# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1396 data_global # 1. SUBMISSION DETAILS _publ_contact_author ; Franz A. Mautner Institut f\"ur Physikalische und Theoretische Chemie Technische Universit\"at Graz Rechbauerstr. 12 A-8010 Graz Austria ; _publ_contact_author_phone '++43 316 873 8234' _publ_contact_author_fax '++43 316 873 8225' _publ_contact_author_email 'mautner@ptc.tu-graz.ac.at' _publ_requested_journal 'J. Chem. Soc., Dalton Comm.' _publ_requested_coeditor_name ? _publ_contact_letter ; ? ; #==================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; A novel 2D polymeric Cu(I) complex with unusual azide bridge. Synthesis and crystal structure of [Cu(pyza)M-1',1',3-N3]n (n = infinity, pyza = pyrazineamide). ; loop_ _publ_author_name _publ_author_address 'Goher, Mohamed A. S.' ; Department of Chemistry, Faculty of Science, Kuwait University, P.O.Box 5969 Safat 13060 Kuwait FAX: 00965 4816482 ; 'Mautner, Franz A.' ; Institut f\"ur Physikalische und Theoretische Chemie, Technische Universit\"at Graz Rechbauerstr. 12 A-8010 Graz Austria ; #=================================================================== data_gcu2b6 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common '[Cu(pyrazineamide)(N3)]n' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C5 H5 Cu N6 O' _chemical_formula_weight 228.69 _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' 'O' 'O' 0.0106 0.0060 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 5.528(2) _cell_length_b 5.442(2) _cell_length_c 25.999(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.59(3) _cell_angle_gamma 90.00 _cell_volume 782.1(5) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 69 _cell_measurement_theta_min 5.2 _cell_measurement_theta_max 15.0 _exptl_crystal_description 'irregular shaped' _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 1.93(3) _exptl_crystal_density_diffrn 1.942 _exptl_crystal_density_method 'suspension method' _exptl_crystal_F_000 456 _exptl_absorpt_coefficient_mu 2.757 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_correction_T_min 0.126 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'mod. STOE 4-circle-diffractometer' _diffrn_measurement_method 'Omega-Scan, delta Omega: 2.00 deg.' _diffrn_standards_number '2 (1 0 -3, 1 1 5)' _diffrn_standards_interval_count 100 _diffrn_standards_interval_time '80 min' _diffrn_standards_decay_% 2 _diffrn_reflns_number 1973 _diffrn_reflns_av_R_equivalents 0.0242 _diffrn_reflns_av_sigmaI/netI 0.0305 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -2 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 26.00 _reflns_number_total 1543 _reflns_number_observed 1296 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL/PC v.5.03 (Siemens Ind. Aut.)' _computing_publication_material 'SHELXTL/PC v.5.03 (Siemens Ind. Aut.)