# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1695 data_cucgpm # paper complex no. 1 _publ_requested_journal 'test' _audit_creation_method CRYSTALS _chemical_name_systematic ; (2,9-dimethyl-1,10-phenanthroline)(2-cyanoguanidine)copper(I) tetrafluoroborate ether adduct (2/1) ; _chemical_name_common ? _chemical_formula_moiety 'C18 H21 B1 Cu1 F4 N6 O0.5' _chemical_formula_structural '[Cu(C14H12N2)(C2H4N4)][BF4].0.5C4H10O' _chemical_formula_analytical 'C36 H42 B2 Cu2 F8 N12 O1' _chemical_formula_sum 'C18 H21 B1 Cu1 F4 N6 O0.5' _chemical_formula_weight 479.75 _chemical_melting_point ? _chemical_compound_source ; Treatment of [Cu(NCMe)4][BF4] with dmp and cnge in dichloromethane; crystallisation by ether diffusion techniques. ; 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 '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' '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' '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' 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International_Tables_Vol_IV_Table_2.2B' _symmetry_cell_setting 'Orthorhombic ' _symmetry_space_group_name_H-M 'P b c n ' 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 16.547(5) _cell_angle_alpha 90 _cell_length_b 19.404(12) _cell_angle_beta 90 _cell_length_c 13.657(4) _cell_angle_gamma 90 _cell_volume 4385(3) _cell_formula_units_Z 8 _cell_measurement_temperature 210(2) _cell_measurement_reflns_used 37 _cell_measurement_theta_min 10.2 _cell_measurement_theta_max 14.9 _exptl_crystal_description 'block' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.380 _exptl_crystal_size_mid 0.230 _exptl_crystal_size_min 0.150 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.45 _exptl_crystal_density_method ? _exptl_crystal_F_000 1960 _exptl_absorpt_coefficient_mu 1.05 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.782 _exptl_absorpt_correction_T_max 0.836 _exptl_special_details ; ? ; _diffrn_ambient_temperature 210(2) _diffrn_measurement_device 'STOE STADI4 4-circle diffractometer D092' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_detector 'NaI (Tl) scintillation counter' _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_method 'omega - theta' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'planar graphite' _diffrn_standards_number 3 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 2.8 _diffrn_reflns_number 5480 _diffrn_reflns_av_R_equivalents 0.03 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -3 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 25.03 _reflns_number_total 3875 _reflns_number_observed 3204 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'STADI4 (Stoe & Cie 1995a)' _computing_cell_refinement 'STADI4 (Stoe & Cie 1995a)' _computing_data_reduction ; X-RED (Stoe & Cie, 1995b) CRYSTALS (Watkin et al, 1996) ; _computing_structure_solution 'SIR92 (Altomare, et al, 1994)' _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin et al, 1996) ; _computing_molecular_graphics 'CAMERON (Watkin, Prout and Pearce, 1996)' _computing_publication_material 'CRYSTALS Issue 10 (Watkin et al, 1996)' _refine_special_details ; Structure solved by direct methods (SIR92). Hydrogen atoms placed by standard routines and allowed to ride on the corresponding parent atom. All non-hydrogen atoms were refined with anisotropic displacement parameters. No disorder in tetrafluoroborate anion Refinement on F^2^ for ALL positive reflections. Weighted R-factors and all goodnesses of fit are based on F^2^, conventional R-factors 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 ; Three parameter Chebychev W = [weight] * [1-(deltaF/6*sigmaF)**2]**2 using parameters 33.1 41.8 9.24 ; _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 3204 _refine_ls_number_parameters 276 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1335 _refine_ls_R_factor_obs 0.0741 _refine_ls_wR_factor_all 0.1411 _refine_ls_wR_factor_obs 0.0922 _refine_ls_goodness_of_fit_ref 1.2031 _refine_ls_shift/esd_max 0.042163 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type CU1 0.83828(5) -0.05369(6) 0.60482(8) 0.0734 1.0000 Uani N1 0.9365(4) -0.1132(4) 0.6152(5) 0.0660 1.0000 Uani N2 0.9215(3) 0.0232(4) 0.6161(4) 0.0607 1.0000 Uani C1 0.8655(6) -0.2218(5) 0.6040(8) 0.1040 1.0000 Uani C2 0.9416(5) -0.1821(5) 0.6141(7) 0.0827 1.0000 Uani C3 1.0175(6) -0.2154(5) 0.6219(7) 0.1009 1.0000 Uani C4 1.0860(6) -0.1785(7) 0.6305(8) 0.1067 1.0000 Uani C5 1.0823(5) -0.1071(6) 0.6318(6) 0.0822 1.0000 Uani C6 1.1516(5) -0.0622(7) 0.6404(7) 0.1052 1.0000 Uani C7 1.1431(5) 0.0066(7) 0.6386(7) 0.0971 1.0000 Uani C8 1.0666(5) 0.0402(6) 0.6289(6) 0.0841 1.0000 Uani C9 1.0539(6) 0.1095(6) 0.6296(7) 0.0973 1.0000 Uani C10 0.9784(6) 0.1371(5) 0.6220(7) 0.0935 1.0000 Uani C11 0.9126(5) 0.0922(5) 0.6160(6) 0.0756 1.0000 Uani C12 0.8281(5) 0.1206(4) 0.6119(7) 0.0859 1.0000 Uani C13 0.9968(4) -0.0023(5) 0.6229(5) 0.0633 1.0000 Uani C14 1.0059(4) -0.0757(5) 0.6225(5) 0.0704 1.0000 Uani N21 0.7297(3) -0.0555(4) 0.5853(6) 0.0891 1.0000 Uani C21 0.6618(5) -0.0545(5) 0.5719(6) 0.0704 1.0000 Uani N22 0.5844(3) -0.0474(4) 0.5498(6) 0.0849 1.0000 Uani C22 0.5304(4) -0.0945(4) 0.5763(6) 0.0682 1.0000 Uani N23 0.5510(4) -0.1500(4) 0.6257(6) 0.0903 1.0000 Uani N24 0.4545(4) -0.0850(4) 0.5507(6) 0.0918 1.0000 Uani B1 0.3280(5) -0.2176(5) 0.6797(9) 0.0751 1.0000 Uani F11 0.2828(3) -0.2720(3) 0.6569(5) 0.1148 1.0000 Uani F12 0.4090(2) -0.2312(3) 0.6782(5) 0.1044 1.0000 Uani F13 0.3152(3) -0.1686(3) 0.6066(6) 0.1400 1.0000 Uani F14 0.3058(3) -0.1911(4) 0.7647(5) 0.1553 1.0000 Uani O31 1.0000 -0.3861(8) 0.7500 0.1596 1.0000 Uani C32 1.069(1) -0.414(1) 0.737(2) 0.3055 1.0000 Uani C33 1.1318(9) -0.402(1) 0.709(1) 0.3190 1.0000 Uani H11 0.8763(6) -0.2725(5) 0.6034(8) 0.0991 1.0000 Uiso H12 0.8294(6) -0.2103(5) 0.6603(8) 0.0991 1.0000 Uiso H13 0.8386(6) -0.2082(5) 0.5413(8) 0.0991 1.0000 Uiso H3 1.0201(6) -0.2669(5) 0.6220(7) 0.0953 1.0000 Uiso H4 1.1395(6) -0.2021(7) 0.6359(8) 0.0934 1.0000 Uiso H6 1.2067(5) -0.0827(7) 0.6482(7) 0.0786 1.0000 Uiso H7 1.1928(5) 0.0358(7) 0.6432(7) 0.0821 1.0000 Uiso H9 1.1019(6) 0.1407(6) 0.6339(7) 0.0880 1.0000 Uiso H10 0.9704(6) 0.1881(5) 0.6219(7) 0.0908 1.0000 Uiso H121 0.8309(5) 0.1721(4) 0.6125(7) 0.0784 1.0000 Uiso H122 0.7964(5) 0.1043(4) 0.6699(7) 0.0784 1.0000 Uiso H123 0.8010(5) 0.1048(4) 0.5504(7) 0.0784 1.0000 Uiso H231 0.6087(4) -0.1570(4) 0.6454(6) 0.0500 1.0000 Uiso H232 0.5093(4) -0.1849(4) 0.6439(6) 0.0500 1.0000 Uiso H241 0.4112(4) -0.1189(4) 0.5677(6) 0.0500 1.0000 Uiso H242 0.4407(4) -0.0422(4) 0.5133(6) 0.0500 1.0000 Uiso H321 1.082(1) -0.436(1) 0.801(2) 0.0500 1.0000 Uiso H322 1.057(1) -0.450(1) 0.688(2) 0.0500 1.0000 Uiso H331 1.1772(9) -0.435(1) 0.703(1) 0.0500 1.0000 Uiso H332 1.1463(9) -0.365(1) 0.758(1) 0.0500 1.0000 Uiso H333 1.1215(9) -0.380(1) 0.644(1) 0.0500 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 0.0429(5) 0.1044(8) 0.0729(6) 0.0098(7) -0.0011(5) -0.0046(5) N1 0.058(4) 0.081(5) 0.059(4) 0.015(4) -0.004(3) 0.004(3) N2 0.043(3) 0.100(5) 0.039(3) -0.003(3) -0.005(3) -0.001(3) C1 0.112(8) 0.086(7) 0.113(8) 0.023(7) 0.016(7) 0.002(6) C2 0.072(5) 0.105(8) 0.071(6) 0.027(6) 0.011(5) 0.005(5) C3 0.104(8) 0.101(7) 0.098(8) 0.012(6) 0.012(7) 0.025(7) C4 0.062(6) 0.16(1) 0.101(8) 0.034(8) 0.006(6) 0.041(7) C5 0.051(5) 0.136(9) 0.059(5) 0.005(6) -0.005(4) 0.020(5) C6 0.040(4) 0.21(1) 0.070(6) -0.008(8) 0.003(4) 0.017(7) C7 0.053(5) 0.18(1) 0.063(6) -0.027(7) -0.002(4) -0.027(7) C8 0.055(5) 0.15(1) 0.045(5) -0.021(6) 0.005(4) -0.021(6) C9 0.089(7) 0.13(1) 0.071(6) -0.027(7) 0.013(6) -0.040(7) C10 0.113(8) 0.077(6) 0.090(7) -0.021(6) 0.021(6) -0.030(6) C11 0.078(6) 0.085(6) 0.063(5) -0.005(5) 0.020(5) -0.009(5) C12 0.091(6) 0.092(6) 0.075(6) -0.008(5) 0.011(5) 0.019(5) C13 0.048(4) 0.105(6) 0.037(4) -0.001(4) -0.006(3) -0.018(5) C14 