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_7708343
_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         'C7 H18 F6 O3 P2 S Sn'
_chemical_formula_sum            'C7 H18 F6 O3 P2 S Sn'
_chemical_formula_weight         476.90
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-01-05
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.4007(2)
_cell_length_b                   11.84650(10)
_cell_length_c                   23.9749(3)
_cell_measurement_reflns_used    43543
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.7230
_cell_measurement_theta_min      2.4710
_cell_volume                     3238.01(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (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 0.923
_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    1.29    --   -8.40 -38.00   0.00  240
  2  \w    -98.00  22.00   0.50    1.29    --   -8.40 -38.00 150.00  240
  3  \w    -98.00  22.00   0.50    1.29    --   -8.40 -60.00  90.00  240
  4  \w    -98.00  40.00   0.50    1.29    --   -8.40 -19.00  30.00  276
  5  \w    -98.00  21.00   0.50    1.29    --   -8.40 -57.00 -90.00  238
  6  \w    -39.00  76.00   0.50    1.29    --   -8.40  38.00 150.00  230
;
_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      0.0417951000
_diffrn_orient_matrix_UB_12      -0.0371831000
_diffrn_orient_matrix_UB_13      -0.0119982000
_diffrn_orient_matrix_UB_21      -0.0156904000
_diffrn_orient_matrix_UB_22      0.0193525000
_diffrn_orient_matrix_UB_23      -0.0269916000
_diffrn_orient_matrix_UB_31      0.0433117000
_diffrn_orient_matrix_UB_32      0.0427571000
_diffrn_orient_matrix_UB_33      0.0017598000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0788
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.923
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            85205
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.923
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.812
_diffrn_reflns_theta_min         2.465
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.967
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.33515
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
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    1.957
_exptl_crystal_description       block
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.825
_refine_diff_density_min         -1.035
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         5553
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0236
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0187P)^2^+2.9732P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0518
_refine_ls_wR_factor_ref         0.0546
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4864
_reflns_number_total             5553
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02948g2.cif
_cod_data_source_block           rksnf3(pme3)2otf
_cod_database_code               7708343
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'Sn F3 P2 C7 H9 O3 S3'
_chemical_oxdiff_usercomment     'colourless- giant crystal, part broken off'
_shelx_estimated_absorpt_t_max   0.943
_shelx_estimated_absorpt_t_min   0.891
_diffrn_oxdiff_digest_frames
;
01af7616e17f0abfcae28bb195f3e2409c000404aa8
;
_diffrn_oxdiff_digest_hkl
;
014501cfc4d0f0369d215cdad130fa4669700c
;
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.64
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C4(H4A,H4B,H4C), C2(H2A,H2B,H2C), C6(H6A,
 H6B,H6C), C3(H3A,H3B,H3C)
;
_shelx_res_checksum              88442
_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 3.154
_oxdiff_exptl_absorpt_empirical_full_min 0.502