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_2104201
_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_moiety         '3(C3 H10 P), Cl9 Sb2'
_chemical_formula_sum            'C9 H30 Cl9 P3 Sb2'
_chemical_formula_weight         793.81
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2c 2n'
_symmetry_space_group_name_H-M   'P n a m'
_atom_sites_solution_hydrogens   geom
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.070(3)
_cell_length_b                   9.3026(19)
_cell_length_c                   22.008(4)
_cell_measurement_reflns_used    4162
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      29.44
_cell_measurement_theta_min      3.17
_cell_volume                     3085.3(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.948
_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  0.0368
_diffrn_reflns_av_sigmaI/netI    0.0402
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            36684
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.44
_diffrn_reflns_theta_min         3.17
_exptl_absorpt_coefficient_mu    2.683
_exptl_absorpt_correction_T_max  0.64
_exptl_absorpt_correction_T_min  0.58
_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    1.709
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.252
_exptl_crystal_size_mid          0.173
_exptl_crystal_size_min          0.168
_refine_diff_density_max         0.559
_refine_diff_density_min         -0.540
_refine_ls_extinction_coef       0.0023(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_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     129
_refine_ls_number_reflns         4156
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0811
_refine_ls_R_factor_gt           0.0311
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0347P)^2^+1.2550P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0819
_refine_ls_wR_factor_ref         0.1069
_reflns_number_gt                2130
_reflns_number_total             4156
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            bm5058.cif
_cod_data_source_block           295K
_cod_original_cell_volume        3085.3(11)
_cod_original_sg_symbol_H-M      Pnam
_cod_database_code               2104201