#------------------------------------------------------------------------------ #$Date: 2011-09-10 06:16:28 +0300 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2003031.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2003031 loop_ _publ_author_name 'Kiralj, Rudolf' 'Koji\'c-Prodi\'c, Biserka' 'Piantanida, Ivo' '\ routine' _computing_data_collection 'EXPRESS-CAD4 (Enraf Nonius 1992) software' _computing_data_reduction 'HELENA (Spek, 1994)' _computing_molecular_graphics ; PLATON93 (Spek, 1982, 1990) & ORTEP (Johnson, 1965), PLUTON93 (Spek 1991) ; _computing_publication_material 'PLATON93 (Spek 1982, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _diffrn_ambient_temperature 295(3) _diffrn_measurement_device 'Enraf-Nonius CAD4 diffractometer' _diffrn_measurement_method \w/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents .0425 _diffrn_reflns_av_sigmaI/netI .0358 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 1108 _diffrn_reflns_reduction_process ; ? ; _diffrn_reflns_theta_max 65.21 _diffrn_reflns_theta_min 5.25 _diffrn_standards_interval_count 44 _diffrn_standards_interval_time 120 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu .60 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.369 _exptl_crystal_density_meas 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 244 _exptl_crystal_size_max .32 _exptl_crystal_size_mid .14 _exptl_crystal_size_min .11 _refine_diff_density_max .19 _refine_diff_density_min -.12 _refine_ls_abs_structure_details ; ? ; _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all .896 _refine_ls_goodness_of_fit_obs 1.055 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_constraints 15 _refine_ls_number_parameters 70 _refine_ls_number_reflns 508 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all .896 _refine_ls_restrained_S_obs 1.055 _refine_ls_R_factor_all .0610 _refine_ls_R_factor_obs .0405 _refine_ls_shift/esd_max .005 _refine_ls_shift/esd_mean .001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0966P)^2^+0.0939P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_wR_factor_all .1380 _refine_ls_wR_factor_obs .1237 _reflns_number_observed 322 _reflns_number_total 508 _reflns_observed_criterion >2sigma(I) _[local]_cod_data_source_file na0085.cif _[local]_cod_data_source_block DIAZA2 _[local]_cod_cif_authors_sg_H-M 'C 2/m' _cod_database_code 2003031 loop_ _symmetry_equiv_pos_as_xyz 'X, Y, Z' '-X, Y, -Z' 'X+1/2, Y+1/2, Z' '-X+1/2, Y+1/2, -Z' '-X, -Y, -Z' 'X, -Y, Z' '-X+1/2, -Y+1/2, -Z' 'X+1/2, -Y+1/2, Z' loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 N4 .105(12) .034(4) .060(6) .009(4) .003(4) -.003(3) C1 .0543(11) .0636(12) .0539(10) -.0104(8) .0012(8) .0054(7) C2 .0513(14) .0742(16) .0450(13) .0000 -.0009(10) .0000 C4 .045(8) .067(8) .083(8) -.015(5) .014(4) .013(5) C11 .0475(12) .0466(12) .0404(11) .0000 -.0044(9) .0000 C21 .0547(17) .105(2) .0714(19) .0000 .0157(14) .0000 C51 .0509(10) .0516(11) .0492(10) -.0019(7) -.0015(7) .0013(6) loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_group N4 .0454(9) .2129(8) .940(3) .067(5) Uani d P .5 A C1 .20167(13) .10471(15) .7671(4) .0577(6) Uani d . 1.0 . C2 .25315(17) .00000 .7111(6) .0574(8) Uani d P .5 . C4 .0510(9) .2091(11) .953(4) .064(5) Uani d P .5 . C11 .05070(15) .00000 .9407(5) .0456(7) Uani d P .5 . C21 .3642(2) .00000 .5974(9) .0764(11) Uani d P .5 . C51 .10093(12) .10675(14) .8818(4) .0512(6) Uani d . 1.0 . H1 .2365(13) .1769(19) .727(5) .075(5) Uiso d . 1.0 . H4 .073(3) .286(3) .892(8) .055(9) Uiso d P .5 A H211 .3727(19) -.064(2) .456(7) .145(11) Uiso calc R 1.0 . H212 .422(3) .00000 .773(11) .155(16) Uiso calc R .5 . loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0181 .0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0311 .0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 -1 0 -1 -3 2 0 -3 -7 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C51 N4 H4 . . 122(2) no C2 C1 C51 . . 121.36(16) no C1 C2 C21 . . 120.39(10) no C1 C2 C1 . 4_555 119.20(18) no C1 C2 C21 4_555 . 120.39(10) no C11 C11 C51 2_557 . 119.57(9) no C51 C11 C51 . 4_555 120.86(16) no C11 C11 C51 2_557 4_555 119.57(9) no N4 C51 C4 . . 2.9(8) no N4 C51 C11 . . 118.6(4) no N4 C51 C1 . . 122.8(5) no C1 C51 C11 . . 118.60(15) no C4 C51 C11 . . 119.1(5) no C1 C51 C4 . . 122.2(5) no C2 C1 H1 . . 119.5(11) no C51 C1 H1 . . 119.2(11) no C51 C4 H4 . . 126(2) no C2 C21 H211 . . 110.6(15) no C2 C21 H212 . . 116(2) no C2 C21 H211 . 4_555 110.6(15) no H211 C21 H212 . . 108(2) no H211 C21 H211 . 4_555 103(2) no H211 C21 H212 4_555 . 108(2) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag N4 C51 . 1.434(10) no N4 H4 . .94(4) no C1 C51 . 1.388(2) no C1 C2 . 1.393(2) no C2 C21 . 1.509(3) no C4 C51 . 1.375(13) no C11 C51 . 1.4084(18) no C11 C11 2_557 1.403(3) no C1 H1 . .96(2) no C4 H4 . .96(4) no C21 H211 . .94(2) no C21 H212 . .94(4) no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C51 C1 C2 C21 . . -178.0(2) no C2 C1 C51 C4 . . 177.0(8) no C51 C1 C2 C1 . 4_555 .9(3) no C2 C1 C51 N4 . . -179.6(6) no C2 C1 C51 C11 . . -.2(3) no C11 C11 C51 C1 2_557 . 179.48(16) no C11 C11 C51 C4 2_557 . 2.2(8) no C51 C11 C51 C1 4_555 . -.6(3) no C51 C11 C51 C4 4_555 . -177.9(7) no C51 C11 C51 N4 4_555 . 178.9(5) no C11 C11 C51 N4 2_557 . -1.1(6) no