Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Ciunik, Zbigniew' 'Drabent, Krzysztof' _publ_contact_author_name 'Dr Krzysztof Drabent' _publ_contact_author_address ; Dr Krzysztof Drabent Faculty of Chemistry University of Wroclaw 14 F Joliot-Curie Str Wroclaw 50-383 POLAND ; _publ_contact_author_email 'DRAB@WCHUWR.CHEM.UNI.WROC.PL' _publ_section_title ; Counter anion dependent symmetry of Cu11 -4-amino-1,2,4,-triazole polymeric chains ; data_cmpd_1 _database_code_CSD 164098 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety '[Cu(amtrz)3](BF4)2.H2O' _chemical_formula_sum 'C6 H14 B2 Cu F8 N12 O' _chemical_formula_weight 507.45 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' 'O' 'O' 0.0106 0.0060 '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 7.8433(15) _cell_length_b 10.5221(14) _cell_length_c 10.8374(12) _cell_angle_alpha 76.796(10) _cell_angle_beta 77.881(12) _cell_angle_gamma 80.354(13) _cell_volume 844.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2500 _cell_measurement_theta_min 3.54 _cell_measurement_theta_max 30.28 _exptl_crystal_description block _exptl_crystal_colour light-blue _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.995 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 506 _exptl_absorpt_coefficient_mu 1.409 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8719 _exptl_absorpt_correction_T_max 0.8719 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Kuma KM4CCD' _diffrn_measurement_method '\o scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 'none (area detector data)' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12363 _diffrn_reflns_av_R_equivalents 0.0379 _diffrn_reflns_av_sigmaI/netI 0.0391 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.54 _diffrn_reflns_theta_max 30.28 _reflns_number_total 4633 _reflns_number_gt 3965 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kuma Diffraction Wroclaw' _computing_cell_refinement 'Kuma Diffraction Wroclaw' _computing_data_reduction 'Kuma Diffraction Wroclaw' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-NT V5.1, Brucker AXS 1999' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0083P)^2^+4.2764P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4633 _refine_ls_number_parameters 274 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0678 _refine_ls_R_factor_gt 0.0546 _refine_ls_wR_factor_ref 0.1158 _refine_ls_wR_factor_gt 0.1107 _refine_ls_goodness_of_fit_ref 1.150 _refine_ls_restrained_S_all 1.150 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.5000 0.0000 0.0000 0.00962(13) Uani 1 d S . . Cu2 Cu 0.0000 0.0000 0.0000 0.01021(13) Uani 1 d S . . O1W O 0.2894(4) 0.2923(3) 0.6604(3) 0.0260(6) Uani 1 d . . . N11 N 0.3571(3) -0.0221(3) -0.1657(3) 0.0115(5) Uani 1 d . . . N12 N 0.1796(4) -0.0272(3) -0.1527(3) 0.0113(5) Uani 1 d . . . N13 N 0.3054(4) -0.0722(3) -0.3378(3) 0.0126(5) Uani 1 d . . . N14 N 0.3391(4) -0.1116(3) -0.4569(3) 0.0173(6) Uani 1 d . . . C11 C 0.4293(4) -0.0481(3) -0.2791(3) 0.0134(6) Uani 1 d . . . C12 C 0.1525(4) -0.0586(3) -0.2563(3) 0.0132(6) Uani 1 d . . . N21 N 0.3288(3) 0.1588(3) 0.0298(3) 0.0110(5) Uani 1 d . . . N22 N 0.1539(3) 0.1742(3) 0.0186(3) 0.0118(5) Uani 1 d . . . N23 N 0.2057(4) 0.3440(3) 0.0815(3) 0.0119(5) Uani 1 d . . . N24 N 0.1769(4) 0.4684(3) 0.1169(3) 0.0159(6) Uani 1 d . . . C21 C 0.3563(4) 0.2621(3) 0.0687(3) 0.0134(6) Uani 1 d . . . C22 C 0.0838(4) 0.2875(3) 0.0489(3) 0.0132(6) Uani 1 d . . . N31 N 0.3284(4) -0.1196(3) 0.1262(3) 0.0116(5) Uani 1 d . . . N32 N 0.1554(3) -0.1255(3) 0.1192(3) 0.0112(5) Uani 1 d . . . N33 N 0.2304(4) -0.2785(3) 0.2767(3) 0.0144(6) Uani 1 d . . . N34 N 0.2147(4) -0.3891(3) 0.3783(3) 0.0192(6) Uani 1 d . . . C31 C 0.3691(4) -0.2117(3) 0.2224(3) 0.0136(6) Uani 1 d . . . C32 C 0.1005(4) -0.2218(3) 0.2105(3) 0.0140(6) Uani 1 d . . . B1 B 0.1093(5) 0.2076(4) 0.4131(4) 0.0173(8) Uani 1 d . . . F1 F -0.0209(3) 0.2951(2) 0.3597(2) 0.0259(5) Uani 1 d . . . F2 F 0.0395(3) 0.1493(2) 0.5377(2) 0.0258(5) Uani 1 d . . . F3 F 0.1692(3) 0.1083(2) 0.3406(2) 0.0222(5) Uani 1 d . . . F4 F 0.2498(3) 0.2725(3) 0.4113(2) 0.0289(5) Uani 1 d . . . B2 B 0.3622(6) 0.5544(4) 0.7778(4) 0.0187(8) Uani 1 d . . . F5 F 0.2130(3) 0.4924(2) 0.8047(2) 0.0219(5) Uani 1 d . . . F6 F 0.4925(3) 0.4702(2) 0.8377(2) 0.0243(5) Uani 1 d . . . F7 F 0.3268(3) 0.6704(2) 0.8250(2) 0.0242(5) Uani 1 d . . . F8 F 0.4214(3) 0.5816(3) 0.6448(2) 0.0296(5) Uani 1 d . . . H1W H 0.2535 0.3780 0.6622 0.060 Uiso 1 d . . . H2W H 0.2924 0.3049 0.5879 0.060 Uiso 1 d . . . H11 H 0.5560 -0.0546 -0.3151 0.016 Uiso 1 d . . . H12 H 0.0375 -0.0710 -0.2761 0.016 Uiso 1 d . . . H21 H 0.4626 0.2806 0.0821 0.016 Uiso 1 d . . . H22 H -0.0470 0.3222 0.0460 0.016 Uiso 1 d . . . H31 H 0.4730 -0.2266 0.2471 0.016 Uiso 1 d . . . H32 H 0.0016 -0.2453 0.2257 0.016 Uiso 1 d . . . H141 H 0.3483 -0.2038 -0.4353 0.034 Uiso 1 d . . . H142 H 0.2670 -0.0738 -0.4939 0.034 Uiso 1 d . . . H241 H 0.1155 0.4587 0.1923 0.030 Uiso 1 d . . . H242 H 0.2794 0.4871 0.1246 0.030 Uiso 1 d . . . H341 H 0.3045 -0.4340 0.3826 0.040 Uiso 1 d . . . H342 H 0.1832 -0.3590 0.4585 0.040 Uiso 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 Cu1 0.0055(2) 0.0108(3) 0.0127(3) -0.0041(2) -0.00101(19) 0.00012(19) Cu2 0.0060(3) 0.0139(3) 0.0105(3) -0.0037(2) -0.00111(19) 0.0008(2) O1W 0.0262(15) 0.0256(14) 0.0310(16) -0.0086(12) -0.0134(12) -0.0023(12) N11 0.0066(12) 0.0143(13) 0.0145(13) -0.0048(11) -0.0017(10) -0.0009(10) N12 0.0069(12) 0.0124(13) 0.0142(13) -0.0034(10) -0.0017(10) 0.0002(10) N13 0.0097(13) 0.0177(14) 0.0094(13) -0.0031(11) 0.0007(10) -0.0021(10) N14 0.0185(15) 0.0231(15) 0.0117(14) -0.0068(12) -0.0035(11) -0.0015(12) C11 0.0127(15) 0.0140(15) 0.0126(15) -0.0038(12) -0.0013(12) 0.0016(12) C12 0.0105(15) 0.0146(15) 0.0146(15) -0.0030(12) -0.0030(12) -0.0010(12) N21 0.0071(12) 0.0114(12) 0.0146(13) -0.0030(10) -0.0032(10) 0.0012(9) N22 0.0055(12) 0.0150(13) 0.0144(13) -0.0037(11) -0.0017(10) 0.0011(10) N23 0.0110(13) 0.0114(13) 0.0151(14) -0.0057(11) -0.0036(10) -0.0009(10) N24 0.0146(14) 0.0124(13) 0.0219(15) -0.0092(12) -0.0010(11) 0.0003(11) C21 0.0124(15) 0.0129(15) 0.0151(15) -0.0027(12) -0.0026(12) -0.0023(12) C22 0.0053(14) 0.0168(16) 0.0186(16) -0.0048(13) -0.0023(12) -0.0021(11) N31 0.0086(12) 0.0140(13) 0.0129(13) -0.0048(11) -0.0021(10) -0.0007(10) N32 0.0073(12) 0.0141(13) 0.0130(13) -0.0056(11) -0.0012(10) 0.0001(10) N33 0.0145(14) 0.0126(13) 0.0147(14) -0.0023(11) -0.0018(11) 0.0005(10) N34 0.0209(16) 0.0143(14) 0.0170(15) 0.0024(12) -0.0007(12) 0.0026(11) C31 0.0134(15) 0.0151(15) 0.0127(15) -0.0048(12) -0.0021(12) -0.0002(12) C32 0.0125(15) 0.0141(15) 0.0157(16) -0.0047(13) -0.0023(12) -0.0007(12) B1 0.0150(18) 0.0195(19) 0.0168(19) -0.0041(15) -0.0016(14) -0.0011(15) F1 0.0210(12) 0.0294(12) 0.0241(12) -0.0007(10) -0.0075(9) 0.0037(9) F2 0.0297(13) 0.0290(12) 0.0146(11) -0.0006(9) -0.0002(9) -0.0024(10) F3 0.0119(10) 0.0339(13) 0.0239(11) -0.0136(10) -0.0037(8) 0.0002(9) F4 0.0215(12) 0.0352(14) 0.0346(14) -0.0109(11) -0.0048(10) -0.0108(10) B2 0.0163(19) 0.0147(18) 0.024(2) -0.0018(16) -0.0039(15) -0.0001(14) F5 0.0169(11) 0.0221(11) 0.0277(12) -0.0052(9) -0.0041(9) -0.0048(8) F6 0.0166(11) 0.0178(11) 0.0393(14) -0.0067(10) -0.0106(10) 0.0037(8) F7 0.0182(11) 0.0175(11) 0.0380(14) -0.0091(10) -0.0054(10) 0.0001(8) F8 0.0246(12) 0.0348(14) 0.0266(13) -0.0057(11) 0.0018(10) -0.0047(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N21 2.003(3) . ? Cu1 N21 2.003(3) 2_655 ? Cu1 N31 2.067(3) 2_655 ? Cu1 N31 2.067(3) . ? Cu1 N11 2.379(3) 2_655 ? Cu1 N11 2.379(3) . ? Cu2 N12 1.977(3) 2 ? Cu2 N12 1.977(3) . ? Cu2 N32 2.060(3) . ? Cu2 N32 2.060(3) 2 ? Cu2 N22 2.423(3) . ? Cu2 N22 2.423(3) 2 ? N11 C11 1.309(4) . ? N11 N12 1.378(4) . ? N12 C12 1.307(4) . ? N13 C12 1.340(4) . ? N13 C11 1.353(4) . ? N13 N14 1.404(4) . ? N21 C21 1.315(4) . ? N21 N22 1.382(4) . ? N22 C22 1.309(4) . ? N23 C21 1.342(4) . ? N23 C22 1.350(4) . ? N23 N24 1.416(4) . ? N31 C31 1.305(4) . ? N31 N32 1.387(4) . ? N32 C32 1.304(4) . ? N33 C32 1.347(4) . ? N33 C31 1.350(4) . ? N33 N34 1.410(4) . ? B1 F1 1.384(5) . ? B1 F4 1.386(5) . ? B1 F2 1.386(5) . ? B1 F3 1.408(5) . ? B2 F5 1.380(5) . ? B2 F7 1.393(5) . ? B2 F8 1.396(5) . ? B2 F6 1.402(5) . ? 