Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'J.Chem.Soc.,Dalton Trans.' loop_ _publ_author_name 'Barnett, Sarah A.' 'Blake, A.' 'Champness, Neil' 'Nicolson, James E. B.' 'Wilson, Claire' _publ_contact_author_name 'Dr Neil Champness' _publ_contact_author_address ; Dr Neil Champness School of Chemistry The University of Nottingham University Park Nottingham NG7 2RD UNITED KINGDOM ; _publ_contact_author_email 'Neil.Champness@nottingham.ac.uk' data_cdtynt _database_code_CSD 151816 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Di-Cadmium(II)-di[bis-2,4-(4-pyridyl)-1,3,5-triazine] (MeCN)tetranitrate.solvate ; _chemical_name_common Cd2(dpt)2(MeCN)(NO3)4.2.5MeCN.0.5CH2Cl2 _chemical_melting_point ? _chemical_formula_moiety Cd2(C13H9N5)2(MeCN)(NO3)4.2.5MeCN.0.5CH2Cl2 _chemical_formula_sum 'C16.58 H12.28 Cd Cl0.50 N8.67 O6' _chemical_formula_weight 559.09 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' 'Cd' 'Cd' -0.8075 1.2024 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/m 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' _cell_length_a 26.578(5) _cell_length_b 26.471(5) _cell_length_c 16.037(3) _cell_angle_alpha 90.00 _cell_angle_beta 126.52(3) _cell_angle_gamma 90.00 _cell_volume 9067(3) _cell_formula_units_Z 16 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7573 _cell_measurement_theta_min 2.205 _cell_measurement_theta_max 28.67 _exptl_crystal_description 'triangular plate' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.638 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4431 _exptl_absorpt_coefficient_mu 1.073 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.602 _exptl_absorpt_correction_T_max 0.796 _exptl_absorpt_process_details ? _exptl_special_details ; Di-Cadmium(II)-di[bis-2,4-(4-pyridyl)-1,3,5-triazine] (MeCN)tetranitrate.solvate ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 9087 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0282 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9087 _reflns_number_gt 8102 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART version 5.054 (Bruker, 1998)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT version 6.01 (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (version 5.03)(Sheldrick,1994)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0434P)^2^+174.3831P] 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 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9087 _refine_ls_number_parameters 625 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.0713 _refine_ls_R_factor_gt 0.0655 _refine_ls_wR_factor_ref 0.1599 _refine_ls_wR_factor_gt 0.1564 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.124 _refine_ls_shift/su_max 0.065 _refine_ls_shift/su_mean 0.003 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 Cd1 Cd 0.5000 0.87838(2) 0.5000 0.02793(16) Uani 1 2 d S . . Cd2 Cd 1.0000 0.87980(2) 1.5000 0.02793(16) Uani 1 2 d S . . Cd3 Cd 0.75740(3) 0.5000 0.81397(5) 0.02903(17) Uani 1 2 d S . . Cd4 Cd 0.87477(4) 0.5000 0.66668(7) 0.0401(2) Uani 1 2 d S . . N100 N 0.5488(3) 0.8481(2) 0.7070(4) 0.0413(15) Uani 1 1 d D . . O101 O 0.5401(3) 0.89315(19) 0.6747(4) 0.0477(13) Uani 1 1 d D . . O102 O 0.5357(2) 0.81358(19) 0.6437(4) 0.0417(12) Uani 1 1 d D . . O103 O 0.5685(3) 0.8392(3) 0.7971(4) 0.072(2) Uani 1 1 d D . . N200 N 0.8941(2) 0.8483(2) 1.4890(4) 0.0336(12) Uani 1 1 d D . . O201 O 0.9098(2) 0.89415(18) 1.4920(4) 0.0425(12) Uani 1 1 d D . . O202 O 0.9293(2) 0.81454(17) 1.4949(4) 0.0364(11) Uani 1 1 d D . . O203 O 0.8451(2) 0.8384(2) 1.4779(4) 0.0482(13) Uani 1 1 d D . . N300 N 0.7111(4) 0.5000 0.9331(6) 0.041(2) Uani 1 2 d SD . . O301 O 0.7695(3) 0.5000 0.9773(5) 0.0454(18) Uani 1 2 d SD . . O302 O 0.6752(3) 0.5000 0.8341(5) 0.0392(16) Uani 1 2 d SD . . O303 O 0.6887(4) 0.5000 0.9823(7) 0.061(2) Uani 1 2 d SD . . N310 N 0.8808(4) 0.5000 0.8571(7) 0.0368(19) Uani 1 2 d S . . O312 O 0.8782(4) 0.5000 0.9312(6) 0.0441(17) Uani 1 2 d S . . O311 O 0.8291(3) 0.5000 0.7651(5) 0.0367(15) Uani 1 2 d S . . O313 O 0.9298(3) 0.5000 0.8642(6) 0.0496(19) Uani 1 2 d S . . N400 N 0.7718(4) 0.5000 0.4567(7) 0.046(2) Uani 1 2 d SD . . O401 O 0.8264(4) 0.5000 0.4826(7) 0.0485(19) Uani 1 2 d SD . . O402 O 0.7644(4) 0.5000 0.5272(6) 0.0487(19) Uani 1 2 d SD . . O403 O 0.7257(5) 0.5000 0.3647(7) 0.071(3) Uani 1 2 d SD . . N31S N 0.6862(4) 0.5000 0.6361(6) 0.0382(19) Uani 1 2 d S . . C31S C 0.6571(4) 0.5000 0.5496(7) 0.033(2) Uani 1 2 d S . . C32S C 0.6182(5) 0.5000 0.4369(8) 0.043(2) Uani 1 2 d S . . H32A H 0.5780 0.4838 0.4096 0.064 Uiso 0.50 1 calc PR . . H32B H 0.6395 0.4813 0.4133 0.064 Uiso 0.50 1 calc PR . . H32C H 0.6109 0.5349 0.4116 0.064 Uiso 0.50 1 calc PR . . N41S N 0.9757(5) 0.5000 0.7163(9) 0.051(2) Uani 1 2 d S . . C41S C 1.0262(6) 0.5000 0.7527(9) 0.048(3) Uani 1 2 d S . . C42S C 1.0930(6) 0.5000 0.7983(15) 0.103(8) Uani 1 2 d S . . H42A H 1.1155 0.5218 0.8598 0.155 Uiso 0.50 1 calc PR . . H42B H 1.0990 0.5127 0.7473 0.155 Uiso 0.50 1 calc PR . . H42C H 1.1094 0.4655 0.8183 0.155 Uiso 0.50 1 calc PR . . N1 N 0.5962(2) 0.8572(2) 0.5417(4) 0.0280(11) Uani 1 1 d . . . C2 C 0.6085(3) 0.8079(2) 0.5420(5) 0.0293(13) Uani 1 1 d . . . H2A H 0.5767 0.7839 0.5226 0.035 Uiso 1 1 calc R . . C3 C 0.6659(3) 0.7909(2) 0.5696(5) 0.0298(13) Uani 1 1 d . . . H3A H 0.6733 0.7557 0.5695 0.036 Uiso 1 1 calc R . . C4 C 0.7124(3) 0.8257(2) 0.5973(5) 0.0286(13) Uani 1 1 d . . . C5 C 0.6990(3) 0.8769(2) 0.5955(5) 0.0317(14) Uani 1 1 d . . . H5A H 0.7299 0.9018 0.6147 0.038 Uiso 1 1 calc R . . C6 C 0.6404(3) 0.8909(2) 0.5658(5) 0.0311(14) Uani 1 1 d . . . H6A H 0.6311 0.9259 0.5624 0.037 Uiso 1 1 calc R . . C7 C 0.7748(3) 0.8087(2) 0.6297(5) 0.0294(13) Uani 1 1 d . . . N8 N 0.7833(2) 0.7590(2) 0.6295(4) 0.0298(12) Uani 1 1 d . . . C9 C 0.8396(3) 0.7445(2) 0.6596(5) 0.0262(13) Uani 1 1 d . . . N10 N 0.8191(3) 0.8436(2) 0.6576(5) 0.0364(13) Uani 1 1 d . . . C11 C 0.8731(3) 0.8248(3) 0.6847(6) 0.0408(17) Uani 1 1 d . . . H11A H 0.9052 0.8484 0.7034 0.049 Uiso 1 1 calc R . . N12 N 0.8871(3) 0.7757(2) 0.6885(4) 0.0327(12) Uani 1 1 d . . . C13 C 0.8512(3) 0.6894(2) 0.6639(5) 0.0297(13) Uani 1 1 d . . . C14 C 0.9066(3) 0.6700(3) 0.6885(5) 0.0326(14) Uani 1 1 d . . . H14A H 0.9394 0.6919 0.7037 0.039 Uiso 1 1 calc R . . C15 C 0.9136(3) 0.6180(3) 0.6907(5) 0.0361(15) Uani 1 1 d . . . H15A H 0.9521 0.6048 0.7085 0.043 Uiso 1 1 calc R . . N16 N 0.8682(3) 0.5853(2) 0.6688(5) 0.0359(13) Uani 1 1 d . . . C17 C 0.8141(3) 0.6048(3) 0.6438(6) 0.0363(15) Uani 1 1 d . . . H17A H 0.7816 0.5822 0.6276 0.044 Uiso 1 1 calc R . . C18 C 0.8035(3) 0.6562(3) 0.6405(5) 0.0329(14) Uani 1 1 d . . . H18A H 0.7647 0.6687 0.6228 0.039 Uiso 1 1 calc R . . N1' N 0.9377(2) 0.8592(2) 1.3263(4) 0.0304(12) Uani 1 1 d . . . C2' C 0.9016(3) 0.8917(2) 1.2487(5) 0.0321(14) Uani 1 1 d . . . H2'A H 0.9039 0.9266 1.2647 0.039 Uiso 1 1 calc R . . C3' C 0.8610(3) 0.8767(2) 1.1460(5) 0.0312(14) Uani 1 1 d . . . H3'A H 0.8369 0.9010 1.0928 0.037 Uiso 1 1 calc R . . C4' C 0.8558(3) 0.8259(2) 1.1216(5) 0.0269(13) Uani 1 1 d . . . C5' C 0.8931(3) 0.7916(2) 1.2020(5) 0.0295(13) Uani 1 1 d . . . H5'A H 0.8912 0.7565 1.1879 0.035 Uiso 1 1 calc R . . C6' C 0.9326(3) 0.8095(2) 1.3020(5) 0.0321(14) Uani 1 1 d . . . H6'A H 0.9574 0.7859 1.3565 0.039 Uiso 1 1 calc R . . C7' C 0.8113(3) 0.8074(2) 1.0129(5) 0.0295(13) Uani 1 1 d . . . N8' N 0.8116(2) 0.75770(19) 0.9963(4) 0.0254(11) Uani 1 1 d . . . C9' C 0.7712(3) 0.7431(2) 0.8980(5) 0.0294(13) Uani 1 1 d . . . N10' N 0.7314(3) 0.7732(2) 0.8189(4) 0.0385(14) Uani 1 1 d . . . C11' C 0.7350(4) 0.8214(3) 0.8445(5) 0.0457(19) Uani 1 1 d . . . H11B H 0.7069 0.8441 0.7902 0.055 Uiso 1 1 calc R . . N12' N 0.7742(3) 0.8411(2) 0.9392(4) 0.0398(14) Uani 1 1 d . . . C13' C 0.7707(3) 0.6883(2) 0.8765(5) 0.0267(13) Uani 1 1 d . . . C14' C 0.8083(3) 0.6552(3) 0.9570(5) 0.0337(15) Uani 1 1 d . . . H14B H 0.8358 0.6672 1.0263 0.040 Uiso 1 1 calc R . . C15' C 0.8053(3) 0.6041(3) 0.9348(5) 0.0357(15) Uani 1 1 d . . . H15B H 0.8314 0.5813 0.9904 0.043 Uiso 1 1 calc R . . N16' N 0.7668(2) 0.5854(2) 0.8378(4) 0.0290(11) Uani 1 1 d . . . C17' C 0.7313(3) 0.6181(2) 0.7597(5) 0.0297(13) Uani 1 1 d . . . H17B H 0.7048 0.6054 0.6908 0.036 Uiso 1 1 calc R . . C18' C 0.7321(3) 0.6693(2) 0.7758(5) 0.0303(14) Uani 1 1 d . . . H18B H 0.7064 0.6914 0.7188 0.036 Uiso 1 1 calc R . . N1S N 0.6151(4) 0.2762(4) 1.1101(7) 0.080(3) Uani 1 1 d . . . C1S C 0.5784(5) 0.2641(5) 1.0254(8) 0.072(3) Uani 1 1 d . . . C2S C 0.5320(4) 0.2503(5) 0.9159(7) 0.075(3) Uani 1 1 d . . . H2SA H 0.5287 0.2134 0.9093 0.112 Uiso 1 1 calc R . . H2SB H 0.5451 0.2637 0.8747 0.112 Uiso 1 1 calc R . . H2SC H 0.4911 0.2645 0.8906 0.112 Uiso 1 1 calc R . . N110 N 0.5000 1.0000 0.5000 0.037(3) Uani 1 4 d SD . . O111 O 0.5360(4) 0.9604(3) 0.5280(10) 0.050(3) Uani 0.50 1 d PD . -1 O112 O 0.4454(6) 1.0000 0.4560(15) 0.067(5) Uiso 0.50 2 d SPD . . N210 N 1.0000 1.0000 1.5000 0.037(3) Uiso 1 4 d SD . . O211 O 0.9869(5) 0.9612(4) 1.4395(8) 0.048(3) Uiso 0.50 1 d PD . . O212 O 1.0196(7) 1.0000 1.5840(9) 0.048(4) Uiso 0.50 2 d SPD . . C1A C 0.4890(10) 0.0991(9) 1.0288(17) 0.072(5) Uiso 0.50 1 d P . -1 Cl1A Cl 0.56851(15) 0.12872(13) 1.0712(2) 0.0844(8) Uani 1 1 d . . . N1V N 0.9964(13) 0.9067(12) 0.813(2) 0.123(9) Uiso 0.50 1 d PD A -1 C1V C 1.0097(11) 0.9481(10) 0.8151(19) 0.080(6) Uiso 0.50 1 d PD A -1 C2V C 1.0329(9) 1.003(4) 0.8213(15) 0.092(8) Uiso 0.50 1 d PD A -1 N1U N 1.0228(10) 0.8762(9) 0.8971(18) 0.092(6) Uiso 0.50 1 d PD B 2 C1U C 1.0613(12) 0.8898(10) 0.985(2) 0.086(7) Uiso 0.50 1 d PD B 2 C2U C 1.1208(12) 0.9100(10) 1.097(2) 0.086(7) Uiso 0.50 1 d PD B 2 N1T N 1.2176(10) 0.5230(8) 0.7861(16) 0.080(6) Uiso 0.33 1 d P . 