0.049(4) 0.116(7) 0.046(5) -0.000(5) 0.001(3) -0.001(5) N21 0.043(3) 0.097(5) 0.127(6) 0.015(5) -0.003(4) -0.021(4) C21 0.057(4) 0.084(6) 0.070(5) 0.016(5) 0.006(4) -0.014(5) N22 0.045(3) 0.096(5) 0.114(6) 0.037(5) -0.011(4) -0.007(4) C22 0.054(4) 0.070(5) 0.081(6) 0.015(4) -0.007(4) 0.011(4) N23 0.049(4) 0.101(6) 0.120(7) 0.033(5) -0.012(4) -0.013(4) N24 0.046(3) 0.100(6) 0.129(7) 0.034(5) -0.021(4) -0.014(4) B1 0.049(5) 0.067(6) 0.109(8) -0.007(6) 0.000(6) 0.005(5) F11 0.070(3) 0.115(4) 0.160(5) -0.022(4) -0.010(3) -0.029(3) F12 0.047(2) 0.085(3) 0.180(6) -0.013(4) 0.006(3) 0.006(2) F13 0.081(4) 0.135(5) 0.204(7) 0.063(6) 0.001(4) -0.008(4) F14 0.082(4) 0.236(8) 0.148(6) -0.098(6) 0.019(4) -0.020(4) O31 0.13(1) 0.15(1) 0.19(2) 0.0000 -0.01(1) 0.0000 C32 0.45(5) 0.27(3) 0.20(2) 0.03(2) 0.20(3) 0.15(3) C33 0.15(2) 0.61(5) 0.20(2) -0.15(3) -0.05(1) 0.14(2) 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 . N1 . 1.999(6) yes CU1 . N2 . 2.036(6) yes CU1 . N21 . 1.818(6) yes N1 . C2 . 1.34(1) yes N1 . C14 . 1.363(9) yes N2 . C11 . 1.35(1) yes N2 . C13 . 1.344(9) yes C1 . C2 . 1.48(1) yes C2 . C3 . 1.42(1) yes C3 . C4 . 1.35(1) yes C4 . C5 . 1.39(1) yes C5 . C6 . 1.44(1) yes C5 . C14 . 1.41(1) yes C6 . C7 . 1.34(1) yes C7 . C8 . 1.43(1) yes C8 . C9 . 1.36(1) yes C8 . C13 . 1.42(1) yes C9 . C10 . 1.36(1) yes C10 . C11 . 1.40(1) yes C11 . C12 . 1.50(1) yes C13 . C14 . 1.43(1) yes N21 . C21 . 1.137(8) yes C21 . N22 . 1.324(9) yes N22 . C22 . 1.328(9) yes C22 . N23 . 1.315(9) yes C22 . N24 . 1.317(9) yes B1 . F11 . 1.33(1) yes B1 . F12 . 1.37(1) yes B1 . F13 . 1.39(1) yes B1 . F14 . 1.32(1) yes O31 . C32 . 1.27(2) yes O31 . C32 6_756 1.27(2) yes C32 . C33 . 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 N1 . CU1 . N2 . 82.4(3) yes N1 . CU1 . N21 . 143.5(3) yes N2 . CU1 . N21 . 133.9(3) yes CU1 . N1 . C2 . 128.8(6) yes CU1 . N1 . C14 . 112.5(6) yes C2 . N1 . C14 . 118.7(7) yes CU1 . N2 . C11 . 130.9(6) yes CU1 . N2 . C13 . 111.2(6) yes C11 . N2 . C13 . 117.9(7) yes N1 . C2 . C1 . 117.8(8) yes N1 . C2 . C3 . 120.7(9) yes C1 . C2 . C3 . 121.5(9) yes C2 . C3 . C4 . 120.7(10) yes C3 . C4 . C5 . 119.7(9) yes C4 . C5 . C6 . 124.7(9) yes C4 . C5 . C14 . 118.0(9) yes C6 . C5 . C14 . 117.3(10) yes C5 . C6 . C7 . 121.0(9) yes C6 . C7 . C8 . 123.3(9) yes C7 . C8 . C9 . 125.9(10) yes C7 . C8 . C13 . 117.4(10) yes C9 . C8 . C13 . 116.6(9) yes C8 . C9 . C10 . 121.9(10) yes C9 . C10 . C11 . 118.3(10) yes N2 . C11 . C10 . 122.3(9) yes N2 . C11 . C12 . 117.7(8) yes C10 . C11 . C12 . 119.9(9) yes N2 . C13 . C8 . 122.9(9) yes N2 . C13 . C14 . 117.6(7) yes C8 . C13 . C14 . 119.5(8) yes N1 . C14 . C5 . 122.1(8) yes N1 . C14 . C13 . 116.2(7) yes C5 . C14 . C13 . 121.6(8) yes CU1 . N21 . C21 . 177.8(8) yes N21 . C21 . N22 . 173.6(9) yes C21 . N22 . C22 . 121.1(7) yes N22 . C22 . N23 . 121.9(7) yes N22 . C22 . N24 . 118.1(7) yes N23 . C22 . N24 . 120.0(8) yes F11 . B1 . F12 . 113.2(8) yes F11 . B1 . F13 . 106.8(9) yes F12 . B1 . F13 . 105.7(8) yes F11 . B1 . F14 . 111.0(9) yes F12 . B1 . F14 . 111.1(9) yes F13 . B1 . F14 . 108.8(8) yes C32 . O31 . C32 6_756 130.2(26) yes O31 . C32 . C33 . 141.6(27) yes _refine_diff_density_min -0.61 _refine_diff_density_max 0.63 #===END data_CUPMCG # paper complex no. 2 _publ_requested_journal 'test' _audit_creation_method CRYSTALS _chemical_name_systematic ; (2,9-dimethyl-1,10-phenanthroline)(2-cyanoguanidine)copper(I) tetrafluoroborate acetonitrile adduct (1/1) ; _chemical_name_common ? _chemical_formula_moiety 'C18 H19 B1 Cu1 F4 N7' _chemical_formula_structural '[Cu(C14H12N2)(C2H4N4)][BF4].C2H3N' _chemical_formula_analytical 'C18 H19 B1 Cu1 F4 N7' _chemical_formula_sum 'C18 H19 B1 Cu1 F4 N7' _chemical_formula_weight 483.74 _chemical_melting_point ? _chemical_compound_source ; Treatment of [Cu(NCMe)4][BF4] with dmp and cnge in MeCN; crystallisation by ether diffusion techniques. ; 