# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2005 data_global _journal_name_full 'New J.Chem.(Nouv.J.Chim.)' _journal_coden_Cambridge 0440 _publ_section_title ; 2D and 3D Coordination Polymers based on 2,2'-bipyrimidine and Cyanide Bridging Ligands Incorporating Coordinated and Guest Ammonia Molecules. Synthesis, crystal structures magnetic properties and thermal analysis of {[(Ni(CN)4]2[(Ni(NH3)2)2(bpym)] 2H2O}n and {[Cu2(CN)2(bpym)]NH3}n ; _publ_contact_author_name 'Enrique Colacio' _publ_contact_author_address ; Prof. Enrique Colacio Departamento de Quimica Inorganica Facultad de Ciencias Universidad de Granada E-18071 Granada Spain ; _publ_contact_author_phone '+34 958 243236' _publ_contact_author_fax '+34 958 248526' _publ_contact_author_email ecolacio@ugr.es loop_ _publ_author_name _publ_author_address 'Enrique Colacio' ; Departamento de Quimica Inorganica Facultad de Ciencias Universidad de Granada E-18071 Granada Spain ; 'Francesc LLoret' ; Departamento de Quimica Inorganica Facultad de Ciencias Universidad de Valencia 46100-Burjassot, Valencia Spain ; 'Miguel Navarrete' ; Departamento de Quimica Inorganica Facultad de Ciencias Universidad de Granada E-18071 Granada Spain ; 'Antonio Romerosa' ; Departamento de Quimica Inorganica Facultad de Ciencias Universidad de Almera 04120-Almera Spain ; 'Helen Stoeckli-Evans' ; Institut de Chimie Universite de Neuchatel Universidad de Granada CH-2000 Neuchatel Switzerland ; ; J.Surez-Varela ; ; Departamento de Quimica Inorganica Facultad de Ciencias Universidad de Granada E-18071 Granada Spain ; data_compound_1 _database_code_depnum_ccdc_archive 'CCDC 265840' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H11 N8 Ni2 O' _chemical_formula_weight 352.67 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.1210(8) _cell_length_b 11.4690(10) _cell_length_c 13.5610(12) _cell_angle_alpha 90.00 _cell_angle_beta 104.623(2) _cell_angle_gamma 90.00 _cell_volume 1372.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1233 _cell_measurement_theta_min 5.829 _cell_measurement_theta_max 45.581 _exptl_crystal_description rhomboic _exptl_crystal_colour red-violet _exptl_crystal_size_max 0.189 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_min 0.066 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.707 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 716 _exptl_absorpt_coefficient_mu 2.747 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _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_% ? _diffrn_reflns_number 6205 _diffrn_reflns_av_R_equivalents 0.0645 _diffrn_reflns_av_sigmaI/netI 0.0759 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 23.27 _reflns_number_total 1967 _reflns_number_gt 1384 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX' _computing_cell_refinement 'Bruker