Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_nc2-143a _database_code_CSD 159168 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(dichromato(VI)-tri(4,4-bipyridine)-diaqua-dicopper(II) ; _publ_requested_journal 'Chem. Commun.' _publ_section_title ; An unprecedented two-fold interpenetrated heterometallic 4^6^6^4^ network constructed by five-connected copper metal nodes ; _publ_contact_author ; Li Jing Department of Chemistry, Rutgers University, Camden, NJ 08102, USA ; _publ_contact_author_email jingli@crab.rutgers.edu _publ_contact_author_fax '+1(856)225-6506' _publ_contact_author_phone '+1(856)225-6160' loop_ _publ_author_name _publ_author_address 'Pan Long' ; Department of Chemistry, Rutgers University, Camden, NJ 08102, USA ; 'Ching Nancy' ; Department of Chemistry, Rutgers University, Camden, NJ 08102, USA ; 'Huang Xiaoying' ; Department of Chemistry, Rutgers University, Camden, NJ 08102, USA ; 'Li Jing' ; Department of Chemistry, Rutgers University, Camden, NJ 08102, USA ; _chemical_name_common ? _chemical_formula_moiety [Cu(4,4'-bpy)1.5Cr2O7)H2O] _chemical_formula_sum 'C15 H14 Cr2 Cu N3 O8' _chemical_formula_weight 531.83 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' 'Cr' 'Cr' 0.3209 0.6236 '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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.176(2) _cell_length_b 14.718(3) _cell_length_c 15.952(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.60(3) _cell_angle_gamma 90.00 _cell_volume 1880.4(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 5.92 _cell_measurement_theta_max 11.99 _exptl_crystal_description block _exptl_crystal_colour dark-red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.879 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1064 _exptl_absorpt_coefficient_mu 2.306 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.896 _exptl_absorpt_correction_T_max 1.000 _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 Enraf-Nonius CAD4 _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time 250 _diffrn_standards_decay_% +-5.5 _diffrn_reflns_number 3952 _diffrn_reflns_av_R_equivalents 0.0388 _diffrn_reflns_av_sigmaI/netI 0.0862 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 25.98 _reflns_number_total 3687 _reflns_number_gt 2240 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4/PC' _computing_cell_refinement 'CAD4/PC' _computing_data_reduction 'XCAD4/PC' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL-97 (Keller, 1997' _computing_publication_material 'Windows Word97' _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^)+(0.0000P)^2^+5.