Tin(IV) fluoride complexes with neutral phosphine coordination and comparisons with hard N- and O-donor ligands
King, Rhus P.; Woodward, Madeleine; Grigg, Julian; McRobbie, Graeme; Levason, William; Reid, Gillian; Dalton Transactions  (2021) –; doi:10.1039/D1DT02948G

data_7708344
_publ_section_title
;
 Tin(IV) fluoride complexes with neutral phosphine coordination and
 comparisons with hard N- and O-donor ligands
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02948G
_journal_year                    2021
_chemical_formula_moiety         'F5 Sn3, C F3 O3 S'
_chemical_formula_sum            'C F8 O3 S Sn3'
_chemical_formula_weight         600.14
_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_primary     dual
_audit_creation_date             2021-04-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-08-20 deposited with the CCDC.	2021-09-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.810(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.4971(4)
_cell_length_b                   7.6953(2)
_cell_length_c                   10.7894(3)
_cell_measurement_reflns_used    9501
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.7590
_cell_measurement_theta_min      3.0270
_cell_volume                     1110.24(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.893
_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    -98.00  22.00   0.50    2.00    --   -8.30 -60.00 -30.00  240
  2  \w    -98.00  22.00   0.50    2.00    --   -8.30 -60.00  90.00  240
  3  \w    -98.00  21.00   0.50    2.00    --   -8.30 -57.00-180.00  238
  4  \w    -39.00  81.00   0.50    2.00    --   -8.30  60.00-180.00  240
  5  \w    -98.00  81.00   0.50    2.00    --   -8.30   0.00 -60.00  358
  6  \w    -39.00  36.00   0.50    2.00    --   -8.30  60.00  30.00  150
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0452285000
_diffrn_orient_matrix_UB_12      0.0472734000
_diffrn_orient_matrix_UB_13      -0.0143938000
_diffrn_orient_matrix_UB_21      -0.0171040000
_diffrn_orient_matrix_UB_22      -0.0334389000
_diffrn_orient_matrix_UB_23      0.0545871000
_diffrn_orient_matrix_UB_31      0.0218260000
_diffrn_orient_matrix_UB_32      0.0717044000
_diffrn_orient_matrix_UB_33      0.0348662000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1220
_diffrn_reflns_av_unetI/netI     0.0675
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.893
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            29342
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.893
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.673
_diffrn_reflns_theta_min         3.047
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.983
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48604
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    3.590
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.383
_refine_diff_density_min         -1.454
_refine_diff_density_rms         0.277
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         3642
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0517
_refine_ls_R_factor_gt           0.0363
_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^)+3.3672P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0749
_refine_ls_wR_factor_ref         0.0797
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3014
_reflns_number_total             3642
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02948g2.cif
_cod_data_source_block           rksnf2(pme3)3(otf)
_cod_database_code               7708344
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'Sn F5 C10 P3 H27 S O36 F3'
_chemical_oxdiff_usercomment     'guessing at what it is'
_shelx_estimated_absorpt_t_max   0.542
_shelx_estimated_absorpt_t_min   0.542
_diffrn_oxdiff_digest_frames
;
010fda25b60988164cd2a1a07206067d1d000335e9f
;
_diffrn_oxdiff_digest_hkl
;
010236bafba24f4632aab004bde2a90a5f71bf
;
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.64
_olex2_refinement_description
;
;
_shelx_res_checksum              3205
_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 3.247
_oxdiff_exptl_absorpt_empirical_full_min 0.171