Palladium-Catalyzed [5 + 2] Cycloaddition of Vinyloxiranes with Sulfamate-Derived Cyclic Imines To Construct 1,3-Oxazepine Heterocycles.
Wu, Yang; Yuan, Chunhao; Wang, Chang; Mao, Biming; Jia, Hao; Gao, Xing; Liao, Jianning; Jiang, Feng; Zhou, Leijie; Wang, Qijun; Guo, Hongchao; Organic letters 19 (2017) 6268–6271; doi:10.1021/acs.orglett.7b02704

data_1548129
_publ_section_title
;
 Palladium-Catalyzed [5 + 2] Cycloaddition of Vinyloxiranes with
 Sulfamate-Derived Cyclic Imines To Construct 1,3-Oxazepine Heterocycles.
;
_journal_issue                   23
_journal_name_full               'Organic letters'
_journal_page_first              6268
_journal_page_last               6271
_journal_paper_doi               10.1021/acs.orglett.7b02704
_journal_volume                  19
_journal_year                    2017
_chemical_formula_moiety         'C18 H17 N O5 S'
_chemical_formula_sum            'C18 H17 N O5 S'
_chemical_formula_weight         359.38
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
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_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
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_cell_length_b                   11.1950(3)
_cell_length_c                   12.7835(3)
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_computing_cell_refinement       'CrysAlisPro 1.171.39.9d (Rigaku OD, 2015)'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
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_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_Laue_measured_fraction_full 0.999
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_diffrn_reflns_limit_l_min       -16
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_diffrn_reflns_point_group_measured_fraction_full 0.999
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_diffrn_reflns_theta_min         3.020
_diffrn_source                   'Sealed Tube'
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0506P)^2^+0.4524P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_refine_ls_wR_factor_ref         0.1207
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3132
_reflns_number_total             3766
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol7b02704_si_005.cif
_cod_data_source_block           sa5128a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/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 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 1548127--1548130.cif.
;
_cod_database_code               1548129
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C3(H3), C6(H6)
2.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C7(H7A,H7B)
2.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C17(H17)
2.d Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C)
;
_shelx_res_checksum              14063
_shelx_hkl_checksum              8056
_olex2_submission_special_instructions 'No special instructions were received'