#------------------------------------------------------------------------------ #$Date: 2010-01-30 15:59:17 +0200 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/1100170.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_1100170 _space_group_IT_number 15 _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _[local]_cod_cif_authors_sg_H-M 'C 2/c' loop_ _publ_author_name 'Mohammad Abul-Haj' 'Miguel Quiros' 'Juan M. Salas' _journal_name_full 'Polyhedron' _journal_volume 23 _journal_page_first 2373 _journal_page_last 2379 _journal_year 2004 _chemical_name_systematic ; Bis(4,5-dihydro-1,2,4-triazolo[1,5-a]pyrimidinate-5-one-mu-N3-N4) bis(phenanthroline)dipalladium(II) nitrate tetrahydrate ; _chemical_formula_sum 'C34 H30 N14 O12 Pd2' _chemical_formula_weight 1039.52 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' 'Pd' 'Pd' -0.9988 1.0072 '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, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.688(12) _cell_length_b 14.219(12) _cell_length_c 14.448(6) _cell_angle_alpha 90.00 _cell_angle_beta 110.02(4) _cell_angle_gamma 90.00 _cell_volume 3800(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 43 _cell_measurement_theta_min 5.04 _cell_measurement_theta_max 12.08 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.817 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2080 _exptl_absorpt_coefficient_mu 1.031 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'MoK\a' _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens P4' _diffrn_measurement_method '2\q/\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_decay_% 40.24 _diffrn_reflns_number 6442 _diffrn_reflns_av_R_equivalents 0.0541 _diffrn_reflns_av_sigmaI/netI 0.0762 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 30.07 _reflns_number_total 5547 _reflns_number_gt 2956 _reflns_threshold_expression >2sigma(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^)+(0.1200P)^2^+2.0000P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5547 _refine_ls_number_parameters 272 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1484 _refine_ls_R_factor_gt 0.0793 _refine_ls_wR_factor_ref 0.2325 _refine_ls_wR_factor_gt 0.1920 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 0.51944(3) 0.28682(4) 0.35998(4) 0.0478(2) Uani 1 1 d . . . N1 N 0.6725(4) 0.0714(7) 0.3822(7) 0.086(2) Uani 1 1 d . . . C2 C 0.6451(5) 0.1433(8) 0.4165(7) 0.083(3) Uani 1 1 d . . . H2 H 0.6591 0.1574 0.4833 0.100 Uiso 1 1 d R . . N3 N 0.5942(3) 0.1954(5) 0.3456(5) 0.0591(17) Uani 1 1 d . . . C3A C 0.5909(4) 0.1535(6) 0.2605(6) 0.0554(18) Uani 1 1 d . . . N4 N 0.5498(3) 0.1772(5) 0.1682(5) 0.0558(15) Uani 1 1 d . . . C5 C 0.5533(5) 0.1210(6) 0.0921(7) 0.064(2) Uani 1 1 d . . . O5 O 0.5137(4) 0.1400(5) 0.0081(5) 0.092(2) Uani 1 1 d . . . C6 C 0.6019(6) 0.0423(7) 0.1187(8) 0.081(3) Uani 1 1 d . . . H6 H 0.6051 0.0032 0.0688 0.098 Uiso 1 1 d R . . C7 C 0.6427(6) 0.0227(8) 0.2114(9) 0.088(3) Uani 1 1 d . . . H7 H 0.6741 -0.0284 0.2265 0.105 Uiso 1 1 d R . . N8 N 0.6364(4) 0.0804(5) 0.2821(6) 0.0686(19) Uani 1 1 d . . . N1P N 0.4453(3) 0.3817(5) 0.3699(4) 0.0520(15) Uani 1 1 d . . . C1AP C 0.4687(4) 0.4707(6) 