# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _publ_contact_author_email Kazuhito@fchem.chem.t.u-tokyo.ac.jp _publ_contact_author_name 'Kazuhito Hashimoto' _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _audit_creation_date 2002-04-18 _audit_creation_method 'by CrystalStructure v2.00' _audit_update_record ? _publ_contact_author_fax +81-3-5452-5083 _publ_contact_author_phone +81-3-5452-5081 _publ_contact_author_address ; Research Center for Advanced Science and Technology, The University of Tokyo, 4-6-1 Komaba, Meguro-Ku, Tokyo 153-8904, Japan ; #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; Two-dimensional Metamagnet Composed of Cyano-bridged CuII -WV Bimetallic Assembly ; loop_ _publ_author_name 'Shin-ichi Ohksohi' 'Yoichi Arimoto' 'Toshiya Hozumi' 'Hidetake Seino' 'Yasushi Mizobe' 'Kazuhito hashimoto' #============================================================================== data_[{Cu(L)2(H2O)}2{Cu(L)2(H2O)2}{W(CN)8}2]_(L=3-cyanopyridine) _database_code_CSD 219124 #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C52 H32 Cu3 N28 O4 W2 ' _chemical_formula_moiety ; [{Cu(L)2(H2O)}2{Cu(L)2(H2O)2}{W(CN)8}2]_(L=3-cyanopyridine) ; _chemical_formula_weight 1671.34 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z #------------------------------------------------------------------------------ _cell_length_a 10.103(1) _cell_length_b 12.361(2) _cell_length_c 12.700(4) _cell_angle_alpha 78.73(2) _cell_angle_beta 86.69(2) _cell_angle_gamma 86.98(1) _cell_volume 1551.3(6) _cell_formula_units_Z 1 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 15.1 _cell_measurement_theta_max 17.8 _cell_measurement_temperature 298.1 #------------------------------------------------------------------------------ _exptl_crystal_description prismatic _exptl_crystal_colour green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.789 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 807.00 _exptl_absorpt_coefficient_mu 4.777 _exptl_absorpt_correction_type ; \y scans (North,Phillips & Matthews, 1968) ; _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.229 _exptl_absorpt_correction_T_max 0.488 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 7452 _diffrn_reflns_av_R_equivalents 0.020 _diffrn_reflns_theta_max 27.51 _diffrn_measured_fraction_theta_max 0.9976 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.9976 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -9.74 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 7131 _reflns_number_gt 6504 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0300 _refine_ls_wR_factor_ref 0.0840 _refine_ls_hydrogen_treatment ? _refine_ls_number_reflns 6504 _refine_ls_number_parameters 464 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0012Fo^2^ + 1.0000\s^2^(Fo) + 0.0000]/(4Fo^2^)' _refine_ls_shift/su_max 0.0040 _refine_diff_density_max 1.85 _refine_diff_density_min -2.70 _refine_ls_extinction_method 'Larson (1970) Crystallographic Computing eq. 22' _refine_ls_extinction_coef 108.3(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.017 0.010 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cu Cu 0.284 1.430 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; W W -1.018 7.231 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 W1 W 0.25943(1) 0.21532(1) 0.30609(1) 0.01801(5) Uani 1.00 1 d . . . Cu1 Cu 0.5000 0.5000 0.0000 0.0265(2) Uani 1.00 1 d . . . Cu2 Cu 0.76790(4) 0.11065(4) 0.34695(4) 0.0217(1) Uani 1.00 1 d . . . O1 O 0.6602(4) 0.3486(3) -0.0037(4) 0.050(1) Uani 1.00 1 d . . . O2 O 0.7804(5) 0.3074(4) 0.2252(4) 0.063(1) Uani 1.00 1 d . . . N1 N 0.4100(4) 0.4000(3) 0.1209(3) 0.0332(9) Uani 1.00 1 d . . . N2 N 0.5756(3) 0.1444(3) 0.3393(3) 0.0296(9) Uani 1.00 1 d . . . N3 N -0.0342(3) 0.1058(3) 0.3413(3) 0.0253(8) Uani 1.00 1 d . . . N4 N 0.2481(4) 0.0573(3) 0.5478(3) 0.0324(9) Uani 1.00 1 d . . . N5 N 0.3276(5) -0.0311(4) 0.2477(4) 0.052(1) Uani 1.00 1 d . . . N6 N 0.1315(5) 0.2324(5) 0.0699(4) 0.058(1) Uani 1.00 1 d . . . N7 N 0.0258(5) 0.4073(4) 0.3204(6) 0.074(2) Uani 1.00 1 d . . . N8 N 0.3799(5) 0.3814(4) 0.4481(4) 0.052(1) Uani 1.00 1 d . . . N9 N 0.6170(3) 0.5497(3) 0.1069(3) 0.0291(9) Uani 1.00 1 d . . . N10 N 1.0788(5) 0.6111(5) 0.1054(5) 0.068(2) Uani 1.00 1 d . . . N11 N 0.7748(3) 0.1959(3) 0.4691(3) 0.0290(9) Uani 1.00 1 d . . . N12 N 1.0360(6) 0.1571(5) 0.7762(4) 0.066(2) Uani 1.00 1 d . . . N13 N 0.7666(3) 0.0585(3) 0.2057(3) 0.0267(8) Uani 1.00 1 d . . . N14 N 0.5089(6) -0.1831(5) 0.0576(6) 0.073(2) Uani 1.00 1 d . . . C1 C 0.3605(4) 0.3373(3) 0.1871(3) 0.0268(9) Uani 1.00 1 d . . . C2 C 0.4664(4) 0.1696(3) 0.3278(3) 0.0245(9) Uani 1.00 1 d . . . C3 C 0.0701(4) 