Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 # 1. SUBMISSION DETAILS _publ_contact_author ; 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 ? #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; 4,4'-Bipyridazine, a new twist for the synthesis of coordination polymers ; loop_ _publ_author_name _publ_author_address K.V.Domasevitch ; Inorganic Chemistry Department Kiev Shevchenko University Volodimirska Str. 64 01033 Kiev Ukraine ; I.A.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 ; E.B.Rusanov ; Institute of Organic Chemistry Murmanskaya Str. 4 253660 Kiev Ukraine ; ; H.Krautscheid ; ; Institute of Inorganic Chemistry Leipzig University Linnestrasse 3 D-04103 Leipzig Germany ; J.A.K.Howard ; Department of Chemistry University of Durham Durham DH1 3LE UK ; A.N.Chernega ; Institute of Organic Chemistry Murmanskaya Str. 4 253660 Kiev Ukraine ; _publ_section_acknowledgements ; KVD and HK acknowledge support from Deutsche Forschungsgemeinschaft. ; _publ_contact_author_name 'Konstantin V. Domasevitch' #============================================================================== data_(1) _database_code_depnum_ccdc_archive 'CCDC 640632' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Copper(II) acetate 2:1 complex with 4,4'-Bipyridazine, Dihydrate ; _chemical_name_common ;Copper(ii) acetate 2:1 complex with 4,4'-Bipyridazine, Dihydrate ; _chemical_melting_point ? _chemical_formula_moiety 'C8 H9 Cu N2 O4, 2(H2 O)' _chemical_formula_sum 'C16 H26 Cu2 N4 O12' _chemical_formula_weight 593.49 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 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 7.4144(9) _cell_length_b 8.2275(9) _cell_length_c 10.9023(13) _cell_angle_alpha 76.965(14) _cell_angle_beta 82.505(13) _cell_angle_gamma 63.267(13) _cell_volume 578.35(14) _cell_formula_units_Z 1 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 6716 _cell_measurement_theta_min 3.08 _cell_measurement_theta_max 28.08 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_diffrn 1.704 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 304 _exptl_absorpt_coefficient_mu 1.907 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.6443 _exptl_absorpt_correction_T_max 0.7351 _exptl_absorpt_process_details 'DIFABS, (Walker & Stuart, 1983)' _exptl_special_details ; Walker, N. & Stuart, D. 1983. Acta Cryst. A39, 158-166. ; _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_standards_decay_% 0 _diffrn_reflns_number 6716 _diffrn_reflns_av_R_equivalents 0.0297 _diffrn_reflns_av_sigmaI/netI 0.0300 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 28.08 _reflns_number_total 2758 _reflns_number_gt 2229 _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^)+(0.0503P)^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_number_reflns 2758 _refine_ls_number_parameters 154 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0319 _refine_ls_R_factor_gt 0.0272 _refine_ls_wR_factor_ref 0.0750 _refine_ls_wR_factor_gt 0.0742 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _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 0.07768(3) 0.49990(3) 0.10176(2) 0.01661(9) Uani 1 1 d . . . O1 O 0.0254(3) 0.2821(2) 0.18107(14) 0.0282(3) Uani 1 1 d . . . O2 O -0.1046(3) 0.2841(2) 0.00717(14) 0.0291(3) Uani 1 1 d . . . O3 O -0.1978(2) 0.6631(2) 0.15231(14) 0.0281(3) Uani 1 1 d . . . O4 O -0.3283(2) 0.6666(2) -0.02247(14) 0.0269(3) Uani 1 1 d . . . O5 O -0.3468(3) 0.8430(3) 0.3848(2) 0.0598(6) Uani 1 1 d . . . H1 H -0.2865 0.8469 0.4452 0.090 Uiso 1 1 d . . . H2 H -0.2549 0.7950 0.3299 0.090 Uiso 1 1 d . . . O6 O -0.2378(4) 0.9451(3) 0.5842(2) 0.0635(6) Uani 1 1 d . . . H3 H -0.3653 1.0015 0.5969 0.095 Uiso 1 1 d . . . H4 H -0.1907 0.8575 0.6478 0.095 Uiso 1 1 d . . . N1 N 0.2387(3) 0.4930(2) 0.25782(16) 0.0215(4) Uani 1 1 d . . . N2 N 0.1377(3) 0.5806(3) 0.3501(2) 0.0436(6) Uani 1 1 d . . . C1 C 0.4367(4) 0.4130(5) 0.2571(3) 0.0576(10) Uani 1 1 d . . . H1A H 0.5068 0.3545 0.1893 0.069 Uiso 1 1 calc R . . C2 C 0.5486(4) 0.4098(5) 0.3510(3) 0.0570(10) Uani 1 1 d . . . H2A H 0.6905 0.3488 0.3475 0.068 Uiso 1 1 calc R . . C3 C 0.4484(3) 0.4966(2) 0.44769(17) 0.0178(4) Uani 1 1 d . . . C4 C 0.2395(4) 0.5824(4) 0.4405(2) 0.0486(8) Uani 1 1 d . . . H4A H 0.1645 0.6468 0.5049 0.058 Uiso 1 1 calc R . . C5 C -0.0518(3) 0.2179(3) 0.11929(19) 0.0224(4) Uani 1 1 d . . . C6 C -0.0823(4) 0.0495(3) 0.1839(2) 0.0346(5) Uani 1 1 d . . . H6A H -0.0139 -0.0478 0.1349 0.052 Uiso 1 1 calc R . . H6B H -0.2256 0.0812 0.1911 0.052 Uiso 1 1 calc R . . H6C H -0.0271 0.0067 0.2672 0.052 Uiso 1 1 calc R . . C7 C -0.3426(3) 0.7141(3) 0.08128(18) 0.0211(4) Uani 1 1 d . . . C8 C -0.5498(3) 0.8420(3) 0.1248(2) 0.0364(6) Uani 1 1 d . . . H8A H -0.6470 0.8725 0.0619 0.055 Uiso 1 1 calc R . . H8B H -0.5481 0.9546 0.1367 0.055 Uiso 1 1 calc R . . H8C H -0.5877 0.7811 0.2039 0.055 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 0.01406(13) 0.01868(13) 0.01703(13) -0.00858(8) -0.00399(8) -0.00377(9) O1 0.0355(9) 0.0278(7) 0.0248(7) -0.0035(6) -0.0055(6) -0.0162(7) O2 0.0373(9) 0.0283(7) 0.0286(8) -0.0053(6) -0.0075(7) -0.0186(7) O3 0.0185(7) 0.0349(8) 0.0260(7) -0.0165(6) -0.0031(6) -0.0016(6) O4 0.0177(7) 0.0329(7) 0.0265(7) -0.0161(6) -0.0027(6) -0.0027(6) O5 0.0528(13) 0.0770(15) 0.0499(12) -0.0324(11) 0.0184(10) -0.0244(12) O6 0.0552(13) 0.0832(16) 0.0444(12) -0.0059(11) -0.0126(10) -0.0235(12) N1 0.0189(8) 0.0255(8) 0.0209(8) -0.0098(6) -0.0056(6) -0.0065(7) N2 0.0183(9) 0.0742(15) 0.0356(11) -0.0360(11) -0.0059(8) -0.0045(10) C1 0.0211(12) 0.101(2) 0.0501(16) -0.0597(17) -0.0052(11) -0.0043(14) C2 0.0156(11) 0.101(2) 0.0489(16) -0.0533(17) -0.0076(10) -0.0010(14) C3 0.0185(9) 0.0225(8) 0.0141(8) -0.0038(7) -0.0042(7) -0.0093(7) C4 0.0202(11) 0.085(2) 0.0375(13) -0.0447(14) -0.0026(9) -0.0044(12) C5 0.0191(9) 0.0194(8) 0.0275(10) -0.0099(7) 0.0039(8) -0.0060(7) C6 0.0412(13) 0.0269(10) 0.0391(13) -0.0061(9) 0.0041(11) -0.0191(10) C7 0.0173(9) 0.0204(8) 0.0221(9) -0.0073(7) -0.0001(7) -0.0037(7) C8 0.0199(10) 0.0440(13) 0.0305(11) -0.0163(10) 0.0007(9) 0.0029(10) _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 O3 1.9624(15) . ? Cu1 O4 1.9752(14) 2_565 ? Cu1 O2 1.9779(15) 2_565 ? Cu1 O1 1.9863(15) . ? Cu1 N1 2.1789(18) . ? Cu1 Cu1 2.6294(6) 2_565 ? O1 C5 1.263(3) . ? O2 C5 1.256(3) . ? O3 C7 1.262(3) . ? O4 C7 1.255(2) . ? O5 H1 0.8562 . ? O5 H2 0.8586 . ? O6 H3 0.8534 . ? O6 H4 0.8566 . ? N1 C1 1.311(3) . ? N1 N2 1.318(3) . ? N2 C4 1.324(3) . ? C1 C2 1.388(3) . ? C1 H1A 0.9400 . ? C2 C3 1.353(3) . ? C2 H2A 0.9400 . ? C3 C4 1.388(3) . ? C3 C3 1.478(4) 2_666 ? C4 H4A 0.9400 . ? C5 C6 1.505(3) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 H6C 0.9700 . ? C7 C8 1.508(3) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? 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 O3 Cu1 O4 168.49(6) . 2_565 ? O3 Cu1 O2 89.93(7) . 2_565 ? O4 Cu1 O2 89.48(7) 2_565 2_565 ? O3 Cu1 O1 89.20(7) . . ? O4 Cu1 O1 89.07(7) 2_565 . ? O2 Cu1 O1 168.41(6) 2_565 . ? O3 Cu1 N1 98.91(6) . . ? O4 Cu1 N1 92.59(6) 2_565 . ? O2 Cu1 N1 95.04(7) 2_565 . ? O1 Cu1 N1 96.51(7) . . ? O3 Cu1 Cu1 86.99(5) . 2_565 ? O4 Cu1 Cu1 81.54(5) 2_565 2_565 ? O2 Cu1 Cu1 82.05(5) 2_565 2_565 ? O1 Cu1 Cu1 86.36(5) . 2_565 ? N1 Cu1 Cu1 173.45(5) . 2_565 ? C5 O1 Cu1 120.65(13) . . ? C5 O2 Cu1 126.33(15) . 2_565 ? C7 O3 Cu1 120.08(13) . . ? C7 O4 Cu1 126.02(14) . 2_565 ? H1 O5 H2 106.7 . . ? H3 O6 H4 107.3 . . ? C1 N1 N2 119.12(19) . . ? C1 N1 Cu1 120.69(15) . . ? N2 N1 Cu1 120.03(14) . . ? N1 N2 C4 118.90(19) . . ? N1 C1 C2 123.6(2) . . ? N1 C1 H1A 118.2 . . ? C2 C1 H1A 118.2 . . ? C3 C2 C1 118.4(2) . . ? C3 C2 H2A 120.8 . . ? C1 C2 H2A 120.8 . . ? C2 C3 C4 114.83(19) . . ? C2 C3 C3 123.1(2) . 2_666 ? C4 C3 C3 122.0(2) . 2_666 ? N2 C4 C3 125.1(2) . . ? N2 C4 H4A 117.4 . . ? C3 C4 H4A 117.4 . . ? O2 C5 O1 124.60(19) . . ? O2 C5 C6 117.4(2) . . ? O1 C5 C6 117.99(19) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O4 C7 O3 125.35(18) . . ? O4 C7 C8 117.29(19) . . ? O3 C7 C8 117.36(18) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? 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 O3 Cu1 O1 C5 87.86(16) . . . . ? O4 Cu1 O1 C5 -80.75(16) 2_565 . . . ? O2 Cu1 O1 C5 2.1(4) 2_565 . . . ? N1 Cu1 O1 C5 -173.26(15) . . . . ? Cu1 Cu1 O1 C5 0.83(15) 2_565 . . . ? O4 Cu1 O3 C7 -6.4(4) 2_565 . . . ? O2 Cu1 O3 C7 80.63(17) 2_565 . . . ? O1 Cu1 O3 C7 -87.81(16) . . . . ? N1 Cu1 O3 C7 175.72(16) . . . . ? Cu1 Cu1 O3 C7 -1.42(16) 2_565 . . . ? O3 Cu1 N1 C1 -172.7(2) . . . . ? O4 Cu1 N1 C1 7.7(2) 2_565 . . . ? O2 Cu1 N1 C1 -82.0(2) 2_565 . . . ? O1 Cu1 N1 C1 97.1(2) . . . . ? O3 Cu1 N1 N2 2.6(2) . . . . ? O4 Cu1 N1 N2 -176.98(19) 2_565 . . . ? O2 Cu1 N1 N2 93.32(19) 2_565 . . . ? O1 Cu1 N1 N2 -87.61(19) . . . . ? C1 N1 N2 C4 -1.1(4) . . . . ? Cu1 N1 N2 C4 -176.5(2) . . . . ? N2 N1 C1 C2 2.1(5) . . . . ? Cu1 N1 C1 C2 177.4(3) . . . . ? N1 C1 C2 C3 -1.2(6) . . . . ? C1 C2 C3 C4 -0.6(5) . . . . ? C1 C2 C3 C3 -179.6(3) . . . 2_666 ? N1 N2 C4 C3 -0.6(5) . . . . ? C2 C3 C4 N2 1.5(5) . . . . ? C3 C3 C4 N2 -179.5(3) 2_666 . . . ? Cu1 O2 C5 O1 1.0(3) 2_565 . . . ? Cu1 O2 C5 C6 -178.69(14) 2_565 . . . ? Cu1 O1 C5 O2 -1.3(3) . . . . ? Cu1 O1 C5 C6 178.39(14) . . . . ? Cu1 O4 C7 O3 0.2(3) 2_565 . . . ? Cu1 O4 C7 C8 -179.58(15) 2_565 . . . ? Cu1 O3 C7 O4 1.2(3) . . . . ? Cu1 O3 C7 C8 -179.04(16) . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 28.08 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.422 _refine_diff_density_min -0.389 _refine_diff_density_rms 0.070 #============================================================================== data_(2) _database_code_depnum_ccdc_archive 'CCDC 640633' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Zinc(II) Nitrate 1:1 Complex with 4,4'-Bipyridazine ; _chemical_name_common "Zinc(ii) Nitrate 1:1 Complex with 4,4'-Bipyridazine" _chemical_melting_point ? _chemical_formula_moiety 'C8 H6 N6 O6 Zn' _chemical_formula_sum 'C8 H6 N6 O6 Zn' _chemical_formula_weight 347.56 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 6.07500(10) _cell_length_b 16.9431(3) _cell_length_c 11.9592(2) _cell_angle_alpha 90.00 _cell_angle_beta 101.3800(10) _cell_angle_gamma 90.00 _cell_volume 1206.75(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7745 _cell_measurement_theta_min 2.97 _cell_measurement_theta_max 28.70 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.913 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 696 _exptl_absorpt_coefficient_mu 2.078 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4104 _exptl_absorpt_correction_T_max 0.6609 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 Apex CCD area-detector diffractometer' _diffrn_measurement_method '\w scans' _diffrn_standards_decay_% 0 _diffrn_reflns_number 7745 _diffrn_reflns_av_R_equivalents 0.0225 _diffrn_reflns_av_sigmaI/netI 0.0283 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 28.70 _reflns_number_total 3070 _reflns_number_gt 2339 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT (Bruker, 1998)' _computing_cell_refinement 'SMART-NT (Bruker, 1998)' _computing_data_reduction 'SMART-NT (Bruker, 1998)' _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^)+(0.0326P)^2^+0.3999P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 3070 _refine_ls_number_parameters 214 