1 C1T' C 1.2176(10) 0.5230(8) 0.7861(16) 0.080(6) Uiso 0.17 1 d P . 2 C1T C 1.2009(13) 0.5574(11) 0.790(2) 0.093(8) 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 Cd1 0.0354(4) 0.0164(3) 0.0370(4) 0.000 0.0242(3) 0.000 Cd2 0.0310(3) 0.0157(3) 0.0250(3) 0.000 0.0102(3) 0.000 Cd3 0.0323(3) 0.0228(3) 0.0250(3) 0.000 0.0132(3) 0.000 Cd4 0.0487(4) 0.0263(4) 0.0586(5) 0.000 0.0392(4) 0.000 N100 0.030(3) 0.050(4) 0.035(3) 0.013(3) 0.015(3) 0.004(3) O101 0.054(3) 0.036(3) 0.040(3) -0.010(2) 0.022(3) -0.006(2) O102 0.048(3) 0.032(3) 0.044(3) 0.005(2) 0.027(2) 0.003(2) O103 0.078(5) 0.087(5) 0.028(3) 0.009(3) 0.020(3) 0.002(4) N200 0.032(3) 0.038(3) 0.025(3) 0.002(2) 0.013(2) 0.003(2) O201 0.045(3) 0.031(3) 0.046(3) -0.001(2) 0.024(2) 0.009(2) O202 0.037(3) 0.029(2) 0.040(3) 0.001(2) 0.020(2) -0.001(2) O203 0.034(3) 0.069(4) 0.043(3) 0.004(3) 0.023(2) 0.003(3) N300 0.052(6) 0.024(4) 0.050(5) 0.000 0.032(5) 0.000 O301 0.046(4) 0.048(5) 0.036(4) 0.000 0.021(3) 0.000 O302 0.035(4) 0.040(4) 0.037(4) 0.000 0.019(3) 0.000 O303 0.079(6) 0.069(6) 0.062(5) 0.000 0.056(5) 0.000 N310 0.036(5) 0.027(4) 0.042(5) 0.000 0.020(4) 0.000 O312 0.045(4) 0.045(4) 0.036(4) 0.000 0.021(3) 0.000 O311 0.034(4) 0.035(4) 0.032(4) 0.000 0.015(3) 0.000 O313 0.037(4) 0.047(5) 0.060(5) 0.000 0.026(4) 0.000 N400 0.064(6) 0.023(4) 0.060(6) 0.000 0.042(6) 0.000 O401 0.066(5) 0.027(4) 0.073(6) 0.000 0.053(5) 0.000 O402 0.060(5) 0.044(4) 0.052(5) 0.000 0.039(4) 0.000 O403 0.078(7) 0.074(7) 0.050(5) 0.000 0.031(5) 0.000 N31S 0.038(5) 0.037(5) 0.030(5) 0.000 0.014(4) 0.000 C31S 0.032(5) 0.032(5) 0.031(5) 0.000 0.016(4) 0.000 C32S 0.045(6) 0.054(7) 0.028(5) 0.000 0.020(5) 0.000 N41S 0.047(6) 0.042(5) 0.072(7) 0.000 0.039(6) 0.000 C41S 0.054(7) 0.023(5) 0.044(6) 0.000 0.017(5) 0.000 C42S 0.032(7) 0.047(8) 0.126(15) 0.000 -0.009(8) 0.000 N1 0.034(3) 0.023(3) 0.030(3) 0.004(2) 0.020(2) 0.008(2) C2 0.038(3) 0.019(3) 0.033(3) 0.003(2) 0.022(3) 0.001(3) C3 0.040(4) 0.023(3) 0.028(3) 0.003(2) 0.020(3) 0.006(3) C4 0.039(3) 0.024(3) 0.025(3) 0.005(2) 0.020(3) 0.005(3) C5 0.037(3) 0.023(3) 0.035(3) 0.005(3) 0.022(3) 0.003(3) C6 0.039(4) 0.016(3) 0.038(3) 0.003(3) 0.023(3) 0.002(3) C7 0.034(3) 0.027(3) 0.026(3) 0.006(3) 0.017(3) 0.004(3) N8 0.030(3) 0.028(3) 0.028(3) 0.003(2) 0.015(2) 0.003(2) C9 0.030(3) 0.031(3) 0.022(3) 0.001(2) 0.017(3) 0.000(3) N10 0.038(3) 0.030(3) 0.042(3) 0.003(3) 0.025(3) 0.002(2) C11 0.039(4) 0.039(4) 0.045(4) 0.005(3) 0.025(3) 0.003(3) N12 0.039(3) 0.025(3) 0.037(3) 0.004(2) 0.024(3) 0.007(2) C13 0.033(3) 0.030(3) 0.027(3) 0.003(3) 0.019(3) 0.005(3) C14 0.033(3) 0.033(4) 0.036(3) 0.002(3) 0.023(3) 0.001(3) C15 0.032(3) 0.037(4) 0.042(4) -0.006(3) 0.024(3) -0.002(3) N16 0.040(3) 0.034(3) 0.039(3) 0.002(3) 0.026(3) 0.004(3) C17 0.038(4) 0.033(4) 0.045(4) -0.004(3) 0.029(3) -0.002(3) C18 0.031(3) 0.036(4) 0.033(3) 0.005(3) 0.020(3) 0.005(3) N1' 0.030(3) 0.023(3) 0.030(3) -0.002(2) 0.014(2) -0.001(2) C2' 0.036(3) 0.020(3) 0.035(3) -0.002(3) 0.019(3) -0.003(3) C3' 0.037(3) 0.025(3) 0.028(3) 0.002(3) 0.017(3) 0.001(3) C4' 0.028(3) 0.026(3) 0.027(3) -0.003(2) 0.017(3) -0.005(2) C5' 0.032(3) 0.021(3) 0.031(3) -0.005(2) 0.017(3) -0.002(2) C6' 0.034(3) 0.022(3) 0.028(3) 0.000(3) 0.012(3) -0.001(3) C7' 0.036(3) 0.027(3) 0.028(3) -0.002(3) 0.021(3) -0.002(3) N8' 0.030(3) 0.024(3) 0.023(2) -0.003(2) 0.016(2) -0.001(2) C9' 0.035(3) 0.020(3) 0.035(3) -0.003(3) 0.023(3) -0.003(3) N10' 0.051(4) 0.027(3) 0.030(3) -0.005(2) 0.020(3) -0.001(3) C11' 0.070(5) 0.027(4) 0.027(3) 0.003(3) 0.021(4) 0.006(3) N12' 0.054(4) 0.026(3) 0.029(3) 0.002(2) 0.019(3) 0.002(3) C13' 0.025(3) 0.029(3) 0.027(3) -0.005(3) 0.016(3) -0.006(2) C14' 0.029(3) 0.033(4) 0.025(3) -0.006(3) 0.008(3) 0.000(3) C15' 0.034(3) 0.024(3) 0.030(3) 0.002(3) 0.009(3) 0.003(3) N16' 0.030(3) 0.026(3) 0.026(3) -0.001(2) 0.014(2) -0.001(2) C17' 0.034(3) 0.031(3) 0.021(3) -0.002(3) 0.015(3) -0.002(3) C18' 0.040(4) 0.026(3) 0.020(3) 0.000(2) 0.016(3) -0.001(3) N1S 0.067(5) 0.128(9) 0.052(5) -0.014(5) 0.039(4) 0.002(6) C1S 0.052(5) 0.124(10) 0.055(6) -0.007(6) 0.041(5) -0.002(6) C2S 0.046(5) 0.128(10) 0.050(5) -0.017(6) 0.028(4) -0.010(6) N110 0.067(8) 0.019(5) 0.036(6) 0.000 0.037(6) 0.000 O111 0.038(6) 0.020(5) 0.088(8) -0.005(5) 0.035(6) -0.003(4) Cl1A 0.0849(19) 0.092(2) 0.0747(17) 0.0021(15) 0.0466(16) 0.0089(16) _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 Cd1 N1 2.296(5) 2_656 y Cd1 N1 2.296(5) . y Cd1 O111 2.306(8) . y Cd1 O111 2.306(8) 2_656 y Cd1 O101 2.363(5) . y Cd1 O101 2.363(5) 2_656 y Cd1 O102 2.560(5) 2_656 y Cd1 O102 2.560(5) . y Cd2 O211 2.302(9) 2_758 y Cd2 O211 2.302(9) . y Cd2 N1' 2.304(5) . y Cd2 N1' 2.304(5) 2_758 y Cd2 O201 2.355(5) 2_758 y Cd2 O201 2.355(5) . y Cd2 O202 2.518(5) . y Cd2 O202 2.518(5) 2_758 y Cd3 N16' 2.283(5) . y Cd3 N16' 2.283(5) 6_565 y Cd3 N31S 2.301(8) . y Cd3 O302 2.392(7) . y Cd3 O301 2.442(7) . y Cd3 O311 2.455(7) . y Cd3 O312 2.581(8) . y Cd4 N16 2.267(6) . y Cd4 N16 2.267(6) 6_565 y Cd4 N41S 2.300(10) . y Cd4 O402 2.409(8) . y Cd4 O401 2.419(8) . y Cd4 O311 2.498(7) . y Cd4 O313 2.581(9) . y N100 O103 1.232(7) . ? N100 O102 1.251(7) . ? N100 O101 1.265(7) . ? N200 O203 1.233(7) . ? N200 O202 1.256(7) . ? N200 O201 1.275(7) . ? N300 O303 1.240(9) . ? N300 O301 1.264(9) . ? N300 O302 1.276(9) . ? N310 O312 1.231(11) . ? N310 O313 1.237(11) . ? N310 O311 1.286(10) . ? N400 O403 1.235(10) . ? N400 O401 1.252(10) . ? N400 O402 1.257(9) . ? N31S C31S 1.115(12) . ? C31S C32S 1.454(13) . ? N41S C41S 1.101(15) . ? C41S C42S 1.463(19) . ? N1 C6 1.335(8) . ? N1 C2 1.343(8) . ? C2 C3 1.389(9) . ? C3 C4 1.385(9) . ? C4 C5 1.398(9) . ? C4 C7 1.482(9) . ? C5 C6 1.382(9) . ? C7 N8 1.336(8) . ? C7 N10 1.346(9) . ? N8 C9 1.326(8) . ? C9 N12 1.339(8) . ? C9 C13 1.484(9) . ? N10 C11 1.324(9) . ? C11 N12 1.343(9) . ? C13 C14 1.378(9) . ? C13 C18 1.397(9) . ? C14 C15 1.386(10) . ? C15 N16 1.351(9) . ? N16 C17 1.344(9) . ? C17 C18 1.385(10) . ? N1' C2' 1.338(8) . ? N1' C6' 1.355(8) . ? C2' C3' 1.386(9) . ? C3' C4' 1.384(9) . ? C4' C5' 1.394(9) . ? C4' C7' 1.490(8) . ? C5' C6' 1.377(9) . ? C7' N12' 1.333(9) . ? C7' N8' 1.343(8) . ? N8' C9' 1.332(8) . ? C9' N10' 1.328(9) . ? C9' C13' 1.490(9) . ? N10' C11' 1.326(9) . ? C11' N12' 1.335(9) . ? C13' C14' 1.376(9) . ? C13' C18' 1.393(8) . ? C14' C15' 1.390(9) . ? C15' N16' 1.348(8) . ? N16' C17' 1.341(8) . ? C17' C18' 1.378(9) . ? N1S C1S 1.151(12) . ? C1S C2S 1.470(13) . ? N110 O112 1.177(14) 5_676 ? N110 O112 1.177(14) . ? N110 O111 1.306(9) 2_656 ? N110 O111 1.306(9) 6_575 ? N110 O111 1.306(9) 5_676 ? N110 O111 1.306(9) . ? O111 O112 1.122(11) 5_676 ? O112 O111 1.122(11) 5_676 ? O112 O111 1.122(11) 2_656 ? N210 O212 1.119(12) 5_778 ? N210 O212 1.119(12) . ? N210 O211 1.310(10) 5_778 ? N210 O211 1.310(10) . ? N210 O211 1.310(10) 6_575 ? N210 O211 1.310(10) 2_758 ? O211 O212 1.073(11) 5_778 ? O211 O211 1.625(19) 2_758 ? O212 O211 1.073(11) 5_778 ? O212 O211 1.073(11) 2_758 ? C1A Cl1A 1.61(2) 2_657 ? C1A Cl1A 1.96(2) . ? Cl1A C1A 1.61(2) 2_657 ? N1V C1V 1.15(3) . ? C1V C2V 1.55(12) . ? N1U C1U 1.21(3) . ? C1U C2U 1.62(3) . ? N1T C1T 1.03(3) . ? N1T N1T 1.22(4) 6_565 ? 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 N1 Cd1 N1 151.7(3) 2_656 . y N1 Cd1 O111 123.2(3) 2_656 . y N1 Cd1 O111 84.9(3) . . y N1 Cd1 O111 84.9(3) 2_656 2_656 y N1 Cd1 O111 123.2(3) . 2_656 y O111 Cd1 O111 39.5(5) . 2_656 y N1 Cd1 O101 91.38(19) 2_656 . y N1 Cd1 O101 93.26(19) . . y O111 Cd1 O101 76.8(4) . . y O111 Cd1 O101 85.2(4) 2_656 . y N1 Cd1 O101 93.26(19) 2_656 2_656 y N1 Cd1 O101 91.38(19) . 2_656 y O111 Cd1 O101 85.2(4) . 2_656 y O111 Cd1 O101 76.8(4) 2_656 2_656 y O101 Cd1 O101 160.9(3) . 2_656 y N1 Cd1 O102 79.78(18) 2_656 2_656 y N1 Cd1 O102 81.37(18) . 2_656 y O111 Cd1 O102 134.0(3) . 2_656 y O111 Cd1 O102 124.5(3) 2_656 2_656 y O101 Cd1 O102 147.41(17) . 2_656 y O101 Cd1 O102 51.64(17) 2_656 2_656 y N1 Cd1 O102 81.37(18) 2_656 . y N1 Cd1 O102 79.78(18) . . y O111 Cd1 O102 124.5(3) . . y O111 Cd1 O102 134.0(3) 2_656 . y O101 Cd1 O102 51.63(17) . . y O101 Cd1 O102 147.41(17) 2_656 . y O102 Cd1 O102 95.9(2) 2_656 . y O211 Cd2 O211 41.3(5) 2_758 . y O211 Cd2 N1' 123.4(3) 2_758 . y O211 Cd2 N1' 83.8(3) . . y O211 Cd2 N1' 83.8(3) 2_758 2_758 y O211 Cd2 N1' 123.4(3) . 2_758 y N1' Cd2 N1' 152.6(3) . 2_758 y O211 Cd2 O201 86.1(3) 2_758 2_758 y O211 Cd2 O201 76.5(3) . 2_758 y N1' Cd2 O201 94.58(19) . 2_758 y N1' Cd2 O201 89.80(19) 2_758 2_758 y O211 Cd2 O201 76.5(3) 2_758 . y O211 Cd2 O201 86.1(3) . . y N1' Cd2 O201 89.80(19) . . y N1' Cd2 O201 94.58(19) 2_758 . y O201 Cd2 O201 161.4(2) 2_758 . y O211 Cd2 O202 125.4(3) 2_758 . y O211 Cd2 O202 134.9(3) . . y N1' Cd2 O202 79.20(18) . . y N1' Cd2 O202 82.07(18) 2_758 . y O201 Cd2 O202 145.95(16) 2_758 . y O201 Cd2 O202 52.61(17) . . y O211 Cd2 O202 134.9(3) 2_758 2_758 y O211 Cd2 O202 125.4(3) . 