One-Pot Cascade Transformations of Zinc Trifluorodiazoethylide and α,β-Unsaturated Enones: Access to Trifluoromethylated Polycyclic Pyrazolines.
Qin, Shuang; Zheng, Yan; Zhang, Fa-Guang; Ma, Jun-An; Organic letters 19 (2017) 3406–3409; doi:10.1021/acs.orglett.7b01362

data_1547098
_publ_section_title
;
 One-Pot Cascade Transformations of Zinc Trifluorodiazoethylide and
 \a,\b-Unsaturated Enones: Access to Trifluoromethylated Polycyclic
 Pyrazolines.
;
_journal_issue                   13
_journal_name_full               'Organic letters'
_journal_page_first              3406
_journal_page_last               3409
_journal_paper_doi               10.1021/acs.orglett.7b01362
_journal_volume                  19
_journal_year                    2017
_chemical_formula_sum            'C32 H25 F3 N2 O2'
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_symmetry_space_group_name_Hall  '-C 2yc'
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_atom_sites_solution_hydrogens   geom
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_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 124.0250(10)
_cell_angle_gamma                90.00
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_cell_length_a                   27.948(3)
_cell_length_b                   10.7810(12)
_cell_length_c                   21.830(2)
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_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.98
_cell_measurement_theta_min      2.59
_cell_volume                     5451.4(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
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_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
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_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
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_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            COLORLESS
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_density_meas      ?
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_exptl_crystal_description       BLOCK
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_exptl_crystal_size_max          0.32
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_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
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_refine_ls_R_factor_all          0.0889
_refine_ls_R_factor_gt           0.0616
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0896P)^2^+4.0526P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1727
_refine_ls_wR_factor_ref         0.1963
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_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol7b01362_si_004.cif
_cod_data_source_block           160320a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/home/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

'_exptl_absorpt_correction_type' value 'MULTI-SCAN' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

'_exptl_crystal_density_meas' value 'NONE' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        5451.5(10)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               1547098