# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1694 data_cr4 # paper complex no. 5 _publ_requested_journal 'test' _audit_creation_method CRYSTALS _chemical_name_systematic ; bis(acetonitrile)tris(mu-pyridazine)dicopper(I) acetonitrile adduct (1/0.5) ; _chemical_name_common ? _chemical_formula_moiety 'C18 H21 Cu2 N9 F8 B2' _chemical_formula_structural '[{Cu(C2H3N)}2(mu-C4H4N2)3][BF4]2.C2H3N' _chemical_formula_analytical 'C18 H21 B2 Cu2 F8 N9' _chemical_formula_sum 'C18 H21 B2 Cu2 F8 N9' _chemical_formula_weight 664.13 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'Cu ' 0.2630 1.2660 13.3380 3.5828 7.1676 0.2470 5.6158 11.3966 1.6735 64.8126 1.1910 'International_Tables_Vol_IV_Table_2.2B' 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' 'B ' 0.0000 0.0010 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 'International_Tables_Vol_IV_Table_2.2B' 'F ' 0.0140 0.0100 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International_Tables_Vol_IV_Table_2.2B' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'C 1 2/c 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' 'x+1/2,y+1/2,z' '-x+1/2,-y+1/2,-z' '-x,y,-z+1/2' 'x,-y,z+1/2' '-x+1/2,y+1/2,-z+1/2' 'x+1/2,-y+1/2,z+1/2' _cell_length_a 12.726(1) _cell_angle_alpha 90 _cell_length_b 41.705(4) _cell_angle_beta 113.57(2) _cell_length_c 12.571(1) _cell_angle_gamma 90 _cell_volume 6115(1) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 12 _cell_measurement_theta_min 8.1 _cell_measurement_theta_max 14.8 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_min 0.05 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_max 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.443 _exptl_crystal_density_method ? _exptl_crystal_F_000 2656 _exptl_absorpt_coefficient_mu 1.463 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 ; Hilger and Watts Y290 4-circle-diffractometer ; _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 4.5 _diffrn_reflns_number 4158 _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 49 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 22.5 _reflns_number_total 4158 _reflns_number_observed 1463 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ; Crystals Users Guide (D.J.Watkin et al, 1985) ; _computing_structure_refinement ; Crystals Users Guide (D.J.Watkin et al 1985) ; _computing_molecular_graphics 'CAMERON (Watkin et al, 1996)' _computing_publication_material 'CRYSTALS Issue 10 (Watkin et al, 1996)' _refine_special_details ; Refinement on F for all reflections with intensity >2sigma(I). Three crystallographically independent tetrafluoroborate anions. Two located on two-fold axes of symmetry, one of which is disordered. Disorder modelled by four fluorine atoms each with 50% occupancy. All hydrogen atoms were placed and allowed to ride on their parent atom. Intensity data so weak that only copper, nitrogen and fluorine atoms could be refined with anisotropic displacement parameters. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme ; Three parameter Chebychev W = [weight] * [1-(deltaF/6*sigmaF)**2]**2 using parameters 3.18 1.47 2.04 ; _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1463 _refine_ls_number_parameters 256 _refine_ls_number_restraints 0 _refine_ls_R_factor_obs 0.0946 _refine_ls_wR_factor_obs 0.1008 _refine_ls_goodness_of_fit_obs 1.0952 _refine_ls_shift/esd_max 0.036673 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 _atom_site_occupancy _atom_site_thermal_displace_type CU1 0.2759(2) 0.34980(6) 0.0078(2) 0.0936 1.0000 Uani CU2 0.3459(2) 0.41254(6) -0.0681(3) 0.0967 1.0000 Uani N11 0.448(1) 0.3559(4) 0.064(1) 0.0858 1.0000 Uani N12 0.478(1) 0.3841(5) 0.030(1) 0.0862 1.0000 Uani N21 0.223(1) 0.3561(5) -0.166(2) 0.0947 1.0000 Uani N22 0.258(1) 0.3826(4) -0.200(2) 0.0898 1.0000 Uani N31 0.212(1) 0.3899(4) 0.054(1) 0.0853 1.0000 Uani N32 0.244(1) 0.4179(4) 0.022(1) 0.0824 1.0000 Uani N41 0.222(2) 0.3103(4) 0.050(2) 0.0936 1.0000 Uani N51 0.377(1) 0.4533(5) -0.115(2) 0.1132 1.0000 Uani C13 0.586(2) 0.3905(6) 0.052(2) 0.103(7) 1.0000 Uiso C14 0.672(2) 0.3694(5) 0.112(2) 0.104(7) 1.0000 Uiso C15 0.647(2) 0.3419(5) 0.143(2) 0.100(7) 1.0000 Uiso C16 0.530(2) 0.3362(6) 0.118(2) 0.092(7) 1.0000 Uiso C23 0.224(2) 0.3897(6) -0.310(2) 0.090(7) 1.0000 Uiso C24 0.156(2) 0.3679(5) -0.398(2) 0.101(7) 1.0000 Uiso C25 0.124(2) 0.3414(6) -0.358(2) 0.118(8) 1.0000 Uiso C26 0.159(2) 0.3364(6) -0.245(2) 0.099(8) 1.0000 Uiso C33 0.206(2) 0.4440(7) 0.040(2) 0.109(8) 1.0000 Uiso C34 0.125(2) 0.4464(6) 0.089(2) 0.111(8) 1.0000 Uiso C35 0.087(2) 0.4198(6) 0.117(2) 0.119(8) 1.0000 Uiso C36 0.136(2) 0.3908(5) 0.099(2) 0.083(6) 1.0000 Uiso C41 0.190(2) 0.2884(7) 0.072(2) 0.093(8) 1.0000 Uiso C42 0.145(2) 0.2590(6) 0.110(2) 0.113(8) 1.0000 Uiso C51 0.385(2) 0.4775(7) -0.145(2) 0.113(9) 1.0000 Uiso C52 0.395(3) 0.5113(7) -0.186(3) 0.16(1) 1.0000 Uiso B1 0.211(2) 0.536(1) -0.011(2) 0.14(1) 1.0000 Uiso F11 0.206(2) 0.5678(4) -0.035(2) 0.2315 1.0000 Uani F12 0.169(3) 0.5213(6) -0.104(2) 0.2949 1.0000 Uani F13 0.160(2) 0.5287(5) 0.050(2) 0.2464 1.0000 Uani F14 0.319(2) 0.5263(7) 0.038(2) 0.2510 1.0000 Uani B2 0.0000 0.330(1) 0.2500 0.08(1) 1.0000 Uiso F21 -0.085(6) 0.3184(9) 0.272(8) 0.1337 0.5000 Uani F22 0.036(2) 0.3609(5) 0.294(3) 0.1092 0.5000 Uani F23 0.093(4) 0.327(4) 0.32(1) 0.2952 0.5000 Uani F24 0.01(1) 0.327(2) 0.352(7) 0.2689 0.5000 Uani B3 0.5000 0.249(1) 0.2500 0.17(3) 1.0000 Uiso F31 0.460(3) 0.2297(5) 0.169(2) 0.3163 1.0000 Uani F32 0.430(2) 0.2654(7) 0.254(4) 0.4030 1.0000 Uani H13 0.608(2) 0.4108(6) 0.023(2) 0.0500 1.0000 Uiso H14 0.755(2) 0.3750(5) 0.135(2) 0.0500 1.0000 Uiso H15 0.706(2) 0.3252(5) 0.181(2) 0.0500 1.0000 Uiso H16 0.509(2) 0.3152(6) 0.142(2) 0.0500 1.0000 Uiso H23 0.252(2) 0.4099(6) -0.333(2) 0.0500 1.0000 Uiso H24 0.127(2) 0.3738(5) -0.482(2) 0.0500 1.0000 Uiso H25 0.078(2) 0.3250(6) -0.416(2) 0.0500 1.0000 Uiso H26 0.135(2) 0.3160(6) -0.219(2) 0.0500 1.0000 Uiso H33 0.235(2) 0.4644(7) 0.019(2) 0.0500 1.0000 Uiso H34 0.096(2) 0.4678(6) 0.102(2) 0.0500 1.0000 Uiso H35 0.028(2) 0.4208(6) 0.151(2) 0.0500 1.0000 Uiso H36 0.109(2) 0.3701(5) 0.119(2) 0.0500 1.0000 Uiso N61 0.0000 0.4693 -0.2500 0.18(2) 1.0000 Uiso C61 0.0000 0.4413 -0.2500 0.12(2) 1.0000 Uiso C62 0.0000 0.4062 -0.2500 0.10(1) 1.0000 Uiso N71 1.0000 0.1630 0.2500 0.41(8) 1.0000 Uiso C71 0.9578 0.1847 0.1980 0.25(4) 0.5000 Uiso C72 0.8888 0.2120 0.1433 0.21(3) 0.5000 Uiso 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 0.100(2) 0.077(2) 0.106(2) 0.019(2) 0.044(2) -0.003(2) CU2 0.092(2) 0.082(2) 0.117(2) 0.018(2) 0.043(2) -0.008(2) N11 0.09(1) 0.07(1) 0.11(1) 0.03(1) 0.04(1) 0.01(1) N12 0.06(1) 0.12(2) 0.08(1) 0.01(1) 0.026(9) -0.00(1) N21 0.08(1) 0.09(1) 0.12(2) 0.01(1) 0.05(1) 0.01(1) N22 0.10(1) 0.08(1) 0.10(2) 0.05(1) 0.05(1) 0.03(1) N31 0.08(1) 0.07(1) 0.12(1) 0.01(1) 0.05(1) -0.01(1) N32 0.09(1) 0.06(1) 0.10(1) 0.01(1) 0.04(1) 0.00(1) N41 0.10(1) 0.08(1) 0.10(1) -0.00(1) 0.04(1) -0.02(1) N51 0.07(1) 0.11(2) 0.16(2) 0.02(1) 0.05(1) -0.00(1) F11 0.30(3) 0.11(1) 0.37(3) -0.02(1) 0.22(2) -0.04(1) F12 0.35(3) 0.27(3) 0.21(2) -0.14(2) 0.05(2) -0.06(2) F13 0.26(2) 0.25(2) 0.32(3) 0.09(2) 0.20(2) -0.00(2) F14 0.13(2) 0.40(3) 0.22(2) 0.08(2) 0.06(2) 0.04(2) F21 0.14(4) 0.14(3) 0.18(5) 0.03(3) 0.13(4) -0.03(3) F22 0.08(4) 0.08(2) 0.15(4) -0.01(2) 0.03(3) -0.02(1) F23 0.07(3) 0.6(2) 0.19(7) 0.03(8) -0.01(3) 0.10(5) F24 0.4(1) 0.28(7) 0.14(5) 0.08(4) 0.18(7) 0.26(7) F31 0.53(5) 0.21(2) 0.14(2) -0.07(1) 0.06(2) -0.10(3) F32 0.18(2) 0.29(3) 0.63(6) -0.13(4) 0.05(3) 0.08(2) _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 CU1 . CU2 . 3.038(4) yes CU1 . N11 . 2.03(2) yes CU1 . N21 . 2.03(2) yes CU1 . N31 . 2.04(2) yes CU1 . N41 . 1.94(2) yes CU2 . N12 . 2.02(2) yes CU2 . N22 . 2.02(2) yes CU2 . N32 . 2.05(2) yes CU2 . N51 . 1.89(2) yes N11 . N12 . 1.35(2) yes N11 . C16 . 1.29(2) yes N12 . C13 . 1.32(2) yes N21 . N22 . 1.33(2) yes N21 . C26 . 1.29(2) yes N22 . C23 . 1.31(2) yes N31 . N32 . 1.35(2) yes N31 . C36 . 1.30(2) yes N32 . C33 . 1.25(3) yes N41 . C41 . 1.08(2) yes N51 . C51 . 1.10(3) yes C13 . C14 . 1.37(3) yes C14 . C15 . 1.29(3) yes C15 . C16 . 1.41(3) yes C23 . C24 . 1.42(3) yes C24 . C25 . 1.34(3) yes C25 . C26 . 1.33(3) yes C33 . C34 . 1.41(3) yes C34 . C35 . 1.31(3) yes C35 . C36 . 1.42(3) yes C41 . C42 . 1.51(3) yes C51 . C52 . 1.52(3) yes B1 . F11 . 1.35(2) yes B1 . F12 . 1.23(2) yes B1 . F13 . 1.23(2) yes B1 . F14 . 1.33(2) yes B2 . F21 . 1.31(3) yes B2 . F21 5_555 1.31(3) yes B2 . F22 . 1.39(2) yes B2 . F22 5_555 1.39(2) yes B2 . F23 . 1.18(4) yes B2 . F23 5_555 1.18(4) yes B2 . F24 . 1.26(5) yes B2 . F24 5_555 1.26(5) yes F21 . F23 5_555 1.2(1) yes F21 . F24 . 1.2(1) yes F22 . F22 5_555 1.13(5) yes F22 . F23 . 1.6(1) yes F23 . F24 . 1.29(7) yes B3 . F31 . 1.26(2) yes B3 . F31 5_655 1.26(2) yes B3 . F32 . 1.12(3) yes B3 . F32 5_655 1.12(3) yes N61 . C61 . 1.1670(1) yes C61 . C62 . 1.4632(1) yes N71 . C71 . 1.1202(3) yes N71 . C71 5_755 1.1202(3) yes C71 . C71 5_755 1.3196(3) yes C71 . C72 . 1.4338(3) yes 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 CU2 . CU1 . N11 . 65.7(5) yes CU2 . CU1 . N21 . 64.1(6) yes N11 . CU1 . N21 . 101.9(7) yes CU2 . CU1 . N31 . 65.3(5) yes N11 . CU1 . N31 . 107.1(7) yes N21 . CU1 . N31 . 101.5(7) yes CU2 . CU1 . N41 . 176.6(5) yes N11 . CU1 . N41 . 117.6(7) yes N21 . CU1 . N41 . 113.7(8) yes N31 . CU1 . N41 . 113.2(7) yes CU1 . CU2 . N12 . 65.2(6) yes CU1 . CU2 . N22 . 65.8(5) yes N12 . CU2 . N22 . 101.2(6) yes CU1 . CU2 . N32 . 65.8(5) yes N12 . CU2 . N32 . 106.2(7) yes N22 . CU2 . N32 . 104.8(7) yes CU1 . CU2 . N51 . 174.7(5) yes N12 . CU2 . N51 . 119.4(8) yes N22 . CU2 . N51 . 114.5(8) yes N32 . CU2 . N51 . 109.5(8) yes CU1 . N11 . N12 . 113.7(12) yes CU1 . N11 . C16 . 129.5(16) yes N12 . N11 . C16 . 116.6(18) yes CU2 . N12 . N11 . 115.4(12) yes CU2 . N12 . C13 . 123.3(17) yes N11 . N12 . C13 . 120.9(19) yes CU1 . N21 . N22 . 116.5(15) yes CU1 . N21 . C26 . 125.5(18) yes N22 . N21 . C26 . 118.0(21) yes CU2 . N22 . N21 . 113.4(14) yes CU2 . N22 . C23 . 124.8(16) yes N21 . N22 . C23 . 121.3(21) yes CU1 . N31 . N32 . 115.1(13) yes CU1 . N31 . C36 . 126.6(15) yes N32 . N31 . C36 . 117.9(18) yes CU2 . N32 . N31 . 113.8(13) yes CU2 . N32 . C33 . 124.8(17) yes N31 . N32 . C33 . 121.1(20) yes CU1 . N41 . C41 . 179.1(20) yes CU2 . N51 . C51 . 173.5(21) yes N12 . C13 . C14 . 121.1(24) yes C13 . C14 . C15 . 119.7(26) yes C14 . C15 . C16 . 116.9(24) yes N11 . C16 . C15 . 124.7(22) yes N22 . C23 . C24 . 121.2(23) yes C23 . C24 . C25 . 114.6(24) yes C24 . C25 . C26 . 120.7(27) yes N21 . C26 . C25 . 124.0(25) yes N32 . C33 . C34 . 123.1(26) yes C33 . C34 . C35 . 118.2(27) yes C34 . C35 . C36 . 116.3(27) yes N31 . C36 . C35 . 123.2(22) yes N41 . C41 . C42 . 176.2(26) yes N51 . C51 . C52 . 179.6(30) yes F11 . B1 . F12 . 108.3(17) yes F11 . B1 . F13 . 113.0(14) yes F12 . B1 . F13 . 109.3(18) yes F11 . B1 . F14 . 110.5(15) yes F12 . B1 . F14 . 105.4(18) yes F13 . B1 . F14 . 110.1(14) yes F21 . B2 . F21 5_555 135.3(35) yes F21 . B2 . F22 . 115.7(28) yes F21 5_555 B2 . F22 . 105.2(28) yes F21 . B2 . F22 5_555 105.2(28) yes F21 5_555 B2 . F22 5_555 115.7(28) yes F22 . B2 . F22 5_555 47.9(21) yes F21 . B2 . F23 . 115.9(41) yes F21 5_555 B2 . F23 . 