Pentacoordinate Organoantimony Compounds That Isomerize by Turnstile Rotation
Shiro Matsukawa; Hideaki Yamamichi; Yohsuke Yamamoto; Kaori Ando; Journal of the American Chemical Society 131 (2009) 3418–3419; doi:10.1021/ja808113q

data_4104000
_publ_contact_author             'Prof. Yohsuke Yamamoto'
_publ_contact_author_email       yyama@hiroshima-u.ac.jp
_publ_section_title
;
 Pentacoordinate Organoantimony Compounds That Isomerize by Turnstile
 Rotation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3418
_journal_page_last               3419
_journal_paper_doi               10.1021/ja808113q
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C28 H21 Cl F3 O Sb'
_chemical_formula_weight         587.65
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                100.104(2)
_cell_angle_beta                 104.778(2)
_cell_angle_gamma                101.806(2)
_cell_formula_units_Z            4
_cell_length_a                   11.9650(6)
_cell_length_b                   13.3750(7)
_cell_length_c                   16.8490(8)
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      1.3
_cell_volume                     2477.1(2)
_computing_cell_refinement       'HKL(Otwinowski, 1997)'
_computing_data_collection       'HKL(Otwinowski, 1997)'
_computing_data_reduction        'HKL(Otwinowski, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.801
_diffrn_measured_fraction_theta_max 0.801
_diffrn_measurement_device_type  'MacScience DIP2030 Imaging Plate'
_diffrn_measurement_method       \w
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    30.2343
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            9535
_diffrn_reflns_theta_full        27.94
_diffrn_reflns_theta_max         27.94
_diffrn_reflns_theta_min         1.29
_exptl_absorpt_coefficient_mu    1.263
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.576
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.280
_refine_diff_density_min         -2.247
_refine_diff_density_rms         0.258
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     617
_refine_ls_number_reflns         9535
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.1562
_refine_ls_R_factor_gt           0.0811
_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^)+(0.1281P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2043
_refine_ls_wR_factor_ref         0.2409
_reflns_number_gt                5520
_reflns_number_total             9535
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja808113q_si_004.cif
_cod_data_source_block           compound3B
_cod_database_code               4104000