Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_cubpcadca _database_code_CSD 174338 _journal_coden_Cambridge 186 _manuscript_identification_number B105981P _publ_requested_journal 'Dalton Transactions' _publ_contact_author_name 'Prof Jorunn Sletten' _publ_contact_author_address ; Prof Jorunn Sletten Department of Chemistry University of Bergen Allegaten 41 N-5007 Bergen NORWAY ; _publ_contact_author_email 'JORUNN.SLETTEN@KJ.UIB.NO' # TITLE AND AUTHOR LIST _publ_section_title ; Syntheses, crystal structures and magnetic properties of copper(II) dicyanamide complexes; dinuclear, chain and ladder compounds ; loop_ _publ_author_name _publ_author_address 'Brita Vangdal' ;Department of Chemistry University of Bergen Allegaten 41 N-5007 Bergen Norway ; 'Jose Carranza' ;Department of Inorganic Chemistry Faculty of Chemistry University of Valencia Dr. Moliner 50 46100 Burjassot (Valencia) Spain ; 'Francesc Lloret' ;Department of Inorganic Chemistry Faculty of Chemistry University of Valencia Dr. Moliner 50 46100 Burjassot (Valencia) Spain ; 'Miguel Julve' ;Department of Inorganic Chemistry Faculty of Chemistry University of Valencia Dr. Moliner 50 46100 Burjassot (Valencia) Spain ; 'Jorunn Sletten' ;Department of Chemistry University of Bergen Allegaten 41 N-5007 Bergen Norway ; _audit_creation_method SHELXL _chemical_name_systematic ? _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[Cu1 (C12 H8 N3) (C2 N3) (H2 O)]2' _chemical_formula_analytical ? _chemical_formula_sum 'C14 H10 Cu N6 O3' _chemical_formula_weight 373.82 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.2838(15) _cell_length_b 10.357(2) _cell_length_c 11.003(2) _cell_angle_alpha 115.50(3) _cell_angle_beta 97.85(3) _cell_angle_gamma 96.98(3) _cell_volume 726.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'irregular shape' _exptl_crystal_colour blue _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.708 _exptl_crystal_density_method ? _exptl_crystal_F_000 378 _exptl_absorpt_coefficient_mu 1.530 _exptl_absorpt_correction_type 'empirical, SADABS' _exptl_absorpt_correction_T_min 'Tmin/Tmax ratio 0.786530' _exptl_absorpt_correction_T_max 'see above' _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 '2K SMART CCD' _diffrn_measurement_method \\w _diffrn_standards_number '50 first frames remeasured at end of experiment' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6562 _diffrn_reflns_av_R_equivalents 0.0206 _diffrn_reflns_av_sigmaI/netI 0.0402 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 30.45 _reflns_number_total 4304 _reflns_number_observed 3477 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART,version 5.054' _computing_cell_refinement 'SAINT, version 5.00' _computing_data_reduction 'SAINT, version 5.00' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'XP, VERSION 4.3, 1992' _computing_publication_material 'ciftab, sHELDRICK, 1993' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 3 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\\s^2^(Fo^2^)+(0.0505P)^2^+0.0302P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom when bound to C, difmap when bound to O' _refine_ls_hydrogen_treatment ?'