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_7708347
_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 H10 F4 N2 O2 Sn, C H2 Cl2'
_chemical_formula_sum            'C11 H12 Cl2 F4 N2 O2 Sn'
_chemical_formula_weight         469.82
_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
_audit_creation_date             2021-08-25
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-08-25 deposited with the CCDC.	2021-09-14 downloaded from the CCDC.
;
_cell_angle_alpha                90.899(3)
_cell_angle_beta                 103.213(3)
_cell_angle_gamma                101.930(3)
_cell_formula_units_Z            4
_cell_length_a                   9.4615(3)
_cell_length_b                   11.2482(3)
_cell_length_c                   15.4968(5)
_cell_measurement_reflns_used    9040
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.8050
_cell_measurement_theta_min      1.8410
_cell_volume                     1567.47(9)
_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 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_temperature      100.0
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.815
_diffrn_measured_fraction_theta_max 0.709
_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    -53.00  73.00   0.50    5.50    --  -16.60  60.00  30.00  252
  2  \w    -53.00  52.00   0.50    5.50    --  -16.60  60.00 150.00  210
  3  \w    -53.00  20.00   0.50    5.50    --  -16.60  60.00   0.00  146
  4  \w    -53.00  23.00   0.50    5.50    --  -16.60  60.00-150.00  152
  5  \w    -53.00  10.00   0.50    5.50    --  -16.60  60.00 -90.00  126
  6  \w    -51.00  29.00   0.50    5.50    --  -16.60  60.00 -60.00  160
  7  \w    -53.00  24.00   0.50    5.50    --  -16.60  60.00  90.00  154
  8  \w    -38.00 -11.00   0.50    5.50    --  -16.60 -60.00 -90.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0769
_diffrn_reflns_av_unetI/netI     0.0617
_diffrn_reflns_Laue_measured_fraction_full 0.815
_diffrn_reflns_Laue_measured_fraction_max 0.709
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            20963
_diffrn_reflns_point_group_measured_fraction_full 0.815
_diffrn_reflns_point_group_measured_fraction_max 0.709
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.854
_diffrn_reflns_theta_min         1.854
_exptl_absorpt_coefficient_mu    2.019
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78662
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.991
_exptl_crystal_description       block
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.268
_refine_diff_density_min         -2.092
_refine_diff_density_rms         0.204
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         7617
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0676
_refine_ls_R_factor_gt           0.0552
_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^)+(0.0967P)^2^+1.9456P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1555
_refine_ls_wR_factor_ref         0.1620
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6185
_reflns_number_total             7617
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.9218\% 
around [0.58 -0.58 0.58] (reciprocal) or [0.83 -0.40 0.40] (direct)
;
_cod_data_source_file            d1dt02948g2.cif
_cod_data_source_block           mw121120twins_twin1_hklf4
_cod_database_code               7708347
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.824
_shelx_estimated_absorpt_t_min   0.794
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C22(H22A,H22B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9),
 C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17),
  C18(H18), C19(H19), C20(H20)
;
_shelx_res_checksum              27970
_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
;