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_2104200
_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_coeditor_code           BM5058
_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), Cl5 Sb, Cl4 Sb'
_chemical_formula_sum            'C9 H30 Cl9 P3 Sb2'
_chemical_formula_weight         793.79
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                   14.842(3)
_cell_length_b                   9.3475(19)
_cell_length_c                   21.624(4)
_cell_measurement_reflns_used    54675
_cell_measurement_temperature    175(2)
_cell_measurement_theta_max      43.86
_cell_measurement_theta_min      3.94
_cell_volume                     3000.0(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      175(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.863
_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  0.0413
_diffrn_reflns_av_sigmaI/netI    0.0447
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            54675
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         43.86
_diffrn_reflns_theta_min         3.94
_exptl_absorpt_coefficient_mu    2.759
_exptl_absorpt_correction_T_max  0.63
_exptl_absorpt_correction_T_min  0.56
_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    1.757
_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         1.324
_refine_diff_density_min         -1.311
_refine_ls_abs_structure_details
'Flack H D (1983), Acta Cryst. A39, 876-881, 6577 Friedel pairs'
_refine_ls_abs_structure_Flack   0.480(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.942
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         16806
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      0.942
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0257
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0280P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0494
_refine_ls_wR_factor_ref         0.0605
_reflns_number_gt                10215
_reflns_number_total             16806
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            bm5058.cif
_cod_data_source_block           175K
_cod_depositor_comments
;
 Removing duplicate rows from the ATOM_TYPE loop.

 Antanas Vaitkus,
 2018-08-07
;
_cod_original_cell_volume        3000.1(10)
_cod_original_sg_symbol_H-M      Pna2(1)
_cod_database_code               2104200
_cod_database_fobs_code          2104200