data_global _journal_name_full Chem.Commun. #==================================================================== # 1. SUBMISSION DETAILS _journal_coden_Cambridge 0182 _publ_contact_author_name 'Prof Xiao-Ming Chen' _publ_contact_author_address ; Chen, Xiao-Ming School of Chemistry and Chemical Engineering Sun Yat-Sen University Guangzhou, 510275 P. R. China ; _publ_contact_author_phone 86-20-84113986 _publ_contact_author_fax '86 20 84112245' _publ_contact_author_email cescxm@zsu.edu.cn _publ_requested_coeditor_name ? _publ_contact_letter ; Dear Sir or Madam: Please consider this CIF as a supplmentary data for a paper submitted to Chem. commun. (CCDC 238972 & 262126) Thanks. Xiao-Ming Chen ; _publ_section_title ; Luminescent zigzag chains and triple-stranded helices of copper(I) 2-ethylimidazolate: Solvent polarity-induced supramolecular isomerism ; loop_ _publ_author_name _publ_author_address 'Xiao-Chun Huang' ; School of Chemistry and Chemical Engineering Sun Yat-Sen University Guangzhou 510275 P. R. China ; 'Jie-Peng Zhang' ; School of Chemistry and Chemical Engineering Sun Yat-Sen University Guangzhou 510275 P. R. China ; 'Yan-Yong Lin' ; School of Chemistry and Chemical Engineering Sun Yat-Sen University Guangzhou 510275 P. R. China ; 'Xiao-Ming Chen' ; School of Chemistry and Chemical Engineering Sun Yat-Sen University Guangzhou 510275 P. R. China ; #====================================== data_compoud_1 _database_code_depnum_ccdc_archive 'CCDC 238972' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C5 H7 Cu N2' _chemical_formula_weight 158.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.6065(13) _cell_length_b 11.0944(5) _cell_length_c 17.0945(9) _cell_angle_alpha 90.00 _cell_angle_beta 106.9610(10) _cell_angle_gamma 90.00 _cell_volume 4826.5(4) _cell_formula_units_Z 32 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.747 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2560 _exptl_absorpt_coefficient_mu 3.501 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.4630 _exptl_absorpt_correction_T_max 0.5714 _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 'Bruker Apex CCD' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14503 _diffrn_reflns_av_R_equivalents 0.0254 _diffrn_reflns_av_sigmaI/netI 0.0341 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 27.98 _reflns_number_total 5616 _reflns_number_gt 4974 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, 1998.' _computing_cell_refinement 'SAINT-PLUS, Ver. 6.0, 1997' _computing_data_reduction 