# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Prof Xiao-Ming Chen' _publ_contact_author_address ; School of Chemistry and Chemical Engineering Sun Yat-Sen University 135 XinGang Xilu Guangzhou 510275 CHINA ; _publ_contact_author_email CESCXM@ZSU.EDU.CN _publ_section_title ; Two mixed-valence copper(I,II) imidazolate coordination polymers: Metal valence tuning approach for new topological structures ; loop_ _publ_author_name 'Xiao-Ming Chen' 'Xiao-Chun Huang' 'Yan-Yong Lin' 'Jie-Peng Zhang' #====================================== data_compoud_1 _database_code_depnum_ccdc_archive 'CCDC 227576' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H9 Cu2 N6' _chemical_formula_weight 328.30 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 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 5.5376(3) _cell_length_b 28.1637(16) _cell_length_c 14.6134(9) _cell_angle_alpha 90.00 _cell_angle_beta 91.3370(10) _cell_angle_gamma 90.00 _cell_volume 2278.5(2) _cell_formula_units_Z 8 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.914 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1304 _exptl_absorpt_coefficient_mu 3.717 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.5235 _exptl_absorpt_correction_T_max 0.6055 _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_reflns_number 16818 _diffrn_reflns_av_R_equivalents 0.0331 _diffrn_reflns_av_sigmaI/netI 0.0368 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 27.00 _reflns_number_total 4948 _reflns_number_gt 4300 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART for Windows NT, Bruker AXS Inc., 1998.' _computing_cell_refinement 'SAINT-PLUS for Windows NT, Ver. 6.0, Bruker AXS Inc., 1997.' _computing_data_reduction 'SAINT-PLUS for Windows NT, Ver. 6.0, Bruker AXS Inc., 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^)+(0.0336P)^2^+3.7144P] 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 4948 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0424 _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_ref 0.0804 _refine_ls_wR_factor_gt 0.0771 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _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 0.67606(7) 0.104524(12) 0.67633(3) 0.01102(10) Uani 1 1 d . . . Cu2 Cu 0.05704(7) 0.098506(12) 0.29676(3) 0.01085(10) Uani 1 1 d . . . Cu3 Cu 0.80404(7) 0.284906(13) 0.48010(3) 0.01132(10) Uani 1 1 d . . . Cu4 Cu 0.31160(7) 0.280429(13) 0.47796(3) 0.01195(10) Uani 1 1 d . . . N1 N 0.7393(5) 0.04108(9) 0.72859(18) 0.0121(5) Uani 1 1 d . . . N2 N 0.8748(5) -0.03346(9) 0.74121(18) 0.0126(5) Uani 1 1 d . . . N3 N 0.7325(5) 0.08480(9) 0.54929(19) 0.0145(6) Uani 1 1 d . . . N4 