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_4517814
_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         'C16 H34 N Sn, Al C16 F36 O4'
_chemical_formula_sum            'C32 H34 Al F36 N O4 Sn'
_chemical_formula_weight         1326.27
_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     iterative
_audit_creation_date             2018-09-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 104.671(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.8706(5)
_cell_length_b                   15.2083(4)
_cell_length_c                   21.9762(6)
_cell_measurement_reflns_used    3840
_cell_measurement_temperature    173.00(14)
_cell_measurement_theta_max      24.9020
_cell_measurement_theta_min      2.4070
_cell_volume                     4808.0(3)
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0382
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.804
_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    -54.00  32.00   1.00   39.67    --   14.27 -37.00   0.00   86
  2  \w     -4.00  84.00   1.00   39.67    --   14.27  37.00-180.00   88
;
_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      0.0177932000
_diffrn_orient_matrix_UB_12      0.0321841000
_diffrn_orient_matrix_UB_13      0.0232976000
_diffrn_orient_matrix_UB_21      0.0386508000
_diffrn_orient_matrix_UB_22      -0.0274577000
_diffrn_orient_matrix_UB_23      0.0129479000
_diffrn_orient_matrix_UB_31      0.0248944000
_diffrn_orient_matrix_UB_32      0.0196731000
_diffrn_orient_matrix_UB_33      -0.0200515000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0272
_diffrn_reflns_av_unetI/netI     0.0556
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.804
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17837
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.804
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.298
_diffrn_reflns_theta_min         2.469
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.726
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.804
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.832
_exptl_crystal_description       plate
_exptl_crystal_F_000             2608
_exptl_crystal_size_max          0.464
_exptl_crystal_size_mid          0.263
_exptl_crystal_size_min          0.054
_refine_diff_density_max         2.046
_refine_diff_density_min         -1.446
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     682
_refine_ls_number_reflns         9605
_refine_ls_number_restraints     216
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1081
_refine_ls_R_factor_gt           0.0701
_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^)+(0.0988P)^2^+13.8844P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1745
_refine_ls_wR_factor_ref         0.2016
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6525
_reflns_number_total             9605
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs0c02023_si_003.cif
_cod_data_source_block           ash1731
_cod_depositor_comments
;Adding full bibliography for 4517813--4517814.cif.

 Adding full bibliography for 4517813--4517814.cif.
;
_cod_database_code               4517814
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C32 H34 Al F36 N O4 Sn'
_chemical_oxdiff_usercomment     JS257
_reflns_odcompleteness_completeness 98.75
_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. Uiso/Uaniso restraints and constraints
Uanis(F34) \\sim Ueq, Uanis(F35) \\sim Ueq, Uanis(F14) \\sim Ueq, Uanis(F10)
\\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(F32) \\sim Ueq, Uanis(F12) \\sim Ueq,
Uanis(F30) \\sim Ueq, Uanis(F29) \\sim Ueq, Uanis(F23) \\sim Ueq, Uanis(F24)
\\sim Ueq, Uanis(F20) \\sim Ueq, Uanis(F27) \\sim Ueq, Uanis(F15) \\sim Ueq,
Uanis(F5) \\sim Ueq, Uanis(F25) \\sim Ueq, Uanis(F19) \\sim Ueq, Uanis(F31)
\\sim Ueq, Uanis(F36) \\sim Ueq, Uanis(F26) \\sim Ueq, Uanis(F1) \\sim Ueq,
Uanis(F9) \\sim Ueq, Uanis(F28) \\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F18)
\\sim Ueq, Uanis(F13) \\sim Ueq, Uanis(F17) \\sim Ueq, Uanis(F7) \\sim Ueq,
Uanis(F2) \\sim Ueq, Uanis(F11) \\sim Ueq, Uanis(F16) \\sim Ueq, Uanis(F33)
\\sim Ueq, Uanis(F22) \\sim Ueq, Uanis(F21) \\sim Ueq, Uanis(F3) \\sim Ueq,
Uanis(F6) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
3.a Ternary CH refined with riding coordinates:
 C7(H7), C4(H4), C12(H12), C1(H1)
3.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C15(H15A,H15B), C14(H14A,H14B), C11(H11A,H11B), C10(H10A,
 H10B), C16(H16A,H16B)
3.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C6(H6A,H6B,H6C), C3(H3A,H3B,H3C), C8(H8A,H8B,H8C), C5(H5A,
 H5B,H5C), C2(H2A,H2B,H2C)
;
_shelx_res_checksum              64430
_shelx_hkl_checksum              79752
_olex2_date_sample_data_collection 2017-08-03
_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 1.116
_oxdiff_exptl_absorpt_empirical_full_min 0.909