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0388 _refine_ls_R_factor_gt 0.0279 _refine_ls_wR_factor_ref 0.0717 _refine_ls_wR_factor_gt 0.0670 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _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 Zn1 Zn 0.83620(4) 1.107448(15) 0.775966(19) 0.03407(9) Uani 1 1 d . . . O1 O 1.1127(3) 1.18787(14) 0.84953(19) 0.0730(6) Uani 1 1 d . . . O2 O 0.9846(3) 1.10280(11) 0.95027(14) 0.0549(4) Uani 1 1 d . . . O3 O 1.2553(3) 1.17951(15) 1.03032(19) 0.0815(7) Uani 1 1 d . . . O4 O 1.0885(3) 1.04650(14) 0.70216(15) 0.0706(6) Uani 1 1 d . . . O5 O 0.8714(3) 1.11812(12) 0.58608(16) 0.0636(5) Uani 1 1 d . . . O6 O 1.1650(3) 1.06808(12) 0.53668(13) 0.0541(4) Uani 1 1 d . . . N1 N 0.6358(3) 1.01033(11) 0.77214(13) 0.0339(4) Uani 1 1 d . . . N2 N 0.5370(3) 1.00153(11) 0.86266(13) 0.0380(4) Uani 1 1 d . . . N3 N -0.1125(3) 0.69886(10) 0.75467(13) 0.0327(4) Uani 1 1 d . . . N4 N -0.1166(3) 0.74666(12) 0.66441(14) 0.0409(4) Uani 1 1 d . . . N5 N 1.1232(3) 1.15792(13) 0.94646(19) 0.0509(5) Uani 1 1 d . . . N6 N 1.0436(3) 1.07747(12) 0.60574(14) 0.0384(4) Uani 1 1 d . . . C1 C 0.3994(4) 0.94113(13) 0.86242(16) 0.0369(5) Uani 1 1 d . . . C2 C 0.3481(3) 0.88624(12) 0.77351(15) 0.0327(4) Uani 1 1 d . . . C3 C 0.4523(4) 0.89689(14) 0.68311(18) 0.0411(5) Uani 1 1 d . . . C4 C 0.5961(4) 0.96016(14) 0.68611(18) 0.0414(5) Uani 1 1 d . . . C5 C 0.0291(4) 0.80462(14) 0.67518(17) 0.0400(5) Uani 1 1 d . . . C6 C 0.1876(3) 0.82155(13) 0.77458(15) 0.0321(4) Uani 1 1 d . . . C7 C 0.1840(3) 0.77343(14) 0.86605(16) 0.0378(5) Uani 1 1 d . . . C8 C 0.0296(4) 0.71215(14) 0.85142(17) 0.0389(5) Uani 1 1 d . . . H1 H 0.334(4) 0.9378(15) 0.9251(19) 0.042(6) Uiso 1 1 d . . . H3 H 0.426(4) 0.8616(17) 0.624(2) 0.054(7) Uiso 1 1 d . . . H4 H 0.675(4) 0.9691(15) 0.627(2) 0.053(7) Uiso 1 1 d . . . H5 H 0.019(4) 0.8388(14) 0.6125(19) 0.040(6) Uiso 1 1 d . . . H7 H 0.279(4) 0.7800(15) 0.934(2) 0.053(7) Uiso 1 1 d . . . H8 H 0.020(4) 0.6777(16) 0.912(2) 0.049(7) 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 0.03210(12) 0.03200(17) 0.03933(13) -0.00089(10) 0.00997(9) -0.00011(10) O1 0.0515(10) 0.0817(16) 0.0826(14) 0.0259(12) 0.0055(9) -0.0130(10) O2 0.0590(10) 0.0536(12) 0.0497(9) 0.0012(8) 0.0047(8) -0.0148(9) O3 0.0546(11) 0.0884(17) 0.0878(14) -0.0302(12) -0.0189(10) -0.0018(11) O4 0.0581(10) 0.1114(19) 0.0442(9) 0.0236(10) 0.0143(8) 0.0139(11) O5 0.0618(11) 0.0663(14) 0.0662(11) 0.0091(9) 0.0212(9) 0.0286(9) O6 0.0559(10) 0.0644(13) 0.0501(9) -0.0037(8) 0.0301(8) 0.0014(8) N1 0.0356(8) 0.0332(10) 0.0341(8) -0.0012(7) 0.0098(6) -0.0024(7) N2 0.0454(9) 0.0392(12) 0.0307(8) -0.0043(7) 0.0108(7) -0.0066(8) N3 0.0345(8) 0.0311(11) 0.0328(8) 0.0024(7) 0.0077(6) -0.0011(7) N4 0.0417(9) 0.0448(12) 0.0335(8) 0.0074(8) 0.0004(7) -0.0083(8) N5 0.0332(9) 0.0512(15) 0.0645(13) -0.0107(10) 0.0006(8) 0.0032(8) N6 0.0391(9) 0.0435(12) 0.0345(8) -0.0014(7) 0.0119(7) -0.0029(8) C1 0.0456(11) 0.0387(14) 0.0280(8) -0.0011(8) 0.0111(8) -0.0058(9) C2 0.0345(9) 0.0317(12) 0.0312(9) 0.0018(8) 0.0045(7) -0.0003(8) C3 0.0493(12) 0.0396(14) 0.0375(10) -0.0112(9) 0.0163(9) -0.0082(10) C4 0.0498(11) 0.0407(15) 0.0389(10) -0.0076(9) 0.0212(9) -0.0095(10) C5 0.0431(11) 0.0423(14) 0.0311(9) 0.0107(9) -0.0007(8) -0.0067(9) C6 0.0336(9) 0.0321(12) 0.0307(9) -0.0005(8) 0.0067(7) -0.0007(8) C7 0.0410(10) 0.0412(14) 0.0288(9) 0.0025(8) 0.0013(8) -0.0043(9) C8 0.0447(11) 0.0367(14) 0.0339(10) 0.0086(9) 0.0045(8) -0.0035(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 2.0421(17) . ? Zn1 N3 2.0452(17) 2_556 ? Zn1 O2 2.1030(17) . ? Zn1 O4 2.175(2) . ? Zn1 O1 2.207(2) . ? Zn1 O5 2.3296(19) . ? O1 N5 1.255(3) . ? O2 N5 1.264(3) . ? O3 N5 1.211(3) . ? O4 N6 1.247(2) . ? O5 N6 1.236(2) . ? O6 N6 1.221(2) . ? N1 C4 1.320(3) . ? N1 N2 1.345(2) . ? N2 C1 1.321(3) . ? N3 C8 1.319(3) . ? N3 N4 1.346(2) . ? N3 Zn1 2.0452(17) 2_546 ? N4 C5 1.312(3) . ? C1 C2 1.401(3) . ? C2 C3 1.368(3) . ? C2 C6 1.469(3) . ? C3 C4 1.379(3) . ? C5 C6 1.404(3) . ? C6 C7 1.368(3) . ? C7 C8 1.387(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 N3 103.54(7) . 2_556 ? N1 Zn1 O2 97.42(7) . . ? N3 Zn1 O2 110.22(7) 2_556 . ? N1 Zn1 O4 94.19(8) . . ? N3 Zn1 O4 141.58(7) 2_556 . ? O2 Zn1 O4 100.72(7) . . ? N1 Zn1 O1 155.52(7) . . ? N3 Zn1 O1 91.74(8) 2_556 . ? O2 Zn1 O1 58.95(7) . . ? O4 Zn1 O1 85.01(9) . . ? N1 Zn1 O5 102.10(7) . . ? N3 Zn1 O5 87.25(6) 2_556 . ? O2 Zn1 O5 149.92(8) . . ? O4 Zn1 O5 55.50(6) . . ? O1 Zn1 O5 97.57(8) . . ? N5 O1 Zn1 90.84(14) . . ? N5 O2 Zn1 95.45(14) . . ? N6 O4 Zn1 97.60(14) . . ? N6 O5 Zn1 90.48(12) . . ? C4 N1 N2 120.94(18) . . ? C4 N1 Zn1 123.56(13) . . ? N2 N1 Zn1 115.46(13) . . ? C1 N2 N1 117.81(16) . . ? C8 N3 N4 120.40(17) . . ? C8 N3 Zn1 125.67(14) . 2_546 ? N4 N3 Zn1 113.93(12) . 2_546 ? C5 N4 N3 117.81(16) . . ? O3 N5 O1 123.2(2) . . ? O3 N5 O2 122.0(2) . . ? O1 N5 O2 114.77(19) . . ? O6 N6 O5 123.06(19) . . ? O6 N6 O4 121.28(19) . . ? O5 N6 O4 115.66(17) . . ? N2 C1 C2 124.17(18) . . ? C3 C2 C1 116.37(19) . . ? C3 C2 C6 121.11(18) . . ? C1 C2 C6 122.50(17) . . ? C2 C3 C4 118.13(19) . . ? N1 C4 C3 122.57(18) . . ? N4 C5 C6 124.96(18) . . ? C7 C6 C5 116.04(19) . . ? C7 C6 C2 124.54(18) . . ? C5 C6 C2 119.38(17) . . ? C6 C7 C8 117.54(18) . . ? N3 C8 C7 123.21(18) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 28.70 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.303 _refine_diff_density_min -0.375 _refine_diff_density_rms 0.068 #============================================================================== data_(3) _database_code_depnum_ccdc_archive 'CCDC 640634' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Copper(II) Dithionate 1:2 Complex with 4,4'-Bipyridazine, Dihydrate ; _chemical_name_common ;Copper(ii) Dithionate 1:2 Complex with 4,4'-Bipyridazine, Dihydrate ; _chemical_melting_point ? _chemical_formula_moiety 'C16 H16 Cu N8 O2, O6 S2' _chemical_formula_sum 'C16 H16 Cu N8 O8 S2' _chemical_formula_weight 576.03 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 Orthorhombic _symmetry_space_group_name_H-M 'Pna2(1) ' _space_group_name_Hall 'P 2c -2n ' _symmetry_Int_Tables_number 33 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 15.1065(13) _cell_length_b 11.8885(9) _cell_length_c 11.0631(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1986.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 28.08 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.18 _exptl_crystal_density_diffrn 1.926 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1172 _exptl_absorpt_coefficient_mu 1.380 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.6950 _exptl_absorpt_correction_T_max 0.7893 _exptl_absorpt_process_details 'DIFABS, (Walker & Stuart, 1983)' _exptl_special_details ; Walker, N. & Stuart, D. 1983. Acta Cryst. A39, 158-166. ; _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_standards_decay_% 0 _diffrn_reflns_number 14287 _diffrn_reflns_av_R_equivalents 0.0465 _diffrn_reflns_av_sigmaI/netI 0.0458 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 28.08 _reflns_number_total 4759 _reflns_number_gt 4051 _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^)+(0.0506P)^2^+3.2575P] 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 0.38(2) _refine_ls_number_reflns 4759 _refine_ls_number_parameters 317 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0506 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.1068 _refine_ls_wR_factor_gt 0.1053 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _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 Cu1 Cu 0.00115(3) -0.73686(3) 0.00486(8) 0.01312(11) Uani 1 1 d . . . S1 S 0.02501(6) -0.30041(8) 0.00697(13) 0.0208(2) Uani 1 1 d . . . S2 S 0.10899(7) -0.15727(8) -0.00838(11) 0.0229(2) Uani 1 1 d . . . O1 O -0.0121(2) -0.5996(2) -0.1369(3) 0.0249(7) Uani 1 1 d . . . H1 H -0.0050 -0.6242 -0.2091 0.037 Uiso 1 1 d . . . H2 H 0.0229 -0.5444 -0.1249 0.037 Uiso 1 1 d . . . O2 O 0.0112(2) -0.8792(3) 0.1603(3) 0.0241(7) Uani 1 1 d . . . H3 H 0.0174 -0.9452 0.1314 0.036 Uiso 1 1 d . . . H4 H -0.0331 -0.8782 0.2083 0.036 Uiso 1 1 d . . . O3 O -0.0639(2) -0.2552(3) -0.0023(6) 0.0377(8) Uani 1 1 d . . . O4 O 0.0502(3) -0.3727(3) -0.0925(3) 0.0279(8) Uani 1 1 d . . . O5 O 0.0472(3) -0.3448(3) 0.1255(3) 0.0336(9) Uani 1 1 d . . . O6 O 0.0882(3) -0.1100(3) -0.1257(3) 0.0394(10) Uani 1 1 d . . . O7 O 0.1993(2) -0.1986(3) 0.0034(5) 0.0408(8) Uani 1 1 d . . . O8 O 0.0808(3) -0.0865(3) 0.0918(4) 0.0369(9) Uani 1 1 d . . . N1 N -0.0914(2) -0.8398(3) -0.0769(3) 0.0147(7) Uani 1 1 d . . . N2 N -0.1559(3) -0.7896(3) -0.1393(4) 0.0237(8) Uani 1 1 d . . . N3 N -0.4056(2) -1.1584(3) -0.3946(3) 0.0154(7) Uani 1 1 d . . . N4 N -0.4085(3) -1.0463(3) -0.3962(4) 0.0272(9) Uani 1 1 d . . . N5 N 0.0954(2) -0.6462(3) 0.0957(3) 0.0154(7) Uani 1 1 d . . . N6 N 0.1437(2) -0.5731(3) 0.0326(3) 0.0200(8) Uani 1 1 d . . . N7 N 0.4046(2) -0.3166(3) 0.4043(3) 0.0144(7) Uani 1 1 d . . . N8 N 0.3335(2) -0.3552(3) 0.4625(3) 0.0160(7) Uani 1 1 d . . . C1 C -0.0854(3) -0.9507(4) -0.0746(4) 0.0197(9) Uani 1 1 d . . . H1A H -0.0374 -0.9845 -0.0309 0.024 Uiso 1 1 calc R . . C2 C -0.1459(3) -1.0206(4) -0.1331(4) 0.0208(9) Uani 1 1 d . . . H2A H -0.1407 -1.1010 -0.1280 0.025 Uiso 1 1 calc R . . C3 C -0.2135(3) -0.9714(3) -0.1986(4) 0.0146(8) Uani 1 1 d . . . C4 C -0.2139(3) -0.8528(4) -0.1985(5) 0.0241(9) Uani 1 1 d . . . H4A H -0.2592 -0.8153 -0.2442 0.029 Uiso 1 1 calc R . . C5 C -0.3451(3) -1.2103(4) -0.3304(4) 0.0216(9) Uani 1 1 d . . . H5A H -0.3444 -1.2911 -0.3302 0.026 Uiso 1 1 calc R . . C6 C -0.2824(3) -1.1535(4) -0.2630(5) 0.0265(10) Uani 1 1 d . . . H6A H -0.2404 -1.1942 -0.2148 0.032 Uiso 1 1 calc R . . C7 C -0.2810(3) -1.0369(3) -0.2658(4) 0.0151(8) Uani 1 1 d . . . C8 C -0.3472(3) -0.9863(4) -0.3349(5) 0.0245(10) Uani 1 1 d . . . H8A H -0.3493 -0.9057 -0.3391 0.029 Uiso 1 1 calc R . . C9 C 0.1030(3) -0.6527(4) 0.2155(4) 0.0213(9) Uani 1 1 d . . . H9A H 0.0656 -0.7040 0.2588 0.026 Uiso 1 1 calc R . . C10 C 0.1635(3) -0.5873(4) 0.2803(4) 0.0195(9) Uani 1 1 d . . . H10A H 0.1702 -0.5960 0.3661 0.023 Uiso 1 1 calc R . . C11 C 0.2140(3) -0.5090(3) 0.2163(4) 0.0175(8) Uani 1 1 d . . . C12 C 0.1985(3) -0.5051(4) 0.0915(4) 0.0223(9) Uani 1 1 d . . . H12A H 0.2296 -0.4493 0.0453 0.027 Uiso 1 1 calc R . . C13 C 0.4132(3) -0.3302(4) 0.2857(4) 0.0197(9) Uani 1 1 d . . . H13A H 0.4632 -0.2974 0.2454 0.024 Uiso 1 1 calc R . . C14 C 0.3518(3) -0.3907(4) 0.2181(4) 0.0179(8) Uani 1 1 d . . . H14A H 0.3593 -0.4002 0.1325 0.021 Uiso 1 1 calc R . . C15 C 0.2801(3) -0.4366(3) 0.2770(4) 0.0143(8) Uani 1 1 d . . . C16 C 0.2736(3) -0.4131(4) 0.4010(4) 0.0171(8) Uani 1 1 d . . . H16A H 0.2228 -0.4407 0.4438 0.021 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 0.00913(17) 0.01543(19) 0.01479(19) -0.0079(3) 0.0001(2) 0.00010(15) S1 0.0236(4) 0.0209(4) 0.0177(4) -0.0023(6) 0.0023(6) -0.0016(3) S2 0.0298(5) 0.0190(4) 0.0199(5) 0.0005(5) -0.0032(5) -0.0037(4) O1 0.044(2) 0.0125(14) 0.0180(16) 0.0005(11) -0.0103(14) -0.0039(13) O2 0.0313(18) 0.0170(14) 0.0239(17) 0.0008(12) 0.0069(14) 0.0066(13) O3 0.0232(14) 0.0436(18) 0.046(2) -0.007(2) 0.006(2) 0.0028(13) O4 0.040(2) 0.0227(17) 0.0208(18) -0.0032(14) 0.0056(16) -0.0030(15) O5 0.053(2) 0.030(2) 0.0180(18) 0.0033(15) 0.0073(16) -0.0025(18) O6 0.062(3) 0.0300(19) 0.0268(19) 