0.1388(3) 0.3312(3) 0.0227(9) Uani 1.00 1 d . . . C4 C 0.2521(4) 0.1169(3) 0.4664(3) 0.0262(9) Uani 1.00 1 d . . . C5 C 0.3024(4) 0.0552(4) 0.2663(4) 0.031(1) Uani 1.00 1 d . . . C6 C 0.1767(5) 0.2274(4) 0.1511(4) 0.036(1) Uani 1.00 1 d . . . C7 C 0.1084(4) 0.3439(4) 0.3146(5) 0.040(1) Uani 1.00 1 d . . . C8 C 0.3362(4) 0.3246(3) 0.4001(4) 0.030(1) Uani 1.00 1 d . . . C9 C 0.7462(4) 0.5646(4) 0.0837(4) 0.031(1) Uani 1.00 1 d . . . C10 C 0.8293(5) 0.5906(4) 0.1564(4) 0.037(1) Uani 1.00 1 d . . . C11 C 0.7784(6) 0.6040(5) 0.2571(4) 0.047(1) Uani 1.00 1 d . . . C12 C 0.6452(5) 0.5900(5) 0.2805(4) 0.048(1) Uani 1.00 1 d . . . C13 C 0.5680(5) 0.5634(4) 0.2035(4) 0.038(1) Uani 1.00 1 d . . . C14 C 0.9690(5) 0.6028(5) 0.1275(5) 0.048(1) Uani 1.00 1 d . . . C15 C 0.8577(4) 0.1641(4) 0.5479(4) 0.031(1) Uani 1.00 1 d . . . C16 C 0.8740(5) 0.2269(4) 0.6255(4) 0.038(1) Uani 1.00 1 d . . . C17 C 0.8047(6) 0.3264(5) 0.6206(5) 0.055(2) Uani 1.00 1 d . . . C18 C 0.7182(6) 0.3590(5) 0.5392(6) 0.059(2) Uani 1.00 1 d . . . C19 C 0.7048(5) 0.2919(4) 0.4656(4) 0.042(1) Uani 1.00 1 d . . . C20 C 0.9653(6) 0.1862(5) 0.7097(4) 0.047(1) Uani 1.00 1 d . . . C21 C 0.6806(4) -0.0156(4) 0.1898(4) 0.035(1) Uani 1.00 1 d . . . C22 C 0.6771(5) -0.0447(4) 0.0900(4) 0.040(1) Uani 1.00 1 d . . . C23 C 0.7638(6) 0.0011(5) 0.0065(4) 0.053(2) Uani 1.00 1 d . . . C24 C 0.8504(6) 0.0742(5) 0.0254(4) 0.048(1) Uani 1.00 1 d . . . C25 C 0.8514(5) 0.1005(4) 0.1250(4) 0.036(1) Uani 1.00 1 d . . . C26 C 0.5827(6) -0.1226(5) 0.0743(5) 0.053(2) Uani 1.00 1 d . . . H1 H 0.768(5) 0.553(5) 0.017(5) 0.04(1) Uiso 1.00 1 d . . . H2 H 0.849(7) 0.614(6) 0.311(6) 0.07(2) Uiso 1.00 1 d . . . H3 H 0.610(7) 0.592(7) 0.355(6) 0.08(2) Uiso 1.00 1 d . . . H4 H 0.474(5) 0.554(4) 0.220(4) 0.04(1) Uiso 1.00 1 d . . . H5 H 0.906(5) 0.093(4) 0.551(4) 0.03(1) Uiso 1.00 1 d . . . H6 H 0.826(6) 0.376(5) 0.673(5) 0.06(2) Uiso 1.00 1 d . . . H7 H 0.665(6) 0.429(6) 0.532(5) 0.07(2) Uiso 1.00 1 d . . . H8 H 0.646(5) 0.304(4) 0.422(4) 0.03(1) Uiso 1.00 1 d . . . H9 H 0.618(5) -0.046(4) 0.242(4) 0.03(1) Uiso 1.00 1 d . . . H10 H 0.772(5) -0.020(5) -0.062(5) 0.05(2) Uiso 1.00 1 d . . . H11 H 0.907(7) 0.100(6) -0.023(6) 0.07(2) Uiso 1.00 1 d . . . H12 H 0.919(5) 0.148(5) 0.142(5) 0.05(2) Uiso 1.00 1 d . . . H13 H 0.615(7) 0.298(5) -0.040(6) 0.08(2) Uiso 1.00 1 d . . . H14 H 0.723(7) 0.348(8) -0.067(5) 0.11(3) Uiso 1.00 1 d . . . H15 H 0.735(7) 0.314(6) 0.155(3) 0.08(2) Uiso 1.00 1 d . . . H16 H 0.8750 0.3262 0.2082 0.0764 Uiso 0.50 1 c P . . H17 H 0.7350 0.3635 0.2645 0.0764 Uiso 0.50 1 c P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 W1 0.01402(9) 0.0205(1) 0.0180(1) -0.00329(5) 0.00011(5) 0.00052(6) Cu1 0.0245(3) 0.0306(4) 0.0219(3) -0.0127(3) -0.0005(3) 0.0036(3) Cu2 0.0148(2) 0.0271(2) 0.0242(2) -0.0019(2) -0.0015(2) -0.0065(2) O1 0.043(2) 0.042(2) 0.069(3) -0.008(2) 0.008(2) -0.021(2) O2 0.069(3) 0.050(2) 0.068(3) -0.009(2) -0.007(2) -0.001(2) N1 0.030(2) 0.037(2) 0.031(2) -0.013(1) -0.005(1) 0.001(1) N2 0.021(2) 0.034(2) 0.034(2) -0.001(1) -0.002(1) -0.009(1) N3 0.017(1) 0.032(2) 0.026(2) -0.004(1) -0.001(1) -0.004(1) N4 0.035(2) 0.032(2) 0.027(2) -0.007(1) -0.004(1) 0.004(1) N5 0.055(3) 0.043(2) 0.065(3) -0.002(2) -0.003(2) -0.030(2) N6 0.064(3) 0.075(3) 0.032(2) -0.036(3) -0.018(2) 0.012(2) N7 0.045(3) 0.049(3) 0.122(5) 0.015(2) 0.001(3) -0.007(3) N8 0.060(3) 0.042(2) 0.062(3) 0.002(2) -0.013(2) -0.027(2) N9 0.027(2) 0.034(2) 0.026(2) -0.007(1) -0.002(1) -0.003(1) N10 0.031(2) 0.089(4) 0.081(4) -0.013(2) -0.007(2) -0.009(3) N11 0.027(2) 0.029(2) 0.033(2) 0.002(1) -0.006(1) -0.010(1) N12 0.078(4) 0.076(4) 0.049(3) 0.015(3) -0.028(3) -0.022(3) N13 0.023(2) 0.030(2) 0.028(2) -0.003(1) -0.002(1) -0.007(1) N14 0.069(3) 0.060(3) 0.106(5) -0.002(3) -0.030(3) -0.044(3) C1 0.023(2) 0.031(2) 0.025(2) -0.008(1) -0.004(1) 0.001(2) C2 0.017(2) 0.032(2) 0.025(2) -0.003(1) -0.000(1) -0.006(1) C3 0.021(2) 0.023(2) 0.021(2) 0.000(1) 0.001(1) 0.001(1) C4 0.022(2) 0.030(2) 0.026(2) -0.005(1) -0.004(1) -0.004(2) C5 0.024(2) 0.037(2) 0.034(2) -0.002(2) -0.003(2) -0.012(2) C6 0.036(2) 0.044(3) 0.027(2) -0.018(2) -0.004(2) 0.003(2) C7 0.031(2) 0.024(2) 0.064(3) 0.007(2) -0.003(2) -0.007(2) C8 0.033(2) 0.026(2) 0.033(2) 0.001(2) -0.004(2) -0.008(2) C9 0.029(2) 0.032(2) 0.029(2) -0.005(2) -0.001(2) -0.002(2) C10 0.032(2) 0.041(2) 0.039(2) -0.011(2) -0.005(2) -0.004(2) C11 0.047(3) 0.057(3) 0.039(3) -0.011(2) -0.009(2) -0.013(2) C12 0.047(3) 0.067(4) 0.033(2) -0.013(2) 0.001(2) -0.018(2) C13 0.033(2) 0.045(3) 0.036(2) -0.008(2) 0.001(2) -0.008(2) C14 0.035(3) 0.056(3) 0.052(3) -0.013(2) -0.010(2) 0.002(2) C15 0.031(2) 0.032(2) 0.031(2) 