'
_publ_contact_author_phone       330169334572
_publ_section_title
;
 Synthesis and X-ray Crystal Structure of a Cationic Homoleptic
 (SPS)2Rh(III) Complex and EPR Study of Its Reduction Process
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1147
_journal_page_last               1152
_journal_paper_doi               10.1021/ic049046+
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C62 H53 Cl6 P4 Rh S2'
_chemical_formula_weight         1301.65
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                82.880(5)
_cell_angle_beta                 74.840(5)
_cell_angle_gamma                68.810(5)
_cell_formula_units_Z            2
_cell_length_a                   13.351(5)
_cell_length_b                   13.715(5)
_cell_length_c                   17.502(5)
_cell_measurement_reflns_used    251
_cell_measurement_temperature    150.0(10)
_cell_measurement_theta_max      20.0
_cell_measurement_theta_min      3.0
_cell_volume                     2882.6(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150.0(10)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_sigmaI/netI    0.0467
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            25603
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         3.66
_exptl_absorpt_coefficient_mu    0.798
_exptl_absorpt_correction_T_max  0.8439
_exptl_absorpt_correction_T_min  0.8439
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_description       cube
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.388
_refine_diff_density_min         -1.335
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     623
_refine_ls_number_reflns         16704
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0401
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0725P)^2^+0.7008P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1179
_refine_ls_wR_factor_ref         0.1246
_reflns_number_gt                13813
_reflns_number_total             16704
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0490462Bsi20040719_053604_1.cif
_cod_data_source_block           rhpscl2
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4327315