2_758 y N1' Cd2 O202 82.07(17) . 2_758 y N1' Cd2 O202 79.20(18) 2_758 2_758 y O201 Cd2 O202 52.61(16) 2_758 2_758 y O201 Cd2 O202 145.95(16) . 2_758 y O202 Cd2 O202 93.3(2) . 2_758 y N16' Cd3 N16' 164.5(3) . 6_565 y N16' Cd3 N31S 97.76(13) . . y N16' Cd3 N31S 97.76(13) 6_565 . y N16' Cd3 O302 89.74(14) . . y N16' Cd3 O302 89.74(14) 6_565 . y N31S Cd3 O302 91.4(3) . . y N16' Cd3 O301 83.63(13) . . y N16' Cd3 O301 83.63(13) 6_565 . y N31S Cd3 O301 144.7(3) . . y O302 Cd3 O301 53.3(2) . . y N16' Cd3 O311 91.42(14) . . y N16' Cd3 O311 91.42(14) 6_565 . y N31S Cd3 O311 80.0(3) . . y O302 Cd3 O311 171.4(2) . . y O301 Cd3 O311 135.3(2) . . y N16' Cd3 O312 85.00(13) . . y N16' Cd3 O312 85.00(13) 6_565 . y N31S Cd3 O312 130.7(3) . . y O302 Cd3 O312 137.9(2) . . y O301 Cd3 O312 84.6(2) . . y O311 Cd3 O312 50.7(2) . . y N16 Cd4 N16 170.0(3) . 6_565 y N16 Cd4 N41S 94.56(15) . . y N16 Cd4 N41S 94.56(15) 6_565 . y N16 Cd4 O402 87.22(15) . . y N16 Cd4 O402 87.22(15) 6_565 . y N41S Cd4 O402 147.9(3) . . y N16 Cd4 O401 91.63(15) . . y N16 Cd4 O401 91.63(15) 6_565 . y N41S Cd4 O401 94.9(3) . . y O402 Cd4 O401 53.0(3) . . y N16 Cd4 O311 85.39(15) . . y N16 Cd4 O311 85.39(15) 6_565 . y N41S Cd4 O311 133.4(3) . . y O402 Cd4 O311 78.8(2) . . y O401 Cd4 O311 131.8(2) . . y N16 Cd4 O313 88.52(15) . . y N16 Cd4 O313 88.52(15) 6_565 . y N41S Cd4 O313 83.3(3) . . y O402 Cd4 O313 128.8(2) . . y O401 Cd4 O313 178.2(3) . . y O311 Cd4 O313 50.1(2) . . y O103 N100 O102 122.0(6) . . ? O103 N100 O101 120.5(7) . . ? O102 N100 O101 117.5(5) . . ? N100 O101 Cd1 100.0(4) . . ? N100 O102 Cd1 90.9(4) . . ? O203 N200 O202 122.4(6) . . ? O203 N200 O201 120.0(6) . . ? O202 N200 O201 117.6(5) . . ? N200 O201 Cd2 98.5(4) . . ? N200 O202 Cd2 91.3(3) . . ? O303 N300 O301 122.5(8) . . ? O303 N300 O302 120.2(8) . . ? O301 N300 O302 117.3(7) . . ? N300 O301 Cd3 93.7(5) . . ? N300 O302 Cd3 95.7(5) . . ? O312 N310 O313 124.9(9) . . ? O312 N310 O311 118.2(8) . . ? O313 N310 O311 116.9(9) . . ? N310 O312 Cd3 93.3(6) . . ? N310 O311 Cd3 97.8(6) . . ? N310 O311 Cd4 97.8(6) . . ? Cd3 O311 Cd4 164.4(3) . . ? N310 O313 Cd4 95.2(6) . . ? O403 N400 O401 121.7(9) . . ? O403 N400 O402 120.0(9) . . ? O401 N400 O402 118.3(9) . . ? N400 O401 Cd4 94.2(6) . . ? N400 O402 Cd4 94.5(6) . . ? C31S N31S Cd3 172.5(9) . . ? N31S C31S C32S 179.1(11) . . ? C41S N41S Cd4 170.9(11) . . ? N41S C41S C42S 178.4(16) . . ? C6 N1 C2 118.7(6) . . ? C6 N1 Cd1 123.7(4) . . ? C2 N1 Cd1 117.6(4) . . ? N1 C2 C3 122.3(6) . . ? C4 C3 C2 119.2(6) . . ? C3 C4 C5 118.0(6) . . ? C3 C4 C7 120.6(6) . . ? C5 C4 C7 121.3(6) . . ? C6 C5 C4 119.3(6) . . ? N1 C6 C5 122.4(6) . . ? N8 C7 N10 124.2(6) . . ? N8 C7 C4 116.9(6) . . ? N10 C7 C4 118.9(6) . . ? C9 N8 C7 116.1(6) . . ? N8 C9 N12 125.0(6) . . ? N8 C9 C13 117.3(6) . . ? N12 C9 C13 117.7(6) . . ? C11 N10 C7 114.5(6) . . ? N10 C11 N12 126.4(7) . . ? C9 N12 C11 113.8(6) . . ? C14 C13 C18 119.2(6) . . ? C14 C13 C9 122.4(6) . . ? C18 C13 C9 118.4(6) . . ? C13 C14 C15 118.7(6) . . ? N16 C15 C14 123.0(6) . . ? C17 N16 C15 117.6(6) . . ? C17 N16 Cd4 117.2(5) . . ? C15 N16 Cd4 125.3(5) . . ? N16 C17 C18 123.1(7) . . ? C17 C18 C13 118.3(6) . . ? C2' N1' C6' 117.6(6) . . ? C2' N1' Cd2 125.0(4) . . ? C6' N1' Cd2 117.0(4) . . ? N1' C2' C3' 122.7(6) . . ? C4' C3' C2' 119.4(6) . . ? C3' C4' C5' 118.2(6) . . ? C3' C4' C7' 121.7(6) . . ? C5' C4' C7' 120.0(6) . . ? C6' C5' C4' 119.0(6) . . ? N1' C6' C5' 123.0(6) . . ? N12' C7' N8' 124.6(6) . . ? N12' C7' C4' 118.1(6) . . ? N8' C7' C4' 117.3(6) . . ? C9' N8' C7' 115.0(5) . . ? N10' C9' N8' 125.4(6) . . ? N10' C9' C13' 118.1(6) . . ? N8' C9' C13' 116.5(6) . . ? C11' N10' C9' 114.3(6) . . ? N10' C11' N12' 126.3(7) . . ? C7' N12' C11' 114.3(6) . . ? C14' C13' C18' 118.7(6) . . ? C14' C13' C9' 120.1(6) . . ? C18' C13' C9' 121.3(6) . . ? C13' C14' C15' 118.7(6) . . ? N16' C15' C14' 122.7(6) . . ? C17' N16' C15' 118.1(6) . . ? C17' N16' Cd3 122.4(4) . . ? C15' N16' Cd3 119.2(4) . . ? N16' C17' C18' 122.3(6) . . ? C17' C18' C13' 119.5(6) . . ? N1S C1S C2S 177.8(14) . . ? O112 N110 O112 180.0(8) 5_676 . ? O112 N110 O111 126.6(4) 5_676 2_656 ? O112 N110 O111 53.4(4) . 2_656 ? O112 N110 O111 53.4(4) 5_676 6_575 ? O112 N110 O111 126.6(4) . 6_575 ? O111 N110 O111 180.000(4) 2_656 6_575 ? O112 N110 O111 126.6(4) 5_676 5_676 ? O112 N110 O111 53.4(4) . 5_676 ? O111 N110 O111 106.8(8) 2_656 5_676 ? O111 N110 O111 73.2(8) 6_575 5_676 ? O112 N110 O111 53.4(4) 5_676 . ? O112 N110 O111 126.6(4) . . ? O111 N110 O111 73.2(8) 2_656 . ? O111 N110 O111 106.8(8) 6_575 . ? O111 N110 O111 180.000(4) 5_676 . ? O112 O111 N110 57.4(6) 5_676 . ? O112 O111 Cd1 178.4(14) 5_676 . ? N110 O111 Cd1 123.7(5) . . ? O111 O112 O111 138.3(14) 5_676 2_656 ? O111 O112 N110 69.2(7) 5_676 . ? O111 O112 N110 69.2(7) 2_656 . ? O212 N210 O212 180.000(10) 5_778 . ? O212 N210 O211 128.3(4) 5_778 5_778 ? O212 N210 O211 51.7(4) . 5_778 ? O212 N210 O211 51.7(4) 5_778 . ? O212 N210 O211 128.3(4) . . ? O211 N210 O211 180.000(5) 5_778 . ? O212 N210 O211 51.7(4) 5_778 6_575 ? O212 N210 O211 128.3(4) . 6_575 ? O211 N210 O211 76.6(8) 5_778 6_575 ? O211 N210 O211 103.4(8) . 6_575 ? O212 N210 O211 128.3(4) 5_778 2_758 ? O212 N210 O211 51.7(4) . 2_758 ? O211 N210 O211 103.4(8) 5_778 2_758 ? O211 N210 O211 76.6(8) . 2_758 ? O211 N210 O211 180.0(9) 6_575 2_758 ? O212 O211 N210 54.9(6) 5_778 . ? O212 O211 O211 106.6(7) 5_778 2_758 ? N210 O211 O211 51.7(4) . 2_758 ? O212 O211 Cd2 175.5(10) 5_778 . ? N210 O211 Cd2 121.0(6) . . ? O211 O211 Cd2 69.3(2) 2_758 . ? O211 O212 O211 146.7(15) 5_778 2_758 ? O211 O212 N210 73.4(7) 5_778 . ? O211 O212 N210 73.4(7) 2_758 . ? Cl1A C1A Cl1A 109.8(12) 2_657 . ? C1A Cl1A C1A 43.3(13) 2_657 . ? N1V C1V C2V 176(3) . . ? N1U C1U C2U 169(3) . . ? C1T N1T N1T 152(2) . 6_565 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.579 _refine_diff_density_min -1.565 _refine_diff_density_rms 0.144 #===END data_CDBPTZ _database_code_CSD 151817 _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'Cadmium(II)-Bis(bis(4-pyridyl)triazine)(Acetonitrile)-bis(nitrate)' ; _chemical_name_common 'Cd(NO3)2(dpt)2(MeCN )' _chemical_formula_moiety 'C28 H21 Cd N13 O6' _chemical_formula_sum 'C28 H21 Cd N13 O6' _chemical_formula_weight 747.98 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' 'Cd' 'Cd' -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.792(2) _cell_length_b 10.319(2) _cell_length_c 15.445(3) _cell_angle_alpha 102.529(3) _cell_angle_beta 96.953(3) _cell_angle_gamma 96.495(3) _cell_volume 1496.4(8) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4162 _cell_measurement_theta_min 2.69 _cell_measurement_theta_max 28.58 _exptl_crystal_description sliver _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.660 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 752 _exptl_absorpt_coefficient_mu 0.797 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.731 _exptl_absorpt_correction_T_max 0.888 _exptl_absorpt_process_details ? _exptl_special_details ; 'Cadmium(II)-Bis(bis(4-pyridyl)triazine)(Acetonitrile)-bis(nitrate)' ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 15595 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0336 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 28.83 _reflns_number_total 6974 _reflns_number_gt 5968 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART version 5.054 (Bruker, 1998)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT version 6.01 (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (version 5.03)(Sheldrick,1994)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0486P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'direct methods' _atom_sites_solution_secondary 'difference Fourier synthesis' _atom_sites_solution_hydrogens 'MeCN from delta-F; others placed geometrically' _refine_ls_hydrogen_treatment 'rigid rotor for MeCN; others riding' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6974 _refine_ls_number_parameters 434 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0388 _refine_ls_R_factor_gt 0.0302 _refine_ls_wR_factor_ref 0.0802 _refine_ls_wR_factor_gt 0.0717 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd -0.301258(16) -0.238695(16) -0.003694(11) 0.02453(6) Uani 1 1 d . . . N100 N -0.1861(2) -0.3852(2) 0.11672(15) 0.0342(5) Uani 1 1 d . . . O101 O -0.31248(18) -0.3721(2) 0.10023(14) 0.0438(5) Uani 1 1 d . . . O102 O -0.10358(18) -0.3272(2) 0.07566(14) 0.0444(5) Uani 1 1 d . . . O103 O -0.1495(2) -0.4526(3) 0.16905(17) 0.0608(7) Uani 1 1 d . . . N200 N -0.2112(2) -0.0757(2) -0.11541(15) 0.0315(5) Uani 1 1 d . . . O201 O -0.12613(17) -0.13438(17) -0.07497(12) 0.0317(4) Uani 1 1 d . . . O202 O -0.33498(18) -0.0882(2) -0.10014(14) 0.0410(5) Uani 1 1 d . . . O203 O -0.1750(2) -0.0071(2) -0.16691(16) 0.0554(6) Uani 1 1 d . . . N1 N -0.3052(2) -0.42260(18) -0.11826(13) 0.0256(4) Uani 1 1 d . . . C2 C -0.4212(2) -0.5118(2) -0.14678(16) 0.0273(5) Uani 1 1 d . . . H2A H -0.5060 -0.4873 -0.1288 0.033 Uiso 1 1 calc R . . C3 C -0.4232(2) -0.6380(2) -0.20136(16) 0.0266(5) Uani 1 1 d . . . H3A H -0.5072 -0.6990 -0.2191 0.032 Uiso 1 1 calc R . . C4 C -0.3008(2) -0.6738(2) -0.22959(15) 0.0223(4) Uani 1 1 d . . . C5 C -0.1809(2) -0.5803(2) -0.20242(16) 0.0277(5) Uani 1 1 d . . . H5A H -0.0956 -0.6008 -0.2215 0.033 Uiso 1 1 calc R . . C6 C -0.1875(2) -0.4569(2) -0.14716(16) 0.0287(5) Uani 1 1 d . . . H6A H -0.1051 -0.3937 -0.1289 0.034 Uiso 1 1 calc R . . C7 C -0.2953(2) -0.8100(2) -0.28451(15) 0.0235(5) Uani 1 1 d . . . N8 N -0.1729(2) -0.83650(18) -0.30732(13) 0.0242(4) Uani 1 1 d . . . C9 C -0.1711(2) -0.9618(2) -0.35403(15) 0.0243(5) Uani 1 1 d . . . N10 N -0.2833(2) -1.0568(2) -0.38065(15) 0.0327(5) Uani 1 1 d . . . C11 C -0.3998(3) -1.0172(2) -0.35508(18) 0.0344(6) Uani 1 1 d . . . H11A H -0.4816 -1.0813 -0.3731 0.041 Uiso 1 1 calc R . . N12 N -0.4139(2) -0.8970(2) -0.30681(14) 0.0310(5) Uani 1 1 d . . . C13 C -0.0350(2) -0.9969(2) -0.37610(15) 0.0243(5) Uani 1 1 d . . . C14 C -0.0241(2) -1.1221(2) -0.42913(15) 0.0264(5) Uani 1 1 d . . . H14A H -0.1042 -1.1873 -0.4523 0.032 Uiso 1 1 calc R . . C15 C 0.1064(3) -1.1493(2) -0.44729(16) 0.0303(5) Uani 1 1 d . . . H15A H 0.1127 -1.2347 -0.4838 0.036 Uiso 1 1 calc R . . N16 N 0.2241(2) -1.0633(2) -0.41682(14) 0.0313(5) Uani 1 1 d . . . C17 C 0.2116(3) -0.9431(2) -0.36576(17) 0.0303(5) Uani 1 1 d . . . H17A H 0.2935 -0.8802 -0.3431 0.036 Uiso 1 1 calc R . . C18 C 0.0864(2) -0.9058(2) -0.34435(16) 0.0279(5) Uani 1 1 d . . . H18A H 0.0831 -0.8192 -0.3085 0.034 Uiso 1 1 calc R . . N31 N -0.27142(19) -0.05287(19) 0.11194(13) 0.0250(4) Uani 1 1 d . . . C32 C -0.1456(2) 0.0179(2) 0.14509(16) 0.0291(5) Uani 1 1 d . . . H32A H -0.0661 -0.0184 0.1264 0.035 Uiso 1 1 calc R . . C33 C -0.1260(2) 0.1419(2) 0.20550(16) 0.0274(5) Uani 1 1 d . . . H33A H -0.0352 0.1894 0.2272 0.033 Uiso 1 1 calc R . . C34 C -0.2409(2) 0.1951(2) 0.23352(15) 0.0228(5) Uani 1 1 d . . . C35 C -0.3714(2) 0.1197(2) 0.20187(17) 0.0315(5) Uani 1 1 d . . . H35A H -0.4522 0.1519 0.2214 0.038 Uiso 1 1 calc R . . C36 C -0.3817(2) -0.0025(2) 0.14166(17) 0.0335(6) Uani 1 1 d . . . H36A H -0.4712 -0.0532 0.1203 0.040 Uiso 1 1 calc R . . C37 C -0.2309(2) 0.3297(2) 0.29488(15) 0.0237(5) Uani 1 1 d . . . N38 N -0.35126(19) 0.36761(19) 0.31504(13) 0.0254(4) Uani 1 1 d . . . C39 C -0.3427(2) 0.4907(2) 0.36731(15) 0.0256(5) Uani 1 1 d . . . N40 N -0.2243(2) 0.5762(2) 0.39771(14) 0.0321(5) Uani 1 1 d . . . C41 C -0.1107(3) 0.5259(2) 0.37445(17) 0.0325(5) Uani 1 1 d . . . H41A H -0.0244 0.5827 0.3958 0.039 Uiso 1 1 calc R . . N42 N -0.1059(2) 0.4036(2) 0.32411(14) 0.0291(4) Uani 1 1 d . . . C43 C -0.4761(2) 0.5317(2) 0.39222(15) 0.0256(5) Uani 1 1 d . . . C44 C -0.4846(3) 0.6607(2) 0.44093(16) 0.0296(5) Uani 1 1 d . . . H44A H -0.4042 0.7265 0.4596 0.035 Uiso 1 1 calc R . . C45 C -0.6129(3) 0.6904(3) 0.46129(17) 0.0329(6) Uani 1 1 d . . . H45A H -0.6178 0.7790 0.4933 0.040 Uiso 1 1 calc R . . N46 N -0.7303(2) 0.6035(2) 0.43917(14) 0.0331(5) Uani 1 1 d . . . C47 C -0.7204(3) 0.4801(2) 0.39236(16) 0.0311(5) Uani 1 1 d . . . H47A H -0.8026 0.4166 0.3751 0.037 Uiso 1 1 calc R . . C48 C -0.5983(3) 0.4398(2) 0.36765(16) 0.0294(5) Uani 1 1 d . . . H48A H -0.5973 0.3509 0.3345 0.035 Uiso 1 1 calc R . . N1S N -0.5501(2) -0.2665(2) -0.01303(14) 0.0329(5) Uani 1 1 d . . . C1S C -0.6643(3) -0.2705(2) -0.00738(16) 0.0281(5) Uani 1 1 d . . . C2S C -0.8112(3) -0.2737(3) 0.0014(2) 0.0477(8) Uani 1 1 d . . . H2S1 H -0.8548 -0.3670 -0.0081 0.071 Uiso 1 1 calc R . . H2S2 H -0.8572 -0.2324 -0.0434 0.071 Uiso 1 1 calc R . . H2S3 H -0.8204 -0.2240 0.0616 0.071 Uiso 1 1 calc R . . 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 Cd1 0.02265(9) 0.02072(9) 0.02650(10) -0.00314(6) 0.00621(6) 0.00172(6) N100 0.0250(10) 0.0373(12) 0.0376(12) 0.0063(10) 0.0027(9) 0.0005(9) O101 0.0241(9) 0.0515(12) 0.0626(13) 0.0276(10) 0.0091(9) 0.0039(8) O102 0.0260(9) 0.0639(13) 0.0486(12) 0.0230(10) 0.0109(8) 0.0041(9) O103 0.0401(12) 0.0840(17) 0.0705(16) 0.0490(14) -0.0001(11) 0.0087(11) N200 0.0245(10) 0.0346(11) 0.0341(12) 0.0067(9) 0.0046(8) 0.0007(9) O201 0.0239(8) 0.0339(9) 0.0388(10) 0.0112(8) 0.0056(7) 0.0050(7) O202 0.0219(9) 0.0539(12) 0.0522(12) 0.0200(10) 0.0092(8) 0.0079(8) O203 0.0391(11) 0.0791(16) 0.0624(14) 0.0452(13) 0.0127(10) 0.0077(11) N1 0.0244(9) 0.0218(9) 0.0263(10) -0.0039(8) 0.0052(8) 0.0021(8) C2 0.0228(11) 0.0269(12) 0.0296(12) -0.0007(10) 0.0079(9) 0.0024(9) C3 0.0231(11) 0.0233(11) 0.0286(12) -0.0025(9) 0.0052(9) -0.0009(9) C4 0.0256(11) 0.0203(10) 0.0193(11) 0.0013(8) 0.0028(8) 0.0042(9) C5 0.0219(11) 0.0255(11) 0.0322(13) -0.0018(10) 0.0061(9) 0.0035(9) C6 0.0209(11) 0.0265(12) 0.0329(13) -0.0041(10) 0.0048(9) 0.0007(9) C7 0.0248(11) 0.0224(11) 0.0214(11) 0.0014(9) 0.0030(9) 0.0036(9) N8 0.0258(9) 0.0207(9) 0.0242(10) 0.0007(8) 0.0041(8) 0.0039(8) C9 0.0270(11) 0.0221(11) 0.0212(11) -0.0006(9) 0.0039(9) 0.0030(9) N10 0.0295(11) 0.0238(10) 0.0377(12) -0.0068(9) 0.0066(9) 0.0003(8) C11 0.0284(12) 0.0278(12) 0.0383(15) -0.0073(11) 0.0053(10) -0.0034(10) N12 0.0258(10) 0.0263(10) 0.0350(12) -0.0037(9) 0.0050(8) 0.0003(8) C13 0.0277(11) 0.0216(11) 0.0224(11) 0.0019(9) 0.0036(9) 0.0055(9) C14 0.0300(12) 0.0208(11) 0.0252(12) -0.0007(9) 0.0018(9) 0.0045(9) C15 0.0366(13) 0.0266(12) 0.0251(12) -0.0017(10) 0.0028(10) 0.0113(10) N16 0.0311(11) 0.0318(11) 0.0306(11) 0.0025(9) 0.0066(9) 0.0109(9) C17 0.0279(12) 0.0279(12) 0.0322(13) 0.0013(10) 0.0038(10) 0.0044(10) C18 0.0322(12) 0.0212(11) 0.0274(12) -0.0017(9) 0.0055(10) 0.0047(9) N31 0.0231(9) 0.0237(9) 0.0251(10) -0.0015(8) 0.0041(8) 0.0032(8) C32 0.0238(11) 0.0266(12) 0.0340(13) -0.0024(10) 0.0089(10) 0.0047(9) C33 0.0211(11) 0.0273(12) 0.0301(13) 0.0000(10) 0.0046(9) 0.0000(9) C34 0.0238(11) 0.0221(11) 0.0210(11) 0.0008(9) 0.0032(8) 0.0052(9) C35 0.0212(11) 0.0307(12) 0.0351(14) -0.0085(10) 0.0034(10) 0.0051(10) C36 0.0231(11) 0.0301(13) 0.0378(14) -0.0106(11) 0.0023(10) 0.0026(10) C37 0.0257(11) 0.0227(11) 0.0212(11) 0.0019(9) 0.0029(9) 0.0048(9) N38 0.0246(9) 0.0237(9) 0.0251(10) -0.0014(8) 0.0031(8) 0.0060(8) C39 0.0301(12) 0.0234(11) 0.0207(11) 0.0004(9) 0.0018(9) 0.0051(9) N40 0.0337(11) 0.0244(10) 0.0330(12) -0.0036(9) 0.0057(9) 0.0022(9) C41 0.0294(12) 0.0265(12) 0.0348(14) -0.0034(10) 0.0026(10) -0.0008(10) N42 0.0262(10) 0.0261(10) 0.0308(11) -0.0006(8) 0.0021(8) 0.0021(8) C43 0.0305(12) 0.0260(11) 0.0199(11) 0.0015(9) 0.0040(9) 0.0095(10) C44 0.0364(13) 0.0261(12) 0.0228(12) -0.0011(9) 0.0015(10) 0.0064(10) C45 0.0405(14) 0.0313(13) 0.0256(13) -0.0012(10) 0.0030(10) 0.0166(11) N46 0.0366(11) 0.0336(11) 0.0287(11) 0.0009(9) 0.0063(9) 0.0141(9) C47 0.0301(12) 0.0321(13) 0.0297(13) 0.0026(10) 0.0048(10) 0.0067(10) C48 0.0341(13) 0.0239(11) 0.0286(13) 0.0006(10) 0.0051(10) 0.0082(10) N1S 0.0265(11) 0.0332(11) 0.0349(12) 0.0009(9) 0.0041(9) 0.0011(9) C1S 0.0279(12) 0.0282(12) 0.0264(12) 0.0053(10) 0.0026(9) 0.0007(10) C2S 0.0250(13) 0.063(2) 0.060(2) 0.0236(17) 0.0082(13) 0.0052(13) _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 Cd1 N31 2.2832(19) . y Cd1 N1 2.2900(18) . y Cd1 O101 2.3346(19) . y Cd1 O202 2.396(2) . y Cd1 N1S 2.404(2) . y Cd1 O201 2.4218(17) . y Cd1 O102 2.529(2) . y N100 O103 1.223(3) . ? N100 O101 1.261(3) . ? N100 O102 1.262(3) . ? N200 O203 1.231(3) . ? N200 O202 1.260(3) . ? N200 O201 1.266(3) . ? N1 C2 1.341(3) . ? N1 C6 1.342(3) . ? C2 C3 1.386(3) . ? C3 C4 1.385(3) . ? C4 C5 1.391(3) . ? C4 C7 1.486(3) . ? C5 C6 1.383(3) . ? C7 N8 1.330(3) . ? C7 N12 1.344(3) . ? N8 C9 1.340(3) . ? C9 N10 1.345(3) . ? C9 C13 1.479(3) . ? N10 C11 1.330(3) . ? C11 N12 1.333(3) . ? C13 C14 1.395(3) . ? C13 C18 1.395(3) . ? C14 C15 1.387(3) . ? C15 N16 1.340(3) . ? N16 C17 1.345(3) . ? C17 C18 1.382(3) . ? N31 C36 1.338(3) . ? N31 C32 1.340(3) . ? C32 C33 1.389(3) . ? C33 C34 1.381(3) . ? C34 C35 1.391(3) . ? C34 C37 1.487(3) . ? C35 C36 1.380(3) . ? C37 N38 1.334(3) . ? C37 N42 1.338(3) . ? N38 C39 1.337(3) . ? C39 N40 1.341(3) . ? C39 C43 1.486(3) . ? N40 C41 1.335(3) . ? C41 N42 1.340(3) . ? C43 C44 1.396(3) . ? C43 C48 1.398(3) . ? C44 C45 1.383(4) . ? C45 N46 1.335(3) . ? N46 C47 1.341(3) . ? C47 C48 1.379(3) . ? N1S C1S 1.129(3) . ? C1S C2S 1.459(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 N31 Cd1 N1 173.72(6) . . y N31 Cd1 O101 88.96(8) . . y N1 Cd1 O101 91.47(8) . . y N31 Cd1 O202 85.98(7) . . y N1 Cd1 O202 94.78(7) . . y O101 Cd1 O202 167.73(6) . . y N31 Cd1 N1S 92.90(7) . . y N1 Cd1 N1S 93.37(7) . . y O101 Cd1 N1S 84.11(7) . . y O202 Cd1 N1S 84.99(7) . . y N31 Cd1 O201 91.03(6) . . y N1 Cd1 O201 84.47(6) . . y O101 Cd1 O201 138.10(6) . . y O202 Cd1 O201 53.29(6) . . y N1S Cd1 O201 137.69(7) . . y N31 Cd1 O102 90.04(7) . . y N1 Cd1 O102 85.29(7) . . y O101 Cd1 O102 52.11(6) . . y O202 Cd1 O102 138.92(6) . . y N1S Cd1 O102 136.07(7) . . y O201 Cd1 O102 85.99(6) . . y O103 N100 O101 120.2(2) . . ? O103 N100 O102 123.5(2) . . ? O101 N100 O102 116.3(2) . . ? N100 O101 Cd1 100.49(15) . . ? N100 O102 Cd1 91.14(14) . . ? O203 N200 O202 120.7(2) . . ? O203 N200 O201 121.7(2) . . ? O202 N200 O201 117.6(2) . . ? N200 O201 Cd1 93.80(13) . . ? N200 O202 Cd1 95.21(14) . . ? C2 N1 C6 117.68(19) . . ? C2 N1 Cd1 120.12(15) . . ? C6 N1 Cd1 121.12(14) . . ? N1 C2 C3 123.0(2) . . ? C4 C3 C2 119.1(2) . . ? C3 C4 C5 118.2(2) . . ? C3 C4 C7 121.40(19) . . ? C5 C4 C7 120.3(2) . . ? C6 C5 C4 119.1(2) . . ? N1 C6 C5 122.9(2) . . ? N8 C7 N12 125.1(2) . . ? N8 C7 C4 117.37(19) . . ? N12 C7 C4 117.6(2) . . ? C7 N8 C9 115.56(19) . . ? N8 C9 N10 124.6(2) . . ? N8 C9 C13 116.97(19) . . ? N10 C9 C13 118.5(2) . . ? C11 N10 C9 114.1(2) . . ? N10 C11 N12 126.8(2) . . ? C11 N12 C7 113.9(2) . . ? C14 C13 C18 117.9(2) . . ? C14 C13 C9 121.1(2) . . ? C18 C13 C9 120.9(2) . . ? C15 C14 C13 118.4(2) . . ? N16 C15 C14 124.4(2) . . ? C15 N16 C17 116.4(2) . . ? N16 C17 C18 123.8(2) . . ? C17 C18 C13 119.1(2) . . ? C36 N31 C32 117.62(19) . . ? C36 N31 Cd1 120.34(15) . . ? C32 N31 Cd1 121.60(15) . . ? N31 C32 C33 123.0(2) . . ? C34 C33 C32 118.9(2) . . ? C33 C34 C35 118.3(2) . . ? C33 C34 C37 122.8(2) . . ? C35 C34 C37 118.9(2) . . ? C36 C35 C34 119.1(2) . . ? N31 C36 C35 123.0(2) . . ? N38 C37 N42 125.1(2) . . ? N38 C37 C34 115.71(19) . . ? N42 C37 C34 119.1(2) . . ? C37 N38 C39 115.70(19) . . ? N38 C39 N40 124.6(2) . . ? N38 C39 C43 115.8(2) . . ? N40 C39 C43 119.5(2) . . ? C41 N40 C39 114.0(2) . . ? N40 C41 N42 126.7(2) . . ? C37 N42 C41 113.7(2) . . ? C44 C43 C48 117.7(2) . . ? C44 C43 C39 122.2(2) . . ? C48 C43 C39 120.1(2) . . ? C45 C44 C43 118.4(2) . . ? N46 C45 C44 124.7(2) . . ? C45 N46 C47 116.2(2) . . ? N46 C47 C48 124.1(2) . . ? C47 C48 C43 118.9(2) . . ? C1S N1S Cd1 171.9(2) . . ? N1S C1S C2S 179.0(3) . . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O103 N100 O101 Cd1 -178.9(2) . . . . ? O102 N100 O101 Cd1 0.1(2) . . . . ? N31 Cd1 O101 N100 -90.93(16) . . . . ? N1 Cd1 O101 N100 82.80(16) . . . . ? O202 Cd1 O101 N100 -156.5(3) . . . . ? N1S Cd1 O101 N100 176.04(17) . . . . ? O201 Cd1 O101 N100 -0.6(2) . . . . ? O102 Cd1 O101 N100 -0.08(14) . . . . ? O103 N100 O102 Cd1 178.9(2) . . . . ? O101 N100 O102 Cd1 -0.1(2) . . . . ? N31 Cd1 O102 N100 88.73(15) . . . . ? N1 Cd1 O102 N100 -95.47(15) . . . . ? O101 Cd1 O102 N100 0.08(14) . . . . ? O202 Cd1 O102 N100 172.65(13) . . . . ? N1S Cd1 O102 N100 -5.50(19) . . . . ? O201 Cd1 O102 N100 179.76(15) . . . . ? O203 N200 O201 Cd1 -177.7(2) . . . . ? O202 N200 O201 Cd1 3.3(2) . . . . ? N31 Cd1 O201 N200 -86.15(14) . . . . ? N1 Cd1 O201 N200 98.24(14) . . . . ? O101 Cd1 O201 N200 -175.73(13) . . . . ? O202 Cd1 O201 N200 -1.93(13) . . . . ? N1S Cd1 O201 N200 9.31(18) . . . . ? O102 Cd1 O201 N200 -176.11(14) . . . . ? O203 N200 O202 Cd1 177.6(2) . . . . ? O201 N200 O202 Cd1 -3.4(2) . . . . ? N31 Cd1 O202 N200 96.24(15) . . . . ? N1 Cd1 O202 N200 -77.51(15) . . . . ? O101 Cd1 O202 N200 162.1(3) . . . . ? N1S Cd1 O202 N200 -170.49(15) . . . . ? O201 Cd1 O202 N200 1.95(13) . . . . ? O102 Cd1 O202 N200 10.8(2) . . . . ? N31 Cd1 N1 C2 163.5(6) . . . . ? O101 Cd1 N1 C2 69.68(18) . . . . ? O202 Cd1 N1 C2 -99.76(18) . . . . ? N1S Cd1 N1 C2 -14.51(19) . . . . ? O201 Cd1 N1 C2 -152.11(19) . . . . ? O102 Cd1 N1 C2 121.47(18) . . . . ? N31 Cd1 N1 C6 -4.3(7) . . . . ? O101 Cd1 N1 C6 -98.14(19) . . . . ? O202 Cd1 N1 C6 92.43(19) . . . . ? N1S Cd1 N1 C6 177.68(19) . . . . ? O201 Cd1 N1 C6 40.07(19) . . . . ? O102 Cd1 N1 C6 -46.35(19) . . . . ? C6 N1 C2 C3 2.5(4) . . . . ? Cd1 N1 C2 C3 -165.73(18) . . . . ? N1 C2 C3 C4 -1.3(4) . . . . ? C2 C3 C4 C5 -0.6(4) . . . . ? C2 C3 C4 C7 177.0(2) . . . . ? C3 C4 C5 C6 1.3(4) . . . . ? C7 C4 C5 C6 -176.4(2) . . . . ? C2 N1 C6 C5 -1.8(4) . . . . ? Cd1 N1 C6 C5 166.31(19) . . . . ? C4 C5 C6 N1 -0.1(4) . . . . ? C3 C4 C7 N8 -178.8(2) . . . . ? C5 C4 C7 N8 -1.2(3) . . . . ? C3 C4 C7 N12 0.8(3) . . . . ? C5 C4 C7 N12 178.4(2) . . . . ? N12 C7 N8 C9 -1.9(3) . . . . ? C4 C7 N8 C9 177.67(19) . . . . ? C7 N8 C9 N10 2.4(3) . . . . ? C7 N8 C9 C13 -176.7(2) . . . . ? N8 C9 N10 C11 -1.2(4) . . . . ? C13 C9 N10 C11 177.8(2) . . . . ? C9 N10 C11 N12 -0.6(4) . . . . ? N10 C11 N12 C7 1.0(4) . . . . ? N8 C7 N12 C11 0.3(4) . . . . ? C4 C7 N12 C11 -179.2(2) . . . . ? N8 C9 C13 C14 -176.0(2) . . . . ? N10 C9 C13 C14 4.9(3) . . . . ? N8 C9 C13 C18 4.1(3) . . . . ? N10 C9 C13 C18 -175.0(2) . . . . ? C18 C13 C14 C15 0.1(3) . . . . ? C9 C13 C14 C15 -179.8(2) . . . . ? C13 C14 C15 N16 0.4(4) . . . . ? C14 C15 N16 C17 -0.3(4) . . . . ? C15 N16 C17 C18 -0.2(4) . . . . ? N16 C17 C18 C13 0.7(4) . . . . ? C14 C13 C18 C17 -0.6(4) . . . . ? C9 C13 C18 C17 179.3(2) . . . . ? N1 Cd1 N31 C36 178.6(6) . . . . ? O101 Cd1 N31 C36 -87.4(2) . . . . ? O202 Cd1 N31 C36 81.4(2) . . . . ? N1S Cd1 N31 C36 -3.4(2) . . . . ? O201 Cd1 N31 C36 134.5(2) . . . . ? O102 Cd1 N31 C36 -139.5(2) . . . . ? N1 Cd1 N31 C32 6.5(7) . . . . ? O101 Cd1 N31 C32 100.42(19) . . . . ? O202 Cd1 N31 C32 -90.76(19) . . . . ? N1S Cd1 N31 C32 -175.53(19) . . . . ? O201 Cd1 N31 C32 -37.68(19) . . . . ? O102 Cd1 N31 C32 48.32(19) . . . . ? C36 N31 C32 C33 -2.5(4) . . . . ? Cd1 N31 C32 C33 169.84(19) . . . . ? N31 C32 C33 C34 0.5(4) . . . . ? C32 C33 C34 C35 1.9(4) . . . . ? C32 C33 C34 C37 -177.3(2) . . . . ? C33 C34 C35 C36 -2.2(4) . . . . ? C37 C34 C35 C36 177.0(2) . . . . ? C32 N31 C36 C35 2.2(4) . . . . ? Cd1 N31 C36 C35 -170.2(2) . . . . ? C34 C35 C36 N31 0.1(4) . . . . ? C33 C34 C37 N38 179.3(2) . . . . ? C35 C34 C37 N38 0.1(3) . . . . ? C33 C34 C37 N42 0.5(3) . . . . ? C35 C34 C37 N42 -178.7(2) . . . . ? N42 C37 N38 C39 1.3(4) . . . . ? C34 C37 N38 C39 -177.43(19) . . . . ? C37 N38 C39 N40 1.6(3) . . . . ? C37 N38 C39 C43 -178.2(2) . . . . ? N38 C39 N40 C41 -2.8(4) . . . . ? C43 C39 N40 C41 177.0(2) . . . . ? C39 N40 C41 N42 1.3(4) . . . . ? N38 C37 N42 C41 -2.6(4) . . . . ? C34 C37 N42 C41 176.1(2) . . . . ? N40 C41 N42 C37 1.2(4) . . . . ? N38 C39 C43 C44 -175.2(2) . . . . ? N40 C39 C43 C44 5.0(4) . . . . ? N38 C39 C43 C48 5.4(3) . . . . ? N40 C39 C43 C48 -174.4(2) . . . . ? C48 C43 C44 C45 -0.6(3) . . . . ? C39 C43 C44 C45 -180.0(2) . . . . ? C43 C44 C45 N46 1.3(4) . . . . ? C44 C45 N46 C47 -1.4(4) . . . . ? C45 N46 C47 C48 0.7(4) . . . . ? N46 C47 C48 C43 0.0(4) . . . . ? C44 C43 C48 C47 0.0(4) . . . . ? C39 C43 C48 C47 179.4(2) . . . . ? N31 Cd1 N1S C1S -20.4(15) . . . . ? N1 Cd1 N1S C1S 159.4(15) . . . . ? O101 Cd1 N1S C1S 68.3(15) . . . . ? O202 Cd1 N1S C1S -106.1(15) . . . . ? O201 Cd1 N1S C1S -115.1(15) . . . . ? O102 Cd1 N1S C1S 72.7(15) . . . . ? Cd1 N1S C1S C2S 13(19) . . . . ? _diffrn_measured_fraction_theta_max 0.891 _diffrn_reflns_theta_full 28.83 _diffrn_measured_fraction_theta_full 0.891 _refine_diff_density_max 0.586 _refine_diff_density_min -0.748 _refine_diff_density_rms 0.113 #===END data_cddptn _database_code_CSD 151818 _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'Cadmium(II)-(bis(4-pyridyl)triazine)(ethanol)-bis(nitrate)' ; _chemical_name_common Cd(NO3)2(dpt)(EtOH) _chemical_formula_moiety 'C15 H15 Cd N7 O7' _chemical_formula_sum 'C15 H15 Cd N7 O7' _chemical_formula_weight 517.74 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' 'Cd' 'Cd' -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9014(10) _cell_length_b 10.3249(12) _cell_length_c 10.4451(12) _cell_angle_alpha 77.397(2) _cell_angle_beta 86.866(2) _cell_angle_gamma 86.988(2) _cell_volume 934.62(19) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4042 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 28.05 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.840 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 516 _exptl_absorpt_coefficient_mu 1.225 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.754 _exptl_absorpt_correction_T_max 0.929 _exptl_absorpt_process_details 'SHELXTL/PC version 5.10 (Bruker, 1997)' _exptl_special_details ; 'Cadmium(II)-(bis(4-pyridyl)triazine)(ethanol)-bis(nitrate)' ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 7088 _diffrn_reflns_av_R_equivalents 0.031 _diffrn_reflns_av_sigmaI/netI 0.033 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 28.53 _reflns_number_total 4097 _reflns_number_gt 3469 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART version 5.054 (Bruker, 1998)' _computing_cell_refinement SAINT _computing_data_reduction 'SAINT; SHELXTL version 5.10 (Bruker,1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (version 5.03)(Sheldrick,1994)' _computing_publication_material 'SHELXL-97; PLATON (Spek, 2000)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0321P)^2^+0.169P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'direct methods' _atom_sites_solution_secondary 'difference Fourier synthesis' _atom_sites_solution_hydrogens ; all placed geometrically except OH of ethanol was found in the diffence map ; _refine_ls_hydrogen_treatment ; all riding model except OH of ethanol free to refine isotropically ; _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4097 _refine_ls_number_parameters 276 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0374 _refine_ls_R_factor_gt 0.0261 _refine_ls_wR_factor_ref 0.0602 _refine_ls_wR_factor_gt 0.0565 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.11830(2) 0.671878(18) 0.174114(18) 0.02356(6) Uani 1 1 d . . . N200 N 0.3210(3) 0.4796(2) 0.3032(2) 0.0321(5) Uani 1 1 d . . . O201 O 0.2933(2) 0.48748(18) 0.18399(19) 0.0354(5) Uani 1 1 d . . . O202 O 0.2528(2) 0.56229(19) 0.3611(2) 0.0370(5) Uani 1 1 d . . . O203 O 0.4107(3) 0.3951(2) 0.3596(2) 0.0496(6) Uani 1 1 d . . . N100 N -0.0400(3) 0.7499(2) -0.0651(2) 0.0266(5) Uani 1 1 d . . . O101 O 0.0435(2) 