0.0101(16) -0.0071(19) -0.0101(19) O7 0.0279(16) 0.0475(19) 0.047(2) -0.007(3) -0.003(3) -0.0047(14) O8 0.056(2) 0.0200(18) 0.035(2) -0.0091(16) -0.0131(19) 0.0002(17) N1 0.0114(16) 0.0188(16) 0.0139(16) -0.0057(13) -0.0027(13) -0.0015(13) N2 0.0218(19) 0.0199(19) 0.029(2) -0.0033(16) -0.0112(16) -0.0010(15) N3 0.0107(16) 0.0173(16) 0.0183(18) -0.0055(14) 0.0003(13) -0.0013(12) N4 0.0225(19) 0.0224(19) 0.037(2) -0.0067(18) -0.0115(18) 0.0017(15) N5 0.0135(17) 0.0173(17) 0.0154(17) -0.0021(14) 0.0010(13) -0.0009(13) N6 0.0225(17) 0.0236(17) 0.0139(19) -0.0005(13) -0.0026(13) -0.0081(14) N7 0.0096(16) 0.0176(17) 0.0161(17) -0.0045(13) 0.0011(13) 0.0009(12) N8 0.0137(15) 0.0196(17) 0.0148(16) -0.0040(13) -0.0003(12) -0.0023(13) C1 0.017(2) 0.020(2) 0.022(2) -0.0026(17) -0.0027(17) 0.0025(16) C2 0.023(2) 0.0140(19) 0.026(2) -0.0013(18) -0.0054(18) 0.0014(16) C3 0.0135(19) 0.0188(19) 0.0116(19) -0.0022(16) 0.0005(15) 0.0013(15) C4 0.021(2) 0.019(2) 0.032(3) -0.0012(19) -0.008(2) -0.0025(17) C5 0.025(2) 0.013(2) 0.027(2) -0.0018(17) -0.0075(18) -0.0020(16) C6 0.025(2) 0.018(2) 0.037(3) -0.0026(19) -0.012(2) -0.0007(18) C7 0.016(2) 0.0175(19) 0.012(2) -0.0058(15) 0.0007(17) -0.0045(16) C8 0.026(2) 0.018(2) 0.030(2) -0.0052(19) -0.008(2) -0.0024(17) C9 0.022(2) 0.021(2) 0.020(2) -0.0014(18) 0.0006(17) -0.0069(17) C10 0.022(2) 0.020(2) 0.016(2) -0.0016(16) -0.0041(17) -0.0063(16) C11 0.013(2) 0.0163(19) 0.023(2) -0.0027(17) -0.0037(17) 0.0027(15) C12 0.026(2) 0.024(2) 0.016(2) -0.0038(17) -0.0018(18) -0.0070(18) C13 0.0182(19) 0.022(2) 0.018(2) 0.0017(17) 0.0001(16) -0.0055(16) C14 0.021(2) 0.022(2) 0.0112(18) -0.0045(16) 0.0019(16) -0.0018(16) C15 0.0135(19) 0.0150(19) 0.015(2) -0.0026(15) -0.0017(16) 0.0011(15) C16 0.0149(19) 0.024(2) 0.013(2) -0.0034(16) 0.0013(15) -0.0040(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 Cu1 N7 2.041(3) 4_544 ? Cu1 N3 2.047(3) 4_455 ? Cu1 N5 2.049(3) . ? Cu1 N1 2.067(3) . ? Cu1 O1 2.272(3) . ? Cu1 O2 2.417(3) . ? S1 O4 1.447(4) . ? S1 O3 1.450(3) . ? S1 O5 1.452(4) . ? S1 S2 2.1294(14) . ? S2 O6 1.449(4) . ? S2 O8 1.455(4) . ? S2 O7 1.456(3) . ? O1 H1 0.8573 . ? O1 H2 0.8535 . ? O2 H3 0.8532 . ? O2 H4 0.8545 . ? N1 C1 1.322(6) . ? N1 N2 1.334(5) . ? N2 C4 1.328(6) . ? N3 C5 1.312(6) . ? N3 N4 1.333(5) . ? N3 Cu1 2.047(3) 4_444 ? N4 C8 1.351(6) . ? N5 N6 1.332(5) . ? N5 C9 1.332(6) . ? N6 C12 1.327(5) . ? N7 C13 1.328(5) . ? N7 N8 1.334(5) . ? N7 Cu1 2.041(3) 4 ? N8 C16 1.324(5) . ? C1 C2 1.395(6) . ? C1 H1A 0.9600 . ? C2 C3 1.382(6) . ? C2 H2A 0.9600 . ? C3 C4 1.411(6) . ? C3 C7 1.483(5) . ? C4 H4A 0.9600 . ? C5 C6 1.382(6) . ? C5 H5A 0.9600 . ? C6 C7 1.386(6) . ? C6 H6A 0.9600 . ? C7 C8 1.395(7) . ? C8 H8A 0.9600 . ? C9 C10 1.397(6) . ? C9 H9A 0.9600 . ? C10 C11 1.396(6) . ? C10 H10A 0.9600 . ? C11 C12 1.401(6) . ? C11 C15 1.480(6) . ? C12 H12A 0.9600 . ? C13 C14 1.391(6) . ? C13 H13A 0.9600 . ? C14 C15 1.376(6) . ? C14 H14A 0.9600 . ? C15 C16 1.404(5) . ? C16 H16A 0.9600 . ? 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 N7 Cu1 N3 179.34(14) 4_544 4_455 ? N7 Cu1 N5 91.55(13) 4_544 . ? N3 Cu1 N5 89.06(14) 4_455 . ? N7 Cu1 N1 87.62(14) 4_544 . ? N3 Cu1 N1 91.75(13) 4_455 . ? N5 Cu1 N1 175.06(15) . . ? N7 Cu1 O1 91.06(14) 4_544 . ? N3 Cu1 O1 89.18(14) 4_455 . ? N5 Cu1 O1 91.25(13) . . ? N1 Cu1 O1 93.64(13) . . ? N7 Cu1 O2 91.09(13) 4_544 . ? N3 Cu1 O2 88.67(13) 4_455 . ? N5 Cu1 O2 88.61(13) . . ? N1 Cu1 O2 86.54(13) . . ? O1 Cu1 O2 177.85(13) . . ? O4 S1 O3 114.2(3) . . ? O4 S1 O5 114.2(2) . . ? O3 S1 O5 114.3(3) . . ? O4 S1 S2 104.90(16) . . ? O3 S1 S2 104.49(15) . . ? O5 S1 S2 103.01(18) . . ? O6 S2 O8 113.3(2) . . ? O6 S2 O7 114.4(3) . . ? O8 S2 O7 113.7(3) . . ? O6 S2 S1 104.61(18) . . ? O8 S2 S1 103.11(18) . . ? O7 S2 S1 106.36(15) . . ? Cu1 O1 H1 112.8 . . ? Cu1 O1 H2 113.0 . . ? H1 O1 H2 109.3 . . ? Cu1 O2 H3 112.6 . . ? Cu1 O2 H4 112.6 . . ? H3 O2 H4 109.3 . . ? C1 N1 N2 120.4(4) . . ? C1 N1 Cu1 122.4(3) . . ? N2 N1 Cu1 117.1(3) . . ? C4 N2 N1 118.9(4) . . ? C5 N3 N4 120.1(4) . . ? C5 N3 Cu1 124.8(3) . 4_444 ? N4 N3 Cu1 115.1(3) . 4_444 ? N3 N4 C8 119.9(4) . . ? N6 N5 C9 120.7(4) . . ? N6 N5 Cu1 117.9(3) . . ? C9 N5 Cu1 121.2(3) . . ? C12 N6 N5 118.8(4) . . ? C13 N7 N8 120.9(3) . . ? C13 N7 Cu1 121.8(3) . 4 ? N8 N7 Cu1 117.3(3) . 4 ? C16 N8 N7 118.7(3) . . ? N1 C1 C2 122.7(4) . . ? N1 C1 H1A 118.7 . . ? C2 C1 H1A 118.7 . . ? C3 C2 C1 118.4(4) . . ? C3 C2 H2A 120.8 . . ? C1 C2 H2A 120.8 . . ? C2 C3 C4 115.2(4) . . ? C2 C3 C7 123.3(3) . . ? C4 C3 C7 121.5(4) . . ? N2 C4 C3 124.3(4) . . ? N2 C4 H4A 117.8 . . ? C3 C4 H4A 117.8 . . ? N3 C5 C6 122.6(4) . . ? N3 C5 H5A 118.7 . . ? C6 C5 H5A 118.7 . . ? C5 C6 C7 119.2(4) . . ? C5 C6 H6A 120.4 . . ? C7 C6 H6A 120.4 . . ? C6 C7 C8 115.6(4) . . ? C6 C7 C3 121.6(4) . . ? C8 C7 C3 122.8(4) . . ? N4 C8 C7 122.6(4) . . ? N4 C8 H8A 118.7 . . ? C7 C8 H8A 118.7 . . ? N5 C9 C10 122.3(4) . . ? N5 C9 H9A 118.8 . . ? C10 C9 H9A 118.8 . . ? C11 C10 C9 117.9(4) . . ? C11 C10 H10A 121.1 . . ? C9 C10 H10A 121.1 . . ? C10 C11 C12 115.5(4) . . ? C10 C11 C15 121.7(4) . . ? C12 C11 C15 122.7(4) . . ? N6 C12 C11 124.6(4) . . ? N6 C12 H12A 117.7 . . ? C11 C12 H12A 117.7 . . ? N7 C13 C14 121.9(4) . . ? N7 C13 H13A 119.0 . . ? C14 C13 H13A 119.0 . . ? C15 C14 C13 118.4(4) . . ? C15 C14 H14A 120.8 . . ? C13 C14 H14A 120.8 . . ? C14 C15 C16 116.0(4) . . ? C14 C15 C11 123.1(4) . . ? C16 C15 C11 120.8(4) . . ? N8 C16 C15 123.9(4) . . ? N8 C16 H16A 118.0 . . ? C15 C16 H16A 118.0 . . ? 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 O4 S1 S2 O6 60.6(3) . . . . ? O3 S1 S2 O6 -59.8(3) . . . . ? O5 S1 S2 O6 -179.6(3) . . . . ? O4 S1 S2 O8 179.3(2) . . . . ? O3 S1 S2 O8 58.8(3) . . . . ? O5 S1 S2 O8 -60.9(2) . . . . ? O4 S1 S2 O7 -60.9(3) . . . . ? O3 S1 S2 O7 178.7(4) . . . . ? O5 S1 S2 O7 58.9(3) . . . . ? N7 Cu1 N1 C1 55.5(4) 4_544 . . . ? N3 Cu1 N1 C1 -124.3(4) 4_455 . . . ? O1 Cu1 N1 C1 146.4(4) . . . . ? O2 Cu1 N1 C1 -35.8(4) . . . . ? N7 Cu1 N1 N2 -120.7(3) 4_544 . . . ? N3 Cu1 N1 N2 59.5(3) 4_455 . . . ? O1 Cu1 N1 N2 -29.8(3) . . . . ? O2 Cu1 N1 N2 148.1(3) . . . . ? C1 N1 N2 C4 0.2(7) . . . . ? Cu1 N1 N2 C4 176.5(4) . . . . ? C5 N3 N4 C8 2.3(7) . . . . ? Cu1 N3 N4 C8 -178.5(4) 4_444 . . . ? N7 Cu1 N5 N6 64.7(3) 4_544 . . . ? N3 Cu1 N5 N6 -115.6(3) 4_455 . . . ? O1 Cu1 N5 N6 -26.4(3) . . . . ? O2 Cu1 N5 N6 155.7(3) . . . . ? N7 Cu1 N5 C9 -121.1(4) 4_544 . . . ? N3 Cu1 N5 C9 58.7(3) 4_455 . . . ? O1 Cu1 N5 C9 147.8(3) . . . . ? O2 Cu1 N5 C9 -30.0(3) . . . . ? C9 N5 N6 C12 -1.4(6) . . . . ? Cu1 N5 N6 C12 172.9(3) . . . . ? C13 N7 N8 C16 3.8(6) . . . . ? Cu1 N7 N8 C16 -176.0(3) 4 . . . ? N2 N1 C1 C2 -1.7(7) . . . . ? Cu1 N1 C1 C2 -177.7(3) . . . . ? N1 C1 C2 C3 1.7(7) . . . . ? C1 C2 C3 C4 -0.3(6) . . . . ? C1 C2 C3 C7 179.2(4) . . . . ? N1 N2 C4 C3 1.2(8) . . . . ? C2 C3 C4 N2 -1.1(7) . . . . ? C7 C3 C4 N2 179.3(4) . . . . ? N4 N3 C5 C6 -0.3(7) . . . . ? Cu1 N3 C5 C6 -179.4(4) 4_444 . . . ? N3 C5 C6 C7 -2.2(8) . . . . ? C5 C6 C7 C8 2.5(7) . . . . ? C5 C6 C7 C3 -178.0(4) . . . . ? C2 C3 C7 C6 2.7(6) . . . . ? C4 C3 C7 C6 -177.9(5) . . . . ? C2 C3 C7 C8 -177.8(5) . . . . ? C4 C3 C7 C8 1.6(6) . . . . ? N3 N4 C8 C7 -1.9(8) . . . . ? C6 C7 C8 N4 -0.6(7) . . . . ? C3 C7 C8 N4 179.9(4) . . . . ? N6 N5 C9 C10 -2.4(7) . . . . ? Cu1 N5 C9 C10 -176.5(3) . . . . ? N5 C9 C10 C11 3.3(7) . . . . ? C9 C10 C11 C12 -0.4(6) . . . . ? C9 C10 C11 C15 -179.6(4) . . . . ? N5 N6 C12 C11 4.4(7) . . . . ? C10 C11 C12 N6 -3.4(7) . . . . ? C15 C11 C12 N6 175.7(4) . . . . ? N8 N7 C13 C14 -4.0(6) . . . . ? Cu1 N7 C13 C14 175.8(3) 4 . . . ? N7 C13 C14 C15 0.5(7) . . . . ? C13 C14 C15 C16 2.9(6) . . . . ? C13 C14 C15 C11 -175.7(4) . . . . ? C10 C11 C15 C14 155.2(4) . . . . ? C12 C11 C15 C14 -23.9(6) . . . . ? C10 C11 C15 C16 -23.3(6) . . . . ? C12 C11 C15 C16 157.6(4) . . . . ? N7 N8 C16 C15 -0.2(6) . . . . ? C14 C15 C16 N8 -3.1(6) . . . . ? C11 C15 C16 N8 175.5(4) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.08 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.788 _refine_diff_density_min -0.482 _refine_diff_density_rms 0.114 #============================================================================== data_(4) _database_code_depnum_ccdc_archive 'CCDC 640635' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Copper(II) Trifluoroacetate 2:3 Complex with 4,4'-Bipyridazine ; _chemical_name_common "Copper(ii) Trifluoroacetate 2:3 Complex with 4,4'-Bipyridazine" _chemical_melting_point ? _chemical_formula_moiety 'C32 H18 CU2 F12 N12 O8' _chemical_formula_sum 'C32 H18 Cu2 F12 N12 O8' _chemical_formula_weight 1053.66 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' F F 0.0171 0.0103 '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 'P2(1)/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 10.4940(6) _cell_length_b 10.9798(8) _cell_length_c 18.3058(13) _cell_angle_alpha 90.00 _cell_angle_beta 98.572(5) _cell_angle_gamma 90.00 _cell_volume 2085.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 10418 _cell_measurement_theta_min 2.70 _cell_measurement_theta_max 27.88 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.678 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1048 _exptl_absorpt_coefficient_mu 1.137 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7267 _exptl_absorpt_correction_T_max 0.8046 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 Apex CCD area-detector diffractometer' _diffrn_measurement_method '\w scans' _diffrn_standards_decay_% 0 _diffrn_reflns_number 10418 _diffrn_reflns_av_R_equivalents 0.0300 _diffrn_reflns_av_sigmaI/netI 0.0436 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.70 _diffrn_reflns_theta_max 27.88 _reflns_number_total 4887 _reflns_number_gt 3555 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT (Bruker, 1998)' _computing_cell_refinement 'SMART-NT (Bruker, 1998)' _computing_data_reduction 'SMART-NT (Bruker, 1998)' _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^)+(0.0588P)^2^+0.0560P] 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_number_reflns 4887 _refine_ls_number_parameters 352 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0657 _refine_ls_R_factor_gt 0.0434 _refine_ls_wR_factor_ref 0.1116 _refine_ls_wR_factor_gt 0.1043 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.069 _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 Cu1 Cu 0.74529(3) 0.84205(3) 0.188767(16) 0.02452(11) Uani 1 1 d . . . O1 O 0.63380(17) 0.83490(18) 0.09447(10) 0.0353(4) Uani 1 1 d . . . O2 O 0.4419(2) 0.8579(2) 0.13207(14) 0.0606(7) Uani 1 1 d . . . O3 O 0.85321(16) 0.84680(18) 0.28777(10) 0.0328(4) Uani 1 1 d . . . O4 O 0.66262(19) 0.8612(2) 0.32690(13) 0.0582(7) Uani 1 1 d . . . N1 N 0.9185(2) 0.8451(2) 0.12320(12) 0.0319(5) Uani 1 1 d . . . N2 N 1.0339(2) 0.8007(3) 0.15184(13) 0.0425(6) Uani 1 1 d . . . N3 N 0.73056(18) 1.0259(2) 0.19248(11) 0.0279(5) Uani 1 1 d . . . N4 N 0.8391(2) 1.0864(2) 0.18443(14) 0.0372(6) Uani 1 1 d . . . N5 N 0.73936(19) 1.6594(2) 0.19436(12) 0.0309(5) Uani 1 1 d . . . N6 N 0.6251(2) 1.6027(2) 0.18048(16) 0.0417(6) Uani 1 1 d . . . C1 C 1.1348(3) 0.8340(4) 0.12089(19) 0.0630(12) Uani 1 1 d . . . H1A H 1.2176 0.8012 0.1406 0.076 Uiso 1 1 calc R . . C2 C 1.1276(3) 0.9130(4) 0.06225(19) 0.0634(12) Uani 1 1 d . . . H2A H 1.2042 0.9366 0.0430 0.076 Uiso 1 1 calc R . . C3 C 1.0096(2) 0.9576(3) 0.03151(14) 