A combined experimental and theoretical study of bimetallic bis- and tris-homocubane analogues
Joseph, Benson; Prakash, Rini; Pathak, Kriti; Roisnel, Thierry; Kahlal, Samia; Halet, Jean-François; Ghosh, Sundargopal; New Journal of Chemistry 44 (2020) 674–683; doi:10.1039/C9NJ05117A

data_7059151
_publ_section_title
;
 A combined experimental and theoretical study of bimetallic bis- and
 tris-homocubane analogues
;
_journal_issue                   3
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              674
_journal_page_last               683
_journal_paper_doi               10.1039/C9NJ05117A
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         '(C20 H32 B2 Ir2 S7) + 0.5(C H2 Cl2)'
_chemical_formula_sum            'C20.5 H33 B2 Cl Ir2 S7'
_chemical_formula_weight         945.36
_space_group_crystal_system      tetragonal
_space_group_IT_number           81
_space_group_name_Hall           'P -4'
_space_group_name_H-M_alt        'P -4'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2019-08-08 deposited with the CCDC.	2019-11-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.7466(13)
_cell_length_b                   18.7466(13)
_cell_length_c                   8.3390(6)
_cell_measurement_reflns_used    5564
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.2
_cell_measurement_theta_min      2.8
_cell_volume                     2930.6(4)
_computing_cell_refinement       'APEX3/SAINT (Bruker, 2016)'
_computing_data_collection       'APEX3(Bruker, 2016)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2016)'
_computing_molecular_graphics
'ORTEP3 (Farrugia, 1997) and Mercury (Bruno et al., 2002)'
_computing_publication_material  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_av_unetI/netI     0.0742
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            11644
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.477
_diffrn_reflns_theta_min         2.173
_diffrn_source                   'Incoatec microfocus sealed tube'
_exptl_absorpt_coefficient_mu    9.673
_exptl_absorpt_correction_T_max  0.42
_exptl_absorpt_correction_T_min  0.16
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2016)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.143
_exptl_crystal_description       block
_exptl_crystal_F_000             1796
_exptl_crystal_size_max          0.410
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.170
_refine_diff_density_max         2.295
_refine_diff_density_min         -2.226
_refine_diff_density_rms         0.252
_refine_ls_abs_structure_details
;
 Twinning involves inversion, so Flack parameter cannot be determined
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         6367
_refine_ls_number_restraints     591
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0743
_refine_ls_R_factor_gt           0.0579
_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^)+(0.0319P)^2^+60.6222P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1344
_refine_ls_wR_factor_ref         0.1450
_reflns_Friedel_coverage         0.844
_reflns_Friedel_fraction_full    0.983
_reflns_Friedel_fraction_max     0.970
_reflns_number_gt                5211
_reflns_number_total             6367
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj05117a2.cif
_cod_data_source_block           sqz-nodis
_cod_depositor_comments
;Adding full bibliography for 7059145--7059151.cif.

 Adding full bibliography for 7059145--7059151.cif.
;
_cod_original_cell_volume        2930.6(5)
_cod_original_formula_sum        'C20.50 H33 B2 Cl Ir2 S7'
_cod_database_code               7059151
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.110
_shelx_estimated_absorpt_t_max   0.290
_shelx_res_checksum              72804