N 0.8955(5) 0.08163(9) 0.41128(18) 0.0137(6) Uani 1 1 d . . . N5 N 0.4651(5) 0.12469(9) 0.77602(18) 0.0127(5) Uani 1 1 d . . . N6 N 0.3135(5) 0.16863(9) 0.88863(18) 0.0109(5) Uani 1 1 d . . . N7 N 0.7759(5) 0.16983(9) 0.64668(18) 0.0120(5) Uani 1 1 d . . . N8 N 0.8222(5) 0.23772(9) 0.57021(18) 0.0122(5) Uani 1 1 d . . . N9 N -0.0579(5) 0.12068(9) 0.17520(18) 0.0120(5) Uani 1 1 d . . . N10 N -0.1743(5) 0.16746(9) 0.05881(18) 0.0125(5) Uani 1 1 d . . . N11 N 0.2170(5) 0.15763(9) 0.33608(18) 0.0118(5) Uani 1 1 d . . . N12 N 0.3123(5) 0.22776(9) 0.39947(18) 0.0124(5) Uani 1 1 d . . . C1 C 0.8325(5) 0.00358(10) 0.6858(2) 0.0127(6) Uani 1 1 d . . . H1A H 0.8701 0.0032 0.6134 0.015 Uiso 1 1 d R . . C2 C 0.8026(6) -0.01845(11) 0.8263(2) 0.0149(7) Uani 1 1 d . . . H2A H 0.8091 -0.0393 0.8886 0.018 Uiso 1 1 d R . . C3 C 0.7227(6) 0.02694(11) 0.8185(2) 0.0167(7) Uani 1 1 d . . . H3A H 0.6564 0.0485 0.8739 0.020 Uiso 1 1 d R . . C4 C 0.9166(6) 0.09800(11) 0.4966(2) 0.0141(7) Uani 1 1 d . . . H4A H 1.0665 0.1196 0.5209 0.017 Uiso 1 1 d R . . C5 C 0.6824(6) 0.05628(11) 0.4087(2) 0.0169(7) Uani 1 1 d . . . H5A H 0.6064 0.0379 0.3496 0.020 Uiso 1 1 d R . . C6 C 0.5836(6) 0.05837(11) 0.4932(2) 0.0167(7) Uani 1 1 d . . . H6A H 0.4158 0.0419 0.5127 0.020 Uiso 1 1 d R . . C7 C 0.4786(6) 0.16536(11) 0.8226(2) 0.0116(6) Uani 1 1 d . . . H7A H 0.6088 0.1930 0.8087 0.014 Uiso 1 1 d R . . C8 C 0.1826(6) 0.12684(11) 0.8818(2) 0.0134(6) Uani 1 1 d . . . H8A H 0.0322 0.1170 0.9239 0.016 Uiso 1 1 d R . . C9 C 0.2753(6) 0.10020(11) 0.8131(2) 0.0139(7) Uani 1 1 d . . . H9A H 0.2105 0.0656 0.7913 0.017 Uiso 1 1 d R . . C10 C 0.6933(6) 0.19805(11) 0.5796(2) 0.0143(7) Uani 1 1 d . . . H10A H 0.5367 0.1896 0.5369 0.017 Uiso 1 1 d R . . C11 C 0.9998(7) 0.23444(12) 0.6371(2) 0.0213(8) Uani 1 1 d . . . H11A H 1.1396 0.2605 0.6507 0.026 Uiso 1 1 d R . . C12 C 0.9713(7) 0.19303(12) 0.6833(2) 0.0208(7) Uani 1 1 d . . . H12A H 1.0847 0.1806 0.7398 0.025 Uiso 1 1 d R . . C13 C -0.0319(6) 0.16260(11) 0.1338(2) 0.0124(6) Uani 1 1 d . . . H13A H 0.0914 0.1899 0.1583 0.015 Uiso 1 1 d R . . C14 C -0.3035(6) 0.12550(11) 0.0530(2) 0.0151(7) Uani 1 1 d . . . H14A H -0.4390 0.1167 0.0011 0.018 Uiso 1 1 d R . . C15 C -0.2313(6) 0.09716(11) 0.1237(2) 0.0142(7) Uani 1 1 d . . . H15A H -0.2994 0.0619 0.1374 0.017 Uiso 1 1 d R . . C16 C 0.1501(6) 0.19227(11) 0.3926(2) 0.0132(6) Uani 1 1 d . . . H16A H -0.0179 0.1919 0.4290 0.016 Uiso 1 1 d R . . C17 C 0.4962(6) 0.21403(12) 0.3430(2) 0.0167(7) Uani 1 1 d . . . H17A H 0.6608 0.2338 0.3318 0.020 Uiso 1 1 d R . . C18 C 0.4378(6) 0.17163(12) 0.3041(2) 0.0170(7) Uani 1 1 d . . . H18A H 0.5461 0.1523 0.2559 