Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_cu _database_code_CSD 183240 _journal_coden_Cambridge 182 loop_ _publ_author_name 'Chen, Xiao-Ming' 'Huang, Xiaoying' 'Li, Jing' 'Lin, C. L.' 'Tao, Jun' 'Tong, Ming-Liang' 'Yuen, Tan' 'Zhang, Yong' _publ_contact_author_name 'Prof Xiao-Ming Chen' _publ_contact_author_address ; School of Chemistry and Chemical Engineering Sun Yat-Sen University 135 Xingang Rd. W. Guangzhou 510275 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_joiurnal 'Chem. Commun.' _publ_requested_coeditor_name ? _publ_contact_letter ; Dear Sir/Madam: Please consider this CIF as supplmentary data for a manuscript submitted to Chem. Commun. Xiao-Ming Chen ; #================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; A mixed-valence copper coordination polymer generated by hydrothermal metal/ligand redox reactions ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H11 Cu2 N2 O5' _chemical_formula_weight 462.37 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 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 5.3310(10) _cell_length_b 22.863(7) _cell_length_c 13.088(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.54 _cell_angle_gamma 90.00 _cell_volume 1594.6(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 15 _exptl_crystal_description prismatic _exptl_crystal_colour 'dark blue' _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.926 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 924 _exptl_absorpt_coefficient_mu 2.703 _exptl_absorpt_correction_type \y-scan _exptl_absorpt_correction_T_min 0.3338 _exptl_absorpt_correction_T_max 0.6716 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Siemens R3m' _diffrn_measurement_method '\w scan' _diffrn_standards_number 2 _diffrn_standards_interval_count 200 _diffrn_standards_decay_% none _diffrn_reflns_number 4024 _diffrn_reflns_av_R_equivalents 0.0336 _diffrn_reflns_av_sigmaI/netI 0.0524 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 27.51 _reflns_number_total 3644 _reflns_number_gt 2438 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SHELXTL-plus (Sheldrick, 1990)' _computing_cell_refinement 'SHELXTL-plus (Sheldrick, 1990)' _computing_data_reduction 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0588P)^2^+6.2256P] 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 SHELXL _refine_ls_extinction_coef 0.0006(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3644 _refine_ls_number_parameters 245 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0941 _refine_ls_R_factor_gt 0.0546 _refine_ls_wR_factor_ref 0.1546 _refine_ls_wR_factor_gt 0.1232 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.10156(14) 0.05367(3) 0.04987(6) 0.0358(2) Uani 1 d . . . Cu2 Cu 0.05601(14) 0.17850(4) 0.37738(6) 0.0388(2) Uani 1 d . . . N1 N 0.3386(9) 0.2103(2) 0.3061(3) 0.0306(10) Uani 1 d . . . N2 N 1.3030(9) 0.3037(2) -0.0219(4) 0.0331(11) Uani 1 d . . . O1 O -0.0660(9) 0.0903(2) 0.3427(3) 0.0436(11) Uani 1 d . . . O2 O 0.0546(8) 0.08533(18) 0.1825(3) 