Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Konstantin V. Domasevitch' _publ_contact_author_email DK@MAIL.UNIV.KIEV.UA _publ_section_title ; New microporous copper(II) coordination polymers based upon bifunctional 1,2,4-triazole/tetrazolate bridges ; loop_ _publ_author_name 'Konstantin V. Domasevitch' 'Oksana A Bondar' 'Alexander N Chernega' 'Harald Krautscheid' ; L.V.Lukashuk ; 'Andrey B. Lysenko' 'Eduard B Rusanov' # Attachment 'cif_data.cif' #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_(1) _database_code_depnum_ccdc_archive 'CCDC 674753' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Copper(II) Fluorophosphate 1:3 Complex with 1,4-bi(1,2,4-triazol-4-yl)benzene ; _chemical_name_common ;Copper(ii) Fluorophosphate 1:3 Complex with 1,4-bi(1,2,4- triazol-4-yl)benzene ; _chemical_melting_point ? _chemical_formula_moiety 'C30 H24 Cu N18, (F O3 P)' _chemical_formula_sum 'C30 H24 Cu F N18 O3 P' _chemical_formula_weight 798.18 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' P P 0.1023 0.0942 '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 Hexagonal _symmetry_space_group_name_H-M 'P 63/m c m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' '-y, -x, -z' '-x+y, y, -z' 'x, x-y, -z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z-1/2' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' 'y, x, z' 'x-y, -y, z' '-x, -x+y, z' _cell_length_a 16.0657(11) _cell_length_b 16.0657(11) _cell_length_c 7.7720(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1737.25(19) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 7443 _cell_measurement_theta_min 3.65 _cell_measurement_theta_max 25.89 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.526 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 814 _exptl_absorpt_coefficient_mu 0.743 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe Imaging plate diffraction system' _diffrn_measurement_method '\f oscillation scans' _diffrn_standards_decay_% 0 _diffrn_reflns_number 7443 _diffrn_reflns_av_R_equivalents 0.0499 _diffrn_reflns_av_sigmaI/netI 0.0311 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 3.65 _diffrn_reflns_theta_max 25.89 _reflns_number_total 649 _reflns_number_gt 477 _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)' #------------------------------- Refinement data-----------------------# _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. The structure was solved by direct methods. The 1,4-phenylene group of the ligand was equally disordered over two symmetry related positions, and thus the corresponding C3 and C4 carbon atoms were refined with partial occupancy factors 0.5. Triazole atoms from non-coordinated side of the ligand possess relatively high parameters for thermal motion. This situation itself is very characteristic for side non-bound fragments of very lengthy groups. It was not possible to resolve the possible disorder and these atoms were refined anisotropically. The CH hydrogen atoms were added geometrically and included as fixed contributions with U~iso~(H) = 1.2U~eq~ (parent carbon atoms). Very short contacts anion-to-anion suggested partial occupancy of the anion position (0.5). This agrees well with a overall charge compensation by dianionic moieties PO~3~F^2-^ (one equivalent per metal ion). The anion was refined with fixed tetrahedral geometry, SIMU restraints for atomic thermal parameters, and with oxygens as the ligand atoms. ; _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^)+(0.0983P)^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 649 _refine_ls_number_parameters 71 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0597 _refine_ls_R_factor_gt 0.0472 _refine_ls_wR_factor_ref 0.1231 _refine_ls_wR_factor_gt 0.1188 _refine_ls_goodness_of_fit_ref 0.939 _refine_ls_restrained_S_all 0.950 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.0000 0.0000 0.0000 0.0372(4) Uani 1 12 d S . . N1 N 0.0000 0.10646(19) 0.1625(5) 0.0559(8) Uani 1 2 d S . . N2 N 0.0000 0.2339(3) 0.2500 0.0710(15) Uani 1 4 d S . . N3 N 0.0000 0.5829(4) 0.2500 0.121(3) Uani 1 4 d S . . N4 N -0.0489(7) 0.6883(5) 0.2500 0.182(6) Uani 1 2 d S . . C1 C 0.0000 0.1837(2) 0.1120(8) 0.0716(13) Uani 1 2 d S . . H1 H 0.0000 0.2016 -0.0032 0.086 Uiso 1 2 calc SR . . C2 C 0.0000 0.3229(4) 0.2500 0.080(2) Uani 1 4 d S . . C3 C 0.0768(7) 0.4044(5) 0.1798(15) 0.114(4) Uani 0.50 1 d P . . H3 H 0.1302 0.4001 0.1294 0.136 Uiso 0.50 1 d P . . C4 C 0.0773(7) 0.4904(5) 0.1836(13) 0.111(4) Uani 0.50 1 d P . . H4 H 0.1289 0.5490 0.1377 0.134 Uiso 0.50 1 d P . . C5 C 0.0000 0.4924(5) 0.2500 0.103(3) Uani 1 4 d S . . C6 C -0.0744(9) 0.5987(6) 0.2500 0.166(4) Uani 1 2 d S . . H6 H -0.1390 0.5491 0.2500 0.199 Uiso 1 2 calc SR . . P1 P 0.3333 0.6667 0.0627(9) 0.175(6) Uani 0.25 3 d SPDU . . O1 O 0.2850(2) 0.5700(5) 0.0000 0.178(6) Uani 0.50 2 d SPDU . . O2 O 0.3333 0.6667 0.2500 0.185(7) Uani 0.50 6 d SPDU . . 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 0.0315(4) 0.0315(4) 0.0486(6) 0.000 0.000 0.01575(19) N1 0.0504(16) 0.0397(10) 0.081(2) 0.0069(12) 0.000 0.0252(8) N2 0.070(3) 0.0461(18) 0.105(5) 0.000 0.000 0.0349(15) N3 0.204(10) 0.085(3) 0.116(6) 0.000 0.000 0.102(5) N4 0.356(19) 0.153(7) 0.143(5) 0.000 0.000 0.206(11) C1 0.080(3) 0.0471(14) 0.098(4) 0.0021(19) 0.000 0.0401(14) C2 0.086(5) 0.052(2) 0.113(6) 0.000 0.000 0.043(2) C3 0.107(6) 0.053(3) 0.181(13) -0.006(4) 0.007(6) 0.041(4) C4 0.129(7) 0.059(4) 0.148(11) 0.008(4) 0.013(6) 0.048(4) C5 0.151(9) 0.072(3) 0.113(7) 0.000 0.000 0.075(4) C6 0.223(10) 0.116(6) 0.223(11) 0.000 0.000 0.132(7) P1 0.122(3) 0.122(3) 0.281(19) 0.000 0.000 0.0610(16) O1 0.129(5) 0.119(5) 0.284(18) 0.000 0.016(5) 0.060(3) O2 0.136(5) 0.136(5) 0.285(19) 0.000 0.000 0.068(2) _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 2.126(3) 15 ? Cu1 N1 2.126(3) 13 ? Cu1 N1 2.126(3) . ? Cu1 N1 2.126(3) 3 ? Cu1 N1 2.126(3) 14 ? Cu1 N1 2.126(3) 2 ? N1 C1 1.302(5) . ? N1 N1 1.360(7) 16_556 ? N2 C1 1.342(6) . ? N2 C1 1.342(6) 16_556 ? N2 C2 1.430(8) . ? N3 C6 1.341(10) . ? N3 C6 1.341(10) 9 ? N3 C5 1.453(10) . ? N4 C6 1.285(9) . ? N4 N4 1.36(2) 9 ? C1 H1 0.9400 . ? C2 C3 1.385(9) . ? C2 C3 1.385(9) 9 ? C3 C4 1.378(10) . ? C3 H3 0.9764 . ? C4 C5 1.360(10) . ? C4 H4 0.9589 . ? C5 C4 1.360(10) 9 ? C6 H6 0.9400 . ? P1 P1 0.974(14) 10_665 ? P1 O1 1.430(6) 3_565 ? P1 O1 1.430(6) . ? P1 O1 1.430(6) 2_665 ? P1 O2 1.456(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 N1 Cu1 N1 88.32(13) 15 13 ? N1 Cu1 N1 91.68(13) 15 . ? N1 Cu1 N1 180.00(19) 13 . ? N1 Cu1 N1 180.00(19) 15 3 ? N1 Cu1 N1 91.68(13) 13 3 ? N1 Cu1 N1 88.32(13) . 3 ? N1 Cu1 N1 88.32(13) 15 14 ? N1 Cu1 N1 88.32(13) 13 14 ? N1 Cu1 N1 91.68(13) . 14 ? N1 Cu1 N1 91.68(13) 3 14 ? N1 Cu1 N1 91.68(13) 15 2 ? N1 Cu1 N1 91.68(13) 13 2 ? N1 Cu1 N1 88.32(13) . 2 ? N1 Cu1 N1 88.32(13) 3 2 ? N1 Cu1 N1 180.0(3) 14 2 ? C1 N1 N1 107.5(3) . 16_556 ? C1 N1 Cu1 126.0(3) . . ? N1 N1 Cu1 126.44(9) 16_556 . ? C1 N2 C1 106.1(5) . 16_556 ? C1 N2 C2 126.9(3) . . ? C1 N2 C2 126.9(3) 16_556 . ? C6 N3 C6 101.1(10) . 9 ? C6 N3 C5 129.4(5) . . ? C6 N3 C5 129.4(5) 9 . ? C6 N4 N4 106.0(7) . 9 ? N1 C1 N2 109.4(5) . . ? N1 C1 H1 125.3 . . ? N2 C1 H1 125.3 . . ? C3 C2 C3 120.1(8) . 9 ? C3 C2 N2 120.0(4) . . ? C4 C3 C2 119.6(8) . . ? C4 C3 H3 121.0 . . ? C2 C3 H3 119.4 . . ? C5 C4 C3 119.0(8) . . ? C5 C4 H4 118.0 . . ? C3 C4 H4 123.0 . . ? C4 C5 C4 122.6(8) . 9 ? C4 C5 N3 118.7(4) . . ? C4 C5 N3 118.7(4) 9 . ? N4 C6 N3 113.4(10) . . ? N4 C6 H6 123.3 . . ? N3 C6 H6 123.3 . . ? O1 P1 O1 109.0(3) 3_565 . ? O1 P1 O1 109.0(3) 3_565 2_665 ? O1 P1 O1 109.0(3) . 2_665 ? O1 P1 O2 109.9(3) 3_565 . ? O1 P1 O2 109.9(3) . . ? O1 P1 O2 109.9(3) 2_665 . ? 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 N1 C1 -44.18(6) 15 . . . ? N1 Cu1 N1 C1 135.82(6) 3 . . . ? N1 Cu1 N1 C1 44.18(6) 14 . . . ? N1 Cu1 N1 C1 -135.82(6) 2 . . . ? N1 Cu1 N1 N1 135.82(6) 15 . . 16_556 ? N1 Cu1 N1 N1 -44.18(6) 3 . . 16_556 ? N1 Cu1 N1 N1 -135.82(6) 14 . . 16_556 ? N1 Cu1 N1 N1 44.18(6) 2 . . 16_556 ? N1 N1 C1 N2 0.0 16_556 . . . ? Cu1 N1 C1 N2 180.0 . . . . ? C1 N2 C1 N1 0.0 16_556 . . . ? C2 N2 C1 N1 180.0 . . . . ? C1 N2 C2 C3 -63.0(5) . . . . ? N2 C2 C3 C4 -178.6(7) . . . . ? C2 C3 C4 C5 -2.7(15) . . . . ? C3 C4 C5 N3 -178.6(7) . . . . ? C6 N3 C5 C4 154.3(5) . . . . ? N4 N4 C6 N3 0.0 9 . . . ? C6 N3 C6 N4 0.0 9 . . . ? C5 N3 C6 N4 180.0 . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.89 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.741 _refine_diff_density_min -0.702 _refine_diff_density_rms 0.060 #----------------------------------------------------# data_(2) _database_code_depnum_ccdc_archive 'CCDC 674754' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Copper(II) Nitrate 2:5 Complex with 1,4-bi(1,2,4-triazol-4-yl)benzene, Dihydrate ; _chemical_name_common ; Copper(ii) Nitrate 2:5 Complex with 1,4-bi(1,2,4-triazol-4- yl)benzene, Dihydrate ; _chemical_melting_point ? _chemical_formula_moiety 'C50 H40 Cu2 N30, 4(N O3), 2(H2 O)' _chemical_formula_sum 'C50 H44 Cu2 N34 O14' _chemical_formula_weight 1472.27 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' 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 24.6600(18) _cell_length_b 15.8459(8) _cell_length_c 7.7808(5) _cell_angle_alpha 90.00 _cell_angle_beta 95.485(8) _cell_angle_gamma 90.00 _cell_volume 3026.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 3.20 _cell_measurement_theta_max 27.10 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_diffrn 1.616 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1504 _exptl_absorpt_coefficient_mu 0.799 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.8315 _exptl_absorpt_correction_T_max 0.8696 _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 11492 _diffrn_reflns_av_R_equivalents 0.0588 _diffrn_reflns_av_sigmaI/netI 0.1352 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.20 _diffrn_reflns_theta_max 27.10 _reflns_number_total 6535 _reflns_number_gt 3344 _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)' #------------------------------- Refinement data-----------------------# _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. The structure was solved by direct methods. All CH hydrogen atoms were located from difference maps and then refined as riding, with C---H distances constrained to 0.94 \%A, and with U~iso~(H) = 1.2U~eq~ (parent carbon atoms). One of the unique nitrate anions [N17, O4, O5, O6] is possibly disordered, as indicated by relatively high values for thermal motion. It was not possible to resolve the disordering scheme and these atoms were left isotropic. Solvate water molecule is disordered over two closely situated positions with partial occupancies 0.67 [O7A] and 0.33 [O7B]. Hydrogen atoms were not added to this water molecule and both contributions of the oxygen atom were refined isotropically. ; _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^)+(0.0564P)^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 6535 _refine_ls_number_parameters 430 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0952 _refine_ls_R_factor_gt 0.0467 _refine_ls_wR_factor_ref 0.1151 _refine_ls_wR_factor_gt 0.1082 _refine_ls_goodness_of_fit_ref 0.812 _refine_ls_restrained_S_all 0.812 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 #----------------Atomic Coordinates and Displacement Parameters---------# 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 0.285463(17) 0.24900(4) 0.13946(4) 0.01080(11) Uani 1 1 d . . . N1 N 0.28268(14) 0.1460(2) 0.3007(3) 0.0163(7) Uani 1 1 d . . . N2 N 0.28549(14) 0.1468(2) 0.4798(3) 0.0151(7) Uani 1 1 d . . . N3 N 0.27814(15) 0.0166(2) 0.3919(4) 0.0194(7) Uani 1 1 d . . . N4 N 0.2252(2) -0.4634(3) 0.3235(6) 0.0501(12) Uani 1 1 d . . . N5 N 0.2780(2) -0.4699(2) 0.3923(4) 0.0429(12) Uani 1 1 d . . . N6 N 0.25822(18) -0.3360(2) 0.3746(4) 0.0313(9) Uani 1 1 d . . . N7 N 0.22406(14) 0.1891(2) -0.0712(3) 0.0196(8) Uani 1 1 d . . . N8 N 0.22292(14) 0.1993(2) -0.2478(3) 0.0161(7) Uani 1 1 d . . . N9 N 0.14788(14) 0.1367(2) -0.1947(4) 0.0173(7) Uani 1 1 d . . . N10 N -0.13846(19) -0.0627(3) -0.3319(5) 0.0442(11) Uani 1 1 d . . . N11 N -0.11156(19) -0.1371(3) -0.2937(4) 0.0430(12) Uani 1 1 d . . . N12 N -0.05137(15) -0.0351(3) -0.2808(4) 0.0290(9) Uani 1 1 d . . . N13 N 0.34610(14) 0.3085(2) 0.3461(3) 0.0186(7) Uani 1 1 d . . . N14 N 0.34607(14) 0.3054(2) 0.5245(3) 0.0166(7) Uani 1 1 d . . . N15 N 0.41351(15) 0.3855(2) 0.4641(3) 0.0223(8) Uani 1 1 d . . . C1 C 0.27851(18) 0.0673(2) 0.2526(4) 0.0192(9) Uani 1 1 d . . . H1 H 0.2761 0.0486 0.1375 0.023 Uiso 1 1 calc R . . C2 C 0.28279(18) 0.0693(2) 0.5294(4) 0.0187(9) Uani 1 1 d . . . H2 H 0.2839 0.0519 0.6452 0.022 Uiso 1 1 calc R . . C3 C 0.2144(3) -0.3821(3) 0.3134(7) 0.0467(14) Uani 1 1 d . . . H3 H 0.1807 -0.3591 0.2695 0.056 Uiso 1 1 calc R . . C4 C 0.2962(3) -0.3935(3) 0.4213(5) 0.0409(14) Uani 1 1 d . . . H4 H 0.3317 -0.3806 0.4691 0.049 Uiso 1 1 calc R . . C5 C 0.27217(18) -0.0735(3) 0.3917(5) 0.0215(9) Uani 1 1 d . . . C6 C 0.3113(2) -0.1218(3) 0.4861(5) 0.0303(11) Uani 1 1 d . . . H6 H 0.3409 -0.0960 0.5509 0.036 Uiso 1 1 calc R . . C7 C 0.3059(2) -0.2096(3) 0.4832(5) 0.0329(11) Uani 1 1 d . . . H7 H 0.3316 -0.2439 0.5473 0.039 Uiso 1 1 calc R . . C8 C 0.26213(18) -0.2452(3) 0.3839(4) 0.0267(9) Uani 1 1 d . . . C9 C 0.2238(2) -0.1968(3) 0.2905(5) 0.0319(11) Uani 1 