0.020 Uiso 1 1 d 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 0.0175(2) 0.00667(17) 0.0091(2) 0.00060(14) 0.00394(15) 0.00093(14) Cu2 0.0180(2) 0.00674(18) 0.00792(19) -0.00005(14) 0.00142(15) 0.00017(14) Cu3 0.0136(2) 0.00963(18) 0.0108(2) 0.00294(14) 0.00128(15) -0.00072(14) Cu4 0.0137(2) 0.01006(18) 0.0121(2) -0.00371(15) -0.00028(15) -0.00068(14) N1 0.0172(14) 0.0080(12) 0.0112(13) 0.0001(10) 0.0015(11) 0.0010(10) N2 0.0203(14) 0.0090(12) 0.0085(13) -0.0011(10) 0.0022(11) 0.0001(10) N3 0.0221(15) 0.0080(12) 0.0136(14) 0.0006(10) 0.0039(12) 0.0003(10) N4 0.0176(14) 0.0130(13) 0.0106(13) 0.0002(11) 0.0018(11) -0.0001(11) N5 0.0174(14) 0.0110(12) 0.0099(13) -0.0011(10) 0.0040(11) 0.0027(10) N6 0.0119(13) 0.0116(12) 0.0092(13) -0.0003(10) -0.0026(10) 0.0021(10) N7 0.0160(14) 0.0095(12) 0.0106(13) -0.0006(10) 0.0010(11) 0.0009(10) N8 0.0172(14) 0.0085(12) 0.0111(14) 0.0016(10) 0.0022(11) 0.0000(10) N9 0.0154(14) 0.0117(13) 0.0090(13) 0.0011(10) 0.0002(11) 0.0002(10) N10 0.0140(13) 0.0119(12) 0.0117(13) 0.0024(10) 0.0011(11) 0.0035(10) N11 0.0126(13) 0.0111(12) 0.0117(13) 0.0003(10) 0.0011(10) -0.0010(10) N12 0.0146(13) 0.0092(12) 0.0133(14) -0.0010(10) 0.0004(11) 0.0001(10) C1 0.0136(16) 0.0109(14) 0.0138(16) 0.0008(12) 0.0018(13) -0.0014(12) C2 0.0208(17) 0.0136(15) 0.0104(16) 0.0018(12) 0.0006(13) 0.0039(13) C3 0.0263(18) 0.0155(16) 0.0084(16) 0.0005(12) 0.0044(14) 0.0050(13) C4 0.0184(17) 0.0108(15) 0.0132(16) 0.0013(12) 0.0017(13) -0.0014(12) C5 0.0208(17) 0.0159(16) 0.0138(17) -0.0032(13) -0.0006(14) -0.0034(13) C6 0.0188(17) 0.0150(15) 0.0163(17) -0.0023(13) 0.0035(14) -0.0015(13) C7 0.0140(15) 0.0109(14) 0.0100(15) 0.0010(12) 0.0004(12) 0.0017(12) C8 0.0141(16) 0.0125(15) 0.0138(16) -0.0004(12) 0.0022(13) -0.0001(12) C9 0.0146(16) 0.0113(15) 0.0157(17) 0.0013(12) 0.0008(13) -0.0006(12) C10 0.0128(15) 0.0121(15) 0.0179(17) 0.0030(13) 0.0000(13) -0.0005(12) C11 0.028(2) 0.0201(17) 0.0156(18) 0.0047(14) -0.0072(15) -0.0096(14) C12 0.0252(19) 0.0211(18) 0.0158(17) 0.0065(14) -0.0076(15) -0.0074(14) C13 0.0147(16) 0.0118(15) 0.0107(15) -0.0005(12) 0.0015(12) 0.0012(12) C14 0.0170(16) 0.0125(15) 0.0158(17) 0.0005(13) -0.0025(13) -0.0003(12) C15 0.0169(16) 0.0115(15) 0.0142(17) 0.0015(12) -0.0002(13) -0.0001(12) C16 0.0157(16) 0.0101(14) 0.0137(16) -0.0012(12) -0.0002(13) 0.0006(12) C17 0.0164(17) 0.0194(17) 0.0144(17) -0.0024(13) 0.0026(13) -0.0040(13) C18 0.0176(17) 0.0174(16) 0.0164(17) -0.0049(13) 0.0052(14) -0.0008(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 1.970(3) . ? Cu1 N1 1.971(3) . ? Cu1 N7 1.972(3) . ? Cu1 N5 1.972(2) . ? Cu2 N2 1.954(3) 3_656 ? Cu2 N11 1.966(3) . ? Cu2 