Asymmetric Aza-Wacker-Type Cyclization of N-Ts Hydrazine-Tethered Tetrasubstituted Olefins: Synthesis of Pyrazolines Bearing One Quaternary or Two Vicinal Stereocenters.
Kou, Xuezhen; Shao, Qihang; Ye, Chenghao; Yang, Guoqiang; Zhang, Wanbin; Journal of the American Chemical Society 140 (2018) 7587–7597; doi:10.1021/jacs.8b02865

data_4132287
_publ_section_title
;
 Asymmetric Aza-Wacker-Type Cyclization of N-Ts Hydrazine-Tethered
 Tetrasubstituted Olefins: Synthesis of Pyrazolines Bearing One Quaternary
 or Two Vicinal Stereocenters.
;
_journal_issue                   24
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7587
_journal_page_last               7597
_journal_paper_doi               10.1021/jacs.8b02865
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C30 H32 N2 O3 S'
_chemical_formula_sum            'C30 H32 N2 O3 S'
_chemical_formula_weight         500.63
_space_group_crystal_system      monoclinic
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_atom_sites_solution_hydrogens   geom
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_cell_angle_alpha                90
_cell_angle_beta                 114.733(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.4195(13)
_cell_length_b                   6.1479(4)
_cell_length_c                   21.5093(12)
_cell_measurement_reflns_used    9934
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      68.16
_cell_measurement_theta_min      4.16
_cell_volume                     2812.8(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker D8 VENTURE CMOS photon 100'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_Laue_measured_fraction_full 0.990
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_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       7
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_diffrn_reflns_limit_l_max       25
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_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.987
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_diffrn_reflns_theta_max         68.360
_diffrn_reflns_theta_min         4.157
_exptl_absorpt_coefficient_mu    1.272
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.6430
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_description       block
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.250
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_refine_diff_density_max         0.279
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_refine_ls_extinction_method     none
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_refine_ls_number_reflns         5098
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_refine_ls_R_factor_all          0.0571
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_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1326
_refine_ls_wR_factor_ref         0.1403
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4049
_reflns_number_total             5098
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b02865_si_005.cif
_cod_data_source_block           a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'MULTI-SCAN' was
changed to 'multi-scan' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4132287
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.742
_shelx_estimated_absorpt_t_max   0.832
_shelx_res_checksum              5046
_shelx_hkl_checksum              49694