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_7717014
_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         'C4 H F10 Sb'
_chemical_formula_sum            'C4 H F10 Sb'
_chemical_formula_weight         360.796
_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             2024-06-22
_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                 106.470(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.5071(3)
_cell_length_b                   14.7672(5)
_cell_length_c                   9.8826(5)
_cell_measurement_reflns_used    17382
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      37.3050
_cell_measurement_theta_min      3.5880
_cell_volume                     910.67(7)
_computing_cell_refinement       'CrysAlisPro 1.171.43.127a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.127a 64-bit (release 16-06-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.127a (Rigaku OD, 2024)'
_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  'olex2.refine 1.5-alpha (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1773
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9970
_diffrn_measured_fraction_theta_max 0.9683
_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    -75.00 -16.00   1.00    4.00    --  -28.95 132.00 -47.00   59
  2  \w    -38.00 -12.00   1.00    4.00    --  -28.95 137.00 128.00   26
  3  \w     12.00  37.00   1.00    4.00    --   29.42-137.00  66.00   25
  4  \w     10.00  68.00   1.00    4.00    --   29.42-132.00-117.00   58
  5  \w   -105.00 -55.00   1.00    4.00    --  -28.95 156.00  29.40   50
  6  \w    -96.00 -13.00   1.00    4.00    --  -28.95 -38.00  90.00   83
  7  \w    -99.00  -2.00   1.00    4.00    --  -28.95 -57.00   0.00   97
  8  \w    -99.00  -2.00   1.00    4.00    --  -28.95 -57.00-120.00   97
  9  \w    -31.00  -6.00   1.00    4.00    --  -28.95 -38.00 -60.00   25
 10  \w    -66.00  49.00   1.00    4.00    --  -28.95  19.00 -30.00  115
 11  \w    -51.00  44.00   1.00    4.00    --  -28.95  38.00 120.00   95
 12  \w    -99.00 -16.00   1.00    4.00    --  -28.95 -57.00-180.00   83
 13  \w    -94.00 -48.00   1.00    4.00    --  -28.95 -38.00 -60.00   46
 14  \w    -95.00 -47.00   1.00    4.00    --  -28.95 143.00-141.46   48
 15  \w    -11.00  14.00   1.00    4.00    --   29.42 101.00 154.10   25
 16  \w    -12.00  13.00   1.00    4.00    --   29.42 104.00  45.00   25
;
_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      -0.1042938000
_diffrn_orient_matrix_UB_12      -0.0062608000
_diffrn_orient_matrix_UB_13      -0.0465505000
_diffrn_orient_matrix_UB_21      -0.0147684000
_diffrn_orient_matrix_UB_22      0.0475914000
_diffrn_orient_matrix_UB_23      -0.0046649000
_diffrn_orient_matrix_UB_31      0.0428335000
_diffrn_orient_matrix_UB_32      0.0011554000
_diffrn_orient_matrix_UB_33      -0.0584423000
_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  0.0373
_diffrn_reflns_av_unetI/netI     0.0176
_diffrn_reflns_Laue_measured_fraction_full 0.9970
_diffrn_reflns_Laue_measured_fraction_max 0.9683
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            35367
_diffrn_reflns_point_group_measured_fraction_full 0.9970
_diffrn_reflns_point_group_measured_fraction_max 0.9683
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         37.81
_diffrn_reflns_theta_min         3.36
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.154
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.187
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.127a (Rigaku Oxford Diffraction, 2024)
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    2.632
_exptl_crystal_description       cyllindrcally
_exptl_crystal_F_000             662.629
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.6235
_refine_diff_density_min         -0.3967
_refine_diff_density_rms         0.0976
_refine_ls_d_res_high            0.5797
_refine_ls_d_res_low             6.0604
_refine_ls_extinction_coef       0.0030(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0659
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    1
_refine_ls_number_parameters     221
_refine_ls_number_reflns         4738
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0659
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0227
_refine_ls_shift/su_max          0.0007
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0148P)^2^+0.3231P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0459
_refine_ls_wR_factor_ref         0.0485
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              7
_reflns_limit_h_min              -10
_reflns_limit_k_max              25
_reflns_limit_k_min              0
_reflns_limit_l_max              16
_reflns_limit_l_min              -7
_reflns_number_gt                4095
_reflns_number_total             4738
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4dt02268h3.cif
_cod_data_source_block           10
_cod_depositor_comments
'Adding full bibliography for 7717007--7717016.cif.'
_cod_database_code               7717014
_chemical_oxdiff_formula         C4HF10Sb
_olex2_refinement_description
;
1. Others
 Sof(F10B)=Sof(F6B)=Sof(F7B)=Sof(F9B)=Sof(F8B)=Sof(C4B)=1-FVAR(1)
 Sof(F10)=Sof(F6)=Sof(F7)=Sof(F9)=Sof(F8)=Sof(C4)=FVAR(1)
;
_olex2_refine_details
;
Refinement using NoSpherA2, an implementation of
NOn-SPHERical Atom-form-factors in Olex2.
Please cite:
F. Kleemiss et al. Chem. Sci. DOI 10.1039/D0SC05526C - 2021
NoSpherA2 implementation of HAR makes use of
tailor-made aspherical atomic form factors calculated
on-the-fly from a Hirshfeld-partitioned electron density (ED) - not from
spherical-atom form factors.

The ED is calculated from a gaussian basis set single determinant SCF
wavefunction - either Hartree-Fock or DFT using selected funtionals
 - for a fragment of the crystal.
This fragment can be embedded in an electrostatic crystal field by employing cluster charges
or modelled using implicit solvation models, depending on the software used.
The following options were used:
   SOFTWARE:       ORCA 5.0
   PARTITIONING:   NoSpherA2
   INT ACCURACY:   Normal
   METHOD:         R2SCAN
   BASIS SET:      x2c-TZVPP
   CHARGE:         0
   MULTIPLICITY:   1
   RELATIVISTIC:   DKH2
   DATE:           2024-06-21_19-18-44
;
_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 2.147
_oxdiff_exptl_absorpt_empirical_full_min 0.798