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_4103588
_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         'C32 H12 B F24, C28 H35 O P Rh'
_chemical_formula_sum            'C60 H47 B F24 O P Rh'
_chemical_formula_weight         1384.67
_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                89.147(2)
_cell_angle_beta                 72.1240(10)
_cell_angle_gamma                86.3190(10)
_cell_formula_units_Z            2
_cell_length_a                   12.1421(3)
_cell_length_b                   12.9364(3)
_cell_length_c                   19.6945(6)
_cell_measurement_reflns_used    9162
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.97
_cell_measurement_theta_min      2.34
_cell_volume                     2938.06(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'CCD area detector'
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_sigmaI/netI    0.0289
_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       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            80405
_diffrn_reflns_theta_full        33.14
_diffrn_reflns_theta_max         33.14
_diffrn_reflns_theta_min         1.09
_exptl_absorpt_coefficient_mu    0.435
_exptl_absorpt_correction_T_max  0.945
_exptl_absorpt_correction_T_min  0.754
_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            orange
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.13
_refine_diff_density_max         2.125
_refine_diff_density_min         -1.413
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     829
_refine_ls_number_reflns         21936
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0604P)^2^+3.4071P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1164
_refine_ls_wR_factor_ref         0.1273
_reflns_number_gt                18154
_reflns_number_total             21936
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja108521b_si_001.cif
_cod_data_source_block           cm03209a
_cod_database_code               4103588