0.3722(5) 0.0506(17) Uani 1 1 d . . . C2P C 0.3784(4) 0.3659(7) 0.3714(5) 0.062(2) Uani 1 1 d . . . H2P H 0.3617 0.3044 0.3695 0.074 Uiso 1 1 d R . . C3P C 0.3334(5) 0.4416(8) 0.3759(6) 0.069(2) Uani 1 1 d . . . H3P H 0.2876 0.4294 0.3784 0.082 Uiso 1 1 d R . . C4P C 0.3553(5) 0.5297(8) 0.3765(6) 0.069(2) Uani 1 1 d . . . H4P H 0.3245 0.5789 0.3777 0.083 Uiso 1 1 d R . . C4AP C 0.4260(5) 0.5494(6) 0.3755(5) 0.064(2) Uani 1 1 d . . . C5P C 0.4573(6) 0.6427(7) 0.3773(6) 0.076(3) Uani 1 1 d . . . H5P H 0.4297 0.6955 0.3784 0.091 Uiso 1 1 d R . . C6P C 0.5255(6) 0.6542(7) 0.3777(6) 0.075(3) Uani 1 1 d . . . H6P H 0.5439 0.7145 0.3778 0.090 Uiso 1 1 d R . . C6AP C 0.5696(5) 0.5741(6) 0.3779(5) 0.064(2) Uani 1 1 d . . . C7P C 0.6429(6) 0.5802(8) 0.3817(6) 0.080(3) Uani 1 1 d . . . H7P H 0.6642 0.6385 0.3812 0.096 Uiso 1 1 d R . . C8P C 0.6808(5) 0.4998(8) 0.3862(6) 0.074(3) Uani 1 1 d . . . H8P H 0.7292 0.5039 0.3915 0.089 Uiso 1 1 d R . . C9P C 0.6500(4) 0.4125(7) 0.3827(6) 0.065(2) Uani 1 1 d . . . H9P H 0.6772 0.3589 0.3834 0.078 Uiso 1 1 d R . . N10P N 0.5804(3) 0.4039(5) 0.3786(4) 0.0512(14) Uani 1 1 d . . . C0AP C 0.5413(4) 0.4834(6) 0.3757(4) 0.0522(18) Uani 1 1 d . . . N1N N 0.7711(13) 0.2618(11) 0.3177(12) 0.100(5) Uiso 0.50 1 d PD . . O1N O 0.7783(12) 0.2267(12) 0.4003(11) 0.130(7) Uiso 0.50 1 d PD . . O2N O 0.7632(15) 0.2094(13) 0.2457(12) 0.139(5) Uiso 0.50 1 d PD . . O3N O 0.7916(14) 0.3454(10) 0.3168(15) 0.164(7) Uiso 0.50 1 d PD . . N1N' N 0.7836(11) 0.2659(13) 0.2589(13) 0.100(5) Uiso 0.50 1 d PD . . O1N' O 0.8207(16) 0.308(2) 0.216(2) 0.225(14) Uiso 0.50 1 d PD . . O2N' O 0.7394(12) 0.2051(15) 0.2126(17) 0.139(5) Uiso 0.50 1 d PD . . O3N' O 0.7896(17) 0.2873(17) 0.3444(14) 0.164(7) Uiso 0.50 1 d PD . . O1W O 0.5458(7) 0.0853(10) -0.1558(8) 0.181(5) Uani 1 1 d . . . O2W O 0.8217(15) 0.325(2) 0.106(2) 0.177(9) Uiso 0.50 1 d P . . O2W' O 0.7987(18) 0.302(2) 0.013(3) 0.211(14) Uiso 0.50 1 d P . . 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 0.0439(3) 0.0606(4) 0.0383(3) -0.0003(3) 0.0134(2) -0.0044(3) N1 0.070(5) 0.094(6) 0.078(5) 0.011(5) 0.003(4) 0.022(5) C2 0.057(5) 0.109(8) 0.065(5) 0.006(6) -0.003(4) 0.010(6) N3 0.049(3) 0.075(5) 0.048(3) -0.001(3) 0.010(3) 0.004(3) C3A 0.044(4) 0.058(5) 0.061(4) -0.001(4) 0.014(3) -0.002(3) N4 0.051(3) 0.056(4) 0.058(4) -0.006(3) 0.016(3) 0.002(3) C5 0.066(5) 0.060(5) 0.064(5) -0.014(4) 0.021(4) 0.005(4) O5 0.112(5) 0.095(5) 0.060(4) -0.006(4) 0.017(4) 0.023(4) C6 0.084(7) 0.075(6) 0.086(7) -0.013(5) 0.031(6) 0.018(5) C7 0.075(6) 0.081(7) 0.108(8) 0.002(6) 0.033(6) 0.027(5) N8 0.056(4) 0.065(4) 0.084(5) 0.003(4) 0.022(4) 0.013(3) N1P 0.049(3) 0.070(4) 0.037(3) -0.004(3) 0.016(2) 0.001(3) C1AP 0.056(4) 0.060(5) 0.032(3) 0.003(3) 0.010(3) 0.004(4) C2P 0.055(4) 0.085(6) 0.048(4) 0.001(4) 0.020(3) -0.005(4) C3P 0.063(5) 0.103(7) 0.042(4) 0.010(5) 0.020(4) 0.012(5) C4P 0.073(5) 0.092(7) 0.041(4) 0.003(4) 0.018(4) 0.028(5) C4AP 0.080(6) 0.072(6) 0.033(3) -0.001(4) 0.012(4) 0.001(5) C5P 0.097(7) 0.079(6) 0.043(4) -0.002(4) 0.012(4) 0.016(6) C6P 0.106(8) 0.052(5) 0.056(5) -0.001(4) 0.012(5) -0.009(5) C6AP 0.088(6) 0.068(5) 0.037(3) 0.000(4) 