Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Dr Konstantin V. Domasevitch' _publ_contact_author_address ; Konstantin V. Domasevitch Inorganic Chemistry Department Kiev Shevchenko University Volodimirska Str. 64 01033 Kiev Ukraine ; _publ_contact_author_phone ? _publ_contact_author_fax +380(44)296-2467 _publ_contact_author_email dk@anorgchemie.univ.kiev.ua _publ_requested_coeditor_name ? _publ_contact_letter ; ? ; #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Self-assembly sodalite-like framework ; loop_ _publ_author_name _publ_author_address P.V.Solntsev ; Inorganic Chemistry Department Kiev Shevchenko University Volodimirska Str. 64 01033 Kiev Ukraine ; J.Sieler ; Institute of Inorganic Chemistry Leipzig University Linnestrasse 3 D-04103 Leipzig Germany ; A.N.Chernega ; Institute of Organic Chemistry Murmanskaya Str. 4 253660 Kiev Ukraine ; J.A.K.Howard ; Department of Chemistry University of Durham Durham DH1 3LE UK ; T.Gelbrich ; Department of Chemistry University of Southampton Highfield Southampton SO17 1BJ UK ; ; K.V.Domasevitch ; ; Inorganic Chemistry Department Kiev Shevchenko University Volodimirska Str. 64 01033 Kiev Ukraine ; _publ_section_acknowledgements ; KVD and JS acknowledge support from Deutsche Forschungsgemeinschaft; Royal Society Fellowship (ANCh). JAKH acknowledges the EPSRC for a Senior Research Fellowship. ; #================================================================== data_c1422 _database_code_depnum_ccdc_archive 'CCDC 228008' _audit_creation_method SHELXL _chemical_name_systematic ; Copper(II) Perchlorate 1:2 Complex with 1,2,3,6,7,8-hexahydro-cinnolino[5,4,3-cde]cinnoline, Chloroform solvate ; _chemical_name_common ; Copper(ii) Perchlorate 1:2 Complex with 1,2,3,6,7,8-hexahydro- cinnolino(5,4,3-cde)cinnoline, Chloroform solvate ; _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C27 H27 Cl11 Cu N8 O8' _chemical_formula_weight 1045.06 _chemical_melting_point ? _chemical_compound_source ? 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 Cubic _symmetry_space_group_name_H-M I-43m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y, x, z' '-y, -x, z' 'y, -x, -z' '-y, x, -z' 'x, z, y' '-x, z, -y' '-x, -z, y' 'x, -z, -y' 'z, y, x' 'z, -y, -x' '-z, y, -x' '-z, -y, x' '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+1/2' 'x+1/2, -y+1/2, -z+1/2' 'z+1/2, 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+1/2, x+1/2, -y+1/2' 'y+1/2, z+1/2, 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+1/2, x+1/2' 'y+1/2, x+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' 'x+1/2, z+1/2, y+1/2' '-x+1/2, z+1/2, -y+1/2' '-x+1/2, -z+1/2, y+1/2' 'x+1/2, -z+1/2, -y+1/2' 'z+1/2, y+1/2, x+1/2' 'z+1/2, -y+1/2, -x+1/2' '-z+1/2, y+1/2, -x+1/2' '-z+1/2, -y+1/2, x+1/2' _cell_length_a 23.7035(14) _cell_length_b 23.7035(14) _cell_length_c 23.7035(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 13318.0(14) _cell_formula_units_Z 12 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description cube _exptl_crystal_colour brown _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 1.59 _exptl_crystal_density_diffrn 1.564 _exptl_crystal_density_method 'immersion in chloroform/bromoform' _exptl_crystal_F_000 6300 _exptl_absorpt_coefficient_mu 1.206 