Zwitterionic half-sandwich Rh and Ir complexes containing a diphosphine nido-carborane ligand: synthesis, structure transformation and application in H2 activation
Zi-Jian Yao; Xian-Kuan Huo; Guo-Xin Jin; Chem.Commun. 48 (2012) 6714–; doi:10.1039/c2cc32036c

data_7107913
_publ_section_title
;
 Zwitterionic half-sandwich Rh and Ir complexes containing a diphosphine
 nido-carborane ligand: synthesis, structure transformation and
 application in H2 activation
;
_journal_name_full               Chem.Commun.
_journal_page_first              6714
_journal_paper_doi               10.1039/c2cc32036c
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C36 H44 B9 P2 Rh'
_chemical_formula_weight         738.85
_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                 104.924(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.469(4)
_cell_length_b                   19.555(7)
_cell_length_c                   17.854(7)
_cell_measurement_reflns_used    831
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.406
_cell_measurement_theta_min      2.641
_cell_volume                     3869(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_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  0.0531
_diffrn_reflns_av_sigmaI/netI    0.0905
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18585
_diffrn_reflns_theta_full        27.01
_diffrn_reflns_theta_max         27.01
_diffrn_reflns_theta_min         1.57
_diffrn_standards_decay_%        3.32
_exptl_absorpt_coefficient_mu    0.549
_exptl_absorpt_correction_T_max  0.9522
_exptl_absorpt_correction_T_min  0.8311
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.126
_refine_diff_density_min         -0.633
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.904
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         8205
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      0.913
_refine_ls_R_factor_all          0.0880
_refine_ls_R_factor_gt           0.0514
_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^)+(0.0694P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1260
_refine_ls_wR_factor_ref         0.1352
_reflns_number_gt                4930
_reflns_number_total             8205
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc32036c.txt
_cod_data_source_block           f91107c
_cod_original_cell_volume        3869(3)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7107913