APEX' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0236P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1967 _refine_ls_number_parameters 184 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0559 _refine_ls_R_factor_gt 0.0363 _refine_ls_wR_factor_ref 0.0767 _refine_ls_wR_factor_gt 0.0731 _refine_ls_goodness_of_fit_ref 0.877 _refine_ls_restrained_S_all 0.877 _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 Ni1 Ni 0.87457(7) 0.15170(5) 0.12527(5) 0.0337(2) Uani 1 1 d . . . Ni2 Ni 0.77926(8) 0.06700(6) 0.46891(5) 0.0383(2) Uani 1 1 d . . . N3 N 0.9578(4) -0.0218(3) 0.1211(3) 0.0310(10) Uani 1 1 d . . . N1 N 0.9386(4) 0.1481(3) -0.0161(3) 0.0307(10) Uani 1 1 d . . . N7 N 0.8328(5) 0.1296(4) 0.2654(3) 0.0420(11) Uani 1 1 d . . . N6 N 0.7987(5) 0.3208(4) 0.1022(3) 0.0449(12) Uani 1 1 d . . . N4 N 1.0910(5) 0.2095(4) 0.1999(3) 0.0479(12) Uani 1 1 d . . . H4A H 1.1421 0.2276 0.1540 0.072 Uiso 1 1 calc R . . H4B H 1.1397 0.1533 0.2405 0.072 Uiso 1 1 calc R . . H4C H 1.0836 0.2723 0.2369 0.072 Uiso 1 1 calc R . . N10 N 0.7091(6) 0.0008(4) 0.6666(3) 0.0643(15) Uani 1 1 d . . . C5 C 1.0210(6) -0.2175(5) 0.1721(4) 0.0396(14) Uani 1 1 d . . . C4 C 0.9688(6) -0.1084(5) 0.1879(4) 0.0394(14) Uani 1 1 d . . . C2 C 1.0067(5) -0.0471(4) 0.0378(3) 0.0278(12) Uani 1 1 d . . . C7 C 0.8143(6) 0.1076(4) 0.3439(4) 0.0386(14) Uani 1 1 d . . . C6 C 0.9326(6) 0.2327(5) -0.0845(4) 0.0402(15) Uani 1 1 d . . . N9 N 0.8268(5) 0.3131(4) 0.5476(3) 0.0577(14) Uani 1 1 d . . . C8 C 0.7647(6) 0.4141(5) 0.0761(4) 0.0395(14) Uani 1 1 d . . . C1O C 0.7375(6) 0.0269(4) 0.5927(4) 0.0439(14) Uani 1 1 d . . . C9 C 0.8145(6) 0.2197(5) 0.5161(4) 0.0416(14) Uani 1 1 d . . . O4 O 0.9291(9) 0.5411(6) 0.6726(4) 0.191(4) Uani 1 1 d . . . N5 N 0.6611(4) 0.0908(4) 0.0541(3) 0.0498(12) Uani 1 1 d . . . H5A H 0.6491 0.0915 -0.0131 0.075 Uiso 1 1 calc R . . H5B H 0.5915 0.1364 0.0701 0.075 Uiso 1 1 calc R . . H5C H 0.6505 0.0183 0.0746 0.075 Uiso 1 1 calc R . . H5 H 1.033(4) -0.272(3) 0.221(3) 0.015(12) Uiso 1 1 d . . . H4 H 0.938(5) -0.090(4) 0.243(3) 0.022(13) Uiso 1 1 d . . . H6 H 0.900(5) 0.299(4) -0.074(3) 0.021(14) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0437(4) 0.0279(4) 0.0347(4) 0.0011(3) 0.0195(3) 0.0019(3) Ni2 0.0549(5) 0.0301(4) 0.0349(4) -0.0019(3) 0.0208(3) -0.0068(4) N3 0.046(3) 0.024(2) 0.026(2) 0.006(2) 0.016(2) 0.000(2) N1 0.040(3) 0.022(2) 0.032(2) 0.005(2) 0.0142(19) 0.003(2) N7 0.055(3) 0.035(3) 0.043(3) 0.001(2) 0.024(2) 0.003(2) N6 0.065(3) 0.032(3) 0.046(3) 0.003(2) 0.029(2) 0.010(2) N4 0.061(3) 0.042(3) 0.042(3) 0.001(2) 0.016(2) -0.007(2) N10 0.104(4) 0.052(3) 0.044(3) 0.002(3) 0.032(3) -0.012(3) C5 0.059(4) 0.034(4) 0.031(3) 0.012(3) 0.020(3) 0.007(3) C4 0.053(4) 0.037(4) 0.033(3) -0.001(3) 0.020(3) 0.001(3) C2 0.031(3) 0.023(3) 0.031(3) 0.002(2) 0.012(2) 0.000(2) C7 0.052(4) 0.026(3) 0.043(3) -0.005(3) 