N4 1.974(3) 1_455 ? Cu2 N9 1.974(3) . ? Cu3 N8 1.872(3) . ? Cu3 N6 1.872(3) 4_665 ? Cu3 Cu4 2.7293(6) . ? Cu3 Cu4 2.8144(5) 1_655 ? Cu4 N12 1.875(3) . ? Cu4 N10 1.884(3) 4_666 ? Cu4 Cu3 2.8144(6) 1_455 ? N1 C1 1.337(4) . ? N1 C3 1.378(4) . ? N2 C1 1.338(4) . ? N2 C2 1.381(4) . ? N2 Cu2 1.954(3) 3_656 ? N3 C4 1.345(4) . ? N3 C6 1.369(4) . ? N4 C4 1.332(4) . ? N4 C5 1.379(4) . ? N4 Cu2 1.974(3) 1_655 ? N5 C7 1.334(4) . ? N5 C9 1.378(4) . ? N6 C7 1.348(4) . ? N6 C8 1.385(4) . ? N6 Cu3 1.872(3) 4_566 ? N7 C10 1.334(4) . ? N7 C12 1.363(4) . ? N8 C10 1.335(4) . ? N8 C11 1.373(4) . ? N9 C13 1.335(4) . ? N9 C15 1.376(4) . ? N10 C13 1.343(4) . ? N10 C14 1.383(4) . ? N10 Cu4 1.884(3) 4_565 ? N11 C16 1.336(4) . ? N11 C18 1.377(4) . ? N12 C16 1.346(4) . ? N12 C17 1.381(4) . ? C2 C3 1.357(4) . ? C5 C6 1.364(4) . ? C8 C9 1.363(4) . ? C11 C12 1.359(5) . ? C14 C15 1.358(5) . ? C17 C18 1.359(5) . ? 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 N1 94.52(11) . . ? N3 Cu1 N7 90.26(11) . . ? N1 Cu1 N7 151.95(11) . . ? N3 Cu1 N5 152.52(12) . . ? N1 Cu1 N5 94.46(11) . . ? N7 Cu1 N5 93.88(10) . . ? N2 Cu2 N11 142.07(11) 3_656 . ? N2 Cu2 N4 96.28(11) 3_656 1_455 ? N11 Cu2 N4 99.57(11) . 1_455 ? N2 Cu2 N9 95.83(11) 3_656 . ? N11 Cu2 N9 97.39(11) . . ? N4 Cu2 N9 134.10(11) 1_455 . ? N8 Cu3 N6 175.23(12) . 4_665 ? N8 Cu3 Cu4 90.71(8) . . ? N6 Cu3 Cu4 93.94(8) 4_665 . ? N8 Cu3 Cu4 86.49(8) . 1_655 ? N6 Cu3 Cu4 88.79(8) 4_665 1_655 ? Cu4 Cu3 Cu4 174.63(2) . 1_655 ? N12 Cu4 N10 177.30(12) . 4_666 ? N12 Cu4 Cu3 91.57(8) . . ? N10 Cu4 Cu3 86.00(8) 4_666 . ? N12 Cu4 Cu3 93.35(8) . 1_455 ? N10 Cu4 Cu3 89.13(8) 4_666 1_455 ? Cu3 Cu4 Cu3 174.63(2) . 1_455 ? C1 N1 C3 104.6(3) . . ? C1 N1 Cu1 127.0(2) . . ? C3 N1 Cu1 128.0(2) . . ? C1 N2 C2 104.8(3) . . ? C1 N2 Cu2 126.3(2) . 3_656 ? C2 N2 Cu2 127.2(2) . 3_656 ? C4 N3 C6 105.2(3) . . ? C4 N3 Cu1 127.0(2) . . ? C6 N3 Cu1 127.7(2) . . ? C4 N4 C5 105.2(3) . . ? C4 N4 Cu2 132.7(2) . 1_655 ? C5 N4 Cu2 120.4(2) . 1_655 ? C7 N5 C9 105.3(2) . . ? C7 N5 Cu1 126.7(2) . . ? C9 N5 Cu1 128.1(2) . . ? C7 N6 C8 104.6(2) . . ? C7 N6 Cu3 126.1(2) . 4_566 ? C8 N6 Cu3 128.5(2) . 4_566 ? C10 N7 C12 105.0(3) . . ? C10 N7 Cu1 128.6(2) . . ? C12 N7 Cu1 125.8(2) . . ? C10 N8 C11 104.3(3) . . ? C10 N8 Cu3 130.3(2) . . ? C11 N8 Cu3 125.0(2) . . ? C13 N9 C15 105.0(3) . . ? C13 N9 Cu2 130.6(2) . . ? C15 N9 Cu2 123.1(2) . . ? C13 N10 C14 104.8(3) . . ? C13 N10 Cu4 127.3(2) . 4_565 ? C14 N10 Cu4 127.8(2) . 