# Electronic Supplementary MAterial for CrystEngcomm # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'A Orpen' 'Chris Adams' 'Mukhtar A Kurawa' 'Matteo Lusi' _publ_contact_author_name 'A Guy Orpen' _publ_contact_author_email GUY.ORPEN@BRIS.AC.UK _publ_section_title ; Solid state synthesis of coordination compounds from basic metal salts. ; # Attachment 'combined cif.cif' data_1RT _database_code_depnum_ccdc_archive 'CCDC 691275' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H10 Cl4 Co N4' _chemical_formula_weight 338.91 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 7.8421(2) _cell_length_b 13.4343(4) _cell_length_c 12.8692(5) _cell_angle_alpha 90.00 _cell_angle_beta 92.665(2) _cell_angle_gamma 90.00 _cell_volume 1354.34(7) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 6888 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Shard _exptl_crystal_colour Blue _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.662 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 676 _exptl_absorpt_coefficient_mu 2.031 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.426 _exptl_absorpt_correction_T_max 0.694 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; 'Bruker-Nonius Roper CCD camera on \k-goniostat' ; _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 9903 _diffrn_reflns_av_R_equivalents 0.0359 _diffrn_reflns_av_sigmaI/netI 0.0228 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.55 _reflns_number_total 1551 _reflns_number_gt 1329 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement ; 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' ; _computing_data_reduction ; 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 2001)' _computing_publication_material 'SHELXTL (Bruker, 2001)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1302P)^2^+0.4300P] 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 0.30(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1551 _refine_ls_number_parameters 71 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1055 _refine_ls_R_factor_gt 0.0998 _refine_ls_wR_factor_ref 0.2155 _refine_ls_wR_factor_gt 0.2077 _refine_ls_goodness_of_fit_ref 1.308 _refine_ls_restrained_S_all 1.308 _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 Co1 Co 1.0000 1.00918(5) 0.2500 0.0574(5) Uani 1 2 d S . . Cl1 Cl 1.20767(16) 1.10996(9) 0.19167(10) 0.0838(6) Uani 1 1 d . . . Cl2 Cl 0.87165(17) 0.91235(10) 0.12553(11) 0.0864(6) Uani 1 1 d . . . C1 C 0.3860(7) 0.1178(4) 0.4486(4) 0.0841(14) Uani 1 1 d . . . H1B H 0.3715 0.0897 0.3827 0.101 Uiso 1 1 calc R A 1 C2 C 0.3623(9) 0.1439(7) 0.6088(5) 0.1093(19) Uani 1 1 d . . . H2B H 0.3264 0.1374 0.6764 0.131 Uiso 1 1 calc R B 1 N1 N 0.3224(7) 0.0866(4) 0.5320(5) 0.1009(15) Uani 1 1 d . C . H1A H 0.2607 0.0340 0.5361 0.121 Uiso 1 1 calc R . . N2 N 0.4780(7) 0.1993(5) 0.4744(7) 0.113(2) Uani 0.67(4) 1 d P C 1 H2A H 0.5358 0.2354 0.4336 0.135 Uiso 0.67(4) 1 calc PR C 1 C3 C 0.4619(7) 0.2126(5) 0.5753(7) 0.109(2) Uani 0.67(4) 1 d P C 1 H3A H 0.5133 0.2628 0.6154 0.130 Uiso 0.67(4) 1 calc PR C 1 C3' C 0.4780(7) 0.1993(5) 0.4744(7) 0.113(2) Uani 0.33(4) 1 d P C 2 H3A' H 0.5405 0.2383 0.4303 0.135 Uiso 0.33(4) 1 calc PR C 2 N2' N 0.4619(7) 0.2126(5) 0.5753(7) 0.109(2) Uani 0.33(4) 1 d P C 2 H2A' H 0.5094 0.2590 0.6124 0.130 Uiso 0.33(4) 1 calc PR C 2 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 Co1 0.0580(6) 0.0538(6) 0.0612(6) 0.000 0.0111(3) 0.000 Cl1 0.0769(8) 0.0802(9) 0.0962(9) 0.0130(5) 0.0247(6) -0.0138(5) Cl2 0.0857(9) 0.0752(9) 0.0970(9) -0.0251(5) -0.0099(6) 0.0058(5) C1 0.080(3) 0.086(3) 0.086(3) -0.009(3) 0.009(2) 0.010(2) C2 0.097(4) 0.144(6) 0.088(4) 0.002(4) 0.007(3) -0.015(4) N1 0.089(3) 0.073(3) 0.140(4) 0.013(3) 0.008(3) -0.012(2) N2 0.076(3) 0.101(4) 0.164(6) 0.045(4) 0.039(3) 0.000(3) C3 0.075(3) 0.081(3) 0.166(7) -0.040(4) -0.025(4) 0.002(3) C3' 0.076(3) 0.101(4) 0.164(6) 0.045(4) 0.039(3) 0.000(3) N2' 0.075(3) 0.081(3) 0.166(7) -0.040(4) -0.025(4) 0.002(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 Co1 Cl2 2.2630(12) 2_755 ? Co1 Cl2 2.2630(12) . ? Co1 Cl1 2.2721(11) 2_755 ? Co1 Cl1 2.2721(11) . ? C1 N1 1.275(8) . ? C1 N2 1.344(10) . ? C1 H1B 0.9300 . ? C2 N1 1.280(10) . ? C2 C3 1.296(11) . ? C2 H2B 0.9300 . ? N1 H1A 0.8600 . ? N2 C3 1.322(10) . ? N2 H2A 0.8600 . ? C3 H3A 0.9300 . ? 