From six- to five-coordinated Sb^III^ in [(CH~3~)~3~PH]~3~[Sb~2~Cl~9~]: transition pathways from single-crystal X-ray diffraction
Gagor, Anna; Wojtaś, Maciej; Pietraszko, Adam; Jakubas, Ryszard; Acta Crystallographica Section B 64 (2008) 558–566; doi:10.1107/S0108768108027353

data_2104202
_publ_section_title
;
 From six- to five-coordinated Sb^III^ in
 [(CH~3~)~3~PH]~3~[Sb~2~Cl~9~]: transition pathways from single-crystal
 X-ray diffraction
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              558
_journal_page_last               566
_journal_paper_doi               10.1107/S0108768108027353
_journal_volume                  64
_journal_year                    2008
_chemical_formula_sum            'C18 H60 Cl18 P6 Sb4'
_chemical_formula_weight         1587.67
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           194
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c 2c'
_symmetry_space_group_name_H-M   'P 63/m m c'
_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                120.00
_cell_formula_units_Z            1
_cell_length_a                   9.1910(13)
_cell_length_b                   9.1910(13)
_cell_length_c                   22.011(4)
_cell_measurement_reflns_used    6828
_cell_measurement_temperature    382(2)
_cell_measurement_theta_max      26.72
_cell_measurement_theta_min      2.56
_cell_volume                     1610.3(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      382(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.965
_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  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0316
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6828
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.72
_diffrn_reflns_theta_min         2.56
_exptl_absorpt_coefficient_mu    2.570
_exptl_absorpt_correction_T_max  0.64
_exptl_absorpt_correction_T_min  0.57
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.6 (release 21-05-2007 CrysAlis171 .NET)
(compiled May 21 2007,16:32:00)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourles
_exptl_crystal_density_diffrn    1.637
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.252
_exptl_crystal_size_mid          0.173
_exptl_crystal_size_min          0.168
_refine_diff_density_max         0.310
_refine_diff_density_min         -0.434
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_matrix_type           full
_refine_ls_number_parameters     34
_refine_ls_number_reflns         680
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.1046
_refine_ls_R_factor_gt           0.0526
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+2.7500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1426
_refine_ls_wR_factor_ref         0.1690
_reflns_number_gt                312
_reflns_number_total             680
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            bm5058.cif
_cod_data_source_block           382K
_cod_original_sg_symbol_H-M      P63/mmc
_cod_database_code               2104202
_cod_database_fobs_code          2104202