# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_(1) _audit_creation_method SHELXL-97 _chemical_name_systematic ; \m-Hexafluorosilicato-tetrakis[\m-1,3-bis(pyridazin-4-yl)benzene- \k^2^N^2^:N^2'^]-dimethanol-dicopper(II) hexafluorosilicate, solvate with 3 methanol ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C58 H48 Cu2 F6 N16 O2 Si, F6 Si, 3(C H4 O)' _chemical_formula_sum 'C61 H60 Cu2 F12 N16 O5 Si2' _chemical_formula_weight 1508.51 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 tetragonal _symmetry_space_group_name_H-M 'I 4/m' _space_group_name_Hall '-I 4' _symmetry_Int_Tables_number 87 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 17.1490(3) _cell_length_b 17.1490(3) _cell_length_c 20.7268(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6095.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 21088 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 29.11 _exptl_crystal_description prism _exptl_crystal_colour blue-green _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.14 _exptl_crystal_density_diffrn 1.644 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3088 _exptl_absorpt_coefficient_mu 0.841 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8048 _exptl_absorpt_correction_T_max 0.8914 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker APEXII area-detector diffractometer' _diffrn_measurement_method '\w scans' _diffrn_standards_decay_% 0 _diffrn_reflns_number 21088 _diffrn_reflns_av_R_equivalents 0.0480 _diffrn_reflns_av_sigmaI/netI 0.0438 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 29.11 _reflns_number_total 4216 _reflns_number_gt 3037 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT (Bruker, 1998)' _computing_cell_refinement 'SAINT-NT (Bruker, 1999)' _computing_data_reduction 'SAINT-NT (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Diamond 2.1e (Brandenburg, 1999)' _computing_publication_material 'WinGX 1.70.01 (Farrugia, 1999)' #------------------------------- Refinement data-----------------------# _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. Cu1 atom lies on a mirror plane and the Si1 and Si2 atoms are at sites with crystallographically-imposed 2/m and 4-fold symmetry, respectively. In the framework of complex cation, [{SiF6}Cu2(L)4(CH3OH)2]2+, the methanol ligands are equally disordered by symmetry, in such a way that the C-atom is common for two components and two components of the disordered O-atom appear to be separated by ca. 1.25 A. The refined C-O distances were reasonable although certainly shortened due to the disorder (1.28 A) and therefore no geometry restraints were applied. All atoms of cationic residue, including methanol ligand, were refined anisotropically. The OH-hydrogen was located and then fixed at d(O-H) = 0.85 A and with Uiso = 1.5Ueq(O). The aromatic CH-atoms were added geometrically [Uiso = 1.2Ueq(C)] and two sets of the methyl CH-atoms were added [Uiso = 1.5Ueq(C)] with partial contributions of 0.5 and considering two orientations of methanol O-atoms. Three unique solvate methanol molecules reside across symmetry elements and are disordered by symmetry over multiple positions. It was impossible to resolve the disordering schemes and therefore the corresponding electron density (218 e/cell found, 216 e/cell calc.) was modelled using a Squeeze routine implemented in Platon. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0532P)^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 constr _refine_ls_extinction_method none _refine_ls_number_reflns 4216 _refine_ls_number_parameters 223 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0600 _refine_ls_R_factor_gt 0.0415 _refine_ls_wR_factor_ref 0.1048 _refine_ls_wR_factor_gt 0.0990 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.358273(18) 0.177570(18) 0.0000 0.03324(12) Uani 1 2 d S . . Si1 Si 0.5000 0.0000 0.0000 0.01518(18) Uani 1 4 d S . . Si2 Si 0.0000 0.0000 0.24622(4) 0.01720(19) Uani 1 4 d S . . F1 F 0.43793(8) 0.07560(8) 0.0000 0.0231(3) Uani 1 2 d S . . F2 F 0.42450(8) -0.06179(8) 0.0000 0.0216(3) Uani 1 2 d S . . F3 F 0.5000 0.0000 0.08117(7) 0.0225(3) Uani 1 2 d S . . F4 F 0.0000 0.0000 0.16523(10) 0.0345(5) Uani 1 4 d S . . F5 F 0.06273(6) 0.07600(6) 0.24679(5) 0.0258(2) Uani 1 1 d . . . F6 F 0.0000 0.0000 0.32813(9) 0.0217(4) Uani 1 4 d S . . N1 N 0.29371(9) 0.11646(10) 0.06901(10) 0.0375(4) Uani 1 1 d . . . N2 N 0.22143(10) 0.14317(12) 0.07980(11) 0.0501(5) Uani 1 1 d . . . N3 N 0.56728(10) -0.22375(9) 0.06874(9) 0.0359(4) Uani 1 1 d . . . N4 N 0.57687(12) -0.30072(10) 0.07799(11) 0.0492(5) Uani 1 1 d . . . C1 C 0.31777(12) 0.05108(12) 0.09759(10) 0.0357(5) Uani 1 1 d . . . H1 H 0.3699 0.0346 0.0901 0.043 Uiso 1 1 calc R . . C2 C 0.27122(12) 0.00532(14) 0.13788(10) 0.0374(5) Uani 1 1 d . . . C3 C 0.19666(13) 0.03268(16) 0.14830(12) 0.0491(6) Uani 1 1 d . . . H3 H 0.1610 0.0052 0.1750 0.059 Uiso 1 1 calc R . . C4 C 0.17575(13) 0.10166(18) 0.11837(14) 0.0560(8) Uani 1 1 d . . . H4 H 0.1246 0.1208 0.1261 0.067 Uiso 1 1 calc R . . C5 C 0.51018(12) -0.18582(12) 0.09802(11) 0.0345(5) Uani 1 1 d . . . H5 H 0.5063 -0.1312 0.0911 0.041 Uiso 1 1 calc R . . C6 C 0.45495(13) -0.22123(13) 0.13868(10) 0.0378(5) Uani 1 1 d . . . C7 C 0.46594(17) -0.30011(14) 0.14745(12) 0.0531(7) Uani 1 1 d . . . H7 H 0.4316 -0.3292 0.1742 0.064 Uiso 1 1 calc R . . C8 C 0.52739(19) -0.33604(14) 0.11690(14) 0.0589(8) Uani 1 1 d . . . H8 H 0.5347 -0.3902 0.1244 0.071 Uiso 1 1 calc R . . C9 C 0.30130(12) -0.06716(14) 0.16808(10) 0.0395(5) Uani 1 1 d . . . C10 C 0.36185(12) -0.10872(13) 0.14011(10) 0.0345(5) Uani 1 1 d . . . H10 H 0.3837 -0.0908 0.1007 0.041 Uiso 1 1 calc R . . C11 C 0.39149(13) -0.17658(14) 0.16873(10) 0.0407(5) Uani 1 1 d . . . C12 C 0.35812(16) -0.20139(18) 0.22693(12) 0.0579(8) Uani 1 1 d . . . H12 H 0.3775 -0.2471 0.2472 0.069 Uiso 1 1 calc R . . C13 C 0.29788(18) -0.1610(2) 0.25529(12) 0.0646(9) Uani 1 1 d . . . H13 H 0.2760 -0.1789 0.2947 0.078 Uiso 1 1 calc R . . C14 C 0.26930(15) -0.09441(18) 0.22639(11) 0.0566(8) Uani 1 1 d . . . H14 H 0.2276 -0.0667 0.2460 0.068 Uiso 1 1 calc R . . O1 O 0.27551(18) 0.27355(17) -0.03015(15) 0.0428(7) Uani 0.50 1 d P . . H1O H 0.2372 0.2491 -0.0464 0.051 Uiso 0.50 1 d PR . . C15 C 0.2430(2) 0.3302(2) 0.0000 0.0691(12) Uani 1 2 d S . . H15A H 0.2106 0.3590 -0.0292 0.104 Uiso 0.50 1 d PR . . H15B H 0.2118 0.3104 0.0348 0.104 Uiso 0.50 1 d PR . . H15C H 0.2828 0.3638 0.0170 0.104 Uiso 0.50 1 d PR . . 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 0.01976(18) 0.01757(18) 0.0624(3) 0.000 0.000 0.00259(12) Si1 0.0138(4) 0.0140(4) 0.0177(4) 0.000 0.000 -0.0010(3) Si2 0.0176(3) 0.0176(3) 0.0163(4) 0.000 0.000 0.000 F1 0.0208(7) 0.0176(7) 0.0308(8) 0.000 0.000 0.0031(5) F2 0.0196(7) 0.0201(7) 0.0251(7) 0.000 0.000 -0.0061(5) F3 0.0239(7) 0.0248(7) 0.0188(7) 0.000 0.000 -0.0048(6) F4 0.0433(8) 0.0433(8) 0.0167(10) 0.000 0.000 0.000 F5 0.0246(6) 0.0219(5) 0.0309(6) 0.0042(4) 0.0015(4) -0.0049(4) F6 0.0230(6) 0.0230(6) 0.0189(9) 0.000 0.000 0.000 N1 0.0195(8) 0.0328(9) 0.0602(12) -0.0191(9) 0.0084(8) -0.0011(7) N2 0.0230(9) 0.0544(13) 0.0730(14) -0.0250(11) 0.0079(9) 0.0065(8) N3 0.0310(9) 0.0202(8) 0.0565(11) 0.0108(8) -0.0127(8) -0.0024(7) N4 0.0598(13) 0.0213(9) 0.0664(13) 0.0144(9) -0.0162(11) 0.0008(8) C1 0.0237(10) 0.0353(11) 0.0482(12) -0.0150(10) 0.0117(9) -0.0041(8) C2 0.0275(10) 0.0512(14) 0.0335(10) -0.0183(10) 0.0095(8) -0.0124(9) C3 0.0274(11) 0.0698(17) 0.0503(14) -0.0229(13) 0.0149(11) -0.0132(11) C4 0.0208(11) 0.080(2) 0.0672(17) -0.0281(15) 0.0134(11) 0.0006(11) C5 0.0301(11) 0.0247(10) 0.0487(12) 0.0172(9) -0.0103(9) -0.0041(8) C6 0.0386(12) 0.0392(12) 0.0355(10) 0.0170(9) -0.0121(9) -0.0148(9) C7 0.0729(18) 0.0368(13) 0.0498(14) 0.0216(11) -0.0098(13) -0.0239(13) C8 0.087(2) 0.0263(12) 0.0631(17) 0.0189(12) -0.0129(16) -0.0099(13) C9 0.0324(11) 0.0565(14) 0.0295(10) -0.0062(10) 0.0076(9) -0.0194(10) C10 0.0312(11) 0.0448(12) 0.0276(9) 0.0059(9) 0.0048(8) -0.0145(9) C11 0.0407(12) 0.0491(13) 0.0324(11) 0.0127(10) -0.0041(9) -0.0217(10) C12 0.0573(16) 0.081(2) 0.0353(12) 0.0247(13) -0.0033(12) -0.0329(15) C13 0.0620(18) 0.101(2) 0.0305(12) 0.0127(14) 0.0088(12) -0.0399(17) C14 0.0461(14) 0.090(2) 0.0335(11) -0.0130(14) 0.0171(11) -0.0306(14) O1 0.0435(17) 0.0353(16) 0.0497(16) -0.0045(13) -0.0023(14) 0.0180(13) C15 0.060(3) 0.047(2) 0.101(3) 0.000 0.000 0.0303(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 N3 2.0705(19) 2_655 ? Cu1 N3 2.0705(19) 9_655 ? Cu1 N1 2.0905(19) 10 ? Cu1 N1 2.0905(19) . ? Cu1 F1 2.2191(14) . ? Cu1 O1 2.261(3) . ? Cu1 O1 2.261(3) 10 ? Si1 F2 1.6731(13) 9_655 ? Si1 F2 1.6731(13) . ? Si1 F1 1.6774(13) . ? Si1 F1 1.6774(13) 9_655 ? Si1 F3 1.6823(14) . ? Si1 F3 1.6823(14) 9_655 ? Si2 F4 1.679(2) . ? Si2 F5 1.6900(10) . ? Si2 F5 1.6900(10) 2 ? Si2 F5 1.6900(10) 4 ? Si2 F5 1.6900(10) 3 ? Si2 F6 1.698(2) . ? N1 C1 1.333(3) . ? N1 N2 1.340(2) . ? N2 C4 1.326(3) . ? N3 C5 1.323(3) . ? N3 N4 1.344(2) . ? N3 Cu1 2.0705(19) 9_655 ? N4 C8 1.318(3) . ? C1 C2 1.397(3) . ? C1 H1 0.9500 . ? C2 C3 1.379(3) . ? C2 C9 1.484(3) . ? C3 C4 1.383(4) . ? C3 H3 0.9500 . ? C4 H4 0.9500 . ? C5 C6 1.406(3) . ? C5 H5 0.9500 . ? C6 C7 1.378(3) . ? C6 C11 1.469(3) . ? C7 C8 1.375(4) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C10 1.387(3) . ? C9 C14 1.407(3) . ? C10 C11 1.402(3) . ? C10 H10 0.9500 . ? C11 C12 1.401(3) . ? C12 C13 1.376(5) . ? C12 H12 0.9500 . ? C13 C14 1.379(4) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? O1 O1 1.250(6) 10 ? O1 C15 1.282(4) . ? O1 H1O 0.8499 . ? C15 O1 1.282(4) 10 ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? 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 N3 Cu1 N3 86.96(10) 2_655 9_655 ? N3 Cu1 N1 171.55(7) 2_655 10 ? N3 Cu1 N1 92.72(7) 9_655 10 ? N3 Cu1 N1 92.72(7) 2_655 . ? N3 Cu1 N1 171.55(7) 9_655 . ? N1 Cu1 N1 86.35(10) 10 . ? N3 Cu1 F1 85.52(5) 2_655 . ? N3 Cu1 F1 85.52(5) 9_655 . ? N1 Cu1 F1 86.04(5) 10 . ? N1 Cu1 F1 86.04(5) . . ? N3 Cu1 O1 107.38(10) 2_655 . ? N3 Cu1 O1 85.32(9) 9_655 . ? N1 Cu1 O1 80.99(9) 10 . ? N1 Cu1 O1 102.80(9) . . ? F1 Cu1 O1 163.73(8) . . ? N3 Cu1 O1 85.32(9) 2_655 10 ? N3 Cu1 O1 107.38(10) 9_655 10 ? N1 Cu1 O1 102.80(9) 10 10 ? N1 Cu1 O1 80.99(9) . 10 ? F1 Cu1 O1 163.73(8) . 10 ? O1 Cu1 O1 32.08(15) . 10 ? F2 Si1 F2 180.0 9_655 . ? F2 Si1 F1 90.09(6) 9_655 . ? F2 Si1 F1 89.91(6) . . ? F2 Si1 F1 89.91(6) 9_655 9_655 ? F2 Si1 F1 90.09(6) . 9_655 ? F1 Si1 F1 180.0 . 9_655 ? F2 Si1 F3 90.0 9_655 . ? F2 Si1 F3 90.0 . . ? F1 Si1 F3 90.0 . . ? F1 Si1 F3 90.0 9_655 . ? F2 Si1 F3 90.0 9_655 9_655 ? F2 Si1 F3 90.0 . 9_655 ? F1 Si1 F3 90.0 . 9_655 ? F1 Si1 F3 90.0 9_655 9_655 ? F3 Si1 F3 180.0 . 9_655 ? F4 Si2 F5 90.40(4) . . ? F4 Si2 F5 90.40(4) . 2 ? F5 Si2 F5 179.21(9) . 2 ? F4 Si2 F5 90.40(4) . 4 ? F5 Si2 F5 90.0 . 4 ? F5 Si2 F5 90.0 2 4 ? F4 Si2 F5 90.40(4) . 3 ? F5 Si2 F5 90.0 . 3 ? F5 Si2 F5 90.0 2 3 ? F5 Si2 F5 179.21(9) 4 3 ? F4 Si2 F6 180.0 . . ? F5 Si2 F6 89.60(4) . . ? F5 Si2 F6 89.60(4) 2 . ? F5 Si2 F6 89.60(4) 4 . ? F5 Si2 F6 89.60(4) 3 . ? Si1 F1 Cu1 178.61(8) . . ? C1 N1 N2 119.96(19) . . ? C1 N1 Cu1 124.16(13) . . ? N2 N1 Cu1 115.63(16) . . ? C4 N2 N1 117.6(2) . . ? C5 N3 N4 120.54(19) . . ? C5 N3 Cu1 125.73(13) . 9_655 ? N4 N3 Cu1 113.48(16) . 9_655 ? C8 N4 N3 117.4(2) . . ? N1 C1 C2 124.1(2) . . ? N1 C1 H1 117.9 . . ? C2 C1 H1 117.9 . . ? C3 C2 C1 115.6(2) . . ? C3 C2 C9 122.8(2) . . ? C1 C2 C9 121.61(19) . . ? C2 C3 C4 117.5(2) . . ? C2 C3 H3 121.3 . . ? C4 C3 H3 121.3 . . ? N2 C4 C3 125.2(2) . . ? N2 C4 H4 117.4 . . ? C3 C4 H4 117.4 . . ? N3 C5 C6 124.14(19) . . ? N3 C5 H5 117.9 . . ? C6 C5 H5 117.9 . . ? C7 C6 C5 114.3(2) . . ? C7 C6 C11 123.9(2) . . ? C5 C6 C11 121.87(19) . . ? C8 C7 C6 118.9(2) . . ? C8 C7 H7 120.5 . . ? C6 C7 H7 120.5 . . ? N4 C8 C7 124.7(2) . . ? N4 C8 H8 117.7 . . ? C7 C8 H8 117.7 . . ? C10 C9 C14 118.7(2) . . ? C10 C9 C2 120.95(18) . . ? C14 C9 C2 120.3(2) . . ? C9 C10 C11 121.42(19) . . ? C9 C10 H10 119.3 . . ? C11 C10 H10 119.3 . . ? C12 C11 C10 117.9(2) . . ? C12 C11 C6 120.6(2) . . ? C10 C11 C6 121.45(19) . . ? C13 C12 C11 121.4(3) . . ? C13 C12 H12 119.3 . . ? C11 C12 H12 119.3 . . ? C12 C13 C14 119.9(2) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? C13 C14 C9 120.6(3) . . ? C13 C14 H14 119.7 . . ? C9 C14 H14 119.7 . . ? O1 O1 C15 60.84(15) 10 . ? O1 O1 Cu1 73.96(8) 10 . ? C15 O1 Cu1 133.6(2) . . ? O1 O1 H1O 113.4 10 . ? C15 O1 H1O 103.4 . . ? Cu1 O1 H1O 103.6 . . ? O1 C15 H15A 109.6 . . ? O1 C15 H15B 109.9 . . ? H15A C15 H15B 109.5 . . ? O1 C15 H15C 109.0 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? 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 N3 Cu1 N1 C1 -75.89(17) 2_655 . . . ? N1 Cu1 N1 C1 95.70(17) 10 . . . ? F1 Cu1 N1 C1 9.43(17) . . . . ? O1 Cu1 N1 C1 175.60(18) . . . . ? O1 Cu1 N1 C1 -160.71(19) 10 . . . ? N3 Cu1 N1 N2 109.74(15) 2_655 . . . ? N1 Cu1 N1 N2 -78.67(15) 10 . . . ? F1 Cu1 N1 N2 -164.94(15) . . . . ? O1 Cu1 N1 N2 1.23(17) . . . . ? O1 Cu1 N1 N2 24.92(16) 10 . . . ? C1 N1 N2 C4 -1.2(3) . . . . ? Cu1 N1 N2 C4 173.46(17) . . . . ? C5 N3 N4 C8 0.1(3) . . . . ? Cu1 N3 N4 C8 -174.38(19) 9_655 . . . ? N2 N1 C1 C2 2.0(3) . . . . ? Cu1 N1 C1 C2 -172.13(15) . . . . ? N1 C1 C2 C3 -1.3(3) . . . . ? N1 C1 C2 C9 179.71(19) . . . . ? C1 C2 C3 C4 -0.1(3) . . . . ? C9 C2 C3 C4 178.9(2) . . . . ? N1 N2 C4 C3 -0.2(4) . . . . ? C2 C3 C4 N2 0.8(4) . . . . ? N4 N3 C5 C6 -1.7(3) . . . . ? Cu1 N3 C5 C6 172.08(15) 9_655 . . . ? N3 C5 C6 C7 1.6(3) . . . . ? N3 C5 C6 C11 -178.45(19) . . . . ? C5 C6 C7 C8 -0.1(3) . . . . ? C11 C6 C7 C8 180.0(2) . . . . ? N3 N4 C8 C7 1.5(4) . . . . ? C6 C7 C8 N4 -1.5(4) . . . . ? C3 C2 C9 C10 155.6(2) . . . . ? C1 C2 C9 C10 -25.6(3) . . . . ? C3 C2 C9 C14 -25.3(3) . . . . ? C1 C2 C9 C14 153.6(2) . . . . ? C14 C9 C10 C11 -0.1(3) . . . . ? C2 C9 C10 C11 179.03(19) . . . . ? C9 C10 C11 C12 -0.2(3) . . . . ? C9 C10 C11 C6 179.16(19) . . . . ? C7 C6 C11 C12 26.5(3) . . . . ? C5 C6 C11 C12 -153.4(2) . . . . ? C7 C6 C11 C10 -152.8(2) . . . . ? C5 C6 C11 C10 27.3(3) . . . . ? C10 C11 C12 C13 0.3(4) . . . . ? C6 C11 C12 C13 -179.0(2) . . . . ? C11 C12 C13 C14 -0.2(4) . . . . ? C12 C13 C14 C9 -0.1(4) . . . . ? C10 C9 C14 C13 0.3(3) . . . . ? C2 C9 C14 C13 -178.9(2) . . . . ? N3 Cu1 O1 O1 -48.68(6) 2_655 . . 10 ? N3 Cu1 O1 O1 -134.01(5) 9_655 . . 10 ? N1 Cu1 O1 O1 132.47(5) 10 . . 10 ? N1 Cu1 O1 O1 48.33(5) . . . 10 ? F1 Cu1 O1 O1 170.0(3) . . . 10 ? N3 Cu1 O1 C15 -35.5(4) 2_655 . . . ? N3 Cu1 O1 C15 -120.8(4) 9_655 . . . ? N1 Cu1 O1 C15 145.7(4) 10 . . . ? N1 Cu1 O1 C15 61.5(4) . . . . ? F1 Cu1 O1 C15 -176.7(3) . . . . ? O1 Cu1 O1 C15 13.2(4) 10 . . . ? Cu1 O1 C15 O1 -14.6(5) . . . 10 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 29.11 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.376 _refine_diff_density_min -0.611 _refine_diff_density_rms 0.060 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 199 59 '3 CH3OH' 2 0.000 0.000 0.500 63 14 CH3OH 3 0.000 0.500 0.250 70 18 CH3OH 4 0.000 0.500 0.750 70 18 CH3OH 5 0.500 0.500 0.500 199 59 '3 CH3OH' 6 0.500 0.500 0.000 63 14 CH3OH 7 0.500 1.000 0.250 70 18 CH3OH 8 0.500 1.000 0.750 70 18 CH3OH _platon_squeeze_details ; ; _iucr_refine_instruction_details ; #--------------------------------------------------------- TITL DK6 in I4/m CELL 0.71073 17.1490 17.1490 20.7268 90.000 90.000 90.000 ZERR 4.00 0.0003 0.0003 0.0009 0.000 0.000 0.000 LATT 2 SYMM - X, - Y, Z SYMM - Y, X, Z SYMM Y, - X, Z SFAC C H N O F SI CU UNIT 244 240 64 20 48 8 8 MERG 2 OMIT -1.00 180.00 OMIT 0 0 6 OMIT 2 2 0 OMIT 0 2 2 SHEL 0.73 8 RTAB H..O H1 F3 RTAB H..O H5 F3 RTAB H..O H10 F2 RTAB O..O C1 F3 RTAB O..O C5 F3 RTAB O..O C10 F2 RTAB XHY C1 H1 F3 RTAB XHY C5 H5 F3 RTAB XHY C10 H10 F2 EQIV $1 Y, -X, Z EQIV $2 0.5-Y, -0.5+X, 0.5-Z EQIV $3 0.5-X, -0.5-Y, 0.5-Z RTAB XHY C3 H3 F5_$1 RTAB XHY C7 H7 F5_$2 RTAB XHY C8 H8 F6_$3 RTAB H..O H3 F5_$1 RTAB H..O H7 F5_$2 RTAB H..O H8 F6_$3 RTAB O..O C3 F5_$1 RTAB O..O C7 F5_$2 RTAB O..O C8 F6_$3 FMAP 2 PLAN 20 SIZE 0.14 0.23 0.27 ACTA BOND BOND $H CONF L.S. 4 TEMP -100.00 WGHT 0.053200 FVAR 1.48019 CU1 7 0.358273 0.177570 0.000000 10.50000 0.01976 0.01757 = 0.06239 0.00000 0.00000 0.00259 SI1 6 0.500000 0.000000 0.000000 10.25000 0.01381 0.01398 = 0.01774 0.00000 0.00000 -0.00100 SI2 6 0.000000 0.000000 0.246224 10.25000 0.01763 0.01763 = 0.01634 0.00000 0.00000 0.00000 F1 5 0.437934 0.075597 0.000000 10.50000 0.02075 0.01758 = 0.03083 0.00000 0.00000 0.00314 F2 5 0.424498 -0.061789 0.000000 10.50000 0.01958 0.02015 = 0.02507 0.00000 0.00000 -0.00615 F3 5 0.500000 0.000000 0.081166 10.50000 0.02389 0.02481 = 0.01878 0.00000 0.00000 -0.00480 F4 5 0.000000 0.000000 0.165225 10.25000 0.04333 0.04333 = 0.01669 0.00000 0.00000 0.00000 F5 5 0.062730 0.076004 0.246788 11.00000 0.02461 0.02193 = 0.03087 0.00419 0.00150 -0.00493 F6 5 0.000000 0.000000 0.328130 10.25000 0.02301 0.02301 = 0.01895 0.00000 0.00000 0.00000 N1 3 0.293712 0.116457 0.069011 11.00000 0.01947 0.03281 = 0.06015 -0.01911 0.00843 -0.00114 N2 3 0.221426 0.143168 0.079797 11.00000 0.02298 0.05436 = 0.07299 -0.02495 0.00788 0.00649 N3 3 0.567281 -0.223755 0.068736 11.00000 0.03101 0.02025 = 0.05648 0.01082 -0.01272 -0.00241 N4 3 0.576871 -0.300722 0.077985 11.00000 0.05976 0.02133 = 0.06643 0.01439 -0.01621 0.00076 C1 1 0.317775 0.051080 0.097589 11.00000 0.02371 0.03529 = 0.04822 -0.01503 0.01169 -0.00409 AFIX 43 H1 2 0.369874 0.034591 0.090068 11.00000 -1.20000 AFIX 0 C2 1 0.271222 0.005315 0.137878 11.00000 0.02746 0.05115 = 0.03345 -0.01826 0.00949 -0.01237 C3 1 0.196660 0.032681 0.148300 11.00000 0.02737 0.06975 = 0.05029 -0.02295 0.01492 -0.01322 AFIX 43 H3 2 0.161016 0.005195 0.175018 11.00000 -1.20000 AFIX 0 C4 1 0.175752 0.101663 0.118374 11.00000 0.02079 0.08008 = 0.06719 -0.02809 0.01337 0.00056 AFIX 43 H4 2 0.124618 0.120844 0.126056 11.00000 -1.20000 AFIX 0 C5 1 0.510177 -0.185815 0.098023 11.00000 0.03015 0.02470 = 0.04866 0.01720 -0.01032 -0.00405 AFIX 43 H5 2 0.506257 -0.131187 0.091142 11.00000 -1.20000 AFIX 0 C6 1 0.454946 -0.221235 0.138676 11.00000 0.03861 0.03923 = 0.03548 0.01703 -0.01207 -0.01480 C7 1 0.465941 -0.300114 0.147452 11.00000 0.07286 0.03678 = 0.04981 0.02157 -0.00984 -0.02390 AFIX 43 H7 2 0.431616 -0.329216 0.174181 11.00000 -1.20000 AFIX 0 C8 1 0.527391 -0.336041 0.116904 11.00000 0.08718 0.02632 = 0.06310 0.01889 -0.01293 -0.00993 AFIX 43 H8 2 0.534708 -0.390202 0.124387 11.00000 -1.20000 AFIX 0 C9 1 0.301297 -0.067165 0.168084 11.00000 0.03243 0.05654 = 0.02946 -0.00625 0.00759 -0.01940 C10 1 0.361855 -0.108719 0.140112 11.00000 0.03120 0.04481 = 0.02763 0.00593 0.00476 -0.01446 AFIX 43 H10 2 0.383735 -0.090806 0.100698 11.00000 -1.20000 AFIX 0 C11 1 0.391486 -0.176583 0.168732 11.00000 0.04072 0.04905 = 0.03241 0.01267 -0.00405 -0.02166 C12 1 0.358116 -0.201391 0.226926 11.00000 0.05731 0.08109 = 0.03531 0.02468 -0.00328 -0.03285 AFIX 43 H12 2 0.377509 -0.247107 0.247239 11.00000 -1.20000 AFIX 0 C13 1 0.297878 -0.160986 0.255289 11.00000 0.06201 0.10125 = 0.03049 0.01266 0.00880 -0.03994 AFIX 43 H13 2 0.276008 -0.178907 0.294703 11.00000 -1.20000 AFIX 0 C14 1 0.269300 -0.094406 0.226389 11.00000 0.04614 0.09008 = 0.03350 -0.01296 0.01712 -0.03058 AFIX 43 H14 2 0.227626 -0.066686 0.246034 11.00000 -1.20000 AFIX 0 O1 4 0.275508 0.273546 -0.030147 10.50000 0.04348 0.03529 = 0.04975 -0.00451 -0.00226 0.01800 AFIX 3 H1O 2 0.237178 0.249066 -0.046437 10.50000 -1.20000 AFIX 0 C15 1 0.243011 0.330174 0.000000 10.50000 0.06023 0.04652 = 0.10055 0.00000 0.00000 0.03027 AFIX 3 H15A 2 0.210551 0.359014 -0.029230 10.50000 -1.50000 H15B 2 0.211831 0.310364 0.034800 10.50000 -1.50000 H15C 2 0.282772 0.363824 0.016960 10.50000 -1.50000 HKLF 4 REM DK6 in I4/m REM R1 = 0.0415 for 3037 Fo > 4sig(Fo) and 0.0600 for all 4216 data REM 223 parameters refined using 0 restraints END WGHT 0.0532 0.0000 REM Highest difference peak 0.376, deepest hole -0.611, 1-sigma level 0.060 Q1 1 0.2026 0.3600 0.0000 10.50000 0.05 0.38 Q2 1 0.4545 -0.0297 0.0000 10.50000 0.05 0.36 Q3 1 0.3877 0.1988 0.0281 11.00000 0.05 0.35 Q4 1 0.3165 0.1575 0.0492 11.00000 0.05 0.31 Q5 1 0.3218 0.2166 0.0000 10.50000 0.05 0.28 Q6 1 0.2226 0.1597 0.0529 11.00000 0.05 0.28 Q7 1 0.0394 0.0395 0.2498 11.00000 0.05 0.27 Q8 1 0.4597 0.0407 0.0000 10.50000 0.05 0.27 ; _database_code_depnum_ccdc_archive 'CCDC 941550' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_(1a) _audit_creation_method SHELXL-97 _chemical_name_systematic ; \m-[Hexafluorosilicato/Hexafluorogermanate 0.93:0.07]- tetrakis[\m-1,3-bis(pyridazin-4-yl)benzene- \k^2^N^2^:N^2'^]-dimethanol-dicopper(II) Hexafluorosilicate/Hexafluorogermanate 0.67:0.33, solvate with 3 methanol ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C58 H48 Cu2 F6 Ge0.07 N16 O2 Si0.93, F6 Ge0.33 Si0.67, 3(C H4 O)' _chemical_formula_sum 'C61 H60 Cu2 F12 Ge0.40 N16 O5 Si1.60' _chemical_formula_weight 1526.31 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' Ge Ge 0.1547 1.8001 '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 tetragonal _symmetry_space_group_name_H-M 'I 4/m' _space_group_name_Hall '-I 4' _symmetry_Int_Tables_number 87 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 17.1776(8) _cell_length_b 17.1776(8) _cell_length_c 20.715(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6112.5(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 15148 _cell_measurement_theta_min 5.14 _cell_measurement_theta_max 26.37 _exptl_crystal_description prism _exptl_crystal_colour blue-green _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _exptl_crystal_density_diffrn 1.659 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3117 _exptl_absorpt_coefficient_mu 1.024 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7987 _exptl_absorpt_correction_T_max 0.8534 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker APEXII area-detector diffractometer' _diffrn_measurement_method '\w scans' _diffrn_standards_decay_% 0 _diffrn_reflns_number 15148 _diffrn_reflns_av_R_equivalents 0.0669 _diffrn_reflns_av_sigmaI/netI 0.0678 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 5.14 _diffrn_reflns_theta_max 26.37 _reflns_number_total 3195 _reflns_number_gt 2031 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT (Bruker, 1998)' _computing_cell_refinement 'SAINT-NT (Bruker, 1999)' _computing_data_reduction 'SAINT-NT (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Diamond 2.1e (Brandenburg, 1999)' _computing_publication_material 'WinGX 1.70.01 (Farrugia, 1999)' #------------------------------- Refinement data-----------------------# _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. Cu1 atom lies on a mirror plane and the "Si1/Ge1" and "Si2/Ge2" mixed atoms are at sites with crystallographically-imposed 2/m and 4-fold symmetry, respectively. In the framework of complex cation, [{SiF6}Cu2(L)4(CH3OH)2]2+, the methanol ligands are equally disordered by symmetry, in such a way that the C-atom is common for two components and two components of the disordered O-atom appear to be separated by ca. 1.25 A. The refined C-O distances were reasonable (although certainly shortened due to the disorder) and therefore no geometry restraints were applied. All atoms of cationic residue, including methanol ligand, were refined anisotropically. The OH-hydrogen was located and then fixed at d(O-H) = 0.85 A and with Uiso = 1.5Ueq(O). The aromatic CH-atoms were added geometrically [Uiso = 1.2Ueq(C)] and two sets of the methyl CH-atoms were added [Uiso = 1.5Ueq(C)] with partial contributions of 0.5 and considering two orientations of methanol O-atoms. Three unique solvate methanol molecules reside across symmetry elements and are disordered by symmetry over multiple positions. It was impossible to resolve the disordering schemes and therefore the corresponding electron density was modelled using a Squeeze routine implemented in Platon. Both positions of hexafluoroanions reveal isomorphic substitution of hexafluorosilicate and hexafluorogermanate. This was clearly indicated at the early stages by refinement of isotropic thermal parameters, and, therefore, in the subsequent refinements, the positions of corresponding central atoms of two hexafluoroanions were treated as "mixed Si/Ge atom", under common constraints for the positional (EXYZ) and thermal parameters (EADP) of the mixed atom and with the partial contributions set as additional free variables. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0414P)^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 constr _refine_ls_extinction_method none _refine_ls_number_reflns 3195 _refine_ls_number_parameters 225 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0750 _refine_ls_R_factor_gt 0.0407 _refine_ls_wR_factor_ref 0.0944 _refine_ls_wR_factor_gt 0.0863 _refine_ls_goodness_of_fit_ref 0.977 _refine_ls_restrained_S_all 0.977 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.64212(3) 0.17683(2) 0.0000 0.03612(18) Uani 1 2 d S . . Si1 Si 0.5000 0.0000 0.0000 0.0163(5) Uani 0.932(4) 4 d SP . . Ge1 Ge 0.5000 0.0000 0.0000 0.0163(5) Uani 0.068(4) 4 d SP . . Si2 Si 0.0000 0.0000 0.24655(5) 0.0189(4) Uani 0.666(4) 4 d SP . . Ge2 Ge 0.0000 0.0000 0.24655(5) 0.0189(4) Uani 0.334(4) 4 d SP . . F1 F 0.56262(10) 0.07548(10) 0.0000 0.0262(5) Uani 1 2 d S . . F2 F 0.42454(10) 0.06216(10) 0.0000 0.0246(5) Uani 1 2 d S . . F3 F 0.5000 0.0000 0.08192(10) 0.0254(5) Uani 1 2 d S . . F4 F 0.0000 0.0000 0.33001(15) 0.0256(7) Uani 1 4 d S . . F5 F 0.07718(8) 0.06431(7) 0.24694(8) 0.0294(4) Uani 1 1 d . . . F6 F 0.0000 0.0000 0.16354(16) 0.0379(8) Uani 1 4 d S . . N1 N 0.56799(13) 0.22321(12) 0.06848(13) 0.0378(7) Uani 1 1 d . . . N2 N 0.57771(15) 0.30027(13) 0.07776(15) 0.0505(8) Uani 1 1 d . . . N3 N 0.29408(12) -0.11555(13) 0.06912(14) 0.0373(7) Uani 1 1 d . . . N4 N 0.22138(14) -0.14222(15) 0.07947(15) 0.0501(8) Uani 1 1 d . . . C1 C 0.51075(16) 0.18561(16) 0.09817(16) 0.0363(8) Uani 1 1 d . . . H1 H 0.5071 0.1309 0.0920 0.044 Uiso 1 1 calc R . . C2 C 0.45561(17) 0.22129(16) 0.13793(15) 0.0389(8) Uani 1 1 d . . . C3 C 0.4665(2) 0.30013(18) 0.14653(18) 0.0545(10) Uani 1 1 d . . . H3 H 0.4321 0.3294 0.1730 0.065 Uiso 1 1 calc R . . C4 C 0.5279(2) 0.33545(19) 0.1161(2) 0.0579(11) Uani 1 1 d . . . H4 H 0.5350 0.3896 0.1232 0.070 Uiso 1 1 calc R . . C5 C 0.31817(16) -0.05071(16) 0.09756(15) 0.0363(8) Uani 1 1 d . . . H5 H 0.3703 -0.0346 0.0902 0.044 Uiso 1 1 calc R . . C6 C 0.27135(16) -0.00425(17) 0.13797(16) 0.0387(8) Uani 1 1 d . . . C7 C 0.19727(17) -0.0316(2) 0.14796(18) 0.0511(10) Uani 1 1 d . . . H7 H 0.1617 -0.0042 0.1747 0.061 Uiso 1 1 calc R . . C8 C 0.17604(18) -0.1002(2) 0.1180(2) 0.0593(11) Uani 1 1 d . . . H8 H 0.1248 -0.1189 0.1256 0.071 Uiso 1 1 calc R . . C9 C 0.39170(17) 0.17642(18) 0.16860(16) 0.0403(8) Uani 1 1 d . . . C10 C 0.36265(15) 0.10861(17) 0.13979(15) 0.0359(7) Uani 1 1 d . . . H10 H 0.3848 0.0906 0.1005 0.043 Uiso 1 1 calc R . . C11 C 0.30153(16) 0.06719(18) 0.16799(16) 0.0412(8) Uani 1 1 d . . . C12 C 0.2703(2) 0.0955(2) 0.22636(17) 0.0569(10) Uani 1 1 d . . . H12 H 0.2285 0.0684 0.2462 0.068 Uiso 1 1 calc R . . C13 C 0.2994(2) 0.1619(3) 0.25535(18) 0.0687(12) Uani 1 1 d . . . H13 H 0.2780 0.1798 0.2950 0.082 Uiso 1 1 calc R . . C14 C 0.3593(2) 0.2019(2) 0.22649(18) 0.0573(10) Uani 1 1 d . . . H14 H 0.3789 0.2477 0.2464 0.069 Uiso 1 1 calc R . . O1 O 0.7265(2) 0.2720(2) 0.0296(2) 0.0479(12) Uani 0.50 1 d P . . H1O H 0.7038 0.2937 0.0613 0.072 Uiso 0.50 1 d PR . . C15 C 0.7576(3) 0.3280(3) 0.0000 0.0750(19) Uani 1 2 d S . . H15A H 0.7901 0.3567 0.0293 0.112 Uiso 0.50 1 d PR . . H15B H 0.7887 0.3081 -0.0348 0.112 Uiso 0.50 1 d PR . . H15C H 0.7181 0.3618 -0.0170 0.112 Uiso 0.50 1 d PR . . 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 0.0236(3) 0.0207(3) 0.0641(4) 0.000 0.000 -0.00256(19) Si1 0.0154(7) 0.0142(7) 0.0193(8) 0.000 0.000 0.0004(4) Ge1 0.0154(7) 0.0142(7) 0.0193(8) 0.000 0.000 0.0004(4) Si2 0.0181(4) 0.0181(4) 0.0204(6) 0.000 0.000 0.000 Ge2 0.0181(4) 0.0181(4) 0.0204(6) 0.000 0.000 0.000 F1 0.0212(10) 0.0224(11) 0.0350(15) 0.000 0.000 -0.0059(8) F2 0.0215(11) 0.0220(10) 0.0302(14) 0.000 0.000 0.0054(8) F3 0.0268(11) 0.0264(11) 0.0230(13) 0.000 0.000 0.0041(8) F4 0.0251(9) 0.0251(9) 0.0267(19) 0.000 0.000 0.000 F5 0.0260(8) 0.0284(8) 0.0338(10) 0.0014(7) 0.0040(7) -0.0049(6) F6 0.0459(12) 0.0459(12) 0.022(2) 0.000 0.000 0.000 N1 0.0330(13) 0.0189(12) 0.0615(19) -0.0080(12) -0.0136(13) 0.0018(10) N2 0.0595(18) 0.0240(14) 0.068(2) -0.0117(14) -0.0161(16) 0.0007(12) N3 0.0213(12) 0.0349(14) 0.0559(19) 0.0207(13) 0.0084(12) 0.0016(10) N4 0.0245(14) 0.0564(17) 0.070(2) 0.0236(15) 0.0076(14) -0.0068(11) C1 0.0326(16) 0.0256(15) 0.051(2) -0.0156(15) -0.0102(15) 0.0051(12) C2 0.0422(18) 0.0389(17) 0.036(2) -0.0168(15) -0.0142(15) 0.0142(13) C3 0.071(2) 0.0378(19) 0.055(3) -0.0217(18) -0.008(2) 0.0238(17) C4 0.080(3) 0.0287(18) 0.065(3) -0.0170(18) -0.014(2) 0.0097(17) C5 0.0231(15) 0.0350(17) 0.051(2) 0.0134(15) 0.0095(14) 0.0002(12) C6 0.0298(16) 0.0489(19) 0.038(2) 0.0195(16) 0.0085(14) 0.0158(13) C7 0.0280(17) 0.072(2) 0.054(3) 0.023(2) 0.0146(17) 0.0154(16) C8 0.0216(17) 0.077(3) 0.079(3) 0.027(2) 0.0160(18) 0.0010(16) C9 0.0397(18) 0.0488(19) 0.032(2) -0.0101(16) -0.0030(15) 0.0232(14) C10 0.0305(16) 0.0480(18) 0.0292(18) -0.0030(15) 0.0062(14) 0.0170(13) C11 0.0338(17) 0.055(2) 0.035(2) 0.0068(16) 0.0070(15) 0.0182(14) C12 0.045(2) 0.085(3) 0.041(2) 0.015(2) 0.0188(18) 0.0289(18) C13 0.070(3) 0.103(3) 0.034(2) -0.014(2) 0.008(2) 0.043(2) C14 0.060(2) 0.072(2) 0.039(2) -0.020(2) -0.0041(19) 0.0295(19) O1 0.048(2) 0.038(2) 0.057(3) 0.001(2) 0.007(2) -0.0199(18) C15 0.059(3) 0.056(3) 0.110(6) 0.000 0.000 -0.033(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 2.066(3) 10 ? Cu1 N1 2.066(3) . ? Cu1 N3 2.088(3) 2_655 ? Cu1 N3 2.088(3) 9_655 ? Cu1 F1 2.2127(17) . ? Cu1 O1 2.270(3) . ? Cu1 O1 2.270(3) 10 ? Si1 F2 1.6793(17) 9_655 ? Si1 F2 1.6793(17) . ? Si1 F1 1.6846(17) 9_655 ? Si1 F1 1.6846(17) . ? Si1 F3 1.697(2) 9_655 ? Si1 F3 1.697(2) . ? Si2 F6 1.720(3) . ? Si2 F5 1.7258(13) . ? Si2 F5 1.7258(13) 3 ? Si2 F5 1.7258(13) 2 ? Si2 F5 1.7258(13) 4 ? Si2 F4 1.729(3) . ? N1 C1 1.328(4) . ? N1 N2 1.348(3) . ? N2 C4 1.314(4) . ? N3 C5 1.326(4) . ? N3 N4 1.347(3) . ? N3 Cu1 2.088(3) 9_655 ? N4 C8 1.328(4) . ? C1 C2 1.397(4) . ? C1 H1 0.9500 . ? C2 C3 1.379(4) . ? C2 C9 1.484(4) . ? C3 C4 1.371(5) . ? C3 H3 0.9500 . ? C4 H4 0.9500 . ? C5 C6 1.409(4) . ? C5 H5 0.9500 . ? C6 C7 1.372(4) . ? C6 C11 1.470(4) . ? C7 C8 1.380(5) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C14 1.393(4) . ? C9 C10 1.401(4) . ? C10 C11 1.396(4) . ? C10 H10 0.9500 . ? C11 C12 1.409(4) . ? C12 C13 1.382(5) . ? C12 H12 0.9500 . ? C13 C14 1.374(5) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? O1 O1 1.228(9) 10 ? O1 C15 1.261(5) . ? O1 H1O 0.8500 . ? C15 O1 1.261(5) 10 ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? 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 N1 Cu1 N1 86.72(13) 10 . ? N1 Cu1 N3 171.41(9) 10 2_655 ? N1 Cu1 N3 92.70(9) . 2_655 ? N1 Cu1 N3 92.70(9) 10 9_655 ? N1 Cu1 N3 171.41(9) . 9_655 ? N3 Cu1 N3 86.60(13) 2_655 9_655 ? N1 Cu1 F1 85.58(7) 10 . ? N1 Cu1 F1 85.58(7) . . ? N3 Cu1 F1 85.83(7) 2_655 . ? N3 Cu1 F1 85.83(7) 9_655 . ? N1 Cu1 O1 107.56(12) 10 . ? N1 Cu1 O1 86.00(12) . . ? N3 Cu1 O1 80.92(12) 2_655 . ? N3 Cu1 O1 102.32(12) 9_655 . ? F1 Cu1 O1 163.93(11) . . ? N1 Cu1 O1 86.00(12) 10 10 ? N1 Cu1 O1 107.56(12) . 10 ? N3 Cu1 O1 102.32(12) 2_655 10 ? N3 Cu1 O1 80.92(12) 9_655 10 ? F1 Cu1 O1 163.93(11) . 10 ? F2 Si1 F2 180.0 9_655 . ? F2 Si1 F1 90.20(9) 9_655 9_655 ? F2 Si1 F1 89.80(9) . 9_655 ? F2 Si1 F1 89.80(9) 9_655 . ? F2 Si1 F1 90.20(9) . . ? F1 Si1 F1 180.0 9_655 . ? F2 Si1 F3 90.0 9_655 9_655 ? F2 Si1 F3 90.0 . 9_655 ? F1 Si1 F3 90.0 9_655 9_655 ? F1 Si1 F3 90.0 . 9_655 ? F2 Si1 F3 90.0 9_655 . ? F2 Si1 F3 90.0 . . ? F1 Si1 F3 90.0 9_655 . ? F1 Si1 F3 90.0 . . ? F3 Si1 F3 180.0 9_655 . ? F6 Si2 F5 90.26(6) . . ? F6 Si2 F5 90.26(6) . 3 ? F5 Si2 F5 90.0 . 3 ? F6 Si2 F5 90.26(6) . 2 ? F5 Si2 F5 179.47(13) . 2 ? F5 Si2 F5 90.0 3 2 ? F6 Si2 F5 90.26(6) . 4 ? F5 Si2 F5 90.0 . 4 ? F5 Si2 F5 179.47(13) 3 4 ? F5 Si2 F5 90.0 2 4 ? F6 Si2 F4 180.0 . . ? F5 Si2 F4 89.74(6) . . ? F5 Si2 F4 89.74(6) 3 . ? F5 Si2 F4 89.74(6) 2 . ? F5 Si2 F4 89.74(6) 4 . ? Si1 F1 Cu1 178.44(11) . . ? C1 N1 N2 120.2(3) . . ? C1 N1 Cu1 125.94(17) . . ? N2 N1 Cu1 113.6(2) . . ? C4 N2 N1 117.2(3) . . ? C5 N3 N4 120.3(3) . . ? C5 N3 Cu1 124.35(18) . 9_655 ? N4 N3 Cu1 115.1(2) . 9_655 ? C8 N4 N3 117.0(3) . . ? N1 C1 C2 124.2(3) . . ? N1 C1 H1 117.9 . . ? C2 C1 H1 117.9 . . ? C3 C2 C1 114.6(3) . . ? C3 C2 C9 123.7(3) . . ? C1 C2 C9 121.7(3) . . ? C4 C3 C2 118.6(3) . . ? C4 C3 H3 120.7 . . ? C2 C3 H3 120.7 . . ? N2 C4 C3 125.1(3) . . ? N2 C4 H4 117.4 . . ? C3 C4 H4 117.4 . . ? N3 C5 C6 124.2(3) . . ? N3 C5 H5 117.9 . . ? C6 C5 H5 117.9 . . ? C7 C6 C5 115.1(3) . . ? C7 C6 C11 123.3(3) . . ? C5 C6 C11 121.5(3) . . ? C6 C7 C8 118.0(3) . . ? C6 C7 H7 121.0 . . ? C8 C7 H7 121.0 . . ? N4 C8 C7 125.4(3) . . ? N4 C8 H8 117.3 . . ? C7 C8 H8 117.3 . . ? C14 C9 C10 119.0(3) . . ? C14 C9 C2 120.1(3) . . ? C10 C9 C2 120.9(3) . . ? C11 C10 C9 120.9(3) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C10 C11 C12 118.0(3) . . ? C10 C11 C6 120.9(3) . . ? C12 C11 C6 121.1(3) . . ? C13 C12 C11 121.4(3) . . ? C13 C12 H12 119.3 . . ? C11 C12 H12 119.3 . . ? C14 C13 C12 119.6(3) . . ? C14 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? C13 C14 C9 121.1(4) . . ? C13 C14 H14 119.4 . . ? C9 C14 H14 119.4 . . ? C15 O1 Cu1 133.5(3) . . ? C15 O1 H1O 103.6 . . ? Cu1 O1 H1O 103.4 . . ? O1 C15 H15A 109.3 . . ? O1 C15 H15B 109.2 . . ? H15A C15 H15B 109.5 . . ? O1 C15 H15C 109.9 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? 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 N1 Cu1 N1 C1 95.9(2) 10 . . . ? N3 Cu1 N1 C1 -75.5(2) 2_655 . . . ? F1 Cu1 N1 C1 10.1(2) . . . . ? O1 Cu1 N1 C1 -156.2(3) . . . . ? O1 Cu1 N1 C1 -179.4(2) 10 . . . ? N1 Cu1 N1 N2 -78.6(2) 10 . . . ? N3 Cu1 N1 N2 110.0(2) 2_655 . . . ? F1 Cu1 N1 N2 -164.37(19) . . . . ? O1 Cu1 N1 N2 29.3(2) . . . . ? O1 Cu1 N1 N2 6.2(2) 10 . . . ? C1 N1 N2 C4 -1.0(4) . . . . ? Cu1 N1 N2 C4 173.8(2) . . . . ? C5 N3 N4 C8 1.0(4) . . . . ? Cu1 N3 N4 C8 -173.2(2) 9_655 . . . ? N2 N1 C1 C2 2.7(5) . . . . ? Cu1 N1 C1 C2 -171.4(2) . . . . ? N1 C1 C2 C3 -2.3(5) . . . . ? N1 C1 C2 C9 178.5(3) . . . . ? C1 C2 C3 C4 0.4(5) . . . . ? C9 C2 C3 C4 179.6(3) . . . . ? N1 N2 C4 C3 -0.9(5) . . . . ? C2 C3 C4 N2 1.2(6) . . . . ? N4 N3 C5 C6 -2.0(5) . . . . ? Cu1 N3 C5 C6 171.7(2) 9_655 . . . ? N3 C5 C6 C7 1.5(5) . . . . ? N3 C5 C6 C11 -179.9(3) . . . . ? C5 C6 C7 C8 -0.3(5) . . . . ? C11 C6 C7 C8 -178.8(3) . . . . ? N3 N4 C8 C7 0.2(5) . . . . ? C6 C7 C8 N4 -0.6(5) . . . . ? C3 C2 C9 C14 -26.6(5) . . . . ? C1 C2 C9 C14 152.5(3) . . . . ? C3 C2 C9 C10 152.9(3) . . . . ? C1 C2 C9 C10 -28.0(4) . . . . ? C14 C9 C10 C11 0.7(4) . . . . ? C2 C9 C10 C11 -178.8(3) . . . . ? C9 C10 C11 C12 -0.3(4) . . . . ? C9 C10 C11 C6 -179.6(3) . . . . ? C7 C6 C11 C10 -155.6(3) . . . . ? C5 C6 C11 C10 25.9(4) . . . . ? C7 C6 C11 C12 25.1(5) . . . . ? C5 C6 C11 C12 -153.4(3) . . . . ? C10 C11 C12 C13 -0.4(5) . . . . ? C6 C11 C12 C13 178.9(3) . . . . ? C11 C12 C13 C14 0.8(5) . . . . ? C12 C13 C14 C9 -0.4(5) . . . . ? C10 C9 C14 C13 -0.3(5) . . . . ? C2 C9 C14 C13 179.1(3) . . . . ? N1 Cu1 O1 O1 -48.77(7) 10 . . 10 ? N1 Cu1 O1 O1 -134.05(7) . . . 10 ? N3 Cu1 O1 O1 132.57(7) 2_655 . . 10 ? N3 Cu1 O1 O1 48.10(7) 9_655 . . 10 ? F1 Cu1 O1 O1 167.4(4) . . . 10 ? N1 Cu1 O1 C15 -33.6(5) 10 . . . ? N1 Cu1 O1 C15 -118.9(5) . . . . ? N3 Cu1 O1 C15 147.7(5) 2_655 . . . ? N3 Cu1 O1 C15 63.3(5) 9_655 . . . ? F1 Cu1 O1 C15 -177.4(4) . . . . ? O1 Cu1 O1 C15 15.2(5) 10 . . . ? Cu1 O1 C15 O1 -16.8(5) . . . 10 ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.272 _refine_diff_density_min -0.486 _refine_diff_density_rms 0.060 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 200 61 '3 CH3OH' 2 0.000 0.000 0.500 64 14 CH3OH 3 0.000 0.500 0.250 70 19 CH3OH 4 0.000 0.500 0.750 70 19 CH3OH 5 0.500 0.500 0.500 200 61 '3 CH3OH' 6 0.500 0.500 0.000 64 14 CH3OH 7 0.500 0.000 0.250 70 19 CH3OH 8 0.500 0.000 0.750 70 19 CH3OH _platon_squeeze_details ; ; _iucr_refine_instruction_details ; #--------------------------------------------------------- TITL dk17 in I4/m CELL 0.71073 17.1776 17.1776 20.7153 90.000 90.000 90.000 ZERR 4.00 0.0008 0.0008 0.0022 0.000 0.000 0.000 LATT 2 SYMM - X, - Y, Z SYMM - Y, X, Z SYMM Y, - X, Z SFAC C H N O F SI GE CU UNIT 244 240 64 20 48 6.40 1.60 8 MERG 2 OMIT -1 7 0 OMIT 2 4 2 OMIT 1 7 4 OMIT 1 3 4 EXYZ Si1 Ge1 EXYZ Si2 Ge2 EADP Si1 Ge1 EADP Si2 Ge2 SHEL 0.80 4 FMAP 2 PLAN 20 SIZE 0.16 0.22 0.23 ACTA BOND BOND $H CONF LIST 4 L.S. 6 TEMP -100.00 WGHT 0.041400 FVAR 1.44694 0.93225 0.66618 CU1 8 0.642124 0.176827 0.000000 10.50000 0.02360 0.02066 = 0.06409 0.00000 0.00000 -0.00256 SI1 6 0.500000 0.000000 0.000000 20.25000 0.01540 0.01423 = 0.01930 0.00000 0.00000 0.00040 GE1 7 0.500000 0.000000 0.000000 -20.25000 0.01540 0.01423 = 0.01930 0.00000 0.00000 0.00040 SI2 6 0.000000 0.000000 0.246554 30.25000 0.01806 0.01806 = 0.02045 0.00000 0.00000 0.00000 GE2 7 0.000000 0.000000 0.246554 -30.25000 0.01806 0.01806 = 0.02045 0.00000 0.00000 0.00000 F1 5 0.562617 0.075481 0.000000 10.50000 0.02120 0.02235 = 0.03498 0.00000 0.00000 -0.00589 F2 5 0.424544 0.062163 0.000000 10.50000 0.02150 0.02204 = 0.03023 0.00000 0.00000 0.00540 F3 5 0.500000 0.000000 0.081921 10.50000 0.02681 0.02640 = 0.02301 0.00000 0.00000 0.00411 F4 5 0.000000 0.000000 0.330013 10.25000 0.02506 0.02506 = 0.02666 0.00000 0.00000 0.00000 F5 5 0.077185 0.064315 0.246939 11.00000 0.02597 0.02836 = 0.03376 0.00136 0.00396 -0.00485 F6 5 0.000000 0.000000 0.163542 10.25000 0.04587 0.04587 = 0.02210 0.00000 0.00000 0.00000 N1 3 0.567993 0.223211 0.068477 11.00000 0.03296 0.01889 = 0.06154 -0.00800 -0.01355 0.00177 N2 3 0.577710 0.300267 0.077764 11.00000 0.05953 0.02402 = 0.06797 -0.01174 -0.01612 0.00074 N3 3 0.294078 -0.115546 0.069124 11.00000 0.02127 0.03486 = 0.05591 0.02069 0.00840 0.00158 N4 3 0.221381 -0.142223 0.079472 11.00000 0.02455 0.05637 = 0.06951 0.02356 0.00759 -0.00679 C1 1 0.510754 0.185609 0.098172 11.00000 0.03257 0.02558 = 0.05064 -0.01561 -0.01024 0.00511 AFIX 43 H1 2 0.507059 0.130934 0.091987 11.00000 -1.20000 AFIX 0 C2 1 0.455612 0.221287 0.137928 11.00000 0.04219 0.03887 = 0.03571 -0.01678 -0.01422 0.01420 C3 1 0.466452 0.300133 0.146526 11.00000 0.07107 0.03778 = 0.05480 -0.02173 -0.00784 0.02376 AFIX 43 H3 2 0.432053 0.329394 0.172998 11.00000 -1.20000 AFIX 0 C4 1 0.527911 0.335449 0.116077 11.00000 0.07967 0.02874 = 0.06540 -0.01701 -0.01388 0.00971 AFIX 43 H4 2 0.535050 0.389606 0.123243 11.00000 -1.20000 AFIX 0 C5 1 0.318167 -0.050714 0.097561 11.00000 0.02306 0.03497 = 0.05098 0.01335 0.00953 0.00016 AFIX 43 H5 2 0.370317 -0.034575 0.090213 11.00000 -1.20000 AFIX 0 C6 1 0.271353 -0.004248 0.137973 11.00000 0.02977 0.04889 = 0.03751 0.01952 0.00849 0.01580 C7 1 0.197272 -0.031624 0.147959 11.00000 0.02800 0.07155 = 0.05379 0.02302 0.01458 0.01536 AFIX 43 H7 2 0.161665 -0.004206 0.174688 11.00000 -1.20000 AFIX 0 C8 1 0.176044 -0.100196 0.117999 11.00000 0.02162 0.07719 = 0.07916 0.02733 0.01599 0.00097 AFIX 43 H8 2 0.124791 -0.118869 0.125555 11.00000 -1.20000 AFIX 0 C9 1 0.391698 0.176417 0.168600 11.00000 0.03974 0.04884 = 0.03223 -0.01012 -0.00304 0.02318 C10 1 0.362646 0.108612 0.139794 11.00000 0.03049 0.04795 = 0.02924 -0.00300 0.00619 0.01695 AFIX 43 H10 2 0.384823 0.090559 0.100540 11.00000 -1.20000 AFIX 0 C11 1 0.301528 0.067190 0.167993 11.00000 0.03381 0.05510 = 0.03471 0.00680 0.00696 0.01824 C12 1 0.270336 0.095487 0.226360 11.00000 0.04497 0.08481 = 0.04079 0.01475 0.01884 0.02893 AFIX 43 H12 2 0.228494 0.068363 0.246194 11.00000 -1.20000 AFIX 0 C13 1 0.299351 0.161886 0.255354 11.00000 0.06952 0.10286 = 0.03385 -0.01401 0.00843 0.04334 AFIX 43 H13 2 0.278012 0.179769 0.294978 11.00000 -1.20000 AFIX 0 C14 1 0.359281 0.201879 0.226491 11.00000 0.06029 0.07224 = 0.03947 -0.02014 -0.00411 0.02952 AFIX 43 H14 2 0.378927 0.247680 0.246374 11.00000 -1.20000 AFIX 0 O1 4 0.726520 0.271985 0.029645 10.50000 0.04844 0.03843 = 0.05671 0.00121 0.00700 -0.01988 AFIX 3 H1O 2 0.703790 0.293706 0.061325 10.50000 -1.50000 AFIX 0 C15 1 0.757629 0.328034 0.000000 10.50000 0.05896 0.05587 = 0.11010 0.00000 0.00000 -0.03300 AFIX 3 H15A 2 0.790139 0.356694 0.029260 10.50000 -1.50000 H15B 2 0.788709 0.308124 -0.034800 10.50000 -1.50000 H15C 2 0.718079 0.361784 -0.016990 10.50000 -1.50000 HKLF 4 REM dk17 in I4/m REM R1 = 0.0407 for 2031 Fo > 4sig(Fo) and 0.0750 for all 3195 data REM 225 parameters refined using 0 restraints END WGHT 0.0408 0.0000 REM Highest difference peak 0.272, deepest hole -0.486, 1-sigma level 0.060 Q1 1 0.8329 0.3306 0.0000 10.50000 0.05 0.27 Q2 1 0.3583 0.3276 0.2489 11.00000 0.05 0.27 Q3 1 0.4309 0.0980 0.0000 10.50000 0.05 0.26 Q4 1 0.3223 0.1838 0.2227 11.00000 0.05 0.25 Q5 1 0.3154 -0.1348 0.0444 11.00000 0.05 0.25 Q6 1 0.6569 0.3315 -0.0269 11.00000 0.05 0.24 Q7 1 0.7851 0.3712 0.0000 10.50000 0.05 0.23 Q8 1 0.0770 0.0967 0.2495 11.00000 0.05 0.23 ; _database_code_depnum_ccdc_archive 'CCDC 941551' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_(1b) _audit_creation_method SHELXL-97 _chemical_name_systematic ; \m-[Hexafluorosilicato/Hexafluorogermanato 0.89:0.11]- tetrakis[\m-1,3-bis(pyridazin-4-yl)benzene- \k^2^N^2^:N^2'^]-dimethanol-dicopper(II) Hexafluorosilicate/Hexafluorogermanate 0.38:0.62, solvate with 3 methanol ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C58 H48 Cu2 F6 Ge0.11 N16 O2 Si0.89, F6 Ge0.62 Si0.38, 3(C H4 O)' _chemical_formula_sum 'C61 H60 Cu2 F12 Ge0.73 N16 O5 Si1.27' _chemical_formula_weight 1540.88 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' Ge Ge 0.1547 1.8001 '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 tetragonal _symmetry_space_group_name_H-M 'I 4/m' _space_group_name_Hall '-I 4' _symmetry_Int_Tables_number 87 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 17.2531(3) _cell_length_b 17.2531(3) _cell_length_c 20.5377(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6113.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 14347 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 26.33 _exptl_crystal_description prism _exptl_crystal_colour blue-green _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.674 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3140 _exptl_absorpt_coefficient_mu 1.175 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7049 _exptl_absorpt_correction_T_max 0.8435 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker APEXII area-detector diffractometer' _diffrn_measurement_method '\w scans' _diffrn_standards_decay_% 0 _diffrn_reflns_number 14347 _diffrn_reflns_av_R_equivalents 0.0705 _diffrn_reflns_av_sigmaI/netI 0.0729 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 26.33 _reflns_number_total 3208 _reflns_number_gt 1978 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT (Bruker, 1998)' _computing_cell_refinement 'SAINT-NT (Bruker, 1999)' _computing_data_reduction 'SAINT-NT (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Diamond 2.1e (Brandenburg, 1999)' _computing_publication_material 'WinGX 1.70.01 (Farrugia, 1999)' #------------------------------- Refinement data-----------------------# _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. Cu1 atom lies on a mirror plane and the "Si1/Ge1" and "Si2/Ge2" mixed atoms are at sites with crystallographically-imposed 2/m and 4-fold symmetry, respectively. In the framework of complex cation, [{SiF6}Cu2(L)4(CH3OH)2]2+, the methanol ligands are equally disordered by symmetry, in such a way that the C-atom is common for two components and two components of the disordered O-atom appear to be separated by ca. 1.25 A. The refined C-O distances were reasonable (although certainly shortened due to the disorder) and therefore no geometry restraints were applied. All atoms of cationic residue, including methanol ligand, were refined anisotropically. The OH-hydrogen was located and then fixed at d(O-H) = 0.85 A and with Uiso = 1.5Ueq(O). The aromatic CH-atoms were added geometrically [Uiso = 1.2Ueq(C)] and two sets of the methyl CH-atoms were added [Uiso = 1.5Ueq(C)] with partial contributions of 0.5 and considering two orientations of methanol O-atoms. Three unique solvate methanol molecules reside across symmetry elements and are disordered by symmetry over multiple positions. It was impossible to resolve the disordering schemes and therefore the corresponding electron density was modelled using a Squeeze routine implemented in Platon. Both positions of hexafluoroanions reveal isomorphic substitution of hexafluorosilicate and hexafluorogermanate. This was clearly indicated at the early stages by refinement of isotropic thermal parameters, and, therefore, in the subsequent refinements, the positions of corresponding central atoms of two hexafluoroanions were treated as "mixed Si/Ge atom", under common constraints for the positional (EXYZ) and thermal parameters (EADP) of the mixed atom and with the partial contributions set as additional free variables. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0435P)^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 constr _refine_ls_extinction_method none _refine_ls_number_reflns 3208 _refine_ls_number_parameters 225 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0846 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.1016 _refine_ls_wR_factor_gt 0.0916 _refine_ls_goodness_of_fit_ref 0.960 _refine_ls_restrained_S_all 0.960 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.67580(3) 0.14209(3) 0.0000 0.0406(2) Uani 1 2 d S . . Si1 Si 0.5000 0.0000 0.0000 0.0168(5) Uani 0.894(4) 4 d SP . . Ge1 Ge 0.5000 0.0000 0.0000 0.0168(5) Uani 0.106(4) 4 d SP . . Si2 Si 0.0000 0.0000 0.25367(4) 0.0187(3) Uani 0.377(4) 4 d SP . . Ge2 Ge 0.0000 0.0000 0.25367(4) 0.0187(3) Uani 0.623(4) 4 d SP . . F1 F 0.57474(12) 0.06271(12) 0.0000 0.0269(6) Uani 1 2 d S . . F2 F 0.5000 0.0000 0.08249(11) 0.0255(6) Uani 1 2 d S . . F3 F 0.43718(12) 0.07463(12) 0.0000 0.0233(6) Uani 1 2 d S . . F4 F 0.0000 0.0000 0.33913(16) 0.0350(9) Uani 1 4 d S . . F5 F 0.06638(9) 0.07701(9) 0.25346(8) 0.0296(4) Uani 1 1 d . . . F6 F 0.0000 0.0000 0.16807(15) 0.0248(8) Uani 1 4 d S . . N1 N 0.61449(16) 0.20558(15) 0.06930(17) 0.0459(9) Uani 1 1 d . . . N2 N 0.63948(19) 0.27930(17) 0.07774(19) 0.0655(11) Uani 1 1 d . . . N3 N 0.27768(15) -0.06875(16) 0.06882(15) 0.0398(8) Uani 1 1 d . . . N4 N 0.20087(16) -0.07786(19) 0.07708(17) 0.0545(9) Uani 1 1 d . . . C1 C 0.5502(2) 0.1811(2) 0.09864(18) 0.0415(10) Uani 1 1 d . . . H1 H 0.5354 0.1286 0.0924 0.050 Uiso 1 1 calc R . . C2 C 0.5028(2) 0.2276(2) 0.13819(19) 0.0442(10) Uani 1 1 d . . . C3 C 0.5277(3) 0.3033(2) 0.1459(2) 0.0614(13) Uani 1 1 d . . . H3 H 0.4989 0.3392 0.1712 0.074 Uiso 1 1 calc R . . C4 C 0.5958(3) 0.3247(2) 0.1157(2) 0.0733(16) Uani 1 1 d . . . H4 H 0.6132 0.3763 0.1225 0.088 Uiso 1 1 calc R . . C5 C 0.3147(2) -0.01128(19) 0.09853(18) 0.0378(9) Uani 1 1 d . . . H5 H 0.3691 -0.0075 0.0922 0.045 Uiso 1 1 calc R . . C6 C 0.2791(2) 0.0446(2) 0.13876(18) 0.0424(10) Uani 1 1 d . . . C7 C 0.2002(2) 0.0340(3) 0.1470(2) 0.0623(13) Uani 1 1 d . . . H7 H 0.1709 0.0683 0.1736 0.075 Uiso 1 1 calc R . . C8 C 0.1652(2) -0.0273(3) 0.1159(2) 0.0653(14) Uani 1 1 d . . . H8 H 0.1112 -0.0341 0.1226 0.078 Uiso 1 1 calc R . . C9 C 0.4313(2) 0.1979(2) 0.16875(18) 0.0454(10) Uani 1 1 d . . . C10 C 0.3904(2) 0.13667(19) 0.14093(17) 0.0397(9) Uani 1 1 d . . . H10 H 0.4090 0.1140 0.1018 0.048 Uiso 1 1 calc R . . C11 C 0.3228(2) 0.1078(2) 0.16930(18) 0.0436(10) Uani 1 1 d . . . C12 C 0.2979(3) 0.1408(3) 0.22759(19) 0.0633(14) Uani 1 1 d . . . H12 H 0.2528 0.1212 0.2484 0.076 Uiso 1 1 calc R . . C13 C 0.3379(3) 0.2011(3) 0.2552(2) 0.0768(16) Uani 1 1 d . . . H13 H 0.3194 0.2232 0.2947 0.092 Uiso 1 1 calc R . . C14 C 0.4040(3) 0.2302(3) 0.2270(2) 0.0639(13) Uani 1 1 d . . . H14 H 0.4310 0.2720 0.2469 0.077 Uiso 1 1 calc R . . O1 O 0.7716(2) 0.2242(3) 0.0321(2) 0.0495(14) Uani 0.50 1 d P . . H1O H 0.7473 0.2621 0.0488 0.074 Uiso 0.50 1 d PR . . C15 C 0.8262(3) 0.2573(3) 0.0000 0.072(2) Uani 1 2 d S . . H15A H 0.8555 0.2898 0.0289 0.108 Uiso 0.50 1 d PR . . H15B H 0.8592 0.2177 -0.0176 0.108 Uiso 0.50 1 d PR . . H15C H 0.8056 0.2881 -0.0349 0.108 Uiso 0.50 1 d PR . . 