New synthesis of unsymmetrically-substituted 2,5-diarylpyrroles from homopropargyl sulfonamides
Van Rossom, Wim; Matsushita, Yoshitaka; Ariga, Katsuhiko; Hill, Jonathan P.; RSC Advances 4 (2014) 4897–; doi:10.1039/c3ra46579a

data_7239432
_publ_section_title
;
 New synthesis of unsymmetrically-substituted 2,5-diarylpyrroles from
 homopropargyl sulfonamides
;
_journal_issue                   10
_journal_name_full               'RSC Advances'
_journal_page_first              4897
_journal_paper_doi               10.1039/c3ra46579a
_journal_volume                  4
_journal_year                    2014
_chemical_formula_sum            'C16 H14 N2 O'
_chemical_formula_weight         249.28
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 98.103(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.6181(4)
_cell_length_b                   21.2320(19)
_cell_length_c                   10.8628(9)
_cell_measurement_reflns_used    2877
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.9375
_cell_measurement_theta_min      2.696
_cell_volume                     1282.82(18)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.773
_diffrn_measurement_device
;
Rigaku AFC11 Saturn724+ (4x4 bin mode)
;
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_unetI/netI     0.0561
_diffrn_reflns_Laue_measured_fraction_full 0.909
_diffrn_reflns_Laue_measured_fraction_max 0.773
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6030
_diffrn_reflns_point_group_measured_fraction_full 0.915
_diffrn_reflns_point_group_measured_fraction_max 0.779
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.070
_diffrn_reflns_theta_min         2.696
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.5166
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_F_000             524
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.219
_refine_diff_density_min         -0.235
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -1(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         3938
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0414
_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^)+(0.0452P)^2^+0.3250P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1013
_refine_ls_wR_factor_ref         0.1152
_reflns_Friedel_coverage         0.966
_reflns_Friedel_fraction_full    0.922
_reflns_Friedel_fraction_max     0.784
_reflns_number_gt                3256
_reflns_number_total             3938
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3ra46579a.txt
_cod_data_source_block           shelx
_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/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/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               7239432
_shelxl_version_number           2013-4
_shelx_res_checksum              63898