#------------------------------------------------------------------------------ #$Date: 2010-12-09 20:44:53 +0200 (Thu, 09 Dec 2010) $ #$Revision: 3898 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/1101085.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_1101085 loop_ _publ_author_name 'Mohammad Abul Haj' 'Miguel Quir\'os' 'Juan M. Salas' _publ_section_title ; Solution and solid state coexistence of head--head and head--tail isomers in dimeric Pd(II) and Pt(II) complexes of the type [M2(a--a)2(µ-L-N3N4)2]2+ with a bridging triazolopyrimidine ligand and chelating bidentate diamines ; _journal_issue 24 _journal_name_full 'J. Chem. Soc., Dalton Trans.' _journal_page_first 4740 _journal_page_last 4745 _journal_year 2002 _chemical_formula_sum 'C26 H29 Cl3 N16 O19 Pd2' _chemical_formula_weight 1188.80 _chemical_name_systematic ; ? ; _space_group_IT_number 59 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ab 2a' _symmetry_space_group_name_H-M 'P m m n :2' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 11.1799(14) _cell_length_b 18.9400(18) _cell_length_c 9.6374(8) _cell_measurement_reflns_used 46 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 17.5 _cell_measurement_theta_min 12.5 _cell_volume 2040.7(4) _computing_cell_refinement 'STADI4 (STOE, 1996)' _computing_data_collection 'STADI4 (STOE, 1996)' _computing_data_reduction 'X-RED (STOE, 1996)' _computing_molecular_graphics 'SHELXTL PLUS' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _database_code_CSD 190495 _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'STOE STADI4 4-circle-diffractometer' _diffrn_measurement_method ; Scan width (omega) = 1.05 - 1.25, scan ratio 2theta:omega = 1.00 I(Net) and sigma(I) calculated according to Blessing (1987) ; _diffrn_radiation_collimation '0.8 mm' _diffrn_radiation_detector 'NaI(Tl) scintillation counter' _diffrn_radiation_monochromator 'planar graphite' _diffrn_radiation_polarisn_norm 90 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0468 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 3193 _diffrn_reflns_theta_full 30.00 _diffrn_reflns_theta_max 30.00 _diffrn_reflns_theta_min 2.11 _diffrn_standards_decay_% 3.7 _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.176 _exptl_absorpt_correction_T_max 0.6505 _exptl_absorpt_correction_T_min 0.5388 _exptl_absorpt_correction_type none _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.935 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prismatic _exptl_crystal_F_000 1184 _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.40 _refine_diff_density_max 0.858 _refine_diff_density_min -0.669 _refine_diff_density_rms 0.119 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 162 _refine_ls_number_reflns 3193 _refine_ls_number_restraints 12 _refine_ls_restrained_S_all 1.115 _refine_ls_R_factor_all 0.1404 _refine_ls_R_factor_gt 0.0821 _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^)+(0.0600P)^2^+10.