Sulfur-Promoted DABCO-Catalyzed Oxidative Trimerization of Phenylacetonitriles.
Nguyen, Thanh Binh; Retailleau, Pascal; The Journal of organic chemistry 84 (2019) 5907–5912; doi:10.1021/acs.joc.9b00408

data_4034364
_publ_section_title
;
 Sulfur-Promoted DABCO-Catalyzed Oxidative Trimerization of
 Phenylacetonitriles.
;
_journal_issue                   9
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              5907
_journal_page_last               5912
_journal_paper_doi               10.1021/acs.joc.9b00408
_journal_volume                  84
_journal_year                    2019
_chemical_formula_moiety         'C24 H17 N3'
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_atom_sites_solution_hydrogens   mixed
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_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 109.472(8)
_cell_angle_gamma                90
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_cell_length_c                   9.3154(7)
_cell_measurement_reflns_used    8459
_cell_measurement_temperature    293(2)
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_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-2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Rigaku Rapid2 IP'
_diffrn_detector_area_resol_mean 10.0000
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_diffrn_measured_fraction_theta_max 0.968
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;
Crystal Goniometer Chi-partial
;
_diffrn_measurement_device_type
;
Rigaku Spider mm007HF Rapid2
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_radiation_monochromator  'OSMIC CMF Confocal'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_av_unetI/netI     0.0416
_diffrn_reflns_Laue_measured_fraction_full 0.970
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_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       10
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_diffrn_reflns_point_group_measured_fraction_max 0.793
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         68.230
_diffrn_reflns_theta_min         3.806
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    0.567
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_exptl_absorpt_correction_T_min  0.841
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Reqab (Higashi-Rigaku, 1998))'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_description       needle
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.228
_refine_diff_density_min         -0.229
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details
;
 Flack x determined using 1119 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.4(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_hydrogen_treatment    mixed
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_refine_ls_number_reflns         5504
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.149
_refine_ls_R_factor_all          0.1005
_refine_ls_R_factor_gt           0.0411
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0365P)^2^+0.9945P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0857
_refine_ls_wR_factor_ref         0.1371
_reflns_Friedel_coverage         0.596
_reflns_Friedel_fraction_full    0.615
_reflns_Friedel_fraction_max     0.609
_reflns_number_gt                3372
_reflns_number_total             5512
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo9b00408_si_002.cif
_cod_data_source_block           bn2890
_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/data/users/saulius/crontab/automatic-downloads/current/ACS/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'
_cod_database_code               4034364
_shelx_res_checksum              63086
_shelx_hkl_checksum              91423