#------------------------------------------------------------------------------ #$Date: 2015-01-27 21:58:39 +0200 (Tue, 27 Jan 2015) $ #$Revision: 130149 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/10/01/1100168.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_1100168 loop_ _publ_author_name 'Esther R. Acuna-Cueva' 'Rene Faure' 'Nuria A. Illan-Cabeza' 'Sonia B. Jimenez-Pulido' 'Miguel N. Moreno-Carretero' 'Miguel Quiros' _journal_name_full Polyhedron _journal_page_first 483 _journal_page_last 488 _journal_paper_doi 10.1016/S0277-5387(02)01374-8 _journal_volume 22 _journal_year 2003 _chemical_formula_sum 'C14 H12 Br2 N8 O4 Pd' _chemical_formula_weight 622.54 _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 94.351(10) _cell_angle_beta 106.036(8) _cell_angle_gamma 109.334(14) _cell_formula_units_Z 1 _cell_length_a 6.5185(9) _cell_length_b 7.5119(11) _cell_length_c 10.7736(9) _cell_measurement_reflns_used 33 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 14.63 _cell_measurement_theta_min 5.06 _cell_volume 470.21(10) _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measurement_device_type 'Siemens P4' _diffrn_measurement_method '2\q/\w scans' _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 0.0273 _diffrn_reflns_av_sigmaI/netI 0.0475 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 3372 _diffrn_reflns_theta_full 29.99 _diffrn_reflns_theta_max 29.99 _diffrn_reflns_theta_min 2.00 _diffrn_standards_decay_% 12.21 _diffrn_standards_interval_count 97 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 5.278 _exptl_absorpt_correction_T_max 0.9040 _exptl_absorpt_correction_T_min 0.5196 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details ? _exptl_crystal_colour ? _exptl_crystal_density_diffrn 2.198 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'flat needles' _exptl_crystal_F_000 300 _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.02 _refine_diff_density_max 2.915 _refine_diff_density_min -2.364 _refine_diff_density_rms 0.279 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 134 _refine_ls_number_reflns 2716 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.074 _refine_ls_R_factor_all 0.0953 _refine_ls_R_factor_gt 0.0720 _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^)+(0.1500P)^2^+0.3000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1998 _refine_ls_wR_factor_ref 0.2209 _reflns_number_gt 2025 _reflns_number_total 2716 _reflns_threshold_expression >2sigma(I) _cod_database_code 1100168 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.5000 0.5000 0.5000 0.0323(2) Uani 1 2 d S . . Br Br 0.67601(14) 0.29558(12) 0.61895(9) 0.0520(3) Uani 1 1 d . . . N1 N 0.0461(12) -0.1330(9) 0.1222(6) 0.0439(14) Uani 1 1 d . . . C1 C -0.1430(18) -0.3256(13) 0.0720(10) 0.062(2) Uani 1 1 d . . . H11 H -0.1343 -0.3836 -0.0080 0.075 Uiso 1 1 d R . . H12 H -0.2885 -0.3109 0.0552 0.075 Uiso 1 1 d R . . H13 H -0.1276 -0.4059 0.1364 0.075 Uiso 1 1 d R . . C1A C 0.0420(13) -0.0108(10) 0.2273(7) 0.0396(14) Uani 1 1 d . . . C2 C 0.2293(16) -0.0880(12) 0.0742(8) 0.0501(18) Uani 1 1 d . . . O2 O 0.2318(14) -0.1898(10) -0.0162(7) 0.0667(19) Uani 1 1 d . . . N3 