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 0.0202(3) 0.0236(3) 0.0780(5) 0.000 0.000 -0.0023(3) Si1 0.0151(8) 0.0162(8) 0.0191(9) 0.000 0.000 0.0005(6) Ge1 0.0151(8) 0.0162(8) 0.0191(9) 0.000 0.000 0.0005(6) Si2 0.0187(4) 0.0187(4) 0.0186(5) 0.000 0.000 0.000 Ge2 0.0187(4) 0.0187(4) 0.0186(5) 0.000 0.000 0.000 F1 0.0201(12) 0.0240(13) 0.0366(16) 0.000 0.000 -0.0049(11) F2 0.0269(13) 0.0280(13) 0.0216(14) 0.000 0.000 0.0083(11) F3 0.0224(12) 0.0238(13) 0.0235(14) 0.000 0.000 0.0058(10) F4 0.0443(14) 0.0443(14) 0.017(2) 0.000 0.000 0.000 F5 0.0305(10) 0.0255(9) 0.0329(11) -0.0046(8) -0.0024(9) -0.0061(8) F6 0.0278(12) 0.0278(12) 0.0188(19) 0.000 0.000 0.000 N1 0.0369(17) 0.0202(15) 0.081(3) -0.0141(15) -0.0208(17) 0.0002(14) N2 0.055(2) 0.0294(18) 0.112(3) -0.018(2) -0.025(2) -0.0036(16) N3 0.0245(15) 0.0325(16) 0.062(2) 0.0159(15) 0.0126(15) 0.0027(14) N4 0.0236(17) 0.063(2) 0.077(3) 0.0223(19) 0.0157(17) 0.0035(16) C1 0.039(2) 0.033(2) 0.053(3) -0.0197(18) -0.0213(19) 0.0061(18) C2 0.053(2) 0.034(2) 0.046(2) -0.0195(19) -0.029(2) 0.0169(19) C3 0.067(3) 0.046(3) 0.071(3) -0.028(2) -0.027(3) 0.016(2) C4 0.094(4) 0.024(2) 0.101(4) -0.027(2) -0.040(3) 0.000(3) C5 0.0298(19) 0.034(2) 0.050(2) 0.0151(18) 0.0181(18) 0.0095(17) C6 0.042(2) 0.045(2) 0.040(2) 0.0143(19) 0.0185(19) 0.0179(19) C7 0.049(3) 0.080(3) 0.057(3) 0.015(3) 0.024(2) 0.032(3) C8 0.028(2) 0.093(4) 0.076(4) 0.030(3) 0.021(2) 0.013(2) C9 0.057(3) 0.042(2) 0.036(2) -0.0156(18) -0.011(2) 0.027(2) C10 0.054(2) 0.038(2) 0.027(2) -0.0092(17) 0.0001(19) 0.0227(19) C11 0.054(2) 0.044(2) 0.032(2) 0.0061(18) 0.0139(19) 0.026(2) C12 0.087(3) 0.071(3) 0.031(2) 0.007(2) 0.026(2) 0.047(3) C13 0.111(4) 0.087(4) 0.033(3) -0.015(3) 0.004(3) 0.061(3) C14 0.089(3) 0.061(3) 0.042(3) -0.022(2) -0.019(3) 0.044(3) O1 0.036(3) 0.052(3) 0.060(3) -0.002(2) 0.012(2) -0.020(2) C15 0.048(4) 0.067(4) 0.102(6) 0.000 0.000 -0.029(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N3 2.060(3) 9_655 ? Cu1 N3 2.060(3) 2_655 ? Cu1 N1 2.084(3) . ? Cu1 N1 2.084(3) 10 ? Cu1 F1 2.217(2) . ? Cu1 O1 2.274(4) . ? Cu1 O1 2.274(4) 10 ? Si1 F3 1.683(2) 9_655 ? Si1 F3 1.683(2) . ? Si1 F1 1.683(2) . ? Si1 F1 1.683(2) 9_655 ? Si1 F2 1.694(2) 9_655 ? Si1 F2 1.694(2) . ? Si2 F5 1.7542(16) 2 ? Si2 F5 1.7542(16) . ? Si2 F5 1.7542(16) 4 ? Si2 F5 1.7542(16) 3 ? Si2 F4 1.755(3) . ? Si2 F6 1.758(3) . ? N1 C1 1.330(4) . ? N1 N2 1.354(4) . ? N2 C4 1.338(5) . ? N3 C5 1.328(4) . ? N3 N4 1.345(3) . ? N3 Cu1 2.060(3) 9_655 ? N4 C8 1.332(5) . ? C1 C2 1.404(5) . ? C1 H1 0.9500 . ? C2 C3 1.384(5) . ? C2 C9 1.476(5) . ? C3 C4 1.378(6) . ? C3 H3 0.9500 . ? C4 H4 0.9500 . ? C5 C6 1.410(5) . ? C5 H5 0.9500 . ? C6 C7 1.383(5) . ? C6 C11 1.468(5) . ? C7 C8 1.376(6) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C10 1.393(5) . ? C9 C14 1.402(5) . ? C10 C11 1.395(5) . ? C10 H10 0.9500 . ? C11 C12 1.393(5) . ? C12 C13 1.371(6) . ? C12 H12 0.9500 . ? C13 C14 1.374(6) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? O1 C15 1.283(5) . ? O1 O1 1.317(9) 10 ? O1 H1O 0.8500 . ? C15 O1 1.283(5) 10 ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? 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 N3 Cu1 N3 86.66(16) 9_655 2_655 ? N3 Cu1 N1 171.53(11) 9_655 . ? N3 Cu1 N1 92.98(11) 2_655 . ? N3 Cu1 N1 92.98(11) 9_655 10 ? N3 Cu1 N1 171.53(11) 2_655 10 ? N1 Cu1 N1 86.13(17) . 10 ? N3 Cu1 F1 85.81(9) 9_655 . ? N3 Cu1 F1 85.81(9) 2_655 . ? N1 Cu1 F1 85.73(9) . . ? N1 Cu1 F1 85.73(9) 10 . ? N3 Cu1 O1 107.35(14) 9_655 . ? N3 Cu1 O1 84.30(14) 2_655 . ? N1 Cu1 O1 81.01(14) . . ? N1 Cu1 O1 103.85(14) 10 . ? F1 Cu1 O1 162.99(12) . . ? N3 Cu1 O1 84.30(14) 9_655 10 ? N3 Cu1 O1 107.35(14) 2_655 10 ? N1 Cu1 O1 103.85(14) . 10 ? N1 Cu1 O1 81.01(14) 10 10 ? F1 Cu1 O1 162.99(12) . 10 ? F3 Si1 F3 180.0 9_655 . ? F3 Si1 F1 89.91(10) 9_655 . ? F3 Si1 F1 90.09(10) . . ? F3 Si1 F1 90.09(10) 9_655 9_655 ? F3 Si1 F1 89.91(10) . 9_655 ? F1 Si1 F1 180.0 . 9_655 ? F3 Si1 F2 90.0 9_655 9_655 ? F3 Si1 F2 90.0 . 9_655 ? F1 Si1 F2 90.0 . 9_655 ? F1 Si1 F2 90.0 9_655 9_655 ? F3 Si1 F2 90.0 9_655 . ? F3 Si1 F2 90.0 . . ? F1 Si1 F2 90.0 . . ? F1 Si1 F2 90.0 9_655 . ? F2 Si1 F2 180.0 9_655 . ? F5 Si2 F5 179.71(12) 2 . ? F5 Si2 F5 90.0 2 4 ? F5 Si2 F5 90.0 . 4 ? F5 Si2 F5 90.0 2 3 ? F5 Si2 F5 90.0 . 3 ? F5 Si2 F5 179.71(12) 4 3 ? F5 Si2 F4 90.14(6) 2 . ? F5 Si2 F4 90.14(6) . . ? F5 Si2 F4 90.14(6) 4 . ? F5 Si2 F4 90.14(6) 3 . ? F5 Si2 F6 89.86(6) 2 . ? F5 Si2 F6 89.86(6) . . ? F5 Si2 F6 89.86(6) 4 . ? F5 Si2 F6 89.86(6) 3 . ? F4 Si2 F6 180.0 . . ? Si1 F1 Cu1 178.16(13) . . ? C1 N1 N2 120.4(3) . . ? C1 N1 Cu1 124.4(2) . . ? N2 N1 Cu1 114.8(3) . . ? C4 N2 N1 116.4(4) . . ? C5 N3 N4 120.2(3) . . ? C5 N3 Cu1 125.9(2) . 9_655 ? N4 N3 Cu1 113.5(2) . 9_655 ? C8 N4 N3 117.0(4) . . ? N1 C1 C2 124.5(3) . . ? N1 C1 H1 117.8 . . ? C2 C1 H1 117.8 . . ? C3 C2 C1 115.1(4) . . ? C3 C2 C9 122.6(4) . . ? C1 C2 C9 122.3(3) . . ? C4 C3 C2 117.8(4) . . ? C4 C3 H3 121.1 . . ? C2 C3 H3 121.1 . . ? N2 C4 C3 125.8(4) . . ? N2 C4 H4 117.1 . . ? C3 C4 H4 117.1 . . ? N3 C5 C6 124.7(3) . . ? N3 C5 H5 117.6 . . ? C6 C5 H5 117.6 . . ? C7 C6 C5 114.2(4) . . ? C7 C6 C11 123.4(4) . . ? C5 C6 C11 122.3(3) . . ? C8 C7 C6 118.4(4) . . ? C8 C7 H7 120.8 . . ? C6 C7 H7 120.8 . . ? N4 C8 C7 125.4(4) . . ? N4 C8 H8 117.3 . . ? C7 C8 H8 117.3 . . ? C10 C9 C14 118.8(4) . . ? C10 C9 C2 120.8(3) . . ? C14 C9 C2 120.4(4) . . ? C9 C10 C11 121.5(3) . . ? C9 C10 H10 119.3 . . ? C11 C10 H10 119.3 . . ? C12 C11 C10 118.1(4) . . ? C12 C11 C6 120.8(4) . . ? C10 C11 C6 121.1(3) . . ? C13 C12 C11 120.7(4) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C12 C13 C14 121.4(4) . . ? C12 C13 H13 119.3 . . ? C14 C13 H13 119.3 . . ? C13 C14 C9 119.6(4) . . ? C13 C14 H14 120.2 . . ? C9 C14 H14 120.2 . . ? C15 O1 Cu1 131.4(3) . . ? C15 O1 H1O 103.1 . . ? Cu1 O1 H1O 103.8 . . ? O1 C15 H15A 109.3 . . ? O1 C15 H15B 108.1 . . ? H15A C15 H15B 109.5 . . ? O1 C15 H15C 111.0 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? 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 N3 Cu1 N1 C1 -75.2(3) 2_655 . . . ? N1 Cu1 N1 C1 96.4(3) 10 . . . ? F1 Cu1 N1 C1 10.4(3) . . . . ? O1 Cu1 N1 C1 -158.9(3) . . . . ? O1 Cu1 N1 C1 176.1(3) 10 . . . ? N3 Cu1 N1 N2 112.2(3) 2_655 . . . ? N1 Cu1 N1 N2 -76.2(3) 10 . . . ? F1 Cu1 N1 N2 -162.2(2) . . . . ? O1 Cu1 N1 N2 28.5(3) . . . . ? O1 Cu1 N1 N2 3.6(3) 10 . . . ? C1 N1 N2 C4 -0.9(5) . . . . ? Cu1 N1 N2 C4 172.0(3) . . . . ? C5 N3 N4 C8 -0.2(5) . . . . ? Cu1 N3 N4 C8 -173.4(3) 9_655 . . . ? N2 N1 C1 C2 1.7(6) . . . . ? Cu1 N1 C1 C2 -170.5(3) . . . . ? N1 C1 C2 C3 -0.6(6) . . . . ? N1 C1 C2 C9 178.9(3) . . . . ? C1 C2 C3 C4 -1.1(6) . . . . ? C9 C2 C3 C4 179.4(4) . . . . ? N1 N2 C4 C3 -0.9(7) . . . . ? C2 C3 C4 N2 2.0(7) . . . . ? N4 N3 C5 C6 -1.4(5) . . . . ? Cu1 N3 C5 C6 171.0(3) 9_655 . . . ? N3 C5 C6 C7 1.7(5) . . . . ? N3 C5 C6 C11 -178.7(3) . . . . ? C5 C6 C7 C8 -0.6(5) . . . . ? C11 C6 C7 C8 179.9(4) . . . . ? N3 N4 C8 C7 1.3(6) . . . . ? C6 C7 C8 N4 -0.9(7) . . . . ? C3 C2 C9 C10 152.9(4) . . . . ? C1 C2 C9 C10 -26.6(5) . . . . ? C3 C2 C9 C14 -28.1(5) . . . . ? C1 C2 C9 C14 152.4(4) . . . . ? C14 C9 C10 C11 0.8(5) . . . . ? C2 C9 C10 C11 179.9(3) . . . . ? C9 C10 C11 C12 -1.6(5) . . . . ? C9 C10 C11 C6 178.5(3) . . . . ? C7 C6 C11 C12 27.2(5) . . . . ? C5 C6 C11 C12 -152.3(4) . . . . ? C7 C6 C11 C10 -152.8(4) . . . . ? C5 C6 C11 C10 27.6(5) . . . . ? C10 C11 C12 C13 1.6(6) . . . . ? C6 C11 C12 C13 -178.4(4) . . . . ? C11 C12 C13 C14 -0.9(6) . . . . ? C12 C13 C14 C9 0.1(6) . . . . ? C10 C9 C14 C13 -0.1(6) . . . . ? C2 C9 C14 C13 -179.1(4) . . . . ? N3 Cu1 O1 C15 38.3(6) 9_655 . . . ? N3 Cu1 O1 C15 123.0(6) 2_655 . . . ? N1 Cu1 O1 C15 -143.1(6) . . . . ? N1 Cu1 O1 C15 -59.4(6) 10 . . . ? F1 Cu1 O1 C15 177.7(4) . . . . ? O1 Cu1 O1 C15 -10.7(6) 10 . . . ? N3 Cu1 O1 O1 48.96(9) 9_655 . . 10 ? N3 Cu1 O1 O1 133.65(9) 2_655 . . 10 ? N1 Cu1 O1 O1 -132.41(9) . . . 10 ? N1 Cu1 O1 O1 -48.69(9) 10 . . 10 ? F1 Cu1 O1 O1 -171.6(5) . . . 10 ? Cu1 O1 C15 O1 11.9(6) . . . 10 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.33 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.404 _refine_diff_density_min -0.622 _refine_diff_density_rms 0.068 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 63 15 CH3OH 2 0.000 0.000 0.500 190 53 '3 CH3OH' 3 0.000 0.500 0.250 68 18 CH3OH 4 0.000 0.500 0.750 68 18 CH3OH 5 0.500 0.500 0.000 190 53 '3 CH3OH' 6 0.500 0.500 0.500 63 15 CH3OH 7 0.500 1.000 0.250 68 18 CH3OH 8 0.500 1.000 0.750 68 18 CH3OH _platon_squeeze_details ; ; _iucr_refine_instruction_details ; #--------------------------------------------------------- TITL dk18 in I4/m CELL 0.71073 17.2531 17.2531 20.5377 90.000 90.000 90.000 ZERR 4.00 0.0003 0.0003 0.0010 0.000 0.000 0.000 LATT 2 SYMM - X, - Y, Z SYMM - Y, X, Z SYMM Y, - X, Z SFAC C H N O F SI GE CU UNIT 244 240 64 20 48 5.09 2.91 8 MERG 2 OMIT 0 0 2 OMIT 0 2 0 SHEL 0.80 8 EXYZ Si1 Ge1 EXYZ Si2 Ge2 EADP Si1 Ge1 EADP Si2 Ge2 FMAP 2 PLAN 12 SIZE 0.15 0.16 0.32 ACTA BOND BOND $H CONF L.S. 8 TEMP -100.00 WGHT 0.043500 FVAR 1.44371 0.89410 0.37690 CU1 8 0.675801 0.142094 0.000000 10.50000 0.02020 0.02355 = 0.07800 0.00000 0.00000 -0.00232 SI1 6 0.500000 0.000000 0.000000 20.25000 0.01513 0.01623 = 0.01910 0.00000 0.00000 0.00053 GE1 7 0.500000 0.000000 0.000000 -20.25000 0.01513 0.01623 = 0.01910 0.00000 0.00000 0.00053 SI2 6 0.000000 0.000000 0.253675 30.25000 0.01871 0.01871 = 0.01861 0.00000 0.00000 0.00000 GE2 7 0.000000 0.000000 0.253675 -30.25000 0.01871 0.01871 = 0.01861 0.00000 0.00000 0.00000 F1 5 0.574740 0.062706 0.000000 10.50000 0.02006 0.02400 = 0.03659 0.00000 0.00000 -0.00494 F2 5 0.500000 0.000000 0.082492 10.50000 0.02688 0.02805 = 0.02155 0.00000 0.00000 0.00835 F3 5 0.437182 0.074625 0.000000 10.50000 0.02240 0.02383 = 0.02353 0.00000 0.00000 0.00583 F4 5 0.000000 0.000000 0.339132 10.25000 0.04427 0.04427 = 0.01659 0.00000 0.00000 0.00000 F5 5 0.066379 0.077014 0.253459 11.00000 0.03046 0.02549 = 0.03291 -0.00462 -0.00236 -0.00615 F6 5 0.000000 0.000000 0.168073 10.25000 0.02777 0.02777 = 0.01882 0.00000 0.00000 0.00000 N1 3 0.614486 0.205575 0.069300 11.00000 0.03686 0.02017 = 0.08069 -0.01411 -0.02083 0.00023 N2 3 0.639482 0.279305 0.077741 11.00000 0.05538 0.02937 = 0.11164 -0.01837 -0.02471 -0.00356 N3 3 0.277679 -0.068753 0.068824 11.00000 0.02454 0.03251 = 0.06235 0.01587 0.01258 0.00273 N4 3 0.200870 -0.077856 0.077077 11.00000 0.02356 0.06332 = 0.07672 0.02234 0.01566 0.00352 C1 1 0.550246 0.181110 0.098644 11.00000 0.03895 0.03265 = 0.05297 -0.01974 -0.02129 0.00614 AFIX 43 H1 2 0.535436 0.128597 0.092416 11.00000 -1.20000 AFIX 0 C2 1 0.502828 0.227575 0.138189 11.00000 0.05318 0.03360 = 0.04570 -0.01947 -0.02891 0.01694 C3 1 0.527745 0.303255 0.145910 11.00000 0.06708 0.04561 = 0.07148 -0.02848 -0.02747 0.01633 AFIX 43 H3 2 0.498896 0.339234 0.171183 11.00000 -1.20000 AFIX 0 C4 1 0.595780 0.324718 0.115734 11.00000 0.09394 0.02447 = 0.10148 -0.02719 -0.03955 0.00029 AFIX 43 H4 2 0.613207 0.376325 0.122499 11.00000 -1.20000 AFIX 0 C5 1 0.314718 -0.011280 0.098527 11.00000 0.02981 0.03357 = 0.04989 0.01510 0.01811 0.00951 AFIX 43 H5 2 0.369136 -0.007527 0.092218 11.00000 -1.20000 AFIX 0 C6 1 0.279113 0.044586 0.138761 11.00000 0.04216 0.04517 = 0.03978 0.01430 0.01848 0.01786 C7 1 0.200246 0.034038 0.147033 11.00000 0.04946 0.07996 = 0.05749 0.01532 0.02386 0.03155 AFIX 43 H7 2 0.170947 0.068308 0.173585 11.00000 -1.20000 AFIX 0 C8 1 0.165242 -0.027305 0.115865 11.00000 0.02752 0.09258 = 0.07566 0.02994 0.02095 0.01329 AFIX 43 H8 2 0.111195 -0.034144 0.122582 11.00000 -1.20000 AFIX 0 C9 1 0.431321 0.197892 0.168752 11.00000 0.05741 0.04249 = 0.03642 -0.01559 -0.01095 0.02717 C10 1 0.390441 0.136671 0.140932 11.00000 0.05376 0.03843 = 0.02703 -0.00923 0.00012 0.02274 AFIX 43 H10 2 0.408996 0.114023 0.101757 11.00000 -1.20000 AFIX 0 C11 1 0.322835 0.107843 0.169304 11.00000 0.05408 0.04423 = 0.03238 0.00614 0.01386 0.02625 C12 1 0.297933 0.140779 0.227589 11.00000 0.08708 0.07143 = 0.03128 0.00715 0.02646 0.04736 AFIX 43 H12 2 0.252810 0.121245 0.248409 11.00000 -1.20000 AFIX 0 C13 1 0.337860 0.201078 0.255213 11.00000 0.11052 0.08696 = 0.03281 -0.01473 0.00431 0.06098 AFIX 43 H13 2 0.319450 0.223190 0.294652 11.00000 -1.20000 AFIX 0 C14 1 0.403974 0.230210 0.227037 11.00000 0.08894 0.06093 = 0.04185 -0.02191 -0.01881 0.04429 AFIX 43 H14 2 0.430969 0.271964 0.246912 11.00000 -1.20000 AFIX 0 O1 4 0.771599 0.224199 0.032074 10.50000 0.03636 0.05218 = 0.05984 -0.00239 0.01207 -0.01962 AFIX 3 H1O 2 0.747280 0.262149 0.048794 10.50000 -1.50000 AFIX 0 C15 1 0.826160 0.257329 0.000000 10.50000 0.04754 0.06693 = 0.10194 0.00000 0.00000 -0.02942 AFIX 3 H15A 2 0.855530 0.289759 0.028870 10.50000 -1.50000 H15B 2 0.859200 0.217729 -0.017560 10.50000 -1.50000 H15C 2 0.805580 0.288129 -0.034880 10.50000 -1.50000 HKLF 4 REM dk18 in I4/m REM R1 = 0.0458 for 1978 Fo > 4sig(Fo) and 0.0846 for all 3208 data REM 225 parameters refined using 0 restraints END WGHT 0.0429 0.0000 REM Highest difference peak 0.404, deepest hole -0.622, 1-sigma level 0.068 Q1 1 0.8669 0.3046 0.0000 10.50000 0.05 0.40 Q2 1 0.6327 0.1845 0.0428 11.00000 0.05 0.30 Q3 1 0.4591 0.1418 0.0000 10.50000 0.05 0.28 Q4 1 0.5389 0.0009 0.0675 11.00000 0.05 0.26 Q5 1 0.7171 0.1839 0.0271 11.00000 0.05 0.25 Q6 1 0.3603 0.1260 0.1604 11.00000 0.05 0.25 Q7 1 0.6429 0.0991 0.0324 11.00000 0.05 0.25 Q8 1 0.6396 0.1480 0.0704 11.00000 0.05 0.24 ; _database_code_depnum_ccdc_archive 'CCDC 941552' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_(1c) _audit_creation_method SHELXL-97 _chemical_name_systematic ; \m-Hexafluorosilicato-tetrakis[\m-1,3-bis(pyridazin-4-yl)benzene- \k^2^N^2^:N^2'^]-dimethanol-dicopper(II) Hexafluorosilicate/Hexafluorostannate(IV) 0.50:0.50, solvate with 3 methanol ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C58 H48 Cu2 F6 N16 O2 Si, F6 Si0.50 Sn0.50, 3(C H4 O)' _chemical_formula_sum 'C61 H60 Cu2 F12 N16 O5 Si1.50 Sn0.50' _chemical_formula_weight 1553.81 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' Sn Sn -0.6537 1.4246 '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 tetragonal _symmetry_space_group_name_H-M 'I 4/m' _space_group_name_Hall '-I 4' _symmetry_Int_Tables_number 87 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 17.2903(3) _cell_length_b 17.2903(3) _cell_length_c 20.5440(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6141.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 15247 _cell_measurement_theta_min 1.54 _cell_measurement_theta_max 26.39 _exptl_crystal_description prism _exptl_crystal_colour blue-green _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.19 _exptl_crystal_density_diffrn 1.680 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3160 _exptl_absorpt_coefficient_mu 1.023 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7768 _exptl_absorpt_correction_T_max 0.8293 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker APEXII area-detector diffractometer' _diffrn_measurement_method '\w scans' _diffrn_standards_decay_% 0 _diffrn_reflns_number 15247 _diffrn_reflns_av_R_equivalents 0.0511 _diffrn_reflns_av_sigmaI/netI 0.0471 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 26.39 _reflns_number_total 3236 _reflns_number_gt 2078 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT (Bruker, 1998)' _computing_cell_refinement 'SAINT-NT (Bruker, 1999)' _computing_data_reduction 'SAINT-NT (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Diamond 2.1e (Brandenburg, 1999)' _computing_publication_material 'WinGX 1.70.01 (Farrugia, 1999)' #------------------------------- Refinement data-----------------------# _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. Cu1 atom lies on a mirror plane and the Si1 atom and "Si2/Sn2" mixed atom are at sites with crystallographically-imposed 2/m and 4-fold symmetry, respectively. In the framework of complex cation, [{SiF6}Cu2(L)4(CH3OH)2]2+, the methanol ligands are equally disordered by symmetry, in such a way that the C-atom is common for two components and two components of the disordered O-atom appear to be separated by ca. 1.25 A. The refined C-O distances were reasonable (although certainly shortened due to the disorder) and therefore no geometry restraints were applied. All atoms of cationic residue, including methanol ligand, were refined anisotropically. The OH-hydrogen was located and then fixed at d(O-H) = 0.85 A and with Uiso = 1.5Ueq(O). The aromatic CH-atoms were added geometrically [Uiso = 1.2Ueq(C)] and two sets of the methyl CH-atoms were added [Uiso = 1.5Ueq(C)] with partial contributions of 0.5 and considering two orientations of methanol O-atoms. Three unique solvate methanol molecules reside across symmetry elements and are disordered by symmetry over multiple positions. It was impossible to resolve the disordering schemes and therefore the corresponding electron density was modelled using a Squeeze routine implemented in Platon. The position of outer-sphere hexafluoroanion reveals isomorphic substitution of hexafluorosilicate and hexafluorostannate. This was clearly indicated at the early stages by refinement of isotropic thermal parameters, and, therefore, in the subsequent refinements, the position of corresponding central atom of the hexafluoroanion was treated as "mixed Si/Sn atom", under common constraints for the positional (EXYZ) and thermal parameters (EADP) of the mixed atom and with the partial contributions set as an additional free variable. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0779P)^2^+2.1511P] 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 constr _refine_ls_extinction_method none _refine_ls_number_reflns 3236 _refine_ls_number_parameters 224 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0803 _refine_ls_R_factor_gt 0.0500 _refine_ls_wR_factor_ref 0.1513 _refine_ls_wR_factor_gt 0.1363 _refine_ls_goodness_of_fit_ref 1.143 _refine_ls_restrained_S_all 1.143 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.64233(4) 0.17438(3) 0.0000 0.0427(3) Uani 1 2 d S . . Si1 Si 0.5000 0.0000 0.0000 0.0192(4) Uani 1 4 d S . . F1 F 0.56227(14) 0.07447(14) 0.0000 0.0276(6) Uani 1 2 d S . . F2 F 0.5000 0.0000 0.08166(13) 0.0270(6) Uani 1 2 d S . . F3 F 0.42614(14) 0.06233(14) 0.0000 0.0252(6) Uani 1 2 d S . . Si2 Si 0.0000 0.0000 0.24762(4) 0.0257(3) Uani 0.496(3) 4 d SP . . Sn2 Sn 0.0000 0.0000 0.24762(4) 0.0257(3) Uani 0.504(3) 4 d SP . . F4 F 0.07892(13) 0.06882(12) 0.24745(9) 0.0381(5) Uani 1 1 d . . . F5 F 0.0000 0.0000 0.3353(2) 0.0337(10) Uani 1 4 d S . . F6 F 0.0000 0.0000 0.1594(2) 0.0422(11) Uani 1 4 d S . . N1 N 0.56955(18) 0.22176(17) 0.06898(18) 0.0416(9) Uani 1 1 d . . . N2 N 0.5778(2) 0.29780(18) 0.0769(2) 0.0551(10) Uani 1 1 d . . . N3 N 0.29450(18) -0.11297(18) 0.06946(19) 0.0467(9) Uani 1 1 d . . . N4 N 0.2214(2) -0.1370(2) 0.0786(2) 0.0642(12) Uani 1 1 d . . . C1 C 0.5125(2) 0.1855(2) 0.0986(2) 0.0433(11) Uani 1 1 d . . . H1 H 0.5091 0.1310 0.0928 0.052 Uiso 1 1 calc R . . C2 C 0.4565(2) 0.2205(2) 0.1377(2) 0.0465(11) Uani 1 1 d . . . C3 C 0.4680(3) 0.3001(3) 0.1453(2) 0.0599(14) Uani 1 1 d . . . H3 H 0.4340 0.3301 0.1714 0.072 Uiso 1 1 calc R . . C4 C 0.5289(3) 0.3336(3) 0.1147(3) 0.0665(15) Uani 1 1 d . . . H4 H 0.5365 0.3874 0.1213 0.080 Uiso 1 1 calc R . . C5 C 0.3189(2) -0.0497(2) 0.0982(2) 0.0419(10) Uani 1 1 d . . . H5 H 0.3713 -0.0351 0.0916 0.050 Uiso 1 1 calc R . . C6 C 0.2728(2) -0.0018(3) 0.1382(2) 0.0461(11) Uani 1 1 d . . . C7 C 0.1980(2) -0.0268(3) 0.1469(2) 0.0598(13) Uani 1 1 d . . . H7 H 0.1623 0.0007 0.1734 0.072 Uiso 1 1 calc R . . C8 C 0.1772(3) -0.0946(4) 0.1149(3) 0.0782(18) Uani 1 1 d . . . H8 H 0.1254 -0.1116 0.1202 0.094 Uiso 1 1 calc R . . C9 C 0.3927(2) 0.1770(3) 0.1688(2) 0.0459(11) Uani 1 1 d . . . C10 C 0.3643(2) 0.1093(2) 0.14056(19) 0.0415(10) Uani 1 1 d . . . H10 H 0.3870 0.0903 0.1016 0.050 Uiso 1 1 calc R . . C11 C 0.3033(2) 0.0696(3) 0.1688(2) 0.0460(11) Uani 1 1 d . . . C12 C 0.2725(3) 0.0981(3) 0.2273(2) 0.0652(16) Uani 1 1 d . . . H12 H 0.2311 0.0713 0.2477 0.078 Uiso 1 1 calc R . . C13 C 0.3010(4) 0.1633(4) 0.2550(2) 0.0777(19) Uani 1 1 d . . . H13 H 0.2793 0.1817 0.2946 0.093 Uiso 1 1 calc R . . C14 C 0.3600(3) 0.2024(3) 0.2269(2) 0.0649(15) Uani 1 1 d . . . H14 H 0.3794 0.2478 0.2471 0.078 Uiso 1 1 calc R . . O1 O 0.7268(3) 0.2689(3) 0.0303(3) 0.0528(15) Uani 0.50 1 d P . . H1O H 0.7038 0.2909 0.0618 0.079 Uiso 0.50 1 d PR . . C15 C 0.7582(4) 0.3249(4) 0.0000 0.084(3) Uani 1 2 d S . . H15A H 0.7902 0.3536 0.0295 0.125 Uiso 0.50 1 d PR . . H15B H 0.7895 0.3045 -0.0346 0.125 Uiso 0.50 1 d PR . . H15C H 0.7193 0.3583 -0.0179 0.125 Uiso 0.50 1 d PR . . 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 0.0254(4) 0.0219(4) 0.0807(6) 0.000 0.000 -0.0027(3) Si1 0.0212(9) 0.0162(9) 0.0203(9) 0.000 0.000 0.0009(7) F1 0.0246(14) 0.0207(14) 0.0375(16) 0.000 0.000 -0.0044(11) F2 0.0298(15) 0.0252(14) 0.0260(14) 0.000 0.000 0.0082(11) F3 0.0231(14) 0.0237(14) 0.0288(15) 0.000 0.000 0.0057(11) Si2 0.0239(3) 0.0239(3) 0.0292(5) 0.000 0.000 0.000 Sn2 0.0239(3) 0.0239(3) 0.0292(5) 0.000 0.000 0.000 F4 0.0369(12) 0.0436(13) 0.0339(12) 0.0026(10) 0.0072(9) 0.0050(10) F5 0.0245(12) 0.0245(12) 0.052(3) 0.000 0.000 0.000 F6 0.0444(16) 0.0444(16) 0.038(2) 0.000 0.000 0.000 N1 0.0331(18) 0.0232(16) 0.069(2) -0.0099(16) -0.0160(17) 0.0035(13) N2 0.060(2) 0.0232(18) 0.082(3) -0.0160(18) -0.014(2) 0.0041(16) N3 0.0277(18) 0.0335(19) 0.079(3) 0.0204(18) 0.0150(17) 0.0015(14) N4 0.032(2) 0.062(3) 0.099(3) 0.021(2) 0.019(2) -0.0052(18) C1 0.042(2) 0.032(2) 0.056(3) -0.020(2) -0.017(2) 0.0097(19) C2 0.046(3) 0.049(3) 0.044(2) -0.024(2) -0.017(2) 0.020(2) C3 0.077(4) 0.041(3) 0.062(3) -0.023(2) -0.013(3) 0.032(3) C4 0.088(4) 0.029(2) 0.083(4) -0.020(3) -0.021(3) 0.009(3) C5 0.030(2) 0.037(2) 0.059(3) 0.023(2) 0.0169(19) 0.0069(18) C6 0.036(2) 0.058(3) 0.044(2) 0.024(2) 0.0198(19) 0.016(2) C7 0.038(3) 0.075(4) 0.066(3) 0.021(3) 0.023(2) 0.016(2) C8 0.024(2) 0.099(5) 0.112(5) 0.029(4) 0.028(3) 0.000(3) C9 0.049(3) 0.054(3) 0.034(2) -0.010(2) -0.005(2) 0.028(2) C10 0.041(2) 0.048(2) 0.035(2) -0.001(2) 0.0098(19) 0.0205(19) C11 0.041(2) 0.056(3) 0.042(2) 0.012(2) 0.014(2) 0.020(2) C12 0.055(3) 0.097(4) 0.043(3) 0.028(3) 0.023(2) 0.043(3) C13 0.087(4) 0.111(5) 0.035(3) -0.006(3) 0.013(3) 0.061(4) C14 0.075(4) 0.082(4) 0.037(2) -0.016(3) -0.001(3) 0.044(3) O1 0.058(4) 0.037(3) 0.063(4) 0.008(3) 0.007(3) -0.021(3) C15 0.065(5) 0.066(5) 0.119(7) 0.000 0.000 -0.032(4) _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 N1 2.065(3) 10 ? Cu1 N1 2.065(3) . ? Cu1 N3 2.087(4) 9_655 ? Cu1 N3 2.087(4) 2_655 ? Cu1 F1 2.214(2) . ? Cu1 O1 2.278(5) 10 ? Cu1 O1 2.278(5) . ? Si1 F3 1.671(2) . ? Si1 F3 1.671(2) 9_655 ? Si1 F2 1.678(3) . ? Si1 F2 1.678(3) 9_655 ? Si1 F1 1.678(2) . ? Si1 F1 1.678(2) 9_655 ? Si2 F5 1.801(4) . ? Si2 F4 1.811(2) . ? Si2 F4 1.811(2) 4 ? Si2 F4 1.811(2) 2 ? Si2 F4 1.811(2) 3 ? Si2 F6 1.813(4) . ? N1 C1 1.318(5) . ? N1 N2 1.332(4) . ? N2 C4 1.305(6) . ? N3 C5 1.312(5) . ? N3 N4 1.343(4) . ? N3 Cu1 2.087(4) 9_655 ? N4 C8 1.295(7) . ? C1 C2 1.396(6) . ? C1 H1 0.9500 . ? C2 C3 1.399(6) . ? C2 C9 1.480(6) . ? C3 C4 1.356(7) . ? C3 H3 0.9500 . ? C4 H4 0.9500 . ? C5 C6 1.413(5) . ? C5 H5 0.9500 . ? C6 C7 1.376(6) . ? C6 C11 1.482(6) . ? C7 C8 1.391(7) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C14 1.391(6) . ? C9 C10 1.396(6) . ? C10 C11 1.386(6) . ? C10 H10 0.9500 . ? C11 C12 1.403(6) . ? C12 C13 1.356(8) . ? C12 H12 0.9500 . ? C13 C14 1.354(8) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? O1 C15 1.273(7) . ? O1 H1O 0.8500 . ? C15 O1 1.273(7) 10 ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? 