0.64458(18) -0.04370(19) 0.0338(4) Uani 1 1 d . . . O102 O -0.0484(2) 0.81769(17) 0.02204(18) 0.0286(4) Uani 1 1 d . . . O103 O -0.1090(3) 0.7847(2) -0.1657(2) 0.0436(5) Uani 1 1 d . . . N1 N 0.0098(2) 0.7993(2) 0.3119(2) 0.0232(4) Uani 1 1 d . . . C2 C -0.0358(3) 0.7428(3) 0.4357(2) 0.0262(5) Uani 1 1 d . . . H2A H -0.0025 0.6540 0.4713 0.031 Uiso 1 1 calc R . . C3 C -0.1286(3) 0.8084(2) 0.5131(2) 0.0243(5) Uani 1 1 d . . . H3A H -0.1600 0.7651 0.5995 0.029 Uiso 1 1 calc R . . C4 C -0.1755(3) 0.9394(2) 0.4621(2) 0.0200(5) Uani 1 1 d . . . C5 C -0.1225(3) 1.0008(2) 0.3372(2) 0.0225(5) Uani 1 1 d . . . H5A H -0.1469 1.0918 0.3020 0.027 Uiso 1 1 calc R . . C6 C -0.0331(3) 0.9261(2) 0.2654(2) 0.0230(5) Uani 1 1 d . . . H6A H -0.0004 0.9670 0.1786 0.028 Uiso 1 1 calc R . . C7 C -0.2820(3) 1.0129(2) 0.5375(2) 0.0201(5) Uani 1 1 d . . . N8 N -0.3531(2) 0.9414(2) 0.6436(2) 0.0223(4) Uani 1 1 d . . . C9 C -0.4502(3) 1.0111(2) 0.7068(2) 0.0206(5) Uani 1 1 d . . . N10 N -0.4793(3) 1.1418(2) 0.6717(2) 0.0270(5) Uani 1 1 d . . . C11 C -0.4027(3) 1.2022(2) 0.5641(3) 0.0280(6) Uani 1 1 d . . . H11A H -0.4206 1.2954 0.5359 0.034 Uiso 1 1 calc R . . N12 N -0.3030(2) 1.1438(2) 0.4923(2) 0.0256(5) Uani 1 1 d . . . C13 C -0.5334(3) 0.9359(2) 0.8242(2) 0.0216(5) Uani 1 1 d . . . C14 C -0.6340(3) 1.0015(2) 0.8975(2) 0.0232(5) Uani 1 1 d . . . H14A H -0.6484 1.0954 0.8748 0.028 Uiso 1 1 calc R . . C15 C -0.7128(3) 0.9273(2) 1.0040(2) 0.0240(5) Uani 1 1 d . . . H15A H -0.7798 0.9728 1.0547 0.029 Uiso 1 1 calc R . . N16 N -0.6993(2) 0.7948(2) 1.0392(2) 0.0247(4) Uani 1 1 d . . . C17 C -0.5998(3) 0.7326(3) 0.9688(3) 0.0323(6) Uani 1 1 d . . . H17A H -0.5870 0.6387 0.9938 0.039 Uiso 1 1 calc R . . C18 C -0.5158(3) 0.7990(3) 0.8621(3) 0.0307(6) Uani 1 1 d . . . H18A H -0.4465 0.7514 0.8151 0.037 Uiso 1 1 calc R . . O1S O -0.0438(2) 0.49833(19) 0.2438(2) 0.0331(4) Uani 1 1 d . . . C1S C -0.2012(3) 0.4979(3) 0.2834(3) 0.0419(7) Uani 1 1 d . . . H1S1 H -0.2153 0.5293 0.3664 0.050 Uiso 1 1 calc R . . H1S2 H -0.2355 0.4058 0.3001 0.050 Uiso 1 1 calc R . . C2S C -0.2951(4) 0.5841(4) 0.1818(4) 0.0577(10) Uani 1 1 d . . . H2S1 H -0.2611 0.6753 0.1646 0.087 Uiso 1 1 calc R . . H2S2 H -0.4008 0.5827 0.2135 0.087 Uiso 1 1 calc R . . H2S3 H -0.2850 0.5509 0.1006 0.087 Uiso 1 1 calc R . . H1S H -0.030(5) 0.452(4) 0.190(4) 0.068(13) Uiso 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 Cd1 0.02408(10) 0.02393(9) 0.02132(10) -0.00430(6) 0.00531(7) 0.00249(6) N200 0.0255(12) 0.0239(11) 0.0428(14) 0.0008(10) 0.0028(10) -0.0016(9) O201 0.0394(12) 0.0311(10) 0.0326(11) -0.0040(8) 0.0087(9) 0.0050(8) O202 0.0388(12) 0.0357(10) 0.0376(11) -0.0109(9) -0.0048(9) 0.0054(9) O203 0.0425(13) 0.0384(12) 0.0601(15) 0.0043(10) -0.0060(11) 0.0124(10) N100 0.0303(12) 0.0262(11) 0.0227(11) -0.0034(8) 0.0033(9) -0.0091(9) O101 0.0419(11) 0.0276(9) 0.0338(10) -0.0123(8) 0.0016(9) 0.0008(8) O102 0.0302(10) 0.0292(9) 0.0285(10) -0.0113(7) -0.0002(8) 0.0004(8) O103 0.0559(14) 0.0457(12) 0.0292(11) -0.0025(9) -0.0152(10) -0.0112(11) N1 0.0214(11) 0.0268(10) 0.0208(10) -0.0054(8) 0.0034(9) 0.0001(8) C2 0.0267(13) 0.0280(12) 0.0216(12) -0.0020(10) 0.0017(10) 0.0026(10) C3 0.0244(13) 0.0278(12) 0.0191(12) -0.0028(9) 0.0023(10) 0.0002(10) C4 0.0157(11) 0.0278(12) 0.0178(11) -0.0072(9) 0.0003(9) -0.0048(9) C5 0.0225(12) 0.0228(11) 0.0219(12) -0.0045(9) 0.0014(10) -0.0028(9) C6 0.0234(13) 0.0272(12) 0.0177(11) -0.0045(9) 0.0043(10) -0.0016(10) C7 0.0180(11) 0.0252(11) 0.0188(11) -0.0074(9) -0.0020(9) -0.0038(9) N8 0.0193(10) 0.0259(10) 0.0210(10) -0.0048(8) 0.0034(8) -0.0005(8) C9 0.0184(12) 0.0255(12) 0.0189(11) -0.0072(9) -0.0005(9) -0.0003(9) N10 0.0310(12) 0.0255(10) 0.0240(11) -0.0062(8) 0.0042(9) 0.0007(9) C11 0.0330(15) 0.0236(12) 0.0271(13) -0.0060(10) 0.0035(11) -0.0006(10) N12 0.0277(11) 0.0256(10) 0.0229(10) -0.0052(8) 0.0036(9) -0.0019(9) C13 0.0178(12) 0.0280(12) 0.0192(11) -0.0061(9) 0.0004(10) 0.0006(9) C14 0.0189(12) 0.0252(12) 0.0260(12) -0.0079(9) 0.0019(10) 0.0000(9) C15 0.0186(12) 0.0319(13) 0.0227(12) -0.0102(10) 0.0036(10) 0.0021(10) N16 0.0201(11) 0.0312(11) 0.0218(10) -0.0051(8) 0.0038(9) 0.0017(9) C17 0.0319(15) 0.0258(13) 0.0347(15) -0.0015(11) 0.0122(12) 0.0046(11) C18 0.0286(14) 0.0292(13) 0.0316(14) -0.0055(10) 0.0125(12) 0.0045(11) O1S 0.0319(11) 0.0333(10) 0.0365(11) -0.0138(9) 0.0077(9) -0.0056(8) C1S 0.0360(17) 0.0464(17) 0.0439(18) -0.0131(14) 0.0160(14) -0.0128(14) C2S 0.0340(18) 0.049(2) 0.083(3) 0.0002(18) 0.0081(18) -0.0029(15) _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 Cd1 N1 2.297(2) . y Cd1 O1S 2.3260(19) . y Cd1 N16 2.328(2) 1_654 y Cd1 O202 2.383(2) . y Cd1 O201 2.3835(19) . y Cd1 O102 2.4433(19) . y Cd1 O101 2.483(2) . y N200 O203 1.225(3) . ? N200 O202 1.262(3) . ? N200 O201 1.267(3) . ? N100 O103 1.222(3) . ? N100 O102 1.261(3) . ? N100 O101 1.269(3) . ? N1 C6 1.336(3) . ? N1 C2 1.348(3) . ? C2 C3 1.378(4) . ? C3 C4 1.392(3) . ? C4 C5 1.389(3) . ? C4 C7 1.483(3) . ? C5 C6 1.383(3) . ? C7 N12 1.337(3) . ? C7 N8 1.338(3) . ? N8 C9 1.334(3) . ? C9 N10 1.335(3) . ? C9 C13 1.483(3) . ? N10 C11 1.331(3) . ? C11 N12 1.336(3) . ? C13 C18 1.385(3) . ? C13 C14 1.391(3) . ? C14 C15 1.384(3) . ? C15 N16 1.338(3) . ? N16 C17 1.346(3) . ? N16 Cd1 2.328(2) 1_456 ? C17 C18 1.379(3) . ? O1S C1S 1.439(3) . ? C1S C2S 1.491(5) . ? 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 N1 Cd1 O1S 94.63(7) . . y N1 Cd1 N16 108.35(7) . 1_654 y O1S Cd1 N16 156.43(8) . 1_654 y N1 Cd1 O202 84.73(7) . . y O1S Cd1 O202 83.32(7) . . y N16 Cd1 O202 103.46(7) 1_654 . y N1 Cd1 O201 138.61(7) . . y O1S Cd1 O201 80.15(7) . . y N16 Cd1 O201 85.74(7) 1_654 . y O202 Cd1 O201 53.92(7) . . y N1 Cd1 O102 80.43(7) . . y O1S Cd1 O102 97.70(7) . . y N16 Cd1 O102 81.51(7) 1_654 . y O202 Cd1 O102 165.17(6) . . y O201 Cd1 O102 140.89(7) . . y N1 Cd1 O101 130.55(7) . . y O1S Cd1 O101 81.11(7) . . y N16 Cd1 O101 79.99(7) 1_654 . y O202 Cd1 O101 142.27(7) . . y O201 Cd1 O101 89.52(7) . . y O102 Cd1 O101 51.94(6) . . y O203 N200 O202 121.5(3) . . ? O203 N200 O201 121.1(2) . . ? O202 N200 O201 117.4(2) . . ? N200 O201 Cd1 94.26(14) . . ? N200 O202 Cd1 94.43(15) . . ? O103 N100 O102 121.2(2) . . ? O103 N100 O101 121.8(2) . . ? O102 N100 O101 117.0(2) . . ? N100 O101 Cd1 94.47(14) . . ? N100 O102 Cd1 96.58(14) . . ? C6 N1 C2 117.7(2) . . ? C6 N1 Cd1 120.70(16) . . ? C2 N1 Cd1 120.62(16) . . ? N1 C2 C3 122.9(2) . . ? C2 C3 C4 118.7(2) . . ? C5 C4 C3 118.8(2) . . ? C5 C4 C7 119.9(2) . . ? C3 C4 C7 121.3(2) . . ? C6 C5 C4 118.3(2) . . ? N1 C6 C5 123.4(2) . . ? N12 C7 N8 125.3(2) . . ? N12 C7 C4 117.9(2) . . ? N8 C7 C4 116.8(2) . . ? C9 N8 C7 114.8(2) . . ? N8 C9 N10 125.2(2) . . ? N8 C9 C13 116.9(2) . . ? N10 C9 C13 117.9(2) . . ? C11 N10 C9 114.6(2) . . ? N10 C11 N12 125.9(2) . . ? C11 N12 C7 114.2(2) . . ? C18 C13 C14 118.3(2) . . ? C18 C13 C9 121.2(2) . . ? C14 C13 C9 120.5(2) . . ? C15 C14 C13 118.7(2) . . ? N16 C15 C14 123.4(2) . . ? C15 N16 C17 117.4(2) . . ? C15 N16 Cd1 121.38(16) . 1_456 ? C17 N16 Cd1 119.10(17) . 1_456 ? N16 C17 C18 123.0(2) . . ? C17 C18 C13 119.2(2) . . ? C1S O1S Cd1 131.38(17) . . ? O1S C1S C2S 112.1(2) . . ? _diffrn_measured_fraction_theta_max 0.866 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.424 _refine_diff_density_min -0.615 _refine_diff_density_rms 0.077 #===END data_ZNTYNT _database_code_CSD 151819 _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Zinc(II)Bis(nitrate)(2,4-bis-(4-pyridyl)-1,3,5-triazine)]n ; _chemical_name_common [Zn(NO3)2(dipyridyl-triazine)]n _chemical_formula_moiety 'C13 H9 N7 O6 Zn' _chemical_formula_sum 'C13 H9 N7 O6 Zn' _chemical_formula_weight 424.64 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' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.8910(10) _cell_length_b 11.8460(10) _cell_length_c 11.8040(10) _cell_angle_alpha 90.00 _cell_angle_beta 110.352(2) _cell_angle_gamma 90.00 _cell_volume 1558.