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_7717013
_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         'C24 H25 Cl F12 P S Sb'
_chemical_formula_sum            'C24 H25 Cl F12 P S Sb'
_chemical_formula_weight         761.67
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-07-07
_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                90
_cell_angle_beta                 113.50(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.351(4)
_cell_length_b                   20.7885(15)
_cell_length_c                   13.006(3)
_cell_measurement_reflns_used    51456
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      36.0400
_cell_measurement_theta_min      3.0860
_cell_volume                     3062.4(14)
_computing_cell_refinement       'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.94a (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      100.01(10)
_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 0.969
_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    -42.00   3.00   1.00    5.50    --  -27.30 -77.00-150.00   45
  2  \w    -42.00   3.00   1.00    5.50    --  -27.30 -77.00  30.00   45
  3  \w    -42.00   3.00   1.00    5.50    --  -27.30 -77.00 -60.00   45
  4  \w      7.00  98.00   1.00    5.50    --   27.30  38.00  90.00   91
  5  \w    -44.00  48.00   1.00    5.50    --   27.30 -38.00 -90.00   92
  6  \w     21.00 101.00   1.00    5.50    --   27.30-154.00  91.80   80
  7  \w      7.00  98.00   1.00    5.50    --   27.30  38.00 -90.00   91
  8  \w    -44.00  48.00   1.00    5.50    --   27.30 -38.00 150.00   92
  9  \w     39.00 111.00   1.00    5.50    --   27.30 178.00-150.00   72
 10  \w      2.00  96.00   1.00    5.50    --   27.30  57.00-180.00   94
 11  \w      7.00  98.00   1.00    5.50    --   27.30  38.00   0.00   91
 12  \w     20.00 100.00   1.00    5.50    --   27.30-153.00 -61.38   80
 13  \w    -42.00   3.00   1.00    5.50    --  -27.30 -77.00 120.00   45
 14  \w    -66.00 -30.00   1.00    5.50    --  -27.30 101.00 151.67   36
 15  \w    -94.00 -37.00   1.00    5.50    --  -27.30 145.00  67.15   57
 16  \w    -54.00  41.00   1.00    5.50    --  -27.30  62.00  48.50   95
 17  \w    -97.00 -39.00   1.00    5.50    --  -27.30 149.00 -91.97   58
 18  \w   -112.00 -58.00   1.00    5.50    --  -27.30 178.00  60.00   54
 19  \w     14.00  91.00   1.00    5.50    --   27.30-141.00 -13.03   77
 20  \w      9.00  85.00   1.00    5.50    --   27.30-132.00 124.04   76
;
_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      -0.0480063000
_diffrn_orient_matrix_UB_12      0.0130292000
_diffrn_orient_matrix_UB_13      -0.0463702000
_diffrn_orient_matrix_UB_21      0.0334138000
_diffrn_orient_matrix_UB_22      -0.0024088000
_diffrn_orient_matrix_UB_23      -0.0332891000
_diffrn_orient_matrix_UB_31      -0.0224034000
_diffrn_orient_matrix_UB_32      -0.0314645000
_diffrn_orient_matrix_UB_33      -0.0166418000
_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  0.0520
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            166717
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.990
_diffrn_reflns_theta_min         2.660
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.195
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.555
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.94a (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    1.652
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.890
_refine_diff_density_min         -0.742
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         15080
_refine_ls_number_restraints     473
_refine_ls_restrained_S_all      1.199
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0398
_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^)+(0.0240P)^2^+3.9846P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0833
_refine_ls_wR_factor_ref         0.0893
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12352
_reflns_number_total             15080
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02268h3.cif
_cod_data_source_block           9
_cod_depositor_comments
'Adding full bibliography for 7717007--7717016.cif.'
_cod_original_cell_volume        3062.6(14)
_cod_database_code               7717013
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C24 H25 Cl F12 P S Sb'
_shelx_estimated_absorpt_t_max   0.932
_shelx_estimated_absorpt_t_min   0.779
_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. Restrained distances
 F9B-C15 \\sim F7B-C15 \\sim F8B-C15 \\sim F9C-C15 \\sim F7C-C15 \\sim F8C-C15
\\sim F7A-C15 \\sim F8A-C15
 \\sim F9A-C15
 with sigma of 0.02
 F10-C16B \\sim F10-C16A \\sim F11A-C16A \\sim F11B-C16B \\sim F12A-C16A \\sim
F12B-C16B
 with sigma of 0.02
 F6-C8 \\sim F5A-C8 \\sim F5B-C8 \\sim F4A-C8 \\sim F4B-C8
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
F7A \\sim F8A \\sim F9A \\sim C15 \\sim F7B \\sim F7C \\sim F8B \\sim F8C \\sim
F9B \\sim F9C: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
F10 \\sim F11A \\sim F12A \\sim C16A \\sim F11B \\sim F12B \\sim C16B: within
2A with sigma of 0.001 and sigma for terminal atoms of 0.002 within 2A
F4A \\sim F5A \\sim F6 \\sim C8 \\sim F4B \\sim F5B: within 2A with sigma of
0.001 and sigma for terminal atoms of 0.002 within 2A
Uanis(C16B) = Uanis(C16A)
4. Rigid body (RIGU) restrains
 F7A, F8A, F9A, C15, F7B, F7C, F8B, F8C, F9B, F9C
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 F10, F11A, F12A, C16A, F11B, F12B, C16B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 F4A, F5A, F6, C8, F4B, F5B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 1*[Sof(F7B)+Sof(F8B)+Sof(F9B)]+1*[Sof(F7C)+Sof(F8C)+Sof(F9C)]+1*[Sof(F7A)+
 Sof(F8A)+Sof(F9A)]=1 with esd of 0
 Sof(F4B)=Sof(F5B)=1-FVAR(1)
 Sof(F4A)=Sof(F5A)=FVAR(1)
 Sof(F7B)=Sof(F8B)=Sof(F9B)=FVAR(2)
 Sof(F7C)=Sof(F8C)=Sof(F9C)=FVAR(3)
 Sof(F7A)=Sof(F8A)=Sof(F9A)=FVAR(4)
 Sof(F11B)=Sof(F12B)=Sof(C16B)=1-FVAR(5)
 Sof(F11A)=Sof(F12A)=Sof(C16A)=FVAR(5)
6.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C10(H10), C12(H12), C14(H14)
6.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              33025
_shelx_hkl_checksum              26803
_olex2_date_sample_data_collection 2023-07-07
_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 1.217
_oxdiff_exptl_absorpt_empirical_full_min 0.876