Salts of the Dianions [Hg(12-X-closo-1-CB11H10)2]2‒(X = I, C≡CH, C≡CFc, C≡CSiiPr3): Synthesis and Spectroscopic and Structural Characterization
Himmelspach, Alexander; Warneke, Jonas; Schäfer, Marius; Hailmann, Michael; Finze, Maik; Organometallics 34 (2015) 462–; doi:10.1021/om5009956

data_4085240
_publ_section_title
;
 Salts of the Dianions [Hg(12-X-closo-1-CB11H10)2]2--(X = I, C\\tb CH,
 C\\tb CFc, C\\tb CSiiPr3): Synthesis and Spectroscopic and Structural
 Characterization
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              462
_journal_paper_doi               10.1021/om5009956
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         '3(C2 H20 B22 Hg I2), 1.98(Cs2), 2(Cs)'
_chemical_formula_sum            'C6 H60 B66 Cs5.96 Hg3 I6'
_chemical_formula_weight         3001.31
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           190
_space_group_name_Hall           'P -6c -2c'
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P -6c -2c'
_symmetry_space_group_name_H-M   'P -6 2 c'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   25.360(4)
_cell_length_b                   25.360(4)
_cell_length_c                   11.528(2)
_cell_measurement_reflns_used    2000
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.34
_cell_volume                     6420.7(18)
_computing_cell_refinement       'CELL (Stoe & Cie, 1996)'
_computing_data_collection       'EXPOSE (Stoe & Cie, 1996)'
_computing_data_reduction        'INTEGRATE (Stoe & Cie, 1996)'
_computing_molecular_graphics    'Diamond3.1 (Crystal Impact GbR, 2006)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       \f-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  0.0805
_diffrn_reflns_av_sigmaI/netI    0.0467
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            82476
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    6.698
_exptl_absorpt_correction_T_max  0.596
_exptl_absorpt_correction_T_min  0.254
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-RED 1.20 (Stoe & Cie, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2623.6
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_platon_squeeze_details
;
;
_refine_diff_density_max         1.487
_refine_diff_density_min         -0.770
_refine_diff_density_rms         0.182
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.049(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         3977
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0431
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0672P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1125
_refine_ls_wR_factor_ref         0.1154
_reflns_number_gt                3008
_reflns_number_total             3977
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5009956_si_001.cif
_cod_data_source_block           Cs2[Hg(12-I-closo-1-CB11H10)2]_Me2COn
_cod_depositor_comments
'Adding full bibliography for 4085239--4085242.cif.'
_cod_original_cell_volume        6421.1(18)
_cod_database_code               4085240