0.000(2) -0.002(2) -0.009(2) C16 0.042(2) 0.041(2) 0.035(2) -0.003(2) -0.006(2) -0.014(2) C17 0.068(4) 0.049(3) 0.057(3) 0.011(3) -0.021(3) -0.031(3) C18 0.065(4) 0.047(3) 0.074(4) 0.024(3) -0.025(3) -0.033(3) C19 0.039(2) 0.042(3) 0.048(3) 0.011(2) -0.016(2) -0.019(2) C20 0.055(3) 0.050(3) 0.040(3) 0.004(2) -0.011(2) -0.020(2) C21 0.028(2) 0.036(2) 0.041(3) -0.002(2) -0.007(2) -0.011(2) C22 0.041(2) 0.037(2) 0.047(3) 0.004(2) -0.015(2) -0.017(2) C23 0.069(4) 0.063(4) 0.031(3) 0.007(3) -0.010(2) -0.021(2) C24 0.053(3) 0.063(4) 0.028(2) -0.002(3) 0.006(2) -0.009(2) C25 0.034(2) 0.043(2) 0.030(2) -0.005(2) 0.004(2) -0.004(2) C26 0.059(3) 0.045(3) 0.065(4) 0.005(2) -0.021(3) -0.033(3) #============================================================================== _computing_data_collection WinAFC _computing_cell_refinement WinAFC _computing_data_reduction CrystalStructure _computing_structure_solution SHELXS97 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure Ver. 3.00' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag W1 . C1 . 2.166(4) yes W1 . C2 . 2.156(4) yes W1 . C3 . 2.158(4) yes W1 . C4 . 2.157(4) yes W1 . C5 . 2.153(4) yes W1 . C6 . 2.158(4) yes W1 . C7 . 2.159(4) yes W1 . C8 . 2.167(4) yes Cu1 . O1 . 2.415(4) yes Cu1 . N1 . 1.982(4) yes Cu1 . N9 . 2.051(3) yes Cu2 . N2 . 1.969(3) yes Cu2 . N11 . 2.044(4) yes Cu2 . N13 . 2.021(3) yes O1 . H13 . 0.99(7) no O1 . H14 . 0.99(6) no O2 . H15 . 1.02(5) no O2 . H16 . 0.997 no O2 . H17 . 1.008 no N1 . C1 . 1.138(5) yes N2 . C2 . 1.140(5) yes N3 . C3 . 1.142(5) yes N4 . C4 . 1.146(5) yes N5 . C5 . 1.149(6) yes N6 . C6 . 1.141(6) yes N7 . C7 . 1.123(6) yes N8 . C8 . 1.136(6) yes N9 . C9 . 1.336(5) yes N9 . C13 . 1.335(6) yes N10 . C14 . 1.133(7) yes N11 . C15 . 1.329(5) yes N11 . C19 . 1.344(6) yes N12 . C20 . 1.130(7) yes N13 . C21 . 1.346(5) yes N13 . C25 . 1.338(5) yes N14 . C26 . 1.140(7) yes C9 . C10 . 1.376(6) yes C9 . H1 . 0.89(6) no C10 . C11 . 1.387(7) yes C10 . C14 . 1.447(7) yes C11 . C12 . 1.374(7) yes C11 . H2 . 1.05(8) no C12 . C13 . 1.383(7) yes C12 . H3 . 0.99(8) no C13 . H4 . 0.96(5) no C15 . C16 . 1.389(6) yes C15 . H5 . 0.98(5) no C16 . C17 . 1.375(7) yes C16 . C20 . 1.450(7) yes C17 . C18 . 1.378(8) yes C17 . H6 . 1.03(7) no C18 . C19 . 1.381(7) yes C18 . H7 . 0.99(7) no C19 . H8 . 0.82(4) no C21 . C22 . 1.387(7) yes C21 . H9 . 0.93(4) no C22 . C23 . 1.387(8) yes C22 . C26 . 1.439(7) yes C23 . C24 . 1.352(9) yes C23 . H10 . 0.96(6) no C24 . C25 . 1.368(7) yes C24 . H11 . 0.85(6) no C25 . H12 . 0.98(6) no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C1 . W1 . C2 . 76.57(15) yes C1 . W1 . C3 . 138.58(14) yes C2 . W1 . C3 . 138.81(14) yes C1 . W1 . C4 . 148.17(14) yes C2 . W1 . C4 . 78.64(15) yes C3 . W1 . C4 . 72.64(14) yes C1 . W1 . C5 . 108.53(16) yes C2 . W1 . C5 . 70.47(15) yes C3 . W1 . C5 . 76.39(15) yes C4 . W1 . C5 . 81.18(16) yes C1 . W1 . C6 . 69.72(15) yes C2 . W1 . C6 . 120.44(17) yes C3 . W1 . C6 . 72.12(15) yes C4 . W1 . C6 . 141.39(15) yes C5 . W1 . C6 . 75.70(18) yes C1 . W1 . C7 . 85.82(17) yes C2 . W1 . C7 . 144.25(17) yes C3 . W1 . C7 . 72.46(16) yes C4 . W1 . C7 . 103.43(18) yes C5 . W1 . C7 . 145.26(17) yes C1 . W1 . C8 . 76.26(16) yes C2 . W1 . C8 . 72.44(15) yes C3 . W1 . C8 . 126.92(15) yes C4 . W1 . C8 . 77.46(16) yes C5 . W1 . C8 . 140.04(15) yes C6 . W1 . C7 . 80.4(2) yes C6 . W1 . C8 . 138.06(17) yes C7 . W1 . C8 . 73.26(17) yes O1 . Cu1 . N1 . 85.80(15) yes O1 . Cu1 . N9 . 87.02(14) yes N1 . Cu1 . N9 . 89.53(14) yes N2 . Cu2 . N11 . 90.28(14) yes N2 . Cu2 . N13 . 89.10(14) yes N11 . Cu2 . N13 . 167.64(15) yes Cu1 . O1 . H13 . 103.7(4) no Cu1 . O1 . H14 . 120.9(4) no H13 . O1 . H14 . 80.1(6) no H15 . O2 . H16 . 108.4(4) no H15 . O2 . H17 . 107.3(4) no H16 . O2 . H17 . 109.1 no Cu1 . N1 . C1 . 175.8(4) yes Cu2 . N2 . C2 . 174.8(4) yes Cu1 . N9 . C9 . 120.8(3) yes Cu1 . N9 . C13 . 121.1(3) yes C9 . N9 . C13 . 118.0(4) yes Cu2 . N11 . C15 . 121.2(3) yes Cu2 . N11 . C19 . 120.3(3) yes C15 . N11 . C19 . 118.2(4) yes Cu2 . N13 . C21 . 121.7(3) yes Cu2 . N13 . C25 . 119.3(3) yes C21 . N13 . C25 . 119.0(4) yes W1 . C1 . N1 . 176.6(4) yes W1 . C2 . N2 . 179.4(4) yes W1 . C3 . N3 . 174.9(3) yes W1 . C4 . N4 . 174.4(4) yes W1 . C5 . N5 . 178.0(4) yes W1 . C6 . N6 . 178.8(4) yes W1 . C7 . N7 . 176.9(5) yes W1 . C8 . N8 . 178.1(4) yes N9 . C9 . C10 . 122.3(4) yes N9 . C9 . H1 . 110.3(3) no C10 . C9 . H1 . 127.4(3) no C9 . C10 . C11 . 119.7(4) yes C9 . C10 . C14 . 119.7(5) yes C11 . C10 . C14 . 120.6(5) yes C10 . C11 . C12 . 118.0(5) yes C10 . C11 . H2 . 115.4(4) no C12 . C11 . H2 . 126.1(4) no C11 . C12 . C13 . 119.0(5) yes C11 . C12 . H3 . 118.3(4) no C13 . C12 . H3 . 