# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. # 1. SUBMISSION DETAILS _journal_coden_Cambridge 0182 _publ_contact_author_name 'Konstantin V. Domasevitch' _publ_contact_author_address ; Konstantin V. Domasevitch Inorganic Chemistry Department Kiev Shevchenko University Volodimirska Str. 64 01033 Kiev Ukraine ; _publ_contact_author_phone ? _publ_contact_author_fax +380(44)296-2467 _publ_contact_author_email dk@univ.kiev.ua _publ_requested_coeditor_name ? _publ_contact_letter ; ? ; #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Metal-organic frameworks exhibiting strong anion-pi interactions ; loop_ _publ_author_name _publ_author_address I.Gural'skiy ; Inorganic Chemistry Department Kiev Shevchenko University Volodimirska Str. 64 01033 Kiev Ukraine ; P.V.Solntsev ; Inorganic Chemistry Department Kiev Shevchenko University Volodimirska Str. 64 01033 Kiev Ukraine ; H.Krautscheid ; Institute of Inorganic Chemistry Leipzig University Linnestrasse 3 D-04103 Leipzig Germany ; K.V.Domasevitch ; Inorganic Chemistry Department Kiev Shevchenko University Volodimirska Str. 64 01033 Kiev Ukraine ; _publ_section_acknowledgements ; KVD and HK acknowledge support from Deutsche Forschungsgemeinschaft. ; #============================================================================== data_1 _database_code_depnum_ccdc_archive 'CCDC 619868' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Zinc Nitrate 1:1 Complex with Pyridazino[4,5-d]pyridazine ; _chemical_name_common 'Zinc Nitrate 1:1 Complex with Pyridazino(4,5-d)pyridazine' _chemical_melting_point ? _chemical_formula_moiety 'C6 H12 N4 O4 Zn, 2(N O3)' _chemical_formula_sum 'C6 H12 N6 O10 Zn' _chemical_formula_weight 393.59 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 Triclinic _symmetry_space_group_name_H-M 'P -1' _space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.3661(7) _cell_length_b 7.5923(9) _cell_length_c 8.0357(9) _cell_angle_alpha 103.580(10) _cell_angle_beta 103.119(10) _cell_angle_gamma 109.693(10) _cell_volume 334.98(8) _cell_formula_units_Z 1 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.951 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 200 _exptl_absorpt_coefficient_mu 1.904 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.6675 _exptl_absorpt_correction_T_max 0.7235 _exptl_absorpt_process_details ; (See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(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 Imaging Plate Diffraction system' _diffrn_measurement_method '\f oscillation scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 4307 _diffrn_reflns_av_R_equivalents 0.0498 _diffrn_reflns_av_sigmaI/netI 0.0350 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 5.51 _diffrn_reflns_theta_max 29.13 _reflns_number_total 1771 _reflns_number_gt 1757 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS Software (Stoe&Cie, 2000)' _computing_cell_refinement 'IPDS Software (Stoe&Cie, 2000)' _computing_data_reduction 'IPDS Software (Stoe&Cie, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e (Brandenburg, 1999)' _computing_publication_material 'WinGX 1.700.00 (Farrugia, 1999)' _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^)+(0.0350P)^2^+0.1298P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1771 _refine_ls_number_parameters 106 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0256 _refine_ls_R_factor_gt 0.0255 _refine_ls_wR_factor_ref 0.0675 _refine_ls_wR_factor_gt 0.0675 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.086 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.0000 0.0000 0.0000 0.01220(9) Uani 1 2 d S . . O1 O 0.1480(2) -0.13050(17) -0.18411(14) 0.0187(2) Uani 1 1 d . . . O2 O -0.24885(19) -0.28949(16) -0.03957(15) 0.0189(2) Uani 1 1 d . . . O3 O -0.2442(2) -0.50659(18) 0.46248(17) 0.0237(2) Uani 1 1 d . . . O4 O -0.0490(2) -0.23372(16) 0.42326(16) 0.0216(2) Uani 1 1 d . . . O5 O -0.2390(2) -0.51022(17) 0.19216(15) 0.0221(2) Uani 1 1 d . . . N1 N 0.2442(2) -0.01986(17) 0.20875(15) 0.0120(2) Uani 1 1 d . . . N2 N 0.7375(2) 0.19872(17) 0.82700(16) 0.0146(2) Uani 1 1 d . . . N3 N -0.1764(2) -0.41610(18) 0.36171(17) 0.0152(2) Uani 1 1 d . . . C1 C 0.3532(2) 0.11956(19) 0.36921(18) 0.0119(2) Uani 1 1 d . . . H1A H 0.3387 0.2412 0.3869 0.014 Uiso 1 1 calc R . . C2 C 0.4923(2) 0.09067(18) 0.51629(17) 0.0109(2) Uani 1 1 d . . . C3 C 0.6130(2) 0.23226(19) 0.69483(18) 0.0137(2) Uani 1 1 d . . . H3A H 0.6026 0.3558 0.7187 0.016 Uiso 1 1 calc R . . H1 H 0.0918 -0.1645 -0.2948 0.020 Uiso 1 1 d . . . H2 H 0.1624 -0.2414 -0.1756 0.020 Uiso 1 1 d . . . H3 H -0.4017 -0.3210 -0.0758 0.020 Uiso 1 1 d . . . H4 H -0.2277 -0.3400 0.0435 0.020 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 Zn1 0.01226(13) 0.01274(13) 0.00977(12) 0.00379(8) 0.00105(8) 0.00476(9) O1 0.0226(5) 0.0215(5) 0.0145(5) 0.0045(4) 0.0063(4) 0.0130(4) O2 0.0170(5) 0.0166(5) 0.0199(5) 0.0089(4) 0.0028(4) 0.0037(4) O3 0.0278(6) 0.0218(5) 0.0237(6) 0.0118(5) 0.0141(5) 0.0065(5) O4 