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 N21 Cu1 N21 180.0 . 2_655 ? N21 Cu1 N31 90.08(11) . 2_655 ? N21 Cu1 N31 89.92(11) 2_655 2_655 ? N21 Cu1 N31 89.92(11) . . ? N21 Cu1 N31 90.08(11) 2_655 . ? N31 Cu1 N31 180.0 2_655 . ? N21 Cu1 N11 90.03(10) . 2_655 ? N21 Cu1 N11 89.97(10) 2_655 2_655 ? N31 Cu1 N11 86.94(10) 2_655 2_655 ? N31 Cu1 N11 93.06(10) . 2_655 ? N21 Cu1 N11 89.97(10) . . ? N21 Cu1 N11 90.03(10) 2_655 . ? N31 Cu1 N11 93.06(10) 2_655 . ? N31 Cu1 N11 86.94(10) . . ? N11 Cu1 N11 180.0 2_655 . ? N12 Cu2 N12 180.0 2 . ? N12 Cu2 N32 89.44(11) 2 . ? N12 Cu2 N32 90.56(11) . . ? N12 Cu2 N32 90.56(11) 2 2 ? N12 Cu2 N32 89.44(11) . 2 ? N32 Cu2 N32 180.0 . 2 ? N12 Cu2 N22 91.80(10) 2 . ? N12 Cu2 N22 88.20(10) . . ? N32 Cu2 N22 86.81(10) . . ? N32 Cu2 N22 93.19(10) 2 . ? N12 Cu2 N22 88.20(10) 2 2 ? N12 Cu2 N22 91.80(10) . 2 ? N32 Cu2 N22 93.19(10) . 2 ? N32 Cu2 N22 86.81(10) 2 2 ? N22 Cu2 N22 180.0 . 2 ? C11 N11 N12 106.3(3) . . ? C11 N11 Cu1 128.0(2) . . ? N12 N11 Cu1 125.2(2) . . ? C12 N12 N11 108.1(3) . . ? C12 N12 Cu2 126.2(2) . . ? N11 N12 Cu2 125.6(2) . . ? C12 N13 C11 106.1(3) . . ? C12 N13 N14 128.8(3) . . ? C11 N13 N14 125.0(3) . . ? N11 C11 N13 110.0(3) . . ? N12 C12 N13 109.5(3) . . ? C21 N21 N22 107.8(3) . . ? C21 N21 Cu1 127.8(2) . . ? N22 N21 Cu1 124.3(2) . . ? C22 N22 N21 106.6(3) . . ? C22 N22 Cu2 127.1(2) . . ? N21 N22 Cu2 124.7(2) . . ? C21 N23 C22 106.6(3) . . ? C21 N23 N24 128.1(3) . . ? C22 N23 N24 125.3(3) . . ? N21 C21 N23 109.0(3) . . ? N22 C22 N23 110.0(3) . . ? C31 N31 N32 107.2(3) . . ? C31 N31 Cu1 125.4(2) . . ? N32 N31 Cu1 127.2(2) . . ? C32 N32 N31 107.2(3) . . ? C32 N32 Cu2 124.4(2) . . ? N31 N32 Cu2 128.1(2) . . ? C32 N33 C31 106.4(3) . . ? C32 N33 N34 123.5(3) . . ? C31 N33 N34 130.1(3) . . ? N31 C31 N33 109.6(3) . . ? N32 C32 N33 109.7(3) . . ? F1 B1 F4 110.0(3) . . ? F1 B1 F2 109.0(3) . . ? F4 B1 F2 111.3(3) . . ? F1 B1 F3 109.5(3) . . ? F4 B1 F3 108.5(3) . . ? F2 B1 F3 108.5(3) . . ? F5 B2 F7 110.4(3) . . ? F5 B2 F8 109.4(3) . . ? F7 B2 F8 110.2(3) . . ? F5 B2 F6 108.7(3) . . ? F7 B2 F6 108.9(3) . . ? F8 B2 F6 109.3(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cu1 N11 N12 Cu2 6.4(4) . . . . ? Cu1 N21 N22 Cu2 12.0(4) . . . . ? Cu1 N31 N32 Cu2 -10.4(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1W F5 0.90 2.11 2.816(4) 134.4 . O1W H2W F4 0.76 2.12 2.838(4) 157.3 . N14 H141 F8 0.94 2.25 3.167(4) 165.3 1_544 N14 H142 F3 0.77 2.45 3.134(4) 149.9 1_554 N24 H241 F1 0.85 2.40 3.114(4) 141.5 . N24 H242 F6 0.88 2.06 2.937(4) 174.0 2_666 N34 H341 F8 0.78 2.44 3.210(4) 168.7 2_656 N34 H342 F1 0.96 2.28 3.212(4) 161.5 2_556 _diffrn_measured_fraction_theta_max 0.917 _diffrn_reflns_theta_full 30.28 _diffrn_measured_fraction_theta_full 0.917 _refine_diff_density_max 1.577 _refine_diff_density_min -0.543 _refine_diff_density_rms 0.122 #===END data_cmpd_2 _database_code_CSD 164099 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety '[Cu(amtrz)3](BF4)(SiF6)0.5.2H2O' _chemical_formula_sum 'C12 H32 B2 Cu2 F14 N24 O4 Si' _chemical_formula_weight 1019.41 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' 'Si' 'Si' 0.0817 0.0704 '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' 'O' 'O' 0.0106 0.0060 '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 10.285(2) _cell_length_b 11.727(2) _cell_length_c 15.521(3) _cell_angle_alpha 104.99(3) _cell_angle_beta 91.45(3) _cell_angle_gamma 103.49(3) _cell_volume 1751.1(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3000 _cell_measurement_theta_min 3.38 _cell_measurement_theta_max 28.77 _exptl_crystal_description 'Block' _exptl_crystal_colour 'light-blue' _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.933 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1024 _exptl_absorpt_coefficient_mu 1.389 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8510 _exptl_absorpt_correction_T_max 0.9213 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Kuma KM4CCD' _diffrn_measurement_method '\o scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 'none (area detector data)' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12688 _diffrn_reflns_av_R_equivalents 0.0321 _diffrn_reflns_av_sigmaI/netI 0.0699 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.38 _diffrn_reflns_theta_max 28.77 _reflns_number_total 8014 _reflns_number_gt 4439 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kuma Diffraction Wroclaw' _computing_cell_refinement 'Kuma Diffraction Wroclaw' _computing_data_reduction 'Kuma Diffraction Wroclaw' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-NT V5.1, Brucker AXS 1999' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1002P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8014 _refine_ls_number_parameters 579 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1038 _refine_ls_R_factor_gt 0.0570 _refine_ls_wR_factor_ref 0.1742 _refine_ls_wR_factor_gt 0.1552 _refine_ls_goodness_of_fit_ref 0.972 _refine_ls_restrained_S_all 0.972 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.5000 0.5000 0.0000 0.01835(18) Uani 1 d S . . Cu2 Cu 0.50479(5) 0.49509(5) 0.24941(3) 0.01763(15) Uani 1 d . . . Cu3 Cu 0.5000 0.5000 0.5000 0.01566(18) Uani 1 d S . . Si1 Si 0.94328(14) 0.27579(13) 0.82671(9) 0.0276(3) Uani 1 d . . . F1 F 0.8904(3) 0.3564(3) 0.76400(17) 0.0378(7) Uani 1 d . . . F2 F 0.8903(3) 0.3579(3) 0.91829(17) 0.0372(7) Uani 1 d . . . F3 F 1.0935(3) 0.3789(3) 0.84870(16) 0.0334(7) Uani 1 d . . . F4 F 0.7923(3) 0.1758(3) 0.8053(2) 0.0498(9) Uani 1 d . . . F5 F 0.9968(3) 0.1942(3) 0.7359(2) 0.0490(9) Uani 1 d . . . F6 F 1.0000(3) 0.1989(3) 0.8907(2) 0.0542(9) Uani 1 d . . . B1 B 0.4304(6) -0.0468(6) 0.6495(4) 0.0336(13) Uani 1 d . . . F11 F 0.4148(3) -0.1529(3) 0.6756(2) 0.0449(8) Uani 1 d . . . F21 F 0.5080(3) 0.0517(3) 0.71592(19) 0.0498(9) Uani 1 d . . . F31 F 0.3064(3) -0.0240(3) 0.6362(2) 0.0587(10) Uani 1 d . . . F41 F 0.4961(3) -0.0587(3) 0.57181(18) 0.0382(7) Uani 1 d . . . B2 B 1.0245(8) 0.7330(8) 0.6788(7) 0.067(3) Uani 1 d . . . F12 F 1.1266(6) 0.6917(6) 0.6892(7) 0.143(4) Uani 0.846(7) d P . . F22 F 1.0163(7) 0.7998(10) 0.6168(8) 0.184(5) Uani 0.846(7) d P . . F32 F 