'SAINT-PLUS, Ver. 6.0, 1997' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP, Ver. 6.10, Bruker AXS Inc., 2000.' _computing_publication_material 'SHELXTL-Bruker AXS Inc., 1998.' _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^)+(0.0311P)^2^+4.7616P] 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 5616 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0387 _refine_ls_R_factor_gt 0.0326 _refine_ls_wR_factor_ref 0.0720 _refine_ls_wR_factor_gt 0.0694 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _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 0.444342(12) 0.44053(3) 0.226633(19) 0.01591(8) Uani 1 1 d . . . Cu2 Cu 0.421413(13) 0.89425(3) 0.056533(19) 0.01611(8) Uani 1 1 d . . . Cu3 Cu 0.340734(12) 1.36539(3) 0.076031(19) 0.01734(8) Uani 1 1 d . . . Cu4 Cu 0.156200(13) 1.61434(3) 0.11334(2) 0.02009(9) Uani 1 1 d . . . N1 N 0.39956(8) 0.18553(18) 0.35961(12) 0.0161(4) Uani 1 1 d . . . N2 N 0.43897(8) 0.31914(18) 0.29949(12) 0.0152(4) Uani 1 1 d . . . N3 N 0.44509(8) 0.55809(18) 0.14910(12) 0.0159(4) Uani 1 1 d . . . N4 N 0.43374(8) 0.73194(18) 0.08070(12) 0.0156(4) Uani 1 1 d . . . N5 N 0.41230(8) 1.05984(18) 0.04244(12) 0.0156(4) Uani 1 1 d . . . N6 N 0.38374(8) 1.24509(18) 0.05547(12) 0.0157(4) Uani 1 1 d . . . N7 N 0.29204(8) 1.47985(19) 0.08562(13) 0.0169(4) Uani 1 1 d . . . N8 N 0.22046(9) 1.5708(2) 0.09959(13) 0.0207(5) Uani 1 1 d . . . C1 C 0.44976(11) 0.1464(2) 0.36742(15) 0.0191(5) Uani 1 1 d . . . H1 H 0.4650 0.0743 0.3940 0.023 Uiso 1 1 calc R . . C2 C 0.47400(10) 0.2269(2) 0.33129(15) 0.0181(5) Uani 1 1 d . . . H2 H 0.5090 0.2211 0.3282 0.022 Uiso 1 1 calc R . . C3 C 0.39523(10) 0.2907(2) 0.31908(14) 0.0152(5) Uani 1 1 d . . . C4 C 0.34762(11) 0.3692(2) 0.30077(17) 0.0233(6) Uani 1 1 d . . . H4A H 0.3167 0.3190 0.2999 0.028 Uiso 1 1 calc R . . H4B H 0.3415 0.4047 0.2456 0.028 Uiso 1 1 calc R . . C5 C 0.35220(15) 0.4696(3) 0.3619(2) 0.0517(11) Uani 1 1 d . . . H5A H 0.3199 0.5179 0.3468 0.078 Uiso 1 1 calc R . . H5B H 0.3822 0.5210 0.3622 0.078 Uiso 1 1 calc R . . H5C H 0.3574 0.4352 0.4165 0.078 Uiso 1 1 calc R . . C6 C 0.46615(10) 0.5472(2) 0.08454(15) 0.0179(5) Uani 1 1 d . . . H6 H 0.4828 0.4773 0.0716 0.021 Uiso 1 1 calc R . . C7 C 0.45916(10) 0.6526(2) 0.04284(15) 0.0170(5) Uani 1 1 d . . . H7 H 0.4699 0.6692 -0.0044 0.020 Uiso 1 1 calc R . . C8 C 0.42628(9) 0.6715(2) 0.14423(15) 0.0146(5) Uani 1 1 d . . . C9 C 0.40014(11) 0.7232(2) 0.20300(16) 0.0207(6) Uani 1 1 d . . . H9A H 0.3816 0.6578 0.2227 0.025 Uiso 1 1 calc R . . H9B