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.72016 _exptl_absorpt_correction_T_max 0.89389 _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'Siemens SMART CCD' _diffrn_measurement_method 'omega scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36502 _diffrn_reflns_av_R_equivalents 0.1437 _diffrn_reflns_av_sigmaI/netI 0.0520 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 26.98 _reflns_number_total 2687 _reflns_number_observed 1555 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 899 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0630P)^2^+71.6000P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(5) _refine_ls_number_reflns 1788 _refine_ls_number_parameters 152 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.1411 _refine_ls_R_factor_obs 0.0820 _refine_ls_wR_factor_all 0.2596 _refine_ls_wR_factor_obs 0.1678 _refine_ls_goodness_of_fit_all 1.134 _refine_ls_goodness_of_fit_obs 1.187 _refine_ls_restrained_S_all 1.532 _refine_ls_restrained_S_obs 1.202 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cu1 Cu -0.2500 -0.5000 0.0000 0.0379(5) Uani 1 d S . N1 N -0.1997(2) -0.5365(2) 0.0588(3) 0.0353(14) Uani 1 d . . N2 N -0.2111(3) -0.5937(3) 0.0687(3) 0.043(2) Uani 1 d . . C1 C -0.1826(3) -0.6197(3) 0.1083(3) 0.040(2) Uani 1 d . . C2 C -0.1406(3) -0.5929(5) 0.1406(3) 0.035(3) Uani 1 d S . C3 C -0.1290(3) -0.5371(4) 0.1290(3) 0.030(2) Uani 1 d S . C4 C -0.1609(3) -0.5096(3) 0.0868(3) 0.029(2) Uani 1 d . . C5 C -0.1497(3) -0.4491(3) 0.0744(3) 0.039(2) Uani 1 d . . H5A H -0.1839(3) -0.4311(3) 0.0623(3) 0.080 Uiso 1 d R . H5B H -0.1226(3) -0.4460(3) 0.0445(3) 0.080 Uiso 1 d R . C6 C -0.1264(3) -0.4190(4) 0.1264(3) 0.037(2) Uani 1 d S . H6A H -0.1550(3) -0.4192(4) 0.1550(3) 0.080 Uiso 1 d SR . H6B H -0.1176(3) -0.3805(4) 0.1177(3) 0.080 Uiso 1 d SR . C7 C -0.1961(4) -0.6808(3) 0.1212(4) 0.059(2) Uani 1 d . . H7A H -0.2051(4) -0.7001(3) 0.0868(4) 0.080 Uiso 1 d R . H7B H -0.2290(4) -0.6819(3) 0.1449(4) 0.080 Uiso 1 d R . C8 C -0.1497(7) -0.7118(6) 0.1497(7) 0.105(6) Uani 1 d S . H8B H -0.1218(7) -0.7214(6) 0.1219(7) 0.080 Uiso 1 d SR . H8A H -0.1644(7) -0.7465(6) 0.1644(7) 0.080 Uiso 1 d SR . Cl1 Cl 0.0000 -0.5000 0.0000 0.0482(11) Uani 1 d S . O1 O -0.0351(3) -0.5342(4) 0.0351(3) 0.067(2) Uani 1 d S . Cl2 Cl -0.2763(3) -0.7237(3) 0.2763(3) 0.112(3) Uani 1 d SD . O2 O -0.2400(6) -0.7600(6) 0.2400(6) 0.170(13) Uani 1 d SD . O3 O -0.3104(5) -0.6896(5) 0.2407(7) 0.137(5) Uani 1 d SD . Cl3 Cl -0.3752(13) -0.3752(13) 0.3752(13) 0.400 Uiso 1 d SD . O4 O -0.4089(12) -0.3357(19) 0.4089(12) 0.400 Uiso 1 d SD . O5 O -0.3398(13) -0.3398(13) 0.3398(13) 0.400 Uiso 1 d SD . C9 C -0.2642(5) -0.5542(7) 0.2642(5) 0.101(5) Uani 1 d SD . Cl4 Cl -0.3065(2) -0.5116(6) 0.3065(2) 0.219(5) Uani 1 d SD . Cl5 Cl -0.1942(2) -0.5414(2) 0.2781(2) 0.126(2) Uani 1 d D . C10 C 0.0000 -0.6596(11) 0.0000 0.139(11) Uani 1 d SD . Cl6 Cl -0.0380(12) -0.7075(19) -0.0380(12) 0.275(42) Uani 0.25 d SPD . Cl7 Cl -0.0422(6) -0.6883(15) 0.0422(6) 0.222(24) Uani 0.25 d SPDU . Cl8 Cl -0.0776(4) -0.6802(5) -0.0033(6) 0.141(4) Uani 0.50 d PD . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0334(8) 0.0401(6) 0.0401(6) 0.000 0.000 0.000 N1 0.036(3) 0.029(3) 0.040(3) -0.002(3) 0.002(3) -0.006(2) N2 0.041(4) 0.038(3) 0.050(4) -0.003(3) 0.000(3) -0.006(3) C1 0.039(4) 0.036(4) 0.045(4) 0.002(3) -0.002(3) -0.009(3) C2 0.033(4) 0.041(6) 0.033(4) 0.005(3) 0.000(4) -0.005(3) C3 0.031(3) 0.028(5) 0.031(3) -0.002(3) 0.000(4) 0.002(3) C4 0.028(3) 0.028(4) 0.032(3) -0.005(3) -0.001(3) 0.001(3) C5 0.036(4) 0.032(4) 0.050(5) 0.004(3) -0.010(3) 0.000(3) C6 0.041(4) 0.028(6) 0.041(4) 0.000(3) -0.011(5) 0.000(3) C7 0.073(6) 0.037(4) 0.068(6) 0.006(4) -0.017(5) -0.011(4) C8 0.138(10) 0.038(8) 0.138(10) 0.022(7) -0.024(13) -0.022(7) Cl1 0.045(2) 0.055(3) 0.045(2) 0.000 0.000 0.000 O1 0.071(4) 0.059(5) 0.071(4) 0.010(3) 0.012(5) -0.010(3) Cl2 0.112(3) 0.112(3) 0.112(3) 0.040(4) -0.040(4) -0.040(4) O2 0.170(13) 0.170(13) 0.170(13) -0.030(13) 0.030(13) 0.030(13) O3 0.146(8) 0.146(8) 0.120(11) 0.040(7) -0.040(7) 0.013(10) C9 0.117(9) 0.069(10) 0.117(9) 0.001(6) 0.018(12) -0.001(6) Cl4 0.154(4) 0.347(14) 0.154(4) -0.057(5) 0.048(5) 0.057(5) Cl5 0.085(2) 0.175(4) 0.119(3) -0.043(3) -0.004(2) 0.005(2) C10 0.154(18) 0.109(19) 0.154(18) 0.000 -0.065(29) 0.000 Cl6 0.335(71) 0.157(40) 0.335(71) -0.017(16) -0.235(80) -0.017(16) Cl7 0.243(37) 0.179(28) 0.243(37) 0.038(10) 0.212(41) -0.038(10) Cl8 0.141(7) 0.128(7) 0.153(9) 0.031(8) -0.046(8) -0.018(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 2.027(6) 42_444 ? Cu1 N1 2.027(6) . ? Cu1 N1 2.027(6) 43_445 ? Cu1 N1 2.027(6) 4_545 ? N1 C4 1.302(8) . ? N1 N2 1.404(8) . ? N2 C1 1.310(9) . ? C1 C2 1.408(9) . ? C1 C7 1.514(11) . ? C2 C3 1.379(13) . ? C2 C1 1.408(9) 23 ? C3 C4 1.413(7) 23 ? C3 C4 1.413(7) . ? C4 C5 1.488(10) . ? C5 C6 1.528(9) . ? C6 C5 1.528(9) 23 ? C7 C8 1.486(12) . ? C8 C7 1.486(12) 23 ? Cl1 O1 1.430(9) 2_545 ? Cl1 O1 1.430(9) . ? Cl1 O1 1.430(9) 3 ? Cl1 O1 1.430(9) 4_545 ? Cl2 O3 1.420(13) 7_546 ? Cl2 O3 1.420(13) 10_445 ? Cl2 O3 1.420(13) . ? Cl2 O2 1.49(2) . ? Cl3 O5 1.46(3) . ? Cl3 O4 1.47(3) 8 ? Cl3 O4 1.47(3) 11 ? Cl3 O4 1.47(3) . ? C9 Cl5 1.719(10) . ? C9 Cl5 1.719(10) 23 ? C9 Cl4 1.74(2) . ? C10 Cl7 1.57(2) . ? C10 Cl7 1.57(2) 3 ? C10 Cl6 1.70(3) 3 ? C10 Cl6 1.70(3) . ? C10 Cl8 1.905(11) 23 ? C10 Cl8 1.905(11) 3 ? C10 Cl8 1.905(11) . ? C10 Cl8 1.905(11) 21 ? Cl6 Cl8 1.41(2) 21 ? Cl6 Cl8 1.41(2) . ? Cl6 Cl7 1.96(3) 3 ? Cl6 Cl7 1.96(3) . ? Cl7 Cl8 1.381(11) 23 ? Cl7 Cl8 1.381(11) . ? Cl7 Cl6 1.96(3) 3 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N1 110.2(2) 42_444 . ? N1 Cu1 N1 108.0(3) 42_444 43_445 ? N1 Cu1 N1 110.2(2) . 43_445 ? N1 Cu1 N1 110.2(2) 42_444 4_545 ? N1 Cu1 N1 108.0(3) . 4_545 ? N1 Cu1 N1 110.2(2) 43_445 4_545 ? C4 N1 N2 121.5(6) . . ? C4 N1 Cu1 124.0(4) . . ? N2 N1 Cu1 114.5(4) . . ? C1 N2 N1 118.4(6) . . ? N2 C1 C2 122.8(7) . . ? N2 C1 C7 119.1(6) . . ? C2 C1 C7 118.1(7) . . ? C3 C2 C1 117.8(5) . 23 ? C3 C2 C1 117.8(5) . . ? C1 C2 C1 124.4(9) 23 . ? C2 C3 C4 118.5(4) . 23 ? C2 C3 C4 118.5(4) . . ? C4 C3 C4 123.0(8) 23 . ? N1 C4 C3 121.0(6) . . ? N1 C4 C5 119.7(6) . . ? C3 C4 C5 119.4(6) . . ? C4 C5 C6 110.7(6) . . ? C5 C6 C5 111.6(8) 23 . ? C8 C7 C1 114.1(8) . . ? C7 C8 C7 115.3(13) 23 . ? O1 Cl1 O1 108.8(4) 2_545 . ? O1 Cl1 O1 108.8(4) 2_545 3 ? O1 Cl1 O1 110.9(7) . 3 ? O1 Cl1 O1 110.9(7) 2_545 4_545 ? O1 Cl1 O1 108.8(4) . 4_545 ? O1 Cl1 O1 108.8(4) 3 4_545 ? O3 Cl2 O3 110.7(8) 7_546 10_445 ? O3 Cl2 O3 110.7(8) 7_546 . ? O3 Cl2 O3 110.7(8) 10_445 . ? O3 Cl2 O2 108.2(8) 7_546 . ? O3 Cl2 O2 108.2(8) 10_445 . ? O3 Cl2 O2 108.2(8) . . ? O5 Cl3 O4 105.0(21) . 