1.0003(6) 0.8105(4) 0.7640(5) 0.138(4) Uani 0.846(7) d P . . F42 F 0.9071(7) 0.6386(7) 0.6566(4) 0.0383(14) Uani 0.846(7) d P . . F12' F 1.119(3) 0.732(2) 0.7191(14) 0.024(5) Uiso 0.154(7) d P . . F22' F 1.0948(19) 0.6993(17) 0.5901(13) 0.037(6) Uiso 0.154(7) d P . . F32' F 1.0279(15) 0.8546(13) 0.6780(9) 0.004(4) Uiso 0.154(7) d P . . F42' F 0.892(4) 0.670(3) 0.663(3) 0.020(7) Uiso 0.154(7) d P . . O1W O 0.4948(4) 0.0318(4) 0.8934(3) 0.0557(11) Uani 1 d . . . O2W O 1.0468(7) -0.0906(6) 0.5056(5) 0.0382(17) Uani 0.50 d P . . O3W O 1.1298(8) 0.1670(7) 0.5799(5) 0.0417(19) Uani 0.50 d P . . O4W O 0.7835(9) -0.1408(7) 0.4337(4) 0.0377(18) Uani 0.50 d P . . O5W O 0.6414(8) -0.1046(6) 0.9453(4) 0.0396(19) Uani 0.50 d P . . O6W O 0.7698(11) -0.0084(9) -0.0819(6) 0.078(3) Uani 0.50 d P . . O7W O 0.9063(10) -0.0140(8) 0.9285(8) 0.089(4) Uani 0.50 d P . . N11 N 0.5987(4) 0.3763(3) 0.0727(2) 0.0195(8) Uani 1 d . . . N12 N 0.5860(3) 0.3773(3) 0.1621(2) 0.0181(8) Uani 1 d . . . N13 N 0.6892(4) 0.2380(3) 0.1030(2) 0.0223(8) Uani 1 d . . . N14 N 0.7579(4) 0.1450(4) 0.0920(3) 0.0369(11) Uani 1 d . . . C11 C 0.6619(4) 0.2910(4) 0.0394(3) 0.0211(9) Uani 1 d . . . H11 H 0.6843 0.2704 -0.0193 0.025 Uiso 1 calc R . . C12 C 0.6413(4) 0.2941(4) 0.1779(3) 0.0231(10) Uani 1 d . . . H12 H 0.6466 0.2764 0.2327 0.028 Uiso 1 calc R . . N21 N 0.5910(4) 0.6502(3) 0.0982(2) 0.0202(8) Uani 1 d . . . N22 N 0.6053(4) 0.6514(3) 0.1878(2) 0.0205(8) Uani 1 d . . . N23 N 0.7176(4) 0.8248(3) 0.1713(2) 0.0227(8) Uani 1 d . . . N24 N 0.8023(4) 0.9450(3) 0.1883(3) 0.0302(9) Uani 1 d . . . C21 C 0.6587(5) 0.7554(4) 0.0911(3) 0.0242(10) Uani 1 d . . . H21 H 0.6652 0.7788 0.0382 0.029 Uiso 1 calc R . . C22 C 0.6837(5) 0.7586(4) 0.2297(3) 0.0223(9) Uani 1 d . . . H22 H 0.7113 0.7846 0.2906 0.027 Uiso 1 calc R . . N31 N 0.3406(4) 0.4638(3) 0.0728(2) 0.0203(8) Uani 1 d . . . N32 N 0.3412(3) 0.4571(3) 0.1599(2) 0.0188(8) Uani 1 d . . . N33 N 0.1338(3) 0.4099(3) 0.1035(2) 0.0193(8) Uani 1 d . . . N34 N -0.0082(4) 0.3796(4) 0.0978(2) 0.0272(9) Uani 1 d . . . C31 C 0.2150(4) 0.4375(4) 0.0407(3) 0.0208(9) Uani 1 d . . . H31 H 0.1861 0.4378 -0.0165 0.025 Uiso 1 calc R . . C32 C 0.2149(4) 0.4231(4) 0.1760(3) 0.0190(9) Uani 1 d . . . H32 H 0.1864 0.4101 0.2299 0.023 Uiso 1 calc R . . N41 N 0.4059(4) 0.6116(3) 0.4242(2) 0.0203(8) Uani 1 d . . . N42 N 0.4249(4) 0.6145(3) 0.3363(2) 0.0190(8) Uani 1 d . . . N43 N 0.3245(4) 0.7566(3) 0.3965(2) 0.0202(8) Uani 1 d . . . N44 N 0.2588(4) 0.8512(3) 0.4096(3) 0.0290(9) Uani 1 d . . . C41 C 0.3451(4) 0.6983(4) 0.4589(3) 0.0213(9) Uani 1 d . . . H41 H 0.3203 0.7167 0.5171 0.026 Uiso 1 calc R . . C42 C 0.3757(4) 0.7016(4) 0.3215(3) 0.0186(9) Uani 1 d . . . H42 H 0.3757 0.7228 0.2677 0.022 Uiso 1 calc R . . N51 N 0.4061(3) 0.3471(3) 0.4058(2) 0.0182(7) Uani 1 d . . . N52 N 0.4032(4) 0.3388(3) 0.3149(2) 0.0211(8) Uani 1 d . . . N53 N 0.2867(4) 0.1693(3) 0.3356(3) 0.0279(9) Uani 1 d . . . N54 N 0.2032(5) 0.0497(4) 0.3233(3) 0.0440(12) Uani 1 d . . . C51 C 0.3367(4) 0.2433(4) 0.4158(3) 0.0231(10) Uani 1 d . . . H51 H 0.3243 0.2245 0.4701 0.028 Uiso 1 calc R . . C52 C 0.3300(5) 0.2307(4) 0.2750(3) 0.0272(10) Uani 1 d . . . H52 H 0.3100 0.1999 0.2133 0.033 Uiso 1 calc R . . N61 N 0.6673(3) 0.5235(3) 0.4261(2) 0.0189(8) Uani 1 d . . . N62 N 0.6675(4) 0.5308(3) 0.3386(2) 0.0195(8) Uani 1 d . . . N63 N 0.8750(4) 0.5749(4) 0.3953(2) 0.0230(8) Uani 1 d . . . N64 N 1.0176(4) 0.6102(4) 0.4084(3) 0.0299(9) Uani 1 d . . . C61 C 0.7928(5) 0.5491(4) 0.4583(3) 0.0245(10) Uani 1 d . . . H61 H 0.8212 0.5496 0.5158 0.029 Uiso 1 calc R . . C62 C 0.7935(4) 0.5628(4) 0.3229(3) 0.0219(9) Uani 1 d . . . H62 H 0.8225 0.5753 0.2690 0.026 Uiso 1 calc R . . H441 H 0.3344 0.9180 0.4274 0.050 Uiso 1 d . . . H442 H 0.1934 0.8101 0.3580 0.050 Uiso 1 d . . . H641 H 1.0484 0.7133 0.4209 0.050 Uiso 1 d . . . H642 H 1.0549 0.5715 0.3545 0.050 Uiso 1 d . . . H541 H 0.2224 -0.0079 0.2621 0.050 Uiso 1 d . . . H542 H 0.1088 0.0530 0.3206 0.050 Uiso 1 d . . . H141 H 0.8237 0.1760 0.1373 0.050 Uiso 1 d . . . H142 H 0.7947 0.1305 0.0342 0.050 Uiso 1 d . . . H341 H -0.0413 0.3476 0.0360 0.050 Uiso 1 d . . . H342 H -0.0328 0.4574 0.1200 0.050 Uiso 1 d . . . H241 H 0.8877 0.9230 0.1961 0.050 Uiso 1 d . . . H242 H 0.7640 0.9913 0.1673 0.050 Uiso 1 d . . . H1 H 0.5804 0.0191 0.9033 0.050 Uiso 1 d . . . H2 H 0.4880 0.0336 0.8235 0.050 Uiso 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 Cu1 0.0208(4) 0.0235(4) 0.0101(3) 0.0048(3) 0.0022(3) 0.0038(3) Cu2 0.0209(3) 0.0218(3) 0.0098(2) 0.0044(2) 0.00040(19) 0.0046(2) Cu3 0.0175(4) 0.0182(4) 0.0104(3) 0.0042(3) 0.0012(3) 0.0024(3) Si1 0.0268(7) 0.0311(8) 0.0256(7) 0.0073(6) 0.0036(6) 0.0091(6) F1 0.0367(17) 0.053(2) 0.0274(15) 0.0138(14) -0.0015(13) 0.0149(14) F2 0.0403(17) 0.0486(19) 0.0260(15) 0.0117(14) 0.0090(13) 0.0149(14) F3 0.0279(15) 0.0536(19) 0.0157(13) 0.0117(13) 0.0006(11) 0.0019(13) F4 0.0369(18) 0.0417(19) 0.062(2) 0.0086(17) 0.0090(16) -0.0008(15) F5 0.0452(19) 0.055(2) 0.0417(18) -0.0029(16) 0.0078(15) 0.0193(16) F6 0.050(2) 0.070(2) 0.071(2) 0.052(2) 0.0227(18) 0.0320(18) B1 0.036(3) 0.040(3) 0.028(3) 0.014(3) 0.008(3) 0.010(3) F11 0.053(2) 0.0397(18) 0.0501(19) 0.0266(16) 0.0171(16) 0.0102(15) F21 0.059(2) 0.0418(19) 0.0360(17) 0.0059(15) 0.0028(16) -0.0074(16) F31 0.057(2) 0.076(3) 0.054(2) 0.0182(19) 0.0052(18) 0.038(2) F41 0.0437(18) 0.0372(17) 0.0324(16) 0.0112(14) 0.0089(14) 0.0050(14) B2 0.047(4) 0.053(5) 0.107(7) 0.067(5) -0.030(5) -0.024(4) F12 0.053(3) 0.057(4) 0.304(12) 0.036(6) -0.077(5) 0.009(3) F22 0.086(5) 0.223(10) 0.326(13) 0.243(11) 0.028(7) 0.013(6) F32 0.119(5) 0.033(3) 0.217(8) -0.028(4) -0.132(5) 0.015(3) F42 0.034(3) 0.056(5) 0.020(2) 0.013(3) 0.0027(18) -0.003(3) O1W 0.059(3) 0.056(3) 0.047(2) 0.016(2) -0.002(2) 0.003(2) O2W 0.030(4) 0.032(4) 0.052(4) 0.009(4) 0.011(3) 0.009(3) O3W 0.049(5) 0.037(5) 0.037(4) 0.014(4) 0.001(4) 0.003(4) O4W 0.056(5) 0.039(5) 0.020(4) 0.012(3) 0.000(4) 0.010(4) O5W 0.072(5) 0.022(4) 0.017(3) 0.004(3) -0.011(3) 0.000(4) O6W 0.087(8) 0.068(7) 0.066(6) -0.009(5) -0.018(6) 0.027(6) O7W 0.080(7) 0.046(6) 0.167(10) 0.049(6) 0.090(7) 0.033(5) N11 0.026(2) 0.024(2) 0.0081(16) 0.0038(14) 0.0016(14) 0.0045(16) N12 0.024(2) 0.0188(19) 0.0114(17) 0.0047(14) 0.0042(15) 0.0046(15) N13 0.026(2) 0.022(2) 0.0192(19) 0.0048(16) 0.0007(16) 0.0084(16) N14 0.049(3) 0.044(3) 0.023(2) 0.0022(19) 0.003(2) 0.030(2) C11 0.026(2) 0.025(2) 0.012(2) 0.0067(18) 0.0030(18) 0.0053(19) C12 0.030(3) 0.024(2) 0.015(2) 0.0057(18) 0.0007(19) 0.0036(19) N21 0.026(2) 0.024(2) 0.0099(17) 0.0056(15) 0.0008(15) 0.0050(16) N22 0.0213(19) 0.026(2) 0.0128(17) 0.0044(15) 0.0020(14) 0.0045(16) N23 0.021(2) 0.024(2) 0.023(2) 0.0087(16) 0.0026(16) 0.0033(16) N24 0.031(2) 0.022(2) 0.039(2) 0.0180(19) -0.0026(19) -0.0022(17) C21 0.028(3) 0.028(3) 0.017(2) 0.0078(19) 0.0007(19) 0.007(2) C22 0.030(3) 0.023(2) 0.013(2) 0.0047(18) 0.0016(18) 0.0055(19) N31 0.025(2) 0.026(2) 0.0097(16) 0.0059(15) 0.0020(15) 0.0046(16) N32 0.0207(19) 0.026(2) 0.0114(17) 0.0062(15) 0.0027(14) 0.0065(15) N33 0.0197(19) 0.027(2) 0.0138(17) 0.0089(15) 0.0044(15) 0.0059(15) N34 0.0153(19) 0.043(3) 0.023(2) 0.0100(18) -0.0002(16) 0.0047(17) C31 0.021(2) 0.028(2) 