Synthesis and Investigation of [Cp*(PMe3)Rh(H)(H2)]+ and Its Partially Deuterated and Tritiated Isotopomers: Evidence for a Hydride/Dihydrogen Structure
Felicia L. Taw; Heather Mellows; Peter S. White; Frederick J. Hollander; Robert G. Bergman; Maurice Brookhart; D. Michael Heinekey; Journal of the American Chemical Society 124 (2002) 5100–5108; doi:10.1021/ja0165990

data_4114780
_publ_section_title
;
 Synthesis and Investigation of [Cp*(PMe3)Rh(H)(H2)]+ and Its Partially
 Deuterated and Tritiated Isotopomers: Evidence for a Hydride/Dihydrogen
 Structure
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5100
_journal_page_last               5108
_journal_paper_doi               10.1021/ja0165990
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C47 H41 B Cl2 F24 P Rh'
_chemical_formula_weight         1277.40
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_date             'Wed Jul 11 10:17:12 2001'
_audit_creation_method           'by teXsan'
_cell_angle_alpha                90
_cell_angle_beta                 100.841(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1814(2)
_cell_length_b                   19.1970(4)
_cell_length_c                   24.7379(5)
_cell_measurement_reflns_used    999
_cell_measurement_temperature    159.2
_cell_measurement_theta_max      45.0
_cell_measurement_theta_min      3.0
_cell_volume                     5681.62(19)
_computing_cell_refinement       'Bruker SAINT v5.04'
_computing_data_collection       'Bruker SMART v5.052d'
_computing_data_reduction        'Bruker SAINT v5.04'
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      159.2
_diffrn_measurement_device       unknown
_diffrn_measurement_method       'omega scans with profile analysis'
_diffrn_orient_matrix_UB_11      0.00000
_diffrn_orient_matrix_UB_12      0.00000
_diffrn_orient_matrix_UB_13      0.00000
_diffrn_orient_matrix_UB_21      0.00000
_diffrn_orient_matrix_UB_22      0.00000
_diffrn_orient_matrix_UB_23      0.00000
_diffrn_orient_matrix_UB_31      0.00000
_diffrn_orient_matrix_UB_32      0.00000
_diffrn_orient_matrix_UB_33      0.00000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            26997
_diffrn_reflns_theta_max         26.02
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.532
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_description       blocklike
_exptl_crystal_F_000             2552.00
_exptl_crystal_size_max          0.370
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.230
_refine_diff_density_max         0.54
_refine_diff_density_min         -0.68
_refine_ls_extinction_coef       0.00000
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.622
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     772
_refine_ls_number_reflns         6377
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0000
_refine_ls_R_factor_gt           0.0412
_refine_ls_shift/su_max          0.0180
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0000
_refine_ls_wR_factor_gt          0.0464
_reflns_number_gt                6377
_reflns_number_total             10262
_reflns_threshold_expression     I>3.00sigma
_cod_data_source_file            ja0165990_s1_3.cif
_cod_data_source_block           Felicia's_Rh_Me_complex
_cod_original_cell_volume        5681.6(2)
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_original_formula_sum        'C47 H41 B Cl2 F24 P Rh '
_cod_database_code               4114780