57.6(46) yes F22 . B2 . F23 . 74.9(77) yes F22 5_555 B2 . F23 . 120.0(72) yes F21 . B2 . F23 5_555 57.6(46) yes F21 5_555 B2 . F23 5_555 115.9(41) yes F22 . B2 . F23 5_555 120.0(72) yes F22 5_555 B2 . F23 5_555 74.9(77) yes F23 . B2 . F23 5_555 165.0(149) yes F21 . B2 . F24 . 57.6(51) yes F21 5_555 B2 . F24 . 116.2(25) yes F22 . B2 . F24 . 80.2(67) yes F22 5_555 B2 . F24 . 113.3(29) yes F23 . B2 . F24 . 63.6(35) yes F21 . B2 . F24 5_555 116.2(25) yes F21 5_555 B2 . F24 5_555 57.6(51) yes F22 . B2 . F24 5_555 113.3(29) yes F22 5_555 B2 . F24 5_555 80.2(67) yes F23 . B2 . F24 5_555 114.3(36) yes F23 5_555 B2 . F24 . 114.3(36) yes F23 5_555 B2 . F24 5_555 63.6(35) yes F24 . B2 . F24 5_555 165.8(91) yes B2 . F21 . F23 5_555 55.6(23) yes B2 . F21 . F24 . 58.8(38) yes F23 5_555 F21 . F24 . 113.6(49) yes B2 . F22 . F22 5_555 66.1(11) yes B2 . F22 . F23 . 46.5(38) yes F22 5_555 F22 . F23 . 110.3(53) yes B2 . F23 . F21 5_555 66.8(43) yes B2 . F23 . F22 . 58.6(44) yes F21 5_555 F23 . F22 . 100.5(50) yes B2 . F23 . F24 . 61.1(31) yes F21 5_555 F23 . F24 . 122.2(95) yes F22 . F23 . F24 . 72.7(91) yes B2 . F24 . F21 . 63.6(37) yes B2 . F24 . F23 . 55.3(30) yes F21 . F24 . F23 . 113.7(79) yes F31 . B3 . F31 5_655 95.9(22) yes F31 . B3 . F32 . 110.3(24) yes F31 5_655 B3 . F32 . 115.2(30) yes F31 . B3 . F32 5_655 115.2(30) yes F31 5_655 B3 . F32 5_655 110.3(24) yes F32 . B3 . F32 5_655 109.5(37) yes N61 . C61 . C62 . 179.99 yes C71 . N71 . C71 5_755 72.18(2) yes N71 . C71 . C71 5_755 53.91(2) yes N71 . C71 . C72 . 168.603(4) yes C71 5_755 C71 . C72 . 125.14(2) yes _refine_diff_density_min -0.57 _refine_diff_density_max 0.99 #===end data_cr3 # paper complex no. 6 _publ_requested_journal 'test' _audit_creation_method CRYSTALS _chemical_name_systematic ; bis(acetonitrile)tris(mu-2-methylpyridazine)dicopper(I) ; _chemical_name_common ? _chemical_formula_moiety 'C9.50 H12 B1 Cu1 F4 N4' _chemical_formula_structural '[{Cu(C2H3N)}2(mu-C5H6N2)3][BF4]2' _chemical_formula_analytical 'C19 H24 B2 Cu2 F8 N8' _chemical_formula_sum 'C9.50 H12 B1 Cu1 F4 N4' _chemical_formula_weight 332.58 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'Cu ' 0.2630 1.2660 13.3380 3.5828 7.1676 0.2470 5.6158 11.3966 1.6735 64.8126 1.1910 'International_Tables_Vol_IV_Table_2.2B' 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'B ' 0.0000 0.0010 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 'International_Tables_Vol_IV_Table_2.2B' 'F ' 0.0140 0.0100 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International_Tables_Vol_IV_Table_2.2B' _symmetry_cell_setting 'monoclinic ' _symmetry_space_group_name_H-M 'C 1 2/c 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' 'x+1/2,y+1/2,z' '-x+1/2,-y+1/2,-z' '-x,y,-z+1/2' 'x,-y,z+1/2' '-x+1/2,y+1/2,-z+1/2' 'x+1/2,-y+1/2,z+1/2' _cell_length_a 25.289(4) _cell_angle_alpha 90 _cell_length_b 8.514(2) _cell_angle_beta 114.31(3) _cell_length_c 14.211(3) _cell_angle_gamma 90 _cell_volume 2789(1) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 12 _cell_measurement_theta_min 11.0 _cell_measurement_theta_max 13.6 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_min 0.08 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_max 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.584 _exptl_crystal_density_method ? _exptl_crystal_F_000 1336 _exptl_absorpt_coefficient_mu 1.605 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 ; Hilger and Watts Y290 4-circle-diffractometer ; _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 5.0 _diffrn_reflns_number 2170 _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 25.0 _reflns_number_total 2170 _reflns_number_observed 1298 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ; Crystals Users Guide (D.J.Watkin et al, 1985) ; _computing_structure_refinement ; Crystals Users Guide (D.J.Watkin et al 1985) ; _computing_molecular_graphics 'CAMERON (Watkin et al, 1996)' _computing_publication_material 'CRYSTALS Issue 10 (Watkin et al, 1996)' _refine_special_details ; Refinement on F for all reflections with intensity >2sigma(I). Cation sited on two-fold axis which bisects the N1-N2 and C4-C5 bonds of one of the methylpyridazine ligands. This results in two positions (50%:50% occupancy) for the methyl group of the methylpyridazine ligand lying across the two-fold axis. Restraints were applied to this ligand to stabilise structure refinement. Disorder in the tetrafluoroborate anion was modelled by six fluorine atoms each with 67% occupancy. Hydrogen atoms on the methylpyridazine ligand lying across the two-fold axis were placed and allowed to ride on their parent atom. Methyl hydrogen atoms on the other methyl-pyridazine ligand were also placed and allowed to ride on their parent atom. Aromatic hydrogen atoms on the other methyl-pyridazine ligand were found in difference maps and refined with isotropic displacement parameters. All non-hydrogen atoms, except boron and those of the methylpyridazine ligand lying across the two-fold axis, which were treated isotropically, were refined with anisotropic displacement parameters. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme ; Three parameter Chebychev W = [weight] * [1-(deltaF/6*sigmaF)**2]**2 using parameters 3.55 0.788 2.00 ; _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1298 _refine_ls_number_parameters 195 _refine_ls_number_restraints 5 _refine_ls_R_factor_obs 0.0828 _refine_ls_wR_factor_obs 0.0933 _refine_ls_goodness_of_fit_obs 1.0860 _refine_ls_shift/esd_max 0.05604 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 _atom_site_occupancy _atom_site_thermal_displace_type CU1 0.43487(5) 0.0402(2) 0.1836(1) 0.0743 1.0000 Uani N11 0.4874(3) -0.0818(8) 0.1257(6) 0.0609 1.0000 Uani N12 0.5452(3) -0.0777(9) 0.1804(6) 0.0626 1.0000 Uani C13 0.5803(4) -0.153(1) 0.1482(9) 0.0740 1.0000 Uani C14 0.5572(7) -0.243(1) 0.058(1) 0.0861 1.0000 Uani C15 0.5009(7) -0.251(1) 0.006(1) 0.0830 1.0000 Uani C16 0.4656(5) -0.166(1) 0.0387(8) 0.0704 1.0000 Uani C131 0.6436(5) -0.141(2) 0.213(1) 0.1135 1.0000 Uani N31 0.3569(5) 0.038(1) 0.0704(8) 0.0950 1.0000 Uani C31 0.3135(6) 0.030(2) 0.008(1) 0.1056 1.0000 Uani C32 0.2564(8) 0.012(4) -0.077(2) 0.1988 1.0000 Uani N21 0.4713(2) 0.2560(9) 0.2269(6) 0.076(2) 1.0000 Uiso C21 0.4433(6) 0.394(1) 0.206(1) 0.111(4) 1.0000 Uiso C22 0.4701(2) 0.539(2) 0.227(1) 0.138(6) 1.0000 Uiso C23 0.3803(7) 0.412(4) 0.160(3) 0.15(1) 0.5000 Uiso F11 0.359(2) 0.435(4) 0.340(3) 0.2788 0.6700 Uani F12 0.3326(9) 0.333(2) 0.478(2) 0.1918 0.6700 Uani F13 0.311(1) 0.555(3) 0.405(3) 0.2738 0.6700 Uani F14 0.2801(8) 0.405(6) 0.330(2) 0.3112 0.6700 Uani F15 0.330(2) 0.264(3) 0.347(2) 0.3073 0.6700 Uani F16 0.379(1) 0.442(2) 0.446(3) 0.2914 0.6700 Uani B1 0.331(1) 0.410(2) 0.395(2) 0.157(8) 1.0000 Uiso H14 0.584(4) -0.29(1) 0.044(8) 0.08(3) 1.0000 Uiso H15 0.488(4) -0.30(1) -0.048(8) 0.07(3) 1.0000 Uiso H16 0.425(4) -0.175(9) 0.013(6) 0.05(2) 1.0000 Uiso H321 0.252(6) -0.01(1) -0.13(1) 0.10(4) 1.0000 Uiso H322 0.239(4) 0.093(9) -0.072(7) 0.04(2) 1.0000 Uiso H323 0.239(5) 0.00(2) -0.028(9) 0.09(4) 1.0000 Uiso H1311 0.6550(5) -0.207(2) 0.276(1) 0.0500 1.0000 Uiso H1312 0.6662(5) -0.173(2) 0.173(1) 0.0500 1.0000 Uiso H1313 0.6518(5) -0.028(2) 0.234(1) 0.0500 1.0000 Uiso H21 0.4000(6) 0.391(1) 0.173(1) 0.0500 1.0000 Uiso H22 0.4481(2) 0.640(2) 0.209(1) 0.0500 0.5000 Uiso H231 0.3617(7) 0.306(4) 0.146(3) 0.0500 0.5000 Uiso H232 0.3675(7) 0.473(4) 0.095(3) 0.0500 0.5000 Uiso H233 0.3687(7) 0.469(4) 0.210(3) 0.0500 0.5000 Uiso 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 0.0669(8) 0.0737(9) 0.0743(9) 0.0048(7) 0.0210(6) 0.0128(7) N11 0.064(5) 0.050(5) 0.071(5) 0.004(4) 0.030(4) 0.004(4) N12 0.062(5) 0.056(5) 0.068(5) 0.009(4) 0.025(4) 0.002(4) C13 0.069(7) 0.076(7) 0.088(7) 0.007(6) 0.044(6) 0.018(5) C14 0.10(1) 0.079(9) 0.09(1) 0.011(7) 0.057(9) 0.024(7) C15 0.13(1) 0.061(8) 0.071(8) -0.002(6) 0.054(8) 0.010(7) C16 0.070(7) 0.068(7) 0.070(7) 0.000(6) 0.025(6) -0.004(6) C131 0.10(1) 0.14(1) 0.13(1) -0.010(9) 0.065(9) 0.013(8) N31 0.089(7) 0.102(7) 0.084(7) -0.005(6) 0.026(6) 0.005(6) C31 0.080(9) 0.14(1) 0.083(8) -0.012(8) 0.021(7) 0.002(8) C32 0.07(1) 0.38(4) 0.12(2) -0.05(2) 0.01(1) 0.06(2) F11 0.29(4) 0.31(4) 0.32(3) -0.14(3) 0.21(3) -0.11(3) F12 0.24(2) 0.16(1) 0.21(2) 0.05(1) 0.13(2) 0.03(1) F13 0.29(3) 0.18(2) 0.45(4) 0.15(2) 0.26(3) 0.08(2) F14 0.11(1) 0.38(5) 0.31(3) -0.00(3) -0.05(2) 0.01(2) F15 0.37(4) 0.23(3) 0.25(3) -0.04(2) 0.05(3) -0.11(3) F16 0.18(2) 0.11(1) 0.37(4) 0.01(2) -0.10(2) -0.01(1) _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 CU1 . CU1 5_655 3.049(2) yes CU1 . N11 . 2.102(7) yes CU1 . N12 5_655 2.048(8) yes CU1 . N31 . 1.97(1) yes CU1 . N21 . 2.034(8) yes N11 . N12 . 1.34(1) yes N11 . C16 . 1.34(1) yes N12 . C13 . 1.32(1) yes C13 . C14 . 1.40(2) yes C13 . C131 . 1.48(2) yes C14 . C15 . 1.31(2) yes C15 . C16 . 1.37(2) yes N31 . C31 . 1.09(1) yes C31 . C32 . 1.46(2) yes N21 . N21 5_655 1.326(8) yes N21 . C21 . 1.336(8) yes C21 . C22 . 1.384(9) yes C21 . C23 . 1.46(1) yes C22 . C22 5_655 1.38(1) yes F11 . F15 . 1.65(4) yes F11 . F16 . 1.38(4) yes F11 . B1 . 1.25(2) yes F12 . B1 . 1.35(2) yes F13 . F14 . 1.64(4) yes F13 . B1 . 1.36(2) yes F14 . B1 . 1.25(2) yes F15 . B1 . 1.41(3) yes F16 . B1 . 1.14(2) yes 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 CU1 5_655 CU1 . N11 . 63.0(2) yes CU1 5_655 CU1 . N12 5_655 68.4(2) yes N11 . CU1 . N12 5_655 100.2(3) yes CU1 5_655 CU1 . N31 . 166.1(3) yes N11 . CU1 . N31 . 104.9(4) yes N12 5_655 CU1 . N31 . 122.9(4) yes CU1 5_655 CU1 . N21 . 64.8(1) yes N11 . CU1 . N21 . 106.6(3) yes N12 5_655 CU1 . N21 . 104.6(3) yes N31 . CU1 . N21 . 115.6(3) yes CU1 . N11 . N12 . 118.2(6) yes CU1 . N11 . C16 . 122.7(7) yes N12 . N11 . C16 . 119.0(8) yes CU1 5_655 N12 . N11 . 110.2(5) yes CU1 5_655 N12 . C13 . 128.7(7) yes N11 . N12 . C13 . 120.9(8) yes N12 . C13 . C14 . 119.8(10) yes N12 . C13 . C131 . 117.3(10) yes C14 . C13 . C131 . 122.9(10) yes C13 . C14 . C15 . 119.5(12) yes C14 . C15 . C16 . 119.6(13) yes N11 . C16 . C15 . 121.2(12) yes CU1 . N31 . C31 . 176.7(13) yes N31 . C31 . C32 . 177.2(19) yes CU1 . N21 . N21 5_655 114.6(2) yes CU1 . N21 . C21 . 126.4(6) yes N21 5_655 N21 . C21 . 118.8(6) yes N21 . C21 . C22 . 124.8(12) yes N21 . C21 . C23 . 125.0(18) yes C22 . C21 . C23 . 110.2(16) yes C21 . C22 . C22 5_655 116.4(6) yes F15 . F11 . F16 . 86.7(24) yes F15 . F11 . B1 . 56.3(17) yes F16 . F11 . B1 . 51.1(16) yes F14 . F13 . B1 . 48.2(12) yes F13 . F14 . B1 . 54.3(14) yes F11 . F15 . B1 . 47.6(11) yes F11 . F16 . B1 . 58.5(14) yes F11 . B1 . F12 . 144.4(21) yes F11 . B1 . F13 . 104.1(18) yes F12 . B1 . F13 . 102.6(13) yes F11 . B1 . F14 . 103.1(25) yes F12 . B1 . F14 . 105.5(20) yes F13 . B1 . F14 . 77.4(20) yes F11 . B1 . F15 . 76.1(17) yes F12 . B1 . F15 . 89.0(15) yes F13 . B1 . F15 . 155.5(20) yes F14 . B1 . F15 . 78.7(20) yes F11 . B1 . F16 . 70.4(21) yes F12 . B1 . F16 . 84.9(20) yes F13 . B1 . F16 . 93.4(19) yes F14 . B1 . F16 . 167.4(25) yes F15 . B1 . F16 . 