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 Cl2 Co1 Cl2 109.83(8) 2_755 . ? Cl2 Co1 Cl1 114.25(5) 2_755 2_755 ? Cl2 Co1 Cl1 105.92(5) . 2_755 ? Cl2 Co1 Cl1 105.92(5) 2_755 . ? Cl2 Co1 Cl1 114.25(5) . . ? Cl1 Co1 Cl1 106.84(7) 2_755 . ? N1 C1 N2 106.6(6) . . ? N1 C1 H1B 126.7 . . ? N2 C1 H1B 126.7 . . ? N1 C2 C3 107.5(6) . . ? N1 C2 H2B 126.3 . . ? C3 C2 H2B 126.3 . . ? C1 N1 C2 111.2(6) . . ? C1 N1 H1A 124.4 . . ? C2 N1 H1A 124.4 . . ? C3 N2 C1 106.2(5) . . ? C3 N2 H2A 126.9 . . ? C1 N2 H2A 126.9 . . ? C2 C3 N2 108.5(6) . . ? C2 C3 H3A 125.8 . . ? N2 C3 H3A 125.8 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.445 _refine_diff_density_min -1.377 _refine_diff_density_rms 0.487 # = = = END data_2RT _database_code_depnum_ccdc_archive 'CCDC 691276' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H10 Cl4 N4 Zn' _chemical_formula_weight 345.35 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 7.8266(2) _cell_length_b 13.4366(4) _cell_length_c 12.8885(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.705(2) _cell_angle_gamma 90.00 _cell_volume 1353.88(6) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 6997 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.66 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.36 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.694 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 688 _exptl_absorpt_coefficient_mu 2.578 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2973 _exptl_absorpt_correction_T_max 0.3952 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; 'Bruker-Nonius Roper CCD camera on \k-goniostat' ; _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 12666 _diffrn_reflns_av_R_equivalents 0.0451 _diffrn_reflns_av_sigmaI/netI 0.0244 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.56 _reflns_number_total 1562 _reflns_number_gt 1294 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement ; 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' ; _computing_data_reduction ; 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 2001)' _computing_publication_material 'SHELXTL (Bruker, 2001)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0869P)^2^+0.4846P] 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 0.061(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1562 _refine_ls_number_parameters 71 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0649 _refine_ls_R_factor_gt 0.0568 _refine_ls_wR_factor_ref 0.1448 _refine_ls_wR_factor_gt 0.1384 _refine_ls_goodness_of_fit_ref 1.179 _refine_ls_restrained_S_all 1.179 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.0000 0.00901(4) 0.2500 0.0556(3) Uani 1 2 d S . . Cl1 Cl 0.20672(13) 0.10951(8) 0.19032(9) 0.0807(4) Uani 1 1 d . . . Cl2 Cl -0.12754(14) -0.08715(8) 0.12542(9) 0.0834(4) Uani 1 1 d . . . N1 N 0.3213(5) 0.0865(3) 0.5318(4) 0.0986(13) Uani 1 1 d . C . H1A H 0.2585 0.0342 0.5359 0.118 Uiso 1 1 calc R . . C1 C 0.3851(6) 0.1182(4) 0.4492(4) 0.0838(11) Uani 1 1 d . . . H1B H 0.3710 0.0907 0.3831 0.101 Uiso 1 1 calc R A 1 C2 C 0.3644(8) 0.1442(5) 0.6085(4) 0.1077(16) Uani 1 1 d . . . H2B H 0.3300 0.1370 0.6763 0.129 Uiso 1 1 calc R B 1 N2 N 0.4779(5) 0.2001(4) 0.4765(6) 0.118(3) Uani 0.93(6) 1 d P C 1 H2A H 0.5360 0.2367 0.4363 0.141 Uiso 0.93(6) 1 calc PR C 1 C3 C 0.4611(6) 0.2122(4) 0.5768(6) 0.096(2) Uani 0.93(6) 1 d P C 1 H3A H 0.5117 0.2622 0.6175 0.116 Uiso 0.93(6) 1 calc PR C 1 C3' C 0.4779(5) 0.2001(4) 0.4765(6) 0.118(3) Uani 0.07(6) 1 d P C 2 H3A' H 0.5407 0.2397 0.4330 0.141 Uiso 0.07(6) 1 calc PR C 2 N2' N 0.4611(6) 0.2122(4) 0.5768(6) 0.096(2) Uani 0.07(6) 1 d P C 2 H2A' H 0.5079 0.2584 0.6144 0.116 Uiso 0.07(6) 1 calc PR C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0558(4) 0.0519(4) 0.0599(4) 0.000 0.0106(2) 0.000 Cl1 0.0746(6) 0.0771(7) 0.0923(7) 0.0138(5) 0.0243(5) -0.0124(4) Cl2 0.0817(7) 0.0723(7) 0.0948(7) -0.0254(5) -0.0103(5) 0.0070(5) N1 0.082(2) 0.075(2) 0.139(4) 0.017(2) 0.005(2) -0.0135(19) C1 0.078(3) 0.088(3) 0.086(3) -0.010(2) 0.009(2) 0.012(2) C2 0.104(4) 0.133(5) 0.086(3) 0.001(3) 0.000(3) -0.010(3) N2 0.073(2) 0.103(4) 0.182(6) 0.052(4) 0.045(3) 0.003(2) C3 0.064(2) 0.075(3) 0.148(6) -0.030(3) -0.017(3) -0.001(2) C3' 0.073(2) 0.103(4) 0.182(6) 0.052(4) 0.045(3) 0.003(2) N2' 0.064(2) 0.075(3) 0.148(6) -0.030(3) -0.017(3) -0.001(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 Zn1 Cl2 2.2567(10) . ? Zn1 Cl2 2.2567(10) 2 ? Zn1 Cl1 2.2694(9) . ? Zn1 Cl1 2.2694(9) 2 ? N1 C1 1.271(7) . ? N1 C2 1.289(8) . ? N1 H1A 0.8600 . ? C1 N2 1.355(8) . ? C1 H1B 0.9300 . ? C2 C3 1.267(8) . ? C2 H2B 0.9300 . ? N2 C3 1.315(8) . ? N2 H2A 0.8600 . ? C3 H3A 0.9300 . ? 