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3687 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1195 _refine_ls_R_factor_gt 0.0538 _refine_ls_wR_factor_ref 0.0993 _refine_ls_wR_factor_gt 0.0883 _refine_ls_goodness_of_fit_ref 1.182 _refine_ls_restrained_S_all 1.182 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu Cu 0.22008(9) 0.78418(5) 0.72133(4) 0.02683(19) Uani 1 d . . . Cr1 Cr 0.02373(14) 0.62813(7) 0.83874(7) 0.0400(3) Uani 1 d . . . Cr2 Cr -0.32456(13) 0.71817(8) 0.82728(6) 0.0360(3) Uani 1 d . . . O1 O 0.1191(5) 0.7091(3) 0.7998(3) 0.0398(11) Uani 1 d . . . O2 O -0.1925(5) 0.6346(3) 0.7976(3) 0.0518(14) Uani 1 d . . . O3 O 0.0839(7) 0.5311(3) 0.8134(5) 0.090(2) Uani 1 d . . . O4 O 0.0484(7) 0.6378(5) 0.9385(3) 0.089(2) Uani 1 d . . . O5 O -0.2561(6) 0.8161(3) 0.8072(3) 0.0538(14) Uani 1 d . . . O6 O -0.5107(5) 0.7005(3) 0.7723(3) 0.0455(12) Uani 1 d . . . O7 O -0.3211(6) 0.7107(4) 0.9270(3) 0.0540(13) Uani 1 d . . . O8 O -0.0450(5) 0.8491(3) 0.6892(3) 0.0434(12) Uani 1 d . . . H1 H -0.0436 0.9140 0.6861 0.052 Uiso 1 d R . . H2 H -0.1381 0.8179 0.7065 0.052 Uiso 1 d R . . N1 N 0.3161(6) 0.8617(3) 0.6387(3) 0.0286(12) Uani 1 d . . . N2 N 0.1560(6) 0.6846(3) 0.6349(3) 0.0284(12) Uani 1 d . . . N3 N 0.3045(6) 0.8679(3) 0.8221(3) 0.0264(12) Uani 1 d . . . C1 C 0.2385(8) 0.9324(4) 0.5972(4) 0.0346(16) Uani 1 d . . . H3 H 0.1433 0.9423 0.6090 0.042 Uiso 1 d R . . C2 C 0.3048(8) 0.9874(4) 0.5440(4) 0.0354(16) Uani 1 d . . . H4 H 0.2480 1.0424 0.5100 0.043 Uiso 1 d R . . C3 C 0.4606(8) 0.9718(4) 0.5292(4) 0.0294(14) Uani 1 d . . . C4 C 0.5435(8) 0.8964(5) 0.5717(4) 0.0465(19) Uani 1 d . . . H5 H 0.6594 0.8823 0.5654 0.056 Uiso 1 d R . . C5 C 0.4667(9) 0.8455(5) 0.6237(4) 0.0433(18) Uani 1 d . . . H6 H 0.5163 0.7880 0.6586 0.052 Uiso 1 d R . . C6 C 0.0392(10) 0.6971(4) 0.5632(4) 0.057(2) Uani 1 d . . . H7 H -0.0018 0.7555 0.5539 0.068 Uiso 1 d R . . C7 C -0.0235(9) 0.6273(4) 0.5104(4) 0.050(2) Uani 1 d . . . H8 H -0.0558 0.6416 0.4528 0.060 Uiso 1 d R . . C8 C 0.0323(7) 0.5389(4) 0.5280(4) 0.0285(15) Uani 1 d . . . C9 C 0.1527(8) 0.5269(4) 0.6024(4) 0.0325(16) Uani 1 d . . . H9 H 0.1955 0.4752 0.6191 0.039 Uiso 1 d R . . C10 C 0.2087(8) 0.6004(4) 0.6532(4) 0.0304(15) Uani 1 d . . . H10 H 0.2795 0.5925 0.7066 0.036 Uiso 1 d R . . C11 C 0.3187(9) 0.9572(4) 0.8159(4) 0.0424(19) Uani 1 d . . . H11 H 0.2498 0.9787 0.7544 0.051 Uiso 1 d R . . C12 C 0.3939(9) 1.0110(4) 0.8844(4) 0.045(2) Uani 1 d . . . H12 H 0.3850 1.0727 0.8770 0.055 Uiso 1 d R . . C13 C 0.4573(7) 0.9720(4) 0.9632(3) 0.0253(14) Uani 1 d . . . C14 C 0.4372(8) 0.8792(4) 0.9690(4) 0.0373(17) Uani 1 d . . . H13 H 0.4708 0.8462 1.0199 0.045 Uiso 1 d R . . C15 C 0.3597(8) 0.8306(4) 0.8993(4) 0.0349(17) Uani 1 d . . . H14 H 0.3384 0.7687 0.9050 0.042 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 Cu 0.0356(4) 0.0191(4) 0.0224(4) -0.0057(4) -0.0023(3) -0.0077(4) Cr1 0.0459(7) 0.0252(6) 0.0506(7) 0.0077(5) 0.0137(6) 0.0018(6) Cr2 0.0358(6) 0.0340(6) 0.0350(6) -0.0003(5) -0.0004(5) -0.0078(6) O1 0.047(3) 0.030(2) 0.039(3) -0.002(2) 0.002(2) -0.015(2) O2 0.032(3) 0.049(3) 0.074(4) -0.022(3) 0.010(3) -0.009(3) O3 0.081(4) 0.025(3) 0.179(7) -0.002(4) 0.063(5) 0.001(3) O4 0.084(4) 0.141(6) 0.046(3) 0.038(4) 0.021(3) 0.052(4) O5 0.066(4) 0.040(3) 0.050(3) -0.001(2) 0.001(3) -0.021(3) O6 0.036(3) 0.041(3) 0.053(3) -0.005(2) -0.006(2) -0.011(2) O7 0.053(3) 0.068(3) 0.040(3) 0.007(3) 0.008(2) 0.010(3) O8 0.037(3) 0.027(2) 0.062(3) 0.008(2) 0.003(2) -0.001(2) N1 0.033(3) 0.023(3) 0.027(3) -0.006(2) -0.001(2) 0.001(3) N2 0.039(3) 0.017(3) 0.026(3) -0.005(2) -0.002(2) -0.004(2) N3 0.034(3) 0.017(3) 0.024(3) -0.004(2) -0.003(2) -0.004(2) C1 0.037(4) 0.033(4) 0.035(4) -0.001(3) 0.009(3) -0.001(3) C2 0.039(4) 0.027(4) 0.037(4) 0.006(3) 0.001(3) 0.005(3) C3 0.033(4) 0.031(3) 0.021(3) -0.005(3) 0.000(3) 0.000(3) C4 0.031(4) 0.065(5) 0.045(4) 0.015(4) 0.009(3) 0.010(4) C5 0.040(4) 0.045(4) 0.045(4) 0.013(4) 0.010(4) 0.006(4) C6 0.086(6) 0.020(4) 0.044(4) -0.008(3) -0.035(4) 0.008(4) C7 0.077(5) 0.023(3) 0.033(4) -0.004(3) -0.030(4) 0.003(4) C8 0.032(4) 0.018(3) 0.029(3) -0.005(3) -0.006(3) 0.000(3) C9 0.041(4) 0.022(3) 0.027(3) -0.001(3) -0.012(3) -0.003(3) C10 0.034(4) 0.026(3) 0.025(3) -0.006(3) -0.007(3) -0.002(3) C11 0.065(5) 0.026(4) 0.026(3) -0.006(3) -0.016(3) -0.003(4) C12 0.079(6) 0.019(3) 0.027(4) -0.007(3) -0.017(4) 0.000(4) C13 0.035(4) 0.021(3) 0.018(3) -0.006(3) 0.000(3) -0.003(3) C14 0.060(5) 0.020(3) 0.024(3) -0.001(3) -0.007(3) -0.007(3) C15 0.057(5) 0.021(3) 0.024(3) -0.001(3) -0.001(3) -0.011(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 Cu O1 1.972(4) . ? Cu N2 2.009(5) . ? Cu N1 2.019(5) . ? Cu N3 2.033(4) . ? Cu O8 2.330(4) . ? Cu O6 2.511(5) 1_655 ? Cu Cr1 3.5453(14) . ? Cu Cr2 5.1629(18) . ? Cu Cu 11.071(2) 3_566 ? Cu Cu 11.135(3) 3_677 ? Cu Cu 11.143(3) 3_676 ? Cr1 O4 1.569(5) . ? Cr1 O3 1.589(5) . ? Cr1 O1 1.615(4) . ? Cr1 O2 1.760(4) . ? Cr1 Cr2 3.1128(17) . ? Cr2 O7 1.589(4) . ? Cr2 O5 1.602(5) . ? Cr2 O6 1.617(4) . ? Cr2 O2 1.764(5) . ? O6 Cu 2.511(4) 1_455 ? O8 H1 0.9558 . ? O8 H2 0.9757 . ? N1 C5 1.321(8) . ? N1 C1 1.324(7) . ? N2 C10 1.325(7) . ? N2 C6 1.347(7) . ? N3 C11 1.325(7) . ? N3 C15 1.341(7) . ? C1 C2 1.362(8) . ? C1 H3 0.8486 . ? C2 C3 1.360(8) . ? C2 H4 1.0311 . ? C3 C4 1.402(8) . ? C3 C3 1.488(12) 3_676 ? C4 C5 1.361(9) . ? C4 H5 0.9952 . ? C5 H6 1.0486 . ? C6 C7 1.361(8) . ? C6 H7 0.9237 . ? C7 C8 1.388(8) . ? C7 H8 0.9274 . ? C8 C9 1.392(7) . ? C8 C8 1.484(10) 3_566 ? C9 C10 1.374(7) . ? C9 H9 0.8580 . ? C10 H10 0.9354 . ? C11 C12 1.389(8) . ? C11 H11 1.0771 . ? C12 C13 1.384(8) . ? C12 H12 0.9168 . ? C13 C14 1.381(8) . ? C13 C13 1.488(10) 3_677 ? C14 C15 1.366(8) . ? C14 H13 0.9382 . ? C15 H14 0.9344 . ? 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 O1 Cu N2 86.69(19) . . ? O1 Cu N1 178.17(19) . . ? N2 Cu N1 92.65(19) . . ? O1 Cu N3 87.50(18) . . ? N2 Cu N3 170.22(19) . . ? N1 Cu N3 93.39(19) . . ? O1 Cu O8 83.08(17) . . ? N2 Cu O8 92.62(18) . . ? N1 Cu O8 95.24(18) . . ? N3 Cu O8 94.48(17) . . ? O1 Cu O6 88.36(16) . 1_655 ? N2 Cu O6 87.41(17) . 1_655 ? N1 Cu O6 93.32(18) . 1_655 ? N3 Cu O6 84.57(17) . 1_655 ? O8 Cu O6 171.43(15) . 1_655 ? O1 Cu Cr1 7.85(12) . . ? N2 Cu Cr1 78.85(14) . . ? N1 Cu Cr1 171.25(13) . . ? N3 Cu Cr1 95.32(14) . . ? O8 Cu Cr1 83.22(11) . . ? O6 Cu Cr1 88.38(11) 1_655 . ? O1 Cu Cr2 35.67(13) . . ? N2 Cu Cr2 87.96(15) . . ? N1 Cu Cr2 142.63(15) . . ? N3 Cu Cr2 91.90(14) . . ? O8 Cu Cr2 47.44(11) . . ? O6 Cu Cr2 124.02(11) 1_655 . ? Cr1 Cu Cr2 36.22(2) . . ? O1 Cu Cu 81.81(12) . 3_566 ? N2 Cu Cu 5.26(14) . 3_566 ? N1 Cu Cu 97.46(13) . 3_566 ? N3 Cu Cu 167.81(13) . 3_566 ? O8 Cu Cu 90.05(11) . 3_566 ? O6 Cu Cu 89.26(10) 1_655 3_566 ? Cr1 Cu Cu 73.96(3) . 3_566 ? Cr2 Cu Cu 82.85(2) . 3_566 ? O1 Cu Cu 88.29(12) . 3_677 ? N2 Cu Cu 166.69(14) . 3_677 ? N1 Cu Cu 92.72(13) . 3_677 ? N3 Cu Cu 4.53(14) . 3_677 ? O8 Cu Cu 99.00(11) . 3_677 ? O6 Cu Cu 80.13(10) 1_655 3_677 ? Cr1 Cu Cu 96.02(3) . 3_677 ? Cr2 Cu Cu 95.11(3) . 3_677 ? Cu Cu Cu 165.709(15) 3_566 3_677 ? O1 Cu Cu 179.27(13) . 3_676 ? N2 Cu Cu 93.71(14) . 3_676 ? N1 Cu Cu 1.52(13) . 3_676 ? N3 Cu Cu 92.19(14) . 3_676 ? O8 Cu Cu 96.28(11) . 3_676 ? O6 Cu Cu 92.27(11) 1_655 3_676 ? Cr1 Cu Cu 172.49(3) . 3_676 ? Cr2 Cu Cu 143.70(2) . 