# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2023 data_Cudcamecn _audit_creation_method SHELXL-97 _chemical_name_systematic ; Cuprous dicyanamide acetonitile ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H3 Cu N4' _chemical_formula_weight 170.64 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 Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 13.0351(4) _cell_length_b 7.7296(2) _cell_length_c 6.1895(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 623.63(3) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.817 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 336 _exptl_absorpt_coefficient_mu 3.403 _exptl_absorpt_correction_type Face-indexed _exptl_absorpt_correction_T_min 0.7235 _exptl_absorpt_correction_T_max 0.7508 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 ? _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8260 _diffrn_reflns_av_R_equivalents 0.0320 _diffrn_reflns_av_sigmaI/netI 0.0189 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 27.89 _reflns_number_total 788 _reflns_number_gt 738 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens 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^)+(0.0129P)^2^+0.4006P] 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 788 _refine_ls_number_parameters 50 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0212 _refine_ls_R_factor_gt 0.0186 _refine_ls_wR_factor_ref 0.0425 _refine_ls_wR_factor_gt 0.0418 _refine_ls_goodness_of_fit_ref 1.119 _refine_ls_restrained_S_all 1.119 _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 0.359357(18) 0.2500 0.57370(4) 0.01636(10) Uani 1 2 d S . . N1 N 0.33870(10) 0.03255(17) 0.4227(2) 0.0203(3) Uani 1 1 d . . . C1 C 0.31659(10) -0.10334(18) 0.3620(2) 0.0151(3) Uani 1 1 d . . . N2 N 0.28630(13) -0.2500 0.2757(3) 0.0174(3) Uani 1 2 d S . . N3 N 0.45252(14) 0.2500 0.8237(3) 0.0216(4) Uani 1 2 d S . . C2 C 0.50012(17) 0.2500 0.9775(4) 0.0211(4) Uani 1 2 d S . . C3 C 0.56244(18) 0.2500 1.1732(4) 0.0295(5) Uani 1 2 d S . . H3A H 0.6292 0.1972 1.1424 0.044 Uiso 0.50 1 calc PR . . H3B H 0.5275 0.1835 1.2861 0.044 Uiso 0.50 1 calc PR . . H3C H 0.5725 0.3693 1.2225 0.044 Uiso 0.50 1 calc PR . . 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 0.01917(15) 0.01139(15) 0.01852(14) 0.000 -0.00105(10) 0.000 N1 0.0248(6) 0.0152(7) 0.0209(6) -0.0005(5) -0.0028(5) 0.0018(5) C1 0.0152(6) 0.0154(7) 0.0147(6) 0.0018(5) -0.0002(5) 0.0026(5) N2 0.0193(8) 0.0120(8) 0.0209(8) 0.000 -0.0045(7) 0.000 N3 0.0187(8) 0.0231(10) 0.0230(10) 0.000 -0.0021(7) 0.000 C2 0.0187(10) 0.0220(11) 0.0226(11) 0.000 0.0016(8) 0.000 C3 0.0236(11) 0.0438(15) 0.0212(11) 0.000 -0.0051(9) 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 N1 1.9418(13) 7_565 ? Cu1 N1 1.9418(13) . ? Cu1 N3 1.9669(18) . ? Cu1 N2 2.2734(17) 2 ? N1 C1 1.152(2) . ? C1 N2 1.3139(17) . ? N2 C1 1.3139(17) 7 ? N2 Cu1 2.2735(17) 2_554 ? N3 C2 1.136(3) . ? C2 C3 1.459(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 119.90(7) 7_565 . ? N1 Cu1 N3 117.65(4) 7_565 . ? N1 Cu1 N3 117.65(4) . . ? N1 Cu1 N2 98.56(4) 7_565 2 ? N1 Cu1 N2 98.56(4) . 2 ? N3 Cu1 N2 94.76(7) . 2 ? C1 N1 Cu1 168.73(12) . . ? N1 C1 N2 173.88(15) . . ? C1 N2 C1 119.26(17) 7 . ? C1 N2 Cu1 118.33(9) 7 2_554 ? C1 N2 Cu1 118.33(9) . 2_554 ? C2 N3 Cu1 174.97(18) . . ? N3 C2 C3 179.3(2) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.242 _refine_diff_density_min -0.274 _refine_diff_density_rms 0.057 _publ_contact_author ; Dr. Stuart Batten Department of Chemistry P.O. Box 23 Monash University Clayton, Vic. 3800 AUSTRALIA ; _publ_contact_author_phone ' +61 3 9905 4606 ' _publ_contact_author_fax ' +61 3 9905 4597 ' _publ_contact_author_email ' stuart.batten@sci.monash.edu.au ' loop_ _publ_author_name _publ_author_address ' Batten, Stuart R. ' ; Department of Chemistry P.O. Box 23 Monash University Clayton, Vic. 3800 AUSTRALIA ; _publ_section_title ; Cuprous dicyanamide coordination polymers: ladders, sheets, layers, diamond-like networks and unusual interpenetration ; #=END data_Cudcame4pyz _audit_creation_method SHELXL-97 _chemical_name_systematic ; Cuprous dicyanamide hemi(tetramethylpyrazine) ; _chemical_name_common Cu(dca)(tmp)0.5 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H6 Cu N4' _chemical_formula_weight 197.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _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 3.8969(1) _cell_length_b 18.5279(9) _cell_length_c 9.9978(5) _cell_angle_alpha 90.00 _cell_angle_beta 92.039(3) _cell_angle_gamma 90.00 _cell_volume 721.40(5) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description acicular _exptl_crystal_colour yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.025 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.820 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 396 _exptl_absorpt_coefficient_mu 2.956 _exptl_absorpt_correction_type Face-indexed _exptl_absorpt_correction_T_min 0.809 _exptl_absorpt_correction_T_max 0.926 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Nonius KappaCCD' _diffrn_measurement_method Phi-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9313 _diffrn_reflns_av_R_equivalents 0.052 _diffrn_reflns_av_sigmaI/netI 0.0469 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 27.87 _reflns_number_total 1658 _reflns_number_gt 1348 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0000P)^2^+0.8543P] 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 1658 _refine_ls_number_parameters 102 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0529 _refine_ls_R_factor_gt 0.0335 _refine_ls_wR_factor_ref 0.0594 _refine_ls_wR_factor_gt 0.0549 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _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 0.12216(8) 0.139188(16) 0.28700(3) 0.01611(10) Uani 1 1 d . . . N1 N 0.3705(6) 0.13946(12) 0.1256(2) 0.0203(5) Uani 1 1 d . . . N2 N 0.6595(6) 0.15706(11) -0.0863(2) 0.0174(5) Uani 1 1 d . . . N3 N 0.9117(6) 0.27160(12) -0.1588(2) 0.0203(5) Uani 1 1 d . . . N4 N 0.0673(5) 0.05512(10) 0.41063(19) 0.0116(4) Uani 1 1 d . . . C1 C 0.5079(6) 0.15106(12) 0.0280(2) 0.0133(5) Uani 1 1 d . . . C2 C 0.7890(6) 0.21960(13) -0.1196(2) 0.0138(5) Uani 1 1 d . . . C3 C -0.0841(6) -0.00676(12) 0.3674(2) 0.0115(5) Uani 1 1 d . . . C4 C -0.1727(6) -0.01396(13) 0.2209(2) 0.0144(5) Uani 1 1 d . . . H4A H -0.4228 -0.0148 0.2070 0.022 Uiso 1 1 calc R . . H4B H -0.0754 -0.0589 0.1872 0.022 Uiso 1 1 calc R . . H4C H -0.0777 0.0271 0.1728 0.022 Uiso 1 1 calc R . . C5 C 0.1537(6) 0.06179(12) 0.5420(2) 0.0112(5) Uani 1 1 d . . . C6 C 0.3214(7) 0.13097(13) 0.5869(2) 0.0164(5) Uani 1 1 d . . . H6A H 0.4509 0.1512 0.5135 0.025 Uiso 1 1 calc R . . H6B H 0.4779 0.1214 0.6637 0.025 Uiso 1 1 calc R . . H6C H 0.1449 0.1654 0.6128 0.025 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 0.02216(18) 0.01255(15) 0.01382(16) 0.00021(14) 0.00364(12) -0.00026(14) N1 0.0264(13) 0.0177(11) 0.0171(11) 0.0007(10) 0.0038(10) -0.0022(10) N2 0.0251(12) 0.0125(11) 0.0148(11) -0.0020(8) 0.0049(9) -0.0039(9) N3 0.0251(13) 0.0170(11) 0.0190(12) 0.0001(10) 0.0044(10) -0.0024(10) N4 0.0118(10) 0.0114(10) 0.0118(10) -0.0018(8) 0.0029(8) 0.0023(8) C1 0.0149(13) 0.0075(12) 0.0173(13) -0.0020(9) -0.0030(10) 0.0010(9) C2 0.0147(13) 0.0175(13) 0.0091(12) -0.0036(10) 0.0004(10) 0.0044(10) C3 0.0090(12) 0.0110(12) 0.0146(13) -0.0021(9) 0.0027(10) 0.0032(9) C4 0.0154(14) 0.0142(12) 0.0135(12) 0.0006(10) -0.0004(10) 0.0001(10) C5 0.0080(12) 0.0118(12) 0.0138(12) -0.0019(10) 0.0011(10) 0.0015(9) C6 0.0201(13) 0.0132(13) 0.0158(13) -0.0006(10) 0.0010(10) -0.0033(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 N1 1.911(2) . ? Cu1 N3 1.931(2) 4_466 ? Cu1 N4 2.005(2) . ? N1 C1 1.150(3) . ? N2 C1 1.310(3) . ? N2 C2 1.312(3) . ? N3 C2 1.151(3) . ? N3 Cu1 1.931(2) 4_665 ? N4 C5 1.349(3) . ? N4 C3 1.353(3) . ? C3 C5 1.397(3) 3_556 ? C3 C4 1.499(3) . ? C5 C3 1.397(3) 3_556 ? C5 C6 1.500(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 N3 117.88(9) . 4_466 ? N1 Cu1 N4 126.23(9) . . ? N3 Cu1 N4 115.87(8) 4_466 . ? C1 N1 Cu1 169.2(2) . . ? C1 N2 C2 119.1(2) . . ? C2 N3 Cu1 176.4(2) . 