0.015(2) 0.0090(18) 0.0024(18) 0.0058(18) C32 0.022(2) 0.022(2) 0.014(2) 0.0079(18) 0.0005(17) 0.0034(17) N41 0.028(2) 0.021(2) 0.0113(17) 0.0052(15) 0.0048(15) 0.0037(16) N42 0.024(2) 0.0197(19) 0.0084(16) 0.0014(14) 0.0002(14) -0.0007(15) N43 0.026(2) 0.0167(19) 0.0192(18) 0.0052(15) 0.0031(15) 0.0068(15) N44 0.034(2) 0.020(2) 0.032(2) 0.0017(17) -0.0037(18) 0.0112(17) C41 0.027(2) 0.021(2) 0.013(2) 0.0023(18) 0.0012(18) 0.0030(18) C42 0.018(2) 0.024(2) 0.014(2) 0.0056(18) 0.0029(17) 0.0040(17) N51 0.0225(19) 0.0198(19) 0.0128(17) 0.0049(15) 0.0013(14) 0.0061(15) N52 0.031(2) 0.024(2) 0.0093(17) 0.0063(15) -0.0010(15) 0.0051(16) N53 0.034(2) 0.016(2) 0.028(2) 0.0055(17) -0.0112(18) -0.0010(16) N54 0.053(3) 0.021(2) 0.048(3) 0.015(2) -0.020(2) -0.012(2) C51 0.021(2) 0.024(2) 0.025(2) 0.012(2) -0.0008(19) 0.0019(18) C52 0.033(3) 0.025(3) 0.021(2) 0.005(2) -0.006(2) 0.002(2) N61 0.0183(19) 0.0219(19) 0.0152(17) 0.0068(15) -0.0003(15) 0.0007(15) N62 0.026(2) 0.0225(19) 0.0108(16) 0.0076(15) 0.0023(15) 0.0041(15) N63 0.0190(19) 0.034(2) 0.0160(18) 0.0083(16) 0.0017(15) 0.0042(16) N64 0.0142(19) 0.044(3) 0.033(2) 0.015(2) 0.0046(17) 0.0030(17) C61 0.027(3) 0.034(3) 0.014(2) 0.0099(19) 0.0022(18) 0.006(2) C62 0.024(2) 0.028(2) 0.014(2) 0.0076(19) 0.0017(18) 0.0046(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N21 2.018(4) 2_665 ? Cu1 N21 2.018(4) . ? Cu1 N31 2.041(3) . ? Cu1 N31 2.041(3) 2_665 ? Cu1 N11 2.426(3) 2_665 ? Cu1 N11 2.426(3) . ? Cu2 N12 2.017(3) . ? Cu2 N42 2.018(4) . ? Cu2 N62 2.037(4) . ? Cu2 N32 2.043(3) . ? Cu2 N22 2.328(4) . ? Cu2 N52 2.367(4) . ? Cu3 N51 2.013(4) . ? Cu3 N51 2.013(4) 2_666 ? Cu3 N61 2.096(3) 2_666 ? Cu3 N61 2.096(3) . ? Cu3 N41 2.315(3) . ? Cu3 N41 2.315(3) 2_666 ? Si1 F5 1.671(3) . ? Si1 F6 1.678(3) . ? Si1 F4 1.679(3) . ? Si1 F2 1.680(3) . ? Si1 F1 1.681(3) . ? Si1 F3 1.689(3) . ? B1 F11 1.381(7) . ? B1 F31 1.383(7) . ? B1 F41 1.389(6) . ? B1 F21 1.395(7) . ? B2 F12' 1.15(3) . ? B2 F12 1.277(10) . ? B2 F42' 1.37(4) . ? B2 F42 1.400(10) . ? B2 F22 1.401(9) . ? B2 F32' 1.421(17) . ? B2 F32 1.462(12) . ? B2 F22' 1.57(2) . ? F12 F12' 0.59(2) . ? F12 F22' 1.59(2) . ? F22 F32' 0.985(17) . ? F22 F22' 1.56(2) . ? F32 F32' 1.562(17) . ? F32 F12' 1.75(2) . ? O3W O4W 1.019(9) 2_756 ? O4W O3W 1.019(9) 2_756 ? O5W O6W 1.665(13) 1_556 ? O6W O7W 1.428(13) 1_554 ? O6W O5W 1.665(13) 1_554 ? O7W O6W 1.428(13) 1_556 ? N11 C11 1.321(5) . ? N11 N12 1.394(4) . ? N12 C12 1.307(5) . ? N13 C12 1.346(5) . ? N13 C11 1.350(5) . ? N13 N14 1.410(5) . ? N21 C21 1.301(6) . ? N21 N22 1.390(4) . ? N22 C22 1.316(5) . ? N23 C21 1.337(5) . ? N23 C22 1.342(5) . ? N23 N24 1.427(5) . ? N31 C31 1.309(5) . ? N31 N32 1.373(4) . ? N32 C32 1.317(5) . ? N33 C32 1.338(5) . ? N33 C31 1.354(5) . ? N33 N34 1.415(5) . ? N41 C41 1.321(5) . ? N41 N42 1.392(4) . ? N42 C42 1.307(5) . ? N43 C41 1.360(5) . ? N43 C42 1.361(5) . ? N43 N44 1.403(5) . ? N51 C51 1.308(5) . ? N51 N52 1.389(4) . ? N52 C52 1.297(6) . ? N53 C51 1.329(5) . ? N53 C52 1.351(6) . ? N53 N54 1.425(5) . ? N61 C61 1.310(5) . ? N61 N62 1.383(4) . ? N62 C62 1.310(5) . ? N63 C62 1.342(5) . ? N63 C61 1.355(5) . ? N63 N64 1.422(5) . ? 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 N21 Cu1 N21 180.0 2_665 . ? N21 Cu1 N31 88.55(14) 2_665 . ? N21 Cu1 N31 91.45(14) . . ? N21 Cu1 N31 91.45(14) 2_665 2_665 ? N21 Cu1 N31 88.55(14) . 2_665 ? N31 Cu1 N31 180.0 . 2_665 ? N21 Cu1 N11 89.91(13) 2_665 2_665 ? N21 Cu1 N11 90.09(13) . 2_665 ? N31 Cu1 N11 93.94(13) . 2_665 ? N31 Cu1 N11 86.06(13) 2_665 2_665 ? N21 Cu1 N11 90.09(13) 2_665 . ? N21 Cu1 N11 89.91(13) . . ? N31 Cu1 N11 86.06(13) . . ? N31 Cu1 N11 93.94(13) 2_665 . ? N11 Cu1 N11 180.0 2_665 . ? N12 Cu2 N42 179.34(14) . . ? N12 Cu2 N62 89.01(14) . . ? N42 Cu2 N62 90.90(14) . . ? N12 Cu2 N32 90.60(14) . . ? N42 Cu2 N32 89.50(14) . . ? N62 Cu2 N32 179.31(14) . . ? N12 Cu2 N22 90.49(13) . . ? N42 Cu2 N22 88.86(13) . . ? N62 Cu2 N22 92.29(13) . . ? N32 Cu2 N22 88.29(13) . . ? N12 Cu2 N52 90.41(13) . . ? N42 Cu2 N52 90.24(13) . . ? N62 Cu2 N52 87.07(13) . . ? N32 Cu2 N52 92.35(13) . . ? N22 Cu2 N52 178.90(12) . . ? N51 Cu3 N51 180.0 . 2_666 ? N51 Cu3 N61 88.78(14) . 2_666 ? N51 Cu3 N61 91.22(14) 2_666 2_666 ? N51 Cu3 N61 91.22(14) . . ? N51 Cu3 N61 88.78(14) 2_666 . ? N61 Cu3 N61 180.0 2_666 . ? N51 Cu3 N41 88.98(13) . . ? N51 Cu3 N41 91.02(13) 2_666 . ? N61 Cu3 N41 90.90(13) 2_666 . ? N61 Cu3 N41 89.10(13) . . ? N51 Cu3 N41 91.02(13) . 2_666 ? N51 Cu3 N41 88.98(13) 2_666 2_666 ? N61 Cu3 N41 89.10(13) 2_666 2_666 ? N61 Cu3 N41 90.90(13) . 2_666 ? N41 Cu3 N41 180.0 . 2_666 ? F5 Si1 F6 90.95(18) . . ? F5 Si1 F4 90.44(18) . . ? F6 Si1 F4 91.60(18) . . ? F5 Si1 F2 179.71(18) . . ? F6 Si1 F2 88.88(16) . . ? F4 Si1 F2 89.80(17) . . ? F5 Si1 F1 89.50(16) . . ? F6 Si1 F1 178.25(19) . . ? F4 Si1 F1 90.09(17) . . ? F2 Si1 F1 90.67(15) . . ? F5 Si1 F3 90.46(17) . . ? F6 Si1 F3 89.28(17) . . ? F4 Si1 F3 178.74(18) . . ? F2 Si1 F3 89.31(16) . . ? F1 Si1 F3 89.03(16) . . ? F11 B1 F31 110.1(5) . . ? F11 B1 F41 108.8(4) . . ? F31 B1 F41 111.1(4) . . ? F11 B1 F21 110.2(4) . . ? F31 B1 F21 108.1(5) . . ? F41 B1 F21 108.5(4) . . ? F12' B2 F12 27.6(11) . . ? F12' B2 F42' 138(2) . . ? F12 B2 F42' 128.0(14) . . ? F12' B2 F42 125.1(14) . . ? F12 B2 F42 110.8(8) . . ? F42' B2 F42 17.7(13) . . ? F12' B2 F22 127.4(13) . . ? F12 B2 F22 122.1(10) . . ? F42' B2 F22 94.5(16) . . ? F42 B2 F22 103.9(7) . . ? F12' B2 F32' 109.5(15) . . ? F12 B2 F32' 125.8(9) . . ? F42' B2 F32' 106.1(15) . . ? F42 B2 F32' 122.9(9) . . ? F22 B2 F32' 40.8(7) . . ? F12' B2 F32 83.3(12) . . ? F12 B2 F32 110.2(8) . . ? F42' B2 F32 91.7(16) . . ? F42 B2 F32 103.3(7) . . ? F22 B2 F32 104.7(9) . . ? F32' B2 F32 65.6(8) . . ? F12' B2 F22' 89.4(14) . . ? F12 B2 F22' 67.0(10) . . ? F42' B2 F22' 108.4(18) . . ? F42 B2 F22' 99.1(10) . . ? F22 B2 F22' 62.8(9) . . ? F32' B2 F22' 96.4(10) . . ? F32 B2 F22' 156.5(9) . . ? F12' F12 B2 64(3) . . ? F12' F12 F22' 117(3) . . ? B2 F12 F22' 65.4(9) . . ? F32' F22 B2 70.7(12) . . ? F32' F22 F22' 121.6(14) . . ? B2 F22 F22' 64.1(9) . . ? B2 F32 F32' 56.0(7) . . ? B2 F32 F12' 40.6(8) . . ? F32' F32 F12' 78.6(10) . . ? F12 F12' B2 89(3) . . ? F12 F12' F32 143(4) . . ? B2 F12' F32 56.1(11) . . ? F22 F22' B2 53.2(7) . . ? F22 F22' F12 96.2(12) . . ? B2 F22' F12 47.5(7) . . ? F22 F32' B2 68.5(11) . . ? F22 F32' F32 124.3(15) . . ? B2 F32' F32 58.5(7) . . ? O7W O6W O5W 123.7(8) 1_554 1_554 ? C11 N11 N12 106.1(3) . . ? C11 N11 Cu1 130.4(3) . . ? N12 N11 Cu1 123.3(2) . . ? C12 N12 N11 107.7(3) . . ? C12 N12 Cu2 128.0(3) . . ? N11 N12 Cu2 124.3(3) . . ? C12 N13 C11 106.2(4) . . ? C12 N13 N14 127.8(4) . . ? C11 N13 N14 125.9(4) . . ? N11 C11 N13 110.1(4) . . ? N12 C12 N13 109.9(4) . . ? C21 N21 N22 107.5(3) . . ? C21 N21 Cu1 128.7(3) . . ? N22 N21 Cu1 123.3(3) . . ? C22 N22 N21 106.2(3) . . ? C22 N22 Cu2 127.7(3) . . ? N21 N22 Cu2 126.1(3) . . ? C21 N23 C22 106.8(4) . . ? C21 N23 N24 125.2(4) . . ? C22 N23 N24 128.1(4) . . ? N21 C21 N23 109.8(4) . . ? N22 C22 N23 109.7(4) . . ? C31 N31 N32 107.4(3) . . ? C31 N31 Cu1 123.9(3) . . ? N32 N31 Cu1 128.6(3) . . ? C32 N32 N31 107.0(3) . . ? C32 N32 Cu2 125.8(3) . . ? N31 N32 Cu2 127.2(3) . . ? C32 N33 C31 106.1(3) . . ? C32 N33 N34 