122.4(4) no N9 . C13 . C12 . 123.0(4) yes N9 . C13 . H4 . 117.7(3) no C12 . C13 . H4 . 119.3(3) no N10 . C14 . C10 . 179.2(6) yes N11 . C15 . C16 . 122.2(4) yes N11 . C15 . H5 . 117.2(3) no C16 . C15 . H5 . 120.7(3) no C15 . C16 . C17 . 119.7(4) yes C15 . C16 . C20 . 119.0(4) yes C17 . C16 . C20 . 121.3(4) yes C16 . C17 . C18 . 118.0(5) yes C16 . C17 . H6 . 118.6(4) no C18 . C17 . H6 . 123.2(4) no C17 . C18 . C19 . 119.4(5) yes C17 . C18 . H7 . 122.1(4) no C19 . C18 . H7 . 118.5(4) no N11 . C19 . C18 . 122.4(5) yes N11 . C19 . H8 . 115.1(3) no C18 . C19 . H8 . 122.0(3) no N12 . C20 . C16 . 178.2(6) yes N13 . C21 . C22 . 120.2(5) yes N13 . C21 . H9 . 123.1(3) no C22 . C21 . H9 . 116.5(3) no C21 . C22 . C23 . 120.1(5) yes C21 . C22 . C26 . 119.3(5) yes C23 . C22 . C26 . 120.6(5) yes C22 . C23 . C24 . 118.3(5) yes C22 . C23 . H10 . 124.0(3) no C24 . C23 . H10 . 117.4(3) no C23 . C24 . C25 . 120.0(5) yes C23 . C24 . H11 . 119.7(4) no C25 . C24 . H11 . 120.2(4) no N13 . C25 . C24 . 122.4(5) yes N13 . C25 . H12 . 116.7(3) no C24 . C25 . H12 . 120.8(3) no N14 . C26 . C22 . 177.3(7) yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_site_symmetry_1 _geom_torsion_atom_site_label_2 _geom_torsion_site_symmetry_2 _geom_torsion_atom_site_label_3 _geom_torsion_site_symmetry_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C2 . W1 . C1 . N1 . 125.3(1) yes C3 . W1 . C1 . N1 . -28.7(1) yes C4 . W1 . C1 . N1 . 165.1(1) yes C5 . W1 . C1 . N1 . 61.6(1) yes C6 . W1 . C1 . N1 . -4.8(1) yes C7 . W1 . C1 . N1 . -86.1(1) yes C8 . W1 . C1 . N1 . -159.8(1) yes C1 . W1 . C2 . N2 . -137.9(7) yes C3 . W1 . C2 . N2 . 15.9(7) yes C4 . W1 . C2 . N2 . 62.2(7) yes C5 . W1 . C2 . N2 . -22.4(7) yes C6 . W1 . C2 . N2 . -81.6(7) yes C7 . W1 . C2 . N2 . 159.4(7) yes C8 . W1 . C2 . N2 . 142.5(7) yes C1 . W1 . C3 . N3 . -38.3(8) yes C2 . W1 . C3 . N3 . -178.0(7) yes C4 . W1 . C3 . N3 . 134.1(7) yes C5 . W1 . C3 . N3 . -141.0(7) yes C6 . W1 . C3 . N3 . -61.9(8) yes C7 . W1 . C3 . N3 . 23.4(8) yes C8 . W1 . C3 . N3 . 75.4(8) yes C1 . W1 . C4 . N4 . -124.1(7) yes C2 . W1 . C4 . N4 . -84.7(7) yes C3 . W1 . C4 . N4 . 65.4(7) yes C5 . W1 . C4 . N4 . -13.0(7) yes C6 . W1 . C4 . N4 . 40.5(8) yes C7 . W1 . C4 . N4 . 131.9(7) yes C8 . W1 . C4 . N4 . -159.0(7) yes C1 . W1 . C5 . N5 . 107.8(2) yes C2 . W1 . C5 . N5 . 40.1(2) yes C3 . W1 . C5 . N5 . -115.1(2) yes C4 . W1 . C5 . N5 . -40.9(2) yes C6 . W1 . C5 . N5 . 170.3(2) yes C7 . W1 . C5 . N5 . -141.8(2) yes C8 . W1 . C5 . N5 . 17.3(2) yes C1 . W1 . C6 . N6 . 177.6(4) yes C2 . W1 . C6 . N6 . 117.9(4) yes C3 . W1 . C6 . N6 . -18.8(4) yes C4 . W1 . C6 . N6 . 6.2(4) yes C5 . W1 . C6 . N6 . 61.2(4) yes C7 . W1 . C6 . N6 . -93.3(4) yes C8 . W1 . C6 . N6 . -144.6(4) yes C1 . W1 . C7 . N7 . 152.3(2) yes C2 . W1 . C7 . N7 . -147.7(2) yes C3 . W1 . C7 . N7 . 8.0(2) yes C4 . W1 . C7 . N7 . -58.6(2) yes C5 . W1 . C7 . N7 . 35.3(2) yes C6 . W1 . C7 . N7 . 82.2(2) yes C8 . W1 . C7 . N7 . -130.8(2) yes C1 . W1 . C8 . N8 . -54.1(2) yes C2 . W1 . C8 . N8 . 26.0(2) yes C3 . W1 . C8 . N8 . 164.5(2) yes C4 . W1 . C8 . N8 . 107.8(2) yes C5 . W1 . C8 . N8 . 48.5(2) yes C6 . W1 . C8 . N8 . -90.3(2) yes C7 . W1 . C8 . N8 . -143.8(2) yes O1 . Cu1 . N1 . C1 . -36.7(9) yes N9 . Cu1 . N1 . C1 . -123.7(8) yes O1 . Cu1 . N9 . C9 . 53.1(7) yes O1 . Cu1 . N9 . C13 . -123.8(6) yes N1 . Cu1 . N9 . C9 . 139.0(6) yes N1 . Cu1 . N9 . C13 . -38.0(7) yes O2 . Cu2 . N2 . C2 . 23.3(7) yes N11 . Cu2 . N2 . C2 . 106.6(6) yes N13 . Cu2 . N2 . C2 . -61.0(6) yes O2 . Cu2 . N11 . C15 . -131.8(6) yes O2 . Cu2 . N11 . C19 . 41.5(7) yes N2 . Cu2 . N11 . C15 . 145.7(6) yes N2 . Cu2 . N11 . C19 . -40.9(7) yes N13 . Cu2 . N11 . C15 . -127.2(2) yes N13 . Cu2 . N11 . C19 . 46.1(2) yes O2 . Cu2 . N13 . C21 . -134.0(6) yes O2 . Cu2 . N13 . C25 . 44.5(7) yes N2 . Cu2 . N13 . C21 . -51.4(6) yes N2 . Cu2 . N13 . C25 . 127.1(6) yes N11 . Cu2 . N13 . C21 . -138.6(2) yes N11 . Cu2 . N13 . C25 . 39.9(2) yes Cu1 . N1 . C1 . W1 . -55.9(8) yes Cu2 . N2 . C2 . W1 . 127.1(3) yes Cu1 . N9 . C9 . C10 . -175.5(4) yes C13 . N9 . C9 . C10 . 2(1) yes Cu1 . N9 . C13 . C12 . 175.8(5) yes C9 . N9 . C13 . C12 . -1(1) yes Cu2 . N11 . C15 . C16 . 173.2(4) yes C19 . N11 . C15 . C16 . -0(1) yes Cu2 . N11 . C19 . C18 . -172.1(5) yes C15 . N11 . C19 . C18 . 1(1) yes Cu2 . N13 . C21 . C22 . 176.2(4) yes C25 . N13 . C21 . C22 . -2(1) yes Cu2 . N13 . C25 . C24 . -175.8(5) yes C21 . N13 . C25 . C24 . 3(1) yes N9 . C9 . C10 . C11 . -1.1(9) yes N9 . C9 . C10 . C14 . 178.4(5) yes C9 . C10 . C11 . C12 . 0(1) yes C14 . C10 . C11 . C12 . -179.2(7) yes C9 . C10 . C14 . N10 . -94.0(5) yes C11 . C10 . C14 . N10 . 85.4(6) yes C10 . C11 . C12 . C13 . -0(1) yes C11 . C12 . C13 . N9 . 