4_665 ? C5 N4 C3 118.6(2) . . ? C5 N4 Cu1 120.02(15) . . ? C3 N4 Cu1 121.10(16) . . ? N1 C1 N2 173.9(3) . . ? N3 C2 N2 174.0(3) . . ? N4 C3 C5 120.3(2) . 3_556 ? N4 C3 C4 118.0(2) . . ? C5 C3 C4 121.7(2) 3_556 . ? N4 C5 C3 121.1(2) . 3_556 ? N4 C5 C6 117.4(2) . . ? C3 C5 C6 121.5(2) 3_556 . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.454 _refine_diff_density_min -0.354 _refine_diff_density_rms 0.092 _publ_contact_author ; Dr. Stuart Batten Department of Chemistry P.O. Box 23 Monash University Clayton, Vic. 3800 AUSTRALIA ; _publ_contact_author_phone ' +61 3 9905 4606 ' _publ_contact_author_fax ' +61 3 9905 4597 ' _publ_contact_author_email ' stuart.batten@sci.monash.edu.au ' loop_ _publ_author_name _publ_author_address ' Batten, Stuart R. ' ; Department of Chemistry P.O. Box 23 Monash University Clayton, Vic. 3800 AUSTRALIA ; _publ_section_title ; Cuprous dicyanamide coordination polymers: ladders, sheets, layers, diamond-like networks and unusual interpenetration ; #=END data_Cudcabipyladd _audit_creation_method SHELXL-97 _chemical_name_systematic ; Di(copper(i)) bis(dicyanamide) 4,4'-bipyridine bis(acetonitrile) hemi(4,4'-bipyridine) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H18 Cu2 N11' _chemical_formula_weight 575.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 C2/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 29.5142(7) _cell_length_b 7.5761(3) _cell_length_c 11.3905(4) _cell_angle_alpha 90.00 _cell_angle_beta 106.141(2) _cell_angle_gamma 90.00 _cell_volume 2446.54(14) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description cube _exptl_crystal_colour yellow-orange _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.563 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1164 _exptl_absorpt_coefficient_mu 1.774 _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 123(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 ? _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10124 _diffrn_reflns_av_R_equivalents 0.0275 _diffrn_reflns_av_sigmaI/netI 0.0384 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 29.14 _reflns_number_total 3407 _reflns_number_gt 2722 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens 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^)+(0.0952P)^2^+12.1942P] 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 3407 _refine_ls_number_parameters 169 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0753 _refine_ls_R_factor_gt 0.0567 _refine_ls_wR_factor_ref 0.1836 _refine_ls_wR_factor_gt 0.1618 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _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 0.33661(2) 0.0000 0.59917(6) 0.0248(2) Uani 1 2 d S . . Cu2 Cu 0.32968(2) 0.0000 0.12128(6) 0.0318(2) Uani 1 2 d S . . N1 N 0.34019(13) 0.2170(4) 0.5068(3) 0.0327(7) Uani 1 1 d . . . C2 C 0.34776(14) 0.3527(5) 0.4709(3) 0.0303(8) Uani 1 1 d . . . N3 N 0.3575(2) 0.5000 0.4234(5) 0.0409(13) Uani 1 2 d S . . N4 N 0.28521(16) 0.0000 0.6830(4) 0.0306(10) Uani 1 2 d S . . C5 C 0.26200(18) 0.0000 0.7472(5) 0.0286(11) Uani 1 2 d S . . C6 C 0.2326(2) 0.0000 0.8318(6) 0.0416(14) Uani 1 2 d S . . H6A H 0.2529 0.0000 0.9161 0.062 Uiso 1 2 calc SR . . H6B H 0.2127 -0.1056 0.8179 0.062 Uiso 0.50 1 calc PR . . H6C H 0.2127 0.1056 0.8179 0.062 Uiso 0.50 1 calc PR . . N11 N 0.39651(16) 0.0000 0.7493(4) 0.0296(10) Uani 1 2 d S . . C12 C 0.4395(2) 0.0000 0.7347(6) 0.080(4) Uani 1 2 d S . . H12A H 0.4421 0.0000 0.6535 0.097 Uiso 1 2 calc SR . . C13 C 0.4804(2) 0.0000 0.8279(6) 0.079(4) Uani 1 2 d S . . H13A H 0.5100 0.0000 0.8105 0.095 Uiso 1 2 calc SR . . C14 C 0.47819(18) 0.0000 0.9475(5) 0.0281(11) Uani 1 2 d S . . C15 C 0.4341(2) 0.0000 0.9635(5) 0.0446(17) Uani 1 2 d S . . H15A H 0.4305 0.0000 1.0438 0.054 Uiso 1 2 calc SR . . C16 C 0.39473(19) 0.0000 0.8642(5) 0.0408(15) Uani 1 2 d S . . H16A H 0.3646 0.0000 0.8790 0.049 Uiso 1 2 calc SR . . N21 N 0.33168(12) 0.2169(5) 0.0265(3) 0.0371(8) Uani 1 1 d . . . C22 C 0.33722(13) 0.3520(6) -0.0122(3) 0.0309(8) Uani 1 1 d . . . N23 N 0.34448(17) 0.5000 -0.0640(4) 0.0347(10) Uani 1 2 d S . . N24 N 0.28024(17) 0.0000 0.2080(4) 0.0356(11) Uani 1 2 d S . . C25 C 0.25664(19) 0.0000 0.2708(5) 0.0303(11) Uani 1 2 d S . . C26 C 0.2264(2) 0.0000 0.3531(5) 0.0368(13) Uani 1 2 d S . . H26A H 0.2460 0.0000 0.4380 0.055 Uiso 1 2 calc SR . . H26B H 0.2064 -0.1056 0.3382 0.055 Uiso 0.50 1 calc PR . . H26C H 0.2064 0.1056 0.3382 0.055 Uiso 0.50 1 calc PR . . N31 N 0.39294(16) 0.0000 0.2607(4) 0.0332(10) Uani 1 2 d S . . C32 C 0.41381(18) 0.1478(7) 0.3087(5) 0.0617(16) Uani 1 1 d . . . H32A H 0.3996 0.2565 0.2767 0.074 Uiso 1 1 calc R . . C33 C 0.45532(18) 0.1535(7) 0.4033(5) 0.0638(17) Uani 1 1 d . . . H33A H 0.4684 0.2640 0.4348 0.077 Uiso 1 1 calc R . . C34 C 0.47735(13) 0.0000 0.4511(3) 0.0307(11) Uani 1 2 d S . . N41 N 0.51868(13) 0.5000 0.3261(3) 0.117(4) Uiso 1 2 d SR . . C42 C 0.47345(13) 0.5000 0.2464(3) 0.100(4) Uiso 1 2 d SR . . C43 C 0.46722(13) 0.5000 0.1209(3) 0.071(2) Uiso 1 2 d SR . . C44 C 0.50622(13) 0.5000 0.0750(3) 0.086(3) Uiso 1 2 d SR . . C45 C 0.55145(13) 0.5000 0.1547(3) 0.088(3) Uiso 1 2 d SR . . C46 C 0.55768(13) 0.5000 0.2802(3) 0.115(4) Uiso 1 2 d SR . . 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 0.0301(3) 0.0208(3) 0.0260(3) 0.000 0.0117(3) 0.000 Cu2 0.0298(4) 0.0406(4) 0.0273(4) 0.000 0.0118(3) 0.000 N1 0.052(2) 0.0195(15) 0.0303(15) -0.0002(12) 0.0178(14) 0.0018(14) C2 0.047(2) 0.0217(18) 0.0257(16) -0.0028(14) 0.0154(15) 0.0034(15) N3 0.076(4) 0.021(2) 0.036(3) 0.000 0.032(3) 0.000 N4 0.029(2) 0.034(2) 0.033(2) 0.000 0.0162(19) 0.000 C5 0.028(2) 0.032(3) 0.027(2) 0.000 0.009(2) 0.000 C6 0.036(3) 0.060(4) 0.036(3) 0.000 0.022(3) 0.000 N11 0.028(2) 0.041(3) 0.024(2) 0.000 0.0126(17) 0.000 C12 0.034(3) 0.194(12) 0.019(3) 0.000 0.015(3) 0.000 C13 0.023(3) 0.196(11) 0.022(3) 0.000 0.013(2) 0.000 C14 0.028(3) 0.037(3) 0.023(2) 0.000 0.014(2) 0.000 C15 0.030(3) 0.088(5) 0.022(2) 0.000 0.016(2) 0.000 C16 0.024(3) 0.075(5) 0.027(3) 0.000 0.014(2) 0.000 N21 0.0402(18) 0.041(2) 0.0356(17) 0.0025(15) 0.0195(15) 0.0050(15) C22 0.0258(17) 0.043(2) 0.0254(17) -0.0008(16) 0.0103(14) 0.0041(16) N23 0.037(3) 0.038(3) 0.032(2) 0.000 0.015(2) 0.000 N24 0.030(2) 0.050(3) 0.028(2) 0.000 0.0101(19) 0.000 C25 0.028(3) 0.038(3) 0.026(2) 0.000 0.009(2) 0.000 C26 0.031(3) 0.054(4) 0.029(3) 0.000 0.015(2) 0.000 N31 0.028(2) 0.049(3) 0.025(2) 0.000 0.0106(18) 0.000 C32 0.055(3) 0.047(3) 0.063(3) -0.027(3) -0.016(2) 0.025(2) C33 0.054(3) 0.043(3) 0.071(3) -0.032(3) -0.022(3) 0.021(2) C34 0.031(3) 0.044(3) 0.021(2) 0.000 0.014(2) 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 N1 1.971(3) . ? Cu1 N1 1.971(3) 6 ? Cu1 N4 2.004(4) . ? Cu1 N11 2.090(5) . ? Cu2 N21 1.976(4) . ? Cu2 N21 1.976(4) 6 ? Cu2 N24 1.977(5) . ? Cu2 N31 2.088(5) . ? N1 C2 1.151(5) . ? C2 N3 1.307(4) . ? N3 C2 1.307(4) 6_565 ? N4 C5 1.133(7) . ? C5 C6 1.465(7) . ? N11 C12 1.323(8) . ? N11 C16 1.325(7) . ? C12 C13 1.367(9) . ? C13 C14 1.381(7) . ? C14 C15 1.363(7) . ? C14 C14 1.494(10) 5_657 ? C15 C16 1.378(8) . ? N21 C22 1.144(5) . ? C22 N23 1.312(5) . ? N23 C22 1.312(5) 6_565 ? N24 C25 1.128(7) . ? C25 C26 1.464(7) . ? N31 C32 1.321(6) 6 ? N31 C32 1.321(6) . ? C32 C33 1.389(6) . ? C33 C34 1.369(5) . ? C34 C33 1.369(5) 6 ? C34 C34 1.484(7) 5_656 ? N41 C42 1.3900 . ? N41 C46 1.3900 . ? C42 C43 1.3900 . ? C43 C44 1.3900 . ? C44 C45 1.3900 . ? C44 C44 1.645(7) 5_665 ? C45 C46 1.3900 . ? 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 113.09(18) . 6 ? N1 Cu1 N4 114.47(11) . . ? N1 Cu1 N4 114.47(11) 6 . ? N1 Cu1 N11 106.14(12) . . ? N1 Cu1 N11 106.14(12) 6 . ? N4 Cu1 N11 100.99(18) . . ? N21 Cu2 N21 112.5(2) . 6 ? N21 Cu2 N24 114.29(11) . . ? N21 Cu2 N24 114.29(11) 6 . ? N21 Cu2 N31 105.03(12) . . ? N21 Cu2 N31 105.03(12) 6 . ? N24 Cu2 N31 104.35(18) . . ? C2 N1 Cu1 168.3(3) . . ? N1 C2 N3 175.4(4) . . ? C2 N3 C2 117.4(5) . 