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4301 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0461 _refine_ls_R_factor_obs 0.0333 _refine_ls_wR_factor_all 0.0853 _refine_ls_wR_factor_obs 0.0807 _refine_ls_goodness_of_fit_all 1.028 _refine_ls_goodness_of_fit_obs 1.090 _refine_ls_restrained_S_all 1.029 _refine_ls_restrained_S_obs 1.090 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cu1 Cu 0.28775(3) 0.45045(2) 0.23923(2) 0.01941(7) Uani 1 d . . O1 O -0.2499(2) 0.45123(14) 0.08211(14) 0.0237(3) Uani 1 d . . O2 O -0.0073(2) 0.72168(14) 0.15594(14) 0.0241(3) Uani 1 d . . O3 O 0.3605(2) 0.32714(14) 0.02009(13) 0.0218(3) Uani 1 d . . H31 H 0.4605 0.37605 0.02110 0.033 Uiso 1 d R . H32 H 0.2874 0.33805 -0.03450 0.033 Uiso 1 d R . N1 N 0.0812(2) 0.2768(2) 0.1920(2) 0.0198(3) Uani 1 d . . N2 N 0.0735(2) 0.5208(2) 0.1799(2) 0.0180(3) Uani 1 d . . N3 N 0.4264(2) 0.6534(2) 0.2837(2) 0.0214(3) Uani 1 d . . N4 N 0.4967(2) 0.3951(2) 0.3263(2) 0.0264(3) Uani 1 d . . N5 N 0.7767(3) 0.4182(2) 0.4930(2) 0.0377(4) Uani 1 d . . N6 N 0.9520(3) 0.2276(2) 0.4909(2) 0.0381(4) Uani 1 d . . C1 C 0.0983(3) 0.1551(2) 0.2037(2) 0.0244(4) Uani 1 d . . H1 H 0.2161 0.1476 0.2420 0.037 Uiso 1 calc R . C2 C -0.0545(3) 0.0394(2) 0.1606(2) 0.0280(4) Uani 1 d . . H2 H -0.0390 -0.0439 0.1699 0.042 Uiso 1 calc R . C3 C -0.2292(3) 0.0504(2) 0.1038(2) 0.0284(4) Uani 1 d . . H3 H -0.3326 -0.0261 0.0733 0.043 Uiso 1 calc R . C4 C -0.2495(3) 0.1775(2) 0.0924(2) 0.0243(4) Uani 1 d . . H4 H -0.3664 0.1875 0.0554 0.036 Uiso 1 calc R . C5 C -0.0909(2) 0.2883(2) 0.1376(2) 0.0184(3) Uani 1 d . . C6 C -0.1009(2) 0.4295(2) 0.1295(2) 0.0177(3) Uani 1 d . . C7 C 0.1054(2) 0.6586(2) 0.1904(2) 0.0182(3) Uani 1 d . . C8 C 0.3110(2) 0.7327(2) 0.2532(2) 0.0206(3) Uani 1 d . . C9 C 0.3750(3) 0.8751(2) 0.2782(2) 0.0272(4) Uani 1 d . . H9 H 0.2925 0.9274 0.2561 0.041 Uiso 1 calc R . C10 C 0.5654(3) 0.9388(2) 0.3371(2) 0.0302(4) Uani 1 d . . H10 H 0.6121 1.0344 0.3552 0.045 Uiso 1 calc R . C11 C 0.6845(3) 0.8572(2) 0.3682(2) 0.0293(4) Uani 1 d . . H11 H 0.8121 0.8975 0.4074 0.044 Uiso 1 calc R . C12 C 0.6108(2) 0.7152(2) 0.3401(2) 0.0263(4) Uani 1 d . . H12 H 0.6910 0.6607 0.3608 0.039 Uiso 1 calc R . C13 C 0.6289(3) 0.3968(2) 0.3999(2) 0.0263(4) Uani 1 d . . C14 C 0.8658(3) 0.3113(2) 0.4843(2) 0.0251(4) Uani 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 0.01467(11) 0.01916(11) 0.02490(12) 0.01144(9) -0.00099(7) 0.00544(7) O1 0.0158(6) 0.0260(6) 0.0331(7) 0.0177(6) 0.0012(5) 0.0053(5) O2 0.0196(6) 0.0203(6) 0.0341(7) 0.0155(6) -0.0008(5) 0.0049(5) O3 0.0149(5) 0.0269(6) 0.0262(7) 0.0152(5) 0.0010(5) 0.0045(5) N1 0.0209(7) 0.0202(7) 0.0215(7) 0.0117(6) 0.0040(5) 0.0073(5) N2 0.0144(6) 0.0180(7) 0.0230(7) 0.0115(6) 0.0000(5) 0.0042(5) N3 0.0147(6) 0.0230(7) 0.0248(8) 0.0104(6) 0.0002(5) 0.0041(5) N4 0.0247(8) 0.0298(8) 0.0275(8) 0.0145(7) 0.0025(6) 0.0121(6) N5 0.0337(9) 0.0350(10) 0.0365(10) 0.0118(8) -0.0077(8) 0.0136(8) N6 0.0345(9) 0.0371(10) 0.0376(10) 0.0137(8) -0.0038(8) 0.0148(8) C1 0.0250(9) 0.0227(9) 0.0312(10) 0.0170(8) 0.0043(7) 0.0085(7) C2 0.0326(10) 0.0222(9) 0.0349(11) 0.0174(8) 0.0080(8) 0.0079(7) C3 0.0289(9) 0.0222(9) 0.0336(10) 0.0140(8) 0.0046(8) 0.0008(7) C4 0.0205(8) 0.0238(9) 0.0297(10) 0.0140(8) 0.0030(7) 0.0033(7) C5 0.0171(7) 0.0198(8) 0.0211(8) 0.0111(7) 0.0050(6) 0.0050(6) C6 0.0156(7) 0.0203(8) 0.0190(8) 0.0104(7) 