125.6(3) . . ? C31 N33 N34 128.3(3) . . ? N31 C31 N33 109.6(4) . . ? N32 C32 N33 109.9(4) . . ? C41 N41 N42 106.9(3) . . ? C41 N41 Cu3 127.1(3) . . ? N42 N41 Cu3 125.1(3) . . ? C42 N42 N41 107.7(3) . . ? C42 N42 Cu2 128.3(3) . . ? N41 N42 Cu2 123.8(3) . . ? C41 N43 C42 106.0(3) . . ? C41 N43 N44 125.0(4) . . ? C42 N43 N44 129.0(4) . . ? N41 C41 N43 109.6(4) . . ? N42 C42 N43 109.8(4) . . ? C51 N51 N52 108.3(3) . . ? C51 N51 Cu3 129.1(3) . . ? N52 N51 Cu3 122.6(3) . . ? C52 N52 N51 105.7(3) . . ? C52 N52 Cu2 128.1(3) . . ? N51 N52 Cu2 126.2(3) . . ? C51 N53 C52 106.7(4) . . ? C51 N53 N54 123.0(4) . . ? C52 N53 N54 130.3(4) . . ? N51 C51 N53 108.9(4) . . ? N52 C52 N53 110.4(4) . . ? C61 N61 N62 107.3(3) . . ? C61 N61 Cu3 125.5(3) . . ? N62 N61 Cu3 126.7(3) . . ? C62 N62 N61 106.8(3) . . ? C62 N62 Cu2 126.1(3) . . ? N61 N62 Cu2 127.1(3) . . ? C62 N63 C61 105.7(4) . . ? C62 N63 N64 129.4(4) . . ? C61 N63 N64 124.9(4) . . ? N61 C61 N63 109.8(4) . . ? N62 C62 N63 110.5(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cu1 N11 N12 Cu2 -7.9(4) . . . . ? Cu1 N21 N22 Cu2 -9.4(4) . . . . ? Cu1 N31 N32 Cu2 5.4(5) . . . . ? Cu2 N42 N41 Cu3 13.9(4) . . . . ? Cu2 N52 N51 Cu3 0.4(4) . . . . ? Cu2 N62 N61 Cu3 -10.3(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H2 F21 1.09 1.75 2.827(5) 169.5 . O1W H1 O5W 0.94 1.95 2.685(8) 133.0 . O1W H1 O6W 0.94 2.06 3.005(11) 176.9 1_556 N14 H141 F32 0.90 2.29 3.156(6) 160.7 2_766 N14 H141 F12' 0.90 2.21 3.01(2) 147.7 2_766 N14 H142 O6W 0.97 2.06 2.854(10) 137.9 . N24 H241 F5 0.98 2.42 3.281(5) 145.5 2_766 N24 H241 F6 0.98 2.25 3.024(5) 135.1 2_766 N24 H242 N14 0.86 2.40 3.197(6) 154.4 1_565 N34 H341 F2 0.96 1.98 2.878(5) 154.7 1_454 N34 H342 F3 0.98 2.10 3.075(5) 173.1 2_666 N44 H441 F41 0.94 2.10 3.015(5) 164.0 2_666 N44 H442 F1 0.97 2.32 3.194(5) 149.6 2_666 N44 H442 F5 0.97 2.39 3.274(5) 150.3 2_666 N54 H541 F4 1.07 1.94 2.883(6) 144.9 2_656 N54 H542 F22 0.98 2.41 3.192(11) 136.3 2_666 N54 H542 F32' 0.98 1.96 2.857(16) 150.4 2_666 N64 H641 O2W 1.14 2.34 3.380(8) 150.9 1_565 N64 H642 F1 0.98 2.25 2.951(5) 128.0 2_766 _diffrn_measured_fraction_theta_max 0.880 _diffrn_reflns_theta_full 28.77 _diffrn_measured_fraction_theta_full 0.880 _refine_diff_density_max 1.345 _refine_diff_density_min -0.915 _refine_diff_density_rms 0.122 #===END data_cmpd_3 _database_code_CSD 164100 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety '[Cu(amtrz)3](SiF6).8/3H2O' _chemical_formula_sum 'C18 H52 Cu3 F18 N36 O8 Si3' _chemical_formula_weight 1517.85 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 '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 12.417(2) _cell_length_b 13.150(3) _cell_length_c 18.030(4) _cell_angle_alpha 73.63(3) _cell_angle_beta 72.64(3) _cell_angle_gamma 70.28(3) _cell_volume 2590.8(9) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 3.32 _cell_measurement_theta_max 27.99 _exptl_crystal_description 'Block' _exptl_crystal_colour 'light-blue' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.946 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1534 _exptl_absorpt_coefficient_mu 1.436 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8134 _exptl_absorpt_correction_T_max 0.8697 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Kuma KM4CCD' _diffrn_measurement_method '\o scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 'none (area detector data)' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18608 _diffrn_reflns_av_R_equivalents 0.0455 _diffrn_reflns_av_sigmaI/netI 0.0685 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.32 _diffrn_reflns_theta_max 27.99 _reflns_number_total 11646 _reflns_number_gt 6844 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kuma Diffraction Wroclaw' _computing_cell_refinement 'Kuma Diffraction Wroclaw' _computing_data_reduction 'Kuma Diffraction Wroclaw' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-NT V5.1, Brucker AXS 1999' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0970P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11646 _refine_ls_number_parameters 778 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0868 _refine_ls_R_factor_gt 0.0511 _refine_ls_wR_factor_ref 0.1575 _refine_ls_wR_factor_gt 0.1420 _refine_ls_goodness_of_fit_ref 0.930 _refine_ls_restrained_S_all 0.930 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 1.0000 0.0000 0.0000 0.01202(15) Uani 1 d S . . Cu2 Cu 0.83288(4) 0.17033(3) 0.16265(2) 0.01176(12) Uani 1 d . . . Cu3 Cu 0.66980(4) 0.34149(3) 0.32749(2) 0.01215(12) Uani 1 d . . . Cu4 Cu 0.5000 0.5000 0.5000 0.01092(14) Uani 1 d S . . Si1 Si 1.38689(11) -0.17293(9) 0.19963(6) 0.0231(3) Uani 1 d . . . F11 F 1.3671(2) -0.2913(2) 0.25746(15) 0.0385(7) Uani 1 d . . . F21 F 1.4505(2) -0.1546(2) 0.26266(14) 0.0415(7) Uani 1 d . . . F31 F 1.4092(2) -0.05221(18) 0.13859(14) 0.0347(6) Uani 1 d . . . F41 F 1.2572(2) -0.1023(2) 0.24642(14) 0.0377(6) Uani 1 d . . . F51 F 1.5176(2) -0.2384(2) 0.15034(15) 0.0382(7) Uani 1 d . . . F61 F 1.3208(2) -0.1854(2) 0.13490(13) 0.0335(6) Uani 1 d . . . Si2 Si 1.74911(9) -0.17780(8) 0.51077(6) 0.0172(2) Uani 1 d . . . F12 F 1.62354(19) -0.19411(19) 0.50363(12) 0.0222(5) Uani 1 d . . . F22 F 1.6829(2) -0.04544(18) 0.51741(14) 0.0292(6) Uani 1 d . . . F32 F 1.71267(19) -0.21624(18) 0.60982(12) 0.0235(5) Uani 1 d . . . F42 F 1.7880(2) -0.14202(19) 0.41179(12) 0.0271(5) Uani 1 d . . . F52 F 1.87747(19) -0.16453(18) 0.51867(12) 0.0236(5) Uani 1 d . . . F62 F 1.8168(2) -0.31117(18) 0.50530(14) 0.0296(6) Uani 1 d . . . Si3 Si 1.91089(9) 0.51348(8) -0.16658(6) 0.0170(2) Uani 1 d . . . F13 F 2.04027(18) 0.52525(18) -0.16176(12) 0.0199(5) Uani 1 d . . . F23 F 1.88479(19) 0.45811(18) -0.06981(12) 0.0242(5) Uani 1 d . . . F33 F 1.93509(19) 0.56958(17) -0.26352(12) 0.0217(5) Uani 1 d . . . F43 F 1.78058(19) 0.50214(18) -0.17300(12) 0.0252(5) Uani 1 d . . . F53 F 1.9797(2) 0.38722(17) -0.18840(13) 0.0264(5) Uani 1 d . . . F63 F 1.84224(19) 0.64035(18) -0.14570(13) 0.0254(5) Uani 1 d . . . O1W O 1.9688(2) -0.0070(2) 0.40132(15) 0.0226(6) Uani 1 d . . . O2W O 1.6704(3) 0.3515(2) -0.06957(16) 0.0270(7) Uani 1 d . . . O3W O 1.5772(2) 0.6988(2) -0.18695(16) 0.0278(7) Uani 1 d . . . O4W O 2.0957(3) -0.3509(2) 0.51658(17) 0.0310(7) Uani 1 d . . . O5W O 1.0482(2) 0.4523(2) 0.58974(17) 0.0303(7) Uani 1 d . . . O6W O 1.6125(3) -0.0893(2) -0.24583(18) 0.0335(7) Uani 1 d . . . O7W O 1.7657(3) -0.1335(3) -0.10278(17) 0.0376(8) Uani 1 d . . . O8W O 0.3052(3) 0.1418(2) 0.83145(16) 0.0280(7) Uani 1 d . . . C11 C 0.7406(3) 0.0464(3) 0.0089(2) 0.0178(8) Uani 1 d . . . C12 C 0.6507(3) 0.1628(3) 0.0866(2) 0.0148(7) Uani 1 d . . . N11 N 0.8202(3) 0.0609(2) 0.03560(16) 0.0147(6) Uani 1 d . . . N12 N 0.7624(3) 0.1338(2) 0.08606(16) 0.0151(7) Uani 1 d . . . N13 N 0.6334(3) 0.1087(2) 0.03950(17) 0.0165(7) Uani 1 d . . . N14 N 0.5230(3) 0.1218(3) 0.02672(18) 0.0205(7) Uani 1 d . . . C21 C 1.0961(3) 0.2180(3) -0.0313(2) 0.0163(8) Uani 1 d . . . C22 C 0.9967(3) 0.3040(3) 0.0639(2) 0.0151(8) Uani 1 d . . . N21 N 1.0197(3) 0.1639(2) 0.01268(17) 0.0160(7) Uani 1 d . . . N22 N 0.9566(3) 0.2189(2) 0.07409(16) 0.0127(6) Uani 1 d . . . N23 N 1.0841(3) 0.3043(2) -0.00077(17) 0.0158(7) Uani 1 d . . . N24 N 