Catalytic Diazosulfonylation of Enynals toward Diazoindenes via Oxidative Radical-Triggered 5-exo-trig Carbocyclizations.
Hao, Wen-Juan; Du, Yan; Wang, Dan; Jiang, Bo; Gao, Qian; Tu, Shu-Jiang; Li, Guigen; Organic letters 18 (2016) 1884–1887; doi:10.1021/acs.orglett.6b00655

data_1542974
_publ_section_title
;
 Catalytic Diazosulfonylation of Enynals toward Diazoindenes via Oxidative
 Radical-Triggered 5-exo-trig Carbocyclizations.
;
_journal_issue                   8
_journal_name_full               'Organic letters'
_journal_page_first              1884
_journal_page_last               1887
_journal_paper_doi               10.1021/acs.orglett.6b00655
_journal_volume                  18
_journal_year                    2016
_chemical_formula_sum            'C44 H32 N2 O5 S'
_chemical_formula_weight         700.78
_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
_cell_angle_alpha                69.4930(10)
_cell_angle_beta                 75.670(2)
_cell_angle_gamma                69.3850(10)
_cell_formula_units_Z            2
_cell_length_a                   11.2207(8)
_cell_length_b                   11.9968(9)
_cell_length_c                   14.8113(12)
_cell_measurement_reflns_used    1187
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      21.21
_cell_measurement_theta_min      2.238
_cell_volume                     1730.2(2)
_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      298(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0344
_diffrn_reflns_av_sigmaI/netI    0.1059
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8917
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    0.146
_exptl_absorpt_correction_T_max  0.9827
_exptl_absorpt_correction_T_min  0.0679
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             732
_exptl_crystal_size_max          40.00
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.196
_refine_diff_density_min         -0.204
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.833
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         6035
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.833
_refine_ls_R_factor_all          0.1347
_refine_ls_R_factor_gt           0.0550
_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^)+(0.0440P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1056
_refine_ls_wR_factor_ref         0.1268
_reflns_number_gt                2651
_reflns_number_total             6035
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol6b00655_si_003.cif
_cod_data_source_block           150413j
_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/ACS/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 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 1542973--1542974.cif.
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1542974