0.0030(6) 0.0047(6) C7 0.0164(7) 0.0193(8) 0.0193(8) 0.0093(6) 0.0015(6) 0.0053(6) C8 0.0189(8) 0.0207(8) 0.0201(8) 0.0083(7) 0.0004(6) 0.0042(6) C9 0.0239(9) 0.0236(9) 0.0345(10) 0.0159(8) -0.0003(7) 0.0026(7) C10 0.0259(9) 0.0229(9) 0.0371(11) 0.0134(8) 0.0001(8) -0.0034(7) C11 0.0176(8) 0.0310(10) 0.0324(10) 0.0109(8) 0.0000(7) -0.0003(7) C12 0.0164(8) 0.0280(9) 0.0314(10) 0.0117(8) 0.0006(7) 0.0055(7) C13 0.0264(9) 0.0309(10) 0.0264(9) 0.0151(8) 0.0064(7) 0.0133(7) C14 0.0215(8) 0.0314(10) 0.0209(9) 0.0110(8) 0.0005(7) 0.0074(7) _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 1.9491(14) . ? Cu1 N4 1.962(2) . ? Cu1 N1 2.023(2) . ? Cu1 N3 2.034(2) . ? Cu1 O3 2.3638(15) . ? Cu1 N5 2.799(2) 2_666 ? O1 C6 1.227(2) . ? O2 C7 1.226(2) . ? O3 H31 0.83 . ? O3 H32 0.80 . ? N1 C1 1.340(2) . ? N1 C5 1.355(2) . ? N2 C7 1.369(2) . ? N2 C6 1.371(2) . ? N3 C12 1.350(2) . ? N3 C8 1.350(2) . ? N4 C13 1.164(3) . ? N5 C13 1.305(3) . ? N5 C14 1.326(3) . ? N6 C14 1.151(3) . ? C1 C2 1.393(3) . ? C1 H1 0.93 . ? C2 C3 1.379(3) . ? C2 H2 0.93 . ? C3 C4 1.398(3) . ? C3 H3 0.93 . ? C4 C5 1.389(2) . ? C4 H4 0.93 . ? C5 C6 1.512(2) . ? C7 C8 1.513(2) . ? C8 C9 1.384(3) . ? C9 C10 1.394(3) . ? C9 H9 0.93 . ? C10 C11 1.389(3) . ? C10 H10 0.93 . ? C11 C12 1.385(3) . ? C11 H11 0.93 . ? C12 H12 0.93 . ? 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 N4 171.57(6) . . ? N2 Cu1 N1 81.51(6) . . ? N4 Cu1 N1 98.86(7) . . ? N2 Cu1 N3 81.64(6) . . ? N4 Cu1 N3 97.15(7) . . ? N1 Cu1 N3 162.57(6) . . ? N2 Cu1 O3 96.76(6) . . ? N4 Cu1 O3 91.67(6) . . ? N1 Cu1 O3 89.70(6) . . ? N3 Cu1 O3 96.70(6) . . ? N2 Cu1 N5 88.48(6) . 2_666 ? N4 Cu1 N5 83.10(7) . 2_666 ? N1 Cu1 N5 89.68(7) . 2_666 ? N3 Cu1 N5 85.44(7) . 2_666 ? O3 Cu1 N5 174.57(5) . 2_666 ? Cu1 O3 H31 106.67 . . ? Cu1 O3 H32 108.05 . . ? H31 O3 H32 100.7 . . ? C1 N1 C5 118.9(2) . . ? C1 N1 Cu1 127.82(13) . . ? C5 N1 Cu1 113.26(11) . . ? C7 N2 C6 123.50(14) . . ? C7 N2 Cu1 118.24(11) . . ? C6 N2 Cu1 118.26(11) . . ? C12 N3 C8 118.7(2) . . ? C12 N3 Cu1 128.58(13) . . ? C8 N3 Cu1 112.73(11) . . ? C13 N4 Cu1 163.9(2) . . ? C13 N5 C14 121.5(2) . . ? N1 C1 C2 122.2(2) . . ? N1 C1 H1 118.90 . . ? C2 C1 H1 118.90 . . ? C3 C2 C1 118.9(2) . . ? C3 C2 H2 120.54 . . ? C1 C2 H2 120.54 . . ? C2 C3 C4 119.5(2) . . ? C2 C3 H3 120.25 . . ? C4 C3 H3 120.25 . . ? C5 C4 C3 118.4(2) . . ? C5 C4 H4 120.81 . . ? C3 C4 H4 120.81 . . ? N1 C5 C4 122.1(2) . . ? N1 C5 C6 116.13(15) . . ? C4 C5 C6 121.7(2) . . ? O1 C6 N2 127.9(2) . . ? O1 C6 C5 121.5(2) . . ? N2 C6 C5 110.65(14) . . ? O2 C7 N2 128.6(2) . . ? O2 C7 C8 120.7(2) . . ? N2 C7 C8 110.73(14) . . ? N3 C8 C9 122.4(2) . . ? N3 C8 C7 116.6(2) . . ? C9 C8 C7 121.0(2) . . ? C8 C9 C10 118.7(2) . . ? C8 C9 H9 120.63 . . ? C10 C9 H9 120.63 . . ? C11 C10 C9 119.0(2) . . ? C11 C10 H10 120.50 . . ? C9 C10 H10 120.50 . . ? C12 C11 C10 119.2(2) . . ? C12 C11 H11 120.42 . . ? C10 C11 H11 120.42 . . ? N3 C12 C11 122.0(2) . . ? N3 C12 H12 118.98 . . ? C11 C12 H12 118.98 . . ? N4 C13 N5 171.9(2) . . ? N6 C14 N5 172.9(2) . . ? _refine_diff_density_max 0.512 _refine_diff_density_min -0.449 _refine_diff_density_rms 0.076 #===END data_cubpydca _database_code_CSD 174339 _journal_coden_Cambridge 186 _manuscript_identification_number B105981P _publ_requested_journal 'Dalton