H 0.3734 0.7825 0.1738 0.025 Uiso 1 1 calc R . . C10 C 0.43768(13) 0.7845(3) 0.27601(19) 0.0420(9) Uani 1 1 d . . . H10A H 0.4180 0.8162 0.3119 0.063 Uiso 1 1 calc R . . H10B H 0.4555 0.8508 0.2572 0.063 Uiso 1 1 calc R . . H10C H 0.4638 0.7260 0.3062 0.063 Uiso 1 1 calc R . . C11 C 0.42650(10) 1.1342(2) -0.01209(15) 0.0171(5) Uani 1 1 d . . . H11 H 0.4454 1.1104 -0.0489 0.021 Uiso 1 1 calc R . . C12 C 0.40909(10) 1.2468(2) -0.00441(15) 0.0172(5) Uani 1 1 d . . . H12 H 0.4135 1.3154 -0.0350 0.021 Uiso 1 1 calc R . . C13 C 0.38671(10) 1.1309(2) 0.08182(15) 0.0157(5) Uani 1 1 d . . . C14 C 0.36331(11) 1.0877(2) 0.14613(15) 0.0204(6) Uani 1 1 d . . . H14A H 0.3607 1.1563 0.1818 0.024 Uiso 1 1 calc R . . H14B H 0.3870 1.0270 0.1805 0.024 Uiso 1 1 calc R . . C15 C 0.30911(12) 1.0321(3) 0.11142(18) 0.0321(7) Uani 1 1 d . . . H15A H 0.2958 1.0056 0.1564 0.048 Uiso 1 1 calc R . . H15B H 0.3114 0.9628 0.0771 0.048 Uiso 1 1 calc R . . H15C H 0.2851 1.0922 0.0784 0.048 Uiso 1 1 calc R . . C16 C 0.29502(11) 1.6007(2) 0.06869(17) 0.0218(6) Uani 1 1 d . . . H16 H 0.3226 1.6387 0.0531 0.026 Uiso 1 1 calc R . . C17 C 0.25170(11) 1.6560(2) 0.07807(17) 0.0241(6) Uani 1 1 d . . . H17 H 0.2441 1.7396 0.0710 0.029 Uiso 1 1 calc R . . C18 C 0.24621(10) 1.4658(2) 0.10339(15) 0.0170(5) Uani 1 1 d . . . C19 C 0.22639(11) 1.3463(2) 0.12200(17) 0.0232(6) Uani 1 1 d . . . H19A H 0.2558 1.2881 0.1345 0.028 Uiso 1 1 calc R . . H19B H 0.1995 1.3172 0.0725 0.028 Uiso 1 1 calc R . . C20 C 0.20271(12) 1.3475(3) 0.19272(19) 0.0305(7) Uani 1 1 d . . . H20A H 0.1907 1.2662 0.2009 0.046 Uiso 1 1 calc R . . H20B H 0.1728 1.4031 0.1804 0.046 Uiso 1 1 calc R . . H20C H 0.2293 1.3739 0.2426 0.046 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 0.01784(17) 0.01278(15) 0.01854(16) 0.00504(12) 0.00756(12) 0.00037(12) Cu2 0.02181(18) 0.01031(15) 0.01644(16) 0.00230(12) 0.00595(13) 0.00309(12) Cu3 0.01641(17) 0.01548(16) 0.02084(17) -0.00137(12) 0.00652(13) 0.00437(12) Cu4 0.01806(18) 0.02331(18) 0.02050(17) -0.00196(13) 0.00814(13) 0.00785(13) N1 0.0183(11) 0.0171(10) 0.0137(10) 0.0001(8) 0.0058(8) -0.0057(9) N2 0.0167(11) 0.0141(10) 0.0157(10) 0.0015(8) 0.0062(8) -0.0024(8) N3 0.0173(11) 0.0138(10) 0.0167(11) 0.0010(8) 0.0054(8) 0.0009(8) N4 0.0187(11) 0.0133(10) 0.0145(10) 0.0015(8) 0.0042(8) 0.0029(8) N5 0.0195(11) 0.0128(10) 0.0140(10) 0.0005(8) 0.0042(8) 0.0021(8) N6 0.0163(11) 0.0141(10) 0.0167(10) -0.0020(8) 0.0047(8) 0.0022(8) N7 0.0140(11) 0.0172(11) 0.0192(11) -0.0009(9) 0.0047(9) 0.0030(8) N8 0.0183(12) 