6_565 ? C5 N4 Cu1 168.9(5) . . ? N4 C5 C6 179.1(6) . . ? C12 N11 C16 115.2(5) . . ? C12 N11 Cu1 121.3(4) . . ? C16 N11 Cu1 123.5(4) . . ? N11 C12 C13 124.9(6) . . ? C12 C13 C14 119.5(5) . . ? C15 C14 C13 116.1(5) . . ? C15 C14 C14 122.3(6) . 5_657 ? C13 C14 C14 121.6(6) . 5_657 ? C14 C15 C16 120.6(5) . . ? N11 C16 C15 123.7(5) . . ? C22 N21 Cu2 169.7(4) . . ? N21 C22 N23 175.3(4) . . ? C22 N23 C22 117.4(5) . 6_565 ? C25 N24 Cu2 171.2(5) . . ? N24 C25 C26 179.5(6) . . ? C32 N31 C32 116.0(5) 6 . ? C32 N31 Cu2 122.0(3) 6 . ? C32 N31 Cu2 122.0(3) . . ? N31 C32 C33 123.8(5) . . ? C34 C33 C32 120.1(4) . . ? C33 C34 C33 116.3(5) . 6 ? C33 C34 C34 121.9(2) . 5_656 ? C33 C34 C34 121.9(2) 6 5_656 ? C42 N41 C46 120.0 . . ? N41 C42 C43 120.0 . . ? C42 C43 C44 120.0 . . ? C45 C44 C43 120.0 . . ? C45 C44 C44 125.1(3) . 5_665 ? C43 C44 C44 114.9(3) . 5_665 ? C44 C45 C46 120.0 . . ? C45 C46 N41 120.0 . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 29.14 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 2.114 _refine_diff_density_min -1.077 _refine_diff_density_rms 0.178 _publ_contact_author ; Dr. Stuart Batten Department of Chemistry P.O. Box 23 Monash University Clayton, Vic. 3800 AUSTRALIA ; _publ_contact_author_phone ' +61 3 9905 4606 ' _publ_contact_author_fax ' +61 3 9905 4597 ' _publ_contact_author_email ' stuart.batten@sci.monash.edu.au ' loop_ _publ_author_name _publ_author_address ' Batten, Stuart R. ' ; Department of Chemistry P.O. Box 23 Monash University Clayton, Vic. 3800 AUSTRALIA ; _publ_section_title ; Cuprous dicyanamide coordination polymers: ladders, sheets, layers, diamond-like networks and unusual interpenetration ; #=END data_Cudcabipylayer _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tetra(copper(I)) tetrakis(dicyanamide) tris(4,4'-bipyridine) bis(acetonitrile) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H30 Cu4 N20' _chemical_formula_weight 1069.02 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.2104(3) _cell_length_b 10.0447(3) _cell_length_c 13.9494(4) _cell_angle_alpha 98.995(2) _cell_angle_beta 93.178(2) _cell_angle_gamma 101.633(2) _cell_volume 1108.43(6) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description irregular _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.602 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 538 _exptl_absorpt_coefficient_mu 1.950 _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 123(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 ? _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10456 _diffrn_reflns_av_R_equivalents 0.0351 _diffrn_reflns_av_sigmaI/netI 0.0507 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 31.98 _reflns_number_total 6753 _reflns_number_gt 5082 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens 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^)+(0.0440P)^2^+0.4770P] 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 6753 _refine_ls_number_parameters 299 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0611 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.0997 _refine_ls_wR_factor_gt 0.0897 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu -1.17525(3) -0.80825(3) -0.600605(19) 0.02252(8) Uani 1 1 d . . . Cu2 Cu -0.59356(3) -0.26825(3) 0.135967(19) 0.02330(8) Uani 1 1 d . . . N13 N -0.7078(2) -0.9280(2) -0.65870(14) 0.0297(4) Uani 1 1 d . . . C11 C -0.8467(3) -0.8842(2) -0.65963(15) 0.0210(4) Uani 1 1 d . . . N11 N -0.9634(2) -0.83642(19) -0.65386(14) 0.0272(4) Uani 1 1 d . . . C12 C -0.6898(3) -1.0321(2) -0.72300(16) 0.0233(4) Uani 1 1 d . . . N12 N -0.6615(2) -1.1234(2) -0.77519(15) 0.0297(4) Uani 1 1 d . . . N23 N -1.5616(3) -0.6367(2) -0.7369(2) 0.0473(6) Uani 1 1 d . . . C21 C -1.4324(3) -0.6708(2) -0.69487(17) 0.0272(5) Uani 1 1 d . . . N21 N -1.3283(2) -0.7113(2) -0.65815(14) 0.0281(4) Uani 1 1 d . . . C22 C -1.5432(3) -0.5203(2) -0.77021(16) 0.0267(4) Uani 1 1 d . . . N22 N -1.5452(3) -0.4231(2) -0.80355(14) 0.0289(4) Uani 1 1 d . . . N31 N -1.0959(2) -0.70805(18) -0.45898(13) 0.0221(4) Uani 1 1 d . . . C30 C -1.1261(3) -0.5844(2) -0.42211(16) 0.0222(4) Uani 1 1 d . . . H30A H -1.1905 -0.5424 -0.4622 0.027 Uiso 1 1 calc R . . C31 C -1.0686(3) -0.5151(2) -0.32924(15) 0.0216(4) Uani 1 1 d . . . H31A H -1.0941 -0.4281 -0.3064 0.026 Uiso 1 1 calc R . . C32 C -0.9726(2) -0.5743(2) -0.26913(15) 0.0195(4) Uani 1 1 d . . . C33 C -0.9406(3) -0.7028(2) -0.30717(16) 0.0250(4) Uani 1 1 d . . . H33A H -0.8754 -0.7468 -0.2691 0.030 Uiso 1 1 calc R . . C34 C -1.0048(3) -0.7651(2) -0.40067(16) 0.0243(4) Uani 1 1 d . . . H34A H -0.9834 -0.8531 -0.4250 0.029 Uiso 1 1 calc R . . C35 C -0.7873(3) -0.2963(2) -0.05566(16) 0.0229(4) Uani 1 1 d . . . H35A H -0.7617 -0.1983 -0.0413 0.027 Uiso 1 1 calc R . . C36 C -0.8642(3) -0.3590(2) -0.14682(15) 0.0214(4) Uani 1 1 d . . . H36A H -0.8911 -0.3048 -0.1930 0.026 Uiso 1 1 calc R . . C37 C -0.9020(2) -0.5028(2) -0.17018(15) 0.0192(4) Uani 1 1 d . . . C38 C -0.8651(3) -0.5752(2) -0.09691(15) 0.0228(4) Uani 1 1 d . . . H38A H -0.8930 -0.6732 -0.1083 0.027 Uiso 1 1 calc R . . C39 C -0.7883(3) -0.5042(2) -0.00823(16) 0.0237(4) Uani 1 1 d . . . H39A H -0.7634 -0.5558 0.0401 0.028 Uiso 1 1 calc R . . N32 N -0.7466(2) -0.36556(17) 0.01380(13) 0.0213(3) Uani 1 1 d . . . N41 N -0.3839(2) -0.16348(18) 0.07990(13) 0.0228(4) Uani 1 1 d . . . C40 C -0.3492(3) -0.1876(2) -0.01304(16) 0.0263(4) Uani 1 1 d . . . H40A H -0.4305 -0.2509 -0.0582 0.032 Uiso 1 1 calc R . . C41 C -0.2039(3) -0.1270(2) -0.04754(16) 0.0258(4) Uani 1 1 d . . . H41A H -0.1879 -0.1479 -0.1147 0.031 Uiso 1 1 calc R . . C42 C -0.0794(3) -0.0343(2) 0.01641(15) 0.0199(4) Uani 1 1 d . . . C43 C -0.1153(3) -0.0092(2) 0.11359(15) 0.0230(4) Uani 1 1 d . . . H43A H -0.0353 0.0521 0.1606 0.028 Uiso 1 1 calc R . . C44 C -0.2657(3) -0.0725(2) 0.14181(16) 0.0248(4) Uani 1 1 d . . . H44A H -0.2873 -0.0512 0.2081 0.030 Uiso 1 1 calc R . . N51 N -1.2995(2) -0.99776(19) -0.58594(14) 0.0276(4) Uani 1 1 d . . . C52 C -1.3711(3) -1.1025(2) -0.57422(15) 0.0241(4) Uani 1 1 d . . . C53 C -1.4630(3) -1.2363(2) -0.56009(18) 0.0341(5) Uani 1 1 d . . . H53A H -1.5256 -1.2249 -0.5026 0.051 Uiso 1 1 calc R . . H53B H -1.3847 -1.2959 -0.5504 0.051 Uiso 1 1 calc R . . H53C H -1.5409 -1.2785 -0.6177 0.051 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 0.02173(13) 0.02433(13) 0.02198(14) 0.00165(10) -0.00124(10) 0.00866(10) Cu2 0.02862(15) 0.02126(13) 0.02052(14) 0.00053(10) 0.00061(10) 0.00925(10) N13 0.0253(9) 0.0295(9) 0.0313(11) -0.0093(8) -0.0049(8) 0.0123(8) C11 0.0232(10) 0.0200(9) 0.0177(10) -0.0023(7) -0.0005(7) 0.0044(7) N11 0.0247(9) 0.0284(9) 0.0272(10) -0.0041(8) 0.0013(7) 0.0100(7) C12 0.0215(10) 0.0243(10) 0.0248(11) 0.0037(8) 0.0001(8) 0.0075(8) N12 0.0299(10) 0.0306(10) 0.0291(10) -0.0018(8) 0.0038(8) 0.0122(8) N23 0.0274(11) 0.0459(13) 0.0740(17) 0.0341(12) -0.0093(11) 0.0059(9) C21 0.0249(11) 0.0290(11) 0.0315(12) 0.0134(9) 0.0043(9) 0.0074(9) N21 0.0236(9) 0.0329(10) 0.0324(10) 0.0148(8) 0.0021(8) 0.0096(8) C22 0.0240(10) 0.0317(11) 0.0259(11) 0.0059(9) -0.0009(8) 0.0095(9) N22 0.0337(10) 0.0307(10) 0.0260(10) 0.0077(8) -0.0002(8) 0.0140(8) N31 0.0204(8) 0.0239(8) 0.0218(9) 0.0020(7) -0.0007(7) 0.0065(7) C30 0.0206(10) 0.0213(9) 0.0256(11) 0.0041(8) -0.0018(8) 0.0078(8) C31 0.0199(9) 0.0190(9) 0.0258(11) 0.0018(8) -0.0001(8) 0.0061(7) C32 0.0179(9) 0.0199(9) 0.0210(10) 0.0022(8) 0.0025(7) 0.0053(7) C33 0.0294(11) 0.0246(10) 0.0224(10) 0.0017(8) -0.0020(8) 0.0120(8) C34 0.0283(11) 0.0230(9) 0.0228(11) 0.0002(8) -0.0011(8) 0.0122(8) C35 0.0267(10) 0.0159(8) 0.0261(11) 0.0021(8) 0.0001(8) 0.0062(8) C36 0.0236(10) 0.0206(9) 0.0216(10) 0.0050(8) 0.0009(8) 0.0075(8) C37 0.0156(9) 0.0199(9) 0.0227(10) 0.0031(8) 0.0027(7) 0.0053(7) C38 0.0283(11) 0.0178(9) 0.0231(11) 0.0034(8) 0.0020(8) 0.0073(8) C39 0.0294(11) 0.0200(9) 0.0234(10) 0.0047(8) 0.0014(8) 0.0086(8) N32 0.0234(9) 0.0208(8) 0.0206(9) 0.0016(7) 0.0001(7) 0.0085(7) N41 0.0267(9) 0.0218(8) 0.0205(9) 0.0008(7) 0.0010(7) 0.0087(7) C40 0.0266(11) 0.0284(11) 0.0207(11) -0.0037(8) -0.0005(8) 0.0049(9) C41 0.0297(11) 0.0289(11) 0.0160(10) -0.0028(8) 0.0001(8) 0.0055(9) C42 0.0256(10) 