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5168 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 28.44 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.809 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 856 _exptl_absorpt_coefficient_mu 1.629 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.412 _exptl_absorpt_correction_T_max 0.773 _exptl_absorpt_process_details 'SADABS (Bruker, 1999b)' _exptl_special_details ; [Zinc(II)Bis(nitrate)(2,4-bis-(4-pyridyl)-1,3,5-triazine)]n ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 10017 _diffrn_reflns_av_R_equivalents 0.039 _diffrn_reflns_av_sigmaI/netI 0.0238 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 28.83 _reflns_number_total 3868 _reflns_number_gt 3038 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART version 5.054 (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1999a)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC version 5.03 (Sheldrick,1994)' _computing_publication_material 'SHELXL97; PLATON (Spek, 2000)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.070P)^2^+0.167P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary 'difference Fourier methods' _atom_sites_solution_hydrogens 'placed geometrically' _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3693 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0454 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.1078 _refine_ls_wR_factor_gt 0.1037 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.63070(2) 0.51777(2) 0.32935(2) 0.02907(11) Uani 1 1 d . . . N100 N 0.5672(3) 0.6319(2) 0.4819(2) 0.0488(6) Uani 1 1 d . . . O101 O 0.55876(18) 0.67182(19) 0.38237(18) 0.0486(5) Uani 1 1 d . . . O102 O 0.6161(3) 0.5361(2) 0.5044(2) 0.0703(8) Uani 1 1 d . . . O103 O 0.5236(3) 0.6803(3) 0.5465(2) 0.0903(10) Uani 1 1 d . . . N200 N 0.80923(19) 0.64102(18) 0.3128(2) 0.0342(5) Uani 1 1 d . . . O201 O 0.71263(16) 0.60876(17) 0.23005(17) 0.0396(4) Uani 1 1 d . . . O202 O 0.82484(18) 0.60837(17) 0.41785(17) 0.0439(5) Uani 1 1 d . . . O203 O 0.88096(18) 0.70026(18) 0.28793(19) 0.0483(5) Uani 1 1 d . . . N1 N 0.71454(16) 0.36596(16) 0.34901(17) 0.0255(4) Uani 1 1 d . . . C2 C 0.68009(19) 0.28983(19) 0.2601(2) 0.0253(4) Uani 1 1 d . . . H2A H 0.6038 0.2989 0.1986 0.030 Uiso 1 1 calc R . . C3 C 0.74929(19) 0.19908(19) 0.25301(19) 0.0246(4) Uani 1 1 d . . . H3A H 0.7213 0.1464 0.1886 0.029 Uiso 1 1 calc R . . C4 C 0.86150(19) 0.18628(18) 0.34257(19) 0.0232(4) Uani 1 1 d . . . C5 C 0.8952(2) 0.26151(19) 0.43870(19) 0.0263(5) Uani 1 1 d . . . H5A H 0.9690 0.2520 0.5037 0.032 Uiso 1 1 calc R . . C6 C 0.8200(2) 0.3503(2) 0.4385(2) 0.0279(5) Uani 1 1 d . . . H6A H 0.8438 0.4022 0.5039 0.033 Uiso 1 1 calc R . . C7 C 0.94372(19) 0.09482(19) 0.33680(19) 0.0241(4) Uani 1 1 d . . . N8 N 1.04994(17) 0.09094(16) 0.42521(16) 0.0249(4) Uani 1 1 d . . . C9 C 1.1240(2) 0.01049(19) 0.4138(2) 0.0247(4) Uani 1 1 d . . . N10 N 1.09678(18) -0.06581(18) 0.32515(18) 0.0300(4) Uani 1 1 d . . . C11 C 0.9870(2) -0.0547(2) 0.2436(2) 0.0327(5) Uani 1 1 d . . . H11A H 0.9633 -0.1086 0.1800 0.039 Uiso 1 1 calc R . . N12 N 0.90747(18) 0.02403(17) 0.24247(19) 0.0294(4) Uani 1 1 d . . . C13 C 1.2448(2) 0.00743(18) 0.5086(2) 0.0249(4) Uani 1 1 d . . . C14 C 1.3278(2) -0.0754(2) 0.5098(2) 0.0283(5) Uani 1 1 d . . . H14A H 1.3085 -0.1318 0.4488 0.034 Uiso 1 1 calc R . . C15 C 1.4382(2) -0.0750(2) 0.6002(2) 0.0304(5) Uani 1 1 d . . . H15A H 1.4949 -0.1312 0.5992 0.037 Uiso 1 1 calc R . . N16 N 1.46948(18) 0.00148(16) 0.68995(19) 0.0284(4) Uani 1 1 d . . . C17 C 1.3889(2) 0.0801(2) 0.6890(2) 0.0355(6) Uani 1 1 d . . . H17A H 1.4096 0.1346 0.7521 0.043 Uiso 1 1 calc R . . C18 C 1.2769(2) 0.0859(2) 0.6006(2) 0.0338(5) Uani 1 1 d . . . H18A H 1.2222 0.1435 0.6031 0.041 Uiso 1 1 calc R . . 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 Zn1 0.01900(16) 0.03010(17) 0.03406(18) -0.00455(11) 0.00410(12) 0.00260(10) N100 0.0622(17) 0.0432(13) 0.0408(13) -0.0046(11) 0.0175(12) 0.0147(12) O101 0.0380(11) 0.0572(13) 0.0437(11) 0.0023(10) 0.0054(9) 0.0086(9) O102 0.099(2) 0.0561(14) 0.0746(17) 0.0260(12) 0.0532(16) 0.0441(14) O103 0.126(3) 0.093(2) 0.0546(14) -0.0118(14) 0.0346(16) 0.0573(19) N200 0.0255(10) 0.0327(11) 0.0442(12) -0.0100(9) 0.0119(9) -0.0012(8) O201 0.0247(9) 0.0445(10) 0.0435(10) -0.0073(8) 0.0044(8) -0.0056(8) O202 0.0413(11) 0.0447(11) 0.0399(10) -0.0046(8) 0.0070(9) -0.0066(9) O203 0.0370(11) 0.0516(12) 0.0619(13) -0.0137(10) 0.0241(10) -0.0166(9) N1 0.0174(9) 0.0304(10) 0.0267(9) 0.0000(7) 0.0052(7) 0.0006(7) C2 0.0151(10) 0.0315(11) 0.0252(10) 0.0013(8) 0.0019(8) 0.0006(8) C3 0.0177(10) 0.0307(11) 0.0235(10) 0.0000(8) 0.0048(8) -0.0007(8) C4 0.0173(10) 0.0264(10) 0.0250(10) 0.0040(8) 0.0062(8) -0.0001(8) C5 0.0184(10) 0.0307(11) 0.0253(11) 0.0022(8) 0.0020(8) 0.0007(8) C6 0.0232(11) 0.0312(11) 0.0251(11) -0.0023(9) 0.0032(9) 0.0004(9) C7 0.0187(10) 0.0258(10) 0.0273(11) 0.0034(8) 0.0075(9) -0.0011(8) N8 0.0189(9) 0.0279(9) 0.0268(9) 0.0021(7) 0.0066(8) 0.0018(7) C9 0.0185(11) 0.0266(10) 0.0285(11) 0.0039(8) 0.0078(9) 0.0007(8) N10 0.0209(9) 0.0342(11) 0.0332(10) -0.0022(8) 0.0072(8) 0.0023(8) C11 0.0263(12) 0.0354(12) 0.0334(12) -0.0064(10) 0.0066(10) 0.0008(10) N12 0.0196(10) 0.0326(10) 0.0325(10) -0.0025(8) 0.0046(8) 0.0018(8) C13 0.0175(10) 0.0279(11) 0.0292(11) 0.0040(8) 0.0080(9) 0.0002(8) C14 0.0241(12) 0.0311(12) 0.0294(11) -0.0013(9) 0.0088(9) 0.0039(9) C15 0.0210(11) 0.0317(12) 0.0366(12) 0.0016(9) 0.0075(10) 0.0041(9) N16 0.0189(10) 0.0286(10) 0.0351(11) 0.0028(8) 0.0061(8) -0.0011(7) C17 0.0233(12) 0.0343(13) 0.0430(14) -0.0095(10) 0.0039(11) 0.0003(9) C18 0.0216(12) 0.0311(12) 0.0441(14) -0.0064(10) 0.0057(10) 0.0033(9) _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 Zn1 N1 2.0300(19) . y Zn1 N16 2.059(2) 4_465 y Zn1 O201 2.069(2) . y Zn1 O102 2.144(3) . y Zn1 O101 2.197(2) . y Zn1 O202 2.428(2) . y N100 O103 1.205(3) . ? N100 O101 1.237(3) . ? N100 O102 1.261(3) . ? N200 O203 1.217(3) . ? N200 O202 1.249(3) . ? N200 O201 1.281(3) . ? N1 C2 1.336(3) . ? N1 C6 1.342(3) . ? C2 C3 1.374(3) . ? C3 C4 1.393(3) . ? C4 C5 1.388(3) . ? C4 C7 1.477(3) . ? C5 C6 1.380(3) . ? C7 N8 1.330(3) . ? C7 N12 1.340(3) . ? N8 C9 1.335(3) . ? C9 N10 1.334(3) . ? C9 C13 1.483(3) . ? N10 C11 1.332(3) . ? C11 N12 1.325(3) . ? C13 C18 1.379(3) . ? C13 C14 1.389(3) . ? C14 C15 1.374(3) . ? C15 N16 1.345(3) . ? N16 C17 1.334(3) . ? N16 Zn1 2.059(2) 4_666 ? C17 C18 1.379(3) . ? 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 N1 Zn1 N16 106.08(8) . 4_465 y N1 Zn1 O201 102.54(8) . . y N16 Zn1 O201 95.51(8) 4_465 . y N1 Zn1 O102 100.40(8) . . y N16 Zn1 O102 114.62(10) 4_465 . y O201 Zn1 O102 134.85(10) . . y N1 Zn1 O101 158.08(8) . . y N16 Zn1 O101 88.46(8) 4_465 . y O201 Zn1 O101 92.03(8) . . y O102 Zn1 O101 58.08(8) . . y N1 Zn1 O202 89.24(7) . . y N16 Zn1 O202 150.97(8) 4_465 . y O201 Zn1 O202 56.55(7) . . y O102 Zn1 O202 85.64(10) . . y O101 Zn1 O202 85.21(8) . . y O103 N100 O101 120.6(3) . . ? O103 N100 O102 124.2(3) . . ? O101 N100 O102 115.0(2) . . ? N100 O101 Zn1 92.42(16) . . ? N100 O102 Zn1 94.23(18) . . ? O203 N200 O202 122.9(2) . . ? O203 N200 O201 120.4(2) . . ? O202 N200 O201 116.7(2) . . ? N200 O201 Zn1 101.38(15) . . ? N200 O202 Zn1 85.36(14) . . ? C2 N1 C6 118.20(19) . . ? C2 N1 Zn1 120.27(15) . . ? C6 N1 Zn1 119.96(16) . . ? N1 C2 C3 123.3(2) . . ? C2 C3 C4 118.4(2) . . ? C5 C4 C3 118.6(2) . . ? C5 C4 C7 120.08(19) . . ? C3 C4 C7 121.3(2) . . ? C6 C5 C4 119.0(2) . . ? N1 C6 C5 122.3(2) . . ? N8 C7 N12 125.0(2) . . ? N8 C7 C4 116.9(2) . . ? N12 C7 C4 118.08(19) . . ? C7 N8 C9 115.1(2) . . ? N10 C9 N8 125.0(2) . . ? N10 C9 C13 118.8(2) . . ? N8 C9 C13 116.1(2) . . ? C11 N10 C9 114.1(2) . . ? N12 C11 N10 126.4(2) . . ? C11 N12 C7 114.2(2) . . ? C18 C13 C14 117.9(2) . . ? C18 C13 C9 120.6(2) . . ? C14 C13 C9 121.6(2) . . ? C15 C14 C13 119.3(2) . . ? N16 C15 C14 122.8(2) . . ? C17 N16 C15 117.6(2) . . ? C17 N16 Zn1 123.39(17) . 4_666 ? C15 N16 Zn1 118.71(16) . 4_666 ? N16 C17 C18 122.9(2) . . ? C17 C18 C13 119.5(2) . . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O103 N100 O101 Zn1 -170.7(3) . . . . ? O102 N100 O101 Zn1 4.6(3) . . . . ? N1 Zn1 O101 N100 -14.8(3) . . . . ? N16 Zn1 O101 N100 117.64(19) 4_465 . . . ? O201 Zn1 O101 N100 -146.91(18) . . . . ? O102 Zn1 O101 N100 -2.88(19) . . . . ? O202 Zn1 O101 N100 -90.72(18) . . . . ? O103 N100 O102 Zn1 170.4(3) . . . . ? O101 N100 O102 Zn1 -4.7(3) . . . . ? N1 Zn1 O102 N100 178.3(2) . . . . ? N16 Zn1 O102 N100 -68.5(2) 4_465 . . . ? O201 Zn1 O102 N100 58.7(3) . . . . ? O101 Zn1 O102 N100 2.83(19) . . . . ? O202 Zn1 O102 N100 89.9(2) . . . . ? O203 N200 O201 Zn1 -178.47(19) . . . . ? O202 N200 O201 Zn1 1.7(2) . . . . ? N1 Zn1 O201 N200 -81.57(15) . . . . ? N16 Zn1 O201 N200 170.58(15) 4_465 . . . ? O102 Zn1 O201 N200 37.2(2) . . . . ? O101 Zn1 O201 N200 81.94(15) . . . . ? O202 Zn1 O201 N200 -0.96(13) . . . . ? O203 N200 O202 Zn1 178.8(2) . . . . ? O201 N200 O202 Zn1 -1.5(2) . . . . ? N1 Zn1 O202 N200 106.57(14) . . . . ? N16 Zn1 O202 N200 -16.6(2) 4_465 . . . ? O201 Zn1 O202 N200 0.97(13) . . . . ? O102 Zn1 O202 N200 -152.94(15) . . . . ? O101 Zn1 O202 N200 -94.65(15) . . . . ? N16 Zn1 N1 C2 18.23(19) 4_465 . . . ? O201 Zn1 N1 C2 -81.35(17) . . . . ? O102 Zn1 N1 C2 137.81(18) . . . . ? O101 Zn1 N1 C2 148.1(2) . . . . ? O202 Zn1 N1 C2 -136.76(17) . . . . ? N16 Zn1 N1 C6 -176.27(17) 4_465 . . . ? O201 Zn1 N1 C6 84.15(18) . . . . ? O102 Zn1 N1 C6 -56.7(2) . . . . ? O101 Zn1 N1 C6 -46.4(3) . . . . ? O202 Zn1 N1 C6 28.74(17) . . . . ? C6 N1 C2 C3 -2.8(3) . . . . ? Zn1 N1 C2 C3 162.96(17) . . . . ? N1 C2 C3 C4 -0.5(3) . . . . ? C2 C3 C4 C5 3.9(3) . . . . ? C2 C3 C4 C7 -176.2(2) . . . . ? C3 C4 C5 C6 -4.0(3) . . . . ? C7 C4 C5 C6 176.1(2) . . . . ? C2 N1 C6 C5 2.7(3) . . . . ? Zn1 N1 C6 C5 -163.12(17) . . . . ? C4 C5 C6 N1 0.7(3) . . . . ? C5 C4 C7 N8 -1.6(3) . . . . ? C3 C4 C7 N8 178.6(2) . . . . ? C5 C4 C7 N12 179.9(2) . . . . ? C3 C4 C7 N12 0.1(3) . . . . ? N12 C7 N8 C9 1.5(3) . . . . ? C4 C7 N8 C9 -176.90(19) . . . . ? C7 N8 C9 N10 -2.8(3) . . . . ? C7 N8 C9 C13 177.59(19) . . . . ? N8 C9 N10 C11 1.4(3) . . . . ? C13 C9 N10 C11 -179.0(2) . . . . ? C9 N10 C11 N12 1.5(4) . . . . ? N10 C11 N12 C7 -2.6(4) . . . . ? N8 C7 N12 C11 0.9(3) . . . . ? C4 C7 N12 C11 179.3(2) . . . . ? N10 C9 C13 C18 179.0(2) . . . . ? N8 C9 C13 C18 -1.3(3) . . . . ? N10 C9 C13 C14 -2.7(3) . . . . ? N8 C9 C13 C14 177.0(2) . . . . ? C18 C13 C14 C15 -1.1(3) . . . . ? C9 C13 C14 C15 -179.5(2) . . . . ? C13 C14 C15 N16 1.2(4) . . . . ? C14 C15 N16 C17 -0.5(4) . . . . ? C14 C15 N16 Zn1 173.53(18) . . . 