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 15 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^)+(0.0615P)^2^+0.8259P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1528 _refine_ls_number_parameters 125 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0531 _refine_ls_R_factor_obs 0.0427 _refine_ls_wR_factor_all 0.1172 _refine_ls_wR_factor_obs 0.1061 _refine_ls_goodness_of_fit_all 1.066 _refine_ls_goodness_of_fit_obs 1.092 _refine_ls_restrained_S_all 1.097 _refine_ls_restrained_S_obs 1.092 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cu1 Cu 0.64940(8) 0.68300(10) 0.21383(2) 0.0382(2) Uani 1 d . . N4 N 0.5725(6) 0.4131(7) 0.26891(13) 0.0376(8) Uani 1 d . . N5 N 0.3677(5) 0.3768(6) 0.28183(12) 0.0295(7) Uani 1 d . . N6 N 0.1713(6) 0.3503(7) 0.2959(2) 0.0471(9) Uani 1 d . . N1 N 0.8805(6) 0.1543(6) 0.07117(13) 0.0382(8) Uani 1 d . . C1 C 1.0023(7) 0.3628(7) 0.08092(14) 0.0308(8) Uani 1 d . . C2 C 0.9423(7) 0.5199(7) 0.12061(14) 0.0336(8) Uani 1 d . . H1 H 1.0329(7) 0.6619(7) 0.12584(14) 0.040 Uiso 1 calc R . N2 N 0.7545(6) 0.4711(6) 0.15198(12) 0.0335(7) Uani 1 d . . C3 C 0.6341(8) 0.2618(7) 0.1427(2) 0.0369(9) Uani 1 d . . H2 H 0.5059(8) 0.2190(7) 0.1638(2) 0.044 Uiso 1 calc R . C4 C 0.6958(8) 0.1068(8) 0.1023(2) 0.0399(9) Uani 1 d . . H3 H 0.6050(8) -0.0349(8) 0.0968(2) 0.048 Uiso 1 calc R . C5 C 1.2155(7) 0.4257(8) 0.04722(14) 0.0344(8) Uani 1 d . . O1 O 1.3247(6) 0.6213(6) 0.05382(12) 0.0503(8) Uani 1 d . . N3 N 1.2707(7) 0.2637(8) 0.0114(2) 0.0498(10) Uani 1 d D . H4 H 1.3982(68) 0.2896(101) -0.0084(19) 0.066(12) Uiso 1 d D . H5 H 1.2073(91) 0.1155(52) 0.0129(22) 0.066(12) Uiso 1 d 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 0.0354(3) 0.0382(3) 0.0410(3) -0.0027(2) 0.0034(2) -0.0041(2) N4 0.032(2) 0.036(2) 0.045(2) 0.010(2) -0.0013(14) 0.0029(15) N5 0.036(2) 0.0219(15) 0.030(2) -0.0007(13) -0.0054(13) 0.0042(13) N6 0.034(2) 0.047(2) 0.060(2) -0.006(2) 0.005(2) -0.004(2) N1 0.047(2) 0.032(2) 0.036(2) -0.0079(15) -0.0018(15) -0.0024(15) C1 0.035(2) 0.030(2) 0.026(2) -0.0025(15) -0.0037(14) -0.001(2) C2 0.041(2) 0.031(2) 0.029(2) -0.005(2) -0.0013(15) -0.006(2) N2 0.040(2) 0.031(2) 0.030(2) -0.0034(14) 0.0001(13) -0.0048(14) C3 0.047(2) 0.028(2) 0.036(2) 0.004(2) 0.000(2) -0.008(2) C4 0.049(2) 0.028(2) 0.042(2) 0.000(2) -0.004(2) -0.011(2) C5 0.040(2) 0.036(2) 0.027(2) -0.005(2) -0.0026(15) -0.003(2) O1 0.056(2) 0.046(2) 0.048(2) -0.0176(15) 