0.0242(5) 0.0135(5) 0.0240(5) 0.0040(4) 0.0118(4) 0.0032(4) O5 0.0273(6) 0.0204(5) 0.0145(5) 0.0032(4) 0.0056(4) 0.0075(5) N1 0.0127(5) 0.0128(5) 0.0113(5) 0.0047(4) 0.0034(4) 0.0062(4) N2 0.0169(5) 0.0136(5) 0.0127(5) 0.0028(4) 0.0037(4) 0.0076(4) N3 0.0139(5) 0.0157(5) 0.0169(6) 0.0053(4) 0.0065(4) 0.0062(4) C1 0.0112(5) 0.0125(6) 0.0130(6) 0.0048(5) 0.0046(4) 0.0052(5) C2 0.0103(5) 0.0116(6) 0.0103(5) 0.0032(4) 0.0031(4) 0.0045(5) C3 0.0151(6) 0.0120(5) 0.0123(6) 0.0018(5) 0.0032(5) 0.0062(5) _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 2.0846(12) 2 ? Zn1 N1 2.0846(12) . ? Zn1 O2 2.1303(11) 2 ? Zn1 O2 2.1303(11) . ? Zn1 O1 2.1521(10) 2 ? Zn1 O1 2.1521(10) . ? O3 N3 1.2385(16) . ? O4 N3 1.2487(16) . ? O5 N3 1.2768(16) . ? N1 C1 1.3124(17) . ? N1 N2 1.3708(16) 2_656 ? N2 C3 1.3045(18) . ? N2 N1 1.3708(16) 2_656 ? C1 C2 1.4166(18) . ? C2 C2 1.381(2) 2_656 ? C2 C3 1.4223(18) . ? 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 N1 180.00(6) 2 . ? N1 Zn1 O2 90.31(4) 2 2 ? N1 Zn1 O2 89.69(4) . 2 ? N1 Zn1 O2 89.69(4) 2 . ? N1 Zn1 O2 90.31(4) . . ? O2 Zn1 O2 180.0 2 . ? N1 Zn1 O1 87.45(4) 2 2 ? N1 Zn1 O1 92.55(4) . 2 ? O2 Zn1 O1 89.71(5) 2 2 ? O2 Zn1 O1 90.29(5) . 2 ? N1 Zn1 O1 92.55(4) 2 . ? N1 Zn1 O1 87.45(4) . . ? O2 Zn1 O1 90.29(5) 2 . ? O2 Zn1 O1 89.71(5) . . ? O1 Zn1 O1 180.00(5) 2 . ? C1 N1 N2 122.14(12) . 2_656 ? C1 N1 Zn1 122.57(9) . . ? N2 N1 Zn1 114.90(9) 2_656 . ? C3 N2 N1 118.41(12) . 2_656 ? O3 N3 O4 120.97(13) . . ? O3 N3 O5 119.59(13) . . ? O4 N3 O5 119.44(12) . . ? N1 C1 C2 121.42(12) . . ? C2 C2 C1 117.13(15) 2_656 . ? C2 C2 C3 117.80(15) 2_656 . ? C1 C2 C3 125.06(12) . . ? N2 C3 C2 123.06(12) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 29.13 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.517 _refine_diff_density_min -0.891 _refine_diff_density_rms 0.077 #============================================================================== data_2 _database_code_depnum_ccdc_archive 'CCDC 619869' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Copper(II) Nitrate 1:2 Complex with Pyridazino[4,5-d]pyridazine, Tetrahydrate ; _chemical_name_common ;Copper(ii) Nitrate 1:2 Complex with Pyridazino(4,5- d)pyridazine, Tetrahydrate ; _chemical_melting_point ? _chemical_formula_moiety 'C12 H12 Cu N8 O2, 2(N O3), 2(H2 O)' _chemical_formula_sum 'C12 H16 Cu N10 O10' _chemical_formula_weight 523.89 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C c' _space_group_name_Hall 'C -2yc' _symmetry_Int_Tables_number 9 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 13.1173(9) _cell_length_b 13.2215(9) _cell_length_c 12.0518(8) _cell_angle_alpha 90.00 _cell_angle_beta 113.404(2) _cell_angle_gamma 90.00 _cell_volume 1918.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour green-blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.814 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1068 _exptl_absorpt_coefficient_mu 1.220 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.7925 _exptl_absorpt_correction_T_max 0.8478 _exptl_absorpt_process_details ; (See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(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 Imaging Plate Diffraction system' _diffrn_measurement_method '\f oscillation scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6790 _diffrn_reflns_av_R_equivalents 0.0255 _diffrn_reflns_av_sigmaI/netI 0.0211 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 5.19 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3769 _reflns_number_gt 3505 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS Software (Stoe&Cie, 2000)' _computing_cell_refinement 'IPDS Software (Stoe&Cie, 2000)' _computing_data_reduction 'IPDS Software (Stoe&Cie, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e (Brandenburg, 1999)' _computing_publication_material 'WinGX 1.700.00 (Farrugia, 1999)' _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^)+(0.0632P)^2^+5.7918P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.36(2) _refine_ls_number_reflns 3769 _refine_ls_number_parameters 308 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0444 _refine_ls_R_factor_gt 0.0413 _refine_ls_wR_factor_ref 0.1145 _refine_ls_wR_factor_gt 0.1124 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.098 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.65691(8) 0.74967(2) 0.17469(9) 0.01353(13) Uani 1 1 d . . . O1 O 0.4657(4) 0.7373(3) 0.1201(5) 0.0245(10) Uani 1 1 d . . . H1 H 0.4224 0.7077 0.1503 0.037 Uiso 1 1 d . . . H2 H 0.4305 0.7538 0.0424 0.037 Uiso 1 1 d . . . O2 O 0.8561(4) 0.7447(2) 0.2300(5) 0.0204(11) Uani 1 1 d . . . H3 H 0.8843 0.7581 0.3031 0.031 Uiso 1 1 d . . . H4 H 0.8985 0.7157 0.2072 0.031 Uiso 1 1 d . . . O3 O 0.4717(4) 0.9034(5) 0.6401(5) 0.0610(15) Uani 1 1 d . . . O4 O 0.6423(4) 0.9276(2) 0.6710(5) 0.0390(9) Uani 1 1 d . . . O5 O 0.5972(5) 0.8044(3) 0.7564(4) 0.0602(13) Uani 1 1 d . . . O6 O 0.4165(5) 0.6795(7) 0.4752(7) 0.131(3) Uani 1 1 d D . . O7 O 0.5755(5) 0.7123(4) 0.4839(6) 