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 Cl2 Zn1 Cl2 110.15(6) . 2 ? Cl2 Zn1 Cl1 113.46(4) . . ? Cl2 Zn1 Cl1 106.46(4) 2 . ? Cl2 Zn1 Cl1 106.46(4) . 2 ? Cl2 Zn1 Cl1 113.45(4) 2 2 ? Cl1 Zn1 Cl1 106.97(6) . 2 ? C1 N1 C2 110.0(5) . . ? C1 N1 H1A 125.0 . . ? C2 N1 H1A 125.0 . . ? N1 C1 N2 106.4(5) . . ? N1 C1 H1B 126.8 . . ? N2 C1 H1B 126.8 . . ? C3 C2 N1 108.9(5) . . ? C3 C2 H2B 125.5 . . ? N1 C2 H2B 125.5 . . ? C3 N2 C1 106.1(4) . . ? C3 N2 H2A 126.9 . . ? C1 N2 H2A 126.9 . . ? C2 C3 N2 108.5(5) . . ? C2 C3 H3A 125.7 . . ? N2 C3 H3A 125.7 . . ? 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 C2 N1 C1 N2 1.5(6) . . . . ? C1 N1 C2 C3 -2.0(7) . . . . ? N1 C1 N2 C3 -0.5(6) . . . . ? N1 C2 C3 N2 1.6(7) . . . . ? C1 N2 C3 C2 -0.7(6) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.737 _refine_diff_density_min -1.025 _refine_diff_density_rms 0.286 # = = = END data_2LT _database_code_depnum_ccdc_archive 'CCDC 691277' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H10 Cl4 N4 Zn' _chemical_formula_weight 345.35 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.5859(19) _cell_length_b 13.524(3) _cell_length_c 12.804(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.434(5) _cell_angle_gamma 90.00 _cell_volume 1311.1(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1521 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.750 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 688 _exptl_absorpt_coefficient_mu 2.662 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5844 _exptl_absorpt_correction_T_max 0.77 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 13753 _diffrn_reflns_av_R_equivalents 0.1255 _diffrn_reflns_av_sigmaI/netI 0.1171 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 27.49 _reflns_number_total 3002 _reflns_number_gt 1594 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_reduction 'SHELXTL (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 2001)' _computing_publication_material 'SHELXTL (Bruker, 2001)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0225P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3002 _refine_ls_number_parameters 136 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1332 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.1006 _refine_ls_wR_factor_gt 0.0802 _refine_ls_goodness_of_fit_ref 0.972 _refine_ls_restrained_S_all 0.972 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.25392(8) 0.24391(4) 0.26564(4) 0.02499(17) Uani 1 1 d . . . Cl1 Cl 0.46997(17) 0.13923(9) 0.21817(9) 0.0326(3) Uani 1 1 d . . . Cl2 Cl 0.38477(19) 0.34321(9) 0.38958(10) 0.0386(4) Uani 1 1 d . . . Cl3 Cl 0.11794(18) 0.33454(9) 0.13774(9) 0.0342(3) Uani 1 1 d . . . Cl4 Cl 0.03869(17) 0.14742(9) 0.33112(9) 0.0324(3) Uani 1 1 d . . . N1 N 0.7661(6) 0.4493(3) 0.5378(3) 0.0375(12) Uani 1 1 d . . . H1A H 0.7051 0.4862 0.5767 0.045 Uiso 1 1 calc R . . N2 N 0.9246(6) 0.3315(3) 0.4877(3) 0.0375(12) Uani 1 1 d . . . H2A H 0.9856 0.2779 0.4875 0.045 Uiso 1 1 calc R . . N3 N 0.7191(6) 0.4698(3) 0.0851(5) 0.0545(15) Uani 1 1 d . . . H3B H 0.7705 0.5182 0.1181 0.065 Uiso 1 1 calc R . . N4 N 0.6274(6) 0.3731(3) -0.0360(3) 0.0396(12) Uani 1 1 d . . . H4A H 0.6078 0.3467 -0.0967 0.048 Uiso 1 1 calc R . . C1 C 0.8480(7) 0.3670(4) 0.5684(4) 0.0359(14) Uani 1 1 d . . . H1B H 0.8506 0.3395 0.6350 0.043 Uiso 1 1 calc R . . C2 C 0.7930(7) 0.4662(4) 0.4362(4) 0.0353(14) Uani 1 1 d . . . H2B H 0.7500 0.5194 0.3963 0.042 Uiso 1 1 calc R . . C3 C 0.8928(7) 0.3926(4) 0.4037(4) 0.0369(14) Uani 1 1 d . . . H3A H 0.9328 0.3845 0.3371 0.044 Uiso 1 1 calc R . . C4 C 0.5688(7) 0.3390(4) 0.0542(4) 0.0302(13) Uani 1 1 d . . . H4B H 0.5000 0.2828 0.0620 0.036 Uiso 1 1 calc R . . C5 C 0.7204(8) 0.4542(5) -0.0153(5) 0.0495(18) Uani 1 1 d . . . H5A H 0.7763 0.4929 -0.0635 0.059 Uiso 1 1 calc R . . C6 C 0.6256(9) 0.3988(5) 0.1291(5) 0.0535(17) Uani 1 1 d . . . H6A H 0.6048 0.3931 0.1997 0.064 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0270(3) 0.0224(3) 0.0258(3) 0.0002(3) 0.0035(2) -0.0001(3) Cl1 0.0346(8) 0.0320(7) 0.0320(7) -0.0036(6) 0.0080(6) 0.0056(6) Cl2 0.0410(9) 0.0317(8) 0.0422(8) -0.0124(6) -0.0041(6) 0.0017(7) Cl3 0.0347(8) 0.0297(8) 0.0376(8) 0.0096(6) -0.0030(6) -0.0027(6) Cl4 0.0299(8) 0.0302(7) 0.0377(8) 0.0075(6) 0.0071(6) -0.0009(6) N1 0.030(3) 0.040(3) 0.044(3) -0.015(2) 0.006(2) 0.002(2) N2 0.034(3) 0.031(3) 0.048(3) 0.001(2) 0.003(2) 0.006(2) N3 0.037(4) 0.029(3) 0.096(5) -0.029(3) -0.013(3) -0.002(2) N4 0.043(3) 0.042(3) 0.034(3) -0.004(2) 0.004(2) 0.002(3) C1 0.036(4) 0.035(3) 0.037(3) 0.004(3) 0.004(3) -0.005(3) C2 0.025(3) 0.033(3) 0.046(4) 0.009(3) -0.010(3) 0.001(3) C3 0.036(4) 0.047(4) 0.027(3) 0.000(3) 0.000(3) 0.004(3) C4 0.036(4) 0.023(3) 0.032(3) 0.001(2) 0.006(3) -0.007(3) C5 0.038(4) 0.035(4) 0.079(5) 0.019(3) 0.031(4) 0.005(3) C6 0.057(5) 0.058(4) 0.044(4) 0.002(3) -0.005(3) 0.004(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 Cl3 2.2463(14) . ? Zn1 Cl2 2.2623(14) . ? Zn1 Cl1 2.2757(14) . ? Zn1 Cl4 2.2881(14) . ? N1 C1 1.322(6) . ? N1 C2 1.348(6) . ? N1 H1A 0.8600 . ? N2 C1 1.306(6) . ? N2 C3 1.366(6) . ? N2 H2A 0.8600 . ? N3 C5 1.304(7) . ? N3 C6 1.338(7) . ? N3 H3B 0.8600 . ? N4 C5 1.322(7) . ? N4 C4 1.344(6) . ? N4 H4A 0.8600 . ? C1 H1B 0.9300 . ? C2 C3 1.331(7) . ? C2 H2B 0.9300 . ? C3 H3A 0.9300 . ? C4 C6 1.307(7) . ? C4 H4B 0.9300 . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? 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 Cl3 Zn1 Cl2 110.52(5) . . ? Cl3 Zn1 Cl1 116.83(5) . . ? Cl2 Zn1 Cl1 105.30(6) . . ? Cl3 Zn1 Cl4 105.77(6) . . ? Cl2 Zn1 Cl4 111.98(5) . . ? Cl1 Zn1 Cl4 106.51(5) . . ? C1 N1 C2 109.5(5) . . ? C1 N1 H1A 125.3 . . ? C2 N1 H1A 125.3 . . ? C1 N2 C3 109.5(5) . . ? C1 N2 H2A 125.2 . . ? C3 N2 H2A 125.2 . . ? C5 N3 C6 109.5(5) . . ? C5 N3 H3B 125.2 . . ? C6 N3 H3B 125.2 . . ? C5 N4 C4 108.2(5) . . ? C5 N4 H4A 125.9 . . ? C4 N4 H4A 125.9 . . ? N2 C1 N1 107.4(5) . . ? N2 C1 H1B 126.3 . . ? N1 C1 H1B 126.3 . . ? C3 C2 N1 107.2(5) . . ? C3 C2 H2B 126.4 . . ? N1 C2 H2B 126.4 . . ? C2 C3 N2 106.5(5) . . ? C2 C3 H3A 126.8 . . ? N2 C3 H3A 126.8 . . ? C6 C4 N4 107.8(5) . . ? C6 C4 H4B 126.1 . . ? N4 C4 H4B 126.1 . . ? N3 C5 N4 107.2(5) . . ? N3 C5 H5A 126.4 . . ? N4 C5 H5A 126.4 . . ? C4 C6 N3 107.2(5) . . ? C4 C6 H6A 126.4 . . ? N3 C6 H6A 126.4 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.466 _refine_diff_density_min -0.456 _refine_diff_density_rms 0.117 # = = = END data_3RT _database_code_depnum_ccdc_archive 'CCDC 691278' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H10 Cl4 Cu N4' _chemical_formula_weight 343.52 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.7538(2) _cell_length_b 11.7092(5) _cell_length_c 14.7529(7) _cell_angle_alpha 85.756(2) _cell_angle_beta 89.684(2) _cell_angle_gamma 86.998(2) _cell_volume 1333.92(9) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 12206 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Needle _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.711 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 684 _exptl_absorpt_coefficient_mu 2.413 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.803675 _exptl_absorpt_correction_T_max 0.95 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; 'Bruker-Nonius Roper CCD camera on \k-goniostat' ; _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 20948 _diffrn_reflns_av_R_equivalents 0.0809 _diffrn_reflns_av_sigmaI/netI 0.1035 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 27.79 _reflns_number_total 6093 _reflns_number_gt 3092 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement ; 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' ; _computing_data_reduction ; 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 2001)' _computing_publication_material 'SHELXTL (Bruker, 2001)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0076P)^2^+10.3527P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6093 _refine_ls_number_parameters 272 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2020 _refine_ls_R_factor_gt 0.1060 _refine_ls_wR_factor_ref 0.1949 _refine_ls_wR_factor_gt 0.1596 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _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 0.51651(15) 0.25136(11) 0.47697(8) 0.0560(4) Uani 1 1 d . . . Cu2 Cu 1.02903(14) 0.24804(11) 0.98661(8) 0.0554(4) Uani 1 1 d . . . Cl1 Cl 0.7863(3) 0.1844(3) 0.45549(19) 0.0748(8) Uani 1 1 d . . . Cl2 Cl 0.5510(4) 0.3256(3) 0.6117(2) 0.0839(9) Uani 1 1 d . . . Cl3 Cl 0.2605(4) 0.1764(3) 0.5110(2) 0.0801(9) Uani 1 1 d . . . Cl4 Cl 0.4549(4) 0.3195(3) 0.33461(19) 0.0797(9) Uani 1 1 d . . . Cl5 Cl 1.2989(3) 0.1811(3) 1.02025(19) 0.0743(8) Uani 1 1 d . . . Cl6 Cl 1.0729(4) 0.3165(3) 0.8434(2) 0.0787(9) Uani 1 1 d . . . Cl7 Cl 0.7736(3) 0.1741(3) 0.96690(19) 0.0796(9) Uani 1 1 d . . . Cl8 Cl 0.9739(3) 0.3240(3) 1.1203(2) 0.0814(9) Uani 1 1 d . . . C1 C 0.3081(19) 0.9100(14) 0.7705(18) 0.111(5) Uani 1 1 d . . . H1A H 0.2692 0.8367 0.7664 0.133 Uiso 1 1 calc R . . C2 C 0.3900(19) 1.0610(15) 0.8226(11) 0.096(4) Uani 1 1 d . . . H2A H 0.4173 1.1150 0.8626 0.115 Uiso 1 1 calc R . . C3 C 0.3992(17) 1.0746(13) 0.7375(13) 0.095(4) Uani 1 1 d . . . H3A H 0.4377 1.1386 0.7039 0.114 Uiso 1 1 calc R . . C4 C 0.1520(19) 0.5248(15) 0.6437(8) 0.085(4) Uani 1 1 d . . . H4A H 0.2526 0.5604 0.6565 0.102 Uiso 1 1 calc R . . C5 C -0.009(2) 0.5647(12) 0.6535(9) 0.095(4) Uani 1 1 d . . . H5A H -0.0432 0.6346 0.6757 0.114 Uiso 1 1 calc R . . C6 C -0.025(2) 0.4056(12) 0.6011(8) 0.082(4) Uani 1 1 d . . . H6A H -0.0703 0.3415 0.5782 0.099 Uiso 1 1 calc R . . C7 C 0.511(4) 0.4233(13) 0.8473(10) 0.115(6) Uani 1 1 d . . . H7A H 0.4914 0.3530 0.8247 0.138 Uiso 1 1 calc R . . C8 C 0.660(2) 0.465(2) 0.8590(10) 0.103(6) Uani 1 1 d . . . H8A H 0.7684 0.4303 0.8488 0.124 Uiso 1 1 calc R . . C9 C 0.459(2) 0.5822(14) 0.8958(8) 0.083(4) Uani 1 1 d . . . H9A H 0.3996 0.6469 0.9153 0.099 Uiso 1 1 calc R . . C10 C 0.1894(19) 0.0838(13) 0.2512(14) 0.101(5) Uani 1 1 d . . . H10A H 0.2272 0.1551 0.2300 0.121 Uiso 1 1 calc R . . C11 C 0.108(2) -0.0540(19) 0.3376(11) 0.112(6) Uani 1 1 d . . . H11A H 0.0792 -0.0994 0.3893 0.135 Uiso 1 1 calc R . . C12 C 0.1013(18) -0.0800(12) 0.2542(14) 0.095(5) Uani 1 1 d . . . H12A H 0.0642 -0.1484 0.2348 0.114 Uiso 1 1 calc R . . N1 N 0.3373(15) 0.9615(16) 0.8456(8) 0.108(4) Uani 1 1 d . . . H1B H 0.3231 0.9328 0.9004 0.130 Uiso 1 1 calc R . . N2 N 0.3448(16) 0.9824(18) 0.7052(8) 0.114(5) Uani 1 1 d . . . H2B H 0.3352 0.9719 0.6484 0.137 Uiso 1 1 calc R . . N3 N -0.1100(13) 0.4898(14) 0.6270(8) 0.097(4) Uani 1 1 d . . . H3B H -0.2209 0.4974 0.6272 0.116 Uiso 1 1 calc R . . N4 N 0.1389(16) 0.4228(12) 0.6117(7) 0.093(4) Uani 1 1 d . . . H4B H 0.2237 0.3759 0.5999 0.112 Uiso 1 1 calc R . . N5 N 0.6235(19) 0.5679(13) 0.8890(7) 0.098(4) Uani 1 1 d . . . H5B H 0.6976 0.6166 0.9015 0.117 Uiso 1 1 calc R . . N6 N 0.3945(15) 0.4960(17) 0.8724(9) 0.113(5) Uani 1 1 d . . . H6B H 0.2854 0.4858 0.8727 0.135 Uiso 1 1 calc R . . N7 N 0.1638(15) 0.0497(16) 0.3338(10) 0.109(4) Uani 1 1 d . . . H7B H 0.1805 0.0887 0.3799 0.131 Uiso 1 1 calc R . . N8 N 0.1539(16) 0.0031(17) 0.2031(8) 0.116(5) Uani 1 1 d . . . H8B H 0.1639 0.0044 0.1449 0.139 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 0.0557(7) 0.0632(9) 0.0499(7) -0.0077(6) -0.0004(5) -0.0078(6) Cu2 0.0527(7) 0.0629(9) 0.0522(8) -0.0108(6) 0.0024(5) -0.0082(6) Cl1 0.0634(16) 0.090(2) 0.0703(19) -0.0061(15) -0.0043(13) 0.0091(14) Cl2 0.0697(18) 0.110(3) 0.079(2) -0.0470(18) 0.0023(14) -0.0229(16) Cl3 0.0736(18) 0.107(2) 0.0661(18) -0.0232(16) 0.0039(14) -0.0407(16) Cl4 0.0824(19) 0.091(2) 0.0610(18) 0.0167(16) -0.0031(14) 0.0082(16) Cl5 0.0579(16) 0.095(2) 0.0705(18) -0.0204(16) 0.0007(13) 0.0115(14) Cl6 0.0770(18) 0.090(2) 0.0675(19) 0.0147(16) 0.0033(14) -0.0193(15) Cl7 0.0697(17) 0.110(3) 0.0625(18) -0.0072(16) 0.0036(13) -0.0383(16) Cl8 0.0665(17) 0.103(2) 0.079(2) -0.0445(18) 0.0028(14) 0.0047(15) C1 0.109(12) 0.066(10) 0.159(18) -0.026(12) -0.018(12) -0.002(8) C2 0.137(13) 0.094(12) 0.059(9) -0.037(8) -0.012(8) 0.010(9) C3 0.105(10) 0.075(10) 0.101(13) 0.014(9) -0.003(9) -0.014(8) C4 0.088(10) 0.103(11) 0.066(8) 0.015(8) -0.021(7) -0.055(9) C5 0.138(14) 0.065(9) 0.081(10) -0.019(7) 0.000(9) 0.024(9) C6 