4_666 ? C15 N16 C17 C18 -0.3(4) . . . . ? Zn1 N16 C17 C18 -174.0(2) 4_666 . . . ? N16 C17 C18 C13 0.3(4) . . . . ? C14 C13 C18 C17 0.4(4) . . . . ? C9 C13 C18 C17 178.8(2) . . . . ? _diffrn_measured_fraction_theta_max 0.907 _diffrn_reflns_theta_full 28.83 _diffrn_measured_fraction_theta_full 0.907 _refine_diff_density_max 0.458 _refine_diff_density_min -0.431 _refine_diff_density_rms 0.078 #===END data_dptnzn _database_code_CSD 151820 _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'Zinc(II)bis(nitrate)2,4-bis(4-pyridyl)-1,3,5-triazine' ; _chemical_name_common Zn(NO3)2(dpt) _chemical_formula_moiety 'C13 H9 N7 O6 Zn' _chemical_formula_sum 'C13 H9 N7 O6 Zn' _chemical_formula_weight 424.64 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' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 6.981(5) _cell_length_b 19.029(7) _cell_length_c 12.222(7) _cell_angle_alpha 90.00 _cell_angle_beta 97.70(6) _cell_angle_gamma 90.00 _cell_volume 1608.9(16) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 40 _cell_measurement_theta_min 10.75 _cell_measurement_theta_max 13.50 _exptl_crystal_description column _exptl_crystal_colour colourless _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.753 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 856 _exptl_absorpt_coefficient_mu 1.578 _exptl_absorpt_correction_type psi-scans _exptl_absorpt_correction_T_min 0.403 _exptl_absorpt_correction_T_max 0.729 _exptl_absorpt_process_details 'X-RED (Stoe & Cie, 1997)' _exptl_special_details ; 'Zinc(II)bis(nitrate)2,4-bis(4-pyridyl)-1,3,5-triazine' ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe Stadi-4 Four Circle' _diffrn_measurement_method omega-theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 'random variation +/- 5' _diffrn_reflns_number 3276 _diffrn_reflns_av_R_equivalents 0.0 _diffrn_reflns_av_sigmaI/netI 0.0848 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 26.01 _reflns_number_total 3164 _reflns_number_gt 2125 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STADI-4 (stoe & cie, 1996a)' _computing_cell_refinement 'STADI-4 (stoe & cie, 1996a)' _computing_data_reduction 'X-RED (stoe & cie, 1996b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (version 5.03)(Sheldrick,1994)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0578P)^2^+13.33P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary 'difference Fourier methods' _atom_sites_solution_hydrogens 'placed geometrically' _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3164 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1446 _refine_ls_R_factor_gt 0.0896 _refine_ls_wR_factor_ref 0.2154 _refine_ls_wR_factor_gt 0.1799 _refine_ls_goodness_of_fit_ref 1.162 _refine_ls_restrained_S_all 1.162 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.19490(15) 0.80026(5) 0.38258(9) 0.0276(3) Uani 1 1 d . . . N1 N 0.0569(9) 0.8561(3) 0.4911(5) 0.0230(15) Uani 1 1 d . . . C2 C 0.1447(12) 0.9127(5) 0.5417(7) 0.0299(19) Uani 1 1 d . . . H2A H 0.2614 0.9290 0.5184 0.036 Uiso 1 1 calc R . . C3 C 0.0728(13) 0.9476(5) 0.6249(8) 0.032(2) Uani 1 1 d . . . H3A H 0.1386 0.9876 0.6579 0.038 Uiso 1 1 calc R . . C4 C -0.0952(12) 0.9248(4) 0.6607(7) 0.0296(19) Uani 1 1 d . . . C5 C -0.1883(15) 0.8664(5) 0.6081(8) 0.041(2) Uani 1 1 d . . . H5A H -0.3051 0.8491 0.6299 0.049 Uiso 1 1 calc R . . C6 C -0.1080(14) 0.8352(5) 0.5253(8) 0.037(2) Uani 1 1 d . . . H6A H -0.1730 0.7959 0.4895 0.045 Uiso 1 1 calc R . . C7 C -0.1738(14) 0.9606(5) 0.7548(8) 0.033(2) Uani 1 1 d . . . N8 N -0.0718(11) 1.0127(4) 0.8036(6) 0.0308(17) Uani 1 1 d . . . C9 C -0.1472(13) 1.0428(4) 0.8870(7) 0.031(2) Uani 1 1 d . . . N10 N -0.3123(11) 1.0245(4) 0.9218(6) 0.0357(18) Uani 1 1 d . . . C11 C -0.3999(15) 0.9706(5) 0.8667(9) 0.043(2) Uani 1 1 d . . . H11A H -0.5180 0.9551 0.8892 0.051 Uiso 1 1 calc R . . N12 N -0.3389(12) 0.9362(4) 0.7833(7) 0.039(2) Uani 1 1 d . . . C13 C -0.0334(13) 1.1017(4) 0.9445(7) 0.0296(19) Uani 1 1 d . . . C14 C 0.1413(13) 1.1232(4) 0.9164(8) 0.033(2) Uani 1 1 d . . . H14A H 0.1969 1.0988 0.8606 0.039 Uiso 1 1 calc R . . C15 C 0.2348(12) 1.1789(4) 0.9676(7) 0.0280(19) Uani 1 1 d . . . H15A H 0.3545 1.1931 0.9457 0.034 Uiso 1 1 calc R . . N16 N 0.1645(10) 1.2153(3) 1.0487(6) 0.0264(16) Uani 1 1 d . . . C17 C -0.0040(13) 1.1940(5) 1.0783(7) 0.0320(19) Uani 1 1 d . . . H17A H -0.0548 1.2189 1.1354 0.038 Uiso 1 1 calc R . . C18 C -0.1072(13) 1.1379(5) 1.0303(8) 0.034(2) Uani 1 1 d . . . H18A H -0.2253 1.1239 1.0544 0.041 Uiso 1 1 calc R . . N100 N 0.5039(12) 0.8715(4) 0.2976(7) 0.0387(19) Uani 1 1 d . . . O101 O 0.3809(11) 0.8782(3) 0.3647(6) 0.0482(19) Uani 1 1 d . . . O102 O 0.4991(12) 0.8182(4) 0.2410(7) 0.058(2) Uani 1 1 d . . . O103 O 0.6222(12) 0.9193(4) 0.2936(7) 0.062(2) Uani 1 1 d . . . N200 N -0.0614(11) 0.7260(4) 0.2540(6) 0.0331(17) Uani 1 1 d . . . O201 O 0.0778(10) 0.7675(4) 0.2336(5) 0.0393(16) Uani 1 1 d . . . O202 O -0.0856(9) 0.7199(4) 0.3517(5) 0.0384(16) Uani 1 1 d . . . O203 O -0.1559(11) 0.6952(4) 0.1789(6) 0.0500(19) 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 Zn1 0.0307(5) 0.0201(5) 0.0328(5) -0.0013(5) 0.0075(4) 0.0003(5) N1 0.021(3) 0.021(4) 0.026(4) -0.003(3) 0.002(3) 0.006(3) C2 0.028(4) 0.025(5) 0.039(5) 0.006(4) 0.012(4) -0.002(4) C3 0.037(5) 0.019(4) 0.042(5) 0.002(4) 0.014(4) -0.004(4) C4 0.029(5) 0.022(4) 0.038(5) -0.002(4) 0.003(4) 0.004(4) C5 0.038(5) 0.047(6) 0.042(6) -0.012(5) 0.018(4) -0.011(5) C6 0.033(5) 0.041(6) 0.040(5) -0.015(4) 0.010(4) -0.009(4) C7 0.037(5) 0.022(5) 0.039(5) 0.000(4) 0.008(4) 0.004(4) N8 0.038(4) 0.024(4) 0.032(4) -0.001(3) 0.010(3) -0.001(3) C9 0.042(5) 0.017(4) 0.035(5) -0.003(4) 0.010(4) 0.002(4) N10 0.045(5) 0.023(4) 0.041(4) -0.008(3) 0.016(4) -0.008(4) C11 0.042(6) 0.035(6) 0.053(6) -0.008(5) 0.018(5) -0.008(5) N12 0.045(5) 0.033(4) 0.041(5) -0.013(4) 0.018(4) -0.015(4) C13 0.035(5) 0.016(4) 0.037(5) 0.007(4) 0.001(4) 0.006(4) C14 0.042(5) 0.022(5) 0.037(5) -0.005(4) 0.014(4) 0.008(4) C15 0.026(4) 0.029(5) 0.031(4) 0.000(4) 0.010(4) 0.001(4) N16 0.033(4) 0.018(4) 0.029(4) 0.000(3) 0.004(3) 0.001(3) C17 0.036(5) 0.024(5) 0.038(5) -0.004(4) 0.015(4) 0.001(4) C18 0.031(5) 0.029(5) 0.043(6) -0.012(4) 0.007(4) -0.010(4) N100 0.041(5) 0.026(4) 0.052(5) 0.002(4) 0.015(4) 0.000(4) O101 0.058(5) 0.032(4) 0.063(5) -0.015(3) 0.040(4) -0.020(3) O102 0.084(6) 0.028(4) 0.069(5) -0.009(4) 0.040(5) -0.004(4) O103 0.068(5) 0.054(5) 0.071(6) -0.009(4) 0.035(4) -0.033(4) N200 0.036(4) 0.026(4) 0.035(4) -0.001(3) 0.000(4) 0.004(3) O201 0.043(4) 0.036(4) 0.038(4) 0.001(3) 0.001(3) -0.003(3) O202 0.035(4) 0.046(4) 0.035(4) -0.013(3) 0.006(3) -0.004(3) O203 0.063(5) 0.032(4) 0.048(4) -0.010(3) -0.017(4) -0.001(4) _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 Zn1 O201 1.994(7) . y Zn1 O101 2.003(6) . y Zn1 N16 2.016(7) 2_546 y Zn1 N1 2.039(7) . y Zn1 O202 2.474(6) . y N1 C6 1.337(11) . ? N1 C2 1.347(11) . ? C2 C3 1.365(12) . ? C3 C4 1.376(12) . ? C4 C5 1.399(13) . ? C4 C7 1.502(12) . ? C5 C6 1.358(13) . ? C7 N8 1.316(12) . ? C7 N12 1.331(12) . ? N8 C9 1.337(11) . ? C9 N10 1.328(11) . ? C9 C13 1.495(12) . ? N10 C11 1.330(12) . ? C11 N12 1.329(12) . ? C13 C14 1.373(13) . ? C13 C18 1.408(12) . ? C14 C15 1.354(12) . ? C15 N16 1.354(10) . ? N16 C17 1.339(11) . ? N16 Zn1 2.016(7) 2_556 ? C17 C18 1.374(12) . ? N100 O102 1.226(10) . ? N100 O103 1.234(10) . ? N100 O101 1.271(10) . ? N200 O203 1.208(10) . ? N200 O202 1.234(9) . ? N200 O201 1.302(10) . ? 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 O201 Zn1 O101 108.9(3) . . y O201 Zn1 N16 104.3(3) . 2_546 y O101 Zn1 N16 110.7(3) . 2_546 y O201 Zn1 N1 125.8(3) . . y O101 Zn1 N1 93.1(3) . . y N16 Zn1 N1 113.2(3) 2_546 . y O201 Zn1 O202 56.5(2) . . y O101 Zn1 O202 162.4(3) . . y N16 Zn1 O202 84.2(3) 2_546 . y N1 Zn1 O202 89.3(2) . . y C6 N1 C2 116.9(7) . . ? C6 N1 Zn1 123.3(6) . . ? C2 N1 Zn1 119.3(6) . . ? N1 C2 C3 122.7(8) . . ? C2 C3 C4 119.8(8) . . ? C3 C4 C5 117.9(8) . . ? C3 C4 C7 121.0(8) . . ? C5 C4 C7 121.1(8) . . ? C6 C5 C4 118.5(9) . . ? N1 C6 C5 124.1(9) . . ? N8 C7 N12 125.4(8) . . ? N8 C7 C4 117.2(8) . . ? N12 C7 C4 117.4(8) . . ? C7 N8 C9 115.1(8) . . ? N10 C9 N8 125.4(8) . . ? N10 C9 C13 118.4(8) . . ? N8 C9 C13 116.2(8) . . ? C9 N10 C11 113.5(8) . . ? N12 C11 N10 126.5(9) . . ? C11 N12 C7 114.0(8) . . ? C14 C13 C18 117.8(8) . . ? C14 C13 C9 122.6(8) . . ? C18 C13 C9 119.5(8) . . ? C15 C14 C13 120.4(8) . . ? N16 C15 C14 122.6(8) . . ? C17 N16 C15 117.5(7) . . ? C17 N16 Zn1 121.8(6) . 2_556 ? C15 N16 Zn1 120.7(6) . 2_556 ? N16 C17 C18 123.3(8) . . ? C17 C18 C13 118.3(8) . . ? O102 N100 O103 123.7(9) . . ? O102 N100 O101 118.5(8) . . ? O103 N100 O101 117.8(8) . . ? N100 O101 Zn1 120.0(6) . . ? O203 N200 O202 123.9(8) . . ? O203 N200 O201 119.7(8) . . ? O202 N200 O201 116.5(7) . . ? N200 O201 Zn1 103.9(5) . . ? N200 O202 Zn1 83.1(5) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.137 _refine_diff_density_min -0.875 _refine_diff_density_rms 0.145 #===END Dr. Neil Champness School of Chemistry University of Nottingham Nottingham NG7 2RD, UK Telephone (44) 115 9513505 FAX (44) 115 9513563