1(1) yes N11 . C15 . C16 . C17 . -1.2(9) yes N11 . C15 . C16 . C20 . 179.4(5) yes C15 . C16 . C17 . C18 . 2(1) yes C20 . C16 . C17 . C18 . -179.1(7) yes C15 . C16 . C20 . N12 . 173.6(2) yes C17 . C16 . C20 . N12 . -5.7(3) yes C16 . C17 . C18 . C19 . -0(1) yes C17 . C18 . C19 . N11 . -1(1) yes N13 . C21 . C22 . C23 . 1.2(9) yes N13 . C21 . C22 . C26 . -178.9(6) yes C21 . C22 . C23 . C24 . -0(1) yes C26 . C22 . C23 . C24 . 179.8(7) yes C21 . C22 . C26 . N14 . 165.0(2) yes C23 . C22 . C26 . N14 . -15.0(2) yes C22 . C23 . C24 . C25 . 1(1) yes C23 . C24 . C25 . N13 . -2(1) yes loop_ _geom_contact_atom_site_label_1 _geom_contact_site_symmetry_1 _geom_contact_atom_site_label_2 _geom_contact_site_symmetry_2 _geom_contact_distance _geom_contact_publ_flag Cu1 . O1 2_665 2.415(4) yes Cu1 . N1 2_665 1.982(4) yes Cu1 . N9 2_665 2.051(3) yes Cu1 . C1 2_665 3.118(4) yes Cu1 . C9 2_665 2.966(4) yes Cu1 . C13 2_665 2.970(5) yes Cu2 . N3 1_655 1.994(3) yes Cu2 . N4 2_656 2.247(3) yes Cu2 . C3 1_655 3.082(4) yes Cu2 . C4 2_656 3.312(4) yes O1 . O2 . 3.153(7) yes O1 . H15 . 2.1(1) no #============================================================================== data_[{Cu(L)2}2{Cu(L)2(H2O)2}{W(CN)8}2]_6(H2O)_(L=4-cyanopyridine) _database_code_CSD 219125 #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C52 H40 Cu3 N28 O8 W2 ' _chemical_formula_moiety ; [{Cu(L)2}2{Cu(L)2(H2O)2}{W(CN)8}2]_6(H2O)_(L=4-cyanopyridine) ; _chemical_formula_weight 1743.40 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z #------------------------------------------------------------------------------ _cell_length_a 10.219(2) _cell_length_b 10.441(2) _cell_length_c 16.094(3) _cell_angle_alpha 79.49(2) _cell_angle_beta 89.55(2) _cell_angle_gamma 73.32(1) _cell_volume 1615.5(5) _cell_formula_units_Z 1 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 15.0 _cell_measurement_theta_max 18.5 _cell_measurement_temperature 298.1 #------------------------------------------------------------------------------ _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 1.792 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 847.00 _exptl_absorpt_coefficient_mu 4.596 _exptl_absorpt_correction_type ; \y scans (North,Phillips & Matthews, 1968) ; _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.535 _exptl_absorpt_correction_T_max 0.725 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 7680 _diffrn_reflns_av_R_equivalents 0.017 _diffrn_reflns_theta_max 27.53 _diffrn_measured_fraction_theta_max 0.9961 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.9961 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.50 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 7416 _reflns_number_gt 6504 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.0930 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 6504 _refine_ls_number_parameters 434 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0014Fo^2^ + 1.0000\s^2^(Fo) + 0.0000]/(4Fo^2^)' _refine_ls_shift/su_max 0.0160 _refine_diff_density_max 3.34 _refine_diff_density_min -3.51 _refine_ls_extinction_method 'Larson (1970) Crystallographic Computing eq. 22' _refine_ls_extinction_coef 103.1(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.017 0.010 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cu Cu 0.284 1.430 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; W W -1.018 7.231 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 W1 W 0.21283(2) 0.13637(2) 0.29411(1) 0.01768(5) Uani 1.00 1 d . . . Cu1 Cu 0.5000 0.0000 0.0000 0.0314(2) Uani 1.00 1 d . . . Cu2 Cu -0.28294(5) 0.11705(5) 0.37457(3) 0.0217(1) Uani 1.00 1 d . . . O1 O 0.3147(4) 0.0134(4) -0.0368(3) 0.043(1) Uani 1.00 1 d D . . O2 O 0.2126(6) -0.1985(6) -0.0104(3) 0.068(2) Uani 1.00 1 d D . . O3 O 0.1099(5) 0.2402(6) -0.0528(4) 0.076(2) Uani 1.00 1 d . . . O4 O 0.1236(5) -0.2889(5) 0.1532(3) 0.056(1) Uani 1.00 1 d D . . N1 N 0.4179(5) 0.0455(5) 0.1408(3) 0.037(1) Uani 1.00 1 d . . . N2 N -0.0961(4) 0.1309(4) 0.3511(3) 0.030(1) Uani 1.00 1 d . . . N3 N 0.5233(4) 0.1285(4) 0.3542(3) 0.027(1) Uani 1.00 1 d . . . N4 N 0.2461(4) -0.0267(4) 0.4925(3) 0.030(1) Uani 1.00 1 d . . . N5 N 0.1174(6) 0.3715(5) 0.4136(4) 0.048(1) Uani 1.00 1 d . . . N6 N 0.2494(7) 0.4238(5) 0.1850(4) 0.057(2) Uani 1.00 1 d . . . N7 N 0.2328(7) -0.1833(6) 0.2868(4) 0.055(2) Uani 1.00 1 d . . . N8 N 0.0149(6) 0.1851(8) 0.1245(4) 0.065(2) Uani 1.00 1 d . . . N9 N 0.5340(5) -0.2076(4) 0.0418(3) 0.032(1) Uani 1.00 1 d . . . N10 N 0.6380(8) -0.7333(6) 0.1830(5) 0.070(2) Uani 1.00 1 d . . . N11 N -0.3356(4) 0.3107(4) 0.3986(3) 0.028(1) Uani 1.00 1 d . . . N12 N -0.4390(7) 0.8187(6) 0.4530(4) 