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 N1 Cu1 N1 86.69(18) 10 . ? N1 Cu1 N3 92.96(14) 10 9_655 ? N1 Cu1 N3 171.89(12) . 9_655 ? N1 Cu1 N3 171.89(12) 10 2_655 ? N1 Cu1 N3 92.96(14) . 2_655 ? N3 Cu1 N3 86.26(19) 9_655 2_655 ? N1 Cu1 F1 85.90(10) 10 . ? N1 Cu1 F1 85.90(10) . . ? N3 Cu1 F1 86.00(10) 9_655 . ? N3 Cu1 F1 86.00(10) 2_655 . ? N1 Cu1 O1 85.33(17) 10 10 ? N1 Cu1 O1 107.10(17) . 10 ? N3 Cu1 O1 80.93(17) 9_655 10 ? N3 Cu1 O1 102.49(18) 2_655 10 ? F1 Cu1 O1 163.83(14) . 10 ? N1 Cu1 O1 107.10(17) 10 . ? N1 Cu1 O1 85.33(17) . . ? N3 Cu1 O1 102.49(18) 9_655 . ? N3 Cu1 O1 80.93(17) 2_655 . ? F1 Cu1 O1 163.83(14) . . ? F3 Si1 F3 180.0 . 9_655 ? F3 Si1 F2 90.0 . . ? F3 Si1 F2 90.0 9_655 . ? F3 Si1 F2 90.0 . 9_655 ? F3 Si1 F2 90.0 9_655 9_655 ? F2 Si1 F2 180.0 . 9_655 ? F3 Si1 F1 89.75(12) . . ? F3 Si1 F1 90.25(12) 9_655 . ? F2 Si1 F1 90.0 . . ? F2 Si1 F1 90.0 9_655 . ? F3 Si1 F1 90.25(12) . 9_655 ? F3 Si1 F1 89.75(12) 9_655 9_655 ? F2 Si1 F1 90.0 . 9_655 ? F2 Si1 F1 90.0 9_655 9_655 ? F1 Si1 F1 180.0 . 9_655 ? Si1 F1 Cu1 178.80(15) . . ? F5 Si2 F4 90.10(6) . . ? F5 Si2 F4 90.10(6) . 4 ? F4 Si2 F4 90.0 . 4 ? F5 Si2 F4 90.11(6) . 2 ? F4 Si2 F4 179.79(13) . 2 ? F4 Si2 F4 90.0 4 2 ? F5 Si2 F4 90.10(6) . 3 ? F4 Si2 F4 90.0 . 3 ? F4 Si2 F4 179.79(13) 4 3 ? F4 Si2 F4 90.0 2 3 ? F5 Si2 F6 180.0 . . ? F4 Si2 F6 89.90(6) . . ? F4 Si2 F6 89.90(6) 4 . ? F4 Si2 F6 89.89(6) 2 . ? F4 Si2 F6 89.90(6) 3 . ? C1 N1 N2 119.6(4) . . ? C1 N1 Cu1 125.7(3) . . ? N2 N1 Cu1 114.2(3) . . ? C4 N2 N1 118.1(4) . . ? C5 N3 N4 119.8(4) . . ? C5 N3 Cu1 124.3(2) . 9_655 ? N4 N3 Cu1 115.5(3) . 9_655 ? C8 N4 N3 117.4(4) . . ? N1 C1 C2 125.3(4) . . ? N1 C1 H1 117.4 . . ? C2 C1 H1 117.4 . . ? C1 C2 C3 113.1(4) . . ? C1 C2 C9 123.0(4) . . ? C3 C2 C9 123.9(4) . . ? C4 C3 C2 118.6(4) . . ? C4 C3 H3 120.7 . . ? C2 C3 H3 120.7 . . ? N2 C4 C3 125.2(4) . . ? N2 C4 H4 117.4 . . ? C3 C4 H4 117.4 . . ? N3 C5 C6 124.7(4) . . ? N3 C5 H5 117.7 . . ? C6 C5 H5 117.7 . . ? C7 C6 C5 114.9(5) . . ? C7 C6 C11 122.7(4) . . ? C5 C6 C11 122.3(4) . . ? C6 C7 C8 116.4(4) . . ? C6 C7 H7 121.8 . . ? C8 C7 H7 121.8 . . ? N4 C8 C7 126.7(4) . . ? N4 C8 H8 116.7 . . ? C7 C8 H8 116.7 . . ? C14 C9 C10 118.5(5) . . ? C14 C9 C2 120.9(4) . . ? C10 C9 C2 120.6(4) . . ? C11 C10 C9 120.7(4) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C10 C11 C12 118.2(5) . . ? C10 C11 C6 120.4(4) . . ? C12 C11 C6 121.4(4) . . ? C13 C12 C11 120.9(5) . . ? C13 C12 H12 119.5 . . ? C11 C12 H12 119.5 . . ? C14 C13 C12 120.6(5) . . ? C14 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? C13 C14 C9 121.1(5) . . ? C13 C14 H14 119.5 . . ? C9 C14 H14 119.5 . . ? C15 O1 Cu1 133.2(4) . . ? C15 O1 H1O 103.3 . . ? Cu1 O1 H1O 103.3 . . ? O1 C15 H15A 109.3 . . ? O1 C15 H15B 108.8 . . ? H15A C15 H15B 109.5 . . ? O1 C15 H15C 110.3 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? 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 N1 Cu1 N1 C1 95.9(3) 10 . . . ? N3 Cu1 N1 C1 -76.0(3) 2_655 . . . ? F1 Cu1 N1 C1 9.7(3) . . . . ? O1 Cu1 N1 C1 179.9(3) 10 . . . ? O1 Cu1 N1 C1 -156.7(4) . . . . ? N1 Cu1 N1 N2 -76.1(3) 10 . . . ? N3 Cu1 N1 N2 112.0(3) 2_655 . . . ? F1 Cu1 N1 N2 -162.2(3) . . . . ? O1 Cu1 N1 N2 8.0(3) 10 . . . ? O1 Cu1 N1 N2 31.4(3) . . . . ? C1 N1 N2 C4 0.8(6) . . . . ? Cu1 N1 N2 C4 173.3(3) . . . . ? C5 N3 N4 C8 1.5(6) . . . . ? Cu1 N3 N4 C8 -171.4(4) 9_655 . . . ? N2 N1 C1 C2 1.6(6) . . . . ? Cu1 N1 C1 C2 -169.9(3) . . . . ? N1 C1 C2 C3 -2.3(6) . . . . ? N1 C1 C2 C9 178.8(4) . . . . ? C1 C2 C3 C4 0.8(6) . . . . ? C9 C2 C3 C4 179.6(4) . . . . ? N1 N2 C4 C3 -2.4(7) . . . . ? C2 C3 C4 N2 1.5(8) . . . . ? N4 N3 C5 C6 -1.6(6) . . . . ? Cu1 N3 C5 C6 170.6(3) 9_655 . . . ? N3 C5 C6 C7 1.3(6) . . . . ? N3 C5 C6 C11 -179.3(4) . . . . ? C5 C6 C7 C8 -0.9(6) . . . . ? C11 C6 C7 C8 179.7(4) . . . . ? N3 N4 C8 C7 -1.3(8) . . . . ? C6 C7 C8 N4 1.1(8) . . . . ? C1 C2 C9 C14 151.6(4) . . . . ? C3 C2 C9 C14 -27.2(6) . . . . ? C1 C2 C9 C10 -28.1(6) . . . . ? C3 C2 C9 C10 153.2(4) . . . . ? C14 C9 C10 C11 1.9(6) . . . . ? C2 C9 C10 C11 -178.4(4) . . . . ? C9 C10 C11 C12 -1.7(6) . . . . ? C9 C10 C11 C6 179.3(3) . . . . ? C7 C6 C11 C10 -154.1(4) . . . . ? C5 C6 C11 C10 26.6(6) . . . . ? C7 C6 C11 C12 27.0(6) . . . . ? C5 C6 C11 C12 -152.4(4) . . . . ? C10 C11 C12 C13 0.8(6) . . . . ? C6 C11 C12 C13 179.8(4) . . . . ? C11 C12 C13 C14 -0.1(7) . . . . ? C12 C13 C14 C9 0.3(8) . . . . ? C10 C9 C14 C13 -1.2(7) . . . . ? C2 C9 C14 C13 179.1(4) . . . . ? N1 Cu1 O1 O1 -48.77(10) 10 . . 10 ? N1 Cu1 O1 O1 -133.84(10) . . . 10 ? N3 Cu1 O1 O1 48.32(10) 9_655 . . 10 ? N3 Cu1 O1 O1 132.40(11) 2_655 . . 10 ? F1 Cu1 O1 O1 168.8(6) . . . 10 ? N1 Cu1 O1 C15 -33.7(8) 10 . . . ? N1 Cu1 O1 C15 -118.8(7) . . . . ? N3 Cu1 O1 C15 63.4(8) 9_655 . . . ? N3 Cu1 O1 C15 147.5(8) 2_655 . . . ? F1 Cu1 O1 C15 -176.1(6) . . . . ? O1 Cu1 O1 C15 15.1(8) 10 . . . ? Cu1 O1 C15 O1 -16.7(9) . . . 10 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.39 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.996 _refine_diff_density_min -0.517 _refine_diff_density_rms 0.091 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 192 56 '3 CH3OH' 2 0.000 0.000 0.500 67 16 CH3OH 3 0.000 0.500 0.250 69 18 CH3OH 4 0.000 0.500 0.750 69 18 CH3OH 5 0.500 0.500 0.500 192 56 '3 CH3OH' 6 0.500 0.500 0.000 67 16 CH3OH 7 0.500 0.000 0.250 69 18 CH3OH 8 0.500 0.000 0.750 69 18 CH3OH _platon_squeeze_details ; ; _iucr_refine_instruction_details ; #--------------------------------------------------------- TITL dk19 in I4/m CELL 0.71073 17.2903 17.2903 20.5440 90.000 90.000 90.000 ZERR 4.00 0.0003 0.0003 0.0010 0.000 0.000 0.000 LATT 2 SYMM - X, - Y, Z SYMM - Y, X, Z SYMM Y, - X, Z SFAC C H N O F SI SN CU UNIT 244 240 64 20 48 6 2 8 MERG 2 OMIT 0.00 180.00 OMIT -1 5 2 OMIT -1 3 6 OMIT 1 3 6 OMIT 1 3 4 OMIT 2 2 2 EADP SI2 SN2 EXYZ SI2 SN2 FMAP 2 PLAN 20 SIZE 0.19 0.20 0.26 ACTA BOND BOND $H CONF L.S. 6 TEMP -100.00 WGHT 0.077900 2.151100 FVAR 0.68701 0.49628 CU1 8 0.642332 0.174384 0.000000 10.50000 0.02535 0.02193 = 0.08071 0.00000 0.00000 -0.00269 SI1 6 0.500000 0.000000 0.000000 10.25000 0.02122 0.01620 = 0.02031 0.00000 0.00000 0.00091 F1 5 0.562275 0.074467 0.000000 10.50000 0.02464 0.02071 = 0.03747 0.00000 0.00000 -0.00439 F2 5 0.500000 0.000000 0.081664 10.50000 0.02977 0.02522 = 0.02604 0.00000 0.00000 0.00818 F3 5 0.426137 0.062327 0.000000 10.50000 0.02314 0.02372 = 0.02875 0.00000 0.00000 0.00572 SI2 6 0.000000 0.000000 0.247615 20.25000 0.02392 0.02392 = 0.02917 0.00000 0.00000 0.00000 SN2 7 0.000000 0.000000 0.247615 -20.25000 0.02392 0.02392 = 0.02917 0.00000 0.00000 0.00000 F4 5 0.078922 0.068825 0.247454 11.00000 0.03685 0.04357 = 0.03386 0.00258 0.00716 0.00502 F5 5 0.000000 0.000000 0.335261 10.25000 0.02451 0.02451 = 0.05204 0.00000 0.00000 0.00000 F6 5 0.000000 0.000000 0.159373 10.25000 0.04436 0.04436 = 0.03797 0.00000 0.00000 0.00000 N1 3 0.569554 0.221759 0.068975 11.00000 0.03311 0.02318 = 0.06852 -0.00988 -0.01596 0.00351 N2 3 0.577804 0.297801 0.076871 11.00000 0.05995 0.02318 = 0.08205 -0.01596 -0.01406 0.00410 N3 3 0.294498 -0.112969 0.069455 11.00000 0.02766 0.03346 = 0.07894 0.02036 0.01498 0.00153 N4 3 0.221445 -0.136967 0.078565 11.00000 0.03226 0.06168 = 0.09861 0.02103 0.01890 -0.00523 C1 1 0.512453 0.185452 0.098561 11.00000 0.04204 0.03167 = 0.05628 -0.02043 -0.01675 0.00965 AFIX 43 H1 2 0.509086 0.131045 0.092768 11.00000 -1.20000 AFIX 0 C2 1 0.456522 0.220516 0.137725 11.00000 0.04618 0.04891 = 0.04429 -0.02427 -0.01664 0.01960 C3 1 0.468044 0.300110 0.145334 11.00000 0.07670 0.04124 = 0.06180 -0.02266 -0.01333 0.03231 AFIX 43 H3 2 0.433955 0.330050 0.171415 11.00000 -1.20000 AFIX 0 C4 1 0.528885 0.333591 0.114697 11.00000 0.08755 0.02856 = 0.08331 -0.02008 -0.02092 0.00863 AFIX 43 H4 2 0.536512 0.387434 0.121300 11.00000 -1.20000 AFIX 0 C5 1 0.318888 -0.049744 0.098181 11.00000 0.02957 0.03735 = 0.05881 0.02272 0.01686 0.00692 AFIX 43 H5 2 0.371284 -0.035150 0.091635 11.00000 -1.20000 AFIX 0 C6 1 0.272792 -0.001787 0.138171 11.00000 0.03637 0.05797 = 0.04399 0.02417 0.01985 0.01608 C7 1 0.197951 -0.026819 0.146928 11.00000 0.03813 0.07537 = 0.06605 0.02150 0.02278 0.01574 AFIX 43 H7 2 0.162340 0.000727 0.173434 11.00000 -1.20000 AFIX 0 C8 1 0.177234 -0.094603 0.114898 11.00000 0.02385 0.09896 = 0.11172 0.02879 0.02780 -0.00019 AFIX 43 H8 2 0.125355 -0.111562 0.120211 11.00000 -1.20000 AFIX 0 C9 1 0.392735 0.177046 0.168807 11.00000 0.04949 0.05441 = 0.03377 -0.00981 -0.00480 0.02753 C10 1 0.364308 0.109326 0.140555 11.00000 0.04114 0.04804 = 0.03531 -0.00057 0.00979 0.02047 AFIX 43 H10 2 0.387005 0.090306 0.101604 11.00000 -1.20000 AFIX 0 C11 1 0.303288 0.069567 0.168783 11.00000 0.04068 0.05568 = 0.04168 0.01159 0.01373 0.02042 C12 1 0.272470 0.098069 0.227253 11.00000 0.05545 0.09725 = 0.04302 0.02757 0.02277 0.04279 AFIX 43 H12 2 0.231064 0.071312 0.247669 11.00000 -1.20000 AFIX 0 C13 1 0.300975 0.163286 0.255021 11.00000 0.08703 0.11107 = 0.03508 -0.00638 0.01316 0.06078 AFIX 43 H13 2 0.279314 0.181712 0.294588 11.00000 -1.20000 AFIX 0 C14 1 0.360021 0.202371 0.226865 11.00000 0.07510 0.08242 = 0.03726 -0.01635 -0.00135 0.04370 AFIX 43 H14 2 0.379411 0.247816 0.247092 11.00000 -1.20000 AFIX 0 O1 4 0.726804 0.268856 0.030331 10.50000 0.05824 0.03701 = 0.06317 0.00822 0.00721 -0.02056 AFIX 3 H1O 2 0.703834 0.290946 0.061831 10.50000 -1.50000 AFIX 0 C15 1 0.758189 0.324884 0.000000 10.50000 0.06546 0.06558 = 0.11947 0.00000 0.00000 -0.03187 AFIX 3 H15A 2 0.790179 0.353644 0.029540 10.50000 -1.50000 H15B 2 0.789479 0.304504 -0.034580 10.50000 -1.50000 H15C 2 0.719269 0.358314 -0.017850 10.50000 -1.50000 HKLF 4 REM dk19 in I4/m REM R1 = 0.0500 for 2078 Fo > 4sig(Fo) and 0.0803 for all 3236 data REM 224 parameters refined using 0 restraints END WGHT 0.0815 0.9503 REM Highest difference peak 0.996, deepest hole -0.517, 1-sigma level 0.091 Q1 1 0.8548 0.3353 0.0000 10.50000 0.05 0.84 Q2 1 0.3548 0.3272 0.2543 11.00000 0.05 0.55 Q3 1 0.3217 0.0296 0.2572 11.00000 0.05 0.52 Q4 1 0.1744 -0.0937 0.1320 11.00000 0.05 0.48 Q5 1 0.0478 0.0347 0.2197 11.00000 0.05 0.44 Q6 1 0.0482 0.0374 0.2703 11.00000 0.05 0.42 Q7 1 0.8026 0.3649 0.0000 10.50000 0.05 0.37 Q8 1 0.6545 0.2451 0.0000 10.50000 0.05 0.37 ; _database_code_depnum_ccdc_archive 'CCDC 941553' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_(1d) _audit_creation_method SHELXL-97 _chemical_name_systematic ; \m-[Hexafluorosilicato-tetrakis[\m-1,3-bis(pyridazin-4-yl)benzene- \k^2^N^2^:N^2'^]-dimethanol-dicopper(II) Hexafluorosilicate/Hexafluorostannate(IV) 0.21:0.79, solvate with 3 methanol ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C58 H48 Cu2 F6 N16 O2 Si, F6 Si0.21 Sn0.79, 3(C H4 O)' _chemical_formula_sum 'C61 H60 Cu2 F12 N16 O5 Si1.21 Sn0.79' _chemical_formula_weight 1580.08 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' Sn Sn -0.6537 1.4246 '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 tetragonal _symmetry_space_group_name_H-M 'I 4/m' _space_group_name_Hall '-I 4' _symmetry_Int_Tables_number 87 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 17.3756(4) _cell_length_b 17.3756(4) _cell_length_c 20.5964(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6218.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 17174 _cell_measurement_theta_min 1.53 _cell_measurement_theta_max 27.71 _exptl_crystal_description prism _exptl_crystal_colour blue-green _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.21 _exptl_crystal_density_diffrn 1.688 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3202 _exptl_absorpt_coefficient_mu 1.119 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7596 _exptl_absorpt_correction_T_max 0.7990 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker APEXII area-detector diffractometer' _diffrn_measurement_method '\w scans' _diffrn_standards_decay_% 0 _diffrn_reflns_number 17174 _diffrn_reflns_av_R_equivalents 0.0410 _diffrn_reflns_av_sigmaI/netI 0.0353 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 27.71 _reflns_number_total 3744 _reflns_number_gt 2894 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT (Bruker, 1998)' _computing_cell_refinement 'SAINT-NT (Bruker, 1999)' _computing_data_reduction 'SAINT-NT (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Diamond 2.1e (Brandenburg, 1999)' _computing_publication_material 'WinGX 1.70.01 (Farrugia, 1999)' #------------------------------- Refinement data-----------------------# _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. Cu1 atom lies on a mirror plane and the Si1 atom and "Si2/Sn2" mixed atom are at sites with crystallographically-imposed 2/m and 4-fold symmetry, respectively. In the framework of complex cation, [{SiF6}Cu2(L)4(CH3OH)2]2+, the methanol ligands are equally disordered by symmetry, in such a way that the C-atom is common for two components and two components of the disordered O-atom appear to be separated by ca. 1.25 A. The refined C-O distances were reasonable (although certainly shortened due to the disorder) and therefore no geometry restraints were applied. All atoms of cationic residue, including methanol ligand, were refined anisotropically. The OH-hydrogen was located and then fixed at d(O-H) = 0.85 A and with Uiso = 1.5Ueq(O). The aromatic CH-atoms were added geometrically [Uiso = 1.2Ueq(C)] and two sets of the methyl CH-atoms were added [Uiso = 1.5Ueq(C)] with partial contributions of 0.5 and considering two orientations of methanol O-atoms. Three unique solvate methanol molecules reside across symmetry elements and are disordered by symmetry over multiple positions. It was impossible to resolve the disordering schemes and therefore the corresponding electron density was modelled using a Squeeze routine implemented in Platon. The position of outer-sphere hexafluoroanion reveals isomorphic substitution of hexafluorosilicate and hexafluorostannate. This was clearly indicated at the early stages by refinement of isotropic thermal parameters, and, therefore, in the subsequent refinements, the position of corresponding central atom of the hexafluoroanion was treated as "mixed Si/Sn atom", under common constraints for the positional (EXYZ) and thermal parameters (EADP) of the mixed atom and with the partial contributions set as an additional free variable. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0356P)^2^+4.6386P] 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 constr _refine_ls_extinction_method none _refine_ls_number_reflns 3744 _refine_ls_number_parameters 224 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0499 _refine_ls_R_factor_gt 0.0354 _refine_ls_wR_factor_ref 0.0849 _refine_ls_wR_factor_gt 0.0805 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.35781(2) 0.17351(2) 0.0000 0.03561(15) Uani 1 2 d S . . Si1 Si 0.5000 0.0000 0.0000 0.0164(2) Uani 1 4 d S . . F1 F 0.43791(10) 0.07380(9) 0.0000 0.0255(4) Uani 1 2 d S . . F2 F 0.5000 0.0000 0.08176(8) 0.0246(4) Uani 1 2 d S . . F3 F 0.42651(9) -0.06216(10) 0.0000 0.0228(4) Uani 1 2 d S . . Si2 Si 0.0000 0.0000 0.247926(17) 0.01910(12) Uani 0.209(2) 4 d SP . . Sn2 Sn 0.0000 0.0000 0.247926(17) 0.01910(12) Uani 0.791(2) 4 d SP . . F4 F 0.0000 0.0000 0.15575(14) 0.0454(8) Uani 1 4 d S . . F5 F -0.08300(8) 0.07157(8) 0.24798(6) 0.0332(3) Uani 1 1 d . . . F6 F 0.0000 0.0000 0.34017(13) 0.0284(6) Uani 1 4 d S . . N1 N 0.29552(12) 0.11218(12) 0.06956(12) 0.0400(6) Uani 1 1 d . . . N2 N 0.22271(13) 0.13706(15) 0.07925(15) 0.0589(8) Uani 1 1 d . . . N3 N 0.56928(12) -0.22076(11) 0.06876(12) 0.0364(5) Uani 1 1 d . . . N4 N 0.57813(15) -0.29710(12) 0.07607(14) 0.0511(7) Uani 1 1 d . . . C1 C 0.31984(14) 0.04883(15) 0.09825(13) 0.0373(6) Uani 1 1 d . . . H1 H 0.3717 0.0338 0.0912 0.045 Uiso 1 1 calc R . . C2 C 0.27440(15) 0.00190(16) 0.13859(14) 0.0398(7) Uani 1 1 d . . . C3 C 0.20042(17) 0.0272(2) 0.14790(16) 0.0553(8) Uani 1 1 d . . . H3 H 0.1655 -0.0009 0.1743 0.066 Uiso 1 1 calc R . . C4 C 0.17836(18) 0.0944(2) 0.11770(19) 0.0688(11) Uani 1 1 d . . . H4 H 0.1272 0.1118 0.1249 0.083 Uiso 1 1 calc R . . C5 C 0.51227(14) -0.18415(14) 0.09847(13) 0.0351(6) Uani 1 1 d . . . H5 H 0.5089 -0.1300 0.0931 0.042 Uiso 1 1 calc R . . C6 C 0.45672(15) -0.22021(15) 0.13729(13) 0.0382(6) Uani 1 1 d . . . C7 C 0.4673(2) -0.29903(17) 0.14377(16) 0.0568(9) Uani 1 1 d . . . H7 H 0.4328 -0.3288 0.1693 0.068 Uiso 1 1 calc R . . C8 C 0.5284(2) -0.33351(17) 0.11273(18) 0.0603(9) Uani 1 1 d . . . H8 H 0.5349 -0.3874 0.1183 0.072 Uiso 1 1 calc R . . C9 C 0.30475(15) -0.06897(17) 0.16880(13) 0.0410(7) Uani 1 1 d . . . C10 C 0.36495(14) -0.10931(15) 0.14057(12) 0.0354(6) Uani 1 1 d . . . H10 H 0.3872 -0.0905 0.1015 0.042 Uiso 1 1 calc R . . C11 C 0.39363(15) -0.17689(16) 0.16814(13) 0.0410(7) Uani 1 1 d . . . C12 C 0.3608(2) -0.2036(2) 0.22618(15) 0.0567(9) Uani 1 1 d . . . H12 H 0.3797 -0.2493 0.2458 0.068 Uiso 1 1 calc R . . C13 C 0.3021(2) -0.1641(2) 0.25446(15) 0.0694(12) Uani 1 1 d . . . H13 H 0.2806 -0.1825 0.2939 0.083 Uiso 1 1 calc R . . C14 C 0.27330(19) -0.0978(2) 0.22672(15) 0.0569(9) Uani 1 1 d . . . H14 H 0.2318 -0.0715 0.2470 0.068 Uiso 1 1 calc R . . C15 C 0.2424(3) 0.3241(3) 0.0000 0.0788(17) Uani 1 2 d S . . H15A H 0.2108 0.3523 0.0300 0.118 Uiso 0.50 1 d PR . . H15B H 0.2809 0.3577 -0.0177 0.118 Uiso 0.50 1 d PR . . H15C H 0.2110 0.3043 -0.0345 0.118 Uiso 0.50 1 d PR . . O1 O 0.2758(2) 0.2691(2) 0.02938(19) 0.0507(11) Uani 0.50 1 d P . . H1O H 0.2384 0.2449 0.0464 0.076 Uiso 0.50 1 d PR . . 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 0.0238(2) 0.0189(2) 0.0642(3) 0.000 0.000 0.00253(16) Si1 0.0169(5) 0.0139(5) 0.0183(5) 0.000 0.000 -0.0005(4) F1 0.0229(9) 0.0191(9) 0.0345(11) 0.000 0.000 0.0038(7) F2 0.0270(9) 0.0254(9) 0.0213(9) 0.000 0.000 -0.0067(8) F3 0.0224(9) 0.0229(9) 0.0231(10) 0.000 0.000 -0.0067(7) Si2 0.01931(14) 0.01931(14) 0.01867(19) 0.000 0.000 0.000 Sn2 0.01931(14) 0.01931(14) 0.01867(19) 0.000 0.000 0.000 F4 0.0544(12) 0.0544(12) 0.0274(16) 0.000 0.000 0.000 F5 0.0311(7) 0.0346(7) 0.0338(8) 0.0033(6) -0.0072(6) 0.0000(6) F6 0.0239(8) 0.0239(8) 0.0373(16) 0.000 0.000 0.000 N1 0.0253(11) 0.0351(12) 0.0596(16) -0.0184(11) 0.0123(10) -0.0037(9) N2 0.0320(13) 0.0569(16) 0.088(2) -0.0146(15) 0.0140(13) 0.0080(12) N3 0.0363(12) 0.0193(10) 0.0537(14) 0.0094(9) -0.0143(11) -0.0019(9) N4 0.0581(15) 0.0234(11) 0.0718(19) 0.0141(12) -0.0156(14) 0.0001(11) C1 0.0278(13) 0.0347(14) 0.0495(17) -0.0153(12) 0.0154(12) -0.0055(11) C2 0.0322(13) 0.0486(16) 0.0386(15) -0.0191(13) 0.0154(12) -0.0130(12) C3 0.0371(16) 0.071(2) 0.058(2) -0.0133(18) 0.0220(15) -0.0099(15) C4 0.0293(15) 0.089(3) 0.089(3) -0.019(2) 0.0246(17) 0.0004(16) C5 0.0352(13) 0.0266(12) 0.0436(15) 0.0142(12) -0.0110(12) -0.0063(10) C6 0.0431(15) 0.0365(14) 0.0350(15) 0.0146(12) -0.0121(12) -0.0165(12) C7 0.075(2) 0.0393(16) 0.056(2) 0.0238(15) -0.0130(18) -0.0268(16) C8 0.080(2) 0.0282(15) 0.072(2) 0.0188(15) -0.013(2) -0.0086(16) C9 0.0401(15) 0.0527(17) 0.0301(14) -0.0070(13) 0.0100(12) -0.0210(13) C10 0.0378(14) 0.0433(15) 0.0250(13) 0.0021(11) 0.0060(11) -0.0170(12) C11 0.0434(15) 0.0469(16) 0.0328(15) 0.0130(13) -0.0046(12) -0.0238(13) C12 0.061(2) 0.074(2) 0.0350(16) 0.0172(16) -0.0022(16) -0.0341(18) C13 0.080(3) 0.099(3) 0.0289(16) 0.0109(18) 0.0095(17) -0.046(2) C14 0.0532(19) 0.081(2) 0.0360(16) -0.0142(17) 0.0205(15) -0.0311(18) C15 0.069(3) 0.051(3) 0.116(5) 0.000 0.000 0.032(3) O1 0.049(2) 0.042(2) 0.061(3) 0.0095(18) 0.0010(19) 0.0206(18) _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 N3 2.070(2) 2_655 ? Cu1 N3 2.070(2) 9_655 ? Cu1 N1 2.088(2) . ? Cu1 N1 2.088(2) 10 ? Cu1 F1 2.2223(17) . ? Cu1 O1 2.271(3) 10 ? Cu1 O1 2.271(3) . ? Si1 F3 1.6725(16) 9_655 ? Si1 F3 1.6725(16) . ? Si1 F1 1.6758(16) 9_655 ? Si1 F1 1.6758(16) . ? Si1 F2 1.6840(17) . ? Si1 F2 1.6840(17) 9_655 ? Si2 F4 1.898(3) . ? Si2 F6 1.900(3) . ? Si2 F5 1.9043(14) 4 ? Si2 F5 1.9043(14) 2 ? Si2 F5 1.9043(14) . ? Si2 F5 1.9043(14) 3 ? N1 C1 1.319(3) . ? N1 N2 1.352(3) . ? N2 C4 1.331(4) . ? N3 C5 1.327(3) . ? N3 N4 1.344(3) . ? N3 Cu1 2.070(2) 9_655 ? N4 C8 1.311(4) . ? C1 C2 1.407(4) . ? C1 H1 0.9500 . ? C2 C3 1.372(4) . ? C2 C9 1.477(4) . ? C3 C4 1.378(5) . ? C3 H3 0.9500 . ? C4 H4 0.9500 . ? C5 C6 1.401(4) . ? C5 H5 0.9500 . ? C6 C7 1.388(4) . ? C6 C11 1.474(4) . ? C7 C8 1.376(5) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C10 1.387(4) . ? C9 C14 1.405(4) . ? C10 C11 1.396(4) . ? C10 H10 0.9500 . ? C11 C12 1.403(4) . ? C12 C13 1.361(5) . ? C12 H12 0.9500 . ? C13 C14 1.379(5) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 O1 1.271(5) . ? C15 O1 1.271(5) 10 ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? O1 H1O 0.8500 . ? 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 N3 Cu1 N3 86.35(12) 2_655 9_655 ? N3 Cu1 N1 92.88(9) 2_655 . ? N3 Cu1 N1 171.55(8) 9_655 . ? N3 Cu1 N1 171.55(8) 2_655 10 ? N3 Cu1 N1 92.88(9) 9_655 10 ? N1 Cu1 N1 86.65(12) . 10 ? N3 Cu1 F1 85.75(6) 2_655 . ? N3 Cu1 F1 85.75(6) 9_655 . ? N1 Cu1 F1 85.80(7) . . ? N1 Cu1 F1 85.80(7) 10 . ? N3 Cu1 O1 106.05(12) 2_655 10 ? N3 Cu1 O1 84.94(12) 9_655 10 ? N1 Cu1 O1 103.34(12) . 10 ? N1 Cu1 O1 82.25(12) 10 10 ? F1 Cu1 O1 164.44(10) . 10 ? N3 Cu1 O1 84.94(12) 2_655 . ? N3 Cu1 O1 106.05(12) 9_655 . ? N1 Cu1 O1 82.25(12) . . ? N1 Cu1 O1 103.34(12) 10 . ? F1 Cu1 O1 164.44(10) . . ? F3 Si1 F3 180.0 9_655 . ? F3 Si1 F1 90.15(8) 9_655 9_655 ? F3 Si1 F1 89.85(8) . 9_655 ? F3 Si1 F1 89.85(8) 9_655 . ? F3 Si1 F1 90.15(8) . . ? F1 Si1 F1 180.0 9_655 . ? F3 Si1 F2 90.0 9_655 . ? F3 Si1 F2 90.0 . . ? F1 Si1 F2 90.0 9_655 . ? F1 Si1 F2 90.0 . . ? F3 Si1 F2 90.0 9_655 9_655 ? F3 Si1 F2 90.0 . 9_655 ? F1 Si1 F2 90.0 9_655 9_655 ? F1 Si1 F2 90.0 . 9_655 ? F2 Si1 F2 180.0 . 9_655 ? Si1 F1 Cu1 178.70(10) . . ? F4 Si2 F6 180.0 . . ? F4 Si2 F5 90.04(4) . 4 ? F6 Si2 F5 89.96(4) . 4 ? F4 Si2 F5 90.04(4) . 2 ? F6 Si2 F5 89.96(4) . 2 ? F5 Si2 F5 90.0 4 2 ? F4 Si2 F5 90.04(4) . . ? F6 Si2 F5 89.96(4) . . ? F5 Si2 F5 90.0 4 . ? F5 Si2 F5 179.93(8) 2 . ? F4 Si2 F5 90.04(4) . 3 ? F6 Si2 F5 89.96(4) . 3 ? F5 Si2 F5 179.93(9) 4 3 ? F5 Si2 F5 90.0 2 3 ? F5 Si2 F5 90.0 . 3 ? C1 N1 N2 120.0(2) . . ? C1 N1 Cu1 124.56(16) . . ? N2 N1 Cu1 115.0(2) . . ? C4 N2 N1 116.9(3) . . ? C5 N3 N4 120.5(2) . . ? C5 N3 Cu1 125.62(16) . 9_655 ? N4 N3 Cu1 113.45(19) . 9_655 ? C8 N4 N3 117.7(3) . . ? N1 C1 C2 124.7(2) . . ? N1 C1 H1 117.7 . . ? C2 C1 H1 117.7 . . ? C3 C2 C1 115.0(3) . . ? C3 C2 C9 122.8(3) . . ? C1 C2 C9 122.1(2) . . ? C2 C3 C4 118.0(3) . . ? C2 C3 H3 121.0 . . ? C4 C3 H3 121.0 . . ? N2 C4 C3 125.4(3) . . ? N2 C4 H4 117.3 . . ? C3 C4 H4 117.3 . . ? N3 C5 C6 124.3(2) . . ? N3 C5 H5 117.9 . . ? C6 C5 H5 117.9 . . ? C7 C6 C5 113.9(3) . . ? C7 C6 C11 124.1(3) . . ? C5 C6 C11 122.0(2) . . ? C8 C7 C6 119.1(3) . . ? C8 C7 H7 120.4 . . ? C6 C7 H7 120.4 . . ? N4 C8 C7 124.5(3) . . ? N4 C8 H8 117.8 . . ? C7 C8 H8 117.8 . . ? C10 C9 C14 118.0(3) . . ? C10 C9 C2 120.9(2) . . ? C14 C9 C2 121.1(3) . . ? C9 C10 C11 121.6(2) . . ? C9 C10 H10 119.2 . . ? C11 C10 H10 119.2 . . ? C10 C11 C12 118.6(3) . . ? C10 C11 C6 121.3(2) . . ? C12 C11 C6 120.0(3) . . ? C13 C12 C11 120.2(3) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C12 C13 C14 121.0(3) . . ? C12 C13 H13 119.5 . . ? C14 C13 H13 119.5 . . ? C13 C14 C9 120.6(3) . . ? C13 C14 H14 119.7 . . ? C9 C14 H14 119.7 . . ? O1 C15 H15A 109.7 . . ? O1 C15 H15B 108.7 . . ? H15A C15 H15B 109.5 . . ? O1 C15 H15C 110.0 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C15 O1 Cu1 135.2(3) . . ? C15 O1 H1O 102.7 . . ? Cu1 O1 H1O 103.2 . . ? 