Transactions' _publ_contact_author_name 'Prof Jorunn Sletten' _publ_contact_author_address ; Prof Jorunn Sletten Department of Chemistry University of Bergen Allegaten 41 N-5007 Bergen NORWAY ; _publ_contact_author_email 'JORUNN.SLETTEN@KJ.UIB.NO' # TITLE AND AUTHOR LIST _publ_section_title ; Syntheses, crystal structures and magnetic properties of copper(II) dicyanamide complexes; dinuclear, chain and ladder compounds ; loop_ _publ_author_name _publ_author_address 'Brita Vangdal' ;Department of Chemistry University of Bergen Allegaten 41 N-5007 Bergen Norway ; 'Jose Carranza' ;Department of Inorganic Chemistry Faculty of Chemistry University of Valencia Dr. Moliner 50 46100 Burjassot (Valencia) Spain ; 'Francesc Lloret' ;Department of Inorganic Chemistry Faculty of Chemistry University of Valencia Dr. Moliner 50 46100 Burjassot (Valencia) Spain ; 'Miguel Julve' ;Department of Inorganic Chemistry Faculty of Chemistry University of Valencia Dr. Moliner 50 46100 Burjassot (Valencia) Spain ; 'Jorunn Sletten' ;Department of Chemistry University of Bergen Allegaten 41 N-5007 Bergen Norway ; _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[Cu1 (C10 H8 N2) (C2 N3)2]n' _chemical_formula_analytical ? _chemical_formula_sum 'C14 H8 Cu N8' _chemical_formula_weight 351.82 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 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' _cell_length_a 8.6391(10) _cell_length_b 17.165(2) _cell_length_c 10.4638(13) _cell_angle_alpha 90.00 _cell_angle_beta 114.307(2) _cell_angle_gamma 90.00 _cell_volume 1414.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour blue _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.653 _exptl_crystal_density_method ? _exptl_crystal_F_000 708 _exptl_absorpt_coefficient_mu 1.557 _exptl_absorpt_correction_type 'empirical, SADABS' _exptl_absorpt_correction_T_min 'Tmin/Tmax ratio 0.752912' _exptl_absorpt_correction_T_max 'see above' _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 '2K SMART CCD' _diffrn_measurement_method \\w _diffrn_standards_number '50 first frames remeasured at end of data collection' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6199 _diffrn_reflns_av_R_equivalents 0.0175 _diffrn_reflns_av_sigmaI/netI 0.0275 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 30.54 _reflns_number_total 3434 _reflns_number_observed 3173 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART, version 5.054' _computing_cell_refinement 'SAINT, version 5.00' _computing_data_reduction 'SAINT, version 5.00' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'XP, version 4.3, 1992' _computing_publication_material 'CIFTAB, Sheldrick, 1993' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\\s^2^(Fo^2^)+(0.0340P)^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 'riding model' _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 0.011(8) _refine_ls_number_reflns 3434 _refine_ls_number_parameters 208 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0247 _refine_ls_R_factor_obs 0.0220 _refine_ls_wR_factor_all 0.0545 _refine_ls_wR_factor_obs 0.0537 _refine_ls_goodness_of_fit_all 1.014 _refine_ls_goodness_of_fit_obs 1.043 _refine_ls_restrained_S_all 1.014 _refine_ls_restrained_S_obs 1.042 _refine_ls_shift/esd_max 0.007 _refine_ls_shift/esd_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cu1 Cu 0.02749(2) 0.183924(9) 0.51052(2) 0.02461(5) Uani 1 d . . N1 N -0.2267(3) 0.18705(8) 0.4306(2) 0.0245(4) Uani 1 d . . N2 N -0.0077(2) 0.30056(8) 0.5014(2) 0.0266(3) Uani 1 d . . N3 N 0.2757(3) 0.19158(11) 0.6078(3) 0.0374(5) Uani 1 d . . N4 N 0.5828(3) 0.17499(11) 0.6889(3) 0.0420(5) Uani 1 d . . N5 N 0.7627(3) 0.06135(10) 0.7956(2) 0.0482(5) Uani 1 d . . N6 N 0.0339(2) 0.07805(10) 0.5915(2) 0.0381(4) Uani 1 d . . N7 N 0.0963(4) -0.05789(13) 0.6585(3) 0.0643(7) Uani 1 d . . N8 N 0.0253(2) -0.14122(9) 0.8149(2) 0.0346(3) Uani 1 d . . C1 C -0.3269(2) 0.12514(10) 0.3875(2) 0.0298(3) Uani 1 d . . H1 H -0.2768 0.07494 0.3981 0.045 Uiso 1 d R . C2 C -0.5029(3) 0.13153(13) 0.3274(2) 0.0342(4) Uani 1 d . . H2 H -0.5721 0.08638 0.2974 0.051 Uiso 1 d R . C3 C -0.5756(3) 0.20472(15) 0.3123(2) 0.0357(4) Uani 1 d . . H3 H -0.6956 0.21038 0.2732 0.054 Uiso 1 d R . C4 C -0.4711(2) 0.26976(11) 0.3550(2) 0.0323(4) Uani 1 d . . H4 H -0.5182 0.32060 0.3446 0.049 Uiso 1 d R . C5 C -0.2968(2) 0.25927(10) 0.4130(2) 0.0246(3) Uani 1 d . . C6 C -0.1714(2) 0.32357(9) 0.4568(2) 0.0250(3) Uani 1 d . . C7 C -0.2155(3) 0.40181(11) 0.4530(2) 0.0326(4) Uani 1 d . . H7 H -0.3308 0.41715 0.4228 0.049 Uiso 1 d R . C8 C -0.0859(3) 0.45705(11) 0.4950(2) 0.0388(4) Uani 1 d . . H8 H -0.1122 0.51087 0.4936 0.058 Uiso 1 d R . C9 C 0.0789(3) 0.43375(12) 0.5377(2) 0.0406(5) Uani 1 d . . H9 H 0.1679 0.47113 0.5657 0.061 Uiso 1 d R . C10 C 0.1153(3) 0.35421(11) 0.5403(2) 0.0348(4) Uani 1 d . . H10 H 0.2300 0.33792 0.5703 0.052 Uiso 1 d R . C11 C 0.4201(3) 0.17973(10) 0.6480(2) 0.0305(4) Uani 1 d . . C12 C 0.6702(2) 0.11206(11) 0.7450(2) 0.0327(4) Uani 1 d . . C13 C 0.0570(3) 0.01453(12) 0.6268(2) 0.0364(4) Uani 1 d . . C14 C 0.0524(2) -0.09828(9) 0.7437(2) 0.0272(3) Uani 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 0.01994(9) 0.02485(8) 0.02748(9) -0.00074(10) 0.00817(7) -0.00055(10) N1 0.0198(9) 0.0260(9) 0.0262(9) -0.0003(5) 0.0079(7) 0.0011(6) N2 0.0245(9) 0.0295(7) 0.0247(7) -0.0016(6) 0.0089(8) -0.0014(5) N3 0.0240(11) 0.0376(11) 0.0444(13) 0.0013(8) 0.0079(9) 0.0017(7) N4 0.0226(9) 0.0371(10) 0.0616(14) 0.0092(8) 0.0126(9) -0.0008(7) N5 0.0361(10) 0.0350(9) 0.0660(13) 0.0007(8) 0.0134(9) -0.0001(8) N6 0.0292(8) 0.0390(8) 0.0418(9) 0.0128(7) 0.0104(7) 0.0020(7) N7 0.084(2) 0.0501(11) 0.092(2) 0.0397(12) 0.070(2) 0.0339(11) N8 0.0361(8) 0.0321(8) 0.0391(8) 0.0053(6) 0.0189(7) 0.0025(6) C1 0.0253(8) 0.0279(8) 0.0340(8) -0.0009(7) 0.0099(7) -0.0034(7) C2 0.0253(9) 0.0375(10) 0.0358(10) 0.0025(8) 0.0086(7) -0.0073(8) C3 0.0200(9) 0.0462(10) 0.0378(10) 0.0061(9) 0.0089(8) -0.0017(9) C4 0.0249(9) 0.0350(9) 0.0367(9) 0.0074(7) 0.0122(7) 0.0085(7) C5 0.0229(8) 0.0275(7) 0.0235(7) 0.0011(6) 0.0096(6) 0.0016(6) C6 0.0251(8) 0.0266(8) 0.0224(7) -0.0002(6) 0.0089(7) 0.0002(6) C7 0.0380(10) 0.0295(9) 0.0297(8) 0.0005(7) 0.0135(7) 0.0024(7) C8 0.0502(13) 0.0258(9) 0.0393(11) -0.0021(7) 0.0174(10) -0.0026(9) C9 0.0489(13) 0.0309(9) 0.0422(13) -0.0068(8) 0.0189(10) -0.0160(8) C10 0.0312(11) 0.0366(10) 0.0350(10) -0.0056(7) 0.0119(8) -0.0103(8) C11 0.0264(9) 0.0309(9) 0.0322(9) -0.0007(6) 0.0101(7) -0.0032(6) C12 0.0251(9) 0.0326(8) 0.0374(9) -0.0056(7) 0.0097(7) -0.0067(7) C13 