σ-Borane Complexes of Iridium: Synthesis and Structural Characterization
Travis J. Hebden; Melanie C. Denney; Vincent Pons; Paula M. B. Piccoli; Thomas F. Koetzle; Arthur J. Schultz; Werner Kaminsky; Karen I. Goldberg; D. Michael Heinekey; Journal of the American Chemical Society 130 (2008) 10812–10820; doi:10.1021/ja801898m

data_4108172
_publ_contact_author_address
;
Department of Chemistry, BOX 351700
University of Washington
Seattle, WA 98195
USA
;
_publ_contact_author_email       wernerka@u.washington.edu
_publ_contact_author_name        'Werner Kaminsky'
_publ_section_title
;
 \s-Borane Complexes of Iridium: Synthesis and Structural Characterization
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10812
_journal_page_last               10820
_journal_paper_doi               10.1021/ja801898m
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         '2(C28 H52 B Ir O4 P2), C4 H8 O'
_chemical_formula_sum            'C60 H112 B2 Ir2 O9 P4'
_chemical_formula_weight         1507.40
_chemical_name_common            TJHI82Ax1
_chemical_name_systematic        TJHI82Ax1
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 90.3735(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   41.2238(2)
_cell_length_b                   11.1233(2)
_cell_length_c                   14.6122(3)
_cell_measurement_reflns_used    1804
_cell_measurement_temperature    130(2)
_cell_volume                     6700.20(19)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       KappaCCD
_computing_data_reduction        'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'maXus, Zortep'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    DIRDIF
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.881
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w 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  0.0974
_diffrn_reflns_av_sigmaI/netI    0.0810
_diffrn_reflns_limit_h_max       61
_diffrn_reflns_limit_h_min       -61
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            26615
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         31.97
_diffrn_reflns_theta_min         2.35
_exptl_absorpt_coefficient_mu    4.114
_exptl_absorpt_correction_T_max  0.2040
_exptl_absorpt_correction_T_min  0.1552
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   HKL2000
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_description       prism
_exptl_crystal_F_000             3072
_exptl_crystal_size_max          0.59
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.38
_refine_diff_density_max         2.822
_refine_diff_density_min         -3.992
_refine_diff_density_rms         0.212
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     381
_refine_ls_number_reflns         10236
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0501
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0415P)^2^+69.0334P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1195
_refine_ls_wR_factor_ref         0.1313
_reflns_number_gt                8134
_reflns_number_total             10236
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja801898m-file003.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        6700.21(19)
_cod_original_sg_symbol_H-M      'C 2/c '
_cod_database_code               4108172