1 d . . . H9 H 0.1944 -0.2223 0.2244 0.038 Uiso 1 1 calc R . . C10 C 0.2291(2) -0.1102(3) 0.2950(5) 0.0276(11) Uani 1 1 d . . . H10 H 0.2031 -0.0762 0.2316 0.033 Uiso 1 1 calc R . . C11 C 0.17899(18) 0.1509(3) -0.0450(4) 0.0234(10) Uani 1 1 d . . . H11 H 0.1692 0.1352 0.0644 0.028 Uiso 1 1 calc R . . C12 C 0.17753(17) 0.1677(3) -0.3182(4) 0.0202(9) Uani 1 1 d . . . H12 H 0.1668 0.1666 -0.4374 0.024 Uiso 1 1 calc R . . C13 C -0.1016(2) -0.0031(4) -0.3257(6) 0.0425(14) Uani 1 1 d . . . H13 H -0.1091 0.0541 -0.3492 0.051 Uiso 1 1 calc R . . C14 C -0.0591(2) -0.1193(3) -0.2643(5) 0.0402(13) Uani 1 1 d . . . H14 H -0.0314 -0.1591 -0.2362 0.048 Uiso 1 1 calc R . . C15 C 0.09633(17) 0.0933(3) -0.2162(4) 0.0206(9) Uani 1 1 d . . . C16 C 0.09251(19) 0.0147(3) -0.1425(5) 0.0265(10) Uani 1 1 d . . . H16 H 0.1229 -0.0097 -0.0791 0.032 Uiso 1 1 calc R . . C17 C 0.04340(19) -0.0277(3) -0.1630(5) 0.0320(11) Uani 1 1 d . . . H17 H 0.0399 -0.0810 -0.1124 0.038 Uiso 1 1 calc R . . C18 C -0.0006(2) 0.0090(3) -0.2589(5) 0.0277(10) Uani 1 1 d . . . C19 C 0.00320(19) 0.0883(3) -0.3323(5) 0.0302(10) Uani 1 1 d . . . H19 H -0.0271 0.1126 -0.3965 0.036 Uiso 1 1 calc R . . C20 C 0.05194(19) 0.1310(3) -0.3094(5) 0.0261(10) Uani 1 1 d . . . H20 H 0.0552 0.1852 -0.3566 0.031 Uiso 1 1 calc R . . C21 C 0.38678(18) 0.3570(3) 0.3140(4) 0.0221(9) Uani 1 1 d . . . H21 H 0.3963 0.3704 0.2031 0.027 Uiso 1 1 calc R . . C22 C 0.38616(18) 0.3512(3) 0.5909(4) 0.0201(9) Uani 1 1 d . . . H22 H 0.3951 0.3596 0.7098 0.024 Uiso 1 1 calc R . . C23 C 0.50011(19) 0.4298(3) 0.6116(5) 0.0307(11) Uani 1 1 d . . . H23 H 0.5003 0.3825 0.6847 0.037 Uiso 1 1 calc R . . C24 C 0.45802(19) 0.4429(3) 0.4824(4) 0.0245(10) Uani 1 1 d . . . C25 C 0.4583(2) 0.5114(3) 0.3711(5) 0.0334(11) Uani 1 1 d . . . H25 H 0.4298 0.5179 0.2828 0.040 Uiso 1 1 calc R . . N16 N 0.0837(3) -0.2354(3) 0.0445(6) 0.0626(15) Uani 1 1 d . . . O1 O 0.0338(2) -0.2307(3) 0.0014(6) 0.0789(15) Uani 1 1 d . . . O2 O 0.1065(3) -0.3051(4) 0.0652(7) 0.0927(18) Uani 1 1 d . . . O3 O 0.1107(2) -0.1684(3) 0.0693(6) 0.0887(17) Uani 1 1 d . . . N17 N 0.4108(4) -0.0946(6) 0.2556(9) 0.101(2) Uiso 1 1 d . . . O4 O 0.3806(3) -0.0375(5) 0.2044(7) 0.1043(18) Uiso 1 1 d . . . O5 O 0.4437(3) -0.0854(5) 0.4022(8) 0.123(2) Uiso 1 1 d . . . O6 O 0.4097(3) -0.1606(6) 0.1805(8) 0.128(2) Uiso 1 1 d . . . O7A O 0.4289(3) 0.4064(4) -0.0304(6) 0.0459(15) Uiso 0.67 1 d P . . O7B O 0.4130(5) 0.4463(9) -0.0492(13) 0.051(3) Uiso 0.33 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0118(2) 0.00982(19) 0.01127(16) 0.00072(18) 0.00364(11) 0.0025(2) N1 0.022(2) 0.0141(17) 0.0136(13) 0.0019(11) 0.0044(12) -0.0008(16) N2 0.021(2) 0.0121(16) 0.0126(13) -0.0017(11) 0.0048(12) -0.0034(15) N3 0.027(2) 0.0100(15) 0.0215(13) 0.0003(13) 0.0039(12) -0.0016(17) N4 0.072(4) 0.018(2) 0.064(3) -0.0021(19) 0.023(2) -0.004(2) N5 0.088(4) 0.014(2) 0.0287(17) -0.0004(17) 0.017(2) 0.003(3) N6 0.050(3) 0.0128(18) 0.0322(17) -0.0017(14) 0.0123(16) -0.0028(19) N7 0.020(2) 0.0255(19) 0.0139(13) -0.0007(12) 0.0058(12) -0.0070(17) N8 0.0162(19) 0.0182(18) 0.0147(13) 0.0001(12) 0.0056(12) -0.0008(15) N9 0.0139(19) 0.0168(17) 0.0219(15) -0.0028(12) 0.0047(12) -0.0067(16) N10 0.028(3) 0.059(3) 0.046(2) -0.013(2) 0.0082(17) -0.013(3) N11 0.037(3) 0.062(3) 0.0320(19) -0.0070(19) 0.0119(17) -0.032(3) N12 0.022(2) 0.037(2) 0.0281(16) -0.0019(15) 0.0071(14) -0.0124(19) N13 0.020(2) 0.0208(18) 0.0152(13) -0.0004(12) 0.0039(12) -0.0049(16) N14 0.0172(19) 0.0191(18) 0.0140(13) 0.0016(11) 0.0049(12) -0.0040(16) N15 0.022(2) 0.028(2) 0.0172(14) -0.0018(13) 0.0049(12) -0.0196(17) C1 0.025(2) 0.013(2) 0.0201(17) -0.0024(14) 0.0058(15) -0.0015(19) C2 0.024(2) 0.013(2) 0.0192(16) 0.0008(14) 0.0028(14) 0.0002(18) C3 0.056(4) 0.024(3) 0.063(3) -0.005(2) 0.019(3) -0.007(3) C4 0.073(5) 0.020(3) 0.030(2) 0.0038(18) 0.007(2) 0.009(3) C5 0.032(3) 0.0088(19) 0.0249(17) 0.0005(15) 0.0100(17) 0.0017(19) C6 0.040(3) 0.019(2) 0.032(2) -0.0015(17) 0.0039(19) -0.002(2) C7 0.050(4) 0.016(2) 0.033(2) 0.0048(17) 0.005(2) 0.006(2) C8 0.044(3) 0.0108(18) 0.0279(16) 0.0012(19) 0.0152(15) -0.004(3) C9 0.039(3) 0.023(2) 0.035(2) -0.0037(18) 0.0065(19) -0.008(2) C10 0.034(3) 0.018(2) 0.031(2) 0.0006(17) 0.0035(18) -0.001(2) C11 0.024(3) 0.029(2) 0.0173(17) 0.0019(15) 0.0053(15) -0.010(2) C12 0.021(2) 0.024(2) 0.0165(16) 0.0019(14) 0.0028(14) -0.0082(19) C13 0.025(3) 0.052(4) 0.051(3) -0.011(2) 0.008(2) -0.014(3) C14 0.039(4) 0.041(3) 0.041(2) 0.007(2) 0.006(2) -0.015(3) C15 0.014(2) 0.025(2) 0.0241(17) -0.0024(15) 0.0068(14) -0.007(2) C16 0.017(3) 0.027(3) 0.035(2) 0.0038(18) 0.0003(17) -0.004(2) C17 0.030(3) 0.030(3) 0.036(2) 0.0067(19) 0.0034(19) -0.012(2) C18 0.020(2) 0.037(3) 0.0274(17) -0.0057(17) 0.0079(15) -0.014(2) C19 0.019(3) 0.037(3) 0.035(2) 0.0028(18) -0.0008(17) -0.003(2) C20 0.026(3) 0.021(2) 0.032(2) 0.0050(17) 0.0036(17) -0.004(2) C21 0.021(2) 0.026(2) 0.0207(17) -0.0007(15) 0.0064(15) -0.010(2) C22 0.020(2) 0.021(2) 0.0195(17) -0.0023(15) 0.0037(15) -0.0109(19) C23 0.029(3) 0.035(3) 0.0278(19) 0.0085(17) -0.0006(17) -0.019(2) C24 0.025(3) 0.029(2) 0.0210(17) -0.0055(16) 0.0081(15) -0.015(2) C25 0.030(3) 0.041(3) 0.029(2) 0.0061(18) -0.0016(17) -0.019(2) N16 0.071(4) 0.048(4) 0.063(3) 0.001(2) -0.020(2) -0.001(3) O1 0.061(4) 0.064(4) 0.107(3) -0.009(2) -0.020(3) -0.005(3) O2 0.100(5) 0.059(3) 0.111(4) -0.002(3) -0.030(3) 0.013(3) O3 0.085(4) 0.058(3) 0.112(3) 0.019(3) -0.045(3) -0.023(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 N14 2.008(3) 4_565 ? Cu1 N8 2.019(3) 4_566 ? Cu1 N1 2.063(3) . ? Cu1 N2 2.066(3) 4_565 ? Cu1 N13 2.291(3) . ? Cu1 N7 2.325(3) . ? N1 C1 1.304(5) . ? N1 N2 1.389(3) . ? N2 C2 1.291(5) . ? N2 Cu1 2.066(3) 4_566 ? N3 C1 1.350(5) . ? N3 C2 1.354(5) . ? N3 C5 1.435(5) . ? N4 C3 1.317(7) . ? N4 N5 1.366(7) . ? N5 C4 1.302(7) . ? N6 C4 1.333(6) . ? N6 C3 1.353(7) . ? N6 C8 1.444(6) . ? N7 C11 1.298(5) . ? N7 N8 1.381(4) . ? N8 C12 1.299(5) . ? N8 Cu1 2.019(3) 4_565 ? N9 C11 1.351(5) . ? N9 C12 1.354(5) . ? N9 C15 1.441(5) . ? N10 C13 1.308(7) . ? N10 N11 1.371(7) . ? N11 C14 1.322(7) . ? N12 C13 1.354(7) . ? N12 C14 1.356(7) . ? N12 C18 1.430(6) . ? N13 C21 1.307(5) . ? N13 N14 1.389(4) . ? N14 C22 1.294(5) . ? N14 Cu1 2.008(3) 4_566 ? N15 C22 1.360(5) . ? N15 C21 1.362(5) . ? N15 C24 1.422(5) . ? C1 H1 0.9400 . ? C2 H2 0.9400 . ? C3 H3 0.9400 . ? C4 H4 0.9400 . ? C5 C10 1.372(6) . ? C5 C6 1.386(6) . ? C6 C7 1.397(6) . ? C6 H6 0.9400 . ? C7 C8 1.387(7) . ? C7 H7 0.9400 . ? C8 C9 1.370(7) . ? C9 C10 1.378(6) . ? C9 H9 0.9400 . ? C10 H10 0.9400 . ? C11 H11 0.9400 . ? C12 H12 0.9400 . ? C13 H13 0.9400 . ? C14 H14 0.9400 . ? C15 C16 1.378(6) . ? C15 C20 1.389(6) . ? C16 C17 1.381(6) . ? C16 H16 0.9400 . ? C17 C18 1.384(7) . ? C17 H17 0.9400 . ? C18 C19 1.388(7) . ? C19 C20 1.375(6) . ? C19 H19 0.9400 . ? C20 H20 0.9400 . ? C21 H21 0.9400 . ? C22 H22 0.9400 . ? C23 C25 1.384(6) 3_666 ? C23 C24 1.390(6) . ? C23 H23 0.9400 . ? C24 C25 1.390(6) . ? C25 C23 1.384(6) 3_666 ? C25 H25 0.9400 . ? N16 O2 1.243(7) . ? N16 O1 1.246(7) . ? N16 O3 1.258(7) . ? N17 O6 1.198(9) . ? N17 O4 1.216(9) . ? N17 O5 1.342(9) . ? O7A O7B 0.751(13) . ? 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 N14 Cu1 N8 178.16(14) 4_565 4_566 ? N14 Cu1 N1 90.06(13) 4_565 . ? N8 Cu1 N1 89.15(13) 4_566 . ? N14 Cu1 N2 91.84(12) 4_565 4_565 ? N8 Cu1 N2 88.93(12) 4_566 4_565 ? N1 Cu1 N2 177.98(15) . 4_565 ? N14 Cu1 N13 91.46(13) 4_565 . ? N8 Cu1 N13 90.16(12) 4_566 . ? N1 Cu1 N13 87.47(12) . . ? N2 Cu1 N13 93.18(12) 4_565 . ? N14 Cu1 N7 88.44(12) 4_565 . ? N8 Cu1 N7 89.94(13) 4_566 . ? N1 Cu1 N7 92.78(12) . . ? N2 Cu1 N7 86.57(12) 4_565 . ? N13 Cu1 N7 179.73(13) . . ? C1 N1 N2 106.9(3) . . ? C1 N1 Cu1 126.0(2) . . ? N2 N1 Cu1 127.0(2) . . ? C2 N2 N1 107.0(3) . . ? C2 N2 Cu1 125.3(2) . 4_566 ? N1 N2 Cu1 127.4(2) . 4_566 ? C1 N3 C2 105.1(3) . . ? C1 N3 C5 126.9(3) . . ? C2 N3 C5 128.0(3) . . ? C3 N4 N5 106.1(5) . . ? C4 N5 N4 107.4(5) . . ? C4 N6 C3 104.2(4) . . ? C4 N6 C8 128.8(4) . . ? C3 N6 C8 127.1(4) . . ? C11 N7 N8 105.9(3) . . ? C11 N7 Cu1 126.1(2) . . ? N8 N7 Cu1 127.1(2) . . ? C12 N8 N7 108.0(3) . . ? C12 N8 Cu1 129.5(2) . 4_565 ? N7 N8 Cu1 122.4(2) . 4_565 ? C11 N9 C12 104.5(4) . . ? C11 N9 C15 127.0(3) . . ? C12 N9 C15 128.4(3) . . ? C13 N10 N11 107.0(5) . . ? C14 N11 N10 107.4(4) . . ? C13 N12 C14 105.0(4) . . ? C13 N12 C18 128.1(5) . . ? C14 N12 C18 126.9(5) . . ? C21 N13 N14 106.5(3) . . ? C21 N13 Cu1 124.7(2) . . ? N14 N13 Cu1 128.6(2) . . ? C22 N14 N13 107.8(3) . . ? C22 N14 Cu1 129.5(2) . 4_566 ? N13 N14 Cu1 122.1(2) . 4_566 ? C22 N15 C21 104.9(3) . . ? C22 N15 C24 127.9(3) . . ? C21 N15 C24 127.1(3) . . ? N1 C1 N3 110.2(3) . . ? N1 C1 H1 124.9 . . ? N3 C1 H1 124.9 . . ? N2 C2 N3 110.7(3) . . ? N2 C2 H2 124.6 . . ? N3 C2 H2 124.6 . . ? N4 C3 N6 110.9(6) . . ? N4 C3 H3 124.5 . . ? N6 C3 H3 124.6 . . ? N5 C4 N6 111.5(5) . . ? N5 C4 H4 124.3 . . ? N6 C4 H4 124.3 . . ? C10 C5 C6 121.4(4) . . ? C10 C5 N3 119.8(4) . . ? C6 C5 N3 118.8(4) . . ? C5 C6 C7 118.8(5) . . ? C5 C6 H6 120.6 . . ? C7 C6 H6 120.6 . . ? C8 C7 C6 118.8(5) . . ? C8 C7 H7 120.6 . . ? C6 C7 H7 120.6 . . ? C9 C8 C7 121.9(4) . . ? C9 C8 N6 119.5(4) . . ? C7 C8 N6 118.6(4) . . ? C8 C9 C10 119.0(5) . . ? C8 C9 H9 120.5 . . ? C10 C9 H9 120.5 . . ? C5 C10 C9 120.1(5) . . ? C5 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? N7 C11 N9 111.5(3) . . ? N7 C11 H11 124.2 . . ? N9 C11 H11 124.2 . . ? N8 C12 N9 110.1(3) . . ? N8 C12 H12 125.0 . . ? N9 C12 H12 125.0 . . ? N10 C13 N12 110.7(5) . . ? N10 C13 H13 124.6 . . ? N12 C13 H13 124.6 . . ? N11 C14 N12 109.7(5) . . ? N11 C14 H14 125.1 . . ? N12 C14 H14 125.1 . . ? C16 C15 C20 121.6(4) . . ? C16 C15 N9 118.5(4) . . ? C20 C15 N9 119.9(4) . . ? C15 C16 C17 119.1(4) . . ? C15 C16 H16 120.5 . . ? C17 C16 H16 120.5 . . ? C16 C17 C18 119.4(4) . . ? C16 C17 H17 120.3 . . ? C18 C17 H17 120.3 . . ? C17 C18 C19 121.5(5) . . ? C17 C18 N12 119.4(4) . . ? C19 C18 N12 119.1(5) . . ? C20 C19 C18 119.0(4) . . ? C20 C19 H19 120.5 . . ? C18 C19 H19 120.5 . . ? C19 C20 C15 119.5(4) . . ? C19 C20 H20 120.3 . . ? C15 C20 H20 120.3 . . ? N13 C21 N15 110.4(3) . . ? N13 C21 H21 124.8 . . ? N15 C21 H21 124.8 . . ? N14 C22 N15 110.3(3) . . ? N14 C22 H22 124.8 . . ? N15 C22 H22 124.8 . . ? C25 C23 C24 117.8(4) 3_666 . ? C25 C23 H23 121.1 3_666 . ? C24 C23 H23 121.1 . . ? C23 C24 C25 121.3(4) . . ? C23 C24 N15 119.6(4) . . ? C25 C24 N15 119.1(4) . . ? C23 C25 C24 120.9(4) 3_666 . ? C23 C25 H25 119.6 3_666 . ? C24 C25 H25 119.6 . . ? O2 N16 O1 120.7(6) . . ? O2 N16 O3 120.3(6) . . ? O1 N16 O3 119.0(6) . . ? O6 N17 O4 120.4(8) . . ? O6 N17 O5 119.6(9) . . ? O4 N17 O5 120.0(8) . . ? 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 N14 Cu1 N1 C1 -52.0(4) 4_565 . . . ? N8 Cu1 N1 C1 126.3(4) 4_566 . . . ? N13 Cu1 N1 C1 -143.5(4) . . . . ? N7 Cu1 N1 C1 36.4(4) . . . . ? N14 Cu1 N1 N2 127.2(3) 4_565 . . . ? N8 Cu1 N1 N2 -54.5(3) 4_566 . . . ? N13 Cu1 N1 N2 35.7(3) . . . . ? N7 Cu1 N1 N2 -144.4(3) . . . . ? C1 N1 N2 C2 -0.1(4) . . . . ? Cu1 N1 N2 C2 -179.4(3) . . . . ? C1 N1 N2 Cu1 -174.0(3) . . . 4_566 ? Cu1 N1 N2 Cu1 6.7(4) . . . 4_566 ? C3 N4 N5 C4 0.5(5) . . . . ? N14 Cu1 N7 C11 135.0(4) 4_565 . . . ? N8 Cu1 N7 C11 -44.2(4) 4_566 . . . ? N1 Cu1 N7 C11 45.0(4) . . . . ? N2 Cu1 N7 C11 -133.1(4) 4_565 . . . ? N14 Cu1 N7 N8 -57.3(3) 4_565 . . . ? N8 Cu1 N7 N8 123.6(3) 4_566 . . . ? N1 Cu1 N7 N8 -147.3(3) . . . . ? N2 Cu1 N7 N8 34.7(3) 4_565 . . . ? C11 N7 N8 C12 0.5(4) . . . . ? Cu1 N7 N8 C12 -169.3(3) . . . . ? C11 N7 N8 Cu1 -177.1(3) . . . 4_565 ? Cu1 N7 N8 Cu1 13.1(4) . . . 4_565 ? C13 N10 N11 C14 0.5(5) . . . . ? N14 Cu1 N13 C21 55.6(4) 4_565 . . . ? N8 Cu1 N13 C21 -125.3(4) 4_566 . . . ? N1 Cu1 N13 C21 145.6(4) . . . . ? N2 Cu1 N13 C21 -36.3(4) 4_565 . . . ? N14 Cu1 N13 N14 -128.5(3) 4_565 . . . ? N8 Cu1 N13 N14 50.7(3) 4_566 . . . ? N1 Cu1 N13 N14 -38.5(3) . . . . ? N2 Cu1 N13 N14 139.6(3) 4_565 . . . ? C21 N13 N14 C22 -0.2(4) . . . . ? Cu1 N13 N14 C22 -176.7(3) . . . . ? C21 N13 N14 Cu1 171.9(3) . . . 4_566 ? Cu1 N13 N14 Cu1 -4.7(4) . . . 