109.3(21) yes _refine_diff_density_min -0.65 _refine_diff_density_max 1.79 #===end data_ph # paper complex no. 7 _audit_creation_method SHELXL _chemical_name_systematic ; bis(benzonitrile)-tris(\m-pyridiazine)dicopper(I) tetrafluoroborate ; _chemical_name_common ? _chemical_formula_moiety 'C26 H22 Cu2 N8 2+,(B F4 1-)2' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C26 H22 B2 Cu2 F8 N8' _chemical_formula_weight 747.22 _chemical_melting_point ? _chemical_compound_source ? 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' 'B' 'B' 0.0013 0.0007 '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' 'F' 'F' 0.0171 0.0103 '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 Triclinic _symmetry_space_group_name_H-M 'P-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.9323(12) _cell_length_b 13.1382(12) _cell_length_c 18.800(2) _cell_angle_alpha 92.45(1) _cell_angle_beta 91.86(1) _cell_angle_gamma 90.07(1) _cell_volume 3189.6(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 14 _exptl_crystal_description Prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.65 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.556 _exptl_crystal_density_method ? _exptl_crystal_F_000 1496 _exptl_absorpt_coefficient_mu 1.411 _exptl_absorpt_correction_type Semi-empirical _exptl_absorpt_correction_T_min 0.338 _exptl_absorpt_correction_T_max 0.363 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _units 1 1 0 0.150 'millimetres' -1 -1 0 0.150 'millimetres' 1 -1 0 0.130 'millimetres' -1 1 0 0.130 'millimetres' 0 0 1 0.325 'millimetres' 0 0 -1 0.325 'millimetres' _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 'Siemens P4 4-circle diffractometer' _diffrn_measurement_method '2\q/\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 9647 _diffrn_reflns_av_R_equivalents 0.0169 _diffrn_reflns_av_sigmaI/netI 0.0518 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 22.50 _reflns_number_total 8311 _reflns_number_observed 4875 _reflns_observed_criterion >2sigma(I) _computing_data_collection XSCAN _computing_cell_refinement XSCAN _computing_data_reduction XSCAN _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.0672P)^2^+7.1272P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8310 _refine_ls_number_parameters 829 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1165 _refine_ls_R_factor_obs 0.0619 _refine_ls_wR_factor_all 0.1735 _refine_ls_wR_factor_obs 0.1393 _refine_ls_goodness_of_fit_all 1.034 _refine_ls_goodness_of_fit_obs 1.123 _refine_ls_restrained_S_all 1.034 _refine_ls_restrained_S_obs 1.123 _refine_ls_shift/esd_max 0.252 _refine_ls_shift/esd_mean 0.008 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cu1A Cu 0.35870(8) 0.21251(8) 0.40475(6) 0.0776(4) Uani 1 d . . Cu2A Cu 0.14268(8) 0.30999(8) 0.41121(6) 0.0818(4) Uani 1 d . . N1A N 0.4922(6) 0.1469(6) 0.4089(4) 0.084(2) Uani 1 d . . C1A C 0.5698(7) 0.1078(7) 0.4156(5) 0.073(2) Uani 1 d . . C11A C 0.6693(6) 0.0597(6) 0.4251(5) 0.071(2) Uani 1 d . . C12A C 0.7129(7) 0.0091(8) 0.3684(5) 0.093(3) Uani 1 d . . H12A H 0.6789(7) 0.0064(8) 0.3240(5) 0.112 Uiso 1 d R . C13A C 0.8103(8) -0.0337(9) 0.3772(6) 0.108(3) Uani 1 d . . H13A H 0.8402(8) -0.0669(9) 0.3384(6) 0.129 Uiso 1 d R . C14A C 0.8604(8) -0.0290(9) 0.4406(7) 0.110(4) Uani 1 d . . H14A H 0.9241(8) -0.0606(9) 0.4469(7) 0.132 Uiso 1 d R . C15A C 0.8180(8) 0.0211(9) 0.4974(6) 0.112(4) Uani 1 d . . H15A H 0.8541(8) 0.0274(9) 0.5410(6) 0.134 Uiso 1 d R . C16A C 0.7211(8) 0.0635(7) 0.4909(5) 0.087(3) Uani 1 d . . H16A H 0.6912(8) 0.0939(7) 0.5307(5) 0.104 Uiso 1 d R . N2A N 0.0017(6) 0.3504(6) 0.4247(4) 0.096(2) Uani 1 d . . C2A C -0.0824(8) 0.3630(7) 0.4389(5) 0.083(3) Uani 1 d . . C21A C -0.1886(6) 0.3753(6) 0.4568(5) 0.070(2) Uani 1 d . . C22A C -0.2288(7) 0.3305(7) 0.5141(5) 0.084(3) Uani 1 d . . H22A H -0.1859(7) 0.2937(7) 0.5442(5) 0.101 Uiso 1 d R . C23A C -0.3325(9) 0.3429(8) 0.5294(6) 0.099(3) Uani 1 d . . H23A H -0.3621(9) 0.3094(8) 0.5663(6) 0.119 Uiso 1 d R . C24A C -0.3930(8) 0.3996(10) 0.4866(8) 0.109(4) Uani 1 d . . H24A H -0.4622(8) 0.4095(10) 0.4970(8) 0.130 Uiso 1 d R . C25A C -0.3545(9) 0.4435(10) 0.4297(8) 0.121(4) Uani 1 d . . H25A H -0.3990(9) 0.4833(10) 0.4028(8) 0.145 Uiso 1 d R . C26A C -0.2519(7) 0.4322(8) 0.4138(5) 0.097(3) Uani 1 d . . H26A H -0.2264(7) 0.4626(8) 0.3741(5) 0.116 Uiso 1 d R . N31A N 0.2413(5) 0.1280(5) 0.3550(4) 0.069(2) Uani 1 d . . N32A N 0.1457(5) 0.1689(5) 0.3592(4) 0.071(2) Uani 1 d . . C33A C 0.0665(7) 0.1154(7) 0.3312(5) 0.080(3) Uani 1 d . . H33A H 0.0007(7) 0.1435(7) 0.3338(5) 0.096 Uiso 1 d R . C34A C 0.0754(8) 0.0212(8) 0.2988(5) 0.089(3) Uani 1 d . . H34A H 0.0176(8) -0.0124(8) 0.2784(5) 0.107 Uiso 1 d R . C35A C 0.1711(8) -0.0213(7) 0.2946(5) 0.092(3) Uani 1 d . . H35A H 0.1811(8) -0.0863(7) 0.2744(5) 0.110 Uiso 1 d R . C36A C 0.2515(7) 0.0371(7) 0.3240(5) 0.079(2) Uani 1 d . . H36A H 0.3177(7) 0.0099(7) 0.3211(5) 0.095 Uiso 1 d R . N41A N 0.3424(5) 0.3492(5) 0.3552(4) 0.068(2) Uani 1 d . . N42A N 0.2493(5) 0.3943(5) 0.3636(3) 0.066(2) Uani 1 d . . C43A C 0.2348(6) 0.4864(6) 0.3385(5) 0.073(2) Uani 1 d . . H43A H 0.1720(6) 0.5188(6) 0.3459(5) 0.087 Uiso 1 d R . C44A C 0.3111(7) 0.5392(7) 0.3038(5) 0.081(3) Uani 1 d . . H44A H 0.2987(7) 0.6030(7) 0.2858(5) 0.098 Uiso 1 d R . C45A C 0.4028(7) 0.4925(7) 0.2958(5) 0.082(3) Uani 1 d . . H45A H 0.4568(7) 0.5241(7) 0.2737(5) 0.098 Uiso 1 d R . C46A C 0.4150(7) 0.3966(7) 0.3221(5) 0.076(2) Uani 1 d . . H46A H 0.4781(7) 0.3640(7) 0.3161(5) 0.091 Uiso 1 d R . N51A N 0.3099(6) 0.2484(5) 0.5056(4) 0.075(2) Uani 1 d . . N52A N 0.2141(5) 0.2882(5) 0.5080(4) 0.079(2) Uani 1 d . . C53A C 0.1762(8) 0.3150(8) 0.5700(6) 0.098(3) Uani 1 d . . H53A H 0.1098(8) 0.3421(8) 0.5702(6) 0.118 Uiso 1 d R . C54A C 0.2290(10) 0.3080(10) 0.6343(7) 0.123(4) Uani 1 d . . H54A H 0.2004(10) 0.3273(10) 0.6776(7) 0.147 Uiso 1 d R . C55A C 0.3268(9) 0.2686(9) 0.6314(6) 0.117(4) Uani 1 d . . H55A H 0.3650(9) 0.2595(9) 0.6734(6) 0.140 Uiso 1 d R . C56A C 0.3647(8) 0.2394(8) 0.5664(6) 0.095(3) Uani 1 d . . H56A H 0.4323(8) 0.2155(8) 0.5650(6) 0.114 Uiso 1 d R . Cu1B Cu 0.29269(8) 0.36338(7) 0.10070(6) 0.0784(4) Uani 1 d . . Cu2B Cu 0.19692(8) 0.14878(7) 0.09208(6) 0.0760(3) Uani 1 d . . N1B N 0.3556(6) 0.4962(6) 0.0953(4) 0.086(2) Uani 1 d . . C1B C 0.3921(7) 0.5739(7) 0.0852(5) 0.080(3) Uani 1 d . . C11B C 0.4355(7) 0.6708(6) 0.0721(5) 0.073(2) Uani 1 d . . C12B C 0.5094(9) 0.7127(7) 0.1193(6) 0.102(3) Uani 1 d . . H12B H 0.5288(9) 0.6785(7) 0.1599(6) 0.123 Uiso 1 d R . C13B C 0.5490(10) 0.8088(8) 0.1070(7) 0.116(4) Uani 1 d . . H13B H 0.6010(10) 0.8370(8) 0.1371(7) 0.139 Uiso 1 d R . C14B C 0.5134(12) 0.8603(8) 0.0501(8) 0.124(5) Uani 1 d . . H14B H 0.5402(12) 0.9241(8) 0.0412(8) 0.148 Uiso 1 d R . C15B C 0.4385(13) 0.8188(10) 0.0033(7) 0.139(5) Uani 1 d . . H15B H 0.4111(13) 0.8566(10) -0.0334(7) 0.166 Uiso 1 d R . C16B C 0.4025(9) 0.7221(8) 0.0148(6) 0.116(4) Uani 1 d . . H16B H 0.3553(9) 0.6922(8) -0.0182(6) 0.140 Uiso 1 d R . N2B N 0.1532(6) 0.0096(6) 0.0786(4) 0.090(2) Uani 1 d . . C2B C 0.1392(7) -0.0748(7) 0.0673(5) 0.076(2) Uani 1 d . . C21B C 0.1230(7) -0.1830(6) 0.0557(5) 0.077(2) Uani 1 d . . C22B C 0.1239(10) -0.2283(8) -0.0085(6) 0.120(4) Uani 1 d . . H22B H 0.1359(10) -0.1901(8) -0.0479(6) 0.144 Uiso 1 d R . C23B C 0.1095(11) -0.3336(9) -0.0177(7) 0.138(5) Uani 1 d . . H23B H 0.1126(11) -0.3676(9) -0.0620(7) 0.165 Uiso 1 d R . C24B C 0.0921(11) -0.3859(9) 0.0389(10) 0.141(5) Uani 1 d . . H24B H 0.0770(11) -0.4549(9) 0.0319(10) 0.169 Uiso 1 d R . C25B C 0.0921(20) -0.3404(11) 0.1030(11) 0.258(13) Uani 1 d . . H25B H 0.0808(20) -0.3811(11) 0.1412(11) 0.309 Uiso 1 d R . C26B C 0.1045(14) -0.2392(8) 0.1115(7) 0.184(8) Uani 1 d . . H26B H 0.1047(14) -0.2069(8) 0.1565(7) 0.221 Uiso 1 d R . N31B N 0.1565(5) 0.3483(5) 0.1559(4) 0.068(2) Uani 1 d . . N32B N 0.1146(5) 0.2530(4) 0.1493(4) 0.067(2) Uani 1 d . . C33B C 0.0232(7) 0.2375(7) 0.1775(5) 0.075(2) Uani 1 d . . H33B H -0.0054(7) 0.1725(7) 0.1735(5) 0.090 Uiso 1 d R . C34B C -0.0317(7) 0.3136(8) 0.2119(5) 0.088(3) Uani 1 d . . H34B H -0.0965(7) 0.3018(8) 0.2300(5) 0.105 Uiso 1 d R . C35B C 0.0105(7) 0.4072(8) 0.2193(5) 0.083(3) Uani 1 d . . H35B H -0.0222(7) 0.4608(8) 0.2433(5) 0.100 Uiso 1 d R . C36B C 0.1059(7) 0.4207(7) 0.1902(5) 0.078(2) Uani 1 d . . H36B H 0.1356(7) 0.4853(7) 0.1950(5) 0.093 Uiso 1 d R . N41B N 0.3854(5) 0.2506(5) 0.1389(4) 0.070(2) Uani 1 d . . N42B N 0.3434(5) 0.1566(5) 0.1383(4) 0.070(2) Uani 1 d . . C43B C 0.3967(8) 0.0800(7) 0.1636(5) 0.081(3) Uani 1 d . . H43B H 0.3650(8) 0.0163(7) 0.1620(5) 0.097 Uiso 1 d R . C44B C 0.4963(8) 0.0909(8) 0.1921(5) 0.095(3) Uani 1 d . . H44B H 0.5327(8) 0.0355(8) 0.2091(5) 0.114 Uiso 1 d R . C45B C 0.5397(7) 0.1843(8) 0.1923(5) 0.092(3) Uani 1 d . . H45B H 0.6061(7) 0.1969(8) 0.2112(5) 0.111 Uiso 1 d R . C46B C 0.4795(7) 0.2625(6) 0.1654(5) 0.084(3) Uani 1 d . . H46B H 0.5080(7) 0.3276(6) 0.1665(5) 0.101 Uiso 1 d R . N51B N 0.2411(6) 0.3146(5) -0.0001(4) 0.079(2) Uani 1 d . . N52B N 0.2032(6) 0.2184(5) -0.0028(4) 0.081(2) Uani 1 d . . C53B C 0.1663(8) 0.1792(8) -0.0639(6) 0.101(3) Uani 1 d . . H53B H 0.1386(8) 0.1138(8) -0.0645(6) 0.122 Uiso 1 d R . C54B C 0.1641(12) 0.2305(10) -0.1261(6) 0.146(5) Uani 1 d . . H54B H 0.1366(12) 0.2006(10) -0.1683(6) 0.176 Uiso 1 d R . C55B C 0.2008(11) 0.3277(10) -0.1241(6) 0.136(5) Uani 1 d . . H55B H 0.2026(11) 0.3663(10) -0.1644(6) 0.164 Uiso 1 d R . C56B C 0.2410(9) 0.3662(7) -0.0588(6) 0.102(3) Uani 1 d . . H56B H 0.2693(9) 0.4314(7) -0.0558(6) 0.122 Uiso 1 d R . B1 B 0.6902(11) 0.4532(9) 0.2123(7) 0.086(3) Uani 1 d . . F11 F 0.6871(11) 0.4337(8) 0.1459(5) 0.275(7) Uani 1 d . . F12 F 0.7806(6) 0.4884(6) 0.2335(5) 0.181(3) Uani 1 d . . F13 F 0.6559(6) 0.3795(5) 0.2512(4) 0.153(3) Uani 1 d . . F14 F 0.6312(8) 0.5297(9) 0.2213(8) 0.289(8) Uani 1 d . . B2 B 0.0431(11) 0.7074(13) 0.3083(9) 0.106(4) Uani 1 d . . F21 F 0.0445(8) 0.7667(8) 0.3703(6) 0.215(4) Uani 1 d . . F22 F -0.0255(7) 0.7559(10) 0.2747(5) 0.251(6) Uani 1 d . . F23 F 0.1341(5) 0.7029(7) 0.2828(4) 0.182(4) Uani 1 d . . F24 F 0.0134(6) 0.6223(6) 0.3355(6) 0.208(5) Uani 1 d . . B3 B 0.4252(12) -0.1758(10) 0.2955(8) 0.098(4) Uani 1 d . . F31 F 0.3910(9) -0.1540(7) 0.3579(4) 0.235(6) Uani 1 d . . F32 F 0.4541(5) -0.2716(4) 0.2890(4) 0.138(2) Uani 1 d . . F33 F 0.3593(5) -0.1455(5) 0.2424(4) 0.138(2) Uani 1 d . . F34 F 0.5086(7) -0.1158(6) 0.2860(5) 0.202(4) Uani 1 d . . B4 B -0.1970(13) 0.0464(11) 0.1758(10) 0.115(5) Uani 1 d . . F41 F -0.2591(7) -0.0217(6) 0.1967(4) 0.183(4) Uani 1 d . . F42 F -0.1951(6) 0.1294(6) 0.2166(5) 0.197(4) Uani 1 d . . F43 F -0.1052(5) 0.0175(5) 0.1583(6) 0.190(4) Uani 1 d . . F44 F -0.2413(10) 0.0665(11) 0.1122(6) 0.279(7) Uani 1 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1A 0.0560(6) 0.0761(7) 0.1006(9) -0.0028(6) 0.0074(6) 0.0096(5) Cu2A 0.0543(6) 0.0847(7) 0.1068(9) 0.0013(6) 0.0130(6) 0.0086(5) N1A 0.060(5) 0.085(5) 0.107(6) -0.004(4) 0.011(4) 0.010(4) C1A 0.062(6) 0.080(6) 0.077(6) -0.005(5) 0.011(5) 0.002(5) C11A 0.051(5) 0.083(6) 0.079(7) 0.011(5) 0.012(5) 0.006(4) C12A 0.058(6) 0.144(9) 0.077(7) -0.005(6) -0.002(5) 0.014(6) C13A 0.064(7) 0.151(10) 0.109(9) -0.007(7) 0.010(6) 0.034(6) C14A 0.054(6) 0.153(10) 0.125(10) 0.038(9) 0.006(7) 0.018(6) C15A 0.076(8) 0.164(11) 0.096(9) 0.032(8) -0.013(7) 0.015(7) C16A 0.087(7) 0.109(7) 0.066(7) 0.001(5) 0.017(6) 0.012(6) N2A 0.065(5) 0.103(6) 0.120(7) 0.007(5) 0.010(5) 0.016(5) C2A 0.062(6) 