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_7708342
_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         'C8 H18 F6 O6 P2 S2 Sn'
_chemical_formula_sum            'C8 H18 F6 O6 P2 S2 Sn'
_chemical_formula_weight         568.97
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-09-24
_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                 110.338(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9043(3)
_cell_length_b                   10.9889(3)
_cell_length_c                   15.1867(6)
_cell_measurement_reflns_used    6426
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.5770
_cell_measurement_theta_min      2.5000
_cell_volume                     2019.28(11)
_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)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.801
_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    5.00    --   -8.40 -38.00 -60.00  240
  2  \w     -4.00  80.00   0.50    5.00    --   -8.40  57.00  60.00  168
;
_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      -0.0044429000
_diffrn_orient_matrix_UB_12      0.0467019000
_diffrn_orient_matrix_UB_13      0.0307218000
_diffrn_orient_matrix_UB_21      -0.0551855000
_diffrn_orient_matrix_UB_22      0.0113449000
_diffrn_orient_matrix_UB_23      -0.0298622000
_diffrn_orient_matrix_UB_31      -0.0193702000
_diffrn_orient_matrix_UB_32      -0.0430426000
_diffrn_orient_matrix_UB_33      0.0254361000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_av_unetI/netI     0.0625
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.801
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15141
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.801
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.802
_diffrn_reflns_theta_min         2.341
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.704
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65503
_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    1.872
_exptl_crystal_description       block
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.656
_refine_diff_density_min         -1.963
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         6008
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0372P)^2^+4.0158P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0975
_refine_ls_wR_factor_ref         0.1034
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4753
_reflns_number_total             6008
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02948g2.cif
_cod_data_source_block           rksnf2(pme3)2(otf)2
_cod_original_cell_volume        2019.27(11)
_cod_database_code               7708342
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'Sn F8 P2 C8 H6 S2 O6'
_shelx_estimated_absorpt_t_max   0.848
_shelx_estimated_absorpt_t_min   0.784
_diffrn_oxdiff_digest_frames
;
018cc715bc72f13a17798c366289b2a936000289208
;
_diffrn_oxdiff_digest_hkl
;
01c86c1ae617592f51d9807d68e73793da15b4
;
_reflns_odcompleteness_completeness 98.29
_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:
 C(HA,HB,HC), C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,
 H4C), C5(H5A,H5B,H5C)
;
_shelx_res_checksum              2153
_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 2.257
_oxdiff_exptl_absorpt_empirical_full_min 0.283