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 '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' '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' '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 'P 1 21/c 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '-x,y+1/2,-z+1/2' 'x,-y+1/2,z+1/2' _cell_length_a 14.959(5) _cell_angle_alpha 90 _cell_length_b 20.000(14) _cell_angle_beta 92.35(5) _cell_length_c 6.803(6) _cell_angle_gamma 90 _cell_volume 2034(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 48 _cell_measurement_theta_min 12.5 _cell_measurement_theta_max 16.6 _exptl_crystal_description 'rectangular block' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.470 _exptl_crystal_size_mid 0.260 _exptl_crystal_size_min 0.150 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.58 _exptl_crystal_density_method ? _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 1.13 _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _diffrn_measurement_device 'STOE STADI4 4-circle diffractometer D092' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_detector 'NaI (Tl) scintillation counter' _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_method 'omega - theta' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'planar graphite' _diffrn_standards_number 3 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 10.7 _diffrn_reflns_number 3699 _diffrn_reflns_av_R_equivalents 0.045 _diffrn_reflns_av_sigmaI/netI 0.0833 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 25.02 _reflns_number_total 3573 _reflns_number_observed 3221 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'STADI4 (Stoe & Cie 1995a)' _computing_cell_refinement 'STADI4 (Stoe & Cie 1995a)' _computing_data_reduction ; X-RED (Stoe & Cie, 1995b) CRYSTALS (Watkin et al, 1996) ; _computing_structure_solution 'SIR92 (Altomare, et al, 1994)' _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin et al, 1996) ; _computing_molecular_graphics 'CAMERON (Watkin, Prout and Pearce, 1996)' _computing_publication_material 'CRYSTALS Issue 10 (Watkin et al, 1996)' _refine_special_details ; Structure solved by direct methods (SIR92). All hydrogen atoms found in difference Fourier syntheses and refined with isotropic displacement parameters. All non-hydrogen atoms were refined with anisotropic displacement parameters. No disorder in the tetrafluoroborate anion. Refinement on F^2^ for ALL positive reflections. Weighted R-factors and all goodnesses of fit are based on F^2^, conventional R-factors 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 ; Three parameter Chebychev W = [weight] * [1-(deltaF/6*sigmaF)**2]**2 using parameters 61.1 77.8 17.6 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment isotropic _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3221 _refine_ls_number_parameters 356 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0724 _refine_ls_R_factor_obs 0.0574 _refine_ls_wR_factor_all 0.0851 _refine_ls_wR_factor_obs 0.0717 _refine_ls_goodness_of_fit_ref 1.0185 _refine_ls_shift/esd_max 0.045226 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type CU1 0.68423(4) 0.20502(3) -0.01470(8) 0.0234 1.0000 Uani N1 0.7875(2) 0.1424(2) -0.0526(5) 0.0191 1.0000 Uani N2 0.7804(2) 0.2768(2) -0.0507(5) 0.0190 1.0000 Uani C1 0.7035(4) 0.0385(3) -0.0308(9) 0.0314 1.0000 Uani C2 0.7895(3) 0.0757(2) -0.0567(6) 0.0209 1.0000 Uani C3 0.8692(3) 0.0407(2) -0.0892(7) 0.0270 1.0000 Uani C4 0.9473(3) 0.0744(2) -0.1050(7) 0.0272 1.0000 Uani C5 0.9485(3) 0.1438(2) -0.0962(6) 0.0225 1.0000 Uani C6 1.0278(3) 0.1843(2) -0.1101(7) 0.0243 1.0000 Uani C7 1.0239(3) 0.2514(3) -0.1057(7) 0.0278 1.0000 Uani C8 0.9402(3) 0.2852(2) -0.0880(6) 0.0238 1.0000 Uani C9 0.9327(3) 0.3556(2) -0.0873(7) 0.0282 1.0000 Uani C10 0.8497(3) 0.3836(2) -0.0715(7) 0.0249 1.0000 Uani C11 0.7735(3) 0.3434(2) -0.0507(7) 0.0230 1.0000 Uani C12 0.6821(4) 0.3723(2) -0.0270(9) 0.0320 