1.1526(3) 0.3793(2) -0.03328(18) 0.0200(7) Uani 1 d . . . C31 C 1.0702(3) -0.1680(3) 0.1404(2) 0.0160(8) Uani 1 d . . . C32 C 0.9873(3) -0.0837(3) 0.2389(2) 0.0186(8) Uani 1 d . . . N31 N 1.0112(3) -0.0685(2) 0.11297(16) 0.0129(6) Uani 1 d . . . N32 N 0.9581(3) -0.0133(2) 0.17546(16) 0.0137(6) Uani 1 d . . . N33 N 1.0564(3) -0.1806(2) 0.21922(17) 0.0176(7) Uani 1 d . . . N34 N 1.1061(3) -0.2745(3) 0.27296(19) 0.0245(8) Uani 1 d . . . C41 C 0.6761(3) 0.0324(3) 0.2664(2) 0.0180(8) Uani 1 d . . . C42 C 0.5779(3) 0.1200(3) 0.3607(2) 0.0193(8) Uani 1 d . . . N41 N 0.7098(3) 0.1213(2) 0.25232(17) 0.0156(7) Uani 1 d . . . N42 N 0.6474(3) 0.1783(2) 0.31235(16) 0.0157(7) Uani 1 d . . . N43 N 0.5937(3) 0.0294(3) 0.33316(18) 0.0194(7) Uani 1 d . . . N44 N 0.5390(3) -0.0566(3) 0.3658(2) 0.0327(9) Uani 1 d . . . C51 C 0.6942(3) 0.4163(3) 0.0866(2) 0.0175(8) Uani 1 d . . . C52 C 0.6061(3) 0.5104(3) 0.1787(2) 0.0171(8) Uani 1 d . . . N51 N 0.7159(3) 0.3509(2) 0.15302(17) 0.0132(6) Uani 1 d . . . N52 N 0.6598(3) 0.4115(2) 0.21200(17) 0.0148(6) Uani 1 d . . . N53 N 0.6262(3) 0.5164(2) 0.09938(17) 0.0159(7) Uani 1 d . . . N54 N 0.5900(3) 0.6050(3) 0.03772(18) 0.0241(8) Uani 1 d . . . C61 C 1.0140(3) 0.1685(3) 0.2427(2) 0.0139(7) Uani 1 d . . . C62 C 0.9248(3) 0.2764(3) 0.3266(2) 0.0156(8) Uani 1 d . . . N61 N 0.9030(3) 0.2030(2) 0.24002(16) 0.0147(6) Uani 1 d . . . N62 N 0.8459(3) 0.2716(2) 0.29416(16) 0.0127(6) Uani 1 d . . . N63 N 1.0305(3) 0.2123(2) 0.29585(17) 0.0154(7) Uani 1 d . . . N64 N 1.1406(3) 0.1965(3) 0.31132(18) 0.0176(7) Uani 1 d . . . C71 C 0.7454(3) 0.1724(3) 0.4686(2) 0.0156(8) Uani 1 d . . . C72 C 0.6453(3) 0.2499(3) 0.5686(2) 0.0188(8) Uani 1 d . . . N71 N 0.6810(3) 0.2706(2) 0.44154(16) 0.0143(6) Uani 1 d . . . N72 N 0.6186(3) 0.3206(2) 0.50512(17) 0.0145(6) Uani 1 d . . . N73 N 0.7235(3) 0.1575(2) 0.54823(17) 0.0147(6) Uani 1 d . . . N74 N 0.7788(3) 0.0616(2) 0.59767(18) 0.0198(7) Uani 1 d . . . C81 C 0.4171(3) 0.3987(3) 0.3292(2) 0.0137(7) Uani 1 d . . . C82 C 0.3221(3) 0.5034(3) 0.4141(2) 0.0135(7) Uani 1 d . . . N81 N 0.4937(3) 0.4068(2) 0.36182(16) 0.0145(6) Uani 1 d . . . N82 N 0.4317(3) 0.4737(2) 0.41686(16) 0.0142(6) Uani 1 d . . . N83 N 0.3090(3) 0.4585(2) 0.35913(17) 0.0152(6) Uani 1 d . . . N84 N 0.2017(3) 0.4672(3) 0.34342(18) 0.0171(7) Uani 1 d . . . C91 C 0.7596(3) 0.5598(3) 0.3035(2) 0.0182(8) Uani 1 d . . . C92 C 0.6617(3) 0.6407(3) 0.4016(2) 0.0175(8) Uani 1 d . . . N91 N 0.6880(3) 0.5015(2) 0.34882(17) 0.0156(7) Uani 1 d . . . N92 N 0.6251(3) 0.5532(2) 0.41147(16) 0.0132(6) Uani 1 d . . . N93 N 0.7451(3) 0.6457(2) 0.33538(18) 0.0179(7) Uani 1 d . . . N94 N 0.8040(3) 0.7291(3) 0.30089(19) 0.0221(7) Uani 1 d . . . H1W1 H 2.0536 -0.0185 0.4059 0.040 Uiso 1 d . . . H2W1 H 1.9422 -0.0652 0.4415 0.040 Uiso 1 d . . . H1W2 H 1.6784 0.2958 -0.0937 0.040 Uiso 1 d . . . H2W2 H 1.7194 0.4031 -0.1111 0.040 Uiso 1 d . . . H1W3 H 1.5773 0.7695 -0.2196 0.040 Uiso 1 d . . . H2W3 H 1.6453 0.6445 -0.1557 0.040 Uiso 1 d . . . H1W4 H 2.0619 -0.4151 0.5438 0.040 Uiso 1 d . . . H2W4 H 2.0198 -0.2926 0.4980 0.040 Uiso 1 d . . . H1W5 H 0.9656 0.4545 0.6039 0.040 Uiso 1 d . . . H2W5 H 1.0603 0.3924 0.5620 0.040 Uiso 1 d . . . H1W6 H 1.6970 -0.1123 -0.2643 0.040 Uiso 1 d . . . H1W7 H 1.7088 -0.0628 -0.1325 0.040 Uiso 1 d . . . H1W8 H 0.2786 0.1865 0.7787 0.040 Uiso 1 d . . . H2W8 H 0.3219 0.1742 0.8608 0.040 Uiso 1 d . . . H13N H 0.5389 0.1248 -0.0297 0.040 Uiso 1 d . . . H14N H 0.5128 0.0517 0.0590 0.040 Uiso 1 d . . . H23N H 1.1201 0.4390 -0.0723 0.040 Uiso 1 d . . . H24N H 1.1502 0.4066 0.0114 0.040 Uiso 1 d . . . H33N H 1.1029 -0.3386 0.2607 0.040 Uiso 1 d . . . H34N H 1.1598 -0.2353 0.2737 0.040 Uiso 1 d . . . H43N H 0.5512 -0.0813 0.4184 0.040 Uiso 1 d . . . H44N H 0.4716 -0.0357 0.3428 0.040 Uiso 1 d . . . H53N H 0.5958 0.6717 0.0452 0.040 Uiso 1 d . . . H54N H 0.5076 0.6147 0.0456 0.040 Uiso 1 d . . . H63N H 1.1533 0.2682 0.2926 0.040 Uiso 1 d . . . H64N H 1.1251 0.1764 0.3682 0.040 Uiso 1 d . . . H73N H 0.7563 0.0709 0.6515 0.040 Uiso 1 d . . . H74N H 0.7552 -0.0006 0.5971 0.040 Uiso 1 d . . . H83N H 0.1906 0.3930 0.3702 0.040 Uiso 1 d . . . H84N H 0.2253 0.4796 0.2869 0.040 Uiso 1 d . . . H93N H 0.8881 0.7059 0.2904 0.040 Uiso 1 d . . . H94N H 0.7995 0.7561 0.3462 0.040 Uiso 1 d . . . H11C H 0.7500 -0.0083 -0.0286 0.040 Uiso 1 d . . . H12C H 0.5781 0.2181 0.1191 0.040 Uiso 1 d . . . H21C H 1.1642 0.2015 -0.0832 0.040 Uiso 1 d . . . H22C H 0.9670 0.3589 0.1047 0.040 Uiso 1 d . . . H31C H 1.1155 -0.2253 0.1013 0.040 Uiso 1 d . . . H32C H 0.9702 -0.0728 0.2989 0.040 Uiso 1 d . . . H41C H 0.7071 -0.0266 0.2282 0.040 Uiso 1 d . . . H42C H 0.5205 0.1355 0.4164 0.040 Uiso 1 d . . . H51C H 0.7232 0.3927 0.0298 0.040 Uiso 1 d . . . H52C H 0.5526 0.5776 0.2083 0.040 Uiso 1 d . . . H61C H 1.0802 0.1168 0.2047 0.040 Uiso 1 d . . . H62C H 0.9146 0.3202 0.3718 0.040 Uiso 1 d . . . H71C H 0.8015 0.1095 0.4356 0.040 Uiso 1 d . . . H72C H 0.6151 0.2557 0.6302 0.040 Uiso 1 d . . . H81C H 0.4304 0.3496 0.2866 0.040 Uiso 1 d . . . H82C H 0.2505 0.5575 0.4480 0.040 Uiso 1 d . . . H91C H 0.8281 0.5411 0.2521 0.040 Uiso 1 d . . . H92C H 0.6268 0.6994 0.4402 0.040 Uiso 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 Cu1 0.0129(3) 0.0116(3) 0.0093(3) -0.0049(2) -0.0007(2) 0.0002(2) Cu2 0.0135(2) 0.0121(2) 0.0087(2) -0.00514(16) -0.00021(17) -0.00177(18) Cu3 0.0121(2) 0.0130(2) 0.0087(2) -0.00533(17) -0.00049(17) 0.00077(18) Cu4 0.0120(3) 0.0121(3) 0.0083(3) -0.0051(2) -0.0007(2) -0.0017(2) Si1 0.0305(7) 0.0217(6) 0.0165(5) -0.0031(4) -0.0043(5) -0.0079(5) F11 0.0507(17) 0.0330(15) 0.0322(14) 0.0056(11) -0.0124(13) -0.0195(13) F21 0.0530(18) 0.0547(18) 0.0261(14) -0.0084(12) -0.0106(13) -0.0247(14) F31 0.0417(16) 0.0211(13) 0.0356(14) -0.0004(10) -0.0047(12) -0.0092(11) F41 0.0338(15) 0.0436(16) 0.0336(14) -0.0182(12) 0.0022(12) -0.0079(12) F51 0.0357(15) 0.0279(14) 0.0422(16) -0.0127(12) 0.0009(12) -0.0014(12) F61 0.0440(16) 0.0384(15) 0.0229(12) -0.0077(11) -0.0095(11) -0.0144(12) Si2 0.0191(6) 0.0165(5) 0.0151(5) -0.0048(4) -0.0030(4) -0.0032(4) F12 0.0202(12) 0.0309(13) 0.0183(11) -0.0107(9) -0.0034(9) -0.0067(10) F22 0.0317(14) 0.0171(12) 0.0358(14) -0.0080(10) -0.0076(11) -0.0006(10) F32 0.0243(13) 0.0335(13) 0.0140(11) -0.0042(9) -0.0032(9) -0.0108(10) F42 0.0295(13) 0.0392(14) 0.0133(11) -0.0025(10) -0.0034(10) -0.0139(11) F52 0.0231(12) 0.0312(13) 0.0178(11) -0.0018(9) -0.0052(9) -0.0110(10) F62 0.0267(13) 0.0194(12) 0.0333(14) -0.0071(10) 0.0026(11) -0.0013(10) Si3 0.0200(6) 0.0177(5) 0.0123(5) -0.0039(4) -0.0024(4) -0.0042(4) F13 0.0182(12) 0.0249(12) 0.0175(11) -0.0086(9) -0.0023(9) -0.0050(9) F23 0.0239(13) 0.0309(13) 0.0137(11) -0.0016(9) -0.0021(9) -0.0068(10) F33 0.0279(13) 0.0244(12) 0.0144(10) -0.0017(9) -0.0038(9) -0.0118(10) F43 0.0237(13) 0.0324(13) 0.0191(11) -0.0007(10) -0.0054(10) -0.0104(10) F53 0.0347(14) 0.0170(12) 0.0250(12) -0.0072(9) -0.0023(10) -0.0056(10) F63 0.0248(13) 0.0251(12) 0.0239(12) -0.0116(10) -0.0034(10) -0.0005(10) O1W 0.0236(15) 0.0200(14) 0.0197(14) 0.0000(11) -0.0032(12) -0.0053(12) O2W 0.0360(18) 0.0244(15) 0.0206(14) -0.0053(12) -0.0033(13) -0.0103(13) O3W 0.0253(16) 0.0297(16) 