4_565 ? C16 N11 C18 105.2(3) . . ? C16 N11 Cu2 132.1(2) . . ? C18 N11 Cu2 122.8(2) . . ? C16 N12 C17 104.3(3) . . ? C16 N12 Cu4 128.5(2) . . ? C17 N12 Cu4 126.8(2) . . ? N1 C1 N2 113.4(3) . . ? C3 C2 N2 108.3(3) . . ? C2 C3 N1 108.9(3) . . ? N4 C4 N3 112.9(3) . . ? C6 C5 N4 108.3(3) . . ? C5 C6 N3 108.5(3) . . ? N5 C7 N6 113.2(3) . . ? C9 C8 N6 108.4(3) . . ? C8 C9 N5 108.5(3) . . ? N7 C10 N8 113.5(3) . . ? C12 C11 N8 108.8(3) . . ? C11 C12 N7 108.4(3) . . ? N9 C13 N10 113.1(3) . . ? C15 C14 N10 108.2(3) . . ? C14 C15 N9 108.8(3) . . ? N11 C16 N12 113.2(3) . . ? C18 C17 N12 108.9(3) . . ? C17 C18 N11 108.3(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.696 _refine_diff_density_min -0.426 _refine_diff_density_rms 0.112 data_cu _database_code_depnum_ccdc_archive 'CCDC 227577' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H12 Cu3 N8' _chemical_formula_weight 458.92 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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.5367(5) _cell_length_b 6.7153(6) _cell_length_c 10.0436(9) _cell_angle_alpha 105.550(2) _cell_angle_beta 90.044(2) _cell_angle_gamma 90.586(2) _cell_volume 359.74(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 ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.118 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 227 _exptl_absorpt_coefficient_mu 4.404 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.6201 _exptl_absorpt_correction_T_max 0.8099 _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 ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3216 _diffrn_reflns_av_R_equivalents 0.0182 _diffrn_reflns_av_sigmaI/netI 0.0364 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.15 _diffrn_reflns_theta_max 28.00 _reflns_number_total 1692 _reflns_number_gt 1583 _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^)+(0.0508P)^2^+2.1590P] 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 1692 _refine_ls_number_parameters 109 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0467 _refine_ls_R_factor_gt 0.0446 _refine_ls_wR_factor_ref 0.1228 _refine_ls_wR_factor_gt 0.1216 _refine_ls_goodness_of_fit_ref 1.156 _refine_ls_restrained_S_all 1.156 _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 1.0000 1.0000 0.0000 0.0083(2) Uani 1 2 d S . . Cu2 Cu 0.5000 1.0000 0.5000 0.0141(2) Uani 1 2 d S . . Cu3 Cu 0.5000 0.5000 -0.5000 0.0131(2) Uani 1 2 d S . . N1 N 0.7801(7) 0.7931(6) -0.1244(4) 0.0148(8) Uani 1 1 d . . . N2 N 0.5941(7) 0.5995(6) -0.3149(4) 0.0138(8) Uani 1 1 d . . . N3 N 0.7299(7) 0.9147(6) 0.3615(4) 0.0145(8) Uani 1 1 d . . . N4 N 0.9128(7) 0.8935(6) 0.1596(4) 0.0119(7) Uani 1 1 d . . . C1 C 0.4694(9) 0.5757(7) -0.2015(5) 0.0162(9) Uani 1 1 d . . . H1A H 0.3083 0.4821 -0.2039 0.019 Uiso 1 1 d R . . C2 C 0.5849(9) 0.6915(7) -0.0850(5) 0.0148(9) Uani 1 1 d . . . H2A H 0.5321 0.7020 0.0206 0.018 