0.0342(7) Uani 1 1 d . . . C4 C 0.9069(2) 0.9171(3) 0.06539(14) 0.0318(6) Uani 1 1 d . . . H4A H 0.8219 0.9437 0.0450 0.038 Uiso 1 1 calc R . . C5 C 0.6252(2) 1.0855(3) 0.20212(15) 0.0318(6) Uani 1 1 d . . . H5A H 0.5496 1.0395 0.2079 0.038 Uiso 1 1 calc R . . C6 C 0.6190(2) 1.2116(3) 0.20423(16) 0.0325(6) Uani 1 1 d . . . H6A H 0.5416 1.2525 0.2126 0.039 Uiso 1 1 calc R . . C7 C 0.7273(2) 1.2762(3) 0.19395(13) 0.0271(6) Uani 1 1 d . . . C8 C 0.8351(2) 1.2053(3) 0.18463(16) 0.0351(6) Uani 1 1 d . . . H8A H 0.9124 1.2479 0.1778 0.042 Uiso 1 1 calc R . . C9 C 0.8480(2) 1.5961(3) 0.20701(17) 0.0372(7) Uani 1 1 d . . . H9A H 0.9282 1.6394 0.2166 0.045 Uiso 1 1 calc R . . C10 C 0.8501(2) 1.4712(3) 0.20687(17) 0.0380(7) Uani 1 1 d . . . H10A H 0.9303 1.4278 0.2156 0.046 Uiso 1 1 calc R . . C11 C 0.7346(2) 1.4092(3) 0.19395(14) 0.0275(6) Uani 1 1 d . . . C12 C 0.6241(2) 1.4826(3) 0.18011(18) 0.0390(7) Uani 1 1 d . . . H12A H 0.5420 1.4426 0.1697 0.047 Uiso 1 1 calc R . . C13 C 0.5130(3) 0.8319(3) 0.08798(17) 0.0414(7) Uani 1 1 d . . . C14 C 0.4514(4) 0.7925(5) 0.0099(2) 0.0902(17) Uani 1 1 d D . . C15 C 0.7801(3) 0.8592(3) 0.33641(16) 0.0368(7) Uani 1 1 d . . . C16 C 0.8530(4) 0.8755(5) 0.4140(2) 0.0785(14) Uani 1 1 d D . . F1 F 0.3845(5) 0.8854(5) -0.0245(2) 0.0977(18) Uani 0.70 1 d PD . . F2 F 0.3548(6) 0.7120(6) 0.0172(5) 0.169(4) Uani 0.70 1 d PD . . F3 F 0.5217(6) 0.7463(11) -0.0322(3) 0.192(5) Uani 0.70 1 d PD . . F1A F 0.3296(7) 0.790(2) -0.0042(10) 0.211(16) Uani 0.30 1 d PD . . F2A F 0.4985(13) 0.6855(8) -0.0019(6) 0.103(5) Uani 0.30 1 d PD . . F3A F 0.500(2) 0.8667(11) -0.0389(6) 0.191(10) Uani 0.30 1 d PD . . F4 F 0.7865(10) 0.8400(18) 0.4646(6) 0.138(6) Uani 0.50 1 d PD . . F5 F 0.9625(8) 0.8210(14) 0.4284(4) 0.113(4) Uani 0.50 1 d PD . . F6 F 0.8753(18) 0.9958(7) 0.4230(7) 0.171(6) Uani 0.50 1 d PD . . F4A F 0.7822(11) 0.9158(17) 0.4602(7) 0.131(5) Uani 0.50 1 d PD . . F5A F 0.890(2) 0.7621(10) 0.4352(7) 0.230(8) Uani 0.50 1 d PD . . F6A F 0.9553(13) 0.941(2) 0.4179(4) 0.162(7) Uani 0.50 1 d PD . . 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 0.02200(16) 0.01219(17) 0.03934(18) 0.00146(15) 0.00442(11) -0.00004(13) O1 0.0295(9) 0.0313(12) 0.0436(10) 0.0021(10) 0.0005(7) 0.0001(9) O2 0.0345(11) 0.0666(19) 0.0809(16) -0.0179(14) 0.0097(11) 0.0002(11) O3 0.0279(9) 0.0282(11) 0.0423(10) 0.0034(9) 0.0052(7) 0.0007(8) O4 0.0324(11) 0.077(2) 0.0674(14) 0.0085(13) 0.0158(10) 0.0038(11) N1 0.0276(10) 0.0302(14) 0.0388(11) 0.0018(11) 0.0084(9) -0.0014(10) N2 0.0333(12) 0.0493(18) 0.0466(13) 0.0123(13) 0.0114(10) 0.0069(12) N3 0.0272(10) 0.0151(11) 0.0410(11) -0.0002(10) 0.0035(9) 0.0004(9) N4 0.0269(11) 0.0195(13) 0.0670(15) -0.0011(13) 0.0128(10) 0.0009(10) N5 0.0268(10) 0.0147(11) 0.0506(13) 0.0006(11) 0.0044(9) -0.0009(10) N6 0.0253(11) 0.0177(13) 0.0819(18) -0.0003(14) 0.0070(11) -0.0005(10) C1 0.0311(14) 0.097(3) 0.064(2) 0.042(2) 0.0154(14) 0.0164(18) C2 0.0277(14) 0.098(3) 0.068(2) 0.039(2) 0.0184(14) 0.0079(18) C3 0.0293(12) 0.0405(19) 0.0346(12) 0.0049(14) 0.0103(10) 0.0013(13) C4 0.0249(11) 0.0341(17) 0.0371(13) 0.0007(13) 0.0069(10) -0.0006(12) C5 0.0270(12) 0.0194(15) 0.0499(15) 0.0027(13) 0.0087(11) -0.0036(12) C6 0.0262(12) 0.0179(14) 0.0541(16) -0.0002(13) 0.0088(11) 0.0025(12) C7 0.0278(13) 0.0161(14) 0.0366(13) -0.0003(12) 0.0025(10) -0.0004(11) C8 0.0269(12) 0.0207(15) 0.0593(17) -0.0008(14) 0.0115(12) -0.0011(12) C9 0.0248(12) 0.0208(16) 0.0633(18) 0.0024(15) -0.0023(12) -0.0013(12) C10 0.0248(12) 0.0187(15) 0.0687(19) 0.0049(15) 0.0009(12) 0.0027(12) C11 0.0245(12) 0.0152(14) 0.0428(14) 0.0005(13) 0.0054(10) 0.0008(11) C12 0.0210(11) 0.0208(15) 0.0746(19) -0.0004(16) 0.0053(12) -0.0017(12) C13 0.0315(13) 0.0348(19) 0.0549(17) -0.0068(15) -0.0038(12) 0.0058(14) C14 0.056(2) 0.120(5) 0.085(3) -0.033(3) -0.024(2) 0.020(3) C15 0.0326(13) 0.0352(19) 0.0434(14) 0.0094(14) 0.0080(11) 0.0038(13) C16 0.069(3) 0.117(5) 0.049(2) 0.000(3) 0.0096(18) 0.011(3) F1 0.069(3) 0.161(5) 0.058(2) 0.009(3) -0.009(2) 0.037(3) F2 0.131(7) 0.132(6) 0.212(7) -0.065(5) -0.080(6) -0.028(5) F3 0.105(4) 0.377(14) 0.080(4) -0.121(7) -0.035(3) 0.128(7) F1A 0.036(6) 0.41(4) 0.168(18) -0.19(2) -0.039(8) 0.057(14) F2A 0.120(10) 0.094(8) 0.092(10) -0.092(8) 0.010(7) -0.014(7) F3A 0.37(3) 0.122(12) 0.057(6) -0.026(8) -0.057(12) 0.038(16) F4 0.103(6) 0.265(18) 0.052(4) 0.045(9) 0.031(4) 0.001(9) F5 0.055(4) 0.223(13) 0.052(3) -0.006(6) -0.018(3) 0.049(6) F6 0.209(12) 0.127(7) 0.148(10) -0.065(7) -0.067(10) -0.030(10) F4A 0.117(7) 0.206(14) 0.074(7) -0.068(8) 0.028(5) -0.014(8) F5A 0.311(19) 0.225(14) 0.130(9) 0.090(9) -0.047(13) 0.105(17) F6A 0.099(7) 0.32(2) 0.059(4) -0.024(9) -0.015(4) -0.091(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 Cu1 O1 1.9372(18) . ? Cu1 O3 1.9894(18) . ? Cu1 N5 2.010(2) 1_545 ? Cu1 N3 2.026(2) . ? Cu1 N1 2.323(2) . ? O1 C13 1.256(3) . ? O2 C13 1.212(4) . ? O3 C15 1.266(3) . ? O4 C15 1.220(3) . ? N1 C4 1.312(3) . ? N1 N2 1.337(3) . ? N2 C1 1.325(4) . ? N3 C5 1.319(3) . ? N3 N4 1.345(3) . ? N4 C8 1.307(4) . ? N5 C9 1.325(3) . ? N5 N6 1.342(3) . ? N6 C12 1.318(4) . ? C1 C2 1.373(5) . ? C2 C3 1.372(4) . ? C3 C4 1.394(3) . ? C3 C3 1.473(5) 3_775 ? C5 C6 1.387(4) . ? C6 C7 1.376(4) . ? C7 C8 1.404(4) . ? C7 C11 1.462(4) . ? C9 C10 1.372(4) . ? C10 C11 1.379(3) . ? C11 C12 1.405(3) . ? C13 C14 1.540(5) . ? C14 F3 1.252(6) . ? C14 F1A 1.266(8) . ? C14 F2A 1.306(8) . ? C14 F1 1.341(6) . ? C14 F3A 1.365(9) . ? C14 F2 1.366(7) . ? C15 C16 1.520(5) . ? C16 F4A 1.285(7) . ? C16 F6A 1.285(7) . ? C16 F5 1.287(6) . ? C16 F4 1.299(7) . ? C16 F5A 1.345(7) . ? C16 F6 1.347(7) . ? 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 O3 177.43(7) . . ? O1 Cu1 N5 89.18(9) . 1_545 ? O3 Cu1 N5 89.86(8) . 1_545 ? O1 Cu1 N3 91.80(8) . . ? O3 Cu1 N3 88.81(8) . . ? N5 Cu1 N3 171.62(8) 1_545 . ? O1 Cu1 N1 87.44(8) . . ? O3 Cu1 N1 95.01(7) . . ? N5 Cu1 N1 94.20(8) 1_545 . ? N3 Cu1 N1 94.16(8) . . ? C13 O1 Cu1 123.5(2) . . ? C15 O3 Cu1 108.74(17) . . ? C4 N1 N2 120.4(2) . . ? C4 N1 Cu1 116.09(17) . . ? N2 N1 Cu1 121.63(16) . . ? C1 N2 N1 117.8(3) . . ? C5 N3 N4 120.6(2) . . ? C5 N3 Cu1 124.64(18) . . ? N4 N3 Cu1 114.73(16) . . ? C8 N4 N3 117.8(2) . . ? C9 N5 N6 120.7(2) . . ? C9 N5 Cu1 119.97(18) . 1_565 ? N6 N5 Cu1 119.15(16) . 1_565 ? C12 N6 N5 118.1(2) . . ? N2 C1 C2 123.7(3) . . ? C3 C2 C1 119.2(3) . . ? C2 C3 C4 114.4(3) . . ? C2 C3 C3 123.9(3) . 3_775 ? C4 C3 C3 121.7(3) . 3_775 ? N1 C4 C3 124.5(2) . . ? N3 C5 C6 122.9(2) . . ? C7 C6 C5 117.9(2) . . ? C6 C7 C8 115.3(3) . . ? C6 C7 C11 124.0(2) . . ? C8 C7 C11 120.7(2) . . ? N4 C8 C7 125.5(2) . . ? N5 C9 C10 122.5(2) . . ? C9 C10 C11 118.7(2) . . ? C10 C11 C12 115.4(2) . . ? C10 C11 C7 122.5(2) . . ? C12 C11 C7 122.1(2) . . ? N6 C12 C11 124.6(2) . . ? O2 C13 O1 130.1(3) . . ? O2 C13 C14 118.0(3) . . ? O1 C13 C14 111.9(3) . . ? F1A C14 F2A 110.0(8) . . ? F3 C14 F1 109.5(6) . . ? F1A C14 F3A 110.3(8) . . ? F2A C14 F3A 103.8(7) . . ? F3 C14 F2 108.1(7) . . ? F1 C14 F2 101.2(4) . . ? F3 C14 C13 118.8(4) . . ? F1A C14 C13 117.9(8) . . ? F2A C14 C13 106.9(6) . . ? F1 C14 C13 109.9(4) . . ? F3A C14 C13 107.0(6) . . ? F2 C14 C13 107.9(5) . . ? O4 C15 O3 127.4(3) . . ? O4 C15 C16 119.2(3) . . ? O3 C15 C16 113.4(3) . . ? F4A C16 F6A 109.4(7) . . ? F5 C16 F4 105.8(6) . . ? F4A C16 F5A 107.5(7) . . ? F6A C16 F5A 107.3(6) . . ? F5 C16 F6 107.3(6) . . ? F4 C16 F6 108.0(7) . . ? F4A C16 C15 113.4(7) . . ? F6A C16 C15 114.6(5) . . ? F5 C16 C15 116.5(4) . . ? F4 C16 C15 112.5(7) . . ? F5A C16 C15 104.1(6) . . ? F6 C16 C15 106.5(5) . . ? F1A F1 F3A 114.0(8) . . ? F1A F1 C14 57.8(6) . . ? F3A F1 C14 62.3(4) . . ? F1A F2 C14 63.1(8) . . ? F1A F2 F2A 106.2(10) . . ? C14 F2 F2A 50.9(4) . . ? F2A F3 C14 72.0(7) . . ? F2A F3 F3A 135.3(9) . . ? C14 F3 F3A 63.4(6) . . ? F2 F1A C14 74.2(8) . . ? F2 F1A F1 137.7(8) . . ? C14 F1A F1 63.6(7) . . ? F3 F2A C14 65.8(6) . . ? F3 F2A F2 109.6(9) . . ? C14 F2A F2 54.3(5) . . ? F1 F3A F3 106.6(9) . . ? F1 F3A C14 60.4(7) . . ? F3 F3A C14 55.1(4) . . ? F4A F4 C16 70.1(8) . . ? F4A F4 F5A 123.3(11) . . ? C16 F4 F5A 55.7(5) . . ? F5A F5 C16 70.3(6) . . ? F5A F5 F6A 128.3(8) . . ? C16 F5 F6A 58.8(4) . . ? F6A F6 C16 63.4(6) . . ? F6A F6 F4A 106.2(9) . . ? C16 F6 F4A 52.2(5) . . ? F4 F4A C16 72.1(8) . . ? F4 F4A F6 125.4(11) . . ? C16 F4A F6 55.9(5) . . ? F5 F5A C16 64.3(6) . . ? F5 F5A F4 105.5(9) . . ? C16 F5A F4 52.9(5) . . ? F6 F6A C16 69.7(6) . . ? F6 F6A F5 125.7(9) . . ? C16 F6A F5 58.9(5) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.500 _refine_diff_density_min -0.405 _refine_diff_density_rms 0.079 #============================================================================== data_(5) _database_code_depnum_ccdc_archive 'CCDC 640636' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Copper(II) Tetrafluoroborate 1:2 Complex with 4,4'-Bipyridazine, Solvate with 3.33 Water ; _chemical_name_common ; Copper(ii) Tetrafluoroborate 1:2 Complex with 4,4'- Bipyridazine, Solvate with 3.33 Water ; _chemical_melting_point ? _chemical_formula_moiety 'C48 H36 Cu3 N24 O4, 6(B F4), 6(H2 O)' _chemical_formula_sum 'C48 H46 B6 Cu3 F24 N24 O10' _chemical_formula_weight 1830.57 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' F F 0.0171 0.0103 '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' B B 0.0013 0.0007 '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 2/c ' _space_group_name_Hall '-P 2yc ' _symmetry_Int_Tables_number 13 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 12.0861(8) _cell_length_b 14.6555(8) _cell_length_c 21.5673(15) _cell_angle_alpha 90.00 _cell_angle_beta 104.025(8) _cell_angle_gamma 90.00 _cell_volume 3706.