0.0269(15) -0.0135(13) -0.0030(13) -0.0019(13) O4W 0.0251(16) 0.0361(18) 0.0307(16) -0.0163(14) -0.0030(13) -0.0022(13) O5W 0.0228(16) 0.0384(18) 0.0302(16) -0.0155(13) -0.0031(13) -0.0046(13) O6W 0.0240(16) 0.0316(17) 0.0415(19) -0.0106(14) -0.0039(14) -0.0038(13) O7W 0.0325(18) 0.043(2) 0.0308(17) -0.0086(14) -0.0082(14) -0.0006(15) O8W 0.0350(18) 0.0303(16) 0.0194(14) -0.0129(12) 0.0016(13) -0.0101(14) C11 0.021(2) 0.0155(19) 0.0127(17) -0.0043(14) -0.0022(15) -0.0003(16) C12 0.0165(19) 0.0147(18) 0.0124(17) -0.0038(14) -0.0020(14) -0.0035(15) N11 0.0200(17) 0.0111(15) 0.0108(14) -0.0054(11) 0.0005(12) -0.0023(12) N12 0.0183(17) 0.0130(15) 0.0117(14) -0.0055(12) -0.0007(12) -0.0012(13) N13 0.0148(16) 0.0188(16) 0.0139(15) -0.0068(12) -0.0024(13) -0.0001(13) N14 0.0170(17) 0.0266(18) 0.0200(16) -0.0063(14) -0.0023(13) -0.0088(14) C21 0.020(2) 0.0161(18) 0.0109(16) -0.0035(14) -0.0017(15) -0.0029(15) C22 0.0137(19) 0.0153(18) 0.0130(17) -0.0035(14) -0.0045(14) 0.0019(15) N21 0.0174(17) 0.0171(16) 0.0104(14) -0.0060(12) 0.0005(12) -0.0013(13) N22 0.0150(16) 0.0108(14) 0.0100(14) -0.0051(11) 0.0001(12) -0.0006(12) N23 0.0187(17) 0.0145(15) 0.0133(15) -0.0037(12) -0.0046(13) -0.0019(13) N24 0.0260(19) 0.0147(16) 0.0179(16) 0.0010(13) 0.0040(14) -0.0153(14) C31 0.0171(19) 0.0128(18) 0.0161(18) -0.0038(14) -0.0045(15) -0.0001(15) C32 0.020(2) 0.0197(19) 0.0146(17) -0.0045(15) -0.0042(15) -0.0018(16) N31 0.0134(15) 0.0128(15) 0.0124(14) -0.0059(11) -0.0025(12) -0.0011(12) N32 0.0178(16) 0.0148(15) 0.0095(14) -0.0060(12) -0.0013(12) -0.0044(13) N33 0.0213(17) 0.0144(16) 0.0141(15) -0.0020(12) -0.0045(13) -0.0014(13) N34 0.036(2) 0.0119(16) 0.0213(17) 0.0045(13) -0.0118(15) -0.0029(14) C41 0.024(2) 0.0161(19) 0.0152(18) -0.0026(14) -0.0053(16) -0.0071(16) C42 0.016(2) 0.020(2) 0.0170(18) -0.0037(15) -0.0015(15) -0.0014(16) N41 0.0191(17) 0.0146(15) 0.0127(14) -0.0071(12) -0.0015(13) -0.0023(13) N42 0.0166(16) 0.0170(16) 0.0100(14) -0.0049(12) -0.0005(12) -0.0006(13) N43 0.0209(18) 0.0193(17) 0.0171(16) 0.0010(13) -0.0050(13) -0.0076(14) N44 0.034(2) 0.029(2) 0.040(2) 0.0171(16) -0.0186(18) -0.0264(17) C51 0.0160(19) 0.0201(19) 0.0145(17) -0.0065(15) -0.0024(15) -0.0011(16) C52 0.018(2) 0.0180(19) 0.0137(17) -0.0062(14) -0.0039(15) -0.0005(15) N51 0.0149(16) 0.0127(15) 0.0124(14) -0.0058(12) -0.0022(12) -0.0022(12) N52 0.0135(15) 0.0151(15) 0.0127(14) -0.0073(12) -0.0032(12) 0.0038(12) N53 0.0183(17) 0.0140(15) 0.0121(14) -0.0019(12) -0.0040(12) -0.0006(13) N54 0.030(2) 0.0170(17) 0.0193(17) 0.0018(13) -0.0082(15) -0.0007(14) C61 0.0176(19) 0.0113(17) 0.0118(16) -0.0027(13) -0.0024(14) -0.0032(15) C62 0.0162(19) 0.0163(18) 0.0115(16) -0.0085(14) -0.0010(14) 0.0018(15) N61 0.0188(17) 0.0116(15) 0.0099(14) -0.0030(11) 0.0010(12) -0.0024(13) N62 0.0168(16) 0.0095(14) 0.0110(14) -0.0046(11) -0.0003(12) -0.0030(12) N63 0.0164(16) 0.0172(16) 0.0126(14) -0.0045(12) -0.0059(13) -0.0009(13) N64 0.0141(16) 0.0200(17) 0.0205(16) -0.0050(13) -0.0076(13) -0.0031(13) C71 0.0173(19) 0.0138(18) 0.0142(17) -0.0030(14) -0.0033(15) -0.0023(15) C72 0.017(2) 0.018(2) 0.0149(18) -0.0061(15) -0.0014(15) 0.0028(16) N71 0.0186(16) 0.0125(15) 0.0101(14) -0.0053(11) -0.0042(12) 0.0011(12) N72 0.0177(16) 0.0144(15) 0.0111(14) -0.0065(12) -0.0034(12) -0.0006(13) N73 0.0182(17) 0.0116(15) 0.0118(14) -0.0020(11) -0.0044(13) -0.0005(13) N74 0.0250(18) 0.0126(15) 0.0149(15) -0.0002(12) -0.0059(14) 0.0026(13) C81 0.0146(19) 0.0119(17) 0.0141(17) -0.0044(13) -0.0027(14) -0.0020(14) C82 0.0137(18) 0.0123(17) 0.0123(17) -0.0033(13) -0.0022(14) -0.0007(14) N81 0.0190(17) 0.0112(15) 0.0117(14) -0.0077(11) -0.0009(12) -0.0001(12) N82 0.0151(16) 0.0117(15) 0.0106(14) -0.0058(11) 0.0019(12) 0.0016(12) N83 0.0153(16) 0.0153(15) 0.0114(14) -0.0037(12) -0.0029(12) 0.0012(13) N84 0.0117(16) 0.0202(16) 0.0187(16) -0.0062(13) -0.0059(13) 0.0005(13) C91 0.019(2) 0.0180(19) 0.0159(18) -0.0069(15) -0.0010(15) -0.0022(16) C92 0.018(2) 0.0161(19) 0.0163(18) -0.0068(15) -0.0027(15) 0.0000(15) N91 0.0183(17) 0.0154(15) 0.0118(14) -0.0079(12) 0.0007(12) -0.0025(13) N92 0.0178(16) 0.0115(15) 0.0098(14) -0.0057(11) -0.0007(12) -0.0027(12) N93 0.0214(18) 0.0157(16) 0.0169(16) -0.0053(12) -0.0031(13) -0.0048(13) N94 0.0222(18) 0.0181(17) 0.0263(18) -0.0014(14) 0.0017(14) -0.0149(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N31 2.007(3) . ? Cu1 N31 2.007(3) 2_755 ? Cu1 N11 2.065(3) . ? Cu1 N11 2.065(3) 2_755 ? Cu1 N21 2.329(3) . ? Cu1 N21 2.329(3) 2_755 ? Cu2 N22 1.986(3) . ? Cu2 N41 1.992(3) . ? Cu2 N61 2.051(3) . ? Cu2 N12 2.070(3) . ? Cu2 N51 2.317(3) . ? Cu2 N32 2.381(3) . ? Cu3 N71 2.030(3) . ? Cu3 N81 2.032(3) . ? Cu3 N62 2.039(3) . ? Cu3 N52 2.048(3) . ? Cu3 N91 2.335(3) . ? Cu3 N42 2.353(3) . ? Cu4 N92 2.019(3) . ? Cu4 N92 2.019(3) 2_666 ? Cu4 N82 2.081(3) 2_666 ? Cu4 N82 2.081(3) . ? Cu4 N72 2.315(3) 2_666 ? Cu4 N72 2.315(3) . ? Si1 F11 1.661(3) . ? Si1 F41 1.670(3) . ? Si1 F21 1.671(3) . ? Si1 F51 1.671(3) . ? Si1 F61 1.683(3) . ? Si1 F31 1.714(3) . ? Si2 F42 1.675(2) . ? Si2 F32 1.677(2) . ? Si2 F22 1.677(2) . ? Si2 F62 1.687(2) . ? Si2 F12 1.690(2) . ? Si2 F52 1.711(2) . ? Si3 F23 1.669(2) . ? Si3 F33 1.673(2) . ? Si3 F53 1.689(2) . ? Si3 F63 1.690(2) . ? Si3 F13 1.694(2) . ? Si3 F43 1.714(2) . ? C11 N11 1.307(5) . ? C11 N13 1.353(4) . ? C12 N12 1.305(5) . ? C12 N13 1.352(4) . ? N11 N12 1.379(4) . ? N13 N14 1.403(4) . ? C21 N21 1.313(5) . ? C21 N23 1.342(5) . ? C22 N22 1.318(5) . ? C22 N23 1.335(4) . ? N21 N22 1.384(4) . ? N23 N24 1.407(4) . ? C31 N31 1.303(4) . ? C31 N33 1.348(4) . ? C32 N32 1.312(4) . ? C32 N33 1.349(5) . ? N31 N32 1.387(4) . ? N33 N34 1.419(4) . ? C41 N41 1.307(5) . ? C41 N43 1.328(5) . ? C42 N42 1.309(5) . ? C42 N43 1.349(5) . ? N41 N42 1.378(4) . ? N43 N44 1.411(4) . ? C51 N51 1.305(4) . ? C51 N53 1.343(4) . ? C52 N52 1.308(4) . ? C52 N53 1.361(4) . ? N51 N52 1.383(4) . ? N53 N54 1.418(4) . ? C61 N61 1.309(5) . ? C61 N63 1.342(4) . ? C62 N62 1.308(5) . ? C62 N63 1.351(4) . ? N61 N62 1.386(4) . ? N63 N64 1.412(4) . ? C71 N71 1.314(4) . ? C71 N73 1.348(4) . ? C72 N72 1.305(4) . ? C72 N73 1.340(4) . ? N71 N72 1.378(4) . ? N73 N74 1.415(4) . ? C81 N81 1.303(5) . ? C81 N83 1.344(4) . ? C82 N82 1.296(5) . ? C82 N83 1.360(4) . ? N81 N82 1.390(4) . ? N83 N84 1.404(4) . ? C91 N91 1.311(5) . ? C91 N93 1.345(5) . ? C92 N92 1.323(5) . ? C92 N93 1.329(5) . ? N91 N92 1.378(4) . ? N93 N94 1.417(4) . ? 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 N31 Cu1 N31 180.0 . 2_755 ? N31 Cu1 N11 90.56(12) . . ? N31 Cu1 N11 89.44(12) 2_755 . ? N31 Cu1 N11 89.44(12) . 2_755 ? N31 Cu1 N11 90.56(12) 2_755 2_755 ? N11 Cu1 N11 180.0 . 2_755 ? N31 Cu1 N21 90.94(11) . . ? N31 Cu1 N21 89.06(11) 2_755 . ? N11 Cu1 N21 88.76(11) . . ? N11 Cu1 N21 91.24(11) 2_755 . ? N31 Cu1 N21 89.06(11) . 2_755 ? N31 Cu1 N21 90.94(11) 2_755 2_755 ? N11 Cu1 N21 91.24(11) . 2_755 ? N11 Cu1 N21 88.76(11) 2_755 2_755 ? N21 Cu1 N21 180.0 . 