0.0178(9) 0.0176(9) 0.0023(7) -0.0016(8) 0.0090(8) C43 0.0304(11) 0.0207(9) 0.0164(10) 0.0001(8) -0.0010(8) 0.0054(8) C44 0.0338(12) 0.0224(10) 0.0182(10) 0.0010(8) 0.0026(8) 0.0083(8) N51 0.0271(10) 0.0279(9) 0.0269(10) 0.0026(8) -0.0006(8) 0.0060(8) C52 0.0243(10) 0.0277(10) 0.0189(10) -0.0011(8) 0.0003(8) 0.0068(8) C53 0.0376(13) 0.0279(11) 0.0313(13) 0.0007(10) 0.0087(10) -0.0040(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 N21 1.9483(18) . ? Cu1 N11 1.9829(19) . ? Cu1 N51 2.017(2) . ? Cu1 N31 2.0764(17) . ? Cu2 N12 1.9506(19) 1_566 ? Cu2 N22 1.9778(19) 1_656 ? Cu2 N32 2.0457(17) . ? Cu2 N41 2.0877(19) . ? N13 C11 1.302(3) . ? N13 C12 1.305(3) . ? C11 N11 1.157(3) . ? C12 N12 1.149(3) . ? N12 Cu2 1.9507(19) 1_544 ? N23 C22 1.308(3) . ? N23 C21 1.314(3) . ? C21 N21 1.147(3) . ? C22 N22 1.148(3) . ? N22 Cu2 1.9778(19) 1_454 ? N31 C34 1.342(3) . ? N31 C30 1.344(3) . ? C30 C31 1.380(3) . ? C31 C32 1.396(3) . ? C32 C33 1.398(3) . ? C32 C37 1.480(3) . ? C33 C34 1.381(3) . ? C35 N32 1.343(3) . ? C35 C36 1.383(3) . ? C36 C37 1.396(3) . ? C37 C38 1.397(3) . ? C38 C39 1.376(3) . ? C39 N32 1.346(3) . ? N41 C40 1.338(3) . ? N41 C44 1.351(3) . ? C40 C41 1.374(3) . ? C41 C42 1.401(3) . ? C42 C43 1.398(3) . ? C42 C42 1.479(4) 2 ? C43 C44 1.379(3) . ? N51 C52 1.137(3) . ? C52 C53 1.451(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 N21 Cu1 N11 124.24(8) . . ? N21 Cu1 N51 109.61(8) . . ? N11 Cu1 N51 105.25(8) . . ? N21 Cu1 N31 108.82(8) . . ? N11 Cu1 N31 102.55(7) . . ? N51 Cu1 N31 104.65(7) . . ? N12 Cu2 N22 114.88(8) 1_566 1_656 ? N12 Cu2 N32 119.47(8) 1_566 . ? N22 Cu2 N32 103.17(7) 1_656 . ? N12 Cu2 N41 103.54(8) 1_566 . ? N22 Cu2 N41 112.04(8) 1_656 . ? N32 Cu2 N41 103.32(7) . . ? C11 N13 C12 120.66(18) . . ? N11 C11 N13 174.1(2) . . ? C11 N11 Cu1 154.69(19) . . ? N12 C12 N13 174.2(2) . . ? C12 N12 Cu2 174.8(2) . 1_544 ? C22 N23 C21 120.1(2) . . ? N21 C21 N23 174.2(3) . . ? C21 N21 Cu1 171.04(19) . . ? N22 C22 N23 172.4(3) . . ? C22 N22 Cu2 169.5(2) . 1_454 ? C34 N31 C30 116.93(17) . . ? C34 N31 Cu1 119.65(14) . . ? C30 N31 Cu1 123.38(14) . . ? N31 C30 C31 123.63(19) . . ? C30 C31 C32 119.25(18) . . ? C31 C32 C33 117.35(18) . . ? C31 C32 C37 121.83(17) . . ? C33 C32 C37 120.79(18) . . ? C34 C33 C32 119.36(19) . . ? N31 C34 C33 123.48(19) . . ? N32 C35 C36 123.92(18) . . ? C35 C36 C37 119.27(19) . . ? C36 C37 C38 116.93(18) . . ? C36 C37 C32 121.20(18) . . ? C38 C37 C32 121.84(18) . . ? C39 C38 C37 119.77(19) . . ? N32 C39 C38 123.63(19) . . ? C35 N32 C39 116.40(18) . . ? C35 N32 Cu2 121.60(14) . . ? C39 N32 Cu2 121.12(14) . . ? C40 N41 C44 116.12(19) . . ? C40 N41 Cu2 124.74(15) . . ? C44 N41 Cu2 118.89(15) . . ? N41 C40 C41 124.4(2) . . ? C40 C41 C42 120.0(2) . . ? C43 C42 C41 115.8(2) . . ? C43 C42 C42 121.8(2) . 2 ? C41 C42 C42 122.4(2) . 2 ? C44 C43 C42 120.57(19) . . ? N41 C44 C43 123.2(2) . . ? C52 N51 Cu1 177.34(19) . . ? N51 C52 C53 179.5(2) . . ? _diffrn_measured_fraction_theta_max 0.880 _diffrn_reflns_theta_full 31.98 _diffrn_measured_fraction_theta_full 0.880 _refine_diff_density_max 0.662 _refine_diff_density_min -0.711 _refine_diff_density_rms 0.090 _publ_contact_author ; Dr. Stuart Batten Department of Chemistry P.O. Box 23 Monash University Clayton, Vic. 3800 AUSTRALIA ; _publ_contact_author_phone ' +61 3 9905 4606 ' _publ_contact_author_fax ' +61 3 9905 4597 ' _publ_contact_author_email ' stuart.batten@sci.monash.edu.au ' loop_ _publ_author_name _publ_author_address ' Batten, Stuart R. ' ; Department of Chemistry P.O. Box 23 Monash University Clayton, Vic. 3800 AUSTRALIA ; _publ_section_title ; Cuprous dicyanamide coordination polymers: ladders, sheets, layers, diamond-like networks and unusual interpenetration ; #=END data_a-cudcabpe _audit_creation_method SHELXL-97 _chemical_name_systematic ; alpha - cuprous dicyanamide 1,2-bis(4-pyridyl)ethene ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H10 Cu N5' _chemical_formula_weight 311.81 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 Orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 7.38350(10) _cell_length_b 15.2140(5) _cell_length_c 12.1963(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1370.04(7) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.512 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 632 _exptl_absorpt_coefficient_mu 1.590 _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 123(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 ? _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11519 _diffrn_reflns_av_R_equivalents 0.0293 _diffrn_reflns_av_sigmaI/netI 0.0356 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 30.00 _reflns_number_total 3039 _reflns_number_gt 2728 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens 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^)+(0.0124P)^2^+0.6149P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.494(12) _refine_ls_number_reflns 3039 _refine_ls_number_parameters 182 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0324 _refine_ls_R_factor_gt 0.0256 _refine_ls_wR_factor_ref 0.0542 _refine_ls_wR_factor_gt 0.0519 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu -0.07212(3) -0.882371(15) -0.16698(3) 0.02210(7) Uani 1 1 d . . . N1 N -0.1679(3) -0.82334(12) -0.30257(14) 0.0216(4) Uani 1 1 d . . . C1 C -0.2106(3) -0.87475(15) -0.38827(19) 0.0267(5) Uani 1 1 d . . . H1A H -0.2044 -0.9367 -0.3788 0.032 Uiso 1 1 calc R . . C2 C -0.2631(3) -0.84286(16) -0.48934(18) 0.0259(5) Uani 1 1 d . . . H2A H -0.2914 -0.8824 -0.5472 0.031 Uiso 1 1 calc R . . C3 C -0.2743(3) -0.75231(15) -0.50623(17) 0.0201(4) Uani 1 1 d . . . C4 C -0.2319(3) -0.69911(16) -0.41772(17) 0.0244(5) Uani 1 1 d . . . H4A H -0.2381 -0.6370 -0.4247 0.029 Uiso 1 1 calc R . . C5 C -0.1802(3) -0.73666(15) -0.31876(19) 0.0257(5) Uani 1 1 d . . . H5A H -0.1520 -0.6987 -0.2593 0.031 Uiso 1 1 calc R . . C6 C -0.3287(3) -0.71378(17) -0.61197(18) 0.0217(5) Uani 1 1 d . . . H6A H -0.3373 -0.6516 -0.6167 0.026 Uiso 1 1 calc R . . C7 C -0.3663(3) -0.76021(16) -0.70093(17) 0.0229(5) Uani 1 1 d . . . H7A H -0.3570 -0.8223 -0.6942 0.027 Uiso 1 1 calc R . . C8 C -0.4869(3) -0.75391(16) -0.99849(18) 0.0246(5) Uani 1 1 d . . . H8A H -0.4961 -0.7948 -1.0571 0.029 Uiso 1 1 calc R . . C9 C -0.4395(3) -0.78519(15) -0.89614(18) 0.0243(5) Uani 1 1 d . . . H9A H -0.4196 -0.8463 -0.8852 0.029 Uiso 1 1 calc R . . C10 C -0.4209(3) -0.72652(15) -0.80894(17) 0.0201(4) Uani 1 1 d . . . C11 C -0.4561(3) -0.63838(15) -0.83012(19) 0.0246(5) Uani 1 1 d . . . H11A H -0.4454 -0.5960 -0.7733 0.030 Uiso 1 1 calc R . . C12 C -0.5066(3) -0.61301(16) -0.93399(19) 0.0257(5) Uani 1 1 d . . . H12A H -0.5329 -0.5527 -0.9462 0.031 Uiso 1 1 calc R . . N2 N -0.5207(3) -0.66872(12) -1.01954(15) 0.0223(4) Uani 1 1 d . . . N23 N 0.4472(3) -1.01807(14) -0.2356(2) 0.0387(6) Uani 1 1 d . . . C21 C 0.2903(3) -0.98163(14) -0.21548(19) 0.0231(5) Uani 1 1 d . . . N21 N 0.1465(3) -0.95433(13) -0.20516(16) 0.0286(5) Uani 1 1 d . . . C22 C 0.5891(3) -0.99418(13) -0.1790(3) 0.0267(6) Uani 1 1 d . . . N22 N 0.7241(3) -0.97791(14) -0.13556(18) 0.0348(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.02426(12) 0.02694(13) 0.01509(11) -0.00093(17) -0.00582(14) 0.00115(10) N1 0.0262(11) 0.0224(10) 0.0162(9) -0.0007(8) -0.0045(7) 0.0047(7) C1 0.0388(14) 0.0221(12) 0.0191(11) 0.0017(10) -0.0042(9) 0.0012(10) C2 0.0373(14) 0.0231(12) 0.0174(11) -0.0032(9) -0.0079(9) -0.0014(10) C3 0.0169(11) 0.0271(12) 0.0164(10) 0.0017(9) 0.0002(8) 0.0004(8) C4 0.0301(12) 0.0245(12) 0.0185(11) -0.0011(9) -0.0033(9) 0.0049(9) C5 0.0339(14) 0.0257(13) 0.0175(11) -0.0055(9) -0.0078(9) 0.0048(9) C6 0.0227(12) 0.0266(13) 0.0159(11) 0.0020(9) -0.0035(8) 0.0024(9) C7 0.0260(11) 0.0251(12) 0.0176(11) 0.0044(9) -0.0013(8) 0.0033(9) C8 0.0317(13) 0.0243(12) 0.0178(11) -0.0039(10) -0.0042(9) 0.0017(9) C9 0.0334(13) 0.0209(11) 0.0185(11) 0.0012(9) -0.0046(9) 0.0026(9) C10 0.0233(12) 0.0242(12) 0.0128(10) 0.0014(8) -0.0020(8) 0.0006(8) C11 0.0322(13) 0.0236(12) 0.0180(11) -0.0013(9) -0.0049(9) 0.0011(9) C12 0.0350(13) 