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 12405 _cell_measurement_theta_min 4.59 _cell_measurement_theta_max 26.55 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.640 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1830 _exptl_absorpt_coefficient_mu 0.982 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8587 _exptl_absorpt_correction_T_max 0.9082 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1999)' _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 'Bruker Apex CCD area-detector diffractometer' _diffrn_measurement_method '\w scans' _diffrn_standards_decay_% 0 _diffrn_reflns_number 12405 _diffrn_reflns_av_R_equivalents 0.0459 _diffrn_reflns_av_sigmaI/netI 0.0621 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 4.59 _diffrn_reflns_theta_max 26.55 _reflns_number_total 7639 _reflns_number_gt 4590 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT (Bruker, 1998)' _computing_cell_refinement 'SMART-NT (Bruker, 1998)' _computing_data_reduction 'SMART-NT (Bruker, 1998)' _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^)+(0.1175P)^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_number_reflns 7639 _refine_ls_number_parameters 529 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0811 _refine_ls_R_factor_gt 0.0594 _refine_ls_wR_factor_ref 0.1657 _refine_ls_wR_factor_gt 0.1574 _refine_ls_goodness_of_fit_ref 0.943 _refine_ls_restrained_S_all 0.943 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 1.0000 0.0000 0.5000 0.02389(19) Uani 1 2 d S . . Cu2 Cu 1.72527(3) -0.25876(3) 0.50477(2) 0.02555(16) Uani 1 1 d . . . O1 O 1.13979(19) 0.12280(19) 0.49626(14) 0.0258(6) Uani 1 1 d . . . O2 O 1.6197(3) -0.3863(2) 0.5226(2) 0.0559(10) Uani 1 1 d . . . O3 O 1.4879(4) -0.2815(5) 0.8291(3) 0.0885(16) Uani 1 1 d . . . O4 O 1.4009(8) -0.4613(6) 0.8075(5) 0.147(3) Uani 1 1 d . . . O5A O 1.2501(9) -0.4930(6) 0.3883(6) 0.099(3) Uani 0.60 1 d P . . O5B O 1.3964(12) -0.4032(13) 0.4924(10) 0.119(7) Uani 0.40 1 d P . . N1 N 0.9909(2) -0.0326(2) 0.40885(16) 0.0240(7) Uani 1 1 d . . . N2 N 1.0746(3) 0.0071(3) 0.3872(2) 0.0421(10) Uani 1 1 d . . . N3 N 1.1299(2) -0.0902(2) 0.52560(18) 0.0276(7) Uani 1 1 d . . . N4 N 1.0913(2) -0.1746(2) 0.5295(2) 0.0321(8) Uani 1 1 d . . . N5 N 1.6211(2) -0.1696(2) 0.53398(17) 0.0247(7) Uani 1 1 d . . . N6 N 1.6726(2) -0.0940(2) 0.56226(19) 0.0305(8) Uani 1 1 d . . . N7 N 1.6342(3) -0.2517(2) 0.41260(18) 0.0290(8) Uani 1 1 d . . . N8 N 1.6232(3) -0.1730(3) 0.3815(2) 0.0413(10) Uani 1 1 d . . . N9 N 1.8181(2) -0.2703(2) 0.59762(18) 0.0262(7) Uani 1 1 d . . . N10 N 1.9298(3) -0.2563(3) 0.60467(19) 0.0330(8) Uani 1 1 d . . . N11 N 1.8439(2) -0.3341(2) 0.47502(18) 0.0268(7) Uani 1 1 d . . . N12 N 1.8784(3) -0.2970(3) 0.4260(2) 0.0354(8) Uani 1 1 d . . . C1 C 0.9132(3) -0.0825(3) 0.3702(2) 0.0329(9) Uani 1 1 d . . . H1A H 0.8557 -0.1100 0.3863 0.039 Uiso 1 1 calc R . . C2 C 0.9133(3) -0.0960(3) 0.3063(2) 0.0349(10) Uani 1 1 d . . . H2A H 0.8567 -0.1316 0.2795 0.042 Uiso 1 1 calc R . . C3 C 0.9979(3) -0.0560(3) 0.2838(2) 0.0279(9) Uani 1 1 d . . . C4 C 1.0780(3) -0.0053(4) 0.3275(2) 0.0404(11) Uani 1 1 d . . . H4A H 1.1380 0.0216 0.3133 0.048 Uiso 1 1 calc R . . C5 C 1.2403(3) -0.0729(3) 0.5347(2) 0.0285(9) Uani 1 1 d . . . H5A H 1.2646 -0.0122 0.5329 0.034 Uiso 1 1 calc R . . C6 C 1.3214(3) -0.1427(3) 0.5468(2) 0.0264(9) Uani 1 1 d . . . C7 C 1.2823(3) -0.2300(3) 0.5512(3) 0.0348(10) Uani 1 1 d . . . H7A H 1.3326 -0.2799 0.5593 0.042 Uiso 1 1 calc R . . C8 C 1.1654(3) -0.2416(3) 0.5431(3) 0.0401(12) Uani 1 1 d . . . H8A H 1.1380 -0.3006 0.5477 0.048 Uiso 1 1 calc R . . C9 C 1.5105(3) -0.1838(3) 0.5289(2) 0.0254(8) Uani 1 1 d . . . H9A H 1.4766 -0.2370 0.5085 0.030 Uiso 1 1 calc R . . C10 C 1.4432(3) -0.1223(3) 0.5530(2) 0.0264(9) Uani 1 1 d . . . C11 C 1.4952(3) -0.0449(3) 0.5820(2) 0.0317(9) Uani 1 1 d . . . H11A H 1.4542 -0.0009 0.5990 0.038 Uiso 1 1 calc R . . C12 C 1.6115(3) -0.0339(3) 0.5854(2) 0.0328(10) Uani 1 1 d . . . H12A H 1.6481 0.0189 0.6051 0.039 Uiso 1 1 calc R . . C13 C 1.5918(5) -0.3260(4) 0.3838(3) 0.0581(17) Uani 1 1 d . . . H13A H 1.5988 -0.3803 0.4075 0.070 Uiso 1 1 calc R . . C14 C 1.5368(6) -0.3288(4) 0.3200(3) 0.0617(18) Uani 1 1 d . . . H14A H 1.5060 -0.3838 0.3008 0.074 Uiso 1 1 calc R . . C15 C 1.5278(3) -0.2497(3) 0.2847(2) 0.0298(10) Uani 1 1 d . . . C16 C 1.5728(4) -0.1731(3) 0.3189(3) 0.0426(12) Uani 1 1 d . . . H16A H 1.5677 -0.1174 0.2968 0.051 Uiso 1 1 calc R . . C17 C 1.7761(3) -0.2850(4) 0.6476(2) 0.0361(10) Uani 1 1 d . . . H17A H 1.6971 -0.2936 0.6411 0.043 Uiso 1 1 calc R . . C18 C 1.8442(3) -0.2885(4) 0.7098(2) 0.0368(10) Uani 1 1 d . . . H18A H 1.8125 -0.3002 0.7447 0.044 Uiso 1 1 calc R . . C19 C 1.9597(3) -0.2741(3) 0.7182(2) 0.0255(9) Uani 1 1 d . . . C20 C 1.9968(3) -0.2573(3) 0.6632(2) 0.0316(9) Uani 1 1 d . . . H20A H 2.0749 -0.2459 0.6678 0.038 Uiso 1 1 calc R . . C21 C 1.8890(3) -0.4099(3) 0.5023(2) 0.0268(8) Uani 1 1 d . . . H21A H 1.8610 -0.4336 0.5360 0.032 Uiso 1 1 calc R . . C22 C 1.9768(3) -0.4575(3) 0.4840(2) 0.0262(9) Uani 1 1 d . . . C23 C 2.0132(4) -0.4186(3) 0.4346(3) 0.0454(13) Uani 1 1 d . . . H23A H 2.0722 -0.4457 0.4195 0.054 Uiso 1 1 calc R . . C24 C 1.9617(4) -0.3387(4) 0.4070(3) 0.0478(13) Uani 1 1 d . . . H24A H 1.9874 -0.3129 0.3731 0.057 Uiso 1 1 calc R . . B1 B 1.2369(8) -0.4396(6) 0.6448(6) 0.076(3) Uani 1 1 d . . . B2 B 1.2965(5) -0.0898(5) 0.7218(4) 0.0500(15) Uani 1 1 d . . . B3 B 1.2596(6) -0.2307(5) 0.3686(4) 0.0593(18) Uani 1 1 d . . . F1 F 1.2614(5) -0.4485(3) 0.5853(3) 0.1008(15) Uani 1 1 d . . . F2 F 1.2939(4) -0.3679(4) 0.6775(3) 0.1028(16) Uani 1 1 d . . . F3 F 1.1227(4) -0.4213(4) 0.6350(4) 0.117(2) Uani 1 1 d . . . F4 F 1.2628(5) -0.5203(4) 0.6759(3) 0.118(2) Uani 1 1 d . . . F5 F 1.1851(3) -0.1074(3) 0.6993(4) 0.124(3) Uani 1 1 d . . . F6 F 1.3327(6) -0.0359(5) 0.6804(3) 0.136(2) Uani 1 1 d . . . F7 F 1.3552(5) -0.1657(5) 0.7321(6) 0.200(5) Uani 1 1 d . . . F8 F 1.3099(6) -0.0389(10) 0.7717(4) 0.217(6) Uani 1 1 d . . . F9 F 1.1789(7) -0.1885(7) 0.3913(5) 0.187(4) Uani 1 1 d . . . F10 F 1.2425(11) -0.2408(8) 0.3090(4) 0.217(5) Uani 1 1 d . . . F11 F 1.3534(6) -0.1865(7) 0.3949(4) 0.171(3) Uani 1 1 d . . . F12 F 1.2913(12) -0.3049(5) 0.4046(6) 0.248(6) 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 Cu1 0.0197(3) 0.0319(4) 0.0206(4) -0.0006(3) 0.0057(2) 0.0069(2) Cu2 0.0238(2) 0.0284(3) 0.0237(3) 0.0012(2) 0.00425(17) 0.01192(17) O1 0.0257(11) 0.0252(15) 0.0274(16) -0.0011(12) 0.0085(10) 0.0009(10) O2 0.072(2) 0.031(2) 0.069(3) 0.0038(19) 0.0257(19) -0.0031(16) O3 0.072(3) 0.121(5) 0.076(4) -0.005(3) 0.026(2) -0.006(3) O4 0.201(8) 0.123(7) 0.112(7) 0.020(5) 0.031(5) 0.039(6) O5A 0.144(8) 0.052(5) 0.124(9) 0.042(5) 0.076(6) 0.036(5) O5B 0.085(8) 0.121(14) 0.140(17) -0.027(12) 0.006(9) 0.019(8) N1 0.0227(13) 0.0284(18) 0.0221(18) -0.0010(15) 0.0075(11) 0.0019(12) N2 0.0389(17) 0.061(3) 0.029(2) -0.012(2) 0.0144(15) -0.0202(17) N3 0.0206(13) 0.0328(19) 0.031(2) 0.0038(16) 0.0087(12) 0.0050(12) N4 0.0242(14) 0.031(2) 0.044(2) 0.0054(17) 0.0131(14) 0.0011(13) N5 0.0203(12) 0.0244(17) 0.0296(19) 0.0009(15) 0.0067(12) 0.0035(11) N6 0.0248(13) 0.0262(19) 0.041(2) -0.0025(16) 0.0084(13) -0.0005(12) N7 0.0289(14) 0.0256(18) 0.0283(19) 0.0021(15) -0.0011(13) 0.0077(12) N8 0.053(2) 0.028(2) 0.034(2) 0.0010(17) -0.0069(17) -0.0004(16) N9 0.0274(14) 0.0254(18) 0.0272(19) 0.0041(15) 0.0090(12) 0.0058(12) N10 0.0290(15) 0.045(2) 0.027(2) 0.0040(17) 0.0091(13) -0.0016(14) N11 0.0298(14) 0.0212(17) 0.0287(19) 0.0002(15) 0.0059(13) 0.0089(12) N12 0.0458(18) 0.028(2) 0.037(2) 0.0024(17) 0.0186(16) 0.0108(15) C1 0.0363(19) 0.034(2) 0.029(2) -0.0012(19) 0.0096(16) -0.0072(16) C2 0.0400(19) 0.037(3) 0.027(2) -0.002(2) 0.0063(17) -0.0126(18) C3 0.0303(17) 0.030(2) 0.023(2) 0.0031(17) 0.0069(15) 0.0043(15) C4 0.0377(19) 0.059(3) 0.029(2) -0.007(2) 0.0178(17) -0.0194(19) C5 0.0202(15) 0.030(2) 0.036(2) 0.0030(19) 0.0084(14) 0.0051(14) C6 0.0197(15) 0.027(2) 0.034(2) 0.0017(18) 0.0082(14) 0.0025(13) C7 0.0267(17) 0.027(2) 0.051(3) 0.006(2) 0.0115(17) 0.0070(15) C8 0.0306(18) 0.029(2) 0.061(4) 0.004(2) 0.0126(19) -0.0033(16) C9 0.0211(15) 0.020(2) 0.034(2) 0.0028(17) 0.0056(14) 0.0035(13) C10 0.0221(15) 0.022(2) 0.035(2) 0.0051(17) 0.0083(14) 0.0042(13) C11 0.0283(17) 0.027(2) 0.041(3) -0.0041(19) 0.0118(16) 0.0058(15) C12 0.0280(17) 0.023(2) 0.046(3) -0.009(2) 0.0079(17) -0.0022(15) C13 0.087(4) 0.024(3) 0.044(3) 0.009(2) -0.021(3) -0.004(2) C14 0.096(4) 0.024(3) 0.045(3) 0.003(2) -0.022(3) -0.010(3) C15 0.0307(17) 0.026(2) 0.027(3) 0.0001(17) -0.0043(15) 0.0050(15) C16 0.059(3) 0.022(2) 0.036(3) 0.003(2) -0.010(2) -0.0009(19) C17 0.0247(16) 0.054(3) 0.030(2) 0.004(2) 0.0080(16) 0.0050(17) C18 0.0309(18) 0.055(3) 0.027(2) 0.007(2) 0.0116(16) 0.0013(18) C19 0.0295(16) 0.024(2) 0.024(2) 0.0024(16) 0.0071(15) 0.0038(14) C20 0.0300(17) 0.043(3) 0.023(2) -0.0002(19) 0.0076(15) -0.0052(16) C21 0.0271(16) 0.027(2) 0.027(2) 0.0001(18) 0.0087(14) 0.0075(14) C22 0.0287(16) 0.018(2) 0.032(2) -0.0049(17) 0.0077(15) 0.0029(14) C23 0.056(2) 0.027(2) 0.066(4) 0.007(2) 0.040(2) 0.014(2) C24 0.061(3) 0.036(3) 0.059(4) 0.016(3) 0.038(2) 0.017(2) B1 0.088(5) 0.045(4) 0.095(8) -0.013(4) 0.022(5) -0.019(4) B2 0.055(3) 0.048(4) 0.050(4) 0.000(3) 0.019(3) 0.011(3) B3 0.056(3) 0.052(4) 0.069(5) 0.005(4) 0.013(3) 0.002(3) F1 0.137(4) 0.080(3) 0.092(4) -0.025(3) 0.038(3) -0.018(3) F2 0.125(3) 0.096(4) 0.093(4) -0.042(3) 0.036(3) -0.043(3) F3 0.094(3) 0.083(3) 0.168(7) -0.030(4) 0.020(3) 0.005(2) F4 0.154(5) 0.072(3) 0.136(6) 0.036(3) 0.053(4) 0.029(3) F5 0.066(2) 0.062(3) 0.228(8) 0.027(3) 0.002(3) -0.007(2) F6 0.179(6) 0.134(5) 0.111(5) 0.002(4) 0.065(4) -0.059(4) F7 0.101(4) 0.088(4) 0.401(15) 0.049(6) 0.040(6) 0.037(3) F8 0.141(5) 0.389(16) 0.105(6) -0.121(8) 0.001(4) 0.064(7) F9 0.156(6) 0.243(10) 0.176(8) 0.046(7) 0.069(5) 0.113(6) F10 0.283(12) 0.263(13) 0.075(5) -0.029(6) -0.018(7) 0.043(8) F11 0.142(5) 0.228(10) 0.139(7) -0.040(6) 0.025(5) -0.054(6) F12 0.422(16) 0.073(5) 0.230(13) 0.034(6) 0.044(11) 0.086(7) _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 2.000(3) 3_756 ? Cu1 N1 2.000(3) . ? Cu1 N3 2.025(3) 3_756 ? Cu1 N3 2.025(3) . ? Cu2 N5 2.019(3) . ? Cu2 N7 2.028(4) . ? Cu2 N11 2.033(3) . ? Cu2 N9 2.051(4) . ? Cu2 O2 2.347(4) . ? N1 C1 1.316(5) . ? N1 N2 1.345(5) . ? N2 C4 1.312(6) . ? N3 C5 1.325(4) . ? N3 N4 1.332(5) . ? N4 C8 1.312(6) . ? N5 C9 1.331(4) . ? N5 N6 1.343(5) . ? N6 C12 1.322(6) . ? N7 C13 1.295(6) . ? N7 N8 1.326(5) . ? N8 C16 1.339(6) . ? N9 C17 1.315(6) . ? N9 N10 1.337(4) . ? N10 C20 1.324(6) . ? N11 C21 1.312(5) . ? N11 N12 1.342(5) . ? N12 C24 1.324(6) . ? C1 C2 1.392(7) . ? C2 C3 1.365(6) . ? C3 C4 1.391(6) . ? C3 C3 1.471(8) 2_755 ? C5 C6 1.396(5) . ? C6 C7 1.375(6) . ? C6 C10 1.476(5) . ? C7 C8 1.391(5) . ? C9 C10 1.395(6) . ? C10 C11 1.372(6) . ? C11 C12 1.400(5) . ? C13 C14 1.376(8) . ? C14 C15 1.377(7) . ? C15 C16 1.380(6) . ? C15 C15 1.485(8) 2_855 ? C17 C18 1.394(6) . ? C18 C19 1.380(5) . ? C19 C20 1.387(6) . ? C19 C19 1.478(8) 2_956 ? C21 C22 1.404(5) . ? C22 C23 1.372(7) . ? C22 C22 1.469(8) 3_946 ? C23 C24 1.391(7) . ? B1 F2 1.356(9) . ? B1 F4 1.360(11) . ? B1 F3 1.370(10) . ? B1 F1 1.390(13) . ? B2 F8 1.286(10) . ? B2 F7 1.310(8) . ? B2 F5 1.340(7) . ? B2 F6 1.342(9) . ? B3 F10 1.261(13) . ? B3 F11 1.309(10) . ? B3 F12 1.337(11) . ? B3 F9 1.345(11) . ? 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 180.0 3_756 . ? N1 Cu1 N3 88.07(14) 3_756 3_756 ? N1 Cu1 N3 91.93(14) . 3_756 ? N1 Cu1 N3 91.93(14) 3_756 . ? N1 Cu1 N3 88.07(14) . . ? N3 Cu1 N3 180.0(2) 3_756 . ? N5 Cu2 N7 92.38(14) . . ? N5 Cu2 N11 172.38(14) . . ? N7 Cu2 N11 88.57(14) . . ? N5 Cu2 N9 89.05(13) . . ? N7 Cu2 N9 178.16(14) . . ? N11 Cu2 N9 90.16(13) . . ? N5 Cu2 O2 93.41(14) . . ? N7 Cu2 O2 90.77(15) . . ? N11 Cu2 O2 94.14(14) . . ? N9 Cu2 O2 88.00(15) . . ? C1 N1 N2 120.1(4) . . ? C1 N1 Cu1 128.0(3) . . ? N2 N1 Cu1 111.8(3) . . ? C4 N2 N1 119.1(3) . . ? C5 N3 N4 121.6(3) . . ? C5 N3 Cu1 127.0(3) . . ? N4 N3 Cu1 111.3(2) . . ? C8 N4 N3 118.5(3) . . ? C9 N5 N6 120.8(3) . . ? C9 N5 Cu2 124.3(3) . . ? N6 N5 Cu2 114.8(2) . . ? C12 N6 N5 118.7(3) . . ? C13 N7 N8 120.6(4) . . ? C13 N7 Cu2 119.0(3) . . ? N8 N7 Cu2 120.3(3) . . ? N7 N8 C16 118.3(4) . . ? C17 N9 N10 120.7(3) . . ? C17 N9 Cu2 125.8(3) . . ? N10 N9 Cu2 113.4(3) . . ? C20 N10 N9 118.3(4) . . ? C21 N11 N12 121.4(3) . . ? C21 N11 Cu2 124.5(3) . . ? N12 N11 Cu2 114.0(2) . . ? C24 N12 N11 117.5(4) . . ? N1 C1 C2 122.3(4) . . ? C3 C2 C1 118.1(4) . . ? C2 C3 C4 116.5(4) . . ? C2 C3 C3 124.2(4) . 2_755 ? C4 C3 C3 119.0(4) . 2_755 ? N2 C4 C3 123.9(4) . . ? N3 C5 C6 121.5(4) . . ? C7 C6 C5 117.2(3) . . ? C7 C6 C10 122.2(3) . . ? C5 C6 C10 120.5(4) . . ? C6 C7 C8 117.4(4) . . ? N4 C8 C7 123.6(4) . . ? N5 C9 C10 122.2(4) . . ? C11 C10 C9 117.3(3) . . ? C11 C10 C6 123.0(3) . . ? C9 C10 C6 119.7(4) . . ? C10 C11 C12 117.5(4) . . ? N6 C12 C11 123.4(4) . . ? N7 C13 C14 123.0(5) . . ? C13 C14 C15 118.8(5) . . ? C14 C15 C16 114.9(4) . . ? C14 C15 C15 120.9(3) . 