0.058(2) Uani 1.00 1 d . . . N13 N -0.2260(4) -0.0619(4) 0.3333(3) 0.027(1) Uani 1.00 1 d . . . N14 N -0.1329(8) -0.5383(6) 0.2336(5) 0.077(2) Uani 1.00 1 d . . . C1 C 0.3488(5) 0.0775(5) 0.1949(3) 0.026(1) Uani 1.00 1 d . . . C2 C 0.0101(5) 0.1336(5) 0.3311(3) 0.025(1) Uani 1.00 1 d . . . C3 C 0.4142(4) 0.1300(5) 0.3372(3) 0.022(1) Uani 1.00 1 d . . . C4 C 0.2378(4) 0.0279(5) 0.4238(3) 0.023(1) Uani 1.00 1 d . . . C5 C 0.1528(5) 0.2915(5) 0.3715(3) 0.028(1) Uani 1.00 1 d . . . C6 C 0.2351(6) 0.3252(5) 0.2214(3) 0.033(1) Uani 1.00 1 d . . . C7 C 0.2248(5) -0.0726(5) 0.2895(3) 0.030(1) Uani 1.00 1 d . . . C8 C 0.0828(6) 0.1713(6) 0.1830(3) 0.038(1) Uani 1.00 1 d . . . C9 C 0.6242(6) -0.3008(6) 0.0083(4) 0.042(2) Uani 1.00 1 d . . . C10 C 0.6519(7) -0.4398(6) 0.0399(4) 0.049(2) Uani 1.00 1 d . . . C11 C 0.5838(6) -0.4808(6) 0.1084(4) 0.040(1) Uani 1.00 1 d . . . C12 C 0.4867(6) -0.3856(6) 0.1422(4) 0.040(1) Uani 1.00 1 d . . . C13 C 0.4641(6) -0.2492(6) 0.1074(4) 0.037(1) Uani 1.00 1 d . . . C14 C 0.6146(7) -0.6239(6) 0.1477(4) 0.049(2) Uani 1.00 1 d . . . C15 C -0.2529(6) 0.3429(6) 0.4488(4) 0.038(1) Uani 1.00 1 d . . . C16 C -0.2766(6) 0.4722(6) 0.4659(4) 0.041(2) Uani 1.00 1 d . . . C17 C -0.3907(6) 0.5725(5) 0.4282(4) 0.035(1) Uani 1.00 1 d . . . C18 C -0.4801(6) 0.5400(5) 0.3760(4) 0.039(1) Uani 1.00 1 d . . . C19 C -0.4480(5) 0.4072(5) 0.3628(3) 0.034(1) Uani 1.00 1 d . . . C20 C -0.4180(7) 0.7098(6) 0.4422(4) 0.043(2) Uani 1.00 1 d . . . C21 C -0.1368(5) -0.1716(5) 0.3784(4) 0.035(1) Uani 1.00 1 d . . . C22 C -0.1021(6) -0.2979(6) 0.3546(4) 0.039(1) Uani 1.00 1 d . . . C23 C -0.1653(5) -0.3090(5) 0.2808(3) 0.032(1) Uani 1.00 1 d . . . C24 C -0.2570(6) -0.1955(6) 0.2337(4) 0.038(1) Uani 1.00 1 d . . . C25 C -0.2835(5) -0.0725(5) 0.2615(3) 0.032(1) Uani 1.00 1 d . . . C26 C -0.1412(7) -0.4398(6) 0.2561(4) 0.049(2) Uani 1.00 1 d . . . H1 H 0.6718(6) -0.2717(6) -0.0390(4) 0.049(2) Uiso 1.00 1 c R . . H2 H 0.7166(7) -0.5046(6) 0.0144(4) 0.057(2) Uiso 1.00 1 c R . . H3 H 0.4362(6) -0.4129(6) 0.1885(4) 0.046(2) Uiso 1.00 1 c R . . H4 H 0.3972(6) -0.1829(6) 0.1305(4) 0.043(2) Uiso 1.00 1 c R . . H5 H -0.1737(6) 0.2739(6) 0.4742(4) 0.046(2) Uiso 1.00 1 c R . . H6 H -0.2158(6) 0.4917(6) 0.5029(4) 0.053(2) Uiso 1.00 1 c R . . H7 H -0.5604(6) 0.6068(5) 0.3504(4) 0.045(2) Uiso 1.00 1 c R . . H8 H -0.5076(5) 0.3838(5) 0.3272(3) 0.040(2) Uiso 1.00 1 c R . . H9 H -0.0954(5) -0.1629(5) 0.4289(4) 0.041(2) Uiso 1.00 1 c R . . H10 H -0.0374(6) -0.3742(6) 0.3875(4) 0.044(2) Uiso 1.00 1 c R . . H11 H -0.3011(6) -0.2013(6) 0.1834(4) 0.044(2) Uiso 1.00 1 c R . . H12 H -0.3443(5) 0.0066(5) 0.2284(3) 0.036(2) Uiso 1.00 1 c R . . H13 H 0.282(7) -0.057(5) -0.022(4) 0.05(2) Uiso 1.00 1 d D . . H14 H 0.243(4) 0.087(4) -0.048(3) 0.05(1) Uiso 1.00 1 d D . . H15 H 0.17(1) -0.19(1) 0.037(4) 0.08(5) Uiso 1.00 1 d D . . H16 H 0.15(1) -0.17(1) -0.056(5) 0.08(5) Uiso 1.00 1 d D . . H17 H 0.166(8) -0.268(8) 0.196(4) 0.07(2) Uiso 1.00 1 d D . . H18 H 0.170(8) -0.377(3) 0.168(5) 0.07(3) Uiso 1.00 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 W1 0.0148(1) 0.0172(1) 0.0215(1) -0.00545(7) 0.00100(6) -0.00365(6) Cu1 0.0278(4) 0.0256(4) 0.0384(5) -0.0099(3) -0.0039(3) 0.0032(3) Cu2 0.0152(2) 0.0208(3) 0.0296(3) -0.0060(2) 0.0008(2) -0.0052(2) O1 0.031(2) 0.040(2) 0.057(3) -0.012(2) -0.010(2) 0.002(2) O2 0.067(3) 0.099(4) 0.051(3) -0.054(3) -0.012(2) 0.002(3) O3 0.046(3) 0.083(4) 0.089(4) -0.000(3) -0.003(3) -0.021(3) O4 0.062(3) 0.040(2) 0.061(3) -0.007(2) -0.011(2) -0.008(2) N1 0.038(2) 0.037(2) 0.035(2) -0.007(2) 0.008(2) -0.010(2) N2 0.024(2) 0.029(2) 0.040(2) -0.010(2) 0.003(2) -0.007(2) N3 0.024(2) 0.026(2) 0.031(2) -0.007(2) 0.004(2) -0.005(2) N4 0.031(2) 0.028(2) 0.029(2) -0.006(2) -0.001(2) -0.003(2) N5 0.053(3) 0.037(3) 0.054(3) -0.005(2) 0.001(2) -0.023(2) N6 0.070(4) 0.032(3) 0.064(4) -0.017(3) 0.011(3) 0.005(2) N7 0.068(4) 0.039(3) 0.066(4) -0.023(3) 0.008(3) -0.018(3) N8 0.054(4) 0.104(5) 0.038(3) -0.020(4) -0.012(3) -0.017(3) N9 0.034(2) 0.028(2) 0.035(2) -0.009(2) -0.001(2) -0.001(2) N10 0.088(5) 0.037(3) 0.080(5) -0.018(3) 0.030(4) -0.003(3) N11 0.027(2) 0.023(2) 0.034(2) -0.008(2) 0.001(2) -0.005(2) N12 0.068(4) 0.034(3) 0.073(4) -0.014(3) 0.019(3) -0.017(3) N13 0.024(2) 0.024(2) 0.032(2) -0.006(2) 0.002(2) -0.007(2) N14 0.098(6) 0.037(3) 0.090(5) -0.003(3) -0.024(4) -0.025(3) C1 0.025(2) 0.027(2) 0.028(2) -0.009(2) 0.001(2) -0.006(2) C2 0.022(2) 0.024(2) 0.030(2) -0.009(2) 0.001(2) -0.006(2) C3 0.016(2) 0.023(2) 0.028(2) -0.008(2) 0.001(2) -0.005(2) C4 0.019(2) 0.025(2) 0.027(2) -0.006(2) -0.000(2) -0.007(2) C5 0.030(2) 0.023(2) 0.030(2) -0.006(2) -0.000(2) -0.006(2) C6 0.037(3) 