0.0221(12) 0.0200(12) 0.0006(10) -0.0062(9) -0.0005(10) N2 0.0286(11) 0.0228(10) 0.0157(9) 0.0019(8) -0.0031(8) -0.0019(8) N23 0.0251(11) 0.0350(12) 0.0558(15) -0.0230(11) -0.0042(10) 0.0030(9) C21 0.0272(13) 0.0178(10) 0.0244(11) -0.0013(9) -0.0041(9) -0.0026(9) N21 0.0291(11) 0.0262(10) 0.0306(11) -0.0022(8) -0.0038(8) 0.0009(8) C22 0.0275(11) 0.0179(9) 0.0347(16) -0.0008(12) 0.0087(11) 0.0005(8) N22 0.0266(11) 0.0337(12) 0.0442(15) -0.0012(9) -0.0002(9) -0.0031(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N2 1.9954(18) 3_536 ? Cu1 N21 2.005(2) . ? Cu1 N1 2.0104(18) . ? Cu1 N22 2.127(2) 1_455 ? N1 C5 1.336(3) . ? N1 C1 1.343(3) . ? C1 C2 1.380(3) . ? C2 C3 1.395(3) . ? C3 C4 1.385(3) . ? C3 C6 1.473(3) . ? C4 C5 1.389(3) . ? C6 C7 1.324(3) . ? C7 C10 1.470(3) . ? C8 N2 1.345(3) . ? C8 C9 1.381(3) . ? C9 C10 1.395(3) . ? C10 C11 1.390(3) . ? C11 C12 1.376(3) . ? C12 N2 1.348(3) . ? N2 Cu1 1.9954(18) 3_434 ? N23 C22 1.306(3) . ? N23 C21 1.307(3) . ? C21 N21 1.147(3) . ? C22 N22 1.156(3) . ? N22 Cu1 2.127(2) 1_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 N2 Cu1 N21 105.60(8) 3_536 . ? N2 Cu1 N1 129.36(7) 3_536 . ? N21 Cu1 N1 109.64(8) . . ? N2 Cu1 N22 103.79(8) 3_536 1_455 ? N21 Cu1 N22 103.77(8) . 1_455 ? N1 Cu1 N22 101.81(8) . 1_455 ? C5 N1 C1 116.34(19) . . ? C5 N1 Cu1 125.89(15) . . ? C1 N1 Cu1 117.55(15) . . ? N1 C1 C2 123.8(2) . . ? C1 C2 C3 119.7(2) . . ? C4 C3 C2 116.64(19) . . ? C4 C3 C6 120.8(2) . . ? C2 C3 C6 122.6(2) . . ? C3 C4 C5 119.9(2) . . ? N1 C5 C4 123.6(2) . . ? C7 C6 C3 124.2(2) . . ? C6 C7 C10 127.3(2) . . ? N2 C8 C9 123.5(2) . . ? C8 C9 C10 119.6(2) . . ? C11 C10 C9 117.2(2) . . ? C11 C10 C7 123.7(2) . . ? C9 C10 C7 119.1(2) . . ? C12 C11 C10 119.5(2) . . ? N2 C12 C11 123.9(2) . . ? C8 N2 C12 116.34(19) . . ? C8 N2 Cu1 125.65(15) . 3_434 ? C12 N2 Cu1 117.86(15) . 3_434 ? C22 N23 C21 119.6(2) . . ? N21 C21 N23 173.9(2) . . ? C21 N21 Cu1 165.53(18) . . ? N22 C22 N23 173.5(3) . . ? C22 N22 Cu1 132.4(2) . 1_655 ? _diffrn_measured_fraction_theta_max 0.939 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.939 _refine_diff_density_max 0.272 _refine_diff_density_min -0.402 _refine_diff_density_rms 0.058 _publ_contact_author ; Dr. Stuart Batten Department of Chemistry P.O. Box 23 Monash University Clayton, Vic. 3800 AUSTRALIA ; _publ_contact_author_phone ' +61 3 9905 4606 ' _publ_contact_author_fax ' +61 3 9905 4597 ' _publ_contact_author_email ' stuart.batten@sci.monash.edu.au ' loop_ _publ_author_name _publ_author_address ' Batten, Stuart R. ' ; Department of Chemistry P.O. Box 23 Monash University Clayton, Vic. 3800 AUSTRALIA ; _publ_section_title ; Cuprous dicyanamide coordination polymers: ladders, sheets, layers, diamond-like networks and unusual interpenetration ; #=END data_b-cudcabpe _audit_creation_method SHELXL-97 _chemical_name_systematic ; beta - cuprous dicyanamide 1,2-bis(4-pyridyl)ethene ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H10 Cu N5' _chemical_formula_weight 311.81 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 Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 12.2904(3) _cell_length_b 44.6752(13) _cell_length_c 14.6413(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.004(2) _cell_angle_gamma 90.00 _cell_volume 8028.1(3) _cell_formula_units_Z 24 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod _exptl_crystal_colour red _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.125 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.548 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3792 _exptl_absorpt_coefficient_mu 1.628 _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 123(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 ? _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 49758 _diffrn_reflns_av_R_equivalents 0.0554 _diffrn_reflns_av_sigmaI/netI 0.0777 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -63 _diffrn_reflns_limit_k_max 63 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 30.45 _reflns_number_total 22290 _reflns_number_gt 16716 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens 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^)+(0.0402P)^2^+27.7813P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.492(13) _refine_ls_number_reflns 22290 _refine_ls_number_parameters 1082 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0884 _refine_ls_R_factor_gt 0.0560 _refine_ls_wR_factor_ref 0.1363 _refine_ls_wR_factor_gt 0.1200 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _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 0.11257(5) -0.146559(15) -0.27975(4) 0.02489(15) Uani 1 1 d . . . Cu2 Cu 0.14955(5) -0.307473(14) -0.01847(4) 0.02665(15) Uani 1 1 d . . . Cu3 Cu 0.11526(5) -0.474020(15) -0.22992(4) 0.02653(15) Uani 1 1 d . . . Cu4 Cu -0.83579(5) -0.014111(14) -0.50244(4) 0.02281(14) Uani 1 1 d . . . Cu5 Cu -0.90110(5) -0.180659(14) -0.74769(4) 0.02632(15) Uani 1 1 d . . . Cu6 Cu -0.83885(5) -0.353326(15) -0.55365(4) 0.02844(16) Uani 1 1 d . . . N1 N 0.0894(5) -0.17965(12) -0.1972(3) 0.0298(11) Uani 1 1 d . . . C1 C 0.0636(5) -0.19868(13) -0.1505(3) 0.0241(11) Uani 1 1 d . . . N2 N 0.0273(5) -0.21894(12) -0.0962(3) 0.0316(12) Uani 1 1 d . . . C2 C 0.0717(5) -0.24493(13) -0.0871(3) 0.0237(11) Uani 1 1 d . . . N3 N 0.1039(5) -0.26862(12) -0.0742(3) 0.0356(12) Uani 1 1 d . . . N4 N 0.1767(4) -0.34102(10) -0.0974(3) 0.0247(10) Uani 1 1 d . . . C3 C 0.2001(5) -0.36214(13) -0.1386(3) 0.0210(11) Uani 1 1 d . . . N5 N 0.2382(5) -0.38382(11) -0.1875(3) 0.0268(11) Uani 1 1 d . . . C4 C 0.1981(5) -0.41070(14) -0.1795(3) 0.0282(12) Uani 1 1 d . . . N6 N 0.1720(6) -0.43551(12) -0.1769(4) 0.0448(15) Uani 1 1 d . . . N7 N -0.8480(5) 0.10874(12) -0.7127(3) 0.0324(12) Uani 1 1 d . . . C5 C -0.8074(5) 0.08693(14) -0.6857(3) 0.0292(13) Uani 1 1 d . . . N8 N -0.7519(5) 0.06390(14) -0.6599(4) 0.0500(18) Uani 1 1 d . . . C6 C -0.7929(5) 0.04126(14) -0.6178(3) 0.0256(12) Uani 1 1 d . . . N9 N -0.8170(5) 0.02022(11) -0.5783(3) 0.0260(11) Uani 1 1 d . . . N10 N -0.8754(5) -0.05178(11) -0.5735(4) 0.0359(12) Uani 1 1 d . . . C7 C -0.9205(5) -0.07262(12) -0.6016(3) 0.0236(12) Uani 1 1 d . . . N11 N -0.9837(5) -0.09437(11) -0.6327(3) 0.0299(11) Uani 1 1 d . . . C8 C -0.9438(5) -0.12004(12) -0.6596(3) 0.0207(10) Uani 1 1 d . . . N12 N -0.9203(5) -0.14284(10) -0.6857(4) 0.0279(11) Uani 1 1 d . . . N13 N -0.8586(5) -0.21774(12) -0.6745(3) 0.0350(12) Uani 1 1 d . . . C9 C -0.8147(5) -0.24036(12) -0.6602(3) 0.0215(11) Uani 1 1 d . . . N14 N -0.7546(5) -0.26364(13) -0.6466(4) 0.0409(14) Uani 1 1 d . . . C10 C -0.7931(5) -0.29016(14) -0.6284(3) 0.0279(13) Uani 1 1 d . . . N15 N -0.8163(5) -0.31483(12) -0.6110(3) 0.0312(12) Uani 1 1 d . . . N16 N -0.8925(5) -0.39127(13) -0.6146(4) 0.0409(14) Uani 1 1 d . . . C11 C -0.9248(5) -0.41564(15) -0.6101(3) 0.0302(14) Uani 1 1 d . . . N17 N -0.9698(5) -0.44151(13) -0.5981(4) 0.0469(16) Uani 1 1 d . . . C12 C -0.9346(5) -0.46678(14) -0.6332(3) 0.0261(12) Uani 1 1 d . . . N18 N -0.9107(4) -0.48984(12) -0.6606(3) 0.0280(11) Uani 1 1 d . . . N19 N -0.0421(4) -0.13791(12) -0.3454(3) 0.0241(10) Uani 1 1 d . . . C13 C -0.1305(5) -0.13829(13) -0.2954(3) 0.0246(12) Uani 1 1 d . . . H13A H -0.1275 -0.1502 -0.2417 0.030 Uiso 1 1 calc R . . C14 C -0.2241(5) -0.12292(12) -0.3156(3) 0.0223(11) Uani 1 1 d . . . H14A H -0.2825 -0.1234 -0.2757 0.027 Uiso 1 1 calc R . . C15 C -0.2323(5) -0.10619(12) -0.3973(3) 0.0215(11) Uani 1 1 d . . . C16 C -0.1449(5) -0.10757(12) -0.4539(4) 0.0229(11) Uani 1 1 d . . . H16A H -0.1487 -0.0978 -0.5116 0.027 Uiso 1 1 calc R . . C17 C -0.0530(5) -0.12320(12) -0.4253(3) 0.0211(10) Uani 1 1 d . . . H17A H 0.0063 -0.1236 -0.4644 0.025 Uiso 1 1 calc R . . C18 C -0.3271(5) -0.08730(12) -0.4224(4) 0.0204(11) Uani 1 1 d . . . H18A H -0.3334 -0.0806 -0.4840 0.024 Uiso 1 1 calc R . . C19 C -0.6704(5) -0.03911(13) -0.3629(4) 0.0268(12) Uani 1 1 d . . . H19A H -0.7283 -0.0380 -0.3225 0.032 Uiso 1 1 calc R . . C20 C -0.5813(5) -0.05633(12) -0.3357(3) 0.0231(11) Uani 1 1 d . . . H20A H -0.5783 -0.0663 -0.2782 0.028 