0.091(7) 0.095(7) -0.003(5) -0.001(5) 0.015(5) C21A 0.051(5) 0.081(6) 0.076(6) -0.006(5) -0.001(5) 0.012(4) C22A 0.074(7) 0.089(7) 0.088(7) 0.001(5) 0.001(6) 0.002(5) C23A 0.090(8) 0.105(8) 0.104(9) -0.004(6) 0.034(7) -0.020(7) C24A 0.064(7) 0.129(10) 0.132(11) -0.015(8) 0.012(8) 0.008(7) C25A 0.066(8) 0.145(11) 0.150(12) 0.007(9) -0.027(8) 0.018(7) C26A 0.063(6) 0.129(9) 0.099(8) 0.020(6) -0.004(6) 0.006(6) N31A 0.064(5) 0.062(4) 0.080(5) -0.005(4) 0.006(4) -0.005(4) N32A 0.054(4) 0.071(4) 0.088(5) 0.005(4) 0.003(4) 0.001(4) C33A 0.054(6) 0.093(7) 0.093(7) 0.024(6) -0.014(5) -0.001(5) C34A 0.090(8) 0.083(7) 0.092(7) 0.001(6) -0.018(6) -0.018(6) C35A 0.094(8) 0.079(6) 0.102(8) -0.012(5) -0.003(6) -0.008(6) C36A 0.078(6) 0.076(6) 0.084(7) -0.004(5) 0.009(5) 0.002(5) N41A 0.051(4) 0.067(4) 0.085(5) -0.004(4) 0.008(4) 0.002(4) N42A 0.055(4) 0.062(4) 0.081(5) -0.004(4) 0.002(3) 0.005(3) C43A 0.059(5) 0.070(6) 0.089(7) -0.002(5) -0.004(5) 0.005(5) C44A 0.075(7) 0.071(6) 0.099(7) 0.014(5) -0.001(6) -0.001(5) C45A 0.065(6) 0.083(7) 0.098(7) 0.006(5) 0.011(5) -0.017(5) C46A 0.061(6) 0.077(6) 0.089(7) -0.007(5) 0.014(5) -0.001(5) N51A 0.060(5) 0.081(5) 0.085(6) 0.000(4) 0.008(4) 0.004(4) N52A 0.064(5) 0.087(5) 0.087(6) -0.007(4) 0.018(4) 0.007(4) C53A 0.072(7) 0.114(8) 0.108(9) -0.017(7) 0.019(7) 0.009(6) C54A 0.106(10) 0.175(12) 0.087(9) -0.009(8) 0.012(8) 0.005(9) C55A 0.097(9) 0.161(11) 0.092(9) 0.011(8) -0.002(7) 0.016(8) C56A 0.070(7) 0.119(8) 0.098(8) -0.003(7) 0.017(7) 0.011(6) Cu1B 0.0781(7) 0.0588(6) 0.0980(9) 0.0075(5) -0.0032(6) -0.0152(5) Cu2B 0.0811(8) 0.0561(6) 0.0906(8) 0.0026(5) -0.0003(6) -0.0143(5) N1B 0.081(5) 0.065(5) 0.112(6) 0.005(4) 0.001(4) -0.018(4) C1B 0.078(6) 0.067(6) 0.095(7) 0.001(5) 0.004(5) 0.000(5) C11B 0.086(6) 0.048(5) 0.088(7) 0.005(5) 0.021(5) -0.011(5) C12B 0.132(9) 0.067(6) 0.109(8) 0.006(6) 0.016(7) -0.023(6) C13B 0.147(11) 0.079(7) 0.122(10) -0.010(7) 0.020(8) -0.035(7) C14B 0.188(14) 0.067(7) 0.120(11) 0.009(7) 0.059(10) -0.011(8) C15B 0.223(16) 0.093(9) 0.105(10) 0.037(7) 0.022(10) -0.006(9) C16B 0.145(10) 0.087(8) 0.118(9) 0.028(7) -0.010(8) -0.007(7) N2B 0.098(6) 0.061(5) 0.112(6) 0.006(4) -0.001(5) -0.013(4) C2B 0.078(6) 0.068(6) 0.083(7) 0.012(5) 0.003(5) -0.013(5) C21B 0.097(7) 0.056(5) 0.079(7) 0.011(5) -0.003(5) -0.010(5) C22B 0.188(13) 0.081(8) 0.091(8) 0.010(6) -0.024(8) -0.029(7) C23B 0.212(15) 0.084(9) 0.111(10) -0.009(7) -0.064(10) -0.022(9) C24B 0.172(13) 0.055(7) 0.195(16) 0.009(9) -0.027(12) -0.017(7) C25B 0.518(39) 0.067(10) 0.195(19) 0.028(10) 0.089(22) -0.016(15) C26B 0.394(25) 0.062(7) 0.100(9) 0.020(7) 0.034(12) -0.002(10) N31B 0.071(5) 0.059(4) 0.075(5) 0.002(4) -0.003(4) -0.009(4) N32B 0.068(5) 0.053(4) 0.081(5) 0.007(3) -0.008(4) -0.011(3) C33B 0.076(6) 0.068(6) 0.081(6) 0.010(5) -0.006(5) -0.006(5) C34B 0.073(6) 0.095(7) 0.096(7) 0.010(6) 0.003(5) -0.001(6) C35B 0.076(7) 0.087(7) 0.086(7) -0.005(5) 0.003(5) 0.017(5) C36B 0.084(7) 0.065(6) 0.082(6) -0.006(5) -0.011(5) -0.001(5) N41B 0.068(5) 0.053(4) 0.087(5) 0.000(3) -0.001(4) -0.009(3) N42B 0.070(5) 0.061(4) 0.078(5) 0.004(4) 0.004(4) -0.006(4) C43B 0.083(7) 0.060(5) 0.100(7) 0.012(5) 0.006(6) 0.002(5) C44B 0.092(8) 0.079(7) 0.114(8) 0.008(6) -0.008(6) 0.011(6) C45B 0.069(6) 0.083(7) 0.123(9) -0.003(6) -0.010(6) 0.011(6) C46B 0.078(7) 0.061(6) 0.113(8) -0.008(5) 0.002(6) -0.004(5) N51B 0.098(6) 0.060(4) 0.080(5) 0.004(4) 0.010(4) -0.013(4) N52B 0.105(6) 0.065(5) 0.072(5) 0.002(4) -0.007(4) -0.009(4) C53B 0.134(9) 0.083(7) 0.086(8) -0.001(6) -0.012(7) -0.017(6) C54B 0.247(17) 0.119(10) 0.071(8) 0.004(7) -0.022(9) -0.032(11) C55B 0.213(15) 0.114(10) 0.081(9) 0.013(7) -0.014(9) -0.025(10) C56B 0.146(10) 0.070(6) 0.091(8) 0.024(6) 0.005(7) -0.015(6) B1 0.089(9) 0.072(7) 0.096(10) 0.018(7) -0.010(7) -0.019(7) F11 0.483(20) 0.244(11) 0.095(6) -0.017(6) 0.032(9) -0.188(12) F12 0.101(5) 0.200(8) 0.244(9) 0.068(7) -0.014(6) -0.051(5) F13 0.195(7) 0.137(5) 0.126(5) 0.039(4) -0.036(5) -0.076(5) F14 0.208(10) 0.237(11) 0.444(20) 0.149(12) 0.149(12) 0.126(9) B2 0.078(9) 0.123(12) 0.121(12) 0.030(10) 0.005(9) 0.027(9) F21 0.206(10) 0.226(10) 0.209(10) -0.043(8) 0.019(8) -0.019(8) F22 0.144(7) 0.452(17) 0.166(8) 0.132(10) 0.003(6) 0.108(9) F23 0.099(5) 0.252(9) 0.206(8) 0.100(7) 0.062(5) 0.062(5) F24 0.151(7) 0.108(6) 0.373(14) 0.021(7) 0.126(8) 0.025(5) B3 0.111(11) 0.079(9) 0.104(11) 0.004(8) -0.003(9) 0.014(8) F31 0.394(15) 0.205(8) 0.116(6) 0.048(6) 0.095(8) 0.165(9) F32 0.142(5) 0.069(4) 0.203(7) 0.005(4) 0.014(5) 0.010(4) F33 0.130(5) 0.162(6) 0.120(5) -0.004(4) 0.007(4) 0.037(5) F34 0.192(8) 0.149(7) 0.264(11) 0.077(7) -0.067(7) -0.076(6) B4 0.115(12) 0.080(9) 0.153(15) 0.006(9) 0.034(11) -0.019(9) F41 0.208(8) 0.161(7) 0.180(7) -0.028(5) 0.069(6) -0.092(6) F42 0.183(8) 0.116(5) 0.291(11) -0.081(6) 0.096(7) -0.054(5) F43 0.081(5) 0.141(6) 0.340(12) -0.101(7) 0.008(6) -0.014(4) F44 0.287(14) 0.378(18) 0.180(10) 0.109(11) -0.009(9) 0.105(12) _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 Cu1A N1A 1.931(8) . ? Cu1A N51A 2.054(7) . ? Cu1A N31A 2.056(6) . ? Cu1A N41A 2.065(7) . ? Cu2A N2A 1.921(8) . ? Cu2A N42A 2.023(6) . ? Cu2A N52A 2.046(8) . ? Cu2A N32A 2.059(7) . ? N1A C1A 1.134(9) . ? C1A C11A 1.444(12) . ? C11A C12A 1.369(11) . ? C11A C16A 1.386(12) . ? C12A C13A 1.388(12) . ? C13A C14A 1.336(14) . ? C14A C15A 1.361(14) . ? C15A C16A 1.376(13) . ? N2A C2A 1.139(10) . ? C2A C21A 1.432(12) . ? C21A C22A 1.366(11) . ? C21A C26A 1.377(12) . ? C22A C23A 1.388(12) . ? C23A C24A 1.350(14) . ? C24A C25A 1.346(15) . ? C25A C26A 1.377(13) . ? N31A C36A 1.315(10) . ? N31A N32A 1.352(8) . ? N32A C33A 1.323(10) . ? C33A C34A 1.363(12) . ? C34A C35A 1.361(12) . ? C35A C36A 1.379(12) . ? N41A C46A 1.314(10) . ? N41A N42A 1.354(8) . ? N42A C43A 1.328(9) . ? C43A C44A 1.399(11) . ? C44A C45A 1.345(11) . ? C45A C46A 1.380(11) . ? N51A C56A 1.335(11) . ? N51A N52A 1.346(9) . ? N52A C53A 1.313(11) . ? C53A C54A 1.376(14) . ? C54A C55A 1.368(14) . ? C55A C56A 1.372(13) . ? Cu1B N1B 1.933(7) . ? Cu1B N41B 2.047(7) . ? Cu1B N51B 2.065(7) . ? Cu1B N31B 2.087(7) . ? Cu2B N2B 1.917(8) . ? Cu2B N32B 2.029(7) . ? Cu2B N52B 2.043(7) . ? Cu2B N42B 2.059(7) . ? N1B C1B 1.149(10) . ? C1B C11B 1.425(12) . ? C11B C16B 1.353(12) . ? C11B C12B 1.380(13) . ? C12B C13B 1.393(13) . ? C13B C14B 1.36(2) . ? C14B C15B 1.38(2) . ? C15B C16B 1.380(14) . ? N2B C2B 1.134(9) . ? C2B C21B 1.443(12) . ? C21B C22B 1.322(12) . ? C21B C26B 1.336(13) . ? C22B C23B 1.399(14) . ? C23B C24B 1.32(2) . ? C24B C25B 1.32(2) . ? C25B C26B 1.34(2) . ? N31B C36B 1.313(10) . ? N31B N32B 1.362(8) . ? N32B C33B 1.330(10) . ? C33B C34B 1.378(12) . ? C34B C35B 1.345(12) . ? C35B C36B 1.381(12) . ? N41B C46B 1.306(10) . ? N41B N42B 1.347(8) . ? N42B C43B 1.318(10) . ? C43B C44B 1.384(12) . ? C44B C45B 1.348(12) . ? C45B C46B 1.392(12) . ? N51B C56B 1.319(11) . ? N51B N52B 1.353(9) . ? N52B C53B 1.313(11) . ? C53B C54B 1.373(13) . ? C54B C55B 1.361(14) . ? C55B C56B 1.392(14) . ? B1 F11 1.263(14) . ? B1 F14 1.271(14) . ? B1 F12 1.301(13) . ? B1 F13 1.323(12) . ? B2 F22 1.262(14) . ? B2 F23 1.285(14) . ? B2 F24 1.313(15) . ? B2 F21 1.37(2) . ? B3 F31 1.287(14) . ? B3 F32 1.316(13) . ? B3 F34 1.356(15) . ? B3 F33 1.364(14) . ? B4 F41 1.284(14) . ? B4 F43 1.30(2) . ? B4 F42 1.31(2) . ? B4 F44 1.35(2) . ? 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 N1A Cu1A N51A 110.5(3) . . ? N1A Cu1A N31A 115.5(3) . . ? N51A Cu1A N31A 105.9(3) . . ? N1A Cu1A N41A 119.7(3) . . ? N51A Cu1A N41A 102.5(3) . . ? N31A Cu1A N41A 101.2(3) . . ? N2A Cu2A N42A 124.6(3) . . ? N2A Cu2A N52A 109.5(3) . . ? N42A Cu2A N52A 101.5(3) . . ? N2A Cu2A N32A 109.5(3) . . ? N42A Cu2A N32A 105.3(3) . . ? N52A Cu2A N32A 104.5(3) . . ? C1A N1A Cu1A 175.9(8) . . ? N1A C1A C11A 178.8(9) . . ? C12A C11A C16A 119.6(8) . . ? C12A C11A C1A 119.5(9) . . ? C16A C11A C1A 121.0(8) . . ? C11A C12A C13A 119.2(9) . . ? C14A C13A C12A 121.0(10) . . ? C13A C14A C15A 120.4(10) . . ? C14A C15A C16A 120.2(10) . . ? C15A C16A C11A 119.5(9) . . ? C2A N2A Cu2A 170.3(8) . . ? N2A C2A C21A 178.1(10) . . ? C22A C21A C26A 119.5(8) . . ? C22A C21A C2A 122.0(8) . . ? C26A C21A C2A 118.5(9) . . ? C21A C22A C23A 120.4(9) . . ? C24A C23A C22A 119.0(10) . . ? C25A C24A C23A 121.1(11) . . ? C24A C25A C26A 120.7(11) . . ? C21A C26A C25A 119.2(10) . . ? C36A N31A N32A 118.9(7) . . ? C36A N31A Cu1A 125.4(6) . . ? N32A N31A Cu1A 115.5(5) . . ? C33A N32A N31A 118.1(7) . . ? C33A N32A Cu2A 127.9(6) . . ? N31A N32A Cu2A 114.1(5) . . ? N32A C33A C34A 123.9(9) . . ? C35A C34A C33A 118.6(9) . . ? C34A C35A C36A 115.6(9) . . ? N31A C36A C35A 124.8(9) . . ? C46A N41A N42A 119.5(7) . . ? C46A N41A Cu1A 126.0(6) . . ? N42A N41A Cu1A 114.3(5) . . ? C43A N42A N41A 118.4(7) . . ? C43A N42A Cu2A 126.2(6) . . ? N41A N42A Cu2A 115.3(5) . . ? N42A C43A C44A 123.3(8) . . ? C45A C44A C43A 117.2(8) . . ? C44A C45A C46A 118.1(8) . . ? N41A C46A C45A 123.6(8) . . ? C56A N51A N52A 118.9(8) . . ? C56A N51A Cu1A 126.5(6) . . ? N52A N51A Cu1A 114.6(6) . . ? C53A N52A N51A 119.3(8) . . ? C53A N52A Cu2A 125.1(7) . . ? N51A N52A Cu2A 115.4(6) . . ? N52A C53A C54A 124.4(10) . . ? C55A C54A C53A 115.9(11) . . ? C54A C55A C56A 119.0(11) . . ? N51A C56A C55A 122.4(10) . . ? N1B Cu1B N41B 116.4(3) . . ? N1B Cu1B N51B 108.7(3) . . ? N41B Cu1B N51B 106.8(3) . . ? N1B Cu1B N31B 119.6(3) . . ? N41B Cu1B N31B 103.6(3) . . ? N51B Cu1B N31B 99.9(3) . . ? N2B Cu2B N32B 122.1(3) . . ? N2B Cu2B N52B 111.4(3) . . ? N32B Cu2B N52B 100.5(3) . . ? N2B Cu2B N42B 110.4(3) . . ? N32B Cu2B N42B 104.4(3) . . ? N52B Cu2B N42B 106.9(3) . . ? C1B N1B Cu1B 173.6(8) . . ? N1B C1B C11B 178.9(10) . . ? C16B C11B C12B 120.5(9) . . ? C16B C11B C1B 120.1(10) . . ? C12B C11B C1B 119.4(9) . . ? C11B C12B C13B 118.9(10) . . ? C14B C13B C12B 119.9(12) . . ? C13B C14B C15B 121.2(11) . . ? C16B C15B C14B 118.3(12) . . ? C11B C16B C15B 121.2(12) . . ? C2B N2B Cu2B 171.4(8) . . ? N2B C2B C21B 177.7(10) . . ? C22B C21B C26B 118.8(9) . . ? C22B C21B C2B 122.3(9) . . ? C26B C21B C2B 118.9(10) . . ? C21B C22B C23B 120.8(11) . . ? C24B C23B C22B 118.2(12) . . ? C23B C24B C25B 120.7(12) . . ? C24B C25B C26B 120.9(15) . . ? C21B C26B C25B 120.5(13) . . ? C36B N31B N32B 119.1(7) . . ? C36B N31B Cu1B 127.2(6) . . ? N32B N31B Cu1B 113.5(5) . . ? C33B N32B N31B 118.3(7) . . ? C33B N32B Cu2B 126.1(6) . . ? N31B N32B Cu2B 115.6(5) . . ? N32B C33B C34B 123.1(8) . . ? C35B C34B C33B 118.5(9) . . ? C34B C35B C36B 117.1(9) . . ? N31B C36B C35B 123.9(8) . . ? C46B N41B N42B 117.9(7) . . ? C46B N41B Cu1B 125.8(6) . . ? N42B N41B Cu1B 116.3(5) . . ? C43B N42B N41B 120.3(7) . . ? C43B N42B Cu2B 126.2(6) . . ? N41B N42B Cu2B 113.4(5) . . ? N42B C43B C44B 122.8(8) . . ? C45B C44B C43B 117.5(9) . . ? C44B C45B C46B 117.2(9) . . ? N41B C46B C45B 124.3(8) . . ? C56B N51B N52B 119.4(8) . . ? C56B N51B Cu1B 127.5(7) . . ? N52B N51B Cu1B 113.1(5) . . ? C53B N52B N51B 118.9(8) . . ? C53B N52B Cu2B 124.6(7) . . ? N51B N52B Cu2B 116.3(6) . . ? N52B C53B C54B 123.6(10) . . ? C55B C54B C53B 118.2(11) . . ? C54B C55B C56B 116.7(11) . . ? N51B C56B C55B 123.2(10) . . ? F11 B1 F14 104.9(13) . . ? F11 B1 F12 110.8(13) . . ? F14 B1 F12 103.2(12) . . ? F11 B1 F13 115.1(11) . . ? F14 B1 F13 107.9(12) . . ? F12 