0.024(2) 0.036(3) -0.011(2) 0.005(2) 0.001(2) C7 0.036(3) 0.022(2) 0.037(3) -0.013(2) 0.006(2) -0.009(2) C8 0.034(3) 0.052(3) 0.029(3) -0.013(2) 0.000(2) -0.008(2) C9 0.046(3) 0.035(3) 0.041(3) -0.010(2) 0.013(2) -0.003(2) C10 0.060(4) 0.032(3) 0.051(4) -0.008(3) 0.017(3) -0.006(3) C11 0.050(3) 0.029(3) 0.043(3) -0.016(2) -0.000(2) -0.004(2) C12 0.043(3) 0.033(3) 0.041(3) -0.011(2) 0.006(2) 0.003(2) C13 0.037(3) 0.032(3) 0.039(3) -0.009(2) 0.002(2) -0.002(2) C14 0.054(4) 0.029(3) 0.059(4) -0.010(3) 0.014(3) -0.001(3) C15 0.034(3) 0.031(3) 0.049(3) -0.004(2) -0.010(2) -0.013(2) C16 0.040(3) 0.036(3) 0.056(4) -0.016(2) 0.002(3) -0.018(3) C17 0.042(3) 0.024(2) 0.040(3) -0.011(2) 0.010(2) -0.006(2) C18 0.041(3) 0.026(2) 0.046(3) -0.002(2) -0.002(2) -0.005(2) C19 0.035(3) 0.027(2) 0.039(3) -0.007(2) -0.003(2) -0.005(2) C20 0.048(3) 0.029(3) 0.050(3) -0.008(2) 0.010(3) -0.009(2) C21 0.032(3) 0.029(2) 0.041(3) -0.002(2) -0.007(2) -0.009(2) C22 0.034(3) 0.028(2) 0.049(3) 0.004(2) -0.009(2) -0.011(2) C23 0.032(3) 0.024(2) 0.038(3) -0.004(2) 0.003(2) -0.008(2) C24 0.041(3) 0.035(3) 0.035(3) -0.006(2) -0.007(2) -0.009(2) C25 0.037(3) 0.024(2) 0.030(2) -0.005(2) -0.002(2) -0.003(2) C26 0.051(4) 0.030(3) 0.062(4) -0.002(3) -0.007(3) -0.019(3) #============================================================================== _computing_data_collection WinAFC _computing_cell_refinement WinAFC _computing_data_reduction CrystalStructure _computing_structure_solution SHELXS97 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure Ver. 3.00' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag W1 . C1 . 2.166(5) yes W1 . C2 . 2.158(5) yes W1 . C3 . 2.156(4) yes W1 . C4 . 2.165(5) yes W1 . C5 . 2.169(5) yes W1 . C6 . 2.173(5) yes W1 . C7 . 2.165(5) yes W1 . C8 . 2.149(5) yes Cu1 . O1 . 1.947(4) yes Cu1 . N1 . 2.489(4) yes Cu1 . N9 . 2.076(4) yes Cu2 . N2 . 1.984(4) yes Cu2 . N11 . 2.046(4) yes Cu2 . N13 . 2.023(4) yes O1 . H13 . 0.89(6) no O1 . H14 . 0.89(3) no O2 . H15 . 0.90(7) no O2 . H16 . 0.91(8) no O4 . H17 . 0.90(7) no O4 . H18 . 0.90(3) no N1 . C1 . 1.154(6) yes N2 . C2 . 1.136(6) yes N3 . C3 . 1.145(6) yes N4 . C4 . 1.139(6) yes N5 . C5 . 1.147(7) yes N6 . C6 . 1.135(7) yes N7 . C7 . 1.144(7) yes N8 . C8 . 1.137(7) yes N9 . C9 . 1.325(7) yes N9 . C13 . 1.346(7) yes N10 . C14 . 1.137(8) yes N11 . C15 . 1.324(6) yes N11 . C19 . 1.342(6) yes N12 . C20 . 1.140(8) yes N13 . C21 . 1.333(6) yes N13 . C25 . 1.336(6) yes N14 . C26 . 1.133(8) yes C9 . C10 . 1.394(8) yes C9 . H1 . 0.95 no C10 . C11 . 1.367(8) yes C10 . H2 . 0.95 no C11 . C12 . 1.375(8) yes C11 . C14 . 1.456(8) yes C12 . C13 . 1.386(7) yes C12 . H3 . 0.95 no C13 . H4 . 0.95 no C15 . C16 . 1.380(7) yes C15 . H5 . 0.95 no C16 . C17 . 1.380(8) yes C16 . H6 . 0.95 no C17 . C18 . 1.396(8) yes C17 . C20 . 1.439(7) yes C18 . C19 . 1.385(7) yes C18 . H7 . 0.95 no C19 . H8 . 0.95 no C21 . C22 . 1.387(7) yes C21 . H9 . 0.95 no C22 . C23 . 1.396(7) yes C22 . H10 . 0.95 no C23 . C24 . 1.379(7) yes C23 . C26 . 1.444(7) yes C24 . C25 . 1.390(7) yes C24 . H11 . 0.95 no C25 . H12 . 0.95 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C1 . W1 . C2 . 138.20(17) yes C1 . W1 . C3 . 73.48(17) yes C2 . W1 . C3 . 145.61(17) yes C1 . W1 . C4 . 124.61(17) yes C2 . W1 . C4 . 74.45(17) yes C3 . W1 . C4 . 74.59(17) yes C1 . W1 . C5 . 141.43(18) yes C2 . W1 . C5 . 75.72(18) yes C3 . W1 . C5 . 81.79(17) yes C4 . W1 . C5 . 74.21(17) yes C1 . W1 . C6 . 74.48(19) yes C2 . W1 . C6 . 117.41(19) yes C3 . W1 . C6 . 78.52(19) yes C4 . W1 . C6 . 139.09(19) yes C5 . W1 . C6 . 71.87(19) yes C1 . W1 . C7 . 72.89(18) yes C2 . W1 . C7 . 79.81(18) yes C3 . W1 . C7 . 105.16(18) yes C4 . W1 . C7 . 73.43(18) yes C5 . W1 . C7 . 143.54(19) yes C1 . W1 . C8 . 74.36(19) yes C2 . W1 . C8 . 70.55(19) yes C3 . W1 . C8 . 143.55(19) yes C4 . W1 . C8 . 139.61(19) yes C5 . W1 . C8 . 114.8(2) yes C6 . W1 . C7 . 144.4(2) yes C6 . W1 . C8 . 76.8(2) yes C7 . W1 . C8 . 81.1(2) yes O1 . Cu1 . N1 . 90.04(18) yes O1 . Cu1 . N9 . 88.98(17) yes N1 . Cu1 . N9 . 90.71(16) yes N2 . Cu2 . N11 . 88.82(17) yes N2 . Cu2 . N13 . 87.28(17) yes N11 . Cu2 . N13 . 171.56(17) yes Cu1 . O1 . H13 . 120.0(4) no Cu1 . O1 . H14 . 128.5(3) no H13 . O1 . H14 . 106.6(5) no H15 . O2 . H16 . 109.8(8) no H17 . O4 . H18 . 91.1(6) no Cu1 . N1 . C1 . 162.9(4) yes Cu2 . N2 . C2 . 173.5(4) yes Cu1 . N9 . C9 . 122.9(4) yes Cu1 . N9 . C13 . 118.5(4) yes C9 . N9 . C13 . 118.6(5) yes Cu2 . N11 . C15 . 118.6(3) yes Cu2 . N11 . C19 . 122.3(3) yes C15 . N11 . C19 . 119.0(4) yes Cu2 . N13 . C21 . 121.3(3) yes Cu2 . N13 . C25 . 119.5(3) yes C21 . N13 . C25 . 119.1(4) yes W1 . C1 . N1 . 177.9(4) yes W1 . C2 . N2 . 