0.123(13) 0.072(10) 0.054(8) -0.005(6) -0.004(7) -0.014(9) C7 0.22(2) 0.056(9) 0.078(10) -0.031(7) -0.001(13) -0.016(12) C8 0.069(9) 0.148(17) 0.083(10) 0.024(10) 0.019(7) 0.047(10) C9 0.093(11) 0.098(12) 0.050(7) 0.012(7) 0.010(7) 0.027(9) C10 0.121(12) 0.067(10) 0.110(13) 0.024(9) 0.031(10) 0.002(8) C11 0.120(12) 0.155(18) 0.054(10) 0.045(10) 0.022(8) -0.004(11) C12 0.106(11) 0.060(9) 0.120(15) -0.004(9) 0.009(9) -0.022(7) N1 0.100(9) 0.149(13) 0.066(8) 0.040(9) 0.018(6) 0.021(8) N2 0.104(9) 0.177(16) 0.060(8) -0.033(10) -0.009(6) 0.038(10) N3 0.065(7) 0.135(12) 0.087(8) 0.015(8) -0.014(6) -0.015(8) N4 0.078(8) 0.116(11) 0.078(8) 0.020(7) 0.022(6) 0.031(7) N5 0.109(10) 0.109(11) 0.077(8) 0.025(7) -0.017(7) -0.063(8) N6 0.074(8) 0.172(16) 0.092(10) 0.029(10) -0.016(7) -0.063(10) N7 0.089(8) 0.164(14) 0.082(10) -0.065(10) -0.014(7) 0.005(8) N8 0.109(9) 0.184(16) 0.056(8) -0.047(10) -0.020(6) 0.037(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 Cl1 2.224(3) . ? Cu1 Cl4 2.236(3) . ? Cu1 Cl2 2.251(3) . ? Cu1 Cl3 2.251(3) . ? Cu2 Cl7 2.232(3) . ? Cu2 Cl6 2.235(3) . ? Cu2 Cl5 2.241(3) . ? Cu2 Cl8 2.253(3) . ? C1 N2 1.28(2) . ? C1 N1 1.326(19) . ? C2 C3 1.255(18) . ? C2 N1 1.277(18) . ? C3 N2 1.303(18) . ? C4 C5 1.320(17) . ? C4 N4 1.325(16) . ? C5 N3 1.289(17) . ? C6 N3 1.238(15) . ? C6 N4 1.312(16) . ? C7 N6 1.279(19) . ? C7 C8 1.30(2) . ? C8 N5 1.332(19) . ? C9 N6 1.224(17) . ? C9 N5 1.280(15) . ? C10 N8 1.266(18) . ? C10 N7 1.272(17) . ? C11 C12 1.29(2) . ? C11 N7 1.309(19) . ? C12 N8 1.270(17) . ? 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 Cl1 Cu1 Cl4 98.94(11) . . ? Cl1 Cu1 Cl2 98.98(11) . . ? Cl4 Cu1 Cl2 136.43(14) . . ? Cl1 Cu1 Cl3 136.59(14) . . ? Cl4 Cu1 Cl3 97.77(12) . . ? Cl2 Cu1 Cl3 95.83(11) . . ? Cl7 Cu2 Cl6 98.20(11) . . ? Cl7 Cu2 Cl5 136.85(14) . . ? Cl6 Cu2 Cl5 98.76(11) . . ? Cl7 Cu2 Cl8 98.42(12) . . ? Cl6 Cu2 Cl8 135.90(14) . . ? Cl5 Cu2 Cl8 96.35(11) . . ? N2 C1 N1 105.3(15) . . ? C3 C2 N1 109.4(13) . . ? C2 C3 N2 107.4(14) . . ? C5 C4 N4 104.9(11) . . ? N3 C5 C4 108.1(12) . . ? N3 C6 N4 107.9(13) . . ? N6 C7 C8 107.9(14) . . ? C7 C8 N5 104.6(13) . . ? N6 C9 N5 108.2(13) . . ? N8 C10 N7 107.5(14) . . ? C12 C11 N7 105.3(13) . . ? N8 C12 C11 108.8(15) . . ? C2 N1 C1 108.2(13) . . ? C1 N2 C3 109.7(14) . . ? C6 N3 C5 110.6(13) . . ? C6 N4 C4 108.4(11) . . ? C9 N5 C8 108.3(12) . . ? C9 N6 C7 110.9(14) . . ? C10 N7 C11 109.1(13) . . ? C10 N8 C12 109.2(13) . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 27.79 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.684 _refine_diff_density_min -0.432 _refine_diff_density_rms 0.112 # = = = END data_3LT _database_code_depnum_ccdc_archive 'CCDC 691279' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H10 Cl4 Cu N4' _chemical_formula_weight 343.52 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.7642(5) _cell_length_b 11.3537(7) _cell_length_c 14.8141(9) _cell_angle_alpha 85.153(11) _cell_angle_beta 88.936(11) _cell_angle_gamma 86.470(11) _cell_volume 1298.64(14) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4726 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.757 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 684 _exptl_absorpt_coefficient_mu 2.478 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5677 _exptl_absorpt_correction_T_max 0.78 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 13909 _diffrn_reflns_av_R_equivalents 0.0409 _diffrn_reflns_av_sigmaI/netI 0.0607 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 27.51 _reflns_number_total 5909 _reflns_number_gt 4287 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_reduction 'SHELXTL (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 2001)' _computing_publication_material 'SHELXTL (Bruker, 2001)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0265P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5909 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0645 _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_ref 0.0768 _refine_ls_wR_factor_gt 0.0698 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _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 0.51223(5) 0.25630(3) 0.47079(2) 0.02370(10) Uani 1 1 d . . . Cu2 Cu 0.03763(5) 0.24593(3) 0.98690(2) 