0.086(2) Uani 1 1 d D . . O8 O 0.5549(8) 0.5938(5) 0.5977(6) 0.124(4) Uani 1 1 d D . . O9 O 0.3597(4) 0.6234(4) 0.2285(5) 0.0507(11) Uani 1 1 d . . . O10A O 0.7866(7) 0.5971(9) 0.7488(11) 0.049(2) Uani 0.50 1 d P . . O10B O 0.8275(11) 0.6319(8) 0.8051(12) 0.070(4) Uani 0.50 1 d P . . N1 N 0.6791(3) 0.6385(3) 0.2985(4) 0.0158(9) Uani 1 1 d . . . N2 N 0.7713(3) 0.6458(3) 0.4062(4) 0.0196(8) Uani 1 1 d . . . N3 N 0.5532(3) 0.3472(3) 0.4415(4) 0.0214(8) Uani 1 1 d . . . N4 N 0.6450(4) 0.3558(3) 0.5473(4) 0.0147(9) Uani 1 1 d . . . N5 N 0.6397(4) 1.1380(4) 0.5537(4) 0.0159(9) Uani 1 1 d . . . N6 N 0.5341(3) 1.1065(3) 0.4925(4) 0.0193(8) Uani 1 1 d . . . N7 N 0.7781(3) 0.8874(3) 0.3650(4) 0.0250(9) Uani 1 1 d . . . N8 N 0.6700(4) 0.8555(3) 0.3008(5) 0.0181(10) Uani 1 1 d . . . N9 N 0.5693(3) 0.8767(3) 0.6871(3) 0.0296(8) Uani 1 1 d . . . N10 N 0.5225(5) 0.6604(4) 0.5246(5) 0.0511(14) Uani 1 1 d D . . C1 C 0.6065(4) 0.5654(4) 0.2780(4) 0.0181(9) Uani 1 1 d . . . H1A H 0.5459 0.5617 0.2028 0.022 Uiso 1 1 calc R . . C2 C 0.6181(4) 0.4916(4) 0.3679(4) 0.0171(9) Uani 1 1 d . . . C3 C 0.5400(4) 0.4137(4) 0.3556(5) 0.0248(10) Uani 1 1 d . . . H3A H 0.4762 0.4094 0.2832 0.030 Uiso 1 1 calc R . . C4 C 0.7848(4) 0.5784(4) 0.4883(5) 0.0216(10) Uani 1 1 d . . . H4A H 0.8482 0.5830 0.5610 0.026 Uiso 1 1 calc R . . C5 C 0.7095(4) 0.4979(4) 0.4752(5) 0.0146(10) Uani 1 1 d . . . C6 C 0.7194(4) 0.4246(3) 0.5640(4) 0.0161(9) Uani 1 1 d . . . H6A H 0.7820 0.4260 0.6376 0.019 Uiso 1 1 calc R . . C7 C 0.5162(4) 1.0298(4) 0.4189(5) 0.0257(11) Uani 1 1 d . . . H7A H 0.4427 1.0081 0.3760 0.031 Uiso 1 1 calc R . . C8 C 0.6021(4) 0.9781(4) 0.4009(4) 0.0178(10) Uani 1 1 d . . . C9 C 0.5868(4) 0.8954(3) 0.3178(4) 0.0176(9) Uani 1 1 d . . . H9A H 0.5149 0.8697 0.2750 0.021 Uiso 1 1 calc R . . C10 C 0.7240(4) 1.0934(4) 0.5424(5) 0.0183(10) Uani 1 1 d . . . H10A H 0.7963 1.1162 0.5890 0.022 Uiso 1 1 calc R . . C11 C 0.7092(4) 1.0124(4) 0.4624(5) 0.0174(10) Uani 1 1 d . . . C12 C 0.7963(4) 0.9633(4) 0.4408(5) 0.0242(10) Uani 1 1 d . . . H12A H 0.8696 0.9861 0.4825 0.029 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 Cu1 0.0218(2) 0.00910(17) 0.01189(19) 0.00003(17) 0.00904(15) 0.00060(18) O1 0.029(2) 0.0262(19) 0.020(2) 0.0045(14) 0.011(2) 0.0058(15) O2 0.0153(19) 0.025(2) 0.023(2) -0.0029(12) 0.0095(19) -0.0005(11) O3 0.022(2) 0.090(4) 0.063(3) -0.008(3) 0.008(2) -0.003(2) O4 0.042(2) 0.0326(15) 0.0526(19) 0.005(2) 0.0297(19) -0.0052(16) O5 0.102(4) 0.033(2) 0.059(3) 0.0113(18) 0.046(3) -0.008(2) O6 0.076(5) 0.174(8) 0.153(8) -0.072(7) 0.057(5) -0.052(5) O7 0.143(5) 0.043(2) 0.141(5) 0.007(3) 0.128(5) 0.002(3) O8 0.266(11) 0.050(3) 0.097(5) 0.024(3) 0.114(7) 0.035(5) O9 0.044(3) 0.060(3) 0.057(3) 0.007(2) 0.030(2) -0.009(2) O10A 0.024(4) 0.049(6) 0.064(7) 0.020(5) 0.007(4) 0.010(4) O10B 0.069(8) 0.039(5) 0.078(8) 0.000(5) 0.003(7) -0.003(5) N1 0.0191(19) 0.013(2) 0.021(2) 0.0049(17) 0.0135(18) -0.0015(16) N2 0.0166(18) 0.0194(18) 0.020(2) 0.0040(15) 0.0050(16) -0.0030(14) N3 0.0250(19) 0.0200(19) 0.016(2) 0.0037(15) 0.0053(17) -0.0050(15) N4 0.0210(19) 0.013(2) 0.008(2) -0.0013(15) 0.0031(17) 0.0040(16) N5 0.0185(18) 0.017(2) 0.011(2) 0.0001(17) 0.0041(17) -0.0022(17) N6 0.0178(18) 0.0199(18) 0.0193(19) -0.0027(15) 0.0063(15) 0.0008(15) N7 0.027(2) 0.022(2) 0.029(2) -0.0076(17) 0.0140(19) 0.0018(17) N8 0.027(2) 0.008(2) 0.023(2) -0.0032(17) 0.014(2) 0.0022(17) N9 0.035(2) 0.0305(19) 0.0260(19) -0.0079(15) 0.0151(17) -0.0095(16) N10 0.072(4) 0.043(3) 0.055(3) -0.026(2) 0.042(3) -0.015(3) C1 0.022(2) 0.017(2) 0.013(2) -0.0007(16) 0.0048(18) 0.0011(16) C2 0.021(2) 0.0145(19) 0.016(2) -0.0019(16) 0.0066(18) -0.0003(16) C3 0.033(2) 0.021(2) 0.018(2) 0.0076(18) 0.007(2) -0.0067(18) C4 0.0125(19) 0.023(2) 0.022(2) 0.0006(18) -0.0008(18) -0.0073(16) C5 0.017(2) 0.0122(19) 0.017(2) 0.0041(16) 0.0085(18) -0.0009(15) C6 0.020(2) 0.017(2) 0.013(2) 0.0022(15) 0.0089(17) -0.0005(15) C7 0.027(3) 0.028(2) 0.023(3) -0.0089(19) 0.011(2) -0.0053(19) C8 0.021(2) 0.017(2) 0.014(2) -0.0006(15) 0.0058(18) -0.0004(16) C9 0.027(2) 0.0114(19) 0.017(2) -0.0020(15) 0.0114(18) -0.0048(16) C10 0.0141(19) 0.020(2) 0.018(2) -0.0048(16) 0.0038(18) -0.0015(15) C11 0.023(2) 0.017(2) 0.015(2) -0.0033(15) 0.0103(18) 0.0020(16) C12 0.017(2) 0.026(2) 0.027(3) -0.0105(19) 0.0066(19) 0.0028(18) _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 Cu1 N8 2.022(5) . ? Cu1 N5 2.030(5) 2_574 ? Cu1 N1 2.032(4) . ? Cu1 N4 2.034(5) 2_564 ? Cu1 O1 2.332(5) . ? Cu1 O2 2.427(5) . ? O3 N9 1.229(6) . ? O4 N9 1.247(5) . ? O5 N9 1.225(5) . ? O6 N10 1.302(6) . ? O7 N10 1.210(5) . ? O8 N10 1.198(6) . ? O10A O10B 0.818(13) . ? N1 C1 1.310(6) . ? N1 N2 1.381(7) . ? N2 C4 1.290(6) . ? N3 C3 1.316(6) . ? N3 N4 1.367(6) . ? N4 C6 1.290(7) . ? N4 Cu1 2.034(5) 2_565 ? N5 C10 1.307(7) . ? N5 N6 1.351(6) . ? N5 Cu1 2.030(5) 2_575 ? N6 C7 1.306(6) . ? N7 C12 1.314(6) . ? N7 N8 1.384(7) . ? N8 C9 1.300(7) . ? C1 C2 1.421(7) . ? C2 C5 1.373(5) . ? C2 C3 1.419(6) . ? C4 C5 1.417(6) . ? C5 C6 1.412(7) . ? C7 C8 1.406(7) . ? C8 C11 1.378(5) . ? C8 C9 1.442(7) . ? C10 C11 1.402(7) . ? C11 C12 1.425(6) . ? 