0.0296(9) 0.0413(10) 0.0416(10) 0.0136(8) 0.0180(8) 0.0067(8) C14 0.0228(8) 0.0272(8) 0.0301(8) 0.0017(6) 0.0094(6) 0.0043(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N3 1.963(3) . ? Cu1 N6 1.996(2) . ? Cu1 N1 2.003(2) . ? Cu1 N2 2.0213(14) . ? Cu1 N8 2.167(2) 2_554 ? N1 C1 1.327(3) . ? N1 C5 1.359(2) . ? N2 C10 1.337(2) . ? N2 C6 1.353(2) . ? N3 C11 1.159(4) . ? N4 C11 1.293(3) . ? N4 C12 1.311(3) . ? N5 C12 1.152(3) . ? N6 C13 1.142(3) . ? N7 C13 1.295(3) . ? N7 C14 1.303(3) . ? N8 C14 1.139(2) . ? N8 Cu1 2.167(2) 2 ? C1 C2 1.390(3) . ? C1 H1 0.95 . ? C2 C3 1.384(3) . ? C2 H2 0.95 . ? C3 C4 1.388(3) . ? C3 H3 0.95 . ? C4 C5 1.384(2) . ? C4 H4 0.95 . ? C5 C6 1.481(2) . ? C6 C7 1.392(2) . ? C7 C8 1.393(3) . ? C7 H7 0.95 . ? C8 C9 1.365(3) . ? C8 H8 0.95 . ? C9 C10 1.399(3) . ? C9 H9 0.95 . ? C10 H10 0.95 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Cu1 N6 90.41(8) . . ? N3 Cu1 N1 172.03(10) . . ? N6 Cu1 N1 92.06(7) . . ? N3 Cu1 N2 93.96(7) . . ? N6 Cu1 N2 154.04(7) . . ? N1 Cu1 N2 80.56(6) . . ? N3 Cu1 N8 95.48(9) . 2_554 ? N6 Cu1 N8 94.64(7) . 2_554 ? N1 Cu1 N8 91.88(8) . 2_554 ? N2 Cu1 N8 110.34(7) . 2_554 ? C1 N1 C5 119.5(2) . . ? C1 N1 Cu1 124.76(14) . . ? C5 N1 Cu1 115.61(14) . . ? C10 N2 C6 119.4(2) . . ? C10 N2 Cu1 125.65(13) . . ? C6 N2 Cu1 114.89(11) . . ? C11 N3 Cu1 163.6(2) . . ? C11 N4 C12 123.2(2) . . ? C13 N6 Cu1 167.7(2) . . ? C13 N7 C14 124.5(2) . . ? C14 N8 Cu1 155.90(15) . 2 ? N1 C1 C2 122.0(2) . . ? N1 C1 H1 118.99 . . ? C2 C1 H1 119.02 . . ? C3 C2 C1 118.9(2) . . ? C3 C2 H2 120.55 . . ? C1 C2 H2 120.52 . . ? C2 C3 C4 119.3(2) . . ? C2 C3 H3 120.36 . . ? C4 C3 H3 120.38 . . ? C5 C4 C3 118.8(2) . . ? C5 C4 H4 120.47 . . ? C3 C4 H4 120.71 . . ? N1 C5 C4 121.5(2) . . ? N1 C5 C6 114.2(2) . . ? C4 C5 C6 124.3(2) . . ? N2 C6 C7 121.8(2) . . ? N2 C6 C5 114.64(14) . . ? C7 C6 C5 123.6(2) . . ? C6 C7 C8 118.2(2) . . ? C6 C7 H7 120.93 . . ? C8 C7 H7 120.85 . . ? C9 C8 C7 119.9(2) . . ? C9 C8 H8 120.02 . . ? C7 C8 H8 120.08 . . ? C8 C9 C10 119.2(2) . . ? C8 C9 H9 120.37 . . ? C10 C9 H9 120.44 . . ? N2 C10 C9 121.5(2) . . ? N2 C10 H10 119.21 . . ? C9 C10 H10 119.28 . . ? N3 C11 N4 173.2(2) . . ? N5 C12 N4 172.4(2) . . ? N6 C13 N7 172.6(2) . . ? N8 C14 N7 171.2(2) . . ? _refine_diff_density_max 0.319 _refine_diff_density_min -0.416 _refine_diff_density_rms 0.051 #===END data_cubpmdca _database_code_CSD 174340 _journal_coden_Cambridge 186 _manuscript_identification_number B105981P _publ_requested_journal 'Dalton Transactions' _publ_contact_author_name 'Prof Jorunn Sletten' _publ_contact_author_address ; Prof Jorunn Sletten Department of Chemistry University of Bergen Allegaten 41 N-5007 Bergen NORWAY ; _publ_contact_author_email 'JORUNN.SLETTEN@KJ.UIB.NO' # TITLE AND AUTHOR LIST _publ_section_title ; Syntheses, crystal structures and magnetic properties of copper(II) dicyanamide complexes; dinuclear, chain and ladder compounds ; loop_ _publ_author_name _publ_author_address 'Brita Vangdal' ;Department of Chemistry University of Bergen Allegaten 41 N-5007 Bergen Norway ; 'Jose Carranza' ;Department of Inorganic Chemistry Faculty of Chemistry University of Valencia Dr. Moliner 50 46100 Burjassot (Valencia) Spain ; 'Francesc Lloret' ;Department of Inorganic Chemistry Faculty of Chemistry