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_1544698
_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            'C23 H26 N2 O4 S'
_chemical_formula_weight         426.52
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.27(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.7498(17)
_cell_length_b                   12.278(3)
_cell_length_c                   20.161(4)
_cell_measurement_reflns_used    17537
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      54.93
_cell_measurement_theta_min      6.16
_cell_volume                     2131.2(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0240
_diffrn_reflns_av_sigmaI/netI    0.0199
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            19982
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         3.21
_exptl_absorpt_coefficient_mu    0.184
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             904
_refine_diff_density_max         0.266
_refine_diff_density_min         -0.273
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       0.0085(14)
_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   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         4865
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0388
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0731P)^2^+0.3821P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1184
_refine_ls_wR_factor_ref         0.1213
_reflns_number_gt                4357
_reflns_number_total             4865
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol6b02710_si_003.cif
_cod_data_source_block           zj
_cod_depositor_comments
'Adding full bibliography for 1544698--1544700.cif.'
_cod_original_cell_volume        2131.2(7)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               1544698