Adducts of Lewis acidic stibanes with phosphane chalcogenides.
Krieft, Jonas; Koch, Hannah; Neumann, Beate; Stammler, Hans-Georg; Lamm, Jan-Hendrik; Mix, Andreas; Mitzel, Norbert W.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 16280–16286; doi:10.1039/d4dt02268h

data_7717010
_publ_section_title
;
 Adducts of Lewis acidic stibanes with phosphane chalcogenides.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16280
_journal_page_last               16286
_journal_paper_doi               10.1039/d4dt02268h
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C12 H19 Cl F10 P S Sb'
_chemical_formula_sum            'C12 H19 Cl F10 P S Sb'
_chemical_formula_weight         573.50
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-06-26
_audit_creation_method
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_audit_update_record
;
2024-07-03 deposited with the CCDC.	2024-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                105.3756(11)
_cell_angle_beta                 102.9282(11)
_cell_angle_gamma                108.4462(13)
_cell_formula_units_Z            2
_cell_length_a                   8.86176(13)
_cell_length_b                   10.95308(16)
_cell_length_c                   11.95144(13)
_cell_measurement_reflns_used    48564
_cell_measurement_temperature    202(140)
_cell_measurement_theta_max      36.4100
_cell_measurement_theta_min      3.2470
_cell_volume                     999.25(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      202(140)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -94.00 -37.00   1.00    7.50    --  -27.30 145.00 -52.86   57
  2  \w    -42.00   3.00   1.00    7.50    --  -27.30 -77.00   0.00   45
  3  \w    -98.00 -41.00   1.00    7.50    --  -27.30 151.00-157.02   57
  4  \w    -92.00 -36.00   1.00    7.50    --  -27.30 142.00  40.93   56
  5  \w    -44.00  48.00   1.00    7.50    --   27.30 -38.00 -30.00   92
  6  \w    -44.00  48.00   1.00    7.50    --   27.30 -38.00-120.00   92
  7  \w      2.00  96.00   1.00    7.50    --   27.30  57.00 150.00   94
  8  \w    -41.00  52.00   1.00    7.50    --   27.30 -57.00 150.00   93
  9  \w    -44.00  48.00   1.00    7.50    --   27.30 -38.00  30.00   92
 10  \w      2.00  96.00   1.00    7.50    --   27.30  57.00 -60.00   94
 11  \w      2.00  96.00   1.00    7.50    --   27.30  57.00-150.00   94
 12  \w      7.00  98.00   1.00    7.50    --   27.30  38.00  60.00   91
 13  \w    -92.00 -36.00   1.00    7.50    --  -27.30 143.00 137.93   56
 14  \w    -57.00  21.00   1.00    7.50    --  -27.30  77.00-180.00   78
 15  \w    -42.00   3.00   1.00    7.50    --  -27.30 -77.00-120.00   45
 16  \w    -42.00   3.00   1.00    7.50    --  -27.30 -77.00 -90.00   45
 17  \w    -42.00   3.00   1.00    7.50    --  -27.30 -77.00-180.00   45
 18  \w    -57.00  21.00   1.00    7.50    --  -27.30  77.00 -30.00   78
 19  \w     39.00 111.00   1.00    7.50    --   27.30 178.00-180.00   72
 20  \w    -41.00  52.00   1.00    7.50    --   27.30 -57.00-180.00   93
 21  \w    -15.00  65.00   1.00    7.50    --   27.30 -99.00   0.00   80
 22  \w     14.00  92.00   1.00    7.50    --   27.30-142.00  70.24   78
 23  \w    -96.00  -2.00   1.00    7.50    --  -27.30 -57.00  60.00   94
 24  \w    -58.00 113.00   1.00    7.50    --   27.30   0.00-150.00  171
 25  \w    -58.00 113.00   1.00    7.50    --   27.30   0.00-120.00  171
 26  \w    -58.00  75.00   1.00    7.50    --   27.30   0.00 -90.00  133
 27  \w    -58.00 113.00   1.00    7.50    --   27.30   0.00-180.00  171
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0320518000
_diffrn_orient_matrix_UB_12      -0.0720759000
_diffrn_orient_matrix_UB_13      -0.0332658000
_diffrn_orient_matrix_UB_21      0.0832894000
_diffrn_orient_matrix_UB_22      0.0049411000
_diffrn_orient_matrix_UB_23      0.0055171000
_diffrn_orient_matrix_UB_31      0.0079251000
_diffrn_orient_matrix_UB_32      -0.0122320000
_diffrn_orient_matrix_UB_33      0.0559888000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_av_unetI/netI     0.0224
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            91566
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.943
_diffrn_reflns_theta_min         2.573
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.782
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.645
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.90a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.906
_exptl_crystal_description       plate
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.785
_refine_diff_density_min         -0.703
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         9773
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0229
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0188P)^2^+0.4890P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0477
_refine_ls_wR_factor_ref         0.0500
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8844
_reflns_number_total             9773
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02268h3.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7717007--7717016.cif.'
_cod_database_code               7717010
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C12 H19 Cl F10 S P Sb'
_shelx_estimated_absorpt_t_max   0.901
_shelx_estimated_absorpt_t_min   0.717
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C),
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              28636
_shelx_hkl_checksum              6079
_olex2_date_sample_data_collection 2023-06-23
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.155
_oxdiff_exptl_absorpt_empirical_full_min 0.787