4_566 ? N2 N1 C1 N3 0.4(4) . . . . ? Cu1 N1 C1 N3 179.7(3) . . . . ? C2 N3 C1 N1 -0.5(5) . . . . ? C5 N3 C1 N1 177.6(4) . . . . ? N1 N2 C2 N3 -0.2(4) . . . . ? Cu1 N2 C2 N3 173.8(3) 4_566 . . . ? C1 N3 C2 N2 0.4(5) . . . . ? C5 N3 C2 N2 -177.7(4) . . . . ? N5 N4 C3 N6 -0.5(5) . . . . ? C4 N6 C3 N4 0.4(5) . . . . ? C8 N6 C3 N4 179.7(4) . . . . ? N4 N5 C4 N6 -0.3(5) . . . . ? C3 N6 C4 N5 -0.1(5) . . . . ? C8 N6 C4 N5 -179.3(3) . . . . ? C1 N3 C5 C10 -52.7(6) . . . . ? C2 N3 C5 C10 125.0(5) . . . . ? C1 N3 C5 C6 125.5(4) . . . . ? C2 N3 C5 C6 -56.8(6) . . . . ? C10 C5 C6 C7 -0.7(6) . . . . ? N3 C5 C6 C7 -178.8(4) . . . . ? C5 C6 C7 C8 0.9(6) . . . . ? C6 C7 C8 C9 -0.7(6) . . . . ? C6 C7 C8 N6 177.1(4) . . . . ? C4 N6 C8 C9 163.4(4) . . . . ? C3 N6 C8 C9 -15.7(6) . . . . ? C4 N6 C8 C7 -14.4(6) . . . . ? C3 N6 C8 C7 166.5(4) . . . . ? C7 C8 C9 C10 0.2(6) . . . . ? N6 C8 C9 C10 -177.5(4) . . . . ? C6 C5 C10 C9 0.2(6) . . . . ? N3 C5 C10 C9 178.3(4) . . . . ? C8 C9 C10 C5 0.0(6) . . . . ? N8 N7 C11 N9 -0.9(5) . . . . ? Cu1 N7 C11 N9 168.9(3) . . . . ? C12 N9 C11 N7 1.0(5) . . . . ? C15 N9 C11 N7 177.6(4) . . . . ? N7 N8 C12 N9 0.2(5) . . . . ? Cu1 N8 C12 N9 177.5(3) 4_565 . . . ? C11 N9 C12 N8 -0.7(5) . . . . ? C15 N9 C12 N8 -177.2(4) . . . . ? N11 N10 C13 N12 -1.4(5) . . . . ? C14 N12 C13 N10 1.7(5) . . . . ? C18 N12 C13 N10 -179.6(4) . . . . ? N10 N11 C14 N12 0.6(5) . . . . ? C13 N12 C14 N11 -1.4(5) . . . . ? C18 N12 C14 N11 179.9(4) . . . . ? C11 N9 C15 C16 -51.3(6) . . . . ? C12 N9 C15 C16 124.5(4) . . . . ? C11 N9 C15 C20 128.7(4) . . . . ? C12 N9 C15 C20 -55.5(6) . . . . ? C20 C15 C16 C17 0.4(6) . . . . ? N9 C15 C16 C17 -179.6(3) . . . . ? C15 C16 C17 C18 0.9(6) . . . . ? C16 C17 C18 C19 -1.3(6) . . . . ? C16 C17 C18 N12 179.7(4) . . . . ? C13 N12 C18 C17 160.0(4) . . . . ? C14 N12 C18 C17 -21.6(6) . . . . ? C13 N12 C18 C19 -19.0(6) . . . . ? C14 N12 C18 C19 159.4(4) . . . . ? C17 C18 C19 C20 0.3(6) . . . . ? N12 C18 C19 C20 179.3(4) . . . . ? C18 C19 C20 C15 1.0(6) . . . . ? C16 C15 C20 C19 -1.4(6) . . . . ? N9 C15 C20 C19 178.6(4) . . . . ? N14 N13 C21 N15 0.3(5) . . . . ? Cu1 N13 C21 N15 177.0(3) . . . . ? C22 N15 C21 N13 -0.2(5) . . . . ? C24 N15 C21 N13 -176.6(4) . . . . ? N13 N14 C22 N15 0.1(5) . . . . ? Cu1 N14 C22 N15 -171.2(3) 4_566 . . . ? C21 N15 C22 N14 0.1(5) . . . . ? C24 N15 C22 N14 176.4(4) . . . . ? C25 C23 C24 C25 1.7(8) 3_666 . . . ? C25 C23 C24 N15 -177.8(4) 3_666 . . . ? C22 N15 C24 C23 43.4(7) . . . . ? C21 N15 C24 C23 -141.1(4) . . . . ? C22 N15 C24 C25 -136.2(5) . . . . ? C21 N15 C24 C25 39.4(7) . . . . ? C23 C24 C25 C23 -1.8(8) . . . 3_666 ? N15 C24 C25 C23 177.8(4) . . . 3_666 ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.207 _refine_diff_density_min -0.418 _refine_diff_density_rms 0.085 #----------------------------------------------------# data_(3) _database_code_depnum_ccdc_archive 'CCDC 674755' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Copper(II) Chloride 1:2 Complex with 1,4-bi(1,2,4-triazol-4-yl)benzene, Dodecahydrate ; _chemical_name_common ; Copper(ii) Chloride 1:2 Complex with 1,4-bi(1,2,4-triazol-4- yl)benzene, Dodecahydrate ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H40 Cl2 Cu N12 O12' _chemical_formula_weight 775.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Cmcm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y, -z-1/2' 'x, -y, z-1/2' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, -z-1/2' 'x+1/2, -y+1/2, z-1/2' '-x+1/2, y+1/2, z' _cell_length_a 28.331(3) _cell_length_b 16.1470(12) _cell_length_c 7.1760(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3282.7(6) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 3.60 _cell_measurement_theta_max 27.88 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.22 _exptl_crystal_density_diffrn 1.568 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1612 _exptl_absorpt_coefficient_mu 0.904 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.7990 _exptl_absorpt_correction_T_max 0.8260 _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 13976 _diffrn_reflns_av_R_equivalents 0.0745 _diffrn_reflns_av_sigmaI/netI 0.0497 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.60 _diffrn_reflns_theta_max 27.88 _reflns_number_total 2114 _reflns_number_gt 1653 _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)' #------------------------------- Refinement data-----------------------# _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. The structure was solved by direct methods. The 1,4-phenylene and non-coordinated triazole groups of the ligand are equally disordered over two closely separated orientations related by a mirror plane. They were refined anisotropically and with minor restraints in geometry. In particular, FLAT restraint was applied for the atoms of non-coordinated triazoel group. The hydrogen atoms were added geometrically and included as fixed contributions with U~iso~(H) = 1.2U~eq~ (parent carbon atoms). Since the ratio of Cu to non-coordinated chloride anion is 1:1 and the copper atom occupies site position 4a, the position of chloride anion is only partially occupied. This anion appears also disordered over two closely separated positions (which correspond to weak CH...Cl hydrogen bonding with CH groups of disordered 1,4-phenylene linkage). Two oxygen atoms of disordered solvate molecules were located from the map (the hydrogen atoms were not added). The remaining water molecules are badly disordered (corresponding voids in the structure over 200 A^3) and they were not included. Number of the solvate water molecules, which was included in molecular weight calculation, was based upon elemental analysis and solvent mass loss from DTA studies. ; _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^)+(0.0650P)^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 2114 _refine_ls_number_parameters 140 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0471 _refine_ls_R_factor_gt 0.0370 _refine_ls_wR_factor_ref 0.0990 _refine_ls_wR_factor_gt 0.0968 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.0000 0.0000 0.5000 0.01712(14) Uani 1 4 d S . . Cl1 Cl 0.0000 0.12312(6) 0.2500 0.0283(2) Uani 1 4 d S . . N1 N 0.04992(5) 0.05646(9) 0.6544(2) 0.0206(3) Uani 1 1 d . . . N2 N 0.10990(7) 0.12802(14) 0.7500 0.0258(5) Uani 1 2 d S . . N3 N 0.32434(14) 0.4257(3) 0.7845(8) 0.0518(18) Uani 0.50 1 d PD . . N4 N 0.34999(9) 0.3556(2) 0.7500 0.0481(8) Uani 1 2 d SD . . N5 N 0.27609(9) 0.31863(17) 0.7500 0.0388(6) Uani 1 2 d SD . . C1 C 0.08604(6) 0.10004(12) 0.5994(3) 0.0273(4) Uani 1 1 d . . . H1 H 0.0942 0.1104 0.4746 0.033 Uiso 1 1 calc R . . C2 C 0.27991(17) 0.4027(3) 0.7848(6) 0.070(2) Uani 0.50 1 d PD . . H2 H 0.2541 0.4406 0.8205 0.084 Uiso 0.50 1 d P . . C3 C 0.32091(13) 0.2926(3) 0.7292(2) 0.0368(8) Uani 0.50 1 d PD . . H3 H 0.3315 0.2356 0.6898 0.044 Uiso 0.50 1 d P . . C4 C 0.15275(9) 0.17738(18) 0.7500 0.0283(6) Uani 1 2 d S . . C5 C 0.19456(12) 0.1391(2) 0.7162(12) 0.035(2) Uani 0.50 1 d P . . H5 H 0.1962 0.0794 0.6981 0.041 Uiso 0.50 1 d P . . C6 C 0.23566(13) 0.1861(3) 0.7130(8) 0.0355(19) Uani 0.50 1 d P . . H6 H 0.2656 0.1599 0.6839 0.043 Uiso 0.50 1 d P . . C7 C 0.23364(10) 0.27012(19) 0.7500 0.0331(6) Uani 1 2 d S . . C8 C 0.19147(15) 0.3074(3) 0.7855(19) 0.052(4) Uani 0.50 1 d P . . H8 H 0.1906 0.3653 0.8083 0.062 Uiso 0.50 1 d P . . C9 C 0.15012(13) 0.2609(3) 0.7876(10) 0.043(2) Uani 0.50 1 d P . . H9 H 0.1200 0.2864 0.8146 0.052 Uiso 0.50 1 d P . . Cl2A Cl 0.1959(4) 0.5000 1.0000 0.139(3) Uiso 0.25 2 d SPU . . Cl2B Cl 0.1801(4) 0.4663(6) 1.1059(17) 0.102(2) Uiso 0.125 1 d PU . . O1A O 0.1439(9) 0.4008(16) 1.2500 0.133(7) Uiso 0.25 2 d SP . . O1B O 0.1676(10) 0.4454(17) 1.2500 0.134(7) Uiso 0.25 2 d SP . . O2A O 0.0571(7) 0.2766(11) 1.041(3) 0.142(6) Uiso 0.25 1 d P . . O2B O 0.0308(6) 0.2567(10) 0.917(3) 0.129(5) Uiso 0.25 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.00824(18) 0.0279(2) 0.0153(2) -0.00441(17) 0.000 0.000 Cl1 0.0323(4) 0.0296(4) 0.0229(5) 0.000 0.000 0.000 N1 0.0149(6) 0.0319(7) 0.0149(8) -0.0017(6) 0.0002(5) -0.0052(5) N2 0.0177(9) 0.0386(12) 0.0212(12) 0.000 0.000 -0.0117(9) N3 0.0418(17) 0.060(2) 0.053(6) 0.000(2) -0.002(2) -0.0286(16) N4 0.0319(14) 0.081(2) 0.0315(15) 0.000 0.000 -0.0327(14) N5 0.0261(12) 0.0463(14) 0.0440(16) 0.000 0.000 -0.0177(10) C1 0.0206(8) 0.0435(10) 0.0179(10) -0.0008(8) 0.0020(7) -0.0118(7) C2 0.041(2) 0.051(2) 0.117(7) 0.004(4) -0.005(4) -0.0257(18) C3 0.0263(14) 0.068(2) 0.016(2) 0.000(3) -0.002(2) -0.0185(14) C4 0.0180(11) 0.0420(15) 0.0249(14) 0.000 0.000 -0.0146(10) C5 0.0246(15) 0.0374(17) 0.042(7) 0.0005(19) -0.0025(18) -0.0086(13) C6 0.0204(14) 0.0456(19) 0.040(6) 0.0007(19) -0.0008(16) -0.0067(14) C7 0.0213(12) 0.0437(15) 0.0342(16) 0.000 0.000 -0.0153(11) C8 0.0346(18) 0.0394(18) 0.081(12) -0.016(3) 0.012(3) -0.0167(15) C9 0.0246(15) 0.050(2) 0.055(8) -0.013(3) 0.009(2) -0.0101(14) _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 2.0146(14) 9_556 ? Cu1 N1 2.0146(14) 12 ? Cu1 N1 2.0146(14) . ? Cu1 N1 2.0146(14) 4_556 ? Cu1 Cl1 2.6778(7) . ? Cu1 Cl1 2.6778(7) 9_556 ? Cl1 Cu1 2.6778(7) 2_554 ? N1 C1 1.303(2) . ? N1 N1 1.372(3) 10_557 ? N2 C1 1.353(2) . ? N2 C1 1.353(2) 10_557 ? N2 C4 1.452(3) . ? N3 C2 1.312(6) . ? N3 N4 1.367(6) . ? N3 C2 1.403(6) 10_557 ? N4 C3 1.318(5) . ? N4 C3 1.318(5) 10_557 ? N4 N3 1.367(6) 10_557 ? N5 C3 1.346(5) 10_557 ? N5 C3 1.346(5) . ? N5 C2 1.385(6) . ? N5 C7 1.435(3) . ? C1 H1 0.9400 . ? C2 N3 1.403(6) 10_557 ? C2 H2 0.9867 . ? C3 H3 1.0071 . ? C4 C5 1.358(5) 10_557 ? C4 C5 1.358(5) . ? C4 C9 1.378(6) . ? C4 C9 1.378(6) 10_557 ? C5 C6 1.390(5) . ? C5 C6 1.480(6) 10_557 ? C5 H5 0.9737 . ? C6 C7 1.384(5) . ? C6 C5 1.480(6) 10_557 ? C6 H6 0.9693 . ? C7 C8 1.362(6) . ? C7 C8 1.362(6) 10_557 ? C7 C6 1.384(5) 10_557 ? C8 C9 1.392(5) . ? C8 C9 1.487(7) 10_557 ? C8 H8 0.9488 . ? C9 H9 0.9668 . ? 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 90.83(8) 9_556 12 ? N1 Cu1 N1 180.00(9) 9_556 . ? N1 Cu1 N1 89.17(8) 12 . ? N1 Cu1 N1 89.17(8) 9_556 4_556 ? N1 Cu1 N1 180.00(6) 12 4_556 ? N1 Cu1 N1 90.83(8) . 4_556 ? N1 Cu1 Cl1 88.14(4) 9_556 . ? N1 Cu1 Cl1 91.86(4) 12 . ? N1 Cu1 Cl1 91.86(4) . . ? N1 Cu1 Cl1 88.14(4) 4_556 . ? N1 Cu1 Cl1 91.86(4) 9_556 9_556 ? N1 Cu1 Cl1 88.14(4) 12 9_556 ? N1 Cu1 Cl1 88.14(4) . 9_556 ? N1 Cu1 Cl1 91.86(4) 4_556 9_556 ? Cl1 Cu1 Cl1 180.00(3) . 9_556 ? Cu1 Cl1 Cu1 84.13(3) 2_554 . ? C1 N1 N1 107.64(11) . 10_557 ? C1 N1 Cu1 128.98(13) . . ? N1 N1 Cu1 123.36(4) 10_557 . ? C1 N2 C4 126.95(10) . . ? C2 N3 N4 106.1(4) . . ? C3 N4 N3 109.1(3) . . ? C3 N5 C2 104.7(3) . . ? C3 N5 C7 128.3(3) . . ? C2 N5 C7 126.9(3) . . ? N1 C1 N2 109.32(17) . . ? N1 C1 H1 125.3 . . ? N2 C1 H1 125.3 . . ? N3 C2 N5 110.6(5) . . ? N3 C2 H2 122.4 . . ? N5 C2 H2 126.7 . . ? N4 C3 N5 109.6(4) . . ? N4 C3 H3 123.4 . . ? N5 C3 H3 126.7 . . ? C5 C4 C9 121.9(3) . . ? C5 C4 N2 118.6(3) . . ? C9 C4 N2 119.5(3) . . ? C4 C5 C6 119.0(3) . . ? C4 C5 H5 121.0 . . ? C6 C5 H5 119.9 . . ? C7 C6 C5 119.8(4) . . ? C7 C6 H6 120.4 . . ? C5 C6 H6 119.8 . . ? C8 C7 C6 120.4(3) . . ? C8 C7 N5 119.6(3) . . ? C6 C7 N5 120.0(3) . . ? C7 C8 C9 120.1(4) . . ? C7 C8 H8 119.5 . . ? C9 C8 H8 120.4 . . ? C4 C9 C8 118.7(4) . . ? C4 C9 H9 120.3 . . ? C8 C9 H9 121.0 . . ? 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 N1 Cu1 Cl1 Cu1 -44.62(4) 9_556 . . 2_554 ? N1 Cu1 Cl1 Cu1 -135.38(4) 12 . . 2_554 ? N1 Cu1 Cl1 Cu1 135.38(4) . . . 2_554 ? N1 Cu1 Cl1 Cu1 44.62(4) 4_556 . . 2_554 ? N1 Cu1 N1 C1 -128.37(15) 12 . . . ? N1 Cu1 N1 C1 51.63(15) 4_556 . . . ? Cl1 Cu1 N1 C1 -36.54(16) . . . . ? Cl1 Cu1 N1 C1 143.46(16) 9_556 . . . ? C2 N3 N4 C3 0.4(3) . . . . ? Cu1 N1 C1 N2 178.65(14) . . . . ? C4 N2 C1 N1 178.6(2) . . . . ? N4 N3 C2 N5 -0.3(3) . . . . ? C3 N5 C2 N3 0.12(16) . . . . ? C7 N5 C2 N3 176.1(2) . . . . ? N3 N4 C3 N5 -0.4(2) . . . . ? C2 N5 C3 N4 0.15(14) . . . . ? C7 N5 C3 N4 -175.80(7) . . . . ? C1 N2 C4 C5 -77.9(5) . . . . ? C1 N2 C4 C9 103.4(4) . . . . ? C9 C4 C5 C6 -2.3(9) . . . . ? N2 C4 C5 C6 179.0(5) . . . . ? C4 C5 C6 C7 2.1(9) . . . . ? C5 C6 C7 C8 -1.5(9) . . . . ? C5 C6 C7 N5 178.9(5) . . . . ? C3 N5 C7 C8 175.7(7) . . . . ? C2 N5 C7 C8 0.6(7) . . . . ? C3 N5 C7 C6 -4.7(3) . . . . ? C2 N5 C7 C6 -179.8(4) . . . . ? C6 C7 C8 C9 1.0(14) . . . . ? N5 C7 C8 C9 -179.4(7) . . . . ? C5 C4 C9 C8 1.9(10) . . . . ? N2 C4 C9 C8 -179.5(7) . . . . ? C7 C8 C9 C4 -1.2(15) . . . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.550 _refine_diff_density_min -0.398 _refine_diff_density_rms 0.073 #----------------------------------------------------# data_(4) _database_code_depnum_ccdc_archive 'CCDC 674756' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Copper(II) Bromide 1:2 Complex with 1,4-bi(1,2,4-triazol-4-yl)benzene, Dodecahydrate ; _chemical_name_common ; Copper(ii) Bromide 1:2 Complex with 1,4-bi(1,2,4-triazol-4- yl)benzene, Dodecahydrate ; _chemical_melting_point ? _chemical_formula_moiety '(C20 H16 Br Cu N12), Br, 12(H2 O)' _chemical_formula_sum 'C20 H40 Br2 Cu N12 O12' _chemical_formula_weight 864.00 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Cmcm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y, -z-1/2' 'x, -y, z-1/2' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, -z-1/2' 'x+1/2, -y+1/2, z-1/2' '-x+1/2, y+1/2, z' _cell_length_a 28.449(3) _cell_length_b 15.7732(17) _cell_length_c 7.2593(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3257.