0.0390(10) Uani 1 d . . . O3 O -0.3844(8) -0.10059(19) -0.0227(4) 0.0461(12) Uani 1 d . . . O4 O -0.7580(8) -0.1184(2) 0.0372(3) 0.0445(11) Uani 1 d . . . O5 O -0.1473(7) -0.00616(17) 0.0697(3) 0.0372(10) Uani 1 d . . . C1 C 0.4054(12) 0.2676(3) 0.3055(5) 0.0376(14) Uani 1 d . . . H1A H 0.3151 0.2944 0.3474 0.080 Uiso 1 d R . . C2 C 0.5973(12) 0.2887(3) 0.2470(5) 0.0347(13) Uani 1 d . . . H2A H 0.6428 0.3293 0.2504 0.080 Uiso 1 d R . . C3 C 0.7261(10) 0.2510(2) 0.1831(4) 0.0275(11) Uani 1 d . . . C4 C 0.6546(10) 0.1924(2) 0.1830(4) 0.0301(12) Uani 1 d . . . H4A H 0.7375 0.1650 0.1398 0.080 Uiso 1 d R . . C5 C 0.4655(10) 0.1740(3) 0.2449(5) 0.0329(13) Uani 1 d . . . H5A H 0.4213 0.1332 0.2444 0.080 Uiso 1 d R . . C6 C 0.9263(11) 0.2710(3) 0.1133(4) 0.0315(12) Uani 1 d . . . C7 C 0.9581(12) 0.3288(3) 0.0839(5) 0.0381(14) Uani 1 d . . . H7A H 0.8482 0.3584 0.1094 0.080 Uiso 1 d R . . C8 C 1.1478(12) 0.3439(3) 0.0180(5) 0.0365(14) Uani 1 d . . . H8A H 1.1689 0.3843 0.0001 0.080 Uiso 1 d R . . C9 C 1.2731(11) 0.2476(3) 0.0077(5) 0.0341(13) Uani 1 d . . . H9A H 1.3886 0.2190 -0.0170 0.080 Uiso 1 d R . . C10 C 1.0886(10) 0.2294(3) 0.0709(4) 0.0315(12) Uani 1 d . . . H10A H 1.0686 0.1886 0.0862 0.080 Uiso 1 d R . . C11 C -0.0837(11) 0.0673(2) 0.2558(4) 0.0319(13) Uani 1 d . . . C12 C -0.2766(11) 0.0202(2) 0.2372(5) 0.0321(13) Uani 1 d . . . C13 C -0.3020(11) -0.0142(2) 0.1471(4) 0.0310(12) Uani 1 d . . . C14 C -0.4999(11) -0.0552(2) 0.1364(4) 0.0305(12) Uani 1 d . . . C15 C -0.5515(11) -0.0931(2) 0.0430(5) 0.0337(13) Uani 1 d . . . C16 C -0.6620(12) -0.0623(3) 0.2191(5) 0.0410(15) Uani 1 d . . . H16A H -0.7933 -0.0910 0.2138 0.080 Uiso 1 d R . . C17 C -0.6367(14) -0.0299(3) 0.3073(6) 0.0502(18) Uani 1 d . . . H17A H -0.7529 -0.0348 0.3614 0.080 Uiso 1 d R . . C18 C -0.4414(13) 0.0104(3) 0.3171(5) 0.0439(16) Uani 1 d . . . H18A H -0.4186 0.0318 0.3798 0.080 Uiso 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 0.0335(4) 0.0308(4) 0.0438(4) -0.0098(3) 0.0140(3) -0.0080(3) Cu2 0.0316(4) 0.0468(5) 0.0388(4) 0.0026(3) 0.0140(3) 0.0002(3) N1 0.028(2) 0.038(3) 0.026(2) 0.001(2) 0.0042(19) 0.002(2) N2 0.028(2) 0.033(3) 0.038(3) 0.004(2) 0.007(2) 0.001(2) O1 0.053(3) 0.042(3) 0.036(2) -0.008(2) 0.007(2) -0.007(2) O2 0.039(2) 0.034(2) 0.044(2) -0.0065(19) 0.009(2) -0.0085(19) O3 0.042(3) 0.039(2) 0.059(3) -0.017(2) 0.021(2) -0.015(2) O4 0.039(3) 0.048(3) 0.047(3) -0.009(2) 0.012(2) -0.012(2) O5 0.034(2) 0.029(2) 0.050(3) -0.0086(19) 0.016(2) -0.0074(17) C1 0.039(3) 0.037(3) 0.037(3) -0.001(3) 0.009(3) 0.007(3) C2 0.043(3) 0.025(3) 0.037(3) -0.003(2) 0.009(3) -0.002(3) C3 0.024(3) 0.030(3) 0.029(3) 0.002(2) 0.004(2) 0.001(2) C4 0.025(3) 0.031(3) 0.035(3) -0.002(2) 0.005(2) 0.002(2) C5 0.026(3) 0.031(3) 0.042(3) 0.002(3) 0.011(2) -0.001(2) C6 0.026(3) 0.035(3) 0.034(3) 0.004(2) 0.005(2) 0.001(2) C7 0.038(3) 0.031(3) 0.046(4) 0.002(3) 0.016(3) 0.005(3) C8 0.041(3) 0.033(3) 0.037(3) 0.004(3) 0.012(3) -0.004(3) C9 0.030(3) 0.033(3) 0.040(3) 0.001(3) 0.010(3) -0.001(2) C10 0.029(3) 