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 N8 Cu1 N5 89.17(11) . 2_574 ? N8 Cu1 N1 90.2(2) . . ? N5 Cu1 N1 178.2(2) 2_574 . ? N8 Cu1 N4 179.3(2) . 2_564 ? N5 Cu1 N4 90.3(2) 2_574 2_564 ? N1 Cu1 N4 90.25(11) . 2_564 ? N8 Cu1 O1 91.23(18) . . ? N5 Cu1 O1 92.75(16) 2_574 . ? N1 Cu1 O1 88.93(17) . . ? N4 Cu1 O1 89.28(16) 2_564 . ? N8 Cu1 O2 92.94(16) . . ? N5 Cu1 O2 91.01(16) 2_574 . ? N1 Cu1 O2 87.36(15) . . ? N4 Cu1 O2 86.58(17) 2_564 . ? O1 Cu1 O2 174.43(9) . . ? C1 N1 N2 121.9(5) . . ? C1 N1 Cu1 120.9(4) . . ? N2 N1 Cu1 117.1(3) . . ? C4 N2 N1 118.3(4) . . ? C3 N3 N4 118.0(4) . . ? C6 N4 N3 122.4(5) . . ? C6 N4 Cu1 122.6(4) . 2_565 ? N3 N4 Cu1 115.0(3) . 2_565 ? C10 N5 N6 122.0(5) . . ? C10 N5 Cu1 123.2(4) . 2_575 ? N6 N5 Cu1 114.5(3) . 2_575 ? C7 N6 N5 118.5(4) . . ? C12 N7 N8 119.0(4) . . ? C9 N8 N7 121.7(5) . . ? C9 N8 Cu1 125.0(4) . . ? N7 N8 Cu1 113.2(3) . . ? O5 N9 O3 120.9(5) . . ? O5 N9 O4 119.1(5) . . ? O3 N9 O4 119.8(5) . . ? O8 N10 O7 128.5(7) . . ? O8 N10 O6 118.7(7) . . ? O7 N10 O6 112.7(6) . . ? N1 C1 C2 120.9(4) . . ? C5 C2 C3 117.9(4) . . ? C5 C2 C1 117.7(3) . . ? C3 C2 C1 124.4(4) . . ? N3 C3 C2 122.6(4) . . ? N2 C4 C5 123.7(4) . . ? C2 C5 C6 117.0(4) . . ? C2 C5 C4 117.4(4) . . ? C6 C5 C4 125.5(4) . . ? N4 C6 C5 122.0(5) . . ? N6 C7 C8 123.0(4) . . ? C11 C8 C7 117.7(4) . . ? C11 C8 C9 117.0(4) . . ? C7 C8 C9 125.2(4) . . ? N8 C9 C8 121.6(5) . . ? N5 C10 C11 121.6(5) . . ? C8 C11 C10 117.0(4) . . ? C8 C11 C12 118.1(4) . . ? C10 C11 C12 124.8(5) . . ? N7 C12 C11 122.5(5) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.231 _refine_diff_density_min -0.615 _refine_diff_density_rms 0.090 #============================================================================== data_3 _database_code_depnum_ccdc_archive 'CCDC 619870' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Copper(II) Perchlorate 1:2 Complex with Pyridazino[4,5-d]pyridazine, Hexahydrate ; _chemical_name_common ; Copper(ii) Perchlorate 1:2 Complex with Pyridazino(4,5- d)pyridazine, Hexahydrate ; _chemical_melting_point ? _chemical_formula_moiety 'C12 H12 Cu N8 O2, 2(Cl O4), 4(H2 O)' _chemical_formula_sum 'C12 H20 Cl2 Cu N8 O14' _chemical_formula_weight 634.80 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' Cu Cu 0.3201 1.2651 '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' _space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.3893(8) _cell_length_b 9.0008(9) _cell_length_c 9.0474(9) _cell_angle_alpha 92.650(10) _cell_angle_beta 107.178(10) _cell_angle_gamma 95.598(10) _cell_volume 570.37(10) _cell_formula_units_Z 1 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour green-blue _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.848 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 323 _exptl_absorpt_coefficient_mu 1.280 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.7403 _exptl_absorpt_correction_T_max 0.8024 _exptl_absorpt_process_details ; (See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(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 Imaging Plate Diffraction system' _diffrn_measurement_method '\f oscillation scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5464 _diffrn_reflns_av_R_equivalents 0.0267 _diffrn_reflns_av_sigmaI/netI 0.0265 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.80 _diffrn_reflns_theta_max 28.10 _reflns_number_total 2691 _reflns_number_gt 2299 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS Software (Stoe&Cie, 2000)' _computing_cell_refinement 'IPDS Software (Stoe&Cie, 2000)' _computing_data_reduction 'IPDS Software (Stoe&Cie, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e (Brandenburg, 1999)' _computing_publication_material 'WinGX 1.700.00 (Farrugia, 1999)' _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^)+(0.0546P)^2^+0.0753P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2691 _refine_ls_number_parameters 175 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0304 _refine_ls_R_factor_gt 0.0280 _refine_ls_wR_factor_ref 0.0787 _refine_ls_wR_factor_gt 0.0779 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.0000 0.0000 0.0000 0.01014(10) Uani 1 2 d S . . Cl1 Cl 0.23633(6) 0.44641(6) -0.32209(5) 0.02803(13) Uani 1 1 d . . . O1 O 0.32628(15) -0.00427(14) 0.11399(12) 0.0169(2) Uani 1 1 d . . . O2 O 0.3675(3) 0.4263(3) -0.1742(2) 0.0723(7) Uani 1 1 d . . . O3 O 0.1950(3) 0.5996(2) -0.3189(2) 0.0473(4) Uani 1 1 d . . . O4 O 0.0668(2) 0.3463(2) -0.3479(2) 0.0461(4) Uani 1 1 d . . . O5 O 0.3205(3) 0.4209(3) -0.4425(3) 0.0645(6) Uani 1 1 d . . . O6 O 0.55293(18) 0.23310(16) 0.04150(16) 0.0279(3) Uani 1 1 d . . . O7 O 0.6172(3) 0.2314(2) -0.4568(2) 0.0469(4) Uani 1 1 d . . . N1 N 0.02411(17) 0.22805(15) 0.01599(14) 0.0131(3) Uani 1 1 d . . . N2 N -0.15940(19) 0.70428(17) -0.14751(15) 0.0176(3) Uani 1 1 d . . . N3 N 0.02552(17) -0.00002(15) -0.22109(14) 