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 6978 _cell_measurement_theta_min 3.82 _cell_measurement_theta_max 26.72 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.762 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1756 _exptl_absorpt_coefficient_mu 3.200 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.5866 _exptl_absorpt_correction_T_max 0.7203 _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 6978 _diffrn_reflns_av_R_equivalents 0.0807 _diffrn_reflns_av_sigmaI/netI 0.0949 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 3.82 _diffrn_reflns_theta_max 26.72 _reflns_number_total 1874 _reflns_number_gt 1197 _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)' #------------------------------- Refinement data-----------------------# _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. The structure was solved by direct methods. The 1,4-phenylene and non-coordinated triazole groups of the ligand are equally disordered over two closely separated orientations related by a mirror plane. They were refined anisotropically and with minor restraints in geometry. In particular, FLAT restraint was applied for the atoms of non-coordinated triazole group and SIMU restraints were used for atoms of each of the carbo- and heterocyle. The hydrogen atoms were added geometrically and included as fixed contributions with U~iso~(H) = 1.2U~eq~ (parent carbon atoms). Since the ratio of Cu to non-coordinated bromide anion is 1:1 and the copper atom occupies site position 4a, the position of the bromide anion is only partially occupied. This anion appears also disordered over two closely separated positions (which correspond to weak CH...Br hydrogen bonding with CH groups of disordered 1,4-phenylene linkage). The non-coordinated Br atom was left isotropic. It was possible to locate only part of oxygen atoms of disordered solvate molecules (the hydrogen atoms were not added). The remaining water molecules are badly disordered and this electron density was modelled using SQUEEZE routine as implemented in PLATON. ; _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^)+(0.1292P)^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 SHELXL _refine_ls_extinction_coef 0.011(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1874 _refine_ls_number_parameters 138 _refine_ls_number_restraints 71 _refine_ls_R_factor_all 0.0963 _refine_ls_R_factor_gt 0.0740 _refine_ls_wR_factor_ref 0.1989 _refine_ls_wR_factor_gt 0.1876 _refine_ls_goodness_of_fit_ref 0.969 _refine_ls_restrained_S_all 0.960 _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 0.0000 0.5000 0.5000 0.0296(5) Uani 1 4 d S . . Br1 Br 0.0000 0.36333(6) 0.2500 0.0397(5) Uani 1 4 d S . . N1 N 0.05000(13) 0.4435(3) 0.6574(7) 0.0342(11) Uani 1 1 d . . . N2 N 0.10990(19) 0.3709(4) 0.7500 0.0363(16) Uani 1 2 d S . . N3 N 0.3509(2) 0.1440(6) 0.7500 0.0530(19) Uani 1 2 d SDU . . N4 N 0.3258(3) 0.0730(6) 0.7932(15) 0.052(3) Uani 0.50 1 d PDU . . N5 N 0.2768(2) 0.1792(5) 0.7500 0.0451(17) Uani 1 2 d SDU . . C1 C 0.08609(15) 0.3992(4) 0.5992(10) 0.0389(14) Uani 1 1 d . . . H1 H 0.0941 0.3885 0.4711 0.047 Uiso 1 1 d . . . C2 C 0.3215(3) 0.2066(7) 0.7247(11) 0.045(2) Uani 0.50 1 d PDU . . H2 H 0.3310 0.2652 0.7089 0.054 Uiso 0.50 1 d P . . C3 C 0.2819(4) 0.0941(8) 0.7936(15) 0.054(3) Uani 0.50 1 d PDU . . H3 H 0.2571 0.0544 0.7990 0.065 Uiso 0.50 1 d P . . C4 C 0.1529(2) 0.3222(5) 0.7500 0.0404(19) Uani 1 2 d SDU . . C5 C 0.1508(3) 0.2360(8) 0.6966(11) 0.050(3) Uani 0.50 1 d PDU . . H5 H 0.1211 0.2095 0.6635 0.060 Uiso 0.50 1 d P . . C6 C 0.1923(3) 0.1891(7) 0.6958(12) 0.051(3) Uani 0.50 1 d PDU . . H6 H 0.1910 0.1292 0.6630 0.062 Uiso 0.50 1 d P . . C7 C 0.2343(2) 0.2294(6) 0.7500 0.045(2) Uani 1 2 d SDU . . C8 C 0.2350(3) 0.3119(7) 0.7974(13) 0.041(3) Uani 0.50 1 d PDU . . H8 H 0.2636 0.3379 0.8319 0.050 Uiso 0.50 1 d P . . C9 C 0.1938(3) 0.3596(6) 0.7981(12) 0.039(3) Uani 0.50 1 d PDU . . H9 H 0.1949 0.4175 0.8327 0.047 Uiso 0.50 1 d P . . Br2A Br 0.1759(3) 0.0408(6) 1.0564(17) 0.084(2) Uiso 0.125 1 d P . . Br2B Br 0.1671(4) 0.0505(7) 1.1646(19) 0.104(3) Uiso 0.125 1 d P . . O1 O 0.1970(9) 0.0000 1.0000 0.106(7) Uiso 0.50 2 d SP . . O2 O 0.0312(11) 0.231(2) 0.610(6) 0.111(9) Uiso 0.25 1 d P . . O3 O 0.1449(12) 0.092(3) 1.2500 0.153(10) Uiso 0.50 2 d SP . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0142(5) 0.0248(6) 0.0498(10) 0.0036(5) 0.000 0.000 Br1 0.0346(6) 0.0256(6) 0.0589(9) 0.000 0.000 0.000 N1 0.0202(15) 0.029(2) 0.054(3) 0.002(2) 0.0011(16) 0.0052(14) N2 0.028(3) 0.032(3) 0.049(5) 0.000 0.000 0.009(2) N3 0.036(3) 0.061(4) 0.062(5) 0.000 0.000 0.021(3) N4 0.040(3) 0.047(4) 0.068(8) -0.002(4) 0.002(4) 0.026(3) N5 0.033(3) 0.041(4) 0.062(5) 0.000 0.000 0.020(2) C1 0.027(2) 0.037(3) 0.053(4) -0.001(3) 0.004(2) 0.008(2) C2 0.027(3) 0.057(5) 0.052(6) -0.004(6) 0.001(5) 0.021(3) C3 0.043(4) 0.045(5) 0.073(9) -0.002(5) 0.004(5) 0.017(4) C4 0.024(3) 0.034(4) 0.063(5) 0.000 0.000 0.010(3) C5 0.031(3) 0.048(5) 0.072(8) -0.008(5) -0.012(4) 0.013(4) C6 0.039(4) 0.043(5) 0.073(8) -0.013(5) -0.004(4) 0.011(4) C7 0.028(3) 0.043(4) 0.065(6) 0.000 0.000 0.017(3) C8 0.023(3) 0.037(4) 0.064(8) 0.003(4) 0.001(4) 0.004(3) C9 0.028(3) 0.030(4) 0.060(8) 0.002(4) 0.004(4) 0.005(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 2.031(4) . ? Cu1 N1 2.031(4) 9_566 ? Cu1 N1 2.031(4) 4_566 ? Cu1 N1 2.031(4) 12 ? Cu1 Br1 2.8179(8) 9_566 ? Cu1 Br1 2.8179(8) . ? Br1 Cu1 2.8179(8) 2_564 ? N1 C1 1.311(6) . ? N1 N1 1.345(10) 10_557 ? N2 C1 1.363(7) . ? N2 C1 1.363(7) 10_557 ? N2 C4 1.444(8) . ? N3 C2 1.308(11) 10_557 ? N3 C2 1.308(11) . ? N3 N4 1.364(13) 10_557 ? N3 N4 1.364(13) . ? N4 C3 1.293(12) . ? N4 C3 1.439(14) 10_557 ? N5 C2 1.356(12) . ? N5 C2 1.356(12) 10_557 ? N5 C3 1.387(14) 10_557 ? N5 C3 1.387(14) . ? N5 C7 1.444(8) . ? C1 H1 0.9722 . ? C2 H2 0.9689 . ? C3 N4 1.439(14) 10_557 ? C3 H3 0.9431 . ? C4 C9 1.349(12) 10_557 ? C4 C9 1.349(12) . ? C4 C5 1.415(14) . ? C5 C6 1.394(13) . ? C5 C6 1.598(14) 10_557 ? C5 H5 0.9730 . ? C6 C7 1.410(14) . ? C6 H6 0.9750 . ? C7 C8 1.345(14) . ? C8 C9 1.395(12) . ? C8 H8 0.9445 . ? C9 H9 0.9488 . ? 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 180.00(14) . 9_566 ? N1 Cu1 N1 91.1(2) . 4_566 ? N1 Cu1 N1 88.9(2) 9_566 4_566 ? N1 Cu1 N1 88.9(2) . 12 ? N1 Cu1 N1 91.1(2) 9_566 12 ? N1 Cu1 N1 180.0(2) 4_566 12 ? N1 Cu1 Br1 88.49(13) . 9_566 ? N1 Cu1 Br1 91.51(13) 9_566 9_566 ? N1 Cu1 Br1 91.51(13) 4_566 9_566 ? N1 Cu1 Br1 88.49(13) 12 9_566 ? N1 Cu1 Br1 91.51(13) . . ? N1 Cu1 Br1 88.49(13) 9_566 . ? N1 Cu1 Br1 88.49(13) 4_566 . ? N1 Cu1 Br1 91.51(13) 12 . ? Br1 Cu1 Br1 180.0 9_566 . ? Cu1 Br1 Cu1 80.19(3) . 2_564 ? C1 N1 N1 108.8(4) . 10_557 ? C1 N1 Cu1 126.9(4) . . ? C1 N2 C4 126.5(3) . . ? C2 N3 N4 108.4(7) . . ? C3 N4 N3 107.2(9) . . ? C2 N5 C3 103.9(7) . . ? C2 N5 C7 127.6(8) . . ? C3 N5 C7 128.2(7) . . ? N1 C1 N2 107.8(5) . . ? N1 C1 H1 125.7 . . ? N2 C1 H1 126.5 . . ? N3 C2 N5 110.0(9) . . ? N3 C2 H2 123.8 . . ? N5 C2 H2 125.6 . . ? N4 C3 N5 110.5(10) . . ? N4 C3 H3 123.5 . . ? N5 C3 H3 125.0 . . ? C9 C4 C5 121.8(7) . . ? C9 C4 N2 119.8(7) . . ? C5 C4 N2 118.3(6) . . ? C6 C5 C4 118.4(9) . . ? C6 C5 H5 120.4 . . ? C4 C5 H5 121.2 . . ? C5 C6 C7 118.5(10) . . ? C5 C6 H6 118.9 . . ? C7 C6 H6 122.5 . . ? C8 C7 C6 121.4(7) . . ? C8 C7 N5 121.1(7) . . ? C6 C7 N5 117.5(8) . . ? C7 C8 C9 120.6(8) . . ? C7 C8 H8 120.2 . . ? C9 C8 H8 119.2 . . ? C4 C9 C8 119.2(9) . . ? C4 C9 H9 121.2 . . ? C8 C9 H9 119.5 . . ? 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 -135.52(12) . . . 2_564 ? N1 Cu1 Br1 Cu1 44.48(12) 9_566 . . 2_564 ? N1 Cu1 Br1 Cu1 -44.48(12) 4_566 . . 2_564 ? N1 Cu1 Br1 Cu1 135.52(12) 12 . . 2_564 ? N1 Cu1 N1 C1 -50.6(4) 4_566 . . . ? N1 Cu1 N1 C1 129.4(4) 12 . . . ? Br1 Cu1 N1 C1 -142.1(4) 9_566 . . . ? Br1 Cu1 N1 C1 37.9(4) . . . . ? C2 N3 N4 C3 -0.2(3) . . . . ? Cu1 N1 C1 N2 -178.3(4) . . . . ? C4 N2 C1 N1 -177.6(6) . . . . ? N4 N3 C2 N5 0.0(2) . . . . ? C3 N5 C2 N3 0.2(3) . . . . ? C7 N5 C2 N3 174.5(2) . . . . ? N3 N4 C3 N5 0.3(3) . . . . ? C2 N5 C3 N4 -0.3(3) . . . . ? C7 N5 C3 N4 -174.5(3) . . . . ? C1 N2 C4 C9 106.4(7) . . . . ? C1 N2 C4 C5 -72.9(8) . . . . ? C9 C4 C5 C6 0.5(3) . . . . ? N2 C4 C5 C6 179.7(2) . . . . ? C4 C5 C6 C7 0.7(3) . . . . ? C5 C6 C7 C8 -1.7(6) . . . . ? C5 C6 C7 N5 179.3(3) . . . . ? C2 N5 C7 C8 -27.2(6) . . . . ? C3 N5 C7 C8 145.7(8) . . . . ? C2 N5 C7 C6 151.8(6) . . . . ? C3 N5 C7 C6 -35.2(7) . . . . ? C6 C7 C8 C9 1.5(8) . . . . ? N5 C7 C8 C9 -179.6(4) . . . . ? C5 C4 C9 C8 -0.8(6) . . . . ? N2 C4 C9 C8 -180.0(4) . . . . ? C7 C8 C9 C4 -0.2(8) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 26.72 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.142 _refine_diff_density_min -1.430 _refine_diff_density_rms 0.144 #----------------------------------------------------# data_(5) _database_code_depnum_ccdc_archive 'CCDC 674757' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Dihydroxo Tetracopper(II) Triflate Complex with 1,4-bi(1,2,4-triazol-4-yl)benzene, Dodecahydrate ; _chemical_name_common ; Dihydroxo Tetracopper(ii) Triflate Complex with 1,4-bi(1,2,4- triazol-4-yl)benzene, Dodecahydrate ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H66 Cu4 F18 N30 O32 S6' _chemical_formula_weight 2459.91 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' 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.3427(11) _cell_length_b 13.4047(12) _cell_length_c 13.5620(12) _cell_angle_alpha 102.339(2) _cell_angle_beta 104.3690(10) _cell_angle_gamma 90.4770(10) _cell_volume 2290.6(3) _cell_formula_units_Z 1 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 9518 _cell_measurement_theta_min 3.11 _cell_measurement_theta_max 26.73 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.14 _exptl_crystal_density_diffrn 1.783 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1242 _exptl_absorpt_coefficient_mu 1.185 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8422 _exptl_absorpt_correction_T_max 0.8516 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'Siemens SMART CCD area-detector diffractometer' _diffrn_measurement_method '\w scans' _diffrn_standards_decay_% 0 _diffrn_reflns_number 19454 _diffrn_reflns_av_R_equivalents 0.0281 _diffrn_reflns_av_sigmaI/netI 0.0458 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 26.73 _reflns_number_total 9518 _reflns_number_gt 7046 _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)' #------------------------------- Refinement data-----------------------# _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. The structure was solved by direct methods. All CH hydrogen atoms were located from difference maps and then refined as riding, with C---H distances constrained to 0.94 \%A, and with U~iso~(H) = 1.2U~eq~ (parent carbon atoms). OH hydrogen atoms (for coordinated hydroxyl and aqua ligands) were located from the map and then fixed with U~iso~(H) = 1.5U~eq~ (parent oxygen atom). One of three unique triflate anions is equally disordered over two positions, in such a way that carbon and two oxygen atoms are common for both contributions of the disorder (these three atoms have occupancies 1.0) and sulfure, three fluorine and one oxygen atoms have partial occupancies 0.5. The disorder was refined without any restraints in geometry and thermal values. One of five unique solvate water molecules is disordered over two closely situated positions. All water oxygen atoms were refined anisotropically. The hydrogen atoms were located only for one of these molecules, and the H atoms were added as fixed contributions with U~iso~(H) = 1.5U~eq~ (parent oxygen atom). Hydrogen atoms of remaining four solvate water molecules were not added. ; _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^)+(0.0252P)^2^+12.9571P] 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 9518 _refine_ls_number_parameters 715 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0828 _refine_ls_R_factor_gt 0.0657 _refine_ls_wR_factor_ref 0.1449 _refine_ls_wR_factor_gt 0.1404 _refine_ls_goodness_of_fit_ref 1.163 _refine_ls_restrained_S_all 1.163 _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 -0.5000 0.5000 0.5000 0.0190(2) Uani 1 2 d S . . Cu2 Cu -0.25871(4) 0.57282(5) 0.52392(5) 0.01457(15) Uani 1 1 d . . . Cu3 Cu 0.0000 0.5000 0.5000 0.01424(19) Uani 1 2 d S . . O1 O -0.3546(3) 0.4775(3) 0.5456(3) 0.0255(9) Uani 1 1 d . . . H1O H -0.3373 0.4641 0.6065 0.038 Uiso 1 1 d . . . O2 O -0.1558(3) 0.4234(3) 0.3818(4) 0.0445(12) Uani 1 1 d . . . H2A H -0.1835 0.3824 0.4096 0.067 Uiso 1 1 d . . . H2B H -0.1419 0.3867 0.3275 0.067 Uiso 1 1 d . . . N1 N -0.4621(3) 0.5258(4) 0.3733(3) 0.0218(10) Uani 1 1 d . . . N2 N -0.3611(3) 0.5596(3) 0.3824(3) 0.0204(9) Uani 1 1 d . . . N3 N -0.4463(3) 0.5308(4) 0.2186(3) 0.0252(10) Uani 1 1 d . . . N4 N -0.4356(4) 0.6836(5) 0.5884(4) 0.0478(16) Uani 1 1 d . . . N5 N -0.3295(3) 0.7025(4) 0.6094(4) 0.0274(11) Uani 1 1 d . . . N6 N -0.3887(4) 0.8244(4) 0.7102(4) 0.0371(13) Uani 1 1 d . . . N7 N -0.5006(4) 1.2758(4) 1.1190(4) 0.0385(13) Uani 1 1 d . . . N8 N -0.4017(5) 1.2689(5) 1.1763(5) 0.0576(18) Uani 1 1 d . . . N9 N -0.4280(4) 1.1574(4) 1.0261(4) 0.0334(12) Uani 1 1 d . . . N10 N -0.1554(3) 0.6632(3) 0.4903(3) 0.0154(8) Uani 1 1 d . . . N11 N -0.0562(3) 0.6362(3) 0.4904(3) 0.0171(9) Uani 1 1 d . . . N12 N -0.0645(3) 0.7980(3) 0.4882(3) 0.0178(9) Uani 1 1 d . . . N13 N 0.0552(3) 0.5012(3) 0.3731(3) 0.0166(9) Uani 1 1 d . . . N14 N 0.1457(3) 0.4579(3) 0.3583(3) 0.0160(8) Uani 1 1 d . . . N15 N 0.0601(3) 0.4895(3) 0.2112(3) 0.0174(9) Uani 1 1 d . . . C1 C -0.5105(4) 0.5083(5) 0.2737(4) 0.0252(12) Uani 1 1 d . . . H1 H -0.5801 0.4835 0.2453 0.030 Uiso 1 1 calc R . . C2 C -0.3539(4) 0.5618(5) 0.2888(4) 0.0256(12) Uani 1 1 d . . . H2 H -0.2935 0.5819 0.2723 0.031 Uiso 1 1 calc R . . C3 C -0.5689(4) 0.5437(5) 0.0564(4) 0.0343(14) Uani 1 1 d . . . H3 H -0.6147 0.5733 0.0952 0.041 Uiso 1 1 calc R . . C4 C -0.4724(4) 0.5168(5) 0.1066(4) 0.0273(13) Uani 1 1 d . . . C5 C -0.4031(4) 0.4737(5) 0.0514(4) 0.0326(14) Uani 1 1 d . . . H5 H -0.3379 0.4564 0.0867 0.039 Uiso 1 1 calc R . . C6 C -0.4683(5) 0.7565(7) 0.6491(6) 0.063(3) Uani 1 1 d . . . H6 H -0.5380 0.7622 0.6510 0.076 Uiso 1 1 calc R . . C7 C -0.3034(4) 0.7863(4) 0.6826(5) 0.0292(13) Uani 1 1 d . . . H7 H -0.2354 0.8156 0.7118 0.035 Uiso 1 1 calc R . . C8 C -0.5134(5) 1.2110(5) 1.0310(5) 0.0351(14) Uani 1 1 d . . . H8 H -0.5744 1.2019 0.9767 0.042 Uiso 1 1 calc R . . C9 C -0.3607(6) 1.1981(7) 1.1195(6) 0.068(3) Uani 1 1 d . . . H9 H -0.2929 1.1778 1.1406 0.081 Uiso 1 1 calc R . . C10 