0.0220(12) 0.0230(12) -0.0030(9) 0.0077(9) 0.0049(9) C1 0.0231(14) 0.0169(12) 0.0167(12) 0.0032(10) 0.0050(11) 0.0015(10) C2 0.0146(13) 0.0202(13) 0.0204(13) 0.0011(10) 0.0068(10) 0.0008(10) C3 0.0151(13) 0.0207(13) 0.0087(11) -0.0009(9) 0.0018(9) -0.0034(10) C4 0.0162(14) 0.0280(15) 0.0251(14) 0.0052(12) 0.0052(11) -0.0004(11) C5 0.050(2) 0.056(2) 0.045(2) -0.0100(18) 0.0073(18) 0.0311(19) C6 0.0239(14) 0.0123(12) 0.0190(13) -0.0006(10) 0.0088(11) 0.0021(10) C7 0.0219(14) 0.0171(12) 0.0134(12) 0.0009(10) 0.0073(10) 0.0017(10) C8 0.0112(12) 0.0155(12) 0.0166(12) 0.0025(10) 0.0032(9) 0.0006(9) C9 0.0217(14) 0.0211(13) 0.0230(14) 0.0040(11) 0.0126(11) 0.0039(11) C10 0.0296(18) 0.069(2) 0.0249(16) -0.0172(16) 0.0046(13) 0.0129(17) C11 0.0200(14) 0.0152(12) 0.0183(12) 0.0003(10) 0.0090(10) 0.0026(10) C12 0.0198(14) 0.0136(12) 0.0186(12) 0.0028(10) 0.0062(10) 0.0007(10) C13 0.0166(13) 0.0162(12) 0.0125(11) -0.0009(10) 0.0015(10) -0.0011(10) C14 0.0266(15) 0.0203(13) 0.0152(12) 0.0003(10) 0.0077(11) -0.0003(11) C15 0.0327(18) 0.0416(18) 0.0255(15) 0.0007(13) 0.0139(13) -0.0114(14) C16 0.0186(14) 0.0207(13) 0.0266(14) 0.0003(11) 0.0077(11) 0.0005(10) C17 0.0256(15) 0.0178(13) 0.0301(15) -0.0018(11) 0.0098(12) 0.0031(11) C18 0.0161(13) 0.0196(13) 0.0152(12) -0.0038(10) 0.0044(10) 0.0018(10) C19 0.0226(15) 0.0214(14) 0.0257(14) -0.0014(11) 0.0072(11) -0.0008(11) C20 0.0235(16) 0.0355(17) 0.0359(17) 0.0067(14) 0.0139(13) 0.0033(13) _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 1.864(2) . ? Cu1 N2 1.868(2) . ? Cu1 Cu1 2.8337(6) 2_655 ? Cu2 N4 1.855(2) . ? Cu2 N5 1.860(2) . ? Cu2 Cu4 3.0343(5) 7_575 ? Cu3 N7 1.855(2) . ? Cu3 N6 1.857(2) . ? Cu4 N1 1.854(2) 4_565 ? Cu4 N8 1.856(2) . ? Cu4 Cu2 3.0343(5) 7_575 ? N1 C3 1.344(3) . ? N1 C1 1.373(3) . ? N1 Cu4 1.854(2) 4_535 ? N2 C3 1.339(3) . ? N2 C2 1.384(3) . ? N3 C8 1.347(3) . ? N3 C6 1.381(3) . ? N4 C8 1.340(3) . ? N4 C7 1.381(3) . ? N5 C13 1.344(3) . ? N5 C11 1.378(3) . ? N6 C13 1.339(3) . ? N6 C12 1.380(3) . ? N7 C18 1.349(3) . ? N7 C16 1.379(3) . ? N8 C18 1.344(3) . ? N8 C17 1.377(4) . ? C1 C2 1.352(4) . ? C3 C4 1.494(4) . ? C4 C5 1.508(4) . ? C6 C7 1.354(3) . ? C8 C9 1.494(3) . ? C9 C10 1.513(4) . ? C11 C12 1.352(3) . ? C13 C14 1.492(4) . ? C14 C15 1.520(4) . ? C16 C17 1.355(4) . ? C18 C19 1.495(4) . ? C19 C20 1.518(4) . ? 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 N2 175.93(9) . . ? N3 Cu1 Cu1 88.47(7) . 2_655 ? N2 Cu1 Cu1 95.10(7) . 2_655 ? N4 Cu2 N5 174.68(9) . . ? N4 Cu2 Cu4 102.09(6) . 7_575 ? N5 Cu2 Cu4 83.13(6) . 