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_7708346
_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         'C10 F4 N2 Sn'
_chemical_formula_sum            'C10 F4 N2 Sn'
_chemical_formula_weight         342.81
_chemical_properties_physical    Hygroscopic
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_primary     dual
_audit_creation_date             2021-09-01
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-09-01 deposited with the CCDC.	2021-09-14 downloaded from the CCDC.
;
_cell_angle_alpha                117.933(5)
_cell_angle_beta                 91.612(4)
_cell_angle_gamma                109.045(5)
_cell_formula_units_Z            1
_cell_length_a                   6.3696(4)
_cell_length_b                   7.2222(4)
_cell_length_c                   7.2263(3)
_cell_measurement_reflns_used    5523
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.9530
_cell_measurement_theta_min      3.8250
_cell_volume                     271.02(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_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     -7.00 104.00   0.50    1.00    --   21.24  38.00  90.00  222
  2  \w     -6.00  62.00   0.50    1.00    --   21.24  57.00 -60.00  136
  3  \w     -6.00  62.00   0.50    1.00    --   21.24  57.00-120.00  136
  4  \w     22.00 104.00   0.50    1.00    --   21.24  19.00-150.00  164
  5  \w    -67.00 -16.00   0.50    1.00    --   21.24 -19.00 -60.00  102
  6  \w    -33.00  -6.00   0.50    1.00    --   21.24 118.00 156.56   54
  7  \w    -23.00   6.00   0.50    1.00    --   21.24 100.00  89.17   58
  8  \w    -62.00  22.00   0.50    1.00    --   21.24 -38.00  60.00  168
  9  \w      0.00  65.00   0.50    1.00    --   21.24 -99.00  60.00  130
 10  \w      0.00  65.00   0.50    1.00    --   21.24 -99.00-120.00  130
 11  \w    -56.00   9.00   0.50    1.00    --  -18.74 -57.00 -90.00  130
 12  \w   -106.00 -16.00   0.50    1.00    --  -18.74 -19.00 -90.00  180
 13  \w    -51.00  24.00   0.50    1.00    --  -18.74  77.00 -60.00  150
 14  \w     22.00  63.00   0.50    1.00    --  -18.74  19.00-180.00   82
 15  \w     22.00  63.00   0.50    1.00    --  -18.74  19.00-150.00   82
 16  \w     22.00  63.00   0.50    1.00    --  -18.74  19.00 -90.00   82
 17  \w     22.00  55.00   0.50    1.00    --  -18.74  19.00-120.00   66
 18  \w    -51.00  24.00   0.50    1.00    --  -18.74  77.00  90.00  150
 19  \w     22.00  63.00   0.50    1.00    --  -18.74  19.00 150.00   82
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0777091000
_diffrn_orient_matrix_UB_12      0.0958765000
_diffrn_orient_matrix_UB_13      -0.0004712000
_diffrn_orient_matrix_UB_21      0.0877863000
_diffrn_orient_matrix_UB_22      -0.0408767000
_diffrn_orient_matrix_UB_23      -0.0027245000
_diffrn_orient_matrix_UB_31      -0.0285822000
_diffrn_orient_matrix_UB_32      -0.0603017000
_diffrn_orient_matrix_UB_33      -0.1137692000
_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  0.0428
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            6755
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.682
_diffrn_reflns_theta_min         3.842
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.387
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85071
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.100
_exptl_crystal_description       plate
_exptl_crystal_F_000             160
_exptl_crystal_recrystallization_method 'Slow evaporation'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         7.559
_refine_diff_density_min         -1.776
_refine_diff_density_rms         0.431
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.182
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     79
_refine_ls_number_reflns         1396
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.182
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0671
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+16.5036P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2114
_refine_ls_wR_factor_ref         0.2115
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1392
_reflns_number_total             1396
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02948g2.cif
_cod_data_source_block           2021dept_gr_mw90_auto
_cod_database_code               7708346
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         SnF3C15H15N3CF3SO3
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.64
_olex2_refinement_description
;
;
_shelx_res_checksum              84221
_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 2.628
_oxdiff_exptl_absorpt_empirical_full_min 0.573