B1 F13 113.8(11) . . ? F22 B2 F23 117.9(14) . . ? F22 B2 F24 116.3(14) . . ? F23 B2 F24 113.6(12) . . ? F22 B2 F21 97.7(13) . . ? F23 B2 F21 110.2(14) . . ? F24 B2 F21 97.3(13) . . ? F31 B3 F32 111.5(12) . . ? F31 B3 F34 108.1(13) . . ? F32 B3 F34 108.4(12) . . ? F31 B3 F33 112.4(12) . . ? F32 B3 F33 114.4(12) . . ? F34 B3 F33 101.2(11) . . ? F41 B4 F43 117.6(13) . . ? F41 B4 F42 113.2(14) . . ? F43 B4 F42 112.2(13) . . ? F41 B4 F44 100.7(15) . . ? F43 B4 F44 102.1(14) . . ? F42 B4 F44 109.3(14) . . ? _refine_diff_density_max 0.800 _refine_diff_density_min -0.400 _refine_diff_density_rms 0.061 #===end data_cupz2tp2 # paper complex no. 13 _publ_requested_journal 'test' _audit_creation_method CRYSTALS _chemical_name_systematic ; Bis(triphenylphosphine)bis(pyridazine)copper(I) tetrafluoroborate ; _chemical_name_common ? _chemical_formula_moiety 'C44 H38 B1 Cu1 F4 N4 P2' _chemical_formula_structural '[Cu(C4H4N2)2{(C6H5)3P}2][BF4]' _chemical_formula_analytical 'C44 H38 B1 Cu1 F4 N4 P2' _chemical_formula_sum 'C44 H38 B1 Cu1 F4 N4 P2' _chemical_formula_weight 835.12 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'Cu ' 0.2630 1.2660 13.3380 3.5828 7.1676 0.2470 5.6158 11.3966 1.6735 64.8126 1.1910 'International_Tables_Vol_IV_Table_2.2B' 'P ' 0.0900 0.0950 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International_Tables_Vol_IV_Table_2.2B' 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' 'B ' 0.0000 0.0010 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 'International_Tables_Vol_IV_Table_2.2B' 'F ' 0.0140 0.0100 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International_Tables_Vol_IV_Table_2.2B' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' _cell_length_a 10.814(4) _cell_angle_alpha 86.86(3) _cell_length_b 15.523(4) _cell_angle_beta 100.39(2) _cell_length_c 26.746(7) _cell_angle_gamma 100.91(2) _cell_volume 4335(1) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 12 _cell_measurement_theta_min 9.5 _cell_measurement_theta_max 13.8 _exptl_crystal_description 'rectangular block' _exptl_crystal_colour 'colourless' _exptl_crystal_size_min 0.50 _exptl_crystal_size_mid 0.55 _exptl_crystal_size_max 0.70 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.28 _exptl_crystal_density_method ? _exptl_crystal_F_000 1720 _exptl_absorpt_coefficient_mu 0.626 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 ; Hilger and Watts Y290 4-circle-diffractometer ; _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 2.2 _diffrn_reflns_number 14527 _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 25.0 _reflns_number_total 14527 _reflns_number_observed 7498 _reflns_observed_criterion >3sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ; MULTAN80 (P.Main et al, 1980) ; _computing_structure_refinement ; Crystals Users Guide (D.J.Watkin et al 1985) ; _computing_molecular_graphics 'CAMERON (Watkin et al, 1996)' _computing_publication_material 'CRYSTALS Issue 10 (Watkin et al, 1996)' _refine_special_details ; Refinement on F for all reflections with intensity >3sigma(I). The structure exhibits no disorder. All hydrogen atoms were placed and allowed to ride on their parent atom. All non-hydrogen atoms refined with anisotropic displacement parameters. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme ; Three parameter Chebychev W = [weight] * [1-(deltaF/6*sigmaF)**2]**2 using parameters 3.25 -3.45 2.47 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7498 _refine_ls_number_parameters 1009 _refine_ls_number_restraints 0 _refine_ls_R_factor_obs 0.069 _refine_ls_wR_factor_obs 0.088 _refine_ls_goodness_of_fit_obs 1.0188 _refine_ls_shift/esd_max 0.025 _refine_diff_density_min -0.65 _refine_diff_density_max 0.78 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 _atom_site_occupancy _atom_site_thermal_displace_type CU1 0.2484(1) 0.2600(1) 0.6395(1) 0.0451 1.0000 Uani N11 0.2939(8) 0.1427(6) 0.6588(4) 0.0493 1.0000 Uani N12 0.2102(12) 0.0665(7) 0.6305(4) 0.0838 1.0000 Uani C13 0.2335(17) -0.0118(9) 0.6445(7) 0.0983 1.0000 Uani C14 0.3277(16) -0.0208(10) 0.6855(7) 0.0901 1.0000 Uani C15 0.4044(14) 0.0563(10) 0.7113(6) 0.0860 1.0000 Uani C16 0.3816(12) 0.1356(8) 0.6972(4) 0.0633 1.0000 Uani N21 0.4358(9) 0.3643(6) 0.6644(3) 0.0581 1.0000 Uani N22 0.5434(9) 0.3423(6) 0.6602(3) 0.0649 1.0000 Uani C23 0.6623(12) 0.4088(8) 0.6696(5) 0.0741 1.0000 Uani C24 0.6849(13) 0.4983(9) 0.6815(5) 0.0810 1.0000 Uani C25 0.5765(13) 0.5208(8) 0.6849(5) 0.0777 1.0000 Uani C26 0.4526(12) 0.4500(8) 0.6762(5) 0.0683 1.0000 Uani P1 0.0862(3) 0.2654(2) 0.6804(1) 0.0430 1.0000 Uani C111 0.1295(10) 0.2805(6) 0.7488(3) 0.0452 1.0000 Uani C112 0.2516(10) 0.2869(7) 0.7736(4) 0.0503 1.0000 Uani C113 0.2881(12) 0.2973(8) 0.8256(4) 0.0642 1.0000 Uani C114 0.1976(13) 0.2996(8) 0.8545(4) 0.0700 1.0000 Uani C115 0.0692(14) 0.2914(8) 0.8307(4) 0.0651 1.0000 Uani C116 0.0321(12) 0.2803(8) 0.7785(4) 0.0621 1.0000 Uani C121 -0.0714(11) 0.1653(7) 0.6718(4) 0.0561 1.0000 Uani C122 -0.1981(12) 0.1724(9) 0.6594(5) 0.0779 1.0000 Uani C123 -0.3091(15) 0.0907(11) 0.6527(6) 0.1063 1.0000 Uani C124 -0.2954(17) 0.0090(11) 0.6589(6) 0.1051 1.0000 Uani C125 -0.1781(18) 0.0004(10) 0.6723(7) 0.1034 1.0000 Uani C126 -0.0595(14) 0.0800(8) 0.6777(6) 0.0823 1.0000 Uani C131 0.0356(10) 0.3625(7) 0.6582(4) 0.0490 1.0000 Uani C132 -0.0324(12) 0.3622(8) 0.6092(4) 0.0612 1.0000 Uani C133 -0.0612(13) 0.4384(9) 0.5892(4) 0.0722 1.0000 Uani C134 -0.0165(14) 0.5173(9) 0.6182(5) 0.0811 1.0000 Uani C135 0.0526(14) 0.5203(8) 0.6663(5) 0.0786 1.0000 Uani C136 0.0821(12) 0.4439(7) 0.6871(4) 0.0625 1.0000 Uani P2 0.2166(3) 0.2719(2) 0.5536(1) 0.0551 1.0000 Uani C211 0.0484(12) 0.2220(10) 0.5195(4) 0.0690 1.0000 Uani C212 -0.0205(12) 0.2723(11) 0.4881(4) 0.0744 1.0000 Uani C213 -0.1537(15) 0.2255(15) 0.4635(5) 0.0923 1.0000 Uani C214 -0.2194(18) 0.1343(17) 0.4704(9) 0.1443 1.0000 Uani C215 -0.1479(19) 0.0857(14) 0.5008(12) 0.1578 1.0000 Uani C216 -0.0176(17) 0.1305(12) 0.5266(8) 0.1209 1.0000 Uani C221 0.3067(12) 0.2177(10) 0.5223(4) 0.0670 1.0000 Uani C222 0.2661(18) 0.1890(17) 0.4722(5) 0.1017 1.0000 Uani C223 0.3442(21) 0.1529(21) 0.4496(6) 0.1241 1.0000 Uani C224 0.4526(21) 0.1422(19) 0.4760(7) 0.1216 1.0000 Uani C225 0.4944(14) 0.1680(12) 0.5254(6) 0.0914 1.0000 Uani C226 0.4206(11) 0.2064(9) 0.5494(4) 0.0673 1.0000 Uani C231 0.2742(11) 0.3910(9) 0.5312(4) 0.0633 1.0000 Uani C232 0.3146(12) 0.4178(12) 0.4848(5) 0.0805 1.0000 Uani C233 0.3552(15) 0.5067(16) 0.4709(6) 0.0988 1.0000 Uani C234 0.3539(15) 0.5687(13) 0.5026(9) 0.1061 1.0000 Uani C235 0.3128(16) 0.5499(11) 0.5478(7) 0.1090 1.0000 Uani C236 0.2701(14) 0.4582(9) 0.5623(5) 0.0830 1.0000 Uani CU2 0.1552(1) 0.2199(1) 0.1455(1) 0.0452 1.0000 Uani N31 0.1940(8) 0.0995(6) 0.1597(3) 0.0508 1.0000 Uani N32 0.1189(10) 0.0319(6) 0.1248(4) 0.0719 1.0000 Uani C33 0.1324(14) -0.0500(9) 0.1321(6) 0.0857 1.0000 Uani C34 0.2110(15) -0.0709(9) 0.1734(6) 0.0873 1.0000 Uani C35 0.2837(14) -0.0017(10) 0.2072(5) 0.0854 1.0000 Uani C36 0.2702(12) 0.0834(9) 0.1994(4) 0.0684 1.0000 Uani N41 0.3374(9) 0.3208(6) 0.1769(3) 0.0606 1.0000 Uani N42 0.4483(10) 0.2997(6) 0.1770(4) 0.0725 1.0000 Uani C43 0.5664(13) 0.3676(9) 0.1855(5) 0.0812 1.0000 Uani C44 0.5836(13) 0.4581(9) 0.1936(5) 0.0832 1.0000 Uani C45 0.4709(13) 0.4785(8) 0.1939(5) 0.0765 1.0000 Uani C46 0.3507(11) 0.4064(8) 0.1856(4) 0.0654 1.0000 Uani P3 0.1655(3) 0.2550(2) 0.0624(1) 0.0490 1.0000 Uani C311 0.0049(10) 0.2226(8) 0.0190(4) 0.0516 1.0000 Uani C312 -0.0876(12) 0.1370(9) 0.0256(5) 0.0782 1.0000 Uani C313 -0.2105(15) 0.1080(11) -0.0086(6) 0.1082 1.0000 Uani C314 -0.2318(15) 0.1696(14) -0.0472(5) 0.0965 1.0000 Uani C315 -0.1397(15) 0.2518(11) -0.0525(5) 0.0938 1.0000 Uani C316 -0.0243(13) 0.2782(9) -0.0202(4) 0.0705 1.0000 Uani C321 0.2435(11) 0.3780(7) 0.0566(4) 0.0590 1.0000 Uani C322 0.3689(17) 0.4228(10) 0.0479(6) 0.1026 1.0000 Uani C323 0.4342(18) 0.5181(12) 0.0528(7) 0.1164 1.0000 Uani C324 0.3603(18) 0.5709(9) 0.0606(7) 0.1076 1.0000 Uani C325 0.2434(19) 0.5296(9) 0.0720(6) 0.1043 1.0000 Uani C326 0.1787(16) 0.4355(9) 0.0695(6) 0.0897 1.0000 Uani C331 0.2638(11) 0.2088(7) 0.0303(4) 0.0563 1.0000 Uani C332 0.2311(15) 0.1863(11) -0.0199(4) 0.0804 1.0000 Uani C333 0.3110(19) 0.1529(13) -0.0433(5) 0.0993 1.0000 Uani C334 0.4223(16) 0.1434(12) -0.0157(6) 0.0966 1.0000 Uani C335 0.4571(13) 0.1645(11) 0.0348(6) 0.0908 1.0000 Uani C336 0.3758(12) 0.1955(10) 0.0588(5) 0.0768 1.0000 Uani P4 -0.0202(3) 0.2234(2) 0.1783(1) 0.0434 1.0000 Uani C411 -0.1703(11) 0.1192(7) 0.1697(4) 0.0559 1.0000 Uani C412 -0.1488(13) 0.0366(8) 0.1770(5) 0.0755 1.0000 Uani C413 -0.2578(18) -0.0453(9) 0.1724(6) 0.0965 1.0000 Uani C414 -0.3828(19) -0.0452(12) 0.1597(6) 0.1047 1.0000 Uani C415 -0.4067(14) 0.0311(12) 0.1534(6) 0.1026 1.0000 Uani C416 -0.3009(13) 0.1182(10) 0.1579(5) 0.0881 1.0000 Uani C421 0.0097(10) 0.2402(6) 0.2466(3) 0.0456 1.0000 Uani C422 0.1313(10) 0.2441(7) 0.2743(4) 0.0533 1.0000 Uani C423 0.1552(11) 0.2513(8) 0.3277(4) 0.0630 1.0000 Uani C424 0.0541(12) 0.2532(8) 0.3528(4) 0.0617 1.0000 Uani C425 -0.0654(12) 0.2499(8) 0.3248(4) 0.0609 1.0000 Uani C426 -0.0906(11) 0.2419(7) 0.2724(4) 0.0551 1.0000 Uani C431 -0.0789(9) 0.3163(7) 0.1525(4) 0.0494 1.0000 Uani C432 -0.0333(11) 0.4002(7) 0.1789(5) 0.0655 1.0000 Uani C433 -0.0668(15) 0.4743(8) 0.1565(6) 0.0821 1.0000 Uani C434 -0.1451(15) 0.4632(10) 0.1092(6) 0.0905 1.0000 Uani C435 -0.1904(14) 0.3804(10) 0.0835(5) 0.0890 1.0000 Uani C436 -0.1557(12) 0.3077(8) 0.1046(4) 0.0669 1.0000 Uani B1 0.5553(16) 0.2495(12) 0.3174(6) 0.0837 1.0000 Uani F11 0.5828(13) 0.2053(10) 0.2804(4) 0.1591 1.0000 Uani F12 0.6018(12) 0.2191(9) 0.3603(4) 0.1549 1.0000 Uani F13 0.4352(9) 0.2395(10) 0.3074(4) 0.1418 1.0000 Uani F14 0.6284(16) 0.3359(8) 0.3103(6) 0.2122 1.0000 Uani B2 0.6664(17) 0.2961(12) 0.8040(6) 0.0861 1.0000 Uani F21 0.5781(10) 0.3282(8) 0.7830(4) 0.1251 1.0000 Uani F22 0.6697(13) 0.2304(9) 0.7739(5) 0.1639 1.0000 Uani F23 0.6356(17) 0.2608(9) 0.8493(5) 0.1998 1.0000 Uani F24 0.7843(12) 0.3566(12) 0.8148(8) 0.2239 1.0000 Uani H13 0.1779 -0.0690 0.6238 0.0700 1.0000 Uiso H14 0.3373 -0.0815 0.6942 0.0700 1.0000 Uiso H15 0.4759 0.0561 0.7405 0.0700 1.0000 Uiso H16 0.4369 0.1928 0.7177 0.0700 1.0000 Uiso H23 0.7403 0.3915 0.6687 0.0700 1.0000 Uiso H24 0.7798 0.5444 0.6877 0.0700 1.0000 Uiso H25 0.5859 0.5851 0.6943 0.0700 1.0000 Uiso H26 0.3676 0.4612 0.6788 0.0700 1.0000 Uiso H112 0.3215 0.2830 0.7547 0.0700 1.0000 Uiso H113 0.3802 0.3032 0.8426 0.0700 1.0000 Uiso H114 0.2232 0.3084 0.8919 0.0700 1.0000 Uiso H115 0.0017 0.2932 0.8517 0.0700 1.0000 Uiso H116 -0.0616 0.2722 0.7616 0.0700 1.0000 Uiso H122 -0.2087 0.2315 0.6556 0.0700 1.0000 Uiso H123 -0.4044 0.0957 0.6445 0.0700 1.0000 Uiso H124 -0.3777 -0.0488 0.6534 0.0700 1.0000 Uiso H125 -0.1696 -0.0623 0.6793 0.0700 1.0000 Uiso H126 0.0315 0.0755 0.6846 0.0700 1.0000 Uiso H132 -0.0615 0.3056 0.5888 0.0700 1.0000 Uiso H133 -0.1045 0.4376 0.5535 0.0700 1.0000 Uiso H134 -0.0380 0.5725 0.6040 0.0700 1.0000 Uiso H135 0.0833 0.5780 0.6872 0.0700 1.0000 Uiso H136 0.1346 0.4468 0.7222 0.0700 1.0000 Uiso H212 0.0230 0.3405 0.4843 0.0700 1.0000 Uiso H213 -0.2001 0.2608 0.4392 0.0700 1.0000 Uiso H214 -0.3091 0.1021 0.4529 0.0700 1.0000 