Dodecamethyl-closo-dodecaborate(2-)
Peymann, Toralf; Knobler, Carolyn B.; Khan, Saeed I.; Hawthorne, M. Frederick; Inorganic Chemistry 40 (2001) 1291–1294; doi:10.1021/ic0010398

data_4319391
_publ_section_title
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 Dodecamethyl-closo-dodecaborate(2-)
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_journal_coden_ASTM              INOCAJ
_journal_issue                   6
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1291
_journal_page_last               1294
_journal_paper_doi               10.1021/ic0010398
_journal_volume                  40
_journal_year                    2001
_chemical_compound_source
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crystallized from methylene chloride/ethanol
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_chemical_formula_sum            'C48 H66 B12 N P2'
_chemical_formula_weight         848.68
_chemical_name_systematic
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[Ph~3~P=N=PPh~3~]^+^ {[closo-B~12~(CH~3~)~12~]^.^}^-^
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_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 122.22(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   34.660(29)
_cell_length_b                   9.342(8)
_cell_length_c                   18.693(15)
_cell_measurement_reflns_used    51
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      10.1
_cell_measurement_theta_min      4.6
_cell_volume                     5121(7)
_computing_cell_refinement       'LEAST (UCLA crystallographic package)'
_computing_data_reduction        'REDUCE (UCLA crystallographic package)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298
_diffrn_measurement_device       'Huber (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_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0967
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            4900
_diffrn_reflns_reduction_process 'modified Lehmann-Larsen algorithm'
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         1.3
_diffrn_standards_decay_%        -0.1
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.118
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.101
_exptl_crystal_description       plate
_exptl_crystal_F_000             1804
_exptl_crystal_preparation       fiber
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.257
_refine_diff_density_min         -0.206
_refine_diff_density_rms         0.046
_refine_ls_extinction_coef       0.0006(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_all   1.035
_refine_ls_goodness_of_fit_obs   1.183
_refine_ls_hydrogen_treatment
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All hydrogen atoms in calculated positions with u value based on value
for attached atom.
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_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         4900
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_restrained_S_obs      1.183
_refine_ls_R_factor_all          0.1461
_refine_ls_R_factor_obs          0.0663
_refine_ls_shift/esd_max         0.013
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0620P)^2^+9.4120P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2096
_refine_ls_wR_factor_obs         0.1668
_reflns_number_observed          2489
_reflns_number_total             4900
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0010398_1.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0620P)^2^+9.4120P] 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^)+(0.0620P)^2^+9.4120P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_cell_volume        5120.3(74)
_cod_database_code               4319391