1.0000 Uani C13 0.8622(3) 0.2482(2) -0.0698(6) 0.0173 1.0000 Uani C14 0.8661(3) 0.1766(2) -0.0731(6) 0.0177 1.0000 Uani N21 0.5646(2) 0.2141(2) 0.0401(5) 0.0254 1.0000 Uani C21 0.4917(3) 0.2275(2) 0.0763(6) 0.0219 1.0000 Uani N22 0.4111(2) 0.2488(2) 0.1070(6) 0.0237 1.0000 Uani C22 0.3498(3) 0.2064(2) 0.1701(6) 0.0222 1.0000 Uani N23 0.3640(3) 0.1415(2) 0.2020(7) 0.0303 1.0000 Uani N24 0.2688(3) 0.2304(3) 0.1956(7) 0.0338 1.0000 Uani N31 0.5045(3) 0.0369(2) 0.2438(7) 0.0348 1.0000 Uani C32 0.5233(3) -0.0174(3) 0.2592(7) 0.0267 1.0000 Uani C33 0.5453(4) -0.0880(3) 0.282(1) 0.0372 1.0000 Uani B1 0.1930(4) 0.0843(3) 0.532(1) 0.0356 1.0000 Uani F11 0.1204(2) 0.0489(1) 0.5918(5) 0.0487 1.0000 Uani F12 0.2622(2) 0.0414(1) 0.4870(5) 0.0428 1.0000 Uani F13 0.1695(2) 0.1191(2) 0.3609(6) 0.0694 1.0000 Uani F14 0.2226(2) 0.1287(2) 0.6749(6) 0.0722 1.0000 Uani H3 0.868(4) 0.001(3) -0.102(8) 0.05(2) 1.0000 Uiso H4 0.997(3) 0.054(2) -0.145(6) 0.01(1) 1.0000 Uiso H6 1.084(3) 0.160(2) -0.126(6) 0.02(1) 1.0000 Uiso H7 1.076(3) 0.275(3) -0.111(7) 0.04(1) 1.0000 Uiso H9 0.983(4) 0.386(3) -0.101(8) 0.06(2) 1.0000 Uiso H10 0.842(3) 0.430(2) -0.072(6) 0.02(1) 1.0000 Uiso H231 0.414(4) 0.126(3) 0.187(8) 0.05(2) 1.0000 Uiso H232 0.328(4) 0.122(3) 0.263(9) 0.06(2) 1.0000 Uiso H241 0.229(5) 0.205(4) 0.245(9) 0.08(2) 1.0000 Uiso H242 0.257(3) 0.267(2) 0.170(7) 0.02(1) 1.0000 Uiso H11 0.686(4) 0.015(3) -0.163(9) 0.05(2) 1.0000 Uiso H12 0.710(5) 0.005(4) 0.09(1) 0.10(3) 1.0000 Uiso H13 0.657(6) 0.064(4) 0.03(1) 0.13(3) 1.0000 Uiso H121 0.687(4) 0.421(3) -0.016(8) 0.05(2) 1.0000 Uiso H122 0.634(3) 0.356(2) -0.132(7) 0.04(1) 1.0000 Uiso H123 0.652(4) 0.356(3) 0.092(9) 0.06(2) 1.0000 Uiso H331 0.596(5) -0.094(3) 0.24(1) 0.08(3) 1.0000 Uiso H332 0.506(5) -0.118(4) 0.20(1) 0.09(2) 1.0000 Uiso H333 0.535(6) -0.104(5) 0.41(1) 0.15(4) 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 0.0167(3) 0.0286(3) 0.0250(3) 0.0002(3) 0.0033(2) 0.0012(3) N1 0.021(2) 0.016(2) 0.021(2) -0.003(1) 0.003(1) 0.002(2) N2 0.022(2) 0.016(2) 0.018(2) -0.004(1) -0.002(1) 0.001(1) C1 0.034(3) 0.027(3) 0.034(3) -0.000(2) 0.009(2) -0.005(2) C2 0.026(2) 0.019(2) 0.018(2) 0.004(2) 0.001(2) -0.000(2) C3 0.035(3) 0.017(3) 0.029(3) 0.003(2) -0.002(2) 0.008(2) C4 0.023(2) 0.026(3) 0.032(3) -0.009(2) 0.005(2) 0.009(2) C5 0.019(2) 0.029(3) 0.019(2) 0.000(2) 0.002(2) 0.003(2) C6 0.015(2) 0.032(3) 0.027(3) -0.006(2) 0.004(2) -0.004(2) C7 0.016(2) 0.044(3) 0.024(3) -0.005(2) -0.001(2) -0.010(2) C8 0.027(2) 0.026(2) 0.018(2) 0.002(2) 0.002(2) -0.005(2) C9 0.034(3) 0.028(3) 0.022(3) -0.000(2) -0.005(2) -0.010(2) C10 0.039(3) 0.014(2) 0.021(2) -0.002(2) -0.005(2) 0.001(2) C11 0.029(3) 0.019(2) 0.021(2) 0.002(2) -0.003(2) 0.006(2) C12 0.035(3) 0.018(3) 0.043(3) -0.006(2) -0.006(2) 0.010(2) C13 0.022(2) 0.020(2) 0.010(2) -0.001(2) 0.004(2) 0.000(2) C14 0.018(2) 0.020(2) 0.015(2) 0.004(2) -0.001(2) -0.003(2) N21 0.020(2) 0.024(2) 0.033(2) 0.002(2) 0.005(2) -0.000(2) C21 0.028(3) 0.015(2) 0.022(2) 0.004(2) -0.001(2) -0.004(2) N22 0.020(2) 0.020(2) 0.031(2) 0.005(2) 0.005(2) -0.000(2) C22 0.022(2) 0.024(2) 0.021(2) -0.001(2) 0.003(2) 0.005(2) N23 0.028(2) 0.026(2) 0.038(3) 0.000(2) 0.016(2) -0.000(2) N24 0.022(2) 0.029(3) 0.051(3) 0.007(2) 0.009(2) 0.007(2) N31 0.037(2) 0.029(2) 0.038(2) -0.003(2) 0.006(2) 0.004(2) C32 0.020(2) 0.036(3) 0.024(2) -0.004(2) 0.007(2) -0.004(2) C33 0.045(4) 0.024(3) 0.043(4) -0.005(2) 0.001(3) -0.001(3) B1 0.034(3) 0.013(3) 0.061(4) -0.006(3) 0.018(3) -0.000(2) F11 0.039(2) 0.032(2) 0.077(2) -0.000(2) 0.026(2) -0.007(1) F12 0.031(2) 0.030(2) 0.068(2) -0.010(2) 0.013(1) 0.009(1) F13 0.053(2) 0.055(2) 0.101(3) 0.047(2) 0.019(2) 0.010(2) F14 0.060(2) 0.050(2) 0.109(3) -0.043(2) 0.029(2) -0.015(2) 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 . N1 . 2.014(4) yes CU1 . N2 . 2.054(4) yes CU1 . N21 . 1.851(3) yes N1 . C2 . 1.335(5) yes N1 . C14 . 1.373(5) yes N2 . C11 . 