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_7107911
_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            'C37 H47 B9 Cl3 Ir P2'
_chemical_formula_weight         949.53
_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                76.059(4)
_cell_angle_beta                 74.745(4)
_cell_angle_gamma                84.583(4)
_cell_formula_units_Z            2
_cell_length_a                   10.584(4)
_cell_length_b                   11.279(4)
_cell_length_c                   18.270(6)
_cell_measurement_reflns_used    993
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.540
_cell_measurement_theta_min      2.538
_cell_volume                     2041.1(13)
_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 0.970
_diffrn_measured_fraction_theta_max 0.970
_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  0.0392
_diffrn_reflns_av_sigmaI/netI    0.0615
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            9254
_diffrn_reflns_theta_full        26.01
_diffrn_reflns_theta_max         26.01
_diffrn_reflns_theta_min         1.86
_diffrn_standards_decay_%        5.77
_exptl_absorpt_coefficient_mu    3.573
_exptl_absorpt_correction_T_max  0.7164
_exptl_absorpt_correction_T_min  0.6737
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.076
_refine_diff_density_min         -1.284
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         7782
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.963
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0609P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1000
_refine_ls_wR_factor_ref         0.1032
_reflns_number_gt                6461
_reflns_number_total             7782
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc32036c.txt
_cod_data_source_block           f90804c
_cod_original_cell_volume        2041.1(12)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7107911