0.0127(3) Uani 1 1 d . . . N4 N -0.21011(18) -0.02665(18) -0.77463(15) 0.0185(3) Uani 1 1 d . . . C1 C -0.0834(2) 0.30709(19) -0.08633(17) 0.0148(3) Uani 1 1 d . . . H1A H -0.1732 0.2573 -0.1754 0.018 Uiso 1 1 calc R . . C2 C -0.0674(2) 0.46479(18) -0.06584(16) 0.0133(3) Uani 1 1 d . . . C3 C -0.1787(2) 0.5583(2) -0.17096(18) 0.0187(3) Uani 1 1 d . . . H3A H -0.2703 0.5128 -0.2614 0.022 Uiso 1 1 calc R . . C4 C -0.1193(2) -0.02053(19) -0.34843(16) 0.0148(3) Uani 1 1 d . . . H4A H -0.2435 -0.0403 -0.3411 0.018 Uiso 1 1 calc R . . C5 C -0.0926(2) -0.01348(19) -0.49673(17) 0.0136(3) Uani 1 1 d . . . C6 C -0.2411(2) -0.0325(2) -0.63975(17) 0.0184(3) Uani 1 1 d . . . H6A H -0.3677 -0.0503 -0.6375 0.022 Uiso 1 1 calc R . . H1 H 0.3553 -0.0686 0.0695 0.027(6) Uiso 1 1 d R . . H2 H 0.3835 0.0806 0.1038 0.036(6) Uiso 1 1 d R . . H3 H 0.6153 0.2850 0.1250 0.055(9) Uiso 1 1 d R . . H5 H 0.5309 0.2860 -0.4647 0.074(11) Uiso 1 1 d R . . H4 H 0.4925 0.2998 -0.0167 0.053(8) Uiso 1 1 d R . . H6 H 0.6981 0.2731 -0.5022 0.076(11) Uiso 1 1 d 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 Cu1 0.01593(14) 0.00750(17) 0.00791(13) 0.00095(8) 0.00460(9) 0.00239(9) Cl1 0.0284(2) 0.0283(3) 0.0265(2) 0.00595(18) 0.00623(17) 0.00389(17) O1 0.0176(5) 0.0179(7) 0.0169(5) 0.0010(4) 0.0076(4) 0.0025(4) O2 0.0843(14) 0.0459(14) 0.0536(11) 0.0168(9) -0.0312(10) 0.0059(11) O3 0.0580(10) 0.0304(11) 0.0486(9) 0.0071(7) 0.0056(8) 0.0125(8) O4 0.0435(9) 0.0440(12) 0.0512(10) -0.0022(8) 0.0205(7) -0.0092(7) O5 0.0665(12) 0.0784(17) 0.0743(13) 0.0219(11) 0.0522(11) 0.0269(11) O6 0.0301(6) 0.0205(8) 0.0327(7) -0.0003(5) 0.0089(5) 0.0046(5) O7 0.0513(10) 0.0366(12) 0.0620(11) 0.0185(8) 0.0263(8) 0.0132(8) N1 0.0173(6) 0.0099(7) 0.0129(6) 0.0004(4) 0.0055(5) 0.0020(4) N2 0.0208(6) 0.0125(8) 0.0167(6) 0.0003(5) 0.0012(5) 0.0025(5) N3 0.0160(6) 0.0126(7) 0.0107(5) 0.0016(4) 0.0056(4) 0.0029(4) N4 0.0151(6) 0.0268(9) 0.0132(6) 0.0016(5) 0.0039(5) 0.0019(5) C1 0.0183(7) 0.0115(9) 0.0143(7) 0.0009(5) 0.0048(5) 0.0015(5) C2 0.0157(6) 0.0111(8) 0.0135(6) 0.0008(5) 0.0050(5) 0.0013(5) C3 0.0201(7) 0.0151(10) 0.0169(7) 0.0005(6) -0.0007(5) 0.0023(6) C4 0.0165(6) 0.0159(9) 0.0133(7) 0.0015(5) 0.0064(5) 0.0023(5) C5 0.0153(7) 0.0145(9) 0.0118(6) 0.0006(5) 0.0049(5) 0.0025(5) C6 0.0141(6) 0.0276(10) 0.0136(7) 0.0016(6) 0.0044(5) 0.0018(6) _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 Cu1 N1 2.0377(14) 2 ? Cu1 N1 2.0377(14) . ? Cu1 N3 2.0639(12) . ? Cu1 N3 2.0639(12) 2 ? Cu1 O1 2.3304(11) 2 ? Cu1 O1 2.3304(11) . ? Cl1 O4 1.4220(17) . ? Cl1 O5 1.4253(18) . ? Cl1 O2 1.4328(17) . ? Cl1 O3 1.4420(19) . ? N1 C1 1.316(2) . ? N1 N2 1.3776(18) 2_565 ? N2 C3 1.308(2) . ? N2 N1 1.3776(18) 2_565 ? N3 C4 1.3117(19) . ? N3 N4 1.3739(17) 2_554 ? N4 C6 1.3087(19) . ? N4 N3 1.3739(17) 2_554 ? C1 C2 1.412(2) . ? C2 C2 1.385(3) 2_565 ? C2 C3 1.427(2) . ? C4 C5 1.4161(19) . ? C5 C5 1.385(3) 2_554 ? C5 C6 1.418(2) . ? 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 Cu1 N1 180.000(7) 2 . ? N1 Cu1 N3 89.91(5) 2 . ? N1 Cu1 N3 90.09(5) . . ? N1 Cu1 N3 90.09(5) 2 2 ? N1 Cu1 N3 89.91(5) . 2 ? N3 Cu1 N3 180.00(11) . 2 ? N1 Cu1 O1 92.86(5) 2 2 ? N1 Cu1 O1 87.14(5) . 2 ? N3 Cu1 O1 87.09(4) . 2 ? N3 Cu1 O1 92.91(4) 2 2 ? N1 Cu1 O1 87.14(5) 2 . ? N1 Cu1 O1 92.86(5) . . ? N3 Cu1 O1 92.91(4) . . ? N3 Cu1 O1 87.09(4) 2 . ? O1 Cu1 O1 180.00(6) 2 . ? O4 Cl1 O5 110.17(13) . . ? O4 Cl1 O2 109.63(13) . . ? O5 Cl1 O2 110.32(15) . . ? O4 Cl1 O3 110.53(11) . . ? O5 Cl1 O3 108.81(13) . . ? O2 Cl1 O3 107.34(12) . . ? C1 N1 N2 121.43(14) . 2_565 ? C1 N1 Cu1 123.95(11) . . ? N2 N1 Cu1 114.57(10) 2_565 . ? C3 N2 N1 118.78(13) . 2_565 ? C4 N3 N4 121.65(12) . 2_554 ? C4 N3 Cu1 124.18(10) . . ? N4 N3 Cu1 114.16(9) 2_554 . ? C6 N4 N3 118.84(12) . 2_554 ? N1 C1 C2 121.72(14) . . ? C2 C2 C1 117.83(18) 2_565 . ? C2 C2 C3 117.06(19) 2_565 . ? C1 C2 C3 125.11(14) . . ? N2 C3 C2 123.17(15) . . ? N3 C4 C5 121.39(13) . . ? C5 C5 C4 117.75(17) 2_554 . ? C5 C5 C6 117.25(16) 2_554 . ? C4 C5 C6 125.00(13) . . ? N4 C6 C5 123.11(13) . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 28.10 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.488 _refine_diff_density_min -0.312 _refine_diff_density_rms 0.072 #============================================================================== data_4 _database_code_depnum_ccdc_archive 'CCDC 619871' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Hydroxocopper(II) Sulfamate Complex with Pyridazino[4,5-d]pyridazine, Monohydrate ; _chemical_name_common ; Hydroxocopper(ii) Sulfamate Complex with Pyridazino(4,5- d)pyridazine, Monohydrate ; _chemical_melting_point ? _chemical_formula_moiety 'C6 H5 Cu N4 O, H2 N O3 S, H2 O' _chemical_formula_sum 'C6 H9 Cu N5 O5 S' _chemical_formula_weight 326.78 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 6.7875(7) _cell_length_b 10.5615(9) _cell_length_c 14.2118(11) _cell_angle_alpha 90.00 _cell_angle_beta 97.567(10) _cell_angle_gamma 90.00 _cell_volume 1009.92(16) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.149 