8 ? O5 Cl3 O4 105.0(21) . 11 ? O4 Cl3 O4 113.5(17) 8 11 ? O5 Cl3 O4 105.0(21) . . ? O4 Cl3 O4 113.5(17) 8 . ? O4 Cl3 O4 113.5(17) 11 . ? Cl5 C9 Cl5 109.7(10) . 23 ? Cl5 C9 Cl4 110.1(6) . . ? Cl5 C9 Cl4 110.1(6) 23 . ? Cl7 C10 Cl7 128.7(30) . 3 ? Cl7 C10 Cl6 73.3(12) . 3 ? Cl7 C10 Cl6 73.3(12) 3 3 ? Cl7 C10 Cl6 73.3(12) . . ? Cl7 C10 Cl6 73.3(12) 3 . ? Cl6 C10 Cl6 96.7(38) 3 . ? Cl7 C10 Cl8 45.6(5) . 23 ? Cl7 C10 Cl8 118.6(12) 3 23 ? Cl6 C10 Cl8 45.4(7) 3 23 ? Cl6 C10 Cl8 111.2(16) . 23 ? Cl7 C10 Cl8 118.6(12) . 3 ? Cl7 C10 Cl8 45.6(5) 3 3 ? Cl6 C10 Cl8 45.4(7) 3 3 ? Cl6 C10 Cl8 111.2(16) . 3 ? Cl8 C10 Cl8 81.7(10) 23 3 ? Cl7 C10 Cl8 45.6(5) . . ? Cl7 C10 Cl8 118.6(12) 3 . ? Cl6 C10 Cl8 111.2(16) 3 . ? Cl6 C10 Cl8 45.4(7) . . ? Cl8 C10 Cl8 90.8(9) 23 . ? Cl8 C10 Cl8 150.3(16) 3 . ? Cl7 C10 Cl8 118.6(12) . 21 ? Cl7 C10 Cl8 45.6(5) 3 21 ? Cl6 C10 Cl8 111.2(16) 3 21 ? Cl6 C10 Cl8 45.4(7) . 21 ? Cl8 C10 Cl8 150.3(16) 23 21 ? Cl8 C10 Cl8 90.8(9) 3 21 ? Cl8 C10 Cl8 81.7(10) . 21 ? Cl8 Cl6 Cl8 124.8(38) 21 . ? Cl8 Cl6 C10 74.9(12) 21 . ? Cl8 Cl6 C10 74.9(12) . . ? Cl8 Cl6 Cl7 44.9(10) 21 3 ? Cl8 Cl6 Cl7 125.0(19) . 3 ? C10 Cl6 Cl7 50.2(9) . 3 ? Cl8 Cl6 Cl7 125.0(19) 21 . ? Cl8 Cl6 Cl7 44.9(10) . . ? C10 Cl6 Cl7 50.2(9) . . ? Cl7 Cl6 Cl7 92.7(15) 3 . ? Cl8 Cl7 Cl8 158.6(20) 23 . ? Cl8 Cl7 C10 80.1(8) 23 . ? Cl8 Cl7 C10 80.1(8) . . ? Cl8 Cl7 Cl6 45.9(13) 23 3 ? Cl8 Cl7 Cl6 125.6(19) . 3 ? C10 Cl7 Cl6 56.5(9) . 3 ? Cl8 Cl7 Cl6 125.6(19) 23 . ? Cl8 Cl7 Cl6 45.9(13) . . ? C10 Cl7 Cl6 56.5(9) . . ? Cl6 Cl7 Cl6 81.2(24) 3 . ? Cl7 Cl8 Cl6 89.2(21) . . ? Cl7 Cl8 C10 54.3(7) . . ? Cl6 Cl8 C10 59.7(11) . . ? _refine_diff_density_max 0.303 _refine_diff_density_min -0.500 _refine_diff_density_rms 0.063 #============================================================================== data_siecu _database_code_depnum_ccdc_archive 'CCDC 228009' _audit_creation_method SHELXL _chemical_name_systematic ; Copper(II) Nitrate 1:2 Complex with 1,2,3,6,7,8-hexahydro-cinnolino[5,4,3-cde]cinnoline, Chloroform solvate ; _chemical_name_common ; Copper(ii) Nitrate 1:2 Complex with 1,2,3,6,7,8-hexahydro- cinnolino(5,4,3-cde)cinnoline, Chloroform solvate ; _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C27 H27 Cl9 Cu N10 O6' _chemical_formula_weight 970.18 _chemical_melting_point ? _chemical_compound_source ? 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 Cubic _symmetry_space_group_name_H-M I-43m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y, x, z' '-y, -x, z' 'y, -x, -z' '-y, x, -z' 'x, z, y' '-x, z, -y' '-x, -z, y' 'x, -z, -y' 'z, y, x' 'z, -y, -x' '-z, y, -x' '-z, -y, x' '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+1/2' 'x+1/2, -y+1/2, -z+1/2' 'z+1/2, 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+1/2, x+1/2, -y+1/2' 'y+1/2, z+1/2, 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+1/2, x+1/2' 'y+1/2, x+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' 'x+1/2, z+1/2, y+1/2' '-x+1/2, z+1/2, -y+1/2' '-x+1/2, -z+1/2, y+1/2' 'x+1/2, -z+1/2, -y+1/2' 'z+1/2, y+1/2, x+1/2' 'z+1/2, -y+1/2, -x+1/2' '-z+1/2, y+1/2, -x+1/2' '-z+1/2, -y+1/2, x+1/2' _cell_length_a 23.5623(10) _cell_length_b 23.5623(10) _cell_length_c 