Catalyst-free direct cross-dehydrogenative coupling of imidazoheterocycles with glyoxal hydrates: an efficient approach to 1,2-diketones.
Guo, Tao; Fu, Xiang-Heng; Zhang, Miao; Li, Yu-Liu; Ma, Yong-Cheng; Organic & biomolecular chemistry 17 (2019) 3150–3158; doi:10.1039/c9ob00095j

data_7156706
_publ_section_title
;
 Catalyst-free direct cross-dehydrogenative coupling of
 imidazoheterocycles with glyoxal hydrates: an efficient approach to
 1,2-diketones.
;
_journal_issue                   12
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              3150
_journal_page_last               3158
_journal_paper_doi               10.1039/c9ob00095j
_journal_volume                  17
_journal_year                    2019
_chemical_formula_sum            'C27 H19 N3 O'
_chemical_formula_weight         401.45
_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
_audit_update_record
;
2019-01-14 deposited with the CCDC.    2019-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                112.5430(10)
_cell_angle_beta                 94.2880(10)
_cell_angle_gamma                106.4650(10)
_cell_formula_units_Z            2
_cell_length_a                   9.8542(2)
_cell_length_b                   10.4047(2)
_cell_length_c                   11.6372(2)
_cell_measurement_reflns_used    9996
_cell_measurement_temperature    200.(2)
_cell_measurement_theta_max      68.5313
_cell_measurement_theta_min      4.7832
_cell_volume                     1033.89(4)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_collection       'Bruker Instrument Service vV6.2.6'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 833)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200.(2)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'D8 Venture PhotonII'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0403
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_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            27772
_diffrn_reflns_theta_full        69.00
_diffrn_reflns_theta_max         69.00
_diffrn_reflns_theta_min         4.78
_exptl_absorpt_coefficient_mu    0.631
_exptl_absorpt_correction_T_max  0.7531
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_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             420
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.169
_refine_diff_density_min         -0.232
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         3786
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0378
_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^)+(0.0583P)^2^+0.2113P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0992
_refine_ls_wR_factor_ref         0.1053
_reflns_number_gt                3317
_reflns_number_total             3786
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ob00095j2.cif
_cod_data_source_block           20180620GT
_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/RSC/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 7156706.cif.
;
_cod_database_code               7156706
_shelx_res_checksum              26953