Uiso H215 -0.1905 0.0180 0.5036 0.0700 1.0000 Uiso H216 0.0289 0.0957 0.5504 0.0700 1.0000 Uiso H222 0.1821 0.1945 0.4523 0.0700 1.0000 Uiso H223 0.3140 0.1309 0.4136 0.0700 1.0000 Uiso H224 0.5056 0.1160 0.4592 0.0700 1.0000 Uiso H225 0.5760 0.1596 0.5439 0.0700 1.0000 Uiso H226 0.4480 0.2247 0.5863 0.0700 1.0000 Uiso H232 0.3142 0.3678 0.4615 0.0700 1.0000 Uiso H233 0.3845 0.5262 0.4355 0.0700 1.0000 Uiso H234 0.3870 0.6395 0.4923 0.0700 1.0000 Uiso H235 0.3126 0.5996 0.5717 0.0700 1.0000 Uiso H236 0.2388 0.4403 0.5956 0.0700 1.0000 Uiso H33 0.0833 -0.0979 0.1058 0.0700 1.0000 Uiso H34 0.2145 -0.1338 0.1774 0.0700 1.0000 Uiso H35 0.3434 -0.0135 0.2376 0.0700 1.0000 Uiso H36 0.3175 0.1338 0.2251 0.0700 1.0000 Uiso H43 0.6481 0.3510 0.1856 0.0700 1.0000 Uiso H44 0.6766 0.5067 0.1989 0.0700 1.0000 Uiso H45 0.4788 0.5436 0.2006 0.0700 1.0000 Uiso H46 0.2655 0.4169 0.1855 0.0700 1.0000 Uiso H312 -0.0661 0.0959 0.0530 0.0700 1.0000 Uiso H313 -0.2795 0.0450 -0.0064 0.0700 1.0000 Uiso H314 -0.3208 0.1519 -0.0705 0.0700 1.0000 Uiso H315 -0.1540 0.2947 -0.0813 0.0700 1.0000 Uiso H316 0.0399 0.3381 -0.0244 0.0700 1.0000 Uiso H322 0.4195 0.3858 0.0381 0.0700 1.0000 Uiso H323 0.5324 0.5478 0.0512 0.0700 1.0000 Uiso H324 0.3956 0.6391 0.0577 0.0700 1.0000 Uiso H325 0.1964 0.5678 0.0826 0.0700 1.0000 Uiso H326 0.0829 0.4074 0.0769 0.0700 1.0000 Uiso H332 0.1452 0.1891 -0.0384 0.0700 1.0000 Uiso H333 0.2868 0.1385 -0.0810 0.0700 1.0000 Uiso H334 0.4800 0.1200 -0.0316 0.0700 1.0000 Uiso H335 0.5407 0.1579 0.0551 0.0700 1.0000 Uiso H336 0.3986 0.2086 0.0968 0.0700 1.0000 Uiso H412 -0.0558 0.0396 0.1845 0.0700 1.0000 Uiso H413 -0.2372 -0.1048 0.1802 0.0700 1.0000 Uiso H414 -0.4607 -0.1086 0.1552 0.0700 1.0000 Uiso H415 -0.5057 0.0325 0.1467 0.0700 1.0000 Uiso H416 -0.3230 0.1719 0.1511 0.0700 1.0000 Uiso H422 0.2097 0.2438 0.2611 0.0700 1.0000 Uiso H423 0.2433 0.2529 0.3459 0.0700 1.0000 Uiso H424 0.0696 0.2584 0.3906 0.0700 1.0000 Uiso H425 -0.1402 0.2524 0.3417 0.0700 1.0000 Uiso H426 -0.1744 0.2395 0.2532 0.0700 1.0000 Uiso H432 0.0239 0.4076 0.2135 0.0700 1.0000 Uiso H433 -0.0376 0.5337 0.1750 0.0700 1.0000 Uiso H434 -0.1673 0.5164 0.0932 0.0700 1.0000 Uiso H435 -0.2484 0.3722 0.0492 0.0700 1.0000 Uiso H436 -0.1810 0.2508 0.0857 0.0700 1.0000 Uiso 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 0.0569(8) 0.0478(7) 0.0425(7) 0.0014(5) 0.0088(6) 0.0286(6) N11 0.0483(52) 0.0561(53) 0.0666(56) 0.0032(43) 0.0186(42) 0.0306(43) N12 0.1196(94) 0.0530(62) 0.0980(82) -0.0125(57) 0.0180(69) 0.0276(62) C13 0.133(14) 0.0476(77) 0.185(17) -0.0099(90) 0.070(13) 0.0225(85) C14 0.132(13) 0.0764(98) 0.223(18) 0.070(11) 0.093(13) 0.0771(97) C15 0.102(11) 0.104(11) 0.130(13) 0.0537(96) 0.0463(95) 0.0725(94) C16 0.0853(87) 0.0738(80) 0.0686(76) 0.0185(62) 0.0182(64) 0.0539(71) N21 0.0621(58) 0.0540(53) 0.0561(53) -0.0065(42) 0.0079(44) 0.0163(45) N22 0.0596(61) 0.0591(58) 0.0777(65) -0.0031(48) 0.0162(49) 0.0179(48) C23 0.0625(81) 0.0687(82) 0.0969(95) -0.0045(69) 0.0210(69) 0.0193(65) C24 0.0822(91) 0.0685(84) 0.0901(94) -0.0110(70) 0.0239(73) 0.0074(69) C25 0.0847(96) 0.0590(77) 0.0958(95) -0.0183(68) 0.0224(75) 0.0119(69) C26 0.0720(81) 0.0569(72) 0.0818(84) -0.0114(62) 0.0174(65) 0.0194(62) P1 0.0516(16) 0.0411(14) 0.0449(15) 0.0013(11) 0.0127(12) 0.0221(12) C111 0.0666(69) 0.0424(55) 0.0416(53) -0.0014(43) 0.0096(48) 0.0288(51) C112 0.0513(63) 0.0540(62) 0.0558(62) -0.0024(49) 0.0105(49) 0.0264(51) C113 0.0777(82) 0.0641(72) 0.0563(69) -0.0028(56) 0.0042(59) 0.0310(63) C114 0.111(10) 0.0667(76) 0.0493(67) 0.0001(57) 0.0103(65) 0.0368(73) C115 0.131(11) 0.0661(78) 0.0538(71) 0.0043(59) 0.0471(73) 0.0431(77) C116 0.0749(79) 0.0623(72) 0.0586(70) 0.0002(56) 0.0246(59) 0.0240(61) C121 0.0744(79) 0.0496(63) 0.0558(65) -0.0102(51) 0.0260(57) 0.0122(56) C122 0.0564(81) 0.0799(91) 0.0936(95) -0.0004(73) 0.0164(68) 0.0029(67) C123 0.090(11) 0.128(13) 0.099(11) 0.0007(96) 0.0295(88) 0.0028(95) C124 0.115(13) 0.099(12) 0.119(13) -0.041(10) 0.047(11) -0.022(10) C125 0.176(17) 0.0544(90) 0.166(15) -0.0260(93) 0.099(13) 0.0004(97) C126 0.102(11) 0.0546(79) 0.134(12) -0.0070(77) 0.0630(93) 0.0173(74) C131 0.0542(64) 0.0505(61) 0.0616(66) 0.0040(50) 0.0173(51) 0.0304(52) C132 0.0799(82) 0.0801(80) 0.0499(64) 0.0029(57) 0.0105(57) 0.0488(68) C133 0.0941(96) 0.109(11) 0.0642(76) 0.0199(70) 0.0229(67) 0.0691(85) C134 0.124(12) 0.0869(94) 0.0901(98) 0.0269(77) 0.0283(85) 0.0722(90) C135 0.118(11) 0.0566(73) 0.0900(96) 0.0045(66) 0.0112(82) 0.0456(76) C136 0.0836(85) 0.0470(63) 0.0724(77) -0.0010(55) 0.0022(63) 0.0327(61) P2 0.0638(19) 0.0846(22) 0.0388(15) 0.0016(14) 0.0056(13) 0.0411(17) C211 0.0664(81) 0.122(11) 0.0557(71) -0.0340(70) 0.0056(59) 0.0441(77) C212 0.0726(86) 0.163(14) 0.0465(67) -0.0100(77) 0.0011(59) 0.0643(92) C213 0.112(12) 0.269(24) 0.0609(86) -0.049(12) -0.0222(78) 0.131(14) C214 0.091(14) 0.298(27) 0.281(26) -0.191(22) -0.071(15) 0.105(17) C215 0.107(15) 0.126(18) 0.406(39) -0.123(22) -0.063(19) 0.043(13) C216 0.101(13) 0.112(13) 0.212(20) -0.066(13) -0.063(13) 0.043(11) C221 0.0794(87) 0.149(13) 0.0407(63) -0.0119(70) 0.0017(58) 0.0721(88) C222 0.157(16) 0.365(30) 0.0645(96) -0.067(14) -0.0276(97) 0.200(19) C223 0.182(20) 0.486(42) 0.093(13) -0.115(19) -0.026(12) 0.212(25) C224 0.187(20) 0.373(33) 0.105(13) -0.066(17) 0.008(13) 0.212(23) C225 0.094(11) 0.163(15) 0.098(11) 0.001(10) 0.0184(86) 0.090(11) C226 0.063(77) 0.1008(96) 0.0640(73) 0.0064(66) 0.0163(59) 0.0457(72) C231 0.0454(66) 0.118(10) 0.0615(75) 0.0382(71) 0.0111(55) 0.0318(66) C232 0.0508(82) 0.221(16) 0.0806(98) 0.077(10) 0.0226(70) 0.0546(92) C233 0.067(10) 0.222(26) 0.143(13) 0.122(15) 0.0287(90) 0.064(13) C234 0.072(11) 0.216(17) 0.203(25) 0.159(18) 0.046(13) 0.062(11) C235 0.103(12) 0.081(11) 0.201(16) 0.059(11) 0.013(11) 0.0370(97) C236 0.093(10) 0.0710(90) 0.107(10) 0.0366(78) 0.0104(80) 0.0320(77) CU2 0.0552(8) 0.0451(7) 0.0422(7) 0.0008(5) 0.0096(6) 0.0233(6) N31 0.0485(51) 0.0640(56) 0.0583(53) -0.0035(43) 0.0067(41) 0.0333(45) N32 0.0895(75) 0.0601(61) 0.0897(75) -0.0187(54) -0.0046(59) 0.0398(56) C33 0.090(10) 0.0598(79) 0.150(14) -0.0196(83) 0.0285(94) 0.0320(74) C34 0.120(12) 0.0731(95) 0.173(15) 0.0456(95) 0.062(11) 0.0686(90) C35 0.099(11) 0.116(12) 0.107(11) 0.0403(91) 0.0254(87) 0.0764(95) C36 0.0795(86) 0.0888(89) 0.0648(75) 0.0121(65) 0.0119(63) 0.0523(73) N41 0.0673(61) 0.0567(56) 0.0585(55) -0.0070(44) 0.0101(45) 0.0199(47) N42 0.0800(71) 0.0590(60) 0.0791(68) -0.0046(50) 0.0047(55) 0.0243(53) C43 0.0720(90) 0.0720(88) 0.0991(99) -0.0074(73) 0.0023(73) 0.0237(72) C44 0.0876(97) 0.0651(83) 0.0884(95) -0.0120(70) 0.0058(75) 0.0027(71) C45 0.0844(94) 0.0605(77) 0.0898(90) -0.0169(66) 0.0135(72) 0.0199(68) C46 0.0690(79) 0.0616(74) 0.0706(76) -0.0134(59) 0.0162(61) 0.0194(61) P3 0.0614(18) 0.0523(16) 0.0436(15) 0.0047(12) 0.0153(13) 0.0265(14) C311 0.0454(63) 0.0856(81) 0.0496(61) -0.0020(55) 0.0088(48) 0.0371(59) C312 0.0738(87) 0.0793(90) 0.0732(83) -0.0044(68) 0.0033(66) 0.0168(71) C313 0.083(11) 0.128(14) 0.113(12) -0.039(10) 0.0049(90) 0.0025(95) C314 0.118(12) 0.237(21) 0.0642(88) -0.028(11) -0.0184(80) 0.124(14) C315 0.116(13) 0.151(14) 0.089(10) -0.0027(94) 0.0085(89) 0.097(12) C316 0.0843(91) 0.107(10) 0.0604(74) 0.0002(68) 0.0009(64) 0.0639(81) C321 0.0628(73) 0.0575(68) 0.0650(71) 0.0107(55) 0.0284(57) 0.0162(57) C322 0.149(15) 0.0731(97) 0.143(14) 0.0000(92) 0.092(12) 0.0122(96) C323 0.131(15) 0.097(13) 0.162(16) -0.000(11) 0.083(13) -0.019(11) C324 0.167(17) 0.0611(90) 0.153(15) 0.0225(93) 0.084(13) 0.0198(99) C325 0.204(18) 0.0587(89) 0.135(14) 0.0134(88) 0.067(13) 0.058(11) C326 0.151(14) 0.0624(87) 0.123(12) 0.0119(81) 0.066(11) 0.0527(93) C331 0.0735(77) 0.0659(71) 0.0459(60) -0.0005(52) 0.0151(54) 0.0350(61) C332 0.136(13) 0.155(14) 0.0448(71) -0.0085(79) 0.0006(74) 0.105(11) C333 0.180(17) 0.205(19) 0.0570(85) -0.013(10) 0.0270(97) 0.132(16) C334 0.137(14) 0.164(16) 0.090(11) 0.006(10) 0.0451(99) 0.104(13) C335 0.0746(94) 0.140(13) 0.110(12) -0.0240(97) 0.0113(81) 0.0615(93) C336 0.0655(82) 0.114(11) 0.0733(83) -0.0205(75) 0.0021(64) 0.0420(77) P4 0.0517(16) 0.0401(14) 0.0438(14) -0.0004(11) 0.0127(12) 0.0186(12) C411 0.0761(79) 0.0514(65) 0.0451(60) -0.0074(49) 0.0199(54) 0.0071(57) C412 0.103(10) 0.0465(73) 0.120(11) -0.0026(71) 0.0644(87) 0.0116(68) C413 0.204(17) 0.0471(88) 0.149(14) -0.0239(89) 0.113(13) -0.0139(97) C414 0.143(17) 0.101(13) 0.101(13) -0.043(10) 0.050(12) -0.028(12) C415 0.0714(99) 0.162(15) 0.100(12) -0.010(10) 0.0074(85) -0.0486(95) C416 0.0727(94) 0.093(10) 0.0902(96) 0.0144(78) 0.0117(74) 0.0020(77) C421 0.0649(68) 0.0386(54) 0.0431(54) 0.0006(43) 0.0130(48) 0.0223(50) C422 0.0574(68) 0.0596(66) 0.0536(63) 0.0001(51) 0.0149(51) 0.0279(55) C423 0.0710(78) 0.0715(75) 0.0575(69) -0.0003(57) 0.0071(57) 0.0364(63) C424 0.0830(85) 0.0693(75) 0.0500(64) -0.0002(55) 0.0123(58) 0.0393(66) C425 0.0900(87) 0.0590(69) 0.0600(70) 0.0021(55) 0.0305(62) 0.0357(64) C426 0.0702(74) 0.0602(67) 0.0494(63) -0.0022(51) 0.0179(54) 0.0301(58) C431 0.0423(59) 0.0546(63) 0.0639(67) 0.0082(51) 0.0170(49) 0.0228(50) C432 0.0701(78) 0.0521(69) 0.0874(86) 0.0006(61) 0.0158(64) 0.0281(60) C433 0.119(12) 0.0626(78) 0.117(12) 0.0124(76) 0.0363(94) 0.0545(81) C434 0.123(12) 0.097(11) 0.123(12) 0.0457(92) 0.0419(99) 0.0759(99) C435 0.106(11) 0.121(12) 0.0844(98) 0.0273(88) 0.0158(83) 0.0728(98) C436 0.0856(87) 0.0783(82) 0.0574(71) 0.0101(61) 0.0113(62) 0.0462(70) B1 0.075(11) 0.105(13) 0.092(12) -0.0097(96) 0.0052(86) 0.0481(95) F11 0.256(14) 0.347(18) 0.1314(88) -0.0057(98) 0.0136(87) 0.249(14) F12 0.223(12) 0.279(15) 0.0875(69) 0.0325(80) -0.0020(72) 0.153(11) F13 0.0884(69) 0.326(17) 0.187(11) -0.043(11) -0.0005(67) 0.1228(91) F14 0.264(17) 0.1088(91) 0.304(19) 0.023(11) -0.036(14) -0.0372(99) B2 0.105(13) 0.111(14) 0.078(11) -0.0182(97) -0.0321(93) 0.062(11) F21 0.1737(96) 0.230(12) 0.1277(76) -0.0098(75) 0.0006(67) 0.1637(94) F22 0.244(14) 0.224(13) 0.233(13) -0.115(11) -0.078(11) 0.182(12) F23 0.352(20) 0.190(13) 0.138(10) 0.0355(91) -0.072(11) 0.071(13) F24 0.0998(93) 0.304(20) 0.436(27) -0.172(19) 0.051(12) -0.039(11) 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 CU1 . N11 . 2.066(8) yes CU1 . N21 . 2.112(8) yes CU1 . P1 . 2.255(3) yes CU1 . P2 . 2.268(3) yes N11 . N12 . 1.37(1) yes N11 . C16 . 1.29(1) yes N12 . C13 . 1.35(2) yes C13 . C14 . 1.39(2) yes C14 . C15 . 1.33(2) yes C15 . C16 . 1.36(2) yes N21 . N22 . 1.35(1) yes N21 . C26 . 1.33(1) yes N22 . C23 . 1.32(2) yes C23 . C24 . 1.37(2) yes C24 . C25 . 1.36(2) yes C25 . C26 . 1.39(2) yes P1 . C111 . 1.813(9) yes P1 . C121 . 1.838(11) yes P1 . C131 . 1.816(9) yes C111 . C112 . 1.34(1) yes C111 . C116 . 1.43(1) yes C112 . C113 . 1.38(1) yes C113 . C114 . 1.36(2) yes C114 . C115 . 1.38(2) yes C115 . C116 . 1.38(2) yes C121 . C122 . 1.39(2) yes C121 . C126 . 1.37(2) yes C122 . C123 . 1.39(2) yes C123 . C124 . 1.33(3) yes C124 . C125 . 1.31(3) yes C125 . C126 . 1.42(2) yes C131 . C132 . 1.38(1) yes C131 . C136 . 1.40(1) yes C132 . C133 . 1.38(2) yes C133 . C134 . 1.37(2) yes C134 . C135 . 1.36(2) yes C135 . C136 . 1.40(2) yes P2 . C211 . 1.79(1) yes P2 . C221 . 1.82(1) yes P2 . C231 . 1.83(1) yes C211 . C212 . 1.41(2) yes C211 . C216 . 