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_7717012
_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_absolute_configuration ad
_chemical_formula_moiety         'C16 H6 Cl F12 Sb'
_chemical_formula_sum            'C16 H6 Cl F12 Sb'
_chemical_formula_weight         583.41
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-06-26
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.74910(10)
_cell_length_b                   8.52600(10)
_cell_length_c                   24.6722(3)
_cell_measurement_reflns_used    44937
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      32.0170
_cell_measurement_theta_min      2.5180
_cell_volume                     1840.42(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_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  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0951
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.977
_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    -46.00  96.00   1.00    5.50    --   24.86   0.00 120.00  142
  2  \w    -13.00  97.00   1.00    5.50    --   24.86  19.00-120.00  110
  3  \w     -4.00  42.00   1.00    5.50    --   24.86  77.00   0.00   46
  4  \w    -46.00  47.00   1.00    5.50    --   24.86 -38.00  60.00   93
  5  \w     -4.00  42.00   1.00    5.50    --   24.86  77.00  60.00   46
  6  \w     11.00  85.00   1.00    5.50    --   24.86-133.00  44.34   74
  7  \w    -44.00  43.00   1.00    5.50    --   24.86 -57.00 -90.00   87
  8  \w     -4.00  42.00   1.00    5.50    --   24.86  77.00-120.00   46
  9  \w      6.00  93.00   1.00    5.50    --   24.86  57.00 -60.00   87
 10  \w      9.00  84.00   1.00    5.50    --   24.86-132.00 140.29   75
 11  \w      6.00  93.00   1.00    5.50    --   24.86  57.00 150.00   87
 12  \w     -1.00  75.00   1.00    5.50    --   24.86-117.00-135.17   76
 13  \w    -95.00  48.00   1.00    5.50    --  -23.50   0.00 -90.00  143
 14  \w    -95.00  48.00   1.00    5.50    --  -23.50   0.00-120.00  143
 15  \w    -97.00 -39.00   1.00    5.50    --  -23.50-178.00 -90.00   58
 16  \w    -95.00  48.00   1.00    5.50    --  -23.50   0.00 -60.00  143
 17  \w    -95.00  48.00   1.00    5.50    --  -23.50   0.00-180.00  143
 18  \w    -95.00  48.00   1.00    5.50    --  -23.50   0.00-150.00  143
 19  \w    -15.00  65.00   1.00    5.50    --   24.86 -99.00 -90.00   80
 20  \w    -43.00  44.00   1.00    5.50    --   24.86 -60.00 139.00   87
 21  \w      6.00  93.00   1.00    5.50    --   24.86  57.00-120.00   87
 22  \w     -4.00  42.00   1.00    5.50    --   24.86  77.00 120.00   46
 23  \w    -95.00  48.00   1.00    5.50    --  -23.50   0.00   0.00  143
 24  \w    -95.00 -37.00   1.00    5.50    --  -23.50   0.00  30.00   58
 25  \w    -95.00  48.00   1.00    5.50    --  -23.50   0.00 -30.00  143
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0547444000
_diffrn_orient_matrix_UB_12      -0.0330089000
_diffrn_orient_matrix_UB_13      0.0178677000
_diffrn_orient_matrix_UB_21      0.0175117000
_diffrn_orient_matrix_UB_22      0.0759003000
_diffrn_orient_matrix_UB_23      0.0099922000
_diffrn_orient_matrix_UB_31      -0.0571633000
_diffrn_orient_matrix_UB_32      -0.0083527000
_diffrn_orient_matrix_UB_33      0.0201897000
_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  0.0413
_diffrn_reflns_av_unetI/netI     0.0188
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            103347
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.145
_diffrn_reflns_theta_min         1.651
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.761
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.649
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
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    2.106
_exptl_crystal_description       block
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.923
_refine_diff_density_min         -0.432
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details
;
 Flack x determined using 2584 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.033(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         6225
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0248
_refine_ls_R_factor_gt           0.0211
_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^)+(0.0164P)^2^+1.1194P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0428
_refine_ls_wR_factor_ref         0.0441
_reflns_Friedel_coverage         0.931
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.948
_reflns_number_gt                5800
_reflns_number_total             6225
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02268h3.cif
_cod_data_source_block           7
_cod_depositor_comments
'Adding full bibliography for 7717007--7717016.cif.'
_cod_database_code               7717012
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C16 H6 Cl F12 Sb'
_shelx_estimated_absorpt_t_max   0.766
_shelx_estimated_absorpt_t_min   0.667
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid body (RIGU) restrains
 C16, F10A, F11A, F12A, F10B, F11B, F12B, F10C, F11C, F12C
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.0005
3. Others
 1*[Sof(F10A)+Sof(F11A)+Sof(F12A)]+1*[Sof(F10B)+Sof(F11B)+Sof(F12B)]+1*
 [Sof(F10C)+Sof(F11C)+Sof(F12C)]=1 with esd of 0
 Sof(F10A)=Sof(F11A)=Sof(F12A)=FVAR(1)
 Sof(F10B)=Sof(F11B)=Sof(F12B)=FVAR(2)
 Sof(F10C)=Sof(F11C)=Sof(F12C)=FVAR(3)
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C10(H10), C12(H12), C14(H14)
;
_shelx_res_checksum              87602
_shelx_hkl_checksum              34918
_olex2_date_sample_data_collection 2020-02-25
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.206
_oxdiff_exptl_absorpt_empirical_full_min 0.883