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 660 _exptl_absorpt_coefficient_mu 2.395 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.6935 _exptl_absorpt_correction_T_max 0.7544 _exptl_absorpt_process_details ; (See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 Imaging Plate Diffraction system' _diffrn_measurement_method '\f oscillation scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9278 _diffrn_reflns_av_R_equivalents 0.0500 _diffrn_reflns_av_sigmaI/netI 0.0460 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 27.97 _reflns_number_total 2365 _reflns_number_gt 1577 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS Software (Stoe&Cie, 2000)' _computing_cell_refinement 'IPDS Software (Stoe&Cie, 2000)' _computing_data_reduction 'IPDS Software (Stoe&Cie, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e (Brandenburg, 1999)' _computing_publication_material 'WinGX 1.700.00 (Farrugia, 1999)' _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^)+(0.0614P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2365 _refine_ls_number_parameters 166 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0537 _refine_ls_R_factor_gt 0.0362 _refine_ls_wR_factor_ref 0.0994 _refine_ls_wR_factor_gt 0.0959 _refine_ls_goodness_of_fit_ref 0.967 _refine_ls_restrained_S_all 0.967 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu -0.5000 0.5000 0.5000 0.01252(16) Uani 1 2 d S . . Cu2 Cu 0.0000 0.5000 0.5000 0.01030(15) Uani 1 2 d S . . S1 S -0.77388(14) 0.04733(8) 0.40877(6) 0.0199(2) Uani 1 1 d . . . O1 O -0.2525(3) 0.58977(19) 0.49363(15) 0.0137(4) Uani 1 1 d . . . H1B H -0.2544 0.6784 0.4873 0.016 Uiso 1 1 calc R . . O2 O -0.6826(4) 0.1474(2) 0.47107(19) 0.0288(6) Uani 1 1 d . . . O3 O -0.9872(4) 0.0656(3) 0.3881(2) 0.0348(7) Uani 1 1 d . . . O4 O -0.6754(5) 0.0356(3) 0.32372(19) 0.0342(7) Uani 1 1 d . . . O5 O -1.2970(5) -0.0851(3) 0.3043(2) 0.0372(7) Uani 1 1 d . . . H3 H -1.1914 -0.0543 0.3289 0.056 Uiso 1 1 d . . . H4 H -1.3862 -0.0440 0.3143 0.056 Uiso 1 1 d . . . N1 N -0.3301(4) 0.3593(2) 0.39243(17) 0.0140(6) Uani 1 1 d . . . N2 N -0.1340(4) 0.3866(2) 0.38737(17) 0.0116(5) Uani 1 1 d . . . N3 N -0.3502(4) 0.1084(2) 0.11073(17) 0.0133(6) Uani 1 1 d . . . N4 N -0.1509(4) 0.1291(2) 0.10904(17) 0.0132(5) Uani 1 1 d . . . N5 N -0.7457(5) -0.0904(3) 0.4606(2) 0.0245(7) Uani 1 1 d . . . H1 H -0.6327 -0.1085 0.4888 0.037 Uiso 1 1 d . . . H2 H -0.8198 -0.0973 0.5007 0.037 Uiso 1 1 d . . . C1 C -0.4288(5) 0.2865(3) 0.3275(2) 0.0143(7) Uani 1 1 d . . . H1A H -0.5630 0.2685 0.3317 0.017 Uiso 1 1 calc R . . C2 C -0.3397(5) 0.2341(3) 0.2512(2) 0.0126(6) Uani 1 1 d . . . C3 C -0.4419(5) 0.1575(3) 0.1778(2) 0.0145(7) Uani 1 1 d . . . H3A H -0.5782 0.1417 0.1776 0.017 Uiso 1 1 calc R . . C4 C -0.0420(5) 0.3410(3) 0.3193(2) 0.0136(6) Uani 1 1 d . . . H4A H 0.0925 0.3612 0.3179 0.016 Uiso 1 1 calc R . . C5 C -0.1420(5) 0.2612(3) 0.2470(2) 0.0129(7) Uani 1 1 d . . . C6 C -0.0510(5) 0.2034(3) 0.1723(2) 0.0144(6) Uani 1 1 d . . . H6A H 0.0840 0.2193 0.1684 0.017 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 Cu1 0.0126(3) 0.0129(2) 0.0113(3) 0.00220(18) -0.0013(2) -0.0003(2) Cu2 0.0108(3) 0.0113(2) 0.0082(2) -0.00140(18) -0.00091(19) -0.00086(19) S1 0.0194(5) 0.0175(4) 0.0222(4) 0.0016(3) 0.0002(3) -0.0022(3) O1 0.0112(13) 0.0107(9) 0.0185(11) 0.0004(8) -0.0006(8) 0.0003(8) O2 0.0322(18) 0.0168(11) 0.0360(14) -0.0066(10) -0.0004(12) 0.0000(10) O3 0.0208(18) 0.0407(16) 0.0416(16) 0.0187(12) -0.0005(12) 0.0005(12) O4 0.041(2) 0.0333(14) 0.0305(14) -0.0045(12) 0.0134(13) -0.0055(13) O5 0.0310(19) 0.0448(16) 0.0355(16) -0.0111(12) 0.0032(12) 0.0019(13) N1 0.0134(17) 0.0170(12) 0.0116(12) -0.0015(10) 0.0020(10) -0.0023(10) N2 0.0113(16) 0.0135(11) 0.0091(11) -0.0022(9) -0.0025(10) -0.0013(10) N3 0.0139(17) 0.0150(12) 0.0105(12) -0.0021(9) 0.0003(10) -0.0024(10) N4 0.0124(16) 0.0156(12) 0.0116(12) -0.0032(10) 0.0012(10) -0.0007(10) N5 0.029(2) 0.0150(13) 0.0272(15) 0.0057(12) -0.0028(13) -0.0007(12) C1 0.0123(19) 0.0175(14) 0.0127(14) -0.0040(11) 0.0005(12) -0.0023(12) C2 0.013(2) 0.0140(13) 0.0102(13) -0.0011(11) -0.0007(12) -0.0007(11) C3 0.0107(19) 0.0194(15) 0.0126(14) -0.0029(11) -0.0009(12) -0.0023(12) C4 0.0111(19) 0.0156(14) 0.0134(14) -0.0007(11) -0.0012(12) -0.0021(12) C5 0.016(2) 0.0129(13) 0.0089(13) 0.0008(10) -0.0013(12) 0.0010(11) C6 0.0100(19) 0.0185(14) 0.0143(14) -0.0027(11) 0.0005(12) 0.0001(12) _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 Cu1 O1 1.941(2) 3_466 ? Cu1 O1 1.941(2) . ? Cu1 N3 2.098(2) 4_566 ? Cu1 N3 2.098(2) 2_455 ? Cu2 O1 1.950(2) . ? Cu2 O1 1.950(2) 3_566 ? Cu2 N2 2.107(2) 3_566 ? Cu2 N2 2.107(2) . ? Cu2 N4 2.393(3) 4_566 ? Cu2 N4 2.393(3) 2 ? S1 O3 1.452(3) . ? S1 O4 1.462(3) . ? S1 O2 1.463(3) . ? S1 N5 1.630(3) . ? N1 C1 1.314(4) . ? N1 N2 1.373(4) . ? N2 C4 1.311(4) . ? N3 C3 1.312(4) . ? N3 N4 1.374(4) . ? N3 Cu1 2.098(2) 2_445 ? N4 C6 1.313(4) . ? N4 Cu2 2.393(3) 2_545 ? C1 C2 1.422(4) . ? C2 C5 1.381(5) . ? C2 C3 1.426(4) . ? C4 C5 1.429(4) . ? C5 C6 1.433(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 O1 Cu1 O1 180.00(10) 3_466 . ? O1 Cu1 N3 92.03(10) 3_466 4_566 ? O1 Cu1 N3 87.97(10) . 