23.5623(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 13081.4(10) _cell_formula_units_Z 12 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description cube _exptl_crystal_colour brown _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 1.48 _exptl_crystal_density_diffrn 1.478 _exptl_crystal_density_method 'immersion in di-/tetrachloromethane' _exptl_crystal_F_000 5868 _exptl_absorpt_coefficient_mu 1.101 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.78901 _exptl_absorpt_correction_T_max 0.91438 _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'Stoe IPDS' _diffrn_measurement_method 'phi rotation' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11804 _diffrn_reflns_av_R_equivalents 0.0675 _diffrn_reflns_av_sigmaI/netI 0.0750 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 25.99 _reflns_number_total 2239 _reflns_number_observed 963 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 112 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0737P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.04(4) _refine_ls_number_reflns 2127 _refine_ls_number_parameters 108 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1110 _refine_ls_R_factor_obs 0.0603 _refine_ls_wR_factor_all 0.2014 _refine_ls_wR_factor_obs 0.1351 _refine_ls_goodness_of_fit_all 0.782 _refine_ls_goodness_of_fit_obs 1.076 _refine_ls_restrained_S_all 1.190 _refine_ls_restrained_S_obs 1.135 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cu1 Cu 0.2500 0.5000 0.0000 0.0656(4) Uani 1 d S . N1 N 0.2007(2) 0.5381(2) -0.0581(2) 0.0589(12) Uani 1 d . . N2 N 0.2108(2) 0.5961(2) -0.0676(2) 0.0649(13) Uani 1 d . . C1 C 0.1836(3) 0.6224(3) -0.1064(3) 0.070(2) Uani 1 d . . C2 C 0.1388(3) 0.5953(4) -0.1388(3) 0.060(2) Uani 1 d S . C3 C 0.1279(2) 0.5398(3) -0.1279(2) 0.056(2) Uani 1 d S . C4 C 0.1613(2) 0.5107(2) -0.0863(2) 0.0540(13) Uani 1 d . . C5 C 0.1494(2) 0.4505(3) -0.0748(3) 0.0633(15) Uani 1 d . . H5A H 0.1213(2) 0.4478(3) -0.0454(3) 0.080 Uiso 1 d R . H5B H 0.1834(2) 0.4323(3) -0.0616(3) 0.080 Uiso 1 d R . C6 C 0.1279(3) 0.4207(4) -0.1279(3) 0.064(2) Uani 1 d S . H6A H 0.1194(3) 0.3818(4) -0.1194(3) 0.080 Uiso 1 d SR . H6B H 0.1567(3) 0.4215(4) -0.1567(3) 0.080 Uiso 1 d SR . C7 C 0.1935(3) 0.6844(3) -0.1187(3) 0.086(2) Uani 1 d . . H7A H 0.2256(3) 0.6868(3) -0.1436(3) 0.080 Uiso 1 d R . H7B H 0.2034(3) 0.7034(3) -0.0840(3) 0.080 Uiso 1 d R . C8 C 0.1464(4) 0.7151(6) -0.1464(4) 0.116(4) Uani 1 d S . H8A H 0.1594(4) 0.7515(6) -0.1594(4) 0.080 Uiso 1 d SR . H8B H 0.1179(4) 0.7217(6) -0.1179(4) 0.080 Uiso 1 d SR . C9 C 0.2628(4) 0.5705(5) -0.2628(4) 0.109(4) Uiso 1 d S . C10 C 0.0000 0.5000 0.0000 0.116(7) Uiso 1 d SD . N3 N 0.2735(5) 0.7265(5) -0.2735(5) 0.122(5) Uiso 1 d SD . O1 O 0.2956(4) 0.7044(4) -0.2325(6) 0.176(4) Uiso 1 d SD . Cl1 Cl 0.1962(3) 0.5327(3) -0.2734(3) 0.125(2) Uiso 0.50 d P . Cl2 Cl 0.3105(4) 0.5296(7) -0.3105(4) 0.187(4) Uiso 0.50 d SP . Cl1A Cl 0.1964(3) 0.5546(3) -0.2849(3) 0.124(2) Uiso 0.50 d P . Cl2A Cl 0.3123(4) 0.5655(7) -0.3123(4) 0.174(4) Uiso 0.50 d SP . Cl3 Cl 0.0371(4) 0.5306(6) -0.0371(4) 0.248(4) Uiso 0.75 d SPD . 