Metal-free oxidative cyclization of urea-tethered alkenes with hypervalent iodine.
Cochran, Brian M.; Michael, Forrest E.; Organic letters 10 (2008) 5039–5042; doi:10.1021/ol8022165

data_1504952
_publ_section_title
;
 Metal-free oxidative cyclization of urea-tethered alkenes with
 hypervalent iodine.
;
_journal_issue                   21
_journal_name_full               'Organic letters'
_journal_page_first              5039
_journal_page_last               5042
_journal_paper_doi               10.1021/ol8022165
_journal_volume                  10
_journal_year                    2008
_chemical_formula_moiety         'C15 H20 N2 O3 S'
_chemical_formula_sum            'C15 H20 N2 O3 S'
_chemical_formula_weight         308.39
_chemical_name_common            BMC-M-63-2
_chemical_name_systematic
; 
 BMC-M-63-2 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                90.000
_cell_angle_beta                 111.272(3)
_cell_angle_gamma                90.000
_cell_formula_units_Z            4
_cell_length_a                   11.0729(6)
_cell_length_b                   11.8754(7)
_cell_length_c                   12.2070(8)
_cell_measurement_reflns_used    62
_cell_measurement_temperature    130(2)
_cell_volume                     1495.80(16)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       KappaCCD
_computing_data_reduction        'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'maXus, Zortep'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w 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  0.0960
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_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11080
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.42
_diffrn_reflns_theta_min         2.48
_exptl_absorpt_coefficient_mu    0.228
_exptl_absorpt_correction_T_max  0.9347
_exptl_absorpt_correction_T_min  0.8944
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   HKL2000
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cut-block
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.423
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_refine_ls_number_reflns         3587
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_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0866
_refine_ls_R_factor_gt           0.0592
_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^)+(0.0980P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1561
_refine_ls_wR_factor_ref         0.1712
_reflns_number_gt                2528
_reflns_number_total             3587
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol8022165_si_002.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1495.76(15)
_cod_original_sg_symbol_Hall     -p_2ybc
_cod_original_sg_symbol_H-M      p_1_21/c_1
_cod_database_code               1504952