C -0.3955(5) 0.9132(5) 0.7883(5) 0.0364(15) Uani 1 1 d . . . C11 C -0.3195(4) 0.9371(5) 0.8815(5) 0.0321(13) Uani 1 1 d . . . H11 H -0.2613 0.8978 0.8920 0.039 Uiso 1 1 calc R . . C12 C -0.3294(5) 1.0189(5) 0.9587(5) 0.0343(14) Uani 1 1 d . . . H12 H -0.2772 1.0363 1.0215 0.041 Uiso 1 1 calc R . . C13 C -0.4158(5) 1.0752(5) 0.9443(5) 0.0345(14) Uani 1 1 d . . . C14 C -0.4910(6) 1.0508(7) 0.8520(6) 0.075(3) Uani 1 1 d . . . H14 H -0.5499 1.0891 0.8421 0.090 Uiso 1 1 calc R . . C15 C -0.4805(7) 0.9701(7) 0.7733(6) 0.078(3) Uani 1 1 d . . . H15 H -0.5317 0.9543 0.7096 0.094 Uiso 1 1 calc R . . C16 C -0.1591(4) 0.7596(4) 0.4890(4) 0.0176(10) Uani 1 1 d . . . H16 H -0.2182 0.7973 0.4886 0.021 Uiso 1 1 calc R . . C17 C -0.0027(4) 0.7178(4) 0.4895(4) 0.0185(10) Uani 1 1 d . . . H17 H 0.0677 0.7207 0.4896 0.022 Uiso 1 1 calc R . . C18 C -0.0737(4) 0.9801(4) 0.5517(5) 0.0284(13) Uani 1 1 d . . . H18 H -0.1232 0.9662 0.5865 0.034 Uiso 1 1 calc R . . C19 C -0.0323(4) 0.9014(4) 0.4935(4) 0.0217(11) Uani 1 1 d . . . C20 C 0.0405(4) 0.9194(4) 0.4424(5) 0.0283(13) Uani 1 1 d . . . H20 H 0.0678 0.8644 0.4038 0.034 Uiso 1 1 calc R . . C21 C 0.0058(4) 0.5205(4) 0.2838(4) 0.0204(11) Uani 1 1 d . . . H21 H -0.0579 0.5513 0.2715 0.024 Uiso 1 1 calc R . . C22 C 0.1465(4) 0.4509(4) 0.2613(4) 0.0176(10) Uani 1 1 d . . . H22 H 0.1991 0.4234 0.2308 0.021 Uiso 1 1 calc R . . C23 C -0.0705(4) 0.4658(5) 0.0467(5) 0.0349(14) Uani 1 1 d . . . H23 H -0.1184 0.4424 0.0785 0.042 Uiso 1 1 calc R . . C24 C 0.0289(4) 0.4948(4) 0.1020(4) 0.0198(11) Uani 1 1 d . . . C25 C 0.1004(5) 0.5287(5) 0.0579(4) 0.0347(15) Uani 1 1 d . . . H25 H 0.1689 0.5481 0.0977 0.042 Uiso 1 1 calc R . . S1 S -0.21536(12) 0.72414(13) 0.16743(13) 0.0384(4) Uani 1 1 d . . . O3 O -0.3097(4) 0.7679(5) 0.1785(5) 0.0755(18) Uani 1 1 d . . . O4 O -0.2252(6) 0.6529(5) 0.0686(5) 0.081(2) Uani 1 1 d . . . O5 O -0.1585(4) 0.6867(4) 0.2556(4) 0.0458(12) Uani 1 1 d . . . C26 C -0.1330(7) 0.8283(8) 0.1586(7) 0.063(2) Uani 1 1 d . . . F1 F -0.1749(5) 0.8661(4) 0.0774(4) 0.0875(18) Uani 1 1 d . . . F2 F -0.0417(4) 0.8039(7) 0.1566(6) 0.126(3) Uani 1 1 d . . . F3 F -0.1250(6) 0.9033(5) 0.2437(5) 0.109(2) Uani 1 1 d . . . S2 S -0.04491(13) 1.20302(13) 1.21574(13) 0.0370(4) Uani 1 1 d . . . O6 O 0.0503(4) 1.2069(5) 1.2918(4) 0.0724(18) Uani 1 1 d . . . O7 O -0.0869(5) 1.3017(4) 1.2106(5) 0.0658(16) Uani 1 1 d . . . O8 O -0.1225(4) 1.1258(5) 1.2089(5) 0.0718(17) Uani 1 1 d . . . C27 C -0.0069(7) 1.1668(7) 1.0923(6) 0.061(2) Uani 1 1 d . . . F4 F 0.0418(6) 1.0842(5) 1.0906(5) 0.119(3) Uani 1 1 d . . . F5 F 0.0587(6) 1.2375(6) 1.0871(5) 0.112(2) Uani 1 1 d . . . F6 F -0.0871(5) 1.1519(6) 1.0130(4) 0.114(2) Uani 1 1 d . . . S3A S -0.7377(2) 0.7262(2) 0.3290(3) 0.0353(7) Uani 0.50 1 d P . . S3B S -0.6520(3) 0.7232(3) 0.3041(3) 0.0408(8) Uani 0.50 1 d P . . O9 O -0.7019(4) 0.6269(4) 0.2773(4) 0.0567(14) Uani 1 1 d . . . O10 O -0.6510(6) 0.7735(6) 0.4162(5) 0.104(3) Uani 1 1 d . . . O11B O -0.5659(9) 0.7401(9) 0.2643(10) 0.070(3) Uani 0.50 1 d P . . O11A O -0.8432(9) 0.7145(8) 0.3378(11) 0.066(3) Uani 0.50 1 d P . . C28 C -0.7481(8) 0.8035(9) 0.2395(11) 0.082(3) Uani 1 1 d . . . F7A F -0.6530(11) 0.8239(12) 0.2224(12) 0.116(5) Uani 0.50 1 d P . . F7B F -0.8419(9) 0.7763(13) 0.2680(16) 0.134(6) Uani 0.50 1 d P . . F8A F -0.807(3) 0.759(3) 0.146(3) 0.126(13) Uani 0.50 1 d P . . F8B F -0.766(4) 0.778(4) 0.143(4) 0.168(19) Uani 0.50 1 d P . . F9A F -0.779(2) 0.8963(19) 0.265(2) 0.129(9) Uani 0.50 1 d P . . F9B F -0.725(2) 0.893(2) 0.279(3) 0.190(15) Uani 0.50 1 d P . . O1W O 0.3024(3) 0.3495(4) 0.1419(3) 0.0461(12) Uani 1 1 d . . . H1W H 0.3628 0.3279 0.1424 0.069 Uiso 1 1 d . . . H2W H 0.2727 0.3512 0.0788 0.069 Uiso 1 1 d . . . O2W O -0.3128(5) 0.8988(5) 0.3799(5) 0.0756(18) Uani 1 1 d . . . O3W O -0.7480(6) 0.9154(6) 0.6597(7) 0.106(3) Uani 1 1 d . . . O4WA O -0.6983(7) 0.6898(8) 0.6065(8) 0.048(2) Uani 0.50 1 d P . . O4WB O -0.7578(7) 0.7388(8) 0.5477(9) 0.051(3) Uani 0.50 1 d P . . O5W O -0.4634(8) 0.9053(8) 0.4847(8) 0.149(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 0.0159(4) 0.0286(5) 0.0137(5) 0.0072(4) 0.0040(3) -0.0009(3) Cu2 0.0145(3) 0.0172(3) 0.0125(3) 0.0055(2) 0.0026(2) -0.0005(2) Cu3 0.0180(4) 0.0136(4) 0.0133(4) 0.0046(3) 0.0066(3) 0.0030(3) O1 0.0177(18) 0.040(2) 0.023(2) 0.0212(18) 0.0018(15) -0.0042(15) O2 0.039(3) 0.033(3) 0.050(3) 0.002(2) -0.006(2) 0.0055(19) N1 0.016(2) 0.033(3) 0.016(2) 0.006(2) 0.0026(16) -0.0044(18) N2 0.016(2) 0.030(3) 0.014(2) 0.0050(19) 0.0021(16) -0.0058(17) N3 0.022(2) 0.041(3) 0.012(2) 0.005(2) 0.0033(17) -0.0021(19) N4 0.021(3) 0.071(4) 0.034(3) -0.018(3) -0.001(2) 0.011(3) N5 0.024(2) 0.030(3) 0.027(3) 0.002(2) 0.0080(19) 0.0070(19) N6 0.030(3) 0.049(3) 0.022(3) -0.007(2) 0.002(2) 0.015(2) N7 0.039(3) 0.036(3) 0.035(3) -0.006(2) 0.011(2) 0.011(2) N8 0.052(4) 0.069(4) 0.033(3) -0.016(3) 0.000(3) 0.021(3) N9 0.032(3) 0.039(3) 0.024(3) -0.002(2) 0.004(2) 0.011(2) N10 0.0146(19) 0.017(2) 0.014(2) 0.0038(17) 0.0030(15) -0.0001(15) N11 0.019(2) 0.016(2) 0.016(2) 0.0046(18) 0.0040(16) 0.0002(16) N12 0.021(2) 0.011(2) 0.023(2) 0.0061(18) 0.0058(17) -0.0008(16) N13 0.0158(19) 0.023(2) 0.013(2) 0.0053(18) 0.0048(16) 0.0042(16) N14 0.019(2) 0.016(2) 0.013(2) 0.0032(17) 0.0049(16) 0.0029(16) N15 0.022(2) 0.021(2) 0.010(2) 0.0051(17) 0.0048(16) 0.0017(17) C1 0.014(2) 0.044(4) 0.017(3) 0.006(2) 0.0015(19) -0.004(2) C2 0.020(3) 0.044(4) 0.013(3) 0.008(2) 0.004(2) -0.002(2) C3 0.026(3) 0.062(4) 0.016(3) 0.008(3) 0.009(2) -0.001(3) C4 0.027(3) 0.044(4) 0.010(3) 0.009(2) 0.001(2) -0.008(2) C5 0.022(3) 0.062(4) 0.015(3) 0.014(3) 0.003(2) 0.000(3) C6 0.027(3) 0.103(7) 0.036(4) -0.022(4) -0.002(3) 0.025(4) C7 0.029(3) 0.030(3) 0.029(3) 0.004(3) 0.009(2) 0.010(2) C8 0.032(3) 0.038(4) 0.032(4) 0.001(3) 0.006(3) 0.012(3) C9 0.042(4) 0.098(7) 0.040(4) -0.018(4) -0.003(3) 0.037(4) C10 0.034(3) 0.049(4) 0.025(3) 0.000(3) 0.010(2) 0.016(3) C11 0.029(3) 0.033(3) 0.032(3) 0.005(3) 0.006(2) 0.009(2) C12 0.033(3) 0.037(4) 0.024(3) -0.003(3) 0.000(2) 0.008(3) C13 0.037(3) 0.040(4) 0.024(3) 0.000(3) 0.010(3) 0.015(3) C14 0.062(5) 0.097(7) 0.038(4) -0.018(4) -0.010(4) 0.061(5) C15 0.074(6) 0.099(7) 0.028(4) -0.026(4) -0.015(4) 0.060(5) C16 0.015(2) 0.021(3) 0.018(3) 0.007(2) 0.0021(18) 0.0018(19) C17 0.021(2) 0.015(3) 0.022(3) 0.007(2) 0.008(2) 0.0031(19) C18 0.033(3) 0.022(3) 0.038(3) 0.012(3) 0.018(3) -0.001(2) C19 0.027(3) 0.016(3) 0.022(3) 0.010(2) 0.003(2) -0.001(2) C20 0.036(3) 0.013(3) 0.040(4) 0.005(2) 0.019(3) 0.003(2) C21 0.024(3) 0.022(3) 0.015(3) 0.006(2) 0.004(2) 0.007(2) C22 0.018(2) 0.020(3) 0.016(3) 0.005(2) 0.0057(19) 0.0021(19) C23 0.028(3) 0.057(4) 0.025(3) 0.020(3) 0.006(2) -0.001(3) C24 0.024(3) 0.024(3) 0.013(3) 0.008(2) 0.004(2) 0.005(2) C25 0.025(3) 0.061(4) 0.018(3) 0.016(3) 0.001(2) -0.006(3) S1 0.0352(8) 0.0448(10) 0.0383(10) 0.0205(8) 0.0054(7) 0.0053(7) O3 0.053(3) 0.104(5) 0.085(5) 0.048(4) 0.022(3) 0.032(3) O4 0.113(5) 0.067(4) 0.047(4) -0.001(3) 0.000(3) 0.004(4) O5 0.048(3) 0.057(3) 0.043(3) 0.029(2) 0.016(2) 0.013(2) C26 0.061(5) 0.081(7) 0.048(5) 0.034(5) 0.000(4) -0.008(4) F1 0.108(4) 0.093(4) 0.071(4) 0.061(3) 0.004(3) -0.013(3) F2 0.050(3) 0.218(8) 0.156(6) 0.123(6) 0.040(4) 0.007(4) F3 0.148(6) 0.068(4) 0.081(4) 0.016(3) -0.026(4) -0.032(4) S2 0.0407(9) 0.0383(9) 0.0298(9) 0.0037(7) 0.0085(7) -0.0081(7) O6 0.060(4) 0.108(5) 0.036(3) 0.010(3) -0.005(3) -0.009(3) O7 0.092(4) 0.044(3) 0.072(4) 0.011(3) 0.042(3) 0.009(3) O8 0.058(4) 0.065(4) 0.103(5) 0.039(4) 0.023(3) -0.007(3) C27 0.062(5) 0.070(6) 0.038(5) -0.008(4) 0.006(4) 0.005(4) F4 0.122(5) 0.107(5) 0.098(5) -0.033(4) 0.021(4) 0.052(4) F5 0.138(6) 0.130(6) 0.087(4) 0.009(4) 0.075(4) -0.023(5) F6 0.097(5) 0.177(7) 0.036(3) -0.009(4) -0.012(3) 0.019(4) S3A 0.0387(17) 0.0290(17) 0.0442(19) 0.0161(14) 0.0146(14) 0.0015(13) S3B 0.0450(19) 0.042(2) 0.040(2) 0.0173(16) 0.0137(15) 0.0025(15) O9 0.047(3) 0.054(3) 0.072(4) 0.026(3) 0.010(3) 0.003(2) O10 0.124(6) 0.121(6) 0.053(4) 0.015(4) 0.002(4) -0.053(5) O11B 0.064(7) 0.064(8) 0.102(10) 0.026(7) 0.051(7) 0.002(6) O11A 0.061(7) 0.039(6) 0.117(10) 0.020(7) 0.057(7) 0.009(5) C28 0.072(7) 0.075(8) 0.111(10) 0.051(7) 0.019(6) 0.022(6) F7A 0.119(11) 0.147(13) 0.129(12) 0.098(10) 0.065(10) -0.005(10) F7B 0.050(7) 0.143(13) 0.22(2) 0.058(13) 0.039(9) 0.042(8) F8A 0.17(3) 0.097(14) 0.084(17) 0.048(12) -0.038(17) 0.004(17) F8B 0.17(3) 0.22(4) 0.12(2) 0.14(2) -0.04(2) -0.03(2) F9A 0.19(3) 0.066(11) 0.162(17) 0.076(11) 0.067(17) 0.068(15) F9B 0.15(2) 0.058(11) 0.39(4) 0.112(17) 0.06(2) 0.058(15) O1W 0.033(2) 0.066(3) 0.034(3) -0.004(2) 0.0109(19) 0.018(2) O2W 0.071(4) 0.077(4) 0.078(4) 0.030(3) 0.007(3) 0.022(3) O3W 0.076(5) 0.099(6) 0.167(8) 0.080(6) 0.031(5) 0.017(4) O4WA 0.042(5) 0.049(6) 0.050(6) -0.007(5) 0.018(5) -0.006(4) O4WB 0.035(5) 0.059(7) 0.070(7) 0.028(6) 0.021(5) 0.003(5) O5W 0.159(9) 0.119(7) 0.166(9) -0.009(7) 0.074(7) -0.054(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.932(3) 2_466 ? Cu1 O1 1.932(3) . ? Cu1 N1 2.003(4) . ? Cu1 N1 2.003(4) 2_466 ? Cu2 O1 1.918(4) . ? Cu2 N14 2.022(4) 2_566 ? Cu2 N10 2.024(4) . ? Cu2 N2 2.033(4) . ? Cu2 N5 2.230(4) . ? Cu3 N11 1.998(4) 2_566 ? Cu3 N11 1.998(4) . ? Cu3 N13 2.036(4) 2_566 ? Cu3 N13 2.036(4) . ? Cu3 O2 2.356(4) 2_566 ? Cu3 O2 2.356(4) . ? O1 H1O 0.8585 . ? O2 H2A 0.8574 . ? O2 H2B 0.8571 . ? N1 C1 1.313(7) . ? N1 N2 1.385(5) . ? N2 C2 1.303(7) . ? N3 C1 1.340(7) . ? N3 C2 1.356(7) . ? N3 C4 1.441(7) . ? N4 C6 1.290(8) . ? N4 N5 1.382(7) . ? N5 C7 1.309(7) . ? N6 C7 1.355(7) . ? N6 C6 1.367(9) . ? N6 C10 1.434(8) . ? N7 C8 1.289(8) . ? N7 N8 1.370(8) . ? N8 C9 1.303(9) . ? N9 C9 1.356(9) . ? N9 C8 1.360(7) . ? N9 C13 1.429(7) . ? N10 C16 1.296(6) . ? N10 N11 1.375(5) . ? N11 C17 1.305(6) . ? N12 C17 1.360(6) . ? N12 C16 1.363(6) . ? N12 C19 1.429(6) . ? N13 C21 1.308(6) . ? N13 N14 1.385(5) . ? N14 C22 1.302(6) . ? N14 Cu2 2.022(4) 2_566 ? N15 C22 1.353(6) . ? N15 C21 1.361(6) . ? N15 C24 1.452(6) . ? C1 H1 0.9400 . ? C2 H2 0.9400 . ? C3 C5 1.384(8) 2_465 ? C3 C4 1.389(8) . ? C3 H3 0.9400 . ? C4 C5 1.385(8) . ? C5 C3 1.384(8) 2_465 ? C5 H5 0.9400 . ? C6 H6 0.9400 . ? C7 H7 0.9400 . ? C8 H8 0.9400 . ? C9 H9 0.9400 . ? C10 C15 1.369(9) . ? C10 C11 1.384(8) . ? C11 C12 1.377(8) . ? C11 H11 0.9400 . ? C12 C13 1.380(8) . ? C12 H12 0.9400 . ? C13 C14 1.370(9) . ? C14 C15 1.383(10) . ? C14 H14 0.9400 . ? C15 H15 0.9400 . ? C16 H16 0.9400 . ? C17 H17 0.9400 . ? C18 C19 1.383(8) . ? C18 C20 1.395(8) 2_576 ? C18 H18 0.9400 . ? C19 C20 1.372(8) . ? C20 C18 1.395(8) 2_576 ? C20 H20 0.9400 . ? C21 H21 0.9400 . ? C22 H22 0.9400 . ? C23 C24 1.358(8) . ? C23 C25 1.394(8) 2_565 ? C23 H23 0.9400 . ? C24 C25 1.367(7) . ? C25 C23 1.394(8) 2_565 ? C25 H25 0.9400 . ? S1 O3 1.420(6) . ? S1 O5 1.439(5) . ? S1 O4 1.445(6) . ? S1 C26 1.812(9) . ? C26 F2 1.269(10) . ? C26 F1 1.312(9) . ? C26 F3 1.339(11) . ? S2 O6 1.416(5) . ? S2 O8 1.430(6) . ? S2 O7 1.449(6) . ? S2 C27 1.836(9) . ? C27 F4 1.286(10) . ? C27 F6 1.294(9) . ? C27 F5 1.310(11) . ? S3A O11A 1.453(10) . ? S3A O10 1.459(7) . ? S3A O9 1.506(6) . ? S3A C28 1.739(11) . ? S3B O9 1.381(6) . ? S3B O11B 1.422(10) . ? S3B O10 1.522(8) . ? S3B C28 1.855(10) . ? C28 F9B 1.21(4) . ? C28 F8B 1.24(5) . ? C28 F9A 1.32(2) . ? C28 F8A 1.32(4) . ? C28 F7A 1.381(16) . ? C28 F7B 1.463(18) . ? O1W H1W 0.8572 . ? O1W H2W 0.8544 . ? 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 180.000(1) 2_466 . ? O1 Cu1 N1 95.97(16) 2_466 . ? O1 Cu1 N1 84.03(16) . . ? O1 Cu1 N1 84.03(16) 2_466 2_466 ? O1 Cu1 N1 95.97(16) . 2_466 ? N1 Cu1 N1 180.000(2) . 2_466 ? O1 Cu2 N14 90.91(16) . 2_566 ? O1 Cu2 N10 174.75(17) . . ? N14 Cu2 N10 89.86(16) 2_566 . ? O1 Cu2 N2 84.54(16) . . ? N14 Cu2 N2 161.76(17) 2_566 . ? N10 Cu2 N2 93.14(16) . . ? O1 Cu2 N5 90.26(18) . . ? N14 Cu2 N5 101.06(16) 2_566 . ? N10 Cu2 N5 94.69(17) . . ? N2 Cu2 N5 96.63(17) . . ? N11 Cu3 N11 180.000(1) 2_566 . ? N11 Cu3 N13 89.06(16) 2_566 2_566 ? N11 Cu3 N13 90.94(16) . 2_566 ? N11 Cu3 N13 90.94(16) 2_566 . ? N11 Cu3 N13 89.06(16) . . ? N13 Cu3 N13 180.000(1) 2_566 . ? N11 Cu3 O2 88.17(16) 2_566 2_566 ? N11 Cu3 O2 91.83(16) . 2_566 ? N13 Cu3 O2 87.01(17) 2_566 2_566 ? N13 Cu3 O2 92.99(17) . 2_566 ? N11 Cu3 O2 91.83(16) 2_566 . ? N11 Cu3 O2 88.17(16) . . ? N13 Cu3 O2 92.99(17) 2_566 . ? N13 Cu3 O2 87.01(17) . . ? O2 Cu3 O2 180.000(1) 2_566 . ? Cu2 O1 Cu1 116.50(18) . . ? Cu2 O1 H1O 113.6 . . ? Cu1 O1 H1O 113.5 . . ? Cu3 O2 H2A 109.0 . . ? Cu3 O2 H2B 109.0 . . ? H2A O2 H2B 106.4 . . ? C1 N1 N2 107.0(4) . . ? C1 N1 Cu1 133.9(4) . . ? N2 N1 Cu1 118.8(3) . . ? C2 N2 N1 107.0(4) . . ? C2 N2 Cu2 135.2(3) . . ? N1 N2 Cu2 117.0(3) . . ? C1 N3 C2 105.8(4) . . ? C1 N3 C4 125.0(4) . . ? C2 N3 C4 129.0(4) . . ? C6 N4 N5 106.6(5) . . ? C7 N5 N4 107.8(4) . . ? C7 N5 Cu2 140.8(4) . . ? N4 N5 Cu2 110.8(4) . . ? C7 N6 C6 104.3(5) . . ? C7 N6 C10 128.8(5) . . ? C6 N6 C10 126.9(5) . . ? C8 N7 N8 107.1(5) . . ? C9 N8 N7 106.6(5) . . ? C9 N9 C8 102.7(5) . . ? C9 N9 C13 129.4(5) . . ? C8 N9 C13 127.8(5) . . ? C16 N10 N11 107.7(4) . . ? C16 N10 Cu2 128.2(3) . . ? N11 N10 Cu2 122.4(3) . . ? C17 N11 N10 107.6(4) . . ? C17 N11 Cu3 125.5(3) . . ? N10 N11 Cu3 126.8(3) . . ? C17 N12 C16 105.2(4) . . ? C17 N12 C19 126.1(4) . . ? C16 N12 C19 128.5(4) . . ? C21 N13 N14 106.6(4) . . ? C21 N13 Cu3 128.1(3) . . ? N14 N13 Cu3 123.8(3) . . ? C22 N14 N13 108.1(4) . . ? C22 N14 Cu2 128.6(3) . 