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_7717009
_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         'C25 H17 F12 Sb'
_chemical_formula_sum            'C25 H17 F12 Sb'
_chemical_formula_weight         667.14
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2024-05-16
_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                 98.062(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.0987(4)
_cell_length_b                   16.0064(3)
_cell_length_c                   9.2650(2)
_cell_measurement_reflns_used    34980
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      34.7000
_cell_measurement_theta_min      3.4720
_cell_volume                     2510.66(9)
_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      100.0(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 0.967
_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    -25.00  30.00   1.00    2.00    --  -23.64  88.00 -42.00   55
  2  \w    -60.00 -33.00   1.00    2.00    --  -23.64  88.00 -42.00   27
  3  \w    -99.00 -25.00   1.00    2.00    --  -23.64 153.00 -42.96   74
  4  \w    -56.00  33.00   1.00    2.00    --  -23.64  77.00  90.00   89
  5  \w    -97.00   5.00   1.00    2.00    --  -23.64 -57.00 -60.00  102
  6  \w    -98.00  -5.00   1.00    2.00    --  -23.64 -38.00-180.00   93
  7  \w    -97.00   5.00   1.00    2.00    --  -23.64 -57.00  60.00  102
  8  \w    -55.00 -30.00   1.00    2.00    --  -23.64  77.00-150.00   25
  9  \w      5.00  35.00   1.00    2.00    --  -23.64  77.00-150.00   30
 10  \w     19.00  98.00   1.00    2.00    --   24.11  38.00-180.00   79
 11  \w     -8.00  42.00   1.00    2.00    --   24.11  77.00 -90.00   50
 12  \w    -13.00  64.00   1.00    2.00    --   24.11 -99.00 -60.00   77
 13  \w    -30.00  60.00   1.00    2.00    --   24.11 -88.00-158.00   90
;
_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      -0.0068129000
_diffrn_orient_matrix_UB_12      -0.0434636000
_diffrn_orient_matrix_UB_13      -0.0095833000
_diffrn_orient_matrix_UB_21      -0.0371077000
_diffrn_orient_matrix_UB_22      0.0044079000
_diffrn_orient_matrix_UB_23      0.0251660000
_diffrn_orient_matrix_UB_31      -0.0182214000
_diffrn_orient_matrix_UB_32      0.0072775000
_diffrn_orient_matrix_UB_33      -0.0725174000
_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  0.0433
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            77775
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.992
_diffrn_reflns_theta_min         3.293
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.201
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.575
_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    1.765
_exptl_crystal_description       block
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.283
_refine_diff_density_min         -0.701
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         10677
_refine_ls_number_restraints     111
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0316
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0270P)^2^+2.4943P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0672
_refine_ls_wR_factor_ref         0.0729
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8897
_reflns_number_total             10677
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02268h3.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 7717007--7717016.cif.'
_cod_database_code               7717009
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C25 H17 F12 Sb'
_shelx_estimated_absorpt_t_max   0.795
_shelx_estimated_absorpt_t_min   0.608
_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
 F11A-C25 \\sim F11B-C25
 with sigma of 0.02
 F10A-C25 \\sim F10B-C25
 with sigma of 0.02
 C25-F12A \\sim C25-F12B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
F10A \\sim F10B \\sim F11A \\sim F11B \\sim F12A \\sim F12B \\sim C25: within
2A with sigma of 0.05 and sigma for terminal atoms of 0.1 within 2A
4. Rigid body (RIGU) restrains
 F10A, F10B, F11A, F11B, F12A, F12B, C25
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Others
 Sof(F10B)=Sof(F11B)=Sof(F12B)=1-FVAR(1)
 Sof(F10A)=Sof(F11A)=Sof(F12A)=FVAR(1)
;
_shelx_res_checksum              51528
_shelx_hkl_checksum              67850
_olex2_date_sample_data_collection 2024-05-14
_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 1.248
_oxdiff_exptl_absorpt_empirical_full_min 0.844