Cyanation of alpha,beta-unsaturated enones by malononitrile in open air under metal-catalyst-free conditions
Shaoxia Lin; Ying Wei; Fushun Liang; Chem.Commun. 48 (2012) 9879–; doi:10.1039/c2cc35528k

data_7108402
_publ_section_title
;
 Cyanation of alpha,beta-unsaturated enones by malononitrile in open air
 under metal-catalyst-free conditions
;
_journal_name_full               Chem.Commun.
_journal_page_first              9879
_journal_paper_doi               10.1039/c2cc35528k
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C16 H13 N O'
_chemical_formula_weight         235.29
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.758(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.3345(8)
_cell_length_b                   9.0779(4)
_cell_length_c                   9.9141(6)
_cell_measurement_temperature    293(2)
_cell_volume                     1271.43(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0215
_diffrn_reflns_av_sigmaI/netI    0.0313
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4670
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.88
_exptl_absorpt_coefficient_mu    0.085
_exptl_crystal_colour            0.3
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             495
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_refine_diff_density_max         0.104
_refine_diff_density_min         -0.145
_refine_diff_density_rms         0.030
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         2214
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0722
_refine_ls_R_factor_gt           0.0463
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0536P)^2^+0.0461P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1032
_refine_ls_wR_factor_ref         0.1169
_reflns_number_gt                1538
_reflns_number_total             2214
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc35528k.txt
_cod_data_source_block           2
_cod_depositor_comments
;

2018-03-15
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C55 H50 N5 O10'
_cod_original_formula_units_Z    1
_cod_original_formula_weight     941.00
_cod_database_code               7108402