N 0.4057(13) 0.0836(10) 0.1341(7) 0.0502(16) Uani 1 1 d . . . H3 H 0.5163 0.1131 0.1015 0.060 Uiso 1 1 d R . . C4 C 0.4324(13) 0.2146(11) 0.2389(7) 0.0409(14) Uani 1 1 d . . . O4 O 0.6003(11) 0.3587(9) 0.2816(6) 0.0586(16) Uani 1 1 d . . . C4A C 0.2313(12) 0.1556(10) 0.2863(7) 0.0378(13) Uani 1 1 d . . . N5 N 0.2313(10) 0.2668(8) 0.3903(6) 0.0358(11) Uani 1 1 d . . . C6 C 0.0416(13) 0.2202(10) 0.4263(8) 0.0420(15) Uani 1 1 d . . . H6 H 0.0340 0.2995 0.4942 0.050 Uiso 1 1 d R . . C7 C -0.1439(13) 0.0518(12) 0.3608(9) 0.0482(17) Uani 1 1 d . . . H7 H -0.2746 0.0204 0.3864 0.058 Uiso 1 1 d R . . N8 N -0.1424(12) -0.0660(10) 0.2631(7) 0.0488(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.0308(4) 0.0313(4) 0.0344(4) 0.0064(2) 0.0135(3) 0.0083(3) Br 0.0436(5) 0.0474(5) 0.0657(6) 0.0252(4) 0.0147(4) 0.0164(4) N1 0.048(4) 0.037(3) 0.043(3) 0.008(2) 0.011(3) 0.013(3) C1 0.059(6) 0.040(4) 0.065(5) -0.001(4) 0.005(4) 0.004(4) C1A 0.040(4) 0.031(3) 0.045(3) 0.008(3) 0.010(3) 0.012(3) C2 0.059(5) 0.043(4) 0.041(4) 0.006(3) 0.013(3) 0.012(4) O2 0.087(5) 0.054(4) 0.055(4) -0.004(3) 0.032(4) 0.016(3) N3 0.051(4) 0.050(4) 0.045(3) -0.002(3) 0.021(3) 0.010(3) C4 0.039(3) 0.043(4) 0.039(3) 0.006(3) 0.016(3) 0.011(3) O4 0.045(3) 0.054(3) 0.064(4) -0.006(3) 0.029(3) -0.004(3) C4A 0.037(3) 0.039(3) 0.037(3) 0.011(2) 0.012(3) 0.012(3) N5 0.035(3) 0.033(3) 0.040(3) 0.008(2) 0.016(2) 0.009(2) C6 0.040(4) 0.037(3) 0.052(4) 0.012(3) 0.021(3) 0.013(3) C7 0.032(3) 0.052(4) 0.061(5) 0.020(4) 0.019(3) 0.011(3) N8 0.038(3) 0.046(3) 0.057(4) 0.016(3) 0.014(3) 0.007(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0.00 0.00 1.00 0.0100 0.00 0.00 -1.00 0.0100 1.00 -1.00 0.00 0.2500 -1.00 1.00 0.00 0.2500 1.00 2.00 2.00 0.0500 -1.00 -2.00 -2.00 0.0500 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Pd N5 180.0 2_666 . ? N5 Pd Br 90.37(17) 2_666 2_666 ? N5 Pd Br 89.63(17) . 2_666 ? N5 Pd Br 89.63(17) 2_666 . ? N5 Pd Br 90.37(17) . . ? Br Pd Br 180.0 2_666 . ? N5 Pd O4 109.8(2) 2_666 . ? N5 Pd O4 70.2(2) . . ? Br Pd O4 93.67(16) 2_666 . ? Br Pd O4 86.33(16) . . ? C2 N1 C1A 122.1(6) . . ? C2 N1 C1 119.3(7) . . ? C1A N1 C1 118.3(7) . . ? N8 C1A C4A 124.5(7) . . ? N8 C1A N1 116.9(7) . . ? C4A C1A N1 118.6(7) . . ? O2 C2 N3 122.0(9) . . ? O2 C2 N1 122.3(8) . . ? N3 C2 N1 115.7(7) . . ? C2 N3 C4 129.6(7) . . ? O4 C4 N3 121.7(7) . . ? O4 C4 C4A 126.7(7) . . ? N3 C4 C4A 111.6(6) . . ? C4 O4 Pd 98.6(5) . . ? N5 C4A C1A 118.4(7) . . ? N5 C4A C4 119.3(6) . . ? C1A C4A C4 122.3(7) . . ? C6 N5 C4A 118.9(6) . . ? C6 N5 Pd 116.5(5) . . ? C4A N5 Pd 124.6(5) . . ? N5 C6 C7 119.2(7) . . ? N8 C7 C6 122.9(7) . . ? C1A N8 C7 115.9(7) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd N5 2.011(6) 2_666 ? Pd N5 2.011(6) . ? Pd Br 2.4432(8) 2_666 ? Pd Br 2.4432(8) . ? Pd O4 2.832(6) . ? N1 C2 1.382(11) . ? N1 C1A 1.414(9) . ? N1 C1 1.496(10) . ? C1A N8 1.310(10) . ? C1A C4A 1.384(10) . ? C2 O2 1.199(10) . ? C2 N3 1.372(10) . ? N3 C4 1.372(9) . ? C4 O4 1.202(9) . ? C4 C4A 1.481(10) . ? C4A N5 1.346(9) . ? N5 C6 1.342(9) . ? C6 C7 1.393(11) . ? C7 N8 1.326(11) . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3 O2 0.86 2.04 2.898(10) 176.6 2_655