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_7717016
_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         'C13 H11 F10 Sb'
_chemical_formula_sum            'C13 H11 F10 Sb'
_chemical_formula_weight         478.976
_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'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     dual
_audit_creation_date             2024-06-13
_audit_creation_method
;
Olex2 1.5-ac6-015
(compiled 2023.12.04 svn.r209d9fb2 for Rigaku Oxford Diffraction, GUI svn.r6873)
;
_audit_update_record
;
2024-07-03 deposited with the CCDC.	2024-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.686(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.8214(1)
_cell_length_b                   15.6118(2)
_cell_length_c                   11.6490(1)
_cell_measurement_reflns_used    77003
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      65.7680
_cell_measurement_theta_min      3.7000
_cell_volume                     1598.91(3)
_computing_cell_refinement       'CrysAlisPro 1.171.43.104a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.43.104a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.43.104a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac6-015 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac6-015 (Dolomanov et al., 2009)'
_computing_structure_refinement
'olex2.refine 1.5-ac6-015 (Bourhis et al., 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 0.9969
_diffrn_measured_fraction_theta_max 0.9982
_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    -78.00 -53.00   1.00    5.00    --  -42.43 139.00  99.00   25
  2  \w   -114.00 -77.00   1.00    5.00    --  -42.43-139.00  38.00   37
  3  \w   -100.00 -47.00   1.00    5.00    --  -42.43 131.00 -75.00   53
  4  \w     36.00  61.00   1.00    5.00    --   42.43-139.00  38.00   25
  5  \w     31.00  56.00   1.00    5.00    --   42.43-131.00-146.00   25
  6  \w     71.00 101.00   1.00    5.00    --   42.43 139.00  99.00   30
  7  \w     82.00 123.00   1.00   15.00    --   90.23-139.00  38.00   41
  8  \w     82.00 117.00   1.00   15.00    --   90.23-131.00-146.00   35
  9  \w    104.00 130.00   1.00   15.00    --   90.23 131.00 -75.00   26
 10  \w     99.00 125.00   1.00   15.00    --   90.23 139.00  99.00   26
 11  \w     14.00  78.00   1.00    5.00    --   42.43  57.00-150.00   64
 12  \w     12.00 115.00   1.00    5.00    --   42.43  69.00  92.89  103
 13  \w     14.00 115.00   1.00    5.00    --   42.43  57.00  60.00  101
 14  \w     15.00  54.00   1.00    5.00    --   42.43  57.00 -90.00   39
 15  \w     74.00 116.00   1.00    5.00    --   42.43  57.00 -90.00   42
 16  \w     12.00 115.00   1.00    5.00    --   42.43  70.00 -42.03  103
 17  \w     91.00 116.00   1.00    5.00    --   42.43  57.00-150.00   25
 18  \w     61.00  88.00   1.00   15.00    --   90.23  61.00  90.00   27
 19  \w    106.00 158.00   1.00   15.00    --   90.23  61.00 -90.00   52
 20  \w     61.00  87.00   1.00   15.00    --   90.23  61.00  30.00   26
 21  \w    108.00 157.00   1.00   15.00    --   90.23  61.00-180.00   49
 22  \w     61.00  87.00   1.00   15.00    --   90.23  61.00 150.00   26
 23  \w    105.00 154.00   1.00   15.00    --   90.23  61.00 150.00   49
 24  \w     61.00  95.00   1.00   15.00    --   90.23  61.00 -30.00   34
 25  \w     18.00 119.00   1.00   15.00    --   90.23 -61.00-180.00  101
 26  \w     21.00 106.00   1.00   15.00    --   90.23 -61.00   0.00   85
 27  \w     61.00  90.00   1.00   15.00    --   90.23  61.00 -90.00   29
 28  \w     61.00  86.00   1.00   15.00    --   90.23  61.00  60.00   25
 29  \w    105.00 157.00   1.00   15.00    --   90.23  61.00  60.00   52
 30  \w     61.00  94.00   1.00   15.00    --   90.23  61.00-120.00   33
 31  \w    108.00 158.00   1.00   15.00    --   90.23  61.00-120.00   50
 32  \w     61.00  87.00   1.00   15.00    --   90.23  61.00-180.00   26
 33  \w     19.00 112.00   1.00   15.00    --   90.23 -77.00 120.00   93
 34  \w     61.00 158.00   1.00   15.00    --   90.23  61.00   0.00   97
 35  \w     61.00  88.00   1.00   15.00    --   90.23  61.00 -60.00   27
 36  \w    111.00 157.00   1.00   15.00    --   90.23  61.00 -60.00   46
 37  \w     61.00  86.00   1.00   15.00    --   90.23  61.00 120.00   25
 38  \w    103.00 132.00   1.00   15.00    --   90.23  61.00 120.00   29
;
_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      0.0550922000
_diffrn_orient_matrix_UB_12      -0.0160310000
_diffrn_orient_matrix_UB_13      -0.0355404000
_diffrn_orient_matrix_UB_21      -0.0191061000
_diffrn_orient_matrix_UB_22      -0.0425081000
_diffrn_orient_matrix_UB_23      0.0148064000
_diffrn_orient_matrix_UB_31      -0.0557546000
_diffrn_orient_matrix_UB_32      -0.0012697000
_diffrn_orient_matrix_UB_33      -0.0474093000
_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  0.0471
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_Laue_measured_fraction_full 0.9969
_diffrn_reflns_Laue_measured_fraction_max 0.9982
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            182602
_diffrn_reflns_point_group_measured_fraction_full 0.9969
_diffrn_reflns_point_group_measured_fraction_max 0.9982
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         45.29
_diffrn_reflns_theta_min         3.29
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.824
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.207
_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    1.990
_exptl_crystal_description       block
_exptl_crystal_F_000             918.559
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.9973
_refine_diff_density_min         -0.7736
_refine_diff_density_rms         0.1165
_refine_ls_d_res_high            0.5000
_refine_ls_d_res_low             6.1947
_refine_ls_extinction_coef       0.0013(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0542
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     262
_refine_ls_number_reflns         13368
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0542
_refine_ls_R_factor_all          0.0250
_refine_ls_R_factor_gt           0.0223
_refine_ls_shift/su_max          -0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0250P)^2^+0.6850P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0555
_refine_ls_wR_factor_ref         0.0572
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              13
_reflns_limit_h_min              -17
_reflns_limit_k_max              31
_reflns_limit_k_min              0
_reflns_limit_l_max              23
_reflns_limit_l_min              -12
_reflns_number_gt                12391
_reflns_number_total             13368
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4dt02268h3.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7717007--7717016.cif.'
_cod_database_code               7717016
_chemical_oxdiff_formula         C13H11F10Sb
_olex2_refinement_description
;
;
_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 3.148
_oxdiff_exptl_absorpt_empirical_full_min 0.751