2_855 ? C16 C15 C15 124.2(3) . 2_855 ? N8 C16 C15 124.3(4) . . ? N9 C17 C18 122.7(4) . . ? C19 C18 C17 117.6(4) . . ? C18 C19 C20 116.2(4) . . ? C18 C19 C19 122.7(5) . 2_956 ? C20 C19 C19 121.2(4) . 2_956 ? N10 C20 C19 124.6(3) . . ? N11 C21 C22 123.7(4) . . ? C23 C22 C21 114.8(4) . . ? C23 C22 C22 124.0(4) . 3_946 ? C21 C22 C22 121.3(5) . 3_946 ? C22 C23 C24 119.2(4) . . ? N12 C24 C23 123.4(5) . . ? F2 B1 F4 113.0(8) . . ? F2 B1 F3 107.2(7) . . ? F4 B1 F3 110.5(7) . . ? F2 B1 F1 110.9(7) . . ? F4 B1 F1 107.4(7) . . ? F3 B1 F1 107.9(8) . . ? F8 B2 F7 113.4(9) . . ? F8 B2 F5 109.1(7) . . ? F7 B2 F5 110.6(6) . . ? F8 B2 F6 102.7(9) . . ? F7 B2 F6 111.3(7) . . ? F5 B2 F6 109.5(6) . . ? F10 B3 F11 114.3(10) . . ? F10 B3 F12 116.7(10) . . ? F11 B3 F12 93.1(9) . . ? F10 B3 F9 118.2(9) . . ? F11 B3 F9 104.0(9) . . ? F12 B3 F9 107.1(10) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.55 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.983 _refine_diff_density_min -0.558 _refine_diff_density_rms 0.093 #============================================================================== data_(6) _database_code_depnum_ccdc_archive 'CCDC 640637' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Dihydroxotricopper(II) Trifluoroacetate Complex with 4,4'-Bipyridazine, Tetrahydrate ; _chemical_name_common ; Dihydroxotricopper(ii) Trifluoroacetate Complex with 4,4'- Bipyridazine, Tetrahydrate ; _chemical_melting_point ? _chemical_formula_moiety '(C28 H24 Cu3 F6 N12 O8), 2(C2 F3 O2), 2(H2 O)' _chemical_formula_sum 'C32 H26 Cu3 F12 N12 O13' _chemical_formula_weight 1205.27 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' F F 0.0171 0.0103 '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 2/c ' _space_group_name_Hall '-C 2yc ' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 15.4234(9) _cell_length_b 15.7761(12) _cell_length_c 19.1034(12) _cell_angle_alpha 90.00 _cell_angle_beta 108.591(6) _cell_angle_gamma 90.00 _cell_volume 4405.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 4.64 _cell_measurement_theta_max 27.00 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.17 _exptl_crystal_density_diffrn 1.817 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2404 _exptl_absorpt_coefficient_mu 1.562 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.6985 _exptl_absorpt_correction_T_max 0.7694 _exptl_absorpt_process_details 'DIFABS, (Walker & Stuart, 1983)' _exptl_special_details ; Walker, N. & Stuart, D. 1983. Acta Cryst. A39, 158-166. ; _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_standards_decay_% 0 _diffrn_reflns_number 11224 _diffrn_reflns_av_R_equivalents 0.0511 _diffrn_reflns_av_sigmaI/netI 0.0511 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 4.64 _diffrn_reflns_theta_max 27.00 _reflns_number_total 4587 _reflns_number_gt 3528 _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^)+(0.0631P)^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_number_reflns 4587 _refine_ls_number_parameters 385 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0472 _refine_ls_R_factor_gt 0.0358 _refine_ls_wR_factor_ref 0.0968 _refine_ls_wR_factor_gt 0.0935 _refine_ls_goodness_of_fit_ref 0.943 _refine_ls_restrained_S_all 0.983 _refine_ls_shift/su_max 0.007 _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 0.2500 0.2500 0.5000 0.02209(12) Uani 1 2 d S . . Cu2 Cu 0.09598(2) 0.291000(19) 0.57719(2) 0.03016(12) Uani 1 1 d . . . O1 O 0.18438(14) 0.21623(10) 0.56348(11) 0.0294(4) Uani 1 1 d . . . H1 H 0.1847 0.1685 0.5801 0.044 Uiso 1 1 d . . . O2 O 0.01880(14) 0.37492(13) 0.60422(15) 0.0448(6) Uani 1 1 d . . . O3 O -0.1232(2) 0.3468(2) 0.53103(18) 0.0712(8) Uani 1 1 d . . . O4 O 0.65780(18) 0.55288(14) 0.61085(13) 0.0479(6) Uani 1 1 d . . . O5 O 0.6946(3) 0.5889(2) 0.72965(17) 0.0906(12) Uani 1 1 d . . . O6 O 0.1850(3) 0.2626(2) 0.7198(2) 0.1010(13) Uani 1 1 d . . . H2 H 0.1814 0.2641 0.7628 0.151 Uiso 1 1 d . . . H3 H 0.2005 0.2123 0.7117 0.151 Uiso 1 1 d . . . O7 O -0.2406(4) 0.2514(4) 0.4109(5) 0.086(2) Uani 0.50 1 d P . . H4 H -0.2059 0.2800 0.4469 0.129 Uiso 0.50 1 d P . . H5 H -0.2785 0.2242 0.4271 0.129 Uiso 0.50 1 d P . . N1 N 0.39150(17) 0.21530(15) 0.58598(13) 0.0314(5) Uani 1 1 d . . . N2 N 0.45913(17) 0.19799(15) 0.55829(14) 0.0341(5) Uani 1 1 d . . . N3 N 0.25228(14) 0.37269(13) 0.54909(12) 0.0243(4) Uani 1 1 d . . . N4 N 0.18604(15) 0.38876(13) 0.57896(13) 0.0267(5) Uani 1 1 d . . . N5 N 0.51032(16) 0.69717(13) 0.58240(14) 0.0281(5) Uani 1 1 d . . . N6 N 0.48003(18) 0.64559(16) 0.52465(15) 0.0385(6) Uani 1 1 d . . . C1 C 0.4079(2) 0.21658(18) 0.65850(16) 0.0331(6) Uani 1 1 d . . . H1A H 0.3581 0.2298 0.6767 0.040 Uiso 1 1 calc R . . C2 C 0.4934(2) 0.19978(19) 0.70986(16) 0.0351(6) Uani 1 1 d . . . C3 C 0.5624(2) 0.1827(3) 0.68150(19) 0.0515(9) Uani 1 1 d . . . H3A H 0.6232 0.1708 0.7133 0.062 Uiso 1 1 calc R . . C4 C 0.5417(2) 0.1829(3) 0.60469(18) 0.0482(8) Uani 1 1 d . . . H4A H 0.5902 0.1715 0.5846 0.058 Uiso 1 1 calc R . . C5 C 0.31335(18) 0.43136(16) 0.55012(15) 0.0258(5) Uani 1 1 d . . . H5A H 0.3601 0.4186 0.5285 0.031 Uiso 1 1 calc R . . C6 C 0.31321(18) 0.51230(16) 0.58166(15) 0.0254(5) Uani 1 1 d . . . C7 C 0.2453(2) 0.52810(17) 0.61170(17) 0.0315(6) Uani 1 1 d . . . H7A H 0.2410 0.5820 0.6337 0.038 Uiso 1 1 calc R . . C8 C 0.1825(2) 0.46367(17) 0.60935(17) 0.0322(6) Uani 1 1 d . . . H8A H 0.1349 0.4740 0.6306 0.039 Uiso 1 1 calc R . . C9 C 0.4171(2) 0.58563(17) 0.52363(16) 0.0337(6) Uani 1 1 d . . . H9A H 0.3953 0.5491 0.4815 0.040 Uiso 1 1 calc R . . C10 C 0.38343(18) 0.57597(16) 0.58236(15) 0.0264(5) Uani 1 1 d . . . C11 C 0.4180(2) 0.63015(17) 0.64197(17) 0.0327(6) Uani 1 1 d . . . H11A H 0.3973 0.6255 0.6842 0.039 Uiso 1 1 calc R . . C12 C 0.48100(19) 0.68970(16) 0.64072(15) 0.0279(6) Uani 1 1 d . . . H12A H 0.5047 0.7268 0.6823 0.034 Uiso 1 1 calc R . . C13 C -0.0664(2) 0.3830(2) 0.5812(2) 0.0400(7) Uani 1 1 d . . . C14 C -0.1018(2) 0.4482(2) 0.6247(2) 0.0605(11) Uani 1 1 d D . . C15 C 0.6643(3) 0.5416(2) 0.67569(19) 0.0490(9) Uani 1 1 d . . . C16 C 0.6251(3) 0.4552(3) 0.69230(19) 0.0625(11) Uani 1 1 d D . . F1 F -0.0437(8) 0.5086(5) 0.6517(7) 0.109(5) Uani 0.50 1 d PD . . F2 F -0.1046(7) 0.4109(6) 0.6863(4) 0.103(3) Uani 0.50 1 d PD . . F3 F -0.1863(6) 0.4683(11) 0.5908(5) 0.136(5) Uani 0.50 1 d PD . . F1A F -0.0415(7) 0.4884(9) 0.6777(7) 0.143(7) Uani 0.50 1 d PD . . F2A F -0.1631(12) 0.4173(7) 0.6509(13) 0.181(8) Uani 0.50 1 d PD . . F3A F -0.1397(9) 0.5135(4) 0.5818(5) 0.106(3) Uani 0.50 1 d PD . . F4 F 0.5395(5) 0.4410(7) 0.6465(4) 0.098(3) Uani 0.50 1 d PD . . F5 F 0.6684(5) 0.3890(3) 0.6689(5) 0.096(2) Uani 0.50 1 d PD . . F6 F 0.6261(7) 0.4329(6) 0.7572(3) 0.135(5) Uani 0.50 1 d PD . . F4A F 0.5709(6) 0.4181(5) 0.6383(3) 0.103(4) Uani 0.50 1 d PD . . F5A F 0.6937(4) 0.4091(3) 0.7323(4) 0.092(2) Uani 0.50 1 d PD . . F6A F 0.5808(5) 0.4777(4) 0.7400(4) 0.086(2) Uani 0.50 1 d PD . . 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 0.0209(2) 0.0233(2) 0.0217(2) -0.00125(16) 0.00625(19) -0.00475(16) Cu2 0.02282(19) 0.02525(16) 0.0454(2) -0.00535(14) 0.01513(17) -0.00764(12) O1 0.0323(11) 0.0244(8) 0.0356(11) 0.0040(7) 0.0166(10) -0.0008(7) O2 0.0280(11) 0.0321(10) 0.0794(18) -0.0112(10) 0.0242(12) -0.0085(8) O3 0.0497(17) 0.088(2) 0.066(2) -0.0246(17) 0.0052(16) 0.0021(15) O4 0.0673(17) 0.0431(12) 0.0349(13) 0.0023(10) 0.0185(13) -0.0006(11) O5 0.159(4) 0.0622(18) 0.0402(16) -0.0056(14) 0.017(2) -0.007(2) O6 0.129(4) 0.080(2) 0.081(3) -0.0234(19) 0.014(3) -0.032(2) O7 0.050(4) 0.077(4) 0.123(6) 0.009(4) 0.017(4) -0.019(3) N1 0.0263(13) 0.0400(12) 0.0255(12) 0.0011(10) 0.0049(11) -0.0005(9) N2 0.0307(14) 0.0432(13) 0.0267(13) -0.0008(10) 0.0068(12) 0.0002(10) N3 0.0202(11) 0.0269(10) 0.0242(11) -0.0024(8) 0.0047(10) -0.0055(8) N4 0.0192(11) 0.0289(10) 0.0312(13) -0.0025(9) 0.0068(10) -0.0046(8) N5 0.0239(12) 0.0289(10) 0.0328(13) -0.0066(9) 0.0105(11) -0.0084(9) N6 0.0405(15) 0.0407(13) 0.0361(14) -0.0075(11) 0.0146(13) -0.0158(11) C1 0.0288(15) 0.0430(15) 0.0249(15) 0.0010(11) 0.0049(13) 0.0001(12) C2 0.0316(16) 0.0460(16) 0.0220(16) -0.0018(12) 0.0007(14) -0.0020(12) C3 0.0303(17) 0.089(3) 0.0280(17) -0.0015(17) -0.0005(15) 0.0114(17) C4 0.0280(16) 0.082(2) 0.0301(18) -0.0042(16) 0.0036(15) 0.0094(16) C5 0.0217(13) 0.0301(12) 0.0242(14) -0.0031(10) 0.0053(12) -0.0077(10) C6 0.0206(13) 0.0289(12) 0.0218(14) 0.0002(10) 0.0001(12) -0.0080(10) C7 0.0291(15) 0.0297(12) 0.0354(16) -0.0068(11) 0.0097(14) -0.0078(11) C8 0.0258(14) 0.0318(13) 0.0407(17) -0.0079(12) 0.0131(14) -0.0073(11) C9 0.0363(16) 0.0354(13) 0.0299(15) -0.0058(11) 0.0113(14) -0.0122(12) C10 0.0221(13) 0.0276(11) 0.0278(14) -0.0011(10) 0.0055(12) -0.0084(10) C11 0.0344(16) 0.0353(13) 0.0308(15) -0.0065(11) 0.0137(14) -0.0131(11) C12 0.0293(14) 0.0285(12) 0.0255(14) -0.0084(10) 0.0082(13) -0.0133(10) C13 0.0349(17) 0.0417(15) 0.047(2) 0.0006(14) 0.0179(17) -0.0009(13) C14 0.042(2) 0.074(3) 0.064(3) -0.008(2) 0.016(2) 0.0182(19) C15 0.064(2) 0.0475(18) 0.035(2) 0.0045(14) 0.0141(19) 0.0132(16) C16 0.067(3) 0.078(3) 0.037(2) 0.016(2) 0.010(2) 0.014(2) F1 0.145(11) 0.049(3) 0.152(12) -0.055(5) 0.074(10) -0.028(5) F2 0.106(6) 0.158(7) 0.068(4) -0.025(4) 0.063(5) -0.012(6) F3 0.074(5) 0.216(13) 0.097(7) -0.036(8) -0.004(5) 0.099(7) F1A 0.112(10) 0.210(15) 0.075(6) -0.064(7) -0.016(6) 0.088(10) F2A 0.174(12) 0.133(8) 0.34(2) -0.033(12) 0.220(16) -0.022(9) F3A 0.158(9) 0.057(4) 0.089(5) -0.001(3) 0.017(7) 0.051(4) F4 0.080(4) 0.084(6) 0.106(8) 0.000(4) -0.006(5) -0.003(4) F5 0.095(5) 0.050(3) 0.162(8) 0.025(4) 0.066(5) 0.013(3) F6 0.216(13) 0.143(8) 0.032(3) 0.016(4) 0.021(5) -0.096(8) F4A 0.202(12) 0.071(5) 0.033(3) -0.010(3) 0.030(5) -0.066(7) F5A 0.127(6) 0.055(3) 0.086(5) 0.030(3) 0.023(5) 0.015(3) F6A 0.100(5) 0.107(5) 0.067(5) -0.003(3) 0.051(4) -0.033(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 Cu1 O1 1.8870(16) 7_556 ? Cu1 O1 1.8870(16) . ? Cu1 N3 2.146(2) . ? Cu1 N3 2.146(2) 7_556 ? Cu1 N1 2.340(3) 7_556 ? Cu1 N1 2.340(3) . ? Cu2 O1 1.8833(18) . ? Cu2 O2 1.957(2) . ? Cu2 N5 2.008(2) 3_445 ? Cu2 N4 2.069(2) . ? Cu2 N2 2.459(2) 7_556 ? O1 H1 0.8167 . ? O2 C13 1.252(4) . ? O3 C13 1.215(4) . ? O4 C15 1.224(4) . ? O5 C15 1.237(5) . ? O6 H2 0.8405 . ? O6 H3 0.8571 . ? O7 H4 0.8532 . ? O7 H5 0.8578 . ? N1 C1 1.327(4) . ? N1 N2 1.339(3) . ? N2 C4 1.321(4) . ? N3 C5 1.316(3) . ? N3 N4 1.344(3) . ? N4 C8 1.326(3) . ? N5 N6 1.330(3) . ? N5 C12 1.334(3) . ? N5 Cu2 2.008(2) 3 ? N6 C9 1.351(3) . ? C1 C2 1.396(5) . ? C1 H1A 0.9600 . ? C2 C3 1.365(4) . ? C2 C2 1.482(6) 2_656 ? C3 C4 1.399(5) . ? C3 H3A 0.9600 . ? C4 H4A 0.9600 . ? C5 C6 1.412(4) . ? C5 H5A 0.9600 . ? C6 C7 1.368(4) . ? C6 C10 1.474(3) . ? C7 C8 1.395(4) . ? C7 H7A 0.9600 . ? C8 H8A 0.9600 . ? C9 C10 1.387(3) . ? C9 H9A 0.9600 . ? C10 C11 1.387(4) . ? C11 C12 1.357(3) . ? C11 H11A 0.9600 . ? C12 H12A 0.9600 . ? C13 C14 1.528(4) . ? C14 F3 1.296(6) . ? C14 F2A 1.296(6) . ? C14 F1 1.297(6) . ? C14 F1A 1.301(7) . ? C14 F2 1.328(6) . ? C14 F3A 1.330(6) . ? C15 C16 1.564(5) . ? C16 F4A 1.248(6) . ? C16 F6 1.284(5) . ? C16 F5A 1.310(5) . ? C16 F6A 1.349(5) . ? C16 F4 1.351(6) . ? C16 F5 1.388(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 O1 Cu1 O1 180.0 7_556 . ? O1 Cu1 N3 95.09(7) 7_556 . ? O1 Cu1 N3 84.91(7) . . ? O1 Cu1 N3 84.91(7) 7_556 7_556 ? O1 Cu1 N3 95.09(7) . 