Heterolytic H2 activation on a carbene-ligated rhodathiaborane promoted by isonido-nido cage opening
Beatriz Calvo; Ramon Macias; Victor Polo; Maria Jose Artigas; Fernando J. Lahoz; Luis A. Oro; Chem.Commun. 49 (2013) 9863–; doi:10.1039/c3cc45880f

data_7109911
_publ_section_title
;
 Heterolytic H2 activation on a carbene-ligated rhodathiaborane promoted
 by isonido-nido cage opening
;
_journal_name_full               Chem.Commun.
_journal_page_first              9863
_journal_paper_doi               10.1039/c3cc45880f
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety         'C28 H36 B9 N3 P Rh S, C H2 Cl2'
_chemical_formula_sum            'C29 H38 B9 Cl2 N3 P Rh S'
_chemical_formula_weight         762.75
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 98.586(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.478(3)
_cell_length_b                   18.762(5)
_cell_length_c                   15.649(5)
_cell_measurement_reflns_used    7351
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.896
_cell_measurement_theta_min      2.3295
_cell_volume                     3332.2(16)
_computing_cell_refinement       'APEX2 v. 2009.7 (Bruker AXS, 2008)'
_computing_data_collection       'APEX2 v. 2009.7 (Bruker AXS, 2008)'
_computing_data_reduction        'APEX2 v. 2009.7 (Bruker AXS, 2008)'
_computing_molecular_graphics    ORTEP
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type  'Bruker APEX system'
_diffrn_measurement_method       '\w rotations 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  0.0690
_diffrn_reflns_av_sigmaI/netI    0.0550
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            39222
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.48
_diffrn_reflns_theta_min         1.71
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    0.812
_exptl_absorpt_correction_T_max  0.9103
_exptl_absorpt_correction_T_min  0.8670
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Multi-scan correction included in APEX2 package (Bruker AXS, 2008)

;
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Cube
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.181
_exptl_crystal_size_mid          0.137
_exptl_crystal_size_min          0.118
_refine_diff_density_max         2.531
_refine_diff_density_min         -1.019
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     477
_refine_ls_number_reflns         7940
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0737
_refine_ls_R_factor_gt           0.0548
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0767P)^2^+3.9757P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1318
_refine_ls_wR_factor_ref         0.1458
_reflns_number_gt                6260
_reflns_number_total             7940
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc45880f.txt
_cod_data_source_block           fjl2161a
_cod_original_cell_volume        3332.5(17)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7109911