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 N3 Cu1 N1 C1 -75.9(2) 2_655 . . . ? N1 Cu1 N1 C1 95.6(2) 10 . . . ? F1 Cu1 N1 C1 9.6(2) . . . . ? O1 Cu1 N1 C1 176.8(2) 10 . . . ? O1 Cu1 N1 C1 -160.4(2) . . . . ? N3 Cu1 N1 N2 110.96(19) 2_655 . . . ? N1 Cu1 N1 N2 -77.5(2) 10 . . . ? F1 Cu1 N1 N2 -163.52(19) . . . . ? O1 Cu1 N1 N2 3.7(2) 10 . . . ? O1 Cu1 N1 N2 26.5(2) . . . . ? C1 N1 N2 C4 -0.8(4) . . . . ? Cu1 N1 N2 C4 172.7(2) . . . . ? C5 N3 N4 C8 0.6(4) . . . . ? Cu1 N3 N4 C8 -172.0(2) 9_655 . . . ? N2 N1 C1 C2 1.5(4) . . . . ? Cu1 N1 C1 C2 -171.3(2) . . . . ? N1 C1 C2 C3 -1.1(4) . . . . ? N1 C1 C2 C9 179.3(2) . . . . ? C1 C2 C3 C4 -0.1(4) . . . . ? C9 C2 C3 C4 179.5(3) . . . . ? N1 N2 C4 C3 -0.4(5) . . . . ? C2 C3 C4 N2 0.8(6) . . . . ? N4 N3 C5 C6 -1.8(4) . . . . ? Cu1 N3 C5 C6 169.91(19) 9_655 . . . ? N3 C5 C6 C7 1.6(4) . . . . ? N3 C5 C6 C11 -178.8(2) . . . . ? C5 C6 C7 C8 -0.3(4) . . . . ? C11 C6 C7 C8 -180.0(3) . . . . ? N3 N4 C8 C7 0.6(5) . . . . ? C6 C7 C8 N4 -0.8(5) . . . . ? C3 C2 C9 C10 154.1(3) . . . . ? C1 C2 C9 C10 -26.3(4) . . . . ? C3 C2 C9 C14 -25.5(4) . . . . ? C1 C2 C9 C14 154.1(3) . . . . ? C14 C9 C10 C11 0.4(4) . . . . ? C2 C9 C10 C11 -179.2(2) . . . . ? C9 C10 C11 C12 -0.7(4) . . . . ? C9 C10 C11 C6 178.9(2) . . . . ? C7 C6 C11 C10 -152.0(3) . . . . ? C5 C6 C11 C10 28.3(4) . . . . ? C7 C6 C11 C12 27.6(4) . . . . ? C5 C6 C11 C12 -152.0(3) . . . . ? C10 C11 C12 C13 0.3(4) . . . . ? C6 C11 C12 C13 -179.4(3) . . . . ? C11 C12 C13 C14 0.5(5) . . . . ? C12 C13 C14 C9 -0.8(5) . . . . ? C10 C9 C14 C13 0.3(4) . . . . ? C2 C9 C14 C13 180.0(3) . . . . ? O1 C15 O1 Cu1 12.9(6) 10 . . . ? N3 Cu1 O1 O1 133.49(7) 2_655 . . 10 ? N3 Cu1 O1 O1 48.77(7) 9_655 . . 10 ? N1 Cu1 O1 O1 -132.91(7) . . . 10 ? N1 Cu1 O1 O1 -48.24(7) 10 . . 10 ? F1 Cu1 O1 O1 -173.1(5) . . . 10 ? N3 Cu1 O1 C15 121.7(5) 2_655 . . . ? N3 Cu1 O1 C15 37.0(6) 9_655 . . . ? N1 Cu1 O1 C15 -144.7(5) . . . . ? N1 Cu1 O1 C15 -60.0(6) 10 . . . ? F1 Cu1 O1 C15 175.2(4) . . . . ? O1 Cu1 O1 C15 -11.8(6) 10 . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.71 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.504 _refine_diff_density_min -0.674 _refine_diff_density_rms 0.065 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 207 61 '3 CH3OH' 2 0.000 0.000 0.500 65 17 CH3OH 3 0.000 0.500 0.250 71 19 CH3OH 4 0.000 0.500 0.750 71 19 CH3OH 5 0.500 0.500 0.500 207 61 '3 CH3OH' 6 0.500 0.500 0.000 65 17 CH3OH 7 0.500 0.000 0.250 71 19 CH3OH 8 0.500 0.000 0.750 71 19 CH3OH _platon_squeeze_details ; ; _iucr_refine_instruction_details ; #--------------------------------------------------------- TITL dk21 in I4/m CELL 0.71073 17.3756 17.3756 20.5964 90.000 90.000 90.000 ZERR 4.00 0.0004 0.0004 0.0009 0.000 0.000 0.000 LATT 2 SYMM - X, - Y, Z SYMM - Y, X, Z SYMM Y, - X, Z SFAC C H N O F SI SN CU UNIT 244 240 64 20 48 4.84 3.16 8 MERG 2 OMIT 0.00 180.00 OMIT 1 1 0 OMIT 1 5 6 OMIT 0 6 4 EADP Si2 Sn2 EXYZ Si2 Sn2 FMAP 2 PLAN 12 ACTA BOND BOND $H CONF L.S. 6 TEMP -100.00 SIZE 0.21 0.23 0.26 WGHT 0.035600 4.638600 FVAR 1.34965 0.20938 CU1 8 0.357814 0.173512 0.000000 10.50000 0.02376 0.01887 = 0.06419 0.00000 0.00000 0.00253 SI1 6 0.500000 0.000000 0.000000 10.25000 0.01694 0.01388 = 0.01832 0.00000 0.00000 -0.00048 F1 5 0.437913 0.073800 0.000000 10.50000 0.02285 0.01912 = 0.03455 0.00000 0.00000 0.00378 F2 5 0.500000 0.000000 0.081760 10.50000 0.02698 0.02537 = 0.02133 0.00000 0.00000 -0.00669 F3 5 0.426513 -0.062163 0.000000 10.50000 0.02244 0.02289 = 0.02307 0.00000 0.00000 -0.00669 SI2 6 0.000000 0.000000 0.247926 20.25000 0.01931 0.01931 = 0.01867 0.00000 0.00000 0.00000 SN2 7 0.000000 0.000000 0.247926 -20.25000 0.01931 0.01931 = 0.01867 0.00000 0.00000 0.00000 F4 5 0.000000 0.000000 0.155752 10.25000 0.05440 0.05440 = 0.02741 0.00000 0.00000 0.00000 F5 5 -0.082998 0.071573 0.247985 11.00000 0.03113 0.03459 = 0.03379 0.00330 -0.00725 0.00003 F6 5 0.000000 0.000000 0.340169 10.25000 0.02395 0.02395 = 0.03727 0.00000 0.00000 0.00000 N1 3 0.295522 0.112182 0.069560 11.00000 0.02532 0.03514 = 0.05964 -0.01842 0.01233 -0.00369 N2 3 0.222710 0.137058 0.079251 11.00000 0.03201 0.05686 = 0.08771 -0.01462 0.01404 0.00800 N3 3 0.569275 -0.220755 0.068762 11.00000 0.03625 0.01929 = 0.05371 0.00939 -0.01434 -0.00194 N4 3 0.578134 -0.297100 0.076070 11.00000 0.05810 0.02342 = 0.07182 0.01411 -0.01558 0.00008 C1 1 0.319844 0.048833 0.098246 11.00000 0.02784 0.03465 = 0.04947 -0.01526 0.01536 -0.00545 AFIX 43 H1 2 0.371742 0.033825 0.091159 11.00000 -1.20000 AFIX 0 C2 1 0.274401 0.001901 0.138592 11.00000 0.03221 0.04862 = 0.03860 -0.01908 0.01544 -0.01296 C3 1 0.200419 0.027151 0.147896 11.00000 0.03714 0.07055 = 0.05835 -0.01331 0.02203 -0.00993 AFIX 43 H3 2 0.165463 -0.000861 0.174342 11.00000 -1.20000 AFIX 0 C4 1 0.178361 0.094402 0.117700 11.00000 0.02927 0.08856 = 0.08851 -0.01851 0.02458 0.00037 AFIX 43 H4 2 0.127227 0.111751 0.124941 11.00000 -1.20000 AFIX 0 C5 1 0.512275 -0.184154 0.098466 11.00000 0.03518 0.02656 = 0.04359 0.01424 -0.01103 -0.00633 AFIX 43 H5 2 0.508893 -0.129961 0.093065 11.00000 -1.20000 AFIX 0 C6 1 0.456721 -0.220212 0.137292 11.00000 0.04307 0.03647 = 0.03503 0.01461 -0.01207 -0.01650 C7 1 0.467301 -0.299029 0.143774 11.00000 0.07470 0.03932 = 0.05638 0.02377 -0.01298 -0.02678 AFIX 43 H7 2 0.432830 -0.328780 0.169305 11.00000 -1.20000 AFIX 0 C8 1 0.528386 -0.333507 0.112728 11.00000 0.08038 0.02822 = 0.07229 0.01878 -0.01270 -0.00861 AFIX 43 H8 2 0.534935 -0.387392 0.118251 11.00000 -1.20000 AFIX 0 C9 1 0.304749 -0.068967 0.168800 11.00000 0.04013 0.05270 = 0.03006 -0.00700 0.00999 -0.02104 C10 1 0.364953 -0.109309 0.140565 11.00000 0.03782 0.04329 = 0.02503 0.00213 0.00602 -0.01699 AFIX 43 H10 2 0.387209 -0.090513 0.101533 11.00000 -1.20000 AFIX 0 C11 1 0.393628 -0.176885 0.168139 11.00000 0.04343 0.04686 = 0.03279 0.01302 -0.00459 -0.02377 C12 1 0.360825 -0.203558 0.226179 11.00000 0.06090 0.07410 = 0.03504 0.01724 -0.00218 -0.03414 AFIX 43 H12 2 0.379686 -0.249310 0.245788 11.00000 -1.20000 AFIX 0 C13 1 0.302081 -0.164092 0.254465 11.00000 0.08013 0.09921 = 0.02886 0.01086 0.00946 -0.04647 AFIX 43 H13 2 0.280563 -0.182463 0.293933 11.00000 -1.20000 AFIX 0 C14 1 0.273298 -0.097837 0.226724 11.00000 0.05323 0.08150 = 0.03598 -0.01424 0.02046 -0.03107 AFIX 43 H14 2 0.231833 -0.071485 0.246964 11.00000 -1.20000 AFIX 0 C15 1 0.242427 0.324127 0.000000 10.50000 0.06901 0.05098 = 0.11644 0.00000 0.00000 0.03247 AFIX 3 H15A 2 0.210807 0.352257 0.029960 10.50000 -1.50000 H15B 2 0.280937 0.357737 -0.017700 10.50000 -1.50000 H15C 2 0.211027 0.304297 -0.034510 10.50000 -1.50000 AFIX 0 O1 4 0.275783 0.269101 0.029380 10.50000 0.04901 0.04236 = 0.06067 0.00947 0.00098 0.02058 AFIX 3 H1O 2 0.238373 0.244881 0.046400 10.50000 -1.50000 HKLF 4 REM dk21 in I4/m REM R1 = 0.0354 for 2894 Fo > 4sig(Fo) and 0.0499 for all 3744 data REM 224 parameters refined using 0 restraints END WGHT 0.0358 4.5808 REM Highest difference peak 0.504, deepest hole -0.674, 1-sigma level 0.065 Q1 1 -0.0353 0.0498 0.2480 11.00000 0.05 0.50 Q2 1 0.3781 0.1918 0.0283 11.00000 0.05 0.46 Q3 1 0.4629 -0.0327 0.0000 10.50000 0.05 0.38 Q4 1 0.2085 0.3620 0.0000 10.50000 0.05 0.36 Q5 1 0.3145 0.1382 0.0385 11.00000 0.05 0.33 Q6 1 0.1566 0.3401 0.0000 10.50000 0.05 0.31 Q7 1 0.3207 0.1459 0.0462 11.00000 0.05 0.30 Q8 1 0.1946 0.0594 0.1182 11.00000 0.05 0.30 ; _database_code_depnum_ccdc_archive 'CCDC 941554' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_(2) _audit_creation_method SHELXL-97 _chemical_name_systematic ; \m-Hexafluorosilicato-tetrakis[\m-1,3-bis(pyridazin-4-yl)benzene- \k^2^N^2^:N^2'^]-diaquadicopper(II) bis-hexafluorophosphate, solvate with 4 chloroform ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H44 Cu2 F6 N16 O2 Si, 2(F6 P), 4(C H Cl3)' _chemical_formula_sum 'C60 H48 Cl12 Cu2 F18 N16 O2 P2 Si' _chemical_formula_weight 2009.65 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' P P 0.1023 0.0942 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2/n' _space_group_name_Hall '-P 2yac' _symmetry_Int_Tables_number 13 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 12.6120(9) _cell_length_b 12.6185(7) _cell_length_c 25.342(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.262(9) _cell_angle_gamma 90.00 _cell_volume 3980.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 3.41 _cell_measurement_theta_max 27.03 _exptl_crystal_description prism _exptl_crystal_colour blue-green _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_diffrn 1.677 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2008 _exptl_absorpt_coefficient_mu 1.088 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7726 _exptl_absorpt_correction_T_max 0.8283 _exptl_absorpt_process_details 'X-RED (Stoe & Cie, 2001) and X-SHAPE (Stoe & Cie, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 'Stoe Imaging plate diffraction system' _diffrn_measurement_method '\f oscillation scans' _diffrn_standards_decay_% 0 _diffrn_reflns_number 30828 _diffrn_reflns_av_R_equivalents 0.0498 _diffrn_reflns_av_sigmaI/netI 0.0625 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 27.03 _reflns_number_total 8401 _reflns_number_gt 5041 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS Software (Stoe & Cie, 2000)' _computing_cell_refinement 'IPDS Software (Stoe & Cie, 2000)' _computing_data_reduction 'IPDS Software (Stoe & Cie, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Diamond 2.1e (Brandenburg, 1999)' _computing_publication_material 'WinGX 1.70.01 (Farrugia, 1999)' #------------------------------- Refinement data-----------------------# _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. The Si1 atom lies on an inversion centre. Non-hydrogen atoms for the coordination framework and for non-coordinated PF6- anions were refined anisotropically, the CH-hydrogens were added geometrically [Uiso = 1.2Ueq(C)], the OH-hydrogens of aqua ligands were located and then included in calculations with fixed bond lengths [d(O-H) = 0.85 A] and with Uiso = 1.5Ueq(O). Two unique solvate chloroform molecules reside in the crystal channels and are badly disordered over several (more than two) overlapping positions. It was not possible to found satisfactory disordering schemes and the consequent refinements led to poorly converged models (R1 = 0.11). This electron density was successfully modelled using a Squeeze routine implemented in Platon, giving reasonable parameters corresponding to 8 chloroform molecules per unit cell (in total, 521 e / unit cell). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0810P)^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 constr _refine_ls_extinction_method none _refine_ls_number_reflns 8401 _refine_ls_number_parameters 439 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0667 _refine_ls_R_factor_gt 0.0482 _refine_ls_wR_factor_ref 0.1268 _refine_ls_wR_factor_gt 0.1224 _refine_ls_goodness_of_fit_ref 0.845 _refine_ls_restrained_S_all 0.845 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.07948(2) 0.49560(3) 0.154665(11) 0.02552(10) Uani 1 1 d . . . Si1 Si 0.0000 0.5000 0.0000 0.01917(19) Uani 1 2 d S . . F1 F 0.03460(11) 0.49840(13) 0.06700(5) 0.0245(3) Uani 1 1 d . . . F2 F -0.01364(11) 0.63264(12) 0.00112(6) 0.0235(3) Uani 1 1 d . . . F3 F 0.12979(11) 0.51413(12) -0.00628(5) 0.0248(3) Uani 1 1 d . . . P1 P -0.43800(7) 1.00288(8) 0.18487(4) 0.0441(2) Uani 1 1 d . . . F4 F -0.32050(19) 0.9911(2) 0.17008(12) 0.0792(8) Uani 1 1 d . . . F5 F -0.44454(19) 0.87612(18) 0.18760(9) 0.0621(6) Uani 1 1 d . . . F6 F -0.5592(2) 1.0117(3) 0.19379(19) 0.1319(15) Uani 1 1 d . . . F7 F -0.4286(2) 1.1285(2) 0.17894(14) 0.0885(9) Uani 1 1 d . . . F8 F -0.4006(3) 1.0041(3) 0.24820(11) 0.1002(10) Uani 1 1 d . . . F9 F -0.4942(3) 0.9982(3) 0.12465(12) 0.1101(12) Uani 1 1 d . . . O1 O 0.12288(18) 0.48245(18) 0.24098(8) 0.0398(5) Uani 1 1 d . . . H1W H 0.1465 0.5374 0.2584 0.060 Uiso 1 1 d R . . H2W H 0.1553 0.4290 0.2563 0.060 Uiso 1 1 d R . . N1 N 0.18661(18) 0.61734(19) 0.14362(9) 0.0289(5) Uani 1 1 d . . . N2 N 0.2669(2) 0.6335(2) 0.18472(10) 0.0435(7) Uani 1 1 d . . . N3 N 0.03149(19) 0.6266(2) -0.15310(9) 0.0302(5) Uani 1 1 d . . . N4 N 0.0561(2) 0.6541(3) -0.20137(10) 0.0472(7) Uani 1 1 d . . . N5 N -0.03953(19) 0.6078(2) 0.15551(9) 0.0316(6) Uani 1 1 d . . . N6 N -0.0303(3) 0.6656(2) 0.20020(11) 0.0479(7) Uani 1 1 d . . . N7 N -0.19267(18) 0.61644(19) -0.14176(9) 0.0291(5) Uani 1 1 d . . . N8 N -0.2297(2) 0.6770(2) -0.18391(10) 0.0446(7) Uani 1 1 d . . . C1 C 0.1793(2) 0.6741(2) 0.09969(11) 0.0273(6) Uani 1 1 d . . . H1 H 0.1201 0.6619 0.0727 0.033 Uiso 1 1 calc R . . C2 C 0.2545(2) 0.7524(2) 0.09037(11) 0.0289(6) Uani 1 1 d . . . C3 C 0.3350(3) 0.7706(3) 0.13304(13) 0.0440(8) Uani 1 1 d . . . H3 H 0.3868 0.8236 0.1315 0.053 Uiso 1 1 calc R . . C4 C 0.3372(3) 0.7085(3) 0.17842(14) 0.0538(10) Uani 1 1 d . . . H4 H 0.3933 0.7207 0.2070 0.065 Uiso 1 1 calc R . . C5 C 0.0756(2) 0.6773(2) -0.10958(11) 0.0302(6) Uani 1 1 d . . . H5 H 0.0541 0.6577 -0.0771 0.036 Uiso 1 1 calc R . . C6 C 0.1519(2) 0.7580(3) -0.10817(11) 0.0318(6) Uani 1 1 d . . . C7 C 0.1764(3) 0.7862(3) -0.15714(14) 0.0540(10) Uani 1 1 d . . . H7 H 0.2252 0.8412 -0.1604 0.065 Uiso 1 1 calc R . . C8 C 0.1266(4) 0.7306(4) -0.20170(14) 0.0636(12) Uani 1 1 d . . . H8 H 0.1449 0.7494 -0.2350 0.076 Uiso 1 1 calc R . . C9 C 0.2458(2) 0.8082(2) 0.03915(12) 0.0305(6) Uani 1 1 d . . . C10 C 0.2045(2) 0.7586(2) -0.00848(11) 0.0288(6) Uani 1 1 d . . . H10 H 0.1793 0.6886 -0.0078 0.035 Uiso 1 1 calc R . . C11 C 0.1994(2) 0.8106(2) -0.05752(11) 0.0306(6) Uani 1 1 d . . . C12 C 0.2373(3) 0.9136(3) -0.05779(13) 0.0416(8) Uani 1 1 d . . . H12 H 0.2351 0.9493 -0.0905 0.050 Uiso 1 1 calc R . . C13 C 0.2786(3) 0.9650(3) -0.01019(14) 0.0436(8) Uani 1 1 d . . . H13 H 0.3033 1.0352 -0.0109 0.052 Uiso 1 1 calc R . . C14 C 0.2830(2) 0.9123(3) 0.03808(13) 0.0388(7) Uani 1 1 d . . . H14 H 0.3112 0.9466 0.0702 0.047 Uiso 1 1 calc R . . C15 C -0.1160(2) 0.6277(2) 0.11456(11) 0.0292(6) Uani 1 1 d . . . H15 H -0.1202 0.5838 0.0843 0.035 Uiso 1 1 calc R . . C16 C -0.1912(2) 0.7098(3) 0.11314(12) 0.0327(6) Uani 1 1 d . . . C17 C -0.1828(3) 0.7689(3) 0.15953(13) 0.0514(10) Uani 1 1 d . . . H17 H -0.2292 0.8261 0.1624 0.062 Uiso 1 1 calc R . . C18 C -0.1038(3) 0.7408(3) 0.20143(15) 0.0611(11) Uani 1 1 d . . . H18 H -0.1018 0.7780 0.2337 0.073 Uiso 1 1 calc R . . C19 C -0.2236(2) 0.6343(2) -0.09459(11) 0.0278(6) Uani 1 1 d . . . H19 H -0.1966 0.5894 -0.0659 0.033 Uiso 1 1 calc R . . C20 C -0.2935(2) 0.7155(2) -0.08524(11) 0.0308(6) Uani 1 1 d . . . C21 C -0.3319(3) 0.7767(3) -0.12913(14) 0.0470(9) Uani 1 1 d . . . H21 H -0.3794 0.8331 -0.1264 0.056 Uiso 1 1 calc R . . C22 C -0.2990(3) 0.7532(3) -0.17724(14) 0.0548(10) Uani 1 1 d . . . H22 H -0.3277 0.7938 -0.2073 0.066 Uiso 1 1 calc R . . C23 C -0.2721(2) 0.7314(2) 0.06513(11) 0.0301(6) Uani 1 1 d . . . C24 C -0.2465(2) 0.7122(2) 0.01407(11) 0.0278(6) Uani 1 1 d . . . H24 H -0.1787 0.6847 0.0106 0.033 Uiso 1 1 calc R . . C25 C -0.3211(2) 0.7338(2) -0.03127(11) 0.0299(6) Uani 1 1 d . . . C26 C -0.4219(2) 0.7739(3) -0.02586(13) 0.0401(7) Uani 1 1 d . . . H26 H -0.4726 0.7885 -0.0564 0.048 Uiso 1 1 calc R . . C27 C -0.4469(2) 0.7921(3) 0.02435(14) 0.0445(8) Uani 1 1 d . . . H27 H -0.5150 0.8187 0.0278 0.053 Uiso 1 1 calc R . . C28 C -0.3724(2) 0.7714(3) 0.07001(13) 0.0402(7) Uani 1 1 d . . . H28 H -0.3901 0.7845 0.1041 0.048 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.03145(16) 0.0272(2) 0.01665(14) -0.00024(15) 0.00002(10) -0.00034(16) Si1 0.0214(4) 0.0204(5) 0.0149(4) 0.0005(4) 0.0003(3) -0.0009(4) F1 0.0302(7) 0.0255(8) 0.0161(6) -0.0011(7) -0.0013(5) -0.0003(7) F2 0.0257(8) 0.0192(8) 0.0251(7) -0.0007(6) 0.0021(6) 0.0011(6) F3 0.0219(7) 0.0254(9) 0.0265(7) -0.0005(6) 0.0020(5) 0.0000(6) P1 0.0403(4) 0.0374(5) 0.0515(5) 0.0006(4) -0.0021(3) -0.0008(4) F4 0.0550(13) 0.0730(19) 0.115(2) 0.0148(16) 0.0310(13) 0.0005(12) F5 0.0777(15) 0.0416(14) 0.0619(14) 0.0089(10) -0.0038(11) -0.0097(11) F6 0.0639(18) 0.143(4) 0.197(4) 0.038(3) 0.047(2) 0.0240(19) F7 0.0854(18) 0.0393(16) 0.135(3) -0.0006(15) 0.0002(17) -0.0007(13) F8 0.134(3) 0.101(3) 0.0584(15) -0.0245(17) -0.0072(15) 0.006(2) F9 0.148(3) 0.075(2) 0.0830(19) 0.0147(17) -0.0542(19) -0.0058(19) O1 0.0558(13) 0.0370(15) 0.0230(9) 0.0013(9) -0.0047(8) -0.0038(10) N1 0.0328(12) 0.0263(14) 0.0254(12) -0.0052(10) -0.0026(9) -0.0012(10) N2 0.0409(14) 0.0520(19) 0.0309(14) 0.0035(12) -0.0143(11) -0.0093(13) N3 0.0392(13) 0.0283(15) 0.0244(12) 0.0028(10) 0.0095(10) -0.0030(10) N4 0.0612(18) 0.057(2) 0.0250(14) 0.0020(12) 0.0119(12) -0.0166(15) N5 0.0385(13) 0.0378(16) 0.0178(11) -0.0056(10) 0.0028(10) 0.0061(11) N6 0.0680(19) 0.0460(19) 0.0269(14) -0.0141(12) -0.0003(12) 0.0167(15) N7 0.0327(12) 0.0291(15) 0.0229(12) -0.0022(10) -0.0035(9) 0.0019(10) N8 0.0608(18) 0.0442(19) 0.0256(13) 0.0020(11) -0.0027(12) 0.0152(14) C1 0.0280(13) 0.0248(17) 0.0270(14) -0.0013(11) -0.0019(11) -0.0032(11) C2 0.0282(13) 0.0253(17) 0.0308(14) -0.0047(11) -0.0025(11) 0.0008(11) C3 0.0417(17) 0.049(2) 0.0361(18) -0.0005(15) -0.0088(13) -0.0159(15) C4 0.048(2) 0.065(3) 0.0396(19) 0.0038(17) -0.0180(15) -0.0182(18) C5 0.0377(15) 0.0296(18) 0.0231(13) 0.0079(11) 0.0043(11) -0.0048(12) C6 0.0346(15) 0.0318(18) 0.0294(15) 0.0059(12) 0.0067(11) -0.0029(12) C7 0.066(2) 0.060(3) 0.041(2) -0.0014(17) 0.0215(17) -0.033(2) C8 0.090(3) 0.075(3) 0.0315(18) -0.0001(18) 0.0265(19) -0.039(2) C9 0.0255(13) 0.0272(17) 0.0376(15) 0.0006(12) 0.0013(11) -0.0047(11) C10 0.0300(14) 0.0242(17) 0.0320(14) 0.0011(11) 0.0041(11) -0.0057(11) C11 0.0288(13) 0.0316(18) 0.0321(15) 0.0003(12) 0.0076(11) -0.0053(12) C12 0.0489(18) 0.039(2) 0.0355(17) 0.0062(14) 0.0018(14) -0.0112(15) C13 0.055(2) 0.0263(19) 0.0495(19) 0.0005(13) 0.0082(15) -0.0180(14) C14 0.0382(16) 0.0319(19) 0.0436(18) -0.0027(13) -0.0016(13) -0.0086(13) C15 0.0344(14) 0.0307(17) 0.0231(13) -0.0033(11) 0.0065(11) 0.0021(12) C16 0.0342(15) 0.0326(19) 0.0324(15) -0.0017(12) 0.0088(12) 0.0029(12) C17 0.067(2) 0.052(2) 0.0333(18) -0.0150(16) 0.0013(16) 0.0222(19) C18 0.078(3) 0.063(3) 0.038(2) -0.0240(18) -0.0053(17) 0.025(2) C19 0.0285(13) 0.0292(17) 0.0238(13) 0.0006(11) -0.0011(10) 0.0019(11) C20 0.0284(14) 0.0302(18) 0.0303(15) -0.0012(12) -0.0055(11) 0.0024(11) C21 0.058(2) 0.040(2) 0.0395(19) 0.0017(15) -0.0024(15) 0.0206(16) C22 0.077(3) 0.049(3) 0.0342(18) 0.0105(16) -0.0022(17) 0.025(2) C23 0.0290(14) 0.0278(17) 0.0333(15) -0.0018(12) 0.0043(11) 0.0043(11) C24 0.0234(12) 0.0254(16) 0.0342(15) -0.0006(11) 0.0037(11) 0.0052(11) C25 0.0288(14) 0.0253(17) 0.0354(15) -0.0009(12) 0.0045(11) 0.0051(11) C26 0.0295(15) 0.042(2) 0.0463(18) -0.0031(14) -0.0004(13) 0.0079(13) C27 0.0280(15) 0.055(2) 0.053(2) -0.0057(16) 0.0123(14) 0.0087(14) C28 0.0404(17) 0.042(2) 0.0401(17) -0.0035(14) 0.0126(13) 0.0108(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 N5 2.066(2) . ? Cu1 N7 2.072(2) 3_565 ? Cu1 N3 2.079(2) 3_565 ? Cu1 N1 2.094(2) . ? Cu1 O1 2.1741(19) . ? Cu1 F1 2.2028(13) . ? Si1 F3 1.6795(14) 3_565 ? Si1 F3 1.6795(14) . ? Si1 F2 1.6832(15) 3_565 ? Si1 F2 1.6832(15) . ? Si1 F1 1.6839(12) . ? Si1 F1 1.6839(12) 3_565 ? P1 F9 1.577(3) . ? P1 F6 1.585(3) . ? P1 F4 1.593(2) . ? P1 F7 1.598(3) . ? P1 F8 1.598(3) . ? P1 F5 1.604(2) . ? O1 H1W 0.8499 . ? O1 H2W 0.8498 . ? N1 C1 1.315(4) . ? N1 N2 1.346(3) . ? N2 C4 1.325(5) . ? N3 C5 1.318(4) . ? N3 N4 1.355(3) . ? N3 Cu1 2.079(2) 3_565 ? N4 C8 1.312(5) . ? N5 C15 1.322(4) . ? N5 N6 1.337(3) . ? N6 C18 1.330(5) . ? N7 C19 1.335(4) . ? N7 N8 1.335(3) . ? N7 Cu1 2.072(2) 3_565 ? N8 C22 1.328(5) . ? C1 C2 1.416(4) . ? C1 H1 0.9400 . ? C2 C3 1.378(4) . ? C2 C9 1.465(4) . ? C3 C4 1.388(5) . ? C3 H3 0.9400 . ? C4 H4 0.9400 . ? C5 C6 1.398(4) . ? C5 H5 0.9400 . ? C6 C7 1.373(4) . ? C6 C11 1.484(4) . ? C7 C8 1.391(5) . ? C7 H7 0.9400 . ? C8 H8 0.9400 . ? C9 C10 1.385(4) . ? C9 C14 1.396(4) . ? C10 C11 1.398(4) . ? C10 H10 0.9400 . ? C11 C12 1.384(4) . ? C12 C13 1.395(5) . ? C12 H12 0.9400 . ? C13 C14 1.386(5) . ? C13 H13 0.9400 . ? C14 H14 0.9400 . ? C15 C16 1.401(4) . ? C15 H15 0.9400 . ? C16 C17 1.382(4) . ? C16 C23 1.482(4) . ? C17 C18 1.380(5) . ? C17 H17 0.9400 . ? C18 H18 0.9400 . ? C19 C20 1.397(4) . ? C19 H19 0.9400 . ? C20 C21 1.377(4) . ? C20 C25 1.483(4) . ? C21 C22 1.382(5) . ? C21 H21 0.9400 . ? C22 H22 0.9400 . ? C23 C28 1.385(4) . ? C23 C24 1.404(4) . ? C24 C25 1.390(4) . ? C24 H24 0.9400 . ? C25 C26 1.395(4) . ? C26 C27 1.379(5) . ? C26 H26 0.9400 . ? C27 C28 1.393(5) . ? C27 H27 0.9400 . ? C28 H28 0.9400 . ? 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 N5 Cu1 N7 171.61(9) . 3_565 ? N5 Cu1 N3 91.18(10) . 3_565 ? N7 Cu1 N3 88.25(10) 3_565 3_565 ? N5 Cu1 N1 89.10(10) . . ? N7 Cu1 N1 90.21(9) 3_565 . ? N3 Cu1 N1 171.34(9) 3_565 . ? N5 Cu1 O1 96.18(9) . . ? N7 Cu1 O1 92.21(9) 3_565 . ? N3 Cu1 O1 91.27(9) 3_565 . ? N1 Cu1 O1 97.30(9) . . ? N5 Cu1 F1 86.00(7) . . ? N7 Cu1 F1 85.61(7) 3_565 . ? N3 Cu1 F1 85.98(8) 3_565 . ? N1 Cu1 F1 85.41(8) . . ? O1 Cu1 F1 176.53(7) . . ? F3 Si1 F3 180.0 3_565 . ? F3 Si1 F2 89.99(7) 3_565 3_565 ? F3 Si1 F2 90.01(7) . 3_565 ? F3 Si1 F2 90.01(7) 3_565 . ? F3 Si1 F2 89.99(7) . . ? F2 Si1 F2 180.0 3_565 . ? F3 Si1 F1 90.08(7) 3_565 . ? F3 Si1 F1 89.92(7) . . ? F2 Si1 F1 89.68(8) 3_565 . ? F2 Si1 F1 90.32(8) . . ? F3 Si1 F1 89.92(7) 3_565 3_565 ? F3 Si1 F1 90.08(7) . 3_565 ? F2 Si1 F1 90.32(8) 3_565 3_565 ? F2 Si1 F1 89.68(8) . 3_565 ? F1 Si1 F1 180.0 . 3_565 ? Si1 F1 Cu1 179.73(11) . . ? F9 P1 F6 81.2(2) . . ? F9 P1 F4 93.4(2) . . ? F6 P1 F4 174.5(2) . . ? F9 P1 F7 88.55(17) . . ? F6 P1 F7 91.82(19) . . ? F4 P1 F7 89.09(15) . . ? F9 P1 F8 170.5(2) . . ? F6 P1 F8 89.5(2) . . ? F4 P1 F8 95.83(17) . . ? F7 P1 F8 94.04(18) . . ? F9 P1 F5 89.22(15) . . ? F6 P1 F5 90.38(18) . . ? F4 P1 F5 88.47(14) . . ? F7 P1 F5 176.59(17) . . ? F8 P1 F5 88.58(15) . . ? Cu1 O1 H1W 118.1 . . ? Cu1 O1 H2W 123.1 . . ? H1W O1 H2W 107.9 . . ? C1 N1 N2 121.0(3) . . ? C1 N1 Cu1 123.63(18) . . ? N2 N1 Cu1 115.37(19) . . ? C4 N2 N1 116.7(3) . . ? C5 N3 N4 120.3(3) . . ? C5 N3 Cu1 124.60(19) . 3_565 ? N4 N3 Cu1 115.12(19) . 3_565 ? C8 N4 N3 116.6(3) . . ? C15 N5 N6 120.9(3) . . ? C15 N5 Cu1 124.18(19) . . ? N6 N5 Cu1 114.77(19) . . ? C18 N6 N5 116.3(3) . . ? C19 N7 N8 120.4(3) . . ? C19 N7 Cu1 124.35(19) . 3_565 ? N8 N7 Cu1 115.16(19) . 3_565 ? C22 N8 N7 117.7(3) . . ? N1 C1 C2 124.3(2) . . ? N1 C1 H1 117.8 . . ? C2 C1 H1 117.8 . . ? C3 C2 C1 114.5(3) . . ? C3 C2 C9 123.8(3) . . ? C1 C2 C9 121.7(2) . . ? C2 C3 C4 118.0(3) . . ? C2 C3 H3 121.0 . . ? C4 C3 H3 121.0 . . ? N2 C4 C3 125.3(3) . . ? N2 C4 H4 117.3 . . ? C3 C4 H4 117.3 . . ? N3 C5 C6 124.8(3) . . ? N3 C5 H5 117.6 . . ? C6 C5 H5 117.6 . . ? C7 C6 C5 114.8(3) . . ? C7 C6 C11 123.2(3) . . ? C5 C6 C11 121.9(2) . . ? C6 C7 C8 117.7(3) . . ? C6 C7 H7 121.2 . . ? C8 C7 H7 121.2 . . ? N4 C8 C7 125.7(3) . . ? N4 C8 H8 117.1 . . ? C7 C8 H8 117.1 . . ? C10 C9 C14 119.2(3) . . ? C10 C9 C2 121.3(3) . . ? C14 C9 C2 119.4(3) . . ? C9 C10 C11 121.3(3) . . ? C9 C10 H10 119.3 . . ? C11 C10 H10 119.3 . . ? C12 C11 C10 118.6(3) . . ? C12 C11 C6 120.5(3) . . ? C10 C11 C6 120.9(3) . . ? C11 C12 C13 120.9(3) . . ? C11 C12 H12 119.6 . . ? C13 C12 H12 119.6 . . ? C14 C13 C12 119.8(3) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C13 C14 C9 120.2(3) . . ? C13 C14 H14 119.9 . . ? C9 C14 H14 119.9 . . ? N5 C15 C16 124.5(3) . . ? N5 C15 H15 117.8 . . ? C16 C15 H15 117.8 . . ? C17 C16 C15 114.7(3) . . ? C17 C16 C23 123.2(3) . . ? C15 C16 C23 122.1(3) . . ? C18 C17 C16 117.6(3) . . ? C18 C17 H17 121.2 . . ? C16 C17 H17 121.2 . . ? N6 C18 C17 125.8(3) . . ? N6 C18 H18 117.1 . . ? C17 C18 H18 117.1 . . ? N7 C19 C20 124.0(3) . . ? N7 C19 H19 118.0 . . ? C20 C19 H19 118.0 . . ? C21 C20 C19 115.1(3) . . ? C21 C20 C25 123.6(3) . . ? C19 C20 C25 121.3(3) . . ? C20 C21 C22 118.4(3) . . ? C20 C21 H21 120.8 . . ? C22 C21 H21 120.8 . . ? N8 C22 C21 124.4(3) . . ? N8 C22 H22 117.8 . . ? C21 C22 H22 117.8 . . ? C28 C23 C24 119.6(3) . . ? C28 C23 C16 120.8(3) . . ? C24 C23 C16 119.6(2) . . ? C25 C24 C23 120.2(2) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C24 C25 C26 119.7(3) . . ? C24 C25 C20 120.3(2) . . ? C26 C25 C20 120.0(3) . . ? C27 C26 C25 119.9(3) . . ? C27 C26 H26 120.1 . . ? C25 C26 H26 120.1 . . ? C26 C27 C28 120.8(3) . . ? C26 C27 H27 119.6 . . ? C28 C27 H27 119.6 . . ? C23 C28 C27 119.8(3) . . ? C23 C28 H28 120.1 . . ? C27 C28 H28 120.1 . . ? 