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_7708348
_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         'C72 H60 F2 O4 P4 Sn, 2(C F3 O3 S)'
_chemical_formula_sum            'C74 H60 F8 O10 P4 S2 Sn'
_chemical_formula_weight         1567.91
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,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_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-19
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-08-23 deposited with the CCDC.	2021-09-14 downloaded from the CCDC.
;
_cell_angle_alpha                69.740(2)
_cell_angle_beta                 70.468(2)
_cell_angle_gamma                76.875(2)
_cell_formula_units_Z            2
_cell_length_a                   13.7031(3)
_cell_length_b                   15.6126(4)
_cell_length_c                   18.1412(4)
_cell_measurement_reflns_used    42760
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      31.2400
_cell_measurement_theta_min      3.5770
_cell_volume                     3404.20(15)
_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      100.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_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     -6.00  62.00   0.50    0.53    --   21.24  57.00  60.00  136
  2  \w     -6.00 104.00   0.50    0.53    --   21.24  39.00  93.00  220
  3  \w   -107.00 -16.00   0.50    0.53    --  -18.58 -19.00  60.00  182
  4  \w   -101.00   9.00   0.50    0.53    --  -18.58 -39.00 -60.00  220
  5  \w     -6.00  62.00   0.50    0.53    --   21.24  57.00-120.00  136
  6  \w    -67.00 -16.00   0.50    0.53    --   21.24 -19.00-180.00  102
  7  \w      0.00  65.00   0.50    0.53    --   21.24 -99.00-120.00  130
  8  \w      0.00  65.00   0.50    0.53    --   21.24 -99.00-150.00  130
  9  \w    -62.00  23.00   0.50    0.53    --   21.24 -39.00 -60.00  170
 10  \w     22.00  64.00   0.50    0.53    --  -18.58  19.00  30.00   84
 11  \w    -42.00  59.00   0.50    0.53    --  -18.58  57.00-180.00  202
 12  \w    -84.00 -19.00   0.50    0.53    --  -18.58 138.00 -40.63  130
 13  \w    -17.00  64.00   0.50    0.53    --  -18.58  39.00  93.00  162
 14  \w     22.00  54.00   0.50    0.53    --  -18.58  19.00  60.00   64
 15  \w    -34.00  -7.00   0.50    0.53    --   21.24 120.00 173.48   54
 16  \w    -36.00 -10.00   0.50    0.53    --   21.24 124.00 137.75   52
 17  \w    -35.00  -9.00   0.50    0.53    --   21.24 122.00 -14.71   52
 18  \w    -30.00  -3.00   0.50    0.53    --   21.24 114.00 -45.98   54
;
_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      0.0258446000
_diffrn_orient_matrix_UB_12      0.0148124000
_diffrn_orient_matrix_UB_13      0.0205516000
_diffrn_orient_matrix_UB_21      0.0321264000
_diffrn_orient_matrix_UB_22      -0.0429740000
_diffrn_orient_matrix_UB_23      0.0059660000
_diffrn_orient_matrix_UB_31      0.0369458000
_diffrn_orient_matrix_UB_32      0.0177984000
_diffrn_orient_matrix_UB_33      -0.0377712000
_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  0.0499
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            80126
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.700
_diffrn_reflns_theta_min         3.449
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.613
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86476
_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    1.530
_exptl_crystal_description       block
_exptl_crystal_F_000             1596
_exptl_crystal_recrystallization_method 'Slow evaporation'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.656
_refine_diff_density_min         -1.380
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     892
_refine_ls_number_reflns         17545
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_gt           0.0469
_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^)+(0.0557P)^2^+7.3862P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1160
_refine_ls_wR_factor_ref         0.1301
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13833
_reflns_number_total             17545
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02948g2.cif
_cod_data_source_block           2021dept_gr_mw98_1
_cod_database_code               7708348
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         SnF2O4P4C70H70C2F6O2S6
_shelx_estimated_absorpt_t_max   0.941
_shelx_estimated_absorpt_t_min   0.887
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.64
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C38(H38), C14(H14), C23(H23), C72(H72), C10(H10), C48(H48), C44(H44),
 C25(H25), C47(H47), C58(H58), C40(H40), C50(H50), C2(H2), C60(H60), C68(H68),
 C6(H6), C69(H69), C21(H21), C8(H8), C71(H71), C39(H39), C54(H54), C19(H19),
 C27(H27), C56(H56), C11(H11), C12(H12), C31(H31), C36(H36), C46(H46), C16(H16),
  C22(H22), C70(H70), C53(H53), C65(H65), C26(H26), C52(H52), C5(H5), C45(H45),
 C15(H15), C4(H4), C59(H59), C51(H51), C20(H20), C42(H42), C57(H57), C17(H17),
 C41(H41), C64(H64), C28(H28), C3(H3), C35(H35), C66(H66), C9(H9), C34(H34),
 C29(H29), C63(H63), C33(H33), C32(H32), C62(H62)
;
_shelx_res_checksum              45720
_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 2.050
_oxdiff_exptl_absorpt_empirical_full_min 0.592