7_575 ? N7 Cu3 N6 173.40(9) . . ? N1 Cu4 N8 167.35(10) 4_565 . ? N1 Cu4 Cu2 83.19(6) 4_565 7_575 ? N8 Cu4 Cu2 105.40(7) . 7_575 ? C3 N1 C1 105.0(2) . . ? C3 N1 Cu4 122.92(18) . 4_535 ? C1 N1 Cu4 131.86(17) . 4_535 ? C3 N2 C2 105.2(2) . . ? C3 N2 Cu1 125.30(17) . . ? C2 N2 Cu1 128.41(18) . . ? C8 N3 C6 105.2(2) . . ? C8 N3 Cu1 128.06(18) . . ? C6 N3 Cu1 126.72(17) . . ? C8 N4 C7 105.6(2) . . ? C8 N4 Cu2 127.46(18) . . ? C7 N4 Cu2 126.39(17) . . ? C13 N5 C11 105.5(2) . . ? C13 N5 Cu2 125.50(18) . . ? C11 N5 Cu2 128.91(18) . . ? C13 N6 C12 105.6(2) . . ? C13 N6 Cu3 126.55(18) . . ? C12 N6 Cu3 126.26(17) . . ? C18 N7 C16 105.7(2) . . ? C18 N7 Cu3 129.89(18) . . ? C16 N7 Cu3 124.24(18) . . ? C18 N8 C17 105.6(2) . . ? C18 N8 Cu4 134.01(19) . . ? C17 N8 Cu4 120.36(18) . . ? C2 C1 N1 109.1(2) . . ? C1 C2 N2 108.2(2) . . ? N2 C3 N1 112.5(2) . . ? N2 C3 C4 123.7(2) . . ? N1 C3 C4 123.7(2) . . ? C3 C4 C5 113.2(2) . . ? C7 C6 N3 108.6(2) . . ? C6 C7 N4 108.3(2) . . ? N4 C8 N3 112.2(2) . . ? N4 C8 C9 124.1(2) . . ? N3 C8 C9 123.7(2) . . ? C8 C9 C10 113.7(2) . . ? C12 C11 N5 108.6(2) . . ? C11 C12 N6 108.3(2) . . ? N6 C13 N5 112.0(2) . . ? N6 C13 C14 123.7(2) . . ? N5 C13 C14 124.2(2) . . ? C13 C14 C15 113.3(2) . . ? C17 C16 N7 108.2(2) . . ? C16 C17 N8 108.8(2) . . ? N8 C18 N7 111.8(2) . . ? N8 C18 C19 124.9(2) . . ? N7 C18 C19 123.3(2) . . ? C18 C19 C20 114.6(2) . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 27.98 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 0.524 _refine_diff_density_min -0.375 _refine_diff_density_rms 0.092 #===============================END data_compound_2 _database_code_depnum_ccdc_archive 'CCDC 262126' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C5 H7 Cu N2' _chemical_formula_weight 158.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.5680(18) _cell_length_b 11.4672(11) _cell_length_c 13.5953(13) _cell_angle_alpha 90.00 _cell_angle_beta 126.6890(10) _cell_angle_gamma 90.00 _cell_volume 2446.3(4) _cell_formula_units_Z 16 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.723 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 3.454 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.5450 _exptl_absorpt_correction_T_max 0.7239 _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 'Bruker Apex CCD' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8050 _diffrn_reflns_av_R_equivalents 0.0216 _diffrn_reflns_av_sigmaI/netI 0.0297 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 27.99 _reflns_number_total 2881 _reflns_number_gt 2394 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, 1998.' _computing_cell_refinement 'SAINT-PLUS Ver. 6.0, 1997.' _computing_data_reduction 'SAINT-PLUS Ver. 6.0, 1997.' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP-Interactive Molecular Graphics, Ver. 6.10, Bruker AXS Inc., 2000.' _computing_publication_material 'SHELXTL-Bruker AXS Inc., 1998.' _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^)+(0.0495P)^2^+1.0844P] 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 2881 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0405 _refine_ls_R_factor_gt 0.0342 _refine_ls_wR_factor_ref 0.0887 _refine_ls_wR_factor_gt 0.0836 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 0.116063(16) -0.38968(2) 0.39678(2) 0.02250(11) Uani 1 1 d . . . Cu2 Cu 0.111038(15) 0.11056(2) 0.38875(2) 0.02070(10) Uani 1 1 d . . . N1 N 0.13130(10) -0.23759(14) 0.36890(15) 0.0209(3) Uani 1 1 d . . . N2 N 0.13010(10) -0.04337(14) 0.36760(15) 0.0213(3) Uani 1 1 d . . . N3 N 0.10175(10) 0.26237(14) 0.42404(15) 0.0205(3) Uani 1 1 d . . . N4 N 0.10437(10) 0.45657(14) 0.42972(16) 0.0226(4) Uani 1 1 d . . . C1 C 0.10225(13) -0.14063(18) 0.38737(18) 0.0189(4) Uani 1 1 d . . . C2 C 0.18149(12) -0.19868(18) 0.33467(18) 0.0237(4) Uani 1 1 d . . . H2A H 0.2112 -0.2469 0.3149 0.028 Uiso 1 1 calc R . . C3 C 0.18102(12) -0.08033(18) 0.33418(18) 0.0223(4) Uani 1 1 d . . . H3A H 0.2104 -0.0314 0.3144 0.027 Uiso 1 1 calc R . . C4 C 0.04732(13) -0.14243(17) 0.4296(2) 0.0245(4) Uani 1 1 d . . . H4A H 0.0264 -0.2229 0.4223 0.029 Uiso 1 1 calc R . . H4B H -0.0029 -0.0919 0.3750 0.029 Uiso 1 1 calc R . . C5 C 0.09307(15) -0.1014(2) 0.5613(2) 0.0353(6) Uani 1 1 d . . . H5A H 0.0538 -0.1047 0.5836 0.053 Uiso 1 1 calc R . . H5B H 0.1127 -0.0210 0.5690 0.053 Uiso 1 1 calc R . . H5C H 0.1421 -0.1521 0.6163 0.053 Uiso 1 1 calc R . . C6 C 0.10383(12) 0.36109(17) 0.3723(2) 0.0178(4) Uani 1 1 d . . . C7 C 0.10059(12) 0.29890(18) 0.52011(18) 0.0239(4) Uani 1 1 d . . . H7A H 0.0989 0.2493 0.5746 0.029 Uiso 1 1 calc R . . C8 C 0.10224(13) 0.41606(19) 0.52376(19) 0.0256(4) Uani 1 1 d . . . H8A H 0.1020 0.4630 0.5811 0.031 Uiso 1 1 calc R . . C9 C 0.10709(12) 0.36357(17) 0.26572(19) 0.0229(4) Uani 1 1 d . . . H9A H 0.0761 0.4333 0.2154 0.028 Uiso 1 1 calc R . . H9C H 0.0773 0.2939 0.2142 0.028 Uiso 1 1 calc R . . C10 C 0.19710(15) 0.3659(2) 0.3023(2) 0.0437(7) Uani 1 1 d . . . H10D H 0.1950 0.3675 0.2285 0.065 Uiso 1 1 calc R . . H10A H 0.2278 0.2962 0.3505 0.065 Uiso 1 1 calc R . . H10B H 0.2266 0.4357 0.3517 