Establishing the Role of Triflate Anions in H2 Activation by a Cationic Triorganotin(IV) Lewis Acid
Sapsford, Joshua S.; Csókás, Dániel; Scott, Daniel J.; Turnell-Ritson, Roland C.; Piascik, Adam D.; Pápai, Imre; Ashley, Andrew E.; ACS Catalysis  (2020) 7573–7583; doi:10.1021/acscatal.0c02023

data_4517813
_publ_section_title
;
 Establishing the Role of Triflate Anions in H2 Activation by a Cationic
 Triorganotin(IV) Lewis Acid
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              7573
_journal_page_last               7583
_journal_paper_doi               10.1021/acscatal.0c02023
_journal_year                    2020
_chemical_formula_moiety         'C17 H34 F3 N O3 S Sn'
_chemical_formula_sum            'C17 H34 F3 N O3 S Sn'
_chemical_formula_weight         508.20
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2020-01-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 92.744(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7228(2)
_cell_length_b                   15.7107(4)
_cell_length_c                   14.3340(3)
_cell_measurement_reflns_used    3016
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      27.8800
_cell_measurement_theta_min      2.8010
_cell_volume                     2187.04(9)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0382
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.811
_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    -56.00  23.00   1.00    3.05    --   14.27 -19.00-180.00   79
  2  \w    -50.00  39.00   1.00    3.05    --   14.27 -19.00 -90.00   89
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0422233000
_diffrn_orient_matrix_UB_12      -0.0331623000
_diffrn_orient_matrix_UB_13      -0.0189275000
_diffrn_orient_matrix_UB_21      0.0563281000
_diffrn_orient_matrix_UB_22      -0.0158471000
_diffrn_orient_matrix_UB_23      -0.0244457000
_diffrn_orient_matrix_UB_31      0.0194284000
_diffrn_orient_matrix_UB_32      -0.0262231000
_diffrn_orient_matrix_UB_33      0.0387139000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.811
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7879
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.811
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.278
_diffrn_reflns_theta_min         2.466
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.304
_exptl_absorpt_correction_T_max  0.963
_exptl_absorpt_correction_T_min  0.928
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_description       block
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.312
_exptl_crystal_size_mid          0.282
_exptl_crystal_size_min          0.164
_refine_diff_density_max         0.459
_refine_diff_density_min         -0.653
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         4397
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0306
_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^)+(0.0217P)^2^+0.8370P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0598
_refine_ls_wR_factor_ref         0.0653
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3551
_reflns_number_total             4397
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs0c02023_si_002.cif
_cod_data_source_block           ash1911
_cod_depositor_comments
;Adding full bibliography for 4517813--4517814.cif.

 Adding full bibliography for 4517813--4517814.cif.
;
_cod_original_cell_volume        2187.03(9)
_cod_database_code               4517813
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C17 H34 F3 N O3 S Sn'
_chemical_oxdiff_usercomment     JS515(DFB/C5)
_reflns_odcompleteness_completeness 98.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_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 Ternary CH refined with riding coordinates:
 C3(H3), C16(H16), C1(H1), C2(H2)
2.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C12(H12A,H12B), C11(H11A,H11B), C15(H15A,H15B), C14(H14A,
 H14B), C13(H13A,H13B)
2.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C9(H9A,H9B,H9C), C6(H6A,H6B,H6C), C8(H8A,
 H8B,H8C), C7(H7A,H7B,H7C)
;
_shelx_res_checksum              1300
_shelx_hkl_checksum              23143
_olex2_date_sample_data_collection 2019-06-18
_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 1.149
_oxdiff_exptl_absorpt_empirical_full_min 0.915