Synthesis, Chemistry, and Electronic Structures of Group 9 Metallaboranes.
Borthakur, Rosmita; Kar, Sourav; Barik, Subrat Kumar; Bhattacharya, Somnath; Kundu, Gargi; Varghese, Babu; Ghosh, Sundargopal; Inorganic chemistry 56 (2017) 1524–1533; doi:10.1021/acs.inorgchem.6b02626

data_1545104
_publ_section_title
;
 Synthesis, Chemistry, and Electronic Structures of Group 9
 Metallaboranes.
;
_journal_issue                   3
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1524
_journal_page_last               1533
_journal_paper_doi               10.1021/acs.inorgchem.6b02626
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         '(C20 H40 B6 Ir2) + 0.333(C H2 Cl)'
_chemical_formula_sum            'C20.33 H40.67 B6 Cl0.67 Ir2'
_chemical_formula_weight         758.09
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                74.729(2)
_cell_angle_beta                 86.099(2)
_cell_angle_gamma                68.806(3)
_cell_formula_units_Z            6
_cell_length_a                   12.7437(7)
_cell_length_b                   15.8667(7)
_cell_length_c                   21.9272(9)
_cell_measurement_reflns_used    9861
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.7
_cell_measurement_theta_min      2.4
_cell_volume                     3986.0(3)
_computing_cell_refinement       'APEX2/SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2004)'
_computing_molecular_graphics
'ORTEP3 (Farrugia, 1997) and Mercury (Bruno et al., 2002)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SIR92 (Altornare et al., 1993)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker axs kappa apex2 CCD Diffractometer'
_diffrn_measurement_method       '\w and \f scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1223
_diffrn_reflns_av_unetI/netI     0.0914
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            107885
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.884
_diffrn_source                   'Sealed tube'
_exptl_absorpt_coefficient_mu    10.078
_exptl_absorpt_correction_T_max  0.68
_exptl_absorpt_correction_T_min  0.52
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 1999)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.895
_exptl_crystal_description       block
_exptl_crystal_F_000             2148
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         2.341
_refine_diff_density_min         -1.859
_refine_diff_density_rms         0.261
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     818
_refine_ls_number_reflns         15667
_refine_ls_number_restraints     523
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.1091
_refine_ls_R_factor_gt           0.0534
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0509P)^2^+22.8679P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1057
_refine_ls_wR_factor_ref         0.1307
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10104
_reflns_number_total             15667
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02626_si_002.cif
_cod_data_source_block           irb5
_cod_depositor_comments
'Adding full bibliography for 1545104--1545108.cif.'
_cod_database_code               1545104
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.432
_shelx_estimated_absorpt_t_max   0.633
_shelx_res_checksum              18004
_shelx_hkl_checksum              70443