Reactions of Persistent Carbenes with Hydrogen-Terminated Silicon Surfaces.
Zhukhovitskiy, Aleksandr V.; Mavros, Michael G.; Queeney, K. T.; Wu, Tony; Voorhis, Troy Van; Johnson, Jeremiah A.; Journal of the American Chemical Society 138 (2016) 8639–8652; doi:10.1021/jacs.6b04962

data_4125117
_publ_section_title
;
 Reactions of Persistent Carbenes with Hydrogen-Terminated Silicon
 Surfaces.
;
_journal_issue                   27
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8639
_journal_page_last               8652
_journal_paper_doi               10.1021/jacs.6b04962
_journal_volume                  138
_journal_year                    2016
_chemical_formula_sum            'C19 H29 F3 N2 O5 S'
_chemical_formula_weight         454.50
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                69.5328(15)
_cell_angle_beta                 88.0275(13)
_cell_angle_gamma                88.8565(13)
_cell_formula_units_Z            6
_cell_length_a                   12.6127(8)
_cell_length_b                   15.2311(10)
_cell_length_c                   17.9955(11)
_cell_measurement_reflns_used    9829
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.24
_cell_measurement_theta_min      2.34
_cell_volume                     3236.8(4)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2015)'
_computing_data_collection       'APEX2 v2011.4.0 (Bruker-AXS, 2015)'
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_computing_structure_solution    'SHELXS-2015 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Smart APEX2 CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0432
_diffrn_reflns_av_unetI/netI     0.0235
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            325213
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.576
_diffrn_reflns_theta_min         1.208
_diffrn_source
'I\mS micro-focus sealed tube, multilayer optics'
_exptl_absorpt_coefficient_mu    0.209
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.7198
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.165
_refine_diff_density_max         0.821
_refine_diff_density_min         -0.452
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1238
_refine_ls_number_reflns         23493
_refine_ls_number_restraints     3992
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0494P)^2^+1.1461P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1002
_refine_ls_wR_factor_ref         0.1081
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18870
_reflns_number_total             23493
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b04962_si_005.cif
_cod_data_source_block           X16076
_cod_depositor_comments
'Adding full bibliography for 4125116--4125119.cif.'
_cod_database_code               4125117
_shelx_estimated_absorpt_t_min   0.936
_shelx_estimated_absorpt_t_max   0.966
_shelxl_version_number           2014/6
_shelx_res_checksum              53328
_shelx_hkl_checksum              78429