An Icosahedral Array of Methyl Groups Supported by an Aromatic Borane Scaffold: The [closo-B12(CH3)12]2- Ion
Toralf Peymann; Carolyn B. Knobler; M. Frederick Hawthorne; Journal of the American Chemical Society 121 (1999) 5601–5602; doi:10.1021/ja990884q

data_4116421
_publ_contact_author
;
Hawthorne, M. F.,
Department of Chemistry and Biochemistry,
University of California,
Los Angeles, CA 90095-1569.  USA
;
_publ_contact_author_email       mfh@chem.ucla.edu
_publ_contact_author_fax         310-825-5490
_publ_contact_author_phone       310-825-7378
_publ_section_title
;
 An Icosahedral Array of Methyl Groups Supported by an Aromatic Borane
 Scaffold: The [closo-B12(CH3)12]2- Ion
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5601
_journal_page_last               5602
_journal_paper_doi               10.1021/ja990884q
_journal_volume                  121
_journal_year                    1999
_chemical_formula_structural
;
[(C~5~H~5~N)~2~CH~2~]^2+^ [B~12~(CH~3~)~12~]^2-^ CH~3~CN
;
_chemical_formula_sum            'C25 H51 B12 N3'
_chemical_formula_weight         523.42
_chemical_name_common
;
dipyridiniomethane dodecamethyl-closo-decaborate(2-) acetonitrile
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P -2n -2ac'
_symmetry_space_group_name_H-M   'P c 21 n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             99-03-08
_audit_creation_method           'JOURNAL(UCLA crystallographic package)'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.715(7)
_cell_length_b                   15.052(10)
_cell_length_c                   22.819(15)
_cell_measurement_reflns_used    54
_cell_measurement_temperature    298
_cell_measurement_theta_max      19.5
_cell_measurement_theta_min      10.0
_cell_volume                     3337(4)
_computing_cell_refinement       'LEAST (UCLA crystallographic package)'
_computing_data_collection       'COLLECT(UCLA crystallographic package)'
_computing_data_reduction        'REDUCE (UCLA crystallographic package)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELX86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measurement_device       'Syntex (Crystal Logic)'
_diffrn_measurement_method       'profile data from \q/2\q scans'
_diffrn_radiation_detector       scintillation
_diffrn_radiation_detector_dtime 3.5
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed  tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_av_sigmaI/netI    .085
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2638
_diffrn_reflns_reduction_process 'modified Lehmann-Larsen algorithm'
_diffrn_reflns_theta_max         57.48
_diffrn_reflns_theta_min         3.87
_diffrn_standards_decay_%        -3.8
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.366
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.042
_exptl_crystal_description       plate
_exptl_crystal_F_000             1128
_exptl_crystal_preparation       capillary
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.237
_refine_diff_density_min         -0.179
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.49(148)
_refine_ls_extinction_coef       0.0038(7)
_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_all   1.042
_refine_ls_goodness_of_fit_obs   1.128
_refine_ls_hydrogen_treatment
;
 calculated positions, displacement parameters riding on those for
attached carbon atom
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         2391
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.043
_refine_ls_restrained_S_obs      1.128
_refine_ls_R_factor_all          0.1351
_refine_ls_R_factor_obs          0.0735
_refine_ls_shift/esd_max         -0.010
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1096P)^2^+2.4971P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2316
_refine_ls_wR_factor_obs         0.1846
_reflns_number_observed          1406
_reflns_number_total             2395
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja990884q.cif
_cod_data_source_block           JA990884Q-68
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1096P)^2^+2.4971P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1096P)^2^+2.4971P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3336.9(39)
_cod_database_code               4116421