0.022(3) -0.004(3) C6 0.048(4) 0.026(4) 0.049(4) 0.001(3) 0.018(3) 0.009(3) N9 0.068(4) 0.045(3) 0.069(4) -0.014(3) 0.035(3) -0.018(3) C8 0.052(4) 0.039(4) 0.035(3) -0.005(3) 0.025(3) 0.002(3) C1O 0.065(4) 0.027(3) 0.040(3) -0.003(3) 0.015(3) -0.010(3) C9 0.052(4) 0.041(4) 0.040(3) -0.006(3) 0.027(3) -0.009(3) O4 0.350(10) 0.164(6) 0.104(4) 0.049(4) 0.143(5) 0.130(6) N5 0.047(3) 0.054(3) 0.052(3) 0.000(2) 0.020(2) 0.003(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 Ni1 N7 2.046(4) . ? Ni1 N6 2.056(4) . ? Ni1 N5 2.065(4) . ? Ni1 N4 2.086(4) . ? Ni1 N3 2.136(4) . ? Ni1 N1 2.140(4) . ? Ni2 C7 1.862(5) . ? Ni2 C9 1.864(6) . ? Ni2 C8 1.867(6) 2_645 ? Ni2 C1O 1.870(5) . ? N3 C4 1.331(6) . ? N3 C2 1.347(5) . ? N1 C2 1.324(5) 3_755 ? N1 C6 1.333(6) . ? N7 C7 1.148(5) . ? N6 C8 1.145(6) . ? N10 C1O 1.137(6) . ? C5 C6 1.370(7) 3_755 ? C5 C4 1.375(7) . ? C2 N1 1.324(5) 3_755 ? C2 C2 1.474(8) 3_755 ? C6 C5 1.370(7) 3_755 ? N9 C9 1.148(6) . ? C8 Ni2 1.867(6) 2_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N7 Ni1 N6 97.13(16) . . ? N7 Ni1 N5 90.99(16) . . ? N6 Ni1 N5 90.36(18) . . ? N7 Ni1 N4 87.96(16) . . ? N6 Ni1 N4 90.86(17) . . ? N5 Ni1 N4 178.48(16) . . ? N7 Ni1 N3 93.43(15) . . ? N6 Ni1 N3 169.39(15) . . ? N5 Ni1 N3 88.40(16) . . ? N4 Ni1 N3 90.57(16) . . ? N7 Ni1 N1 170.47(16) . . ? N6 Ni1 N1 92.22(15) . . ? N5 Ni1 N1 90.76(15) . . ? N4 Ni1 N1 90.09(15) . . ? N3 Ni1 N1 77.26(14) . . ? C7 Ni2 C9 91.3(2) . . ? C7 Ni2 C8 90.5(2) . 2_645 ? C9 Ni2 C8 177.2(2) . 2_645 ? C7 Ni2 C1O 178.2(2) . . ? C9 Ni2 C1O 88.8(2) . . ? C8 Ni2 C1O 89.3(2) 2_645 . ? C4 N3 C2 115.2(4) . . ? C4 N3 Ni1 130.1(3) . . ? C2 N3 Ni1 114.7(3) . . ? C2 N1 C6 115.6(4) 3_755 . ? C2 N1 Ni1 114.8(3) 3_755 . ? C6 N1 Ni1 129.6(4) . . ? C7 N7 Ni1 174.1(4) . . ? C8 N6 Ni1 169.4(4) . . ? C6 C5 C4 116.4(5) 3_755 . ? N3 C4 C5 122.9(5) . . ? N1 C2 N3 126.8(4) 3_755 . ? N1 C2 C2 117.2(5) 3_755 3_755 ? N3 C2 C2 116.0(5) . 3_755 ? N7 C7 Ni2 177.7(5) . . ? N1 C6 C5 123.0(5) . 3_755 ? N6 C8 Ni2 176.4(5) . 2_655 ? N10 C1O Ni2 178.3(5) . . ? N9 C9 Ni2 175.1(5) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 23.27 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.355 _refine_diff_density_min -0.324 _refine_diff_density_rms 0.076 data_compound_2 _database_code_depnum_ccdc_archive 'CCDC 265841' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H9 Cu2 N7' _chemical_formula_weight 354.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/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 5.8736(12) _cell_length_b 17.266(3) _cell_length_c 12.983(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.40(2) _cell_angle_gamma 90.00 _cell_volume 1314.