University of Valencia Dr. Moliner 50 46100 Burjassot (Valencia) Spain ; 'Miguel Julve' ;Department of Inorganic Chemistry Faculty of Chemistry University of Valencia Dr. Moliner 50 46100 Burjassot (Valencia) Spain ; 'Jorunn Sletten' ;Department of Chemistry University of Bergen Allegaten 41 N-5007 Bergen Norway ; _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[Cu2 (C8 H6 N4) (C2 N3)4]n' _chemical_formula_analytical ? _chemical_formula_sum 'C16 H6 Cu2 N16' _chemical_formula_weight 549.45 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21 / c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.5550(2) _cell_length_b 11.3017(5) _cell_length_c 11.8904(4) _cell_angle_alpha 90.00 _cell_angle_beta 107.142(2) _cell_angle_gamma 90.00 _cell_volume 970.15(6) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour green _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.881 _exptl_crystal_density_method ? _exptl_crystal_F_000 544 _exptl_absorpt_coefficient_mu 2.239 _exptl_absorpt_correction_type 'empirical, SADABS' _exptl_absorpt_correction_T_min 'Tmin/Tmax ratio 0.822880' _exptl_absorpt_correction_T_max 'see above' _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 '2K SMART CCD' _diffrn_measurement_method \\w _diffrn_standards_number '50 first frames remeasured at end of data collection' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8482 _diffrn_reflns_av_R_equivalents 0.0200 _diffrn_reflns_av_sigmaI/netI 0.0206 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 30.48 _reflns_number_total 2938 _reflns_number_observed 2570 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART, version 5.051' _computing_cell_refinement 'SAINT, version 5.00' _computing_data_reduction 'SAINT, version 5.00' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'XP, version 4.3, 1992' _computing_publication_material 'CIFTAB, Sheldrick, 1993' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\\s^2^(Fo^2^)+(0.0286P)^2^+0.4227P] 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 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2937 _refine_ls_number_parameters 154 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0273 _refine_ls_R_factor_obs 0.0224 _refine_ls_wR_factor_all 0.0624 _refine_ls_wR_factor_obs 0.0608 _refine_ls_goodness_of_fit_all 1.086 _refine_ls_goodness_of_fit_obs 1.135 _refine_ls_restrained_S_all 1.086 _refine_ls_restrained_S_obs 1.135 _refine_ls_shift/esd_max 0.005 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cu1 Cu 0.32845(2) 0.04027(2) 0.261733(14) 0.01943(6) Uani 1 d . . N1 N 0.3357(2) -0.08593(11) 0.39188(10) 0.0198(2) Uani 1 d . . N2 N 0.4807(2) -0.11688(11) 0.59708(10) 0.0199(2) Uani 1 d . . N3 N 0.2803(2) 0.19143(13) 0.17628(12) 0.0307(3) Uani 1 d . . N4 N 0.1928(2) 0.35836(14) 0.04058(14) 0.0404(4) Uani 1 d . . N5 N -0.0184(2) 0.35921(14) -0.16225(13) 0.0373(3) Uani 1 d . . N6 N 0.1089(2) -0.03899(12) 0.15800(11) 0.0250(3) Uani 1 d . . N7 N -0.2272(2) -0.0616(2) 0.08972(13) 0.0387(4) Uani 1 d . . N8 N -0.4604(2) -0.02884(13) 0.19279(13) 0.0278(3) Uani 1 d . . C1 C 0.4491(2) -0.05579(12) 0.49662(12) 0.0188(2) Uani 1 d . . C2 C 0.2437(2) -0.18961(13) 0.38605(13) 0.0229(3) Uani 1 d . . H2 H 0.1631 -0.21568 0.31286 0.034 Uiso 1 calc R . C3 C 0.2664(2) -0.25815(14) 0.48618(13) 