2_566 ? N13 N14 Cu2 123.1(3) . 2_566 ? C22 N15 C21 105.8(4) . . ? C22 N15 C24 127.8(4) . . ? C21 N15 C24 126.4(4) . . ? N1 C1 N3 110.1(4) . . ? N1 C1 H1 124.9 . . ? N3 C1 H1 124.9 . . ? N2 C2 N3 110.1(5) . . ? N2 C2 H2 125.0 . . ? N3 C2 H2 125.0 . . ? C5 C3 C4 119.3(5) 2_465 . ? C5 C3 H3 120.3 2_465 . ? C4 C3 H3 120.3 . . ? C5 C4 C3 121.6(5) . . ? C5 C4 N3 119.7(5) . . ? C3 C4 N3 118.7(5) . . ? C3 C5 C4 119.1(5) 2_465 . ? C3 C5 H5 120.4 2_465 . ? C4 C5 H5 120.4 . . ? N4 C6 N6 111.3(6) . . ? N4 C6 H6 124.3 . . ? N6 C6 H6 124.3 . . ? N5 C7 N6 110.0(5) . . ? N5 C7 H7 125.0 . . ? N6 C7 H7 125.0 . . ? N7 C8 N9 111.9(5) . . ? N7 C8 H8 124.0 . . ? N9 C8 H8 124.0 . . ? N8 C9 N9 111.7(6) . . ? N8 C9 H9 124.2 . . ? N9 C9 H9 124.2 . . ? C15 C10 C11 120.1(6) . . ? C15 C10 N6 120.0(6) . . ? C11 C10 N6 119.8(5) . . ? C12 C11 C10 119.6(5) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? C11 C12 C13 120.2(6) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C14 C13 C12 119.8(6) . . ? C14 C13 N9 120.0(5) . . ? C12 C13 N9 120.1(5) . . ? C13 C14 C15 120.3(6) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C10 C15 C14 119.9(6) . . ? C10 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? N10 C16 N12 109.9(4) . . ? N10 C16 H16 125.1 . . ? N12 C16 H16 125.1 . . ? N11 C17 N12 109.6(4) . . ? N11 C17 H17 125.2 . . ? N12 C17 H17 125.2 . . ? C19 C18 C20 118.5(5) . 2_576 ? C19 C18 H18 120.7 . . ? C20 C18 H18 120.7 2_576 . ? C20 C19 C18 122.0(5) . . ? C20 C19 N12 118.9(5) . . ? C18 C19 N12 119.1(5) . . ? C19 C20 C18 119.5(5) . 2_576 ? C19 C20 H20 120.3 . . ? C18 C20 H20 120.3 2_576 . ? N13 C21 N15 109.9(4) . . ? N13 C21 H21 125.0 . . ? N15 C21 H21 125.0 . . ? N14 C22 N15 109.6(4) . . ? N14 C22 H22 125.2 . . ? N15 C22 H22 125.2 . . ? C24 C23 C25 119.0(5) . 2_565 ? C24 C23 H23 120.5 . . ? C25 C23 H23 120.5 2_565 . ? C23 C24 C25 121.9(5) . . ? C23 C24 N15 119.1(5) . . ? C25 C24 N15 119.0(5) . . ? C24 C25 C23 119.1(5) . 2_565 ? C24 C25 H25 120.5 . . ? C23 C25 H25 120.5 2_565 . ? O3 S1 O5 115.1(3) . . ? O3 S1 O4 113.5(4) . . ? O5 S1 O4 113.4(3) . . ? O3 S1 C26 105.3(4) . . ? O5 S1 C26 105.3(3) . . ? O4 S1 C26 102.6(4) . . ? F2 C26 F1 109.9(8) . . ? F2 C26 F3 107.2(8) . . ? F1 C26 F3 107.1(8) . . ? F2 C26 S1 113.5(7) . . ? F1 C26 S1 111.0(6) . . ? F3 C26 S1 107.8(6) . . ? O6 S2 O8 117.3(4) . . ? O6 S2 O7 114.6(4) . . ? O8 S2 O7 112.6(4) . . ? O6 S2 C27 102.9(4) . . ? O8 S2 C27 104.6(4) . . ? O7 S2 C27 102.5(4) . . ? F4 C27 F6 109.1(8) . . ? F4 C27 F5 106.2(8) . . ? F6 C27 F5 111.1(9) . . ? F4 C27 S2 109.5(7) . . ? F6 C27 S2 111.2(6) . . ? F5 C27 S2 109.5(6) . . ? O10 S3A O9 106.3(5) . . ? O11A S3A C28 103.4(7) . . ? O9 S3B O10 109.6(4) . . ? O11B S3B C28 101.4(7) . . ? F9B C28 F8B 116(3) . . ? F9A C28 F8A 108(2) . . ? F9A C28 F7A 101.8(16) . . ? F8A C28 F7A 104(2) . . ? F9B C28 F7B 107.6(19) . . ? F8B C28 F7B 107(2) . . ? F9A C28 S3A 117.8(13) . . ? F8A C28 S3A 112.4(17) . . ? F7A C28 S3A 111.3(8) . . ? F9B C28 S3B 110.1(16) . . ? F8B C28 S3B 112(3) . . ? F7B C28 S3B 102.2(9) . . ? 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 N14 Cu2 O1 Cu1 155.4(2) 2_566 . . . ? N2 Cu2 O1 Cu1 -42.3(2) . . . . ? N5 Cu2 O1 Cu1 54.3(2) . . . . ? N1 Cu1 O1 Cu2 43.5(2) . . . . ? N1 Cu1 O1 Cu2 -136.5(2) 2_466 . . . ? O1 Cu1 N1 C1 -34.1(6) 2_466 . . . ? O1 Cu1 N1 C1 145.9(6) . . . . ? O1 Cu1 N1 N2 154.0(4) 2_466 . . . ? O1 Cu1 N1 N2 -26.0(4) . . . . ? C1 N1 N2 C2 0.6(6) . . . . ? Cu1 N1 N2 C2 174.5(4) . . . . ? C1 N1 N2 Cu2 -170.8(4) . . . . ? Cu1 N1 N2 Cu2 3.1(5) . . . . ? O1 Cu2 N2 C2 -146.4(6) . . . . ? N14 Cu2 N2 C2 -70.2(8) 2_566 . . . ? N10 Cu2 N2 C2 28.9(6) . . . . ? N5 Cu2 N2 C2 124.0(6) . . . . ? O1 Cu2 N2 N1 21.9(4) . . . . ? N14 Cu2 N2 N1 98.1(6) 2_566 . . . ? N10 Cu2 N2 N1 -162.8(4) . . . . ? N5 Cu2 N2 N1 -67.7(4) . . . . ? C6 N4 N5 C7 0.3(8) . . . . ? C6 N4 N5 Cu2 173.3(5) . . . . ? O1 Cu2 N5 C7 132.6(7) . . . . ? N14 Cu2 N5 C7 41.7(7) 2_566 . . . ? N10 Cu2 N5 C7 -49.1(7) . . . . ? N2 Cu2 N5 C7 -142.8(6) . . . . ? O1 Cu2 N5 N4 -36.6(4) . . . . ? N14 Cu2 N5 N4 -127.6(4) 2_566 . . . ? N10 Cu2 N5 N4 141.6(4) . . . . ? N2 Cu2 N5 N4 47.9(4) . . . . ? C8 N7 N8 C9 -1.1(9) . . . . ? N14 Cu2 N10 C16 -121.3(4) 2_566 . . . ? N2 Cu2 N10 C16 76.7(4) . . . . ? N5 Cu2 N10 C16 -20.2(4) . . . . ? N14 Cu2 N10 N11 41.8(3) 2_566 . . . ? N2 Cu2 N10 N11 -120.2(4) . . . . ? N5 Cu2 N10 N11 142.9(3) . . . . ? C16 N10 N11 C17 0.2(5) . . . . ? Cu2 N10 N11 C17 -165.9(3) . . . . ? C16 N10 N11 Cu3 176.4(3) . . . . ? Cu2 N10 N11 Cu3 10.3(5) . . . . ? N13 Cu3 N11 C17 125.1(4) 2_566 . . . ? N13 Cu3 N11 C17 -54.9(4) . . . . ? O2 Cu3 N11 C17 38.1(4) 2_566 . . . ? O2 Cu3 N11 C17 -141.9(4) . . . . ? N13 Cu3 N11 N10 -50.4(4) 2_566 . . . ? N13 Cu3 N11 N10 129.6(4) . . . . ? O2 Cu3 N11 N10 -137.5(4) 2_566 . . . ? O2 Cu3 N11 N10 42.5(4) . . . . ? N11 Cu3 N13 C21 130.8(5) 2_566 . . . ? N11 Cu3 N13 C21 -49.2(5) . . . . ? O2 Cu3 N13 C21 -141.0(4) 2_566 . . . ? O2 Cu3 N13 C21 39.0(4) . . . . ? N11 Cu3 N13 N14 -33.2(4) 2_566 . . . ? N11 Cu3 N13 N14 146.8(4) . . . . ? O2 Cu3 N13 N14 55.0(4) 2_566 . . . ? O2 Cu3 N13 N14 -125.0(4) . . . . ? C21 N13 N14 C22 -1.2(5) . . . . ? Cu3 N13 N14 C22 165.7(3) . . . . ? C21 N13 N14 Cu2 173.2(3) . . . 2_566 ? Cu3 N13 N14 Cu2 -19.9(5) . . . 2_566 ? N2 N1 C1 N3 -1.1(6) . . . . ? Cu1 N1 C1 N3 -173.6(4) . . . . ? C2 N3 C1 N1 1.1(7) . . . . ? C4 N3 C1 N1 177.4(5) . . . . ? N1 N2 C2 N3 0.1(6) . . . . ? Cu2 N2 C2 N3 169.2(4) . . . . ? C1 N3 C2 N2 -0.7(7) . . . . ? C4 N3 C2 N2 -176.8(5) . . . . ? C5 C3 C4 C5 0.4(11) 2_465 . . . ? C5 C3 C4 N3 -177.1(6) 2_465 . . . ? C1 N3 C4 C5 -135.3(6) . . . . ? C2 N3 C4 C5 40.0(9) . . . . ? C1 N3 C4 C3 42.2(9) . . . . ? C2 N3 C4 C3 -142.4(6) . . . . ? C3 C4 C5 C3 -0.4(11) . . . 2_465 ? N3 C4 C5 C3 177.1(6) . . . 2_465 ? N5 N4 C6 N6 0.2(9) . . . . ? C7 N6 C6 N4 -0.6(9) . . . . ? C10 N6 C6 N4 -178.5(7) . . . . ? N4 N5 C7 N6 -0.7(7) . . . . ? Cu2 N5 C7 N6 -170.2(5) . . . . ? C6 N6 C7 N5 0.8(7) . . . . ? C10 N6 C7 N5 178.6(6) . . . . ? N8 N7 C8 N9 1.7(8) . . . . ? C9 N9 C8 N7 -1.5(8) . . . . ? C13 N9 C8 N7 175.7(6) . . . . ? N7 N8 C9 N9 0.2(11) . . . . ? C8 N9 C9 N8 0.7(10) . . . . ? C13 N9 C9 N8 -176.4(7) . . . . ? C7 N6 C10 C15 146.5(8) . . . . ? C6 N6 C10 C15 -36.2(12) . . . . ? C7 N6 C10 C11 -37.8(10) . . . . ? C6 N6 C10 C11 139.6(8) . . . . ? C15 C10 C11 C12 -0.4(11) . . . . ? N6 C10 C11 C12 -176.1(6) . . . . ? C10 C11 C12 C13 1.4(10) . . . . ? C11 C12 C13 C14 -1.2(11) . . . . ? C11 C12 C13 N9 177.4(6) . . . . ? C9 N9 C13 C14 -175.0(9) . . . . ? C8 N9 C13 C14 8.5(11) . . . . ? C9 N9 C13 C12 6.4(12) . . . . ? C8 N9 C13 C12 -170.1(7) . . . . ? C12 C13 C14 C15 -0.1(15) . . . . ? N9 C13 C14 C15 -178.7(9) . . . . ? C11 C10 C15 C14 -0.9(15) . . . . ? N6 C10 C15 C14 174.9(9) . . . . ? C13 C14 C15 C10 1.1(17) . . . . ? N11 N10 C16 N12 0.0(5) . . . . ? Cu2 N10 C16 N12 165.0(3) . . . . ? C17 N12 C16 N10 -0.2(6) . . . . ? C19 N12 C16 N10 -175.6(5) . . . . ? N10 N11 C17 N12 -0.3(5) . . . . ? Cu3 N11 C17 N12 -176.5(3) . . . . ? C16 N12 C17 N11 0.3(6) . . . . ? C19 N12 C17 N11 175.9(5) . . . . ? C20 C18 C19 C20 0.4(10) 2_576 . . . ? C20 C18 C19 N12 179.0(5) 2_576 . . . ? C17 N12 C19 C20 37.6(8) . . . . ? C16 N12 C19 C20 -147.8(5) . . . . ? C17 N12 C19 C18 -141.0(5) . . . . ? C16 N12 C19 C18 33.5(8) . . . . ? C18 C19 C20 C18 -0.4(10) . . . 2_576 ? N12 C19 C20 C18 -179.0(5) . . . 2_576 ? N14 N13 C21 N15 1.1(6) . . . . ? Cu3 N13 C21 N15 -165.0(3) . . . . ? C22 N15 C21 N13 -0.7(6) . . . . ? C24 N15 C21 N13 177.8(5) . . . . ? N13 N14 C22 N15 0.8(6) . . . . ? Cu2 N14 C22 N15 -173.2(3) 2_566 . . . ? C21 N15 C22 N14 -0.1(6) . . . . ? C24 N15 C22 N14 -178.6(5) . . . . ? C25 C23 C24 C25 -0.3(11) 2_565 . . . ? C25 C23 C24 N15 179.8(5) 2_565 . . . ? C22 N15 C24 C23 134.0(6) . . . . ? C21 N15 C24 C23 -44.2(8) . . . . ? C22 N15 C24 C25 -46.0(8) . . . . ? C21 N15 C24 C25 135.9(6) . . . . ? C23 C24 C25 C23 0.3(11) . . . 2_565 ? N15 C24 C25 C23 -179.8(5) . . . 2_565 ? O3 S1 C26 F2 174.8(7) . . . . ? O5 S1 C26 F2 52.7(8) . . . . ? O4 S1 C26 F2 -66.2(7) . . . . ? O3 S1 C26 F1 -60.8(8) . . . . ? O5 S1 C26 F1 177.1(6) . . . . ? O4 S1 C26 F1 58.3(8) . . . . ? O3 S1 C26 F3 56.2(7) . . . . ? O5 S1 C26 F3 -65.9(6) . . . . ? O4 S1 C26 F3 175.3(6) . . . . ? O6 S2 C27 F4 54.4(8) . . . . ? O8 S2 C27 F4 -68.8(7) . . . . ? O7 S2 C27 F4 173.6(7) . . . . ? O6 S2 C27 F6 175.1(7) . . . . ? O8 S2 C27 F6 51.9(8) . . . . ? O7 S2 C27 F6 -65.7(8) . . . . ? O6 S2 C27 F5 -61.7(8) . . . . ? O8 S2 C27 F5 175.1(7) . . . . ? O7 S2 C27 F5 57.4(7) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 26.73 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.762 _refine_diff_density_min -0.643 _refine_diff_density_rms 0.100 #----------------------------------------------------# data_(6) _database_code_depnum_ccdc_archive 'CCDC 674758' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Dihydroxo Tricopper(II) Sulfate Complex with 1,4-bi(1,2,4-triazol-4-yl)benzene, Dihydrate ; _chemical_name_common ; Dihydroxo Tricopper(ii) Sulfate Complex with 1,4-bi(1,2,4- triazol-4-yl)benzene, Dihydrate ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H14 Cu3 N6 O12 S2' _chemical_formula_weight 665.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' 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 5.1275(4) _cell_length_b 16.3726(11) _cell_length_c 10.8005(9) _cell_angle_alpha 90.00 _cell_angle_beta 99.531(10) _cell_angle_gamma 90.00 _cell_volume 894.19(12) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 28.09 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.17 _exptl_crystal_density_diffrn 2.470 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 662 _exptl_absorpt_coefficient_mu 3.855 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.4260 _exptl_absorpt_correction_T_max 0.5216 _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 8104 _diffrn_reflns_av_R_equivalents 0.0358 _diffrn_reflns_av_sigmaI/netI 0.0224 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 28.09 _reflns_number_total 2140 _reflns_number_gt 1817 _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)' #------------------------------- Refinement data-----------------------# _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. The structure was solved by direct methods. All CH hydrogen atoms were located from difference maps and then refined as riding, with C---H distances constrained to 0.94 \%A, and with U~iso~(H) = 1.2U~eq~ (parent carbon atoms). OH hydrogen atoms (hydroxyl and water) were located from the map and then fixed with U~iso~(H) = 1.5U~eq~ (parent oxygen atom). ; _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^)+(0.0526P)^2^+0.2230P] 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 2140 _refine_ls_number_parameters 151 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0276 _refine_ls_R_factor_gt 0.0251 _refine_ls_wR_factor_ref 0.0727 _refine_ls_wR_factor_gt 0.0718 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 #----------------Atomic Coordinates and Displacement Parameters---------# loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.5000 0.5000 0.5000 0.00861(11) Uani 1 2 d S . . Cu2 Cu 0.45756(5) 0.684336(13) 0.62846(2) 0.00950(10) Uani 1 1 d . . . S1 S 0.54780(11) 0.81127(3) 0.84611(5) 0.00894(13) Uani 1 1 d . . . O1 O 0.2844(3) 0.58844(8) 0.55140(13) 0.0109(3) Uani 1 1 d . . . H1O H 0.1681 0.6009 0.4985 0.016 Uiso 1 1 d . . . O2 O 0.6454(3) 0.76960(8) 0.73888(14) 0.0131(3) Uani 1 1 d . . . O3 O 0.6470(3) 0.76574(9) 0.96383(14) 0.0146(3) Uani 1 1 d . . . O4 O 0.6529(4) 0.89422(8) 0.85652(15) 0.0186(3) Uani 1 1 d . . . O5 O 0.2564(4) 0.80954(9) 0.82347(15) 0.0174(3) Uani 1 1 d . . . O6 O 0.1446(3) 0.75608(9) 0.59000(14) 0.0154(3) Uani 1 1 d . . . H2O H 0.1240 0.7755 0.6577 0.023 Uiso 1 1 d . . . H3O H 0.0016 0.7414 0.5461 0.023 Uiso 1 1 d . . . N1 N 0.7551(4) 0.53137(9) 0.65249(15) 0.0102(3) Uani 1 1 d . . . N2 N 0.7513(4) 0.60939(9) 0.69979(16) 0.0114(3) Uani 1 1 d . . . N3 N 1.0655(4) 0.54151(10) 0.81611(15) 0.0097(3) Uani 1 1 d . . . C1 C 0.9422(5) 0.49176(11) 0.72336(19) 0.0114(4) Uani 1 1 d . . . H1 H 0.9862 0.4368 0.7123 0.014 Uiso 1 1 calc R . . C2 C 0.9385(5) 0.61461(12) 0.79727(18) 0.0130(4) Uani 1 1 d . . . H2 H 0.9794 0.6616 0.8468 0.016 Uiso 1 1 calc R . . C3 C 1.2861(4) 0.52046(12) 0.91055(18) 0.0104(4) Uani 1 1 d . . . C4 C 1.3428(5) 0.43875(12) 0.9368(2) 0.0160(4) Uani 1 1 d . . . H4 H 1.2359 0.3977 0.8938 0.019 Uiso 1 1 calc R . . C5 C 1.4418(5) 0.58185(12) 0.9733(2) 0.0149(4) Uani 1 1 d . . . H5 H 1.4015 0.6370 0.9550 0.018 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 0.0085(2) 0.00706(18) 0.00873(17) -0.00277(10) -0.00297(13) 0.00163(11) Cu2 0.01054(19) 0.00615(14) 0.01070(14) -0.00131(8) -0.00147(10) 0.00165(8) S1 0.0112(3) 0.0058(2) 0.0094(2) -0.00181(15) 0.00028(18) 0.00002(15) O1 0.0098(9) 0.0086(6) 0.0126(6) -0.0014(5) -0.0030(5) 0.0022(5) O2 0.0131(9) 0.0118(6) 0.0143(7) -0.0056(5) 0.0021(6) 0.0008(5) O3 0.0164(10) 0.0138(7) 0.0124(7) 0.0024(5) -0.0012(6) 0.0011(5) O4 0.0278(10) 0.0068(6) 0.0239(8) -0.0048(6) 0.0120(7) -0.0048(6) O5 0.0124(10) 0.0230(8) 0.0160(7) -0.0060(6) -0.0002(6) 0.0021(6) O6 0.0129(9) 0.0142(7) 0.0171(7) -0.0057(5) -0.0028(6) 0.0030(5) N1 0.0143(10) 0.0037(7) 0.0115(7) -0.0024(6) -0.0011(6) 0.0013(6) N2 0.0145(10) 0.0057(7) 0.0124(7) -0.0032(6) -0.0024(6) 0.0014(6) N3 0.0103(10) 0.0075(7) 0.0098(7) -0.0010(6) -0.0029(6) 0.0016(6) C1 0.0106(12) 0.0093(8) 0.0120(9) -0.0035(6) -0.0046(8) 0.0009(7) C2 0.0166(13) 0.0068(8) 0.0135(9) -0.0014(6) -0.0033(8) 0.0037(7) C3 0.0107(12) 0.0097(8) 0.0093(8) 0.0006(7) -0.0030(7) 0.0018(7) C4 0.0186(13) 0.0077(8) 0.0183(10) -0.0010(7) -0.0069(8) -0.0006(7) C5 0.0176(13) 0.0067(8) 0.0173(9) 0.0006(7) -0.0062(8) 0.0016(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 O1 1.9571(14) 3_666 ? Cu1 O1 1.9571(14) . ? Cu1 N1 1.9934(17) 3_666 ? Cu1 N1 1.9934(17) . ? Cu2 O1 1.9238(14) . ? Cu2 O6 1.9767(16) . ? Cu2 O2 1.9795(15) . ? Cu2 N2 1.9958(18) . ? Cu2 O3 2.3119(16) 4_575 ? S1 O4 1.4585(15) . ? S1 O5 1.4738(19) . ? S1 O3 1.4888(15) . ? S1 O2 1.4999(14) . ? O1 H1O 0.7813 . ? O3 Cu2 2.3119(16) 4_576 ? O6 H2O 0.8197 . ? O6 H3O 0.8395 . ? N1 C1 1.297(3) . ? N1 N2 1.377(2) . ? N2 C2 1.305(3) . ? N3 C2 1.361(2) . ? N3 C1 1.363(2) . ? N3 C3 1.434(3) . ? C1 H1 0.9400 . ? C2 H2 0.9400 . ? C3 C4 1.388(3) . ? C3 C5 1.389(3) . ? C4 C5 1.386(3) 3_867 ? C4 H4 0.9400 . ? C5 C4 1.386(3) 3_867 ? C5 H5 0.9400 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 O1 180.00(8) 3_666 . ? O1 Cu1 N1 84.21(6) 3_666 3_666 ? O1 Cu1 N1 95.79(6) . 