3_676 ? Cu Cu Cu 98.559(18) 3_566 3_676 ? Cu Cu Cu 91.457(18) 3_677 3_676 ? O4 Cr1 O3 110.9(4) . . ? O4 Cr1 O1 110.5(3) . . ? O3 Cr1 O1 111.6(3) . . ? O4 Cr1 O2 106.7(3) . . ? O3 Cr1 O2 107.0(3) . . ? O1 Cr1 O2 110.1(2) . . ? O4 Cr1 Cr2 87.2(2) . . ? O3 Cr1 Cr2 133.9(2) . . ? O1 Cr1 Cr2 99.78(17) . . ? O2 Cr1 Cr2 27.97(15) . . ? O4 Cr1 Cu 119.8(3) . . ? O3 Cr1 Cu 104.6(2) . . ? O1 Cr1 Cu 9.60(15) . . ? O2 Cr1 Cu 107.20(17) . . ? Cr2 Cr1 Cu 101.49(4) . . ? O7 Cr2 O5 109.0(3) . . ? O7 Cr2 O6 110.9(3) . . ? O5 Cr2 O6 111.4(3) . . ? O7 Cr2 O2 109.4(3) . . ? O5 Cr2 O2 108.5(3) . . ? O6 Cr2 O2 107.6(2) . . ? O7 Cr2 Cr1 94.58(18) . . ? O5 Cr2 Cr1 92.44(19) . . ? O6 Cr2 Cr1 135.48(17) . . ? O2 Cr2 Cr1 27.91(14) . . ? O7 Cr2 Cu 119.85(18) . . ? O5 Cr2 Cu 53.57(19) . . ? O6 Cr2 Cu 129.19(17) . . ? O2 Cr2 Cu 55.14(16) . . ? Cr1 Cr2 Cu 42.29(3) . . ? Cr1 O1 Cu 162.6(3) . . ? Cr1 O2 Cr2 124.1(3) . . ? Cr2 O6 Cu 139.9(2) . 1_455 ? Cu O8 H1 113.6 . . ? Cu O8 H2 119.2 . . ? H1 O8 H2 120.2 . . ? C5 N1 C1 115.0(6) . . ? C5 N1 Cu 121.0(4) . . ? C1 N1 Cu 124.0(4) . . ? C10 N2 C6 117.3(5) . . ? C10 N2 Cu 120.2(4) . . ? C6 N2 Cu 121.7(4) . . ? C11 N3 C15 117.1(5) . . ? C11 N3 Cu 124.3(4) . . ? C15 N3 Cu 118.4(4) . . ? N1 C1 C2 124.5(6) . . ? N1 C1 H3 113.1 . . ? C2 C1 H3 122.3 . . ? C3 C2 C1 120.8(6) . . ? C3 C2 H4 112.3 . . ? C1 C2 H4 126.9 . . ? C2 C3 C4 115.3(6) . . ? C2 C3 C3 123.6(7) . 3_676 ? C4 C3 C3 121.1(7) . 3_676 ? C5 C4 C3 119.5(6) . . ? C5 C4 H5 120.9 . . ? C3 C4 H5 119.6 . . ? N1 C5 C4 124.8(7) . . ? N1 C5 H6 109.0 . . ? C4 C5 H6 126.2 . . ? N2 C6 C7 122.5(6) . . ? N2 C6 H7 115.8 . . ? C7 C6 H7 121.6 . . ? C6 C7 C8 120.9(6) . . ? C6 C7 H8 116.0 . . ? C8 C7 H8 115.4 . . ? C7 C8 C9 116.0(5) . . ? C7 C8 C8 122.6(6) . 3_566 ? C9 C8 C8 121.4(7) . 3_566 ? C10 C9 C8 119.8(6) . . ? C10 C9 H9 116.6 . . ? C8 C9 H9 123.6 . . ? N2 C10 C9 123.4(5) . . ? N2 C10 H10 115.5 . . ? C9 C10 H10 120.8 . . ? N3 C11 C12 122.6(6) . . ? N3 C11 H11 108.7 . . ? C12 C11 H11 128.1 . . ? C13 C12 C11 120.2(6) . . ? C13 C12 H12 122.3 . . ? C11 C12 H12 116.9 . . ? C14 C13 C12 116.3(5) . . ? C14 C13 C13 122.5(7) . 3_677 ? C12 C13 C13 121.1(6) . 3_677 ? C15 C14 C13 120.4(6) . . ? C15 C14 H13 116.1 . . ? C13 C14 H13 123.5 . . ? N3 C15 C14 123.2(5) . . ? N3 C15 H14 117.0 . . ? C14 C15 H14 119.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Cu Cr1 O4 -12.7(10) . . . . ? N2 Cu Cr1 O4 164.7(3) . . . . ? N1 Cu Cr1 O4 178.4(10) . . . . ? N3 Cu Cr1 O4 -7.4(3) . . . . ? O8 Cu Cr1 O4 -101.3(3) . . . . ? O6 Cu Cr1 O4 77.0(3) 1_655 . . . ? Cr2 Cu Cr1 O4 -93.3(2) . . . . ? Cu Cu Cr1 O4 166.7(2) 3_566 . . . ? Cu Cu Cr1 O4 -2.9(2) 3_677 . . . ? Cu Cu Cr1 O4 172.1(3) 3_676 . . . ? O1 Cu Cr1 O3 -137.7(10) . . . . ? N2 Cu Cr1 O3 39.7(3) . . . . ? N1 Cu Cr1 O3 53.4(10) . . . . ? N3 Cu Cr1 O3 -132.4(3) . . . . ? O8 Cu Cr1 O3 133.7(3) . . . . ? O6 Cu Cr1 O3 -48.0(3) 1_655 . . . ? Cr2 Cu Cr1 O3 141.7(3) . . . . ? Cu Cu Cr1 O3 