4_566 ? O1 Cu1 N3 87.97(10) 3_466 2_455 ? O1 Cu1 N3 92.03(10) . 2_455 ? N3 Cu1 N3 180.000(1) 4_566 2_455 ? O1 Cu2 O1 180.000(1) . 3_566 ? O1 Cu2 N2 92.74(10) . 3_566 ? O1 Cu2 N2 87.26(10) 3_566 3_566 ? O1 Cu2 N2 87.26(10) . . ? O1 Cu2 N2 92.74(10) 3_566 . ? N2 Cu2 N2 180.0 3_566 . ? O1 Cu2 N4 81.87(9) . 4_566 ? O1 Cu2 N4 98.13(9) 3_566 4_566 ? N2 Cu2 N4 90.60(9) 3_566 4_566 ? N2 Cu2 N4 89.40(9) . 4_566 ? O1 Cu2 N4 98.13(9) . 2 ? O1 Cu2 N4 81.87(9) 3_566 2 ? N2 Cu2 N4 89.40(9) 3_566 2 ? N2 Cu2 N4 90.60(9) . 2 ? N4 Cu2 N4 180.0 4_566 2 ? O3 S1 O4 113.37(17) . . ? O3 S1 O2 110.97(18) . . ? O4 S1 O2 110.99(17) . . ? O3 S1 N5 105.32(16) . . ? O4 S1 N5 105.01(17) . . ? O2 S1 N5 110.86(16) . . ? Cu1 O1 Cu2 121.40(10) . . ? C1 N1 N2 119.6(3) . . ? C4 N2 N1 121.4(3) . . ? C4 N2 Cu2 124.8(2) . . ? N1 N2 Cu2 113.83(18) . . ? C3 N3 N4 120.8(3) . . ? C3 N3 Cu1 122.1(2) . 2_445 ? N4 N3 Cu1 117.05(18) . 2_445 ? C6 N4 N3 120.3(3) . . ? C6 N4 Cu2 123.9(2) . 2_545 ? N3 N4 Cu2 115.29(17) . 2_545 ? N1 C1 C2 122.3(3) . . ? C5 C2 C1 117.8(3) . . ? C5 C2 C3 117.9(3) . . ? C1 C2 C3 124.3(3) . . ? N3 C3 C2 121.6(3) . . ? N2 C4 C5 121.4(3) . . ? C2 C5 C4 117.6(3) . . ? C2 C5 C6 117.4(3) . . ? C4 C5 C6 125.0(3) . . ? N4 C6 C5 121.9(3) . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 27.97 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.720 _refine_diff_density_min -0.587 _refine_diff_density_rms 0.110 #============================================================================== data_5 _database_code_depnum_ccdc_archive 'CCDC 622647' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Silver(I) Methanesulfonate Complex with Pyridazino[4,5-d]pyridazine, Dihydrate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H6 Ag N4 O, C H3 O3 S, H2 O' _chemical_formula_sum 'C7 H11 Ag N4 O5 S' _chemical_formula_weight 371.13 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _space_group_name_Hall 'P 2ac 2ab' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 7.4389(5) _cell_length_b 10.5720(10) _cell_length_c 14.7775(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1162.16(16) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 2762 _cell_measurement_theta_min 3.07 _cell_measurement_theta_max 28.06 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.14 _exptl_crystal_density_diffrn 2.121 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 736 _exptl_absorpt_coefficient_mu 1.934 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.6884 _exptl_absorpt_correction_T_max 0.7631 _exptl_absorpt_process_details ; (See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 Imaging Plate Diffraction system' _diffrn_measurement_method '\f oscillation scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9681 _diffrn_reflns_av_R_equivalents 0.0389 _diffrn_reflns_av_sigmaI/netI 0.0341 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 28.06 _reflns_number_total 2762 _reflns_number_gt 2309 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS Software (Stoe&Cie, 2000)' _computing_cell_refinement 'IPDS Software (Stoe&Cie, 2000)' _computing_data_reduction 'IPDS Software (Stoe&Cie, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e (Brandenburg, 1999)' _computing_publication_material 'WinGX 1.700.00 (Farrugia, 1999)' _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^)+(0.0229P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.44(2) _refine_ls_number_reflns 2762 _refine_ls_number_parameters 164 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0244 _refine_ls_R_factor_gt 0.0201 _refine_ls_wR_factor_ref 0.0431 _refine_ls_wR_factor_gt 0.0425 _refine_ls_goodness_of_fit_ref 0.952 _refine_ls_restrained_S_all 0.952 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag -0.03506(3) -0.235654(14) 1.499506(15) 0.02655(6) Uani 1 1 d . . . S1 S 0.30029(9) -0.24839(5) 1.11585(4) 0.02386(13) Uani 1 1 d . . . O1 O 0.4673(3) -0.2109(2) 1.15874(13) 0.0403(5) Uani 1 1 d . . . O2 O 0.2993(4) -0.38163(17) 1.09396(15) 0.0483(7) Uani 1 1 d . . . O3 O 0.1455(3) -0.2116(2) 1.16794(13) 0.0403(5) Uani 1 1 d . . . O4 O -0.2936(3) -0.07517(17) 1.52752(13) 0.0363(5) Uani 1 1 d . . . H1 H -0.2886 -0.0213 1.4886 0.054 Uiso 1 1 d R . . H2 H -0.2850 -0.0418 1.5777 0.054 Uiso 1 1 d R . . O5 O -0.1978(3) -0.09530(18) 1.17482(14) 0.0382(5) Uani 1 1 d . . . H3 H -0.2814 -0.1402 1.1661 0.057 Uiso 1 1 d R . . H4 H -0.1022 -0.1385 1.1673 0.057 Uiso 1 1 d R . . N1 N 0.1381(3) -0.10306(19) 1.39279(14) 0.0238(5) Uani 1 1 d . . . N2 N 0.3203(3) -0.1225(2) 1.38997(14) 0.0243(5) Uani 1 1 d . . . N3 N 0.1826(3) 0.17613(19) 1.13839(13) 0.0253(5) Uani 1 1 d . . . N4 N 0.3651(4) 0.15679(19) 1.13577(13) 0.0246(5) Uani 1 1 d . . . C1 C 0.0616(4) -0.0248(2) 1.33602(16) 0.0234(6) Uani 1 1 d . . . H1A H -0.0621 -0.0130 1.3391 0.028 Uiso 1 