# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1462 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 Trans.' _publ_requested_coeditor_name ? _publ_contact_letter ; ? ; #==================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; The first copper(I) complex containing a cyanato ligand. Sythesis and structural characterization of [Cu(pyz)(mu!2$-NCO) complex (pyz = pyrazine). ; 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_gcu12c _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common '[Cu(pyrazine)(NCO)]n' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C5 H4 Cu N3 O' _chemical_formula_weight 185.65 _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 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 5.904(2) _cell_length_b 11.593(3) _cell_length_c 9.038(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 618.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 42 _cell_measurement_theta_min 5.4 _cell_measurement_theta_max 14.4 _exptl_crystal_description 'irregular shaped' _exptl_crystal_colour red _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 1.98(3) _exptl_crystal_density_diffrn 1.993 _exptl_crystal_density_method 'suspension method' _exptl_crystal_F_000 368 _exptl_absorpt_coefficient_mu 3.447 _exptl_absorpt_correction_type 'DIFABS' _exptl_absorpt_correction_T_min 0.469 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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: 1.25 deg.' _diffrn_standards_number '3 (2 1 0; -1 2 2; 1 2 1)' _diffrn_standards_interval_count 100 _diffrn_standards_interval_time '80 min' _diffrn_standards_decay_% 2 _diffrn_reflns_number 1410 _diffrn_reflns_av_R_equivalents 0.0308 _diffrn_reflns_av_sigmaI/netI 0.0278 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 1 _diffrn_reflns_theta_min 2.86 _diffrn_reflns_theta_max 24.97 _reflns_number_total 573 _reflns_number_observed 520 _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 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^)+(0.0314P)^2^+0.3063P] 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 SHELXL _refine_ls_extinction_coef 0.0291(24) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 573 _refine_ls_number_parameters 53 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0307 _refine_ls_R_factor_obs 0.0261 _refine_ls_wR_factor_all 0.0655 _refine_ls_wR_factor_obs 0.0617 _refine_ls_goodness_of_fit_all 1.095 _refine_ls_goodness_of_fit_obs 1.087 _refine_ls_restrained_S_all 1.095 _refine_ls_restrained_S_obs 1.087 _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 0.19250(8) 0.2500 0.66435(5) 0.0324(3) Uani 1 d S . N1 N 0.5449(6) 0.2500 0.6322(4) 0.0339(8) Uani 1 d S . C1 C 0.6037(7) 0.2500 0.5097(5) 0.0416(11) Uani 1 d S . O1 O 0.6616(7) 0.2500 0.3837(4) 0.094(2) Uani 1 d S . N2 N 0.0805(4) 0.3991(2) 0.5651(3) 0.0297(5) Uani 1 d . . C2 C -0.0295(5) 0.4786(3) 0.6420(3) 0.0321(6) Uani 1 d . . H2 H -0.0529(5) 0.4666(3) 0.7426(3) 0.039 Uiso 1 calc R . C3 C -0.1103(5) 0.5780(3) 0.5786(3) 0.0345(7) Uani 1 d . . H3 H -0.1877(5) 0.6308(3) 0.6371(3) 0.041 Uiso 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 0.0398(4) 0.0259(3) 0.0314(4) 0.000 0.0017(2) 0.000 N1 0.029(2) 0.045(2) 0.027(2) 0.000 -0.0032(14) 0.000 C1 0.030(2) 0.061(3) 0.034(3) 0.000 -0.007(2) 0.000 O1 0.083(3) 0.169(6) 0.029(2) 0.000 0.006(2) 0.000 N2 0.0316(12) 0.0278(12) 0.0296(12) 0.0047(11) -0.0020(10) 0.0020(10) C2 0.0355(15) 0.0351(15) 0.0258(14) 0.0036(13) 0.0041(11) 0.0014(13) C3 0.041(2) 0.034(2) 0.0286(15) 0.0012(13) 0.0056(12) 0.0050(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 Cu1 6.899(2) 5_655 yes Cu1 Cu1 3.333(1) 6_657 yes Cu1 Cu1 3.333(1) 6_557 ? Cu1 N1 2.035(3) 6_557 yes Cu1 N2 2.056(2) 7_565 yes Cu1 N2 2.056(2) . yes Cu1 N1 2.101(3) . yes N1 C1 1.160(5) . yes N1 Cu1 2.035(3) 6_657 yes C1 O1 1.189(6) . yes N2 C2 1.325(4) . yes N2 C3 1.337(4) 5_566 yes C2 C3 1.373(4) . yes C2 H2 0.93 . ? C3 N2 1.337(4) 5_566 ? C3 H3 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 N1 Cu1 N2 104.87(8) 6_557 7_565 yes N1 Cu1 N2 104.87(8) 6_557 . yes N2 Cu1 N2 114.37(13) 7_565 . yes N1 Cu1 N1 123.31(11) 6_557 . yes N2 Cu1 N1 104.95(8) 7_565 . yes N2 Cu1 N1 104.95(8) . . yes C1 N1 Cu1 137.2(3) . 6_657 ? C1 N1 Cu1 115.4(3) . . ? Cu1 N1 Cu1 107.39(15) 6_657 . yes N1 C1 O1 179.3(5) . . yes C2 N2 C3 115.8(2) . 5_566 ? C2 N2 Cu1 120.9(2) . . ? C3 N2 Cu1 123.3(2) 5_566 . ? N2 C2 C3 122.4(3) . . ? N2 C2 H2 118.8(2) . . ? C3 C2 H2 118.8(2) . . ? N2 C3 C2 121.8(3) 5_566 . ? N2 C3 H3 119.1(2) 5_566 . ? C2 C3 H3 119.1(2) . . ? Cu1 Cu1 Cu1 124.65(4) 6_657 6_557 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Cu1 N1 C1 180.0 6_557 . . . ? N2 Cu1 N1 C1 60.44(7) 7_565 . . . ? N2 Cu1 N1 C1 -60.44(7) . . . . ? N1 Cu1 N1 Cu1 0.0 6_557 . . 6_657 ? N2 Cu1 N1 Cu1 -119.56(7) 7_565 . . 6_657 ? N2 Cu1 N1 Cu1 119.56(7) . . . 6_657 ? Cu1 N1 C1 O1 180.00(7) 6_657 . . . ? Cu1 N1 C1 O1 0.00(7) . . . . ? N1 Cu1 N2 C2 10.3(2) 6_557 . . . ? N2 Cu1 N2 C2 124.6(2) 7_565 . . . ? N1 Cu1 N2 C2 -120.9(2) . . . . ? N1 Cu1 N2 C3 -169.0(2) 6_557 . . 5_566 ? N2 Cu1 N2 C3 -54.6(3) 7_565 . . 5_566 ? N1 Cu1 N2 C3 59.8(3) . . . 5_566 ? C3 N2 C2 C3 0.6(5) 5_566 . . . ? Cu1 N2 C2 C3 -178.7(2) . . . . ? N2 C2 C3 N2 -0.6(5) . . . 5_566 ? _refine_diff_density_max 0.270 _refine_diff_density_min -0.386 _refine_diff_density_rms 0.065 #======================================================END