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_7708345
_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         'C41 H39 F4 P3 Sn'
_chemical_formula_sum            'C41 H39 F4 P3 Sn'
_chemical_formula_weight         819.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-01-06
_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                90.0
_cell_angle_beta                 98.7350(17)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   13.8624(2)
_cell_length_b                   12.9086(2)
_cell_length_c                   20.5379(4)
_cell_measurement_reflns_used    26108
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.6380
_cell_measurement_theta_min      2.0150
_cell_volume                     3632.51(11)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.874
_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    -82.00   3.00   0.50    1.43    --   -8.30 -60.00-150.00  170
  2  \w    -89.00  15.00   0.50    1.43    --   -8.30 -60.00 -30.00  208
  3  \w    -82.00 -56.00   0.50    1.43    --   -8.30 -60.00  60.00   52
  4  \w    -35.00  15.00   0.50    1.43    --   -8.30 -60.00  60.00  100
  5  \w    -98.00  81.00   0.50    1.43    --   -8.30   0.00-180.00  358
;
_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      0.0287527000
_diffrn_orient_matrix_UB_12      0.0052985000
_diffrn_orient_matrix_UB_13      0.0314913000
_diffrn_orient_matrix_UB_21      -0.0429385000
_diffrn_orient_matrix_UB_22      0.0076136000
_diffrn_orient_matrix_UB_23      0.0142946000
_diffrn_orient_matrix_UB_31      -0.0032135000
_diffrn_orient_matrix_UB_32      -0.0541276000
_diffrn_orient_matrix_UB_33      0.0050946000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.874
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            59518
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.874
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.720
_diffrn_reflns_theta_min         1.870
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.886
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86062
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    1.498
_exptl_crystal_description       needle
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.208
_refine_diff_density_min         -1.047
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         11707
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0303P)^2^+3.3764P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0724
_refine_ls_wR_factor_ref         0.0774
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9437
_reflns_number_total             11707
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02948g2.cif
_cod_data_source_block           rksnf4(triphos)-2
_cod_original_cell_volume        3632.50(11)
_cod_database_code               7708345
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'Sn F4 P3 C20 H20'
_chemical_oxdiff_usercomment
'colourless rod - needle crystals (from CHCl3/Hex)'
_cell_oxdiff_angle_alpha         89.9998(14)
_cell_oxdiff_angle_beta          98.7489(13)
_cell_oxdiff_angle_gamma         89.9874(14)
_cell_oxdiff_length_a            13.8607(2)
_cell_oxdiff_length_b            12.9159(2)
_cell_oxdiff_length_c            20.5295(3)
_cell_oxdiff_measurement_reflns_used 26108
_cell_oxdiff_volume              3632.50(10)
_shelx_estimated_absorpt_t_max   0.991
_shelx_estimated_absorpt_t_min   0.917
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.64
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C3(H3A,H3B), C4(H4A,H4B)
2.b Aromatic/amide H refined with riding coordinates:
 C41(H41), C37(H37), C35(H35), C34(H34), C22(H22), C7(H7), C23(H23), C38(H38),
 C40(H40), C11(H11), C8(H8), C39(H39), C9(H9), C10(H10), C17(H17), C29(H29),
 C25(H25), C21(H21), C33(H33), C31(H31), C19(H19), C15(H15), C16(H16), C13(H13),
  C27(H27), C28(H28), C26(H26), C20(H20), C14(H14), C32(H32)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_shelx_res_checksum              10462
_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 2.104
_oxdiff_exptl_absorpt_empirical_full_min 0.391