1.36(2) yes C212 . C213 . 1.41(2) yes C213 . C214 . 1.36(3) yes C214 . C215 . 1.40(3) yes C215 . C216 . 1.40(2) yes C221 . C222 . 1.38(2) yes C221 . C226 . 1.38(2) yes C222 . C223 . 1.40(2) yes C223 . C224 . 1.31(2) yes C224 . C225 . 1.35(2) yes C225 . C226 . 1.40(1) yes C231 . C232 . 1.38(2) yes C231 . C236 . 1.39(2) yes C232 . C233 . 1.34(2) yes C233 . C234 . 1.32(3) yes C234 . C235 . 1.34(3) yes C235 . C236 . 1.39(2) yes CU2 . N31 . 2.059(8) yes CU2 . N41 . 2.094(9) yes CU2 . P3 . 2.271(3) yes CU2 . P4 . 2.248(3) yes N31 . N32 . 1.36(1) yes N31 . C36 . 1.29(1) yes N32 . C33 . 1.33(2) yes C33 . C34 . 1.37(2) yes C34 . C35 . 1.36(2) yes C35 . C36 . 1.38(2) yes N41 . N42 . 1.35(1) yes N41 . C46 . 1.31(1) yes N42 . C43 . 1.32(2) yes C43 . C44 . 1.37(2) yes C44 . C45 . 1.37(2) yes C45 . C46 . 1.37(2) yes P3 . C311 . 1.83(1) yes P3 . C321 . 1.80(1) yes P3 . C331 . 1.82(1) yes C311 . C312 . 1.37(2) yes C311 . C316 . 1.39(2) yes C312 . C313 . 1.41(2) yes C313 . C314 . 1.41(2) yes C314 . C315 . 1.33(2) yes C315 . C316 . 1.33(2) yes C321 . C322 . 1.34(2) yes C321 . C326 . 1.41(2) yes C322 . C323 . 1.40(2) yes C323 . C324 . 1.38(3) yes C324 . C325 . 1.28(2) yes C325 . C326 . 1.38(2) yes C331 . C332 . 1.36(2) yes C331 . C336 . 1.39(2) yes C332 . C333 . 1.40(2) yes C333 . C334 . 1.35(2) yes C334 . C335 . 1.36(2) yes C335 . C336 . 1.40(2) yes P4 . C411 . 1.83(1) yes P4 . C421 . 1.812(9) yes P4 . C431 . 1.83(1) yes C411 . C412 . 1.38(2) yes C411 . C416 . 1.39(1) yes C412 . C413 . 1.38(2) yes C413 . C414 . 1.33(3) yes C414 . C415 . 1.30(3) yes C415 . C416 . 1.42(2) yes C421 . C422 . 1.37(1) yes C421 . C426 . 1.39(1) yes C422 . C423 . 1.41(2) yes C423 . C424 . 1.39(2) yes C424 . C425 . 1.36(2) yes C425 . C426 . 1.38(2) yes C431 . C432 . 1.40(2) yes C431 . C436 . 1.38(2) yes C432 . C433 . 1.40(2) yes C433 . C434 . 1.37(2) yes C434 . C435 . 1.37(2) yes C435 . C436 . 1.37(2) yes B1 . F11 . 1.37(2) yes B1 . F12 . 1.30(2) yes B1 . F13 . 1.23(2) yes B1 . F14 . 1.31(2) yes B2 . F21 . 1.26(2) yes B2 . F22 . 1.35(2) yes B2 . F23 . 1.35(2) yes B2 . F24 . 1.28(2) yes 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 P1 . CU1 . N11 . 115.0(2) yes N11 . CU1 . N21 . 101.1(3) yes N11 . CU1 . P1 . 110.7(2) yes N21 . CU1 . P1 . 112.6(2) yes N11 . CU1 . P2 . 108.4(2) yes N21 . CU1 . P2 . 104.2(3) yes P1 . CU1 . P2 . 118.3(1) yes CU1 . N11 . N12 . 113.5(6) yes CU1 . N11 . C16 . 125.4(2) yes N12 . N11 . C16 . 120.7(9) yes N11 . N12 . C13 . 114(1) yes N12 . C13 . C14 . 126(1) yes C13 . C14 . C15 . 116(1) yes C14 . C15 . C16 . 118(1) yes N11 . C16 . C15 . 125(1) yes CU1 . N21 . N22 . 114.6(6) yes CU1 . N21 . C26 . 125.0(7) yes N22 . N21 . C26 . 119.7(9) yes N21 . N22 . C23 . 116.9(9) yes N22 . C23 . C24 . 126(1) yes C23 . C24 . C25 . 117(1) yes C24 . C25 . C26 . 116(1) yes N21 . C26 . C25 . 124(1) yes CU1 . P1 . C111 . 116.7(3) yes CU1 . P1 . C121 . 116.6(3) yes C111 . P1 . C121 . 103.2(5) yes CU1 . P1 . C131 . 110.0(3) yes C111 . P1 . C131 . 104.4(4) yes C121 . P1 . C131 . 104.4(5) yes P1 . C111 . C112 . 121.1(7) yes P1 . C111 . C116 . 121.1(8) yes C112 . C111 . C116 . 117.6(9) yes C111 . C112 . C113 . 123(1) yes C112 . C113 . C114 . 120(1) yes C113 . C114 . C115 . 119(1) yes C114 . C115 . C116 . 121(1) yes C111 . C116 . C115 . 119(1) yes P1 . C121 . C122 . 123.6(9) yes P1 . C121 . C126 . 116.5(9) yes C122 . C121 . C126 . 120(1) yes C121 . C122 . C123 . 118(1) yes C122 . C123 . C124 . 122(1) yes C123 . C124 . C125 . 122(1) yes C124 . C125 . C126 . 120(1) yes C121 . C126 . C125 . 119(1) yes P1 . C131 . C132 . 119.9(8) yes P1 . C131 . C136 . 120.7(8) yes C132 . C131 . C136 . 118.6(9) yes C131 . C132 . C133 . 122(1) yes C132 . C133 . C134 . 119(1) yes C133 . C134 . C135 . 121(1) yes C134 . C135 . C136 . 121(1) yes C131 . C136 . C135 . 119(1) yes CU1 . P2 . C211 . 117.6(4) yes CU1 . P2 . C221 . 114.5(4) yes C211 . P2 . C221 . 101.8(5) yes CU1 . P2 . C231 . 113.7(4) yes C211 . P2 . C231 . 104.2(6) yes C221 . P2 . C231 . 103.2(6) yes P2 . C211 . C212 . 124(1) yes P2 . C211 . C216 . 117(1) yes C212 . C211 . C216 . 119(1) yes C211 . C212 . C213 . 119(1) yes C212 . C213 . C214 . 122(1) yes C213 . C214 . C215 . 118(1) yes C214 . C215 . C216 . 121(2) yes C211 . C216 . C215 . 120(2) yes P2 . C221 . C222 . 122.4(9) yes P2 . C221 . C226 . 118.8(8) yes C222 . C221 . C226 . 119(1) yes C221 . C222 . C223 . 119(1) yes C222 . C223 . C224 . 121(1) yes C223 . C224 . C225 . 121(1) yes C224 . C225 . C226 . 120(1) yes C221 . C226 . C225 . 120(1) yes P2 . C231 . C232 . 125(1) yes P2 . C231 . C236 . 116.9(8) yes C232 . C231 . C236 . 118(1) yes C231 . C232 . C233 . 122(1) yes C232 . C233 . C234 . 118(1) yes C233 . C234 . C235 . 125(2) yes C234 . C235 . C236 . 117(2) yes C231 . C236 . C235 . 120(1) yes N31 . CU2 . N41 . 102.8(3) yes N31 . CU2 . P3 . 107.7(2) yes N41 . CU2 . P3 . 97.6(3) yes N31 . CU2 . P4 . 113.8(2) yes N41 . CU2 . P4 . 113.0(3) yes P3 . CU2 . P4 . 119.6(1) yes CU2 . N31 . N32 . 112.7(6) yes CU2 . N31 . C36 . 125.6(8) yes N32 . N31 . C36 . 121.3(9) yes N31 . N32 . C33 . 117(1) yes N32 . C33 . C34 . 124(1) yes C33 . C34 . C35 . 117(1) yes C34 . C35 . C36 . 119(1) yes N31 . C36 . C35 . 122(1) yes CU2 . N41 . N42 . 115.4(6) yes CU2 . N41 . C46 . 123.6(8) yes N42 . N41 . C46 . 119.3(9) yes N41 . N42 . C43 . 117.7(9) yes N42 . C43 . C44 . 124(1) yes C43 . C44 . C45 . 117(1) yes C44 . C45 . C46 . 117(1) yes N41 . C46 . C45 . 125(1) yes CU2 . P3 . C311 . 116.1(4) yes CU2 . P3 . C321 . 109.2(4) yes C311 . P3 . C321 . 105.9(5) yes CU2 . P3 . C331 . 118.3(3) yes C311 . P3 . C331 . 102.5(2) yes C321 . P3 . C331 . 103.6(5) yes P3 . C311 . C312 . 116.6(8) yes P3 . C311 . C316 . 123.3(9) yes C312 . C311 . C316 . 120(1) yes C311 . C312 . C313 . 118(1) yes C312 . C313 . C314 . 118(1) yes C313 . C314 . C315 . 122(1) yes C314 . C315 . C316 . 119(1) yes C311 . C316 . C315 . 122(1) yes P3 . C321 . C322 . 126(1) yes P3 . C321 . C326 . 118.9(9) yes C322 . C321 . C326 . 114(1) yes C321 . C322 . C323 . 124(1) yes C322 . C323 . C324 . 118(1) yes C323 . C324 . C325 . 118(1) yes C324 . C325 . C326 . 124(1) yes C321 . C326 . C325 . 120(1) yes P3 . C331 . C332 . 122.8(9) yes P3 . C331 . C336 . 118.1(8) yes C332 . C331 . C336 . 119(1) yes C331 . C332 . C333 . 121(1) yes C332 . C333 . C334 . 120(1) yes C333 . C334 . C335 . 121(1) yes C334 . C335 . C336 . 120(1) yes C331 . C336 . C335 . 120(1) yes CU2 . P4 . C411 . 116.4(4) yes CU2 . P4 . C421 . 115.7(3) yes C411 . P4 . C421 . 101.3(4) yes CU2 . P4 . C431 . 112.9(3) yes C411 . P4 . C431 . 104.9(5) yes C421 . P4 . C431 . 104.2(4) yes P4 . C411 . C412 . 116.1(9) yes P4 . C411 . C416 . 124.8(9) yes C412 . C411 . C416 . 119(1) yes C411 . C412 . C413 . 119(1) yes C412 . C413 . C414 . 121(1) yes C413 . C414 . C415 . 121(1) yes C414 . C415 . C416 . 122(1) yes C411 . C416 . C415 . 118(1) yes P4 . C421 . C422 . 119.0(7) yes P4 . C421 . C426 . 122.1(8) yes C422 . C421 . C426 . 118.7(9) yes C421 . C422 . C423 . 120.6(9) yes C422 . C423 . C424 . 120(1) yes C423 . C424 . C425 . 119(1) yes C424 . C425 . C426 . 122(1) yes C421 . C426 . C425 . 120(1) yes P4 . C431 . C432 . 119.7(8) yes P4 . C431 . C436 . 120.2(8) yes C432 . C431 . C436 . 120(1) yes C431 . C432 . C433 . 120(1) yes C432 . C433 . C434 . 119(1) yes C433 . C434 . C435 . 121(1) yes C434 . C435 . C436 . 120(1) yes C431 . C436 . C435 . 120(1) yes F11 . B1 . F12 . 106(1) yes F11 . B1 . F13 . 108(1) yes F12 . B1 . F13 . 119(2) yes F11 . B1 . F14 . 102(2) yes F12 . B1 . F14 . 111(2) yes F13 . B1 . F14 . 110(2) yes F21 . B2 . F22 . 110(1) yes F21 . B2 . F23 . 108(2) yes F22 . B2 . F23 . 111(2) yes F21 . B2 . F24 . 114(2) yes F22 . B2 . F24 . 109(2) yes F23 . B2 . F24 . 105(2) yes #===end data_cupz3tp3 # paper complex no. 14 _publ_requested_journal 'test' _audit_creation_method CRYSTALS _chemical_name_systematic ; Bis(triphenylphosphine)tris(mu-pyridazine)dicopper(I) hexafluorophosphate dichloromethane adduct (1/1) ; _chemical_name_common ? _chemical_formula_moiety 'Cu2(C18H15P)2(C4H4N2)3(PF6)2 CH2Cl2' _chemical_formula_structural '[{Cu(C6H5)3P}2(mu-C4H4N2)3][PF6]2 CH2Cl2' _chemical_formula_analytical 'C98 H88 Cl4 Cu4 F24 N12 P8' _chemical_formula_sum 'C49 H44 Cl2 Cu2 F12 N6 P4' _chemical_formula_weight 1266.81 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'Cu ' 0.2630 1.2660 13.3380 3.5828 7.1676 0.2470 5.6158 11.3966 1.6735 64.8126 1.1910 'International_Tables_Vol_IV_Table_2.2B' 'P ' 0.0900 0.0950 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International_Tables_Vol_IV_Table_2.2B' 'Cl ' 0.1320 0.1590 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International_Tables_Vol_IV_Table_2.2B' 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'F ' 0.0140 0.0100 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International_Tables_Vol_IV_Table_2.2B' _symmetry_cell_setting 'Orthorhombic' _symmetry_space_group_name_H-M 'Pnam' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '-x+1/2,y+1/2,z+1/2' 'x+1/2,-y+1/2,-z+1/2' 'x+1/2,-y+1/2,z' '-x+1/2,y+1/2,-z' '-x,-y,z+1/2' 'x,y,-z+1/2' _cell_length_a 29.281(9) _cell_angle_alpha 90 _cell_length_b 8.567(3) _cell_angle_beta 90 _cell_length_c 21.389(7) _cell_angle_gamma 90 _cell_volume 5365(1) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 12 _cell_measurement_theta_min 10.5 _cell_measurement_theta_max 14.1 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_min 0.20 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_max 0.70 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.568 _exptl_crystal_density_method ? _exptl_crystal_F_000 2560 _exptl_absorpt_coefficient_mu 1.093 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 ; Hilger and Watts Y290 4-circle-diffractometer ; _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 3.7 _diffrn_reflns_number 4829 _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 25.0 _reflns_number_total 5329 _reflns_number_observed 2929 _reflns_observed_criterion >3sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ; Crystals Users Guide (D.J.Watkin et al, 1985) ; _computing_structure_refinement ; Crystals Users Guide (D.J.Watkin et al 1985) ; _computing_molecular_graphics 'CAMERON (Watkin et al, 1996)' _computing_publication_material 'CRYSTALS Issue 10 (Watkin et al, 1996)' _refine_special_details ; Refinement on F for all reflections with intensity >3sigma(I). The cation lies across a mirror at z = 0.25; both copper atoms and one pyridazine molecule lie in the mirror plane and two phenyl groups, one from each PPh3 ligand, are bisected by the mirror plane. The only disorder in the structure is associated with the dichloromethane solvate molecule, which also lies across the mirror plane. It occupies one of two positions (50:50 occupancy) but with common chlorine atoms. Hydrogen atoms were placed (X-H 1.00A; U[iso] 0.04) and allowed to ride on their parent atom. All non-hydrogen atoms were refined with anisotropic displacement parameters. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme ; Three parameter Chebychev W = [weight] * [1-(deltaF/6*sigmaF)**2]**2 using parameters 4.67 2.83 -0.33 ; _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2929 _refine_ls_number_parameters 364 _refine_ls_number_restraints 0 _refine_ls_R_factor_obs 0.063 _refine_ls_wR_factor_obs 0.090 _refine_ls_goodness_of_fit_obs 1.0223 _refine_ls_shift/esd_max 0.024784 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 _atom_site_occupancy _atom_site_thermal_displace_type CU1 0.3812 0.2023(1) 0.2500 0.0393 1.0000 Uani CU2 0.2728 0.1466(1) 0.2500 0.0397 1.0000 Uani N11 0.3583(2) -0.0276(9) 0.2500 0.0436 1.0000 Uani N12 0.3125(2) -0.0510(9) 0.2500 0.0455 1.0000 Uani C13 0.2964(4) -0.1963(12) 0.2500 0.0552 1.0000 Uani C14 0.3227(4) -0.3265(13) 0.2500 0.0656 1.0000 Uani C15 0.3696(4) -0.3096(13) 0.2500 0.0593 1.0000 Uani C16 0.3851(3) -0.1535(13) 0.2500 0.0562 1.0000 Uani N21 0.3446(2) 0.2966(7) 0.3243(3) 0.0453 1.0000 Uani N22 0.3000(2) 0.2690(7) 0.3251(3) 0.0455 1.0000 Uani C23 0.2751(3) 0.3271(10) 0.3721(4) 0.0600 1.0000 Uani C24 0.2930(3) 0.4168(12) 0.4200(4) 0.0699 1.0000 Uani C25 0.3383(3) 0.4483(10) 0.4172(4) 0.0658 1.0000 Uani C26 0.3632(2) 0.3829(10) 0.3697(4) 0.0566 1.0000 Uani P1 0.4565(1) 0.2302(3) 0.2500 0.0371 1.0000 Uani C111 0.4840(2) 0.1432(9) 0.3184(3) 0.0455 1.0000 Uani C112 0.4575(2) 0.0573(9) 0.3597(3) 0.0500 1.0000 Uani C113 0.4770(3) -0.0134(10) 0.4096(4) 0.0656 1.0000 Uani C114 0.5224(3) -0.0035(12) 0.4215(4) 0.0671 1.0000 Uani C115 0.5487(3) 0.0825(17) 0.3816(5) 0.0836 1.0000 Uani C116 0.5300(3) 0.1564(13) 0.3298(4) 0.0690 1.0000 Uani C121 0.4792(3) 0.4272(11) 0.2500 0.0498 1.0000 Uani C122 0.4860(3) 0.5055(11) 0.3045(6) 0.0778 1.0000 Uani C123 0.5027(5) 0.6625(14) 0.3018(11) 0.0972 1.0000 Uani C124 0.5114(7) 0.7360(22) 0.2500 0.1062 1.0000 Uani P2 0.1978(1) 0.1217(3) 0.2500 0.0369 1.0000 Uani C211 0.1743(2) 0.0218(8) 0.3186(3) 0.0446 1.0000 Uani C212 0.2039(2) -0.0511(9) 0.3583(4) 0.0561 1.0000 Uani C213 0.1881(3) -0.1348(10) 0.4095(4) 0.0662 1.0000 Uani C214 0.1420(4) -0.1445(12) 0.4210(4) 0.0738 1.0000 Uani C215 0.1127(3) -0.0696(17) 0.3820(6) 0.0895 1.0000 Uani C216 0.1285(3) 0.0102(14) 0.3299(5) 0.0749 1.0000 Uani C221 0.1704(3) 0.3086(12) 0.2500 0.0498 1.0000 Uani C222 0.1622(3) 0.3893(12) 0.3060(5) 0.0794 1.0000 Uani C223 0.1474(4) 0.5404(13) 0.3063(9) 0.0934 1.0000 Uani C224 0.1405(7) 0.6181(18) 0.2500 0.0930 1.0000 Uani C1 0.0340(9) 0.0699(24) 0.5161(14) 0.0822 0.5000 Uani CL1 0.0328(2) -0.1144(6) 0.5197(2) 0.1546 1.0000 Uani P3 0.3366(1) 0.9127(3) 0.0310(1) 0.0655 1.0000 Uani F1 0.3720(3) 1.0439(11) 0.0280(7) 0.1631 1.0000 Uani F2 0.2964(3) 1.0284(10) 0.0249(6) 0.1578 1.0000 Uani F3 0.3028(3) 0.7850(10) 0.0332(10) 0.1650 1.0000 Uani F4 0.3755(3) 0.7992(9) 0.0346(9) 0.1595 1.0000 Uani F5 0.3352(6) 0.9264(24) -0.0360(6) 0.2467 1.0000 Uani F6 0.3382(6) 0.9222(28) 0.0968(5) 0.2455 1.0000 Uani H13 0.2619 -0.2127 0.2500 0.040 1.0000 Uiso H14 0.3095 -0.4359 0.2500 0.040 1.0000 Uiso H15 0.3918 -0.3955 0.2500 0.040 1.0000 Uiso H16 0.4192 -0.1335 0.2500 0.040 1.0000 Uiso H23 0.2411 0.2990 0.3739 0.040 1.0000 Uiso H24 0.2725 0.4582 0.4547 0.040 1.0000 Uiso H25 0.3533 0.5185 0.4501 0.040 1.0000 Uiso H26 0.3967 0.4006 0.3694 0.040 1.0000 Uiso H112 0.4234 0.0469 0.3518 0.040 1.0000 Uiso H113 0.4569 -0.0784 0.4393 0.040 1.0000 Uiso H114 0.5373 -0.0554 0.4588 0.040 1.0000 Uiso H115 0.5832 0.0930 0.3911 0.040 1.0000 Uiso H116 0.5506 0.2140 0.3002 0.040 1.0000 Uiso H122 0.4806 0.4454 0.3467 0.040 1.0000 Uiso H123 0.5067 0.7183 0.3474 0.040 1.0000 Uiso H124 0.5233 0.8393 0.2500 0.040 1.0000 Uiso H212 0.2384 -0.0465 0.3498 0.040 1.0000 Uiso H213 0.2100 -0.1881 0.4383 0.040 1.0000 Uiso H214 0.1295 -0.2002 0.4574 0.040 1.0000 Uiso H215 0.0778 -0.0745 0.3886 0.040 1.0000 Uiso H216 0.1059 0.0586 0.3000 0.040 1.0000 Uiso H222 0.1671 0.3284 0.3479 0.040 1.0000 Uiso H223 0.1426 0.5967 0.3493 0.040 1.0000 Uiso H224 0.1306 0.7260 0.2500 0.040 1.0000 Uiso H1 0.0400 0.1338 0.5539 0.040 0.5000 Uiso H2 0.0580 0.1150 0.4821 0.040 0.5000 Uiso 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 0.0269(6) 0.0440(7) 0.0515(7) 0.0000 0.0000 0.0006(5) CU2 0.0288(6) 0.0397(7) 0.0546(7) 0.0000 0.0000 -0.0010(5) N11 0.0354(39) 0.0456(43) 0.0566(49) 0.0000 0.0000 0.0030(34) N12 0.0328(37) 0.0423(45) 0.0683(54) 0.0000 0.0000 -0.0028(34) C13 0.0490(56) 0.0414(56) 0.0839(79) 0.0000 0.0000 0.0047(49) C14 0.0763(84) 0.0347(58) 0.107(10) 0.0000 0.0000 -0.0006(54) C15 0.0575(69) 0.0423(58) 0.0922(87) 0.0000 0.0000 0.0133(50) C16 0.0447(59) 0.0556(63) 0.0744(74) 0.0000 0.0000 0.0102(49) N21 0.0365(28) 0.0472(32) 0.0541(35) -0.0016(28) -0.0019(24) 0.0014(24) N22 0.0415(29) 0.0528(34) 0.0446(31) -0.0080(27) 0.0032(24) 0.0005(25) C23 0.0471(40) 0.0790(54) 0.0653(49) -0.0194(43) 0.0115(36) -0.0012(38) C24 0.0639(50) 0.0930(65) 0.0715(58) -0.0327(51) 0.0035(42) 0.0123(48) C25 0.0766(54) 0.0677(54) 0.0610(51) -0.0192(43) -0.0065(41) -0.0001(44) C26 0.0437(38) 0.0765(54) 0.0589(48) -0.0170(44) -0.0046(33) -0.0026(36) P1 0.0285(11) 0.0409(14) 0.0436(13) 0.0000 0.0000 0.0001(9) C111 0.0381(32) 0.0583(41) 0.0429(37) 0.0040(32) 0.0015(27) 0.0038(31) C112 0.0546(39) 0.0593(45) 0.0399(36) -0.0038(33) 0.0075(31) -0.0026(34) C113 0.0787(56) 0.0761(56) 0.0485(46) 0.0074(41) 0.0070(39) 0.0027(46) C114 0.0776(59) 0.1051(75) 0.0448(45) 0.0217(46) 0.0022(40) 0.0249(53) C115 0.0544(50) 0.176(12) 0.0774(64) 0.0236(72) -0.0221(47) 0.0165(65) C116 0.0364(39) 0.1268(84) 0.0853(63) 0.0391(59) -0.0083(40) -0.0081(46) C121 0.0293(48) 0.0334(60) 0.0788(79) 0.0000 0.0000 0.0108(41) C122 0.0678(54) 0.0665(59) 0.1297(87) -0.0292(61) 0.0061(57) -0.0215(46) C123 0.0945(88) 0.0618(78) 0.275(22) -0.084(11) -0.023(12) 0.0015(73) C124 0.063(11) 0.0420(10) 0.4762(67) 0.0000 0.0000 0.0115(93) P2 0.0280(11) 0.0376(13) 0.0479(14) 0.0000 0.0000 0.0012(9) C211 0.0411(34) 0.0452(38) 0.0483(36) -0.0011(31) 0.0046(29) 0.0018(29) C212 0.0482(38) 0.0626(46) 0.0589(47) 0.0002(39) -0.0023(34) -0.0031(35) C213 0.0753(53) 0.0757(53) 0.0543(45) 0.0116(43) -0.0079(40) 0.0070(46) C214 0.0901(66) 0.0929(66) 0.0579(52) 0.0052(49) 0.0128(47) -0.0322(58) C215 0.0536(54) 0.174(12) 0.1030(82) 0.0623(83) 0.0121(52) -0.0051(62) C216 0.0408(43) 0.1367(95) 0.1001(77) 0.0555(71) 0.0099(44) 0.0013(47) C221 0.0337(48) 0.0443(60) 0.0900(79) 0.0000 0.0000 0.0108(41) C222 0.0688(54) 0.0845(71) 0.1103(79) -0.0382(63) -0.0091(53) 0.0206(49) C223 0.0828(71) 0.0604(70) 0.253(20) -0.0717(97) -0.004(10) 0.0114(63) C224 0.079(11) 0.0295(79) 0.350(41) 0.0000 0.0000 -0.0052(78) C1 0.126(18) 0.062(12) 0.174(23) -0.057(14) 0.076(18) -0.053(13) CL1 0.1790(40) 0.1751(43) 0.1375(33) 0.0361(30) 0.0345(31) 0.0458(34) P3 0.0631(12) 0.0643(14) 0.0732(15) -0.0043(12) 0.0029(10) -0.0034(10) F1 0.1342(67) 0.1422(68) 0.366(18) 0.1004(95) -0.0965(93) -0.0516(57) F2 0.1127(57) 0.1356(62) 0.288(13) 0.0200(80) -0.0317(71) 0.0293(53) F3 0.0996(56) 0.1062(56) 0.590(26) 0.082(11) -0.051(11) -0.0446(48) F4 0.0928(49) 0.0924(52) 0.560(25) 0.0437(98) 0.0563(97) 0.0268(41) F5 0.355(21) 0.392(23) 0.1123(79) -0.024(12) 0.0201(92) 0.0450(18) F6 0.334(20) 0.487(28) 0.0926(66) -0.001(12) 0.0059(87) 0.055(21) _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 CU1 . CU2 8_555 3.209(1) yes CU1 . P1 . 2.217(2) yes CU1 . N11 . 2.080(7) yes CU1 . N21 . 2.080(5) yes CU1 . N21 8_555 2.080(5) yes CU2 . P2 . 2.208(2) yes CU2 . N12 . 2.055(7) yes CU2 . N22 . 2.076(5) yes CU2 . N22 8_555 2.076(5) yes N11 . N12 . 1.36(1) yes N11 . C16 . 1.33(1) yes N12 . C13 . 1.33(1) yes C13 . C14 . 1.36(1) yes C14 . C15 . 1.38(2) yes C15 . C16 . 1.41(2) yes N21 . N22 . 1.329(7) yes N21 . C26 . 1.336(9) yes N22 . C23 . 1.338(9) yes C23 . C24 . 1.38(1) yes C24 . C25 . 1.35(1) yes C25 . C26 . 1.37(1) yes P1 . C121 . 1.816(9) yes P1 . C111 . 1.829(6) yes P1 . C111 8_555 1.829(6) yes C111 . C112 . 1.386(9) yes C111 . C116 . 1.374(9) yes C112 . C113 . 1.35(1) yes C113 . C114 . 1.36(1) yes C114 . C115 . 1.37(1) yes C115 . C116 . 1.39(1) yes C121 . C122 . 1.36(1) yes C122 . C123 . 1.43(1) yes C123 . C124 . 1.30(2) yes P2 . C221 . 1.791(9) yes P2 . C211 . 1.831(6) yes P2 . C211 8_555 1.831(6) yes C211 . C212 . 1.365(9) yes C211 . C216 . 1.367(9) yes C212 . C213 . 1.39(1) yes C213 . C214 . 1.37(1) yes C214 . C215 . 1.36(1) yes C215 . C216 . 1.39(1) yes C221 . C222 . 1.40(1) yes C222 . C223 . 1.37(1) yes C223 . C224 . 1.39(2) yes C1 . CL1 . 1.58(2) yes C1 . CL1 5_556 2.14(3) yes P3 . F1 . 1.530(7) yes P3 . F2 . 1.543(7) yes P3 . F3 . 1.477(7) yes P3 . F4 . 1.499(7) yes P3 . F5 . 1.44(1) yes P3 . F6 . 1.41(1) yes 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 P1 . CU1 . N11 . 115.0(2) yes P1 . CU1 . N21 . 118.1(1) yes P1 . CU1 . N21 8_555 118.1(1) yes N11 . CU1 . N21 . 101.6(2) yes N11 . CU1 . N21 8_555 101.6(2) yes N21 . CU1 . N21 8_555 99.6(3) yes P2 . CU2 . N12 . 118.9(2) yes P2 . CU2 . N22 . 115.5(2) yes P2 . CU2 . N22 8_555 115.5(2) yes N12 . CU2 . N22 . 101.5(2) yes N12 . CU2 . N22 8_555 101.5(2) yes N22 . CU2 . N22 8_555 101.3(3) yes CU1 . N11 . N12 . 117.3(5) yes CU1 . N11 . C16 . 125.2(6) yes CU2 . N12 . N11 . 116.0(6) yes CU2 . N12 . C13 . 124.8(6) yes N12 . N11 . C16 . 117.5(8) yes N11 . N12 . C13 . 119.2(7) yes N12 . C13 . C14 . 124.6(9) yes C13 . C14 . C15 . 118.6(9) yes C14 . C15 . C16 . 114.8(9) yes N11 . C16 . C15 . 125.2(9) yes CU1 . N21 . N22 . 116.6(4) yes CU1 . N21 . C26 . 124.1(4) yes CU2 . N22 . N21 . 117.2(4) yes CU2 . N22 . C23 . 124.1(5) yes N22 . N21 . C26 . 119.4(5) yes N21 . N22 . C23 . 118.7(5) yes N22 . C23 . C24 . 123.8(6) yes C23 . C24 . C25 . 116.7(7) yes C24 . C25 . C26 . 118.2(7) yes N21 . C26 . C25 . 123.2(6) yes CU1 . P1 . C121 . 117.7(3) yes CU1 . P1 . C111 . 113.2(2) yes CU1 . P1 . C111 8_555 113.2(2) yes C121 . P1 . C111 . 102.6(3) yes C121 . P1 . C111 8_555 102.6(3) yes C111 . P1 . C111 8_555 106.3(4) yes P1 . C111 . C112 . 118.7(5) yes P1 . C111 . C116 8_555 122.7(5) yes P1 . C121 . C122 . 120.9(5) yes P1 . C121 . C122 8_555 120.9(5) yes C112 . C111 . C116 . 118.6(6) yes C111 . C112 . C113 . 120.2(6) yes C112 . C113 . C114 . 122.2(7) yes C113 . C114 . C115 . 118.0(7) yes C114 . C115 . C116 . 121.5(8) yes C111 . C116 . C115 . 119.4(8) yes C122 . C121 . C122 8_555 118(1) yes C121 . C122 . C123 . 119(1) yes C122 . C123 . C124 . 124(1) yes C123 . C124 . C123 8_555 117(1) yes CU2 . P2 . C221 . 111.1(3) yes CU2 . P2 . C211 . 114.8(2) yes CU2 . P2 . C211 8_555 114.8(2) yes C221 . P2 . C211 . 104.4(3) yes C221 . P2 . C211 8_555 104.4(3) yes C211 . P2 . C211 8_555 106.4(4) yes P2 . C211 . C212 . 118.3(5) yes P2 . C211 . C216 . 123.0(6) yes P2 . C221 . C222 . 121.1(5) yes P2 . C221 . C222 8_555 121.1(5) yes C212 . C211 . C216 . 118.7(6) yes C211 . C212 . C213 . 121.0(6) yes C212 . C213 . C214 . 120.0(7) yes C213 . C214 . C215 . 118.8(7) yes C214 . C215 . C216 . 121.1(8) yes C211 . C216 . C215 . 120.4(8) yes C222 . C221 . C222 8_555 117(1) yes C221 . C222 . C223 . 122(1) yes C222 . C223 . C224 . 118(1) yes C223 . C224 . C223 8_555 121(1) yes CL1 . C1 . Cl1 5_556 100(1) yes F1 . P3 . F2 . 92.4(5) yes F1 . P3 . F3 . 179.2(6) yes F1 . P3 . F4 . 87.9(5) yes F1 . P3 . F5 . 85.3(8) yes F1 . P3 . F6 . 88.7(9) yes F2 . P3 . F3 . 88.1(5) yes F2 . P3 . F4 . 178.1(8) yes F2 . P3 . F5 . 80.9(7) yes F2 . P3 . F6 . 94.2(8) yes F3 . P3 . F4 . 91.6(4) yes F3 . P3 . F5 . 94.2(9) yes F3 . P3 . F6 . 92(1) yes F4 . P3 . F5 . 97.2(9) yes F4 . P3 . F6 . 87.8(9) yes F5 . P3 . F6 . 172(1) yes _refine_diff_density_min -0.85 _refine_diff_density_max 0.95 #===end