179.3(4) yes W1 . C3 . N3 . 175.2(4) yes W1 . C4 . N4 . 177.5(4) yes W1 . C5 . N5 . 177.5(5) yes W1 . C6 . N6 . 178.1(5) yes W1 . C7 . N7 . 179.2(5) yes W1 . C8 . N8 . 177.6(6) yes N9 . C9 . C10 . 122.4(5) yes N9 . C9 . H1 . 118.8(8) no C10 . C9 . H1 . 118.8(8) no C9 . C10 . C11 . 118.4(6) yes C9 . C10 . H2 . 120.8(8) no C11 . C10 . H2 . 120.8(8) no C10 . C11 . C12 . 119.8(5) yes C10 . C11 . C14 . 121.0(6) yes C12 . C11 . C14 . 119.1(5) yes C11 . C12 . C13 . 118.5(5) yes C11 . C12 . H3 . 120.7(7) no C13 . C12 . H3 . 120.7(7) no N9 . C13 . C12 . 122.0(5) yes N9 . C13 . H4 . 119.0(7) no C12 . C13 . H4 . 119.0(7) no N10 . C14 . C11 . 175.9(8) yes N11 . C15 . C16 . 122.9(5) yes N11 . C15 . H5 . 118.6(7) no C16 . C15 . H5 . 118.6(7) no C15 . C16 . C17 . 118.4(5) yes C15 . C16 . H6 . 120.8(7) no C17 . C16 . H6 . 120.8(7) no C16 . C17 . C18 . 119.5(5) yes C16 . C17 . C20 . 120.6(5) yes C18 . C17 . C20 . 120.0(5) yes C17 . C18 . C19 . 117.9(5) yes C17 . C18 . H7 . 121.0(7) no C19 . C18 . H7 . 121.0(7) no N11 . C19 . C18 . 122.3(5) yes N11 . C19 . H8 . 118.9(6) no C18 . C19 . H8 . 118.9(7) no N12 . C20 . C17 . 179.6(7) yes N13 . C21 . C22 . 122.8(5) yes N13 . C21 . H9 . 118.6(6) no C22 . C21 . H9 . 118.6(7) no C21 . C22 . C23 . 117.8(5) yes C21 . C22 . H10 . 121.1(7) no C23 . C22 . H10 . 121.1(7) no C22 . C23 . C24 . 119.6(5) yes C22 . C23 . C26 . 120.4(5) yes C24 . C23 . C26 . 119.9(5) yes C23 . C24 . C25 . 118.6(5) yes C23 . C24 . H11 . 120.7(7) no C25 . C24 . H11 . 120.7(7) no N13 . C25 . C24 . 122.1(5) yes N13 . C25 . H12 . 119.0(6) no C24 . C25 . H12 . 118.9(6) no N14 . C26 . C23 . 174.3(7) yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_site_symmetry_1 _geom_torsion_atom_site_label_2 _geom_torsion_site_symmetry_2 _geom_torsion_atom_site_label_3 _geom_torsion_site_symmetry_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag O1 . Cu1 . N1 . C1 . -16.3(3) yes N9 . Cu1 . N1 . C1 . -105.3(3) yes O1 . Cu1 . N9 . C9 . 115.3(8) yes O1 . Cu1 . N9 . C13 . -66.6(8) yes N1 . Cu1 . N9 . C9 . -154.7(8) yes N1 . Cu1 . N9 . C13 . 23.4(8) yes N11 . Cu2 . N2 . C2 . -135.2(7) yes N13 . Cu2 . N2 . C2 . 37.3(7) yes N2 . Cu2 . N11 . C15 . -47.5(8) yes N2 . Cu2 . N11 . C19 . 129.9(7) yes N13 . Cu2 . N11 . C15 . -110.0(4) yes N13 . Cu2 . N11 . C19 . 67.4(4) yes N2 . Cu2 . N13 . C21 . 70.6(8) yes N2 . Cu2 . N13 . C25 . -112.6(7) yes N11 . Cu2 . N13 . C21 . 133.1(4) yes N11 . Cu2 . N13 . C25 . -50.0(4) yes Cu1 . N1 . C1 . W1 . 23.5(1) yes Cu2 . N2 . C2 . W1 . -91.6(4) yes Cu1 . N9 . C9 . C10 . 176.3(6) yes C13 . N9 . C9 . C10 . -2(1) yes Cu1 . N9 . C13 . C12 . -176.1(5) yes C9 . N9 . C13 . C12 . 2(1) yes Cu2 . N11 . C15 . C16 . 177.1(6) yes C19 . N11 . C15 . C16 . -0(1) yes Cu2 . N11 . C19 . C18 . -176.9(5) yes C15 . N11 . C19 . C18 . 1(1) yes Cu2 . N13 . C21 . C22 . 175.9(5) yes C25 . N13 . C21 . C22 . -1(1) yes Cu2 . N13 . C25 . C24 . -174.5(5) yes C21 . N13 . C25 . C24 . 2(1) yes N9 . C9 . C10 . C11 . -0(1) yes C9 . C10 . C11 . C12 . 3(1) yes C9 . C10 . C11 . C14 . -176.0(8) yes C10 . C11 . C12 . C13 . -2(1) yes C14 . C11 . C12 . C13 . 176.2(8) yes C10 . C11 . C14 . N10 . 139(1) yes C12 . C11 . C14 . N10 . -40(1) yes C11 . C12 . C13 . N9 . 0(1) yes N11 . C15 . C16 . C17 . -0(1) yes C15 . C16 . C17 . C18 . 2(1) yes C15 . C16 . C17 . C20 . -178.4(7) yes C16 . C17 . C18 . C19 . -2(1) yes C20 . C17 . C18 . C19 . 178.6(7) yes C16 . C17 . C20 . N12 . 77(1) yes C18 . C17 . C20 . N12 . -103(1) yes C17 . C18 . C19 . N11 . 0(1) yes N13 . C21 . C22 . C23 . -1(1) yes C21 . C22 . C23 . C24 . 1(1) yes C21 . C22 . C23 . C26 . -175.4(7) yes C22 . C23 . C24 . C25 . 0(1) yes C26 . C23 . C24 . C25 . 176.7(8) yes C22 . C23 . C26 . N14 . 150.9(9) yes C24 . C23 . C26 . N14 . -25.6(10) yes C23 . C24 . C25 . N13 . -2(1) yes loop_ _geom_contact_atom_site_label_1 _geom_contact_site_symmetry_1 _geom_contact_atom_site_label_2 _geom_contact_site_symmetry_2 _geom_contact_distance _geom_contact_publ_flag Cu1 . O1 2_655 1.947(4) yes Cu1 . N1 2_655 2.489(4) yes Cu1 . N9 2_655 2.076(4) yes Cu2 . N3 1_455 1.976(4) yes Cu2 . N4 2_556 2.164(4) yes Cu2 . N10 1_465 3.188(7) yes O1 . O2 . 2.672(7) yes O1 . O3 . 2.646(7) yes O2 . O3 2_555 3.563(8) yes O2 . O4 . 2.863(7) yes O2 . N8 2_555 2.929(7) yes O2 . H13 . 1.8(1) no O3 . O4 2_555 2.762(7) yes O3 . N8 . 3.014(9) yes O3 . H14 . 1.77(6) no O4 . N6 1_545 2.855(7) yes O4 . N7 . 2.948(7) yes O4 . H15 . 2.1(2) no O4 . H17 . 0.90(7) no O4 . H18 . 0.90(3) no N7 . H17 . 2.1(2) no N8 . H16 2_555 2.1(6) no #============================================================================== # End of CIF #==============================================================================