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 1776 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 25.88 _exptl_crystal_description rod _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.791 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 3.231 _exptl_absorpt_correction_type emirical_DIFFABS _exptl_absorpt_correction_T_min 0.127 _exptl_absorpt_correction_T_max 0.597 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 IPDS' _diffrn_measurement_method 'phi oscillation' _diffrn_detector_area_resol_mean 0.81\%A _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 5034 _diffrn_reflns_av_R_equivalents 0.2081 _diffrn_reflns_av_sigmaI/netI 0.1886 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 25.88 _reflns_number_total 1257 _reflns_number_gt 578 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'EXPOSE (Stoe IPDS Software, 2000)' _computing_cell_refinement 'CELL (Stoe IPDS Software, 2000)' _computing_data_reduction 'INTEGRATE (Stoe IPDS Software, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON99 (Spek, 1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0950P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0074(17) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1257 _refine_ls_number_parameters 88 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1331 _refine_ls_R_factor_gt 0.0743 _refine_ls_wR_factor_ref 0.1897 _refine_ls_wR_factor_gt 0.1702 _refine_ls_goodness_of_fit_ref 0.827 _refine_ls_restrained_S_all 0.827 _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 0.2414(2) 0.40080(7) 0.59167(8) 0.0476(6) Uani 1 1 d . . . N1 N 0.0579(13) 0.2916(4) 0.5890(5) 0.0372(18) Uani 1 1 d . . . N2 N 0.4136(13) 0.3358(4) 0.4791(5) 0.0375(19) Uani 1 1 d . . . C1 C -0.1226(17) 0.2697(6) 0.6387(6) 0.038(2) Uani 1 1 d . . . H1 H -0.1998 0.3070 0.6775 0.046 Uiso 1 1 calc R . . C2 C -0.2012(17) 0.1946(7) 0.6355(7) 0.048(3) Uani 1 1 d . . . H2 H -0.3277 0.1789 0.6728 0.057 Uiso 1 1 calc R . . C3 C 0.5883(18) 0.3569(6) 0.4243(7) 0.043(2) Uani 1 1 d . . . H3 H 0.6366 0.4094 0.4266 0.052 Uiso 1 1 calc R . . C4 C 0.3477(15) 0.2628(5) 0.4708(6) 0.035(2) Uani 1 1 d . . . C11A C 0.4362(17) 0.4061(5) 0.7136(6) 0.046(2) Uani 0.50 1 d P . . N11B N 0.0570(16) 0.4773(5) 0.5222(6) 0.045(2) Uani 0.50 1 d P . . N11A N 0.4362(17) 0.4061(5) 0.7136(6) 0.046(2) Uani 0.50 1 d P . . C11B C 0.0570(16) 0.4773(5) 0.5222(6) 0.045(2) Uani 0.50 1 d P . . N12 N 0.0000 0.5650(8) 0.7500 0.116(8) Uani 1 2 d S . . 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 0.0547(10) 0.0411(7) 0.0457(7) -0.0034(6) -0.0079(5) 0.0017(7) N1 0.037(5) 0.040(4) 0.034(3) -0.002(3) -0.005(3) 0.003(4) N2 0.038(5) 0.033(4) 0.040(4) 0.002(3) -0.012(3) -0.007(4) C1 0.033(6) 0.056(6) 0.025(4) -0.006(4) -0.007(4) 0.003(5) C2 0.039(7) 0.069(7) 0.034(5) 0.008(5) 0.000(4) -0.010(6) C3 0.038(7) 0.048(6) 0.043(5) 0.001(5) -0.008(4) -0.014(5) C4 0.026(6) 0.041(5) 0.036(4) 0.003(4) -0.009(3) 0.002(4) C11A 0.058(6) 0.032(4) 0.048(5) -0.005(4) -0.002(4) -0.003(5) N11B 0.047(6) 0.045(5) 