2_755 ? N22 Cu2 N41 179.38(11) . . ? N22 Cu2 N61 88.90(12) . . ? N41 Cu2 N61 90.52(12) . . ? N22 Cu2 N12 91.87(12) . . ? N41 Cu2 N12 88.71(12) . . ? N61 Cu2 N12 178.73(11) . . ? N22 Cu2 N51 90.07(11) . . ? N41 Cu2 N51 90.11(11) . . ? N61 Cu2 N51 86.80(11) . . ? N12 Cu2 N51 94.21(11) . . ? N22 Cu2 N32 89.35(11) . . ? N41 Cu2 N32 90.44(11) . . ? N61 Cu2 N32 90.70(11) . . ? N12 Cu2 N32 88.29(11) . . ? N51 Cu2 N32 177.45(10) . . ? N71 Cu3 N81 91.19(12) . . ? N71 Cu3 N62 88.10(12) . . ? N81 Cu3 N62 178.37(11) . . ? N71 Cu3 N52 179.35(10) . . ? N81 Cu3 N52 89.32(12) . . ? N62 Cu3 N52 91.37(12) . . ? N71 Cu3 N91 88.04(11) . . ? N81 Cu3 N91 86.23(12) . . ? N62 Cu3 N91 95.21(11) . . ? N52 Cu3 N91 92.40(11) . . ? N71 Cu3 N42 89.61(11) . . ? N81 Cu3 N42 92.55(11) . . ? N62 Cu3 N42 85.98(11) . . ? N52 Cu3 N42 89.97(11) . . ? N91 Cu3 N42 177.32(9) . . ? N92 Cu4 N92 180.0 . 2_666 ? N92 Cu4 N82 90.28(12) . 2_666 ? N92 Cu4 N82 89.72(12) 2_666 2_666 ? N92 Cu4 N82 89.72(12) . . ? N92 Cu4 N82 90.28(12) 2_666 . ? N82 Cu4 N82 180.0 2_666 . ? N92 Cu4 N72 90.25(11) . 2_666 ? N92 Cu4 N72 89.75(11) 2_666 2_666 ? N82 Cu4 N72 87.17(11) 2_666 2_666 ? N82 Cu4 N72 92.83(11) . 2_666 ? N92 Cu4 N72 89.75(11) . . ? N92 Cu4 N72 90.25(11) 2_666 . ? N82 Cu4 N72 92.83(11) 2_666 . ? N82 Cu4 N72 87.17(11) . . ? N72 Cu4 N72 180.0 2_666 . ? F11 Si1 F41 91.26(14) . . ? F11 Si1 F21 91.73(14) . . ? F41 Si1 F21 89.28(14) . . ? F11 Si1 F51 91.24(14) . . ? F41 Si1 F51 177.50(14) . . ? F21 Si1 F51 90.58(14) . . ? F11 Si1 F61 90.42(14) . . ? F41 Si1 F61 89.48(13) . . ? F21 Si1 F61 177.54(15) . . ? F51 Si1 F61 90.56(14) . . ? F11 Si1 F31 178.90(15) . . ? F41 Si1 F31 89.75(14) . . ? F21 Si1 F31 88.74(14) . . ? F51 Si1 F31 87.76(13) . . ? F61 Si1 F31 89.13(13) . . ? F42 Si2 F32 178.71(13) . . ? F42 Si2 F22 90.88(13) . . ? F32 Si2 F22 90.30(12) . . ? F42 Si2 F62 89.76(12) . . ? F32 Si2 F62 89.06(12) . . ? F22 Si2 F62 179.05(14) . . ? F42 Si2 F12 90.09(12) . . ? F32 Si2 F12 90.41(12) . . ? F22 Si2 F12 91.17(13) . . ? F62 Si2 F12 89.53(12) . . ? F42 Si2 F52 90.35(12) . . ? F32 Si2 F52 89.12(12) . . ? F22 Si2 F52 90.07(13) . . ? F62 Si2 F52 89.22(13) . . ? F12 Si2 F52 178.67(13) . . ? F23 Si3 F33 179.22(13) . . ? F23 Si3 F53 90.72(12) . . ? F33 Si3 F53 89.62(12) . . ? F23 Si3 F63 89.83(12) . . ? F33 Si3 F63 89.83(12) . . ? F53 Si3 F63 179.45(12) . . ? F23 Si3 F13 90.14(12) . . ? F33 Si3 F13 90.56(12) . . ? F53 Si3 F13 89.99(12) . . ? F63 Si3 F13 90.06(12) . . ? F23 Si3 F43 90.72(12) . . ? F33 Si3 F43 88.58(12) . . ? F53 Si3 F43 89.88(12) . . ? F63 Si3 F43 90.07(12) . . ? F13 Si3 F43 179.13(12) . . ? N11 C11 N13 109.6(3) . . ? N12 C12 N13 109.3(3) . . ? C11 N11 N12 107.1(3) . . ? C11 N11 Cu1 126.6(2) . . ? N12 N11 Cu1 126.0(2) . . ? C12 N12 N11 107.8(3) . . ? C12 N12 Cu2 125.0(2) . . ? N11 N12 Cu2 126.4(2) . . ? C12 N13 C11 106.2(3) . . ? C12 N13 N14 123.7(3) . . ? C11 N13 N14 130.0(3) . . ? N21 C21 N23 110.1(3) . . ? N22 C22 N23 108.9(3) . . ? C21 N21 N22 106.1(3) . . ? C21 N21 Cu1 128.5(2) . . ? N22 N21 Cu1 125.2(2) . . ? C22 N22 N21 107.9(3) . . ? C22 N22 Cu2 127.8(2) . . ? N21 N22 Cu2 124.3(2) . . ? C22 N23 C21 107.0(3) . . ? C22 N23 N24 128.2(3) . . ? C21 N23 N24 124.8(3) . . ? N31 C31 N33 108.9(3) . . ? N32 C32 N33 109.6(3) . . ? C31 N31 N32 108.3(3) . . ? C31 N31 Cu1 127.5(2) . . ? N32 N31 Cu1 124.1(2) . . ? C32 N32 N31 106.3(3) . . ? C32 N32 Cu2 129.8(2) . . ? N31 N32 Cu2 123.9(2) . . ? C31 N33 C32 106.8(3) . . ? C31 N33 N34 128.3(3) . . ? C32 N33 N34 124.8(3) . . ? N41 C41 N43 108.8(3) . . ? N42 C42 N43 109.9(3) . . ? C41 N41 N42 108.6(3) . . ? C41 N41 Cu2 128.0(2) . . ? N42 N41 Cu2 123.4(2) . . ? C42 N42 N41 105.7(3) . . ? C42 N42 Cu3 127.5(2) . . ? N41 N42 Cu3 126.7(2) . . ? C41 N43 C42 106.9(3) . . ? C41 N43 N44 123.5(3) . . ? C42 N43 N44 129.7(3) . . ? N51 C51 N53 110.5(3) . . ? N52 C52 N53 109.3(3) . . ? C51 N51 N52 106.9(3) . . ? C51 N51 Cu2 124.0(2) . . ? N52 N51 Cu2 129.0(2) . . ? C52 N52 N51 107.6(3) . . ? C52 N52 Cu3 131.8(2) . . ? N51 N52 Cu3 120.6(2) . . ? C51 N53 C52 105.8(3) . . ? C51 N53 N54 123.0(3) . . ? C52 N53 N54 131.2(3) . . ? N61 C61 N63 109.5(3) . . ? N62 C62 N63 109.0(3) . . ? C61 N61 N62 107.1(3) . . ? C61 N61 Cu2 125.3(2) . . ? N62 N61 Cu2 127.4(2) . . ? C62 N62 N61 107.5(3) . . ? C62 N62 Cu3 124.7(2) . . ? N61 N62 Cu3 127.5(2) . . ? C61 N63 C62 106.9(3) . . ? C61 N63 N64 124.6(3) . . ? C62 N63 N64 128.4(3) . . ? N71 C71 N73 108.3(3) . . ? N72 C72 N73 109.7(3) . . ? C71 N71 N72 108.0(3) . . ? C71 N71 Cu3 128.0(2) . . ? N72 N71 Cu3 124.0(2) . . ? C72 N72 N71 106.9(3) . . ? C72 N72 Cu4 126.3(2) . . ? N71 N72 Cu4 126.7(2) . . ? C72 N73 C71 107.1(3) . . ? C72 N73 N74 128.6(3) . . ? C71 N73 N74 124.2(3) . . ? N81 C81 N83 110.3(3) . . ? N82 C82 N83 109.7(3) . . ? C81 N81 N82 106.8(3) . . ? C81 N81 Cu3 123.8(2) . . ? N82 N81 Cu3 129.2(2) . . ? C82 N82 N81 107.5(3) . . ? C82 N82 Cu4 126.4(2) . . ? N81 N82 Cu4 125.5(2) . . ? C81 N83 C82 105.7(3) . . ? C81 N83 N84 128.5(3) . . ? C82 N83 N84 125.6(3) . . ? N91 C91 N93 109.6(3) . . ? N92 C92 N93 108.7(3) . . ? C91 N91 N92 106.6(3) . . ? C91 N91 Cu3 126.8(2) . . ? N92 N91 Cu3 126.6(2) . . ? C92 N92 N91 107.8(3) . . ? C92 N92 Cu4 128.3(2) . . ? N91 N92 Cu4 124.0(2) . . ? C92 N93 C91 107.4(3) . . ? C92 N93 N94 127.2(3) . . ? C91 N93 N94 125.3(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cu1 N11 N12 Cu2 -17.5(4) . . . . ? Cu1 N21 N22 Cu2 -1.7(4) . . . . ? Cu1 N31 N32 Cu2 4.1(4) . . . . ? Cu2 N41 N42 Cu3 -1.4(4) . . . . ? Cu2 N51 N52 Cu3 -1.9(4) . . . . ? Cu2 N61 N62 Cu3 11.1(4) . . . . ? Cu3 N71 N72 Cu4 -6.1(4) . . . . ? Cu3 N81 N82 Cu4 -14.5(4) . . . . ? Cu3 N91 N92 Cu4 -0.3(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1W1 N74 1.04 1.95 2.975(4) 168.9 2_856 O1W H2W1 F52 0.97 1.82 2.781(4) 174.2 . O2W H1W2 F61 0.92 1.80 2.717(4) 174.0 2_855 O2W H2W2 F43 1.05 1.69 2.738(4) 171.2 . O3W H1W3 O6W 0.95 1.95 2.822(4) 152.0 1_565 O3W H2W3 F43 1.09 2.08 2.955(4) 135.3 . O4W H1W4 O5W 1.01 1.75 2.726(4) 162.6 1_645 O4W H2W4 F52 1.07 2.01 2.976(4) 148.3 . O5W H1W5 N84 0.97 2.05 2.911(4) 146.3 2_666 O5W H2W5 F62 0.99 1.86 2.677(4) 137.0 2_856 O6W H1W6 N64 0.97 2.00 2.939(4) 162.1 2_855 O7W H1W7 F31 1.07 1.72 2.732(4) 155.6 2_855 O8W H1W8 N94 1.05 1.89 2.917(5) 166.8 2_666 O8W H2W8 F51 0.87 2.35 3.020(4) 133.8 2_756 N14 H13N F31 0.97 2.25 3.154(4) 154.7 2_755 N14 H13N F51 0.97 2.41 3.237(4) 142.6 2_755 N14 H13N F61 0.97 2.32 3.050(4) 131.6 2_755 N24 H23N F13 0.96 2.01 2.934(4) 161.8 1_455 N24 H24N F23 0.96 2.17 3.049(4) 151.1 2_865 N24 H24N F63 0.96 2.35 3.182(4) 145.3 2_865 N34 H33N F53 0.95 2.21 2.994(4) 140.2 2_855 N34 H34N F11 0.98 2.38 3.105(4) 131.1 . N34 H34N F41 0.98 2.31 3.256(4) 162.1 . N44 H43N F12 0.95 2.00 2.879(4) 152.3 1_455 N44 H44N O6W 0.97 2.27 3.091(5) 141.9 2_755 N54 H53N F51 0.95 2.31 3.032(4) 132.3 1_465 N54 H54N O2W 0.96 2.04 2.990(5) 173.4 2_765 N64 H63N F33 0.96 2.04 2.851(4) 141.2 2_865 N64 H64N F32 0.96 2.41 2.735(4) 99.5 2_856 N64 H64N F52 0.96 1.99 2.924(4) 162.9 2_856 N74 H73N F41 0.96 1.94 2.885(4) 166.7 2_756 N74 H74N F22 0.96 2.20 2.967(4) 136.4 1_455 N84 H83N F32 1.00 2.21 3.054(4) 142.0 2_756 N84 H83N F62 1.00 2.19 2.914(4) 128.6 2_756 N84 H84N F43 0.95 2.02 2.934(4) 159.8 2_765 N94 H93N F53 0.96 2.39 3.065(4) 127.5 2_865 N94 H94N F42 0.96 1.97 2.891(4) 160.5 1_465 _diffrn_measured_fraction_theta_max 0.930 _diffrn_reflns_theta_full 27.99 _diffrn_measured_fraction_theta_full 0.930 _refine_diff_density_max 1.591 _refine_diff_density_min -1.110 _refine_diff_density_rms 0.145 #===END