A Cationic Rh(III) Complex That Efficiently Catalyzes Hydrogen Isotope Exchange in Hydrosilanes
Jesús Campos; Ana C. Esqueda; Joaquín López-Serrano; Luis Sánchez; Fernando P. Cossio; Abel de Cozar; Eleuterio Álvarez; Celia Maya; Ernesto Carmona; Journal of the American Chemical Society 132 (2010) 16765–16767; doi:10.1021/ja108521b

data_4103589
_publ_contact_author
;
        Celia M. Maya 
        Instituto de Investigaciones Qu\'imicas
        CSIC-Universidad de Sevilla
        Am\'erico Vespucio, 49
        Isla de la Cartuja 
        41092 SEVILLA
        Spain
;
_publ_contact_author_email       maya@us.es
_publ_contact_author_fax         '34 954460565'
_publ_contact_author_phone       '34 954489554'
_publ_section_title
;
 A Cationic Rh(III) Complex That Efficiently Catalyzes Hydrogen Isotope
 Exchange in Hydrosilanes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16765
_journal_page_last               16767
_journal_paper_doi               10.1021/ja108521b
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C27 H35 P Rh, F6 Sb'
_chemical_formula_sum            'C27 H35 F6 P Rh Sb'
_chemical_formula_weight         729.18
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.6591(13)
_cell_length_b                   7.8808(4)
_cell_length_c                   13.9773(8)
_cell_measurement_reflns_used    7660
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.23
_cell_measurement_theta_min      2.58
_cell_volume                     2826.4(3)
_computing_cell_refinement       'Bruker (2006). APEX 2. Version 2.1.'
_computing_data_collection       'Bruker (2006). APEX 2. Version 2.1.'
_computing_data_reduction        'Bruker (2006). APEX 2. Version 2.1.'
_computing_molecular_graphics    'XP, SHELXTL v. 6.14 (Bruker, 2003)'
_computing_publication_material  'XCIF, SHELXTL v. 6.14 (Bruker, 2003)'
_computing_structure_refinement  'XL, SHELXTL v. 6.14 (Bruker, 2003)'
_computing_structure_solution    'Bruker (2006). APEX 2. Version 2.1.'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type
;
 Bruker-Nonius X8kappa APEX II CCD area detector'
;
_diffrn_measurement_method       'phi and omega scans with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0694
_diffrn_reflns_av_sigmaI/netI    0.0392
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            49284
_diffrn_reflns_theta_full        30.63
_diffrn_reflns_theta_max         30.63
_diffrn_reflns_theta_min         2.58
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.650
_exptl_absorpt_correction_T_max  0.8793
_exptl_absorpt_correction_T_min  0.7445
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS, Bruker (2006). APEX 2. Version 2.1. Bruker Analytical
 X-ray Solutions, Madison, Wisconsin, USA.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.714
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.508
_refine_diff_density_min         -0.862
_refine_diff_density_rms         0.115
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.27(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         6139
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0333
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0213P)^2^+4.2734P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0608
_refine_ls_wR_factor_ref         0.0700
_reflns_number_gt                4714
_reflns_number_total             6139
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja108521b_si_002.cif
_cod_data_source_block           ea11309x
_cod_database_code               4103589