1 d R . . C2 C 0.1619(4) 0.0434(2) 1.26971(15) 0.0200(5) Uani 1 1 d . . . C3 C 0.0861(4) 0.1242(2) 1.20291(16) 0.0233(6) Uani 1 1 d . . . H3A H -0.0364 0.1413 1.2054 0.028 Uiso 1 1 d R . . C4 C 0.4194(4) -0.0624(2) 1.33046(16) 0.0224(6) Uani 1 1 d . . . H4A H 0.5427 -0.0771 1.3295 0.027 Uiso 1 1 d R . . C5 C 0.3445(4) 0.0242(2) 1.26688(15) 0.0202(5) Uani 1 1 d . . . C6 C 0.4432(4) 0.0870(2) 1.19806(17) 0.0233(6) Uani 1 1 d . . . H6A H 0.5677 0.0785 1.1970 0.028 Uiso 1 1 d R . . C7 C 0.2910(5) -0.1647(3) 1.01295(19) 0.0447(8) Uani 1 1 d . . . H7A H 0.1732 -0.1737 0.9872 0.067 Uiso 1 1 d R . . H7B H 0.3790 -0.1970 0.9714 0.067 Uiso 1 1 d R . . H7C H 0.3157 -0.0767 1.0232 0.067 Uiso 1 1 d 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 Ag1 0.02732(11) 0.02773(8) 0.02460(7) 0.00128(12) 0.00092(9) -0.00424(7) S1 0.0244(4) 0.0197(3) 0.0274(2) -0.0013(2) 0.0020(2) -0.0017(2) O1 0.0292(15) 0.0472(11) 0.0444(11) -0.0021(9) -0.0061(9) -0.0063(10) O2 0.067(2) 0.0217(9) 0.0565(14) -0.0103(9) 0.0056(12) -0.0051(10) O3 0.0303(16) 0.0438(11) 0.0467(10) -0.0016(9) 0.0110(10) 0.0037(10) O4 0.0414(16) 0.0267(9) 0.0407(11) 0.0032(7) -0.0010(8) 0.0012(8) O5 0.0296(16) 0.0334(10) 0.0516(13) -0.0036(9) -0.0039(10) 0.0001(9) N1 0.0193(15) 0.0252(10) 0.0267(10) 0.0003(8) 0.0006(10) -0.0011(9) N2 0.0215(16) 0.0252(10) 0.0263(10) 0.0012(8) -0.0013(9) -0.0008(9) N3 0.0238(17) 0.0251(11) 0.0269(10) 0.0014(8) 0.0005(9) 0.0036(9) N4 0.0216(16) 0.0232(10) 0.0290(11) 0.0007(8) 0.0003(10) -0.0017(9) C1 0.019(2) 0.0279(12) 0.0236(11) -0.0021(9) 0.0016(10) -0.0005(10) C2 0.0200(17) 0.0165(10) 0.0236(11) -0.0029(9) 0.0014(10) -0.0007(9) C3 0.0162(17) 0.0262(12) 0.0276(12) 0.0007(10) 0.0009(10) 0.0044(10) C4 0.0151(18) 0.0244(11) 0.0277(12) -0.0022(10) 0.0000(10) 0.0013(9) C5 0.0201(17) 0.0178(10) 0.0226(10) -0.0019(9) -0.0010(10) -0.0018(9) C6 0.0146(18) 0.0249(11) 0.0303(13) 0.0017(10) -0.0002(11) -0.0013(10) C7 0.051(2) 0.0486(15) 0.0342(15) 0.0109(14) -0.0029(15) -0.0011(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 Ag1 N2 2.464(2) 3_448 ? Ag1 N1 2.472(2) . ? Ag1 N3 2.495(2) 4_547 ? Ag1 N4 2.520(2) 2 ? Ag1 O4 2.598(2) . ? S1 O3 1.438(2) . ? S1 O2 1.4453(19) . ? S1 O1 1.450(2) . ? S1 C7 1.761(3) . ? N1 C1 1.309(3) . ? N1 N2 1.371(4) . ? N2 C4 1.312(3) . ? N3 C3 1.313(3) . ? N3 N4 1.374(4) . ? N4 C6 1.315(3) . ? C1 C2 1.427(3) . ? C2 C5 1.374(4) . ? C2 C3 1.422(3) . ? C4 C5 1.426(3) . ? C5 C6 1.419(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 N2 Ag1 N1 174.41(8) 3_448 . ? N2 Ag1 N3 97.00(8) 3_448 4_547 ? N1 Ag1 N3 85.42(7) . 4_547 ? N2 Ag1 N4 83.73(7) 3_448 2 ? N1 Ag1 N4 93.48(8) . 2 ? N3 Ag1 N4 175.56(8) 4_547 2 ? N2 Ag1 O4 88.20(7) 3_448 . ? N1 Ag1 O4 96.73(7) . . ? N3 Ag1 O4 92.79(7) 4_547 . ? N4 Ag1 O4 91.61(7) 2 . ? O3 S1 O2 112.28(15) . . ? O3 S1 O1 112.22(14) . . ? O2 S1 O1 111.62(15) . . ? O3 S1 C7 107.15(15) . . ? O2 S1 C7 107.24(14) . . ? O1 S1 C7 105.89(15) . . ? C1 N1 N2 120.3(2) . . ? C1 N1 Ag1 122.7(2) . . ? N2 N1 Ag1 116.70(15) . . ? C4 N2 N1 120.2(2) . . ? C4 N2 Ag1 119.59(19) . 3_548 ? N1 N2 Ag1 120.17(15) . 3_548 ? C3 N3 N4 119.9(2) . . ? C3 N3 Ag1 120.6(2) . 4_557 ? N4 N3 Ag1 117.86(14) . 4_557 ? C6 N4 N3 120.0(2) . . ? C6 N4 Ag1 121.5(2) . 2_554 ? N3 N4 Ag1 117.99(14) . 2_554 ? N1 C1 C2 122.2(3) . . ? C5 C2 C3 117.4(2) . . ? C5 C2 C1 117.6(2) . . ? C3 C2 C1 124.9(3) . . ? N3 C3 C2 122.6(3) . . ? N2 C4 C5 122.2(3) . . ? C2 C5 C6 117.7(2) . . ? C2 C5 C4 117.5(2) . . ? C6 C5 C4 124.8(3) . . ? N4 C6 C5 122.3(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 N2 Ag1 N1 C1 174.7(7) 3_448 . . . ? N3 Ag1 N1 C1 58.72(19) 4_547 . . . ? N4 Ag1 N1 C1 -125.59(19) 2 . . . ? O4 Ag1 N1 C1 -33.6(2) . . . . ? N2 Ag1 N1 N2 0.0(9) 3_448 . . . ? N3 Ag1 N1 N2 -115.94(17) 4_547 . . . ? N4 Ag1 N1 N2 59.75(18) 2 . . . ? O4 Ag1 N1 N2 151.79(17) . . . . ? C1 N1 N2 C4 0.2(4) . . . . ? Ag1 N1 N2 C4 175.04(18) . . . . ? C1 N1 N2 Ag1 177.86(17) . . . 3_548 ? Ag1 N1 N2 Ag1 -7.3(2) . . . 3_548 ? C3 N3 N4 C6 -0.4(3) . . . . ? Ag1 N3 N4 C6 -165.72(18) 4_557 . . . ? C3 N3 N4 Ag1 172.31(17) . . . 2_554 ? Ag1 N3 N4 Ag1 7.0(2) 4_557 . . 2_554 ? N2 N1 C1 C2 -0.2(4) . . . . ? Ag1 N1 C1 C2 -174.71(17) . . . . ? N1 C1 C2 C5 0.1(4) . . . . ? N1 C1 C2 C3 176.3(2) . . . . ? N4 N3 C3 C2 -2.5(4) . . . . ? Ag1 N3 C3 C2 162.50(18) 4_557 . . . ? C5 C2 C3 N3 2.4(4) . . . . ? C1 C2 C3 N3 -173.8(2) . . . . ? N1 N2 C4 C5 -0.1(4) . . . . ? Ag1 N2 C4 C5 -177.77(18) 3_548 . . . ? C3 C2 C5 C6 0.4(3) . . . . ? C1 C2 C5 C6 176.9(2) . . . . ? C3 C2 C5 C4 -176.5(2) . . . . ? C1 C2 C5 C4 0.0(3) . . . . ? N2 C4 C5 C2 0.0(4) . . . . ? N2 C4 C5 C6 -176.6(2) . . . . ? N3 N4 C6 C5 3.2(4) . . . . ? Ag1 N4 C6 C5 -169.20(17) 2_554 . . . ? C2 C5 C6 N4 -3.2(4) . . . . ? C4 C5 C6 N4 173.4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 28.06 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.402 _refine_diff_density_min -0.714 _refine_diff_density_rms 0.067 #==============================================================================