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 N5 Cu1 N1 C1 -68.3(2) . . . . ? N7 Cu1 N1 C1 103.4(2) 3_565 . . . ? O1 Cu1 N1 C1 -164.4(2) . . . . ? F1 Cu1 N1 C1 17.8(2) . . . . ? N5 Cu1 N1 N2 113.0(2) . . . . ? N7 Cu1 N1 N2 -75.4(2) 3_565 . . . ? O1 Cu1 N1 N2 16.8(2) . . . . ? F1 Cu1 N1 N2 -161.0(2) . . . . ? C1 N1 N2 C4 -0.2(5) . . . . ? Cu1 N1 N2 C4 178.6(3) . . . . ? C5 N3 N4 C8 1.4(5) . . . . ? Cu1 N3 N4 C8 -179.5(3) 3_565 . . . ? N3 Cu1 N5 C15 -69.5(2) 3_565 . . . ? N1 Cu1 N5 C15 101.8(3) . . . . ? O1 Cu1 N5 C15 -161.0(2) . . . . ? F1 Cu1 N5 C15 16.3(2) . . . . ? N3 Cu1 N5 N6 114.7(2) 3_565 . . . ? N1 Cu1 N5 N6 -74.0(2) . . . . ? O1 Cu1 N5 N6 23.3(2) . . . . ? F1 Cu1 N5 N6 -159.4(2) . . . . ? C15 N5 N6 C18 2.1(5) . . . . ? Cu1 N5 N6 C18 178.0(3) . . . . ? C19 N7 N8 C22 -1.3(5) . . . . ? Cu1 N7 N8 C22 -177.2(3) 3_565 . . . ? N2 N1 C1 C2 2.6(5) . . . . ? Cu1 N1 C1 C2 -176.1(2) . . . . ? N1 C1 C2 C3 -4.1(5) . . . . ? N1 C1 C2 C9 175.9(3) . . . . ? C1 C2 C3 C4 3.2(5) . . . . ? C9 C2 C3 C4 -176.7(3) . . . . ? N1 N2 C4 C3 -0.4(6) . . . . ? C2 C3 C4 N2 -1.2(6) . . . . ? N4 N3 C5 C6 -2.5(5) . . . . ? Cu1 N3 C5 C6 178.6(2) 3_565 . . . ? N3 C5 C6 C7 2.8(5) . . . . ? N3 C5 C6 C11 -179.1(3) . . . . ? C5 C6 C7 C8 -2.0(6) . . . . ? C11 C6 C7 C8 179.9(4) . . . . ? N3 N4 C8 C7 -0.9(7) . . . . ? C6 C7 C8 N4 1.3(7) . . . . ? C3 C2 C9 C10 147.2(3) . . . . ? C1 C2 C9 C10 -32.7(4) . . . . ? C3 C2 C9 C14 -30.7(5) . . . . ? C1 C2 C9 C14 149.4(3) . . . . ? C14 C9 C10 C11 0.0(4) . . . . ? C2 C9 C10 C11 -177.8(3) . . . . ? C9 C10 C11 C12 0.3(4) . . . . ? C9 C10 C11 C6 -178.1(3) . . . . ? C7 C6 C11 C12 24.9(5) . . . . ? C5 C6 C11 C12 -153.0(3) . . . . ? C7 C6 C11 C10 -156.7(3) . . . . ? C5 C6 C11 C10 25.3(4) . . . . ? C10 C11 C12 C13 -0.7(5) . . . . ? C6 C11 C12 C13 177.7(3) . . . . ? C11 C12 C13 C14 0.7(5) . . . . ? C12 C13 C14 C9 -0.4(5) . . . . ? C10 C9 C14 C13 0.0(5) . . . . ? C2 C9 C14 C13 177.9(3) . . . . ? N6 N5 C15 C16 1.4(5) . . . . ? Cu1 N5 C15 C16 -174.1(2) . . . . ? N5 C15 C16 C17 -2.2(5) . . . . ? N5 C15 C16 C23 177.2(3) . . . . ? C15 C16 C17 C18 -0.6(5) . . . . ? C23 C16 C17 C18 -179.9(4) . . . . ? N5 N6 C18 C17 -5.1(7) . . . . ? C16 C17 C18 N6 4.4(7) . . . . ? N8 N7 C19 C20 -0.8(4) . . . . ? Cu1 N7 C19 C20 174.7(2) 3_565 . . . ? N7 C19 C20 C21 1.4(4) . . . . ? N7 C19 C20 C25 -177.4(3) . . . . ? C19 C20 C21 C22 0.0(5) . . . . ? C25 C20 C21 C22 178.9(3) . . . . ? N7 N8 C22 C21 2.9(6) . . . . ? C20 C21 C22 N8 -2.2(6) . . . . ? C17 C16 C23 C28 -32.5(5) . . . . ? C15 C16 C23 C28 148.2(3) . . . . ? C17 C16 C23 C24 146.8(3) . . . . ? C15 C16 C23 C24 -32.4(4) . . . . ? C28 C23 C24 C25 0.4(5) . . . . ? C16 C23 C24 C25 -179.0(3) . . . . ? C23 C24 C25 C26 -0.4(5) . . . . ? C23 C24 C25 C20 178.8(3) . . . . ? C21 C20 C25 C24 -146.8(3) . . . . ? C19 C20 C25 C24 31.9(4) . . . . ? C21 C20 C25 C26 32.4(5) . . . . ? C19 C20 C25 C26 -148.8(3) . . . . ? C24 C25 C26 C27 0.1(5) . . . . ? C20 C25 C26 C27 -179.2(3) . . . . ? C25 C26 C27 C28 0.3(5) . . . . ? C24 C23 C28 C27 0.0(5) . . . . ? C16 C23 C28 C27 179.4(3) . . . . ? C26 C27 C28 C23 -0.4(6) . . . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 27.03 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 0.709 _refine_diff_density_min -0.541 _refine_diff_density_rms 0.073 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.010 0.000 -0.010 638 258 '4 CHCl3' 2 -0.167 0.500 0.333 675 263 '4 CHCl3' _platon_squeeze_details ; ; _iucr_refine_instruction_details ; #--------------------------------------------------------- TITL ip1353 in P2/n CELL 0.71073 12.6120 12.6185 25.3424 90.000 99.262 90.000 ZERR 2.00 0.0009 0.0007 0.0020 0.000 0.009 0.000 LATT 1 SYMM 1/2 - X, Y, 1/2 - Z SFAC C H N O F SI P CU CL UNIT 120 96 32 4 36 2 4 4 24 MERG 2 SHEL 0.78 6 FMAP 2 PLAN 25 SIZE 0.18 0.20 0.25 ACTA BOND $H EQIV $1 -X, 1-Y, -Z RTAB H..O H1 F2 RTAB H..O H5 F2 RTAB H..O H24 F2 RTAB H..O H10 F3 RTAB H..O H15 F3_$1 RTAB H..O H19 F3_$1 RTAB O..O C1 F2 RTAB O..O C5 F2 RTAB O..O C24 F2 RTAB O..O C10 F3 RTAB O..O C15 F3_$1 RTAB O..O C19 F3_$1 RTAB XHY C1 H1 F2 RTAB XHY C5 H5 F2 RTAB XHY C24 H24 F2 RTAB XHY C10 H10 F3 RTAB XHY C15 H15 F3_$1 RTAB XHY C19 H19 F3_$1 MPLA 4 N1 N5 N3_$1 N7_$1 Cu1 CONF LIST 4 L.S. 4 TEMP -60.00 WGHT 0.081000 FVAR 9.74304 CU1 8 0.079479 0.495600 0.154665 11.00000 0.03145 0.02721 = 0.01665 -0.00024 0.00002 -0.00034 SI1 6 0.000000 0.500000 0.000000 10.50000 0.02135 0.02043 = 0.01488 0.00048 0.00031 -0.00087 F1 5 0.034600 0.498402 0.067001 11.00000 0.03020 0.02547 = 0.01606 -0.00107 -0.00129 -0.00032 F2 5 -0.013644 0.632636 0.001118 11.00000 0.02574 0.01915 = 0.02511 -0.00067 0.00214 0.00110 F3 5 0.129791 0.514131 -0.006284 11.00000 0.02194 0.02540 = 0.02653 -0.00049 0.00203 0.00000 P1 7 -0.438004 1.002876 0.184871 11.00000 0.04028 0.03740 = 0.05153 0.00061 -0.00210 -0.00082 F4 5 -0.320499 0.991092 0.170077 11.00000 0.05497 0.07299 = 0.11534 0.01477 0.03103 0.00048 F5 5 -0.444537 0.876116 0.187602 11.00000 0.07775 0.04163 = 0.06194 0.00887 -0.00383 -0.00974 F6 5 -0.559233 1.011719 0.193789 11.00000 0.06394 0.14325 = 0.19705 0.03823 0.04693 0.02405 F7 5 -0.428556 1.128484 0.178944 11.00000 0.08539 0.03928 = 0.13516 -0.00063 0.00021 -0.00065 F8 5 -0.400576 1.004093 0.248198 11.00000 0.13350 0.10110 = 0.05842 -0.02448 -0.00715 0.00580 F9 5 -0.494205 0.998230 0.124650 11.00000 0.14833 0.07490 = 0.08305 0.01468 -0.05425 -0.00582 O1 4 0.122882 0.482450 0.240982 11.00000 0.05582 0.03695 = 0.02301 0.00131 -0.00466 -0.00375 AFIX 3 H1W 2 0.146522 0.537400 0.258411 11.00000 -1.50000 H2W 2 0.155322 0.429000 0.256321 11.00000 -1.50000 AFIX 0 N1 3 0.186606 0.617342 0.143621 11.00000 0.03278 0.02627 = 0.02539 -0.00522 -0.00260 -0.00119 N2 3 0.266854 0.633466 0.184717 11.00000 0.04092 0.05198 = 0.03092 0.00353 -0.01430 -0.00929 N3 3 0.031486 0.626644 -0.153105 11.00000 0.03920 0.02826 = 0.02445 0.00283 0.00951 -0.00302 N4 3 0.056147 0.654134 -0.201367 11.00000 0.06123 0.05704 = 0.02503 0.00202 0.01193 -0.01657 N5 3 -0.039529 0.607759 0.155507 11.00000 0.03849 0.03783 = 0.01778 -0.00557 0.00276 0.00609 N6 3 -0.030342 0.665620 0.200200 11.00000 0.06804 0.04604 = 0.02690 -0.01413 -0.00030 0.01667 N7 3 -0.192666 0.616444 -0.141755 11.00000 0.03274 0.02912 = 0.02292 -0.00216 -0.00352 0.00195 N8 3 -0.229655 0.677029 -0.183913 11.00000 0.06076 0.04418 = 0.02561 0.00203 -0.00274 0.01516 C1 1 0.179251 0.674116 0.099687 11.00000 0.02799 0.02476 = 0.02697 -0.00125 -0.00188 -0.00320 AFIX 43 H1 2 0.120135 0.661940 0.072682 11.00000 -1.20000 AFIX 0 C2 1 0.254519 0.752399 0.090370 11.00000 0.02822 0.02526 = 0.03082 -0.00470 -0.00247 0.00083 C3 1 0.334992 0.770648 0.133042 11.00000 0.04169 0.04921 = 0.03613 -0.00047 -0.00884 -0.01591 AFIX 43 H3 2 0.386820 0.823593 0.131469 11.00000 -1.20000 AFIX 0 C4 1 0.337250 0.708523 0.178422 11.00000 0.04848 0.06518 = 0.03957 0.00377 -0.01796 -0.01818 AFIX 43 H4 2 0.393294 0.720692 0.207022 11.00000 -1.20000 AFIX 0 C5 1 0.075594 0.677280 -0.109576 11.00000 0.03770 0.02961 = 0.02312 0.00794 0.00432 -0.00481 AFIX 43 H5 2 0.054147 0.657694 -0.077093 11.00000 -1.20000 AFIX 0 C6 1 0.151934 0.757978 -0.108173 11.00000 0.03461 0.03182 = 0.02944 0.00595 0.00668 -0.00286 C7 1 0.176430 0.786209 -0.157142 11.00000 0.06566 0.05952 = 0.04109 -0.00143 0.02149 -0.03251 AFIX 43 H7 2 0.225206 0.841210 -0.160434 11.00000 -1.20000 AFIX 0 C8 1 0.126567 0.730597 -0.201696 11.00000 0.08960 0.07510 = 0.03150 -0.00006 0.02648 -0.03928 AFIX 43 H8 2 0.144916 0.749432 -0.234963 11.00000 -1.20000 AFIX 0 C9 1 0.245777 0.808211 0.039151 11.00000 0.02549 0.02717 = 0.03761 0.00061 0.00128 -0.00472 C10 1 0.204481 0.758650 -0.008479 11.00000 0.02999 0.02419 = 0.03199 0.00109 0.00406 -0.00570 AFIX 43 H10 2 0.179330 0.688614 -0.007821 11.00000 -1.20000 AFIX 0 C11 1 0.199433 0.810641 -0.057516 11.00000 0.02883 0.03162 = 0.03211 0.00034 0.00760 -0.00531 C12 1 0.237276 0.913568 -0.057794 11.00000 0.04885 0.03885 = 0.03551 0.00622 0.00177 -0.01122 AFIX 43 H12 2 0.235125 0.949277 -0.090502 11.00000 -1.20000 AFIX 0 C13 1 0.278567 0.965027 -0.010189 11.00000 0.05484 0.02629 = 0.04947 0.00051 0.00823 -0.01802 AFIX 43 H13 2 0.303267 1.035224 -0.010851 11.00000 -1.20000 AFIX 0 C14 1 0.283038 0.912276 0.038082 11.00000 0.03820 0.03187 = 0.04360 -0.00271 -0.00163 -0.00863 AFIX 43 H14 2 0.311231 0.946643 0.070194 11.00000 -1.20000 AFIX 0 C15 1 -0.116005 0.627703 0.114558 11.00000 0.03445 0.03067 = 0.02308 -0.00330 0.00651 0.00207 AFIX 43 H15 2 -0.120213 0.583793 0.084329 11.00000 -1.20000 AFIX 0 C16 1 -0.191176 0.709783 0.113143 11.00000 0.03422 0.03263 = 0.03238 -0.00171 0.00881 0.00287 C17 1 -0.182798 0.768887 0.159528 11.00000 0.06695 0.05176 = 0.03329 -0.01502 0.00133 0.02218 AFIX 43 H17 2 -0.229180 0.826146 0.162442 11.00000 -1.20000 AFIX 0 C18 1 -0.103814 0.740756 0.201431 11.00000 0.07784 0.06251 = 0.03822 -0.02404 -0.00533 0.02549 AFIX 43 H18 2 -0.101792 0.778023 0.233694 11.00000 -1.20000 AFIX 0 C19 1 -0.223566 0.634257 -0.094591 11.00000 0.02855 0.02919 = 0.02382 0.00065 -0.00113 0.00191 AFIX 43 H19 2 -0.196648 0.589429 -0.065925 11.00000 -1.20000 AFIX 0 C20 1 -0.293472 0.715459 -0.085236 11.00000 0.02836 0.03020 = 0.03035 -0.00116 -0.00555 0.00236 C21 1 -0.331903 0.776689 -0.129133 11.00000 0.05798 0.04016 = 0.03946 0.00172 -0.00240 0.02061 AFIX 43 H21 2 -0.379364 0.833144 -0.126437 11.00000 -1.20000 AFIX 0 C22 1 -0.299031 0.753159 -0.177243 11.00000 0.07743 0.04899 = 0.03417 0.01052 -0.00220 0.02514 AFIX 43 H22 2 -0.327687 0.793753 -0.207271 11.00000 -1.20000 AFIX 0 C23 1 -0.272120 0.731424 0.065129 11.00000 0.02897 0.02780 = 0.03325 -0.00180 0.00430 0.00431 C24 1 -0.246524 0.712235 0.014073 11.00000 0.02335 0.02538 = 0.03423 -0.00059 0.00372 0.00525 AFIX 43 H24 2 -0.178742 0.684745 0.010555 11.00000 -1.20000 AFIX 0 C25 1 -0.321102 0.733763 -0.031273 11.00000 0.02883 0.02531 = 0.03537 -0.00085 0.00453 0.00514 C26 1 -0.421859 0.773875 -0.025865 11.00000 0.02948 0.04219 = 0.04634 -0.00311 -0.00043 0.00786 AFIX 43 H26 2 -0.472628 0.788487 -0.056409 11.00000 -1.20000 AFIX 0 C27 1 -0.446855 0.792051 0.024349 11.00000 0.02796 0.05470 = 0.05283 -0.00572 0.01229 0.00867 AFIX 43 H27 2 -0.514984 0.818734 0.027807 11.00000 -1.20000 AFIX 0 C28 1 -0.372393 0.771359 0.070013 11.00000 0.04035 0.04204 = 0.04014 -0.00349 0.01259 0.01079 AFIX 43 H28 2 -0.390126 0.784455 0.104053 11.00000 -1.20000 HKLF 4 REM ip1353 in P2/n REM R1 = 0.0482 for 5041 Fo > 4sig(Fo) and 0.0667 for all 8401 data REM 439 parameters refined using 0 restraints END WGHT 0.0809 0.0000 REM Highest difference peak 0.709, deepest hole -0.541, 1-sigma level 0.073 Q1 1 -0.5422 1.0016 0.1534 11.00000 0.05 0.71 Q2 1 -0.4711 1.0075 0.2145 11.00000 0.05 0.45 Q3 1 -0.4964 1.1159 0.2140 11.00000 0.05 0.41 Q4 1 -0.5212 0.9056 0.2205 11.00000 0.05 0.37 Q5 1 0.1616 0.5350 0.0173 11.00000 0.05 0.31 Q6 1 -0.3542 1.1048 0.2052 11.00000 0.05 0.30 Q7 1 0.4350 0.9984 0.0589 11.00000 0.05 0.30 Q8 1 -0.2191 0.6780 0.0095 11.00000 0.05 0.28 ; _database_code_depnum_ccdc_archive 'CCDC 941555' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_(3) _audit_creation_method SHELXL-97 _chemical_name_systematic ; \m-Hexafluorosilicato-tetrakis[\m-1,3-bis(pyridazin-4-yl)benzene- \k^2^N^2^:N^2'^]-aqua-methanoldicopper(II) bis-perchlorate, solvate with 5.5 chloroform ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C57 H46 Cu2 F6 N16 O2 Si), 4(Cl O4), 11(C H Cl3)' _chemical_formula_sum 'C62.50 H51.50 Cl18.50 Cu2 F6 N16 O10 Si' _chemical_formula_weight 2111.69 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' Cl Cl 0.1484 0.1585 '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 monoclinic _symmetry_space_group_name_H-M 'P 21/c' _space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.8708(6) _cell_length_b 12.5785(5) _cell_length_c 50.263(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.272(3) _cell_angle_gamma 90.00 _cell_volume 8124.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 45147 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 26.02 _exptl_crystal_description prism _exptl_crystal_colour blue-green _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.14 _exptl_crystal_density_diffrn 1.726 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4236 _exptl_absorpt_coefficient_mu 1.227 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7656 _exptl_absorpt_correction_T_max 0.8470 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker APEXII area-detector diffractometer' _diffrn_measurement_method '\w scans' _diffrn_standards_decay_% 0 _diffrn_reflns_number 45147 _diffrn_reflns_av_R_equivalents 0.0892 _diffrn_reflns_av_sigmaI/netI 0.1157 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -56 _diffrn_reflns_limit_l_max 62 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 26.02 _reflns_number_total 15944 _reflns_number_gt 9456 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT (Bruker, 1998)' _computing_cell_refinement 'SAINT-NT (Bruker, 1999)' _computing_data_reduction 'SAINT-NT (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Diamond 2.1e (Brandenburg, 1999)' _computing_publication_material 'WinGX 1.70.01 (Farrugia, 1999)' #------------------------------- Refinement data-----------------------# _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. For the [{SiF6}Cu2(L)4(CH3OH)(H2O)]2+ portion of the structure, the refinement was standard. All the atoms were refined anisotropically, CH-hydrogen atoms were placed in calculated positions [d(C-H) = 0.95 A], the OH-hydrogen atoms were located and included in calculations with fixed d(O-H) = 0.85 A and Uiso = 1.5Ueq(O). Atoms of two non-coordinated ClO4- anions were also refined anisotropically. The most appreciable problems during the structure refinement were connected with the solvent chloroform molecules. It was possible to resolve disorder in the solvent regions. In total, there are 6 independent CHCl3 molecules, one of which lies across a centre of inversion (referenced by C61 carbon atom) and thus it is equally disordered by symmetry. Two other CHCl3 molecules (C62 and C63) are unequally disordered over two overlapping positions and refinement of thermal parametres in both the cases led to the partial contribution factors 0.60 and 0.40. It was possible to resolve the disorders without restrains in geometry parameters and to refine all solvent atoms anisotropically. To improve the stability of the model, the only constraint applied was uniform displacement parameters assigned to C62A and C62B carbon atoms. The hydrogen atoms were added geometrically and considering partial contributions of the disorder components. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0489P)^2^+28.7127P] 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 constr _refine_ls_extinction_method none _refine_ls_number_reflns 15944 _refine_ls_number_parameters 1130 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1395 _refine_ls_R_factor_gt 0.0793 _refine_ls_wR_factor_ref 0.1834 _refine_ls_wR_factor_gt 0.1639 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.09826(6) 0.18866(6) 0.448967(14) 0.02332(18) Uani 1 1 d . . . Cu2 Cu 0.11174(5) 0.18813(6) 0.293966(14) 0.02026(17) Uani 1 1 d . . . Si1 Si 0.10499(12) 0.18921(12) 0.37153(3) 0.0178(3) Uani 1 1 d . . . F1 F 0.1018(2) 0.1899(2) 0.40465(6) 0.0206(7) Uani 1 1 d . . . F2 F 0.1075(2) 0.1891(2) 0.33801(6) 0.0201(7) Uani 1 1 d . . . F3 F 0.1099(2) 0.0557(2) 0.37142(6) 0.0210(7) Uani 1 1 d . . . F4 F 0.2351(2) 0.1946(2) 0.37380(6) 0.0222(7) Uani 1 1 d . . . F5 F 0.0995(2) 0.3230(2) 0.37119(6) 0.0229(7) Uani 1 1 d . . . F6 F -0.0261(2) 0.1842(2) 0.36862(6) 0.0221(7) Uani 1 1 d . . . O1 O 0.1188(3) 0.1948(3) 0.49337(8) 0.0342(11) Uani 1 1 d . . . H1O H 0.1776 0.2208 0.4984 0.051 Uiso 1 1 d R . . O2 O 0.1121(3) 0.1989(3) 0.24886(8) 0.0301(10) Uani 1 1 d . . . H2O H 0.0897 0.2624 0.2474 0.045 Uiso 1 1 d R . . H3O H 0.1693 0.1950 0.2413 0.045 Uiso 1 1 d R . . N1 N -0.0205(4) 0.0849(4) 0.44397(10) 0.0247(12) Uani 1 1 d . . . N2 N -0.0851(4) 0.0766(4) 0.46429(10) 0.0331(13) Uani 1 1 d . . . N3 N -0.0034(4) 0.0724(4) 0.29536(9) 0.0211(11) Uani 1 1 d . . . N4 N -0.0600(4) 0.0573(4) 0.27222(10) 0.0264(12) Uani 1 1 d . . . N5 N 0.1993(4) 0.0595(4) 0.44629(10) 0.0267(12) Uani 1 1 d . . . N6 N 0.1898(5) -0.0165(4) 0.46503(11) 0.0377(14) Uani 1 1 d . . . N7 N 0.2263(4) 0.0771(4) 0.29846(9) 0.0213(11) Uani 1 1 d . . . N8 N 0.2544(4) 0.0311(4) 0.27567(10) 0.0291(12) Uani 1 1 d . . . N9 N 0.2225(4) 0.2896(4) 0.44724(10) 0.0244(12) Uani 1 1 d . . . N10 N 0.2880(4) 0.2869(4) 0.46905(11) 0.0341(13) Uani 1 1 d . . . N11 N 0.2244(4) 0.3071(4) 0.29918(10) 0.0249(11) Uani 1 1 d . . . N12 N 0.2811(4) 0.3254(4) 0.27772(10) 0.0299(12) Uani 1 1 d . . . N13 N -0.0015(4) 0.3175(4) 0.44205(9) 0.0244(11) Uani 1 1 d . . . N14 N 0.0044(4) 0.3946(4) 0.46057(10) 0.0295(12) Uani 1 1 d . . . N15 N -0.0035(4) 0.3003(4) 0.29402(10) 0.0241(11) Uani 1 1 d . . . N16 N -0.0178(4) 0.3565(4) 0.27123(10) 0.0281(12) Uani 1 1 d . . . C1 C -0.0366(5) 0.0267(5) 0.42197(12) 0.0227(13) Uani 1 1 d . . . H1 H 0.0117 0.0329 0.4085 0.027 Uiso 1 1 calc R . . C2 C -0.1210(5) -0.0433(5) 0.41757(12) 0.0252(14) Uani 1 1 d . . . C3 C -0.1842(5) -0.0539(5) 0.43881(13) 0.0362(17) Uani 1 1 d . . . H3 H -0.2412 -0.1020 0.4380 0.043 Uiso 1 1 calc R . . C4 C -0.1618(6) 0.0083(5) 0.46145(14) 0.0395(18) Uani 1 1 d . . . H4 H -0.2056 0.0005 0.4759 0.047 Uiso 1 1 calc R . . C5 C -0.0259(5) 0.0196(4) 0.31744(12) 0.0235(13) Uani 1 1 d . . . H5 H 0.0163 0.0320 0.3333 0.028 Uiso 1 1 calc R . . C6 C -0.1078(5) -0.0526(4) 0.31851(12) 0.0255(14) Uani 1 1 d . . . C7 C -0.1644(5) -0.0690(5) 0.29486(13) 0.0289(15) Uani 1 1 d . . . H7 H -0.2213 -0.1173 0.2938 0.035 Uiso 1 1 calc R . . C8 C -0.1362(5) -0.0128(5) 0.27236(12) 0.0304(15) Uani 1 1 d . . . H8 H -0.1748 -0.0260 0.2560 0.036 Uiso 1 1 calc R . . C9 C -0.1377(5) -0.1011(5) 0.39204(13) 0.0261(14) Uani 1 1 d . . . C10 C -0.1141(5) -0.0520(5) 0.36821(11) 0.0220(13) Uani 1 1 d . . . H10 H -0.0862 0.0179 0.3685 0.026 Uiso 1 1 calc R . . C11 C -0.1314(5) -0.1054(5) 0.34381(13) 0.0261(14) Uani 1 1 d . . . C12 C -0.1710(5) -0.2083(5) 0.34389(14) 0.0338(16) Uani 1 1 d . . . H12 H -0.1829 -0.2455 0.3275 0.041 Uiso 1 1 calc R . . C13 C -0.1931(6) -0.2565(5) 0.36734(14) 0.0377(17) Uani 1 1 d . . . H13 H -0.2207 -0.3266 0.3670 0.045 Uiso 1 1 calc R . . C14 C -0.1760(5) -0.2053(5) 0.39119(14) 0.0328(16) Uani 1 1 d . . . H14 H -0.1902 -0.2407 0.4073 0.039 Uiso 1 1 calc R . . C15 C 0.2627(5) 0.0452(5) 0.42647(12) 0.0244(14) Uani 1 1 d . . . H15 H 0.2670 0.1007 0.4138 0.029 Uiso 1 1 calc R . . C16 C 0.3226(5) -0.0449(5) 0.42307(12) 0.0284(15) Uani 1 1 d . . . C17 C 0.3153(6) -0.1208(6) 0.44291(13) 0.0368(17) Uani 1 1 d . . . H17 H 0.3560 -0.1838 0.4429 0.044 Uiso 1 1 calc R . . C18 C 0.2480(6) -0.1028(6) 0.46255(14) 0.0438(19) Uani 1 1 d . . . H18 H 0.2424 -0.1569 0.4756 0.053 Uiso 1 1 calc R . . C19 C 0.2747(5) 0.0507(5) 0.32197(12) 0.0244(14) Uani 1 1 d . . . H19 H 0.2555 0.0873 0.3375 0.029 Uiso 1 1 calc R . . C20 C 0.3511(5) -0.0271(5) 0.32487(12) 0.0259(14) Uani 1 1 d . . . C21 C 0.3771(5) -0.0763(5) 0.30188(13) 0.0315(15) Uani 1 1 d . . . H21 H 0.4271 -0.1319 0.3022 0.038 Uiso 1 1 calc R . . C22 C 0.3275(5) -0.0419(5) 0.27797(13) 0.0351(16) Uani 1 1 d . . . H22 H 0.3484 -0.0740 0.2620 0.042 Uiso 1 1 calc R . . C23 C 0.3859(5) -0.0599(5) 0.39998(12) 0.0275(14) Uani 1 1 d . . . C24 C 0.3436(5) -0.0352(5) 0.37443(12) 0.0273(14) Uani 1 1 d . . . H24 H 0.2750 -0.0073 0.3725 0.033 Uiso 1 1 calc R . . C25 C 0.3994(5) -0.0506(5) 0.35183(12) 0.0257(14) Uani 1 1 d . . . C26 C 0.4995(5) -0.0922(5) 0.35500(14) 0.0311(15) Uani 1 1 d . . . H26 H 0.5381 -0.1055 0.3398 0.037 Uiso 1 1 calc R . . C27 C 0.5434(5) -0.1145(5) 0.38044(14) 0.0303(15) Uani 1 1 d . . . H27 H 0.6131 -0.1393 0.3825 0.036 Uiso 1 1 calc R . . C28 C 0.4861(5) -0.1009(5) 0.40253(13) 0.0283(15) Uani 1 1 d . . . H28 H 0.5155 -0.1196 0.4197 0.034 Uiso 1 1 calc R . . C29 C 0.2429(5) 0.3494(5) 0.42650(12) 0.0243(14) Uani 1 1 d . . . H29 H 0.1932 0.3515 0.4118 0.029 Uiso 1 1 calc R . . C30 C 0.3335(5) 0.4096(5) 0.42509(12) 0.0266(14) Uani 1 1 d . . . C31 C 0.4001(5) 0.4065(6) 0.44753(14) 0.0377(17) Uani 1 1 d . . . H31 H 0.4634 0.4454 0.4483 0.045 Uiso 1 1 calc R . . C32 C 0.3725(6) 0.3450(6) 0.46906(14) 0.0417(18) Uani 1 1 d . . . H32 H 0.4176 0.3452 0.4847 0.050 Uiso 1 1 calc R . . C33 C 0.2447(5) 0.3586(4) 0.32190(12) 0.0226(13) Uani 1 1 d . . . H33 H 0.2011 0.3453 0.3362 0.027 Uiso 1 1 calc R . . C34 C 0.3262(5) 0.4311(5) 0.32620(12) 0.0231(13) Uani 1 1 d . . . C35 C 0.3834(5) 0.4511(5) 0.30437(12) 0.0285(15) Uani 1 1 d . . . H35 H 0.4384 0.5015 0.3053 0.034 Uiso 1 1 calc R . . C36 C 0.3580(5) 0.3952(5) 0.28097(13) 0.0341(16) Uani 1 1 d . . . H36 H 0.3991 0.4081 0.2662 0.041 Uiso 1 1 calc R . . C37 C 0.3538(5) 0.4714(5) 0.40076(13) 0.0263(14) Uani 1 1 d . . . C38 C 0.3292(5) 0.4272(5) 0.37597(12) 0.0259(14) Uani 1 1 d . . . H38 H 0.2994 0.3581 0.3749 0.031 Uiso 1 1 calc R . . C39 C 0.3475(4) 0.4828(5) 0.35213(12) 0.0238(14) Uani 1 1 d . . . C40 C 0.3888(5) 0.5835(5) 0.35457(14) 0.0338(16) Uani 1 1 d . . . H40 H 0.4002 0.6234 0.3389 0.041 Uiso 1 1 calc R . . C41 C 0.4142(5) 0.6281(5) 0.37934(14) 0.0355(17) Uani 1 1 d . . . H41 H 0.4430 0.6976 0.3805 0.043 Uiso 1 1 calc R . . C42 C 0.3979(5) 0.5721(5) 0.40216(14) 0.0338(16) Uani 1 1 d . . . H42 H 0.4170 0.6024 0.4190 0.041 Uiso 1 1 calc R . . C43 C -0.0632(5) 0.3275(5) 0.42022(12) 0.0240(14) Uani 1 1 d . . . H43 H -0.0670 0.2701 0.4079 0.029 Uiso 1 1 calc R . . C44 C -0.1231(5) 0.4180(4) 0.41430(12) 0.0237(14) Uani 1 1 d . . . C45 C -0.1198(5) 0.4968(5) 0.43348(13) 0.0303(15) Uani 1 1 d . . . H45 H -0.1610 0.5592 0.4314 0.036 Uiso 1 1 calc R . . C46 C -0.0536(5) 0.4809(5) 0.45609(13) 0.0322(16) Uani 1 1 d . . . H46 H -0.0498 0.5355 0.4692 0.039 Uiso 1 1 calc R . . C47 C -0.0586(5) 0.3204(5) 0.31477(12) 0.0244(13) Uani 1 1 d . . . H47 H -0.0482 0.2768 0.3301 0.029 Uiso 1 1 calc R . . C48 C -0.1320(5) 0.4031(5) 0.31536(12) 0.0236(14) Uani 1 1 d . . . C49 C -0.1493(5) 0.4596(5) 0.29193(13) 0.0298(15) Uani 1 1 d . . . H49 H -0.2007 0.5139 0.2903 0.036 Uiso 1 1 calc R . . C50 C -0.0884(5) 0.4338(5) 0.27073(13) 0.0315(15) Uani 1 1 d . . . H50 H -0.0981 0.4743 0.2548 0.038 Uiso 1 1 calc R . . C51 C -0.1837(5) 0.4322(4) 0.38852(12) 0.0250(14) Uani 1 1 d . . . C52 C -0.1363(5) 0.4069(5) 0.36462(12) 0.0232(13) Uani 1 1 d . . . H52 H -0.0682 0.3774 0.3654 0.028 Uiso 1 1 calc R . . C53 C -0.1874(5) 0.4243(4) 0.34013(12) 0.0244(14) Uani 1 1 d . . . C54 C -0.2878(5) 0.4660(5) 0.33916(14) 0.0323(15) Uani 1 1 d . . . H54 H -0.3237 0.4790 0.3224 0.039 Uiso 1 1 calc R . . C55 C -0.3350(5) 0.4883(5) 0.36227(14) 0.0336(16) Uani 1 1 d . . . H55 H -0.4043 0.5148 0.3614 0.040 Uiso 1 1 calc R . . C56 C -0.2834(5) 0.4729(5) 0.38702(13) 0.0292(15) Uani 1 1 d . . . H56 H -0.3166 0.4904 0.4028 0.035 Uiso 1 1 calc R . . C57 C 0.0435(5) 0.2208(6) 0.51198(13) 0.0400(18) Uani 1 1 d . . . H57A H 0.0107 0.2888 0.5070 0.060 Uiso 1 1 calc R . . H57B H 0.0776 0.2265 0.5299 0.060 Uiso 1 1 calc R . . H57C H -0.0096 0.1649 0.5119 0.060 Uiso 1 1 calc R . . Cl1 Cl 0.40515(12) 0.18908(13) 0.21488(3) 0.0314(4) Uani 1 1 d . . . O3 O 0.2936(4) 0.1920(4) 0.21470(10) 0.0503(14) Uani 1 1 d . . . O4 O 0.4384(5) 0.0926(6) 0.22789(15) 0.098(3) Uani 1 1 d . . . O5 O 0.4478(6) 0.2752(6) 0.22910(15) 0.110(3) Uani 1 1 d . . . O6 O 0.4387(5) 0.1885(5) 0.18833(10) 0.0609(16) Uani 1 1 d . . . Cl2 Cl 0.36304(12) 0.16994(13) 0.04969(3) 0.0318(4) Uani 1 1 d . . . O7 O 0.3572(5) 0.1878(5) 0.07745(11) 0.0676(17) Uani 1 1 d . . . O8 