Uiso 1 1 d R . . C3 C 0.7791(8) 0.7298(7) -0.2629(5) 0.0133(9) Uani 1 1 d . . . H3A H 0.9128 0.7785 -0.3266 0.016 Uiso 1 1 d R . . C4 C 1.0516(8) 0.7926(7) 0.2337(5) 0.0118(8) Uani 1 1 d . . . H4A H 1.2204 0.7159 0.1998 0.014 Uiso 1 1 d R . . C5 C 0.9419(8) 0.8051(7) 0.3568(5) 0.0127(9) Uani 1 1 d . . . H5A H 1.0087 0.7405 0.4375 0.015 Uiso 1 1 d R . . C6 C 0.7230(8) 0.9632(7) 0.2411(5) 0.0123(8) Uani 1 1 d . . . H6A H 0.5783 1.0502 0.2118 0.015 Uiso 1 1 d 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 0.0100(4) 0.0098(4) 0.0048(3) 0.0016(3) -0.0016(3) -0.0033(3) Cu2 0.0141(4) 0.0200(4) 0.0068(4) 0.0014(3) 0.0030(3) -0.0022(3) Cu3 0.0152(4) 0.0154(4) 0.0064(4) -0.0010(3) -0.0043(3) -0.0031(3) N1 0.0178(19) 0.0148(19) 0.0105(18) 0.0014(15) -0.0048(15) -0.0041(15) N2 0.0153(19) 0.0120(18) 0.0126(19) 0.0010(15) -0.0041(15) 0.0000(14) N3 0.0165(19) 0.0163(19) 0.0099(18) 0.0024(15) 0.0004(15) -0.0021(15) N4 0.0125(18) 0.0127(18) 0.0098(17) 0.0021(14) -0.0029(14) -0.0040(14) C1 0.018(2) 0.015(2) 0.015(2) 0.0029(18) -0.0055(18) -0.0038(18) C2 0.018(2) 0.015(2) 0.012(2) 0.0042(17) -0.0032(17) -0.0046(17) C3 0.015(2) 0.013(2) 0.012(2) 0.0021(17) -0.0039(16) -0.0032(17) C4 0.013(2) 0.0080(19) 0.013(2) 0.0001(16) -0.0015(16) -0.0024(16) C5 0.017(2) 0.011(2) 0.010(2) 0.0012(16) -0.0041(16) -0.0043(16) C6 0.012(2) 0.011(2) 0.013(2) 0.0006(16) -0.0008(16) -0.0024(16) _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 N4 1.981(4) 2_775 ? Cu1 N4 1.981(4) . ? Cu1 N1 2.001(4) . ? Cu1 N1 2.001(4) 2_775 ? Cu2 N3 1.864(4) 2_676 ? Cu2 N3 1.864(4) . ? Cu3 N2 1.871(4) 2_664 ? Cu3 N2 1.871(4) . ? N1 C3 1.341(6) . ? N1 C2 1.386(6) . ? N2 C3 1.350(6) . ? N2 C1 1.376(6) . ? N3 C6 1.335(6) . ? N3 C5 1.386(6) . ? N4 C6 1.341(6) . ? N4 C4 1.373(6) . ? C1 C2 1.373(6) . ? C4 C5 1.360(6) . ? 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 N4 Cu1 N4 180.000(1) 2_775 . ? N4 Cu1 N1 88.87(16) 2_775 . ? N4 Cu1 N1 91.13(16) . . ? N4 Cu1 N1 91.13(16) 2_775 2_775 ? N4 Cu1 N1 88.87(16) . 2_775 ? N1 Cu1 N1 180.0(2) . 2_775 ? N3 Cu2 N3 180.000(1) 2_676 . ? N2 Cu3 N2 180.0 2_664 . ? C3 N1 C2 104.6(4) . . ? C3 N1 Cu1 128.4(3) . . ? C2 N1 Cu1 126.8(3) . . ? C3 N2 C1 105.3(4) . . ? C3 N2 Cu3 127.7(3) . . ? C1 N2 Cu3 126.5(3) . . ? C6 N3 C5 104.6(4) . . ? C6 N3 Cu2 123.7(3) . . ? C5 N3 Cu2 131.7(3) . . ? C6 N4 C4 104.8(4) . . ? C6 N4 Cu1 122.7(3) . . ? C4 N4 Cu1 129.8(3) . . ? C2 C1 N2 108.1(4) . . ? C1 C2 N1 108.8(4) . . ? N1 C3 N2 113.2(4) . . ? C5 C4 N4 108.7(4) . . ? C4 C5 N3 108.4(4) . . ? N3 C6 N4 113.5(4) . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.868 _refine_diff_density_min -0.978 _refine_diff_density_rms 0.182