Uiso 1 1 calc R . . C21 C -0.4966(5) -0.05886(12) -0.3934(3) 0.0206(10) Uani 1 1 d . . . C22 C -0.5033(5) -0.04199(13) -0.4734(4) 0.0256(11) Uani 1 1 d . . . H22A H -0.4453 -0.0422 -0.5139 0.031 Uiso 1 1 calc R . . C23 C -0.5961(5) -0.02486(11) -0.4933(4) 0.0224(11) Uani 1 1 d . . . H23A H -0.5988 -0.0131 -0.5473 0.027 Uiso 1 1 calc R . . C24 C -0.4043(5) -0.07862(12) -0.3691(4) 0.0240(12) Uani 1 1 d . . . H24A H -0.3996 -0.0860 -0.3081 0.029 Uiso 1 1 calc R . . N20 N -0.6819(4) -0.02405(10) -0.4405(3) 0.0247(10) Uani 1 1 d . . . N21 N -0.0354(4) -0.46232(11) -0.2961(3) 0.0322(11) Uani 1 1 d . . . C25 C -0.1240(6) -0.45743(16) -0.2469(4) 0.0408(16) Uani 1 1 d . . . H25A H -0.1199 -0.4627 -0.1839 0.049 Uiso 1 1 calc R . . C26 C -0.2188(6) -0.44535(17) -0.2830(4) 0.0396(16) Uani 1 1 d . . . H26A H -0.2797 -0.4434 -0.2461 0.048 Uiso 1 1 calc R . . C27 C -0.2266(5) -0.43585(12) -0.3734(3) 0.0232(11) Uani 1 1 d . . . C28 C -0.1365(5) -0.44170(12) -0.4254(4) 0.0230(11) Uani 1 1 d . . . H28A H -0.1388 -0.4366 -0.4885 0.028 Uiso 1 1 calc R . . C29 C -0.0451(5) -0.45471(12) -0.3854(4) 0.0273(12) Uani 1 1 d . . . H29A H 0.0146 -0.4586 -0.4224 0.033 Uiso 1 1 calc R . . C30 C -0.3215(5) -0.42073(12) -0.4153(3) 0.0215(11) Uani 1 1 d . . . H30A H -0.3194 -0.4161 -0.4786 0.026 Uiso 1 1 calc R . . C31 C -0.6823(5) -0.37513(12) -0.4022(3) 0.0200(10) Uani 1 1 d . . . H31A H -0.7413 -0.3710 -0.3647 0.024 Uiso 1 1 calc R . . C32 C -0.5924(5) -0.38967(12) -0.3636(3) 0.0217(11) Uani 1 1 d . . . H32A H -0.5906 -0.3951 -0.3009 0.026 Uiso 1 1 calc R . . C33 C -0.5055(5) -0.39639(12) -0.4148(3) 0.0212(11) Uani 1 1 d . . . C34 C -0.5133(6) -0.38778(18) -0.5072(4) 0.0440(19) Uani 1 1 d . . . H34A H -0.4568 -0.3923 -0.5469 0.053 Uiso 1 1 calc R . . C35 C -0.6064(6) -0.3725(2) -0.5387(5) 0.073(3) Uani 1 1 d . . . H35A H -0.6099 -0.3657 -0.6003 0.087 Uiso 1 1 calc R . . C36 C -0.4103(5) -0.41277(12) -0.3745(3) 0.0224(11) Uani 1 1 d . . . H36A H -0.4133 -0.4182 -0.3119 0.027 Uiso 1 1 calc R . . N22 N -0.6908(4) -0.36667(13) -0.4883(3) 0.0372(13) Uani 1 1 d . . . N23 N 0.3023(4) -0.30004(11) 0.0528(3) 0.0304(11) Uani 1 1 d . . . C37 C 0.3121(5) -0.28871(13) 0.1363(4) 0.0255(11) Uani 1 1 d . . . H37A H 0.2514 -0.2900 0.1737 0.031 Uiso 1 1 calc R . . C38 C 0.4069(5) -0.27497(12) 0.1723(3) 0.0210(11) Uani 1 1 d . . . H38A H 0.4100 -0.2675 0.2331 0.025 Uiso 1 1 calc R . . C39 C 0.4968(5) -0.27227(13) 0.1190(3) 0.0230(11) Uani 1 1 d . . . C40 C 0.4877(5) -0.28530(17) 0.0336(4) 0.0384(16) Uani 1 1 d . . . H40A H 0.5476 -0.2847 -0.0048 0.046 Uiso 1 1 calc R . . C41 C 0.3908(5) -0.29949(18) 0.0031(5) 0.0447(17) Uani 1 1 d . . . H41A H 0.3878 -0.3091 -0.0550 0.054 Uiso 1 1 calc R . . C42 C 0.5920(6) -0.25534(13) 0.1543(3) 0.0257(12) Uani 1 1 d . . . H42A H 0.5959 -0.2503 0.2175 0.031 Uiso 1 1 calc R . . C43 C 0.8615(6) -0.19530(18) 0.2424(4) 0.0462(19) Uani 1 1 d . . . H43A H 0.8630 -0.1849 0.2990 0.055 Uiso 1 1 calc R . . C44 C 0.7714(6) -0.21231(17) 0.2172(4) 0.0394(16) Uani 1 1 d . . . H44A H 0.7127 -0.2134 0.2567 0.047 Uiso 1 1 calc R . . C45 C 0.7649(5) -0.22784(13) 0.1357(3) 0.0232(11) Uani 1 1 d . . . C46 C 0.8509(5) -0.22283(13) 0.0794(3) 0.0241(12) Uani 1 1 d . . . H46A H 0.8484 -0.2312 0.0197 0.029 Uiso 1 1 calc R . . C47 C 0.9389(5) -0.20597(13) 0.1088(4) 0.0261(12) Uani 1 1 d . . . H47A H 0.9967 -0.2036 0.0689 0.031 Uiso 1 1 calc R . . C48 C 0.6738(5) -0.24646(13) 0.1041(3) 0.0225(12) Uani 1 1 d . . . H48A H 0.6722 -0.2529 0.0422 0.027 Uiso 1 1 calc R . . N24 N 0.9478(4) -0.19286(12) 0.1896(3) 0.0309(11) Uani 1 1 d . . . N25 N 0.0503(4) -0.31283(11) 0.0881(3) 0.0238(10) Uani 1 1 d . . . C49 C 0.0164(6) -0.28897(14) 0.1344(4) 0.0306(14) Uani 1 1 d . . . H49A H 0.0307 -0.2696 0.1110 0.037 Uiso 1 1 calc R . . C50 C -0.0376(6) -0.29106(15) 0.2134(4) 0.0354(14) Uani 1 1 d . . . H50A H -0.0611 -0.2735 0.2434 0.042 Uiso 1 1 calc R . . C51 C -0.0580(5) -0.32008(14) 0.2501(4) 0.0282(12) Uani 1 1 d . . . C52 C -0.0237(5) -0.34450(14) 0.2002(4) 0.0276(11) Uani 1 1 d . . . H52A H -0.0367 -0.3643 0.2210 0.033 Uiso 1 1 calc R . . C53 C 0.0294(5) -0.34009(12) 0.1205(4) 0.0266(12) Uani 1 1 d . . . H53A H 0.0518 -0.3571 0.0873 0.032 Uiso 1 1 calc R . . C54 C -0.1124(5) -0.32510(13) 0.3361(4) 0.0305(12) Uani 1 1 d . . . H54A H -0.1278 -0.3452 0.3523 0.037 Uiso 1 1 calc R . . C55 C -0.2676(5) -0.28961(13) 0.6149(4) 0.0243(12) Uani 1 1 d . . . H55A H -0.2805 -0.2725 0.6512 0.029 Uiso 1 1 calc R . . C56 C -0.2169(5) -0.28554(13) 0.5345(4) 0.0256(12) Uani 1 1 d . . . H56A H -0.1950 -0.2660 0.5176 0.031 Uiso 1 1 calc R . . C57 C -0.1974(5) -0.30931(13) 0.4782(4) 0.0264(12) Uani 1 1 d . . . C58 C -0.2301(5) -0.33726(15) 0.5071(4) 0.0356(14) Uani 1 1 d . . . H58A H -0.2185 -0.3545 0.4710 0.043 Uiso 1 1 calc R . . C59 C -0.2797(5) -0.33963(13) 0.5887(5) 0.0353(14) Uani 1 1 d . . . H59A H -0.3014 -0.3590 0.6069 0.042 Uiso 1 1 calc R . . C60 C -0.1413(5) -0.30386(14) 0.3919(4) 0.0328(13) Uani 1 1 d . . . H60A H -0.1253 -0.2837 0.3764 0.039 Uiso 1 1 calc R . . N26 N -0.3001(4) -0.31643(10) 0.6455(3) 0.0223(10) Uani 1 1 d . . . N27 N -0.9357(4) -0.01780(10) -0.3957(3) 0.0202(10) Uani 1 1 d . . . C61 C -0.9589(5) 0.00596(12) -0.3417(4) 0.0252(12) Uani 1 1 d . . . H61A H -0.9376 0.0254 -0.3604 0.030 Uiso 1 1 calc R . . C62 C -1.0114(5) 0.00329(13) -0.2616(4) 0.0272(12) Uani 1 1 d . . . H62A H -1.0250 0.0206 -0.2263 0.033 Uiso 1 1 calc R . . C63 C -1.0448(5) -0.02457(14) -0.2323(4) 0.0245(12) Uani 1 1 d . . . C64 C -1.0213(5) -0.04910(13) -0.2885(4) 0.0281(12) Uani 1 1 d . . . H64A H -1.0435 -0.0687 -0.2724 0.034 Uiso 1 1 calc R . . C65 C -0.9664(5) -0.04464(12) -0.3663(4) 0.0257(12) Uani 1 1 d . . . H65A H -0.9491 -0.0617 -0.4015 0.031 Uiso 1 1 calc R . . C66 C -1.0989(6) -0.02963(15) -0.1472(4) 0.0311(14) Uani 1 1 d . . . H66A H -1.1130 -0.0498 -0.1310 0.037 Uiso 1 1 calc R . . C67 C -1.2669(5) 0.00704(12) 0.1279(4) 0.0234(11) Uani 1 1 d . . . H67A H -1.2884 0.0241 0.1612 0.028 Uiso 1 1 calc R . . C68 C -1.2167(5) 0.01114(13) 0.0477(4) 0.0266(12) Uani 1 1 d . . . H68A H -1.2035 0.0309 0.0270 0.032 Uiso 1 1 calc R . . C69 C -1.1843(5) -0.01328(12) -0.0044(4) 0.0222(11) Uani 1 1 d . . . C70 C -1.2044(5) -0.04155(13) 0.0307(4) 0.0229(11) Uani 1 1 d . . . H70A H -1.1835 -0.0590 -0.0010 0.027 Uiso 1 1 calc R . . C71 C -1.2545(5) -0.04381(12) 0.1115(4) 0.0251(12) Uani 1 1 d . . . H71A H -1.2675 -0.0633 0.1347 0.030 Uiso 1 1 calc R . . C72 C -1.1301(5) -0.00830(14) -0.0902(4) 0.0287(12) Uani 1 1 d . . . H72A H -1.1161 0.0119 -0.1067 0.034 Uiso 1 1 calc R . . N28 N -1.2868(4) -0.02003(10) 0.1606(3) 0.0196(9) Uani 1 1 d . . . N29 N -0.9378(4) -0.35097(10) -0.4445(3) 0.0227(10) Uani 1 1 d . . . C73 C -0.9569(5) -0.32452(13) -0.4024(4) 0.0279(12) Uani 1 1 d . . . H73A H -0.9347 -0.3067 -0.4316 0.034 Uiso 1 1 calc R . . C74 C -1.0056(5) -0.32178(14) -0.3212(4) 0.0341(14) Uani 1 1 d . . . H74A H -1.0161 -0.3025 -0.2957 0.041 Uiso 1 1 calc R . . C75 C -1.0392(5) -0.34674(15) -0.2765(4) 0.0301(13) Uani 1 1 d . . . C76 C -1.0196(6) -0.37439(15) -0.3186(4) 0.0331(14) Uani 1 1 d . . . H76A H -1.0406 -0.3925 -0.2902 0.040 Uiso 1 1 calc R . . C77 C -0.9703(5) -0.37543(13) -0.4006(4) 0.0260(12) Uani 1 1 d . . . H77A H -0.9586 -0.3944 -0.4275 0.031 Uiso 1 1 calc R . . C78 C -1.0921(5) -0.34264(15) -0.1898(4) 0.0331(13) Uani 1 1 d . . . H78A H -1.1030 -0.3226 -0.1704 0.040 Uiso 1 1 calc R . . C79 C -1.2617(5) -0.33065(13) 0.0653(4) 0.0273(12) Uani 1 1 d . . . H79A H -1.2804 -0.3115 0.0878 0.033 Uiso 1 1 calc R . . C80 C -1.2092(5) -0.33221(16) -0.0170(4) 0.0369(15) Uani 1 1 d . . . H80A H -1.1935 -0.3145 -0.0500 0.044 Uiso 1 1 calc R . . C81 C -1.1802(5) -0.36053(14) -0.0498(4) 0.0294(12) Uani 1 1 d . . . C82 C -1.2038(5) -0.38486(14) 0.0018(4) 0.0331(14) Uani 1 1 d . . . H82A H -1.1844 -0.4043 -0.0176 0.040 Uiso 1 1 calc R . . C83 C -1.2552(6) -0.38114(14) 0.0813(4) 0.0286(13) Uani 1 1 d . . . H83A H -1.2696 -0.3985 0.1161 0.034 Uiso 1 1 calc R . . C84 C -1.1256(5) -0.36382(15) -0.1367(4) 0.0323(13) Uani 1 1 d . . . H84A H -1.1135 -0.3838 -0.1563 0.039 