Aryldihydroborane Coordination to Iridium and Osmium Hydrido Complexes
Arnold, Nicole; Mozo, Silvia; Paul, Ursula; Radius, Udo; Braunschweig, Holger; Organometallics 34 (2015) 5709–; doi:10.1021/acs.organomet.5b00788

data_4087994
_publ_section_title
;
 Aryldihydroborane Coordination to Iridium and Osmium Hydrido Complexes
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              5709
_journal_paper_doi               10.1021/acs.organomet.5b00788
_journal_volume                  34
_journal_year                    2015
_chemical_formula_sum            'C32 H56 B Ir O2 P2'
_chemical_formula_weight         737.71
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                73.0670(10)
_cell_angle_beta                 80.836(2)
_cell_angle_gamma                77.115(2)
_cell_formula_units_Z            2
_cell_length_a                   8.4018(9)
_cell_length_b                   12.8783(14)
_cell_length_c                   16.9736(19)
_cell_measurement_reflns_used    9915
_cell_measurement_temperature    168(2)
_cell_measurement_theta_max      26.19
_cell_measurement_theta_min      2.35
_cell_volume                     1703.9(3)
_computing_cell_refinement       'Saint-NT v. 7.23'
_computing_data_collection       'APEX2 ver. 2014.1 (Bruker AXS)'
_computing_data_reduction        'Saint-NT v. 7.23'
_computing_molecular_graphics    'XP ver. 5.1 (Bruker AXS, 1998)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      168(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25277
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.175
_diffrn_reflns_theta_min         2.356
_exptl_absorpt_coefficient_mu    4.037
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.57
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   'Sadabs 2014/3 (Bruker 2014)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_description       plate
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.114
_refine_diff_density_min         -0.612
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         6799
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0264
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0241P)^2^+0.8019P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0581
_refine_ls_wR_factor_ref         0.0597
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6368
_reflns_number_total             6799
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00788_si_003.cif
_cod_data_source_block           7a
_cod_database_code               4087994
_shelx_estimated_absorpt_t_min   0.530
_shelx_estimated_absorpt_t_max   0.924
_shelxl_version_number           2014/6
_shelx_res_checksum              30182
_shelx_hkl_checksum              44154