Bis(1-cyanovinyl acetate) Is a Linear Precursor to 3-Oxidopyrylium Ions.
Wilkerson-Hill, Sidney Malik; Sawano, Shota; Sarpong, Richmond; The Journal of organic chemistry 81 (2016) 11132–11144; doi:10.1021/acs.joc.6b02111

data_4037388
_publ_section_title
;
 Bis(1-cyanovinyl acetate) Is a Linear Precursor to 3-Oxidopyrylium Ions.
;
_journal_issue                   22
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              11132
_journal_page_last               11144
_journal_paper_doi               10.1021/acs.joc.6b02111
_journal_volume                  81
_journal_year                    2016
_chemical_formula_sum            'C34 H34 N2 O7'
_chemical_formula_weight         582.63
_chemical_name_common            SMHVII-020C
_chemical_name_systematic
;
 sarpong81
;
_space_group.centring_type       primitive
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 106.013(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.4287(4)
_cell_length_b                   20.8084(6)
_cell_length_c                   20.8192(6)
_cell_measurement_reflns_used    9362
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.50
_cell_measurement_theta_min      3.06
_cell_volume                     6008.2(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX
_computing_structure_refinement  SHELXL-2014
_computing_structure_solution    SHELXT
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_unetI/netI     0.0184
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_refln_scan_rate          10
_diffrn_refln_scan_width         1.0
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            83552
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         68.733
_diffrn_reflns_theta_min         3.064
_diffrn_source                   'microfocus rotating anode'
_exptl_absorpt_coefficient_mu    0.739
_exptl_absorpt_correction_T_max  0.929
_exptl_absorpt_correction_T_min  0.887
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_description       plate
_exptl_crystal_F_000             2464
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.093
_refine_diff_density_min         -0.603
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     785
_refine_ls_number_reflns         11014
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0990
_refine_ls_R_factor_gt           0.0896
_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^)+(0.1758P)^2^+3.8032P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2587
_refine_ls_wR_factor_ref         0.2705
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9126
_reflns_number_total             11014
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo6b02111_si_005.cif
_cod_data_source_block           sarpong81
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4037388
_shelx_estimated_absorpt_t_min   0.964
_shelx_estimated_absorpt_t_max   0.985
_shelxl_version_number           2014-1
_shelx_res_checksum              13263
_shelx_hkl_checksum              49262