3_666 ? O1 Cu1 N1 95.79(6) 3_666 . ? O1 Cu1 N1 84.21(6) . . ? N1 Cu1 N1 180.0 3_666 . ? O1 Cu2 O6 95.37(6) . . ? O1 Cu2 O2 168.47(6) . . ? O6 Cu2 O2 90.27(6) . . ? O1 Cu2 N2 85.98(6) . . ? O6 Cu2 N2 168.82(7) . . ? O2 Cu2 N2 86.57(7) . . ? O1 Cu2 O3 100.27(6) . 4_575 ? O6 Cu2 O3 93.33(6) . 4_575 ? O2 Cu2 O3 89.40(6) . 4_575 ? N2 Cu2 O3 97.35(7) . 4_575 ? O4 S1 O5 112.46(10) . . ? O4 S1 O3 109.32(10) . . ? O5 S1 O3 109.00(10) . . ? O4 S1 O2 108.47(9) . . ? O5 S1 O2 108.79(9) . . ? O3 S1 O2 108.74(9) . . ? Cu2 O1 Cu1 118.99(8) . . ? Cu2 O1 H1O 110.2 . . ? Cu1 O1 H1O 112.6 . . ? S1 O2 Cu2 126.48(10) . . ? S1 O3 Cu2 110.62(8) . 4_576 ? Cu2 O6 H2O 105.2 . . ? Cu2 O6 H3O 123.4 . . ? H2O O6 H3O 112.7 . . ? C1 N1 N2 107.41(16) . . ? C1 N1 Cu1 132.73(13) . . ? N2 N1 Cu1 119.86(13) . . ? C2 N2 N1 107.84(16) . . ? C2 N2 Cu2 132.73(13) . . ? N1 N2 Cu2 118.90(13) . . ? C2 N3 C1 105.27(17) . . ? C2 N3 C3 128.24(17) . . ? C1 N3 C3 126.48(17) . . ? N1 C1 N3 110.04(17) . . ? N1 C1 H1 125.0 . . ? N3 C1 H1 125.0 . . ? N2 C2 N3 109.44(17) . . ? N2 C2 H2 125.3 . . ? N3 C2 H2 125.3 . . ? C4 C3 C5 120.92(19) . . ? C4 C3 N3 119.38(18) . . ? C5 C3 N3 119.70(18) . . ? C5 C4 C3 119.54(19) 3_867 . ? C5 C4 H4 120.2 3_867 . ? C3 C4 H4 120.2 . . ? C4 C5 C3 119.54(18) 3_867 . ? C4 C5 H5 120.2 3_867 . ? C3 C5 H5 120.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 Cu2 O1 Cu1 158.77(8) . . . . ? O2 Cu2 O1 Cu1 -82.2(3) . . . . ? N2 Cu2 O1 Cu1 -32.36(9) . . . . ? O3 Cu2 O1 Cu1 64.40(8) 4_575 . . . ? N1 Cu1 O1 Cu2 -144.84(8) 3_666 . . . ? N1 Cu1 O1 Cu2 35.16(8) . . . . ? O4 S1 O2 Cu2 -148.67(11) . . . . ? O5 S1 O2 Cu2 -26.05(13) . . . . ? O3 S1 O2 Cu2 92.53(13) . . . . ? O1 Cu2 O2 S1 -65.6(4) . . . . ? O6 Cu2 O2 S1 53.87(12) . . . . ? N2 Cu2 O2 S1 -115.40(12) . . . . ? O3 Cu2 O2 S1 147.20(11) 4_575 . . . ? O4 S1 O3 Cu2 69.58(11) . . . 4_576 ? O5 S1 O3 Cu2 -53.72(10) . . . 4_576 ? O2 S1 O3 Cu2 -172.17(8) . . . 4_576 ? O1 Cu1 N1 C1 -23.9(2) 3_666 . . . ? O1 Cu1 N1 C1 156.1(2) . . . . ? O1 Cu1 N1 N2 155.42(14) 3_666 . . . ? O1 Cu1 N1 N2 -24.58(14) . . . . ? C1 N1 N2 C2 0.6(2) . . . . ? Cu1 N1 N2 C2 -178.89(15) . . . . ? C1 N1 N2 Cu2 -172.04(15) . . . . ? Cu1 N1 N2 Cu2 8.5(2) . . . . ? O1 Cu2 N2 C2 -157.1(2) . . . . ? O6 Cu2 N2 C2 -59.8(4) . . . . ? O2 Cu2 N2 C2 14.1(2) . . . . ? O3 Cu2 N2 C2 103.0(2) 4_575 . . . ? O1 Cu2 N2 N1 13.33(15) . . . . ? O6 Cu2 N2 N1 110.7(3) . . . . ? O2 Cu2 N2 N1 -175.47(15) . . . . ? O3 Cu2 N2 N1 -86.52(15) 4_575 . . . ? N2 N1 C1 N3 -0.6(2) . . . . ? Cu1 N1 C1 N3 178.79(14) . . . . ? C2 N3 C1 N1 0.4(3) . . . . ? C3 N3 C1 N1 -178.22(19) . . . . ? N1 N2 C2 N3 -0.4(2) . . . . ? Cu2 N2 C2 N3 170.88(15) . . . . ? C1 N3 C2 N2 0.0(3) . . . . ? C3 N3 C2 N2 178.58(19) . . . . ? C2 N3 C3 C4 162.5(2) . . . . ? C1 N3 C3 C4 -19.2(3) . . . . ? C2 N3 C3 C5 -18.3(3) . . . . ? C1 N3 C3 C5 160.0(2) . . . . ? C5 C3 C4 C5 -0.1(4) . . . 3_867 ? N3 C3 C4 C5 179.1(2) . . . 3_867 ? C4 C3 C5 C4 0.1(4) . . . 3_867 ? N3 C3 C5 C4 -179.1(2) . . . 3_867 ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 28.09 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.772 _refine_diff_density_min -0.607 _refine_diff_density_rms 0.112 #----------------------------------------------------# data_(7) _database_code_depnum_ccdc_archive 'CCDC 674759' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Copper(II) Sulfate Complex with 1,4-bi(1,2,4-triazol-4-yl)benzene, Hexahydrate ; _chemical_name_common ;Copper(ii) Sulfate Complex with 1,4-bi(1,2,4-triazol-4- yl)benzene, Hexahydrate ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H20 Cu N6 O10 S' _chemical_formula_weight 479.92 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 'P nma' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 7.1442(4) _cell_length_b 19.4387(15) _cell_length_c 17.3114(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2404.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 3.42 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.326 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 988 _exptl_absorpt_coefficient_mu 1.045 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.8182 _exptl_absorpt_correction_T_max 0.8590 _exptl_absorpt_process_details 'DIFABS, (Walker & Stuart, 1983)' _exptl_special_details ; Walker, N. & Stuart, D. 1983. Acta Cryst. A39, 158-166. ; _diffrn_ambient_temperature 291(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 12811 _diffrn_reflns_av_R_equivalents 0.0475 _diffrn_reflns_av_sigmaI/netI 0.0439 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.42 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2780 _reflns_number_gt 2056 _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)' #------------------------------- Refinement data-----------------------# _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. The structure was solved by direct methods. All CH hydrogen atoms were located from difference maps and then refined as riding, with C---H distances constrained to 0.93 \%A, and with U~iso~(H) = 1.2U~eq~ (parent carbon atoms). Sulfate anion was coordinated via one oxygen atom and three other (non-coordinated) oxygens show rotational disorder over two equally 0.5/0.5 populated positions related by a mirror plane. The disordered atoms were refinened anisotropically and without restraints in geometry. Solvate water molecules are disoreder, each over two closely separated positions. The partial contribution factors were 0.5/0.5 (two components related by a mirror plane) and two 0.65/0.35. Only one of such disordered oxygen atoms [O5] was refined anisotropically, while other ones were left isotropic and the hydrogen atoms were not added in all the cases. ; _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^)+(0.0793P)^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 2780 _refine_ls_number_parameters 147 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0557 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.1171 _refine_ls_wR_factor_gt 0.1130 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.994 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 #----------------Atomic Coordinates and Displacement Parameters---------# 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 0.21540(6) 0.7500 0.25440(2) 0.01641(15) Uani 1 2 d S . . S1 S 0.46508(16) 0.7500 0.07183(5) 0.0317(3) Uani 1 2 d S . . O1 O 0.4674(5) 0.7500 0.15749(16) 0.0369(7) Uani 1 2 d S . . O2 O 0.2941(9) 0.7785(3) 0.0411(3) 0.0576(16) Uani 0.50 1 d P . . O3 O 0.6301(9) 0.7810(3) 0.0392(3) 0.0576(15) Uani 0.50 1 d P . . O4 O 0.4696(8) 0.6734(3) 0.0540(3) 0.0496(13) Uani 0.50 1 d P . . N1 N 0.0666(3) 0.67796(10) 0.19876(12) 0.0202(5) Uani 1 1 d . . . N2 N -0.1254(3) 0.67760(9) 0.19458(11) 0.0202(5) Uani 1 1 d . . . N3 N -0.0187(4) 0.59919(11) 0.11729(14) 0.0282(5) Uani 1 1 d . . . C1 C 0.1296(4) 0.63046(13) 0.15152(15) 0.0265(6) Uani 1 1 d . . . H1 H 0.2549 0.6200 0.1429 0.032 Uiso 1 1 calc R . . C2 C -0.1749(4) 0.62997(13) 0.14561(15) 0.0277(6) Uani 1 1 d . . . H2 H -0.2974 0.6189 0.1323 0.033 Uiso 1 1 calc R . . C3 C -0.0098(4) 0.54760(14) 0.05727(17) 0.0320(7) Uani 1 1 d . . . C4 C -0.1308(8) 0.4926(2) 0.0586(3) 0.0837(18) Uani 1 1 d . . . H4 H -0.2187 0.4881 0.0979 0.100 Uiso 1 1 calc R . . C5 C 0.1193(8) 0.5558(2) -0.0007(3) 0.0805(17) Uani 1 1 d . . . H5 H 0.1985 0.5938 -0.0008 0.097 Uiso 1 1 calc R . . O5 O 0.9618(13) 0.7766(4) -0.0150(6) 0.113(4) Uani 0.50 1 d P . . O6A O 0.591(2) 0.6110(7) -0.0698(8) 0.182(5) Uiso 0.65 1 d P . . O6B O 0.499(4) 0.6268(12) -0.0970(15) 0.158(8) Uiso 0.35 1 d P . . O7A O 0.4600(17) 0.5185(7) 0.1640(9) 0.173(4) Uiso 0.65 1 d P . . O7B O 0.468(3) 0.5336(13) 0.0994(17) 0.178(8) Uiso 0.35 1 d P . . O8 O 0.908(4) 0.8390(13) -0.1567(15) 0.256(9) Uiso 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0172(3) 0.01362(19) 0.0184(2) 0.000 -0.00598(15) 0.000 S1 0.0305(6) 0.0458(5) 0.0187(4) 0.000 -0.0018(3) 0.000 O1 0.0261(19) 0.065(2) 0.0192(13) 0.000 -0.0012(11) 0.000 O2 0.053(4) 0.082(4) 0.038(2) -0.003(2) -0.021(2) 0.024(2) O3 0.055(4) 0.079(3) 0.039(2) 0.002(2) 0.013(2) -0.023(3) O4 0.055(4) 0.048(3) 0.046(3) -0.020(2) -0.001(2) -0.001(2) N1 0.0168(15) 0.0186(9) 0.0252(10) -0.0062(7) -0.0006(8) 0.0013(7) N2 0.0158(14) 0.0202(9) 0.0246(10) -0.0067(7) 0.0011(8) 0.0000(8) N3 0.0211(14) 0.0282(11) 0.0353(12) -0.0172(9) 0.0008(9) -0.0003(9) C1 0.0195(17) 0.0272(12) 0.0328(13) -0.0126(9) 0.0015(11) 0.0018(10) C2 0.0206(17) 0.0301(13) 0.0325(13) -0.0139(10) 0.0009(11) -0.0027(10) C3 0.0308(19) 0.0294(13) 0.0357(15) -0.0214(11) 0.0030(12) -0.0029(11) C4 0.088(4) 0.079(3) 0.084(3) -0.050(3) 0.050(3) -0.041(3) C5 0.090(4) 0.070(3) 0.081(3) -0.049(2) 0.040(3) -0.045(3) O5 0.061(6) 0.129(9) 0.148(8) 0.056(6) 0.004(5) -0.001(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 2.005(2) . ? Cu1 N1 2.005(2) 7_575 ? Cu1 N2 2.013(2) 6_656 ? Cu1 N2 2.013(2) 4_565 ? Cu1 O1 2.338(3) 6_556 ? S1 O3 1.439(6) . ? S1 O3 1.439(6) 7_575 ? S1 O2 1.443(5) 7_575 ? S1 O2 1.443(5) . ? S1 O1 1.483(3) . ? S1 O4 1.521(5) . ? S1 O4 1.521(5) 7_575 ? N1 C1 1.313(3) . ? N1 N2 1.374(3) . ? N2 C2 1.304(3) . ? N2 Cu1 2.013(2) 6_556 ? N3 C1 1.357(4) . ? N3 C2 1.358(4) . ? N3 C3 1.446(3) . ? C1 H1 0.9300 . ? C2 H2 0.9300 . ? C3 C5 1.372(5) . ? C3 C4 1.376(5) . ? C4 C5 1.378(5) 5_565 ? C4 H4 0.9300 . ? C5 C4 1.378(5) 5_565 ? C5 H5 0.9300 . ? O5 O5 1.033(17) 7_575 ? 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 88.62(12) . 7_575 ? N1 Cu1 N2 91.26(8) . 6_656 ? N1 Cu1 N2 176.90(9) 7_575 6_656 ? N1 Cu1 N2 176.90(9) . 4_565 ? N1 Cu1 N2 91.26(8) 7_575 4_565 ? N2 Cu1 N2 88.69(12) 6_656 4_565 ? N1 Cu1 O1 84.93(8) . 6_556 ? N1 Cu1 O1 84.93(8) 7_575 6_556 ? N2 Cu1 O1 98.15(8) 6_656 6_556 ? N2 Cu1 O1 98.15(8) 4_565 6_556 ? O3 S1 O2 112.8(4) 7_575 7_575 ? O3 S1 O2 112.8(4) . . ? O3 S1 O1 112.6(2) . . ? O3 S1 O1 112.6(2) 7_575 . ? O2 S1 O1 112.2(2) 7_575 . ? O2 S1 O1 112.2(2) . . ? O3 S1 O4 108.2(3) . . ? O2 S1 O4 108.6(3) . . ? O1 S1 O4 101.7(2) . . ? O3 S1 O4 108.2(3) 7_575 7_575 ? O2 S1 O4 108.6(3) 7_575 7_575 ? O1 S1 O4 101.7(2) . 7_575 ? C1 N1 N2 107.8(2) . . ? C1 N1 Cu1 127.5(2) . . ? N2 N1 Cu1 123.95(14) . . ? C2 N2 N1 108.0(2) . . ? C2 N2 Cu1 128.9(2) . 6_556 ? N1 N2 Cu1 122.49(14) . 6_556 ? C1 N3 C2 106.7(2) . . ? C1 N3 C3 126.2(2) . . ? C2 N3 C3 127.0(2) . . ? N1 C1 N3 108.6(3) . . ? N1 C1 H1 125.7 . . ? N3 C1 H1 125.7 . . ? N2 C2 N3 108.9(3) . . ? N2 C2 H2 125.5 . . ? N3 C2 H2 125.5 . . ? C5 C3 C4 121.7(3) . . ? C5 C3 N3 118.3(3) . . ? C4 C3 N3 120.0(3) . . ? C3 C4 C5 118.8(4) . 5_565 ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 5_565 . ? C3 C5 C4 119.5(3) . 5_565 ? C3 C5 H5 120.2 . . ? C4 C5 H5 120.2 5_565 . ? 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 S1 O1 Cu1 -26.9(3) . . . 6_656 ? O3 S1 O1 Cu1 26.9(3) 7_575 . . 6_656 ? O2 S1 O1 Cu1 155.5(3) 7_575 . . 6_656 ? O2 S1 O1 Cu1 -155.5(3) . . . 6_656 ? O4 S1 O1 Cu1 88.6(2) . . . 6_656 ? O4 S1 O1 Cu1 -88.6(2) 7_575 . . 6_656 ? O3 S1 O2 O2 131.8(3) . . . 7_575 ? O3 S1 O2 O2 77.1(4) 7_575 . . 7_575 ? O1 S1 O2 O2 -99.77(17) . . . 7_575 ? O4 S1 O2 O2 11.9(2) . . . 7_575 ? O4 S1 O2 O2 167.5(2) 7_575 . . 7_575 ? O3 S1 O2 O4 -35.7(4) . . . 7_575 ? O3 S1 O2 O4 -90.4(5) 7_575 . . 7_575 ? O2 S1 O2 O4 -167.5(2) 7_575 . . 7_575 ? O1 S1 O2 O4 92.7(3) . . . 7_575 ? O4 S1 O2 O4 -155.6(4) . . . 7_575 ? O2 S1 O3 O3 -82.1(4) 7_575 . . 7_575 ? O2 S1 O3 O3 -130.8(3) . . . 7_575 ? O1 S1 O3 O3 101.03(18) . . . 7_575 ? O4 S1 O3 O3 -10.6(2) . . . 7_575 ? O4 S1 O3 O3 -168.3(2) 7_575 . . 7_575 ? O3 S1 O3 O4 168.3(2) 7_575 . . 7_575 ? O2 S1 O3 O4 86.2(5) 7_575 . . 7_575 ? O2 S1 O3 O4 37.6(4) . . . 7_575 ? O1 S1 O3 O4 -90.6(3) . . . 7_575 ? O4 S1 O3 O4 157.8(5) . . . 7_575 ? O3 S1 O4 O3 9.3(2) . . . 7_575 ? O2 S1 O4 O3 141.4(4) 7_575 . . 7_575 ? O2 S1 O4 O3 132.1(4) . . . 7_575 ? O1 S1 O4 O3 -109.4(3) . . . 7_575 ? O4 S1 O4 O3 63.9(11) 7_575 . . 7_575 ? O3 S1 O4 O2 -132.1(4) . . . 7_575 ? O3 S1 O4 O2 -141.4(4) 7_575 . . 7_575 ? O2 S1 O4 O2 -9.3(2) . . . 7_575 ? O1 S1 O4 O2 109.2(3) . . . 7_575 ? O4 S1 O4 O2 -77.6(11) 7_575 . . 