DIPEA-Promoted Reaction of 2-Nitrochalcones with Elemental Sulfur: An Unusual Approach to 2-Benzoylbenzothiophenes.
Nguyen, Thanh Binh; Retailleau, Pascal; Organic letters 19 (2017) 4858–4860; doi:10.1021/acs.orglett.7b02321

data_1547551
_publ_section_title
;
 DIPEA-Promoted Reaction of 2-Nitrochalcones with Elemental Sulfur: An
 Unusual Approach to 2-Benzoylbenzothiophenes.
;
_journal_issue                   18
_journal_name_full               'Organic letters'
_journal_page_first              4858
_journal_page_last               4860
_journal_paper_doi               10.1021/acs.orglett.7b02321
_journal_volume                  19
_journal_year                    2017
_chemical_absolute_configuration ad
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_cell_angle_beta                 90
_cell_angle_gamma                90
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_cell_length_c                   13.7183(10)
_cell_measurement_reflns_used    4837
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.1
_cell_measurement_theta_min      3.2
_cell_volume                     1302.39(16)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)
;
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 RX
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device
;
Crystal Goniometer
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_diffrn_measurement_device_type
;
Rigaku RAXIS conversion
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           CuK\a
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_diffrn_reflns_av_R_equivalents  0.0503
_diffrn_reflns_av_unetI/netI     0.0591
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.988
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_diffrn_reflns_limit_h_min       -8
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_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
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_diffrn_reflns_point_group_measured_fraction_full 0.984
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_diffrn_reflns_theta_max         68.222
_diffrn_reflns_theta_min         4.763
_diffrn_source                   'Rotating Anode'
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_exptl_absorpt_correction_T_max  1.000
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_exptl_absorpt_process_details
;
 Reqab (Higashi, Rigaku 1998)
;
_exptl_crystal_colour            yellow
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_exptl_crystal_description       'thick stick'
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
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_refine_ls_abs_structure_details
;
 Flack x determined using 493 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.015(12)
_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         2339
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0544
_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^)+(0.0639P)^2^+0.1601P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1299
_refine_ls_wR_factor_ref         0.1469
_reflns_Friedel_coverage         0.701
_reflns_Friedel_fraction_full    0.978
_reflns_Friedel_fraction_max     0.975
_reflns_number_gt                1687
_reflns_number_total             2349
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol7b02321_si_002.cif
_cod_data_source_block           bn0707p
_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/current/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 
;
_cod_database_code               1547551
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              50977
_shelx_hkl_checksum              78841