# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Jay Siegel' 'Jeremy K. Klosterman' 'Anthony Linden' _publ_contact_author_name 'Jay Siegel' _publ_contact_author_email JSS@OCI.UZH.CH _publ_section_title ; Manisyl-substituted polypyridine coordination compounds: Metallo-supramolecular networks of interdigitated double helices assembled via CH***? and ?-? interactions ; # Attachment 'pherpy_xtals.cif' data_3a' _database_code_depnum_ccdc_archive 'CCDC 735248' # SG0317 _audit_creation_method SHELXL-97 _audit_creation_date 03-09-03 _chemical_name_systematic ; bis{8-(4-methoxy-2,6-dimethylphenyl)-2-[5-(4-methoxy-2,6- dimethylphenyl)-pyridin-2-yl]-1,10-phenanthroline}iron(II) hexafluorophosphate ; _chemical_name_common ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_moiety 'C70 H62 Fe N6 O4 2+, 2(F6 P 1-)' _chemical_formula_sum 'C70 H62 F12 Fe N6 O4 P2' _chemical_formula_weight 1397.06 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 280 0.0033 0.0016 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; H H 248 0.0000 0.0000 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; F F 48 0.0171 0.0103 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; Fe Fe 4 0.3463 0.8444 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; N N 24 0.0061 0.0033 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; O O 16 0.0106 0.0060 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; P P 8 0.1023 0.0942 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c n ' _symmetry_space_group_name_Hall ? _symmetry_Int_Tables_number 60 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 23.8915(5) _cell_length_b 11.6189(3) _cell_length_c 23.1604(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6429.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 160(1) _cell_measurement_reflns_used 263548 _cell_measurement_theta_min 2.9 _cell_measurement_theta_max 25.0 _exptl_crystal_description prism _exptl_crystal_colour dark-red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.443 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2880 _exptl_absorpt_coefficient_mu 0.374 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Blessing, 1995)' _exptl_absorpt_correction_T_min 0.815 _exptl_absorpt_correction_T_max 0.946 _exptl_special_details ; Solvent used: diethylether / dichloromethane Cooling Device: Oxford Cryosystems Cryostream 700 Crystal mount: glued on a glass fibre Mosaicity (deg.): 1.109(1) Frames collected: 899 Seconds exposure per frame: 75 Degrees rotation per frame: 0.5 Crystal-Detector distance (mm): 36.0 ; _diffrn_ambient_temperature 160(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Nonius FR590 sealed tube generator' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_detector '65 mm CCD camera on \k goniostat' _diffrn_measurement_device_type 'Nonius KappaCCD area-detector diffractometer' _diffrn_measurement_method '\w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 70344 _diffrn_reflns_av_R_equivalents 0.0830 _diffrn_reflns_av_sigmaI/netI 0.0344 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 24.96 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 24.96 _diffrn_measured_fraction_theta_full 0.995 _reflns_number_total 5618 _reflns_number_gt 3949 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'COLLECT (Nonius, 2000)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN and SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'SHELXL97 and PLATON (Spek, 2009)' _refine_special_details ; The asymmetric unit contains one half of a cation with the Fe-atom on a two-fold axis and one disordered anion. In the cation, the two central CH groups of the phenanthroline moiety are disordered over two sites which effectively complete six-membered rings between all pyridine rings, thereby indicating that the ligand must be disordered through a 180\% rotation about the central N-atom. The site occupation factor for the major conformation refined to 0.854(8). The chemically equivalent C-C bonds involving the disordered C-atoms were restrained to have similar lengths and the atomic displacement parameters of the C-atoms of the minor conformation were given light pseudo-isotropic restraints. The PF6- anion is highly disordered. Three sets of F-atoms were defined about a common P-atom and refinement of the site occupation factors of each set led to values of 0.364(4), 0.326(14) and 0.310(15). The P-F and F...F distances were restrained tightly, so as to maintain octahedral geometry and uniform P-F bond lengths and the atomic displacement parameters of the F-atoms were given light pseudo-isotropic restraints with neighbouring F-atoms also restrained to have similar atomic displacement parameters. Validation reports a short contact as an A alert. This involves a disordered component of the cation where one atom has very low occupancy and so its position may not be optimally defined and a methyl H-atom whose calculated orientation based on a delta(F) calculation might also be less than optimal. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0830P)^2^+10.5796P] 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_extinction_coef ? _refine_ls_number_reflns 5618 _refine_ls_number_parameters 566 _refine_ls_number_restraints 1109 _refine_ls_R_factor_all 0.1040 _refine_ls_R_factor_gt 0.0699 _refine_ls_wR_factor_ref 0.2015 _refine_ls_wR_factor_gt 0.1778 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.552 _refine_diff_density_min -0.520 _refine_diff_density_rms 0.063 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 Fe Fe 0.0000 0.19381(7) 0.2500 0.0445(3) Uani 1 2 d S . . O1 O 0.29207(16) -0.3009(3) 0.31498(17) 0.0876(11) Uani 1 1 d . . . O2 O -0.00635(13) 0.7313(3) -0.04782(12) 0.0662(9) Uani 1 1 d . A . N1 N 0.02319(14) 0.0694(3) 0.30374(13) 0.0481(8) Uani 1 1 d . . . N2 N -0.06142(13) 0.1930(3) 0.30078(13) 0.0465(8) Uani 1 1 d . A . N3 N -0.04547(13) 0.3191(3) 0.21340(13) 0.0465(8) Uani 1 1 d . . . C1 C 0.3267(3) -0.3131(6) 0.3643(3) 0.101(2) Uani 1 1 d . . . H11 H 0.3343 -0.2371 0.3808 0.151 Uiso 1 1 calc R . . H12 H 0.3620 -0.3498 0.3532 0.151 Uiso 1 1 calc R . . H13 H 0.3076 -0.3610 0.3931 0.151 Uiso 1 1 calc R . . C2 C 0.2406(2) -0.2498(4) 0.3237(2) 0.0646(12) Uani 1 1 d . . . C3 C 0.2232(2) -0.2070(4) 0.37633(19) 0.0627(12) Uani 1 1 d . . . H3 H 0.2469 -0.2126 0.4091 0.075 Uiso 1 1 calc R . . C4 C 0.17062(19) -0.1554(4) 0.38152(18) 0.0558(11) Uani 1 1 d . . . C5 C 0.1548(2) -0.1096(4) 0.44037(18) 0.0670(12) Uani 1 1 d . . . H51 H 0.1339 -0.0375 0.4359 0.100 Uiso 1 1 calc R . . H52 H 0.1888 -0.0954 0.4630 0.100 Uiso 1 1 calc R . . H53 H 0.1314 -0.1662 0.4604 0.100 Uiso 1 1 calc R . . C6 C 0.13615(18) -0.1460(3) 0.33307(17) 0.0522(10) Uani 1 1 d . . . C7 C 0.07020(16) 0.0083(4) 0.30176(16) 0.0472(9) Uani 1 1 d . . . H7 H 0.0979 0.0298 0.2744 0.057 Uiso 1 1 calc R . . C8 C 0.08110(17) -0.0859(3) 0.33764(17) 0.0496(10) Uani 1 1 d . . . C9 C 0.03971(18) -0.1171(4) 0.37680(18) 0.0585(11) Uani 1 1 d . A . H9 H 0.0449 -0.1821 0.4011 0.070 Uiso 1 1 calc R . . C10 C -0.00887(18) -0.0534(4) 0.38024(17) 0.0580(11) Uani 1 1 d D . . H10 H -0.0369 -0.0737 0.4074 0.070 Uiso 0.854(8) 1 calc PR A 1 C11 C -0.01680(17) 0.0399(4) 0.34422(16) 0.0514(10) Uani 1 1 d . A . C12 C -0.06521(17) 0.1149(4) 0.34379(16) 0.0520(10) Uani 1 1 d . . . C13 C -0.11167(19) 0.1171(4) 0.38102(18) 0.0622(12) Uani 1 1 d D A . H131 H -0.1151 0.0613 0.4108 0.075 Uiso 0.854(8) 1 calc PR A 1 C14 C -0.1520(2) 0.2002(5) 0.3743(2) 0.0691(13) Uani 1 1 d . . . H14 H -0.1831 0.2022 0.3998 0.083 Uiso 1 1 calc R A . C15 C -0.14790(18) 0.2820(4) 0.33007(19) 0.0618(12) Uani 1 1 d D A . H15 H -0.1750 0.3410 0.3253 0.074 Uiso 0.146(8) 1 calc PR A 2 C16A C -0.1849(2) 0.3766(5) 0.3164(3) 0.0730(18) Uani 0.854(8) 1 d PD A 1 H161 H -0.2170 0.3891 0.3399 0.088 Uiso 0.854(8) 1 calc PR A 1 C17A C -0.1754(2) 0.4485(5) 0.2710(2) 0.0695(17) Uani 0.854(8) 1 d PD A 1 H171 H -0.2009 0.5097 0.2642 0.083 Uiso 0.854(8) 1 calc PR A 1 C16B C -0.0526(10) -0.046(3) 0.4228(11) 0.086(12) Uani 0.146(8) 1 d PDU A 2 H162 H -0.0490 -0.0925 0.4563 0.103 Uiso 0.146(8) 1 calc PR A 2 C17B C -0.0985(13) 0.022(2) 0.4189(12) 0.076(11) Uani 0.146(8) 1 d PDU A 2 H172 H -0.1271 0.0044 0.4459 0.091 Uiso 0.146(8) 1 calc PR A 2 C18 C -0.12817(17) 0.4356(4) 0.23289(18) 0.0574(11) Uani 1 1 d D . . H18 H -0.1602 0.4507 0.2560 0.069 Uiso 0.146(8) 1 calc PR A 2 C19 C -0.11537(18) 0.5042(4) 0.18444(19) 0.0604(11) Uani 1 1 d . A . H19 H -0.1387 0.5676 0.1748 0.072 Uiso 1 1 calc R . . C20 C -0.06889(17) 0.4797(3) 0.15086(17) 0.0523(10) Uani 1 1 d . . . C21 C -0.03536(16) 0.3845(3) 0.16709(16) 0.0486(9) Uani 1 1 d . A . H21 H -0.0039 0.3661 0.1437 0.058 Uiso 1 1 calc R . . C22 C -0.09236(17) 0.3454(4) 0.24545(17) 0.0513(10) Uani 1 1 d . A . C23 C -0.10150(17) 0.2721(4) 0.29329(17) 0.0509(10) Uani 1 1 d . . . C24 C -0.05120(18) 0.5502(3) 0.09821(16) 0.0495(10) Uani 1 1 d . A . C25 C 0.0004(2) 0.5872(3) 0.09501(17) 0.0560(11) Uani 1 1 d . . . C26 C 0.0468(2) 0.5713(5) 0.1403(2) 0.0738(14) Uani 1 1 d . A . H261 H 0.0308 0.5790 0.1791 0.111 Uiso 1 1 calc R . . H262 H 0.0757 0.6301 0.1346 0.111 Uiso 1 1 calc R . . H263 H 0.0635 0.4947 0.1360 0.111 Uiso 1 1 calc R . . C27 C 0.01895(19) 0.6480(4) 0.04497(17) 0.0572(11) Uani 1 1 d . A . H27 H 0.0566 0.6734 0.0418 0.069 Uiso 1 1 calc R . . C28 C -0.0193(2) 0.6694(4) 0.00100(17) 0.0568(11) Uani 1 1 d . . . C29 C 0.0480(2) 0.7804(5) -0.0490(2) 0.0782(15) Uani 1 1 d . . . H291 H 0.0530 0.8300 -0.0151 0.117 Uiso 1 1 calc R A . H292 H 0.0525 0.8261 -0.0842 0.117 Uiso 1 1 calc R . . H293 H 0.0761 0.7189 -0.0483 0.117 Uiso 1 1 calc R . . C30 C -0.07389(19) 0.6293(4) 0.00549(18) 0.0587(11) Uani 1 1 d . A . H30 H -0.0997 0.6444 -0.0248 0.070 Uiso 1 1 calc R . . C31 C -0.09143(19) 0.5675(4) 0.05360(19) 0.0605(11) Uani 1 1 d . . . C32 C -0.1517(2) 0.5267(4) 0.0555(2) 0.0757(14) Uani 1 1 d . A . H321 H -0.1733 0.5767 0.0813 0.114 Uiso 1 1 calc R . . H322 H -0.1530 0.4474 0.0699 0.114 Uiso 1 1 calc R . . H323 H -0.1677 0.5296 0.0166 0.114 Uiso 1 1 calc R . . C33 C 0.1175(2) -0.1874(5) 0.2263(2) 0.0787(15) Uani 1 1 d . . . H331 H 0.0782 -0.1969 0.2375 0.118 Uiso 1 1 calc R . . H332 H 0.1282 -0.2498 0.2001 0.118 Uiso 1 1 calc R . . H333 H 0.1223 -0.1132 0.2068 0.118 Uiso 1 1 calc R . . C34 C 0.15394(19) -0.1912(4) 0.27953(18) 0.0567(11) Uani 1 1 d . . . C35 C 0.2063(2) -0.2417(4) 0.2759(2) 0.0650(12) Uani 1 1 d . . . H35 H 0.2188 -0.2713 0.2399 0.078 Uiso 1 1 calc R . . P1 P 0.31013(6) 0.30274(14) 0.05564(6) 0.0842(5) Uani 1 1 d D . . F1A F 0.3712(2) 0.2821(12) 0.0789(5) 0.121(6) Uani 0.364(4) 1 d PDU B 1 F2A F 0.2489(3) 0.3227(12) 0.0328(6) 0.151(7) Uani 0.364(4) 1 d PDU B 1 F3A F 0.3014(5) 0.3991(9) 0.1026(5) 0.105(4) Uani 0.364(4) 1 d PDU B 1 F4A F 0.3193(5) 0.2067(10) 0.0087(5) 0.183(9) Uani 0.364(4) 1 d PDU B 1 F5A F 0.2875(6) 0.2093(10) 0.0990(5) 0.150(8) Uani 0.364(4) 1 d PDU B 1 F6A F 0.3327(6) 0.3962(10) 0.0123(5) 0.171(8) Uani 0.364(4) 1 d PDU B 1 F1B F 0.2530(3) 0.2478(15) 0.0358(6) 0.142(8) Uani 0.326(14) 1 d PDU C 2 F2B F 0.3673(3) 0.3567(15) 0.0757(7) 0.180(11) Uani 0.326(14) 1 d PDU B 2 F3B F 0.3292(5) 0.311(2) -0.0093(2) 0.124(6) Uani 0.326(14) 1 d PDU B 2 F4B F 0.2903(5) 0.294(2) 0.1203(2) 0.129(6) Uani 0.326(14) 1 d PDU B 2 F5B F 0.3365(6) 0.1789(6) 0.0599(10) 0.160(7) Uani 0.326(14) 1 d PDU B 2 F6B F 0.2839(6) 0.4266(6) 0.0509(10) 0.154(7) Uani 0.326(14) 1 d PDU B 2 F1C F 0.2511(2) 0.2766(11) 0.0285(5) 0.094(6) Uani 0.310(15) 1 d PDU B 3 F2C F 0.3693(2) 0.3279(10) 0.0827(4) 0.058(4) Uani 0.310(15) 1 d PDU B 3 F3C F 0.3269(6) 0.3720(13) -0.0001(4) 0.165(10) Uani 0.310(15) 1 d PDU B 3 F4C F 0.2931(5) 0.2339(12) 0.1115(4) 0.063(4) Uani 0.310(15) 1 d PDU B 3 F5C F 0.3343(4) 0.1896(8) 0.0278(7) 0.100(6) Uani 0.310(15) 1 d PDU B 3 F6C F 0.2868(5) 0.4167(8) 0.0834(7) 0.125(8) Uani 0.310(15) 1 d PDU B 3 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 Fe 0.0472(5) 0.0488(5) 0.0375(4) 0.000 0.0066(3) 0.000 O1 0.082(2) 0.089(3) 0.092(3) 0.001(2) 0.009(2) 0.025(2) O2 0.079(2) 0.072(2) 0.0469(16) 0.0060(15) -0.0008(15) 0.0147(17) N1 0.0543(19) 0.0515(19) 0.0384(17) -0.0012(15) -0.0029(15) -0.0053(17) N2 0.0482(18) 0.053(2) 0.0381(16) -0.0045(15) 0.0061(14) -0.0026(16) N3 0.0514(18) 0.0471(19) 0.0410(17) -0.0034(15) 0.0069(14) -0.0004(15) C1 0.096(4) 0.116(5) 0.090(4) 0.001(4) -0.003(4) 0.051(4) C2 0.069(3) 0.056(3) 0.069(3) 0.008(2) 0.009(2) 0.006(2) C3 0.070(3) 0.062(3) 0.056(3) 0.010(2) -0.005(2) 0.007(2) C4 0.068(3) 0.047(2) 0.053(2) 0.004(2) -0.001(2) 0.000(2) C5 0.073(3) 0.073(3) 0.055(3) 0.001(2) -0.009(2) 0.006(3) C6 0.067(3) 0.042(2) 0.048(2) 0.0066(18) 0.000(2) -0.008(2) C7 0.052(2) 0.051(2) 0.0392(19) 0.0022(18) 0.0014(17) -0.0044(19) C8 0.058(2) 0.047(2) 0.044(2) 0.0009(18) -0.0048(18) -0.0058(19) C9 0.064(3) 0.060(3) 0.052(2) 0.011(2) -0.002(2) -0.008(2) C10 0.061(3) 0.068(3) 0.045(2) 0.010(2) 0.0053(19) -0.011(2) C11 0.057(2) 0.060(3) 0.038(2) -0.0012(18) -0.0002(18) -0.010(2) C12 0.057(2) 0.059(3) 0.040(2) -0.0030(19) 0.0053(18) -0.010(2) C13 0.066(3) 0.072(3) 0.049(2) 0.006(2) 0.010(2) -0.017(2) C14 0.059(3) 0.087(4) 0.062(3) -0.005(3) 0.021(2) -0.010(3) C15 0.056(3) 0.069(3) 0.061(3) -0.006(2) 0.011(2) -0.001(2) C16A 0.060(3) 0.082(4) 0.077(4) -0.007(3) 0.022(3) 0.001(3) C17A 0.060(3) 0.068(4) 0.081(4) -0.004(3) 0.014(3) 0.017(3) C16B 0.103(19) 0.078(18) 0.076(17) 0.015(14) 0.017(15) -0.010(15) C17B 0.081(17) 0.080(18) 0.067(16) 0.005(13) 0.029(13) 0.000(14) C18 0.057(3) 0.060(3) 0.056(2) -0.006(2) 0.007(2) 0.005(2) C19 0.063(3) 0.053(3) 0.065(3) -0.006(2) 0.002(2) 0.016(2) C20 0.058(2) 0.046(2) 0.053(2) -0.0042(19) 0.000(2) 0.009(2) C21 0.052(2) 0.050(2) 0.043(2) -0.0035(18) 0.0031(18) 0.0039(19) C22 0.051(2) 0.052(2) 0.050(2) -0.008(2) 0.0065(19) 0.0010(19) C23 0.051(2) 0.055(2) 0.047(2) -0.0062(19) 0.0103(18) -0.003(2) C24 0.061(3) 0.046(2) 0.041(2) -0.0018(18) 0.0023(19) 0.021(2) C25 0.084(3) 0.036(2) 0.048(2) 0.0037(17) -0.021(2) 0.005(2) C26 0.085(3) 0.079(3) 0.058(3) 0.014(2) -0.017(2) -0.020(3) C27 0.065(3) 0.054(3) 0.052(2) -0.005(2) -0.004(2) 0.010(2) C28 0.075(3) 0.053(3) 0.042(2) -0.0036(19) -0.002(2) 0.019(2) C29 0.075(3) 0.078(4) 0.082(3) 0.018(3) -0.008(3) -0.001(3) C30 0.071(3) 0.055(3) 0.051(2) -0.003(2) -0.010(2) 0.016(2) C31 0.069(3) 0.051(3) 0.061(3) -0.006(2) 0.000(2) 0.015(2) C32 0.080(3) 0.067(3) 0.081(3) -0.002(3) -0.015(3) 0.006(3) C33 0.094(4) 0.086(4) 0.056(3) -0.018(3) -0.006(3) 0.003(3) C34 0.069(3) 0.050(3) 0.050(2) 0.000(2) -0.001(2) -0.007(2) C35 0.075(3) 0.058(3) 0.062(3) -0.007(2) 0.010(2) 0.002(2) P1 0.0834(10) 0.1027(12) 0.0665(9) -0.0013(8) 0.0125(7) -0.0020(9) F1A 0.088(8) 0.148(15) 0.126(10) -0.007(9) 0.021(7) 0.054(8) F2A 0.142(12) 0.138(13) 0.174(13) 0.010(10) -0.049(10) 0.049(9) F3A 0.083(7) 0.098(9) 0.135(10) -0.020(7) 0.045(7) 0.014(6) F4A 0.238(18) 0.152(14) 0.158(15) -0.063(11) -0.016(13) 0.031(13) F5A 0.144(13) 0.130(12) 0.177(16) 0.026(12) 0.004(12) -0.023(10) F6A 0.243(18) 0.149(13) 0.120(11) 0.068(10) 0.065(12) 0.020(13) F1B 0.081(11) 0.235(19) 0.110(12) 0.013(13) 0.011(9) -0.044(11) F2B 0.128(15) 0.147(16) 0.27(2) -0.061(15) -0.019(14) -0.065(12) F3B 0.113(9) 0.174(16) 0.084(8) -0.018(10) 0.030(7) 0.000(10) F4B 0.127(10) 0.185(17) 0.074(7) -0.042(10) 0.019(7) -0.028(12) F5B 0.200(15) 0.102(10) 0.178(17) -0.042(10) -0.049(13) 0.000(10) F6B 0.150(13) 0.126(11) 0.187(16) 0.040(11) -0.001(12) 0.037(10) F1C 0.101(13) 0.123(12) 0.056(7) 0.018(7) -0.027(8) -0.019(8) F2C 0.040(6) 0.058(7) 0.076(7) -0.044(5) 0.018(5) -0.012(4) F3C 0.206(19) 0.159(17) 0.129(15) 0.037(14) 0.061(15) 0.005(16) F4C 0.070(7) 0.090(10) 0.030(5) -0.005(5) 0.002(4) -0.036(6) F5C 0.064(6) 0.130(11) 0.106(11) -0.090(9) 0.009(7) -0.022(7) F6C 0.082(10) 0.116(12) 0.179(18) 0.003(11) 0.004(11) 0.038(9) _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 Fe N2 1.881(3) . ? Fe N1 1.986(3) . ? Fe N3 2.005(3) . ? O1 C2 1.380(6) . ? O1 C1 1.417(6) . ? O2 C28 1.376(5) . ? O2 C29 1.418(6) . ? N1 C7 1.330(5) . ? N1 C11 1.382(5) . ? N2 C23 1.338(5) . ? N2 C12 1.351(5) . ? N3 C21 1.336(5) . ? N3 C22 1.378(5) . ? C1 H11 0.9800 . ? C1 H12 0.9800 . ? C1 H13 0.9800 . ? C2 C3 1.382(6) . ? C2 C35 1.382(6) . ? C3 C4 1.396(6) . ? C3 H3 0.9500 . ? C4 C6 1.396(6) . ? C4 C5 1.511(6) . ? C5 H51 0.9800 . ? C5 H52 0.9800 . ? C5 H53 0.9800 . ? C6 C34 1.412(6) . ? C6 C8 1.493(6) . ? C7 C8 1.399(5) . ? C7 H7 0.9500 . ? C8 C9 1.390(6) . ? C9 C10 1.379(6) . ? C9 H9 0.9500 . ? C10 C11 1.381(6) . ? C10 C16B 1.438(9) . ? C10 H10 0.9500 . ? C11 C12 1.448(6) . ? C12 C13 1.406(6) . ? C13 C14 1.374(7) . ? C13 C17B 1.443(9) . ? C13 H131 0.9500 . ? C14 C15 1.400(7) . ? C14 H14 0.9500 . ? C15 C23 1.403(6) . ? C15 C16A 1.446(6) . ? C15 H15 0.9500 . ? C16A C17A 1.362(8) . ? C16A H161 0.9500 . ? C17A C18 1.440(6) . ? C17A H171 0.9500 . ? C16B C17B 1.357(12) . ? C16B H162 0.9500 . ? C17B H172 0.9500 . ? C18 C22 1.383(6) . ? C18 C19 1.410(6) . ? C18 H18 0.9500 . ? C19 C20 1.385(6) . ? C19 H19 0.9500 . ? C20 C21 1.417(5) . ? C20 C24 1.528(6) . ? C21 H21 0.9500 . ? C22 C23 1.415(6) . ? C24 C25 1.307(6) . ? C24 C31 1.425(6) . ? C25 C27 1.428(6) . ? C25 C26 1.537(6) . ? C26 H261 0.9800 . ? C26 H262 0.9800 . ? C26 H263 0.9800 . ? C27 C28 1.391(6) . ? C27 H27 0.9500 . ? C28 C30 1.388(6) . ? C29 H291 0.9800 . ? C29 H292 0.9800 . ? C29 H293 0.9800 . ? C30 C31 1.390(6) . ? C30 H30 0.9500 . ? C31 C32 1.516(7) . ? C32 H321 0.9800 . ? C32 H322 0.9800 . ? C32 H323 0.9800 . ? C33 C34 1.510(6) . ? C33 H331 0.9800 . ? C33 H332 0.9800 . ? C33 H333 0.9800 . ? C34 C35 1.384(6) . ? C35 H35 0.9500 . ? 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 N2 Fe N2 179.4(2) . 4 ? N2 Fe N1 99.83(13) . 4 ? N2 Fe N1 79.76(14) . . ? N1 Fe N1 86.63(18) 4 . ? N2 Fe N3 81.09(13) . . ? N1 Fe N3 160.85(13) . . ? N2 Fe N3 99.32(13) . 4 ? N1 Fe N3 96.45(13) . 4 ? N3 Fe N3 86.85(18) . 4 ? C2 O1 C1 116.4(4) . . ? C28 O2 C29 115.6(4) . . ? C7 N1 C11 118.4(3) . . ? C7 N1 Fe 127.1(3) . . ? C11 N1 Fe 114.4(3) . . ? C23 N2 C12 120.6(3) . . ? C23 N2 Fe 118.3(3) . . ? C12 N2 Fe 121.1(3) . . ? C21 N3 C22 117.0(3) . . ? C21 N3 Fe 130.9(3) . . ? C22 N3 Fe 111.9(3) . . ? O1 C1 H11 109.5 . . ? O1 C1 H12 109.5 . . ? H11 C1 H12 109.5 . . ? O1 C1 H13 109.5 . . ? H11 C1 H13 109.5 . . ? H12 C1 H13 109.5 . . ? O1 C2 C3 123.6(4) . . ? O1 C2 C35 116.2(4) . . ? C3 C2 C35 120.2(4) . . ? C2 C3 C4 120.2(4) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C6 C4 C3 119.6(4) . . ? C6 C4 C5 123.4(4) . . ? C3 C4 C5 117.0(4) . . ? C4 C5 H51 109.5 . . ? C4 C5 H52 109.5 . . ? H51 C5 H52 109.5 . . ? C4 C5 H53 109.5 . . ? H51 C5 H53 109.5 . . ? H52 C5 H53 109.5 . . ? C4 C6 C34 120.0(4) . . ? C4 C6 C8 119.9(4) . . ? C34 C6 C8 120.1(4) . . ? N1 C7 C8 123.7(4) . . ? N1 C7 H7 118.2 . . ? C8 C7 H7 118.2 . . ? C9 C8 C7 117.3(4) . . ? C9 C8 C6 123.4(4) . . ? C7 C8 C6 119.2(4) . . ? C10 C9 C8 119.8(4) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C9 C10 C11 120.1(4) . . ? C9 C10 C16B 133.1(12) . . ? C11 C10 C16B 105.5(12) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C10 C11 N1 120.6(4) . . ? C10 C11 C12 125.9(4) . . ? N1 C11 C12 113.5(4) . . ? N2 C12 C13 119.6(4) . . ? N2 C12 C11 110.8(3) . . ? C13 C12 C11 129.6(4) . . ? C14 C13 C12 119.8(4) . . ? C14 C13 C17B 139.4(12) . . ? C12 C13 C17B 100.8(12) . . ? C14 C13 H131 120.1 . . ? C12 C13 H131 120.1 . . ? C13 C14 C15 120.7(4) . . ? C13 C14 H14 119.6 . . ? C15 C14 H14 119.6 . . ? C14 C15 C23 116.3(4) . . ? C14 C15 C16A 129.2(4) . . ? C23 C15 C16A 114.5(4) . . ? C14 C15 H15 121.8 . . ? C23 C15 H15 121.8 . . ? C17A C16A C15 122.1(5) . . ? C17A C16A H161 119.0 . . ? C15 C16A H161 119.0 . . ? C16A C17A C18 122.8(5) . . ? C16A C17A H171 118.6 . . ? C18 C17A H171 118.6 . . ? C17B C16B C10 125(3) . . ? C17B C16B H162 117.4 . . ? C10 C16B H162 117.4 . . ? C16B C17B C13 132(3) . . ? C16B C17B H172 114.2 . . ? C13 C17B H172 114.2 . . ? C22 C18 C19 117.5(4) . . ? C22 C18 C17A 115.7(4) . . ? C19 C18 C17A 126.8(4) . . ? C22 C18 H18 121.3 . . ? C19 C18 H18 121.3 . . ? C20 C19 C18 120.3(4) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C19 C20 C21 117.7(4) . . ? C19 C20 C24 124.0(4) . . ? C21 C20 C24 118.3(3) . . ? N3 C21 C20 123.7(4) . . ? N3 C21 H21 118.2 . . ? C20 C21 H21 118.2 . . ? N3 C22 C18 123.9(4) . . ? N3 C22 C23 114.4(4) . . ? C18 C22 C23 121.7(4) . . ? N2 C23 C15 122.9(4) . . ? N2 C23 C22 113.9(3) . . ? C15 C23 C22 123.2(4) . . ? C25 C24 C31 123.2(4) . . ? C25 C24 C20 118.8(4) . . ? C31 C24 C20 117.9(4) . . ? C24 C25 C27 120.1(4) . . ? C24 C25 C26 127.0(4) . . ? C27 C25 C26 112.9(4) . . ? C25 C26 H261 109.5 . . ? C25 C26 H262 109.5 . . ? H261 C26 H262 109.5 . . ? C25 C26 H263 109.5 . . ? H261 C26 H263 109.5 . . ? H262 C26 H263 109.5 . . ? C28 C27 C25 118.5(4) . . ? C28 C27 H27 120.7 . . ? C25 C27 H27 120.7 . . ? O2 C28 C30 116.6(4) . . ? O2 C28 C27 123.2(4) . . ? C30 C28 C27 120.2(4) . . ? O2 C29 H291 109.5 . . ? O2 C29 H292 109.5 . . ? H291 C29 H292 109.5 . . ? O2 C29 H293 109.5 . . ? H291 C29 H293 109.5 . . ? H292 C29 H293 109.5 . . ? C28 C30 C31 121.1(4) . . ? C28 C30 H30 119.5 . . ? C31 C30 H30 119.5 . . ? C30 C31 C24 116.8(4) . . ? C30 C31 C32 118.1(4) . . ? C24 C31 C32 125.1(4) . . ? C31 C32 H321 109.5 . . ? C31 C32 H322 109.5 . . ? H321 C32 H322 109.5 . . ? C31 C32 H323 109.5 . . ? H321 C32 H323 109.5 . . ? H322 C32 H323 109.5 . . ? C34 C33 H331 109.5 . . ? C34 C33 H332 109.5 . . ? H331 C33 H332 109.5 . . ? C34 C33 H333 109.5 . . ? H331 C33 H333 109.5 . . ? H332 C33 H333 109.5 . . ? C35 C34 C6 118.9(4) . . ? C35 C34 C33 118.9(4) . . ? C6 C34 C33 122.2(4) . . ? C2 C35 C34 121.1(4) . . ? C2 C35 H35 119.5 . . ? C34 C35 H35 119.5 . . ? 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 N2 Fe N1 C7 -179.4(3) . . . . ? N2 Fe N1 C7 0.9(3) 4 . . . ? N1 Fe N1 C7 79.9(3) 4 . . . ? N3 Fe N1 C7 179.9(3) . . . . ? N3 Fe N1 C7 -81.1(3) 4 . . . ? N2 Fe N1 C11 5.8(3) . . . . ? N2 Fe N1 C11 -173.8(3) 4 . . . ? N1 Fe N1 C11 -94.8(3) 4 . . . ? N3 Fe N1 C11 5.2(6) . . . . ? N3 Fe N1 C11 104.2(3) 4 . . . ? N2 Fe N2 C23 -141.3(3) 4 . . . ? N1 Fe N2 C23 -99.1(3) 4 . . . ? N1 Fe N2 C23 176.1(3) . . . . ? N3 Fe N2 C23 -4.1(3) . . . . ? N3 Fe N2 C23 81.2(3) 4 . . . ? N2 Fe N2 C12 38.7(3) 4 . . . ? N1 Fe N2 C12 80.9(3) 4 . . . ? N1 Fe N2 C12 -3.8(3) . . . . ? N3 Fe N2 C12 175.9(3) . . . . ? N3 Fe N2 C12 -98.8(3) 4 . . . ? N2 Fe N3 C21 179.6(4) . . . . ? N2 Fe N3 C21 -0.8(4) 4 . . . ? N1 Fe N3 C21 -81.4(3) 4 . . . ? N1 Fe N3 C21 -179.7(4) . . . . ? N3 Fe N3 C21 79.7(3) 4 . . . ? N2 Fe N3 C22 5.5(3) . . . . ? N2 Fe N3 C22 -174.9(3) 4 . . . ? N1 Fe N3 C22 104.5(3) 4 . . . ? N1 Fe N3 C22 6.1(6) . . . . ? N3 Fe N3 C22 -94.5(3) 4 . . . ? C1 O1 C2 C3 2.9(7) . . . . ? C1 O1 C2 C35 -177.8(5) . . . . ? O1 C2 C3 C4 179.4(4) . . . . ? C35 C2 C3 C4 0.1(7) . . . . ? C2 C3 C4 C6 -0.8(7) . . . . ? C2 C3 C4 C5 -179.4(4) . . . . ? C3 C4 C6 C34 1.5(6) . . . . ? C5 C4 C6 C34 -179.9(4) . . . . ? C3 C4 C6 C8 -177.0(4) . . . . ? C5 C4 C6 C8 1.5(6) . . . . ? C11 N1 C7 C8 1.3(6) . . . . ? Fe N1 C7 C8 -173.3(3) . . . . ? N1 C7 C8 C9 0.9(6) . . . . ? N1 C7 C8 C6 -178.0(4) . . . . ? C4 C6 C8 C9 -56.4(6) . . . . ? C34 C6 C8 C9 125.0(4) . . . . ? C4 C6 C8 C7 122.4(4) . . . . ? C34 C6 C8 C7 -56.2(5) . . . . ? C7 C8 C9 C10 -2.1(6) . . . . ? C6 C8 C9 C10 176.7(4) . . . . ? C8 C9 C10 C11 1.1(6) . . . . ? C8 C9 C10 C16B -164(2) . . . . ? C9 C10 C11 N1 1.1(6) . . . . ? C16B C10 C11 N1 169.7(17) . . . . ? C9 C10 C11 C12 -179.1(4) . . . . ? C16B C10 C11 C12 -10.5(17) . . . . ? C7 N1 C11 C10 -2.3(5) . . . . ? Fe N1 C11 C10 172.9(3) . . . . ? C7 N1 C11 C12 177.9(3) . . . . ? Fe N1 C11 C12 -6.9(4) . . . . ? C23 N2 C12 C13 -0.1(6) . . . . ? Fe N2 C12 C13 179.8(3) . . . . ? C23 N2 C12 C11 -178.9(3) . . . . ? Fe N2 C12 C11 1.1(4) . . . . ? C10 C11 C12 N2 -175.9(4) . . . . ? N1 C11 C12 N2 3.9(5) . . . . ? C10 C11 C12 C13 5.5(7) . . . . ? N1 C11 C12 C13 -174.7(4) . . . . ? N2 C12 C13 C14 -1.6(6) . . . . ? C11 C12 C13 C14 176.8(4) . . . . ? N2 C12 C13 C17B -179.8(15) . . . . ? C11 C12 C13 C17B -1.4(16) . . . . ? C12 C13 C14 C15 1.0(7) . . . . ? C17B C13 C14 C15 178(2) . . . . ? C13 C14 C15 C23 1.3(7) . . . . ? C13 C14 C15 C16A -178.8(5) . . . . ? C14 C15 C16A C17A -179.1(5) . . . . ? C23 C15 C16A C17A 0.8(8) . . . . ? C15 C16A C17A C18 0.5(9) . . . . ? C9 C10 C16B C17B -179(3) . . . . ? C11 C10 C16B C17B 14(4) . . . . ? C10 C16B C17B C13 -14(7) . . . . ? C14 C13 C17B C16B -172(3) . . . . ? C12 C13 C17B C16B 5(4) . . . . ? C16A C17A C18 C22 -0.5(8) . . . . ? C16A C17A C18 C19 178.9(5) . . . . ? C22 C18 C19 C20 0.9(7) . . . . ? C17A C18 C19 C20 -178.5(5) . . . . ? C18 C19 C20 C21 -0.1(6) . . . . ? C18 C19 C20 C24 -179.0(4) . . . . ? C22 N3 C21 C20 2.0(6) . . . . ? Fe N3 C21 C20 -171.9(3) . . . . ? C19 C20 C21 N3 -1.5(6) . . . . ? C24 C20 C21 N3 177.5(4) . . . . ? C21 N3 C22 C18 -1.2(6) . . . . ? Fe N3 C22 C18 173.9(3) . . . . ? C21 N3 C22 C23 178.9(3) . . . . ? Fe N3 C22 C23 -6.1(4) . . . . ? C19 C18 C22 N3 -0.2(6) . . . . ? C17A C18 C22 N3 179.2(4) . . . . ? C19 C18 C22 C23 179.7(4) . . . . ? C17A C18 C22 C23 -0.8(7) . . . . ? C12 N2 C23 C15 2.6(6) . . . . ? Fe N2 C23 C15 -177.4(3) . . . . ? C12 N2 C23 C22 -178.2(3) . . . . ? Fe N2 C23 C22 1.8(5) . . . . ? C14 C15 C23 N2 -3.1(6) . . . . ? C16A C15 C23 N2 176.9(4) . . . . ? C14 C15 C23 C22 177.7(4) . . . . ? C16A C15 C23 C22 -2.2(6) . . . . ? N3 C22 C23 N2 3.1(5) . . . . ? C18 C22 C23 N2 -176.9(4) . . . . ? N3 C22 C23 C15 -177.7(4) . . . . ? C18 C22 C23 C15 2.3(7) . . . . ? C19 C20 C24 C25 128.3(5) . . . . ? C21 C20 C24 C25 -50.6(5) . . . . ? C19 C20 C24 C31 -54.6(6) . . . . ? C21 C20 C24 C31 126.4(4) . . . . ? C31 C24 C25 C27 -0.2(6) . . . . ? C20 C24 C25 C27 176.7(4) . . . . ? C31 C24 C25 C26 -179.1(4) . . . . ? C20 C24 C25 C26 -2.2(7) . . . . ? C24 C25 C27 C28 1.7(6) . . . . ? C26 C25 C27 C28 -179.2(4) . . . . ? C29 O2 C28 C30 174.3(4) . . . . ? C29 O2 C28 C27 -4.5(6) . . . . ? C25 C27 C28 O2 177.2(4) . . . . ? C25 C27 C28 C30 -1.6(6) . . . . ? O2 C28 C30 C31 -178.9(4) . . . . ? C27 C28 C30 C31 0.0(6) . . . . ? C28 C30 C31 C24 1.5(6) . . . . ? C28 C30 C31 C32 179.9(4) . . . . ? C25 C24 C31 C30 -1.5(6) . . . . ? C20 C24 C31 C30 -178.4(4) . . . . ? C25 C24 C31 C32 -179.7(4) . . . . ? C20 C24 C31 C32 3.4(6) . . . . ? C4 C6 C34 C35 -1.6(6) . . . . ? C8 C6 C34 C35 177.0(4) . . . . ? C4 C6 C34 C33 177.7(4) . . . . ? C8 C6 C34 C33 -3.8(6) . . . . ? O1 C2 C35 C34 -179.5(4) . . . . ? C3 C2 C35 C34 -0.2(7) . . . . ? C6 C34 C35 C2 0.9(7) . . . . ? C33 C34 C35 C2 -178.4(5) . . . . ? #===END data_3a _database_code_depnum_ccdc_archive 'CCDC 735249' # SG0314 _audit_creation_method SHELXL-97 _audit_creation_date 03-08-26 _chemical_name_systematic ; bis{8-(4-methoxy-2,6-dimethylphenyl)-2-[5-(4-methoxy-2,6- dimethylphenyl)-pyridin-2-yl]-1,10-phenanthroline}iron(II) hexafluorophosphate di-acetonitrile solvate ; _chemical_name_common ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_moiety 'C70 H62 Fe N6 O4 2+, 2(F6 P 1-), 2(C2 H3 N)' _chemical_formula_sum 'C74 H68 F12 Fe N8 O4 P2' _chemical_formula_weight 1479.17 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 296 0.0033 0.0016 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; H H 272 0.0000 0.0000 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; F F 48 0.0171 0.0103 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; Fe Fe 4 0.3463 0.8444 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; N N 32 0.0061 0.0033 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; O O 16 0.0106 0.0060 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; P P 8 0.1023 0.0942 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c c a ' _symmetry_space_group_name_Hall ? _symmetry_Int_Tables_number 54 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' 'x+1/2, -y, -z+1/2' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' '-x-1/2, y, z-1/2' 'x, -y, z-1/2' _cell_length_a 25.6038(5) _cell_length_b 12.2125(2) _cell_length_c 21.8379(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6828.