0.0249(3) Uani 1 d . . H3 H 0.2016 -0.33080 0.48241 0.037 Uiso 1 calc R . C4 C 0.3859(2) -0.21819(13) 0.59229(13) 0.0229(3) Uani 1 d . . H4 H 0.4006 -0.26309 0.66199 0.034 Uiso 1 calc R . C5 C 0.2338(2) 0.26558(14) 0.10802(13) 0.0238(3) Uani 1 d . . C6 C 0.0785(2) 0.35245(14) -0.06717(14) 0.0260(3) Uani 1 d . . C7 C -0.0506(2) -0.04748(13) 0.13245(12) 0.0211(3) Uani 1 d . . C8 C -0.3432(2) -0.04192(13) 0.15026(13) 0.0226(3) Uani 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 0.02126(9) 0.02042(10) 0.01582(9) 0.00066(6) 0.00426(6) -0.00106(6) N1 0.0215(5) 0.0199(6) 0.0174(5) 0.0002(4) 0.0048(4) -0.0011(4) N2 0.0224(5) 0.0185(5) 0.0184(5) 0.0020(4) 0.0055(4) -0.0001(4) N3 0.0373(7) 0.0287(7) 0.0218(6) 0.0023(5) 0.0018(5) -0.0021(6) N4 0.0491(9) 0.0277(7) 0.0314(7) 0.0078(6) -0.0082(6) -0.0104(7) N5 0.0458(8) 0.0347(8) 0.0267(7) 0.0054(6) 0.0036(6) -0.0048(6) N6 0.0239(6) 0.0311(7) 0.0194(6) -0.0025(5) 0.0056(4) -0.0012(5) N7 0.0228(6) 0.0671(11) 0.0265(7) -0.0136(7) 0.0078(5) -0.0023(7) N8 0.0223(6) 0.0317(7) 0.0299(7) -0.0047(5) 0.0085(5) -0.0023(5) C1 0.0204(6) 0.0183(6) 0.0178(6) -0.0001(5) 0.0058(5) 0.0000(5) C2 0.0250(6) 0.0219(7) 0.0213(6) -0.0032(5) 0.0060(5) -0.0042(5) C3 0.0291(7) 0.0195(7) 0.0268(7) -0.0012(5) 0.0092(5) -0.0054(5) C4 0.0277(7) 0.0197(7) 0.0222(6) 0.0023(5) 0.0086(5) -0.0009(5) C5 0.0229(6) 0.0261(7) 0.0207(6) -0.0013(5) 0.0040(5) -0.0036(5) C6 0.0286(7) 0.0224(7) 0.0268(7) 0.0039(6) 0.0081(6) -0.0044(5) C7 0.0250(6) 0.0225(7) 0.0166(6) -0.0008(5) 0.0073(5) 0.0015(5) C8 0.0206(6) 0.0237(7) 0.0211(6) 0.0000(5) 0.0024(5) -0.0012(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N3 1.9661(14) . ? Cu1 N6 1.9672(13) . ? Cu1 N2 2.0543(12) 3_656 ? Cu1 N1 2.0934(12) . ? Cu1 N8 2.1444(13) 1_655 ? N1 C1 1.331(2) . ? N1 C2 1.353(2) . ? N2 C1 1.339(2) . ? N2 C4 1.343(2) . ? N2 Cu1 2.0543(12) 3_656 ? N3 C5 1.147(2) . ? N4 C5 1.301(2) . ? N4 C6 1.319(2) . ? N5 C6 1.154(2) . ? N6 C7 1.157(2) . ? N7 C7 1.290(2) . ? N7 C8 1.307(2) . ? N8 C8 1.151(2) . ? N8 Cu1 2.1444(13) 1_455 ? C1 C1 1.467(3) 3_656 ? C2 C3 1.388(2) . ? C2 H2 0.95 . ? C3 C4 1.393(2) . ? C3 H3 0.95 . ? C4 H4 0.95 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Cu1 N6 94.49(6) . . ? N3 Cu1 N2 91.97(5) . 3_656 ? N6 Cu1 N2 164.46(5) . 3_656 ? N3 Cu1 N1 159.17(6) . . ? N6 Cu1 N1 89.24(5) . . ? N2 Cu1 N1 79.86(5) 3_656 . ? N3 Cu1 N8 99.44(6) . 1_655 ? N6 Cu1 N8 100.34(5) . 1_655 ? N2 Cu1 N8 92.51(5) 3_656 1_655 ? N1 Cu1 N8 100.04(5) . 1_655 ? C1 N1 C2 116.65(12) . . ? C1 N1 Cu1 112.75(9) . . ? C2 N1 Cu1 130.60(10) . . ? C1 N2 C4 116.69(12) . . ? C1 N2 Cu1 114.17(9) . 3_656 ? C4 N2 Cu1 129.14(10) . 3_656 ? C5 N3 Cu1 166.33(13) . . ? C5 N4 C6 121.78(15) . . ? C7 N6 Cu1 145.41(12) . . ? C7 N7 C8 123.07(14) . . ? C8 N8 Cu1 165.89(13) . 1_455 ? N1 C1 N2 126.81(12) . . ? N1 C1 C1 116.98(15) . 3_656 ? N2 C1 C1 116.21(15) . 3_656 ? N1 C2 C3 120.50(13) . . ? N1 C2 H2 119.75 . . ? C3 C2 H2 119.75 . . ? C2 C3 C4 118.62(13) . . ? C2 C3 H3 120.69 . . ? C4 C3 H3 120.69 . . ? N2 C4 C3 120.69(13) . . ? N2 C4 H4 119.66 . . ? C3 C4 H4 119.66 . . ? N3 C5 N4 173.0(2) . . ? N5 C6 N4 173.2(2) . . ? N6 C7 N7 172.0(2) . . ? N8 C8 N7 172.4(2) . . ? _refine_diff_density_max 0.526 _refine_diff_density_min -0.377 _refine_diff_density_rms 0.060 #===END