Uiso 1 1 calc R . . N30 N -1.2868(5) -0.35461(11) 0.1137(4) 0.0276(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0250(3) 0.0265(3) 0.0236(3) 0.0076(3) 0.0054(2) 0.0031(3) Cu2 0.0285(4) 0.0183(3) 0.0334(3) -0.0065(3) 0.0039(3) -0.0003(3) Cu3 0.0263(4) 0.0194(3) 0.0339(4) -0.0050(3) 0.0013(3) 0.0020(3) Cu4 0.0228(3) 0.0166(3) 0.0287(3) -0.0023(2) -0.0026(2) 0.0008(2) Cu5 0.0238(3) 0.0187(3) 0.0364(4) -0.0121(3) 0.0020(3) 0.0010(2) Cu6 0.0275(4) 0.0323(4) 0.0262(3) 0.0110(3) 0.0079(3) 0.0070(3) N1 0.026(3) 0.037(3) 0.026(2) 0.009(2) -0.0010(19) 0.002(2) C1 0.029(3) 0.026(3) 0.017(2) 0.002(2) -0.003(2) 0.002(2) N2 0.039(3) 0.033(3) 0.024(2) 0.0105(19) 0.011(2) 0.007(2) C2 0.030(3) 0.029(3) 0.013(2) 0.0039(19) 0.009(2) -0.007(2) N3 0.045(3) 0.026(3) 0.036(3) 0.008(2) 0.008(2) 0.007(2) N4 0.029(3) 0.017(2) 0.028(2) -0.0031(18) 0.0020(19) -0.0003(19) C3 0.018(3) 0.024(3) 0.021(2) -0.004(2) 0.0008(19) 0.000(2) N5 0.040(3) 0.024(2) 0.019(2) -0.0015(17) 0.0158(19) 0.001(2) C4 0.034(3) 0.034(3) 0.016(2) -0.012(2) 0.001(2) -0.002(2) N6 0.054(4) 0.025(3) 0.055(3) -0.023(2) 0.007(3) -0.004(2) N7 0.040(3) 0.033(3) 0.026(2) 0.0039(19) 0.009(2) -0.002(2) C5 0.030(3) 0.043(3) 0.015(2) 0.004(2) 0.005(2) 0.002(2) N8 0.029(3) 0.069(4) 0.054(3) 0.043(3) 0.018(3) 0.016(3) C6 0.026(3) 0.039(3) 0.011(2) 0.002(2) 0.0020(19) 0.010(2) N9 0.027(3) 0.030(3) 0.021(2) -0.0052(19) -0.0012(19) 0.001(2) N10 0.043(3) 0.019(2) 0.046(3) -0.021(2) 0.003(2) -0.001(2) C7 0.034(3) 0.025(3) 0.013(2) -0.0027(18) 0.010(2) 0.010(2) N11 0.028(3) 0.021(2) 0.040(3) -0.0159(19) 0.002(2) 0.0032(19) C8 0.024(3) 0.019(2) 0.019(2) -0.0025(18) -0.0001(19) -0.004(2) N12 0.029(3) 0.020(2) 0.033(3) -0.0060(18) -0.006(2) 0.0003(19) N13 0.039(3) 0.027(3) 0.040(3) -0.005(2) 0.008(2) 0.003(2) C9 0.026(3) 0.030(3) 0.0095(19) 0.0027(18) 0.0031(18) 0.001(2) N14 0.030(3) 0.040(3) 0.054(3) 0.031(3) 0.015(2) 0.007(2) C10 0.022(3) 0.041(3) 0.021(2) 0.016(2) 0.003(2) 0.008(2) N15 0.034(3) 0.033(3) 0.027(2) 0.015(2) 0.003(2) -0.001(2) N16 0.050(4) 0.043(3) 0.030(3) -0.008(2) 0.007(2) 0.011(3) C11 0.035(3) 0.043(4) 0.013(2) -0.012(2) 0.003(2) 0.014(3) N17 0.039(3) 0.052(4) 0.052(3) -0.030(3) 0.020(3) -0.011(3) C12 0.023(3) 0.039(3) 0.016(2) -0.002(2) 0.007(2) -0.001(2) N18 0.025(3) 0.033(3) 0.026(2) 0.002(2) 0.0005(19) -0.003(2) N19 0.027(3) 0.036(2) 0.0095(18) 0.0006(17) -0.0014(17) 0.006(2) C13 0.029(3) 0.031(3) 0.014(2) 0.006(2) 0.007(2) 0.000(2) C14 0.022(3) 0.026(3) 0.020(2) 0.0010(19) 0.008(2) 0.001(2) C15 0.024(3) 0.019(2) 0.021(2) -0.0024(19) 0.001(2) 0.000(2) C16 0.022(3) 0.022(3) 0.024(2) 0.0019(19) -0.001(2) 0.001(2) C17 0.023(3) 0.025(3) 0.016(2) 0.0010(19) 0.0049(19) 0.002(2) C18 0.016(3) 0.016(2) 0.029(2) 0.0050(18) -0.004(2) -0.0044(19) C19 0.028(3) 0.027(3) 0.025(3) 0.005(2) 0.000(2) 0.005(2) C20 0.026(3) 0.025(3) 0.018(2) 0.0047(19) 0.000(2) -0.001(2) C21 0.017(3) 0.021(2) 0.023(2) 0.0003(19) -0.0025(19) -0.0012(19) C22 0.018(3) 0.025(3) 0.033(3) -0.001(2) 0.001(2) -0.002(2) C23 0.024(3) 0.015(2) 0.028(3) 0.0015(18) -0.004(2) -0.0025(19) C24 0.025(3) 0.023(3) 0.024(2) 0.004(2) -0.002(2) 0.002(2) N20 0.024(3) 0.019(2) 0.031(2) -0.0031(17) -0.0013(19) 0.0015(17) N21 0.028(3) 0.030(3) 0.038(3) 0.010(2) 0.003(2) 0.004(2) C25 0.037(4) 0.054(4) 0.031(3) 0.025(3) 0.006(3) 0.008(3) C26 0.023(3) 0.063(4) 0.033(3) 0.023(3) 0.005(2) 0.007(3) C27 0.026(3) 0.017(2) 0.026(3) 0.0019(19) 0.000(2) -0.002(2) C28 0.020(3) 0.022(2) 0.027(2) -0.0026(19) -0.003(2) 0.000(2) C29 0.026(3) 0.023(3) 0.034(3) -0.003(2) 0.008(2) 0.001(2) C30 0.022(3) 0.021(2) 0.022(2) -0.0015(19) -0.001(2) -0.001(2) C31 0.020(3) 0.023(2) 0.017(2) 0.0020(18) 0.0048(19) 0.0021(19) C32 0.028(3) 0.020(2) 0.018(2) -0.0062(18) 0.009(2) -0.001(2) C33 0.020(3) 0.023(3) 0.021(2) -0.0012(19) 0.001(2) 0.004(2) C34 0.031(4) 0.078(5) 0.024(3) 0.012(3) 0.015(3) 0.027(3) C35 0.035(4) 0.153(9) 0.032(3) 0.055(5) 0.019(3) 0.039(5) C36 0.025(3) 0.022(3) 0.020(2) -0.0008(19) 0.000(2) -0.001(2) N22 0.026(3) 0.061(4) 0.026(2) 0.021(2) 0.009(2) 0.013(2) N23 0.018(2) 0.031(3) 0.042(3) -0.013(2) 0.004(2) -0.0044(19) C37 0.024(3) 0.027(3) 0.026(2) 0.004(2) 0.001(2) 0.001(2) C38 0.024(3) 0.024(3) 0.014(2) -0.0007(18) 0.0004(19) 0.003(2) C39 0.020(3) 0.025(3) 0.024(2) 0.0052(19) -0.004(2) 0.005(2) C40 0.022(3) 0.059(4) 0.035(3) -0.019(3) 0.008(2) -0.001(3) C41 0.025(3) 0.067(5) 0.042(4) -0.021(3) 0.002(3) -0.003(3) C42 0.028(3) 0.030(3) 0.019(2) 0.003(2) 0.006(2) 0.001(2) C43 0.025(3) 0.083(5) 0.031(3) -0.029(3) 0.004(2) -0.002(3) C44 0.025(3) 0.070(5) 0.024(3) -0.016(3) 0.005(2) -0.002(3) C45 0.022(3) 0.031(3) 0.016(2) -0.0021(19) -0.0005(19) 0.004(2) C46 0.025(3) 0.030(3) 0.017(2) -0.0071(19) -0.002(2) 0.001(2) C47 0.021(3) 0.028(3) 0.029(3) -0.004(2) 0.000(2) 0.001(2) C48 0.027(3) 0.024(3) 0.017(2) -0.0015(19) 0.001(2) 0.003(2) N24 0.019(2) 0.042(3) 0.031(2) -0.019(2) 0.0033(19) -0.0039(19) N25 0.024(3) 0.020(2) 0.027(2) 0.0052(18) 0.0033(19) 0.0040(18) C49 0.036(4) 0.025(3) 0.032(3) 0.004(2) 0.009(3) 0.004(2) C50 0.037(4) 0.037(3) 0.033(3) 0.003(3) 0.012(3) 0.009(3) C51 0.017(3) 0.044(4) 0.023(3) 0.008(2) -0.002(2) -0.005(2) C52 0.024(3) 0.030(3) 0.029(3) 0.011(2) 0.002(2) 0.003(2) C53 0.024(3) 0.022(3) 0.033(3) 0.010(2) -0.001(2) 0.000(2) C54 0.031(3) 0.030(3) 0.031(3) 0.003(2) 0.003(2) 0.000(2) C55 0.030(3) 0.022(3) 0.021(2) 0.004(2) 0.001(2) -0.001(2) C56 0.028(3) 0.026(3) 0.024(3) 0.003(2) 0.006(2) -0.002(2) C57 0.016(3) 0.033(3) 0.030(3) 0.000(2) 0.000(2) -0.001(2) C58 0.035(3) 0.037(3) 0.036(3) -0.011(3) 0.011(3) -0.005(3) C59 0.030(3) 0.019(3) 0.057(4) -0.004(3) 0.002(3) -0.005(2) C60 0.028(3) 0.023(3) 0.047(4) 0.000(2) -0.001(2) -0.003(2) N26 0.019(3) 0.017(2) 0.031(2) 0.0010(17) 0.0018(19) -0.0018(16) N27 0.021(3) 0.016(2) 0.023(2) 0.0033(16) -0.0028(18) 0.0007(17) C61 0.032(3) 0.016(2) 0.028(3) -0.002(2) 0.000(2) -0.003(2) C62 0.034(3) 0.018(3) 0.030(3) -0.003(2) 0.004(2) 0.000(2) C63 0.022(3) 0.031(3) 0.020(2) 0.003(2) -0.002(2) -0.005(2) C64 0.027(3) 0.020(3) 0.038(3) 0.000(2) 0.006(2) -0.002(2) C65 0.022(3) 0.015(2) 0.040(3) -0.003(2) 0.001(2) 0.000(2) C66 0.031(4) 0.035(3) 0.027(3) 0.004(2) 0.000(2) 0.001(3) C67 0.019(3) 0.018(2) 0.033(3) 0.004(2) -0.001(2) 0.002(2) C68 0.027(3) 0.016(2) 0.036(3) 0.005(2) -0.006(2) -0.003(2) C69 0.023(3) 0.018(2) 0.026(3) 0.0024(19) -0.002(2) 0.002(2) C70 0.022(3) 0.023(3) 0.024(2) 0.006(2) -0.001(2) 0.003(2) C71 0.027(3) 0.017(2) 0.031(3) 0.007(2) 0.002(2) 0.000(2) C72 0.028(3) 0.024(3) 0.033(3) 0.001(2) -0.001(2) 0.000(2) N28 0.014(2) 0.022(2) 0.023(2) 0.0036(16) 0.0005(17) -0.0024(17) N29 0.023(3) 0.016(2) 0.030(2) 0.0002(16) 0.007(2) -0.0011(16) C73 0.028(3) 0.021(3) 0.035(3) -0.007(2) 0.005(2) 0.001(2) C74 0.027(3) 0.032(3) 0.044(3) -0.011(3) 0.007(3) -0.001(2) C75 0.021(3) 0.046(4) 0.023(3) -0.002(2) 0.001(2) 0.002(3) C76 0.039(4) 0.028(3) 0.032(3) 0.007(2) 0.006(3) -0.006(3) C77 0.028(3) 0.018(3) 0.033(3) 0.003(2) 0.011(2) -0.003(2) C78 0.029(3) 0.035(3) 0.036(3) -0.002(3) 0.010(2) 0.001(2) C79 0.022(3) 0.026(3) 0.034(3) 0.005(2) 0.003(2) 0.005(2) C80 0.028(3) 0.049(4) 0.032(3) 0.020(3) -0.006(2) -0.003(3) C81 0.023(3) 0.032(3) 0.033(3) -0.006(2) -0.004(2) -0.001(2) C82 0.027(3) 0.033(3) 0.040(3) -0.008(2) 0.001(3) 0.003(2) C83 0.023(3) 0.027(3) 0.036(3) -0.006(2) 0.008(2) 0.001(2) C84 0.031(3) 0.029(3) 0.037(3) -0.006(2) 0.005(2) 0.004(2) N30 0.020(3) 0.031(3) 0.032(3) 0.001(2) 0.005(2) -0.0008(19) _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 1.940(5) . ? Cu1 N7 2.001(5) 2_655 ? Cu1 N30 2.042(5) 4_644 ? Cu1 N19 2.120(5) . ? Cu2 N4 1.932(5) . ? Cu2 N3 1.986(5) . ? Cu2 N25 2.045(5) . ? Cu2 N23 2.125(5) . ? Cu3 N18 1.942(5) 2_645 ? Cu3 N6 1.998(5) . ? Cu3 N28 2.071(4) 4_644 ? Cu3 N21 2.110(5) . ? Cu4 N9 1.915(5) . ? Cu4 N10 2.024(5) . ? Cu4 N27 2.044(5) . ? Cu4 N20 2.102(5) . ? Cu5 N12 1.938(5) . ? Cu5 N13 2.026(5) . ? Cu5 N26 2.051(5) 4_443 ? Cu5 N24 2.101(5) 1_354 ? Cu6 N15 1.940(5) . ? Cu6 N16 2.011(6) . ? Cu6 N29 2.061(5) . ? Cu6 N22 2.098(5) . ? N1 C1 1.145(7) . ? C1 N2 1.299(7) . ? N2 C2 1.287(8) . ? C2 N3 