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1705 _refine_ls_wR_factor_ref 0.2107 _reflns_number_gt 1900 _reflns_number_total 3193 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file b207263g.txt _[local]_cod_data_source_block compound6 _[local]_cod_cif_authors_sg_H-M 'P m m n' _cod_database_code 1101085 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z' 'x+1/2, -y, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z' '-x-1/2, 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 0.39204(8) 0.2500 0.53000(8) 0.0569(3) Uani 1 2 d S . . N1 N 0.3916(10) 0.4104(9) 0.8390(17) 0.075(4) Uiso 0.50 1 d PD A -1 C2 C 0.4428(11) 0.3648(11) 0.752(2) 0.069(7) Uiso 0.50 1 d PD A -1 H2 H 0.5283 0.3619 0.7445 0.082 Uiso 0.50 1 d PR A -1 N3 N 0.3718(10) 0.3220(7) 0.6749(14) 0.051(3) Uiso 0.50 1 d PD A -1 C3A C 0.2635(9) 0.3451(5) 0.7167(9) 0.046(2) Uiso 0.50 1 d PD A -1 N4 N 0.1558(10) 0.3287(7) 0.6722(14) 0.048(3) Uiso 0.50 1 d PD . -1 C5 C 0.0559(15) 0.3528(14) 0.738(3) 0.082(8) Uiso 0.50 1 d PD A -1 H5 H -0.0215 0.3345 0.7138 0.098 Uiso 0.50 1 d PR A -1 C6 C 0.0682(14) 0.4025(10) 0.840(2) 0.073(5) Uiso 0.50 1 d PD A -1 H6 H -0.0031 0.4187 0.8855 0.088 Uiso 0.50 1 d PR A -1 C7 C 0.1767(10) 0.4309(8) 0.8837(16) 0.080(5) Uiso 0.50 1 d PD A -1 O7 O 0.2073(10) 0.4767(6) 0.9664(12) 0.096(4) Uiso 0.50 1 d PD A -1 N8 N 0.2726(9) 0.3958(5) 0.8183(9) 0.058(3) Uiso 0.50 1 d PD A -1 N1P N 0.4419(6) 0.3179(4) 0.3814(6) 0.0691(17) Uani 1 1 d . A . C2P C 0.4282(10) 0.3887(6) 0.3823(9) 0.090(3) Uani 1 1 d . . . H2P H 0.3881 0.4104 0.4553 0.107 Uiso 1 1 d R A . C3P C 0.4739(12) 0.4284(6) 0.2738(11) 0.118(4) Uani 1 1 d . A . H3P H 0.4626 0.4770 0.2700 0.142 Uiso 1 1 d R . . C4P C 0.5375(14) 0.3919(9) 0.1737(12) 0.144(6) Uani 1 1 d . . . H4P H 0.5733 0.4180 0.1034 0.173 Uiso 1 1 d R A . N5P N 0.5492(9) 0.3229(6) 0.1714(8) 0.109(3) Uani 1 1 d . A . C6P C 0.4992(8) 0.2887(5) 0.2758(7) 0.081(3) Uani 1 1 d . . . Cl1 Cl 0.2500 0.2500 0.0583(4) 0.0679(10) Uani 1 4 d S . . O1Q O 0.3519(10) 0.2500 -0.0262(9) 0.096(3) Uani 1 2 d S . . O2Q O 0.2500 0.1891(6) 0.1438(11) 0.126(4) Uani 1 2 d S . . Cl2 Cl 0.2500 0.56295(19) 0.5095(4) 0.0891(10) Uani 1 2 d S . . O3Q O 0.3488(9) 0.5628(5) 0.4235(9) 0.147(3) Uani 1 1 d . . . O4Q O 0.2500 0.5034(6) 0.5949(11) 0.123(4) Uani 1 2 d S . . O5Q O 0.2500 0.6234(7) 0.5939(15) 0.170(6) Uani 1 2 d S . . O1W O 0.2500 0.5837(5) 0.1318(10) 0.118(4) Uani 1 2 d S . . O2W O 0.1676(12) 0.7096(6) 0.0628(10) 0.086(3) Uani 0.50 1 d P . -1 O3W O 0.684(3) 0.2500 0.578(3) 0.170(11) Uiso 0.50 2 d SP . . 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 0.0615(5) 0.0675(5) 0.0418(4) 0.000 -0.0001(4) 0.000 N1P 0.078(4) 0.086(5) 0.044(3) 0.005(3) -0.001(3) -0.014(4) C2P 0.112(8) 0.098(7) 0.059(5) 0.003(5) 0.005(5) -0.027(6) C3P 0.176(12) 0.113(8) 0.066(6) 0.015(6) 0.008(7) -0.058(9) C4P 0.170(13) 0.188(14) 0.073(7) 0.013(9) 0.019(8) -0.107(12) N5P 0.117(7) 0.156(9) 0.054(4) -0.005(6) 0.021(4) -0.051(7) C6P 0.074(5) 0.127(7) 0.042(4) -0.001(4) 0.004(4) -0.022(5) Cl1 0.082(3) 0.076(2) 0.0450(19) 0.000 0.000 0.000 O1Q 0.123(8) 0.092(6) 0.074(5) 0.000 0.034(6) 0.000 O2Q 0.104(8) 0.163(10) 0.111(8) 0.082(8) 0.000 0.000 Cl2 0.120(3) 0.082(2) 0.0647(18) 0.0053(16) 0.000 0.000 O3Q 0.153(7) 0.167(8) 0.122(6) 0.015(6) 0.040(6) -0.015(7) O4Q 0.162(10) 0.112(8) 0.096(7) 0.042(7) 0.000 0.000 O5Q 0.262(18) 0.110(9) 0.138(11) -0.038(9) 0.000 0.000 O1W 0.188(12) 0.088(7) 0.077(6) 0.010(5) 0.000 0.000 O2W 0.101(8) 0.103(8) 0.054(6) 0.004(6) -0.015(6) -0.007(7) 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' Cl Cl 0.1484 0.1585 '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_ _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 N3 Pd N3 87.9(9) . 