0.02361(10) Uani 1 1 d . . . Cl1 Cl 0.78274(10) 0.18294(7) 0.45002(5) 0.03113(19) Uani 1 1 d . . . Cl2 Cl 0.54291(10) 0.34222(8) 0.60068(5) 0.0334(2) Uani 1 1 d . . . Cl3 Cl 0.25735(10) 0.17730(8) 0.51091(5) 0.03080(19) Uani 1 1 d . . . Cl4 Cl 0.44876(10) 0.31506(7) 0.32646(5) 0.02863(18) Uani 1 1 d . . . Cl5 Cl 0.30705(10) 0.17469(7) 1.02299(5) 0.02987(19) Uani 1 1 d . . . Cl6 Cl 0.08715(10) 0.32113(7) 0.84469(5) 0.03027(19) Uani 1 1 d . . . Cl7 Cl -0.21654(10) 0.16766(7) 0.96607(5) 0.02899(19) Uani 1 1 d . . . Cl8 Cl -0.02454(10) 0.32374(8) 1.12004(5) 0.0332(2) Uani 1 1 d . . . C1 C 0.2901(5) 0.9095(3) 0.7760(3) 0.0506(11) Uani 1 1 d . . . H1A H 0.2371 0.8361 0.7779 0.061 Uiso 1 1 calc R . . C2 C 0.4038(5) 1.0655(4) 0.8171(2) 0.0460(10) Uani 1 1 d . . . H2A H 0.4451 1.1220 0.8539 0.055 Uiso 1 1 calc R . . C3 C 0.4075(4) 1.0713(3) 0.7276(2) 0.0368(8) Uani 1 1 d . . . H3A H 0.4522 1.1326 0.6880 0.044 Uiso 1 1 calc R . . C4 C 0.1475(4) 0.5216(3) 0.6456(2) 0.0345(8) Uani 1 1 d . . . H4A H 0.2516 0.5551 0.6601 0.041 Uiso 1 1 calc R . . C5 C -0.0121(5) 0.5678(3) 0.6568(2) 0.0369(8) Uani 1 1 d . . . H5A H -0.0439 0.6414 0.6805 0.044 Uiso 1 1 calc R . . C6 C -0.0318(5) 0.3998(3) 0.5992(2) 0.0328(8) Uani 1 1 d . . . H6A H -0.0772 0.3335 0.5751 0.039 Uiso 1 1 calc R . . C7 C 0.5094(6) 0.4233(3) 0.8447(2) 0.0491(11) Uani 1 1 d . . . H7A H 0.4901 0.3503 0.8207 0.059 Uiso 1 1 calc R . . C8 C 0.6621(5) 0.4669(4) 0.8571(2) 0.0467(10) Uani 1 1 d . . . H8A H 0.7726 0.4315 0.8436 0.056 Uiso 1 1 calc R . . C9 C 0.4613(5) 0.5906(3) 0.9013(2) 0.0386(9) Uani 1 1 d . . . H9A H 0.4027 0.6577 0.9246 0.046 Uiso 1 1 calc R . . C10 C 0.2088(4) 0.0918(3) 0.2469(2) 0.0352(8) Uani 1 1 d . . . H10A H 0.2605 0.1623 0.2245 0.042 Uiso 1 1 calc R . . C11 C 0.0980(5) -0.0446(4) 0.3381(2) 0.0449(10) Uani 1 1 d . . . H11A H 0.0583 -0.0865 0.3920 0.054 Uiso 1 1 calc R . . C12 C 0.0928(5) -0.0792(3) 0.2535(2) 0.0389(9) Uani 1 1 d . . . H12A H 0.0491 -0.1499 0.2357 0.047 Uiso 1 1 calc R . . N1 N 0.3303(4) 0.9644(3) 0.84609(19) 0.0510(9) Uani 1 1 d . . . H1B H 0.3123 0.9393 0.9031 0.061 Uiso 1 1 calc R . . N2 N 0.3355(4) 0.9733(3) 0.70297(19) 0.0405(8) Uani 1 1 d . . . H2B H 0.3216 0.9556 0.6470 0.049 Uiso 1 1 calc R . . N3 N -0.1215(3) 0.4900(3) 0.62803(17) 0.0333(7) Uani 1 1 d . . . H3B H -0.2348 0.4993 0.6288 0.040 Uiso 1 1 calc R . . N4 N 0.1320(4) 0.4165(3) 0.60918(17) 0.0332(7) Uani 1 1 d . . . H4B H 0.2184 0.3675 0.5946 0.040 Uiso 1 1 calc R . . N5 N 0.6275(4) 0.5727(3) 0.89297(18) 0.0415(8) Uani 1 1 d . . . H5B H 0.7048 0.6208 0.9080 0.050 Uiso 1 1 calc R . . N6 N 0.3894(4) 0.5015(3) 0.87241(18) 0.0399(8) Uani 1 1 d . . . H6B H 0.2774 0.4936 0.8712 0.048 Uiso 1 1 calc R . . N7 N 0.1704(4) 0.0610(3) 0.33175(17) 0.0382(7) Uani 1 1 d . . . H7B H 0.1891 0.1027 0.3776 0.046 Uiso 1 1 calc R . . N8 N 0.1631(4) 0.0081(3) 0.19854(17) 0.0342(7) Uani 1 1 d . . . H8B H 0.1758 0.0081 0.1394 0.041 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0227(2) 0.0278(2) 0.02123(19) -0.00300(16) -0.00145(15) -0.00463(17) Cu2 0.0227(2) 0.0267(2) 0.02206(19) -0.00410(16) 0.00103(15) -0.00435(17) Cl1 0.0252(4) 0.0347(5) 0.0340(4) -0.0079(4) -0.0054(3) 0.0026(4) Cl2 0.0296(4) 0.0420(5) 0.0320(4) -0.0163(4) -0.0003(3) -0.0107(4) Cl3 0.0314(4) 0.0389(5) 0.0247(4) -0.0087(3) 0.0031(3) -0.0164(4) Cl4 0.0296(4) 0.0318(5) 0.0237(4) 0.0020(3) -0.0027(3) -0.0013(4) Cl5 0.0250(4) 0.0358(5) 0.0286(4) -0.0054(3) 0.0013(3) 0.0030(4) Cl6 0.0316(5) 0.0326(5) 0.0264(4) 0.0037(3) 0.0008(3) -0.0096(4) Cl7 0.0285(4) 0.0353(5) 0.0248(4) -0.0047(3) 0.0025(3) -0.0128(4) Cl8 0.0278(4) 0.0431(5) 0.0307(4) -0.0168(4) 0.0012(3) 0.0001(4) C1 0.030(2) 0.026(2) 0.093(3) 0.006(2) -0.002(2) 0.0014(17) C2 0.048(2) 0.051(3) 0.041(2) -0.0213(19) -0.0050(18) 0.009(2) C3 0.041(2) 0.033(2) 0.0350(19) 0.0081(16) -0.0001(15) -0.0026(17) C4 0.034(2) 0.033(2) 0.0372(19) 0.0015(16) -0.0060(15) -0.0149(17) C5 0.047(2) 0.029(2) 0.0355(18) -0.0086(16) 0.0002(16) -0.0050(18) C6 0.042(2) 0.027(2) 0.0308(17) -0.0043(15) -0.0036(15) -0.0077(17) C7 0.085(3) 0.026(2) 0.038(2) -0.0041(17) 0.003(2) -0.013(2) C8 0.036(2) 0.056(3) 0.042(2) 0.015(2) 0.0106(17) 0.019(2) C9 0.050(3) 0.037(2) 0.0272(17) 0.0002(16) 0.0002(16) 0.0072(19) C10 0.033(2) 0.031(2) 