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 0.0611(8) 0.0678(6) 0.0678(6) 0.000 0.000 0.000 N1 0.058(3) 0.056(3) 0.063(3) -0.007(2) 0.007(2) -0.010(2) N2 0.065(3) 0.059(3) 0.071(3) 0.007(3) -0.007(3) -0.006(2) C1 0.087(5) 0.057(4) 0.066(4) -0.003(3) 0.010(3) -0.010(3) C2 0.067(3) 0.048(5) 0.067(3) 0.007(3) -0.007(4) -0.007(3) C3 0.058(3) 0.051(5) 0.058(3) -0.004(3) 0.016(4) 0.004(3) C4 0.063(3) 0.043(4) 0.056(3) -0.003(2) 0.004(2) 0.006(2) C5 0.057(3) 0.064(4) 0.069(4) 0.005(3) -0.011(3) 0.001(3) C6 0.071(4) 0.051(5) 0.071(4) 0.001(3) -0.006(5) -0.001(3) C7 0.103(5) 0.065(4) 0.091(5) 0.013(4) -0.016(4) -0.022(4) C8 0.123(6) 0.101(9) 0.123(6) 0.009(5) 0.004(8) -0.009(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 2.008(5) 42 ? Cu1 N1 2.008(5) 43_554 ? Cu1 N1 2.008(5) . ? Cu1 N1 2.008(5) 4_565 ? N1 C4 1.312(7) . ? N1 N2 1.405(7) . ? N2 C1 1.276(8) . ? C1 C2 1.450(8) . ? C1 C7 1.510(9) . ? C2 C3 1.358(11) . ? C2 C1 1.450(8) 23 ? C3 C4 1.430(6) 23 ? C3 C4 1.430(6) . ? C4 C5 1.471(8) . ? C5 C6 1.521(8) . ? C6 C5 1.521(8) 23 ? C7 C8 1.477(10) . ? C8 C7 1.477(10) 23 ? C9 Cl2A 1.65(2) . ? C9 Cl1A 1.691(9) . ? C9 Cl1A 1.691(9) 23 ? C9 Cl1 1.822(11) . ? C9 Cl1 1.822(11) 23 ? C9 Cl2 1.86(2) . ? C10 Cl3 1.430(14) 2_565 ? C10 Cl3 1.430(14) 4_565 ? C10 Cl3 1.430(14) . ? C10 Cl3 1.430(14) 3 ? N3 O1 1.216(14) 7_564 ? N3 O1 1.216(14) . ? N3 O1 1.216(14) 10_665 ? Cl1 Cl1A 0.583(8) . ? Cl2 Cl2A 0.848(13) . ? Cl3 Cl3 2.27(2) 2_565 ? Cl3 Cl3 2.27(2) 4_565 ? Cl3 Cl3 2.47(3) 3 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N1 109.2(3) 42 43_554 ? N1 Cu1 N1 109.60(13) 42 . ? N1 Cu1 N1 109.60(13) 43_554 . ? N1 Cu1 N1 109.60(13) 42 4_565 ? N1 Cu1 N1 109.60(13) 43_554 4_565 ? N1 Cu1 N1 109.2(3) . 4_565 ? C4 N1 N2 121.1(5) . . ? C4 N1 Cu1 122.4(3) . . ? N2 N1 Cu1 116.5(3) . . ? C1 N2 N1 120.1(5) . . ? N2 C1 C2 121.9(6) . . ? N2 C1 C7 122.0(6) . . ? C2 C1 C7 116.0(6) . . ? C3 C2 C1 117.5(4) . 23 ? C3 C2 C1 117.5(4) . . ? C1 C2 C1 125.0(8) 23 . ? C2 C3 C4 119.1(3) . 23 ? C2 C3 C4 119.1(3) . . ? C4 C3 C4 121.6(7) 23 . ? N1 C4 C3 120.1(5) . . ? N1 C4 C5 121.0(5) . . ? C3 C4 C5 118.9(5) . . ? C4 C5 C6 110.9(5) . . ? C5 C6 C5 109.6(7) . 23 ? C8 C7 C1 116.3(7) . . ? C7 C8 C7 115.1(10) 23 . ? Cl2A C9 Cl1A 114.8(5) . . ? Cl2A C9 Cl1A 114.8(5) . 23 ? Cl1A C9 Cl1A 121.4(9) . 23 ? Cl2A C9 Cl1 118.5(7) . . ? Cl1A C9 Cl1 18.6(3) . . ? Cl1A C9 Cl1 106.5(8) 23 . ? Cl2A C9 Cl1 118.5(7) . 23 ? Cl1A C9 Cl1 106.5(8) . 23 ? Cl1A C9 Cl1 18.6(3) 23 23 ? Cl1 C9 Cl1 89.8(7) . 23 ? Cl2A C9 Cl2 27.1(5) . . ? Cl1A C9 Cl2 105.0(6) . . ? Cl1A C9 Cl2 105.0(6) 23 . ? Cl1 C9 Cl2 100.7(6) . . ? Cl1 C9 Cl2 100.7(6) 23 . ? Cl3 C10 Cl3 119.4(11) 2_565 4_565 ? Cl3 C10 Cl3 104.8(5) 2_565 . ? Cl3 C10 Cl3 104.8(5) 4_565 . ? Cl3 C10 Cl3 104.8(5) 2_565 3 ? Cl3 C10 Cl3 104.8(5) 4_565 3 ? Cl3 C10 Cl3 119.4(10) . 3 ? O1 N3 O1 119.86(15) 7_564 . ? O1 N3 O1 119.86(15) 7_564 10_665 ? O1 N3 O1 119.86(15) . 10_665 ? Cl1A Cl1 C9 67.9(11) . . ? Cl2A Cl2 C9 62.8(14) . . ? Cl1 Cl1A C9 93.5(12) . . ? Cl2 Cl2A C9 90.1(16) . . ? C10 Cl3 Cl3 37.6(2) . 2_565 ? C10 Cl3 Cl3 37.6(2) . 4_565 ? Cl3 Cl3 Cl3 66.0(6) 2_565 4_565 ? C10 Cl3 Cl3 30.3(5) . 