#------------------------------------------------------------------------------ #$Date: 2009-11-16 03:43:51 +0200 (Mon, 16 Nov 2009) $ #$Revision: 853 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/1100677.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100677 _publ_requested_journal 'ANALYTICAL SCIENCES' _publ_section_title ; Synthesis and Crystal Structure of 3,5-dicyano-2,6- dimethyl-4-phenyl-1,4-dihydropyridine ; _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _[local]_cod_cif_authors_sg_H-M 'P 21/c' loop_ _publ_author_name 'M. Mahendra, B. H. Doreswamy, M. A. Sridhar, J. S. Prasad' 'Priti Adlakha, Kena Reval, Bharat Varu, Anamik Shah' _chemical_name_systematic ; 3,5-dicyano-2,6-dimethyl-4-phenyl-1,4-dihydropyridine ; _chemical_formula_moiety 'C15 H13 N3' _chemical_formula_sum 'C15 H13 N3' _chemical_formula_weight 235.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-z x,1/2-y,1/2+z _cell_length_a 8.7220(7) _cell_length_b 11.4200(11) _cell_length_c 13.3070(12) _cell_angle_alpha 90 _cell_angle_beta 104.101(5) _cell_angle_gamma 90 _cell_volume 1285.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_special_details ; ? ; _exptl_crystal_description '?' _exptl_crystal_colour '?' _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.216 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 496 _exptl_absorpt_coefficient_mu 0.074 _exptl_crystal_density_meas_temp ? _exptl_absorpt_correction_type ' ?' _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_ambient_temperature 293 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_probe 'x-ray' _diffrn_radiation_type 'MoK\a' loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 7541 _diffrn_reflns_av_R_equivalents 0.0260 _diffrn_reflns_av_sigmaI/netI 0.0321 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 32.40 _diffrn_reflns_theta_full 32.40 _diffrn_measured_fraction_theta_max 0.866 _diffrn_measured_fraction_theta_full 0.866 _diffrn_reflns_reduction_process ; ? ; _reflns_number_total 4001 _reflns_number_gt 2190 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc' _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1190P)^2^+0.2704P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'direct' _atom_sites_solution_secondary 'difmap' _atom_sites_solution_hydrogens 'geom' _refine_ls_hydrogen_treatment 'mixed' _refine_ls_extinction_method 'shelxl' _refine_ls_extinction_coef 0.087(10) _refine_ls_extinction_expression 'FC^*^=KFC[1+0.001XFC^2^\L^3^/SIN(2\Q)]^-1/4^' _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack none _refine_ls_number_reflns 4001 _refine_ls_number_parameters 164 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.1096 _refine_ls_R_factor_gt 0.0625 _refine_ls_wR_factor_ref 0.2265 _refine_ls_wR_factor_gt 0.1755 _refine_ls_goodness_of_fit_ref 0.908 _refine_ls_restrained_S_all 0.908 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.373 _refine_diff_density_min -0.330 _refine_diff_density_rms 0.119 loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags N10 N Uani 0.6271(3) 1.16323(18) 0.02184(17) 1.000 0.0923(8) . . N13 N Uani 0.86547(19) 0.78752(14) 0.02215(12) 1.000 0.0678(5) . . N18 N Uani 1.0157(2) 0.8649(2) -0.29337(16) 1.000 0.0929(8) . . C1 C Uani 0.6409(3) 1.08230(16) -0.28316(16) 1.000 0.0689(7) . . C2 C Uani 0.5119(3) 1.08631(19) -0.36767(16) 1.000 0.0795(8) . . C3 C Uani 0.4045(3) 0.9969(2) -0.38603(17) 1.000 0.0790(7) . . C4 C Uani 0.4248(2) 0.90351(19) -0.31988(17) 1.000 0.0766(7) . . C5 C Uani 0.5531(2) 0.89846(16) -0.23507(15) 1.000 0.0658(6) . . C6 C Uani 0.6639(2) 0.98761(14) -0.21567(13) 1.000 0.0561(5) . . C7 C Uani 0.8071(2) 0.97909(15) -0.12403(14) 1.000 0.0598(5) . . C8 C Uani 0.7615(2) 0.97578(15) -0.02075(14) 1.000 0.0604(5) . . C9 C Uani 0.6853(2) 1.07891(18) 0.00436(15) 1.000 0.0692(6) . . C11 C Uani 0.7856(2) 0.88537(16) 0.04464(14) 1.000 0.0617(6) . . C12 C Uani 0.7358(3) 0.8798(2) 0.14394(16) 1.000 0.0783(8) . . C14 C Uani 0.9281(2) 0.78180(16) -0.06265(14) 1.000 0.0620(6) . . C15 C Uani 1.0193(3) 0.67317(19) -0.07043(17) 1.000 0.0774(8) . . C16 C Uani 0.9061(2) 0.87090(16) -0.13110(15) 1.000 0.0612(6) . . C17 C Uani 0.9700(2) 0.86490(18) -0.21969(16) 1.000 0.0700(7) . . H1 H Uiso 0.71500 1.14600 -0.27100 1.000 0.0830 . R H2 H Uiso 0.49630 1.15220 -0.41380 1.000 0.0950 . R H3 H Uiso 0.31670 0.99970 -0.44570 1.000 0.0950 . R H4 H Uiso 0.34850 0.84130 -0.33150 1.000 0.0920 . R H5 H Uiso 0.56590 0.83150 -0.19010 1.000 0.0790 . R H7 H Uiso 0.87310 1.04840 -0.12460 1.000 0.0720 calc R H12A H Uiso 0.68250 0.95110 0.15300 1.000 0.0940 . R H12B H Uiso 0.82730 0.87030 0.20040 1.000 0.0940 . R H12C H Uiso 0.66550 0.81470 0.14250 1.000 0.0940 . R H13 H Uiso 0.87520 0.72170 0.06820 1.000 0.0810 . R H15A H Uiso 1.05840 0.67740 -0.13180 1.000 0.0930 . R H15B H Uiso 0.95290 0.60550 -0.07400 1.000 0.0930 . R H15C H Uiso 1.10670 0.66740 -0.01070 1.000 0.0930 . R