Photosensitizer-free visible light-mediated gold-catalysed cis-difunctionalization of silyl-substituted alkynes
Wong, Man Kin; Deng, Jie-Ren; Chan, Wing-Cheung; Lai, Nathanael Chun-Him; Yang, Bin; Tsang, Chui-Shan; Ko, Ben, Chi-Bun; Chan, Sharon Lai-Fung; Chem. Sci.  (2017) –; doi:10.1039/C7SC02294H

data_1546941
_publ_section_title
;
 Photosensitizer-free visible light-mediated gold-catalysed
 cis-difunctionalization of silyl-substituted alkynes
;
_journal_name_full               'Chem. Sci.'
_journal_paper_doi               10.1039/C7SC02294H
_journal_year                    2017
_chemical_formula_moiety         'C27 H26 N O Si, B F4'
_chemical_formula_sum            'C27 H26 B F4 N O Si'
_chemical_formula_weight         495.39
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2017-04-21 deposited with the CCDC.
2017-09-01 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 92.186(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.6894(7)
_cell_length_b                   14.7175(11)
_cell_length_c                   17.3626(13)
_cell_measurement_reflns_used    9043
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      23.96
_cell_measurement_theta_min      2.37
_cell_volume                     2474.2(3)
_computing_cell_refinement       'Bruker APEX3'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.913
_diffrn_measured_fraction_theta_max 0.913
_diffrn_measurement_device_type  'D8_VENTURE PHOTON 100 CMOS area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'micro-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0837
_diffrn_reflns_av_sigmaI/netI    0.0453
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            118973
_diffrn_reflns_theta_full        27.41
_diffrn_reflns_theta_max         27.41
_diffrn_reflns_theta_min         2.37
_exptl_absorpt_coefficient_mu    0.146
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7110
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SAINT ver 8.34A; BRUKER SADABS'
_exptl_crystal_colour            gold
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PRISM
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.405
_refine_diff_density_min         -0.613
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         5151
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.1167
_refine_ls_R_factor_gt           0.0745
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0678P)^2^+4.0100P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1647
_refine_ls_wR_factor_ref         0.1865
_reflns_number_gt                3583
_reflns_number_total             5151
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7sc02294h2.cif
_cod_data_source_block           djr1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1546941