3 ? Cl3 Cl3 Cl3 57.0(3) 2_565 3 ? Cl3 Cl3 Cl3 57.0(3) 4_565 3 ? _refine_diff_density_max 0.214 _refine_diff_density_min -0.268 _refine_diff_density_rms 0.047 #============================================================================== data_c1570 _database_code_depnum_ccdc_archive 'CCDC 228010' _audit_creation_method SHELXL _chemical_name_systematic ; Copper(II) Perchlorate 1:2 Complex with 2,2,7,7-tetramethyl-1,2,3,6,7,8-hexahydro-cinnolino[5,4,3-cde]cinnoline ; _chemical_name_common ; Copper(ii) Perchlorate 1:2 Complex with 2,2,7,7-tetramethyl- 1,2,3,6,7,8-hexahydro-cinnolino(5,4,3-cde)cinnoline ; _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C32 H40 Cl2 Cu N8 O8' _chemical_formula_weight 799.16 _chemical_melting_point ? _chemical_compound_source ? 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 Tetragonal _symmetry_space_group_name_H-M P4/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z' 'y, -x+1/2, z' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z' '-y, x-1/2, -z' _cell_length_a 12.2179(11) _cell_length_b 12.2179(11) _cell_length_c 11.7783(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1758.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour light-browm _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.510 _exptl_crystal_density_method ? _exptl_crystal_F_000 830 _exptl_absorpt_coefficient_mu 0.836 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.82368 _exptl_absorpt_correction_T_max 0.94267 _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'Siemens SMART CCD' _diffrn_measurement_method 'omega scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6056 _diffrn_reflns_av_R_equivalents 0.0286 _diffrn_reflns_av_sigmaI/netI 0.0292 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 28.99 _reflns_number_total 2198 _reflns_number_observed 1857 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 71 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0544P)^2^+2.2805P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2127 _refine_ls_number_parameters 120 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0608 _refine_ls_R_factor_obs 0.0494 _refine_ls_wR_factor_all 0.1234 _refine_ls_wR_factor_obs 0.1181 _refine_ls_goodness_of_fit_all 1.078 _refine_ls_goodness_of_fit_obs 1.121 _refine_ls_restrained_S_all 1.076 _refine_ls_restrained_S_obs 1.121 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cu1 Cu 0.2500 0.2500 0.07485(5) 0.0180(2) Uani 1 d S . Cl1 Cl 0.7500 0.2500 0.0000 0.0399(3) Uani 1 d S . Cl2 Cl 0.2500 0.2500 0.4786(2) 0.0576(5) Uani 1 d S . O1 O 0.7954(3) 0.1656(2) -0.0700(2) 0.0637(8) Uani 1 d . . O2 O 0.2500 0.2500 0.3551(6) 0.074(2) Uani 1 d S . O3 O 0.2165(9) 0.1466(6) 0.5144(7) 0.160(3) Uani 0.75 d P . N1 N 0.1494(2) 0.1239(2) 0.0521(2) 0.0207(4) Uani 1 d . . N2 N 0.1793(2) 0.0818(2) -0.0520(2) 0.0233(4) Uani 1 d . . C1 C 0.0571(2) 0.0985(2) 0.1039(2) 0.0215(5) Uani 1 d . . C2 C -0.0143(2) 0.0215(2) 0.0520(2) 0.0215(5) Uani 1 d . . C3 C -0.1144(2) -0.0119(2) 0.1030(2) 0.0232(5) Uani 1 d . . C4 C -0.1473(2) 0.0345(2) 0.2159(2) 0.0297(6) Uani 1 d . . H4A H -0.1964(2) 0.0946(2) 0.2032(2) 0.080 Uiso 1 d R . H4B H -0.1862(2) -0.0206(2) 0.2577(2) 0.080 Uiso 1 d R . C5 C -0.0480(2) 0.0741(2) 0.2862(2) 0.0301(6) Uani 1 d . . C6 C 0.0243(2) 0.1507(2) 0.2133(2) 0.0280(5) Uani 1 d . . H6A H -0.0156(2) 0.2167(2) 0.1973(2) 0.080 Uiso 1 d R . H6B H 0.0890(2) 0.1703(2) 0.2549(2) 0.080 Uiso 1 d R . C7 C -0.0918(3) 0.1397(3) 0.3875(3) 0.0451(8) Uani 1 d . . H7A H -0.1332(3) 0.0923(3) 0.4364(3) 0.080 Uiso 1 d R . H7B H -0.1381(3) 0.1976(3) 0.3606(3) 0.080 Uiso 1 d R . H7C H -0.0325(3) 0.1715(3) 0.4296(3) 0.080 Uiso 1 d R . C8 C 0.0196(3) -0.0235(3) 0.3275(3) 0.0440(8) Uani 1 d . . H8A H -0.0160(3) -0.0590(3) 0.3902(3) 0.080 Uiso 1 d R . H8B H 0.0914(3) 0.0000(3) 0.3500(3) 0.080 Uiso 1 d R . H8C H 0.0272(3) -0.0741(3) 0.2655(3) 0.080 Uiso 1 d R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0123(2) 0.0123(2) 0.0293(3) 0.000 0.000 0.000 Cl1 0.0367(5) 0.0367(5) 0.0465(8) 0.000 0.000 0.000 Cl2 0.0450(6) 0.0450(6) 0.0826(14) 0.000 0.000 0.000 O1 0.080(2) 0.0406(14) 0.071(2) -0.0075(13) 0.005(2) 0.0172(14) O2 0.066(2) 0.066(2) 0.091(5) 0.000 0.000 0.000 O3 0.238(9) 0.099(5) 0.144(6) 0.039(4) 0.040(7) -0.040(6) N1 0.0171(9) 0.0164(9) 0.0286(10) 0.0018(8) -0.0026(8) -0.0014(7) N2 0.0212(10) 0.0195(10) 0.0292(11) 0.0006(8) 0.0005(8) -0.0029(8) C1 0.0189(11) 0.0177(11) 0.0279(12) 0.0033(9) -0.0031(9) -0.0034(9) C2 0.0187(11) 0.0195(11) 0.0263(11) 0.0023(9) -0.0025(9) -0.0031(9) C3 0.0212(11) 0.0205(11) 0.0280(12) 0.0014(9) 0.0000(9) -0.0027(9) C4 0.0263(13) 0.0333(14) 0.0295(12) -0.0029(11) 0.0039(11) -0.0081(11) C5 0.0318(14) 0.0345(14) 0.0239(12) -0.0014(11) -0.0002(11) -0.0076(11) C6 0.0275(13) 0.0276(13) 0.0290(12) -0.0033(11) -0.0011(11) -0.0062(10) C7 0.048(2) 0.056(2) 0.0307(14) -0.0119(14) 0.0078(14) -0.012(2) C8 0.046(2) 0.046(2) 0.040(2) 0.0132(14) -0.0055(14) -0.0048(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 1.989(2) . ? Cu1 N1 1.989(2) 2 ? Cu1 N1 1.989(2) 3 ? Cu1 N1 1.989(2) 4 ? Cl1 O1 1.433(3) 8_655 ? Cl1 O1 1.433(3) 7_665 ? Cl1 O1 1.433(3) . ? Cl1 O1 1.433(3) 2_655 ? Cl2 O3 1.393(6) 3 ? Cl2 O3 1.393(6) . ? Cl2 O3 1.393(6) 2 ? Cl2 O3 1.393(6) 4 ? Cl2 O2 1.455(8) . ? N1 C1 1.320(3) . ? N1 N2 1.378(3) . ? N2 C3 1.312(3) 5 ? C1 C2 1.421(3) . ? C1 C6 1.492(4) . ? C2 C2 1.378(5) 5 ? C2 C3 1.422(3) . ? C3 N2 1.312(3) 5 ? C3 C4 1.499(4) . ? C4 C5 1.547(4) . ? C5 C8 1.529(4) . ? C5 C7 1.533(4) . ? C5 C6 1.548(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N1 164.50(12) . 2 ? N1 Cu1 N1 88.96(2) . 3 ? N1 Cu1 N1 88.96(2) 2 3 ? N1 Cu1 N1 88.96(2) . 4 ? N1 Cu1 N1 88.96(2) 2 4 ? N1 Cu1 N1 164.50(12) 3 4 ? O1 Cl1 O1 109.7(2) 8_655 7_665 ? O1 Cl1 O1 109.37(12) 8_655 . ? O1 Cl1 O1 109.37(12) 7_665 . ? O1 Cl1 O1 109.37(12) 8_655 2_655 ? O1 Cl1 O1 109.37(12) 7_665 2_655 ? O1 Cl1 O1 109.7(2) . 2_655 ? O3 Cl2 O3 84.8(2) 3 . ? O3 Cl2 O3 84.8(2) 3 2 ? O3 Cl2 O3 144.8(7) . 2 ? O3 Cl2 O3 144.8(7) 3 4 ? O3 Cl2 O3 84.8(2) . 4 ? O3 Cl2 O3 84.8(2) 2 4 ? O3 Cl2 O2 107.6(4) 3 . ? O3 Cl2 O2 107.6(4) . . ? O3 Cl2 O2 107.6(4) 2 . ? O3 Cl2 O2 107.6(4) 4 . ? C1 N1 N2 123.3(2) . . ? C1 N1 Cu1 130.4(2) . . ? N2 N1 Cu1 104.20(14) . . ? C3 N2 N1 119.4(2) 5 . ? N1 C1 C2 118.8(2) . . ? N1 C1 C6 121.9(2) . . ? C2 C1 C6 119.3(2) . . ? C2 C2 C1 118.6(3) 5 . ? C2 C2 C3 119.0(3) 5 . ? C1 C2 C3 122.4(2) . . ? N2 C3 C2 120.8(2) 5 . ? N2 C3 C4 119.4(2) 5 . ? C2 C3 C4 119.8(2) . . ? C3 C4 C5 112.5(2) . . ? C8 C5 C7 110.4(3) . . ? C8 C5 C4 110.5(2) . . ? C7 C5 C4 107.9(2) . . ? C8 C5 C6 109.9(2) . . ? C7 C5 C6 108.4(2) . . ? C4 C5 C6 109.8(2) . . ? C1 C6 C5 112.0(2) . . ? _refine_diff_density_max 0.777 _refine_diff_density_min -0.553 _refine_diff_density_rms 0.074 #=========================================================================