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_7717011
_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 O P Sb'
_chemical_formula_sum            'C12 H19 Cl F10 O P Sb'
_chemical_formula_weight         557.44
_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             2024-06-22
_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                 97.791(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.7947(3)
_cell_length_b                   17.4038(7)
_cell_length_c                   15.4407(6)
_cell_measurement_reflns_used    18122
_cell_measurement_temperature    173.0(1)
_cell_measurement_theta_max      29.4300
_cell_measurement_theta_min      3.6880
_cell_volume                     2075.31(14)
_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-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1773
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_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    -71.00 -46.00   1.00    4.00    --  -21.26 136.00-163.00   25
  2  \w    -56.00 -30.00   1.00    4.00    --  -21.26 133.00  18.00   26
  3  \w     47.00  80.00   1.00    4.00    --   21.42-133.00 -49.00   33
  4  \w     12.00  82.00   1.00    4.00    --   21.42-136.00 132.00   70
  5  \w    -73.00   4.00   1.00    4.00    --  -21.26 -57.00  30.00   77
  6  \w    -92.00  -1.00   1.00    4.00    --  -21.26 -38.00-150.00   91
  7  \w    -92.00  -1.00   1.00    4.00    --  -21.26 -38.00 120.00   91
  8  \w    -55.00  56.00   1.00    4.00    --  -21.26  19.00 -60.00  111
  9  \w    -91.00 -18.00   1.00    4.00    --  -21.26 149.00 -80.07   73
 10  \w    -92.00  -6.00   1.00    4.00    --  -21.26 -38.00 -60.00   86
 11  \w    -42.00   6.00   1.00    4.00    --  -21.26 -77.00 -60.00   48
 12  \w    -81.00 -11.00   1.00    4.00    --  -21.26 135.00  88.77   70
 13  \w     -6.00  42.00   1.00    4.00    --   21.42  77.00-150.00   48
;
_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      0.0157426000
_diffrn_orient_matrix_UB_12      0.0392598000
_diffrn_orient_matrix_UB_13      0.0105792000
_diffrn_orient_matrix_UB_21      0.0528527000
_diffrn_orient_matrix_UB_22      -0.0109132000
_diffrn_orient_matrix_UB_23      0.0391253000
_diffrn_orient_matrix_UB_31      0.0734265000
_diffrn_orient_matrix_UB_32      -0.0005555000
_diffrn_orient_matrix_UB_33      -0.0225494000
_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  0.0468
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            52993
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.034
_diffrn_reflns_theta_min         3.325
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.620
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.686
_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    1.784
_exptl_crystal_description       block
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.228
_exptl_crystal_size_mid          0.154
_exptl_crystal_size_min          0.132
_refine_diff_density_max         0.933
_refine_diff_density_min         -0.590
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         6055
_refine_ls_number_restraints     689
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0328
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0289P)^2^+1.9987P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0711
_refine_ls_wR_factor_ref         0.0809
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4754
_reflns_number_total             6055
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02268h3.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7717007--7717016.cif.'
_cod_database_code               7717011
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C12 H19 Cl F10 O Sb'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All P(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 P1-H1 \\sim P1B-H1B
 with sigma of 0.02
 H1B-O1 \\sim O1-H1
 with sigma of 0.02
 H1B-C9B \\sim C5-H1
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
P1 \\sim P1B \\sim F3 \\sim F4 \\sim F5 \\sim F6 \\sim F6B \\sim F7 \\sim F7B
\\sim F8 \\sim F8B \\sim F9B \\sim F10B \\sim F12 \\sim F13 \\sim C3 \\sim C3B
\\sim C4 \\sim C4B \\sim C5 \\sim C5B \\sim C6 \\sim C6B \\sim C7 \\sim C7B
\\sim C8 \\sim C8B \\sim C9 \\sim C9B \\sim C10 \\sim C10B \\sim C11 \\sim C11B
\\sim C12 \\sim C12B: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08 within 2A
4. Rigid body (RIGU) restrains
 P1, P1B, F3, F4, F5, F6, F6B, F7, F7B, F8, F8B, F9B, F10B, F12, F13, C3, C3B,
 C4, C4B, C5, C5B, C6, C6B, C7, C7B, C8, C8B, C9, C9B, C10, C10B, C11, C11B,
 C12, C12B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(P1B)=Sof(H1B)=Sof(F6B)=Sof(F7B)=Sof(F8B)=Sof(F9B)=Sof(F10B)=Sof(C3B)=
 Sof(C4B)=Sof(C5B)=Sof(C6B)=Sof(H6BA)=Sof(H6BB)=Sof(H6BC)=Sof(C7B)=Sof(H7BA)=
 Sof(H7BB)=Sof(H7BC)=Sof(C8B)=Sof(H8BA)=Sof(H8BB)=Sof(H8BC)=Sof(C9B)=Sof(C10B)=
 Sof(H10D)=Sof(H10E)=Sof(H10F)=Sof(C11B)=Sof(H11D)=Sof(H11E)=Sof(H11F)=
 Sof(C12B)=Sof(H12D)=Sof(H12E)=Sof(H12F)=1-FVAR(1)
 Sof(P1)=Sof(H1)=Sof(F6)=Sof(F7)=Sof(F8)=Sof(F12)=Sof(F13)=Sof(C3)=Sof(C4)=
 Sof(C5)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=
 Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C9)=Sof(C10)=Sof(H10A)=Sof(H10B)=
 Sof(H10C)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(C12)=Sof(H12A)=Sof(H12B)=
 Sof(H12C)=FVAR(1)
6.a Me refined with riding coordinates:
 C6B(H6BA,H6BB,H6BC), C7B(H7BA,H7BB,H7BC)
6.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C8B(H8BA,H8BB,H8BC),
 C10(H10A,H10B,H10C), C10B(H10D,H10E,H10F), C11(H11A,H11B,H11C), C11B(H11D,H11E,
 H11F), C12(H12A,H12B,H12C), C12B(H12D,H12E,H12F)
;
_shelx_res_checksum              86432
_shelx_hkl_checksum              75382
_olex2_date_sample_data_collection 2023-06-07
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.217
_oxdiff_exptl_absorpt_empirical_full_min 0.840