0.042(2) -0.0014(16) -0.0026(15) -0.0044(16) C11 0.055(3) 0.048(3) 0.0285(18) 0.0099(17) 0.0029(17) -0.004(2) C12 0.040(2) 0.028(2) 0.051(2) -0.0103(17) -0.0056(17) -0.0068(17) N1 0.043(2) 0.073(3) 0.0303(16) 0.0210(17) 0.0073(14) 0.0129(19) N2 0.0367(18) 0.053(2) 0.0338(16) -0.0173(15) -0.0006(13) 0.0040(16) N3 0.0238(15) 0.0397(19) 0.0361(15) -0.0018(13) -0.0008(12) -0.0024(14) N4 0.0294(16) 0.0366(18) 0.0315(14) -0.0006(13) 0.0078(12) 0.0088(13) N5 0.043(2) 0.048(2) 0.0342(16) 0.0098(14) -0.0150(14) -0.0222(16) N6 0.0245(16) 0.060(2) 0.0345(16) 0.0038(15) -0.0011(12) -0.0124(16) N7 0.0427(18) 0.046(2) 0.0283(15) -0.0160(14) -0.0095(13) 0.0010(15) N8 0.0400(18) 0.0402(19) 0.0230(13) -0.0069(13) -0.0030(12) 0.0009(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 Cl1 2.2369(9) . ? Cu1 Cl4 2.2399(8) . ? Cu1 Cl2 2.2525(8) . ? Cu1 Cl3 2.2713(8) . ? Cu2 Cl6 2.2408(8) . ? Cu2 Cl7 2.2503(8) . ? Cu2 Cl5 2.2530(9) . ? Cu2 Cl8 2.2605(8) . ? C1 N2 1.306(5) . ? C1 N1 1.307(5) . ? C1 H1A 0.9500 . ? C2 C3 1.321(4) . ? C2 N1 1.348(5) . ? C2 H2A 0.9500 . ? C3 N2 1.355(4) . ? C3 H3A 0.9500 . ? C4 C5 1.329(5) . ? C4 N4 1.363(4) . ? C4 H4A 0.9500 . ? C5 N3 1.361(4) . ? C5 H5A 0.9500 . ? C6 N3 1.300(4) . ? C6 N4 1.310(4) . ? C6 H6A 0.9500 . ? C7 N6 1.331(5) . ? C7 C8 1.334(5) . ? C7 H7A 0.9500 . ? C8 N5 1.364(5) . ? C8 H8A 0.9500 . ? C9 N6 1.292(4) . ? C9 N5 1.299(4) . ? C9 H9A 0.9500 . ? C10 N8 1.306(4) . ? C10 N7 1.310(4) . ? C10 H10A 0.9500 . ? C11 C12 1.348(4) . ? C11 N7 1.351(5) . ? C11 H11A 0.9500 . ? C12 N8 1.362(4) . ? C12 H12A 0.9500 . ? N1 H1B 0.8800 . ? N2 H2B 0.8800 . ? N3 H3B 0.8800 . ? N4 H4B 0.8800 . ? N5 H5B 0.8800 . ? N6 H6B 0.8800 . ? N7 H7B 0.8800 . ? N8 H8B 0.8800 . ? 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 Cl1 Cu1 Cl4 98.83(3) . . ? Cl1 Cu1 Cl2 100.03(3) . . ? Cl4 Cu1 Cl2 137.09(4) . . ? Cl1 Cu1 Cl3 134.97(4) . . ? Cl4 Cu1 Cl3 97.68(3) . . ? Cl2 Cu1 Cl3 95.60(3) . . ? Cl6 Cu2 Cl7 98.91(3) . . ? Cl6 Cu2 Cl5 99.31(3) . . ? Cl7 Cu2 Cl5 135.90(4) . . ? Cl6 Cu2 Cl8 134.86(4) . . ? Cl7 Cu2 Cl8 98.62(3) . . ? Cl5 Cu2 Cl8 96.26(3) . . ? N2 C1 N1 108.0(4) . . ? N2 C1 H1A 126.0 . . ? N1 C1 H1A 126.0 . . ? C3 C2 N1 107.0(3) . . ? C3 C2 H2A 126.5 . . ? N1 C2 H2A 126.5 . . ? C2 C3 N2 107.1(3) . . ? C2 C3 H3A 126.4 . . ? N2 C3 H3A 126.4 . . ? C5 C4 N4 106.3(3) . . ? C5 C4 H4A 126.8 . . ? N4 C4 H4A 126.8 . . ? C4 C5 N3 107.1(3) . . ? C4 C5 H5A 126.4 . . ? N3 C5 H5A 126.4 . . ? N3 C6 N4 108.1(3) . . ? N3 C6 H6A 126.0 . . ? N4 C6 H6A 126.0 . . ? N6 C7 C8 106.9(3) . . ? N6 C7 H7A 126.5 . . ? C8 C7 H7A 126.5 . . ? C7 C8 N5 106.1(3) . . ? C7 C8 H8A 126.9 . . ? N5 C8 H8A 126.9 . . ? N6 C9 N5 108.3(3) . . ? N6 C9 H9A 125.9 . . ? N5 C9 H9A 125.9 . . ? N8 C10 N7 107.8(3) . . ? N8 C10 H10A 126.1 . . ? N7 C10 H10A 126.1 . . ? C12 C11 N7 106.9(3) . . ? C12 C11 H11A 126.6 . . ? N7 C11 H11A 126.6 . . ? C11 C12 N8 105.9(3) . . ? C11 C12 H12A 127.0 . . ? N8 C12 H12A 127.0 . . ? C1 N1 C2 109.1(3) . . ? C1 N1 H1B 125.4 . . ? C2 N1 H1B 125.4 . . ? C1 N2 C3 108.7(3) . . ? C1 N2 H2B 125.6 . . ? C3 N2 H2B 125.6 . . ? C6 N3 C5 109.2(3) . . ? C6 N3 H3B 125.4 . . ? C5 N3 H3B 125.4 . . ? C6 N4 C4 109.3(3) . . ? C6 N4 H4B 125.4 . . ? C4 N4 H4B 125.4 . . ? C9 N5 C8 108.7(3) . . ? C9 N5 H5B 125.7 . . ? C8 N5 H5B 125.7 . . ? C9 N6 C7 110.1(3) . . ? C9 N6 H6B 125.0 . . ? C7 N6 H6B 125.0 . . ? C10 N7 C11 109.7(3) . . ? C10 N7 H7B 125.2 . . ? C11 N7 H7B 125.2 . . ? C10 N8 C12 109.8(3) . . ? C10 N8 H8B 125.1 . . ? C12 N8 H8B 125.1 . . ? 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 C2 C3 N2 0.2(4) . . . . ? N4 C4 C5 N3 0.6(4) . . . . ? N6 C7 C8 N5 0.1(4) . . . . ? N7 C11 C12 N8 -0.1(4) . . . . ? N2 C1 N1 C2 -0.3(4) . . . . ? C3 C2 N1 C1 0.1(4) . . . . ? N1 C1 N2 C3 0.3(4) . . . . ? C2 C3 N2 C1 -0.3(4) . . . . ? N4 C6 N3 C5 0.5(4) . . . . ? C4 C5 N3 C6 -0.7(4) . . . . ? N3 C6 N4 C4 -0.1(4) . . . . ? C5 C4 N4 C6 -0.3(4) . . . . ? N6 C9 N5 C8 0.0(4) . . . . ? C7 C8 N5 C9 -0.1(4) . . . . ? N5 C9 N6 C7 0.1(4) . . . . ? C8 C7 N6 C9 -0.1(4) . . . . ? N8 C10 N7 C11 -0.2(4) . . . . ? C12 C11 N7 C10 0.2(4) . . . . ? N7 C10 N8 C12 0.2(4) . . . . ? C11 C12 N8 C10 -0.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.431 _refine_diff_density_min -0.415 _refine_diff_density_rms 0.089