41.7(3) 3_566 . . . ? Cu Cu Cr1 O3 -127.9(3) 3_677 . . . ? Cu Cu Cr1 O3 47.2(4) 3_676 . . . ? N2 Cu Cr1 O1 177.4(10) . . . . ? N1 Cu Cr1 O1 -168.9(13) . . . . ? N3 Cu Cr1 O1 5.3(9) . . . . ? O8 Cu Cr1 O1 -88.6(9) . . . . ? O6 Cu Cr1 O1 89.7(9) 1_655 . . . ? Cr2 Cu Cr1 O1 -80.6(9) . . . . ? Cu Cu Cr1 O1 179.4(9) 3_566 . . . ? Cu Cu Cr1 O1 9.8(9) 3_677 . . . ? Cu Cu Cr1 O1 -175.1(10) 3_676 . . . ? O1 Cu Cr1 O2 108.9(10) . . . . ? N2 Cu Cr1 O2 -73.7(2) . . . . ? N1 Cu Cr1 O2 -60.0(10) . . . . ? N3 Cu Cr1 O2 114.2(2) . . . . ? O8 Cu Cr1 O2 20.34(19) . . . . ? O6 Cu Cr1 O2 -161.37(19) 1_655 . . . ? Cr2 Cu Cr1 O2 28.30(16) . . . . ? Cu Cu Cr1 O2 -71.67(16) 3_566 . . . ? Cu Cu Cr1 O2 118.73(16) 3_677 . . . ? Cu Cu Cr1 O2 -66.2(3) 3_676 . . . ? O1 Cu Cr1 Cr2 80.6(9) . . . . ? N2 Cu Cr1 Cr2 -101.99(15) . . . . ? N1 Cu Cr1 Cr2 -88.3(10) . . . . ? N3 Cu Cr1 Cr2 85.94(14) . . . . ? O8 Cu Cr1 Cr2 -7.96(11) . . . . ? O6 Cu Cr1 Cr2 170.34(10) 1_655 . . . ? Cu Cu Cr1 Cr2 -99.97(4) 3_566 . . . ? Cu Cu Cr1 Cr2 90.44(4) 3_677 . . . ? Cu Cu Cr1 Cr2 -94.5(2) 3_676 . . . ? O4 Cr1 Cr2 O7 -11.0(3) . . . . ? O3 Cr1 Cr2 O7 105.6(4) . . . . ? O1 Cr1 Cr2 O7 -121.2(3) . . . . ? O2 Cr1 Cr2 O7 124.1(4) . . . . ? Cu Cr1 Cr2 O7 -130.8(2) . . . . ? O4 Cr1 Cr2 O5 98.3(3) . . . . ? O3 Cr1 Cr2 O5 -145.1(4) . . . . ? O1 Cr1 Cr2 O5 -11.9(2) . . . . ? O2 Cr1 Cr2 O5 -126.6(4) . . . . ? Cu Cr1 Cr2 O5 -21.54(17) . . . . ? O4 Cr1 Cr2 O6 -137.3(4) . . . . ? O3 Cr1 Cr2 O6 -20.7(4) . . . . ? O1 Cr1 Cr2 O6 112.4(3) . . . . ? O2 Cr1 Cr2 O6 -2.3(4) . . . . ? Cu Cr1 Cr2 O6 102.8(2) . . . . ? O4 Cr1 Cr2 O2 -135.0(4) . . . . ? O3 Cr1 Cr2 O2 -18.4(5) . . . . ? O1 Cr1 Cr2 O2 114.7(4) . . . . ? Cu Cr1 Cr2 O2 105.1(4) . . . . ? O4 Cr1 Cr2 Cu 119.9(3) . . . . ? O3 Cr1 Cr2 Cu -123.5(4) . . . . ? O1 Cr1 Cr2 Cu 9.61(15) . . . . ? O2 Cr1 Cr2 Cu -105.1(4) . . . . ? O1 Cu Cr2 O7 47.0(3) . . . . ? N2 Cu Cr2 O7 134.2(3) . . . . ? N1 Cu Cr2 O7 -134.1(3) . . . . ? N3 Cu Cr2 O7 -36.0(3) . . . . ? O8 Cu Cr2 O7 -130.4(3) . . . . ? O6 Cu Cr2 O7 48.7(3) 1_655 . . . ? Cr1 Cu Cr2 O7 60.4(2) . . . . ? Cu Cu Cr2 O7 132.9(2) 3_566 . . . ? Cu Cu Cr2 O7 -32.8(2) 3_677 . . . ? Cu Cu Cr2 O7 -132.3(2) 3_676 . . . ? O1 Cu Cr2 O5 139.5(3) . . . . ? N2 Cu Cr2 O5 -133.3(3) . . . . ? N1 Cu Cr2 O5 -41.6(3) . . . . ? N3 Cu Cr2 O5 56.5(2) . . . . ? O8 Cu Cr2 O5 -37.9(3) . . . . ? O6 Cu Cr2 O5 141.2(2) 1_655 . . . ? Cr1 Cu Cr2 O5 152.9(2) . . . . ? Cu Cu Cr2 O5 -134.6(2) 3_566 . . . ? Cu Cu Cr2 O5 59.7(2) 3_677 . . . ? Cu Cu Cr2 O5 -39.8(2) 3_676 . . . ? O1 Cu Cr2 O6 -131.4(3) . . . . ? N2 Cu Cr2 O6 -44.3(3) . . . . ? N1 Cu Cr2 O6 47.4(3) . . . . ? N3 Cu Cr2 O6 145.5(3) . . . . ? O8 Cu Cr2 O6 51.2(3) . . . . ? O6 Cu Cr2 O6 -129.8(3) 1_655 . . . ? Cr1 Cu Cr2 O6 -118.1(2) . . . . ? Cu Cu Cr2 O6 -45.5(2) 3_566 . . . ? Cu Cu Cr2 O6 148.7(2) 3_677 . . . ? Cu Cu Cr2 O6 49.2(2) 3_676 . . . ? O1 Cu Cr2 O2 -46.8(3) . . . . ? N2 Cu Cr2 O2 40.4(2) . . . . ? N1 Cu Cr2 O2 132.1(3) . . . . ? N3 Cu Cr2 O2 -129.8(2) . . . . ? O8 Cu Cr2 O2 135.8(2) . . . . ? O6 Cu Cr2 O2 -45.1(2) 1_655 . . . ? Cr1 Cu Cr2 O2 -33.42(19) . . . . ? Cu Cu Cr2 O2 39.13(19) 3_566 . . . ? Cu Cu Cr2 O2 -126.64(19) 3_677 . . . ? Cu Cu Cr2 O2 133.87(19) 3_676 . . . ? O1 Cu Cr2 Cr1 -13.4(2) . . . . ? N2 Cu Cr2 Cr1 73.81(14) . . . . ? N1 Cu Cr2 Cr1 165.5(2) . . . . ? N3 Cu Cr2 Cr1 -96.41(14) . . . . ? O8 Cu Cr2 Cr1 169.25(15) . . . . ? O6 Cu Cr2 Cr1 -11.68(13) 1_655 . . . ? Cu Cu Cr2 Cr1 72.55(4) 3_566 . . . ? Cu Cu Cr2 Cr1 -93.22(4) 3_677 . . . ? Cu Cu Cr2 Cr1 167.29(4) 3_676 . . . ? O4 Cr1 O1 Cu 168.2(9) . . . . ? O3 Cr1 O1 Cu 44.5(10) . . . . ? O2 Cr1 O1 Cu -74.2(10) . . . . ? Cr2 Cr1 O1 Cu -101.2(9) . . . . ? N2 Cu O1 Cr1 -2.6(9) . . . . ? N1 Cu O1 Cr1 66(6) . . . . ? N3 Cu O1 Cr1 -174.7(9) . . . . ? O8 Cu O1 Cr1 90.5(9) . . . . ? O6 Cu O1 Cr1 -90.1(9) 1_655 . . . ? Cr2 Cu O1 Cr1 88.6(9) . . . . ? Cu Cu O1 Cr1 -0.6(9) 3_566 . . . ? Cu Cu O1 Cr1 -170.2(9) 3_677 . . . ? Cu Cu O1 Cr1 120(9) 3_676 . . . ? O4 Cr1 O2 Cr2 47.5(4) . . . . ? O3 Cr1 O2 Cr2 166.2(4) . . . . ? O1 Cr1 O2 Cr2 -72.4(4) . . . . ? Cu Cr1 O2 Cr2 -82.1(3) . . . . ? O7 Cr2 O2 Cr1 -61.1(4) . . . . ? O5 Cr2 O2 Cr1 57.7(4) . . . . ? O6 Cr2 O2 Cr1 178.3(3) . . . . ? Cu Cr2 O2 Cr1 52.4(3) . . . . ? O7 Cr2 O6 Cu 82.6(4) . . . 1_455 ? O5 Cr2 O6 Cu -39.0(5) . . . 1_455 ? O2 Cr2 O6 Cu -157.8(4) . . . 1_455 ? Cr1 Cr2 O6 Cu -156.6(2) . . . 1_455 ? Cu Cr2 O6 Cu -98.8(4) . . . 1_455 ? O1 Cu N1 C5 -148(6) . . . . ? N2 Cu N1 C5 -79.5(5) . . . . ? N3 Cu N1 C5 92.8(5) . . . . ? O8 Cu N1 C5 -172.4(5) . . . . ? O6 Cu N1 C5 8.0(5) 1_655 . . . ? Cr1 Cu N1 C5 -93.0(11) . . . . ? Cr2 Cu N1 C5 -169.6(4) . . . . ? Cu Cu N1 C5 -81.7(5) 3_566 . . . ? Cu Cu N1 C5 88.3(5) 3_677 . . . ? Cu Cu N1 C5 55(5) 3_676 . . . ? O1 Cu N1 C1 33(6) . . . . ? N2 Cu N1 C1 102.0(5) . . . . ? N3 Cu N1 C1 -85.7(5) . . . . ? O8 Cu N1 C1 9.1(5) . . . . ? O6 Cu N1 C1 -170.4(5) 1_655 . . . ? Cr1 Cu N1 C1 88.5(11) . . . . ? Cr2 Cu N1 C1 11.9(6) . . . . ? Cu Cu N1 C1 99.9(5) 3_566 . . . ? Cu Cu N1 C1 -90.2(5) 3_677 . . . ? Cu Cu N1 C1 -124(5) 3_676 . . . ? O1 Cu N2 C10 -56.5(5) . . . . ? N1 Cu N2 C10 125.2(5) . . . . ? N3 Cu N2 C10 -2.9(15) . . . . ? O8 