O 0.3852(5) 0.0610(5) 0.04568(14) 0.077(2) Uani 1 1 d . . . O9 O 0.2646(5) 0.1949(5) 0.03673(13) 0.0775(19) Uani 1 1 d . . . O10 O 0.4440(5) 0.2338(5) 0.04079(13) 0.084(2) Uani 1 1 d . . . C58 C 0.2771(5) -0.1018(6) 0.00602(14) 0.0371(17) Uani 1 1 d . . . H58 H 0.3026 -0.0519 0.0204 0.045 Uiso 1 1 calc R . . Cl3 Cl 0.38383(14) -0.14033(16) -0.01215(4) 0.0484(5) Uani 1 1 d . . . Cl4 Cl 0.18456(15) -0.03503(19) -0.01483(4) 0.0617(6) Uani 1 1 d . . . Cl5 Cl 0.22119(16) -0.21228(14) 0.02079(4) 0.0492(5) Uani 1 1 d . . . C59 C 0.8781(6) 0.1812(6) 0.21415(15) 0.049(2) Uani 1 1 d . . . H59 H 0.9243 0.1663 0.2304 0.059 Uiso 1 1 calc R . . Cl6 Cl 0.74846(19) 0.17426(18) 0.22251(5) 0.0734(7) Uani 1 1 d . . . Cl7 Cl 0.90592(18) 0.30757(16) 0.20231(5) 0.0615(6) Uani 1 1 d . . . Cl8 Cl 0.90129(19) 0.08571(18) 0.18968(6) 0.0767(8) Uani 1 1 d . . . C60 C 0.5559(7) 0.1811(6) 0.28876(17) 0.055(2) Uani 1 1 d . . . H60 H 0.5005 0.1936 0.2743 0.066 Uiso 1 1 calc R . . Cl9 Cl 0.6536(3) 0.2727(3) 0.28471(6) 0.1359(16) Uani 1 1 d . . . Cl10 Cl 0.60123(19) 0.0490(2) 0.28536(5) 0.0768(7) Uani 1 1 d . . . Cl11 Cl 0.50073(19) 0.19914(17) 0.31881(5) 0.0695(7) Uani 1 1 d . . . C61 C 0.5068(19) 0.032(2) 0.5078(7) 0.127(12) Uani 0.50 1 d P . . H61A H 0.5514 0.0845 0.5163 0.152 Uiso 0.50 1 d PR . . Cl12 Cl 0.5762(8) -0.0571(8) 0.49140(19) 0.124(3) Uani 0.50 1 d P . . Cl13 Cl 0.4495(6) -0.0617(7) 0.53470(14) 0.129(3) Uani 0.50 1 d P . . Cl14 Cl 0.4068(7) 0.0866(6) 0.49258(16) 0.111(3) Uani 0.50 1 d P . . C62A C 0.3884(14) -0.2798(13) 0.1107(4) 0.088(5) Uani 0.60 1 d P A -1 H62A H 0.3828 -0.2084 0.1192 0.105 Uiso 0.60 1 calc PR A -1 Cl1A Cl 0.3430(5) -0.2611(6) 0.07734(10) 0.124(2) Uani 0.60 1 d P A -1 Cl2A Cl 0.5152(3) -0.3100(4) 0.11335(9) 0.0586(10) Uani 0.60 1 d P A -1 Cl3A Cl 0.3048(7) -0.3572(9) 0.1259(2) 0.119(3) Uani 0.60 1 d P A -1 C62B C 0.402(2) -0.348(2) 0.1027(7) 0.088(5) Uani 0.40 1 d P . -2 H62B H 0.4296 -0.4147 0.1116 0.105 Uiso 0.40 1 calc PR . -2 Cl1B Cl 0.4917(5) -0.2434(6) 0.11201(15) 0.0700(19) Uani 0.40 1 d P . -2 Cl2B Cl 0.2872(10) -0.3340(10) 0.1106(4) 0.143(8) Uani 0.40 1 d P . -2 Cl3B Cl 0.4119(8) -0.3665(7) 0.06577(17) 0.118(3) Uani 0.40 1 d P . -2 C63A C 0.9236(16) 0.1974(11) 0.1082(3) 0.062(4) Uani 0.60 1 d P B -3 H63A H 0.9939 0.2145 0.1166 0.075 Uiso 0.60 1 calc PR B -3 Cl4A Cl 0.9045(6) 0.0630(8) 0.1144(2) 0.0583(18) Uani 0.60 1 d P B -3 Cl5A Cl 0.9322(4) 0.2236(4) 0.07412(11) 0.0667(13) Uani 0.60 1 d P B -3 Cl6A Cl 0.8405(5) 0.2781(6) 0.12299(16) 0.085(2) Uani 0.60 1 d P B -3 C63B C 0.8561(19) 0.1754(19) 0.1046(6) 0.071(9) Uani 0.40 1 d P C -4 H63B H 0.7828 0.1562 0.1081 0.086 Uiso 0.40 1 calc PR C -4 Cl4B Cl 0.9425(11) 0.0801(12) 0.1205(4) 0.091(5) Uani 0.40 1 d P C -4 Cl5B Cl 0.8704(10) 0.1707(10) 0.07254(19) 0.136(4) Uani 0.40 1 d P C -4 Cl6B Cl 0.8873(6) 0.2987(9) 0.1199(3) 0.072(3) Uani 0.40 1 d P C -4 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 0.0264(4) 0.0239(4) 0.0198(4) -0.0007(3) 0.0028(3) -0.0012(3) Cu2 0.0224(4) 0.0211(4) 0.0173(4) -0.0004(3) 0.0008(3) -0.0012(3) Si1 0.0187(8) 0.0159(7) 0.0187(8) -0.0001(7) 0.0004(6) -0.0015(7) F1 0.0226(17) 0.0233(17) 0.0159(16) 0.0001(14) 0.0002(14) -0.0012(15) F2 0.0230(17) 0.0192(16) 0.0179(16) -0.0008(14) -0.0013(14) -0.0021(14) F3 0.0252(18) 0.0195(16) 0.0187(17) -0.0010(14) 0.0041(14) -0.0009(15) F4 0.0186(17) 0.0250(17) 0.0235(18) 0.0005(15) 0.0059(14) -0.0016(15) F5 0.0232(17) 0.0169(16) 0.0287(18) 0.0007(15) 0.0015(14) -0.0002(14) F6 0.0186(16) 0.0228(17) 0.0246(18) 0.0007(15) 0.0001(14) -0.0034(14) O1 0.033(3) 0.045(3) 0.025(2) 0.001(2) 0.002(2) -0.003(2) O2 0.036(3) 0.031(2) 0.024(2) -0.001(2) 0.007(2) -0.004(2) N1 0.029(3) 0.023(3) 0.023(3) 0.003(2) 0.006(2) 0.000(2) N2 0.040(3) 0.033(3) 0.028(3) 0.005(3) 0.017(3) -0.005(3) N3 0.023(3) 0.023(3) 0.017(3) -0.002(2) 0.001(2) 0.000(2) N4 0.026(3) 0.032(3) 0.020(3) -0.006(2) -0.007(2) -0.002(2) N5 0.030(3) 0.031(3) 0.020(3) 0.003(2) 0.004(2) 0.001(2) N6 0.051(4) 0.033(3) 0.031(3) 0.008(3) 0.012(3) 0.009(3) N7 0.023(3) 0.020(3) 0.020(3) -0.004(2) 0.000(2) -0.002(2) N8 0.038(3) 0.028(3) 0.022(3) -0.008(2) 0.007(2) 0.003(3) N9 0.024(3) 0.024(3) 0.026(3) -0.002(2) -0.002(2) 0.002(2) N10 0.028(3) 0.037(3) 0.037(3) -0.005(3) -0.003(3) -0.003(3) N11 0.028(3) 0.025(3) 0.022(3) 0.004(2) 0.004(2) 0.000(2) N12 0.030(3) 0.037(3) 0.024(3) 0.003(3) 0.007(2) -0.002(3) N13 0.028(3) 0.026(3) 0.019(3) -0.006(2) 0.006(2) 0.001(2) N14 0.033(3) 0.028(3) 0.027(3) -0.005(2) 0.002(2) -0.005(2) N15 0.028(3) 0.018(3) 0.026(3) 0.003(2) -0.002(2) 0.000(2) N16 0.033(3) 0.032(3) 0.019(3) 0.003(2) -0.002(2) 0.001(3) C1 0.024(3) 0.025(3) 0.020(3) 0.004(3) 0.006(3) -0.003(3) C2 0.024(3) 0.020(3) 0.032(4) 0.006(3) 0.001(3) 0.000(3) C3 0.040(4) 0.034(4) 0.035(4) -0.002(3) 0.012(3) -0.006(3) C4 0.048(5) 0.040(4) 0.033(4) 0.000(3) 0.022(3) -0.009(4) C5 0.027(3) 0.018(3) 0.026(3) -0.005(3) 0.001(3) -0.003(3) C6 0.030(3) 0.015(3) 0.031(4) -0.005(3) 0.003(3) 0.002(3) C7 0.027(3) 0.025(3) 0.034(4) -0.001(3) 0.003(3) 0.001(3) C8 0.036(4) 0.033(4) 0.020(3) 0.001(3) -0.011(3) -0.004(3) C9 0.018(3) 0.023(3) 0.039(4) 0.001(3) 0.009(3) -0.004(3) C10 0.025(3) 0.017(3) 0.024(3) 0.003(3) -0.002(3) -0.003(3) C11 0.019(3) 0.022(3) 0.037(4) -0.001(3) -0.004(3) -0.001(3) C12 0.039(4) 0.026(4) 0.035(4) -0.006(3) -0.003(3) -0.010(3) C13 0.049(5) 0.023(3) 0.041(4) 0.005(3) 0.002(4) -0.014(3) C14 0.039(4) 0.025(3) 0.034(4) 0.004(3) 0.003(3) -0.008(3) C15 0.028(3) 0.023(3) 0.021(3) 0.006(3) -0.003(3) 0.003(3) C16 0.030(4) 0.028(3) 0.027(4) -0.003(3) 0.004(3) -0.002(3) C17 0.046(4) 0.036(4) 0.029(4) 0.007(3) 0.005(3) 0.008(3) C18 0.057(5) 0.039(4) 0.036(4) 0.014(3) 0.015(4) 0.019(4) C19 0.027(3) 0.021(3) 0.026(3) -0.002(3) 0.007(3) 0.001(3) C20 0.023(3) 0.027(3) 0.028(4) -0.003(3) 0.002(3) -0.005(3) C21 0.032(4) 0.033(4) 0.029(4) -0.002(3) 0.006(3) 0.003(3) C22 0.038(4) 0.042(4) 0.026(4) -0.010(3) 0.006(3) 0.004(3) C23 0.030(4) 0.024(3) 0.029(4) 0.002(3) 0.002(3) 0.002(3) C24 0.029(3) 0.025(3) 0.028(4) 0.003(3) 0.002(3) 0.006(3) C25 0.032(4) 0.018(3) 0.028(3) 0.006(3) 0.008(3) 0.007(3) C26 0.025(3) 0.029(3) 0.040(4) -0.004(3) 0.008(3) 0.003(3) C27 0.021(3) 0.026(3) 0.044(4) -0.001(3) 0.000(3) 0.001(3) C28 0.033(4) 0.022(3) 0.028(4) -0.002(3) -0.004(3) -0.001(3) C29 0.026(3) 0.025(3) 0.022(3) -0.010(3) 0.000(3) -0.001(3) C30 0.024(3) 0.033(4) 0.022(3) -0.012(3) 0.001(3) -0.003(3) C31 0.026(4) 0.041(4) 0.046(4) -0.006(4) 0.002(3) -0.007(3) C32 0.037(4) 0.052(5) 0.035(4) -0.004(4) -0.006(3) -0.004(4) C33 0.031(3) 0.019(3) 0.019(3) 0.002(3) 0.008(3) 0.001(3) C34 0.022(3) 0.021(3) 0.027(3) 0.001(3) 0.006(3) 0.000(3) C35 0.030(4) 0.027(3) 0.029(4) 0.003(3) 0.004(3) -0.008(3) C36 0.031(4) 0.040(4) 0.033(4) 0.004(3) 0.011(3) -0.004(3) C37 0.017(3) 0.025(3) 0.037(4) -0.005(3) 0.005(3) -0.008(3) C38 0.025(3) 0.022(3) 0.031(4) -0.005(3) 0.009(3) -0.006(3) C39 0.017(3) 0.021(3) 0.034(4) -0.003(3) 0.002(3) -0.004(2) C40 0.028(4) 0.028(4) 0.046(4) 0.005(3) 0.009(3) -0.004(3) C41 0.037(4) 0.026(4) 0.044(4) -0.008(3) 0.006(3) -0.016(3) C42 0.028(4) 0.027(3) 0.047(4) -0.010(3) 0.012(3) -0.003(3) C43 0.026(3) 0.023(3) 0.024(3) -0.009(3) 0.010(3) -0.003(3) C44 0.023(3) 0.019(3) 0.030(4) 0.001(3) 0.008(3) -0.003(3) C45 0.029(4) 0.028(3) 0.034(4) -0.002(3) 0.009(3) -0.006(3) C46 0.035(4) 0.028(4) 0.034(4) -0.006(3) 0.008(3) -0.004(3) C47 0.027(3) 0.023(3) 0.022(3) 0.001(3) -0.004(3) -0.004(3) C48 0.021(3) 0.022(3) 0.028(3) -0.003(3) 0.001(3) 0.000(3) C49 0.032(4) 0.022(3) 0.035(4) 0.011(3) -0.001(3) 0.011(3) C50 0.039(4) 0.035(4) 0.021(3) 0.007(3) 0.002(3) 0.001(3) C51 0.029(3) 0.016(3) 0.030(4) -0.003(3) 0.006(3) -0.002(3) C52 0.022(3) 0.025(3) 0.022(3) -0.003(3) 0.000(3) 0.000(3) C53 0.024(3) 0.018(3) 0.031(4) 0.001(3) -0.002(3) -0.001(3) C54 0.024(3) 0.032(4) 0.040(4) 0.003(3) -0.001(3) 0.000(3) C55 0.020(3) 0.036(4) 0.044(4) -0.008(3) -0.001(3) 0.005(3) C56 0.027(3) 0.027(3) 0.035(4) -0.006(3) 0.011(3) 0.002(3) C57 0.036(4) 0.057(5) 0.029(4) -0.001(3) 0.008(3) 0.006(4) Cl1 0.0325(9) 0.0336(8) 0.0287(8) -0.0035(8) 0.0074(7) -0.0004(7) O3 0.034(3) 0.072(4) 0.045(3) -0.001(3) 0.009(2) 0.006(3) O4 0.087(5) 0.109(6) 0.101(5) 0.066(5) 0.036(4) 0.059(4) O5 0.108(6) 0.123(6) 0.105(6) -0.071(5) 0.060(5) -0.082(5) O6 0.063(4) 0.088(4) 0.034(3) -0.010(3) 0.019(3) -0.004(3) Cl2 0.0275(8) 0.0352(9) 0.0331(9) -0.0040(7) 0.0049(7) 0.0036(7) O7 0.076(4) 0.077(4) 0.053(4) -0.016(3) 0.030(3) -0.011(3) O8 0.065(4) 0.051(4) 0.113(5) -0.044(4) -0.022(4) 0.018(3) O9 0.059(4) 0.089(5) 0.081(5) 0.021(4) -0.026(3) 0.019(4) O10 0.080(5) 0.093(5) 0.085(5) -0.020(4) 0.049(4) -0.047(4) C58 0.030(4) 0.047(4) 0.034(4) -0.007(3) 0.000(3) 0.004(3) Cl3 0.0328(10) 0.0603(12) 0.0527(12) -0.0038(10) 0.0074(9) 0.0021(9) Cl4 0.0365(11) 0.0891(16) 0.0595(13) 0.0310(12) 0.0033(10) 0.0099(11) Cl5 0.0604(13) 0.0412(11) 0.0482(11) 0.0034(9) 0.0217(10) 0.0084(9) C59 0.063(5) 0.045(4) 0.038(4) 0.012(4) -0.004(4) -0.017(4) Cl6 0.0642(15) 0.0610(14) 0.0976(19) 0.0186(13) 0.0270(14) -0.0092(12) Cl7 0.0724(15) 0.0442(11) 0.0683(14) 0.0090(11) 0.0081(12) -0.0221(11) Cl8 0.0651(15) 0.0544(14) 0.109(2) -0.0277(14) -0.0051(14) 0.0067(12) C60 0.056(5) 0.053(5) 0.054(5) 0.007(4) -0.006(4) -0.016(4) Cl9 0.191(4) 0.144(3) 0.079(2) -0.0294(19) 0.056(2) -0.128(3) Cl10 0.0641(15) 0.0818(17) 0.0868(18) 0.0032(14) 0.0253(13) 0.0261(13) Cl11 0.0735(16) 0.0498(13) 0.0881(18) 0.0066(12) 0.0301(14) 0.0026(11) C61 0.046(13) 0.10(2) 0.23(4) -0.09(2) -0.010(18) 0.022(14) Cl12 0.119(7) 0.146(7) 0.112(7) 0.019(6) 0.038(6) 0.046(6) Cl13 0.111(5) 0.185(8) 0.094(5) 0.024(5) 0.020(4) -0.052(5) Cl14 0.131(6) 0.094(5) 0.102(6) -0.012(4) -0.050(5) 0.014(4) C62A 0.065(9) 0.039(8) 0.156(16) 0.009(10) -0.026(10) 0.018(8) Cl1A 0.124(5) 0.183(6) 0.064(3) -0.007(3) -0.015(3) 0.080(5) Cl2A 0.047(2) 0.060(2) 0.068(3) -0.005(2) -0.0010(18) 0.002(2) Cl3A 0.042(4) 0.155(9) 0.160(7) 0.019(5) 0.002(4) -0.026(4) C62B 0.065(9) 0.039(8) 0.156(16) 0.009(10) -0.026(10) 0.018(8) Cl1B 0.052(4) 0.072(4) 0.087(5) -0.012(4) 0.010(3) -0.023(4) Cl2B 0.050(5) 0.060(5) 0.32(2) 0.001(10) -0.012(10) -0.013(4) Cl3B 0.149(8) 0.097(6) 0.100(6) -0.009(5) -0.064(6) 0.004(6) C63A 0.091(13) 0.033(8) 0.064(10) 0.006(7) 0.017(10) -0.006(9) Cl4A 0.056(4) 0.040(2) 0.079(4) -0.003(2) 0.008(3) -0.002(3) Cl5A 0.072(3) 0.063(3) 0.066(3) 0.016(2) 0.010(2) -0.006(2) Cl6A 0.105(5) 0.062(4) 0.089(4) -0.008(3) 0.015(5) 0.042(4) C63B 0.046(14) 0.063(16) 0.11(2) -0.035(14) 0.019(14) -0.046(13) Cl4B 0.115(12) 0.063(9) 0.101(11) 0.019(7) 0.042(9) 0.047(8) Cl5B 0.173(11) 0.158(10) 0.075(6) -0.035(7) -0.016(7) 0.099(9) Cl6B 0.054(5) 0.057(4) 0.109(7) -0.044(4) 0.018(5) -0.003(4) _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 N1 2.015(5) . ? Cu1 N9 2.047(5) . ? Cu1 N13 2.085(5) . ? Cu1 N5 2.090(5) . ? Cu1 F1 2.231(3) . ? Cu1 O1 2.234(4) . ? Cu2 N7 2.034(5) . ? Cu2 N15 2.047(5) . ? Cu2 N3 2.081(5) . ? Cu2 N11 2.090(5) . ? Cu2 F2 2.218(3) . ? Cu2 O2 2.271(4) . ? Si1 F1 1.668(3) . ? Si1 F4 1.673(3) . ? Si1 F3 1.681(3) . ? Si1 F5 1.684(3) . ? Si1 F6 1.686(3) . ? Si1 F2 1.687(3) . ? O1 C57 1.423(7) . ? O1 H1O 0.8500 . ? O2 H2O 0.8500 . ? O2 H3O 0.8500 . ? N1 C1 1.333(7) . ? N1 N2 1.358(6) . ? N2 C4 1.310(8) . ? N3 C5 1.339(7) . ? N3 N4 1.350(6) . ? N4 C8 1.320(8) . ? N5 C15 1.336(7) . ? N5 N6 1.353(7) . ? N6 C18 1.329(8) . ? N7 C19 1.346(7) . ? N7 N8 1.351(6) . ? N8 C22 1.316(8) . ? N9 C29 1.324(8) . ? N9 N10 1.345(7) . ? N10 C32 1.310(9) . ? N11 C33 1.326(7) . ? N11 N12 1.356(6) . ? N12 C36 1.326(8) . ? N13 C43 1.323(8) . ? N13 N14 1.343(7) . ? N14 C46 1.330(8) . ? N15 C47 1.319(7) . ? N15 N16 1.350(7) . ? N16 C50 1.330(8) . ? C1 C2 1.405(8) . ? C1 H1 0.9500 . ? C2 C3 1.385(8) . ? C2 C9 1.480(9) . ? C3 C4 1.397(9) . ? C3 H3 0.9500 . ? C4 H4 0.9500 . ? C5 C6 1.395(8) . ? C5 H5 0.9500 . ? C6 C7 1.374(9) . ? C6 C11 1.482(9) . ? C7 C8 1.399(9) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C10 1.397(8) . ? C9 C14 1.400(8) . ? C10 C11 1.405(8) . ? C10 H10 0.9500 . ? C11 C12 1.391(8) . ? C12 C13 1.370(9) . ? C12 H12 0.9500 . ? C13 C14 1.367(9) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.386(8) . ? C15 H15 0.9500 . ? C16 C17 1.388(9) . ? C16 C23 1.468(8) . ? C17 C18 1.369(9) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.389(8) . ? C19 H19 0.9500 . ? C20 C21 1.369(8) . ? C20 C25 1.488(9) . ? C21 C22 1.397(9) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C28 1.388(9) . ? C23 C24 1.401(8) . ? C24 C25 1.392(8) . ? C24 H24 0.9500 . ? C25 C26 1.392(8) . ? C26 C27 1.396(9) . ? C26 H26 0.9500 . ? C27 C28 1.378(9) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C30 1.396(8) . ? C29 H29 0.9500 . ? C30 C31 1.377(9) . ? C30 C37 1.484(9) . ? C31 C32 1.393(10) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C34 1.398(8) . ? C33 H33 0.9500 . ? C34 C35 1.378(8) . ? C34 C39 1.469(8) . ? C35 C36 1.393(9) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C38 1.385(8) . ? C37 C42 1.388(8) . ? C38 C39 1.419(8) . ? C38 H38 0.9500 . ? C39 C40 1.377(8) . ? C40 C41 1.387(9) . ? C40 H40 0.9500 . ? C41 C42 1.372(9) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C44 1.397(8) . ? C43 H43 0.9500 . ? C44 C45 1.382(8) . ? C44 C51 1.485(9) . ? C45 C46 1.395(9) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 C48 1.406(8) . ? C47 H47 0.9500 . ? C48 C49 1.383(8) . ? C48 C53 1.494(8) . ? C49 C50 1.397(9) . ? C49 H49 0.9500 . ? C50 H50 0.9500 . ? C51 C56 1.379(8) . ? C51 C52 1.415(8) . ? C52 C53 1.380(8) . ? C52 H52 0.9500 . ? C53 C54 1.394(8) . ? C54 C55 1.370(9) . ? C54 H54 0.9500 . ? C55 C56 1.391(9) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? Cl1 O5 1.393(6) . ? Cl1 O6 1.425(5) . ? Cl1 O4 1.432(6) . ? Cl1 O3 1.436(5) . ? Cl2 O10 1.409(6) . ? Cl2 O8 1.416(5) . ? Cl2 O7 1.420(6) . ? Cl2 O9 1.426(6) . ? C58 Cl5 1.750(7) . ? C58 Cl4 1.755(7) . ? C58 Cl3 1.760(7) . ? C58 H58 1.0000 . ? C59 Cl7 1.741(7) . ? C59 Cl6 1.746(8) . ? C59 Cl8 1.757(8) . ? C59 H59 1.0000 . ? C60 Cl11 1.720(9) . ? C60 Cl9 1.726(8) . ? C60 Cl10 1.772(9) . ? C60 H60 1.0000 . ? C61 Cl12 1.12(2) 3_656 ? C61 Cl14 1.61(3) . ? C61 Cl12 1.68(2) . ? C61 Cl13 1.97(4) . ? C61 H61A 0.9601 . ? C62A Cl3A 1.67(2) . ? C62A Cl2A 1.674(17) . ? C62A Cl1A 1.76(2) . ? C62A H62A 1.0000 . ? C62B Cl2B 1.57(3) . ? C62B Cl1B 1.79(3) . ? C62B Cl3B 1.88(3) . ? C62B H62B 1.0000 . ? Cl3B Cl13 1.890(11) 4 ? C63A Cl6A 1.679(17) . ? C63A Cl4A 1.739(17) . ? C63A Cl5A 1.754(16) . ? C63A H63A 1.0000 . ? C63B Cl5B 1.63(3) . ? C63B Cl6B 1.77(2) . ? C63B Cl4B 1.79(3) . ? C63B H63B 1.0000 . ? 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 N1 Cu1 N9 170.1(2) . . ? N1 Cu1 N13 91.6(2) . . ? N9 Cu1 N13 89.18(19) . . ? N1 Cu1 N5 87.6(2) . . ? N9 Cu1 N5 89.38(19) . . ? N13 Cu1 N5 166.70(19) . . ? N1 Cu1 F1 86.49(16) . . ? N9 Cu1 F1 83.84(16) . . ? N13 Cu1 F1 82.85(15) . . ? N5 Cu1 F1 83.86(16) . . ? N1 Cu1 O1 101.11(18) . . ? N9 Cu1 O1 88.44(18) . . ? N13 Cu1 O1 100.18(17) . . ? N5 Cu1 O1 92.99(18) . . ? F1 Cu1 O1 171.68(14) . . ? N7 Cu2 N15 173.56(19) . . ? N7 Cu2 N3 91.68(19) . . ? N15 Cu2 N3 87.97(18) . . ? N7 Cu2 N11 89.09(19) . . ? N15 Cu2 N11 90.23(19) . . ? N3 Cu2 N11 170.71(18) . . ? N7 Cu2 F2 87.25(16) . . ? N15 Cu2 F2 86.31(16) . . ? N3 Cu2 F2 84.96(15) . . ? N11 Cu2 F2 85.83(15) . . ? N7 Cu2 O2 96.26(17) . . ? N15 Cu2 O2 90.16(18) . . ? N3 Cu2 O2 96.75(17) . . ? N11 Cu2 O2 92.36(17) . . ? F2 Cu2 O2 176.03(14) . . ? F1 Si1 F4 90.76(17) . . ? F1 Si1 F3 90.67(17) . . ? F4 Si1 F3 90.16(17) . . ? F1 Si1 F5 90.08(17) . . ? F4 Si1 F5 90.11(17) . . ? F3 Si1 F5 179.2(2) . . ? F1 Si1 F6 90.31(17) . . ? F4 Si1 F6 178.92(18) . . ? F3 Si1 F6 89.99(17) . . ? F5 Si1 F6 89.73(17) . . ? F1 Si1 F2 179.6(2) . . ? F4 Si1 F2 89.54(16) . . ? F3 Si1 F2 89.60(16) . . ? F5 Si1 F2 89.64(17) . . ? F6 Si1 F2 89.39(17) . . ? Si1 F1 Cu1 179.3(2) . . ? Si1 F2 Cu2 179.6(2) . . ? C57 O1 Cu1 128.2(4) . . ? C57 O1 H1O 110.1 . . ? Cu1 O1 H1O 111.4 . . ? Cu2 O2 H2O 97.0 . . ? Cu2 O2 H3O 119.7 . . ? H2O O2 H3O 108.4 . . ? C1 N1 N2 120.6(5) . . ? C1 N1 Cu1 122.7(4) . . ? N2 N1 Cu1 116.7(4) . . ? C4 N2 N1 117.3(5) . . ? C5 N3 N4 120.8(5) . . ? C5 N3 Cu2 124.2(4) . . ? N4 N3 Cu2 114.8(4) . . ? C8 N4 N3 117.0(5) . . ? C15 N5 N6 120.5(5) . . ? C15 N5 Cu1 124.2(4) . . ? N6 N5 Cu1 115.1(4) . . ? C18 N6 N5 116.0(5) . . ? C19 N7 N8 120.4(5) . . ? C19 N7 Cu2 124.3(4) . . ? N8 N7 Cu2 115.3(4) . . ? C22 N8 N7 116.7(5) . . ? C29 N9 N10 120.9(5) . . ? C29 N9 Cu1 125.2(4) . . ? N10 N9 Cu1 113.9(4) . . ? C32 N10 N9 117.9(6) . . ? C33 N11 N12 120.9(5) . . ? C33 N11 Cu2 124.0(4) . . ? N12 N11 Cu2 115.0(4) . . ? C36 N12 N11 116.5(5) . . ? C43 N13 N14 120.9(5) . . ? C43 N13 Cu1 123.2(4) . . ? N14 N13 Cu1 115.9(4) . . ? C46 N14 N13 117.6(5) . . ? C47 N15 N16 121.1(5) . . ? C47 N15 Cu2 123.8(4) . . ? N16 N15 Cu2 115.1(4) . . ? C50 N16 N15 117.3(5) . . ? N1 C1 C2 123.9(5) . . ? N1 C1 H1 118.1 . . ? C2 C1 H1 118.1 . . ? C3 C2 C1 114.9(6) . . ? C3 C2 C9 123.9(6) . . ? C1 C2 C9 121.1(5) . . ? C2 C3 C4 118.1(6) . . ? C2 C3 H3 121.0 . . ? C4 C3 H3 121.0 . . ? N2 C4 C3 125.1(6) . . ? N2 C4 H4 117.4 . . ? C3 C4 H4 117.4 . . ? N3 C5 C6 123.7(6) . . ? N3 C5 H5 118.2 . . ? C6 C5 H5 118.2 . . ? C7 C6 C5 115.4(6) . . ? C7 C6 C11 123.4(6) . . ? C5 C6 C11 121.2(6) . . ? C6 C7 C8 118.3(6) . . ? C6 C7 H7 120.9 . . ? C8 C7 H7 120.9 . . ? N4 C8 C7 124.7(6) . . ? N4 C8 H8 117.7 . . ? C7 C8 H8 117.7 . . ? C10 C9 C14 118.8(6) . . ? C10 C9 C2 119.9(5) . . ? C14 C9 C2 121.4(6) . . ? C9 C10 C11 120.4(5) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C12 C11 C10 118.8(6) . . ? C12 C11 C6 120.9(6) . . ? C10 C11 C6 120.3(5) . . ? C13 C12 C11 120.5(6) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C14 C13 C12 121.0(6) . . ? C14 C13 H13 119.5 . . ? C12 C13 H13 119.5 . . ? C13 C14 C9 120.4(6) . . ? C13 C14 H14 119.8 . . ? C9 C14 H14 119.8 . . ? N5 C15 C16 124.8(6) . . ? N5 C15 H15 117.6 . . ? C16 C15 H15 117.6 . . ? C15 C16 C17 114.4(6) . . ? C15 C16 C23 122.7(6) . . ? C17 C16 C23 122.9(6) . . ? C18 C17 C16 118.5(6) . . ? C18 C17 H17 120.8 . . ? C16 C17 H17 120.8 . . ? N6 C18 C17 125.9(6) . . ? N6 C18 H18 117.1 . . ? C17 C18 H18 117.1 . . ? N7 C19 C20 123.7(5) . . ? N7 C19 H19 118.1 . . ? C20 C19 H19 118.1 . . ? C21 C20 C19 115.8(6) . . ? C21 C20 C25 124.7(6) . . ? C19 C20 C25 119.4(5) . . ? C20 C21 C22 117.7(6) . . ? C20 C21 H21 121.1 . . ? C22 C21 H21 121.1 . . ? N8 C22 C21 125.5(6) . . ? N8 C22 H22 117.3 . . ? C21 C22 H22 117.3 . . ? C28 C23 C24 118.6(6) . . ? C28 C23 C16 122.0(6) . . ? C24 C23 C16 119.5(6) . . ? C25 C24 C23 121.7(6) . . ? C25 C24 H24 119.2 . . ? C23 C24 H24 119.2 . . ? C26 C25 C24 118.4(6) . . ? C26 C25 C20 121.0(5) . . ? C24 C25 C20 120.5(5) . . ? C25 C26 C27 120.3(6) . . ? C25 C26 H26 119.9 . . ? C27 C26 H26 119.9 . . ? C28 C27 C26 120.4(6) . . ? C28 C27 H27 119.8 . . ? C26 C27 H27 119.8 . . ? C27 C28 C23 120.6(6) . . ? C27 C28 H28 119.7 . . ? C23 C28 H28 119.7 . . ? N9 C29 C30 123.5(6) . . ? N9 C29 H29 118.2 . . ? C30 C29 H29 118.2 . . ? C31 C30 C29 115.2(6) . . ? C31 C30 C37 124.0(6) . . ? C29 C30 C37 120.8(6) . . ? C30 C31 C32 118.6(6) . . ? C30 C31 H31 120.7 . . ? C32 C31 H31 120.7 . . ? N10 C32 C31 123.9(7) . . ? N10 C32 H32 118.0 . . ? C31 C32 H32 118.0 . . ? N11 C33 C34 124.1(5) . . ? N11 C33 H33 117.9 . . ? C34 C33 H33 117.9 . . ? C35 C34 C33 115.2(5) . . ? C35 C34 C39 123.0(5) . . ? C33 C34 C39 121.8(5) . . ? C34 C35 C36 118.1(6) . . ? C34 C35 H35 121.0 . . ? C36 C35 H35 121.0 . . ? N12 C36 C35 125.1(6) . . ? N12 C36 H36 117.4 . . ? C35 C36 H36 117.4 . . ? C38 C37 C42 118.9(6) . . ? C38 C37 C30 119.3(5) . . ? C42 C37 C30 121.8(6) . . ? C37 C38 C39 121.4(6) . . ? C37 C38 H38 119.3 . . ? C39 C38 H38 119.3 . . ? C40 C39 C38 117.4(6) . . ? C40 C39 C34 122.6(6) . . ? C38 C39 C34 120.0(5) . . ? C39 C40 C41 121.4(6) . . ? C39 C40 H40 119.3 . . ? C41 C40 H40 119.3 . . ? C42 C41 C40 120.2(6) . . ? C42 C41 H41 119.9 . . ? C40 C41 H41 119.9 . . ? C41 C42 C37 120.5(6) . . ? C41 C42 H42 119.7 . . ? C37 C42 H42 119.7 . . ? N13 C43 C44 123.5(5) . . ? N13 C43 H43 118.2 . . ? C44 C43 H43 118.2 . . ? C45 C44 C43 116.2(6) . . ? C45 C44 C51 121.1(6) . . ? C43 C44 C51 122.7(5) . . ? C44 C45 C46 117.3(6) . . ? C44 C45 H45 121.4 . . ? C46 C45 H45 121.4 . . ? N14 C46 C45 124.4(6) . . ? N14 C46 H46 117.8 . . ? C45 C46 H46 117.8 . . ? N15 C47 C48 123.4(5) . . ? N15 C47 H47 118.3 . . ? C48 C47 H47 118.3 . . ? C49 C48 C47 116.0(5) . . ? C49 C48 C53 123.8(5) . . ? C47 C48 C53 120.2(5) . . ? C48 C49 C50 117.3(6) . . ? C48 C49 H49 121.3 . . ? C50 C49 H49 121.3 . . ? N16 C50 C49 124.6(6) . . ? N16 C50 H50 117.7 . . ? C49 C50 H50 117.7 . . ? C56 C51 C52 118.8(6) . . ? C56 C51 C44 122.2(5) . . ? C52 C51 C44 118.9(5) . . ? C53 C52 C51 121.0(6) . . ? C53 C52 H52 119.5 . . ? C51 C52 H52 119.5 . . ? C52 C53 C54 119.0(6) . . ? C52 C53 C48 119.3(5) . . ? C54 C53 C48 121.6(6) . . ? C55 C54 C53 120.2(6) . . ? C55 C54 H54 119.9 . . ? C53 C54 H54 119.9 . . ? C54 C55 C56 121.2(6) . . ? C54 C55 H55 119.4 . . ? C56 C55 H55 119.4 . . ? C51 C56 C55 119.7(6) . . ? C51 C56 H56 120.1 . . ? C55 C56 H56 120.1 . . ? O1 C57 H57A 109.5 . . ? O1 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? O1 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? O5 Cl1 O6 110.6(4) . . ? O5 Cl1 O4 109.0(6) . . ? O6 Cl1 O4 109.0(4) . . ? O5 Cl1 O3 110.4(4) . . ? O6 Cl1 O3 110.5(3) . . ? O4 Cl1 O3 107.3(4) . . ? O10 Cl2 O8 110.3(4) . . ? O10 Cl2 O7 107.7(4) . . ? O8 Cl2 O7 108.4(4) . . ? O10 Cl2 O9 112.6(4) . . ? O8 Cl2 O9 109.2(4) . . ? O7 Cl2 O9 108.6(4) . . ? Cl5 C58 Cl4 110.6(4) . . ? Cl5 C58 Cl3 110.7(4) . . ? Cl4 C58 Cl3 110.2(4) . . ? Cl5 C58 H58 108.4 . . ? Cl4 C58 H58 108.4 . . ? Cl3 C58 H58 108.4 . . ? Cl7 C59 Cl6 110.3(5) . . ? Cl7 C59 Cl8 109.8(4) . . ? Cl6 C59 Cl8 109.7(4) . . ? Cl7 C59 H59 109.0 . . ? Cl6 C59 H59 109.0 . . ? Cl8 C59 H59 109.0 . . ? Cl11 C60 Cl9 110.8(5) . . ? Cl11 C60 Cl10 111.3(4) . . ? Cl9 C60 Cl10 111.6(5) . . ? Cl11 C60 H60 107.6 . . ? Cl9 C60 H60 107.6 . . ? Cl10 C60 H60 107.6 . . ? Cl14 C61 Cl12 119.0(18) . . ? Cl14 C61 Cl13 105.1(15) . . ? Cl12 C61 Cl13 99.7(14) . . ? Cl14 C61 H61A 110.9 . . ? Cl12 C61 H61A 110.9 . . ? Cl14 C61 H61A 102.4 3_656 . ? Cl13 C61 H61A 110.2 . . ? Cl3A C62A Cl2A 118.8(10) . . ? Cl3A C62A Cl1A 109.1(11) . . ? Cl2A C62A Cl1A 112.1(12) . . ? Cl3A C62A H62A 105.2 . . ? Cl2A C62A H62A 105.2 . . ? Cl1A C62A H62A 105.2 . . ? Cl2B C62B Cl1B 116.9(17) . . ? Cl2B C62B Cl3B 112.2(17) . . ? Cl1B C62B Cl3B 105.6(15) . . ? Cl2B C62B H62B 107.2 . . ? Cl1B C62B H62B 107.2 . . ? Cl3B C62B H62B 107.2 . . ? C62B Cl3B Cl13 155.2(9) . 4 ? Cl6A C63A Cl4A 114.1(11) . . ? Cl6A C63A Cl5A 113.4(10) . . ? Cl4A C63A Cl5A 112.0(10) . . ? Cl6A C63A H63A 105.5 . . ? Cl4A C63A H63A 105.5 . . ? Cl5A C63A H63A 105.5 . . ? Cl5B C63B Cl6B 115.3(15) . . ? Cl5B C63B Cl4B 108.3(16) . . ? Cl6B C63B Cl4B 105.9(15) . . ? Cl5B C63B H63B 109.1 . . ? Cl6B C63B H63B 109.1 . . ? Cl4B C63B H63B 109.1 . . ? 