7_556 ? N3 Cu1 N3 180.0 . 7_556 ? O1 Cu1 N1 93.10(8) 7_556 7_556 ? O1 Cu1 N1 86.90(8) . 7_556 ? N3 Cu1 N1 88.70(8) . 7_556 ? N3 Cu1 N1 91.30(8) 7_556 7_556 ? O1 Cu1 N1 86.90(8) 7_556 . ? O1 Cu1 N1 93.10(8) . . ? N3 Cu1 N1 91.30(8) . . ? N3 Cu1 N1 88.70(8) 7_556 . ? N1 Cu1 N1 180.0 7_556 . ? O1 Cu2 O2 171.45(10) . . ? O1 Cu2 N5 93.57(8) . 3_445 ? O2 Cu2 N5 91.17(8) . 3_445 ? O1 Cu2 N4 87.54(8) . . ? O2 Cu2 N4 87.31(8) . . ? N5 Cu2 N4 176.37(9) 3_445 . ? O1 Cu2 N2 85.44(8) . 7_556 ? O2 Cu2 N2 101.22(10) . 7_556 ? N5 Cu2 N2 95.29(9) 3_445 7_556 ? N4 Cu2 N2 88.25(9) . 7_556 ? Cu2 O1 Cu1 118.23(9) . . ? Cu2 O1 H1 116.0 . . ? Cu1 O1 H1 124.9 . . ? C13 O2 Cu2 129.4(2) . . ? H2 O6 H3 108.1 . . ? H4 O7 H5 107.4 . . ? C1 N1 N2 120.2(3) . . ? C1 N1 Cu1 123.63(19) . . ? N2 N1 Cu1 116.10(18) . . ? C4 N2 N1 118.5(2) . . ? C4 N2 Cu2 130.89(19) . 7_556 ? N1 N2 Cu2 110.48(18) . 7_556 ? C5 N3 N4 119.9(2) . . ? C5 N3 Cu1 123.55(16) . . ? N4 N3 Cu1 116.55(15) . . ? C8 N4 N3 119.8(2) . . ? C8 N4 Cu2 123.43(17) . . ? N3 N4 Cu2 116.74(15) . . ? N6 N5 C12 121.0(2) . . ? N6 N5 Cu2 118.21(16) . 3 ? C12 N5 Cu2 120.67(18) . 3 ? N5 N6 C9 120.1(2) . . ? N1 C1 C2 123.6(3) . . ? N1 C1 H1A 118.2 . . ? C2 C1 H1A 118.2 . . ? C3 C2 C1 116.1(3) . . ? C3 C2 C2 123.0(4) . 2_656 ? C1 C2 C2 120.9(3) . 2_656 ? C2 C3 C4 118.0(3) . . ? C2 C3 H3A 121.0 . . ? C4 C3 H3A 121.0 . . ? N2 C4 C3 123.6(3) . . ? N2 C4 H4A 118.2 . . ? C3 C4 H4A 118.2 . . ? N3 C5 C6 122.9(2) . . ? N3 C5 H5A 118.5 . . ? C6 C5 H5A 118.5 . . ? C7 C6 C5 116.7(2) . . ? C7 C6 C10 122.0(2) . . ? C5 C6 C10 121.3(2) . . ? C6 C7 C8 118.1(2) . . ? C6 C7 H7A 121.0 . . ? C8 C7 H7A 121.0 . . ? N4 C8 C7 122.6(2) . . ? N4 C8 H8A 118.7 . . ? C7 C8 H8A 118.7 . . ? N6 C9 C10 121.2(3) . . ? N6 C9 H9A 119.4 . . ? C10 C9 H9A 119.4 . . ? C9 C10 C11 116.8(2) . . ? C9 C10 C6 122.1(2) . . ? C11 C10 C6 121.1(2) . . ? C12 C11 C10 120.1(2) . . ? C12 C11 H11A 119.9 . . ? C10 C11 H11A 119.9 . . ? N5 C12 C11 120.7(2) . . ? N5 C12 H12A 119.6 . . ? C11 C12 H12A 119.6 . . ? O3 C13 O2 129.9(3) . . ? O3 C13 C14 116.9(3) . . ? O2 C13 C14 113.2(3) . . ? F3 C14 F1 118.4(10) . . ? F2A C14 F1A 108.2(11) . . ? F3 C14 F2 103.9(7) . . ? F1 C14 F2 100.7(8) . . ? F2A C14 F3A 107.2(9) . . ? F1A C14 F3A 99.5(8) . . ? F3 C14 C13 111.7(5) . . ? F2A C14 C13 112.8(6) . . ? F1 C14 C13 112.9(6) . . ? F1A C14 C13 117.4(6) . . ? F2 C14 C13 107.6(5) . . ? F3A C14 C13 110.5(5) . . ? O4 C15 O5 130.0(4) . . ? O4 C15 C16 114.8(3) . . ? O5 C15 C16 115.1(3) . . ? F4A C16 F5A 115.2(5) . . ? F4A C16 F6A 109.4(5) . . ? F5A C16 F6A 103.9(4) . . ? F6 C16 F4 106.7(6) . . ? F6 C16 F5 104.3(5) . . ? F4 C16 F5 97.9(4) . . ? F4A C16 C15 116.2(4) . . ? F6 C16 C15 123.2(5) . . ? F5A C16 C15 108.1(4) . . ? F6A C16 C15 102.7(4) . . ? F4 C16 C15 112.0(5) . . ? F5 C16 C15 109.5(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 N5 Cu2 O1 Cu1 143.49(13) 3_445 . . . ? N4 Cu2 O1 Cu1 -39.97(13) . . . . ? N2 Cu2 O1 Cu1 48.47(12) 7_556 . . . ? N3 Cu1 O1 Cu2 40.04(12) . . . . ? N3 Cu1 O1 Cu2 -139.96(12) 7_556 . . . ? N1 Cu1 O1 Cu2 -48.94(12) 7_556 . . . ? N1 Cu1 O1 Cu2 131.06(12) . . . . ? N5 Cu2 O2 C13 -44.1(3) 3_445 . . . ? N4 Cu2 O2 C13 139.2(3) . . . . ? N2 Cu2 O2 C13 51.5(3) 7_556 . . . ? O1 Cu1 N1 C1 152.0(2) 7_556 . . . ? O1 Cu1 N1 C1 -28.0(2) . . . . ? N3 Cu1 N1 C1 57.0(2) . . . . ? N3 Cu1 N1 C1 -123.0(2) 7_556 . . . ? O1 Cu1 N1 N2 -24.32(19) 7_556 . . . ? O1 Cu1 N1 N2 155.68(19) . . . . ? N3 Cu1 N1 N2 -119.35(19) . . . . ? N3 Cu1 N1 N2 60.65(19) 7_556 . . . ? C1 N1 N2 C4 -0.4(4) . . . . ? Cu1 N1 N2 C4 176.1(2) . . . . ? C1 N1 N2 Cu2 -177.0(2) . . . 7_556 ? Cu1 N1 N2 Cu2 -0.5(2) . . . 7_556 ? O1 Cu1 N3 C5 -22.7(2) 7_556 . . . ? O1 Cu1 N3 C5 157.3(2) . . . . ? N1 Cu1 N3 C5 -115.7(2) 7_556 . . . ? N1 Cu1 N3 C5 64.3(2) . . . . ? O1 Cu1 N3 N4 156.34(19) 7_556 . . . ? O1 Cu1 N3 N4 -23.66(19) . . . . ? N1 Cu1 N3 N4 63.34(19) 7_556 . . . ? N1 Cu1 N3 N4 -116.66(19) . . . . ? C5 N3 N4 C8 0.0(4) . . . . ? Cu1 N3 N4 C8 -179.1(2) . . . . ? C5 N3 N4 Cu2 -178.2(2) . . . . ? Cu1 N3 N4 Cu2 2.7(2) . . . . ? O1 Cu2 N4 C8 -158.5(3) . . . . ? O2 Cu2 N4 C8 14.7(3) . . . . ? N2 Cu2 N4 C8 116.0(3) 7_556 . . . ? O1 Cu2 N4 N3 19.67(19) . . . . ? O2 Cu2 N4 N3 -167.2(2) . . . . ? N2 Cu2 N4 N3 -65.84(19) 7_556 . . . ? C12 N5 N6 C9 1.5(4) . . . . ? Cu2 N5 N6 C9 -175.1(2) 3 . . . ? N2 N1 C1 C2 -0.7(4) . . . . ? Cu1 N1 C1 C2 -176.8(2) . . . . ? N1 C1 C2 C3 1.0(5) . . . . ? N1 C1 C2 C2 -178.2(2) . . . 2_656 ? C1 C2 C3 C4 -0.4(5) . . . . ? C2 C2 C3 C4 178.8(3) 2_656 . . . ? N1 N2 C4 C3 1.0(5) . . . . ? Cu2 N2 C4 C3 176.9(3) 7_556 . . . ? C2 C3 C4 N2 -0.7(6) . . . . ? N4 N3 C5 C6 0.0(4) . . . . ? Cu1 N3 C5 C6 179.0(2) . . . . ? N3 C5 C6 C7 -0.2(4) . . . . ? N3 C5 C6 C10 179.4(3) . . . . ? C5 C6 C7 C8 0.4(4) . . . . ? C10 C6 C7 C8 -179.2(3) . . . . ? N3 N4 C8 C7 0.2(5) . . . . ? Cu2 N4 C8 C7 178.3(2) . . . . ? C6 C7 C8 N4 -0.4(5) . . . . ? N5 N6 C9 C10 -0.6(5) . . . . ? N6 C9 C10 C11 -0.5(4) . . . . ? N6 C9 C10 C6 178.6(3) . . . . ? C7 C6 C10 C9 -142.8(3) . . . . ? C5 C6 C10 C9 37.7(4) . . . . ? C7 C6 C10 C11 36.3(4) . . . . ? C5 C6 C10 C11 -143.3(3) . . . . ? C9 C10 C11 C12 0.7(4) . . . . ? C6 C10 C11 C12 -178.4(3) . . . . ? N6 N5 C12 C11 -1.3(4) . . . . ? Cu2 N5 C12 C11 175.2(2) 3 . . . ? C10 C11 C12 N5 0.2(5) . . . . ? Cu2 O2 C13 O3 -8.3(5) . . . . ? Cu2 O2 C13 C14 171.0(2) . . . . ? O3 C13 C14 F3 -14.2(11) . . . . ? O2 C13 C14 F3 166.4(10) . . . . ? O3 C13 C14 F2A 54.4(13) . . . . ? O2 C13 C14 F2A -125.0(13) . . . . ? O3 C13 C14 F1 -150.5(7) . . . . ? O2 C13 C14 F1 30.0(8) . . . . ? O3 C13 C14 F1A -178.7(10) . . . . ? O2 C13 C14 F1A 1.8(10) . . . . ? O3 C13 C14 F2 99.2(6) . . . . ? O2 C13 C14 F2 -80.2(6) . . . . ? O3 C13 C14 F3A -65.6(7) . . . . ? O2 C13 C14 F3A 115.0(7) . . . . ? O4 C15 C16 F4A -18.7(7) . . . . ? O5 C15 C16 F4A 159.4(6) . . . . ? O4 C15 C16 F6 -180.0(7) . . . . ? O5 C15 C16 F6 -1.9(8) . . . . ? O4 C15 C16 F5A 112.6(5) . . . . ? O5 C15 C16 F5A -69.3(6) . . . . ? O4 C15 C16 F6A -138.0(5) . . . . ? O5 C15 C16 F6A 40.1(6) . . . . ? O4 C15 C16 F4 -50.4(6) . . . . ? O5 C15 C16 F4 127.7(6) . . . . ? O4 C15 C16 F5 57.1(6) . . . . ? O5 C15 C16 F5 -124.8(6) . . . . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 0.740 _refine_diff_density_min -0.397 _refine_diff_density_rms 0.072 #============================================================================== data_(7) _database_code_depnum_ccdc_archive 'CCDC 640638' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Copper(I) Chloride 2:1 Complex with 4,4'-Bipyridazine ; _chemical_name_common "Copper(i) Chloride 2:1 Complex with 4,4'-Bipyridazine" _chemical_melting_point ? _chemical_formula_moiety 'C8 H6 CL2 CU2 N4' _chemical_formula_sum 'C8 H6 Cl2 Cu2 N4' _chemical_formula_weight 356.15 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' 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' N N 0.0061 0.0033 '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 ' _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 6.617(2) _cell_length_b 13.132(4) _cell_length_c 6.642(2) _cell_angle_alpha 90.00 _cell_angle_beta 114.23(2) _cell_angle_gamma 90.00 _cell_volume 526.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 22 _cell_measurement_theta_min 12.11 _cell_measurement_theta_max 17.77 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 2.247 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 348 _exptl_absorpt_coefficient_mu 4.518 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.2686 _exptl_absorpt_correction_T_max 0.4047 _exptl_absorpt_process_details '(North et al., 1968)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'Enraf-Nonius CAD4' _diffrn_measurement_method 'non-profiled \w-2\q scans' _diffrn_standards_number 3 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 1003 _diffrn_reflns_av_R_equivalents 0.0309 _diffrn_reflns_av_sigmaI/netI 0.0287 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 24.97 _reflns_number_total 923 _reflns_number_gt 796 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1c (Brandenburg, 1999)' _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^)+(0.0505P)^2^+0.4239P] 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_number_reflns 923 _refine_ls_number_parameters 73 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0399 _refine_ls_R_factor_gt 0.0315 _refine_ls_wR_factor_ref 0.0890 _refine_ls_wR_factor_gt 0.0845 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _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 0.04439(8) 0.72742(4) 0.23373(8) 0.0329(2) Uani 1 1 d . . . Cl1 Cl 0.25679(17) 0.67673(8) 0.05449(16) 0.0414(3) Uani 1 1 d . . . N1 N -0.1202(5) 0.6320(2) 0.3481(5) 0.0256(6) Uani 1 1 d . . . N2 N -0.1694(5) 0.6665(2) 0.5157(5) 0.0309(7) Uani 1 1 d . . . C1 C -0.3159(6) 0.6164(3) 0.5664(7) 0.0321(8) Uani 1 1 d . . . H1A H -0.3557 0.6450 0.6783 0.039 Uiso 1 1 calc R . . C2 C -0.4171(5) 0.5248(3) 0.4683(6) 0.0243(7) Uani 1 1 d . . . C3 C -0.3509(6) 0.4866(3) 0.3127(6) 0.0306(8) Uani 1 1 d . . . H3A H -0.4046 0.4219 0.2443 0.037 Uiso 1 1 calc R . . C4 C -0.2051(6) 0.5432(3) 0.2558(6) 0.0304(8) Uani 1 1 d . . . H4A H -0.1631 0.5169 0.1437 0.036 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 0.0336(3) 0.0322(3) 0.0340(3) 0.00374(18) 0.0149(2) 0.00028(19) Cl1 0.0435(6) 0.0478(6) 0.0331(5) 0.0074(4) 0.0159(5) 0.0223(5) N1 0.0224(15) 0.0258(14) 0.0253(16) -0.0016(12) 0.0063(12) -0.0008(12) N2 0.0292(17) 0.0298(16) 0.0336(17) -0.0070(13) 0.0128(14) -0.0080(13) C1 0.031(2) 0.033(2) 0.032(2) -0.0068(15) 0.0122(16) -0.0081(16) C2 0.0167(16) 0.0263(17) 0.0228(18) 0.0022(14) 0.0010(14) 0.0008(14) C3 0.0250(19) 0.0273(19) 0.038(2) -0.0055(16) 0.0120(17) -0.0016(15) C4 0.029(2) 0.0317(19) 0.031(2) -0.0037(15) 0.0128(17) -0.0019(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 Cu1 N1 2.003(3) . ? Cu1 N2 2.087(3) 4_575 ? Cu1 Cl1 2.2825(11) . ? Cu1 Cl1 2.3749(12) 4_576 ? N1 C4 1.330(5) . ? N1 N2 1.359(4) . ? N2 C1 1.324(5) . ? C1 C2 1.401(5) . ? C2 C3 1.372(5) . ? C2 C2 1.478(7) 3_466 ? C3 C4 1.388(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 Cu1 N2 111.18(12) . 4_575 ? N1 Cu1 Cl1 124.23(9) . . ? N2 Cu1 Cl1 102.71(9) 4_575 . ? N1 Cu1 Cl1 101.83(9) . 4_576 ? N2 Cu1 Cl1 104.56(10) 4_575 4_576 ? Cl1 Cu1 Cl1 110.98(6) . 4_576 ? Cu1 Cl1 Cu1 92.80(4) . 4_575 ? C4 N1 N2 118.1(3) . . ? C4 N1 Cu1 124.5(3) . . ? N2 N1 Cu1 116.9(2) . . ? C1 N2 N1 119.3(3) . . ? C1 N2 Cu1 120.9(2) . 4_576 ? N1 N2 Cu1 117.9(2) . 4_576 ? N2 C1 C2 124.6(3) . . ? C3 C2 C1 115.1(3) . . ? C3 C2 C2 123.9(4) . 3_466 ? C1 C2 C2 121.0(4) . 3_466 ? C2 C3 C4 118.8(3) . . ? N1 C4 C3 123.6(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 N1 Cu1 Cl1 Cu1 121.42(10) . . . 4_575 ? N2 Cu1 Cl1 Cu1 -5.56(10) 4_575 . . 4_575 ? Cl1 Cu1 Cl1 Cu1 -116.81(6) 4_576 . . 4_575 ? N2 Cu1 N1 C4 91.7(3) 4_575 . . . ? Cl1 Cu1 N1 C4 -31.6(3) . . . . ? Cl1 Cu1 N1 C4 -157.4(3) 4_576 . . . ? N2 Cu1 N1 N2 -80.3(2) 4_575 . . . ? Cl1 Cu1 N1 N2 156.4(2) . . . . ? Cl1 Cu1 N1 N2 30.6(3) 4_576 . . . ? C4 N1 N2 C1 -6.7(5) . . . . ? Cu1 N1 N2 C1 165.9(3) . . . . ? C4 N1 N2 Cu1 157.9(3) . . . 4_576 ? Cu1 N1 N2 Cu1 -29.5(3) . . . 4_576 ? N1 N2 C1 C2 4.4(6) . . . . ? Cu1 N2 C1 C2 -159.8(3) 4_576 . . . ? N2 C1 C2 C3 1.2(6) . . . . ? N2 C1 C2 C2 -178.6(4) . . . 