Cu N2 C10 -139.5(5) . . . . ? O6 Cu N2 C10 32.0(5) 1_655 . . . ? Cr1 Cu N2 C10 -56.9(5) . . . . ? Cr2 Cu N2 C10 -92.2(5) . . . . ? Cu Cu N2 C10 -78.5(15) 3_566 . . . ? Cu Cu N2 C10 11.5(10) 3_677 . . . ? Cu Cu N2 C10 124.1(5) 3_676 . . . ? O1 Cu N2 C6 112.9(6) . . . . ? N1 Cu N2 C6 -65.4(6) . . . . ? N3 Cu N2 C6 166.5(11) . . . . ? O8 Cu N2 C6 30.0(6) . . . . ? O6 Cu N2 C6 -158.6(6) 1_655 . . . ? Cr1 Cu N2 C6 112.5(6) . . . . ? Cr2 Cu N2 C6 77.2(6) . . . . ? Cu Cu N2 C6 90.9(16) 3_566 . . . ? Cu Cu N2 C6 -179.1(5) 3_677 . . . ? Cu Cu N2 C6 -66.5(6) 3_676 . . . ? O1 Cu N3 C11 -145.7(6) . . . . ? N2 Cu N3 C11 160.7(11) . . . . ? N1 Cu N3 C11 32.7(6) . . . . ? O8 Cu N3 C11 -62.9(6) . . . . ? O6 Cu N3 C11 125.7(6) 1_655 . . . ? Cr1 Cu N3 C11 -146.5(5) . . . . ? Cr2 Cu N3 C11 -110.3(5) . . . . ? Cu Cu N3 C11 -174.4(5) 3_566 . . . ? Cu Cu N3 C11 114.3(19) 3_677 . . . ? Cu Cu N3 C11 33.6(5) 3_676 . . . ? O1 Cu N3 C15 38.7(5) . . . . ? N2 Cu N3 C15 -14.8(15) . . . . ? N1 Cu N3 C15 -142.9(5) . . . . ? O8 Cu N3 C15 121.6(5) . . . . ? O6 Cu N3 C15 -49.9(5) 1_655 . . . ? Cr1 Cu N3 C15 38.0(5) . . . . ? Cr2 Cu N3 C15 74.1(5) . . . . ? Cu Cu N3 C15 10.0(10) 3_566 . . . ? Cu Cu N3 C15 -61.2(16) 3_677 . . . ? Cu Cu N3 C15 -141.9(5) 3_676 . . . ? C5 N1 C1 C2 -1.3(9) . . . . ? Cu N1 C1 C2 177.3(5) . . . . ? N1 C1 C2 C3 0.4(10) . . . . ? C1 C2 C3 C4 0.5(9) . . . . ? C1 C2 C3 C3 179.0(7) . . . 3_676 ? C2 C3 C4 C5 -0.4(10) . . . . ? C3 C3 C4 C5 -179.0(7) 3_676 . . . ? C1 N1 C5 C4 1.3(10) . . . . ? Cu N1 C5 C4 -177.3(6) . . . . ? C3 C4 C5 N1 -0.5(11) . . . . ? C10 N2 C6 C7 -0.3(12) . . . . ? Cu N2 C6 C7 -170.0(6) . . . . ? N2 C6 C7 C8 -0.7(13) . . . . ? C6 C7 C8 C9 0.7(11) . . . . ? C6 C7 C8 C8 -179.7(8) . . . 3_566 ? C7 C8 C9 C10 0.1(10) . . . . ? C8 C8 C9 C10 -179.5(7) 3_566 . . . ? C6 N2 C10 C9 1.2(10) . . . . ? Cu N2 C10 C9 171.1(5) . . . . ? C8 C9 C10 N2 -1.1(10) . . . . ? C15 N3 C11 C12 2.9(10) . . . . ? Cu N3 C11 C12 -172.7(5) . . . . ? N3 C11 C12 C13 -0.2(12) . . . . ? C11 C12 C13 C14 -1.5(10) . . . . ? C11 C12 C13 C13 178.2(7) . . . 3_677 ? C12 C13 C14 C15 0.5(10) . . . . ? C13 C13 C14 C15 -179.1(7) 3_677 . . . ? C11 N3 C15 C14 -3.9(10) . . . . ? Cu N3 C15 C14 171.9(5) . . . . ? C13 C14 C15 N3 2.3(11) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O8 H1 O3 0.96 1.76 2.696(6) 167.5 2_556 O8 H2 O5 0.98 2.03 2.839(7) 138.6 . _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 25.98 _diffrn_measured_fraction_theta_full 0.959 _refine_diff_density_max 0.658 _refine_diff_density_min -0.595 _refine_diff_density_rms 0.115