0.041(5) -0.007(4) -0.011(4) -0.003(4) N11A 0.058(6) 0.032(4) 0.048(5) -0.005(4) -0.002(4) -0.003(5) C11B 0.047(6) 0.045(5) 0.041(5) -0.007(4) -0.011(4) -0.003(4) N12 0.22(2) 0.029(7) 0.113(13) 0.000 0.126(15) 0.000 _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 C11A 1.900(8) . ? Cu1 N11B 1.901(8) . ? Cu1 N2 2.143(8) . ? Cu1 N1 2.171(8) . ? N1 C1 1.328(12) . ? N1 C4 1.357(11) 7_556 ? N2 C4 1.321(11) . ? N2 C3 1.334(12) . ? C1 C2 1.377(14) . ? C2 C3 1.375(14) 7_556 ? C3 C2 1.375(14) 7_556 ? C4 N1 1.357(11) 7_556 ? C4 C4 1.480(18) 7_556 ? C11A N11A 1.171(16) 2_656 ? C11A C11A 1.171(16) 2_656 ? N11B C11B 1.163(16) 5_566 ? N11B N11B 1.163(16) 5_566 ? 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 C11A Cu1 N11B 131.3(3) . . ? C11A Cu1 N2 107.9(4) . . ? N11B Cu1 N2 108.6(3) . . ? C11A Cu1 N1 109.2(3) . . ? N11B Cu1 N1 109.1(3) . . ? N2 Cu1 N1 77.8(3) . . ? C1 N1 C4 116.5(8) . 7_556 ? C1 N1 Cu1 130.4(6) . . ? C4 N1 Cu1 113.0(6) 7_556 . ? C4 N2 C3 116.6(8) . . ? C4 N2 Cu1 114.0(6) . . ? C3 N2 Cu1 129.1(6) . . ? N1 C1 C2 121.9(9) . . ? C3 C2 C1 117.0(9) 7_556 . ? N2 C3 C2 122.5(9) . 7_556 ? N2 C4 N1 125.4(8) . 7_556 ? N2 C4 C4 118.4(10) . 7_556 ? N1 C4 C4 116.2(10) 7_556 7_556 ? N11A C11A C11A 0.0(9) 2_656 2_656 ? N11A C11A Cu1 176.1(9) 2_656 . ? C11A C11A Cu1 176.1(9) 2_656 . ? C11B N11B N11B 0.0(9) 5_566 5_566 ? C11B N11B Cu1 178.3(10) 5_566 . ? N11B N11B Cu1 178.3(10) 5_566 . ? 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 C11A Cu1 N1 C1 78.3(8) . . . . ? N11B Cu1 N1 C1 -71.0(8) . . . . ? N2 Cu1 N1 C1 -176.7(8) . . . . ? C11A Cu1 N1 C4 -98.9(6) . . . 7_556 ? N11B Cu1 N1 C4 111.7(6) . . . 7_556 ? N2 Cu1 N1 C4 6.0(5) . . . 7_556 ? C11A Cu1 N2 C4 99.8(6) . . . . ? N11B Cu1 N2 C4 -113.0(6) . . . . ? N1 Cu1 N2 C4 -6.7(5) . . . . ? C11A Cu1 N2 C3 -73.7(8) . . . . ? N11B Cu1 N2 C3 73.5(8) . . . . ? N1 Cu1 N2 C3 179.8(8) . . . . ? C4 N1 C1 C2 4.2(12) 7_556 . . . ? Cu1 N1 C1 C2 -172.9(6) . . . . ? N1 C1 C2 C3 -1.9(12) . . . 7_556 ? C4 N2 C3 C2 -2.2(12) . . . 7_556 ? Cu1 N2 C3 C2 171.2(7) . . . 7_556 ? C3 N2 C4 N1 -0.4(12) . . . 7_556 ? Cu1 N2 C4 N1 -174.8(6) . . . 7_556 ? C3 N2 C4 C4 -179.2(9) . . . 7_556 ? Cu1 N2 C4 C4 6.5(11) . . . 7_556 ? N11B Cu1 C11A N11A -151(14) . . . 2_656 ? N2 Cu1 C11A N11A -14(14) . . . 2_656 ? N1 Cu1 C11A N11A 69(14) . . . 2_656 ? N11B Cu1 C11A C11A -151(14) . . . 2_656 ? N2 Cu1 C11A C11A -14(14) . . . 2_656 ? N1 Cu1 C11A C11A 69(14) . . . 2_656 ? C11A Cu1 N11B C11B 175(100) . . . 5_566 ? N2 Cu1 N11B C11B 38(44) . . . 5_566 ? N1 Cu1 N11B C11B -45(44) . . . 5_566 ? C11A Cu1 N11B N11B 175(100) . . . 5_566 ? N2 Cu1 N11B N11B 38(44) . . . 5_566 ? N1 Cu1 N11B N11B -45(44) . . . 5_566 ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.88 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.051 _refine_diff_density_min -0.946 _refine_diff_density_rms 0.202 #===END