Synthesis and Structural Characterization ofcloso-exo,exo-nido, andpseudoclosoGroup 1 Carborane Compounds of the C2B10System
Chui, Kwoli; Li, Hung-Wing; Xie, Zuowei; Organometallics 19 (2000) 5447–; doi:10.1021/om000547m

data_4077588
_publ_section_title
;
 Synthesis and Structural Characterization ofcloso-exo,exo-nido,
 andpseudoclosoGroup 1 Carborane Compounds of the C2B10System
;
_journal_issue                   25
_journal_name_full               Organometallics
_journal_page_first              5447
_journal_paper_doi               10.1021/om000547m
_journal_volume                  19
_journal_year                    2000
_chemical_formula_sum            'C32 H55 B10 K O7'
_chemical_formula_weight         698.96
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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                   21.524(2)
_cell_length_b                   11.0456(11)
_cell_length_c                   16.7460(17)
_cell_measurement_temperature    293(2)
_cell_volume                     3981.3(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0867
_diffrn_reflns_av_sigmaI/netI    0.0902
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21440
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    0.175
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9132
_exptl_absorpt_correction_type   abscor
_exptl_crystal_colour            'bright yellow'
_exptl_crystal_density_diffrn    1.166
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.335
_refine_diff_density_min         -0.259
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.07(7)
_refine_ls_extinction_coef       0.0000(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.840
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         6842
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      0.847
_refine_ls_R_factor_all          0.1151
_refine_ls_R_factor_gt           0.0564
_refine_ls_shift/su_max          2.395
_refine_ls_shift/su_mean         0.018
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0832P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1283
_refine_ls_wR_factor_ref         0.1534
_reflns_number_gt                3531
_reflns_number_total             6842
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om000547m.cif
_cod_data_source_block           compound_5
_cod_original_sg_symbol_H-M      Pca2(1)
_cod_database_code               4077588