NMR analysis of a series of 1,2-bis(1-<i>R</i>-5-oxo-2,3-dihydro-1<i>H</i>-pyrrol-4-ylidene)ethanes and X-ray crystal structure analysis of the <i>R</i> = mesityl compound
Liu, Qi; Song, Xiu-Qing; Yan, Hong; Acta Crystallographica Section C 70 (2014) 965–970; doi:10.1107/S2053229614020099

data_2019675
_publ_section_title
;
 NMR analysis of a series of
 1,2-bis(1-<i>R</i>-5-oxo-2,3-dihydro-1<i>H</i>-pyrrol-4-ylidene)ethanes
 and X-ray crystal structure analysis of the <i>R</i> = mesityl compound
;
_journal_coeditor_code           FN3174
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              965
_journal_page_last               970
_journal_paper_doi               10.1107/S2053229614020099
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'C36 H36 N2 O10'
_chemical_formula_moiety         'C36 H36 N2 O10'
_chemical_formula_sum            'C36 H36 N2 O10'
_chemical_formula_weight         656.67
_chemical_name_common
'Tetramethyl 4,4'-(ethane-1,2-diylidene)bis(5-oxo-1-mesityl-4,5-dihydro-1<i>H</i>-pyrrole-2,3-dicarboxylate)'
_chemical_name_systematic
;Tetramethyl
4,4'-(ethane-1,2-diylidene)bis[5-oxo-1-(2,4,6-trimethylphenyl)-4,5-dihydro-1<i>H</i>-pyrrole-2,3-dicarboxylate]
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 103.74(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.4573(17)
_cell_length_b                   19.181(4)
_cell_length_c                   10.936(2)
_cell_measurement_reflns_used    3848
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.8864
_cell_measurement_theta_min      2.1236
_cell_volume                     1723.3(6)
_computing_cell_refinement       'CrystalClear (Rigaku, 2013)'
_computing_data_collection       'CrystalClear (Rigaku, 2013)'
_computing_data_reduction        'CrystalClear (Rigaku, 2013)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku Saturn 70 CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            15252
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_min         2.124
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7832
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrystalClear; Rigaku, 2013)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_description       prism
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.301
_refine_diff_density_min         -0.236
_refine_ls_extinction_coef       0.035(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL2013 (Sheldrick, 2013)'
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         3376
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0920
_refine_ls_R_factor_gt           0.0677
_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^)+(0.1170P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1779
_refine_ls_wR_factor_ref         0.1977
_reflns_number_gt                2339
_reflns_number_total             3376
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fn3174sup1.cf
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 2019675.cif.'
_cod_database_code               2019675
_cod_database_fobs_code          2019675
_shelx_estimated_absorpt_t_min   0.983
_shelx_estimated_absorpt_t_max   0.989
_shelx_hkl_checksum              40800
_shelx_res_checksum              31875
_shelxl_version_number           2.013