0.033(3) 0.032(3) 0.000(2) 0.004(2) 0.002(2) C11 0.036(3) 0.027(3) 0.033(3) 0.002(2) 0.007(2) 0.004(2) C12 0.033(3) 0.026(3) 0.038(3) 0.000(2) 0.005(2) 0.004(2) C13 0.030(3) 0.027(3) 0.037(3) 0.001(2) 0.011(2) 0.001(2) C14 0.030(3) 0.026(3) 0.036(3) 0.002(2) 0.008(2) 0.001(2) C15 0.033(3) 0.026(3) 0.043(3) -0.005(2) 0.009(3) -0.002(2) C16 0.034(3) 0.030(3) 0.059(4) 0.002(3) 0.016(3) -0.006(3) C17 0.054(4) 0.045(4) 0.053(4) 0.002(3) 0.028(4) -0.008(3) C18 0.056(4) 0.037(3) 0.040(4) -0.004(3) 0.019(3) -0.001(3) _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 O3 1.892(4) 3 ? Cu1 O2 1.904(4) . ? Cu1 O5 1.925(4) 3 ? Cu1 O5 1.928(4) . ? Cu1 Cu1 2.9705(15) 3 ? Cu2 N1 1.935(5) . ? Cu2 N2 1.953(5) 4_466 ? Cu2 O1 2.163(5) . ? N1 C5 1.348(7) . ? N1 C1 1.358(8) . ? N2 C9 1.350(7) . ? N2 C8 1.351(8) . ? N2 Cu2 1.953(5) 4_765 ? O1 C11 1.254(7) . ? O2 C11 1.292(7) . ? O3 C15 1.267(7) . ? O3 Cu1 1.892(4) 3 ? O4 C15 1.244(7) . ? O5 C13 1.336(6) . ? O5 Cu1 1.925(4) 3 ? C1 C2 1.382(8) . ? C2 C3 1.395(8) . ? C3 C4 1.393(8) . ? C3 C6 1.495(7) . ? C4 C5 1.376(7) . ? C6 C7 1.389(8) . ? C6 C10 1.409(8) . ? C7 C8 1.391(8) . ? C9 C10 1.367(8) . ? C11 C12 1.505(8) . ? C12 C18 1.402(8) . ? C12 C13 1.421(8) . ? C13 C14 1.415(8) . ? C14 C16 1.413(8) . ? C14 C15 1.518(8) . ? C16 C17 1.374(10) . ? C17 C18 1.394(10) . ? 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 O3 Cu1 O2 94.63(18) 3 . ? O3 Cu1 O5 92.77(17) 3 3 ? O2 Cu1 O5 167.99(18) . 3 ? O3 Cu1 O5 169.21(18) 3 . ? O2 Cu1 O5 92.26(17) . . ? O5 Cu1 O5 79.14(18) 3 . ? O3 Cu1 Cu1 131.98(13) 3 3 ? O2 Cu1 Cu1 131.27(13) . 3 ? O5 Cu1 Cu1 39.60(11) 3 3 ? O5 Cu1 Cu1 39.54(12) . 3 ? N1 Cu2 N2 143.9(2) . 4_466 ? N1 Cu2 O1 118.83(19) . . ? N2 Cu2 O1 97.26(18) 4_466 . ? C5 N1 C1 117.0(5) . . ? C5 N1 Cu2 117.7(4) . . ? C1 N1 Cu2 124.9(4) . . ? C9 N2 C8 117.2(5) . . ? C9 N2 Cu2 118.7(4) . 4_765 ? C8 N2 Cu2 124.1(4) . 4_765 ? C11 O1 Cu2 126.5(4) . . ? C11 O2 Cu1 130.3(4) . . ? C15 O3 Cu1 129.0(4) . 3 ? C13 O5 Cu1 129.3(4) . 3 ? C13 O5 Cu1 129.8(4) . . ? Cu1 O5 Cu1 100.86(18) 3 . ? N1 C1 C2 122.6(5) . . ? C1 C2 C3 120.0(5) . . ? C4 C3 C2 117.1(5) . . ? C4 C3 C6 119.5(5) . . ? C2 C3 C6 123.3(5) . . ? C5 C4 C3 119.9(5) . . ? N1 C5 C4 123.2(5) . . ? C7 C6 C10 116.9(5) . . ? C7 C6 C3 123.6(5) . . ? C10 C6 C3 119.4(5) . . ? C6 C7 C8 120.3(5) . . ? N2 C8 C7 122.3(5) . . ? N2 C9 C10 123.8(5) . . ? C9 C10 C6 119.5(5) . . ? O1 C11 O2 120.6(5) . . ? O1 C11 C12 118.7(5) . . ? O2 C11 C12 120.6(5) . . ? C18 C12 C13 118.9(6) . . ? C18 C12 C11 115.7(5) . . ? C13 C12 C11 125.4(5) . . ? O5 C13 C14 119.4(5) . . ? O5 C13 C12 120.4(5) . . ? C14 C13 C12 120.1(5) . . ? C16 C14 C13 118.1(5) . . ? C16 C14 C15 116.7(5) . . ? C13 C14 C15 125.2(5) . . ? O4 C15 O3 122.2(6) . . ? O4 C15 C14 117.1(5) . . ? O3 C15 C14 120.6(5) . . ? C17 C16 C14 122.2(6) . . ? C16 C17 C18 119.3(6) . . ? C17 C18 C12 121.2(6) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 1.110 _refine_diff_density_min -0.691 _refine_diff_density_rms 0.140 #_eof #End of Crystallographic Information File