Synthesis and First X-ray Structural Analysis of Monomeric Imino-λ5-stibanes
Yoshihiro Matano; Hazumi Nomura; Hitomi Suzuki; Inorganic Chemistry 39 (2000) 1340–1341; doi:10.1021/ic991120e

data_4320832
_publ_contact_author_address
;
    Sakyo-ku, Kyoto 606-8502, JAPAN
;
_publ_contact_author_email       ' matano@kuchem.kyoto-u.ac.jp '
_publ_contact_author_fax         ' +81-75-753-4000 '
_publ_contact_author_name        ' Yoshihiro Matano'
_publ_contact_author_phone       ' +81-75-753-4042 '
_publ_section_title
;
 Synthesis and First X-ray Structural Analysis of Monomeric
 Imino-\l5-stibanes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1340
_journal_page_last               1341
_journal_paper_doi               10.1021/ic991120e
_journal_volume                  39
_journal_year                    2000
_chemical_formula_moiety         'C22 H21 F3 N O2 S Sb '
_chemical_formula_sum            'C22 H21 F3 N O2 S Sb'
_chemical_formula_weight         542.22
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_date             'Sat Sep 11 17:13:34 1999'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 103.10(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.285(2)
_cell_length_b                   15.234(3)
_cell_length_c                   13.410(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298.2
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      14.6
_cell_volume                     2245.4(7)
_computing_cell_refinement       'Rigaku/AFC Diffractometer Control'
_computing_data_collection       'Rigaku/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_diffrn_ambient_temperature      298.2
_diffrn_measurement_device_type  'Rigaku AFC7S'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.04934
_diffrn_orient_matrix_UB_12      -0.03002
_diffrn_orient_matrix_UB_13      -0.04315
_diffrn_orient_matrix_UB_21      0.02173
_diffrn_orient_matrix_UB_22      0.05830
_diffrn_orient_matrix_UB_23      -0.02513
_diffrn_orient_matrix_UB_31      0.07329
_diffrn_orient_matrix_UB_32      0.00291
_diffrn_orient_matrix_UB_33      0.05804
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.023
_diffrn_reflns_av_sigmaI/netI    0.075
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5406
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.52
_diffrn_standards_decay_%        -0.60
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.362
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.713
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1080.00
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.68
_refine_diff_density_min         -0.45
_refine_ls_extinction_coef       0.0022(4)
_refine_ls_extinction_method     'Zachariasen(1967) type 2 Gaussian isotropic'
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     272
_refine_ls_number_reflns         3682
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0327
_refine_ls_shift/su_max          0.0300
_refine_ls_shift/su_mean         0.0010
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00048|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0436
_refine_ls_wR_factor_ref         0.0435
_reflns_number_gt                3682
_reflns_number_total             5175
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            ic991120e_1.cif
_cod_data_source_block           o-Tol3Sb_NSO2CF3
_cod_original_cell_volume        2245.3(7)
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_original_formula_sum        'C22 H21 F3 N O2 S Sb '
_cod_database_code               4320832