1.337(5) yes N2 . C13 . 1.362(5) yes C1 . C2 . 1.503(6) yes C2 . C3 . 1.408(6) yes C3 . C4 . 1.356(7) yes C4 . C5 . 1.390(7) yes C5 . C6 . 1.442(6) yes C5 . C14 . 1.410(6) yes C6 . C7 . 1.344(7) yes C7 . C8 . 1.432(6) yes C8 . C9 . 1.413(7) yes C8 . C13 . 1.392(6) yes C9 . C10 . 1.370(7) yes C10 . C11 . 1.406(6) yes C11 . C12 . 1.499(7) yes C13 . C14 . 1.432(6) yes N21 . C21 . 1.159(5) yes C21 . N22 . 1.304(6) yes N22 . C22 . 1.334(6) yes C22 . N23 . 1.331(6) yes C22 . N24 . 1.322(6) yes N31 . C32 . 1.124(6) yes C32 . C33 . 1.457(7) yes B1 . F11 . 1.373(6) yes B1 . F12 . 1.387(6) yes B1 . F13 . 1.388(7) yes B1 . F14 . 1.379(7) 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 N1 . CU1 . N2 . 82.8(1) yes N1 . CU1 . N21 . 147.1(2) yes N2 . CU1 . N21 . 130.0(2) yes CU1 . N1 . C2 . 130.0(3) yes CU1 . N1 . C14 . 111.5(3) yes C2 . N1 . C14 . 118.5(4) yes CU1 . N2 . C11 . 130.0(3) yes CU1 . N2 . C13 . 110.7(3) yes C11 . N2 . C13 . 119.3(4) yes N1 . C2 . C1 . 118.1(4) yes N1 . C2 . C3 . 121.3(4) yes C1 . C2 . C3 . 120.5(4) yes C2 . C3 . C4 . 120.2(4) yes C3 . C4 . C5 . 120.2(4) yes C4 . C5 . C6 . 124.5(4) yes C4 . C5 . C14 . 117.4(4) yes C6 . C5 . C14 . 118.1(4) yes C5 . C6 . C7 . 121.5(4) yes C6 . C7 . C8 . 120.7(4) yes C7 . C8 . C9 . 122.7(4) yes C7 . C8 . C13 . 119.7(4) yes C9 . C8 . C13 . 117.5(4) yes C8 . C9 . C10 . 118.7(4) yes C9 . C10 . C11 . 121.0(4) yes N2 . C11 . C10 . 120.4(4) yes N2 . C11 . C12 . 117.1(4) yes C10 . C11 . C12 . 122.5(4) yes N2 . C13 . C8 . 123.0(4) yes N2 . C13 . C14 . 117.3(4) yes C8 . C13 . C14 . 119.6(4) yes N1 . C14 . C5 . 122.3(4) yes N1 . C14 . C13 . 117.4(4) yes C5 . C14 . C13 . 120.2(4) yes CU1 . N21 . C21 . 172.2(4) yes N21 . C21 . N22 . 173.7(5) yes C21 . N22 . C22 . 119.7(4) yes N22 . C22 . N23 . 124.5(4) yes N22 . C22 . N24 . 117.2(4) yes N23 . C22 . N24 . 118.2(5) yes N31 . C32 . C33 . 178.4(5) yes F11 . B1 . F12 . 110.7(4) yes F11 . B1 . F13 . 109.3(5) yes F12 . B1 . F13 . 107.0(5) yes F11 . B1 . F14 . 110.9(5) yes F12 . B1 . F14 . 109.5(5) yes F13 . B1 . F14 . 109.3(4) yes _refine_diff_density_min -0.58 _refine_diff_density_max 0.59 #===END data_CUMEPH # paper complex no. 3 _publ_requested_journal 'test' _audit_creation_method CRYSTALS _chemical_name_systematic ; (2,9-dimethyl-1,10-phenanthroline)(2-cyanoguanidine)copper(I) tetrafluoroborate ether adduct (2/1) ; _chemical_name_common ? _chemical_formula_moiety 'C16 H15 B1 Cu1 F4 N3' _chemical_formula_structural '[Cu(C14H12N2)(C2H3N)][BF4]' _chemical_formula_analytical 'C16 H15 B1 Cu1 F4 N3' _chemical_formula_sum 'C16 H15 B1 Cu1 F4 N3' _chemical_formula_weight 399.66 _chemical_melting_point ? _chemical_compound_source ; Treatment of [Cu(NCMe)4][BF4] with dmp in dichloromethane. ; 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 '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' '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' _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'P 1 21/c 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '-x,y+1/2,-z+1/2' 'x,-y+1/2,z+1/2' _cell_length_a 11.848(16) _cell_angle_alpha 90 _cell_length_b 19.296(3) _cell_angle_beta 108.29(2) _cell_length_c 7.506(11) _cell_angle_gamma 90 _cell_volume 1629(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 34 _cell_measurement_theta_min 12.6 _cell_measurement_theta_max 17.0 _exptl_crystal_description 'rectangular block' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.600 _exptl_crystal_size_mid 0.460 _exptl_crystal_size_min 0.220 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.63 _exptl_crystal_density_method ? _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 1.39 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3841 _exptl_absorpt_correction_T_max 0.6217 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _diffrn_measurement_device 'STOE STADI4 4-circle diffractometer D092' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_detector 