Synthesis of Halogenated Polyhedral Phosphaboranes. Crystal Structure of closo-1,7-P2B10Cl10
Willi Keller; Gisela Sawitzki; Wolfgang Haubold; Inorganic Chemistry 39 (2000) 1282–1287; doi:10.1021/ic990112v

data_4300007
_publ_section_title
;
Synthesis of Halogenated Polyhedral Phosphaboranes. Crystal Structure
of closo-1,7-P2B10Cl10
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1282
_journal_page_last               1287
_journal_paper_doi               10.1021/ic990112v
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C7 H8 B10 Cl10 P2'
_chemical_formula_weight         616.67
_chemical_name_common            closo-1,7-P2B10Cl10.toluene
_chemical_name_systematic
2,3,4,5,6,8,9,10,11,12-Decachloro-1,7-diphospha-closo-dodecaborane(10)-toluene
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 93.25(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.239(2)
_cell_length_b                   16.786(3)
_cell_length_c                   15.739(3)
_cell_measurement_reflns_used    27
_cell_measurement_temperature    293
_cell_measurement_theta_max      12.0
_cell_measurement_theta_min      9.3
_cell_volume                     2437.0(8)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'SHELXL-93 (Sheldrick, 1993)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       'w scans'
_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  0.0397
_diffrn_reflns_av_sigmaI/netI    0.0677
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            6234
_diffrn_reflns_theta_max         28.02
_diffrn_reflns_theta_min         1.78
_diffrn_standards_interval_count 98
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.272
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.681
_exptl_crystal_description       rhomb
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.658
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.088
_refine_ls_goodness_of_fit_obs   1.149
_refine_ls_hydrogen_treatment    'fixed isotropic U'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         5890
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_restrained_S_obs      1.149
_refine_ls_R_factor_all          0.1276
_refine_ls_R_factor_obs          0.0669
_refine_ls_shift/esd_max         0.044
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0749P)^2^+2.8147P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1812
_refine_ls_wR_factor_obs         0.1441
_reflns_number_observed          3431
_reflns_number_total             5893
_reflns_observed_criterion       >2sigma(I)
_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^)+(0.0749P)^2^+2.8147P] 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^)+(0.0749P)^2^+2.8147P] 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_database_code               4300007