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 N1 Cu1 O1 C57 -56.2(5) . . . . ? N9 Cu1 O1 C57 126.3(5) . . . . ? N13 Cu1 O1 C57 37.4(5) . . . . ? N5 Cu1 O1 C57 -144.4(5) . . . . ? N13 Cu1 N1 C1 104.4(5) . . . . ? N5 Cu1 N1 C1 -62.4(5) . . . . ? F1 Cu1 N1 C1 21.6(5) . . . . ? O1 Cu1 N1 C1 -154.9(5) . . . . ? N13 Cu1 N1 N2 -75.4(4) . . . . ? N5 Cu1 N1 N2 117.9(4) . . . . ? F1 Cu1 N1 N2 -158.1(4) . . . . ? O1 Cu1 N1 N2 25.3(4) . . . . ? C1 N1 N2 C4 1.2(8) . . . . ? Cu1 N1 N2 C4 -179.1(5) . . . . ? N7 Cu2 N3 C5 71.7(5) . . . . ? N15 Cu2 N3 C5 -101.9(5) . . . . ? F2 Cu2 N3 C5 -15.4(4) . . . . ? O2 Cu2 N3 C5 168.2(4) . . . . ? N7 Cu2 N3 N4 -111.9(4) . . . . ? N15 Cu2 N3 N4 74.5(4) . . . . ? F2 Cu2 N3 N4 161.0(4) . . . . ? O2 Cu2 N3 N4 -15.4(4) . . . . ? C5 N3 N4 C8 -1.3(8) . . . . ? Cu2 N3 N4 C8 -177.8(4) . . . . ? N1 Cu1 N5 C15 113.8(5) . . . . ? N9 Cu1 N5 C15 -56.7(5) . . . . ? N13 Cu1 N5 C15 27.0(12) . . . . ? F1 Cu1 N5 C15 27.1(5) . . . . ? O1 Cu1 N5 C15 -145.1(5) . . . . ? N1 Cu1 N5 N6 -60.1(4) . . . . ? N9 Cu1 N5 N6 129.4(4) . . . . ? N13 Cu1 N5 N6 -146.9(8) . . . . ? F1 Cu1 N5 N6 -146.8(4) . . . . ? O1 Cu1 N5 N6 41.0(4) . . . . ? C15 N5 N6 C18 1.2(9) . . . . ? Cu1 N5 N6 C18 175.3(5) . . . . ? N3 Cu2 N7 C19 -95.3(5) . . . . ? N11 Cu2 N7 C19 75.5(5) . . . . ? F2 Cu2 N7 C19 -10.4(4) . . . . ? O2 Cu2 N7 C19 167.7(4) . . . . ? N3 Cu2 N7 N8 86.3(4) . . . . ? N11 Cu2 N7 N8 -103.0(4) . . . . ? F2 Cu2 N7 N8 171.2(4) . . . . ? O2 Cu2 N7 N8 -10.7(4) . . . . ? C19 N7 N8 C22 2.2(8) . . . . ? Cu2 N7 N8 C22 -179.3(4) . . . . ? N13 Cu1 N9 C29 -59.3(5) . . . . ? N5 Cu1 N9 C29 107.5(5) . . . . ? F1 Cu1 N9 C29 23.6(5) . . . . ? O1 Cu1 N9 C29 -159.5(5) . . . . ? N13 Cu1 N9 N10 124.1(4) . . . . ? N5 Cu1 N9 N10 -69.1(4) . . . . ? F1 Cu1 N9 N10 -153.0(4) . . . . ? O1 Cu1 N9 N10 23.9(4) . . . . ? C29 N9 N10 C32 -0.1(9) . . . . ? Cu1 N9 N10 C32 176.6(5) . . . . ? N7 Cu2 N11 C33 -99.9(5) . . . . ? N15 Cu2 N11 C33 73.7(5) . . . . ? F2 Cu2 N11 C33 -12.6(5) . . . . ? O2 Cu2 N11 C33 163.9(5) . . . . ? N7 Cu2 N11 N12 76.7(4) . . . . ? N15 Cu2 N11 N12 -109.7(4) . . . . ? F2 Cu2 N11 N12 164.0(4) . . . . ? O2 Cu2 N11 N12 -19.5(4) . . . . ? C33 N11 N12 C36 1.3(8) . . . . ? Cu2 N11 N12 C36 -175.5(4) . . . . ? N1 Cu1 N13 C43 -55.6(5) . . . . ? N9 Cu1 N13 C43 114.5(5) . . . . ? F1 Cu1 N13 C43 30.6(4) . . . . ? O1 Cu1 N13 C43 -157.2(4) . . . . ? N1 Cu1 N13 N14 128.0(4) . . . . ? N9 Cu1 N13 N14 -61.8(4) . . . . ? N5 Cu1 N13 N14 -145.6(8) . . . . ? F1 Cu1 N13 N14 -145.7(4) . . . . ? O1 Cu1 N13 N14 26.5(4) . . . . ? C43 N13 N14 C46 -0.2(8) . . . . ? Cu1 N13 N14 C46 176.2(4) . . . . ? N3 Cu2 N15 C47 69.7(5) . . . . ? N11 Cu2 N15 C47 -101.2(5) . . . . ? F2 Cu2 N15 C47 -15.4(5) . . . . ? O2 Cu2 N15 C47 166.4(5) . . . . ? N3 Cu2 N15 N16 -112.6(4) . . . . ? N11 Cu2 N15 N16 76.5(4) . . . . ? F2 Cu2 N15 N16 162.4(4) . . . . ? O2 Cu2 N15 N16 -15.8(4) . . . . ? C47 N15 N16 C50 0.9(8) . . . . ? Cu2 N15 N16 C50 -176.9(4) . . . . ? N2 N1 C1 C2 2.2(9) . . . . ? Cu1 N1 C1 C2 -177.6(4) . . . . ? N1 C1 C2 C3 -4.3(9) . . . . ? N1 C1 C2 C9 176.5(6) . . . . ? C1 C2 C3 C4 3.1(9) . . . . ? C9 C2 C3 C4 -177.8(6) . . . . ? N1 N2 C4 C3 -2.3(10) . . . . ? C2 C3 C4 N2 0.0(11) . . . . ? N4 N3 C5 C6 -0.7(9) . . . . ? Cu2 N3 C5 C6 175.5(4) . . . . ? N3 C5 C6 C7 1.5(9) . . . . ? N3 C5 C6 C11 -177.5(5) . . . . ? C5 C6 C7 C8 -0.4(8) . . . . ? C11 C6 C7 C8 178.5(6) . . . . ? N3 N4 C8 C7 2.4(9) . . . . ? C6 C7 C8 N4 -1.6(10) . . . . ? C3 C2 C9 C10 145.3(6) . . . . ? C1 C2 C9 C10 -35.6(9) . . . . ? C3 C2 C9 C14 -35.4(9) . . . . ? C1 C2 C9 C14 143.8(6) . . . . ? C14 C9 C10 C11 1.8(9) . . . . ? C2 C9 C10 C11 -178.8(5) . . . . ? C9 C10 C11 C12 -0.9(9) . . . . ? C9 C10 C11 C6 179.1(6) . . . . ? C7 C6 C11 C12 33.8(9) . . . . ? C5 C6 C11 C12 -147.3(6) . . . . ? C7 C6 C11 C10 -146.2(6) . . . . ? C5 C6 C11 C10 32.7(9) . . . . ? C10 C11 C12 C13 0.2(10) . . . . ? C6 C11 C12 C13 -179.7(6) . . . . ? C11 C12 C13 C14 -0.6(11) . . . . ? C12 C13 C14 C9 1.5(11) . . . . ? C10 C9 C14 C13 -2.1(10) . . . . ? C2 C9 C14 C13 178.5(6) . . . . ? N6 N5 C15 C16 0.1(9) . . . . ? Cu1 N5 C15 C16 -173.5(5) . . . . ? N5 C15 C16 C17 -2.3(9) . . . . ? N5 C15 C16 C23 175.8(6) . . . . ? C15 C16 C17 C18 3.1(10) . . . . ? C23 C16 C17 C18 -175.0(7) . . . . ? N5 N6 C18 C17 -0.2(11) . . . . ? C16 C17 C18 N6 -2.1(12) . . . . ? N8 N7 C19 C20 -3.2(9) . . . . ? Cu2 N7 C19 C20 178.4(4) . . . . ? N7 C19 C20 C21 0.9(9) . . . . ? N7 C19 C20 C25 -179.7(5) . . . . ? C19 C20 C21 C22 2.0(9) . . . . ? C25 C20 C21 C22 -177.3(6) . . . . ? N7 N8 C22 C21 0.9(10) . . . . ? C20 C21 C22 N8 -3.0(10) . . . . ? C15 C16 C23 C28 137.5(7) . . . . ? C17 C16 C23 C28 -44.5(9) . . . . ? C15 C16 C23 C24 -44.3(9) . . . . ? C17 C16 C23 C24 133.7(7) . . . . ? C28 C23 C24 C25 -0.1(9) . . . . ? C16 C23 C24 C25 -178.4(6) . . . . ? C23 C24 C25 C26 0.5(9) . . . . ? C23 C24 C25 C20 177.9(6) . . . . ? C21 C20 C25 C26 25.5(9) . . . . ? C19 C20 C25 C26 -153.8(6) . . . . ? C21 C20 C25 C24 -151.9(6) . . . . ? C19 C20 C25 C24 28.8(8) . . . . ? C24 C25 C26 C27 -2.1(9) . . . . ? C20 C25 C26 C27 -179.5(6) . . . . ? C25 C26 C27 C28 3.4(9) . . . . ? C26 C27 C28 C23 -3.1(9) . . . . ? C24 C23 C28 C27 1.5(9) . . . . ? C16 C23 C28 C27 179.7(6) . . . . ? N10 N9 C29 C30 2.7(9) . . . . ? Cu1 N9 C29 C30 -173.7(4) . . . . ? N9 C29 C30 C31 -2.6(9) . . . . ? N9 C29 C30 C37 177.3(5) . . . . ? C29 C30 C31 C32 0.3(9) . . . . ? C37 C30 C31 C32 -179.7(6) . . . . ? N9 N10 C32 C31 -2.3(10) . . . . ? C30 C31 C32 N10 2.2(11) . . . . ? N12 N11 C33 C34 -2.5(9) . . . . ? Cu2 N11 C33 C34 173.9(4) . . . . ? N11 C33 C34 C35 3.2(9) . . . . ? N11 C33 C34 C39 -177.7(6) . . . . ? C33 C34 C35 C36 -2.6(9) . . . . ? C39 C34 C35 C36 178.3(6) . . . . ? N11 N12 C36 C35 -0.9(9) . . . . ? C34 C35 C36 N12 1.7(10) . . . . ? C31 C30 C37 C38 139.7(7) . . . . ? C29 C30 C37 C38 -40.2(9) . . . . ? C31 C30 C37 C42 -39.6(9) . . . . ? C29 C30 C37 C42 140.5(6) . . . . ? C42 C37 C38 C39 -0.4(9) . . . . ? C30 C37 C38 C39 -179.7(6) . . . . ? C37 C38 C39 C40 -1.3(9) . . . . ? C37 C38 C39 C34 176.3(5) . . . . ? C35 C34 C39 C40 30.1(9) . . . . ? C33 C34 C39 C40 -149.0(6) . . . . ? C35 C34 C39 C38 -147.4(6) . . . . ? C33 C34 C39 C38 33.6(9) . . . . ? C38 C39 C40 C41 1.6(9) . . . . ? C34 C39 C40 C41 -175.9(6) . . . . ? C39 C40 C41 C42 -0.3(10) . . . . ? C40 C41 C42 C37 -1.5(10) . . . . ? C38 C37 C42 C41 1.8(9) . . . . ? C30 C37 C42 C41 -178.9(6) . . . . ? N14 N13 C43 C44 2.2(8) . . . . ? Cu1 N13 C43 C44 -173.9(4) . . . . ? N13 C43 C44 C45 -3.7(8) . . . . ? N13 C43 C44 C51 173.7(5) . . . . ? C43 C44 C45 C46 3.1(8) . . . . ? C51 C44 C45 C46 -174.3(5) . . . . ? N13 N14 C46 C45 -0.1(9) . . . . ? C44 C45 C46 N14 -1.4(9) . . . . ? N16 N15 C47 C48 -2.8(9) . . . . ? Cu2 N15 C47 C48 174.9(4) . . . . ? N15 C47 C48 C49 4.2(9) . . . . ? N15 C47 C48 C53 -176.9(5) . . . . ? C47 C48 C49 C50 -3.8(9) . . . . ? C53 C48 C49 C50 177.3(6) . . . . ? N15 N16 C50 C49 -0.8(9) . . . . ? C48 C49 C50 N16 2.4(10) . . . . ? C45 C44 C51 C56 -45.0(8) . . . . ? C43 C44 C51 C56 137.7(6) . . . . ? C45 C44 C51 C52 132.5(6) . . . . ? C43 C44 C51 C52 -44.7(8) . . . . ? C56 C51 C52 C53 1.3(9) . . . . ? C44 C51 C52 C53 -176.4(5) . . . . ? C51 C52 C53 C54 -1.0(9) . . . . ? C51 C52 C53 C48 176.1(5) . . . . ? C49 C48 C53 C52 -148.1(6) . . . . ? C47 C48 C53 C52 33.1(8) . . . . ? C49 C48 C53 C54 29.0(9) . . . . ? C47 C48 C53 C54 -149.9(6) . . . . ? C52 C53 C54 C55 -0.5(9) . . . . ? C48 C53 C54 C55 -177.5(6) . . . . ? C53 C54 C55 C56 1.8(10) . . . . ? C52 C51 C56 C55 0.0(9) . . . . ? C44 C51 C56 C55 177.6(6) . . . . ? C54 C55 C56 C51 -1.5(10) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.690 _refine_diff_density_min -0.858 _refine_diff_density_rms 0.106 _iucr_refine_instruction_details ; #--------------------------------------------------------- TITL dk4 in P2(1)/c CELL 0.71073 12.8708 12.5785 50.2634 90.000 93.272 90.000 ZERR 4.00 0.0006 0.0005 0.0020 0.000 0.003 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O F SI CL CU UNIT 250 206 64 40 24 4 74 8 MERG 2 OMIT 0.00 180.00 SHEL 0.81 9 EADP C62A C62B FMAP 2 PLAN 12 SIZE 0.14 0.19 0.23 RTAB H..O H1 F3 RTAB H..O H5 F3 RTAB H..O H10 F6 RTAB H..O H15 F4 RTAB H..O H19 F4 RTAB H..O H24 F3 RTAB H..O H29 F5 RTAB H..O H33 F5 RTAB H..O H38 F4 RTAB H..O H43 F6 RTAB H..O H47 F6 RTAB H..O H52 F5 RTAB O..O C1 F3 RTAB O..O C5 F3 RTAB O..O C10 F6 RTAB O..O C15 F4 RTAB O..O C19 F4 RTAB O..O C24 F3 RTAB O..O C29 F5 RTAB O..O C33 F5 RTAB O..O C38 F4 RTAB O..O C43 F6 RTAB O..O C47 F6 RTAB O..O C52 F5 RTAB XHY C1 H1 F3 RTAB XHY C5 H5 F3 RTAB XHY C10 H10 F6 RTAB XHY C15 H15 F4 RTAB XHY C19 H19 F4 RTAB XHY C24 H24 F3 RTAB XHY C29 H29 F5 RTAB XHY C33 H33 F5 RTAB XHY C38 H38 F4 RTAB XHY C43 H43 F6 RTAB XHY C47 H47 F6 RTAB XHY C52 H52 F5 MPLA 4 N1 N5 N9 N13 Cu1 MPLA 4 N3 N7 N11 N15 Cu2 ACTA BOND $H CONF LIST 4 L.S. 5 TEMP -100.00 WGHT 0.048900 28.712702 FVAR 0.16210 CU1 8 0.098255 0.188663 0.448967 11.00000 0.02638 0.02393 = 0.01982 -0.00068 0.00281 -0.00117 CU2 8 0.111740 0.188127 0.293966 11.00000 0.02236 0.02106 = 0.01732 -0.00043 0.00075 -0.00124 SI1 6 0.104992 0.189214 0.371529 11.00000 0.01870 0.01585 = 0.01871 -0.00009 0.00038 -0.00147 F1 5 0.101820 0.189916 0.404648 11.00000 0.02257 0.02327 = 0.01589 0.00013 0.00024 -0.00116 F2 5 0.107492 0.189112 0.338012 11.00000 0.02295 0.01916 = 0.01789 -0.00079 -0.00127 -0.00215 F3 5 0.109931 0.055706 0.371417 11.00000 0.02524 0.01952 = 0.01867 -0.00098 0.00406 -0.00092 F4 5 0.235095 0.194595 0.373797 11.00000 0.01857 0.02500 = 0.02352 0.00046 0.00585 -0.00155 F5 5 0.099450 0.322957 0.371186 11.00000 0.02318 0.01693 = 0.02871 0.00070 0.00147 -0.00017 F6 5 -0.026092 0.184151 0.368618 11.00000 0.01856 0.02283 = 0.02464 0.00066 0.00014 -0.00336 O1 4 0.118830 0.194762 0.493365 11.00000 0.03314 0.04467 = 0.02474 0.00111 0.00210 -0.00302 AFIX 3 H1O 2 0.177629 0.220802 0.498415 11.00000 -1.50000 AFIX 0 O2 4 0.112130 0.198945 0.248861 11.00000 0.03554 0.03094 = 0.02434 -0.00148 0.00749 -0.00378 AFIX 3 H2O 2 0.089690 0.262355 0.247411 11.00000 -1.50000 H3O 2 0.169350 0.194985 0.241271 11.00000 -1.50000 AFIX 0 N1 3 -0.020493 0.084882 0.443968 11.00000 0.02923 0.02254 = 0.02288 0.00301 0.00635 -0.00006 N2 3 -0.085101 0.076607 0.464292 11.00000 0.03998 0.03330 = 0.02788 0.00499 0.01730 -0.00487 N3 3 -0.003394 0.072414 0.295356 11.00000 0.02302 0.02276 = 0.01744 -0.00205 0.00147 0.00042 N4 3 -0.059963 0.057290 0.272225 11.00000 0.02617 0.03201 = 0.02014 -0.00553 -0.00724 -0.00169 N5 3 0.199257 0.059518 0.446295 11.00000 0.02973 0.03056 = 0.02024 0.00332 0.00407 0.00129 N6 3 0.189769 -0.016528 0.465033 11.00000 0.05065 0.03294 = 0.03061 0.00842 0.01182 0.00864 N7 3 0.226333 0.077107 0.298462 11.00000 0.02344 0.02014 = 0.02008 -0.00389 0.00035 -0.00233 N8 3 0.254384 0.031078 0.275671 11.00000 0.03816 0.02752 = 0.02227 -0.00843 0.00661 0.00279 N9 3 0.222490 0.289602 0.447240 11.00000 0.02354 0.02376 = 0.02561 -0.00186 -0.00215 0.00218 N10 3 0.288026 0.286858 0.469053 11.00000 0.02823 0.03708 = 0.03654 -0.00520 -0.00276 -0.00267 N11 3 0.224432 0.307121 0.299181 11.00000 0.02765 0.02536 = 0.02192 0.00357 0.00434 -0.00047 N12 3 0.281126 0.325426 0.277716 11.00000 0.02973 0.03710 = 0.02363 0.00315 0.00717 -0.00165 N13 3 -0.001472 0.317541 0.442048 11.00000 0.02837 0.02649 = 0.01873 -0.00552 0.00595 0.00063 N14 3 0.004386 0.394630 0.460566 11.00000 0.03316 0.02821 = 0.02711 -0.00496 0.00231 -0.00530 N15 3 -0.003486 0.300273 0.294018 11.00000 0.02795 0.01818 = 0.02582 0.00329 -0.00153 0.00017 N16 3 -0.017752 0.356508 0.271232 11.00000 0.03317 0.03171 = 0.01898 0.00314 -0.00182 0.00110 C1 1 -0.036638 0.026674 0.421965 11.00000 0.02353 0.02490 = 0.02033 0.00388 0.00573 -0.00272 AFIX 43 H1 2 0.011712 0.032856 0.408458 11.00000 -1.20000 AFIX 0 C2 1 -0.120974 -0.043305 0.417571 11.00000 0.02380 0.02024 = 0.03158 0.00573 0.00127 0.00040 C3 1 -0.184192 -0.053870 0.438808 11.00000 0.04015 0.03433 = 0.03532 -0.00170 0.01194 -0.00639 AFIX 43 H3 2 -0.241155 -0.102014 0.438009 11.00000 -1.20000 AFIX 0 C4 1 -0.161758 0.008338 0.461447 11.00000 0.04842 0.03975 = 0.03262 0.00000 0.02220 -0.00913 AFIX 43 H4 2 -0.205552 0.000490 0.475907 11.00000 -1.20000 AFIX 0 C5 1 -0.025882 0.019577 0.317439 11.00000 0.02663 0.01803 = 0.02570 -0.00476 0.00119 -0.00317 AFIX 43 H5 2 0.016323 0.031978 0.333260 11.00000 -1.20000 AFIX 0 C6 1 -0.107767 -0.052614 0.318509 11.00000 0.03046 0.01546 = 0.03068 -0.00477 0.00260 0.00215 C7 1 -0.164430 -0.069003 0.294858 11.00000 0.02744 0.02526 = 0.03414 -0.00136 0.00265 0.00057 AFIX 43 H7 2 -0.221286 -0.117272 0.293812 11.00000 -1.20000 AFIX 0 C8 1 -0.136239 -0.012775 0.272357 11.00000 0.03621 0.03335 = 0.02016 0.00052 -0.01080 -0.00352 AFIX 43 H8 2 -0.174768 -0.025987 0.256005 11.00000 -1.20000 AFIX 0 C9 1 -0.137700 -0.101133 0.392042 11.00000 0.01762 0.02253 = 0.03886 0.00064 0.00880 -0.00405 C10 1 -0.114101 -0.052024 0.368207 11.00000 0.02504 0.01668 = 0.02379 0.00284 -0.00213 -0.00294 AFIX 43 H10 2 -0.086173 0.017904 0.368494 11.00000 -1.20000 AFIX 0 C11 1 -0.131420 -0.105429 0.343810 11.00000 0.01902 0.02204 = 0.03661 -0.00116 -0.00390 -0.00053 C12 1 -0.171035 -0.208324 0.343887 11.00000 0.03926 0.02629 = 0.03514 -0.00551 -0.00277 -0.00974 AFIX 43 H12 2 -0.182881 -0.245472 0.327539 11.00000 -1.20000 AFIX 0 C13 1 -0.193096 -0.256502 0.367339 11.00000 0.04917 0.02254 = 0.04123 0.00490 0.00191 -0.01430 AFIX 43 H13 2 -0.220716 -0.326558 0.367034 11.00000 -1.20000 AFIX 0 C14 1 -0.175981 -0.205326 0.391186 11.00000 0.03892 0.02505 = 0.03448 0.00382 0.00339 -0.00849 AFIX 43 H14 2 -0.190160 -0.240704 0.407280 11.00000 -1.20000 AFIX 0 C15 1 0.262689 0.045152 0.426470 11.00000 0.02812 0.02324 = 0.02147 0.00570 -0.00272 0.00331 AFIX 43 H15 2 0.267035 0.100690 0.413774 11.00000 -1.20000 AFIX 0 C16 1 0.322620 -0.044864 0.423075 11.00000 0.02992 0.02801 = 0.02744 -0.00313 0.00409 -0.00151 C17 1 0.315270 -0.120795 0.442908 11.00000 0.04615 0.03557 = 0.02914 0.00700 0.00500 0.00815 AFIX 43 H17 2 0.355993 -0.183776 0.442853 11.00000 -1.20000 AFIX 0 C18 1 0.247984 -0.102841 0.462552 11.00000 0.05743 0.03914 = 0.03609 0.01366 0.01458 0.01937 AFIX 43 H18 2 0.242395 -0.156934 0.475583 11.00000 -1.20000 AFIX 0 C19 1 0.274707 0.050688 0.321975 11.00000 0.02660 0.02074 = 0.02632 -0.00192 0.00679 0.00128 AFIX 43 H19 2 0.255484 0.087299 0.337478 11.00000 -1.20000 AFIX 0 C20 1 0.351138 -0.027060 0.324867 11.00000 0.02269 0.02662 = 0.02849 -0.00307 0.00248 -0.00536 C21 1 0.377095 -0.076294 0.301885 11.00000 0.03213 0.03347 = 0.02947 -0.00243 0.00595 0.00298 AFIX 43 H21 2 0.427088 -0.131908 0.302190 11.00000 -1.20000 AFIX 0 C22 1 0.327539 -0.041943 0.277966 11.00000 0.03843 0.04179 = 0.02556 -0.00970 0.00615 0.00368 AFIX 43 H22 2 0.348417 -0.074009 0.262012 11.00000 -1.20000 AFIX 0 C23 1 0.385908 -0.059904 0.399976 11.00000 0.03020 0.02363 = 0.02881 0.00176 0.00239 0.00232 C24 1 0.343551 -0.035234 0.374433 11.00000 0.02939 0.02481 = 0.02785 0.00302 0.00193 0.00560 AFIX 43 H24 2 0.274951 -0.007329 0.372486 11.00000 -1.20000 AFIX 0 C25 1 0.399392 -0.050555 0.351828 11.00000 0.03159 0.01827 = 0.02783 0.00570 0.00775 0.00667 C26 1 0.499493 -0.092207 0.355002 11.00000 0.02489 0.02901 = 0.03995 -0.00410 0.00754 0.00271 AFIX 43 H26 2 0.538137 -0.105502 0.339802 11.00000 -1.20000 AFIX 0 C27 1 0.543384 -0.114548 0.380438 11.00000 0.02099 0.02587 = 0.04374 -0.00054 0.00049 0.00135 AFIX 43 H27 2 0.613099 -0.139323 0.382523 11.00000 -1.20000 AFIX 0 C28 1 0.486129 -0.100855 0.402534 11.00000 0.03326 0.02243 = 0.02846 -0.00195 -0.00426 -0.00073 AFIX 43 H28 2 0.515505 -0.119603 0.419661 11.00000 -1.20000 AFIX 0 C29 1 0.242876 0.349440 0.426499 11.00000 0.02591 0.02455 = 0.02218 -0.00957 0.00019 -0.00109 AFIX 43 H29 2 0.193164 0.351514 0.411793 11.00000 -1.20000 AFIX 0 C30 1 0.333530 0.409649 0.425089 11.00000 0.02423 0.03323 = 0.02245 -0.01241 0.00129 -0.00276 C31 1 0.400070 0.406475 0.447528 11.00000 0.02636 0.04051 = 0.04618 -0.00627 0.00187 -0.00698 AFIX 43 H31 2 0.463434 0.445380 0.448300 11.00000 -1.20000 AFIX 0 C32 1 0.372455 0.344987 0.469064 11.00000 0.03683 0.05236 = 0.03504 -0.00406 -0.00585 -0.00373 AFIX 43 H32 2 0.417565 0.345229 0.484698 11.00000 -1.20000 AFIX 0 C33 1 0.244731 0.358556 0.321901 11.00000 0.03059 0.01864 = 0.01922 0.00167 0.00750 0.00121 AFIX 43 H33 2 0.201143 0.345275 0.336164 11.00000 -1.20000 AFIX 0 C34 1 0.326226 0.431105 0.326198 11.00000 0.02250 0.02068 = 0.02677 0.00104 0.00602 -0.00011 C35 1 0.383382 0.451073 0.304375 11.00000 0.02965 0.02738 = 0.02878 0.00269 0.00436 -0.00808 AFIX 43 H35 2 0.438444 0.501470 0.305268 11.00000 -1.20000 AFIX 0 C36 1 0.358050 0.395191 0.280967 11.00000 0.03088 0.03979 = 0.03272 0.00413 0.01080 -0.00412 AFIX 43 H36 2 0.399087 0.408069 0.266179 11.00000 -1.20000 AFIX 0 C37 1 0.353835 0.471413 0.400762 11.00000 0.01741 0.02535 = 0.03652 -0.00466 0.00467 -0.00797 C38 1 0.329179 0.427185 0.375966 11.00000 0.02543 0.02237 = 0.03080 -0.00532 0.00895 -0.00586 AFIX 43 H38 2 0.299385 0.358110 0.374895 11.00000 -1.20000 AFIX 0 C39 1 0.347472 0.482845 0.352130 11.00000 0.01721 0.02059 = 0.03361 -0.00317 0.00214 -0.00354 C40 1 0.388841 0.583535 0.354566 11.00000 0.02829 0.02751 = 0.04633 0.00463 0.00930 -0.00369 AFIX 43 H40 2 0.400246 0.623382 0.338944 11.00000 -1.20000 AFIX 0 C41 1 0.414241 0.628089 0.379339 11.00000 0.03708 0.02584 = 0.04396 -0.00762 0.00643 -0.01615 AFIX 43 H41 2 0.443002 0.697601 0.380510 11.00000 -1.20000 AFIX 0 C42 1 0.397949 0.572058 0.402159 11.00000 0.02826 0.02705 = 0.04715 -0.01020 0.01170 -0.00314 AFIX 43 H42 2 0.417024 0.602419 0.419042 11.00000 -1.20000 AFIX 0 C43 1 -0.063206 0.327527 0.420221 11.00000 0.02621 0.02333 = 0.02353 -0.00885 0.00985 -0.00260 AFIX 43 H43 2 -0.066971 0.270122 0.407921 11.00000 -1.20000 AFIX 0 C44 1 -0.123121 0.417950 0.414301 11.00000 0.02321 0.01902 = 0.02970 0.00131 0.00800 -0.00293 C45 1 -0.119836 0.496793 0.433477 11.00000 0.02935 0.02797 = 0.03436 -0.00158 0.00870 -0.00577 AFIX 43 H45 2 -0.160974 0.559250 0.431351 11.00000 -1.20000 AFIX 0 C46 1 -0.053637 0.480933 0.456088 11.00000 0.03506 0.02779 = 0.03445 -0.00586 0.00839 -0.00446 AFIX 43 H46 2 -0.049763 0.535509 0.469172 11.00000 -1.20000 AFIX 0 C47 1 -0.058616 0.320429 0.314774 11.00000 0.02745 0.02328 = 0.02175 0.00070 -0.00446 -0.00410 AFIX 43 H47 2 -0.048202 0.276813 0.330125 11.00000 -1.20000 AFIX 0 C48 1 -0.131971 0.403093 0.315358 11.00000 0.02091 0.02199 = 0.02781 -0.00282 0.00052 0.00011 C49 1 -0.149344 0.459641 0.291931 11.00000 0.03208 0.02169 = 0.03525 0.01142 -0.00119 0.01113 AFIX 43 H49 2 -0.200662 0.513898 0.290318 11.00000 -1.20000 AFIX 0 C50 1 -0.088405 0.433787 0.270729 11.00000 0.03852 0.03452 = 0.02134 0.00680 0.00181 0.00088 AFIX 43 H50 2 -0.098111 0.474266 0.254825 11.00000 -1.20000 AFIX 0 C51 1 -0.183707 0.432181 0.388517 11.00000 0.02883 0.01601 = 0.03048 -0.00282 0.00560 -0.00249 C52 1 -0.136279 0.406877 0.364616 11.00000 0.02190 0.02511 = 0.02236 -0.00283 0.00031 -0.00035 AFIX 43 H52 2 -0.068210 0.377410 0.365439 11.00000 -1.20000 AFIX 0 C53 1 -0.187378 0.424343 0.340128 11.00000 0.02400 0.01787 = 0.03081 0.00064 -0.00240 -0.00050 C54 1 -0.287844 0.466008 0.339157 11.00000 0.02420 0.03235 = 0.04003 0.00292 -0.00130 -0.00026 AFIX 43 H54 2 -0.323718 0.478960 0.322427 11.00000 -1.20000 AFIX 0 C55 1 -0.335029 0.488345 0.362265 11.00000 0.01982 0.03629 = 0.04432 -0.00802 -0.00122 0.00484 AFIX 43 H55 2 -0.404267 0.514821 0.361359 11.00000 -1.20000 AFIX 0 C56 1 -0.283353 0.472941 0.387024 11.00000 0.02720 0.02666 = 0.03484 -0.00645 0.01145 0.00168 AFIX 43 H56 2 -0.316560 0.490427 0.402849 11.00000 -1.20000 AFIX 0 C57 1 0.043523 0.220763 0.511976 11.00000 0.03553 0.05663 = 0.02859 -0.00129 0.00813 0.00600 AFIX 137 H57A 2 0.010693 0.288768 0.507015 11.00000 -1.50000 H57B 2 0.077635 0.226481 0.529854 11.00000 -1.50000 H57C 2 -0.009619 0.164946 0.511875 11.00000 -1.50000 AFIX 0 CL1 7 0.405145 0.189080 0.214875 11.00000 0.03249 0.03355 = 0.02869 -0.00345 0.00742 -0.00039 O3 4 0.293588 0.191962 0.214702 11.00000 0.03404 0.07240 = 0.04539 -0.00134 0.00930 0.00551 O4 4 0.438363 0.092621 0.227885 11.00000 0.08738 0.10911 = 0.10119 0.06624 0.03551 0.05917 O5 4 0.447756 0.275185 0.229099 11.00000 0.10757 0.12297 = 0.10507 -0.07127 0.06018 -0.08248 O6 4 0.438696 0.188550 0.188334 11.00000 0.06342 0.08754 = 0.03364 -0.01027 0.01943 -0.00398 CL2 7 0.363039 0.169935 0.049690 11.00000 0.02749 0.03524 = 0.03313 -0.00399 0.00489 0.00363 O7 4 0.357160 0.187762 0.077453 11.00000 0.07630 0.07655 = 0.05304 -0.01628 0.02962 -0.01082 O8 4 0.385246 0.061045 0.045681 11.00000 0.06462 0.05085 = 0.11297 -0.04432 -0.02213 0.01755 O9 4 0.264620 0.194861 0.036734 11.00000 0.05933 0.08881 = 0.08104 0.02134 -0.02567 0.01861 O10 4 0.444039 0.233796 0.040786 11.00000 0.08024 0.09288 = 0.08517 -0.01978 0.04892 -0.04671 C58 1 0.277145 -0.101815 0.006017 11.00000 0.03044 0.04698 = 0.03372 -0.00662 0.00029 0.00356 AFIX 13 H58 2 0.302602 -0.051943 0.020450 11.00000 -1.20000 AFIX 0 CL3 7 0.383832 -0.140330 -0.012146 11.00000 0.03280 0.06025 = 0.05269 -0.00381 0.00739 0.00213 CL4 7 0.184560 -0.035030 -0.014830 11.00000 0.03648 0.08914 = 0.05947 0.03098 0.00329 0.00992 CL5 7 0.221194 -0.212284 0.020793 11.00000 0.06040 0.04116 = 0.04816 0.00345 0.02170 0.00835 C59 1 0.878078 0.181248 0.214147 11.00000 0.06329 0.04502 = 0.03848 0.01246 -0.00378 -0.01666 AFIX 13 H59 2 0.924287 0.166317 0.230388 11.00000 -1.20000 AFIX 0 CL6 7 0.748460 0.174260 0.222513 11.00000 0.06419 0.06104 = 0.09765 0.01860 0.02701 -0.00919 CL7 7 0.905918 0.307572 0.202312 11.00000 0.07237 0.04417 = 0.06834 0.00903 0.00807 -0.02210 CL8 7 0.901287 0.085708 0.189682 11.00000 0.06514 0.05437 = 0.10929 -0.02767 -0.00508 0.00674 C60 1 0.555927 0.181072 0.288763 11.00000 0.05646 0.05319 = 0.05445 0.00677 -0.00588 -0.01647 AFIX 13 H60 2 0.500544 0.193618 0.274334 11.00000 -1.20000 AFIX 0 CL9 7 0.653623 0.272717 0.284707 11.00000 0.19082 0.14354 = 0.07871 -0.02939 0.05566 -0.12788 CL10 7 0.601229 0.049006 0.285362 11.00000 0.06415 0.08182 = 0.08676 0.00319 0.02527 0.02610 CL11 7 0.500729 0.199141 0.318810 11.00000 0.07352 0.04975 = 0.08815 0.00660 0.03014 0.00264 C61 1 0.506848 0.031929 0.507791 10.50000 0.04564 0.10441 = 0.22894 -0.09089 -0.00968 0.02192 AFIX 3 H61A 2 0.551448 0.084550 0.516281 10.50000 -1.20000 AFIX 0 CL12 7 0.576162 -0.057079 0.491400 10.50000 0.11859 0.14585 = 0.11170 0.01944 0.03792 0.04581 CL13 7 0.449530 -0.061749 0.534704 10.50000 0.11130 0.18507 = 0.09355 0.02376 0.01998 -0.05209 CL14 7 0.406841 0.086650 0.492578 10.50000 0.13093 0.09370 = 0.10220 -0.01195 -0.05035 0.01416 PART -1 C62A 1 0.388373 -0.279801 0.110659 10.60000 0.06486 0.03859 = 0.15585 0.00865 -0.02557 0.01775 AFIX 13 H62A 2 0.382807 -0.208443 0.119232 10.60000 -1.20000 AFIX 0 CL1A 7 0.343018 -0.261081 0.077338 10.60000 0.12383 0.18261 = 0.06384 -0.00696 -0.01476 0.07970 CL2A 7 0.515243 -0.309995 0.113351 10.60000 0.04704 0.06000 = 0.06821 -0.00459 -0.00095 0.00174 CL3A 7 0.304794 -0.357207 0.125878 10.60000 0.04182 0.15458 = 0.16036 0.01947 0.00248 -0.02648 PART -2 C62B 1 0.402434 -0.348294 0.102732 10.40000 0.06486 0.03859 = 0.15585 0.00865 -0.02557 0.01775 AFIX 13 H62B 2 0.429607 -0.414701 0.111578 10.40000 -1.20000 AFIX 0 CL1B 7 0.491744 -0.243381 0.112011 10.40000 0.05205 0.07205 = 0.08655 -0.01249 0.01044 -0.02302 CL2B 7 0.287219 -0.333980 0.110577 10.40000 0.05020 0.06027 = 0.31530 0.00108 -0.01164 -0.01260 CL3B 7 0.411909 -0.366550 0.065769 10.40000 0.14868 0.09669 = 0.10010 -0.00923 -0.06391 0.00422 PART -3 C63A 1 0.923565 0.197417 0.108188 10.60000 0.09054 0.03310 = 0.06428 0.00571 0.01736 -0.00611 AFIX 13 H63A 2 0.993863 0.214490 0.116604 10.60000 -1.20000 AFIX 0 CL4A 7 0.904513 0.063042 0.114375 10.60000 0.05624 0.03984 = 0.07915 -0.00282 0.00785 -0.00157 CL5A 7 0.932183 0.223621 0.074116 10.60000 0.07198 0.06262 = 0.06623 0.01565 0.01012 -0.00630 CL6A 7 0.840462 0.278146 0.122989 10.60000 0.10470 0.06158 = 0.08891 -0.00785 0.01497 0.04202 PART -4 C63B 1 0.856101 0.175433 0.104595 10.40000 0.04636 0.06301 = 0.10632 -0.03450 0.01930 -0.04628 AFIX 13 H63B 2 0.782765 0.156244 0.108135 10.40000 -1.20000 AFIX 0 CL4B 7 0.942485 0.080084 0.120475 10.40000 0.11492 0.06266 = 0.10090 0.01871 0.04233 0.04701 CL5B 7 0.870366 0.170726 0.072537 10.40000 0.17310 0.15777 = 0.07549 -0.03451 -0.01622 0.09881 CL6B 7 0.887279 0.298693 0.119938 10.40000 0.05363 0.05654 = 0.10855 -0.04388 0.01848 -0.00268 HKLF 4 REM dk4 in P2(1)/c REM R1 = 0.0793 for 9456 Fo > 4sig(Fo) and 0.1395 for all 15944 data REM 1130 parameters refined using 0 restraints END WGHT 0.0489 28.6991 REM Highest difference peak 0.690, deepest hole -0.858, 1-sigma level 0.106 Q1 1 0.7800 0.2058 0.2390 11.00000 0.05 0.69 Q2 1 0.3991 0.3056 0.2126 11.00000 0.05 0.64 Q3 1 0.8949 0.3048 0.1811 11.00000 0.05 0.62 Q4 1 0.6612 0.0988 0.2875 11.00000 0.05 0.61 Q5 1 0.1810 -0.1014 -0.0231 11.00000 0.05 0.60 Q6 1 0.7057 0.2021 0.2969 11.00000 0.05 0.60 Q7 1 0.3831 -0.3187 0.0892 11.00000 0.05 0.51 Q8 1 0.1179 0.3924 0.3067 11.00000 0.05 0.50 ; # ------------- END of CIF -----------------# _database_code_depnum_ccdc_archive 'CCDC 941556'