0.065 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 0.02888(17) 0.01147(17) 0.02913(18) -0.00129(9) 0.01840(14) -0.00099(9) Cu2 0.02646(16) 0.01148(17) 0.02612(17) 0.00034(9) 0.01675(13) 0.00005(8) N1 0.0251(8) 0.0135(8) 0.0241(9) -0.0014(6) 0.0146(7) -0.0001(6) N2 0.0255(8) 0.0158(8) 0.0247(9) -0.0003(6) 0.0161(7) -0.0001(6) N3 0.0236(8) 0.0141(8) 0.0248(9) 0.0012(6) 0.0150(7) -0.0005(6) N4 0.0269(8) 0.0148(8) 0.0285(9) -0.0012(7) 0.0179(8) -0.0008(6) C1 0.0224(9) 0.0123(11) 0.0217(11) -0.0022(6) 0.0130(9) -0.0006(7) C2 0.0229(9) 0.0249(11) 0.0247(10) 0.0009(8) 0.0150(8) 0.0043(8) C3 0.0236(9) 0.0175(10) 0.0259(10) 0.0004(8) 0.0148(8) -0.0019(8) C4 0.0291(10) 0.0186(11) 0.0314(12) -0.0025(8) 0.0211(10) -0.0008(8) C5 0.0368(12) 0.0457(15) 0.0291(12) 0.0024(10) 0.0229(11) 0.0028(10) C6 0.0178(9) 0.0138(11) 0.0215(10) 0.0002(7) 0.0116(8) -0.0008(6) C7 0.0278(10) 0.0227(11) 0.0238(10) 0.0021(8) 0.0169(9) -0.0007(8) C8 0.0294(10) 0.0248(11) 0.0240(11) -0.0053(9) 0.0168(9) -0.0017(9) C9 0.0236(10) 0.0227(11) 0.0262(11) 0.0023(8) 0.0169(9) 0.0021(7) C10 0.0243(11) 0.075(2) 0.0378(15) 0.0026(12) 0.0218(11) 0.0022(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 1.8464(16) . ? Cu1 N4 1.8665(16) 1_545 ? Cu2 N3 1.8433(16) . ? Cu2 N2 1.8617(16) . ? N1 C1 1.339(2) . ? N1 C2 1.388(2) . ? N2 C1 1.337(3) . ? N2 C3 1.386(2) . ? N3 C6 1.346(2) . ? N3 C7 1.385(2) . ? N4 C6 1.341(2) . ? N4 C8 1.384(3) . ? N4 Cu1 1.8665(16) 1_565 ? C1 C4 1.491(3) . ? C2 C3 1.357(3) . ? C4 C5 1.521(3) . ? C6 C9 1.488(3) . ? C7 C8 1.344(3) . ? C9 C10 1.518(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 N4 178.10(7) . 1_545 ? N3 Cu2 N2 174.65(7) . . ? C1 N1 C2 105.11(17) . . ? C1 N1 Cu1 127.38(14) . . ? C2 N1 Cu1 127.29(14) . . ? C1 N2 C3 105.67(17) . . ? C1 N2 Cu2 128.05(14) . . ? C3 N2 Cu2 126.18(14) . . ? C6 N3 C7 105.15(16) . . ? C6 N3 Cu2 128.29(14) . . ? C7 N3 Cu2 126.22(14) . . ? C6 N4 C8 105.65(17) . . ? C6 N4 Cu1 126.22(14) . 1_565 ? C8 N4 Cu1 127.90(14) . 1_565 ? N2 C1 N1 112.65(18) . . ? N2 C1 C4 124.27(18) . . ? N1 C1 C4 123.04(18) . . ? C3 C2 N1 108.61(17) . . ? C2 C3 N2 107.95(17) . . ? C1 C4 C5 113.37(18) . . ? N4 C6 N3 111.99(18) . . ? N4 C6 C9 124.14(18) . . ? N3 C6 C9 123.86(18) . . ? C8 C7 N3 108.88(17) . . ? C7 C8 N4 108.35(18) . . ? C6 C9 C10 113.41(18) . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 27.99 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.296 _refine_diff_density_min -0.443 _refine_diff_density_rms 0.120 #End of Crystallographic Information File