0.0163(15) -0.017(2) N3 0.050(2) 0.053(2) 0.046(2) -0.020(2) 0.012(2) -0.013(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N6 2.007(4) 2 ? Cu1 N4 2.030(3) 2_655 ? Cu1 N2 2.067(3) . ? Cu1 N4 2.098(3) . ? N4 N5 1.200(4) . ? N4 Cu1 2.030(3) 2_645 ? N5 N6 1.158(4) . ? N6 Cu1 2.007(4) 2_545 ? N1 C4 1.334(5) . ? N1 C1 1.343(5) . ? C1 C2 1.383(5) . ? C1 C5 1.515(5) . ? C2 N2 1.353(5) . ? C2 H1 0.93 . ? N2 C3 1.340(5) . ? C3 C4 1.392(6) . ? C3 H2 0.93 . ? C4 H3 0.93 . ? C5 O1 1.235(5) . ? C5 N3 1.320(5) . ? N3 H4 0.89(2) . ? N3 H5 0.88(2) . ? Cu1 Cu1 3.484(1) 2_655 ? Cu1 Cu1 3.484(1) 2 ? Cu1 Cu1 5.533(2) 2_545 ? N3 O1 2.890(5) 3_865 ? H4 O1 2.00(2) 3_865 ? 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 N6 Cu1 N4 114.5(2) 2 2_655 ? N6 Cu1 N2 114.2(2) 2 . ? N4 Cu1 N2 107.33(13) 2_655 . ? N6 Cu1 N4 102.63(14) 2 . ? N4 Cu1 N4 116.07(7) 2_655 . ? N2 Cu1 N4 101.60(14) . . ? N5 N4 Cu1 123.4(3) . 2_645 ? N5 N4 Cu1 120.3(3) . . ? Cu1 N4 Cu1 115.12(15) 2_645 . ? N6 N5 N4 176.9(4) . . ? N5 N6 Cu1 147.8(3) . 2_545 ? C4 N1 C1 115.8(3) . . ? N1 C1 C2 122.7(3) . . ? N1 C1 C5 118.3(3) . . ? C2 C1 C5 119.1(3) . . ? N2 C2 C1 121.3(3) . . ? N2 C2 H1 119.3(2) . . ? C1 C2 H1 119.3(2) . . ? C3 N2 C2 116.2(3) . . ? C3 N2 Cu1 118.1(3) . . ? C2 N2 Cu1 125.7(3) . . ? N2 C3 C4 121.7(4) . . ? N2 C3 H2 119.1(2) . . ? C4 C3 H2 119.1(2) . . ? N1 C4 C3 122.3(4) . . ? N1 C4 H3 118.8(2) . . ? C3 C4 H3 118.8(2) . . ? O1 C5 N3 123.9(4) . . ? O1 C5 C1 119.7(3) . . ? N3 C5 C1 116.4(4) . . ? C5 N3 H4 119.6(38) . . ? C5 N3 H5 119.0(36) . . ? H4 N3 H5 119.3(51) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N6 Cu1 N4 N5 7.7(4) 2 . . . ? N4 Cu1 N4 N5 133.3(3) 2_655 . . . ? N2 Cu1 N4 N5 -110.6(3) . . . . ? N6 Cu1 N4 Cu1 175.9(2) 2 . . 2_645 ? N4 Cu1 N4 Cu1 -58.5(2) 2_655 . . 2_645 ? N2 Cu1 N4 Cu1 57.5(2) . . . 2_645 ? Cu1 N4 N5 N6 107.5(75) 2_645 . . . ? Cu1 N4 N5 N6 -85.3(75) . . . . ? N4 N5 N6 Cu1 172.7(71) . . . 2_545 ? C4 N1 C1 C2 0.1(6) . . . . ? C4 N1 C1 C5 179.4(4) . . . . ? N1 C1 C2 N2 -0.2(6) . . . . ? C5 C1 C2 N2 -179.6(3) . . . . ? C1 C2 N2 C3 0.9(6) . . . . ? C1 C2 N2 Cu1 178.3(3) . . . . ? N6 Cu1 N2 C3 -70.6(3) 2 . . . ? N4 Cu1 N2 C3 161.4(3) 2_655 . . . ? N4 Cu1 N2 C3 39.1(3) . . . . ? N6 Cu1 N2 C2 112.0(3) 2 . . . ? N4 Cu1 N2 C2 -16.0(4) 2_655 . . . ? N4 Cu1 N2 C2 -138.3(3) . . . . ? C2 N2 C3 C4 -1.4(6) . . . . ? Cu1 N2 C3 C4 -179.0(3) . . . . ? C1 N1 C4 C3 -0.6(6) . . . . ? N2 C3 C4 N1 1.4(7) . . . . ? N1 C1 C5 O1 176.9(4) . . . . ? C2 C1 C5 O1 -3.7(6) . . . . ? N1 C1 C5 N3 -2.2(6) . . . . ? C2 C1 C5 N3 177.2(4) . . . . ? _refine_diff_density_max 0.515 _refine_diff_density_min -0.723 _refine_diff_density_rms 0.092