Unfairly Forgotten Member of the Iodocarborane Family: Synthesis and Structural Characterization of 8-Iodo-1,2-dicarba-closo-dodecaborane, Its Precursors, and Derivatives.
Alexander V. Safronov; Yulia V. Sevryugina; Satish S. Jalisatgi; Robert D. Kennedy; Charles L. Barnes; M. Frederick Hawthorne; Inorganic Chemistry 51 (2012) 2629–2637; doi:10.1021/ic2025846

data_4328436
_publ_section_title
;
 Unfairly Forgotten Member of the Iodocarborane Family: Synthesis and
 Structural Characterization of 8-Iodo-1,2-dicarba-closo-dodecaborane, Its
 Precursors, and Derivatives.
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2629
_journal_page_last               2637
_journal_paper_doi               10.1021/ic2025846
_journal_volume                  51
_journal_year                    2012
_chemical_absolute_configuration ad
_chemical_formula_moiety
;
 B10 C2 H10 I2
;
_chemical_formula_sum            'C2 H10 B10 I2'
_chemical_formula_weight         396.00
_chemical_name_systematic
; 
 3,10-diiodo-1,2-dicarba-closo-dodecaborane(10) 
;
_space_group_IT_number           76
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      76
_symmetry_space_group_name_Hall  'P 4w'
_symmetry_space_group_name_H-M   'P 41'
_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                   7.5280(3)
_cell_length_b                   7.5280(3)
_cell_length_c                   21.1968(15)
_cell_measurement_reflns_used    9904
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      2.87
_cell_volume                     1201.24(11)
_computing_cell_refinement       'Apex II'
_computing_data_collection       'Apex II'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXP-01 (Sheldrick, 2001)'
_computing_publication_material  'SHELXCIF-01 (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXL-01 (Sheldrick, 2001)'
_computing_structure_solution    'SHELXS-01 (Sheldrick, 2001)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '0.5 deg wide \w exposures'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_sigmaI/netI    0.0174
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            14202
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    5.180
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.55
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS  (Bruker-AXS, 2007)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.190
_exptl_crystal_density_method    none
_exptl_crystal_description       plate
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.652
_refine_diff_density_min         -0.689
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.04(4)
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         2752
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0217
_refine_ls_R_factor_gt           0.0206
_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^)+(0.0253P)^2^+0.8049P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0506
_refine_ls_wR_factor_ref         0.0516
_reflns_number_gt                2640
_reflns_number_total             2752
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic2025846_si_001_6.cif
_cod_data_source_block           '[B10C2H10](3,10-I)2_(15)'
_cod_original_sg_symbol_Hall     'P 4w        '
_cod_original_sg_symbol_H-M      'P 41 '
_cod_database_code               4328436