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 160(1) _cell_measurement_reflns_used 106882 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.439 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3056 _exptl_absorpt_coefficient_mu 0.358 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Blessing, 1995)' _exptl_absorpt_correction_T_min 0.817 _exptl_absorpt_correction_T_max 0.917 _exptl_special_details ; Solvent used: acetonitrile / diethylether Cooling Device: Oxford Cryosystems Cryostream 700 Crystal mount: glued on a glass fibre Mosaicity (deg.): 0.682(1) Frames collected: 467 Seconds exposure per frame: 33 Degrees rotation per frame: 1.1 Crystal-Detector distance (mm): 38.7 ; _diffrn_ambient_temperature 160(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Nonius FR590 sealed tube generator' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_detector '65 mm CCD camera on \k goniostat' _diffrn_measurement_device_type 'Nonius KappaCCD area-detector diffractometer' _diffrn_measurement_method '\f and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 85406 _diffrn_reflns_av_R_equivalents 0.0846 _diffrn_reflns_av_sigmaI/netI 0.0425 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 25.03 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.999 _reflns_number_total 6034 _reflns_number_gt 4164 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'COLLECT (Nonius, 2000)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN and SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'SHELXL97 and PLATON (Spek, 2009)' _refine_special_details ; The asymmetric unit contains one half of a cation with the Fe-atom on a two-fold axis, one anion and two closely adjacent sites in general positions which represent two equally occupied disordered positions for an acetonitrile molecule. In the cation, the two central CH groups of the phenanthroline moiety are disordered over two sites which effectively complete six-membered rings between all pyridine rings, thereby indicating that the ligand must be disordered through a 180\% rotation about the central N-atom. The site occupation factor for the major conformation refined to 0.713(8). The PF6- anion is highly disordered. Three sets of P- and F-atoms were defined for this anion and refinement of the site occupation factors of each set led to values of 0.511(4), 0.292(8) and 0.197(8). The P-F and F...F distances were restrained tightly, so as to maintain octahedral geometry and uniform P-F bond lengths and the atomic displacement parameters of the P- and F-atoms were given light pseudo-isotropic restraints. The bond lengths within the disordered MeCN molecule were also restrained to logical values. Validation reports some short contacts as A alerts. These are mostly between different disordered components of anions and cations where the sums of the SOF of the relevant atoms is < 1.0, so that one can conceive that the "conflicting" sites are never occupied simultanously for adjacent moieties. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1069P)^2^+6.6299P] 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 SHELXL _refine_ls_extinction_coef 0.0027(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6034 _refine_ls_number_parameters 640 _refine_ls_number_restraints 944 _refine_ls_R_factor_all 0.1013 _refine_ls_R_factor_gt 0.0663 _refine_ls_wR_factor_ref 0.1991 _refine_ls_wR_factor_gt 0.1729 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.041 _refine_diff_density_min -0.411 _refine_diff_density_rms 0.082 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 Fe Fe 1.0000 0.29313(6) 0.2500 0.0407(3) Uani 1 2 d S . . O1 O 1.24202(13) 0.8453(3) 0.32757(15) 0.0877(10) Uani 1 1 d . . . O2 O 1.01604(12) -0.2567(2) -0.05010(13) 0.0659(8) Uani 1 1 d . A . N1 N 1.01787(11) 0.4133(2) 0.30874(12) 0.0417(7) Uani 1 1 d . . . N2 N 0.93920(11) 0.2945(2) 0.29811(13) 0.0436(7) Uani 1 1 d . A . N3 N 0.96067(10) 0.1724(2) 0.20753(13) 0.0426(7) Uani 1 1 d . . . C1 C 1.2749(3) 0.8607(7) 0.3800(3) 0.140(3) Uani 1 1 d . . . H11 H 1.2536 0.8839 0.4150 0.210 Uiso 1 1 calc R . . H12 H 1.3011 0.9170 0.3710 0.210 Uiso 1 1 calc R . . H13 H 1.2925 0.7917 0.3899 0.210 Uiso 1 1 calc R . . C2 C 1.20068(17) 0.7752(3) 0.3350(2) 0.0616(11) Uani 1 1 d . . . C3 C 1.18454(17) 0.7336(4) 0.3903(2) 0.0620(11) Uani 1 1 d . . . H3 H 1.2032 0.7521 0.4265 0.074 Uiso 1 1 calc R . . C4 C 1.14154(16) 0.6652(3) 0.39425(17) 0.0548(10) Uani 1 1 d . . . C5 C 1.12808(18) 0.6166(4) 0.45603(18) 0.0682(12) Uani 1 1 d . . . H51 H 1.0968 0.6527 0.4723 0.102 Uiso 1 1 calc R . . H52 H 1.1573 0.6277 0.4843 0.102 Uiso 1 1 calc R . . H53 H 1.1214 0.5380 0.4515 0.102 Uiso 1 1 calc R . . C6 C 1.11388(15) 0.6394(3) 0.34093(16) 0.0474(9) Uani 1 1 d . . . C7 C 1.06099(13) 0.4755(3) 0.30954(15) 0.0408(8) Uani 1 1 d . . . H7 H 1.0897 0.4538 0.2847 0.049 Uiso 1 1 calc R . . C8 C 1.06619(14) 0.5708(3) 0.34490(15) 0.0449(8) Uani 1 1 d . . . C9 C 1.02415(16) 0.5986(3) 0.38210(16) 0.0540(10) Uani 1 1 d . A . H9 H 1.0258 0.6631 0.4064 0.065 Uiso 1 1 calc R . . C10 C 0.98004(15) 0.5336(3) 0.38417(16) 0.0523(10) Uani 1 1 d . . . H10 H 0.9519 0.5513 0.4108 0.063 Uiso 0.713(8) 1 calc PR A 1 C11 C 0.97745(14) 0.4424(3) 0.34694(15) 0.0462(9) Uani 1 1 d . A . C12 C 0.93257(14) 0.3704(3) 0.34222(16) 0.0463(9) Uani 1 1 d . . . C13 C 0.88634(15) 0.3716(4) 0.37639(19) 0.0581(10) Uani 1 1 d . A . H131 H 0.8808 0.4267 0.4064 0.070 Uiso 0.713(8) 1 calc PR A 1 C14 C 0.84902(16) 0.2928(4) 0.3663(2) 0.0697(13) Uani 1 1 d . . . H14 H 0.8180 0.2925 0.3903 0.084 Uiso 1 1 calc R A . C15 C 0.85618(15) 0.2130(4) 0.3211(2) 0.0623(11) Uani 1 1 d . A . H15 H 0.8309 0.1575 0.3139 0.075 Uiso 0.287(8) 1 calc PR A 2 C16A C 0.8238(2) 0.1191(5) 0.3064(3) 0.0603(18) Uani 0.713(8) 1 d P A 1 H161 H 0.7931 0.1065 0.3299 0.072 Uiso 0.713(8) 1 calc PR A 1 C17A C 0.8358(2) 0.0488(5) 0.2605(2) 0.0541(16) Uani 0.713(8) 1 d P A 1 H171 H 0.8124 -0.0097 0.2521 0.065 Uiso 0.713(8) 1 calc PR A 1 C16B C 0.9289(9) 0.5367(17) 0.4117(8) 0.091(7) Uani 0.287(8) 1 d P A 2 H162 H 0.9245 0.5972 0.4385 0.109 Uiso 0.287(8) 1 calc PR A 2 C17B C 0.8876(8) 0.4758(19) 0.4082(8) 0.093(7) Uani 0.287(8) 1 d P A 2 H172 H 0.8566 0.5006 0.4275 0.111 Uiso 0.287(8) 1 calc PR A 2 C18 C 0.88375(14) 0.0588(3) 0.22254(18) 0.0540(10) Uani 1 1 d . . . H18 H 0.8520 0.0450 0.2436 0.065 Uiso 0.287(8) 1 calc PR A 2 C19 C 0.90051(15) -0.0089(3) 0.17512(18) 0.0545(10) Uani 1 1 d . A . H19 H 0.8805 -0.0715 0.1644 0.065 Uiso 1 1 calc R . . C20 C 0.94604(14) 0.0139(3) 0.14346(17) 0.0479(9) Uani 1 1 d . . . C21 C 0.97431(13) 0.1074(3) 0.16160(16) 0.0442(8) Uani 1 1 d . A . H21 H 1.0051 0.1250 0.1395 0.053 Uiso 1 1 calc R . . C22 C 0.91540(13) 0.1479(3) 0.23795(17) 0.0478(9) Uani 1 1 d . A . C23 C 0.90236(13) 0.2191(3) 0.28707(17) 0.0474(9) Uani 1 1 d . . . C24 C 0.96564(14) -0.0571(3) 0.09223(16) 0.0470(9) Uani 1 1 d . A . C25 C 0.93405(15) -0.0795(3) 0.04107(18) 0.0535(10) Uani 1 1 d . . . C26 C 0.87982(16) -0.0304(4) 0.0334(2) 0.0704(12) Uani 1 1 d . A . H261 H 0.8709 -0.0275 -0.0102 0.106 Uiso 1 1 calc R . . H262 H 0.8794 0.0438 0.0505 0.106 Uiso 1 1 calc R . . H263 H 0.8542 -0.0759 0.0550 0.106 Uiso 1 1 calc R . . C27 C 0.95277(16) -0.1463(3) -0.00436(18) 0.0572(10) Uani 1 1 d . A . H27 H 0.9310 -0.1625 -0.0384 0.069 Uiso 1 1 calc R . . C28 C 1.00221(16) -0.1907(3) -0.00221(18) 0.0508(9) Uani 1 1 d . . . C29 C 1.0683(2) -0.2943(4) -0.0522(2) 0.0767(14) Uani 1 1 d . . . H291 H 1.0921 -0.2315 -0.0524 0.115 Uiso 1 1 calc R A . H292 H 1.0736 -0.3377 -0.0894 0.115 Uiso 1 1 calc R . . H293 H 1.0754 -0.3399 -0.0162 0.115 Uiso 1 1 calc R . . C30 C 1.03426(15) -0.1664(3) 0.04698(17) 0.0498(9) Uani 1 1 d . A . H30 H 1.0686 -0.1955 0.0486 0.060 Uiso 1 1 calc R . . C31 C 1.01608(15) -0.0991(3) 0.09433(17) 0.0492(9) Uani 1 1 d . . . C32 C 1.05340(17) -0.0777(4) 0.1470(2) 0.0651(12) Uani 1 1 d . A . H321 H 1.0804 -0.1346 0.1477 0.098 Uiso 1 1 calc R . . H322 H 1.0341 -0.0789 0.1858 0.098 Uiso 1 1 calc R . . H323 H 1.0698 -0.0059 0.1417 0.098 Uiso 1 1 calc R . . C33 C 1.10218(19) 0.6589(4) 0.22556(19) 0.0697(12) Uani 1 1 d . . . H331 H 1.1160 0.7061 0.1931 0.105 Uiso 1 1 calc R . . H332 H 1.0648 0.6734 0.2309 0.105 Uiso 1 1 calc R . . H333 H 1.1072 0.5820 0.2142 0.105 Uiso 1 1 calc R . . C34 C 1.13059(16) 0.6821(3) 0.28477(17) 0.0487(9) Uani 1 1 d . . . C35 C 1.17418(17) 0.7483(3) 0.28238(19) 0.0559(10) Uani 1 1 d . . . H35 H 1.1860 0.7756 0.2441 0.067 Uiso 1 1 calc R . . P1A P 0.80326(11) 0.3127(3) -0.05400(13) 0.0651(10) Uani 0.511(4) 1 d PD B 1 F1A F 0.74911(19) 0.2679(7) -0.0316(3) 0.110(4) Uani 0.511(4) 1 d PDU B 1 F2A F 0.85730(19) 0.3591(5) -0.0758(3) 0.093(2) Uani 0.511(4) 1 d PDU B 1 F3A F 0.7772(3) 0.4263(5) -0.0678(3) 0.157(4) Uani 0.511(4) 1 d PDU B 1 F4A F 0.8297(2) 0.2000(4) -0.0391(4) 0.099(3) Uani 0.511(4) 1 d PDU B 1 F5A F 0.7908(3) 0.2741(7) -0.1209(2) 0.106(4) Uani 0.511(4) 1 d PDU B 1 F6A F 0.8160(2) 0.3518(6) 0.01284(19) 0.100(2) Uani 0.511(4) 1 d PDU B 1 P1B P 0.79845(18) 0.2475(7) -0.0641(2) 0.073(3) Uani 0.292(8) 1 d PDU C 2 F1B F 0.7535(4) 0.1648(11) -0.0484(7) 0.162(9) Uani 0.292(8) 1 d PDU C 2 F2B F 0.8431(5) 0.3308(13) -0.0800(7) 0.217(15) Uani 0.292(8) 1 d PDU C 2 F3B F 0.7615(5) 0.3452(10) -0.0470(6) 0.125(6) Uani 0.292(8) 1 d PDU C 2 F4B F 0.8354(5) 0.1499(12) -0.0815(7) 0.207(10) Uani 0.292(8) 1 d PDU C 2 F5B F 0.7785(5) 0.2531(13) -0.1319(3) 0.105(6) Uani 0.292(8) 1 d PDU C 2 F6B F 0.8185(5) 0.2421(15) 0.0037(3) 0.138(7) Uani 0.292(8) 1 d PDU C 2 P1C P 0.7975(4) 0.2438(11) -0.0627(5) 0.177(13) Uani 0.197(8) 1 d PDU D 3 F1C F 0.7416(5) 0.218(2) -0.0368(9) 0.085(8) Uani 0.197(8) 1 d PDU D 3 F2C F 0.8533(4) 0.2684(17) -0.0889(7) 0.085(6) Uani 0.197(8) 1 d PDU D 3 F3C F 0.7739(6) 0.334(2) -0.1055(11) 0.155(12) Uani 0.197(8) 1 d PDU D 3 F4C F 0.8213(7) 0.1537(17) -0.0198(10) 0.146(11) Uani 0.197(8) 1 d PDU D 3 F5C F 0.7889(9) 0.156(2) -0.1143(10) 0.254(19) Uani 0.197(8) 1 d PDU D 3 F6C F 0.8061(9) 0.3317(18) -0.0113(10) 0.202(18) Uani 0.197(8) 1 d PDU D 3 C37 C 0.7561(8) 0.514(3) 0.2882(6) 0.106(7) Uani 0.50 1 d PD E 1 H371 H 0.7771 0.5726 0.3062 0.158 Uiso 0.50 1 calc PR E 1 H372 H 0.7783 0.4684 0.2618 0.158 Uiso 0.50 1 calc PR E 1 H373 H 0.7413 0.4683 0.3209 0.158 Uiso 0.50 1 calc PR E 1 C38 C 0.7142(4) 0.5608(10) 0.2521(5) 0.086(3) Uani 0.50 1 d PD . 1 N39 N 0.6825(4) 0.6039(9) 0.2245(6) 0.099(3) Uani 0.50 1 d PD F 1 N40 N 0.6726(5) 0.6241(11) 0.1683(8) 0.133(5) Uani 0.50 1 d PD G 2 C41 C 0.7016(5) 0.5814(10) 0.1370(7) 0.110(5) Uani 0.50 1 d PD G 2 C42 C 0.7378(7) 0.5257(18) 0.0964(7) 0.139(7) Uani 0.50 1 d PD G 2 H421 H 0.7514 0.4602 0.1168 0.208 Uiso 0.50 1 calc PR G 2 H422 H 0.7667 0.5750 0.0862 0.208 Uiso 0.50 1 calc PR G 2 H423 H 0.7195 0.5044 0.0588 0.208 Uiso 0.50 1 calc PR G 2 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 Fe 0.0308(4) 0.0476(5) 0.0438(4) 0.000 0.0058(3) 0.000 O1 0.081(2) 0.097(2) 0.085(2) 0.0008(19) 0.0002(18) -0.037(2) O2 0.078(2) 0.0642(18) 0.0560(17) -0.0105(15) -0.0135(15) -0.0030(16) N1 0.0393(15) 0.0445(17) 0.0413(15) 0.0032(13) 0.0018(12) 0.0052(13) N2 0.0332(15) 0.0519(18) 0.0458(16) 0.0071(15) 0.0033(12) 0.0015(14) N3 0.0336(15) 0.0489(17) 0.0454(16) 0.0007(14) 0.0042(13) -0.0012(13) C1 0.105(5) 0.226(9) 0.090(4) -0.001(5) -0.018(4) -0.097(6) C2 0.063(3) 0.056(3) 0.066(3) -0.002(2) 0.001(2) -0.005(2) C3 0.067(3) 0.062(3) 0.056(2) -0.009(2) -0.005(2) -0.007(2) C4 0.062(2) 0.056(2) 0.046(2) -0.0063(18) -0.0030(18) -0.001(2) C5 0.076(3) 0.082(3) 0.047(2) 0.000(2) -0.006(2) -0.009(2) C6 0.056(2) 0.0400(19) 0.047(2) -0.0087(16) 0.0028(17) 0.0031(17) C7 0.0389(19) 0.045(2) 0.0383(18) 0.0013(15) 0.0025(14) 0.0018(16) C8 0.051(2) 0.046(2) 0.0375(18) -0.0025(16) -0.0008(16) 0.0036(17) C9 0.064(3) 0.055(2) 0.043(2) -0.0066(18) 0.0024(18) 0.007(2) C10 0.053(2) 0.064(3) 0.040(2) -0.0037(18) 0.0110(17) 0.012(2) C11 0.042(2) 0.057(2) 0.0400(19) 0.0058(17) 0.0016(16) 0.0072(18) C12 0.042(2) 0.052(2) 0.045(2) 0.0059(18) 0.0046(16) 0.0089(17) C13 0.045(2) 0.072(3) 0.058(2) -0.006(2) 0.0106(18) 0.010(2) C14 0.045(2) 0.093(3) 0.071(3) -0.010(3) 0.024(2) -0.001(2) C15 0.041(2) 0.081(3) 0.065(3) -0.005(2) 0.0186(19) -0.011(2) C16A 0.033(3) 0.085(4) 0.063(4) 0.001(3) 0.012(2) -0.016(3) C17A 0.037(3) 0.065(4) 0.060(3) 0.002(3) 0.005(2) -0.017(3) C16B 0.110(16) 0.088(13) 0.076(12) -0.002(10) 0.046(11) 0.033(12) C17B 0.079(13) 0.115(17) 0.084(13) 0.020(12) 0.042(10) 0.025(12) C18 0.040(2) 0.062(2) 0.059(2) 0.016(2) -0.0003(17) -0.0076(19) C19 0.050(2) 0.050(2) 0.064(2) 0.007(2) -0.0097(19) -0.0146(19) C20 0.047(2) 0.042(2) 0.054(2) 0.0056(17) -0.0089(17) -0.0076(17) C21 0.0387(19) 0.044(2) 0.050(2) 0.0028(17) 0.0002(16) -0.0011(16) C22 0.0346(18) 0.054(2) 0.055(2) 0.0099(18) 0.0043(16) -0.0033(17) C23 0.0379(19) 0.052(2) 0.052(2) 0.0069(18) 0.0055(16) 0.0045(17) C24 0.052(2) 0.0388(19) 0.050(2) 0.0036(16) -0.0070(17) -0.0091(17) C25 0.053(2) 0.050(2) 0.057(2) 0.0057(19) -0.0083(18) -0.0127(19) C26 0.054(3) 0.081(3) 0.076(3) 0.004(2) -0.015(2) -0.008(2) C27 0.060(3) 0.061(2) 0.051(2) 0.005(2) -0.0168(19) -0.016(2) C28 0.064(2) 0.041(2) 0.048(2) 0.0025(17) -0.0106(18) -0.0089(19) C29 0.085(3) 0.079(3) 0.066(3) -0.023(2) -0.017(2) 0.018(3) C30 0.054(2) 0.0387(19) 0.056(2) 0.0029(18) -0.0114(18) -0.0015(17) C31 0.061(2) 0.0358(19) 0.051(2) 0.0011(17) -0.0138(17) -0.0058(17) C32 0.066(3) 0.063(3) 0.067(3) -0.011(2) -0.023(2) 0.015(2) C33 0.085(3) 0.070(3) 0.055(2) 0.014(2) -0.011(2) -0.008(2) C34 0.062(2) 0.0366(19) 0.047(2) -0.0010(17) -0.0016(18) 0.0049(18) C35 0.069(3) 0.043(2) 0.056(2) 0.0012(19) 0.005(2) -0.003(2) P1A 0.0514(17) 0.090(2) 0.0535(19) 0.0134(17) -0.0094(12) 0.0013(17) F1A 0.047(4) 0.200(12) 0.084(5) 0.001(7) 0.002(3) -0.027(6) F2A 0.092(4) 0.120(6) 0.066(4) 0.025(4) -0.004(3) -0.044(4) F3A 0.194(9) 0.136(7) 0.143(7) 0.027(6) -0.047(6) 0.068(7) F4A 0.083(5) 0.076(5) 0.139(7) 0.003(5) -0.038(5) 0.007(4) F5A 0.076(5) 0.191(9) 0.050(4) -0.006(5) -0.010(3) -0.015(6) F6A 0.089(4) 0.139(6) 0.071(4) -0.001(4) -0.016(3) 0.002(4) P1B 0.031(3) 0.145(7) 0.043(3) 0.009(4) -0.018(2) 0.031(3) F1B 0.161(15) 0.174(15) 0.152(13) 0.029(12) -0.015(11) 0.033(12) F2B 0.20(2) 0.26(2) 0.19(2) 0.022(17) -0.007(16) -0.017(17) F3B 0.103(11) 0.153(14) 0.118(12) -0.040(10) -0.026(9) 0.015(10) F4B 0.151(13) 0.256(17) 0.214(17) -0.048(14) -0.034(12) 0.128(13) F5B 0.073(8) 0.186(14) 0.056(7) -0.010(8) -0.023(6) 0.036(9) F6B 0.129(10) 0.195(16) 0.091(9) 0.041(10) -0.056(8) 0.008(11) P1C 0.175(16) 0.186(16) 0.169(15) -0.001(10) 0.004(9) 0.019(10) F1C 0.037(8) 0.125(16) 0.094(12) 0.028(11) -0.025(8) -0.005(10) F2C 0.043(7) 0.129(14) 0.082(9) 0.027(10) 0.000(6) 0.012(8) F3C 0.128(16) 0.173(19) 0.164(19) 0.037(15) -0.049(14) 0.028(14) F4C 0.131(16) 0.135(17) 0.171(19) 0.046(14) -0.014(13) 0.046(13) F5C 0.25(2) 0.26(2) 0.25(2) -0.034(19) -0.032(18) 0.010(18) F6C 0.22(2) 0.20(2) 0.19(2) -0.046(18) -0.014(18) 0.002(17) C37 0.101(13) 0.103(16) 0.113(7) 0.002(12) 0.002(12) -0.040(13) C38 0.064(7) 0.094(9) 0.101(9) -0.017(7) 0.011(6) -0.024(6) N39 0.062(6) 0.113(8) 0.121(9) -0.020(7) -0.003(6) -0.018(6) N40 0.092(9) 0.141(11) 0.165(13) 0.015(10) 0.020(9) -0.041(8) C41 0.083(10) 0.097(10) 0.150(14) 0.026(10) -0.005(8) -0.038(8) C42 0.093(19) 0.11(2) 0.212(15) -0.001(12) -0.023(12) -0.038(11) _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 Fe N2 1.878(3) . ? Fe N1 2.002(3) . ? Fe N3 2.012(3) . ? O1 C2 1.372(5) . ? O1 C1 1.434(6) . ? O2 C28 1.368(5) . ? O2 C29 1.416(5) . ? N1 C7 1.340(4) . ? N1 C11 1.376(4) . ? N2 C23 1.340(5) . ? N2 C12 1.347(5) . ? N3 C21 1.325(4) . ? N3 C22 1.369(4) . ? C1 H11 0.9800 . ? C1 H12 0.9800 . ? C1 H13 0.9800 . ? C2 C3 1.373(6) . ? C2 C35 1.375(6) . ? C3 C4 1.385(6) . ? C3 H3 0.9500 . ? C4 C6 1.399(5) . ? C4 C5 1.514(6) . ? C5 H51 0.9800 . ? C5 H52 0.9800 . ? C5 H53 0.9800 . ? C6 C34 1.400(5) . ? C6 C8 1.484(5) . ? C7 C8 1.403(5) . ? C7 H7 0.9500 . ? C8 C9 1.391(5) . ? C9 C10 1.382(6) . ? C9 H9 0.9500 . ? C10 C11 1.380(5) . ? C10 C16B 1.442(19) . ? C10 H10 0.9500 . ? C11 C12 1.450(5) . ? C12 C13 1.399(5) . ? C13 C14 1.374(6) . ? C13 C17B 1.45(2) . ? C13 H131 0.9500 . ? C14 C15 1.399(6) . ? C14 H14 0.9500 . ? C15 C23 1.399(5) . ? C15 C16A 1.450(7) . ? C15 H15 0.9500 . ? C16A C17A 1.357(8) . ? C16A H161 0.9500 . ? C17A C18 1.487(6) . ? C17A H171 0.9500 . ? C16B C17B 1.29(3) . ? C16B H162 0.9500 . ? C17B H172 0.9500 . ? C18 C19 1.393(6) . ? C18 C22 1.397(5) . ? C18 H18 0.9500 . ? C19 C20 1.384(5) . ? C19 H19 0.9500 . ? C20 C21 1.408(5) . ? C20 C24 1.502(5) . ? C21 H21 0.9500 . ? C22 C23 1.421(5) . ? C24 C31 1.390(5) . ? C24 C25 1.406(5) . ? C25 C27 1.371(6) . ? C25 C26 1.522(6) . ? C26 H261 0.9800 . ? C26 H262 0.9800 . ? C26 H263 0.9800 . ? C27 C28 1.378(6) . ? C27 H27 0.9500 . ? C28 C30 1.384(5) . ? C29 H291 0.9800 . ? C29 H292 0.9800 . ? C29 H293 0.9800 . ? C30 C31 1.401(5) . ? C30 H30 0.9500 . ? C31 C32 1.519(5) . ? C32 H321 0.9800 . ? C32 H322 0.9800 . ? C32 H323 0.9800 . ? C33 C34 1.511(5) . ? C33 H331 0.9800 . ? C33 H332 0.9800 . ? C33 H333 0.9800 . ? C34 C35 1.379(6) . ? C35 H35 0.9500 . ? P1A F3A 1.568(3) . ? P1A F4A 1.568(3) . ? P1A F5A 1.568(3) . ? P1A F1A 1.569(3) . ? P1A F2A 1.569(3) . ? P1A F6A 1.570(3) . ? P1B F6B 1.568(3) . ? P1B F4B 1.568(3) . ? P1B F1B 1.569(3) . ? P1B F2B 1.569(3) . ? P1B F5B 1.569(3) . ? P1B F3B 1.569(3) . ? P1C F4C 1.568(3) . ? P1C F2C 1.568(3) . ? P1C F1C 1.569(3) . ? P1C F5C 1.569(3) . ? P1C F6C 1.569(3) . ? P1C F3C 1.569(3) . ? C37 C38 1.451(5) . ? C37 H371 0.9800 . ? C37 H372 0.9800 . ? C37 H373 0.9800 . ? C38 N39 1.139(5) . ? N40 C41 1.137(5) . ? C41 C42 1.450(5) . ? C42 H421 0.9800 . ? C42 H422 0.9800 . ? C42 H423 0.9800 . ? 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 N2 Fe N2 178.98(19) 4_755 . ? N2 Fe N1 79.89(12) . . ? N2 Fe N1 99.35(12) . 4_755 ? N1 Fe N1 85.73(16) . 4_755 ? N2 Fe N3 99.41(12) . 4_755 ? N1 Fe N3 97.33(11) . 4_755 ? N2 Fe N3 81.35(12) . . ? N1 Fe N3 161.24(11) . . ? C2 O1 C1 116.1(4) . . ? C28 O2 C29 117.4(3) . . ? C7 N1 C11 117.7(3) . . ? C7 N1 Fe 127.7(2) . . ? C11 N1 Fe 113.9(2) . . ? C23 N2 C12 120.8(3) . . ? C23 N2 Fe 118.5(2) . . ? C12 N2 Fe 120.7(2) . . ? C21 N3 C22 117.3(3) . . ? C21 N3 Fe 131.0(2) . . ? C22 N3 Fe 111.1(2) . . ? O1 C1 H11 109.5 . . ? O1 C1 H12 109.5 . . ? H11 C1 H12 109.5 . . ? O1 C1 H13 109.5 . . ? H11 C1 H13 109.5 . . ? H12 C1 H13 109.5 . . ? O1 C2 C3 124.6(4) . . ? O1 C2 C35 115.5(4) . . ? C3 C2 C35 119.9(4) . . ? C2 C3 C4 121.1(4) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? C3 C4 C6 119.2(4) . . ? C3 C4 C5 118.2(4) . . ? C6 C4 C5 122.6(4) . . ? C4 C5 H51 109.5 . . ? C4 C5 H52 109.5 . . ? H51 C5 H52 109.5 . . ? C4 C5 H53 109.5 . . ? H51 C5 H53 109.5 . . ? H52 C5 H53 109.5 . . ? C4 C6 C34 119.4(4) . . ? C4 C6 C8 119.7(3) . . ? C34 C6 C8 120.9(3) . . ? N1 C7 C8 123.7(3) . . ? N1 C7 H7 118.1 . . ? C8 C7 H7 118.1 . . ? C9 C8 C7 116.8(3) . . ? C9 C8 C6 122.2(3) . . ? C7 C8 C6 121.0(3) . . ? C10 C9 C8 120.8(4) . . ? C10 C9 H9 119.6 . . ? C8 C9 H9 119.6 . . ? C11 C10 C9 118.9(3) . . ? C11 C10 C16B 102.9(10) . . ? C9 C10 C16B 137.8(10) . . ? C11 C10 H10 120.5 . . ? C9 C10 H10 120.5 . . ? N1 C11 C10 122.0(3) . . ? N1 C11 C12 113.3(3) . . ? C10 C11 C12 124.7(3) . . ? N2 C12 C13 119.7(4) . . ? N2 C12 C11 111.6(3) . . ? C13 C12 C11 128.7(4) . . ? C14 C13 C12 119.7(4) . . ? C14 C13 C17B 135.0(9) . . ? C12 C13 C17B 104.2(8) . . ? C14 C13 H131 120.1 . . ? C12 C13 H131 120.1 . . ? C13 C14 C15 120.6(4) . . ? C13 C14 H14 119.7 . . ? C15 C14 H14 119.7 . . ? C23 C15 C14 116.6(4) . . ? C23 C15 C16A 114.1(4) . . ? C14 C15 C16A 129.1(4) . . ? C23 C15 H15 121.7 . . ? C14 C15 H15 121.7 . . ? C17A C16A C15 122.3(4) . . ? C17A C16A H161 118.8 . . ? C15 C16A H161 118.8 . . ? C16A C17A C18 123.1(5) . . ? C16A C17A H171 118.4 . . ? C18 C17A H171 118.4 . . ? C17B C16B C10 134.6(17) . . ? C17B C16B H162 112.7 . . ? C10 C16B H162 112.7 . . ? C16B C17B C13 123.4(15) . . ? C16B C17B H172 118.3 . . ? C13 C17B H172 118.3 . . ? C19 C18 C22 117.5(3) . . ? C19 C18 C17A 128.3(4) . . ? C22 C18 C17A 114.2(4) . . ? C19 C18 H18 121.2 . . ? C22 C18 H18 121.2 . . ? C20 C19 C18 120.7(3) . . ? C20 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? C19 C20 C21 117.1(4) . . ? C19 C20 C24 122.5(3) . . ? C21 C20 C24 120.4(3) . . ? N3 C21 C20 124.2(3) . . ? N3 C21 H21 117.9 . . ? C20 C21 H21 117.9 . . ? N3 C22 C18 123.0(4) . . ? N3 C22 C23 115.6(3) . . ? C18 C22 C23 121.5(3) . . ? N2 C23 C15 122.4(4) . . ? N2 C23 C22 113.0(3) . . ? C15 C23 C22 124.5(4) . . ? C31 C24 C25 119.3(3) . . ? C31 C24 C20 119.9(3) . . ? C25 C24 C20 120.8(3) . . ? C27 C25 C24 119.3(4) . . ? C27 C25 C26 118.3(3) . . ? C24 C25 C26 122.4(4) . . ? C25 C26 H261 109.5 . . ? C25 C26 H262 109.5 . . ? H261 C26 H262 109.5 . . ? C25 C26 H263 109.5 . . ? H261 C26 H263 109.5 . . ? H262 C26 H263 109.5 . . ? C25 C27 C28 122.0(4) . . ? C25 C27 H27 119.0 . . ? C28 C27 H27 119.0 . . ? O2 C28 C27 116.4(3) . . ? O2 C28 C30 124.5(4) . . ? C27 C28 C30 119.2(4) . . ? O2 C29 H291 109.5 . . ? O2 C29 H292 109.5 . . ? H291 C29 H292 109.5 . . ? O2 C29 H293 109.5 . . ? H291 C29 H293 109.5 . . ? H292 C29 H293 109.5 . . ? C28 C30 C31 120.1(4) . . ? C28 C30 H30 119.9 . . ? C31 C30 H30 119.9 . . ? C24 C31 C30 120.0(3) . . ? C24 C31 C32 123.1(3) . . ? C30 C31 C32 116.8(3) . . ? C31 C32 H321 109.5 . . ? C31 C32 H322 109.5 . . ? H321 C32 H322 109.5 . . ? C31 C32 H323 109.5 . . ? H321 C32 H323 109.5 . . ? H322 C32 H323 109.5 . . ? C34 C33 H331 109.5 . . ? C34 C33 H332 109.5 . . ? H331 C33 H332 109.5 . . ? C34 C33 H333 109.5 . . ? H331 C33 H333 109.5 . . ? H332 C33 H333 109.5 . . ? C35 C34 C6 119.9(4) . . ? C35 C34 C33 117.9(4) . . ? C6 C34 C33 122.2(4) . . ? C2 C35 C34 120.5(4) . . ? C2 C35 H35 119.7 . . ? C34 C35 H35 119.7 . . ? F3A P1A F4A 179.0(3) . . ? F3A P1A F5A 90.0(3) . . ? F4A P1A F5A 91.0(3) . . ? F3A P1A F1A 89.6(3) . . ? F4A P1A F1A 90.6(3) . . ? F5A P1A F1A 90.3(3) . . ? F3A P1A F2A 89.9(3) . . ? F4A P1A F2A 90.0(3) . . ? F5A P1A F2A 90.3(3) . . ? F1A P1A F2A 179.2(4) . . ? F3A P1A F6A 89.9(3) . . ? F4A P1A F6A 89.1(3) . . ? F5A P1A F6A 179.7(4) . . ? F1A P1A F6A 90.0(3) . . ? F2A P1A F6A 89.4(3) . . ? F6B P1B F4B 90.0(3) . . ? F6B P1B F1B 90.4(3) . . ? F4B P1B F1B 90.3(3) . . ? F6B P1B F2B 89.9(3) . . ? F4B P1B F2B 90.0(3) . . ? F1B P1B F2B 179.6(4) . . ? F6B P1B F5B 179.8(4) . . ? F4B P1B F5B 90.0(3) . . ? F1B P1B F5B 89.8(3) . . ? F2B P1B F5B 89.9(3) . . ? F6B P1B F3B 90.3(3) . . ? F4B P1B F3B 179.7(4) . . ? F1B P1B F3B 89.7(3) . . ? F2B P1B F3B 90.0(3) . . ? F5B P1B F3B 89.7(3) . . ? F4C P1C F2C 89.8(3) . . ? F4C P1C F1C 90.0(3) . . ? F2C P1C F1C 179.5(4) . . ? F4C P1C F5C 90.3(3) . . ? F2C P1C F5C 89.8(3) . . ? F1C P1C F5C 89.8(3) . . ? F4C P1C F6C 89.9(3) . . ? F2C P1C F6C 90.1(3) . . ? F1C P1C F6C 90.4(3) . . ? F5C P1C F6C 179.8(5) . . ? F4C P1C F3C 179.7(4) . . ? F2C P1C F3C 89.9(3) . . ? F1C P1C F3C 90.3(3) . . ? F5C P1C F3C 90.0(3) . . ? F6C P1C F3C 89.9(3) . . ? N39 C38 C37 175.8(17) . . ? N40 C41 C42 178.8(18) . . ? C41 C42 H421 109.5 . . ? C41 C42 H422 109.5 . . ? H421 C42 H422 109.5 . . ? C41 C42 H423 109.5 . . ? H421 C42 H423 109.5 . . ? H422 C42 H423 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 N2 Fe N1 C7 1.7(3) 4_755 . . . ? N2 Fe N1 C7 -177.6(3) . . . . ? N1 Fe N1 C7 -77.3(3) 4_755 . . . ? N3 Fe N1 C7 84.1(3) 4_755 . . . ? N3 Fe N1 C7 -177.6(3) . . . . ? N2 Fe N1 C11 172.6(2) 4_755 . . . ? N2 Fe N1 C11 -6.7(2) . . . . ? N1 Fe N1 C11 93.6(2) 4_755 . . . ? N3 Fe N1 C11 -105.0(2) 4_755 . . . ? N3 Fe N1 C11 -6.6(5) . . . . ? N1 Fe N2 C23 -176.1(3) . . . . ? N1 Fe N2 C23 100.0(3) 4_755 . . . ? N3 Fe N2 C23 -80.3(3) 4_755 . . . ? N3 Fe N2 C23 3.9(3) . . . . ? N1 Fe N2 C12 4.6(3) . . . . ? N1 Fe N2 C12 -79.3(3) 4_755 . . . ? N3 Fe N2 C12 100.5(3) 4_755 . . . ? N3 Fe N2 C12 -175.3(3) . . . . ? N2 Fe N3 C21 3.8(3) 4_755 . . . ? N2 Fe N3 C21 -176.9(3) . . . . ? N1 Fe N3 C21 -177.0(3) . . . . ? N1 Fe N3 C21 84.7(3) 4_755 . . . ? N3 Fe N3 C21 -76.7(3) 4_755 . . . ? N2 Fe N3 C22 174.6(2) 4_755 . . . ? N2 Fe N3 C22 -6.1(2) . . . . ? N1 Fe N3 C22 -6.2(5) . . . . ? N1 Fe N3 C22 -104.5(2) 4_755 . . . ? N3 Fe N3 C22 94.1(2) 4_755 . . . ? C1 O1 C2 C3 10.5(7) . . . . ? C1 O1 C2 C35 -170.6(5) . . . . ? O1 C2 C3 C4 178.4(4) . . . . ? C35 C2 C3 C4 -0.5(7) . . . . ? C2 C3 C4 C6 -0.8(6) . . . . ? C2 C3 C4 C5 176.1(4) . . . . ? C3 C4 C6 C34 0.8(6) . . . . ? C5 C4 C6 C34 -176.0(4) . . . . ? C3 C4 C6 C8 -176.9(4) . . . . ? C5 C4 C6 C8 6.3(6) . . . . ? C11 N1 C7 C8 -3.0(5) . . . . ? Fe N1 C7 C8 167.6(2) . . . . ? N1 C7 C8 C9 1.9(5) . . . . ? N1 C7 C8 C6 -176.4(3) . . . . ? C4 C6 C8 C9 55.8(5) . . . . ? C34 C6 C8 C9 -121.9(4) . . . . ? C4 C6 C8 C7 -126.0(4) . . . . ? C34 C6 C8 C7 56.3(5) . . . . ? C7 C8 C9 C10 0.9(5) . . . . ? C6 C8 C9 C10 179.2(3) . . . . ? C8 C9 C10 C11 -2.4(6) . . . . ? C8 C9 C10 C16B -174.5(12) . . . . ? C7 N1 C11 C10 1.4(5) . . . . ? Fe N1 C11 C10 -170.5(3) . . . . ? C7 N1 C11 C12 179.6(3) . . . . ? Fe N1 C11 C12 7.6(4) . . . . ? C9 C10 C11 N1 1.2(5) . . . . ? C16B C10 C11 N1 175.8(8) . . . . ? C9 C10 C11 C12 -176.7(3) . . . . ? C16B C10 C11 C12 -2.1(9) . . . . ? C23 N2 C12 C13 -0.9(5) . . . . ? Fe N2 C12 C13 178.3(3) . . . . ? C23 N2 C12 C11 179.1(3) . . . . ? Fe N2 C12 C11 -1.7(4) . . . . ? N1 C11 C12 N2 -4.1(4) . . . . ? C10 C11 C12 N2 174.0(3) . . . . ? N1 C11 C12 C13 175.9(4) . . . . ? C10 C11 C12 C13 -6.0(6) . . . . ? N2 C12 C13 C14 2.6(6) . . . . ? C11 C12 C13 C14 -177.4(4) . . . . ? N2 C12 C13 C17B -167.3(8) . . . . ? C11 C12 C13 C17B 12.7(10) . . . . ? C12 C13 C14 C15 -1.7(7) . . . . ? C17B C13 C14 C15 164.3(11) . . . . ? C13 C14 C15 C23 -0.7(7) . . . . ? C13 C14 C15 C16A 175.0(5) . . . . ? C23 C15 C16A C17A -4.7(8) . . . . ? C14 C15 C16A C17A 179.5(5) . . . . ? C15 C16A C17A C18 2.2(9) . . . . ? C11 C10 C16B C17B 1(3) . . . . ? C9 C10 C16B C17B 174.0(17) . . . . ? C10 C16B C17B C13 8(4) . . . . ? C14 C13 C17B C16B 179.5(14) . . . . ? C12 C13 C17B C16B -13(2) . . . . ? C16A C17A C18 C19 178.9(5) . . . . ? C16A C17A C18 C22 -0.6(7) . . . . ? C22 C18 C19 C20 -2.1(6) . . . . ? C17A C18 C19 C20 178.6(4) . . . . ? C18 C19 C20 C21 0.4(5) . . . . ? C18 C19 C20 C24 179.7(3) . . . . ? C22 N3 C21 C20 -1.8(5) . . . . ? Fe N3 C21 C20 168.6(3) . . . . ? C19 C20 C21 N3 1.6(5) . . . . ? C24 C20 C21 N3 -177.7(3) . . . . ? C21 N3 C22 C18 -0.1(5) . . . . ? Fe N3 C22 C18 -172.3(3) . . . . ? C21 N3 C22 C23 179.7(3) . . . . ? Fe N3 C22 C23 7.5(4) . . . . ? C19 C18 C22 N3 2.0(6) . . . . ? C17A C18 C22 N3 -178.6(4) . . . . ? C19 C18 C22 C23 -177.8(3) . . . . ? C17A C18 C22 C23 1.7(5) . . . . ? C12 N2 C23 C15 -1.6(5) . . . . ? Fe N2 C23 C15 179.1(3) . . . . ? C12 N2 C23 C22 178.4(3) . . . . ? Fe N2 C23 C22 -0.9(4) . . . . ? C14 C15 C23 N2 2.4(6) . . . . ? C16A C15 C23 N2 -173.9(4) . . . . ? C14 C15 C23 C22 -177.6(4) . . . . ? C16A C15 C23 C22 6.1(6) . . . . ? N3 C22 C23 N2 -4.7(5) . . . . ? C18 C22 C23 N2 175.1(3) . . . . ? N3 C22 C23 C15 175.4(4) . . . . ? C18 C22 C23 C15 -4.9(6) . . . . ? C19 C20 C24 C31 -125.4(4) . . . . ? C21 C20 C24 C31 53.9(5) . . . . ? C19 C20 C24 C25 56.4(5) . . . . ? C21 C20 C24 C25 -124.3(4) . . . . ? C31 C24 C25 C27 2.9(5) . . . . ? C20 C24 C25 C27 -178.8(3) . . . . ? C31 C24 C25 C26 -175.8(4) . . . . ? C20 C24 C25 C26 2.4(5) . . . . ? C24 C25 C27 C28 -1.4(6) . . . . ? C26 C25 C27 C28 177.4(4) . . . . ? C29 O2 C28 C27 173.8(4) . . . . ? C29 O2 C28 C30 -6.2(6) . . . . ? C25 C27 C28 O2 179.4(3) . . . . ? C25 C27 C28 C30 -0.6(6) . . . . ? O2 C28 C30 C31 -179.0(3) . . . . ? C27 C28 C30 C31 1.0(5) . . . . ? C25 C24 C31 C30 -2.5(5) . . . . ? C20 C24 C31 C30 179.3(3) . . . . ? C25 C24 C31 C32 178.9(4) . . . . ? C20 C24 C31 C32 0.6(5) . . . . ? C28 C30 C31 C24 0.5(5) . . . . ? C28 C30 C31 C32 179.2(4) . . . . ? C4 C6 C34 C35 0.4(6) . . . . ? C8 C6 C34 C35 178.1(3) . . . . ? C4 C6 C34 C33 -179.2(4) . . . . ? C8 C6 C34 C33 -1.5(6) . . . . ? O1 C2 C35 C34 -177.2(4) . . . . ? C3 C2 C35 C34 1.7(6) . . . . ? C6 C34 C35 C2 -1.7(6) . . . . ? C33 C34 C35 C2 177.9(4) . . . . ? #===END data_4a _database_code_depnum_ccdc_archive 'CCDC 735250' # SG0315 _audit_creation_method SHELXL-97 _audit_creation_date 03-08-27 _chemical_name_systematic ; bis{8-(4-methoxy-2,6-dimethylphenyl)-2-[5-(4-methoxy-2,6- dimethylphenyl)-pyridin-2-yl]-1,10-phenanthroline}cobalt(II) hexafluorophosphate di-acetonitrile solvate ; _chemical_name_common ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_moiety 'C70 H62 Co N6 O4 2+, 2(F6 P 1-), 2(C2 H3 N)' _chemical_formula_sum 'C74 H68 Co F12 N8 O4 P2' _chemical_formula_weight 1482.26 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 296 0.0033 0.0016 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; H H 272 0.0000 0.0000 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; Co Co 4 0.3494 0.9721 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; F F 48 0.0171 0.0103 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; N N 32 0.0061 0.0033 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; O O 16 0.0106 0.0060 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; P P 8 0.1023 0.0942 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c c a ' _symmetry_space_group_name_Hall ? _symmetry_Int_Tables_number 54 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' 'x+1/2, -y, -z+1/2' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' '-x-1/2, y, z-1/2' 'x, -y, z-1/2' _cell_length_a 25.3072(4) _cell_length_b 12.5642(1) _cell_length_c 21.8238(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6939.20(16) _cell_formula_units_Z 4 _cell_measurement_temperature 160(1) _cell_measurement_reflns_used 88463 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_description prism _exptl_crystal_colour orange-brown _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.419 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3060 _exptl_absorpt_coefficient_mu 0.382 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Blessing, 1995)' _exptl_absorpt_correction_T_min 0.834 _exptl_absorpt_correction_T_max 0.914 _exptl_special_details ; Solvent used: acetonitrile / diethylether Cooling Device: Oxford Cryosystems Cryostream 700 Crystal mount: glued on a glass fibre Mosaicity (deg.): 0.636(1) Frames collected: 395 Seconds exposure per frame: 60 Degrees rotation per frame: 1.0 Crystal-Detector distance (mm): 38.0 ; _diffrn_ambient_temperature 160(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Nonius FR590 sealed tube generator' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_detector '65 mm CCD camera on \k goniostat' _diffrn_measurement_device_type 'Nonius KappaCCD area-detector diffractometer' _diffrn_measurement_method '\f and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 68072 _diffrn_reflns_av_R_equivalents 0.0746 _diffrn_reflns_av_sigmaI/netI 0.0419 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 25.02 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.998 _reflns_number_total 6108 _reflns_number_gt 4150 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'COLLECT (Nonius, 2000)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN and SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'SHELXL97 and PLATON (Spek, 2009)' _refine_special_details ; The asymmetric unit contains one half of a cation with the Co-atom on a two-fold axis, one anion and two closely adjacent sites in general positions which represent two equally occupied disordered positions for an acetonitrile molecule. In the cation, the two central CH groups of the phenanthroline moiety are disordered over two sites which effectively complete six-membered rings between all pyridine rings, thereby indicating that the ligand must be disordered through a 180\% rotation about the central N-atom. The site occupation factor for the major conformation refined to 0.737(8). The PF6- anion is highly disordered. Three sets of P- and F-atoms were defined for this anion and refinement of the site occupation factors of each set led to values of 0.525(4), 0.291(8) and 0.184(7). The P-F and F...F distances were restrained tightly, so as to maintain octahedral geometry and uniform P-F bond lengths and the atomic displacement parameters of the P- and F-atoms were given pseudo-isotropic restraints. The bond lengths within the disordered MeCN molecule were also restrained to logical values. Validation reports some short contacts as A alerts. These are mostly between different disordered components of anions and cations where the sums of the SOF of the relevant atoms is < 1.0, so that one can conceive that the "conflicting" sites are never occupied simultanously for adjacent moieties. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1010P)^2^+3.9221P] 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_extinction_coef ? _refine_ls_number_reflns 6108 _refine_ls_number_parameters 637 _refine_ls_number_restraints 944 _refine_ls_R_factor_all 0.0969 _refine_ls_R_factor_gt 0.0587 _refine_ls_wR_factor_ref 0.1839 _refine_ls_wR_factor_gt 0.1593 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.932 _refine_diff_density_min -0.405 _refine_diff_density_rms 0.080 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 Co Co 1.0000 0.29206(5) 0.2500 0.0478(2) Uani 1 2 d S . . O1 O 1.23841(13) 0.8433(2) 0.33098(14) 0.0866(9) Uani 1 1 d . . . O2 O 1.01215(12) -0.2527(2) -0.04991(12) 0.0743(8) Uani 1 1 d . A . N1 N 1.01695(11) 0.4137(2) 0.31198(11) 0.0460(7) Uani 1 1 d . . . N2 N 0.93774(10) 0.2931(2) 0.29688(13) 0.0500(7) Uani 1 1 d . A . N3 N 0.95856(10) 0.1689(2) 0.20561(13) 0.0513(7) Uani 1 1 d . . . C1 C 1.2725(2) 0.8587(5) 0.3828(2) 0.113(2) Uani 1 1 d . . . H11 H 1.2517 0.8841 0.4177 0.169 Uiso 1 1 calc R . . H12 H 1.2996 0.9115 0.3725 0.169 Uiso 1 1 calc R . . H13 H 1.2895 0.7911 0.3934 0.169 Uiso 1 1 calc R . . C2 C 1.19736(16) 0.7741(3) 0.33889(19) 0.0631(10) Uani 1 1 d . . . C3 C 1.18187(15) 0.7322(3) 0.39400(18) 0.0610(10) Uani 1 1 d . . . H3 H 1.2012 0.7492 0.4300 0.073 Uiso 1 1 calc R . . C4 C 1.13811(15) 0.6651(3) 0.39794(15) 0.0539(9) Uani 1 1 d . . . C5 C 1.12459(17) 0.6169(3) 0.45938(16) 0.0679(10) Uani 1 1 d . . . H51 H 1.0923 0.6501 0.4753 0.102 Uiso 1 1 calc R . . H52 H 1.1538 0.6292 0.4881 0.102 Uiso 1 1 calc R . . H53 H 1.1189 0.5402 0.4546 0.102 Uiso 1 1 calc R . . C6 C 1.10959(14) 0.6406(3) 0.34475(15) 0.0514(8) Uani 1 1 d . . . C7 C 1.05929(13) 0.4769(3) 0.31375(14) 0.0457(8) Uani 1 1 d . . . H7 H 1.0893 0.4569 0.2903 0.055 Uiso 1 1 calc R . . C8 C 1.06219(14) 0.5710(3) 0.34815(14) 0.0484(8) Uani 1 1 d . . . C9 C 1.01851(15) 0.5949(3) 0.38398(15) 0.0581(9) Uani 1 1 d . A . H9 H 1.0189 0.6572 0.4087 0.070 Uiso 1 1 calc R . . C10 C 0.97472(15) 0.5303(3) 0.38435(15) 0.0597(10) Uani 1 1 d . . . H10 H 0.9451 0.5467 0.4094 0.072 Uiso 0.737(8) 1 calc PR A 1 C11 C 0.97463(13) 0.4405(3) 0.34730(14) 0.0512(8) Uani 1 1 d . A . C12 C 0.93013(13) 0.3669(3) 0.34071(15) 0.0546(9) Uani 1 1 d . . . C13 C 0.88282(16) 0.3681(4) 0.37394(19) 0.0713(11) Uani 1 1 d . A . H131 H 0.8764 0.4222 0.4034 0.086 Uiso 0.737(8) 1 calc PR A 1 C14 C 0.84578(17) 0.2900(4) 0.3635(2) 0.0879(14) Uani 1 1 d . . . H14 H 0.8140 0.2896 0.3866 0.105 Uiso 1 1 calc R A . C15 C 0.85415(16) 0.2114(4) 0.3195(2) 0.0774(13) Uani 1 1 d . A . H15 H 0.8293 0.1559 0.3126 0.093 Uiso 0.263(8) 1 calc PR A 2 C16A C 0.8212(2) 0.1204(5) 0.3065(3) 0.0729(19) Uani 0.737(8) 1 d P A 1 H161 H 0.7901 0.1094 0.3301 0.087 Uiso 0.737(8) 1 calc PR A 1 C17A C 0.8334(2) 0.0503(5) 0.2615(2) 0.0691(18) Uani 0.737(8) 1 d P A 1 H171 H 0.8099 -0.0075 0.2544 0.083 Uiso 0.737(8) 1 calc PR A 1 C16B C 0.9230(9) 0.5346(17) 0.4099(8) 0.091(7) Uani 0.263(8) 1 d P A 2 H162 H 0.9162 0.5940 0.4357 0.109 Uiso 0.263(8) 1 calc PR A 2 C17B C 0.8817(10) 0.466(2) 0.4026(9) 0.119(10) Uani 0.263(8) 1 d P A 2 H172 H 0.8487 0.4877 0.4190 0.143 Uiso 0.263(8) 1 calc PR A 2 C18 C 0.88140(14) 0.0591(3) 0.22289(18) 0.0643(10) Uani 1 1 d . . . H18 H 0.8497 0.0461 0.2449 0.077 Uiso 0.263(8) 1 calc PR A 2 C19 C 0.89731(15) -0.0079(3) 0.17592(18) 0.0644(10) Uani 1 1 d . A . H19 H 0.8767 -0.0688 0.1663 0.077 Uiso 1 1 calc R . . C20 C 0.94310(14) 0.0129(3) 0.14273(17) 0.0559(9) Uani 1 1 d . . . C21 C 0.97169(13) 0.1041(3) 0.16030(16) 0.0527(8) Uani 1 1 d . A . H21 H 1.0028 0.1203 0.1379 0.063 Uiso 1 1 calc R . . C22 C 0.91357(13) 0.1465(3) 0.23695(17) 0.0547(9) Uani 1 1 d . A . C23 C 0.90113(13) 0.2188(3) 0.28579(17) 0.0563(9) Uani 1 1 d . . . C24 C 0.96140(14) -0.0572(3) 0.09170(16) 0.0542(9) Uani 1 1 d . A . C25 C 0.92996(15) -0.0768(3) 0.04099(19) 0.0622(10) Uani 1 1 d . . . C26 C 0.87616(16) -0.0266(4) 0.0329(2) 0.0779(12) Uani 1 1 d . A . H261 H 0.8661 -0.0293 -0.0104 0.117 Uiso 1 1 calc R . . H262 H 0.8774 0.0477 0.0465 0.117 Uiso 1 1 calc R . . H263 H 0.8501 -0.0656 0.0574 0.117 Uiso 1 1 calc R . . C27 C 0.94869(16) -0.1420(3) -0.00517(18) 0.0635(10) Uani 1 1 d . A . H27 H 0.9268 -0.1560 -0.0396 0.076 Uiso 1 1 calc R . . C28 C 0.99863(16) -0.1874(3) -0.00252(18) 0.0585(9) Uani 1 1 d . . . C29 C 1.06443(19) -0.2922(4) -0.0509(2) 0.0817(13) Uani 1 1 d . . . H291 H 1.0893 -0.2325 -0.0513 0.123 Uiso 1 1 calc R A . H292 H 1.0696 -0.3356 -0.0877 0.123 Uiso 1 1 calc R . . H293 H 1.0706 -0.3359 -0.0144 0.123 Uiso 1 1 calc R . . C30 C 1.03097(15) -0.1655(3) 0.04759(16) 0.0569(9) Uani 1 1 d . A . H30 H 1.0655 -0.1952 0.0496 0.068 Uiso 1 1 calc R . . C31 C 1.01291(15) -0.1006(3) 0.09442(16) 0.0552(9) Uani 1 1 d . . . C32 C 1.05040(17) -0.0819(3) 0.14791(19) 0.0749(12) Uani 1 1 d . A . H321 H 1.0768 -0.1390 0.1492 0.112 Uiso 1 1 calc R . . H322 H 1.0303 -0.0815 0.1863 0.112 Uiso 1 1 calc R . . H323 H 1.0682 -0.0133 0.1427 0.112 Uiso 1 1 calc R . . C33 C 1.09707(19) 0.6595(4) 0.22974(18) 0.0776(12) Uani 1 1 d . . . H331 H 1.1091 0.7082 0.1976 0.116 Uiso 1 1 calc R . . H332 H 1.0591 0.6694 0.2365 0.116 Uiso 1 1 calc R . . H333 H 1.1038 0.5859 0.2171 0.116 Uiso 1 1 calc R . . C34 C 1.12645(16) 0.6823(3) 0.28796(16) 0.0565(9) Uani 1 1 d . . . C35 C 1.17002(17) 0.7484(3) 0.28589(18) 0.0630(10) Uani 1 1 d . . . H35 H 1.1814 0.7766 0.2477 0.076 Uiso 1 1 calc R . . P1A P 0.80453(11) 0.3110(3) -0.05601(12) 0.0601(8) Uani 0.525(4) 1 d PD B 1 F1A F 0.74909(18) 0.2713(7) -0.0334(3) 0.118(4) Uani 0.525(4) 1 d PDU B 1 F2A F 0.8599(2) 0.3526(7) -0.0776(3) 0.121(4) Uani 0.525(4) 1 d PDU B 1 F3A F 0.7792(3) 0.4210(5) -0.0731(4) 0.173(4) Uani 0.525(4) 1 d PDU B 1 F4A F 0.8299(3) 0.2017(4) -0.0376(4) 0.105(2) Uani 0.525(4) 1 d PDU B 1 F5A F 0.7922(3) 0.2675(7) -0.1218(2) 0.119(4) Uani 0.525(4) 1 d PDU B 1 F6A F 0.8170(3) 0.3532(5) 0.0102(2) 0.106(2) Uani 0.525(4) 1 d PDU B 1 P1B P 0.8024(3) 0.2679(9) -0.0638(4) 0.175(8) Uani 0.291(8) 1 d PDU C 2 F1B F 0.7585(5) 0.1843(10) -0.0478(8) 0.175(9) Uani 0.291(8) 1 d PDU C 2 F2B F 0.8464(5) 0.3516(15) -0.0796(8) 0.205(13) Uani 0.291(8) 1 d PDU C 2 F3B F 0.7623(4) 0.3608(10) -0.0518(5) 0.111(5) Uani 0.291(8) 1 d PDU C 2 F4B F 0.8425(6) 0.1750(14) -0.0762(8) 0.216(11) Uani 0.291(8) 1 d PDU C 2 F5B F 0.7849(7) 0.2644(14) -0.1327(4) 0.117(7) Uani 0.291(8) 1 d PDU C 2 F6B F 0.8199(5) 0.2707(15) 0.0052(4) 0.146(7) Uani 0.291(8) 1 d PDU C 2 P1C P 0.8001(2) 0.2420(9) -0.0643(3) 0.061(3) Uani 0.185(7) 1 d PDU D 3 F1C F 0.7435(4) 0.225(2) -0.0368(8) 0.098(9) Uani 0.185(7) 1 d PDU D 3 F2C F 0.8566(3) 0.2590(13) -0.0921(6) 0.069(5) Uani 0.185(7) 1 d PDU D 3 F3C F 0.7765(6) 0.318(2) -0.1144(9) 0.143(12) Uani 0.185(7) 1 d PDU D 3 F4C F 0.8239(6) 0.1665(19) -0.0142(9) 0.148(12) Uani 0.185(7) 1 d PDU D 3 F5C F 0.7914(8) 0.1442(17) -0.1079(10) 0.30(2) Uani 0.185(7) 1 d PDU D 3 F6C F 0.8088(9) 0.3401(17) -0.0210(10) 0.24(2) Uani 0.185(7) 1 d PDU D 3 C37 C 0.7548(17) 0.514(6) 0.2885(5) 0.129(14) Uani 0.50 1 d PD E 1 H371 H 0.7674 0.5650 0.3192 0.193 Uiso 0.50 1 calc PR E 1 H372 H 0.7843 0.4934 0.2618 0.193 Uiso 0.50 1 calc PR E 1 H373 H 0.7408 0.4508 0.3090 0.193 Uiso 0.50 1 calc PR E 1 C38 C 0.7136(4) 0.5628(9) 0.2519(5) 0.090(3) Uani 0.50 1 d PD . 1 N39 N 0.6826(4) 0.6059(9) 0.2232(6) 0.111(3) Uani 0.50 1 d PD F 1 N40 N 0.6744(4) 0.6189(9) 0.1659(6) 0.122(4) Uani 0.50 1 d PD G 2 C41 C 0.7031(5) 0.5760(8) 0.1340(5) 0.103(4) Uani 0.50 1 d PD G 2 C42 C 0.7394(9) 0.521(2) 0.0936(6) 0.125(7) Uani 0.50 1 d PD G 2 H421 H 0.7486 0.4516 0.1115 0.187 Uiso 0.50 1 calc PR G 2 H422 H 0.7715 0.5633 0.0883 0.187 Uiso 0.50 1 calc PR G 2 H423 H 0.7225 0.5097 0.0536 0.187 Uiso 0.50 1 calc PR G 2 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 Co 0.0379(4) 0.0515(4) 0.0540(4) 0.000 0.0013(3) 0.000 O1 0.089(2) 0.078(2) 0.093(2) 0.0049(17) -0.0069(17) -0.0228(17) O2 0.081(2) 0.0765(18) 0.0650(17) -0.0105(15) -0.0185(14) -0.0045(16) N1 0.0489(16) 0.0481(16) 0.0409(14) 0.0040(12) 0.0003(12) 0.0066(13) N2 0.0379(15) 0.0581(18) 0.0540(17) 0.0085(14) 0.0030(12) 0.0034(14) N3 0.0364(15) 0.0514(16) 0.0662(18) 0.0031(15) 0.0055(13) -0.0029(13) C1 0.085(4) 0.153(5) 0.100(4) -0.001(4) -0.013(3) -0.052(4) C2 0.065(2) 0.049(2) 0.075(3) 0.0020(19) -0.002(2) 0.0022(19) C3 0.068(3) 0.055(2) 0.060(2) -0.0059(18) -0.0106(19) 0.0065(19) C4 0.065(2) 0.047(2) 0.050(2) -0.0047(16) -0.0019(16) 0.0121(18) C5 0.079(3) 0.079(3) 0.046(2) -0.0053(19) -0.0057(18) 0.004(2) C6 0.060(2) 0.0381(18) 0.056(2) -0.0045(15) -0.0044(16) 0.0088(16) C7 0.049(2) 0.048(2) 0.0411(17) 0.0000(15) -0.0010(14) 0.0064(16) C8 0.058(2) 0.0456(19) 0.0417(17) -0.0040(15) -0.0038(15) 0.0093(16) C9 0.068(2) 0.062(2) 0.0442(19) -0.0124(16) -0.0010(17) 0.015(2) C10 0.058(2) 0.079(3) 0.0419(18) -0.0030(18) 0.0066(16) 0.022(2) C11 0.046(2) 0.065(2) 0.0429(18) 0.0070(16) 0.0020(15) 0.0089(17) C12 0.046(2) 0.068(2) 0.0496(19) 0.0083(18) 0.0040(15) 0.0138(18) C13 0.055(3) 0.090(3) 0.069(3) -0.011(2) 0.0105(19) 0.014(2) C14 0.049(2) 0.121(4) 0.094(3) -0.015(3) 0.026(2) 0.001(3) C15 0.050(2) 0.102(3) 0.081(3) -0.010(3) 0.018(2) -0.014(2) C16A 0.040(3) 0.102(5) 0.077(4) 0.004(3) 0.018(2) -0.017(3) C17A 0.045(3) 0.086(4) 0.076(4) 0.005(3) 0.011(3) -0.025(3) C16B 0.110(16) 0.093(14) 0.070(11) 0.005(10) 0.039(11) 0.044(12) C17B 0.106(17) 0.17(3) 0.083(14) 0.052(15) 0.062(13) 0.056(17) C18 0.047(2) 0.078(3) 0.068(2) 0.018(2) 0.0011(18) -0.011(2) C19 0.057(2) 0.060(2) 0.076(2) 0.011(2) -0.0090(19) -0.0199(19) C20 0.050(2) 0.049(2) 0.068(2) 0.0109(18) -0.0068(17) -0.0111(17) C21 0.0417(19) 0.047(2) 0.070(2) 0.0077(18) 0.0013(16) -0.0041(16) C22 0.0389(19) 0.057(2) 0.068(2) 0.0095(18) 0.0027(16) -0.0052(17) C23 0.0397(19) 0.065(2) 0.064(2) 0.0103(19) 0.0044(16) 0.0026(18) C24 0.064(2) 0.0405(18) 0.058(2) 0.0073(16) -0.0047(17) -0.0114(17) C25 0.057(2) 0.055(2) 0.074(3) 0.017(2) -0.0100(19) -0.0153(18) C26 0.057(2) 0.088(3) 0.089(3) 0.008(2) -0.015(2) -0.006(2) C27 0.066(3) 0.063(2) 0.061(2) 0.010(2) -0.0182(19) -0.016(2) C28 0.072(3) 0.050(2) 0.053(2) 0.0058(17) -0.0118(18) -0.0152(19) C29 0.093(3) 0.081(3) 0.071(3) -0.019(2) -0.022(2) 0.011(3) C30 0.064(2) 0.0435(19) 0.063(2) 0.0069(17) -0.0127(18) -0.0074(17) C31 0.064(2) 0.0407(19) 0.061(2) 0.0061(17) -0.0140(17) -0.0078(17) C32 0.081(3) 0.071(3) 0.073(3) -0.014(2) -0.030(2) 0.015(2) C33 0.106(4) 0.069(3) 0.058(2) 0.010(2) -0.013(2) -0.011(2) C34 0.078(3) 0.0395(19) 0.052(2) 0.0010(16) -0.0053(18) 0.0069(18) C35 0.084(3) 0.046(2) 0.059(2) 0.0039(18) -0.001(2) 0.003(2) P1A 0.0403(14) 0.087(2) 0.0534(16) 0.0164(15) -0.0103(10) -0.0033(14) F1A 0.047(4) 0.226(12) 0.081(5) 0.011(6) 0.004(3) -0.011(5) F2A 0.080(4) 0.201(9) 0.082(4) 0.051(5) -0.011(3) -0.068(5) F3A 0.196(9) 0.159(8) 0.163(7) 0.059(7) -0.046(6) 0.047(7) F4A 0.093(5) 0.084(4) 0.139(7) 0.011(5) -0.038(5) 0.016(4) F5A 0.075(5) 0.233(12) 0.050(4) 0.001(5) -0.006(3) -0.003(6) F6A 0.111(5) 0.121(5) 0.086(4) -0.005(4) -0.027(3) 0.004(4) P1B 0.173(11) 0.208(11) 0.143(10) 0.011(9) -0.033(8) 0.017(9) F1B 0.196(17) 0.148(12) 0.180(15) 0.010(11) -0.016(12) 0.059(12) F2B 0.152(16) 0.27(2) 0.188(18) 0.005(16) -0.018(13) -0.046(16) F3B 0.088(9) 0.147(11) 0.097(9) -0.019(8) -0.029(7) 0.011(9) F4B 0.158(14) 0.286(19) 0.204(17) -0.037(15) -0.038(12) 0.131(14) F5B 0.082(10) 0.200(16) 0.069(8) 0.004(9) -0.017(7) 0.052(10) F6B 0.106(9) 0.246(18) 0.086(8) 0.058(11) -0.027(7) 0.013(12) P1C 0.019(3) 0.121(7) 0.044(4) 0.015(4) -0.008(3) 0.023(4) F1C 0.049(10) 0.162(18) 0.084(13) 0.035(13) -0.011(9) -0.010(11) F2C 0.032(7) 0.081(10) 0.095(9) 0.014(8) -0.001(6) 0.004(6) F3C 0.080(13) 0.183(19) 0.17(2) 0.071(15) -0.028(13) 0.021(13) F4C 0.132(16) 0.147(18) 0.166(18) 0.076(14) -0.017(13) 0.031(13) F5C 0.29(3) 0.29(3) 0.31(3) -0.06(2) 0.010(19) -0.042(19) F6C 0.25(3) 0.21(3) 0.24(3) -0.03(2) 0.00(2) 0.025(19) C37 0.130(17) 0.14(3) 0.115(7) -0.006(15) 0.006(15) -0.02(2) C38 0.072(7) 0.094(8) 0.105(8) -0.017(7) 0.018(6) -0.025(6) N39 0.075(6) 0.134(9) 0.125(9) -0.018(7) -0.002(6) -0.014(6) N40 0.085(7) 0.141(10) 0.140(10) 0.017(8) 0.015(7) -0.050(7) C41 0.100(9) 0.097(9) 0.112(9) 0.021(7) 0.005(7) -0.050(7) C42 0.10(2) 0.11(2) 0.166(10) -0.006(10) -0.013(10) -0.046(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co N2 1.879(3) . ? Co N1 2.086(3) . ? Co N3 2.105(3) . ? O1 C2 1.366(5) . ? O1 C1 1.435(5) . ? O2 C28 1.364(5) . ? O2 C29 1.413(5) . ? N1 C7 1.334(4) . ? N1 C11 1.362(4) . ? N2 C23 1.337(5) . ? N2 C12 1.346(4) . ? N3 C21 1.324(4) . ? N3 C22 1.358(4) . ? C1 H11 0.9800 . ? C1 H12 0.9800 . ? C1 H13 0.9800 . ? C2 C3 1.370(5) . ? C2 C35 1.386(5) . ? C3 C4 1.394(5) . ? C3 H3 0.9500 . ? C4 C6 1.401(5) . ? C4 C5 1.511(5) . ? C5 H51 0.9800 . ? C5 H52 0.9800 . ? C5 H53 0.9800 . ? C6 C34 1.412(5) . ? C6 C8 1.487(5) . ? C7 C8 1.402(4) . ? C7 H7 0.9500 . ? C8 C9 1.387(5) . ? C9 C10 1.374(6) . ? C9 H9 0.9500 . ? C10 C11 1.388(5) . ? C10 C16B 1.42(2) . ? C10 H10 0.9500 . ? C11 C12 1.465(5) . ? C12 C13 1.400(5) . ? C13 C14 1.376(6) . ? C13 C17B 1.38(3) . ? C13 H131 0.9500 . ? C14 C15 1.394(6) . ? C14 H14 0.9500 . ? C15 C23 1.401(5) . ? C15 C16A 1.444(7) . ? C15 H15 0.9500 . ? C16A C17A 1.354(8) . ? C16A H161 0.9500 . ? C17A C18 1.484(6) . ? C17A H171 0.9500 . ? C16B C17B 1.37(3) . ? C16B H162 0.9500 . ? C17B H172 0.9500 . ? C18 C19 1.386(6) . ? C18 C22 1.401(5) . ? C18 H18 0.9500 . ? C19 C20 1.391(5) . ? C19 H19 0.9500 . ? C20 C21 1.408(5) . ? C20 C24 1.493(5) . ? C21 H21 0.9500 . ? C22 C23 1.435(5) . ? C24 C25 1.385(5) . ? C24 C31 1.414(5) . ? C25 C27 1.382(6) . ? C25 C26 1.511(6) . ? C26 H261 0.9800 . ? C26 H262 0.9800 . ? C26 H263 0.9800 . ? C27 C28 1.388(5) . ? C27 H27 0.9500 . ? C28 C30 1.393(5) . ? C29 H291 0.9800 . ? C29 H292 0.9800 . ? C29 H293 0.9800 . ? C30 C31 1.385(5) . ? C30 H30 0.9500 . ? C31 C32 1.523(5) . ? C32 H321 0.9800 . ? C32 H322 0.9800 . ? C32 H323 0.9800 . ? C33 C34 1.500(5) . ? C33 H331 0.9800 . ? C33 H332 0.9800 . ? C33 H333 0.9800 . ? C34 C35 1.381(6) . ? C35 H35 0.9500 . ? P1A F3A 1.568(3) . ? P1A F5A 1.568(3) . ? P1A F2A 1.568(3) . ? P1A F4A 1.569(3) . ? P1A F1A 1.569(3) . ? P1A F6A 1.571(3) . ? P1B F2B 1.569(3) . ? P1B F3B 1.569(3) . ? P1B F4B 1.569(3) . ? P1B F6B 1.569(3) . ? P1B F5B 1.569(3) . ? P1B F1B 1.569(3) . ? P1C F5C 1.569(3) . ? P1C F2C 1.569(3) . ? P1C F4C 1.569(3) . ? P1C F1C 1.569(3) . ? P1C F6C 1.569(3) . ? P1C F3C 1.569(3) . ? C37 C38 1.450(5) . ? C37 H371 0.9800 . ? C37 H372 0.9800 . ? C37 H373 0.9800 . ? C38 N39 1.140(5) . ? N40 C41 1.141(5) . ? C41 C42 1.450(5) . ? C42 H421 0.9800 . ? C42 H422 0.9800 . ? C42 H423 0.9800 . ? 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 N2 Co N2 179.23(18) 4_755 . ? N2 Co N1 100.12(11) . 4_755 ? N2 Co N1 79.31(12) . . ? N1 Co N1 85.73(14) 4_755 . ? N2 Co N3 80.66(12) . . ? N1 Co N3 159.97(11) . . ? N2 Co N3 99.91(11) . 4_755 ? N1 Co N3 97.92(10) . 4_755 ? N3 Co N3 85.41(16) . 4_755 ? C2 O1 C1 116.4(3) . . ? C28 O2 C29 117.2(3) . . ? C7 N1 C11 117.9(3) . . ? C7 N1 Co 128.3(2) . . ? C11 N1 Co 112.7(2) . . ? C23 N2 C12 120.7(3) . . ? C23 N2 Co 118.6(2) . . ? C12 N2 Co 120.8(2) . . ? C21 N3 C22 117.3(3) . . ? C21 N3 Co 132.2(2) . . ? C22 N3 Co 109.8(2) . . ? O1 C1 H11 109.5 . . ? O1 C1 H12 109.5 . . ? H11 C1 H12 109.5 . . ? O1 C1 H13 109.5 . . ? H11 C1 H13 109.5 . . ? H12 C1 H13 109.5 . . ? O1 C2 C3 125.0(4) . . ? O1 C2 C35 115.0(4) . . ? C3 C2 C35 120.0(4) . . ? C2 C3 C4 120.9(4) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C3 C4 C6 119.4(3) . . ? C3 C4 C5 118.5(3) . . ? C6 C4 C5 122.0(3) . . ? C4 C5 H51 109.5 . . ? C4 C5 H52 109.5 . . ? H51 C5 H52 109.5 . . ? C4 C5 H53 109.5 . . ? H51 C5 H53 109.5 . . ? H52 C5 H53 109.5 . . ? C4 C6 C34 119.3(3) . . ? C4 C6 C8 120.2(3) . . ? C34 C6 C8 120.4(3) . . ? N1 C7 C8 124.0(3) . . ? N1 C7 H7 118.0 . . ? C8 C7 H7 118.0 . . ? C9 C8 C7 116.3(3) . . ? C9 C8 C6 122.9(3) . . ? C7 C8 C6 120.8(3) . . ? C10 C9 C8 121.2(3) . . ? C10 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? C9 C10 C11 118.6(3) . . ? C9 C10 C16B 136.2(10) . . ? C11 C10 C16B 104.9(10) . . ? C9 C10 H10 120.7 . . ? C11 C10 H10 120.7 . . ? N1 C11 C10 122.0(3) . . ? N1 C11 C12 113.2(3) . . ? C10 C11 C12 124.9(3) . . ? N2 C12 C13 119.9(4) . . ? N2 C12 C11 113.3(3) . . ? C13 C12 C11 126.9(4) . . ? C14 C13 C17B 134.1(11) . . ? C14 C13 C12 119.3(4) . . ? C17B C13 C12 105.2(10) . . ? C14 C13 H131 120.4 . . ? C12 C13 H131 120.4 . . ? C13 C14 C15 121.1(4) . . ? C13 C14 H14 119.5 . . ? C15 C14 H14 119.5 . . ? C14 C15 C23 116.3(4) . . ? C14 C15 C16A 127.5(4) . . ? C23 C15 C16A 116.1(4) . . ? C14 C15 H15 121.8 . . ? C23 C15 H15 121.8 . . ? C17A C16A C15 121.7(4) . . ? C17A C16A H161 119.1 . . ? C15 C16A H161 119.1 . . ? C16A C17A C18 123.4(5) . . ? C16A C17A H171 118.3 . . ? C18 C17A H171 118.3 . . ? C17B C16B C10 129.4(17) . . ? C17B C16B H162 115.3 . . ? C10 C16B H162 115.3 . . ? C16B C17B C13 126.9(16) . . ? C16B C17B H172 116.6 . . ? C13 C17B H172 116.6 . . ? C19 C18 C22 118.0(3) . . ? C19 C18 C17A 127.8(4) . . ? C22 C18 C17A 114.2(4) . . ? C19 C18 H18 121.0 . . ? C22 C18 H18 121.0 . . ? C18 C19 C20 120.8(3) . . ? C18 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? C19 C20 C21 116.0(4) . . ? C19 C20 C24 122.4(3) . . ? C21 C20 C24 121.6(3) . . ? N3 C21 C20 125.1(3) . . ? N3 C21 H21 117.4 . . ? C20 C21 H21 117.4 . . ? N3 C22 C18 122.7(3) . . ? N3 C22 C23 115.3(3) . . ? C18 C22 C23 122.1(3) . . ? N2 C23 C15 122.7(4) . . ? N2 C23 C22 115.1(3) . . ? C15 C23 C22 122.3(4) . . ? C25 C24 C31 119.6(3) . . ? C25 C24 C20 121.5(3) . . ? C31 C24 C20 118.8(3) . . ? C27 C25 C24 119.4(4) . . ? C27 C25 C26 118.1(3) . . ? C24 C25 C26 122.4(4) . . ? C25 C26 H261 109.5 . . ? C25 C26 H262 109.5 . . ? H261 C26 H262 109.5 . . ? C25 C26 H263 109.5 . . ? H261 C26 H263 109.5 . . ? H262 C26 H263 109.5 . . ? C25 C27 C28 121.7(3) . . ? C25 C27 H27 119.1 . . ? C28 C27 H27 119.1 . . ? O2 C28 C27 116.4(3) . . ? O2 C28 C30 124.5(4) . . ? C27 C28 C30 119.1(4) . . ? O2 C29 H291 109.5 . . ? O2 C29 H292 109.5 . . ? H291 C29 H292 109.5 . . ? O2 C29 H293 109.5 . . ? H291 C29 H293 109.5 . . ? H292 C29 H293 109.5 . . ? C31 C30 C28 120.1(4) . . ? C31 C30 H30 120.0 . . ? C28 C30 H30 120.0 . . ? C30 C31 C24 120.0(3) . . ? C30 C31 C32 116.8(3) . . ? C24 C31 C32 123.2(3) . . ? C31 C32 H321 109.5 . . ? C31 C32 H322 109.5 . . ? H321 C32 H322 109.5 . . ? C31 C32 H323 109.5 . . ? H321 C32 H323 109.5 . . ? H322 C32 H323 109.5 . . ? C34 C33 H331 109.5 . . ? C34 C33 H332 109.5 . . ? H331 C33 H332 109.5 . . ? C34 C33 H333 109.5 . . ? H331 C33 H333 109.5 . . ? H332 C33 H333 109.5 . . ? C35 C34 C6 119.5(3) . . ? C35 C34 C33 118.9(3) . . ? C6 C34 C33 121.5(4) . . ? C34 C35 C2 120.7(4) . . ? C34 C35 H35 119.6 . . ? C2 C35 H35 119.6 . . ? F3A P1A F5A 90.5(3) . . ? F3A P1A F2A 90.0(3) . . ? F5A P1A F2A 91.0(3) . . ? F3A P1A F4A 178.9(3) . . ? F5A P1A F4A 90.6(3) . . ? F2A P1A F4A 90.2(3) . . ? F3A P1A F1A 89.4(3) . . ? F5A P1A F1A 90.0(3) . . ? F2A P1A F1A 178.8(4) . . ? F4A P1A F1A 90.4(3) . . ? F3A P1A F6A 90.2(3) . . ? F5A P1A F6A 179.3(3) . . ? F2A P1A F6A 89.1(3) . . ? F4A P1A F6A 88.7(3) . . ? F1A P1A F6A 89.9(3) . . ? F2B P1B F3B 89.8(3) . . ? F2B P1B F4B 90.1(3) . . ? F3B P1B F4B 179.7(4) . . ? F2B P1B F6B 89.8(3) . . ? F3B P1B F6B 90.3(3) . . ? F4B P1B F6B 90.0(3) . . ? F2B P1B F5B 90.5(3) . . ? F3B P1B F5B 89.9(3) . . ? F4B P1B F5B 89.8(3) . . ? F6B P1B F5B 179.7(4) . . ? F2B P1B F1B 179.8(4) . . ? F3B P1B F1B 90.1(3) . . ? F4B P1B F1B 89.9(3) . . ? F6B P1B F1B 90.0(3) . . ? F5B P1B F1B 89.7(3) . . ? F5C P1C F2C 90.0(3) . . ? F5C P1C F4C 90.1(3) . . ? F2C P1C F4C 90.1(3) . . ? F5C P1C F1C 89.8(3) . . ? F2C P1C F1C 179.8(5) . . ? F4C P1C F1C 90.0(3) . . ? F5C P1C F6C 179.8(5) . . ? F2C P1C F6C 89.9(3) . . ? F4C P1C F6C 90.0(3) . . ? F1C P1C F6C 90.3(3) . . ? F5C P1C F3C 90.1(3) . . ? F2C P1C F3C 89.8(3) . . ? F4C P1C F3C 179.7(4) . . ? F1C P1C F3C 90.2(3) . . ? F6C P1C F3C 89.8(3) . . ? C38 C37 H371 109.5 . . ? C38 C37 H372 109.5 . . ? H371 C37 H372 109.5 . . ? C38 C37 H373 109.5 . . ? H371 C37 H373 109.5 . . ? H372 C37 H373 109.5 . . ? N39 C38 C37 176(3) . . ? N40 C41 C42 179.5(18) . . ? C41 C42 H421 109.5 . . ? C41 C42 H422 109.5 . . ? H421 C42 H422 109.5 . . ? C41 C42 H423 109.5 . . ? H421 C42 H423 109.5 . . ? H422 C42 H423 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 N2 Co N1 C7 3.6(3) 4_755 . . . ? N2 Co N1 C7 -175.9(3) . . . . ? N1 Co N1 C7 -74.7(3) 4_755 . . . ? N3 Co N1 C7 -176.2(3) . . . . ? N3 Co N1 C7 85.4(3) 4_755 . . . ? N2 Co N1 C11 171.6(2) 4_755 . . . ? N2 Co N1 C11 -7.9(2) . . . . ? N1 Co N1 C11 93.3(2) 4_755 . . . ? N3 Co N1 C11 -8.2(4) . . . . ? N3 Co N1 C11 -106.5(2) 4_755 . . . ? N2 Co N2 C23 143.1(2) 4_755 . . . ? N1 Co N2 C23 101.2(3) 4_755 . . . ? N1 Co N2 C23 -175.2(3) . . . . ? N3 Co N2 C23 4.7(2) . . . . ? N3 Co N2 C23 -78.9(3) 4_755 . . . ? N2 Co N2 C12 -36.9(3) 4_755 . . . ? N1 Co N2 C12 -78.8(3) 4_755 . . . ? N1 Co N2 C12 4.8(2) . . . . ? N3 Co N2 C12 -175.3(3) . . . . ? N3 Co N2 C12 101.1(3) 4_755 . . . ? N2 Co N3 C21 3.8(3) 4_755 . . . ? N2 Co N3 C21 -176.7(3) . . . . ? N1 Co N3 C21 84.2(3) 4_755 . . . ? N1 Co N3 C21 -176.5(3) . . . . ? N3 Co N3 C21 -75.9(3) 4_755 . . . ? N2 Co N3 C22 173.4(2) 4_755 . . . ? N2 Co N3 C22 -7.2(2) . . . . ? N1 Co N3 C22 -106.2(2) 4_755 . . . ? N1 Co N3 C22 -6.9(5) . . . . ? N3 Co N3 C22 93.7(2) 4_755 . . . ? C1 O1 C2 C3 10.6(6) . . . . ? C1 O1 C2 C35 -170.7(4) . . . . ? O1 C2 C3 C4 177.5(3) . . . . ? C35 C2 C3 C4 -1.1(6) . . . . ? C2 C3 C4 C6 -0.2(5) . . . . ? C2 C3 C4 C5 176.9(3) . . . . ? C3 C4 C6 C34 1.5(5) . . . . ? C5 C4 C6 C34 -175.5(3) . . . . ? C3 C4 C6 C8 -178.8(3) . . . . ? C5 C4 C6 C8 4.2(5) . . . . ? C11 N1 C7 C8 -2.2(4) . . . . ? Co N1 C7 C8 165.3(2) . . . . ? N1 C7 C8 C9 2.8(5) . . . . ? N1 C7 C8 C6 -176.2(3) . . . . ? C4 C6 C8 C9 58.6(5) . . . . ? C34 C6 C8 C9 -121.7(4) . . . . ? C4 C6 C8 C7 -122.5(3) . . . . ? C34 C6 C8 C7 57.3(4) . . . . ? C7 C8 C9 C10 -1.2(5) . . . . ? C6 C8 C9 C10 177.8(3) . . . . ? C8 C9 C10 C11 -0.9(5) . . . . ? C8 C9 C10 C16B -173.0(11) . . . . ? C7 N1 C11 C10 -0.1(4) . . . . ? Co N1 C11 C10 -169.5(3) . . . . ? C7 N1 C11 C12 178.8(3) . . . . ? Co N1 C11 C12 9.4(3) . . . . ? C9 C10 C11 N1 1.6(5) . . . . ? C16B C10 C11 N1 176.0(8) . . . . ? C9 C10 C11 C12 -177.1(3) . . . . ? C16B C10 C11 C12 -2.7(9) . . . . ? C23 N2 C12 C13 -1.8(5) . . . . ? Co N2 C12 C13 178.2(3) . . . . ? C23 N2 C12 C11 178.9(3) . . . . ? Co N2 C12 C11 -1.0(4) . . . . ? N1 C11 C12 N2 -5.9(4) . . . . ? C10 C11 C12 N2 172.9(3) . . . . ? N1 C11 C12 C13 174.9(3) . . . . ? C10 C11 C12 C13 -6.3(6) . . . . ? N2 C12 C13 C14 3.4(6) . . . . ? C11 C12 C13 C14 -177.5(4) . . . . ? N2 C12 C13 C17B -165.1(9) . . . . ? C11 C12 C13 C17B 14.1(10) . . . . ? C17B C13 C14 C15 162.9(12) . . . . ? C12 C13 C14 C15 -1.5(7) . . . . ? C13 C14 C15 C23 -1.9(7) . . . . ? C13 C14 C15 C16A 174.9(5) . . . . ? C14 C15 C16A C17A 178.9(5) . . . . ? C23 C15 C16A C17A -4.3(8) . . . . ? C15 C16A C17A C18 1.2(9) . . . . ? C9 C10 C16B C17B 174.9(14) . . . . ? C11 C10 C16B C17B 2(2) . . . . ? C10 C16B C17B C13 8(3) . . . . ? C14 C13 C17B C16B 179.1(14) . . . . ? C12 C13 C17B C16B -15(2) . . . . ? C16A C17A C18 C19 -179.8(5) . . . . ? C16A C17A C18 C22 0.2(7) . . . . ? C22 C18 C19 C20 -1.7(6) . . . . ? C17A C18 C19 C20 178.3(4) . . . . ? C18 C19 C20 C21 0.6(5) . . . . ? C18 C19 C20 C24 -179.8(3) . . . . ? C22 N3 C21 C20 -1.0(5) . . . . ? Co N3 C21 C20 168.0(3) . . . . ? C19 C20 C21 N3 0.8(5) . . . . ? C24 C20 C21 N3 -178.8(3) . . . . ? C21 N3 C22 C18 -0.2(5) . . . . ? Co N3 C22 C18 -171.6(3) . . . . ? C21 N3 C22 C23 179.7(3) . . . . ? Co N3 C22 C23 8.4(4) . . . . ? C19 C18 C22 N3 1.6(6) . . . . ? C17A C18 C22 N3 -178.5(4) . . . . ? C19 C18 C22 C23 -178.4(3) . . . . ? C17A C18 C22 C23 1.6(6) . . . . ? C12 N2 C23 C15 -1.7(5) . . . . ? Co N2 C23 C15 178.2(3) . . . . ? C12 N2 C23 C22 178.6(3) . . . . ? Co N2 C23 C22 -1.5(4) . . . . ? C14 C15 C23 N2 3.6(6) . . . . ? C16A C15 C23 N2 -173.6(4) . . . . ? C14 C15 C23 C22 -176.8(4) . . . . ? C16A C15 C23 C22 6.1(6) . . . . ? N3 C22 C23 N2 -5.2(5) . . . . ? C18 C22 C23 N2 174.7(3) . . . . ? N3 C22 C23 C15 175.1(4) . . . . ? C18 C22 C23 C15 -5.0(6) . . . . ? C19 C20 C24 C25 58.5(5) . . . . ? C21 C20 C24 C25 -121.9(4) . . . . ? C19 C20 C24 C31 -124.1(4) . . . . ? C21 C20 C24 C31 55.5(5) . . . . ? C31 C24 C25 C27 2.5(5) . . . . ? C20 C24 C25 C27 179.8(3) . . . . ? C31 C24 C25 C26 -175.5(3) . . . . ? C20 C24 C25 C26 1.9(5) . . . . ? C24 C25 C27 C28 -0.8(5) . . . . ? C26 C25 C27 C28 177.2(3) . . . . ? C29 O2 C28 C27 174.5(4) . . . . ? C29 O2 C28 C30 -6.4(5) . . . . ? C25 C27 C28 O2 178.2(3) . . . . ? C25 C27 C28 C30 -0.9(5) . . . . ? O2 C28 C30 C31 -178.0(3) . . . . ? C27 C28 C30 C31 1.0(5) . . . . ? C28 C30 C31 C24 0.6(5) . . . . ? C28 C30 C31 C32 179.2(3) . . . . ? C25 C24 C31 C30 -2.4(5) . . . . ? C20 C24 C31 C30 -179.8(3) . . . . ? C25 C24 C31 C32 179.2(3) . . . . ? C20 C24 C31 C32 1.8(5) . . . . ? C4 C6 C34 C35 -1.5(5) . . . . ? C8 C6 C34 C35 178.8(3) . . . . ? C4 C6 C34 C33 -179.4(3) . . . . ? C8 C6 C34 C33 0.9(5) . . . . ? C6 C34 C35 C2 0.1(6) . . . . ? C33 C34 C35 C2 178.1(4) . . . . ? O1 C2 C35 C34 -177.6(3) . . . . ? C3 C2 C35 C34 1.2(6) . . . . ? #===END data_5a _database_code_depnum_ccdc_archive 'CCDC 735251' # SG0316 _audit_creation_method SHELXL-97 _audit_creation_date 03-08-28 _chemical_name_systematic ; bis{8-(4-methoxy-2,6-dimethylphenyl)-2-[5-(4-methoxy-2,6- dimethylphenyl)-pyridin-2-yl]-1,10-phenanthroline}nickel(II) hexafluorophosphate di-acetonitrile solvate ; _chemical_name_common ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_moiety 'C70 H62 N6 Ni O4 2+, 2(F6 P 1-), 2(C2 H3 N)' _chemical_formula_sum 'C74 H68 F12 N8 Ni O4 P2' _chemical_formula_weight 1482.03 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 296 0.0033 0.0016 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; H H 272 0.0000 0.0000 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; F F 48 0.0171 0.0103 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; N N 32 0.0061 0.0033 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; Ni Ni 4 0.3393 1.1124 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; O O 16 0.0106 0.0060 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; P P 8 0.1023 0.0942 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c c a ' _symmetry_space_group_name_Hall ? _symmetry_Int_Tables_number 54 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' 'x+1/2, -y, -z+1/2' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' '-x-1/2, y, z-1/2' 'x, -y, z-1/2' _cell_length_a 25.3094(4) _cell_length_b 12.6402(2) _cell_length_c 21.9538(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7023.37(18) _cell_formula_units_Z 4 _cell_measurement_temperature 160(1) _cell_measurement_reflns_used 99688 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.401 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3064 _exptl_absorpt_coefficient_mu 0.409 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Blessing, 1995)' _exptl_absorpt_correction_T_min 0.885 _exptl_absorpt_correction_T_max 0.961 _exptl_special_details ; Solvent used: acetonitrile / diethylether Cooling Device: Oxford Cryosystems Cryostream 700 Crystal mount: glued on a glass fibre Mosaicity (deg.): 0.650(1) Frames collected: 428 Seconds exposure per frame: 140 Degrees rotation per frame: 1.0 Crystal-Detector distance (mm): 38.1 ; _diffrn_ambient_temperature 160(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Nonius FR590 sealed tube generator' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_detector '65 mm CCD camera on \k goniostat' _diffrn_measurement_device_type 'Nonius KappaCCD area-detector diffractometer' _diffrn_measurement_method '\f and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 77907 _diffrn_reflns_av_R_equivalents 0.0619 _diffrn_reflns_av_sigmaI/netI 0.0370 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _reflns_number_total 8070 _reflns_number_gt 5148 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'COLLECT (Nonius, 2000)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN and SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'SHELXL97 and PLATON (Spek, 2009)' _refine_special_details ; The asymmetric unit contains one half of a cation with the Ni-atom on a two-fold axis, one anion and two closely adjacent sites in general positions which represent two equally occupied disordered positions for an acetonitrile molecule. In the cation, the two central CH groups of the phenanthroline moiety are disordered over two sites which effectively complete six-membered rings between all pyridine rings, thereby indicating that the ligand must be disordered through a 180\% rotation about the central N-atom. The site occupation factor for the major conformation refined to 0.754(9). The PF6- anion is highly disordered. Three sets of P- and F-atoms were defined for this anion and refinement of the site occupation factors of each set led to values of 0.600(4), 0.206(7) and 0.194(6). The P-F and F...F distances were restrained tightly, so as to maintain octahedral geometry and uniform P-F bond lengths and the atomic displacement parameters of the P- and F-atoms were given pseudo-isotropic restraints. The bond lengths within the disordered MeCN molecule were also restrained to logical values. Validation reports some short contacts as A alerts. These are mostly between different disordered components of anions and cations where the sums of the SOF of the relevant atoms is < 1.0, so that one can conceive that the "conflicting" sites are never occupied simultanously for adjacent moieties. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1093P)^2^+6.1409P] 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_extinction_coef ? _refine_ls_number_reflns 8068 _refine_ls_number_parameters 639 _refine_ls_number_restraints 944 _refine_ls_R_factor_all 0.1186 _refine_ls_R_factor_gt 0.0737 _refine_ls_wR_factor_ref 0.2276 _refine_ls_wR_factor_gt 0.1962 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.095 _refine_diff_density_min -0.328 _refine_diff_density_rms 0.068 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 Ni Ni 1.0000 0.28986(5) 0.2500 0.0484(2) Uani 1 2 d S . . O1 O 1.23590(14) 0.8392(3) 0.33432(17) 0.0960(10) Uani 1 1 d . . . O2 O 1.01041(13) -0.2464(3) -0.05016(13) 0.0783(8) Uani 1 1 d . A . N1 N 1.01432(11) 0.4130(2) 0.31390(12) 0.0501(7) Uani 1 1 d . . . N2 N 0.93415(11) 0.2916(2) 0.29766(13) 0.0551(7) Uani 1 1 d . A . N3 N 0.95640(11) 0.1668(2) 0.20634(14) 0.0544(7) Uani 1 1 d . . . C1 C 1.2702(2) 0.8554(6) 0.3862(3) 0.120(2) Uani 1 1 d . . . H11 H 1.2495 0.8833 0.4204 0.179 Uiso 1 1 calc R . . H12 H 1.2980 0.9061 0.3755 0.179 Uiso 1 1 calc R . . H13 H 1.2863 0.7879 0.3980 0.179 Uiso 1 1 calc R . . C2 C 1.19469(18) 0.7709(3) 0.3418(2) 0.0709(11) Uani 1 1 d . . . C3 C 1.17908(17) 0.7294(3) 0.3968(2) 0.0658(11) Uani 1 1 d . . . H3 H 1.1985 0.7459 0.4326 0.079 Uiso 1 1 calc R . . C4 C 1.13489(17) 0.6628(3) 0.40062(16) 0.0609(10) Uani 1 1 d . . . C5 C 1.12119(18) 0.6152(4) 0.46117(17) 0.0732(11) Uani 1 1 d . . . H51 H 1.0879 0.6456 0.4759 0.110 Uiso 1 1 calc R . . H52 H 1.1494 0.6304 0.4904 0.110 Uiso 1 1 calc R . . H53 H 1.1172 0.5384 0.4568 0.110 Uiso 1 1 calc R . . C6 C 1.10627(16) 0.6391(3) 0.34780(16) 0.0572(9) Uani 1 1 d . . . C7 C 1.05668(14) 0.4758(3) 0.31613(14) 0.0495(8) Uani 1 1 d . . . H7 H 1.0869 0.4562 0.2931 0.059 Uiso 1 1 calc R . . C8 C 1.05902(15) 0.5694(3) 0.35075(15) 0.0547(9) Uani 1 1 d . . . C9 C 1.01473(18) 0.5919(3) 0.38561(17) 0.0658(10) Uani 1 1 d . A . H9 H 1.0144 0.6536 0.4103 0.079 Uiso 1 1 calc R . . C10 C 0.97145(18) 0.5270(3) 0.38511(16) 0.0684(11) Uani 1 1 d . . . H10 H 0.9416 0.5429 0.4097 0.082 Uiso 0.754(9) 1 calc PR A 1 C11 C 0.97154(14) 0.4375(3) 0.34833(15) 0.0557(9) Uani 1 1 d . A . C12 C 0.92681(15) 0.3649(3) 0.34100(17) 0.0630(10) Uani 1 1 d . . . C13 C 0.87936(18) 0.3672(5) 0.3737(2) 0.0856(14) Uani 1 1 d . A . H131 H 0.8727 0.4214 0.4027 0.103 Uiso 0.754(9) 1 calc PR A 1 C14 C 0.8427(2) 0.2892(6) 0.3629(3) 0.112(2) Uani 1 1 d . . . H14 H 0.8110 0.2879 0.3861 0.134 Uiso 1 1 calc R A . C15 C 0.85089(18) 0.2121(5) 0.3187(3) 0.0989(17) Uani 1 1 d . A . H15 H 0.8257 0.1579 0.3111 0.119 Uiso 0.246(9) 1 calc PR A 2 C16A C 0.8183(2) 0.1170(7) 0.3041(3) 0.098(2) Uani 0.754(9) 1 d P A 1 H161 H 0.7873 0.1043 0.3272 0.117 Uiso 0.754(9) 1 calc PR A 1 C17A C 0.8309(2) 0.0495(6) 0.2600(3) 0.088(2) Uani 0.754(9) 1 d P A 1 H171 H 0.8080 -0.0087 0.2527 0.105 Uiso 0.754(9) 1 calc PR A 1 C16B C 0.9158(12) 0.5319(18) 0.4062(10) 0.106(9) Uani 0.246(9) 1 d P A 2 H162 H 0.9075 0.5930 0.4295 0.128 Uiso 0.246(9) 1 calc PR A 2 C17B C 0.8741(11) 0.463(3) 0.3979(11) 0.116(10) Uani 0.246(9) 1 d P A 2 H172 H 0.8399 0.4851 0.4102 0.139 Uiso 0.246(9) 1 calc PR A 2 C18 C 0.87830(16) 0.0599(4) 0.2222(2) 0.0774(12) Uani 1 1 d . . . H18 H 0.8463 0.0476 0.2437 0.093 Uiso 0.246(9) 1 calc PR A 2 C19 C 0.89461(17) -0.0068(4) 0.1753(2) 0.0746(11) Uani 1 1 d . A . H19 H 0.8738 -0.0669 0.1652 0.090 Uiso 1 1 calc R . . C20 C 0.94040(15) 0.0128(3) 0.14323(18) 0.0634(10) Uani 1 1 d . . . C21 C 0.96968(14) 0.1026(3) 0.16107(17) 0.0557(8) Uani 1 1 d . A . H21 H 1.0011 0.1181 0.1391 0.067 Uiso 1 1 calc R . . C22 C 0.91111(14) 0.1458(3) 0.23663(18) 0.0627(10) Uani 1 1 d . A . C23 C 0.89843(15) 0.2185(3) 0.28571(19) 0.0648(10) Uani 1 1 d . . . C24 C 0.95755(16) -0.0560(3) 0.09203(16) 0.0583(9) Uani 1 1 d . A . C25 C 0.92840(16) -0.0734(3) 0.0408(2) 0.0671(10) Uani 1 1 d . . . C26 C 0.87480(18) -0.0229(4) 0.0324(2) 0.0858(13) Uani 1 1 d . A . H261 H 0.8486 -0.0611 0.0567 0.129 Uiso 1 1 calc R . . H262 H 0.8648 -0.0258 -0.0107 0.129 Uiso 1 1 calc R . . H263 H 0.8762 0.0511 0.0456 0.129 Uiso 1 1 calc R . . C27 C 0.94694(17) -0.1375(3) -0.00593(19) 0.0679(10) Uani 1 1 d . A . H27 H 0.9253 -0.1504 -0.0405 0.081 Uiso 1 1 calc R . . C28 C 0.99695(17) -0.1832(3) -0.00255(19) 0.0631(10) Uani 1 1 d . . . C29 C 1.0625(2) -0.2881(4) -0.0503(2) 0.0863(14) Uani 1 1 d . . . H291 H 1.0880 -0.2298 -0.0515 0.129 Uiso 1 1 calc R A . H292 H 1.0674 -0.3331 -0.0863 0.129 Uiso 1 1 calc R . . H293 H 1.0681 -0.3302 -0.0134 0.129 Uiso 1 1 calc R . . C30 C 1.02841(16) -0.1645(3) 0.04760(17) 0.0600(9) Uani 1 1 d . A . H30 H 1.0626 -0.1952 0.0498 0.072 Uiso 1 1 calc R . . C31 C 1.01036(16) -0.1009(3) 0.09497(18) 0.0615(10) Uani 1 1 d . . . C32 C 1.0474(2) -0.0850(4) 0.1487(2) 0.0847(14) Uani 1 1 d . A . H321 H 1.0732 -0.1429 0.1499 0.127 Uiso 1 1 calc R . . H322 H 1.0270 -0.0844 0.1866 0.127 Uiso 1 1 calc R . . H323 H 1.0660 -0.0175 0.1442 0.127 Uiso 1 1 calc R . . C33 C 1.0943(2) 0.6576(4) 0.23302(19) 0.0861(15) Uani 1 1 d . . . H331 H 1.1069 0.7051 0.2009 0.129 Uiso 1 1 calc R . . H332 H 1.0564 0.6686 0.2393 0.129 Uiso 1 1 calc R . . H333 H 1.1007 0.5840 0.2209 0.129 Uiso 1 1 calc R . . C34 C 1.12355(18) 0.6807(3) 0.29138(18) 0.0643(10) Uani 1 1 d . . . C35 C 1.16691(19) 0.7453(3) 0.28912(19) 0.0704(11) Uani 1 1 d . . . H35 H 1.1782 0.7731 0.2511 0.085 Uiso 1 1 calc R . . P1A P 0.80722(7) 0.3084(2) -0.05813(10) 0.0686(8) Uani 0.600(4) 1 d PD B 1 F1A F 0.75051(13) 0.2784(6) -0.0347(2) 0.114(2) Uani 0.600(4) 1 d PDU B 1 F2A F 0.86383(16) 0.3394(7) -0.0810(3) 0.129(3) Uani 0.600(4) 1 d PDU B 1 F3A F 0.7849(3) 0.4177(4) -0.0801(3) 0.196(4) Uani 0.600(4) 1 d PDU B 1 F4A F 0.8287(2) 0.1988(3) -0.0356(3) 0.113(2) Uani 0.600(4) 1 d PDU B 1 F5A F 0.7935(3) 0.2589(6) -0.1217(2) 0.136(4) Uani 0.600(4) 1 d PDU B 1 F6A F 0.8204(3) 0.3577(5) 0.0057(2) 0.125(3) Uani 0.600(4) 1 d PDU B 1 P1B P 0.8074(4) 0.2942(9) -0.0635(5) 0.194(12) Uani 0.206(7) 1 d PDU C 2 F1B F 0.7722(9) 0.1943(13) -0.0510(9) 0.190(13) Uani 0.206(7) 1 d PDU C 2 F2B F 0.8426(7) 0.3940(14) -0.0758(8) 0.158(11) Uani 0.206(7) 1 d PDU C 2 F3B F 0.7590(5) 0.3677(15) -0.0491(7) 0.116(7) Uani 0.206(7) 1 d PDU C 2 F4B F 0.8554(7) 0.2204(17) -0.0785(9) 0.149(11) Uani 0.206(7) 1 d PDU C 2 F5B F 0.7903(6) 0.2920(14) -0.1321(5) 0.094(6) Uani 0.206(7) 1 d PDU C 2 F6B F 0.8239(6) 0.2968(15) 0.0054(5) 0.109(7) Uani 0.206(7) 1 d PDU C 2 P1C P 0.8005(2) 0.2323(8) -0.0653(3) 0.069(3) Uani 0.194(6) 1 d PDU D 3 F1C F 0.7447(3) 0.1999(17) -0.0403(7) 0.115(7) Uani 0.194(6) 1 d PDU D 3 F2C F 0.8561(4) 0.2647(16) -0.0906(7) 0.106(7) Uani 0.194(6) 1 d PDU D 3 F3C F 0.7749(6) 0.262(2) -0.1281(6) 0.192(18) Uani 0.194(6) 1 d PDU D 3 F4C F 0.8259(6) 0.202(2) -0.0025(5) 0.137(10) Uani 0.194(6) 1 d PDU D 3 F5C F 0.8094(9) 0.1163(10) -0.0884(11) 0.40(4) Uani 0.194(6) 1 d PDU D 3 F6C F 0.7914(9) 0.3485(10) -0.0424(12) 0.30(3) Uani 0.194(6) 1 d PDU D 3 C37 C 0.7538(8) 0.5225(18) 0.2845(6) 0.126(7) Uani 0.50 1 d PD E 1 H371 H 0.7751 0.5802 0.3015 0.189 Uiso 0.50 1 calc PR E 1 H372 H 0.7760 0.4776 0.2587 0.189 Uiso 0.50 1 calc PR E 1 H373 H 0.7390 0.4800 0.3178 0.189 Uiso 0.50 1 calc PR E 1 C38 C 0.7111(5) 0.5663(11) 0.2484(6) 0.109(4) Uani 0.50 1 d PD . 1 N39 N 0.6804(4) 0.6066(10) 0.2184(8) 0.126(4) Uani 0.50 1 d PD F 1 N40 N 0.6753(5) 0.6142(12) 0.1620(8) 0.136(5) Uani 0.50 1 d PD G 2 C41 C 0.7048(6) 0.5731(11) 0.1309(7) 0.118(5) Uani 0.50 1 d PD G 2 C42 C 0.742(2) 0.517(5) 0.0923(7) 0.150(10) Uani 0.50 1 d PD G 2 H421 H 0.7424 0.4421 0.1032 0.225 Uiso 0.50 1 calc PR G 2 H422 H 0.7774 0.5471 0.0979 0.225 Uiso 0.50 1 calc PR G 2 H423 H 0.7314 0.5250 0.0496 0.225 Uiso 0.50 1 calc PR G 2 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 Ni 0.0412(3) 0.0485(4) 0.0555(4) 0.000 0.0093(3) 0.000 O1 0.100(3) 0.079(2) 0.109(2) 0.0055(19) -0.020(2) -0.0208(19) O2 0.090(2) 0.0770(18) 0.0684(17) -0.0105(15) -0.0211(15) -0.0085(16) N1 0.0524(16) 0.0486(15) 0.0493(15) 0.0047(12) 0.0022(12) 0.0110(12) N2 0.0436(15) 0.0636(18) 0.0581(17) 0.0113(15) 0.0111(13) 0.0044(14) N3 0.0458(15) 0.0505(15) 0.0668(18) 0.0060(14) 0.0071(13) -0.0065(13) C1 0.095(4) 0.142(5) 0.122(5) -0.003(4) -0.026(4) -0.035(4) C2 0.080(3) 0.045(2) 0.088(3) -0.002(2) -0.013(2) 0.0060(19) C3 0.075(3) 0.049(2) 0.073(3) -0.0134(18) -0.019(2) 0.0114(19) C4 0.080(3) 0.0467(19) 0.056(2) -0.0084(16) -0.0096(18) 0.0241(19) C5 0.088(3) 0.077(3) 0.054(2) -0.0072(19) -0.013(2) 0.015(2) C6 0.075(2) 0.0387(17) 0.058(2) -0.0030(15) -0.0110(18) 0.0107(16) C7 0.0546(19) 0.0465(18) 0.0473(17) 0.0016(14) -0.0015(15) 0.0070(15) C8 0.070(2) 0.0470(18) 0.0474(17) -0.0024(15) -0.0066(16) 0.0180(17) C9 0.081(3) 0.061(2) 0.055(2) -0.0108(17) -0.0063(19) 0.021(2) C10 0.075(3) 0.079(3) 0.0506(19) -0.0018(19) 0.0087(19) 0.035(2) C11 0.058(2) 0.065(2) 0.0448(17) 0.0077(16) 0.0013(15) 0.0186(18) C12 0.053(2) 0.078(3) 0.058(2) 0.0116(19) 0.0096(17) 0.0179(19) C13 0.058(3) 0.116(4) 0.082(3) -0.016(3) 0.017(2) 0.015(3) C14 0.060(3) 0.169(6) 0.107(4) -0.031(4) 0.037(3) -0.009(3) C15 0.056(3) 0.137(5) 0.104(4) -0.013(3) 0.032(3) -0.023(3) C16A 0.052(3) 0.136(6) 0.104(5) 0.003(5) 0.026(3) -0.028(4) C17A 0.062(4) 0.113(5) 0.088(4) 0.003(4) 0.013(3) -0.035(4) C16B 0.15(2) 0.077(14) 0.095(15) -0.014(12) 0.034(15) 0.046(15) C17B 0.105(18) 0.15(2) 0.094(16) 0.035(16) 0.049(14) 0.064(18) C18 0.054(2) 0.089(3) 0.090(3) 0.021(3) 0.004(2) -0.022(2) C19 0.070(3) 0.072(3) 0.081(3) 0.005(2) -0.006(2) -0.030(2) C20 0.060(2) 0.054(2) 0.076(2) 0.0095(19) -0.0090(19) -0.0161(17) C21 0.0514(19) 0.0469(18) 0.069(2) 0.0014(17) 0.0004(17) -0.0059(15) C22 0.0489(19) 0.066(2) 0.073(2) 0.0121(19) 0.0089(17) -0.0065(18) C23 0.0471(19) 0.077(3) 0.070(2) 0.012(2) 0.0111(17) 0.0003(19) C24 0.085(3) 0.0325(15) 0.0572(19) 0.0011(14) -0.0069(18) -0.0134(17) C25 0.061(2) 0.054(2) 0.087(3) 0.017(2) -0.009(2) -0.0161(18) C26 0.067(3) 0.090(3) 0.100(3) 0.006(3) -0.016(2) -0.013(2) C27 0.071(3) 0.065(2) 0.068(2) 0.006(2) -0.016(2) -0.020(2) C28 0.081(3) 0.0472(18) 0.061(2) 0.0034(16) -0.0134(19) -0.0160(19) C29 0.101(4) 0.083(3) 0.075(3) -0.017(2) -0.023(3) 0.007(3) C30 0.071(2) 0.0416(17) 0.067(2) 0.0019(16) -0.0158(19) -0.0092(17) C31 0.079(3) 0.0390(17) 0.066(2) 0.0034(16) -0.0190(19) -0.0088(17) C32 0.098(3) 0.072(3) 0.084(3) -0.016(2) -0.038(3) 0.013(2) C33 0.123(4) 0.077(3) 0.058(2) 0.015(2) -0.022(2) -0.025(3) C34 0.090(3) 0.0429(18) 0.060(2) 0.0006(16) -0.013(2) 0.0053(19) C35 0.097(3) 0.0468(19) 0.068(2) 0.0061(18) -0.011(2) -0.001(2) P1A 0.0444(10) 0.096(2) 0.0650(12) 0.0200(12) -0.0147(9) -0.0026(11) F1A 0.051(3) 0.206(8) 0.085(3) -0.004(5) -0.004(2) 0.006(4) F2A 0.083(4) 0.172(7) 0.133(5) 0.073(6) -0.017(3) -0.046(5) F3A 0.178(8) 0.195(8) 0.216(8) 0.102(7) -0.036(7) 0.045(6) F4A 0.090(4) 0.118(5) 0.131(6) 0.028(5) -0.036(4) 0.001(3) F5A 0.089(5) 0.265(11) 0.054(3) 0.008(5) -0.010(3) 0.017(6) F6A 0.123(5) 0.121(5) 0.131(5) -0.017(4) -0.037(4) 0.017(4) P1B 0.195(14) 0.201(15) 0.187(14) -0.015(9) -0.007(9) -0.001(9) F1B 0.19(2) 0.154(17) 0.23(2) 0.023(15) 0.007(17) -0.007(16) F2B 0.146(17) 0.131(15) 0.196(18) 0.018(13) 0.011(14) -0.054(13) F3B 0.080(10) 0.146(14) 0.122(12) -0.005(11) -0.036(9) 0.031(10) F4B 0.098(13) 0.183(19) 0.167(18) 0.000(14) -0.008(12) 0.071(12) F5B 0.040(7) 0.154(13) 0.089(10) 0.059(9) -0.036(7) -0.023(8) F6B 0.097(10) 0.153(17) 0.078(9) 0.019(10) -0.013(8) 0.025(12) P1C 0.035(3) 0.094(6) 0.077(4) 0.018(4) -0.017(2) 0.005(3) F1C 0.091(12) 0.156(16) 0.098(11) 0.021(11) -0.001(9) -0.011(11) F2C 0.089(12) 0.109(12) 0.120(12) 0.057(12) 0.012(9) -0.003(10) F3C 0.15(2) 0.26(3) 0.16(2) 0.032(17) 0.015(15) 0.016(17) F4C 0.123(14) 0.185(18) 0.102(14) 0.028(13) -0.026(11) 0.031(13) F5C 0.42(4) 0.40(4) 0.40(4) 0.01(2) 0.02(2) 0.00(2) F6C 0.31(3) 0.28(3) 0.30(3) 0.00(2) 0.03(2) 0.01(2) C37 0.131(11) 0.13(2) 0.115(8) 0.010(11) -0.004(12) -0.033(13) C38 0.081(8) 0.123(11) 0.125(11) -0.026(8) 0.020(7) -0.034(8) N39 0.073(7) 0.127(9) 0.179(14) -0.033(10) 0.006(8) -0.029(6) N40 0.106(9) 0.144(11) 0.159(12) 0.012(10) 0.020(9) -0.057(8) C41 0.090(9) 0.107(11) 0.157(14) 0.035(10) 0.002(8) -0.050(8) C42 0.14(3) 0.13(4) 0.179(12) 0.04(2) -0.02(2) -0.076(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 Ni N2 1.968(3) . ? Ni N1 2.127(3) . ? Ni N3 2.135(3) . ? O1 C2 1.363(5) . ? O1 C1 1.447(6) . ? O2 C28 1.360(5) . ? O2 C29 1.420(6) . ? N1 C7 1.334(4) . ? N1 C11 1.356(4) . ? N2 C23 1.320(5) . ? N2 C12 1.340(5) . ? N3 C21 1.326(5) . ? N3 C22 1.351(4) . ? C1 H11 0.9800 . ? C1 H12 0.9800 . ? C1 H13 0.9800 . ? C2 C3 1.375(6) . ? C2 C35 1.391(6) . ? C3 C4 1.402(6) . ? C3 H3 0.9500 . ? C4 C6 1.400(5) . ? C4 C5 1.500(6) . ? C5 H51 0.9800 . ? C5 H52 0.9800 . ? C5 H53 0.9800 . ? C6 C34 1.415(5) . ? C6 C8 1.487(5) . ? C7 C8 1.408(5) . ? C7 H7 0.9500 . ? C8 C9 1.387(5) . ? C9 C10 1.369(6) . ? C9 H9 0.9500 . ? C10 C11 1.389(5) . ? C10 C16B 1.48(3) . ? C10 H10 0.9500 . ? C11 C12 1.467(6) . ? C12 C13 1.400(6) . ? C13 C17B 1.33(3) . ? C13 C14 1.376(8) . ? C13 H131 0.9500 . ? C14 C15 1.391(8) . ? C14 H14 0.9500 . ? C15 C23 1.406(5) . ? C15 C16A 1.491(9) . ? C15 H15 0.9500 . ? C16A C17A 1.329(10) . ? C16A H161 0.9500 . ? C17A C18 1.464(7) . ? C17A H171 0.9500 . ? C16B C17B 1.38(4) . ? C16B H162 0.9500 . ? C17B H172 0.9500 . ? C18 C19 1.394(6) . ? C18 C22 1.404(6) . ? C18 H18 0.9500 . ? C19 C20 1.378(6) . ? C19 H19 0.9500 . ? C20 C21 1.411(5) . ? C20 C24 1.486(5) . ? C21 H21 0.9500 . ? C22 C23 1.452(6) . ? C24 C25 1.363(5) . ? C24 C31 1.454(6) . ? C25 C27 1.389(6) . ? C25 C26 1.511(6) . ? C26 H261 0.9800 . ? C26 H262 0.9800 . ? C26 H263 0.9800 . ? C27 C28 1.393(6) . ? C27 H27 0.9500 . ? C28 C30 1.379(5) . ? C29 H291 0.9800 . ? C29 H292 0.9800 . ? C29 H293 0.9800 . ? C30 C31 1.391(5) . ? C30 H30 0.9500 . ? C31 C32 1.520(5) . ? C32 H321 0.9800 . ? C32 H322 0.9800 . ? C32 H323 0.9800 . ? C33 C34 1.508(6) . ? C33 H331 0.9800 . ? C33 H332 0.9800 . ? C33 H333 0.9800 . ? C34 C35 1.369(6) . ? C35 H35 0.9500 . ? P1A F5A 1.568(3) . ? P1A F2A 1.568(2) . ? P1A F4A 1.569(3) . ? P1A F3A 1.569(3) . ? P1A F6A 1.569(3) . ? P1A F1A 1.571(3) . ? P1B F5B 1.569(3) . ? P1B F3B 1.569(3) . ? P1B F4B 1.569(3) . ? P1B F6B 1.569(3) . ? P1B F2B 1.569(3) . ? P1B F1B 1.569(3) . ? P1C F4C 1.568(3) . ? P1C F6C 1.569(3) . ? P1C F1C 1.569(3) . ? P1C F5C 1.569(3) . ? P1C F3C 1.569(3) . ? P1C F2C 1.569(3) . ? C37 C38 1.450(5) . ? C37 H371 0.9800 . ? C37 H372 0.9800 . ? C37 H373 0.9800 . ? C38 N39 1.138(5) . ? N40 C41 1.138(5) . ? C41 C42 1.450(5) . ? C42 H421 0.9800 . ? C42 H422 0.9800 . ? C42 H423 0.9800 . ? 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 N2 Ni N2 178.69(18) . 4_755 ? N2 Ni N1 77.60(12) . . ? N2 Ni N1 101.42(11) . 4_755 ? N1 Ni N1 85.88(14) . 4_755 ? N2 Ni N3 101.97(11) . 4_755 ? N1 Ni N3 98.59(11) . 4_755 ? N2 Ni N3 79.00(12) . . ? N1 Ni N3 156.60(11) . . ? N3 Ni N3 86.43(16) 4_755 . ? C2 O1 C1 117.0(4) . . ? C28 O2 C29 116.9(3) . . ? C7 N1 C11 119.0(3) . . ? C7 N1 Ni 126.6(2) . . ? C11 N1 Ni 113.5(2) . . ? C23 N2 C12 122.0(3) . . ? C23 N2 Ni 117.8(3) . . ? C12 N2 Ni 120.2(3) . . ? C21 N3 C22 117.6(3) . . ? C21 N3 Ni 130.6(2) . . ? C22 N3 Ni 111.1(3) . . ? O1 C1 H11 109.5 . . ? O1 C1 H12 109.5 . . ? H11 C1 H12 109.5 . . ? O1 C1 H13 109.5 . . ? H11 C1 H13 109.5 . . ? H12 C1 H13 109.5 . . ? O1 C2 C3 124.5(4) . . ? O1 C2 C35 115.8(4) . . ? C3 C2 C35 119.7(4) . . ? C2 C3 C4 120.7(4) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C6 C4 C3 119.5(4) . . ? C6 C4 C5 121.9(4) . . ? C3 C4 C5 118.6(4) . . ? C4 C5 H51 109.5 . . ? C4 C5 H52 109.5 . . ? H51 C5 H52 109.5 . . ? C4 C5 H53 109.5 . . ? H51 C5 H53 109.5 . . ? H52 C5 H53 109.5 . . ? C4 C6 C34 119.0(4) . . ? C4 C6 C8 120.5(3) . . ? C34 C6 C8 120.5(3) . . ? N1 C7 C8 123.6(3) . . ? N1 C7 H7 118.2 . . ? C8 C7 H7 118.2 . . ? C9 C8 C7 115.9(4) . . ? C9 C8 C6 123.6(3) . . ? C7 C8 C6 120.6(3) . . ? C10 C9 C8 121.3(4) . . ? C10 C9 H9 119.3 . . ? C8 C9 H9 119.3 . . ? C9 C10 C11 119.4(4) . . ? C9 C10 C16B 137.0(10) . . ? C11 C10 C16B 102.6(10) . . ? C9 C10 H10 120.3 . . ? C11 C10 H10 120.3 . . ? N1 C11 C10 120.7(4) . . ? N1 C11 C12 114.3(3) . . ? C10 C11 C12 124.9(3) . . ? N2 C12 C13 119.9(4) . . ? N2 C12 C11 113.8(3) . . ? C13 C12 C11 126.3(4) . . ? C17B C13 C14 131.0(13) . . ? C17B C13 C12 108.1(12) . . ? C14 C13 C12 118.4(5) . . ? C14 C13 H131 120.8 . . ? C12 C13 H131 120.8 . . ? C13 C14 C15 121.5(4) . . ? C13 C14 H14 119.3 . . ? C15 C14 H14 119.3 . . ? C14 C15 C23 116.5(5) . . ? C14 C15 C16A 129.1(5) . . ? C23 C15 C16A 114.1(5) . . ? C14 C15 H15 121.7 . . ? C23 C15 H15 121.7 . . ? C17A C16A C15 122.8(5) . . ? C17A C16A H161 118.6 . . ? C15 C16A H161 118.6 . . ? C16A C17A C18 123.5(6) . . ? C16A C17A H171 118.3 . . ? C18 C17A H171 118.3 . . ? C17B C16B C10 131.1(17) . . ? C17B C16B H162 114.4 . . ? C10 C16B H162 114.4 . . ? C13 C17B C16B 123.5(18) . . ? C13 C17B H172 118.3 . . ? C16B C17B H172 118.3 . . ? C19 C18 C22 117.3(4) . . ? C19 C18 C17A 127.4(5) . . ? C22 C18 C17A 115.2(5) . . ? C19 C18 H18 121.3 . . ? C22 C18 H18 121.3 . . ? C20 C19 C18 121.2(4) . . ? C20 C19 H19 119.4 . . ? C18 C19 H19 119.4 . . ? C19 C20 C21 116.4(4) . . ? C19 C20 C24 121.8(3) . . ? C21 C20 C24 121.8(3) . . ? N3 C21 C20 124.5(3) . . ? N3 C21 H21 117.7 . . ? C20 C21 H21 117.7 . . ? N3 C22 C18 122.9(4) . . ? N3 C22 C23 115.4(3) . . ? C18 C22 C23 121.7(4) . . ? N2 C23 C15 121.6(4) . . ? N2 C23 C22 116.1(3) . . ? C15 C23 C22 122.3(4) . . ? C25 C24 C31 118.1(4) . . ? C25 C24 C20 124.1(4) . . ? C31 C24 C20 117.6(3) . . ? C24 C25 C27 121.4(4) . . ? C24 C25 C26 121.3(4) . . ? C27 C25 C26 117.4(4) . . ? C25 C26 H261 109.5 . . ? C25 C26 H262 109.5 . . ? H261 C26 H262 109.5 . . ? C25 C26 H263 109.5 . . ? H261 C26 H263 109.5 . . ? H262 C26 H263 109.5 . . ? C25 C27 C28 120.6(4) . . ? C25 C27 H27 119.7 . . ? C28 C27 H27 119.7 . . ? O2 C28 C30 124.7(4) . . ? O2 C28 C27 115.5(4) . . ? C30 C28 C27 119.8(4) . . ? O2 C29 H291 109.5 . . ? O2 C29 H292 109.5 . . ? H291 C29 H292 109.5 . . ? O2 C29 H293 109.5 . . ? H291 C29 H293 109.5 . . ? H292 C29 H293 109.5 . . ? C28 C30 C31 120.4(4) . . ? C28 C30 H30 119.8 . . ? C31 C30 H30 119.8 . . ? C30 C31 C24 119.6(3) . . ? C30 C31 C32 117.0(4) . . ? C24 C31 C32 123.4(4) . . ? C31 C32 H321 109.5 . . ? C31 C32 H322 109.5 . . ? H321 C32 H322 109.5 . . ? C31 C32 H323 109.5 . . ? H321 C32 H323 109.5 . . ? H322 C32 H323 109.5 . . ? C34 C33 H331 109.5 . . ? C34 C33 H332 109.5 . . ? H331 C33 H332 109.5 . . ? C34 C33 H333 109.5 . . ? H331 C33 H333 109.5 . . ? H332 C33 H333 109.5 . . ? C35 C34 C6 120.1(4) . . ? C35 C34 C33 118.5(4) . . ? C6 C34 C33 121.3(4) . . ? C34 C35 C2 120.9(4) . . ? C34 C35 H35 119.5 . . ? C2 C35 H35 119.5 . . ? F5A P1A F2A 91.0(3) . . ? F5A P1A F4A 90.3(3) . . ? F2A P1A F4A 90.3(3) . . ? F5A P1A F3A 89.9(3) . . ? F2A P1A F3A 90.5(3) . . ? F4A P1A F3A 179.1(3) . . ? F5A P1A F6A 179.4(3) . . ? F2A P1A F6A 89.6(3) . . ? F4A P1A F6A 89.7(3) . . ? F3A P1A F6A 90.1(3) . . ? F5A P1A F1A 89.6(3) . . ? F2A P1A F1A 179.4(3) . . ? F4A P1A F1A 90.1(3) . . ? F3A P1A F1A 89.1(3) . . ? F6A P1A F1A 89.8(3) . . ? F5B P1B F3B 89.4(3) . . ? F5B P1B F4B 90.0(3) . . ? F3B P1B F4B 179.4(4) . . ? F5B P1B F6B 179.4(4) . . ? F3B P1B F6B 90.1(3) . . ? F4B P1B F6B 90.5(3) . . ? F5B P1B F2B 90.2(3) . . ? F3B P1B F2B 90.1(3) . . ? F4B P1B F2B 90.1(3) . . ? F6B P1B F2B 89.9(3) . . ? F5B P1B F1B 89.9(3) . . ? F3B P1B F1B 89.9(3) . . ? F4B P1B F1B 89.9(3) . . ? F6B P1B F1B 90.0(3) . . ? F2B P1B F1B 179.9(5) . . ? F4C P1C F6C 90.3(3) . . ? F4C P1C F1C 90.0(3) . . ? F6C P1C F1C 90.1(3) . . ? F4C P1C F5C 89.9(3) . . ? F6C P1C F5C 179.8(4) . . ? F1C P1C F5C 90.0(3) . . ? F4C P1C F3C 179.7(4) . . ? F6C P1C F3C 90.0(3) . . ? F1C P1C F3C 89.9(3) . . ? F5C P1C F3C 89.9(3) . . ? F4C P1C F2C 90.3(3) . . ? F6C P1C F2C 90.0(3) . . ? F1C P1C F2C 179.7(4) . . ? F5C P1C F2C 89.9(3) . . ? F3C P1C F2C 89.8(3) . . ? N39 C38 C37 174.4(15) . . ? N40 C41 C42 178(3) . . ? C41 C42 H421 109.5 . . ? C41 C42 H422 109.5 . . ? H421 C42 H422 109.5 . . ? C41 C42 H423 109.5 . . ? H421 C42 H423 109.5 . . ? H422 C42 H423 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 N2 Ni N1 C7 -175.9(3) . . . . ? N2 Ni N1 C7 3.2(3) 4_755 . . . ? N1 Ni N1 C7 -73.2(3) 4_755 . . . ? N3 Ni N1 C7 83.7(3) 4_755 . . . ? N3 Ni N1 C7 -175.4(3) . . . . ? N2 Ni N1 C11 -6.8(2) . . . . ? N2 Ni N1 C11 172.3(2) 4_755 . . . ? N1 Ni N1 C11 95.8(2) 4_755 . . . ? N3 Ni N1 C11 -107.3(2) 4_755 . . . ? N3 Ni N1 C11 -6.3(4) . . . . ? N1 Ni N2 C23 -175.4(3) . . . . ? N1 Ni N2 C23 101.5(3) 4_755 . . . ? N3 Ni N2 C23 -79.1(3) 4_755 . . . ? N3 Ni N2 C23 4.8(3) . . . . ? N1 Ni N2 C12 4.1(3) . . . . ? N1 Ni N2 C12 -79.1(3) 4_755 . . . ? N3 Ni N2 C12 100.4(3) 4_755 . . . ? N3 Ni N2 C12 -175.7(3) . . . . ? N2 Ni N3 C21 -177.6(3) . . . . ? N2 Ni N3 C21 3.3(3) 4_755 . . . ? N1 Ni N3 C21 -178.1(3) . . . . ? N1 Ni N3 C21 82.3(3) 4_755 . . . ? N3 Ni N3 C21 -74.7(3) 4_755 . . . ? N2 Ni N3 C22 -6.9(2) . . . . ? N2 Ni N3 C22 174.0(3) 4_755 . . . ? N1 Ni N3 C22 -7.4(4) . . . . ? N1 Ni N3 C22 -107.0(3) 4_755 . . . ? N3 Ni N3 C22 96.0(3) 4_755 . . . ? C1 O1 C2 C3 10.1(7) . . . . ? C1 O1 C2 C35 -171.3(5) . . . . ? O1 C2 C3 C4 177.5(4) . . . . ? C35 C2 C3 C4 -1.1(6) . . . . ? C2 C3 C4 C6 -0.3(5) . . . . ? C2 C3 C4 C5 176.9(4) . . . . ? C3 C4 C6 C34 1.7(5) . . . . ? C5 C4 C6 C34 -175.5(3) . . . . ? C3 C4 C6 C8 -179.5(3) . . . . ? C5 C4 C6 C8 3.3(5) . . . . ? C11 N1 C7 C8 -2.5(5) . . . . ? Ni N1 C7 C8 166.0(2) . . . . ? N1 C7 C8 C9 2.7(5) . . . . ? N1 C7 C8 C6 -175.9(3) . . . . ? C4 C6 C8 C9 59.6(5) . . . . ? C34 C6 C8 C9 -121.6(4) . . . . ? C4 C6 C8 C7 -121.8(4) . . . . ? C34 C6 C8 C7 56.9(5) . . . . ? C7 C8 C9 C10 -0.9(5) . . . . ? C6 C8 C9 C10 177.7(3) . . . . ? C8 C9 C10 C11 -0.9(6) . . . . ? C8 C9 C10 C16B -167.2(14) . . . . ? C7 N1 C11 C10 0.5(5) . . . . ? Ni N1 C11 C10 -169.5(3) . . . . ? C7 N1 C11 C12 178.4(3) . . . . ? Ni N1 C11 C12 8.4(3) . . . . ? C9 C10 C11 N1 1.2(5) . . . . ? C16B C10 C11 N1 171.7(9) . . . . ? C9 C10 C11 C12 -176.4(4) . . . . ? C16B C10 C11 C12 -6.0(10) . . . . ? C23 N2 C12 C13 -2.1(6) . . . . ? Ni N2 C12 C13 178.5(3) . . . . ? C23 N2 C12 C11 178.6(3) . . . . ? Ni N2 C12 C11 -0.8(4) . . . . ? N1 C11 C12 N2 -5.3(4) . . . . ? C10 C11 C12 N2 172.5(3) . . . . ? N1 C11 C12 C13 175.5(4) . . . . ? C10 C11 C12 C13 -6.7(6) . . . . ? N2 C12 C13 C17B -159.6(12) . . . . ? C11 C12 C13 C17B 19.6(13) . . . . ? N2 C12 C13 C14 4.1(7) . . . . ? C11 C12 C13 C14 -176.7(5) . . . . ? C17B C13 C14 C15 156.4(14) . . . . ? C12 C13 C14 C15 -2.9(9) . . . . ? C13 C14 C15 C23 -0.2(9) . . . . ? C13 C14 C15 C16A 174.3(7) . . . . ? C14 C15 C16A C17A 179.8(7) . . . . ? C23 C15 C16A C17A -5.6(10) . . . . ? C15 C16A C17A C18 1.2(12) . . . . ? C9 C10 C16B C17B 173.3(18) . . . . ? C11 C10 C16B C17B 5(3) . . . . ? C14 C13 C17B C16B 179.3(17) . . . . ? C12 C13 C17B C16B -20(3) . . . . ? C10 C16B C17B C13 9(4) . . . . ? C16A C17A C18 C19 -180.0(6) . . . . ? C16A C17A C18 C22 1.6(9) . . . . ? C22 C18 C19 C20 -1.8(7) . . . . ? C17A C18 C19 C20 179.9(5) . . . . ? C18 C19 C20 C21 0.7(6) . . . . ? C18 C19 C20 C24 -178.4(4) . . . . ? C22 N3 C21 C20 -1.4(5) . . . . ? Ni N3 C21 C20 168.8(3) . . . . ? C19 C20 C21 N3 1.0(6) . . . . ? C24 C20 C21 N3 -179.9(3) . . . . ? C21 N3 C22 C18 0.2(6) . . . . ? Ni N3 C22 C18 -171.8(3) . . . . ? C21 N3 C22 C23 -180.0(3) . . . . ? Ni N3 C22 C23 8.0(4) . . . . ? C19 C18 C22 N3 1.3(6) . . . . ? C17A C18 C22 N3 179.9(4) . . . . ? C19 C18 C22 C23 -178.5(4) . . . . ? C17A C18 C22 C23 0.1(7) . . . . ? C12 N2 C23 C15 -1.2(6) . . . . ? Ni N2 C23 C15 178.2(4) . . . . ? C12 N2 C23 C22 178.6(3) . . . . ? Ni N2 C23 C22 -2.0(5) . . . . ? C14 C15 C23 N2 2.3(8) . . . . ? C16A C15 C23 N2 -173.0(5) . . . . ? C14 C15 C23 C22 -177.4(5) . . . . ? C16A C15 C23 C22 7.3(8) . . . . ? N3 C22 C23 N2 -4.5(5) . . . . ? C18 C22 C23 N2 175.3(4) . . . . ? N3 C22 C23 C15 175.3(4) . . . . ? C18 C22 C23 C15 -4.9(7) . . . . ? C19 C20 C24 C25 59.5(5) . . . . ? C21 C20 C24 C25 -119.6(4) . . . . ? C19 C20 C24 C31 -125.4(4) . . . . ? C21 C20 C24 C31 55.6(5) . . . . ? C31 C24 C25 C27 4.0(5) . . . . ? C20 C24 C25 C27 179.1(3) . . . . ? C31 C24 C25 C26 -175.5(3) . . . . ? C20 C24 C25 C26 -0.4(6) . . . . ? C24 C25 C27 C28 -2.3(6) . . . . ? C26 C25 C27 C28 177.3(4) . . . . ? C29 O2 C28 C30 -6.0(6) . . . . ? C29 O2 C28 C27 175.6(4) . . . . ? C25 C27 C28 O2 178.5(3) . . . . ? C25 C27 C28 C30 -0.1(6) . . . . ? O2 C28 C30 C31 -178.0(4) . . . . ? C27 C28 C30 C31 0.4(5) . . . . ? C28 C30 C31 C24 1.4(5) . . . . ? C28 C30 C31 C32 179.6(4) . . . . ? C25 C24 C31 C30 -3.5(5) . . . . ? C20 C24 C31 C30 -179.0(3) . . . . ? C25 C24 C31 C32 178.3(4) . . . . ? C20 C24 C31 C32 2.8(5) . . . . ? C4 C6 C34 C35 -1.6(6) . . . . ? C8 C6 C34 C35 179.6(3) . . . . ? C4 C6 C34 C33 179.9(4) . . . . ? C8 C6 C34 C33 1.1(6) . . . . ? C6 C34 C35 C2 0.2(6) . . . . ? C33 C34 C35 C2 178.7(4) . . . . ? O1 C2 C35 C34 -177.5(4) . . . . ? C3 C2 C35 C34 1.2(6) . . . . ? #===END data_6a _database_code_depnum_ccdc_archive 'CCDC 735252' # SG0318 _audit_creation_method SHELXL-97 _audit_creation_date 03-09-16 _chemical_name_systematic ; bis{8-(4-methoxy-2,6-dimethylphenyl)-2-[5-(4-methoxy-2,6- dimethylphenyl)-pyridin-2-yl]-1,10-phenanthroline}copper(II) hexafluorophosphate di-acetonitrile solvate ; _chemical_name_common ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_moiety 'C70 H62 Cu N6 O4 2+, 2(F6 P 1-), 2(C2 H3 N)' _chemical_formula_sum 'C74 H68 Cu F12 N8 O4 P2' _chemical_formula_weight 1486.87 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 296 0.0033 0.0016 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; H H 272 0.0000 0.0000 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; Cu Cu 4 0.0171 0.0103 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; F F 48 0.3201 1.2651 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; N N 32 0.0061 0.0033 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; O O 16 0.0106 0.0060 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; P P 8 0.1023 0.0942 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c c a ' _symmetry_space_group_name_Hall ? _symmetry_Int_Tables_number 54 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' 'x+1/2, -y, -z+1/2' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' '-x-1/2, y, z-1/2' 'x, -y, z-1/2' _cell_length_a 24.9866(3) _cell_length_b 12.9263(2) _cell_length_c 21.9263(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7081.85(17) _cell_formula_units_Z 4 _cell_measurement_temperature 160(1) _cell_measurement_reflns_used 103896 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_description prism _exptl_crystal_colour lime-green _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.394 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3068 _exptl_absorpt_coefficient_mu 0.440 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Blessing, 1995)' _exptl_absorpt_correction_T_min 0.811 _exptl_absorpt_correction_T_max 0.940 _exptl_special_details ; Solvent used: acetonitrile / diethylether Cooling Device: Oxford Cryosystems Cryostream 700 Crystal mount: glued on a glass fibre Mosaicity (deg.): 0.556(1) Frames collected: 500 Seconds exposure per frame: 80 Degrees rotation per frame: 0.8 Crystal-Detector distance (mm): 37.4 ; _diffrn_ambient_temperature 160(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Nonius FR590 sealed tube generator' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_detector '65 mm CCD camera on \k goniostat' _diffrn_measurement_device_type 'Nonius KappaCCD area-detector diffractometer' _diffrn_measurement_method '\f and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 71951 _diffrn_reflns_av_R_equivalents 0.0709 _diffrn_reflns_av_sigmaI/netI 0.0395 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 25.03 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.999 _reflns_number_total 6270 _reflns_number_gt 4433 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'COLLECT (Nonius, 2000)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN and SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'SHELXL97 and PLATON (Spek, 2009)' _refine_special_details ; The asymmetric unit contains one half of a cation with the Cu-atom on a two-fold axis, one anion and two closely adjacent sites in general positions which represent two equally occupied disordered positions for an acetonitrile molecule. In the cation, the two central CH groups of the phenanthroline moiety are disordered over two sites which effectively complete six-membered rings between all pyridine rings, thereby indicating that the ligand must be disordered through a 180\% rotation about the central N-atom. The site occupation factor for the major conformation refined to 0.757(9). The PF6- anion is highly disordered. Three sets of P- and F-atoms were defined for this anion and refinement of the site occupation factors of each set led to values of 0.493(4), 0.288(8) and 0.219(7). The P-F and F...F distances were restrained tightly, so as to maintain octahedral geometry and uniform P-F bond lengths and the atomic displacement parameters of the P- and F-atoms were given light pseudo-isotropic restraints. Despite thesre restraints, validation reports that one position for the P atom has a large ellipsoid. The bond lengths within the disordered MeCN molecule were also restrained to logical values. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0950P)^2^+5.7769P] 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 SHELXL _refine_ls_extinction_coef 0.0053(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6269 _refine_ls_number_parameters 640 _refine_ls_number_restraints 944 _refine_ls_R_factor_all 0.0975 _refine_ls_R_factor_gt 0.0662 _refine_ls_wR_factor_ref 0.1918 _refine_ls_wR_factor_gt 0.1698 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.919 _refine_diff_density_min -0.362 _refine_diff_density_rms 0.093 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 Cu Cu 1.0000 0.28734(5) 0.2500 0.0535(3) Uani 1 2 d S . . O1 O 1.23457(14) 0.8345(3) 0.33445(16) 0.0954(10) Uani 1 1 d . . . O2 O 1.00638(12) -0.2425(3) -0.05020(14) 0.0754(8) Uani 1 1 d . A . N1 N 1.01458(12) 0.4115(2) 0.31560(13) 0.0514(7) Uani 1 1 d . . . N2 N 0.93428(12) 0.2885(2) 0.29688(14) 0.0554(8) Uani 1 1 d . A . N3 N 0.95505(12) 0.1627(2) 0.20497(15) 0.0590(8) Uani 1 1 d . . . C1 C 1.2700(2) 0.8491(6) 0.3853(3) 0.129(2) Uani 1 1 d . . . H11 H 1.2496 0.8738 0.4206 0.193 Uiso 1 1 calc R . . H12 H 1.2974 0.9003 0.3746 0.193 Uiso 1 1 calc R . . H13 H 1.2873 0.7833 0.3955 0.193 Uiso 1 1 calc R . . C2 C 1.19268(18) 0.7674(3) 0.3421(2) 0.0721(12) Uani 1 1 d . . . C3 C 1.17711(17) 0.7268(3) 0.3978(2) 0.0685(11) Uani 1 1 d . . . H3 H 1.1967 0.7437 0.4336 0.082 Uiso 1 1 calc R . . C4 C 1.13302(17) 0.6613(3) 0.40179(17) 0.0613(10) Uani 1 1 d . . . C5 C 1.11932(19) 0.6143(4) 0.46262(18) 0.0780(12) Uani 1 1 d . . . H51 H 1.0872 0.6478 0.4791 0.117 Uiso 1 1 calc R . . H52 H 1.1493 0.6243 0.4909 0.117 Uiso 1 1 calc R . . H53 H 1.1126 0.5401 0.4575 0.117 Uiso 1 1 calc R . . C6 C 1.10374(16) 0.6372(3) 0.34905(17) 0.0592(10) Uani 1 1 d . . . C7 C 1.05630(15) 0.4754(3) 0.31851(15) 0.0521(8) Uani 1 1 d . . . H7 H 1.0877 0.4573 0.2965 0.063 Uiso 1 1 calc R . . C8 C 1.05671(15) 0.5675(3) 0.35205(15) 0.0548(9) Uani 1 1 d . . . C9 C 1.01099(17) 0.5876(3) 0.38563(17) 0.0639(11) Uani 1 1 d . A . H9 H 1.0093 0.6484 0.4099 0.077 Uiso 1 1 calc R . . C10 C 0.96779(17) 0.5213(3) 0.38468(17) 0.0652(11) Uani 1 1 d . . . H10 H 0.9370 0.5353 0.4087 0.078 Uiso 0.757(9) 1 calc PR A 1 C11 C 0.97009(15) 0.4342(3) 0.34818(15) 0.0558(9) Uani 1 1 d . A . C12 C 0.92584(15) 0.3606(3) 0.33957(17) 0.0618(10) Uani 1 1 d . . . C13 C 0.87782(18) 0.3615(5) 0.3725(2) 0.0867(14) Uani 1 1 d . A . H131 H 0.8710 0.4146 0.4014 0.104 Uiso 0.757(9) 1 calc PR A 1 C14 C 0.8409(2) 0.2851(5) 0.3627(3) 0.114(2) Uani 1 1 d . . . H14 H 0.8086 0.2844 0.3856 0.136 Uiso 1 1 calc R A . C15 C 0.85037(18) 0.2079(5) 0.3191(3) 0.0969(17) Uani 1 1 d . A . H15 H 0.8256 0.1532 0.3127 0.116 Uiso 0.243(9) 1 calc PR A 2 C16A C 0.8170(2) 0.1152(6) 0.3073(3) 0.097(2) Uani 0.757(9) 1 d P A 1 H161 H 0.7862 0.1034 0.3317 0.116 Uiso 0.757(9) 1 calc PR A 1 C17A C 0.8294(2) 0.0472(6) 0.2630(3) 0.087(2) Uani 0.757(9) 1 d P A 1 H171 H 0.8064 -0.0101 0.2562 0.105 Uiso 0.757(9) 1 calc PR A 1 C16B C 0.9141(11) 0.5281(18) 0.4067(8) 0.102(9) Uani 0.243(9) 1 d P A 2 H162 H 0.9065 0.5871 0.4310 0.122 Uiso 0.243(9) 1 calc PR A 2 C17B C 0.8723(10) 0.463(2) 0.3979(11) 0.106(9) Uani 0.243(9) 1 d P A 2 H172 H 0.8376 0.4854 0.4093 0.127 Uiso 0.243(9) 1 calc PR A 2 C18 C 0.87703(16) 0.0583(4) 0.2249(2) 0.0749(12) Uani 1 1 d . . . H18 H 0.8455 0.0456 0.2479 0.090 Uiso 0.243(9) 1 calc PR A 2 C19 C 0.89216(17) -0.0073(3) 0.1777(2) 0.0745(12) Uani 1 1 d . A . H19 H 0.8706 -0.0657 0.1682 0.089 Uiso 1 1 calc R . . C20 C 0.93774(15) 0.0107(3) 0.14446(18) 0.0615(10) Uani 1 1 d . . . C21 C 0.96751(14) 0.0988(3) 0.16049(19) 0.0601(10) Uani 1 1 d . A . H21 H 0.9989 0.1133 0.1376 0.072 Uiso 1 1 calc R . . C22 C 0.90974(14) 0.1434(3) 0.23724(19) 0.0628(10) Uani 1 1 d . A . C23 C 0.89766(15) 0.2149(3) 0.28560(19) 0.0652(10) Uani 1 1 d . . . C24 C 0.95642(15) -0.0560(3) 0.09297(19) 0.0618(10) Uani 1 1 d . A . C25 C 0.92460(16) -0.0726(3) 0.0410(2) 0.0684(11) Uani 1 1 d . . . C26 C 0.87096(18) -0.0201(4) 0.0333(3) 0.0930(15) Uani 1 1 d . A . H261 H 0.8579 -0.0310 -0.0083 0.140 Uiso 1 1 calc R . . H262 H 0.8748 0.0542 0.0409 0.140 Uiso 1 1 calc R . . H263 H 0.8453 -0.0494 0.0624 0.140 Uiso 1 1 calc R . . C27 C 0.94310(17) -0.1345(3) -0.0052(2) 0.0688(11) Uani 1 1 d . A . H27 H 0.9212 -0.1459 -0.0400 0.083 Uiso 1 1 calc R . . C28 C 0.99306(16) -0.1809(3) -0.0022(2) 0.0641(10) Uani 1 1 d . . . C29 C 1.05897(19) -0.2844(4) -0.0504(2) 0.0837(13) Uani 1 1 d . . . H291 H 1.0851 -0.2281 -0.0472 0.126 Uiso 1 1 calc R A . H292 H 1.0649 -0.3226 -0.0884 0.126 Uiso 1 1 calc R . . H293 H 1.0632 -0.3314 -0.0156 0.126 Uiso 1 1 calc R . . C30 C 1.02500(17) -0.1649(3) 0.04843(18) 0.0611(10) Uani 1 1 d . A . H30 H 1.0592 -0.1966 0.0507 0.073 Uiso 1 1 calc R . . C31 C 1.00736(16) -0.1028(3) 0.09598(18) 0.0606(10) Uani 1 1 d . . . C32 C 1.0439(2) -0.0888(4) 0.1502(2) 0.0879(14) Uani 1 1 d . A . H321 H 1.0693 -0.1463 0.1520 0.132 Uiso 1 1 calc R . . H322 H 1.0225 -0.0874 0.1876 0.132 Uiso 1 1 calc R . . H323 H 1.0634 -0.0234 0.1461 0.132 Uiso 1 1 calc R . . C33 C 1.0911(2) 0.6551(4) 0.2345(2) 0.0905(16) Uani 1 1 d . . . H331 H 1.1049 0.6994 0.2018 0.136 Uiso 1 1 calc R . . H332 H 1.0529 0.6687 0.2403 0.136 Uiso 1 1 calc R . . H333 H 1.0963 0.5823 0.2235 0.136 Uiso 1 1 calc R . . C34 C 1.12083(18) 0.6782(3) 0.29304(18) 0.0661(11) Uani 1 1 d . . . C35 C 1.16456(19) 0.7419(3) 0.2903(2) 0.0723(12) Uani 1 1 d . . . H35 H 1.1756 0.7689 0.2520 0.087 Uiso 1 1 calc R . . P1A P 0.80879(13) 0.3153(2) -0.05842(16) 0.0613(9) Uani 0.493(4) 1 d PD B 1 F1A F 0.75030(15) 0.2968(8) -0.0359(3) 0.145(6) Uani 0.493(4) 1 d PDU B 1 F2A F 0.8674(2) 0.3349(7) -0.0802(3) 0.150(5) Uani 0.493(4) 1 d PDU B 1 F3A F 0.7939(4) 0.4282(4) -0.0771(4) 0.204(5) Uani 0.493(4) 1 d PDU B 1 F4A F 0.8241(4) 0.2029(3) -0.0394(4) 0.136(4) Uani 0.493(4) 1 d PDU B 1 F5A F 0.7929(3) 0.2769(7) -0.1234(2) 0.092(3) Uani 0.493(4) 1 d PDU B 1 F6A F 0.8243(3) 0.3540(6) 0.0067(2) 0.104(2) Uani 0.493(4) 1 d PDU B 1 P1B P 0.8041(2) 0.2667(7) -0.0615(3) 0.099(3) Uani 0.288(8) 1 d PDU C 2 F1B F 0.7544(4) 0.2041(10) -0.0393(5) 0.124(5) Uani 0.288(8) 1 d PDU C 2 F2B F 0.8534(4) 0.3301(14) -0.0841(7) 0.263(18) Uani 0.288(8) 1 d PDU C 2 F3B F 0.7694(5) 0.3672(8) -0.0619(7) 0.137(6) Uani 0.288(8) 1 d PDU C 2 F4B F 0.8388(5) 0.1664(11) -0.0607(9) 0.224(11) Uani 0.288(8) 1 d PDU C 2 F5B F 0.7879(6) 0.2444(13) -0.1290(3) 0.134(9) Uani 0.288(8) 1 d PDU C 2 F6B F 0.8205(5) 0.2890(14) 0.0059(4) 0.180(10) Uani 0.288(8) 1 d PDU C 2 P1C P 0.8056(3) 0.2772(9) -0.0622(5) 0.36(3) Uani 0.219(7) 1 d PDU D 3 F1C F 0.7504(5) 0.2949(19) -0.0306(9) 0.26(3) Uani 0.219(7) 1 d PDU D 3 F2C F 0.8609(4) 0.2587(11) -0.0934(5) 0.075(4) Uani 0.219(7) 1 d PDU D 3 F3C F 0.7869(6) 0.3428(17) -0.1180(8) 0.165(12) Uani 0.219(7) 1 d PDU D 3 F4C F 0.8246(6) 0.2110(14) -0.0068(6) 0.104(7) Uani 0.219(7) 1 d PDU D 3 F5C F 0.7832(6) 0.1776(14) -0.0933(10) 0.228(14) Uani 0.219(7) 1 d PDU D 3 F6C F 0.8280(8) 0.3769(11) -0.0312(10) 0.209(13) Uani 0.219(7) 1 d PDU D 3 C37 C 0.750(2) 0.509(5) 0.2872(6) 0.184(9) Uani 0.50 1 d PD E 1 H371 H 0.7823 0.5504 0.2940 0.276 Uiso 0.50 1 calc PR E 1 H372 H 0.7596 0.4448 0.2660 0.276 Uiso 0.50 1 calc PR E 1 H373 H 0.7336 0.4919 0.3266 0.276 Uiso 0.50 1 calc PR E 1 C38 C 0.7124(6) 0.5670(11) 0.2505(7) 0.107(4) Uani 0.50 1 d PD E 1 N39 N 0.6815(5) 0.6073(11) 0.2205(8) 0.128(4) Uani 0.50 1 d PD E 1 N40 N 0.6761(6) 0.6117(12) 0.1630(8) 0.139(5) Uani 0.50 1 d PD F 2 C41 C 0.7061(6) 0.5710(11) 0.1321(8) 0.128(6) Uani 0.50 1 d PD F 2 C42 C 0.7433(14) 0.520(3) 0.0914(7) 0.148(10) Uani 0.50 1 d PD F 2 H421 H 0.7787 0.5167 0.1106 0.221 Uiso 0.50 1 calc PR F 2 H422 H 0.7457 0.5582 0.0530 0.221 Uiso 0.50 1 calc PR F 2 H423 H 0.7307 0.4492 0.0832 0.221 Uiso 0.50 1 calc PR F 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu 0.0524(4) 0.0426(4) 0.0654(4) 0.000 0.0065(3) 0.000 O1 0.100(2) 0.078(2) 0.108(3) 0.0024(19) -0.018(2) -0.0181(18) O2 0.080(2) 0.0752(19) 0.0711(18) -0.0121(16) -0.0154(14) -0.0031(15) N1 0.0657(18) 0.0409(16) 0.0475(16) 0.0040(13) 0.0062(14) 0.0077(14) N2 0.0522(16) 0.0512(17) 0.0628(19) 0.0061(15) 0.0067(14) 0.0055(14) N3 0.0519(17) 0.0457(17) 0.079(2) -0.0007(16) 0.0144(15) -0.0073(14) C1 0.092(4) 0.159(6) 0.135(5) -0.003(5) -0.031(4) -0.039(4) C2 0.081(3) 0.044(2) 0.091(3) 0.000(2) -0.014(2) 0.004(2) C3 0.078(3) 0.053(2) 0.074(3) -0.013(2) -0.019(2) 0.011(2) C4 0.084(3) 0.046(2) 0.054(2) -0.0074(17) -0.0102(19) 0.0188(19) C5 0.098(3) 0.081(3) 0.055(2) -0.008(2) -0.012(2) 0.012(2) C6 0.083(3) 0.0351(18) 0.060(2) -0.0073(16) -0.0100(19) 0.0115(17) C7 0.067(2) 0.0424(19) 0.0466(18) 0.0005(15) 0.0032(17) 0.0058(17) C8 0.078(2) 0.0425(19) 0.0444(19) -0.0013(15) -0.0033(18) 0.0146(18) C9 0.088(3) 0.052(2) 0.051(2) -0.0097(17) -0.006(2) 0.018(2) C10 0.076(3) 0.069(3) 0.050(2) -0.0040(19) 0.0087(19) 0.029(2) C11 0.063(2) 0.056(2) 0.0481(19) 0.0079(17) 0.0011(17) 0.0153(18) C12 0.064(2) 0.065(2) 0.057(2) 0.007(2) 0.0044(18) 0.0171(19) C13 0.067(3) 0.114(4) 0.079(3) -0.019(3) 0.013(2) 0.014(3) C14 0.060(3) 0.165(6) 0.116(4) -0.036(4) 0.031(3) -0.008(3) C15 0.062(3) 0.128(5) 0.100(4) -0.024(3) 0.030(3) -0.020(3) C16A 0.056(3) 0.135(6) 0.100(5) -0.006(5) 0.028(3) -0.023(4) C17A 0.065(4) 0.100(5) 0.096(5) -0.002(4) 0.014(3) -0.032(3) C16B 0.16(2) 0.094(16) 0.055(11) 0.013(11) 0.031(13) 0.069(16) C17B 0.089(15) 0.13(2) 0.100(17) 0.003(15) 0.045(13) 0.025(15) C18 0.055(2) 0.078(3) 0.091(3) 0.009(3) 0.010(2) -0.016(2) C19 0.071(3) 0.060(2) 0.093(3) 0.004(2) 0.000(2) -0.025(2) C20 0.063(2) 0.043(2) 0.078(2) 0.0057(19) 0.000(2) -0.0094(17) C21 0.055(2) 0.043(2) 0.083(3) 0.0029(19) 0.0096(19) -0.0060(17) C22 0.050(2) 0.055(2) 0.083(3) 0.008(2) 0.0089(19) -0.0051(17) C23 0.054(2) 0.068(3) 0.074(3) 0.006(2) 0.009(2) -0.0002(19) C24 0.067(2) 0.0395(19) 0.079(3) 0.0073(18) -0.002(2) -0.0119(18) C25 0.067(2) 0.054(2) 0.084(3) 0.008(2) -0.010(2) -0.0136(19) C26 0.070(3) 0.086(3) 0.123(4) 0.000(3) -0.013(3) 0.004(2) C27 0.071(3) 0.061(2) 0.075(3) 0.004(2) -0.014(2) -0.013(2) C28 0.078(3) 0.046(2) 0.069(3) 0.0015(19) -0.009(2) -0.0146(19) C29 0.091(3) 0.081(3) 0.080(3) -0.022(2) -0.018(3) 0.003(3) C30 0.075(2) 0.0353(19) 0.073(3) 0.0041(18) -0.012(2) -0.0031(17) C31 0.074(3) 0.0375(19) 0.070(2) 0.0031(18) -0.0117(19) -0.0073(17) C32 0.103(3) 0.073(3) 0.088(3) -0.014(2) -0.031(3) 0.018(3) C33 0.130(4) 0.078(3) 0.064(3) 0.013(2) -0.019(3) -0.032(3) C34 0.099(3) 0.0394(19) 0.060(2) 0.0034(17) -0.012(2) 0.001(2) C35 0.100(3) 0.046(2) 0.071(3) 0.005(2) -0.013(2) 0.000(2) P1A 0.0502(16) 0.0645(18) 0.0692(18) 0.0096(14) -0.0093(12) -0.0087(14) F1A 0.036(3) 0.320(17) 0.078(5) -0.021(7) -0.005(3) 0.034(6) F2A 0.095(5) 0.260(11) 0.096(6) 0.068(7) -0.031(4) -0.110(7) F3A 0.324(14) 0.099(6) 0.188(9) 0.044(6) -0.067(9) 0.029(8) F4A 0.181(10) 0.075(5) 0.151(9) -0.035(6) 0.041(8) -0.006(6) F5A 0.062(4) 0.146(8) 0.067(5) -0.008(5) -0.006(3) -0.008(5) F6A 0.112(5) 0.120(6) 0.080(5) -0.003(4) -0.024(4) -0.005(4) P1B 0.043(3) 0.189(9) 0.065(4) 0.034(4) -0.016(2) 0.038(4) F1B 0.114(9) 0.166(12) 0.093(8) 0.042(8) 0.006(7) 0.006(8) F2B 0.23(2) 0.34(3) 0.21(2) 0.016(19) 0.012(17) -0.028(19) F3B 0.146(12) 0.123(11) 0.143(13) -0.007(9) -0.048(10) -0.019(10) F4B 0.143(12) 0.278(19) 0.251(19) 0.009(15) -0.046(12) 0.116(13) F5B 0.139(14) 0.176(15) 0.088(11) -0.016(10) -0.004(9) 0.019(11) F6B 0.151(13) 0.228(19) 0.162(15) 0.089(14) -0.023(11) -0.022(15) P1C 0.37(3) 0.37(3) 0.35(3) -0.001(10) -0.007(10) 0.003(10) F1C 0.25(3) 0.30(3) 0.24(3) 0.002(19) 0.005(19) 0.007(19) F2C 0.028(5) 0.089(9) 0.107(9) -0.009(7) 0.004(5) 0.018(5) F3C 0.144(15) 0.21(2) 0.136(16) 0.052(14) -0.067(12) 0.036(14) F4C 0.070(8) 0.117(13) 0.125(13) -0.010(10) -0.031(8) 0.029(8) F5C 0.21(2) 0.22(2) 0.25(2) 0.007(17) -0.006(18) 0.004(16) F6C 0.201(19) 0.181(18) 0.24(2) -0.047(17) -0.021(17) 0.071(15) C37 0.166(13) 0.26(2) 0.129(11) -0.04(3) 0.06(2) 0.020(13) C38 0.082(8) 0.121(11) 0.119(11) -0.031(8) 0.024(7) -0.032(7) N39 0.080(7) 0.145(10) 0.159(13) -0.035(10) 0.000(8) -0.019(7) N40 0.122(11) 0.154(12) 0.140(12) 0.016(10) 0.013(9) -0.060(9) C41 0.106(11) 0.125(13) 0.153(15) 0.038(11) 0.001(9) -0.061(10) C42 0.131(17) 0.12(3) 0.190(12) 0.039(18) 0.006(18) -0.067(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu N2 1.937(3) . ? Cu N1 2.186(3) . ? Cu N3 2.198(3) . ? O1 C2 1.370(5) . ? O1 C1 1.437(6) . ? O2 C28 1.362(5) . ? O2 C29 1.421(5) . ? N1 C7 1.331(4) . ? N1 C11 1.354(4) . ? N2 C12 1.337(5) . ? N2 C23 1.343(5) . ? N3 C21 1.315(5) . ? N3 C22 1.358(5) . ? C1 H11 0.9800 . ? C1 H12 0.9800 . ? C1 H13 0.9800 . ? C2 C35 1.376(6) . ? C2 C3 1.386(6) . ? C3 C4 1.392(6) . ? C3 H3 0.9500 . ? C4 C6 1.403(5) . ? C4 C5 1.505(6) . ? C5 H51 0.9800 . ? C5 H52 0.9800 . ? C5 H53 0.9800 . ? C6 C34 1.404(5) . ? C6 C8 1.482(5) . ? C7 C8 1.400(5) . ? C7 H7 0.9500 . ? C8 C9 1.384(5) . ? C9 C10 1.378(6) . ? C9 H9 0.9500 . ? C10 C11 1.383(5) . ? C10 C16B 1.43(3) . ? C10 H10 0.9500 . ? C11 C12 1.471(6) . ? C12 C13 1.400(6) . ? C13 C14 1.368(7) . ? C13 C17B 1.43(3) . ? C13 H131 0.9500 . ? C14 C15 1.401(7) . ? C14 H14 0.9500 . ? C15 C23 1.394(6) . ? C15 C16A 1.482(9) . ? C15 H15 0.9500 . ? C16A C17A 1.346(9) . ? C16A H161 0.9500 . ? C17A C18 1.461(7) . ? C17A H171 0.9500 . ? C16B C17B 1.36(3) . ? C16B H162 0.9500 . ? C17B H172 0.9500 . ? C18 C19 1.391(6) . ? C18 C22 1.397(6) . ? C18 H18 0.9500 . ? C19 C20 1.372(6) . ? C19 H19 0.9500 . ? C20 C21 1.405(5) . ? C20 C24 1.496(6) . ? C21 H21 0.9500 . ? C22 C23 1.439(6) . ? C24 C25 1.406(6) . ? C24 C31 1.410(5) . ? C25 C27 1.372(6) . ? C25 C26 1.512(6) . ? C26 H261 0.9800 . ? C26 H262 0.9800 . ? C26 H263 0.9800 . ? C27 C28 1.387(6) . ? C27 H27 0.9500 . ? C28 C30 1.382(6) . ? C29 H291 0.9800 . ? C29 H292 0.9800 . ? C29 H293 0.9800 . ? C30 C31 1.388(5) . ? C30 H30 0.9500 . ? C31 C32 1.508(6) . ? C32 H321 0.9800 . ? C32 H322 0.9800 . ? C32 H323 0.9800 . ? C33 C34 1.511(6) . ? C33 H331 0.9800 . ? C33 H332 0.9800 . ? C33 H333 0.9800 . ? C34 C35 1.369(6) . ? C35 H35 0.9500 . ? P1A F4A 1.560(3) . ? P1A F3A 1.560(3) . ? P1A F2A 1.560(3) . ? P1A F5A 1.561(3) . ? P1A F1A 1.561(3) . ? P1A F6A 1.562(3) . ? P1B F1B 1.560(3) . ? P1B F4B 1.560(3) . ? P1B F2B 1.560(3) . ? P1B F6B 1.561(3) . ? P1B F5B 1.561(3) . ? P1B F3B 1.561(3) . ? P1C F2C 1.560(3) . ? P1C F1C 1.560(3) . ? P1C F4C 1.560(3) . ? P1C F5C 1.560(3) . ? P1C F3C 1.560(3) . ? P1C F6C 1.561(3) . ? C37 C38 1.449(5) . ? C37 H371 0.9800 . ? C37 H372 0.9800 . ? C37 H373 0.9800 . ? C38 N39 1.139(5) . ? N40 C41 1.138(5) . ? C41 C42 1.451(5) . ? C42 H421 0.9800 . ? C42 H422 0.9800 . ? C42 H423 0.9800 . ? 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 N2 Cu N2 179.08(18) 4_755 . ? N2 Cu N1 101.65(11) . 4_755 ? N2 Cu N1 77.66(12) . . ? N1 Cu N1 85.50(14) 4_755 . ? N2 Cu N3 79.11(12) . . ? N1 Cu N3 156.77(11) . . ? N2 Cu N3 101.57(11) . 4_755 ? N1 Cu N3 99.07(11) . 4_755 ? N3 Cu N3 85.72(17) . 4_755 ? C2 O1 C1 117.4(4) . . ? C28 O2 C29 116.8(3) . . ? C7 N1 C11 118.9(3) . . ? C7 N1 Cu 128.1(2) . . ? C11 N1 Cu 111.7(2) . . ? C12 N2 C23 121.0(3) . . ? C12 N2 Cu 120.7(3) . . ? C23 N2 Cu 118.3(3) . . ? C21 N3 C22 117.9(3) . . ? C21 N3 Cu 132.2(2) . . ? C22 N3 Cu 109.1(3) . . ? O1 C1 H11 109.5 . . ? O1 C1 H12 109.5 . . ? H11 C1 H12 109.5 . . ? O1 C1 H13 109.5 . . ? H11 C1 H13 109.5 . . ? H12 C1 H13 109.5 . . ? O1 C2 C35 116.1(4) . . ? O1 C2 C3 124.2(4) . . ? C35 C2 C3 119.6(4) . . ? C2 C3 C4 120.5(4) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C3 C4 C6 119.7(4) . . ? C3 C4 C5 118.7(4) . . ? C6 C4 C5 121.5(4) . . ? C4 C5 H51 109.5 . . ? C4 C5 H52 109.5 . . ? H51 C5 H52 109.5 . . ? C4 C5 H53 109.5 . . ? H51 C5 H53 109.5 . . ? H52 C5 H53 109.5 . . ? C4 C6 C34 118.6(4) . . ? C4 C6 C8 120.8(4) . . ? C34 C6 C8 120.6(3) . . ? N1 C7 C8 123.9(3) . . ? N1 C7 H7 118.0 . . ? C8 C7 H7 118.0 . . ? C9 C8 C7 115.6(4) . . ? C9 C8 C6 124.4(3) . . ? C7 C8 C6 120.0(3) . . ? C10 C9 C8 121.5(4) . . ? C10 C9 H9 119.3 . . ? C8 C9 H9 119.3 . . ? C9 C10 C11 118.8(3) . . ? C9 C10 C16B 133.9(11) . . ? C11 C10 C16B 106.5(12) . . ? C9 C10 H10 120.6 . . ? C11 C10 H10 120.6 . . ? N1 C11 C10 121.1(4) . . ? N1 C11 C12 114.2(3) . . ? C10 C11 C12 124.7(3) . . ? N2 C12 C13 120.1(4) . . ? N2 C12 C11 115.0(3) . . ? C13 C12 C11 124.9(4) . . ? C14 C13 C12 119.4(5) . . ? C14 C13 C17B 131.1(11) . . ? C12 C13 C17B 106.9(10) . . ? C14 C13 H131 120.3 . . ? C12 C13 H131 120.3 . . ? C13 C14 C15 120.5(4) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C23 C15 C14 117.1(5) . . ? C23 C15 C16A 115.9(5) . . ? C14 C15 C16A 126.9(5) . . ? C23 C15 H15 121.4 . . ? C14 C15 H15 121.4 . . ? C17A C16A C15 121.6(5) . . ? C17A C16A H161 119.2 . . ? C15 C16A H161 119.2 . . ? C16A C17A C18 122.4(6) . . ? C16A C17A H171 118.8 . . ? C18 C17A H171 118.8 . . ? C17B C16B C10 129.5(18) . . ? C17B C16B H162 115.2 . . ? C10 C16B H162 115.2 . . ? C16B C17B C13 123.5(17) . . ? C16B C17B H172 118.2 . . ? C13 C17B H172 118.2 . . ? C19 C18 C22 117.8(4) . . ? C19 C18 C17A 126.0(5) . . ? C22 C18 C17A 116.3(5) . . ? C19 C18 H18 121.1 . . ? C22 C18 H18 121.1 . . ? C20 C19 C18 121.1(4) . . ? C20 C19 H19 119.4 . . ? C18 C19 H19 119.4 . . ? C19 C20 C21 116.4(4) . . ? C19 C20 C24 124.1(3) . . ? C21 C20 C24 119.4(3) . . ? N3 C21 C20 124.7(3) . . ? N3 C21 H21 117.7 . . ? C20 C21 H21 117.7 . . ? N3 C22 C18 122.1(4) . . ? N3 C22 C23 116.1(3) . . ? C18 C22 C23 121.8(4) . . ? N2 C23 C15 121.8(4) . . ? N2 C23 C22 116.6(3) . . ? C15 C23 C22 121.6(4) . . ? C25 C24 C31 118.9(4) . . ? C25 C24 C20 121.5(4) . . ? C31 C24 C20 119.6(4) . . ? C27 C25 C24 119.8(4) . . ? C27 C25 C26 118.6(4) . . ? C24 C25 C26 121.5(4) . . ? C25 C26 H261 109.5 . . ? C25 C26 H262 109.5 . . ? H261 C26 H262 109.5 . . ? C25 C26 H263 109.5 . . ? H261 C26 H263 109.5 . . ? H262 C26 H263 109.5 . . ? C25 C27 C28 121.3(4) . . ? C25 C27 H27 119.3 . . ? C28 C27 H27 119.3 . . ? O2 C28 C30 124.6(4) . . ? O2 C28 C27 115.8(4) . . ? C30 C28 C27 119.6(4) . . ? O2 C29 H291 109.5 . . ? O2 C29 H292 109.5 . . ? H291 C29 H292 109.5 . . ? O2 C29 H293 109.5 . . ? H291 C29 H293 109.5 . . ? H292 C29 H293 109.5 . . ? C28 C30 C31 120.4(4) . . ? C28 C30 H30 119.8 . . ? C31 C30 H30 119.8 . . ? C30 C31 C24 120.0(4) . . ? C30 C31 C32 118.0(4) . . ? C24 C31 C32 122.1(4) . . ? C31 C32 H321 109.5 . . ? C31 C32 H322 109.5 . . ? H321 C32 H322 109.5 . . ? C31 C32 H323 109.5 . . ? H321 C32 H323 109.5 . . ? H322 C32 H323 109.5 . . ? C34 C33 H331 109.5 . . ? C34 C33 H332 109.5 . . ? H331 C33 H332 109.5 . . ? C34 C33 H333 109.5 . . ? H331 C33 H333 109.5 . . ? H332 C33 H333 109.5 . . ? C35 C34 C6 120.6(4) . . ? C35 C34 C33 118.2(4) . . ? C6 C34 C33 121.2(4) . . ? C34 C35 C2 121.0(4) . . ? C34 C35 H35 119.5 . . ? C2 C35 H35 119.5 . . ? F4A P1A F3A 179.5(4) . . ? F4A P1A F2A 90.2(3) . . ? F3A P1A F2A 89.5(3) . . ? F4A P1A F5A 90.5(3) . . ? F3A P1A F5A 89.9(3) . . ? F2A P1A F5A 90.6(3) . . ? F4A P1A F1A 90.1(3) . . ? F3A P1A F1A 90.2(3) . . ? F2A P1A F1A 179.3(4) . . ? F5A P1A F1A 90.0(3) . . ? F4A P1A F6A 89.6(3) . . ? F3A P1A F6A 90.0(3) . . ? F2A P1A F6A 89.7(3) . . ? F5A P1A F6A 179.6(3) . . ? F1A P1A F6A 89.6(3) . . ? F1B P1B F4B 90.4(3) . . ? F1B P1B F2B 179.4(4) . . ? F4B P1B F2B 90.1(3) . . ? F1B P1B F6B 90.5(3) . . ? F4B P1B F6B 89.8(3) . . ? F2B P1B F6B 89.8(3) . . ? F1B P1B F5B 89.6(3) . . ? F4B P1B F5B 90.1(3) . . ? F2B P1B F5B 90.1(3) . . ? F6B P1B F5B 179.8(4) . . ? F1B P1B F3B 89.5(3) . . ? F4B P1B F3B 179.6(4) . . ? F2B P1B F3B 90.0(3) . . ? F6B P1B F3B 89.8(3) . . ? F5B P1B F3B 90.3(3) . . ? F2C P1C F1C 179.5(4) . . ? F2C P1C F4C 89.3(3) . . ? F1C P1C F4C 90.2(3) . . ? F2C P1C F5C 90.0(3) . . ? F1C P1C F5C 89.9(3) . . ? F4C P1C F5C 89.9(3) . . ? F2C P1C F3C 90.3(3) . . ? F1C P1C F3C 90.2(3) . . ? F4C P1C F3C 179.5(4) . . ? F5C P1C F3C 89.9(3) . . ? F2C P1C F6C 90.0(3) . . ? F1C P1C F6C 90.1(3) . . ? F4C P1C F6C 90.3(3) . . ? F5C P1C F6C 179.8(5) . . ? F3C P1C F6C 90.0(3) . . ? N39 C38 C37 176(3) . . ? N40 C41 C42 179(2) . . ? C41 C42 H421 109.5 . . ? C41 C42 H422 109.5 . . ? H421 C42 H422 109.5 . . ? C41 C42 H423 109.5 . . ? H421 C42 H423 109.5 . . ? H422 C42 H423 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 N2 Cu N1 C7 4.6(3) 4_755 . . . ? N2 Cu N1 C7 -174.8(3) . . . . ? N1 Cu N1 C7 -71.8(3) 4_755 . . . ? N3 Cu N1 C7 -174.4(3) . . . . ? N3 Cu N1 C7 85.2(3) 4_755 . . . ? N2 Cu N1 C11 171.4(2) 4_755 . . . ? N2 Cu N1 C11 -8.0(2) . . . . ? N1 Cu N1 C11 95.0(2) 4_755 . . . ? N3 Cu N1 C11 -7.6(4) . . . . ? N3 Cu N1 C11 -108.0(2) 4_755 . . . ? N1 Cu N2 C12 -77.6(3) 4_755 . . . ? N1 Cu N2 C12 5.1(3) . . . . ? N3 Cu N2 C12 -174.8(3) . . . . ? N3 Cu N2 C12 101.9(3) 4_755 . . . ? N1 Cu N2 C23 102.7(3) 4_755 . . . ? N1 Cu N2 C23 -174.6(3) . . . . ? N3 Cu N2 C23 5.6(3) . . . . ? N3 Cu N2 C23 -77.7(3) 4_755 . . . ? N2 Cu N3 C21 3.5(4) 4_755 . . . ? N2 Cu N3 C21 -177.1(4) . . . . ? N1 Cu N3 C21 82.7(4) 4_755 . . . ? N1 Cu N3 C21 -177.5(3) . . . . ? N3 Cu N3 C21 -74.5(3) 4_755 . . . ? N2 Cu N3 C22 172.9(3) 4_755 . . . ? N2 Cu N3 C22 -7.7(2) . . . . ? N1 Cu N3 C22 -107.9(3) 4_755 . . . ? N1 Cu N3 C22 -8.1(4) . . . . ? N3 Cu N3 C22 95.0(3) 4_755 . . . ? C1 O1 C2 C35 -169.9(5) . . . . ? C1 O1 C2 C3 11.4(7) . . . . ? O1 C2 C3 C4 178.1(4) . . . . ? C35 C2 C3 C4 -0.6(6) . . . . ? C2 C3 C4 C6 -0.7(6) . . . . ? C2 C3 C4 C5 176.7(4) . . . . ? C3 C4 C6 C34 1.6(5) . . . . ? C5 C4 C6 C34 -175.7(4) . . . . ? C3 C4 C6 C8 179.9(3) . . . . ? C5 C4 C6 C8 2.5(5) . . . . ? C11 N1 C7 C8 -2.1(5) . . . . ? Cu N1 C7 C8 163.9(2) . . . . ? N1 C7 C8 C9 3.1(5) . . . . ? N1 C7 C8 C6 -175.8(3) . . . . ? C4 C6 C8 C9 61.5(5) . . . . ? C34 C6 C8 C9 -120.3(4) . . . . ? C4 C6 C8 C7 -119.8(4) . . . . ? C34 C6 C8 C7 58.4(5) . . . . ? C7 C8 C9 C10 -1.2(5) . . . . ? C6 C8 C9 C10 177.5(4) . . . . ? C8 C9 C10 C11 -1.4(6) . . . . ? C8 C9 C10 C16B -169.5(11) . . . . ? C7 N1 C11 C10 -0.8(5) . . . . ? Cu N1 C11 C10 -169.0(3) . . . . ? C7 N1 C11 C12 177.7(3) . . . . ? Cu N1 C11 C12 9.5(3) . . . . ? C9 C10 C11 N1 2.5(5) . . . . ? C16B C10 C11 N1 173.6(8) . . . . ? C9 C10 C11 C12 -175.8(3) . . . . ? C16B C10 C11 C12 -4.7(9) . . . . ? C23 N2 C12 C13 -1.3(6) . . . . ? Cu N2 C12 C13 179.1(3) . . . . ? C23 N2 C12 C11 178.2(3) . . . . ? Cu N2 C12 C11 -1.4(4) . . . . ? N1 C11 C12 N2 -6.0(4) . . . . ? C10 C11 C12 N2 172.4(3) . . . . ? N1 C11 C12 C13 173.4(4) . . . . ? C10 C11 C12 C13 -8.1(6) . . . . ? N2 C12 C13 C14 3.2(7) . . . . ? C11 C12 C13 C14 -176.3(5) . . . . ? N2 C12 C13 C17B -160.5(11) . . . . ? C11 C12 C13 C17B 20.1(12) . . . . ? C12 C13 C14 C15 -1.4(9) . . . . ? C17B C13 C14 C15 157.6(14) . . . . ? C13 C14 C15 C23 -2.0(9) . . . . ? C13 C14 C15 C16A 173.8(6) . . . . ? C23 C15 C16A C17A -5.9(10) . . . . ? C14 C15 C16A C17A 178.3(7) . . . . ? C15 C16A C17A C18 1.8(11) . . . . ? C9 C10 C16B C17B 172.1(17) . . . . ? C11 C10 C16B C17B 3(2) . . . . ? C10 C16B C17B C13 12(4) . . . . ? C14 C13 C17B C16B 177.4(15) . . . . ? C12 C13 C17B C16B -22(3) . . . . ? C16A C17A C18 C19 -178.9(6) . . . . ? C16A C17A C18 C22 0.6(9) . . . . ? C22 C18 C19 C20 0.2(7) . . . . ? C17A C18 C19 C20 179.7(5) . . . . ? C18 C19 C20 C21 -0.6(6) . . . . ? C18 C19 C20 C24 -179.8(4) . . . . ? C22 N3 C21 C20 -1.1(6) . . . . ? Cu N3 C21 C20 167.6(3) . . . . ? C19 C20 C21 N3 1.0(6) . . . . ? C24 C20 C21 N3 -179.7(4) . . . . ? C21 N3 C22 C18 0.7(6) . . . . ? Cu N3 C22 C18 -170.5(3) . . . . ? C21 N3 C22 C23 179.8(3) . . . . ? Cu N3 C22 C23 8.7(4) . . . . ? C19 C18 C22 N3 -0.2(6) . . . . ? C17A C18 C22 N3 -179.7(4) . . . . ? C19 C18 C22 C23 -179.4(4) . . . . ? C17A C18 C22 C23 1.1(7) . . . . ? C12 N2 C23 C15 -2.4(6) . . . . ? Cu N2 C23 C15 177.3(4) . . . . ? C12 N2 C23 C22 177.8(3) . . . . ? Cu N2 C23 C22 -2.6(5) . . . . ? C14 C15 C23 N2 4.0(8) . . . . ? C16A C15 C23 N2 -172.2(5) . . . . ? C14 C15 C23 C22 -176.2(5) . . . . ? C16A C15 C23 C22 7.6(8) . . . . ? N3 C22 C23 N2 -4.9(5) . . . . ? C18 C22 C23 N2 174.3(4) . . . . ? N3 C22 C23 C15 175.3(4) . . . . ? C18 C22 C23 C15 -5.5(7) . . . . ? C19 C20 C24 C25 59.4(5) . . . . ? C21 C20 C24 C25 -119.8(4) . . . . ? C19 C20 C24 C31 -121.3(4) . . . . ? C21 C20 C24 C31 59.5(5) . . . . ? C31 C24 C25 C27 0.9(5) . . . . ? C20 C24 C25 C27 -179.9(3) . . . . ? C31 C24 C25 C26 -176.6(4) . . . . ? C20 C24 C25 C26 2.6(6) . . . . ? C24 C25 C27 C28 -0.6(6) . . . . ? C26 C25 C27 C28 177.0(4) . . . . ? C29 O2 C28 C30 -6.5(6) . . . . ? C29 O2 C28 C27 175.2(4) . . . . ? C25 C27 C28 O2 178.5(4) . . . . ? C25 C27 C28 C30 0.2(6) . . . . ? O2 C28 C30 C31 -178.2(4) . . . . ? C27 C28 C30 C31 0.0(6) . . . . ? C28 C30 C31 C24 0.3(5) . . . . ? C28 C30 C31 C32 179.6(4) . . . . ? C25 C24 C31 C30 -0.8(5) . . . . ? C20 C24 C31 C30 180.0(3) . . . . ? C25 C24 C31 C32 180.0(4) . . . . ? C20 C24 C31 C32 0.7(6) . . . . ? C4 C6 C34 C35 -1.2(6) . . . . ? C8 C6 C34 C35 -179.5(4) . . . . ? C4 C6 C34 C33 179.9(4) . . . . ? C8 C6 C34 C33 1.7(6) . . . . ? C6 C34 C35 C2 -0.1(6) . . . . ? C33 C34 C35 C2 178.8(4) . . . . ? O1 C2 C35 C34 -177.8(4) . . . . ? C3 C2 C35 C34 1.0(6) . . . . ? #===END data_7a _database_code_depnum_ccdc_archive 'CCDC 735253' # SG0319 _audit_creation_method SHELXL-97 _audit_creation_date 03-10-09 _chemical_name_systematic ; bis{8-(4-methoxy-2,6-dimethylphenyl)-2-[5-(4-methoxy-2,6- dimethylphenyl)-pyridin-2-yl]-1,10-phenanthroline}zinc(II) hexafluorophosphate tri-acetonitrile solvate ; _chemical_name_common ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_moiety 'C70 H62 N6 O4 Zn 2+, 2(F6 P 1-), 3(C2 H3 N)' _chemical_formula_sum 'C76 H71 F12 N9 O4 P2 Zn' _chemical_formula_weight 1529.76 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 304 0.0033 0.0016 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; H H 284 0.0000 0.0000 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; F F 48 0.0171 0.0103 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; N N 36 0.0061 0.0033 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; O O 16 0.0106 0.0060 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; P P 8 0.1023 0.0942 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; Zn Zn 4 0.2839 1.4301 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall ? _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 12.9177(1) _cell_length_b 25.4666(3) _cell_length_c 22.1526(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.0097(8) _cell_angle_gamma 90.00 _cell_volume 7277.49(14) _cell_formula_units_Z 4 _cell_measurement_temperature 160(1) _cell_measurement_reflns_used 256696 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.396 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3160 _exptl_absorpt_coefficient_mu 0.468 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Blessing, 1995)' _exptl_absorpt_correction_T_min 0.771 _exptl_absorpt_correction_T_max 0.895 _exptl_special_details ; Solvent used: acetonitrile / diethylether Cooling Device: Oxford Cryosystems Cryostream 700 Crystal mount: glued on a glass fibre Mosaicity (deg.): 0.5930 Frames collected: 1287 Seconds exposure per frame: 30 Degrees rotation per frame: 0.5 Crystal-Detector distance (mm): 39.0 ; _diffrn_ambient_temperature 160(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Nonius FR590 sealed tube generator' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_detector '65 mm CCD camera on \k goniostat' _diffrn_measurement_device_type 'Nonius KappaCCD area-detector diffractometer' _diffrn_measurement_method '\f and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 110992 _diffrn_reflns_av_R_equivalents 0.0763 _diffrn_reflns_av_sigmaI/netI 0.0484 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 25.04 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.998 _reflns_number_total 12861 _reflns_number_gt 8514 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'COLLECT (Nonius, 2000)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN and SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'SHELXL97 and PLATON (Spek, 2009)' _refine_special_details ; The asymmetric unit contains one cation, two anions and three acetonitrile molecules. In the cation, the two central CH groups of the phenanthroline moiety of each ligand are disordered over two sites which effectively complete six-membered rings between all pyridine rings, thereby indicating that each ligand must be disordered through a 180\% rotation about the central N-atom. The site occupation factor for the major conformation refined to 0.87(1) for one ligand and 0.68(1) for the other ligand. The chemically equivalent C-C bonds involving the disordered C-atoms were restrained to have similar lengths and the atomic displacement parameters of the disordered C-atoms were given light pseudo-isotropic restraints. The PF6- anions are highly disordered. Two sets of P- and F-atoms were defined for each anion and refinement of the site occupation factors led to values of 0.68(1) and 0.80(1) for the major conformations in each anion. The P-F and F...F distances were restrained tightly, so as to maintain octahedral geometry and uniform P-F bond lengths and the atomic displacement parameters of the P- and F-atoms were given light pseudo-isotropic restraints. The bond lengths within the MeCN molecules were also restrained to logical values and the atoms given light pseudo-isotropic restraints. Validation reports some short contacts as A alerts. These are mostly between different disordered components of anions and cations where the sums of the SOF of the relevant atoms is < 1.0, so that one can conceive that the "conflicting" sites are never occupied simultanously for adjacent moieties. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0956P)^2^+23.8126P] 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 SHELXL _refine_ls_extinction_coef 0.0013(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 12858 _refine_ls_number_parameters 1119 _refine_ls_number_restraints 1780 _refine_ls_R_factor_all 0.1515 _refine_ls_R_factor_gt 0.1065 _refine_ls_wR_factor_ref 0.2818 _refine_ls_wR_factor_gt 0.2540 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.185 _refine_diff_density_min -0.968 _refine_diff_density_rms 0.072 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 Zn Zn 0.20742(6) 0.48394(3) 0.25370(4) 0.0731(3) Uani 1 1 d . . . O1 O -0.3505(4) 0.2613(3) 0.3321(3) 0.1039(18) Uani 1 1 d . . . O2 O 0.7236(5) 0.4799(3) -0.0423(3) 0.1063(19) Uani 1 1 d . A . O3 O -0.3173(4) 0.7179(3) 0.1199(3) 0.115(2) Uani 1 1 d . . . O4 O 0.7454(4) 0.5094(2) 0.5541(2) 0.0844(15) Uani 1 1 d . B . N1 N 0.0772(4) 0.4751(2) 0.3169(2) 0.0637(14) Uani 1 1 d . . . N2 N 0.2058(5) 0.5531(2) 0.3006(3) 0.0768(18) Uani 1 1 d . A . N3 N 0.3343(5) 0.5283(2) 0.2145(3) 0.0748(17) Uani 1 1 d . . . N4 N 0.0862(4) 0.4942(2) 0.1814(3) 0.0660(14) Uani 1 1 d . . . N5 N 0.1932(4) 0.4114(2) 0.2161(3) 0.0663(14) Uani 1 1 d . B . N6 N 0.3268(4) 0.4375(2) 0.3051(3) 0.0673(15) Uani 1 1 d . . . C1 C -0.3652(9) 0.2277(5) 0.3819(5) 0.135(4) Uani 1 1 d . . . H11 H -0.3876 0.2485 0.4161 0.202 Uiso 1 1 calc R . . H12 H -0.2999 0.2099 0.3935 0.202 Uiso 1 1 calc R . . H13 H -0.4184 0.2015 0.3707 0.202 Uiso 1 1 calc R . . C2 C -0.2834(6) 0.3029(4) 0.3396(4) 0.084(2) Uani 1 1 d . . . C3 C -0.2403(6) 0.3196(4) 0.3958(4) 0.089(3) Uani 1 1 d . . . H3 H -0.2562 0.3012 0.4314 0.107 Uiso 1 1 calc R . . C4 C -0.1748(6) 0.3626(3) 0.3999(3) 0.078(2) Uani 1 1 d . . . C5 C -0.1290(7) 0.3783(4) 0.4609(3) 0.100(3) Uani 1 1 d . . . H51 H -0.1423 0.3508 0.4904 0.150 Uiso 1 1 calc R . . H52 H -0.1608 0.4113 0.4735 0.150 Uiso 1 1 calc R . . H53 H -0.0541 0.3833 0.4587 0.150 Uiso 1 1 calc R . . C6 C -0.1506(5) 0.3897(3) 0.3471(3) 0.0697(19) Uani 1 1 d . . . C7 C 0.0129(5) 0.4351(3) 0.3196(3) 0.0650(18) Uani 1 1 d . . . H7 H 0.0303 0.4038 0.2992 0.078 Uiso 1 1 calc R . . C8 C -0.0791(6) 0.4352(3) 0.3502(3) 0.0705(19) Uani 1 1 d . . . C9 C -0.0980(7) 0.4817(4) 0.3807(3) 0.086(2) Uani 1 1 d . A . H9 H -0.1590 0.4850 0.4025 0.104 Uiso 1 1 calc R . . C10 C -0.0290(9) 0.5234(3) 0.3797(3) 0.094(3) Uani 1 1 d D . . H10 H -0.0417 0.5544 0.4020 0.113 Uiso 0.866(12) 1 calc PR A 1 C11 C 0.0590(6) 0.5198(3) 0.3460(3) 0.075(2) Uani 1 1 d . A . C12 C 0.1356(7) 0.5617(3) 0.3401(3) 0.078(2) Uani 1 1 d . . . C13 C 0.1363(9) 0.6106(3) 0.3721(4) 0.104(3) Uani 1 1 d D A . H131 H 0.0838 0.6192 0.3989 0.125 Uiso 0.866(12) 1 calc PR A 1 C14 C 0.2152(10) 0.6439(3) 0.3624(4) 0.115(4) Uani 1 1 d . . . H14 H 0.2173 0.6761 0.3840 0.138 Uiso 1 1 calc R A . C15 C 0.2939(8) 0.6343(3) 0.3229(4) 0.106(3) Uani 1 1 d D A . H15 H 0.3497 0.6581 0.3186 0.127 Uiso 0.134(12) 1 calc PR A 2 C16A C 0.3838(8) 0.6651(4) 0.3100(5) 0.107(4) Uani 0.866(12) 1 d PDU A 1 H161 H 0.3939 0.6976 0.3307 0.128 Uiso 0.866(12) 1 calc PR A 1 C17A C 0.4536(9) 0.6511(4) 0.2709(5) 0.114(4) Uani 0.866(12) 1 d PDU A 1 H171 H 0.5129 0.6727 0.2670 0.137 Uiso 0.866(12) 1 calc PR A 1 C16B C -0.028(4) 0.5765(9) 0.403(3) 0.11(2) Uani 0.134(12) 1 d PDU A 2 H162 H -0.0846 0.5842 0.4264 0.127 Uiso 0.134(12) 1 calc PR A 2 C17B C 0.0363(18) 0.6171(16) 0.397(2) 0.067(15) Uani 0.134(12) 1 d PDU A 2 H172 H 0.0157 0.6509 0.4103 0.080 Uiso 0.134(12) 1 calc PR A 2 C18 C 0.4427(8) 0.6044(3) 0.2342(4) 0.094(3) Uani 1 1 d D . . H18 H 0.4566 0.6359 0.2562 0.113 Uiso 0.134(12) 1 calc PR A 2 C19 C 0.5076(7) 0.5873(4) 0.1897(4) 0.097(3) Uani 1 1 d . A . H19 H 0.5672 0.6077 0.1824 0.116 Uiso 1 1 calc R . . C20 C 0.4897(6) 0.5421(3) 0.1554(4) 0.079(2) Uani 1 1 d . . . C21 C 0.3978(5) 0.5147(3) 0.1710(4) 0.080(2) Uani 1 1 d . A . H21 H 0.3802 0.4840 0.1483 0.096 Uiso 1 1 calc R . . C22 C 0.3543(6) 0.5724(3) 0.2455(4) 0.077(2) Uani 1 1 d . A . C23 C 0.2851(7) 0.5865(2) 0.2894(3) 0.080(2) Uani 1 1 d . . . C24 C 0.5515(5) 0.5256(3) 0.1063(4) 0.084(2) Uani 1 1 d . A . C25 C 0.5153(7) 0.6118(3) 0.0529(4) 0.099(3) Uani 1 1 d . A . H251 H 0.5639 0.6385 0.0691 0.149 Uiso 1 1 calc R . . H252 H 0.4522 0.6126 0.0756 0.149 Uiso 1 1 calc R . . H253 H 0.4976 0.6193 0.0102 0.149 Uiso 1 1 calc R . . C26 C 0.5655(6) 0.5576(3) 0.0588(4) 0.082(2) Uani 1 1 d . . . C27 C 0.6227(6) 0.5407(3) 0.0113(5) 0.095(3) Uani 1 1 d . A . H27 H 0.6305 0.5634 -0.0222 0.114 Uiso 1 1 calc R . . C28 C 0.6714(7) 0.4888(4) 0.0113(5) 0.099(3) Uani 1 1 d . . . C29 C 0.7703(8) 0.4284(4) -0.0453(5) 0.120(3) Uani 1 1 d . . . H291 H 0.7179 0.4015 -0.0387 0.180 Uiso 1 1 calc R A . H292 H 0.8267 0.4255 -0.0141 0.180 Uiso 1 1 calc R . . H293 H 0.7980 0.4234 -0.0853 0.180 Uiso 1 1 calc R . . C30 C 0.6528(6) 0.4589(4) 0.0583(6) 0.108(3) Uani 1 1 d . A . H30 H 0.6797 0.4242 0.0585 0.130 Uiso 1 1 calc R . . C31 C 0.5965(6) 0.4741(3) 0.1082(5) 0.093(3) Uani 1 1 d . . . C32 C 0.5813(7) 0.4396(4) 0.1625(6) 0.144(5) Uani 1 1 d . A . H321 H 0.6309 0.4104 0.1628 0.216 Uiso 1 1 calc R . . H322 H 0.5105 0.4256 0.1604 0.216 Uiso 1 1 calc R . . H323 H 0.5926 0.4603 0.1995 0.216 Uiso 1 1 calc R . . C33 C -0.1673(7) 0.3975(4) 0.2332(3) 0.113(3) Uani 1 1 d . . . H331 H -0.2126 0.3842 0.1998 0.169 Uiso 1 1 calc R . . H332 H -0.0949 0.3899 0.2252 0.169 Uiso 1 1 calc R . . H333 H -0.1765 0.4356 0.2368 0.169 Uiso 1 1 calc R . . C34 C -0.1943(5) 0.3716(4) 0.2905(3) 0.082(2) Uani 1 1 d . . . C35 C -0.2601(5) 0.3291(4) 0.2894(4) 0.088(2) Uani 1 1 d . . . H35 H -0.2902 0.3178 0.2516 0.105 Uiso 1 1 calc R . . C36 C -0.3313(8) 0.7476(4) 0.0656(5) 0.133(4) Uani 1 1 d . . . H361 H -0.3549 0.7244 0.0324 0.200 Uiso 1 1 calc R . . H362 H -0.2654 0.7639 0.0561 0.200 Uiso 1 1 calc R . . H363 H -0.3833 0.7750 0.0709 0.200 Uiso 1 1 calc R . . C37 C -0.2520(6) 0.6750(4) 0.1193(5) 0.093(3) Uani 1 1 d . . . C38 C -0.2081(6) 0.6557(4) 0.0693(4) 0.090(3) Uani 1 1 d . . . H38 H -0.2213 0.6728 0.0315 0.108 Uiso 1 1 calc R . . C39 C -0.1439(5) 0.6112(3) 0.0722(3) 0.082(2) Uani 1 1 d . . . C40 C -0.0962(7) 0.5923(4) 0.0155(4) 0.114(3) Uani 1 1 d . . . H401 H -0.1371 0.5631 -0.0018 0.171 Uiso 1 1 calc R . . H402 H -0.0251 0.5805 0.0254 0.171 Uiso 1 1 calc R . . H403 H -0.0951 0.6211 -0.0138 0.171 Uiso 1 1 calc R . . C41 C -0.1260(5) 0.5856(3) 0.1280(3) 0.0715(19) Uani 1 1 d . . . C42 C 0.0298(5) 0.5368(3) 0.1702(3) 0.0694(18) Uani 1 1 d . . . H42 H 0.0530 0.5688 0.1883 0.083 Uiso 1 1 calc R . . C43 C -0.0612(5) 0.5378(3) 0.1338(3) 0.0702(19) Uani 1 1 d . . . C44 C -0.0899(5) 0.4908(3) 0.1062(3) 0.077(2) Uani 1 1 d . B . H44 H -0.1506 0.4894 0.0801 0.092 Uiso 1 1 calc R . . C45 C -0.0309(6) 0.4459(3) 0.1162(3) 0.072(2) Uani 1 1 d D . . H45 H -0.0500 0.4139 0.0966 0.086 Uiso 0.683(12) 1 calc PR B 1 C46 C 0.0560(5) 0.4484(3) 0.1552(3) 0.0659(17) Uani 1 1 d . B . C47 C 0.1172(5) 0.4022(3) 0.1739(3) 0.0656(17) Uani 1 1 d . . . C48 C 0.0992(6) 0.3507(3) 0.1531(3) 0.0726(19) Uani 1 1 d D B . H48 H 0.0452 0.3437 0.1234 0.087 Uiso 0.683(12) 1 calc PR B 1 C49 C 0.1600(7) 0.3109(3) 0.1758(4) 0.088(2) Uani 1 1 d . . . H49 H 0.1478 0.2760 0.1622 0.106 Uiso 1 1 calc R B . C50 C 0.2396(6) 0.3212(3) 0.2186(4) 0.083(2) Uani 1 1 d D B . H50 H 0.2840 0.2939 0.2335 0.100 Uiso 0.317(12) 1 calc PR B 2 C51A C 0.3137(8) 0.2839(4) 0.2440(5) 0.083(4) Uani 0.683(12) 1 d PDU B 1 H511 H 0.3086 0.2480 0.2329 0.100 Uiso 0.683(12) 1 calc PR B 1 C52A C 0.3893(8) 0.2996(3) 0.2831(5) 0.080(3) Uani 0.683(12) 1 d PDU B 1 H521 H 0.4373 0.2736 0.2974 0.096 Uiso 0.683(12) 1 calc PR B 1 C51B C -0.034(2) 0.3908(4) 0.1013(13) 0.108(10) Uani 0.317(12) 1 d PDU B 2 H512 H -0.0893 0.3858 0.0715 0.130 Uiso 0.317(12) 1 calc PR B 2 C52B C 0.0088(13) 0.3441(8) 0.1128(10) 0.098(9) Uani 0.317(12) 1 d PDU B 2 H522 H -0.0161 0.3116 0.0969 0.117 Uiso 0.317(12) 1 calc PR B 2 C53 C 0.4052(6) 0.3522(3) 0.3059(4) 0.082(2) Uani 1 1 d D . . H531 H 0.4063 0.3172 0.2911 0.098 Uiso 0.317(12) 1 calc PR B 2 C54 C 0.4794(6) 0.3700(3) 0.3503(3) 0.079(2) Uani 1 1 d . B . H54 H 0.5318 0.3467 0.3656 0.095 Uiso 1 1 calc R . . C55 C 0.4772(5) 0.4209(3) 0.3719(3) 0.0664(17) Uani 1 1 d . . . C56 C 0.3954(5) 0.4529(2) 0.3468(3) 0.0684(18) Uani 1 1 d . B . H56 H 0.3903 0.4878 0.3614 0.082 Uiso 1 1 calc R . . C57 C 0.3305(5) 0.3879(2) 0.2847(3) 0.0667(18) Uani 1 1 d . B . C58 C 0.2529(5) 0.3727(2) 0.2390(3) 0.0657(17) Uani 1 1 d . . . C59 C 0.5498(5) 0.4437(3) 0.4186(3) 0.0657(17) Uani 1 1 d . B . C60 C 0.5960(7) 0.5169(4) 0.3456(4) 0.120(4) Uani 1 1 d . B . H601 H 0.6601 0.5364 0.3399 0.180 Uiso 1 1 calc R . . H602 H 0.5370 0.5411 0.3432 0.180 Uiso 1 1 calc R . . H603 H 0.5868 0.4901 0.3139 0.180 Uiso 1 1 calc R . . C61 C 0.6025(5) 0.4906(3) 0.4069(3) 0.076(2) Uani 1 1 d . . . C62 C 0.6676(5) 0.5136(3) 0.4519(3) 0.0711(19) Uani 1 1 d . B . H62 H 0.7023 0.5456 0.4440 0.085 Uiso 1 1 calc R . . C63 C 0.6815(5) 0.4899(3) 0.5079(3) 0.0690(18) Uani 1 1 d . . . C64 C 0.7943(6) 0.5584(3) 0.5449(4) 0.095(3) Uani 1 1 d . . . H641 H 0.7414 0.5854 0.5367 0.142 Uiso 1 1 calc R B . H642 H 0.8385 0.5557 0.5104 0.142 Uiso 1 1 calc R . . H643 H 0.8368 0.5679 0.5812 0.142 Uiso 1 1 calc R . . C65 C 0.6309(6) 0.4435(3) 0.5195(4) 0.079(2) Uani 1 1 d . B . H65 H 0.6410 0.4273 0.5580 0.094 Uiso 1 1 calc R . . C66 C 0.5661(5) 0.4203(3) 0.4762(3) 0.0722(19) Uani 1 1 d . . . C67 C 0.5119(7) 0.3706(3) 0.4928(4) 0.093(2) Uani 1 1 d . B . H671 H 0.5045 0.3697 0.5366 0.139 Uiso 1 1 calc R . . H672 H 0.5527 0.3403 0.4807 0.139 Uiso 1 1 calc R . . H673 H 0.4432 0.3694 0.4719 0.139 Uiso 1 1 calc R . . C68 C -0.1580(8) 0.5797(4) 0.2402(4) 0.120(4) Uani 1 1 d . . . H681 H -0.0861 0.5840 0.2558 0.181 Uiso 1 1 calc R . . H682 H -0.1741 0.5423 0.2362 0.181 Uiso 1 1 calc R . . H683 H -0.2047 0.5959 0.2683 0.181 Uiso 1 1 calc R . . C69 C -0.1719(6) 0.6058(4) 0.1795(4) 0.087(2) Uani 1 1 d . . . C70 C -0.2339(6) 0.6503(4) 0.1745(4) 0.091(2) Uani 1 1 d . . . H70 H -0.2642 0.6639 0.2094 0.110 Uiso 1 1 calc R . . P1A P 0.7842(4) 0.29373(11) 0.06223(13) 0.0726(14) Uani 0.675(11) 1 d PDU C 1 F1A F 0.7413(7) 0.23904(18) 0.0388(3) 0.151(5) Uani 0.675(11) 1 d PDU C 1 F2A F 0.8256(7) 0.34865(18) 0.0855(3) 0.130(4) Uani 0.675(11) 1 d PDU C 1 F3A F 0.8875(5) 0.2665(3) 0.0868(4) 0.166(5) Uani 0.675(11) 1 d PDU C 1 F4A F 0.6807(5) 0.3208(2) 0.0374(3) 0.127(3) Uani 0.675(11) 1 d PDU C 1 F5A F 0.8334(7) 0.3036(4) -0.0004(2) 0.143(4) Uani 0.675(11) 1 d PDU C 1 F6A F 0.7353(6) 0.2831(3) 0.1248(2) 0.114(3) Uani 0.675(11) 1 d PDU C 1 P1B P 0.7214(9) 0.2856(3) 0.0568(4) 0.109(4) Uani 0.325(11) 1 d PDU C 2 F1B F 0.7063(13) 0.2302(4) 0.0259(8) 0.159(10) Uani 0.325(11) 1 d PDU C 2 F2B F 0.7366(16) 0.3409(4) 0.0879(7) 0.135(7) Uani 0.325(11) 1 d PDU C 2 F3B F 0.8249(11) 0.2658(5) 0.0902(7) 0.139(8) Uani 0.325(11) 1 d PDU C 2 F4B F 0.6182(11) 0.3055(7) 0.0233(8) 0.190(11) Uani 0.325(11) 1 d PDU C 2 F5B F 0.7847(13) 0.3049(6) 0.0021(5) 0.120(7) Uani 0.325(11) 1 d PDU C 2 F6B F 0.6580(14) 0.2663(7) 0.1115(6) 0.190(11) Uani 0.325(11) 1 d PDU C 2 P2A P 0.2541(15) 0.1793(6) 0.0943(7) 0.134(7) Uani 0.204(10) 1 d PDU D 1 F7A F 0.253(3) 0.1181(6) 0.1046(14) 0.155(16) Uani 0.204(10) 1 d PDU D 1 F8A F 0.255(3) 0.2405(7) 0.0840(14) 0.183(18) Uani 0.204(10) 1 d PDU D 1 F9A F 0.151(2) 0.1750(15) 0.0535(13) 0.43(7) Uani 0.204(10) 1 d PDU D 1 F10A F 0.358(2) 0.1836(15) 0.1350(17) 0.62(11) Uani 0.204(10) 1 d PDU D 1 F11A F 0.319(3) 0.1714(13) 0.0367(14) 0.33(4) Uani 0.204(10) 1 d PDU D 1 F12A F 0.189(3) 0.1872(8) 0.1518(10) 0.106(10) Uani 0.204(10) 1 d PDU D 1 P2B P 0.1926(3) 0.17159(10) 0.08977(12) 0.0877(13) Uani 0.796(10) 1 d PDU D 2 F7B F 0.2045(5) 0.11297(14) 0.1120(3) 0.110(3) Uani 0.796(10) 1 d PDU D 2 F8B F 0.1788(6) 0.22995(15) 0.0671(3) 0.134(3) Uani 0.796(10) 1 d PDU D 2 F9B F 0.1112(4) 0.1525(3) 0.0389(3) 0.162(4) Uani 0.796(10) 1 d PDU D 2 F10B F 0.2734(5) 0.1900(2) 0.1413(3) 0.137(3) Uani 0.796(10) 1 d PDU D 2 F11B F 0.2817(4) 0.1630(2) 0.0449(2) 0.117(3) Uani 0.796(10) 1 d PDU D 2 F12B F 0.1024(5) 0.1801(3) 0.1340(3) 0.157(4) Uani 0.796(10) 1 d PDU D 2 N7 N 0.8758(8) 0.1601(4) 0.3059(5) 0.153(4) Uani 1 1 d DU . . C71 C 0.9098(11) 0.1904(5) 0.2748(5) 0.147(4) Uani 1 1 d DU . . C72 C 0.9461(11) 0.2350(5) 0.2410(6) 0.162(5) Uani 1 1 d DU . . H721 H 0.8891 0.2488 0.2147 0.243 Uiso 1 1 calc R . . H722 H 1.0029 0.2239 0.2163 0.243 Uiso 1 1 calc R . . H723 H 0.9708 0.2625 0.2693 0.243 Uiso 1 1 calc R . . N8 N 0.3584(11) 0.3690(6) 0.1051(6) 0.188(5) Uani 1 1 d DU . . C73 C 0.3975(14) 0.3289(6) 0.1009(8) 0.178(6) Uani 1 1 d DU . . C74 C 0.4573(14) 0.2807(7) 0.1020(9) 0.230(8) Uani 1 1 d DU . . H741 H 0.5213 0.2862 0.0809 0.345 Uiso 1 1 calc R . . H742 H 0.4164 0.2528 0.0818 0.345 Uiso 1 1 calc R . . H743 H 0.4746 0.2706 0.1440 0.345 Uiso 1 1 calc R . . N9 N 0.1027(9) 0.3169(5) 0.3565(6) 0.174(5) Uani 1 1 d DU . . C75 C 0.0618(9) 0.2894(5) 0.3882(6) 0.133(4) Uani 1 1 d DU . . C76 C 0.0128(8) 0.2561(5) 0.4318(5) 0.148(4) Uani 1 1 d DU . . H761 H 0.0161 0.2194 0.4187 0.221 Uiso 1 1 calc R . . H762 H -0.0598 0.2666 0.4345 0.221 Uiso 1 1 calc R . . H763 H 0.0491 0.2599 0.4715 0.221 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 Zn 0.0593(5) 0.0483(4) 0.1083(7) -0.0244(4) -0.0284(4) 0.0052(3) O1 0.080(4) 0.129(5) 0.102(4) 0.015(4) -0.002(3) -0.003(4) O2 0.092(4) 0.106(5) 0.122(5) -0.015(4) 0.011(4) 0.006(3) O3 0.085(4) 0.120(5) 0.139(5) 0.045(4) -0.003(4) 0.025(4) O4 0.095(4) 0.083(3) 0.073(3) 0.024(3) -0.020(3) -0.003(3) N1 0.064(3) 0.059(3) 0.066(3) -0.018(3) -0.023(3) 0.018(3) N2 0.099(5) 0.051(3) 0.076(4) -0.015(3) -0.040(4) 0.016(3) N3 0.076(4) 0.040(3) 0.104(5) -0.008(3) -0.040(4) -0.009(3) N4 0.051(3) 0.065(3) 0.080(4) -0.019(3) -0.014(3) -0.006(3) N5 0.062(3) 0.052(3) 0.085(4) -0.016(3) 0.006(3) -0.004(3) N6 0.052(3) 0.050(3) 0.099(4) -0.014(3) -0.012(3) 0.004(2) C1 0.132(9) 0.144(10) 0.128(9) 0.039(8) 0.011(7) -0.015(7) C2 0.056(4) 0.113(7) 0.084(6) 0.004(5) -0.001(4) 0.016(4) C3 0.073(5) 0.124(7) 0.072(5) 0.016(5) 0.015(4) 0.034(5) C4 0.067(5) 0.100(6) 0.067(5) -0.003(4) 0.004(4) 0.025(4) C5 0.126(7) 0.109(7) 0.064(5) 0.000(5) 0.001(5) 0.026(6) C6 0.049(4) 0.105(6) 0.055(4) -0.002(4) 0.002(3) 0.025(4) C7 0.056(4) 0.071(4) 0.066(4) -0.017(3) -0.017(3) 0.016(3) C8 0.073(5) 0.090(5) 0.048(4) -0.005(3) -0.007(3) 0.031(4) C9 0.091(6) 0.106(7) 0.062(5) -0.004(5) 0.006(4) 0.039(5) C10 0.148(8) 0.077(6) 0.055(4) -0.014(4) -0.018(5) 0.050(6) C11 0.096(5) 0.068(5) 0.058(4) -0.014(3) -0.024(4) 0.035(4) C12 0.116(6) 0.053(4) 0.059(4) -0.007(3) -0.042(4) 0.018(4) C13 0.182(10) 0.057(5) 0.070(5) -0.010(4) -0.028(6) 0.022(6) C14 0.212(12) 0.040(4) 0.087(6) -0.013(4) -0.035(7) -0.009(6) C15 0.174(10) 0.064(5) 0.075(6) -0.008(4) -0.034(6) -0.006(6) C16A 0.143(7) 0.059(5) 0.116(7) -0.007(5) -0.013(6) -0.041(5) C17A 0.134(7) 0.095(7) 0.111(7) 0.003(5) -0.015(6) -0.038(6) C16B 0.11(2) 0.11(2) 0.10(2) 0.001(10) 0.002(10) 0.003(10) C17B 0.071(17) 0.061(17) 0.067(17) -0.002(10) -0.007(10) 0.000(10) C18 0.128(7) 0.048(4) 0.100(6) 0.011(4) -0.059(6) -0.038(5) C19 0.099(6) 0.085(6) 0.104(7) 0.018(5) -0.033(5) -0.026(5) C20 0.074(5) 0.052(4) 0.107(6) 0.020(4) -0.043(5) -0.029(4) C21 0.058(4) 0.050(4) 0.130(7) -0.011(4) -0.028(4) 0.003(3) C22 0.092(5) 0.050(4) 0.084(5) -0.007(4) -0.033(4) 0.007(4) C23 0.117(6) 0.036(3) 0.080(5) -0.002(3) -0.058(5) -0.008(4) C24 0.049(4) 0.080(5) 0.121(7) -0.001(5) -0.009(4) -0.016(4) C25 0.122(7) 0.062(5) 0.111(7) -0.007(4) -0.023(5) 0.002(5) C26 0.075(5) 0.051(4) 0.116(7) 0.006(4) -0.030(5) -0.013(4) C27 0.078(5) 0.062(5) 0.139(8) 0.002(5) -0.033(5) -0.013(4) C28 0.085(6) 0.082(6) 0.128(8) 0.010(6) -0.016(6) -0.040(5) C29 0.116(8) 0.117(8) 0.127(8) -0.020(6) 0.000(6) 0.010(6) C30 0.040(4) 0.093(6) 0.191(11) 0.015(7) -0.008(5) -0.003(4) C31 0.056(4) 0.064(5) 0.156(8) 0.030(5) -0.010(5) -0.010(4) C32 0.068(5) 0.116(8) 0.249(14) 0.072(9) 0.020(7) 0.020(5) C33 0.088(6) 0.191(11) 0.057(5) 0.007(5) -0.018(4) -0.037(6) C34 0.047(4) 0.134(7) 0.065(5) 0.002(4) -0.003(3) 0.008(4) C35 0.054(4) 0.144(8) 0.064(5) 0.005(5) -0.006(4) -0.002(5) C36 0.107(7) 0.125(8) 0.165(10) 0.061(8) -0.020(7) 0.014(6) C37 0.056(4) 0.115(7) 0.107(7) 0.031(6) -0.007(5) 0.007(4) C38 0.060(4) 0.108(7) 0.099(6) 0.042(5) -0.021(4) -0.010(4) C39 0.055(4) 0.115(6) 0.074(5) 0.025(4) -0.013(4) -0.020(4) C40 0.105(7) 0.159(10) 0.078(6) 0.024(6) 0.014(5) 0.002(6) C41 0.048(4) 0.104(6) 0.061(4) 0.010(4) -0.010(3) -0.001(4) C42 0.057(4) 0.073(4) 0.076(5) -0.016(4) -0.019(3) 0.003(3) C43 0.049(4) 0.099(5) 0.062(4) -0.006(4) -0.007(3) -0.007(4) C44 0.059(4) 0.106(6) 0.063(4) -0.004(4) -0.010(3) -0.016(4) C45 0.074(4) 0.090(5) 0.052(4) -0.020(4) 0.002(3) -0.028(4) C46 0.059(4) 0.070(4) 0.067(4) -0.023(3) 0.000(3) -0.014(3) C47 0.065(4) 0.059(4) 0.074(4) -0.021(3) 0.005(3) -0.009(3) C48 0.079(5) 0.061(4) 0.077(5) -0.023(4) 0.008(4) -0.014(4) C49 0.113(6) 0.059(5) 0.093(6) -0.029(4) 0.015(5) -0.014(4) C50 0.101(6) 0.055(4) 0.093(6) -0.020(4) 0.010(5) 0.005(4) C51A 0.115(7) 0.054(5) 0.080(6) -0.007(5) 0.000(6) 0.015(5) C52A 0.098(7) 0.058(5) 0.082(6) -0.006(5) -0.004(5) 0.025(5) C51B 0.108(13) 0.111(13) 0.105(13) 0.006(9) 0.002(9) -0.002(9) C52B 0.096(12) 0.100(12) 0.097(12) -0.009(9) 0.016(9) -0.012(9) C53 0.099(6) 0.056(4) 0.092(6) 0.000(4) 0.008(5) 0.015(4) C54 0.088(5) 0.071(5) 0.079(5) 0.011(4) 0.013(4) 0.034(4) C55 0.051(4) 0.062(4) 0.086(5) 0.015(3) -0.001(3) 0.006(3) C56 0.050(3) 0.047(3) 0.106(5) -0.001(3) -0.017(4) 0.001(3) C57 0.065(4) 0.042(3) 0.093(5) -0.010(3) 0.010(4) 0.004(3) C58 0.064(4) 0.051(4) 0.083(5) -0.015(3) 0.015(3) -0.006(3) C59 0.048(3) 0.071(4) 0.078(5) 0.023(4) 0.000(3) 0.008(3) C60 0.117(7) 0.141(8) 0.098(6) 0.061(6) -0.044(5) -0.061(6) C61 0.060(4) 0.095(5) 0.071(4) 0.034(4) -0.014(3) 0.003(4) C62 0.049(3) 0.084(5) 0.078(5) 0.034(4) -0.009(3) -0.003(3) C63 0.056(4) 0.082(5) 0.068(4) 0.014(4) -0.012(3) 0.012(3) C64 0.089(5) 0.106(6) 0.085(5) 0.026(5) -0.032(4) -0.009(5) C65 0.084(5) 0.069(5) 0.081(5) 0.026(4) -0.009(4) 0.014(4) C66 0.064(4) 0.066(4) 0.087(5) 0.022(4) 0.001(4) 0.014(3) C67 0.113(6) 0.067(5) 0.098(6) 0.023(4) -0.001(5) 0.003(4) C68 0.140(8) 0.134(8) 0.088(6) 0.027(6) 0.021(6) 0.063(7) C69 0.065(4) 0.112(6) 0.082(5) 0.025(5) -0.003(4) 0.013(4) C70 0.075(5) 0.116(7) 0.084(5) 0.023(5) 0.010(4) 0.027(5) P1A 0.095(3) 0.0492(17) 0.071(2) 0.0003(13) -0.0198(18) 0.0067(17) F1A 0.285(13) 0.050(4) 0.109(6) -0.006(4) -0.065(7) -0.007(6) F2A 0.151(8) 0.087(5) 0.145(7) -0.004(5) -0.044(6) -0.042(5) F3A 0.115(8) 0.190(10) 0.192(9) 0.075(8) -0.006(7) 0.055(7) F4A 0.114(7) 0.083(5) 0.177(8) 0.039(5) -0.052(6) 0.010(5) F5A 0.134(8) 0.166(9) 0.131(8) 0.038(7) 0.022(6) 0.023(7) F6A 0.144(8) 0.121(6) 0.076(5) 0.001(4) 0.002(5) -0.017(5) P1B 0.113(7) 0.074(5) 0.136(7) 0.010(5) -0.019(6) 0.011(5) F1B 0.148(14) 0.152(16) 0.173(17) 0.015(13) -0.022(13) -0.036(13) F2B 0.154(15) 0.072(9) 0.174(14) -0.032(10) -0.022(12) 0.020(10) F3B 0.099(13) 0.113(12) 0.199(16) 0.053(12) -0.038(13) -0.006(11) F4B 0.183(18) 0.192(18) 0.190(17) 0.053(14) -0.044(14) 0.029(15) F5B 0.149(16) 0.101(12) 0.107(13) 0.020(10) -0.009(10) -0.014(11) F6B 0.196(18) 0.178(17) 0.194(18) 0.029(14) 0.002(15) -0.010(15) P2A 0.139(11) 0.120(10) 0.142(11) -0.028(8) 0.007(9) 0.004(8) F7A 0.18(2) 0.13(2) 0.16(2) 0.023(16) 0.039(17) 0.059(16) F8A 0.20(2) 0.17(2) 0.18(2) -0.026(17) 0.027(18) -0.013(17) F9A 0.43(7) 0.43(7) 0.43(7) 0.00(2) 0.00(2) 0.00(2) F10A 0.62(11) 0.62(11) 0.62(11) 0.00(2) 0.02(2) 0.00(2) F11A 0.33(5) 0.33(5) 0.33(5) 0.00(2) 0.04(2) 0.01(2) F12A 0.165(19) 0.049(11) 0.107(15) -0.008(10) 0.032(15) 0.017(13) P2B 0.106(3) 0.0617(17) 0.097(2) -0.0255(14) 0.0256(19) 0.0003(16) F7B 0.144(6) 0.065(4) 0.125(5) -0.025(3) 0.055(5) -0.017(4) F8B 0.198(8) 0.086(5) 0.119(5) -0.029(4) 0.005(5) 0.035(5) F9B 0.141(6) 0.156(7) 0.184(8) -0.071(6) -0.041(6) 0.040(5) F10B 0.172(8) 0.105(5) 0.130(6) -0.040(5) -0.015(6) -0.021(5) F11B 0.157(6) 0.085(4) 0.116(5) -0.027(4) 0.073(5) -0.004(4) F12B 0.152(8) 0.143(7) 0.183(8) -0.045(6) 0.068(6) 0.021(6) N7 0.143(8) 0.092(6) 0.220(10) 0.039(6) -0.034(7) -0.011(5) C71 0.167(8) 0.131(8) 0.139(8) -0.021(7) -0.016(7) 0.002(7) C72 0.176(11) 0.156(10) 0.156(10) 0.020(8) 0.028(9) -0.027(9) N8 0.190(10) 0.229(12) 0.148(9) 0.072(9) 0.050(8) -0.007(10) C73 0.180(10) 0.192(10) 0.163(9) 0.023(8) 0.021(8) 0.000(8) C74 0.214(14) 0.243(15) 0.237(15) 0.047(13) 0.050(12) 0.026(13) N9 0.164(9) 0.173(10) 0.188(10) 0.046(8) 0.034(8) 0.080(8) C75 0.121(7) 0.136(8) 0.143(8) 0.008(6) 0.003(6) 0.045(6) C76 0.123(8) 0.163(10) 0.157(9) 0.036(8) 0.015(7) 0.057(7) _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 Zn N5 2.032(5) . ? Zn N2 2.045(6) . ? Zn N4 2.196(5) . ? Zn N3 2.206(7) . ? Zn N6 2.211(5) . ? Zn N1 2.255(6) . ? O1 C2 1.374(10) . ? O1 C1 1.417(11) . ? O2 C28 1.414(12) . ? O2 C29 1.446(11) . ? O3 C37 1.381(10) . ? O3 C36 1.424(10) . ? O4 C63 1.374(8) . ? O4 C64 1.418(9) . ? N1 C7 1.317(8) . ? N1 C11 1.335(8) . ? N2 C12 1.312(10) . ? N2 C23 1.364(10) . ? N3 C22 1.334(8) . ? N3 C21 1.344(10) . ? N4 C42 1.323(8) . ? N4 C46 1.351(8) . ? N5 C58 1.335(8) . ? N5 C47 1.339(8) . ? N6 C56 1.306(8) . ? N6 C57 1.343(8) . ? C1 H11 0.9800 . ? C1 H12 0.9800 . ? C1 H13 0.9800 . ? C2 C35 1.345(11) . ? C2 C3 1.404(11) . ? C3 C4 1.382(12) . ? C3 H3 0.9500 . ? C4 C6 1.407(10) . ? C4 C5 1.502(11) . ? C5 H51 0.9800 . ? C5 H52 0.9800 . ? C5 H53 0.9800 . ? C6 C34 1.424(10) . ? C6 C8 1.482(11) . ? C7 C8 1.399(10) . ? C7 H7 0.9500 . ? C8 C9 1.391(10) . ? C9 C10 1.387(12) . ? C9 H9 0.9500 . ? C10 C11 1.397(12) . ? C10 C16B 1.443(6) . ? C10 H10 0.9500 . ? C11 C12 1.465(11) . ? C12 C13 1.433(10) . ? C13 C14 1.352(14) . ? C13 C17B 1.443(6) . ? C13 H131 0.9500 . ? C14 C15 1.397(14) . ? C14 H14 0.9500 . ? C15 C23 1.428(11) . ? C15 C16A 1.443(6) . ? C15 H15 0.9500 . ? C16A C17A 1.331(10) . ? C16A H161 0.9500 . ? C17A C18 1.443(6) . ? C17A H171 0.9500 . ? C16B C17B 1.331(10) . ? C16B H162 0.9500 . ? C17B H172 0.9500 . ? C18 C19 1.397(12) . ? C18 C22 1.436(11) . ? C18 H18 0.9500 . ? C19 C20 1.392(12) . ? C19 H19 0.9500 . ? C20 C21 1.435(10) . ? C20 C24 1.445(11) . ? C21 H21 0.9500 . ? C22 C23 1.402(11) . ? C24 C26 1.351(11) . ? C24 C31 1.434(11) . ? C25 C26 1.530(10) . ? C25 H251 0.9800 . ? C25 H252 0.9800 . ? C25 H253 0.9800 . ? C26 C27 1.385(12) . ? C27 C28 1.463(12) . ? C27 H27 0.9500 . ? C28 C30 1.322(13) . ? C29 H291 0.9800 . ? C29 H292 0.9800 . ? C29 H293 0.9800 . ? C30 C31 1.408(13) . ? C30 H30 0.9500 . ? C31 C32 1.511(13) . ? C32 H321 0.9800 . ? C32 H322 0.9800 . ? C32 H323 0.9800 . ? C33 C34 1.489(11) . ? C33 H331 0.9800 . ? C33 H332 0.9800 . ? C33 H333 0.9800 . ? C34 C35 1.375(11) . ? C35 H35 0.9500 . ? C36 H361 0.9800 . ? C36 H362 0.9800 . ? C36 H363 0.9800 . ? C37 C38 1.364(12) . ? C37 C70 1.385(11) . ? C38 C39 1.404(12) . ? C38 H38 0.9500 . ? C39 C41 1.407(10) . ? C39 C40 1.506(12) . ? C40 H401 0.9800 . ? C40 H402 0.9800 . ? C40 H403 0.9800 . ? C41 C69 1.411(11) . ? C41 C43 1.480(10) . ? C42 C43 1.390(8) . ? C42 H42 0.9500 . ? C43 C44 1.385(10) . ? C44 C45 1.385(10) . ? C44 H44 0.9500 . ? C45 C46 1.382(9) . ? C45 C51B 1.443(6) . ? C45 H45 0.9500 . ? C46 C47 1.466(10) . ? C47 C48 1.405(9) . ? C48 C49 1.362(11) . ? C48 C52B 1.443(6) . ? C48 H48 0.9500 . ? C49 C50 1.385(11) . ? C49 H49 0.9500 . ? C50 C58 1.395(9) . ? C50 C51A 1.442(6) . ? C50 H50 0.9500 . ? C51A C52A 1.331(10) . ? C51A H511 0.9500 . ? C52A C53 1.443(6) . ? C52A H521 0.9500 . ? C51B C52B 1.331(10) . ? C51B H512 0.9500 . ? C52B H522 0.9500 . ? C53 C57 1.389(9) . ? C53 C54 1.412(11) . ? C53 H531 0.9500 . ? C54 C55 1.381(10) . ? C54 H54 0.9500 . ? C55 C56 1.423(8) . ? C55 C59 1.480(9) . ? C56 H56 0.9500 . ? C57 C58 1.440(9) . ? C59 C61 1.405(10) . ? C59 C66 1.413(9) . ? C60 C61 1.512(10) . ? C60 H601 0.9800 . ? C60 H602 0.9800 . ? C60 H603 0.9800 . ? C61 C62 1.400(10) . ? C62 C63 1.384(9) . ? C62 H62 0.9500 . ? C63 C65 1.381(10) . ? C64 H641 0.9800 . ? C64 H642 0.9800 . ? C64 H643 0.9800 . ? C65 C66 1.372(10) . ? C65 H65 0.9500 . ? C66 C67 1.501(10) . ? C67 H671 0.9800 . ? C67 H672 0.9800 . ? C67 H673 0.9800 . ? C68 C69 1.502(11) . ? C68 H681 0.9800 . ? C68 H682 0.9800 . ? C68 H683 0.9800 . ? C69 C70 1.388(11) . ? C70 H70 0.9500 . ? P1A F2A 1.575(3) . ? P1A F3A 1.575(3) . ? P1A F5A 1.576(3) . ? P1A F1A 1.576(3) . ? P1A F6A 1.577(3) . ? P1A F4A 1.577(3) . ? P1B F1B 1.576(3) . ? P1B F6B 1.576(3) . ? P1B F4B 1.576(3) . ? P1B F2B 1.576(3) . ? P1B F5B 1.576(3) . ? P1B F3B 1.577(3) . ? P2A F12A 1.576(3) . ? P2A F8A 1.576(3) . ? P2A F9A 1.576(3) . ? P2A F7A 1.576(3) . ? P2A F10A 1.576(3) . ? P2A F11A 1.576(3) . ? P2B F10B 1.576(3) . ? P2B F12B 1.576(3) . ? P2B F11B 1.576(3) . ? P2B F8B 1.576(3) . ? P2B F7B 1.577(2) . ? P2B F9B 1.577(3) . ? N7 C71 1.137(5) . ? C71 C72 1.452(5) . ? C72 H721 0.9800 . ? C72 H722 0.9800 . ? C72 H723 0.9800 . ? N8 C73 1.145(5) . ? C73 C74 1.451(5) . ? C74 H741 0.9800 . ? C74 H742 0.9800 . ? C74 H743 0.9800 . ? N9 C75 1.141(5) . ? C75 C76 1.455(5) . ? C76 H761 0.9800 . ? C76 H762 0.9800 . ? C76 H763 0.9800 . ? 