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_7717007
_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         'C9 H11 Cl2 Sb'
_chemical_formula_sum            'C9 H11 Cl2 Sb'
_chemical_formula_weight         311.83
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-06-06
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-07-03 deposited with the CCDC.	2024-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                103.911(2)
_cell_angle_beta                 90.528(2)
_cell_angle_gamma                93.576(2)
_cell_formula_units_Z            6
_cell_length_a                   8.3946(2)
_cell_length_b                   12.6338(3)
_cell_length_c                   16.1582(5)
_cell_measurement_reflns_used    18508
_cell_measurement_temperature    200.0(1)
_cell_measurement_theta_max      32.7220
_cell_measurement_theta_min      3.5630
_cell_volume                     1659.65(8)
_computing_cell_refinement       'CrysAlisPro 1.171.43.104a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 43.104a 64-bit (release 22-12-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.104a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1773
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.945
_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    -90.00 -65.00   1.00    2.00    --  -23.64 164.00-168.00   25
  2  \w   -101.00 -76.00   1.00    2.00    --  -23.64-164.00 165.00   25
  3  \w      1.00  71.00   1.00    2.00    --   23.80-116.00 -45.00   70
  4  \w     52.00  77.00   1.00    2.00    --   23.80 164.00-168.00   25
  5  \w     78.00 103.00   1.00    2.00    --   23.80-164.00 165.00   25
  6  \w     32.00  72.00   1.00    2.00    --   23.80-164.00 165.00   40
  7  \w    -98.00 -10.00   1.00    2.00    --  -23.64 -38.00-150.00   88
  8  \w    -99.00 -20.00   1.00    2.00    --  -23.64 153.00  61.58   79
  9  \w   -112.00 -42.00   1.00    2.00    --  -23.64-178.00 -90.00   70
 10  \w    -59.00 -34.00   1.00    2.00    --  -23.64 116.00  42.00   25
 11  \w    -40.00  -1.00   1.00    2.00    --  -23.64 -77.00-180.00   39
 12  \w      3.00  96.00   1.00    2.00    --   23.80  38.00-150.00   93
 13  \w      3.00  98.00   1.00    2.00    --   23.80  38.00 120.00   95
 14  \w     -6.00  42.00   1.00    2.00    --   23.80  77.00  60.00   48
 15  \w    -50.00  48.00   1.00    2.00    --   23.80 -38.00-180.00   98
 16  \w     10.00  97.00   1.00    2.00    --   23.80  57.00 -30.00   87
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0109348000
_diffrn_orient_matrix_UB_12      0.0078507000
_diffrn_orient_matrix_UB_13      0.0446986000
_diffrn_orient_matrix_UB_21      -0.0509234000
_diffrn_orient_matrix_UB_22      -0.0473509000
_diffrn_orient_matrix_UB_23      -0.0012611000
_diffrn_orient_matrix_UB_31      0.0667749000
_diffrn_orient_matrix_UB_32      -0.0325043000
_diffrn_orient_matrix_UB_33      -0.0068477000
_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  0.0397
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            55276
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.928
_diffrn_reflns_theta_min         3.275
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.923
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.739
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.104a (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    1.872
_exptl_crystal_description       irregular
_exptl_crystal_F_000             900
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.375
_refine_diff_density_min         -1.630
_refine_diff_density_rms         0.104
_refine_ls_extinction_coef       0.00237(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         13754
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0348
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0246P)^2^+0.6819P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0668
_refine_ls_wR_factor_ref         0.0784
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9642
_reflns_number_total             13754
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02268h3.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7717007--7717016.cif.'
_cod_database_code               7717007
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C9 H11 Cl2 Sb'
_shelx_estimated_absorpt_t_max   0.668
_shelx_estimated_absorpt_t_min   0.579
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C12(H12), C14(H14), C21(H21), C23(H23)
2.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C16(H16A,H16B,H16C),
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C27(H27A,H27B,H27C)
;
_shelx_res_checksum              44793
_shelx_hkl_checksum              53988
_olex2_date_sample_data_collection 2024-06-06
_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 1.272
_oxdiff_exptl_absorpt_empirical_full_min 0.828