'NaI (Tl) scintillation counter' _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_method 'omega - theta' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'planar graphite' _diffrn_standards_number 3 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 3.7 _diffrn_reflns_number 3648 _diffrn_reflns_av_R_equivalents 0.01 _diffrn_reflns_av_sigmaI/netI 0.0287 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -3 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 25.01 _reflns_number_total 2849 _reflns_number_observed 2726 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'STADI4 (Stoe & Cie 1995a)' _computing_cell_refinement 'STADI4 (Stoe & Cie 1995a)' _computing_data_reduction ; X-RED (Stoe & Cie, 1995b) CRYSTALS (Watkin et al, 1996) ; _computing_structure_solution 'SIR92 (Altomare, et al, 1994)' _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin et al, 1996) ; _computing_molecular_graphics 'CAMERON (Watkin, Prout and Pearce, 1996)' _computing_publication_material 'CRYSTALS Issue 10 (Watkin et al, 1996)' _refine_special_details ; Structure solved by direct methods (SIR92). Hydrogen atoms found in difference Fourier syntheses and refined with isotropic displacement parameters. All non-hydrogen atoms refined with anisotropic displacement parameters. No disorder in tetrafluoroborate anion. Refinement on F^2^ for ALL positive reflections. Weighted R-factors and all goodnesses of fit are based on F^2^, conventional R-factors 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 ; Three parameter Chebychev W = [weight] * [1-(deltaF/6*sigmaF)**2]**2 using parameters 18.5 22.1 4.25 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment isotropic _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2726 _refine_ls_number_parameters 286 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0384 _refine_ls_R_factor_obs 0.0344 _refine_ls_wR_factor_all 0.0390 _refine_ls_wR_factor_obs 0.0373 _refine_ls_goodness_of_fit_ref 1.1804 _refine_ls_shift/esd_max 0.000820 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type CU1 0.77624(2) 0.35722(1) 0.44086(4) 0.0270 1.0000 Uani N1 0.9216(1) 0.31201(8) 0.4061(2) 0.0226 1.0000 Uani N2 0.7272(1) 0.25748(9) 0.4645(2) 0.0218 1.0000 Uani C1 1.0290(2) 0.4177(1) 0.3931(4) 0.0347 1.0000 Uani C2 1.0179(2) 0.3408(1) 0.3815(3) 0.0269 1.0000 Uani C3 1.1082(2) 0.2996(1) 0.3509(3) 0.0298 1.0000 Uani C4 1.0990(2) 0.2292(1) 0.3470(3) 0.0293 1.0000 Uani C5 0.9987(2) 0.1978(1) 0.3745(3) 0.0243 1.0000 Uani C6 0.9814(2) 0.1240(1) 0.3744(3) 0.0285 1.0000 Uani C7 0.8850(2) 0.0967(1) 0.4059(3) 0.0291 1.0000 Uani C8 0.7962(2) 0.1402(1) 0.4413(3) 0.0253 1.0000 Uani C9 0.6965(2) 0.1147(1) 0.4850(3) 0.0286 1.0000 Uani C10 0.6158(2) 0.1603(1) 0.5150(3) 0.0285 1.0000 Uani C11 0.6310(2) 0.2320(1) 0.4993(3) 0.0250 1.0000 Uani C12 0.5398(2) 0.2830(1) 0.5152(4) 0.0309 1.0000 Uani C13 0.8088(2) 0.2125(1) 0.4370(3) 0.0213 1.0000 Uani C14 0.9124(2) 0.2415(1) 0.4040(2) 0.0206 1.0000 Uani N21 0.7073(2) 0.44387(9) 0.4364(2) 0.0274 1.0000 Uani C22 0.6594(2) 0.4957(1) 0.4183(3) 0.0265 1.0000 Uani C23 0.5958(2) 0.5610(1) 0.3921(4) 0.0355 1.0000 Uani B1 0.6853(2) 0.5854(1) -0.0716(4) 0.0291 1.0000 Uani F11 0.5807(1) 0.54824(8) -0.1306(2) 0.0580 1.0000 Uani F12 0.7464(1) 0.5706(1) 0.1115(2) 0.0681 1.0000 Uani F13 0.7567(1) 0.5668(1) -0.1775(2) 0.0689 1.0000 Uani F14 0.6598(1) 0.65411(8) -0.0963(3) 0.0766 1.0000 Uani H3 1.169(2) 0.321(1) 0.330(3) 0.042(7) 1.0000 Uiso H4 1.156(2) 0.205(1) 0.330(3) 0.024(6) 1.0000 Uiso H6 1.037(2) 0.096(1) 0.349(3) 0.034(6) 1.0000 Uiso H7 0.874(2) 0.048(1) 0.402(3) 0.033(6) 1.0000 Uiso H9 0.688(2) 0.069(1) 0.498(3) 0.040(7) 1.0000 Uiso H10 0.551(2) 0.146(1) 0.545(3) 0.037(6) 1.0000 Uiso H11 1.075(3) 0.430(1) 0.517(4) 0.062(9) 1.0000 Uiso H12 1.067(3) 0.436(1) 0.311(4) 0.058(8) 1.0000 Uiso H13 0.958(3) 0.439(2) 0.347(4) 0.064(9) 1.0000 Uiso H121 0.577(2) 0.317(1) 