Controllable O-Nucleometalation Cyclization Strategy: Access to Divergent Ring-Functionalized Molecules.
Zheng, Jia; Li, Zun; Wu, Wanqing; Jiang, Huanfeng; Organic letters 18 (2016) 6232–6235; doi:10.1021/acs.orglett.6b02710

data_1544700
_publ_section_title
;
 Controllable O-Nucleometalation Cyclization Strategy: Access to Divergent
 Ring-Functionalized Molecules.
;
_journal_issue                   24
_journal_name_full               'Organic letters'
_journal_page_first              6232
_journal_page_last               6235
_journal_paper_doi               10.1021/acs.orglett.6b02710
_journal_volume                  18
_journal_year                    2016
_chemical_formula_sum            'C21 H22 N2 O4 S'
_chemical_formula_weight         398.47
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_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                70.74(3)
_cell_angle_beta                 73.72(3)
_cell_angle_gamma                67.38(3)
_cell_formula_units_Z            2
_cell_length_a                   8.3281(17)
_cell_length_b                   10.784(2)
_cell_length_c                   12.649(3)
_cell_measurement_reflns_used    4353
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      54.96
_cell_measurement_theta_min      6.10
_cell_volume                     974.5(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type  Rigaku
_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  0.0186
_diffrn_reflns_av_sigmaI/netI    0.0290
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5205
_diffrn_reflns_theta_full        24.00
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    0.196
_exptl_absorpt_correction_T_max  0.9806
_exptl_absorpt_correction_T_min  0.9618
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             420
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.422
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.111
_refine_ls_extinction_coef       0.009(6)
_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   1.148
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         2894
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0428
_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^)+(0.1190P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1331
_refine_ls_wR_factor_ref         0.1831
_reflns_number_gt                1960
_reflns_number_total             2894
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol6b02710_si_002.cif
_cod_data_source_block           zj
_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 1544698--1544700.cif.
;
_cod_original_cell_volume        974.5(3)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1544700