7_565 ? N3 Pd N1P 170.2(4) . 7_565 ? N3 Pd N1P 95.4(5) 7_565 7_565 ? N3 Pd N1P 95.4(5) . . ? N3 Pd N1P 170.2(4) 7_565 . ? N1P Pd N1P 79.9(4) 7_565 . ? N3 Pd N4 8.7(6) . 8_655 ? N3 Pd N4 90.0(3) 7_565 8_655 ? N1P Pd N4 174.5(5) 7_565 8_655 ? N1P Pd N4 94.7(5) . 8_655 ? N3 Pd N4 90.0(3) . 2 ? N3 Pd N4 8.7(6) 7_565 2 ? N1P Pd N4 94.7(5) 7_565 2 ? N1P Pd N4 174.5(5) . 2 ? N4 Pd N4 90.8(9) 8_655 2 ? N3 Pd Pd 83.4(3) . 2 ? N3 Pd Pd 83.4(3) 7_565 2 ? N1P Pd Pd 106.2(2) 7_565 2 ? N1P Pd Pd 106.2(2) . 2 ? N4 Pd Pd 75.2(3) 8_655 2 ? N4 Pd Pd 75.2(3) 2 2 ? C2 N1 N8 101.2(11) . . ? N1 C2 N3 118.7(10) . . ? C3A N3 C2 99.6(7) . . ? C3A N3 Pd 122.8(8) . . ? C2 N3 Pd 137.5(8) . . ? N4 C3A N3 130.4(8) . . ? N4 C3A N8 117.6(10) . . ? N3 C3A N8 111.9(8) . . ? C3A N4 C5 121.4(12) . . ? C3A N4 Pd 127.9(9) . 2 ? C5 N4 Pd 109.4(9) . 2 ? N4 C5 C6 118.8(17) . . ? C5 C6 C7 124.8(18) . . ? O7 C7 C6 135.5(12) . . ? O7 C7 N8 114.3(11) . . ? C6 C7 N8 110.2(12) . . ? N1 N8 C3A 108.4(11) . . ? N1 N8 C7 125.2(11) . . ? C3A N8 C7 126.3(10) . . ? C6P N1P C2P 118.4(8) . . ? C6P N1P Pd 114.6(6) . . ? C2P N1P Pd 127.0(6) . . ? N1P C2P C3P 119.5(10) . . ? C4P C3P C2P 116.4(12) . . ? N5P C4P C3P 124.1(11) . . ? C4P N5P C6P 115.6(10) . . ? N5P C6P N1P 125.9(10) . . ? N5P C6P C6P 119.3(6) . 7_565 ? N1P C6P C6P 114.7(5) . 7_565 ? O1Q Cl1 O1Q 108.9(9) 2 . ? O1Q Cl1 O2Q 109.8(3) 2 2 ? O1Q Cl1 O2Q 109.8(3) . 2 ? O1Q Cl1 O2Q 109.8(3) 2 . ? O1Q Cl1 O2Q 109.8(3) . . ? O2Q Cl1 O2Q 108.9(11) 2 . ? O3Q Cl2 O3Q 106.2(9) . 8_655 ? O3Q Cl2 O4Q 110.6(5) . . ? O3Q Cl2 O4Q 110.6(5) 8_655 . ? O3Q Cl2 O5Q 110.5(6) . . ? O3Q Cl2 O5Q 110.5(6) 8_655 . ? O4Q Cl2 O5Q 108.5(8) . . ? O7 O1W O2W 118.8(5) 1_554 . ? O2W O2W O1W 108.0(7) 2_565 . ? O2W O2W N5P 121.7(4) 2_565 4_465 ? O1W O2W N5P 100.1(5) . 4_465 ? O3W O3W O5Q 75.8(5) 2_655 5_666 ? 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 N3 1.964(10) . ? Pd N3 1.964(10) 7_565 ? Pd N1P 2.004(6) 7_565 ? Pd N1P 2.004(6) . ? Pd N4 2.095(11) 8_655 ? Pd N4 2.095(11) 2 ? Pd Pd 3.1760(17) 2 ? N1 C2 1.333(5) . ? N1 N8 1.373(5) . ? C2 N3 1.357(5) . ? N3 C3A 1.349(5) . ? C3A N4 1.315(5) . ? C3A N8 1.375(5) . ? N4 C5 1.362(5) . ? N4 Pd 2.095(11) 2 ? C5 C6 1.368(5) . ? C6 C7 1.393(5) . ? C7 O7 1.227(5) . ? C7 N8 1.410(5) . ? N1P C6P 1.323(10) . ? N1P C2P 1.350(11) . ? C2P C3P 1.385(12) . ? C3P C4P 1.384(18) . ? C4P N5P 1.314(16) . ? N5P C6P 1.321(10) . ? C6P C6P 1.466(19) 7_565 ? Cl1 O1Q 1.400(9) 2 ? Cl1 O1Q 1.400(9) . ? Cl1 O2Q 1.417(10) 2 ? Cl1 O2Q 1.417(10) . ? Cl2 O3Q 1.381(9) . ? Cl2 O3Q 1.381(9) 8_655 ? Cl2 O4Q 1.397(10) . ? Cl2 O5Q 1.404(12) . ? O1W O7 2.622(15) 1_554 ? O1W O2W 2.641(15) . ? O2W O2W 2.39(3) 2_565 ? O2W N5P 2.688(13) 4_465 ? O3W O3W 1.47(6) 2_655 ? O3W O5Q 3.01(2) 5_666 ?