Gold(i)-catalyzed cycloisomerization of vinylidenecyclopropane-enes via carbene or non-carbene processes
Li, De-Yao; Wei, Yin; Marek, Ilan; Tang, Xiang-Ying; Shi, Min; Chem. Sci. 6 (2015) 5519–; doi:10.1039/C5SC01806D

data_1520661
_publ_section_title
;
 Gold(i)-catalyzed cycloisomerization of vinylidenecyclopropane-enes via
 carbene or non-carbene processes
;
_journal_issue                   10
_journal_name_full               'Chem. Sci.'
_journal_page_first              5519
_journal_paper_doi               10.1039/C5SC01806D
_journal_volume                  6
_journal_year                    2015
_chemical_formula_sum            'C20 H16 Br2 O'
_chemical_formula_weight         432.15
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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-97
_audit_update_record
;
2014-01-08 deposited with the CCDC.
2015-06-23 downloaded from the CCDC.
;
_cell_angle_alpha                84.231(5)
_cell_angle_beta                 84.177(5)
_cell_angle_gamma                89.834(5)
_cell_formula_units_Z            4
_cell_length_a                   7.1574(15)
_cell_length_b                   11.250(2)
_cell_length_c                   22.434(5)
_cell_measurement_reflns_used    2079
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      40.883
_cell_measurement_theta_min      4.901
_cell_volume                     1787.9(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_av_sigmaI/netI    0.0912
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            10743
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         0.92
_exptl_absorpt_coefficient_mu    4.536
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.11579
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.186
_exptl_crystal_size_mid          0.145
_exptl_crystal_size_min          0.121
_refine_diff_density_max         1.180
_refine_diff_density_min         -0.621
_refine_diff_density_rms         0.136
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         6983
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1242
_refine_ls_R_factor_gt           0.0788
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1075P)^2^+5.6999P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2136
_refine_ls_wR_factor_ref         0.2416
_reflns_number_gt                4295
_reflns_number_total             6983
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5sc01806d2.cif
_cod_data_source_block           cd21401
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/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 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 1520661--1520664.cif.
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1520661