3_466 ? C1 C2 C3 C4 -4.1(5) . . . . ? C2 C2 C3 C4 175.7(4) 3_466 . . . ? N2 N1 C4 C3 3.8(6) . . . . ? Cu1 N1 C4 C3 -168.2(3) . . . . ? C2 C3 C4 N1 1.8(6) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.383 _refine_diff_density_min -0.433 _refine_diff_density_rms 0.096 #============================================================================== data_(8) _database_code_depnum_ccdc_archive 'CCDC 640639' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Copper(I) Bromide 2:1 Complex with 4,4'-Bipyridazine ; _chemical_name_common "Copper(i) Bromide 2:1 Complex with 4,4'-Bipyridazine" _chemical_melting_point ? _chemical_formula_moiety 'C8 H6 Br2 Cu2 N4' _chemical_formula_sum 'C8 H6 Br2 Cu2 N4' _chemical_formula_weight 445.07 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' Br Br -0.2901 2.4595 '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' N N 0.0061 0.0033 '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 ' _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 6.712(2) _cell_length_b 13.450(4) _cell_length_c 6.807(3) _cell_angle_alpha 90.00 _cell_angle_beta 112.79(3) _cell_angle_gamma 90.00 _cell_volume 566.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 13.25 _cell_measurement_theta_max 19.12 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.22 _exptl_crystal_density_diffrn 2.609 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 420 _exptl_absorpt_coefficient_mu 10.779 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.0659 _exptl_absorpt_correction_T_max 0.0941 _exptl_absorpt_process_details '(North et al., 1968)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'Enraf-Nonius CAD4' _diffrn_measurement_method 'non-profiled \w-2\q scans' _diffrn_standards_number 3 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 1068 _diffrn_reflns_av_R_equivalents 0.0765 _diffrn_reflns_av_sigmaI/netI 0.0347 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 24.99 _reflns_number_total 983 _reflns_number_gt 830 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1c (Brandenburg, 1999)' _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^)+(0.0607P)^2^+0.4807P] 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_number_reflns 983 _refine_ls_number_parameters 73 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0491 _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_ref 0.0987 _refine_ls_wR_factor_gt 0.0933 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _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 0.02625(12) 0.73438(6) 0.24493(11) 0.0285(3) Uani 1 1 d . . . Br1 Br 0.24053(11) 0.66585(5) 0.06106(10) 0.0412(3) Uani 1 1 d . . . N1 N -0.1263(7) 0.6352(4) 0.3645(7) 0.0228(10) Uani 1 1 d . . . N2 N -0.1772(8) 0.6654(4) 0.5275(8) 0.0253(11) Uani 1 1 d . . . C1 C -0.3203(10) 0.6137(5) 0.5741(9) 0.0307(14) Uani 1 1 d . . . H1A H -0.3609 0.6381 0.6860 0.037 Uiso 1 1 calc R . . C2 C -0.4165(8) 0.5259(4) 0.4714(8) 0.0217(12) Uani 1 1 d . . . C3 C -0.3443(9) 0.4912(5) 0.3209(9) 0.0282(13) Uani 1 1 d . . . H3A H -0.3904 0.4278 0.2539 0.034 Uiso 1 1 calc R . . C4 C -0.2027(9) 0.5504(5) 0.2684(9) 0.0266(13) Uani 1 1 d . . . H4A H -0.1586 0.5285 0.1571 0.032 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 0.0342(5) 0.0299(5) 0.0274(4) 0.0035(3) 0.0185(3) 0.0011(3) Br1 0.0495(5) 0.0524(5) 0.0282(4) 0.0097(3) 0.0221(3) 0.0285(3) N1 0.024(2) 0.026(3) 0.021(2) 0.002(2) 0.011(2) 0.003(2) N2 0.031(3) 0.027(3) 0.023(2) -0.002(2) 0.016(2) -0.007(2) C1 0.037(3) 0.038(4) 0.027(3) -0.011(3) 0.022(3) -0.012(3) C2 0.021(3) 0.026(3) 0.019(3) 0.004(2) 0.008(2) -0.001(2) C3 0.028(3) 0.029(3) 0.033(3) -0.003(3) 0.018(3) -0.005(3) C4 0.032(3) 0.026(3) 0.027(3) -0.005(3) 0.018(3) -0.001(3) _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 2.033(5) . ? Cu1 N2 2.076(5) 4_575 ? Cu1 Br1 2.4247(11) . ? Cu1 Br1 2.4703(13) 4_576 ? N1 C4 1.316(7) . ? N1 N2 1.344(6) . ? N2 C1 1.320(7) . ? C1 C2 1.397(8) . ? C2 C3 1.373(8) . ? C2 C2 1.494(11) 3_466 ? C3 C4 1.389(8) . ? 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 N2 114.66(19) . 4_575 ? N1 Cu1 Br1 116.65(14) . . ? N2 Cu1 Br1 103.70(13) 4_575 . ? N1 Cu1 Br1 102.79(13) . 4_576 ? N2 Cu1 Br1 105.58(14) 4_575 4_576 ? Br1 Cu1 Br1 113.23(5) . 4_576 ? Cu1 Br1 Cu1 88.94(4) . 4_575 ? C4 N1 N2 119.8(5) . . ? C4 N1 Cu1 122.0(4) . . ? N2 N1 Cu1 117.5(4) . . ? C1 N2 N1 118.8(5) . . ? C1 N2 Cu1 120.6(4) . 4_576 ? N1 N2 Cu1 118.5(3) . 4_576 ? N2 C1 C2 124.3(5) . . ? C3 C2 C1 115.6(5) . . ? C3 C2 C2 123.6(6) . 3_466 ? C1 C2 C2 120.8(6) . 3_466 ? C2 C3 C4 118.1(6) . . ? N1 C4 C3 122.9(5) . . ? 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 N1 Cu1 Br1 Cu1 124.00(15) . . . 4_575 ? N2 Cu1 Br1 Cu1 -3.08(15) 4_575 . . 4_575 ? Br1 Cu1 Br1 Cu1 -117.00(6) 4_576 . . 4_575 ? N2 Cu1 N1 C4 87.4(5) 4_575 . . . ? Br1 Cu1 N1 C4 -34.0(5) . . . . ? Br1 Cu1 N1 C4 -158.5(4) 4_576 . . . ? N2 Cu1 N1 N2 -82.4(3) 4_575 . . . ? Br1 Cu1 N1 N2 156.2(3) . . . . ? Br1 Cu1 N1 N2 31.7(4) 4_576 . . . ? C4 N1 N2 C1 -6.5(8) . . . . ? Cu1 N1 N2 C1 163.5(5) . . . . ? C4 N1 N2 Cu1 157.1(4) . . . 4_576 ? Cu1 N1 N2 Cu1 -32.9(5) . . . 4_576 ? N1 N2 C1 C2 3.3(9) . . . . ? Cu1 N2 C1 C2 -160.0(5) 4_576 . . . ? N2 C1 C2 C3 3.5(9) . . . . ? N2 C1 C2 C2 -177.6(7) . . . 3_466 ? C1 C2 C3 C4 -6.7(8) . . . . ? C2 C2 C3 C4 174.4(6) 3_466 . . . ? N2 N1 C4 C3 3.1(8) . . . . ? Cu1 N1 C4 C3 -166.5(5) . . . . ? C2 C3 C4 N1 3.8(9) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.976 _refine_diff_density_min -0.600 _refine_diff_density_rms 0.152 #============================================================================== data_(9) _database_code_depnum_ccdc_archive 'CCDC 640640' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Copper(I) Iodide 2:1 Complex with 4,4'-Bipyridazine ; _chemical_name_common "Copper(i) Iodide 2:1 Complex with 4,4'-Bipyridazine" _chemical_melting_point ? _chemical_formula_moiety 'C8 H6 Cu2 I2 N4' _chemical_formula_sum 'C8 H6 Cu2 I2 N4' _chemical_formula_weight 539.05 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'P 4(3)2(1)2 ' _space_group_name_Hall 'P 4nw 2abw ' _symmetry_Int_Tables_number 96 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+3/4' 'y+1/2, -x+1/2, z+1/4' '-x+1/2, y+1/2, -z+3/4' 'x+1/2, -y+1/2, -z+1/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 10.1405(5) _cell_length_b 10.1405(5) _cell_length_c 11.9784(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1231.74(11) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 11901 _cell_measurement_theta_min 2.84 _cell_measurement_theta_max 27.97 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 2.907 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 8.441 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3230 _exptl_absorpt_correction_T_max 0.3618 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1999)' _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 'Bruker Apex CCD area-detector diffractometer' _diffrn_measurement_method '\w scans' _diffrn_standards_decay_% 0 _diffrn_reflns_number 11901 _diffrn_reflns_av_R_equivalents 0.0386 _diffrn_reflns_av_sigmaI/netI 0.0180 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_max 27.97 _reflns_number_total 1478 _reflns_number_gt 1409 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT (Bruker, 1998)' _computing_cell_refinement 'SMART-NT (Bruker, 1998)' _computing_data_reduction 'SMART-NT (Bruker, 1998)' _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^)+(0.0114P)^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 mixed _refine_ls_extinction_method none _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.013(19) _refine_ls_number_reflns 1478 _refine_ls_number_parameters 85 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0130 _refine_ls_R_factor_gt 0.0117 _refine_ls_wR_factor_ref 0.0240 _refine_ls_wR_factor_gt 0.0238 _refine_ls_goodness_of_fit_ref 0.966 _refine_ls_restrained_S_all 0.966 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.59427(3) 0.02883(3) -0.12512(2) 0.02612(7) Uani 1 1 d . . . I1 I 0.726470(16) 0.053282(16) 0.060164(13) 0.02692(4) Uani 1 1 d . . . N1 N 0.71334(19) -0.00881(19) -0.26072(15) 0.0209(4) Uani 1 1 d . . . N2 N 0.6581(2) 0.0069(2) -0.36284(15) 0.0225(4) Uani 1 1 d . . . C1 C 0.8302(2) -0.0659(3) -0.25263(18) 0.0245(5) Uani 1 1 d . . . H1 H 0.861(3) -0.073(3) -0.180(2) 0.023(6) Uiso 1 1 d . . . C2 C 0.9011(3) -0.1134(3) -0.34394(18) 0.0265(5) Uani 1 1 d . . . H2 H 0.979(3) -0.161(3) -0.334(2) 0.041(9) Uiso 1 1 d . . . C4 C 0.7232(2) -0.0341(2) -0.45243(17) 0.0240(4) Uani 1 1 d . . . H4 H 0.678(3) -0.024(3) -0.521(2) 0.036(8) Uiso 1 1 d . . . C3 C 0.8460(2) -0.0970(2) -0.44833(18) 0.0204(4) 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 Cu1 0.03032(15) 0.02814(16) 0.01990(12) -0.00010(12) 0.00186(11) -0.00130(12) I1 0.02623(8) 0.03162(9) 0.02289(6) 0.00085(7) -0.00354(6) -0.00288(6) N1 0.0238(10) 0.0224(9) 0.0166(8) 0.0002(7) -0.0019(7) 0.0012(8) N2 0.0228(10) 0.0273(10) 0.0175(8) 0.0002(8) 0.0002(8) 0.0033(8) C1 0.0237(12) 0.0312(13) 0.0186(10) -0.0001(10) -0.0039(9) 0.0036(10) C2 0.0237(12) 0.0302(14) 0.0256(11) -0.0008(10) -0.0025(9) 0.0042(10) C4 0.0273(12) 0.0282(12) 0.0165(9) 0.0004(9) -0.0011(9) 0.0043(9) C3 0.0196(10) 0.0205(10) 0.0210(10) -0.0023(9) 0.0011(9) 0.0000(8) _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 2.0595(19) . ? Cu1 N2 2.097(2) 4 ? Cu1 I1 2.6047(4) . ? Cu1 I1 2.6185(4) 3_544 ? N1 C1 1.323(3) . ? N1 N2 1.355(2) . ? N2 C4 1.327(3) . ? C1 C2 1.394(3) . ? C1 H1 0.93(3) . ? C2 C3 1.380(3) . ? C2 H2 0.93(3) . ? C4 C3 1.399(3) . ? C4 H4 0.94(3) . ? C3 C3 1.484(4) 7_644 ? 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 N2 97.79(8) . 4 ? N1 Cu1 I1 112.82(5) . . ? N2 Cu1 I1 104.11(5) 4 . ? N1 Cu1 I1 104.08(5) . 3_544 ? N2 Cu1 I1 118.10(6) 4 3_544 ? I1 Cu1 I1 118.259(12) . 3_544 ? Cu1 I1 Cu1 78.691(10) . 4 ? C1 N1 N2 119.22(19) . . ? C1 N1 Cu1 123.27(15) . . ? N2 N1 Cu1 116.60(14) . . ? C4 N2 N1 119.17(19) . . ? C4 N2 Cu1 121.71(16) . 3_544 ? N1 N2 Cu1 119.12(14) . 3_544 ? N1 C1 C2 123.7(2) . . ? N1 C1 H1 113.6(16) . . ? C2 C1 H1 122.7(16) . . ? C3 C2 C1 117.4(2) . . ? C3 C2 H2 121.0(18) . . ? C1 C2 H2 121.3(18) . . ? N2 C4 C3 123.9(2) . . ? N2 C4 H4 115.0(18) . . ? C3 C4 H4 120.9(18) . . ? C2 C3 C4 116.5(2) . . ? C2 C3 C3 123.5(3) . 7_644 ? C4 C3 C3 119.7(2) . 7_644 ? 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 N1 Cu1 I1 Cu1 -136.20(6) . . . 4 ? N2 Cu1 I1 Cu1 -31.28(6) 4 . . 4 ? I1 Cu1 I1 Cu1 102.061(6) 3_544 . . 4 ? N2 Cu1 N1 C1 -83.3(2) 4 . . . ? I1 Cu1 N1 C1 25.6(2) . . . . ? I1 Cu1 N1 C1 155.07(18) 3_544 . . . ? N2 Cu1 N1 N2 85.72(19) 4 . . . ? I1 Cu1 N1 N2 -165.35(14) . . . . ? I1 Cu1 N1 N2 -35.91(16) 3_544 . . . ? C1 N1 N2 C4 -0.8(3) . . . . ? Cu1 N1 N2 C4 -170.25(17) . . . . ? C1 N1 N2 Cu1 178.87(18) . . . 3_544 ? Cu1 N1 N2 Cu1 9.4(2) . . . 3_544 ? N2 N1 C1 C2 -0.8(4) . . . . ? Cu1 N1 C1 C2 168.0(2) . . . . ? N1 C1 C2 C3 1.2(4) . . . . ? N1 N2 C4 C3 1.9(4) . . . . ? Cu1 N2 C4 C3 -177.73(18) 3_544 . . . ? C1 C2 C3 C4 -0.1(4) . . . . ? C1 C2 C3 C3 -173.62(18) . . . 7_644 ? N2 C4 C3 C2 -1.4(4) . . . . ? N2 C4 C3 C3 172.34(19) . . . 7_644 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.97 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.444 _refine_diff_density_min -0.280 _refine_diff_density_rms 0.060 #==============================================================================