Synthesis of Monohalogeno Derivatives of closo-[B~9~H~9~]^2-^. Crystal Structures of (Ph~4~P)~2~[1-XB~9~H~8~]*CH~3~CN (X = Cl, Br, I)
Katja Siegburg; Wilhelm Preetz; Inorganic Chemistry 39 (2000) 3280–3282; doi:10.1021/ic9913334

data_4321184
_publ_contact_author
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    Wilhelm Preetz
    Institut f\"ur Anorganische Chemie
    Universit \"at Kiel
    Olshausenstrasse 40
    D-24098 Kiel
    Germany
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_publ_contact_author_email       siegburg@ac.uni-kiel.de
_publ_contact_author_fax         '049 431 880 1520'
_publ_contact_author_phone       '049 431 880 2406'
_publ_section_title
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 Synthesis of Monohalogeno Derivatives of closo-[B~9~H~9~]^2-^. Crystal
 Structures of (Ph~4~P)~2~[1-XB~9~H~8~]*CH~3~CN (X = Cl, Br, I)
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3280
_journal_page_last               3282
_journal_paper_doi               10.1021/ic9913334
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C50 H51 B9 Cl N P2'
_chemical_formula_weight         860.60
_chemical_name_systematic
; 
 ? 
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_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 96.470(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   10.658(10)
_cell_length_b                   32.862(6)
_cell_length_c                   13.787(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    208(2)
_cell_measurement_theta_max      22.96
_cell_measurement_theta_min      2.02
_cell_volume                     4798(5)
_computing_cell_refinement       'CAD-4-PC ver. 1.5 (Enraf-Nonius, 1994)'
_computing_data_collection       'CAD-4-PC ver. 1.5 (Enraf-Nonius, 1994)'
_computing_data_reduction        'MolEN (Fair, 1990)'
_computing_molecular_graphics    'DIAMOND 2.0 (Bergerhoff, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare, 1993)'
_diffrn_ambient_temperature      208(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_method       omega/2theta
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0205
_diffrn_reflns_av_sigmaI/netI    0.0217
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12902
_diffrn_reflns_theta_full        22.96
_diffrn_reflns_theta_max         22.96
_diffrn_reflns_theta_min         2.02
_diffrn_standards_decay_%        0.2
_diffrn_standards_interval_time  15000s
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.182
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.853
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.191
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1800
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.292
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.46(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1199
_refine_ls_number_reflns         11655
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0388
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0997P)^2^+1.8118P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1137
_refine_ls_wR_factor_ref         0.1361
_reflns_number_gt                10738
_reflns_number_total             11655
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9913334_1.cif
_cod_data_source_block           f
_cod_depositor_comments
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The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
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_cod_original_cell_volume        4798(2)
_cod_database_code               4321184