Electrophilic Reaction of 2,2,2-Trifluorodiazoethane with the in Situ Generated N-Heterocyclic Carbenes: Access to N-Aminoguanidines.
Guo, Ran; Zheng, Yan; Ma, Jun-An; Organic letters 18 (2016) 4170–4173; doi:10.1021/acs.orglett.6b01191

data_1543938
_publ_section_title
;
 Electrophilic Reaction of 2,2,2-Trifluorodiazoethane with the in Situ
 Generated N-Heterocyclic Carbenes: Access to N-Aminoguanidines.
;
_journal_issue                   17
_journal_name_full               'Organic letters'
_journal_page_first              4170
_journal_page_last               4173
_journal_paper_doi               10.1021/acs.orglett.6b01191
_journal_volume                  18
_journal_year                    2016
_chemical_formula_sum            'C32 H27 F3 N6 O2 S'
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_symmetry_cell_setting           monoclinic
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_atom_sites_solution_hydrogens   geom
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_cell_angle_alpha                90.00
_cell_angle_beta                 94.032(2)
_cell_angle_gamma                90.00
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_cell_length_a                   9.6443(14)
_cell_length_b                   11.0756(15)
_cell_length_c                   28.466(4)
_cell_measurement_reflns_used    5624
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.78
_cell_measurement_theta_min      2.64
_cell_volume                     3033.1(7)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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
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_exptl_absorpt_correction_T_max  0.9677
_exptl_absorpt_correction_T_min  0.9398
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            COLORLESS
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.38
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_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.410
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_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
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_refine_ls_number_reflns         9494
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_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0481
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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^)+(0.0748P)^2^+0.6586P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1234
_refine_ls_wR_factor_ref         0.1348
_reflns_number_gt                7799
_reflns_number_total             9494
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol6b01191_si_003.cif
_cod_data_source_block           150412a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/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.

'_exptl_absorpt_correction_type' value 'MULTI-SCAN' changed to
'multi-scan' according to
/usr/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.

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

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 1543936--1543938.cif.

2019-02-12
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_sg_symbol_H-M      P2(1)
_cod_original_formula_sum        'C64 H54 F6 N12 O4 S2'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     1233.31
_cod_database_code               1543938