7_575 ? N1 Cu1 N1 C1 119.3(2) 7_575 . . . ? N2 Cu1 N1 C1 -57.6(2) 6_656 . . . ? O1 Cu1 N1 C1 -155.7(2) 6_556 . . . ? N1 Cu1 N1 N2 -49.6(2) 7_575 . . . ? N2 Cu1 N1 N2 133.53(16) 6_656 . . . ? O1 Cu1 N1 N2 35.46(17) 6_556 . . . ? C1 N1 N2 C2 0.4(3) . . . . ? Cu1 N1 N2 C2 171.14(18) . . . . ? C1 N1 N2 Cu1 -171.45(17) . . . 6_556 ? Cu1 N1 N2 Cu1 -0.7(2) . . . 6_556 ? N2 N1 C1 N3 -0.4(3) . . . . ? Cu1 N1 C1 N3 -170.70(17) . . . . ? C2 N3 C1 N1 0.2(3) . . . . ? C3 N3 C1 N1 175.1(3) . . . . ? N1 N2 C2 N3 -0.2(3) . . . . ? Cu1 N2 C2 N3 170.90(18) 6_556 . . . ? C1 N3 C2 N2 0.0(3) . . . . ? C3 N3 C2 N2 -174.8(3) . . . . ? C1 N3 C3 C5 -40.9(5) . . . . ? C2 N3 C3 C5 133.0(4) . . . . ? C1 N3 C3 C4 140.1(4) . . . . ? C2 N3 C3 C4 -46.0(5) . . . . ? C5 C3 C4 C5 1.0(10) . . . 5_565 ? N3 C3 C4 C5 180.0(5) . . . 5_565 ? C4 C3 C5 C4 -1.0(10) . . . 5_565 ? N3 C3 C5 C4 -180.0(5) . . . 5_565 ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.695 _refine_diff_density_min -0.354 _refine_diff_density_rms 0.080 #----------------------------------------------------# data_(8) _database_code_depnum_ccdc_archive 'CCDC 674760' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tris[5-(4-(1,2,4-triazol-4-yl)phenyl)tetrazolato] dicopper(II) Chloride, Dodecahydrate ; _chemical_name_common ; Tris(5-(4-(1,2,4-triazol-4-yl)phenyl)tetrazolato) dicopper(ii) Chloride, Dodecahydrate ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H42 Cl Cu2 N21 O12' _chemical_formula_weight 1015.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Cmcm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y, -z-1/2' 'x, -y, z-1/2' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, -z-1/2' 'x+1/2, -y+1/2, z-1/2' '-x+1/2, y+1/2, z' _cell_length_a 25.822(2) _cell_length_b 7.7119(7) _cell_length_c 25.1892(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5016.2(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 3.40 _cell_measurement_theta_max 26.30 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 1.344 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2088 _exptl_absorpt_coefficient_mu 0.971 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.8523 _exptl_absorpt_correction_T_max 0.8924 _exptl_absorpt_process_details 'DIFABS, (Walker & Stuart, 1983)' _exptl_special_details ; Walker, N. & Stuart, D. 1983. Acta Cryst. A39, 158-166. ; _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 'Stoe Imaging plate diffraction system' _diffrn_measurement_method '\f oscillation scans' _diffrn_standards_decay_% 0 _diffrn_reflns_number 15901 _diffrn_reflns_av_R_equivalents 0.0402 _diffrn_reflns_av_sigmaI/netI 0.0269 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 6.40 _diffrn_reflns_theta_max 26.30 _reflns_number_total 2581 _reflns_number_gt 1851 _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)' #------------------------------- Refinement data-----------------------# _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. The structure was solved by direct methods. All CH hydrogen atoms (for 1,4-phenylene fragment) were located from difference maps and then refined as riding, with C---H distances constrained to 0.95 \%A, and with U~iso~(H) = 1.2U~eq~ (parent carbon atoms). Both unique molecules of the ligand are crystallographically centrosymmetric, and centroids of the benzene cycles occupy center of inversion. Therefore, the TETRAZOLE and TRIAZOLE functions of the ligand (which are uniform either in view of shape, geometry or their structural role) were related by symmetry and are not distinguishable. On this reason, C/N (non-coordinated) atoms of the heterocycles could not be attributed and these positions were refined as mixed 0.5/0.5 carbon/nitrogen atoms, using the corresponding SHELXL functions EXYZ and EADP. The hydrogen atoms were also added, with occupancy factors 0.5. For one of the unique ligands, para-phenylene linker -C~6~H~4~- is disordered over two unequal positions. The disorder was refined with partial contributions 0.6 and 0.4, without restraints in geometry, and the hydrogen atoms were also added considering the occupancy factors of the parent carbon atoms. Since the Cu to non-coordinated chloride ratio is 2:1, the copper atom occupies a special position (Wyck.lett. 8d) and the chloride anion appears in general position (Wyck.lett.16h), then occupancy of this site of chloride anion is 0.25. Therefore, the Cl atom was refined anisotropically with this partial occupancy. Solvate water molecules are disordered inside the large voids. Oxygen atoms for two of solvate water molecules were located and refined. One of them appears close to the partially occupied position of the chloride anion and it was refined with occupancy factor 0.75. Water hydrogen atoms were not added. Other water molecules are badly disordered and therefore the remaining electron density was modelled using a SQUEEZE routine as implemented in PLATON. ; _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^)+(0.0849P)^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 2581 _refine_ls_number_parameters 147 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0612 _refine_ls_R_factor_gt 0.0431 _refine_ls_wR_factor_ref 0.1302 _refine_ls_wR_factor_gt 0.1226 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 #----------------Atomic Coordinates and Displacement Parameters---------# 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 0.00954(18) Uani 1 2 d S . . N1 N 0.21661(7) 0.1149(3) 0.43981(7) 0.0149(4) Uani 1 1 d . . . N2 N 0.21024(8) -0.0584(3) 0.43969(8) 0.0171(4) Uani 1 1 d . . . N3 N 0.31190(7) 0.0879(3) 0.50002(7) 0.0121(4) Uani 1 1 d . . . C1N C 0.20484(9) 0.1787(3) 0.39265(8) 0.0196(5) Uani 0.50 1 d P . . N1C N 0.20484(9) 0.1787(3) 0.39265(8) 0.0196(5) Uani 0.50 1 d P . . H1N H 0.2061 0.2954 0.3827 0.024 Uiso 0.50 1 d P . . C2N C 0.19113(9) 0.0441(3) 0.36215(9) 0.0197(5) Uani 0.50 1 d P . . N2C N 0.19113(9) 0.0441(3) 0.36215(9) 0.0197(5) Uani 0.50 1 d P . . C3N C 0.19461(9) -0.1021(3) 0.39170(9) 0.0210(5) Uani 0.50 1 d P . . N3C N 0.19461(9) -0.1021(3) 0.39170(9) 0.0210(5) Uani 0.50 1 d P . . H3N H 0.1869 -0.2138 0.3804 0.025 Uiso 0.50 1 d P . . C4 C 0.18401(10) 0.0503(4) 0.30484(10) 0.0207(6) Uani 1 1 d . . . C5 C 0.16616(18) -0.0892(5) 0.27782(12) 0.0569(12) Uani 1 1 d . . . H5 H 0.1536 -0.1874 0.2966 0.068 Uiso 1 1 calc R . . C6 C 0.19884(18) 0.1952(5) 0.27743(12) 0.0552(11) Uani 1 1 d . . . H6 H 0.2092 0.2962 0.2962 0.066 Uiso 1 1 calc R . . C7N C 0.36020(9) 0.1423(3) 0.50001(10) 0.0205(5) Uani 0.50 1 d P . . N7C N 0.36020(9) 0.1423(3) 0.50001(10) 0.0205(5) Uani 0.50 1 d P . . H7N H 0.3710 0.2572 0.5001 0.025 Uiso 0.50 1 d P . . C8N C 0.39084(13) 0.0000 0.5000 0.0147(7) Uani 0.50 2 d SP . . N8C C 0.39084(13) 0.0000 0.5000 0.0147(7) Uani 0.50 2 d SP . . C9 C 0.44708(15) 0.0000 0.5000 0.0260(9) Uani 1 2 d S . . C10A C 0.47318(16) 0.1124(7) 0.5329(2) 0.0323(12) Uani 0.60 1 d P . . H10A H 0.4547 0.1904 0.5556 0.039 Uiso 0.60 1 d P . . C10B C 0.4729(3) 0.1071(10) 0.4655(3) 0.0319(17) Uani 0.40 1 d P . . H10B H 0.4547 0.1805 0.4417 0.038 Uiso 0.40 1 d P . . Cl1 Cl 0.1281(2) 0.5224(6) 0.3661(2) 0.0754(14) Uani 0.25 1 d P . . O1 O 0.17462(18) 0.5327(4) 0.36519(17) 0.0593(11) Uani 0.75 1 d P . . O2 O 0.41049(18) 0.5004(8) 0.51176(18) 0.0426(13) Uiso 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0099(2) 0.0088(3) 0.0099(2) -0.00138(14) -0.00152(14) 0.00127(14) N1 0.0160(9) 0.0169(11) 0.0119(9) 0.0001(8) -0.0006(7) 0.0022(8) N2 0.0190(10) 0.0207(11) 0.0115(9) -0.0025(8) -0.0012(8) -0.0024(8) N3 0.0109(9) 0.0082(10) 0.0172(9) -0.0022(7) 0.0006(7) -0.0018(8) C1N 0.0249(11) 0.0234(13) 0.0107(10) 0.0023(9) -0.0025(9) 0.0021(10) N1C 0.0249(11) 0.0234(13) 0.0107(10) 0.0023(9) -0.0025(9) 0.0021(10) C2N 0.0212(12) 0.0236(13) 0.0142(11) 0.0011(9) -0.0001(9) -0.0018(10) N2C 0.0212(12) 0.0236(13) 0.0142(11) 0.0011(9) -0.0001(9) -0.0018(10) C3N 0.0236(12) 0.0237(13) 0.0157(12) -0.0017(10) -0.0030(9) -0.0038(10) N3C 0.0236(12) 0.0237(13) 0.0157(12) -0.0017(10) -0.0030(9) -0.0038(10) C4 0.0212(12) 0.0275(15) 0.0133(11) 0.0001(10) -0.0016(9) -0.0021(11) C5 0.110(3) 0.044(2) 0.0166(16) 0.0055(15) -0.0015(18) -0.041(2) C6 0.123(4) 0.0282(19) 0.0146(16) -0.0029(13) -0.0023(19) -0.023(2) C7N 0.0108(10) 0.0130(12) 0.0377(13) -0.0010(10) -0.0013(9) 0.0010(9) N7C 0.0108(10) 0.0130(12) 0.0377(13) -0.0010(10) -0.0013(9) 0.0010(9) C8N 0.0068(15) 0.0089(17) 0.0285(18) 0.0003(14) 0.000 0.000 N8C 0.0068(15) 0.0089(17) 0.0285(18) 0.0003(14) 0.000 0.000 C9 0.0127(17) 0.016(2) 0.049(3) -0.0030(17) 0.000 0.000 C10A 0.010(2) 0.020(3) 0.067(4) -0.013(2) 0.003(2) 0.0018(18) C10B 0.022(4) 0.020(4) 0.054(5) 0.011(3) 0.002(3) 0.004(3) Cl1 0.067(3) 0.070(3) 0.089(3) 0.001(3) -0.019(3) -0.004(2) O1 0.077(3) 0.0309(19) 0.070(2) -0.0065(17) -0.040(2) 0.0090(17) _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 N3 2.0291(19) 13_556 ? Cu1 N3 2.0291(19) . ? Cu1 N1 2.0315(19) . ? Cu1 N1 2.0315(19) 13_556 ? Cu1 N2 2.355(2) 4_556 ? Cu1 N2 2.355(2) 16 ? N1 C1N 1.321(3) . ? N1 N2 1.346(3) . ? N2 C3N 1.318(3) . ? N2 Cu1 2.355(2) 4_556 ? N3 C7N 1.316(3) . ? N3 N3 1.356(4) 4_556 ? C1N C2N 1.339(3) . ? C1N H1N 0.9345 . ? C2N C3N 1.354(3) . ? C2N C4 1.456(3) . ? C3N H3N 0.9287 . ? C4 C5 1.354(4) . ? C4 C6 1.368(4) . ? C5 C5 1.402(6) 10_556 ? C5 H5 0.9500 . ? C6 C6 1.382(6) 10_556 ? C6 H6 0.9500 . ? C7N C8N 1.353(3) . ? C7N H7N 0.9287 . ? C8N N7C 1.353(3) 4_556 ? C8N C7N 1.353(3) 4_556 ? C8N C9 1.452(5) . ? C9 C10B 1.371(8) . ? C9 C10B 1.371(8) 4_556 ? C9 C10A 1.375(5) . ? C9 C10A 1.375(5) 4_556 ? C10A C10A 1.385(8) 12_655 ? C10A C10B 1.694(9) 4_556 ? C10A C10B 1.697(11) . ? C10A H10A 0.9575 . ? C10B C10B 1.402(14) 12_655 ? C10B C10A 1.694(9) 4_556 ? C10B H10B 0.9479 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Cu1 N3 180.000(1) 13_556 . ? N3 Cu1 N1 88.94(8) 13_556 . ? N3 Cu1 N1 91.06(8) . . ? N3 Cu1 N1 91.06(8) 13_556 13_556 ? N3 Cu1 N1 88.94(8) . 13_556 ? N1 Cu1 N1 180.0 . 13_556 ? N3 Cu1 N2 92.48(8) 13_556 4_556 ? N3 Cu1 N2 87.52(8) . 4_556 ? N1 Cu1 N2 88.54(7) . 4_556 ? N1 Cu1 N2 91.46(7) 13_556 4_556 ? N3 Cu1 N2 87.52(8) 13_556 16 ? N3 Cu1 N2 92.48(8) . 16 ? N1 Cu1 N2 91.46(7) . 16 ? N1 Cu1 N2 88.54(7) 13_556 16 ? N2 Cu1 N2 180.0 4_556 16 ? C1N N1 N2 109.83(19) . . ? C1N N1 Cu1 125.29(17) . . ? N2 N1 Cu1 124.24(14) . . ? C3N N2 N1 107.08(19) . . ? N1 N2 Cu1 124.61(14) . 4_556 ? C7N N3 N3 108.58(14) . 4_556 ? C7N N3 Cu1 123.39(17) . . ? N1 C1N C2N 106.8(2) . . ? N1 C1N H1N 126.2 . . ? C2N C1N H1N 127.0 . . ? C1N C2N C3N 108.2(2) . . ? C1N C2N C4 125.2(2) . . ? C3N C2N C4 125.5(2) . . ? N2 C3N C2N 108.1(2) . . ? N2 C3N H3N 125.7 . . ? C2N C3N H3N 126.2 . . ? C5 C4 C6 119.4(3) . . ? C5 C4 C2N 121.0(3) . . ? C6 C4 C2N 119.5(3) . . ? C4 C5 C5 120.17(17) . 10_556 ? C4 C5 H5 119.9 . . ? C5 C5 H5 119.9 10_556 . ? C4 C6 C6 120.32(17) . 10_556 ? C4 C6 H6 119.8 . . ? C6 C6 H6 119.8 10_556 . ? N3 C7N C8N 107.2(2) . . ? N3 C7N H7N 126.0 . . ? C8N C7N H7N 126.8 . . ? N7C C8N C7N 108.4(3) 4_556 . ? C7N C8N C7N 108.4(3) 4_556 . ? N7C C8N C9 125.80(15) 4_556 . ? C7N C8N C9 125.80(15) 4_556 . ? C7N C8N C9 125.80(15) . . ? C10B C9 C10B 121.9(6) . 4_556 ? C10A C9 C10A 121.3(5) . 4_556 ? C10B C9 C8N 119.0(3) . . ? C10B C9 C8N 119.0(3) 4_556 . ? C10A C9 C8N 119.3(2) . . ? C10A C9 C8N 119.3(2) 4_556 . ? C9 C10A C10A 119.3(2) . 12_655 ? C9 C10A H10A 120.8 . . ? C10A C10A H10A 119.8 12_655 . ? C9 C10B C10B 119.0(3) . 12_655 ? C9 C10B H10B 121.4 . . ? 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 N3 Cu1 N1 C1N 60.65(19) 13_556 . . . ? N3 Cu1 N1 C1N -119.35(19) . . . . ? N2 Cu1 N1 C1N 153.16(19) 4_556 . . . ? N2 Cu1 N1 C1N -26.84(19) 16 . . . ? N3 Cu1 N1 N2 -129.47(18) 13_556 . . . ? N3 Cu1 N1 N2 50.53(18) . . . . ? N2 Cu1 N1 N2 -36.96(16) 4_556 . . . ? N2 Cu1 N1 N2 143.04(16) 16 . . . ? C1N N1 N2 C3N 0.4(3) . . . . ? Cu1 N1 N2 C3N -170.87(15) . . . . ? C1N N1 N2 Cu1 158.68(15) . . . 4_556 ? Cu1 N1 N2 Cu1 -12.6(2) . . . 4_556 ? N1 Cu1 N3 C7N 131.70(19) . . . . ? N1 Cu1 N3 C7N -48.30(19) 13_556 . . . ? N2 Cu1 N3 C7N -139.81(19) 4_556 . . . ? N2 Cu1 N3 C7N 40.19(19) 16 . . . ? N1 Cu1 N3 N3 -48.2(2) . . . 4_556 ? N1 Cu1 N3 N3 131.8(2) 13_556 . . 4_556 ? N2 Cu1 N3 N3 40.3(2) 4_556 . . 4_556 ? N2 Cu1 N3 N3 -139.7(2) 16 . . 4_556 ? N2 N1 C1N C2N -0.4(3) . . . . ? Cu1 N1 C1N C2N 170.75(15) . . . . ? N1 C1N C2N C3N 0.2(3) . . . . ? N1 C1N C2N C4 -168.5(2) . . . . ? N1 N2 C3N C2N -0.2(3) . . . . ? Cu1 N2 C3N C2N -158.60(16) 4_556 . . . ? C1N C2N C3N N2 0.0(3) . . . . ? C4 C2N C3N N2 168.7(2) . . . . ? C1N C2N C4 C5 -174.8(3) . . . . ? C3N C2N C4 C5 18.4(4) . . . . ? C1N C2N C4 C6 9.6(4) . . . . ? C3N C2N C4 C6 -157.2(3) . . . . ? C6 C4 C5 C5 4.2(4) . . . 10_556 ? C2N C4 C5 C5 -171.34(17) . . . 10_556 ? C5 C4 C6 C6 -4.2(4) . . . 10_556 ? C2N C4 C6 C6 171.41(16) . . . 10_556 ? N3 N3 C7N C8N 0.0(3) 4_556 . . . ? Cu1 N3 C7N C8N -179.97(12) . . . . ? N3 C7N C8N N7C 0.02(11) . . . 4_556 ? N3 C7N C8N C7N 0.02(11) . . . 4_556 ? N3 C7N C8N C9 -179.98(11) . . . . ? C7N C8N C9 C10B -46.5(4) . . . . ? N7C C8N C9 C10B -46.5(4) 4_556 . . 4_556 ? C7N C8N C9 C10B -46.5(4) 4_556 . . 4_556 ? C7N C8N C9 C10B 133.5(4) . . . 4_556 ? N7C C8N C9 C10A -136.3(3) 4_556 . . . ? C7N C8N C9 C10A -136.3(3) 4_556 . . . ? C7N C8N C9 C10A -136.3(3) . . . 4_556 ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 26.30 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 0.572 _refine_diff_density_min -0.505 _refine_diff_density_rms 0.080 #------------- END of CIF -----------------#