0.606(4) 0.055(8) 1.0000 Uiso H122 0.501(2) 0.303(1) 0.398(4) 0.055(8) 1.0000 Uiso H123 0.493(2) 0.263(2) 0.558(4) 0.056(9) 1.0000 Uiso H231 0.640(3) 0.595(2) 0.372(5) 0.09(1) 1.0000 Uiso H232 0.583(3) 0.576(2) 0.501(5) 0.09(1) 1.0000 Uiso H233 0.515(3) 0.559(2) 0.291(4) 0.08(1) 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 0.0340(1) 0.0199(1) 0.0263(1) 0.0006(1) 0.0081(1) 0.0059(1) N1 0.0267(9) 0.0215(9) 0.0173(8) -0.0004(7) 0.0034(7) -0.0013(7) N2 0.0241(9) 0.0227(9) 0.0165(8) -0.0004(7) 0.0031(7) 0.0022(7) C1 0.040(1) 0.030(1) 0.034(1) -0.003(1) 0.013(1) -0.009(1) C2 0.028(1) 0.030(1) 0.019(1) 0.0013(8) 0.0032(9) -0.0057(9) C3 0.025(1) 0.041(1) 0.023(1) -0.0005(9) 0.0074(9) -0.004(1) C4 0.023(1) 0.043(1) 0.020(1) -0.0008(9) 0.0036(9) 0.007(1) C5 0.028(1) 0.028(1) 0.013(1) -0.0006(8) 0.0008(8) 0.0053(9) C6 0.032(1) 0.027(1) 0.023(1) -0.0040(8) 0.0040(9) 0.0091(9) C7 0.038(1) 0.019(1) 0.025(1) -0.0016(9) 0.0024(9) 0.0035(9) C8 0.031(1) 0.0231(9) 0.0172(9) -0.0004(9) 0.0011(8) 0.0004(9) C9 0.036(1) 0.022(1) 0.022(1) 0.0003(8) 0.0016(9) -0.0063(9) C10 0.028(1) 0.034(1) 0.022(1) -0.0006(9) 0.0056(9) -0.008(1) C11 0.026(1) 0.030(1) 0.016(1) -0.0005(8) 0.0030(8) 0.0000(9) C12 0.029(1) 0.036(1) 0.029(1) 0.001(1) 0.012(1) 0.002(1) C13 0.025(1) 0.021(1) 0.0141(9) -0.0008(8) 0.0010(8) 0.0007(8) C14 0.024(1) 0.023(1) 0.0117(9) 0.0001(8) 0.0002(8) 0.0010(8) N21 0.029(1) 0.025(1) 0.029(1) -0.0012(8) 0.0105(8) -0.0004(8) C22 0.027(1) 0.026(1) 0.025(1) -0.0015(9) 0.0075(9) 0.0012(9) C23 0.039(1) 0.026(1) 0.041(1) -0.001(1) 0.012(1) 0.011(1) B1 0.021(1) 0.027(1) 0.038(1) -0.001(1) 0.008(1) -0.002(1) F11 0.0292(7) 0.0427(9) 0.096(1) -0.0093(8) 0.0100(8) -0.0117(6) F12 0.0484(9) 0.113(1) 0.0399(9) 0.0251(9) 0.0095(7) -0.022(1) F13 0.0480(9) 0.112(1) 0.054(1) -0.019(1) 0.0265(8) 0.002(1) F14 0.0447(9) 0.0294(9) 0.135(2) -0.0046(9) -0.002(1) 0.0023(7) 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 . N1 . 2.019(2) yes CU1 . N2 . 2.034(2) yes CU1 . N21 . 1.856(2) yes N1 . C2 . 1.333(3) yes N1 . C14 . 1.365(3) yes N2 . C11 . 1.340(3) yes N2 . C13 . 1.362(2) yes C1 . C2 . 1.490(3) yes C2 . C3 . 1.409(3) yes C3 . C4 . 1.362(3) yes C4 . C5 . 1.406(3) yes C5 . C6 . 1.439(3) yes C5 . C14 . 1.397(3) yes C6 . C7 . 1.344(3) yes C7 . C8 . 1.434(3) yes C8 . C9 . 1.410(3) yes C8 . C13 . 1.405(3) yes C9 . C10 . 1.369(3) yes C10 . C11 . 1.405(3) yes C11 . C12 . 1.493(3) yes C13 . C14 . 1.439(3) yes N21 . C22 . 1.137(3) yes C22 . C23 . 1.450(3) yes B1 . F11 . 1.379(3) yes B1 . F12 . 1.368(3) yes B1 . F13 . 1.377(3) yes B1 . F14 . 1.359(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 N1 . CU1 . N2 . 83.17(7) yes N1 . CU1 . N21 . 140.79(7) yes N2 . CU1 . N21 . 135.88(7) yes CU1 . N1 . C2 . 129.8(1) yes CU1 . N1 . C14 . 111.3(1) yes C2 . N1 . C14 . 118.9(2) yes CU1 . N2 . C11 . 130.4(1) yes CU1 . N2 . C13 . 110.7(1) yes C11 . N2 . C13 . 118.9(2) yes N1 . C2 . C1 . 118.1(2) yes N1 . C2 . C3 . 120.9(2) yes C1 . C2 . C3 . 121.0(2) yes C2 . C3 . C4 . 120.5(2) yes C3 . C4 . C5 . 119.5(2) yes C4 . C5 . C6 . 123.7(2) yes C4 . C5 . C14 . 117.2(2) yes C6 . C5 . C14 . 119.1(2) yes C5 . C6 . C7 . 121.1(2) yes C6 . C7 . C8 . 121.1(2) yes C7 . C8 . C9 . 123.7(2) yes C7 . C8 . C13 . 119.2(2) yes C9 . C8 . C13 . 117.0(2) yes C8 . C9 . C10 . 119.6(2) yes C9 . C10 . C11 . 120.3(2) yes N2 . C11 . C10 . 121.1(2) yes N2 . C11 . C12 . 117.1(2) yes C10 . C11 . C12 . 121.8(2) yes N2 . C13 . C8 . 123.0(2) yes N2 . C13 . C14 . 117.5(2) yes C8 . C13 . C14 . 119.5(2) yes N1 . C14 . C5 . 123.0(2) yes N1 . C14 . C13 . 117.1(2) yes C5 . C14 . C13 . 119.9(2) yes CU1 . N21 . C22 . 174.1(2) yes N21 . C22 . C23 . 178.7(2) yes F11 . B1 . F12 . 110.6(2) yes F11 . B1 . F13 . 109.4(2) yes F12 . B1 . F13 . 107.4(2) yes F11 . B1 . F14 . 108.9(2) yes F12 . B1 . F14 . 111.5(2) yes F13 . B1 . F14 . 109.0(2) yes _refine_diff_density_min -0.52 _refine_diff_density_max 0.79 #===END