0.021(4) -0.021(5) C7P 0.095(7) 0.094(7) 0.048(4) -0.007(5) 0.020(5) -0.050(6) C8P 0.076(6) 0.098(7) 0.056(5) -0.018(5) 0.034(4) -0.036(6) C9P 0.054(4) 0.095(7) 0.049(4) -0.014(4) 0.021(4) -0.017(4) N10P 0.053(3) 0.066(4) 0.036(3) -0.005(3) 0.016(2) -0.013(3) C0AP 0.063(4) 0.069(5) 0.026(3) -0.002(3) 0.017(3) -0.005(4) O1W 0.197(11) 0.264(15) 0.107(7) 0.013(8) 0.083(8) 0.075(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 N10P 2.016(6) . ? Pd N4 2.018(7) 2_655 ? Pd N3 2.026(7) . ? Pd N1P 2.029(6) . ? Pd Pd 3.0031(18) 2_655 ? N1 C2 1.329(13) . ? N1 N8 1.381(11) . ? C2 N3 1.379(11) . ? N3 C3A 1.347(10) . ? C3A N8 1.337(10) . ? C3A N4 1.345(10) . ? N4 C5 1.381(10) . ? N4 Pd 2.018(7) 2_655 ? C5 O5 1.227(10) . ? C5 C6 1.436(12) . ? O5 O1W 2.764(12) . ? C6 C7 1.334(14) . ? C7 N8 1.349(12) . ? N1P C2P 1.343(10) . ? N1P C1AP 1.343(10) . ? C1AP C4AP 1.411(11) . ? C1AP C0AP 1.424(11) . ? C2P C3P 1.411(12) . ? C3P C4P 1.325(13) . ? C4P C4AP 1.423(13) . ? C4AP C5P 1.460(14) . ? C5P C6P 1.351(13) . ? C6P C6AP 1.431(13) . ? C6AP C0AP 1.401(11) . ? C6AP C7P 1.427(14) . ? C7P C8P 1.356(15) . ? C8P C9P 1.374(13) . ? C9P N10P 1.357(9) . ? N10P C0AP 1.361(10) . ? N1N O2N 1.246(9) . ? N1N O1N 1.256(9) . ? N1N O3N 1.258(9) . ? N1N' O3N' 1.238(9) . ? N1N' O2N' 1.246(9) . ? N1N' O1N' 1.258(9) . ? O1N' O2W' 2.82(4) . ? O1W O1W 2.70(2) 2_654 ? O1W O2W 2.77(3) 7_655 ? 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 N10P Pd N4 174.2(2) . 2_655 ? N10P Pd N3 97.1(3) . . ? N4 Pd N3 87.0(3) 2_655 . ? N10P Pd N1P 81.5(3) . . ? N4 Pd N1P 94.3(3) 2_655 . ? N3 Pd N1P 177.6(3) . . ? C2 N1 N8 101.0(7) . . ? N1 C2 N3 114.9(9) . . ? C3A N3 C2 103.6(7) . . ? C3A N3 Pd 124.6(5) . . ? C2 N3 Pd 129.6(6) . . ? N8 C3A N4 123.6(8) . . ? N8 C3A N3 108.2(7) . . ? N4 C3A N3 128.1(7) . . ? C3A N4 C5 117.9(7) . . ? C3A N4 Pd 122.0(5) . 2_655 ? C5 N4 Pd 120.1(6) . 2_655 ? O5 C5 N4 118.1(8) . . ? O5 C5 C6 125.2(8) . . ? N4 C5 C6 116.6(8) . . ? C7 C6 C5 123.2(9) . . ? C6 C7 N8 117.0(9) . . ? C3A N8 C7 121.6(8) . . ? C3A N8 N1 112.3(8) . . ? C7 N8 N1 126.1(8) . . ? C2P N1P C1AP 119.2(7) . . ? C2P N1P Pd 128.5(6) . . ? C1AP N1P Pd 112.3(5) . . ? N1P C1AP C4AP 123.0(7) . . ? N1P C1AP C0AP 116.9(7) . . ? C4AP C1AP C0AP 120.1(8) . . ? N1P C2P C3P 120.5(9) . . ? C4P C3P C2P 120.9(9) . . ? C3P C4P C4AP 120.3(9) . . ? C1AP C4AP C4P 116.2(8) . . ? C1AP C4AP C5P 117.9(8) . . ? C4P C4AP C5P 125.9(9) . . ? C6P C5P C4AP 121.6(9) . . ? C5P C6P C6AP 120.3(9) . . ? C0AP C6AP C7P 116.5(9) . . ? C0AP C6AP C6P 119.8(8) . . ? C7P C6AP C6P 123.8(9) . . ? C8P C7P C6AP 118.9(9) . . ? C7P C8P C9P 122.1(9) . . ? N10P C9P C8P 120.6(9) . . ? C9P N10P C0AP 118.6(7) . . ? C9P N10P Pd 128.8(6) . . ? C0AP N10P Pd 112.1(5) . . ? N10P C0AP C6AP 123.2(7) . . ? N10P C0AP C1AP 116.5(7) . . ? C6AP C0AP C1AP 120.3(8) . . ? O2N N1N O1N 119.8(10) . . ? O2N N1N O3N 120.3(10) . . ? O1N N1N O3N 117.0(10) . . ? O3N' N1N' O2N' 121.1(10) . . ? O3N' N1N' O1N' 120.0(10) . . ? O2N' N1N' O1N' 118.9(10) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.07 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.733 _refine_diff_density_min -1.256 _refine_diff_density_rms 0.194 _cod_database_code 1100170