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_4085241
_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         'C6 H22 B22 Hg, 2(C8 H20 N)'
_chemical_formula_sum            'C22 H62 B22 Hg N2'
_chemical_formula_weight         793.15
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           57
_space_group_name_Hall           '-P 2c 2b'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2c 2b'
_symmetry_space_group_name_H-M   'P b c m'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.2713(7)
_cell_length_b                   18.7533(9)
_cell_length_c                   16.8241(8)
_cell_measurement_reflns_used    18834
_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      27.1764
_cell_measurement_theta_min      3.2441
_cell_volume                     5764.7(4)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_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      290(2)
_diffrn_detector_area_resol_mean 16.2711
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_sigmaI/netI    0.0276
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            37090
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.25
_exptl_absorpt_coefficient_mu    2.684
_exptl_absorpt_correction_T_max  0.575
_exptl_absorpt_correction_T_min  0.371
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-RED 1.20 (Stoe & Cie, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.914
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_platon_squeeze_details
;
;
_refine_diff_density_max         4.401
_refine_diff_density_min         -1.058
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.170
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     233
_refine_ls_number_reflns         5253
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.170
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0443
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0854P)^2^+1.0179P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1437
_refine_ls_wR_factor_ref         0.1490
_reflns_number_gt                3576
_reflns_number_total             5267
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5009956_si_001.cif
_cod_data_source_block           '[Et4N]2[Hg(12-HCC-closo-1-CB11H10)2]_Et2On'
_cod_depositor_comments
'Adding full bibliography for 4085239--4085242.cif.'
_cod_database_code               4085241