1.142(8) . ? N4 C3 1.164(7) . ? C3 N5 1.306(7) . ? N5 C4 1.306(8) . ? C4 N6 1.155(8) . ? N7 C5 1.155(8) . ? N7 Cu1 2.001(5) 2_454 ? C5 N8 1.281(8) . ? N8 C6 1.300(8) . ? C6 N9 1.150(8) . ? N10 C7 1.149(8) . ? C7 N11 1.310(8) . ? N11 C8 1.316(7) . ? C8 N12 1.130(7) . ? N13 C9 1.159(7) . ? C9 N14 1.285(7) . ? N14 C10 1.308(8) . ? C10 N15 1.170(8) . ? N16 C11 1.162(8) . ? C11 N17 1.297(9) . ? N17 C12 1.323(8) . ? C12 N18 1.149(8) . ? N18 Cu3 1.942(5) 2_444 ? N19 C13 1.342(8) . ? N19 C17 1.343(6) . ? C13 C14 1.358(8) . ? C14 C15 1.409(7) . ? C15 C16 1.392(8) . ? C15 C18 1.469(8) . ? C16 C17 1.374(8) . ? C18 C24 1.318(6) . ? C19 N20 1.321(7) . ? C19 C20 1.381(8) . ? C20 C21 1.378(8) . ? C21 C22 1.393(7) . ? C21 C24 1.467(8) . ? C22 C23 1.392(8) . ? C23 N20 1.341(8) . ? N21 C29 1.350(7) . ? N21 C25 1.355(8) . ? C25 C26 1.366(9) . ? C26 C27 1.388(8) . ? C27 C28 1.401(8) . ? C27 C30 1.456(8) . ? C28 C29 1.369(8) . ? C30 C36 1.321(6) . ? C31 N22 1.315(6) . ? C31 C32 1.378(8) . ? C32 C33 1.368(8) . ? C33 C34 1.405(8) . ? C33 C36 1.477(8) . ? C34 C35 1.391(10) . ? C35 N22 1.330(9) . ? N23 C37 1.324(7) . ? N23 C41 1.340(8) . ? C37 C38 1.396(8) . ? C38 C39 1.392(8) . ? C39 C40 1.378(8) . ? C39 C42 1.465(9) . ? C40 C41 1.402(9) . ? C42 C48 1.337(8) . ? C43 N24 1.348(8) . ? C43 C44 1.377(10) . ? C44 C45 1.378(7) . ? C45 C46 1.392(8) . ? C45 C48 1.451(8) . ? C46 C47 1.369(8) . ? C47 N24 1.319(7) . ? N24 Cu5 2.101(5) 1_756 ? N25 C53 1.337(7) . ? N25 C49 1.340(8) . ? C49 C50 1.367(8) . ? C50 C51 1.431(9) . ? C51 C52 1.391(8) . ? C51 C54 1.473(7) . ? C52 C53 1.380(8) . ? C54 C60 1.314(8) . ? C55 N26 1.347(7) . ? C55 C56 1.373(8) . ? C56 C57 1.373(8) . ? C57 C58 1.385(9) . ? C57 C60 1.490(8) . ? C58 C59 1.373(9) . ? C59 N26 1.361(7) . ? N26 Cu5 2.051(5) 4_546 ? N27 C65 1.335(7) . ? N27 C61 1.363(7) . ? C61 C62 1.373(8) . ? C62 C63 1.386(8) . ? C63 C64 1.410(8) . ? C63 C66 1.460(8) . ? C64 C65 1.367(8) . ? C66 C72 1.336(8) . ? C67 N28 1.328(7) . ? C67 C68 1.367(8) . ? C68 C69 1.400(8) . ? C69 C70 1.390(8) . ? C69 C72 1.470(8) . ? C70 C71 1.366(8) . ? C71 N28 1.354(7) . ? N28 Cu3 2.071(4) 4_345 ? N29 C77 1.339(7) . ? N29 C73 1.358(7) . ? C73 C74 1.364(8) . ? C74 C75 1.369(9) . ? C75 C76 1.407(9) . ? C75 C78 1.468(8) . ? C76 C77 1.373(8) . ? C78 C84 1.305(9) . ? C79 N30 1.329(7) . ? C79 C80 1.399(9) . ? C80 C81 1.406(9) . ? C81 C82 1.364(9) . ? C81 C84 1.476(8) . ? C82 C83 1.364(9) . ? C83 N30 1.342(8) . ? N30 Cu1 2.042(5) 4_345 ? 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 N7 112.2(2) . 2_655 ? N1 Cu1 N30 127.6(2) . 4_644 ? N7 Cu1 N30 102.3(2) 2_655 4_644 ? N1 Cu1 N19 105.3(2) . . ? N7 Cu1 N19 104.9(2) 2_655 . ? N30 Cu1 N19 102.4(2) 4_644 . ? N4 Cu2 N3 119.1(2) . . ? N4 Cu2 N25 119.6(2) . . ? N3 Cu2 N25 104.4(2) . . ? N4 Cu2 N23 103.8(2) . . ? N3 Cu2 N23 106.7(2) . . ? N25 Cu2 N23 101.0(2) . . ? N18 Cu3 N6 125.2(2) 2_645 . ? N18 Cu3 N28 114.56(19) 2_645 4_644 ? N6 Cu3 N28 101.9(2) . 4_644 ? N18 Cu3 N21 106.4(2) 2_645 . ? N6 Cu3 N21 104.2(2) . . ? N28 Cu3 N21 102.02(19) 4_644 . ? N9 Cu4 N10 113.6(2) . . ? N9 Cu4 N27 127.1(2) . . ? N10 Cu4 N27 100.8(2) . . ? N9 Cu4 N20 106.7(2) . . ? N10 Cu4 N20 103.5(2) . . ? N27 Cu4 N20 102.48(19) . . ? N12 Cu5 N13 120.0(2) . . ? N12 Cu5 N26 120.4(2) . 4_443 ? N13 Cu5 N26 101.6(2) . 4_443 ? N12 Cu5 N24 107.7(2) . 1_354 ? N13 Cu5 N24 102.5(2) . 1_354 ? N26 Cu5 N24 101.94(19) 4_443 1_354 ? N15 Cu6 N16 127.3(2) . . ? N15 Cu6 N29 113.2(2) . . ? N16 Cu6 N29 101.2(2) . . ? N15 Cu6 N22 108.0(2) . . ? N16 Cu6 N22 102.7(2) . . ? N29 Cu6 N22 101.2(2) . . ? C1 N1 Cu1 172.4(5) . . ? N1 C1 N2 175.3(7) . . ? C2 N2 C1 122.4(5) . . ? N3 C2 N2 174.0(6) . . ? C2 N3 Cu2 164.9(5) . . ? C3 N4 Cu2 173.6(5) . . ? N4 C3 N5 172.2(7) . . ? C4 N5 C3 119.0(5) . . ? N6 C4 N5 172.9(7) . . ? C4 N6 Cu3 154.9(5) . . ? C5 N7 Cu1 165.8(5) . 2_454 ? N7 C5 N8 173.1(7) . . ? C5 N8 C6 123.4(6) . . ? N9 C6 N8 172.1(7) . . ? C6 N9 Cu4 171.1(5) . . ? C7 N10 Cu4 163.0(5) . . ? N10 C7 N11 172.5(6) . . ? C7 N11 C8 121.8(5) . . ? N12 C8 N11 172.8(7) . . ? C8 N12 Cu5 169.5(5) . . ? C9 N13 Cu5 155.9(5) . . ? N13 C9 N14 172.6(7) . . ? C9 N14 C10 123.7(6) . . ? N15 C10 N14 172.9(7) . . ? C10 N15 Cu6 166.2(5) . . ? C11 N16 Cu6 150.5(5) . . ? N16 C11 N17 172.7(6) . . ? C11 N17 C12 123.9(5) . . ? N18 C12 N17 174.6(7) . . ? C12 N18 Cu3 168.4(5) . 2_444 ? C13 N19 C17 115.8(5) . . ? C13 N19 Cu1 118.9(3) . . ? C17 N19 Cu1 122.0(4) . . ? N19 C13 C14 125.1(5) . . ? C13 C14 C15 118.4(5) . . ? C16 C15 C14 117.3(5) . . ? C16 C15 C18 120.2(5) . . ? C14 C15 C18 122.5(5) . . ? C17 C16 C15 119.2(5) . . ? N19 C17 C16 123.9(5) . . ? C24 C18 C15 127.3(4) . . ? N20 C19 C20 125.4(6) . . ? C21 C20 C19 118.8(5) . . ? C20 C21 C22 117.3(5) . . ? C20 C21 C24 120.0(5) . . ? C22 C21 C24 122.7(5) . . ? C23 C22 C21 119.0(5) . . ? N20 C23 C22 123.8(5) . . ? C18 C24 C21 127.2(4) . . ? C19 N20 C23 115.5(5) . . ? C19 N20 Cu4 122.1(4) . . ? C23 N20 Cu4 118.3(4) . . ? C29 N21 C25 116.2(5) . . ? C29 N21 Cu3 122.5(4) . . ? C25 N21 Cu3 120.4(4) . . ? N21 C25 C26 123.4(5) . . ? C25 C26 C27 120.4(6) . . ? C26 C27 C28 116.3(6) . . ? C26 C27 C30 123.9(6) . . ? C28 C27 C30 119.8(5) . . ? C29 C28 C27 120.1(5) . . ? N21 C29 C28 123.4(5) . . ? C36 C30 C27 126.6(5) . . ? N22 C31 C32 123.3(5) . . ? C33 C32 C31 120.8(5) . . ? C32 C33 C34 116.8(5) . . ? C32 C33 C36 121.0(5) . . ? C34 C33 C36 122.2(5) . . ? C35 C34 C33 117.8(6) . . ? N22 C35 C34 124.3(5) . . ? C30 C36 C33 127.5(4) . . ? C31 N22 C35 116.8(5) . . ? C31 N22 Cu6 122.8(4) . . ? C35 N22 Cu6 119.0(4) . . ? C37 N23 C41 117.2(5) . . ? C37 N23 Cu2 123.3(4) . . ? C41 N23 Cu2 117.2(4) . . ? N23 C37 C38 123.4(5) . . ? C39 C38 C37 119.9(5) . . ? C40 C39 C38 116.3(6) . . ? C40 C39 C42 124.3(5) . . ? C38 C39 C42 119.3(5) . . ? C39 C40 C41 120.5(6) . . ? N23 C41 C40 122.4(6) . . ? C48 C42 C39 124.6(5) . . ? N24 C43 C44 122.4(5) . . ? C43 C44 C45 121.3(6) . . ? C44 C45 C46 114.8(6) . . ? C44 C45 C48 125.0(5) . . ? C46 C45 C48 120.0(5) . . ? C47 C46 C45 120.9(5) . . ? N24 C47 C46 123.6(5) . . ? C42 C48 C45 125.7(5) . . ? C47 N24 C43 116.6(5) . . ? C47 N24 Cu5 122.5(4) . 1_756 ? C43 N24 Cu5 118.3(4) . 1_756 ? C53 N25 C49 118.4(5) . . ? C53 N25 Cu2 120.7(4) . . ? C49 N25 Cu2 120.4(4) . . ? N25 C49 C50 123.4(6) . . ? C49 C50 C51 118.9(6) . . ? C52 C51 C50 116.7(5) . . ? C52 C51 C54 119.6(5) . . ? C50 C51 C54 123.8(6) . . ? C53 C52 C51 120.2(5) . . ? N25 C53 C52 122.5(5) . . ? C60 C54 C51 124.8(5) . . ? N26 C55 C56 124.0(5) . . ? C55 C56 C57 120.9(5) . . ? C56 C57 C58 116.8(5) . . ? C56 C57 C60 119.0(5) . . ? C58 C57 C60 124.1(5) . . ? C59 C58 C57 119.0(6) . . ? N26 C59 C58 125.3(6) . . ? C54 C60 C57 124.1(6) . . ? C55 N26 C59 114.0(5) . . ? C55 N26 Cu5 120.8(4) . 4_546 ? C59 N26 Cu5 123.8(4) . 4_546 ? C65 N27 C61 116.2(5) . . ? C65 N27 Cu4 120.7(4) . . ? C61 N27 Cu4 122.2(4) . . ? N27 C61 C62 123.3(5) . . ? C61 C62 C63 120.2(5) . . ? C62 C63 C64 116.4(5) . . ? C62 C63 C66 124.0(6) . . ? C64 C63 C66 119.6(5) . . ? C65 C64 C63 119.9(5) . . ? N27 C65 C64 124.0(5) . . ? C72 C66 C63 125.5(6) . . ? N28 C67 C68 122.1(5) . . ? C67 C68 C69 121.2(5) . . ? C70 C69 C68 116.4(5) . . ? C70 C69 C72 123.4(5) . . ? C68 C69 C72 120.1(5) . . ? C71 C70 C69 119.0(5) . . ? N28 C71 C70 124.0(5) . . ? C66 C72 C69 125.7(6) . . ? C67 N28 C71 117.3(5) . . ? C67 N28 Cu3 121.4(4) . 4_345 ? C71 N28 Cu3 120.6(4) . 4_345 ? C77 N29 C73 115.4(5) . . ? C77 N29 Cu6 122.2(4) . . ? C73 N29 Cu6 121.2(4) . . ? N29 C73 C74 124.6(6) . . ? C73 C74 C75 120.1(6) . . ? C74 C75 C76 116.2(6) . . ? C74 C75 C78 118.1(6) . . ? C76 C75 C78 125.6(6) . . ? C77 C76 C75 120.4(6) . . ? N29 C77 C76 123.2(5) . . ? C84 C78 C75 126.4(6) . . ? N30 C79 C80 123.4(6) . . ? C79 C80 C81 118.4(6) . . ? C82 C81 C80 117.6(6) . . ? C82 C81 C84 121.2(6) . . ? C80 C81 C84 121.3(6) . . ? C83 C82 C81 119.8(6) . . ? N30 C83 C82 124.4(6) . . ? C78 C84 C81 127.8(6) . . ? C79 N30 C83 116.3(5) . . ? C79 N30 Cu1 123.6(4) . 4_345 ? C83 N30 Cu1 119.4(4) . 4_345 ? _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.792 _refine_diff_density_min -1.072 _refine_diff_density_rms 0.133 #=END