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 Zn N2 171.3(3) . . ? N5 Zn N4 76.3(2) . . ? N2 Zn N4 104.0(2) . . ? N5 Zn N3 110.9(2) . . ? N2 Zn N3 77.7(3) . . ? N4 Zn N3 99.7(2) . . ? N5 Zn N6 76.7(2) . . ? N2 Zn N6 103.0(2) . . ? N4 Zn N6 152.9(2) . . ? N3 Zn N6 88.0(2) . . ? N5 Zn N1 96.3(2) . . ? N2 Zn N1 75.1(3) . . ? N4 Zn N1 86.48(19) . . ? N3 Zn N1 152.8(2) . . ? N6 Zn N1 98.6(2) . . ? C2 O1 C1 118.7(7) . . ? C28 O2 C29 113.7(8) . . ? C37 O3 C36 117.6(8) . . ? C63 O4 C64 117.7(5) . . ? C7 N1 C11 120.6(7) . . ? C7 N1 Zn 126.7(4) . . ? C11 N1 Zn 111.8(5) . . ? C12 N2 C23 124.7(7) . . ? C12 N2 Zn 120.6(5) . . ? C23 N2 Zn 114.6(6) . . ? C22 N3 C21 118.5(7) . . ? C22 N3 Zn 110.9(6) . . ? C21 N3 Zn 130.1(4) . . ? C42 N4 C46 118.9(5) . . ? C42 N4 Zn 126.7(4) . . ? C46 N4 Zn 113.0(4) . . ? C58 N5 C47 121.6(6) . . ? C58 N5 Zn 118.5(4) . . ? C47 N5 Zn 119.5(4) . . ? C56 N6 C57 119.1(6) . . ? C56 N6 Zn 129.2(4) . . ? C57 N6 Zn 111.4(4) . . ? O1 C1 H11 109.5 . . ? O1 C1 H12 109.5 . . ? H11 C1 H12 109.5 . . ? O1 C1 H13 109.5 . . ? H11 C1 H13 109.5 . . ? H12 C1 H13 109.5 . . ? C35 C2 O1 116.8(8) . . ? C35 C2 C3 119.2(9) . . ? O1 C2 C3 124.0(8) . . ? C4 C3 C2 120.7(8) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C3 C4 C6 119.7(7) . . ? C3 C4 C5 118.8(8) . . ? C6 C4 C5 121.5(8) . . ? C4 C5 H51 109.5 . . ? C4 C5 H52 109.5 . . ? H51 C5 H52 109.5 . . ? C4 C5 H53 109.5 . . ? H51 C5 H53 109.5 . . ? H52 C5 H53 109.5 . . ? C4 C6 C34 118.6(8) . . ? C4 C6 C8 120.7(6) . . ? C34 C6 C8 120.7(7) . . ? N1 C7 C8 125.1(6) . . ? N1 C7 H7 117.4 . . ? C8 C7 H7 117.4 . . ? C9 C8 C7 114.3(8) . . ? C9 C8 C6 124.3(7) . . ? C7 C8 C6 121.3(6) . . ? C10 C9 C8 121.0(8) . . ? C10 C9 H9 119.5 . . ? C8 C9 H9 119.5 . . ? C9 C10 C11 119.9(7) . . ? C9 C10 C16B 135(2) . . ? C11 C10 C16B 105(2) . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? N1 C11 C10 119.0(8) . . ? N1 C11 C12 116.2(7) . . ? C10 C11 C12 124.9(7) . . ? N2 C12 C13 119.3(9) . . ? N2 C12 C11 115.6(6) . . ? C13 C12 C11 125.1(9) . . ? C14 C13 C12 116.8(10) . . ? C14 C13 C17B 133.4(18) . . ? C12 C13 C17B 108.0(19) . . ? C14 C13 H131 121.6 . . ? C12 C13 H131 121.6 . . ? C13 C14 C15 124.8(8) . . ? C13 C14 H14 117.6 . . ? C15 C14 H14 117.6 . . ? C14 C15 C23 115.7(8) . . ? C14 C15 C16A 130.5(9) . . ? C23 C15 C16A 113.8(9) . . ? C14 C15 H15 122.2 . . ? C23 C15 H15 122.2 . . ? C17A C16A C15 124.2(10) . . ? C17A C16A H161 117.9 . . ? C15 C16A H161 117.9 . . ? C16A C17A C18 122.6(10) . . ? C16A C17A H171 118.7 . . ? C18 C17A H171 118.7 . . ? C17B C16B C10 134(4) . . ? C17B C16B H162 113.1 . . ? C10 C16B H162 113.1 . . ? C16B C17B C13 121(4) . . ? C16B C17B H172 119.5 . . ? C13 C17B H172 119.5 . . ? C19 C18 C22 117.3(7) . . ? C19 C18 C17A 127.6(9) . . ? C22 C18 C17A 115.1(10) . . ? C19 C18 H18 121.4 . . ? C22 C18 H18 121.4 . . ? C20 C19 C18 123.6(8) . . ? C20 C19 H19 118.2 . . ? C18 C19 H19 118.2 . . ? C19 C20 C21 112.8(9) . . ? C19 C20 C24 124.7(7) . . ? C21 C20 C24 122.4(7) . . ? N3 C21 C20 126.2(7) . . ? N3 C21 H21 116.9 . . ? C20 C21 H21 116.9 . . ? N3 C22 C23 117.3(7) . . ? N3 C22 C18 121.5(8) . . ? C23 C22 C18 121.2(7) . . ? N2 C23 C22 118.6(6) . . ? N2 C23 C15 118.5(9) . . ? C22 C23 C15 122.9(8) . . ? C26 C24 C31 120.2(9) . . ? C26 C24 C20 120.9(8) . . ? C31 C24 C20 118.9(8) . . ? C26 C25 H251 109.5 . . ? C26 C25 H252 109.5 . . ? H251 C25 H252 109.5 . . ? C26 C25 H253 109.5 . . ? H251 C25 H253 109.5 . . ? H252 C25 H253 109.5 . . ? C24 C26 C27 120.2(8) . . ? C24 C26 C25 122.5(9) . . ? C27 C26 C25 117.2(8) . . ? C26 C27 C28 121.8(9) . . ? C26 C27 H27 119.1 . . ? C28 C27 H27 119.1 . . ? C30 C28 O2 133.2(10) . . ? C30 C28 C27 115.0(10) . . ? O2 C28 C27 111.6(9) . . ? O2 C29 H291 109.5 . . ? O2 C29 H292 109.5 . . ? H291 C29 H292 109.5 . . ? O2 C29 H293 109.5 . . ? H291 C29 H293 109.5 . . ? H292 C29 H293 109.5 . . ? C28 C30 C31 125.7(9) . . ? C28 C30 H30 117.1 . . ? C31 C30 H30 117.1 . . ? C30 C31 C24 116.9(8) . . ? C30 C31 C32 124.0(8) . . ? C24 C31 C32 119.1(10) . . ? C31 C32 H321 109.5 . . ? C31 C32 H322 109.5 . . ? H321 C32 H322 109.5 . . ? C31 C32 H323 109.5 . . ? H321 C32 H323 109.5 . . ? H322 C32 H323 109.5 . . ? C34 C33 H331 109.5 . . ? C34 C33 H332 109.5 . . ? H331 C33 H332 109.5 . . ? C34 C33 H333 109.5 . . ? H331 C33 H333 109.5 . . ? H332 C33 H333 109.5 . . ? C35 C34 C6 119.0(7) . . ? C35 C34 C33 120.4(7) . . ? C6 C34 C33 120.6(8) . . ? C2 C35 C34 122.8(8) . . ? C2 C35 H35 118.6 . . ? C34 C35 H35 118.6 . . ? O3 C36 H361 109.5 . . ? O3 C36 H362 109.5 . . ? H361 C36 H362 109.5 . . ? O3 C36 H363 109.5 . . ? H361 C36 H363 109.5 . . ? H362 C36 H363 109.5 . . ? C38 C37 O3 124.9(8) . . ? C38 C37 C70 119.8(8) . . ? O3 C37 C70 115.3(9) . . ? C37 C38 C39 121.5(8) . . ? C37 C38 H38 119.2 . . ? C39 C38 H38 119.2 . . ? C38 C39 C41 119.0(8) . . ? C38 C39 C40 119.1(7) . . ? C41 C39 C40 121.9(8) . . ? C39 C40 H401 109.5 . . ? C39 C40 H402 109.5 . . ? H401 C40 H402 109.5 . . ? C39 C40 H403 109.5 . . ? H401 C40 H403 109.5 . . ? H402 C40 H403 109.5 . . ? C39 C41 C69 119.0(7) . . ? C39 C41 C43 121.7(7) . . ? C69 C41 C43 119.3(6) . . ? N4 C42 C43 124.3(6) . . ? N4 C42 H42 117.8 . . ? C43 C42 H42 117.8 . . ? C44 C43 C42 116.1(7) . . ? C44 C43 C41 122.3(6) . . ? C42 C43 C41 121.5(7) . . ? C43 C44 C45 120.6(6) . . ? C43 C44 H44 119.7 . . ? C45 C44 H44 119.7 . . ? C46 C45 C44 119.0(6) . . ? C46 C45 C51B 101.7(14) . . ? C44 C45 C51B 139.1(13) . . ? C46 C45 H45 120.5 . . ? C44 C45 H45 120.5 . . ? N4 C46 C45 121.0(7) . . ? N4 C46 C47 115.6(5) . . ? C45 C46 C47 123.3(6) . . ? N5 C47 C48 119.7(7) . . ? N5 C47 C46 115.0(5) . . ? C48 C47 C46 125.3(6) . . ? C49 C48 C47 119.3(7) . . ? C49 C48 C52B 125.1(10) . . ? C47 C48 C52B 115.3(10) . . ? C49 C48 H48 120.3 . . ? C47 C48 H48 120.3 . . ? C48 C49 C50 120.4(7) . . ? C48 C49 H49 119.8 . . ? C50 C49 H49 119.8 . . ? C49 C50 C58 118.3(7) . . ? C49 C50 C51A 126.7(7) . . ? C58 C50 C51A 115.0(7) . . ? C49 C50 H50 120.9 . . ? C58 C50 H50 120.9 . . ? C52A C51A C50 120.5(9) . . ? C52A C51A H511 119.8 . . ? C50 C51A H511 119.8 . . ? C51A C52A C53 126.3(9) . . ? C51A C52A H521 116.9 . . ? C53 C52A H521 116.9 . . ? C52B C51B C45 145(2) . . ? C52B C51B H512 107.6 . . ? C45 C51B H512 107.6 . . ? C51B C52B C48 109(2) . . ? C51B C52B H522 125.3 . . ? C48 C52B H522 125.3 . . ? C57 C53 C54 117.3(6) . . ? C57 C53 C52A 114.0(7) . . ? C54 C53 C52A 128.4(7) . . ? C57 C53 H531 121.3 . . ? C54 C53 H531 121.3 . . ? C55 C54 C53 121.1(6) . . ? C55 C54 H54 119.5 . . ? C53 C54 H54 119.5 . . ? C54 C55 C56 115.5(6) . . ? C54 C55 C59 125.9(6) . . ? C56 C55 C59 118.6(6) . . ? N6 C56 C55 124.4(6) . . ? N6 C56 H56 117.8 . . ? C55 C56 H56 117.8 . . ? N6 C57 C53 122.5(6) . . ? N6 C57 C58 117.0(6) . . ? C53 C57 C58 120.4(6) . . ? N5 C58 C50 120.7(6) . . ? N5 C58 C57 115.8(5) . . ? C50 C58 C57 123.4(7) . . ? C61 C59 C66 118.4(6) . . ? C61 C59 C55 119.9(6) . . ? C66 C59 C55 121.7(6) . . ? C61 C60 H601 109.5 . . ? C61 C60 H602 109.5 . . ? H601 C60 H602 109.5 . . ? C61 C60 H603 109.5 . . ? H601 C60 H603 109.5 . . ? H602 C60 H603 109.5 . . ? C62 C61 C59 120.2(6) . . ? C62 C61 C60 117.2(7) . . ? C59 C61 C60 122.6(7) . . ? C63 C62 C61 120.0(7) . . ? C63 C62 H62 120.0 . . ? C61 C62 H62 120.0 . . ? O4 C63 C65 116.4(6) . . ? O4 C63 C62 123.7(7) . . ? C65 C63 C62 120.0(7) . . ? O4 C64 H641 109.5 . . ? O4 C64 H642 109.5 . . ? H641 C64 H642 109.5 . . ? O4 C64 H643 109.5 . . ? H641 C64 H643 109.5 . . ? H642 C64 H643 109.5 . . ? C66 C65 C63 121.1(7) . . ? C66 C65 H65 119.5 . . ? C63 C65 H65 119.5 . . ? C65 C66 C59 120.3(7) . . ? C65 C66 C67 117.8(7) . . ? C59 C66 C67 121.8(7) . . ? C66 C67 H671 109.5 . . ? C66 C67 H672 109.5 . . ? H671 C67 H672 109.5 . . ? C66 C67 H673 109.5 . . ? H671 C67 H673 109.5 . . ? H672 C67 H673 109.5 . . ? C69 C68 H681 109.5 . . ? C69 C68 H682 109.5 . . ? H681 C68 H682 109.5 . . ? C69 C68 H683 109.5 . . ? H681 C68 H683 109.5 . . ? H682 C68 H683 109.5 . . ? C70 C69 C41 119.9(7) . . ? C70 C69 C68 118.2(8) . . ? C41 C69 C68 121.9(7) . . ? C37 C70 C69 120.7(8) . . ? C37 C70 H70 119.6 . . ? C69 C70 H70 119.6 . . ? F2A P1A F3A 90.6(3) . . ? F2A P1A F5A 90.1(3) . . ? F3A P1A F5A 90.0(3) . . ? F2A P1A F1A 179.3(3) . . ? F3A P1A F1A 90.0(3) . . ? F5A P1A F1A 90.1(3) . . ? F2A P1A F6A 90.5(3) . . ? F3A P1A F6A 89.5(3) . . ? F5A P1A F6A 179.3(3) . . ? F1A P1A F6A 89.3(3) . . ? F2A P1A F4A 89.6(3) . . ? F3A P1A F4A 179.7(4) . . ? F5A P1A F4A 89.8(3) . . ? F1A P1A F4A 89.7(3) . . ? F6A P1A F4A 90.6(3) . . ? F1B P1B F6B 89.9(3) . . ? F1B P1B F4B 90.0(3) . . ? F6B P1B F4B 90.2(3) . . ? F1B P1B F2B 179.9(5) . . ? F6B P1B F2B 90.0(3) . . ? F4B P1B F2B 90.1(3) . . ? F1B P1B F5B 90.1(3) . . ? F6B P1B F5B 180.0(4) . . ? F4B P1B F5B 89.8(3) . . ? F2B P1B F5B 89.9(3) . . ? F1B P1B F3B 90.0(3) . . ? F6B P1B F3B 90.1(3) . . ? F4B P1B F3B 179.7(4) . . ? F2B P1B F3B 89.8(3) . . ? F5B P1B F3B 89.9(3) . . ? F12A P2A F8A 90.0(3) . . ? F12A P2A F9A 90.1(3) . . ? F8A P2A F9A 90.0(3) . . ? F12A P2A F7A 90.0(3) . . ? F8A P2A F7A 179.9(5) . . ? F9A P2A F7A 90.1(3) . . ? F12A P2A F10A 90.0(3) . . ? F8A P2A F10A 90.0(3) . . ? F9A P2A F10A 180.0(5) . . ? F7A P2A F10A 89.9(3) . . ? F12A P2A F11A 179.9(5) . . ? F8A P2A F11A 90.0(3) . . ? F9A P2A F11A 90.0(3) . . ? F7A P2A F11A 90.1(3) . . ? F10A P2A F11A 90.0(3) . . ? F10B P2B F12B 89.6(3) . . ? F10B P2B F11B 91.2(3) . . ? F12B P2B F11B 179.3(3) . . ? F10B P2B F8B 90.6(3) . . ? F12B P2B F8B 89.7(3) . . ? F11B P2B F8B 90.2(3) . . ? F10B P2B F7B 90.3(3) . . ? F12B P2B F7B 89.9(3) . . ? F11B P2B F7B 90.1(3) . . ? F8B P2B F7B 179.0(3) . . ? F10B P2B F9B 179.1(3) . . ? F12B P2B F9B 89.9(3) . . ? F11B P2B F9B 89.3(3) . . ? F8B P2B F9B 90.2(3) . . ? F7B P2B F9B 89.0(3) . . ? N7 C71 C72 171.2(15) . . ? C71 C72 H721 109.5 . . ? C71 C72 H722 109.5 . . ? H721 C72 H722 109.5 . . ? C71 C72 H723 109.5 . . ? H721 C72 H723 109.5 . . ? H722 C72 H723 109.5 . . ? N8 C73 C74 172(2) . . ? C73 C74 H741 109.5 . . ? C73 C74 H742 109.5 . . ? H741 C74 H742 109.5 . . ? C73 C74 H743 109.5 . . ? H741 C74 H743 109.5 . . ? H742 C74 H743 109.5 . . ? N9 C75 C76 176.5(17) . . ? C75 C76 H761 109.5 . . ? C75 C76 H762 109.5 . . ? H761 C76 H762 109.5 . . ? C75 C76 H763 109.5 . . ? H761 C76 H763 109.5 . . ? H762 C76 H763 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 N5 Zn N1 C7 -5.2(5) . . . . ? N2 Zn N1 C7 176.1(5) . . . . ? N4 Zn N1 C7 70.6(5) . . . . ? N3 Zn N1 C7 174.9(5) . . . . ? N6 Zn N1 C7 -82.7(5) . . . . ? N5 Zn N1 C11 -174.2(4) . . . . ? N2 Zn N1 C11 7.0(4) . . . . ? N4 Zn N1 C11 -98.5(4) . . . . ? N3 Zn N1 C11 5.9(6) . . . . ? N6 Zn N1 C11 108.3(4) . . . . ? N4 Zn N2 C12 79.9(5) . . . . ? N3 Zn N2 C12 176.9(5) . . . . ? N6 Zn N2 C12 -98.1(5) . . . . ? N1 Zn N2 C12 -2.5(5) . . . . ? N4 Zn N2 C23 -103.5(4) . . . . ? N3 Zn N2 C23 -6.5(4) . . . . ? N6 Zn N2 C23 78.4(5) . . . . ? N1 Zn N2 C23 174.0(5) . . . . ? N5 Zn N3 C22 -170.2(4) . . . . ? N2 Zn N3 C22 8.5(4) . . . . ? N4 Zn N3 C22 110.9(4) . . . . ? N6 Zn N3 C22 -95.3(4) . . . . ? N1 Zn N3 C22 9.6(7) . . . . ? N5 Zn N3 C21 1.3(6) . . . . ? N2 Zn N3 C21 -179.9(6) . . . . ? N4 Zn N3 C21 -77.6(6) . . . . ? N6 Zn N3 C21 76.3(6) . . . . ? N1 Zn N3 C21 -178.8(5) . . . . ? N5 Zn N4 C42 173.9(6) . . . . ? N2 Zn N4 C42 2.8(7) . . . . ? N3 Zn N4 C42 -76.8(6) . . . . ? N6 Zn N4 C42 178.6(5) . . . . ? N1 Zn N4 C42 76.5(6) . . . . ? N5 Zn N4 C46 7.6(5) . . . . ? N2 Zn N4 C46 -163.5(5) . . . . ? N3 Zn N4 C46 116.9(5) . . . . ? N6 Zn N4 C46 12.3(8) . . . . ? N1 Zn N4 C46 -89.8(5) . . . . ? N4 Zn N5 C58 -179.5(5) . . . . ? N3 Zn N5 C58 85.2(5) . . . . ? N6 Zn N5 C58 2.7(5) . . . . ? N1 Zn N5 C58 -94.7(5) . . . . ? N4 Zn N5 C47 -6.9(5) . . . . ? N3 Zn N5 C47 -102.2(5) . . . . ? N6 Zn N5 C47 175.3(5) . . . . ? N1 Zn N5 C47 77.9(5) . . . . ? N5 Zn N6 C56 175.8(7) . . . . ? N2 Zn N6 C56 -13.1(7) . . . . ? N4 Zn N6 C56 171.1(6) . . . . ? N3 Zn N6 C56 63.7(6) . . . . ? N1 Zn N6 C56 -89.7(6) . . . . ? N5 Zn N6 C57 1.9(5) . . . . ? N2 Zn N6 C57 172.9(5) . . . . ? N4 Zn N6 C57 -2.8(8) . . . . ? N3 Zn N6 C57 -110.2(5) . . . . ? N1 Zn N6 C57 96.3(5) . . . . ? C1 O1 C2 C35 170.6(8) . . . . ? C1 O1 C2 C3 -10.4(12) . . . . ? C35 C2 C3 C4 0.3(11) . . . . ? O1 C2 C3 C4 -178.7(7) . . . . ? C2 C3 C4 C6 -0.4(11) . . . . ? C2 C3 C4 C5 -178.9(7) . . . . ? C3 C4 C6 C34 -0.4(10) . . . . ? C5 C4 C6 C34 178.1(7) . . . . ? C3 C4 C6 C8 -178.8(6) . . . . ? C5 C4 C6 C8 -0.4(10) . . . . ? C11 N1 C7 C8 1.8(9) . . . . ? Zn N1 C7 C8 -166.3(5) . . . . ? N1 C7 C8 C9 -1.9(9) . . . . ? N1 C7 C8 C6 175.5(6) . . . . ? C4 C6 C8 C9 -62.7(9) . . . . ? C34 C6 C8 C9 118.8(8) . . . . ? C4 C6 C8 C7 120.1(7) . . . . ? C34 C6 C8 C7 -58.3(9) . . . . ? C7 C8 C9 C10 -0.2(10) . . . . ? C6 C8 C9 C10 -177.6(7) . . . . ? C8 C9 C10 C11 2.4(11) . . . . ? C8 C9 C10 C16B 176(4) . . . . ? C7 N1 C11 C10 0.5(9) . . . . ? Zn N1 C11 C10 170.3(5) . . . . ? C7 N1 C11 C12 179.8(5) . . . . ? Zn N1 C11 C12 -10.4(6) . . . . ? C9 C10 C11 N1 -2.6(10) . . . . ? C16B C10 C11 N1 -178(3) . . . . ? C9 C10 C11 C12 178.2(6) . . . . ? C16B C10 C11 C12 3(3) . . . . ? C23 N2 C12 C13 4.0(10) . . . . ? Zn N2 C12 C13 -179.8(5) . . . . ? C23 N2 C12 C11 -178.3(5) . . . . ? Zn N2 C12 C11 -2.1(8) . . . . ? N1 C11 C12 N2 8.8(8) . . . . ? C10 C11 C12 N2 -171.9(6) . . . . ? N1 C11 C12 C13 -173.6(6) . . . . ? C10 C11 C12 C13 5.6(10) . . . . ? N2 C12 C13 C14 -4.6(11) . . . . ? C11 C12 C13 C14 177.9(7) . . . . ? N2 C12 C13 C17B 162(2) . . . . ? C11 C12 C13 C17B -15(2) . . . . ? C12 C13 C14 C15 1.3(13) . . . . ? C17B C13 C14 C15 -161(3) . . . . ? C13 C14 C15 C23 2.7(14) . . . . ? C13 C14 C15 C16A -177.4(10) . . . . ? C14 C15 C16A C17A 179.8(11) . . . . ? C23 C15 C16A C17A -0.3(15) . . . . ? C15 C16A C17A C18 3.9(18) . . . . ? C9 C10 C16B C17B -174(5) . . . . ? C11 C10 C16B C17B 0(8) . . . . ? C10 C16B C17B C13 -11(10) . . . . ? C14 C13 C17B C16B -179(4) . . . . ? C12 C13 C17B C16B 17(5) . . . . ? C16A C17A C18 C19 176.2(10) . . . . ? C16A C17A C18 C22 -3.6(15) . . . . ? C22 C18 C19 C20 1.4(12) . . . . ? C17A C18 C19 C20 -178.4(8) . . . . ? C18 C19 C20 C21 -0.3(11) . . . . ? C18 C19 C20 C24 175.5(8) . . . . ? C22 N3 C21 C20 2.7(10) . . . . ? Zn N3 C21 C20 -168.4(5) . . . . ? C19 C20 C21 N3 -1.7(10) . . . . ? C24 C20 C21 N3 -177.7(7) . . . . ? C21 N3 C22 C23 178.1(6) . . . . ? Zn N3 C22 C23 -9.2(7) . . . . ? C21 N3 C22 C18 -1.4(10) . . . . ? Zn N3 C22 C18 171.2(5) . . . . ? C19 C18 C22 N3 -0.5(11) . . . . ? C17A C18 C22 N3 179.4(7) . . . . ? C19 C18 C22 C23 -180.0(7) . . . . ? C17A C18 C22 C23 -0.2(11) . . . . ? C12 N2 C23 C22 -179.7(6) . . . . ? Zn N2 C23 C22 3.9(7) . . . . ? C12 N2 C23 C15 0.2(10) . . . . ? Zn N2 C23 C15 -176.2(5) . . . . ? N3 C22 C23 N2 4.1(9) . . . . ? C18 C22 C23 N2 -176.3(6) . . . . ? N3 C22 C23 C15 -175.8(6) . . . . ? C18 C22 C23 C15 3.7(11) . . . . ? C14 C15 C23 N2 -3.5(11) . . . . ? C16A C15 C23 N2 176.6(7) . . . . ? C14 C15 C23 C22 176.4(7) . . . . ? C16A C15 C23 C22 -3.5(11) . . . . ? C19 C20 C24 C26 -56.4(10) . . . . ? C21 C20 C24 C26 119.1(8) . . . . ? C19 C20 C24 C31 124.6(8) . . . . ? C21 C20 C24 C31 -59.8(10) . . . . ? C31 C24 C26 C27 0.6(11) . . . . ? C20 C24 C26 C27 -178.3(6) . . . . ? C31 C24 C26 C25 177.1(7) . . . . ? C20 C24 C26 C25 -1.8(11) . . . . ? C24 C26 C27 C28 -1.4(11) . . . . ? C25 C26 C27 C28 -178.1(7) . . . . ? C29 O2 C28 C30 -3.3(13) . . . . ? C29 O2 C28 C27 -178.1(7) . . . . ? C26 C27 C28 C30 2.9(11) . . . . ? C26 C27 C28 O2 178.7(7) . . . . ? O2 C28 C30 C31 -178.5(8) . . . . ? C27 C28 C30 C31 -3.8(12) . . . . ? C28 C30 C31 C24 3.1(12) . . . . ? C28 C30 C31 C32 -177.0(9) . . . . ? C26 C24 C31 C30 -1.3(11) . . . . ? C20 C24 C31 C30 177.7(7) . . . . ? C26 C24 C31 C32 178.8(8) . . . . ? C20 C24 C31 C32 -2.2(11) . . . . ? C4 C6 C34 C35 1.3(10) . . . . ? C8 C6 C34 C35 179.8(7) . . . . ? C4 C6 C34 C33 -177.3(7) . . . . ? C8 C6 C34 C33 1.2(11) . . . . ? O1 C2 C35 C34 179.8(7) . . . . ? C3 C2 C35 C34 0.7(12) . . . . ? C6 C34 C35 C2 -1.5(12) . . . . ? C33 C34 C35 C2 177.1(8) . . . . ? C36 O3 C37 C38 -7.0(13) . . . . ? C36 O3 C37 C70 174.5(8) . . . . ? O3 C37 C38 C39 -178.8(7) . . . . ? C70 C37 C38 C39 -0.4(13) . . . . ? C37 C38 C39 C41 1.0(11) . . . . ? C37 C38 C39 C40 -178.9(8) . . . . ? C38 C39 C41 C69 -0.9(10) . . . . ? C40 C39 C41 C69 179.1(8) . . . . ? C38 C39 C41 C43 178.6(6) . . . . ? C40 C39 C41 C43 -1.5(11) . . . . ? C46 N4 C42 C43 1.4(11) . . . . ? Zn N4 C42 C43 -164.2(5) . . . . ? N4 C42 C43 C44 -2.8(11) . . . . ? N4 C42 C43 C41 173.9(7) . . . . ? C39 C41 C43 C44 -65.7(10) . . . . ? C69 C41 C43 C44 113.7(8) . . . . ? C39 C41 C43 C42 117.9(8) . . . . ? C69 C41 C43 C42 -62.7(10) . . . . ? C42 C43 C44 C45 1.3(10) . . . . ? C41 C43 C44 C45 -175.3(7) . . . . ? C43 C44 C45 C46 1.3(11) . . . . ? C43 C44 C45 C51B 175(2) . . . . ? C42 N4 C46 C45 1.5(10) . . . . ? Zn N4 C46 C45 168.9(5) . . . . ? C42 N4 C46 C47 -174.8(6) . . . . ? Zn N4 C46 C47 -7.3(7) . . . . ? C44 C45 C46 N4 -2.8(10) . . . . ? C51B C45 C46 N4 -178.4(13) . . . . ? C44 C45 C46 C47 173.2(7) . . . . ? C51B C45 C46 C47 -2.4(15) . . . . ? C58 N5 C47 C48 0.0(10) . . . . ? Zn N5 C47 C48 -172.4(5) . . . . ? C58 N5 C47 C46 177.6(6) . . . . ? Zn N5 C47 C46 5.2(8) . . . . ? N4 C46 C47 N5 2.0(9) . . . . ? C45 C46 C47 N5 -174.2(6) . . . . ? N4 C46 C47 C48 179.4(7) . . . . ? C45 C46 C47 C48 3.2(11) . . . . ? N5 C47 C48 C49 -0.5(11) . . . . ? C46 C47 C48 C49 -177.8(7) . . . . ? N5 C47 C48 C52B 173.5(13) . . . . ? C46 C47 C48 C52B -3.8(16) . . . . ? C47 C48 C49 C50 -0.7(12) . . . . ? C52B C48 C49 C50 -174.0(14) . . . . ? C48 C49 C50 C58 2.3(12) . . . . ? C48 C49 C50 C51A -176.2(9) . . . . ? C49 C50 C51A C52A 177.2(10) . . . . ? C58 C50 C51A C52A -1.3(15) . . . . ? C50 C51A C52A C53 2.1(18) . . . . ? C46 C45 C51B C52B 5(5) . . . . ? C44 C45 C51B C52B -169(3) . . . . ? C45 C51B C52B C48 -6(6) . . . . ? C49 C48 C52B C51B 177.7(18) . . . . ? C47 C48 C52B C51B 4(3) . . . . ? C51A C52A C53 C57 1.9(16) . . . . ? C51A C52A C53 C54 175.2(10) . . . . ? C57 C53 C54 C55 0.3(11) . . . . ? C52A C53 C54 C55 -172.8(9) . . . . ? C53 C54 C55 C56 0.7(11) . . . . ? C53 C54 C55 C59 179.2(7) . . . . ? C57 N6 C56 C55 1.7(11) . . . . ? Zn N6 C56 C55 -171.9(5) . . . . ? C54 C55 C56 N6 -1.7(11) . . . . ? C59 C55 C56 N6 179.6(7) . . . . ? C56 N6 C57 C53 -0.5(11) . . . . ? Zn N6 C57 C53 174.1(6) . . . . ? C56 N6 C57 C58 179.5(6) . . . . ? Zn N6 C57 C58 -5.8(8) . . . . ? C54 C53 C57 N6 -0.4(11) . . . . ? C52A C53 C57 N6 173.6(8) . . . . ? C54 C53 C57 C58 179.5(7) . . . . ? C52A C53 C57 C58 -6.4(11) . . . . ? C47 N5 C58 C50 1.7(10) . . . . ? Zn N5 C58 C50 174.1(5) . . . . ? C47 N5 C58 C57 -179.1(6) . . . . ? Zn N5 C58 C57 -6.6(8) . . . . ? C49 C50 C58 N5 -2.8(11) . . . . ? C51A C50 C58 N5 175.8(8) . . . . ? C49 C50 C58 C57 178.0(7) . . . . ? C51A C50 C58 C57 -3.3(12) . . . . ? N6 C57 C58 N5 8.3(9) . . . . ? C53 C57 C58 N5 -171.6(7) . . . . ? N6 C57 C58 C50 -172.5(7) . . . . ? C53 C57 C58 C50 7.6(11) . . . . ? C54 C55 C59 C61 126.8(8) . . . . ? C56 C55 C59 C61 -54.6(9) . . . . ? C54 C55 C59 C66 -54.9(10) . . . . ? C56 C55 C59 C66 123.7(7) . . . . ? C66 C59 C61 C62 -1.3(10) . . . . ? C55 C59 C61 C62 177.1(6) . . . . ? C66 C59 C61 C60 175.8(8) . . . . ? C55 C59 C61 C60 -5.8(11) . . . . ? C59 C61 C62 C63 1.0(11) . . . . ? C60 C61 C62 C63 -176.3(8) . . . . ? C64 O4 C63 C65 -176.7(7) . . . . ? C64 O4 C63 C62 4.3(10) . . . . ? C61 C62 C63 O4 178.8(7) . . . . ? C61 C62 C63 C65 -0.2(11) . . . . ? O4 C63 C65 C66 -179.3(6) . . . . ? C62 C63 C65 C66 -0.2(11) . . . . ? C63 C65 C66 C59 -0.1(11) . . . . ? C63 C65 C66 C67 -178.5(7) . . . . ? C61 C59 C66 C65 0.9(10) . . . . ? C55 C59 C66 C65 -177.4(6) . . . . ? C61 C59 C66 C67 179.2(7) . . . . ? C55 C59 C66 C67 0.9(10) . . . . ? C39 C41 C69 C70 0.2(11) . . . . ? C43 C41 C69 C70 -179.3(7) . . . . ? C39 C41 C69 C68 178.7(8) . . . . ? C43 C41 C69 C68 -0.8(12) . . . . ? C38 C37 C70 C69 -0.4(13) . . . . ? O3 C37 C70 C69 178.2(8) . . . . ? C41 C69 C70 C37 0.5(13) . . . . ? C68 C69 C70 C37 -178.1(9) . . . . ? #===END data_8a _database_code_depnum_ccdc_archive 'CCDC 735254' # SG0320 _audit_creation_method SHELXL-97 _audit_creation_date 03-10-03 _chemical_name_systematic ; bis{8-(4-methoxy-2,6-dimethylphenyl)-2-[5-(4-methoxy-2,6- dimethylphenyl)-pyridin-2-yl]-1,10-phenanthroline}ruthenium(II) hexafluorophosphate di-acetonitrile solvate ; _chemical_name_common ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_moiety 'C70 H62 N6 O4 Ru 2+, 2(F6 P 1-), 2(C2 H3 N)' _chemical_formula_sum 'C74 H68 F12 N8 O4 P2 Ru' _chemical_formula_weight 1524.33 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 296 0.0033 0.0016 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; H H 272 0.0000 0.0000 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; F F 48 0.0171 0.0103 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; N N 32 0.0061 0.0033 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; O O 16 0.0106 0.0060 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; P P 8 0.1023 0.0942 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; Ru Ru 4 -1.2594 0.8363 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c c a ' _symmetry_space_group_name_Hall ? _symmetry_Int_Tables_number 54 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' 'x+1/2, -y, -z+1/2' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' '-x-1/2, y, z-1/2' 'x, -y, z-1/2' _cell_length_a 25.3777(5) _cell_length_b 12.5601(3) _cell_length_c 21.8678(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6970.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 160(1) _cell_measurement_reflns_used 140159 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.452 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3128 _exptl_absorpt_coefficient_mu 0.359 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Blessing, 1995)' _exptl_absorpt_correction_T_min 0.613 _exptl_absorpt_correction_T_max 0.993 _exptl_special_details ; Solvent used: acetonitrile / diethylether Cooling Device: Oxford Cryosystems Cryostream 700 Crystal mount: glued on a glass fibre Mosaicity (deg.): 0.794(1) Frames collected: 578 Seconds exposure per frame: 96 Degrees rotation per frame: 0.8 Crystal-Detector distance (mm): 38.0 ; _diffrn_ambient_temperature 160(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Nonius FR590 sealed tube generator' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_detector '65 mm CCD camera on \k goniostat' _diffrn_measurement_device_type 'Nonius KappaCCD area-detector diffractometer' _diffrn_measurement_method '\f and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 78747 _diffrn_reflns_av_R_equivalents 0.1419 _diffrn_reflns_av_sigmaI/netI 0.0558 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 25.04 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.998 _reflns_number_total 6150 _reflns_number_gt 4026 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'COLLECT (Nonius, 2000)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN and SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'SHELXL97 and PLATON (Spek, 2009)' _refine_special_details ; The asymmetric unit contains one half of a cation with the Ru-atom on a two-fold axis, one anion and two closely adjacent sites in general positions which represent two equally occupied disordered positions for an acetonitrile molecule. In the cation, the two central CH groups of the phenanthroline moiety are disordered over two sites which effectively complete six-membered rings between all pyridine rings, thereby indicating that the ligand must be disordered through a 180\% rotation about the central N-atom. The site occupation factor for the major conformation refined to 0.75(1). The PF6- anion is highly disordered. Three sets of P- and F-atoms were defined for this anion and refinement of the site occupation factors of each set led to values of 0.615(4), 0.174(8) and 0.211(8). The P-F and F...F distances were restrained tightly, so as to maintain octahedral geometry and uniform P-F bond lengths and the atomic displacement parameters of the P- and F-atoms were given light pseudo-isotropic restraints. The bond lengths within the disordered MeCN molecule were also restrained to logical values. Validation reports some short contacts as A alerts. These are mostly between different disordered components of anions and cations where the sums of the SOF of the relevant atoms is < 1.0, so that one can conceive that the "conflicting" sites are never occupied simultanously for adjacent moieties. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0950P)^2^+12.6316P] 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_extinction_coef ? _refine_ls_number_reflns 6149 _refine_ls_number_parameters 639 _refine_ls_number_restraints 944 _refine_ls_R_factor_all 0.1094 _refine_ls_R_factor_gt 0.0647 _refine_ls_wR_factor_ref 0.1984 _refine_ls_wR_factor_gt 0.1672 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.108 _refine_diff_density_min -0.640 _refine_diff_density_rms 0.099 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 Ru Ru 1.0000 0.28912(4) 0.2500 0.0450(2) Uani 1 2 d S . . O1 O 1.23648(19) 0.8396(4) 0.3315(2) 0.0862(14) Uani 1 1 d . . . O2 O 1.01087(17) -0.2478(4) -0.05116(19) 0.0717(11) Uani 1 1 d . A . N1 N 1.01471(16) 0.4118(3) 0.31184(18) 0.0468(10) Uani 1 1 d . . . N2 N 0.93448(15) 0.2901(3) 0.29897(19) 0.0475(10) Uani 1 1 d . A . N3 N 0.95757(15) 0.1666(3) 0.20745(19) 0.0479(10) Uani 1 1 d . . . C1 C 1.2698(3) 0.8561(7) 0.3830(4) 0.108(3) Uani 1 1 d . . . H11 H 1.2485 0.8781 0.4182 0.162 Uiso 1 1 calc R . . H12 H 1.2956 0.9118 0.3736 0.162 Uiso 1 1 calc R . . H13 H 1.2883 0.7898 0.3928 0.162 Uiso 1 1 calc R . . C2 C 1.1953(2) 0.7711(4) 0.3391(3) 0.0602(15) Uani 1 1 d . . . C3 C 1.1795(2) 0.7293(4) 0.3947(3) 0.0604(15) Uani 1 1 d . . . H3 H 1.1987 0.7466 0.4306 0.073 Uiso 1 1 calc R . . C4 C 1.1358(2) 0.6622(4) 0.3988(2) 0.0515(13) Uani 1 1 d . . . C5 C 1.1227(2) 0.6148(5) 0.4598(2) 0.0644(15) Uani 1 1 d . . . H51 H 1.0926 0.6526 0.4776 0.097 Uiso 1 1 calc R . . H52 H 1.1531 0.6213 0.4871 0.097 Uiso 1 1 calc R . . H53 H 1.1137 0.5394 0.4547 0.097 Uiso 1 1 calc R . . C6 C 1.1075(2) 0.6379(4) 0.3454(2) 0.0510(13) Uani 1 1 d . . . C7 C 1.0574(2) 0.4752(4) 0.3135(2) 0.0456(12) Uani 1 1 d . . . H7 H 1.0872 0.4561 0.2896 0.055 Uiso 1 1 calc R . . C8 C 1.0600(2) 0.5681(4) 0.3488(2) 0.0486(12) Uani 1 1 d . . . C9 C 1.0168(2) 0.5906(4) 0.3853(2) 0.0576(14) Uani 1 1 d . A . H9 H 1.0172 0.6522 0.4104 0.069 Uiso 1 1 calc R . . C10 C 0.9734(2) 0.5254(5) 0.3856(2) 0.0598(15) Uani 1 1 d . . . H10 H 0.9442 0.5412 0.4114 0.072 Uiso 0.746(11) 1 calc PR A 1 C11 C 0.9724(2) 0.4368(4) 0.3483(2) 0.0513(13) Uani 1 1 d . A . C12 C 0.9276(2) 0.3642(5) 0.3422(2) 0.0557(14) Uani 1 1 d . . . C13 C 0.8795(2) 0.3658(6) 0.3752(3) 0.0756(18) Uani 1 1 d . A . H131 H 0.8729 0.4194 0.4048 0.091 Uiso 0.746(11) 1 calc PR A 1 C14 C 0.8427(2) 0.2883(7) 0.3635(4) 0.093(2) Uani 1 1 d . . . H14 H 0.8108 0.2879 0.3862 0.111 Uiso 1 1 calc R A . C15 C 0.8509(2) 0.2110(6) 0.3197(3) 0.082(2) Uani 1 1 d . A . H15 H 0.8256 0.1568 0.3122 0.098 Uiso 0.254(11) 1 calc PR A 2 C16A C 0.8188(3) 0.1190(8) 0.3049(4) 0.083(3) Uani 0.746(11) 1 d P A 1 H161 H 0.7874 0.1075 0.3274 0.100 Uiso 0.746(11) 1 calc PR A 1 C17A C 0.8316(3) 0.0491(8) 0.2606(4) 0.074(3) Uani 0.746(11) 1 d P A 1 H171 H 0.8090 -0.0099 0.2535 0.088 Uiso 0.746(11) 1 calc PR A 1 C16B C 0.9226(12) 0.539(2) 0.4122(12) 0.079(8) Uani 0.254(11) 1 d P A 2 H162 H 0.9175 0.5992 0.4378 0.094 Uiso 0.254(11) 1 calc PR A 2 C17B C 0.8812(13) 0.473(3) 0.4040(11) 0.091(11) Uani 0.254(11) 1 d P A 2 H172 H 0.8484 0.4989 0.4187 0.109 Uiso 0.254(11) 1 calc PR A 2 C18 C 0.8796(2) 0.0604(5) 0.2226(3) 0.0656(15) Uani 1 1 d . . . H18 H 0.8476 0.0477 0.2441 0.079 Uiso 0.254(11) 1 calc PR A 2 C19 C 0.8953(2) -0.0069(5) 0.1751(3) 0.0652(16) Uani 1 1 d . A . H19 H 0.8739 -0.0659 0.1641 0.078 Uiso 1 1 calc R . . C20 C 0.9419(2) 0.0121(4) 0.1439(2) 0.0538(13) Uani 1 1 d . . . C21 C 0.97128(19) 0.1026(4) 0.1618(2) 0.0472(12) Uani 1 1 d . A . H21 H 1.0026 0.1185 0.1399 0.057 Uiso 1 1 calc R . . C22 C 0.9115(2) 0.1462(4) 0.2379(2) 0.0544(14) Uani 1 1 d . A . C23 C 0.8983(2) 0.2160(4) 0.2865(3) 0.0560(14) Uani 1 1 d . . . C24 C 0.9609(2) -0.0555(4) 0.0929(2) 0.0544(13) Uani 1 1 d . A . C25 C 0.9291(2) -0.0748(4) 0.0412(3) 0.0577(14) Uani 1 1 d . . . C26 C 0.8754(2) -0.0239(5) 0.0333(3) 0.0761(18) Uani 1 1 d . A . H261 H 0.8652 -0.0264 -0.0098 0.114 Uiso 1 1 calc R . . H262 H 0.8768 0.0504 0.0469 0.114 Uiso 1 1 calc R . . H263 H 0.8494 -0.0627 0.0579 0.114 Uiso 1 1 calc R . . C27 C 0.9480(2) -0.1381(4) -0.0050(3) 0.0623(15) Uani 1 1 d . A . H27 H 0.9264 -0.1506 -0.0398 0.075 Uiso 1 1 calc R . . C28 C 0.9973(2) -0.1843(4) -0.0025(3) 0.0558(13) Uani 1 1 d . . . C29 C 1.0627(3) -0.2885(5) -0.0520(3) 0.0789(19) Uani 1 1 d . . . H291 H 1.0879 -0.2296 -0.0484 0.118 Uiso 1 1 calc R A . H292 H 1.0688 -0.3263 -0.0906 0.118 Uiso 1 1 calc R . . H293 H 1.0675 -0.3377 -0.0177 0.118 Uiso 1 1 calc R . . C30 C 1.0293(2) -0.1648(4) 0.0473(2) 0.0567(14) Uani 1 1 d . A . H30 H 1.0636 -0.1949 0.0490 0.068 Uiso 1 1 calc R . . C31 C 1.0114(2) -0.1009(4) 0.0953(2) 0.0548(14) Uani 1 1 d . . . C32 C 1.0485(3) -0.0843(5) 0.1487(3) 0.0752(18) Uani 1 1 d . A . H321 H 1.0746 -0.1418 0.1495 0.113 Uiso 1 1 calc R . . H322 H 1.0284 -0.0846 0.1869 0.113 Uiso 1 1 calc R . . H323 H 1.0666 -0.0158 0.1441 0.113 Uiso 1 1 calc R . . C33 C 1.0954(3) 0.6558(5) 0.2299(3) 0.080(2) Uani 1 1 d . . . H331 H 1.1063 0.7069 0.1985 0.120 Uiso 1 1 calc R . . H332 H 1.0573 0.6617 0.2366 0.120 Uiso 1 1 calc R . . H333 H 1.1040 0.5834 0.2164 0.120 Uiso 1 1 calc R . . C34 C 1.1240(2) 0.6793(4) 0.2888(2) 0.0563(14) Uani 1 1 d . . . C35 C 1.1678(3) 0.7450(4) 0.2868(3) 0.0635(15) Uani 1 1 d . . . H35 H 1.1792 0.7726 0.2486 0.076 Uiso 1 1 calc R . . P1A P 0.80665(10) 0.3106(3) -0.05537(12) 0.0641(9) Uani 0.615(4) 1 d PD B 1 F1A F 0.75097(17) 0.2705(7) -0.0333(3) 0.132(5) Uani 0.615(4) 1 d PDU B 1 F2A F 0.8620(2) 0.3534(6) -0.0768(3) 0.117(3) Uani 0.615(4) 1 d PDU B 1 F3A F 0.7820(3) 0.4231(5) -0.0697(4) 0.177(5) Uani 0.615(4) 1 d PDU B 1 F4A F 0.8313(3) 0.1986(4) -0.0404(4) 0.121(4) Uani 0.615(4) 1 d PDU B 1 F5A F 0.7932(2) 0.2738(6) -0.1224(2) 0.085(2) Uani 0.615(4) 1 d PDU B 1 F6A F 0.8195(3) 0.3480(6) 0.0118(2) 0.111(3) Uani 0.615(4) 1 d PDU B 1 P1B P 0.8003(3) 0.2365(10) -0.0640(4) 0.064(4) Uani 0.174(8) 1 d PDU C 2 F1B F 0.7503(5) 0.1752(16) -0.0401(8) 0.116(11) Uani 0.174(8) 1 d PDU C 2 F2B F 0.8504(6) 0.2976(19) -0.0881(9) 0.139(19) Uani 0.174(8) 1 d PDU C 2 F3B F 0.7702(8) 0.3454(12) -0.0567(9) 0.097(9) Uani 0.174(8) 1 d PDU C 2 F4B F 0.8304(8) 0.1275(14) -0.0712(11) 0.171(16) Uani 0.174(8) 1 d PDU C 2 F5B F 0.7793(7) 0.2264(17) -0.1315(5) 0.087(10) Uani 0.174(8) 1 d PDU C 2 F6B F 0.8215(7) 0.247(2) 0.0034(5) 0.101(10) Uani 0.174(8) 1 d PDU C 2 P1C P 0.8036(5) 0.2619(13) -0.0587(7) 0.200(16) Uani 0.211(8) 1 d PDU D 3 F1C F 0.7498(8) 0.278(3) -0.0240(13) 0.25(3) Uani 0.211(8) 1 d PDU D 3 F2C F 0.8575(6) 0.2462(19) -0.0933(9) 0.085(7) Uani 0.211(8) 1 d PDU D 3 F3C F 0.7837(8) 0.337(2) -0.1117(11) 0.122(11) Uani 0.211(8) 1 d PDU D 3 F4C F 0.8237(11) 0.187(2) -0.0059(10) 0.134(13) Uani 0.211(8) 1 d PDU D 3 F5C F 0.7800(10) 0.1626(19) -0.0931(14) 0.31(3) Uani 0.211(8) 1 d PDU D 3 F6C F 0.8273(11) 0.3612(18) -0.0243(13) 0.192(18) Uani 0.211(8) 1 d PDU D 3 C37 C 0.754(2) 0.516(7) 0.2882(8) 0.14(2) Uani 0.50 1 d PD E 1 H371 H 0.7677 0.5692 0.3173 0.207 Uiso 0.50 1 calc PR E 1 H372 H 0.7830 0.4924 0.2616 0.207 Uiso 0.50 1 calc PR E 1 H373 H 0.7399 0.4555 0.3107 0.207 Uiso 0.50 1 calc PR E 1 C38 C 0.7131(7) 0.5642(14) 0.2513(9) 0.095(5) Uani 0.50 1 d PD E 1 N39 O 0.6809(6) 0.6035(13) 0.2230(9) 0.139(5) Uani 0.50 1 d PD E 1 N40 O 0.6739(6) 0.6163(14) 0.1643(10) 0.154(6) Uani 0.50 1 d PD F 2 C41 C 0.7034(7) 0.5749(12) 0.1330(9) 0.112(6) Uani 0.50 1 d PD F 2 C42 C 0.7400(13) 0.520(3) 0.0927(9) 0.119(8) Uani 0.50 1 d PD F 2 H421 H 0.7564 0.4610 0.1147 0.178 Uiso 0.50 1 calc PR F 2 H422 H 0.7674 0.5704 0.0794 0.178 Uiso 0.50 1 calc PR F 2 H423 H 0.7210 0.4933 0.0570 0.178 Uiso 0.50 1 calc PR F 2 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 Ru 0.0384(3) 0.0408(3) 0.0557(4) 0.000 0.0070(3) 0.000 O1 0.090(3) 0.068(3) 0.100(3) 0.003(3) -0.013(3) -0.019(3) O2 0.084(3) 0.063(2) 0.068(3) -0.008(2) -0.019(2) -0.008(2) N1 0.051(3) 0.037(2) 0.053(2) 0.0013(19) 0.0009(18) 0.0081(19) N2 0.041(2) 0.046(2) 0.055(2) 0.008(2) 0.0106(19) 0.004(2) N3 0.042(2) 0.042(2) 0.060(3) 0.004(2) 0.0039(19) -0.0045(18) C1 0.084(5) 0.131(7) 0.111(6) 0.004(5) -0.021(4) -0.044(5) C2 0.069(4) 0.040(3) 0.072(4) -0.002(3) -0.004(3) 0.007(3) C3 0.069(4) 0.041(3) 0.071(4) -0.014(3) -0.015(3) 0.011(3) C4 0.066(3) 0.036(3) 0.053(3) -0.004(2) -0.007(3) 0.019(3) C5 0.072(4) 0.065(4) 0.056(3) -0.010(3) -0.011(3) 0.006(3) C6 0.068(3) 0.029(2) 0.056(3) -0.006(2) -0.006(3) 0.013(2) C7 0.049(3) 0.040(3) 0.048(3) 0.000(2) -0.001(2) 0.005(2) C8 0.062(3) 0.036(3) 0.048(3) 0.000(2) -0.004(2) 0.010(2) C9 0.069(4) 0.049(3) 0.055(3) -0.008(3) -0.007(3) 0.014(3) C10 0.058(4) 0.065(4) 0.057(3) 0.000(3) 0.011(3) 0.024(3) C11 0.047(3) 0.054(3) 0.053(3) 0.003(3) 0.002(2) 0.014(3) C12 0.048(3) 0.061(3) 0.058(3) 0.007(3) 0.006(2) 0.021(3) C13 0.061(4) 0.091(5) 0.075(4) -0.012(4) 0.009(3) 0.018(4) C14 0.045(4) 0.130(7) 0.103(5) -0.019(5) 0.028(4) -0.006(4) C15 0.055(4) 0.107(6) 0.082(4) -0.011(4) 0.024(3) -0.018(4) C16A 0.051(5) 0.114(8) 0.085(6) -0.003(6) 0.028(4) -0.025(5) C17A 0.045(5) 0.091(6) 0.085(6) 0.007(5) 0.009(4) -0.027(4) C16B 0.09(2) 0.076(18) 0.067(16) 0.006(14) 0.019(14) 0.024(16) C17B 0.10(2) 0.11(3) 0.064(16) 0.023(16) 0.027(15) 0.06(2) C18 0.054(3) 0.066(4) 0.077(4) 0.012(3) 0.005(3) -0.014(3) C19 0.059(3) 0.059(4) 0.078(4) 0.011(3) -0.007(3) -0.026(3) C20 0.058(3) 0.037(3) 0.067(3) 0.006(3) -0.006(3) -0.010(2) C21 0.043(3) 0.038(3) 0.060(3) 0.004(2) 0.001(2) -0.006(2) C22 0.045(3) 0.053(3) 0.065(4) 0.010(3) 0.011(2) -0.009(2) C23 0.043(3) 0.056(3) 0.068(4) 0.010(3) 0.009(3) -0.004(3) C24 0.060(3) 0.038(3) 0.065(3) 0.008(2) -0.003(3) -0.013(2) C25 0.061(3) 0.043(3) 0.070(4) 0.005(3) -0.011(3) -0.014(3) C26 0.059(4) 0.082(5) 0.088(4) 0.005(4) -0.013(3) -0.010(3) C27 0.068(4) 0.052(3) 0.067(4) 0.012(3) -0.016(3) -0.019(3) C28 0.073(4) 0.036(3) 0.059(3) 0.005(2) -0.012(3) -0.016(3) C29 0.098(5) 0.064(4) 0.075(4) -0.019(3) -0.019(4) 0.012(4) C30 0.069(4) 0.034(3) 0.068(4) 0.007(3) -0.014(3) -0.006(3) C31 0.071(4) 0.031(3) 0.062(3) 0.004(2) -0.014(3) -0.011(2) C32 0.087(5) 0.057(4) 0.081(4) -0.017(3) -0.029(3) 0.013(3) C33 0.110(6) 0.067(4) 0.064(4) 0.010(3) -0.019(4) -0.016(4) C34 0.081(4) 0.033(3) 0.055(3) 0.000(2) -0.006(3) 0.010(3) C35 0.088(4) 0.035(3) 0.067(4) 0.004(3) -0.005(3) -0.002(3) P1A 0.0427(16) 0.084(3) 0.0654(19) 0.0147(17) -0.0097(13) 0.0008(16) F1A 0.045(4) 0.270(15) 0.080(5) 0.020(7) -0.008(3) 0.002(6) F2A 0.097(5) 0.170(8) 0.086(5) 0.035(5) -0.009(4) -0.076(6) F3A 0.222(11) 0.143(8) 0.166(8) 0.016(7) -0.058(8) 0.062(8) F4A 0.120(7) 0.091(6) 0.153(10) -0.003(6) -0.048(8) 0.019(5) F5A 0.068(5) 0.118(7) 0.068(4) -0.012(5) -0.006(3) -0.008(5) F6A 0.107(6) 0.145(7) 0.082(5) 0.000(5) -0.018(4) -0.007(5) P1B 0.035(5) 0.101(8) 0.055(6) 0.005(5) -0.023(4) 0.022(5) F1B 0.116(17) 0.122(17) 0.110(16) 0.018(14) -0.001(13) 0.014(14) F2B 0.14(2) 0.13(2) 0.15(2) 0.013(17) -0.016(17) -0.012(17) F3B 0.111(17) 0.069(14) 0.112(17) 0.026(12) -0.034(14) 0.001(13) F4B 0.15(2) 0.17(2) 0.19(2) 0.003(17) -0.027(16) 0.064(17) F5B 0.070(14) 0.103(17) 0.088(14) -0.019(13) -0.023(11) -0.011(12) F6B 0.081(14) 0.132(19) 0.092(15) 0.038(14) -0.039(12) -0.001(14) P1C 0.194(18) 0.205(18) 0.202(18) -0.012(10) 0.004(10) 0.026(10) F1C 0.24(4) 0.27(4) 0.24(4) 0.00(2) 0.013(19) 0.01(2) F2C 0.050(9) 0.102(14) 0.105(13) -0.002(11) 0.016(9) 0.024(9) F3C 0.097(15) 0.151(19) 0.119(17) 0.043(15) -0.026(13) 0.014(14) F4C 0.129(18) 0.15(2) 0.120(19) -0.012(15) 0.005(14) 0.039(15) F5C 0.29(4) 0.32(4) 0.32(4) -0.01(2) -0.03(2) 0.01(2) F6C 0.18(2) 0.19(2) 0.21(2) -0.023(18) -0.026(18) 0.028(17) C37 0.094(19) 0.18(5) 0.136(13) 0.02(3) 0.00(2) -0.03(3) C38 0.077(11) 0.093(12) 0.115(13) -0.010(10) 0.002(10) -0.016(9) N39 0.099(11) 0.150(14) 0.169(15) -0.020(12) 0.014(11) -0.028(10) N40 0.115(13) 0.159(15) 0.187(17) 0.013(14) 0.017(12) -0.046(11) C41 0.087(13) 0.082(12) 0.17(2) 0.034(13) 0.012(12) -0.034(10) C42 0.09(2) 0.08(3) 0.184(16) 0.002(14) 0.002(14) -0.021(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 Ru N2 1.978(4) . ? Ru N1 2.084(4) . ? Ru N3 2.096(4) . ? O1 C2 1.364(7) . ? O1 C1 1.425(8) . ? O2 C28 1.373(7) . ? O2 C29 1.412(8) . ? N1 C7 1.344(6) . ? N1 C11 1.373(6) . ? N2 C23 1.335(7) . ? N2 C12 1.338(7) . ? N3 C21 1.328(6) . ? N3 C22 1.369(6) . ? C1 H11 0.9800 . ? C1 H12 0.9800 . ? C1 H13 0.9800 . ? C2 C35 1.380(8) . ? C2 C3 1.382(8) . ? C3 C4 1.396(8) . ? C3 H3 0.9500 . ? C4 C6 1.404(7) . ? C4 C5 1.499(8) . ? C5 H51 0.9800 . ? C5 H52 0.9800 . ? C5 H53 0.9800 . ? C6 C34 1.406(7) . ? C6 C8 1.493(8) . ? C7 C8 1.401(7) . ? C7 H7 0.9500 . ? C8 C9 1.385(7) . ? C9 C10 1.372(8) . ? C9 H9 0.9500 . ? C10 C11 1.381(7) . ? C10 C16B 1.42(3) . ? C10 H10 0.9500 . ? C11 C12 1.464(8) . ? C12 C13 1.418(8) . ? C13 C14 1.373(10) . ? C13 C17B 1.49(3) . ? C13 H131 0.9500 . ? C14 C15 1.380(10) . ? C14 H14 0.9500 . ? C15 C23 1.406(8) . ? C15 C16A 1.450(11) . ? C15 H15 0.9500 . ? C16A C17A 1.347(12) . ? C16A H161 0.9500 . ? C17A C18 1.479(9) . ? C17A H171 0.9500 . ? C16B C17B 1.35(4) . ? C16B H162 0.9500 . ? C17B H172 0.9500 . ? C18 C22 1.389(8) . ? C18 C19 1.397(8) . ? C18 H18 0.9500 . ? C19 C20 1.387(8) . ? C19 H19 0.9500 . ? C20 C21 1.414(7) . ? C20 C24 1.483(8) . ? C21 H21 0.9500 . ? C22 C23 1.419(8) . ? C24 C31 1.403(7) . ? C24 C25 1.410(7) . ? C25 C27 1.371(8) . ? C25 C26 1.516(8) . ? C26 H261 0.9800 . ? C26 H262 0.9800 . ? C26 H263 0.9800 . ? C27 C28 1.381(8) . ? C27 H27 0.9500 . ? C28 C30 1.380(7) . ? C29 H291 0.9800 . ? C29 H292 0.9800 . ? C29 H293 0.9800 . ? C30 C31 1.397(8) . ? C30 H30 0.9500 . ? C31 C32 1.514(7) . ? C32 H321 0.9800 . ? C32 H322 0.9800 . ? C32 H323 0.9800 . ? C33 C34 1.506(8) . ? C33 H331 0.9800 . ? C33 H332 0.9800 . ? C33 H333 0.9800 . ? C34 C35 1.385(8) . ? C35 H35 0.9500 . ? P1A F4A 1.574(3) . ? P1A F2A 1.575(3) . ? P1A F5A 1.575(3) . ? P1A F3A 1.575(3) . ? P1A F6A 1.576(3) . ? P1A F1A 1.576(3) . ? P1B F1B 1.575(3) . ? P1B F6B 1.575(3) . ? P1B F2B 1.575(3) . ? P1B F5B 1.575(3) . ? P1B F4B 1.575(3) . ? P1B F3B 1.575(3) . ? P1C F3C 1.575(3) . ? P1C F4C 1.575(3) . ? P1C F1C 1.575(3) . ? P1C F6C 1.575(3) . ? P1C F2C 1.575(3) . ? P1C F5C 1.575(3) . ? C37 C38 1.450(5) . ? C37 H371 0.9800 . ? C37 H372 0.9800 . ? C37 H373 0.9800 . ? C38 N39 1.138(5) . ? N40 C41 1.140(5) . ? C41 C42 1.451(5) . ? C42 H421 0.9800 . ? C42 H422 0.9800 . ? C42 H423 0.9800 . ? 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 N2 Ru N2 179.3(2) . 4_755 ? N2 Ru N1 101.32(16) . 4_755 ? N2 Ru N1 78.16(17) . . ? N1 Ru N1 84.6(2) 4_755 . ? N2 Ru N3 79.22(17) . . ? N1 Ru N3 157.37(16) . . ? N2 Ru N3 101.30(16) . 4_755 ? N1 Ru N3 99.37(15) . 4_755 ? N3 Ru N3 85.5(2) . 4_755 ? C2 O1 C1 116.7(5) . . ? C28 O2 C29 117.0(4) . . ? C7 N1 C11 118.6(4) . . ? C7 N1 Ru 126.8(3) . . ? C11 N1 Ru 113.9(3) . . ? C23 N2 C12 122.6(4) . . ? C23 N2 Ru 117.6(4) . . ? C12 N2 Ru 119.7(4) . . ? C21 N3 C22 118.4(4) . . ? C21 N3 Ru 130.1(3) . . ? C22 N3 Ru 111.1(3) . . ? O1 C1 H11 109.5 . . ? O1 C1 H12 109.5 . . ? H11 C1 H12 109.5 . . ? O1 C1 H13 109.5 . . ? H11 C1 H13 109.5 . . ? H12 C1 H13 109.5 . . ? O1 C2 C35 115.8(6) . . ? O1 C2 C3 124.8(5) . . ? C35 C2 C3 119.4(6) . . ? C2 C3 C4 121.1(5) . . ? C2 C3 H3 119.4 . . ? C4 C3 H3 119.4 . . ? C3 C4 C6 118.9(5) . . ? C3 C4 C5 118.3(5) . . ? C6 C4 C5 122.8(5) . . ? C4 C5 H51 109.5 . . ? C4 C5 H52 109.5 . . ? H51 C5 H52 109.5 . . ? C4 C5 H53 109.5 . . ? H51 C5 H53 109.5 . . ? H52 C5 H53 109.5 . . ? C4 C6 C34 120.0(5) . . ? C4 C6 C8 119.9(5) . . ? C34 C6 C8 120.1(5) . . ? N1 C7 C8 123.1(5) . . ? N1 C7 H7 118.5 . . ? C8 C7 H7 118.5 . . ? C9 C8 C7 116.7(5) . . ? C9 C8 C6 123.3(5) . . ? C7 C8 C6 120.0(5) . . ? C10 C9 C8 121.2(5) . . ? C10 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? C9 C10 C11 119.4(5) . . ? C9 C10 C16B 131.2(14) . . ? C11 C10 C16B 108.8(14) . . ? C9 C10 H10 120.3 . . ? C11 C10 H10 120.3 . . ? N1 C11 C10 121.0(5) . . ? N1 C11 C12 114.3(5) . . ? C10 C11 C12 124.7(5) . . ? N2 C12 C13 118.8(5) . . ? N2 C12 C11 113.4(4) . . ? C13 C12 C11 127.8(5) . . ? C14 C13 C12 118.8(6) . . ? C14 C13 C17B 137.6(14) . . ? C12 C13 C17B 101.8(13) . . ? C14 C13 H131 120.6 . . ? C12 C13 H131 120.6 . . ? C13 C14 C15 121.7(6) . . ? C13 C14 H14 119.2 . . ? C15 C14 H14 119.2 . . ? C14 C15 C23 117.1(6) . . ? C14 C15 C16A 129.2(6) . . ? C23 C15 C16A 113.6(6) . . ? C14 C15 H15 121.4 . . ? C23 C15 H15 121.4 . . ? C17A C16A C15 123.0(7) . . ? C17A C16A H161 118.5 . . ? C15 C16A H161 118.5 . . ? C16A C17A C18 122.6(7) . . ? C16A C17A H171 118.7 . . ? C18 C17A H171 118.7 . . ? C17B C16B C10 125(2) . . ? C17B C16B H162 117.3 . . ? C10 C16B H162 117.3 . . ? C16B C17B C13 129(2) . . ? C16B C17B H172 115.4 . . ? C13 C17B H172 115.4 . . ? C22 C18 C19 118.7(5) . . ? C22 C18 C17A 114.8(6) . . ? C19 C18 C17A 126.4(6) . . ? C22 C18 H18 120.6 . . ? C19 C18 H18 120.6 . . ? C20 C19 C18 120.4(5) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C19 C20 C21 116.8(5) . . ? C19 C20 C24 123.3(5) . . ? C21 C20 C24 119.9(5) . . ? N3 C21 C20 123.8(5) . . ? N3 C21 H21 118.1 . . ? C20 C21 H21 118.1 . . ? N3 C22 C18 121.8(5) . . ? N3 C22 C23 116.8(5) . . ? C18 C22 C23 121.4(5) . . ? N2 C23 C15 121.0(6) . . ? N2 C23 C22 114.8(4) . . ? C15 C23 C22 124.2(5) . . ? C31 C24 C25 118.9(5) . . ? C31 C24 C20 120.0(5) . . ? C25 C24 C20 121.1(5) . . ? C27 C25 C24 119.3(5) . . ? C27 C25 C26 118.4(5) . . ? C24 C25 C26 122.2(5) . . ? C25 C26 H261 109.5 . . ? C25 C26 H262 109.5 . . ? H261 C26 H262 109.5 . . ? C25 C26 H263 109.5 . . ? H261 C26 H263 109.5 . . ? H262 C26 H263 109.5 . . ? C25 C27 C28 122.1(5) . . ? C25 C27 H27 118.9 . . ? C28 C27 H27 118.9 . . ? O2 C28 C30 124.6(6) . . ? O2 C28 C27 116.2(5) . . ? C30 C28 C27 119.2(6) . . ? O2 C29 H291 109.5 . . ? O2 C29 H292 109.5 . . ? H291 C29 H292 109.5 . . ? O2 C29 H293 109.5 . . ? H291 C29 H293 109.5 . . ? H292 C29 H293 109.5 . . ? C28 C30 C31 120.3(6) . . ? C28 C30 H30 119.8 . . ? C31 C30 H30 119.8 . . ? C30 C31 C24 120.1(5) . . ? C30 C31 C32 117.1(5) . . ? C24 C31 C32 122.8(5) . . ? C31 C32 H321 109.5 . . ? C31 C32 H322 109.5 . . ? H321 C32 H322 109.5 . . ? C31 C32 H323 109.5 . . ? H321 C32 H323 109.5 . . ? H322 C32 H323 109.5 . . ? C34 C33 H331 109.5 . . ? C34 C33 H332 109.5 . . ? H331 C33 H332 109.5 . . ? C34 C33 H333 109.5 . . ? H331 C33 H333 109.5 . . ? H332 C33 H333 109.5 . . ? C35 C34 C6 119.1(5) . . ? C35 C34 C33 118.5(5) . . ? C6 C34 C33 122.4(5) . . ? C2 C35 C34 121.5(6) . . ? C2 C35 H35 119.3 . . ? C34 C35 H35 119.3 . . ? F4A P1A F2A 90.7(3) . . ? F4A P1A F5A 91.0(3) . . ? F2A P1A F5A 91.0(3) . . ? F4A P1A F3A 179.4(3) . . ? F2A P1A F3A 89.4(3) . . ? F5A P1A F3A 89.5(3) . . ? F4A P1A F6A 89.4(3) . . ? F2A P1A F6A 89.5(3) . . ? F5A P1A F6A 179.4(3) . . ? F3A P1A F6A 90.0(3) . . ? F4A P1A F1A 90.4(3) . . ? F2A P1A F1A 178.7(4) . . ? F5A P1A F1A 89.8(3) . . ? F3A P1A F1A 89.6(3) . . ? F6A P1A F1A 89.8(3) . . ? F1B P1B F6B 90.3(3) . . ? F1B P1B F2B 179.8(4) . . ? F6B P1B F2B 89.8(3) . . ? F1B P1B F5B 89.9(3) . . ? F6B P1B F5B 179.8(4) . . ? F2B P1B F5B 90.0(3) . . ? F1B P1B F4B 89.9(3) . . ? F6B P1B F4B 90.0(3) . . ? F2B P1B F4B 90.0(3) . . ? F5B P1B F4B 90.0(3) . . ? F1B P1B F3B 89.9(3) . . ? F6B P1B F3B 90.0(3) . . ? F2B P1B F3B 90.2(3) . . ? F5B P1B F3B 90.0(3) . . ? F4B P1B F3B 179.8(5) . . ? F3C P1C F4C 179.7(5) . . ? F3C P1C F1C 90.1(3) . . ? F4C P1C F1C 90.1(3) . . ? F3C P1C F6C 90.1(3) . . ? F4C P1C F6C 90.1(3) . . ? F1C P1C F6C 90.0(3) . . ? F3C P1C F2C 90.0(3) . . ? F4C P1C F2C 89.8(3) . . ? F1C P1C F2C 179.9(5) . . ? F6C P1C F2C 89.9(3) . . ? F3C P1C F5C 89.9(3) . . ? F4C P1C F5C 89.9(3) . . ? F1C P1C F5C 89.9(3) . . ? F6C P1C F5C 179.9(5) . . ? F2C P1C F5C 90.1(3) . . ? N39 C38 C37 179(4) . . ? N40 C41 C42 179(3) . . ? C41 C42 H421 109.5 . . ? C41 C42 H422 109.5 . . ? H421 C42 H422 109.5 . . ? C41 C42 H423 109.5 . . ? H421 C42 H423 109.5 . . ? H422 C42 H423 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 N2 Ru N1 C7 -176.8(4) . . . . ? N2 Ru N1 C7 2.8(4) 4_755 . . . ? N1 Ru N1 C7 -74.0(4) 4_755 . . . ? N3 Ru N1 C7 -175.5(4) . . . . ? N3 Ru N1 C7 83.5(4) 4_755 . . . ? N2 Ru N1 C11 -6.1(3) . . . . ? N2 Ru N1 C11 173.4(3) 4_755 . . . ? N1 Ru N1 C11 96.7(3) 4_755 . . . ? N3 Ru N1 C11 -4.8(6) . . . . ? N3 Ru N1 C11 -105.8(3) 4_755 . . . ? N1 Ru N2 C23 101.2(4) 4_755 . . . ? N1 Ru N2 C23 -176.8(4) . . . . ? N3 Ru N2 C23 3.7(4) . . . . ? N3 Ru N2 C23 -79.5(4) 4_755 . . . ? N1 Ru N2 C12 -78.0(4) 4_755 . . . ? N1 Ru N2 C12 3.9(4) . . . . ? N3 Ru N2 C12 -175.6(4) . . . . ? N3 Ru N2 C12 101.3(4) 4_755 . . . ? N2 Ru N3 C21 -177.6(5) . . . . ? N2 Ru N3 C21 2.9(5) 4_755 . . . ? N1 Ru N3 C21 82.6(4) 4_755 . . . ? N1 Ru N3 C21 -178.9(4) . . . . ? N3 Ru N3 C21 -75.2(4) 4_755 . . . ? N2 Ru N3 C22 -5.5(3) . . . . ? N2 Ru N3 C22 175.0(3) 4_755 . . . ? N1 Ru N3 C22 -105.3(3) 4_755 . . . ? N1 Ru N3 C22 -6.7(6) . . . . ? N3 Ru N3 C22 97.0(4) 4_755 . . . ? C1 O1 C2 C35 -171.5(6) . . . . ? C1 O1 C2 C3 9.7(9) . . . . ? O1 C2 C3 C4 178.0(5) . . . . ? C35 C2 C3 C4 -0.8(8) . . . . ? C2 C3 C4 C6 -0.5(7) . . . . ? C2 C3 C4 C5 176.6(5) . . . . ? C3 C4 C6 C34 1.2(7) . . . . ? C5 C4 C6 C34 -175.7(5) . . . . ? C3 C4 C6 C8 -178.7(4) . . . . ? C5 C4 C6 C8 4.4(7) . . . . ? C11 N1 C7 C8 -2.7(7) . . . . ? Ru N1 C7 C8 167.6(3) . . . . ? N1 C7 C8 C9 3.0(7) . . . . ? N1 C7 C8 C6 -176.3(4) . . . . ? C4 C6 C8 C9 57.3(7) . . . . ? C34 C6 C8 C9 -122.7(6) . . . . ? C4 C6 C8 C7 -123.5(5) . . . . ? C34 C6 C8 C7 56.5(6) . . . . ? C7 C8 C9 C10 -1.0(7) . . . . ? C6 C8 C9 C10 178.2(5) . . . . ? C8 C9 C10 C11 -1.1(8) . . . . ? C8 C9 C10 C16B -170.5(15) . . . . ? C7 N1 C11 C10 0.4(7) . . . . ? Ru N1 C11 C10 -171.1(4) . . . . ? C7 N1 C11 C12 178.8(4) . . . . ? Ru N1 C11 C12 7.4(5) . . . . ? C9 C10 C11 N1 1.4(8) . . . . ? C16B C10 C11 N1 173.0(11) . . . . ? C9 C10 C11 C12 -176.8(5) . . . . ? C16B C10 C11 C12 -5.2(13) . . . . ? C23 N2 C12 C13 -1.5(8) . . . . ? Ru N2 C12 C13 177.7(4) . . . . ? C23 N2 C12 C11 179.7(5) . . . . ? Ru N2 C12 C11 -1.1(6) . . . . ? N1 C11 C12 N2 -4.3(6) . . . . ? C10 C11 C12 N2 174.1(5) . . . . ? N1 C11 C12 C13 177.0(5) . . . . ? C10 C11 C12 C13 -4.6(9) . . . . ? N2 C12 C13 C14 2.9(9) . . . . ? C11 C12 C13 C14 -178.5(6) . . . . ? N2 C12 C13 C17B -164.5(11) . . . . ? C11 C12 C13 C17B 14.1(13) . . . . ? C12 C13 C14 C15 -1.6(11) . . . . ? C17B C13 C14 C15 160.0(16) . . . . ? C13 C14 C15 C23 -1.1(12) . . . . ? C13 C14 C15 C16A 174.3(8) . . . . ? C14 C15 C16A C17A -179.8(9) . . . . ? C23 C15 C16A C17A -4.3(13) . . . . ? C15 C16A C17A C18 -0.5(15) . . . . ? C9 C10 C16B C17B 172.8(19) . . . . ? C11 C10 C16B C17B 2(3) . . . . ? C10 C16B C17B C13 11(4) . . . . ? C14 C13 C17B C16B 179(2) . . . . ? C12 C13 C17B C16B -17(3) . . . . ? C16A C17A C18 C22 2.7(12) . . . . ? C16A C17A C18 C19 -178.6(8) . . . . ? C22 C18 C19 C20 -0.1(9) . . . . ? C17A C18 C19 C20 -178.7(6) . . . . ? C18 C19 C20 C21 -1.3(8) . . . . ? C18 C19 C20 C24 -179.7(5) . . . . ? C22 N3 C21 C20 -2.1(7) . . . . ? Ru N3 C21 C20 169.5(4) . . . . ? C19 C20 C21 N3 2.4(8) . . . . ? C24 C20 C21 N3 -179.1(5) . . . . ? C21 N3 C22 C18 0.6(8) . . . . ? Ru N3 C22 C18 -172.6(4) . . . . ? C21 N3 C22 C23 179.8(5) . . . . ? Ru N3 C22 C23 6.6(6) . . . . ? C19 C18 C22 N3 0.5(9) . . . . ? C17A C18 C22 N3 179.3(6) . . . . ? C19 C18 C22 C23 -178.7(5) . . . . ? C17A C18 C22 C23 0.2(9) . . . . ? C12 N2 C23 C15 -1.2(8) . . . . ? Ru N2 C23 C15 179.5(5) . . . . ? C12 N2 C23 C22 178.0(5) . . . . ? Ru N2 C23 C22 -1.2(6) . . . . ? C14 C15 C23 N2 2.5(10) . . . . ? C16A C15 C23 N2 -173.5(6) . . . . ? C14 C15 C23 C22 -176.6(6) . . . . ? C16A C15 C23 C22 7.3(10) . . . . ? N3 C22 C23 N2 -3.9(7) . . . . ? C18 C22 C23 N2 175.3(5) . . . . ? N3 C22 C23 C15 175.4(6) . . . . ? C18 C22 C23 C15 -5.5(9) . . . . ? C19 C20 C24 C31 -125.2(6) . . . . ? C21 C20 C24 C31 56.5(7) . . . . ? C19 C20 C24 C25 55.4(7) . . . . ? C21 C20 C24 C25 -122.9(5) . . . . ? C31 C24 C25 C27 0.8(7) . . . . ? C20 C24 C25 C27 -179.8(5) . . . . ? C31 C24 C25 C26 -176.5(5) . . . . ? C20 C24 C25 C26 2.9(8) . . . . ? C24 C25 C27 C28 0.2(8) . . . . ? C26 C25 C27 C28 177.6(5) . . . . ? C29 O2 C28 C30 -5.3(8) . . . . ? C29 O2 C28 C27 174.8(5) . . . . ? C25 C27 C28 O2 178.6(5) . . . . ? C25 C27 C28 C30 -1.3(8) . . . . ? O2 C28 C30 C31 -178.5(5) . . . . ? C27 C28 C30 C31 1.4(7) . . . . ? C28 C30 C31 C24 -0.4(7) . . . . ? C28 C30 C31 C32 179.3(5) . . . . ? C25 C24 C31 C30 -0.7(7) . . . . ? C20 C24 C31 C30 179.9(5) . . . . ? C25 C24 C31 C32 179.6(5) . . . . ? C20 C24 C31 C32 0.2(8) . . . . ? C4 C6 C34 C35 -0.7(7) . . . . ? C8 C6 C34 C35 179.2(5) . . . . ? C4 C6 C34 C33 179.8(5) . . . . ? C8 C6 C34 C33 -0.3(8) . . . . ? O1 C2 C35 C34 -177.6(5) . . . . ? C3 C2 C35 C34 1.3(8) . . . . ? C6 C34 C35 C2 -0.5(8) . . . . ? C33 C34 C35 C2 179.0(5) . . . . ? #===END data_9a _database_code_depnum_ccdc_archive 'CCDC 735255' # SG0608 _audit_creation_method SHELXL-97 _audit_creation_date 06-02-13 _chemical_name_systematic ; bis{8-(4-methoxy-2,6-dimethylphenyl)-2-[5-(4-methoxy-2,6- dimethylphenyl)-pyridin-2-yl]-1,10-phenanthroline}osmium(II) hexafluorophosphate di-acetonitrile solvate ; _chemical_name_common ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_moiety 'C70 H62 N6 O4 Os 2+, 2(F6 P -), 2(C2 H3 N)' _chemical_formula_sum 'C74 H68 F12 N8 O4 Os P2' _chemical_formula_weight 1613.53 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 296 0.0033 0.0016 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; H H 272 0.0000 0.0000 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; F F 48 0.0171 0.0103 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; N N 32 0.0061 0.0033 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; O O 16 0.0106 0.0060 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; Os Os 4 -1.2165 7.6030 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; P P 8 0.1023 0.0942 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c c a ' _symmetry_space_group_name_Hall ? _symmetry_Int_Tables_number 54 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' 'x+1/2, -y, -z+1/2' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' '-x-1/2, y, z-1/2' 'x, -y, z-1/2' _cell_length_a 25.3861(5) _cell_length_b 12.5157(3) _cell_length_c 21.8136(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6930.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 160(1) _cell_measurement_reflns_used 45814 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_description prism _exptl_crystal_colour purple-brown _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.546 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3256 _exptl_absorpt_coefficient_mu 1.974 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Blessing, 1995)' _exptl_absorpt_correction_T_min 0.595 _exptl_absorpt_correction_T_max 0.712 _exptl_special_details ; Solvent used: MeCN / diethyl ether Cooling Device: Oxford Cryosystems Cryostream 700 Crystal mount: glued on a glass fibre Mosaicity (deg.): 0.504(1) Frames collected: 290 Seconds exposure per frame: 33 Degrees rotation per frame: 1.5 Crystal-Detector distance (mm): 38.1 ; _diffrn_ambient_temperature 160(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Nonius FR590 sealed tube generator' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_detector '65 mm CCD camera on \k goniostat' _diffrn_measurement_device_type 'Nonius KappaCCD area-detector diffractometer' _diffrn_measurement_method '\f and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 70390 _diffrn_reflns_av_R_equivalents 0.1000 _diffrn_reflns_av_sigmaI/netI 0.0468 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 25.01 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _reflns_number_total 6111 _reflns_number_gt 3820 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'COLLECT (Nonius, 2000)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN and SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'SHELXL97 and PLATON (Spek, 2009)' _refine_special_details ; The asymmetric unit contains one half of a cation with the Os-atom on a two-fold axis, one anion and two closely adjacent sites in general positions which represent two equally occupied disordered positions for an acetonitrile molecule. The PF6- anion is highly disordered. Two sets of P- and F-atoms were defined for this anion and the site occupation factor of the major orientation refined to 0.682(6). The P-F and F...F distances were restrained tightly, so as to maintain octahedral geometry and uniform P-F bond lengths while neighbouring atoms within and between each orientation of the anion were restrained to have similar atomic displacement parameters. The bond lengths within the disordered MeCN molecule were also restrained to logical values. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0756P)^2^+38.0393P] 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 SHELXL _refine_ls_extinction_coef 0.0039(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6107 _refine_ls_number_parameters 552 _refine_ls_number_restraints 577 _refine_ls_R_factor_all 0.1058 _refine_ls_R_factor_gt 0.0616 _refine_ls_wR_factor_ref 0.1822 _refine_ls_wR_factor_gt 0.1528 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.110 _refine_diff_density_min -1.078 _refine_diff_density_rms 0.157 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 Os1 Os 0.5000 0.21022(4) 0.2500 0.0496(2) Uani 1 2 d S . . O1 O 0.7370(3) -0.3389(7) 0.3310(4) 0.100(2) Uani 1 1 d . . . O2 O 0.5106(3) 0.7468(6) -0.0513(3) 0.080(2) Uani 1 1 d . . . N1 N 0.5144(3) 0.0862(6) 0.3118(3) 0.0539(17) Uani 1 1 d . . . N2 N 0.4349(3) 0.2084(5) 0.3000(3) 0.0543(17) Uani 1 1 d . . . N3 N 0.4582(2) 0.3325(5) 0.2079(3) 0.0534(16) Uani 1 1 d . . . C1 C 0.7705(5) -0.3557(13) 0.3820(6) 0.124(5) Uani 1 1 d . . . H11 H 0.7949 -0.2954 0.3859 0.186 Uiso 1 1 calc R . . H12 H 0.7905 -0.4218 0.3760 0.186 Uiso 1 1 calc R . . H13 H 0.7492 -0.3616 0.4193 0.186 Uiso 1 1 calc R . . C2 C 0.6954(4) -0.2704(7) 0.3392(5) 0.069(2) Uani 1 1 d . . . C3 C 0.6807(4) -0.2298(7) 0.3937(5) 0.072(3) Uani 1 1 d . . . H3 H 0.7004 -0.2466 0.4294 0.086 Uiso 1 1 calc R . . C4 C 0.6357(4) -0.1616(7) 0.3983(4) 0.059(2) Uani 1 1 d . . . C5 C 0.6229(4) -0.1129(9) 0.4591(4) 0.079(3) Uani 1 1 d . . . H51 H 0.6007 -0.0497 0.4530 0.119 Uiso 1 1 calc R . . H52 H 0.6556 -0.0918 0.4798 0.119 Uiso 1 1 calc R . . H53 H 0.6041 -0.1651 0.4844 0.119 Uiso 1 1 calc R . . C6 C 0.6081(4) -0.1384(7) 0.3457(4) 0.060(2) Uani 1 1 d . . . C7 C 0.5569(3) 0.0251(6) 0.3135(3) 0.0481(18) Uani 1 1 d . . . H7 H 0.5866 0.0458 0.2897 0.058 Uiso 1 1 calc R . . C8 C 0.5607(4) -0.0693(7) 0.3487(4) 0.057(2) Uani 1 1 d . . . C9 C 0.5176(4) -0.0908(8) 0.3858(4) 0.068(3) Uani 1 1 d . . . H9 H 0.5185 -0.1518 0.4116 0.081 Uiso 1 1 calc R . . C10 C 0.4739(4) -0.0271(8) 0.3864(4) 0.070(3) Uani 1 1 d . . . H10 H 0.4451 -0.0439 0.4124 0.084 Uiso 1 1 calc R . . C11 C 0.4719(4) 0.0628(7) 0.3486(4) 0.060(2) Uani 1 1 d . . . C12 C 0.4274(3) 0.1350(8) 0.3431(4) 0.062(2) Uani 1 1 d . . . C13 C 0.3806(4) 0.1321(11) 0.3768(4) 0.084(3) Uani 1 1 d . . . H131 H 0.3741 0.0771 0.4059 0.101 Uiso 1 1 calc R . . C14 C 0.3444(4) 0.2112(12) 0.3663(5) 0.100(4) Uani 1 1 d . . . H14 H 0.3134 0.2138 0.3907 0.120 Uiso 1 1 calc R . . C15 C 0.3518(4) 0.2871(10) 0.3215(5) 0.085(3) Uani 1 1 d . . . C16 C 0.3189(5) 0.3816(15) 0.3071(7) 0.134(6) Uani 1 1 d . . . H16 H 0.2883 0.3951 0.3310 0.161 Uiso 1 1 calc R . . C17 C 0.3316(5) 0.4507(13) 0.2600(7) 0.115(5) Uani 1 1 d . . . H17 H 0.3078 0.5072 0.2510 0.137 Uiso 1 1 calc R . . C18 C 0.3797(4) 0.4413(9) 0.2231(5) 0.074(3) Uani 1 1 d . . . C19 C 0.3962(4) 0.5087(8) 0.1760(5) 0.073(3) Uani 1 1 d . . . H19 H 0.3757 0.5696 0.1656 0.087 Uiso 1 1 calc R . . C20 C 0.4420(3) 0.4875(7) 0.1442(4) 0.062(2) Uani 1 1 d . . . C21 C 0.4714(3) 0.3978(6) 0.1616(4) 0.0526(19) Uani 1 1 d . . . H21 H 0.5026 0.3823 0.1392 0.063 Uiso 1 1 calc R . . C22 C 0.4116(3) 0.3556(8) 0.2392(4) 0.063(2) Uani 1 1 d . . . C23 C 0.3984(3) 0.2834(8) 0.2878(4) 0.064(2) Uani 1 1 d . . . C24 C 0.4610(4) 0.5563(7) 0.0932(4) 0.061(2) Uani 1 1 d . . . C25 C 0.4287(4) 0.5730(7) 0.0414(4) 0.067(2) Uani 1 1 d . . . C26 C 0.3754(4) 0.5243(9) 0.0340(5) 0.081(3) Uani 1 1 d . . . H261 H 0.3761 0.4504 0.0489 0.121 Uiso 1 1 calc R . . H262 H 0.3655 0.5249 -0.0094 0.121 Uiso 1 1 calc R . . H263 H 0.3496 0.5655 0.0576 0.121 Uiso 1 1 calc R . . C27 C 0.4475(4) 0.6371(8) -0.0057(4) 0.071(3) Uani 1 1 d . . . H27 H 0.4260 0.6487 -0.0408 0.086 Uiso 1 1 calc R . . C28 C 0.4968(4) 0.6843(7) -0.0029(4) 0.064(2) Uani 1 1 d . . . C29 C 0.5637(5) 0.7875(9) -0.0520(5) 0.087(3) Uani 1 1 d . . . H291 H 0.5675 0.8424 -0.0203 0.130 Uiso 1 1 calc R . . H292 H 0.5712 0.8188 -0.0922 0.130 Uiso 1 1 calc R . . H293 H 0.5884 0.7291 -0.0440 0.130 Uiso 1 1 calc R . . C30 C 0.5295(4) 0.6634(7) 0.0473(4) 0.064(2) Uani 1 1 d . . . H30 H 0.5641 0.6923 0.0488 0.077 Uiso 1 1 calc R . . C31 C 0.5109(4) 0.5999(7) 0.0951(4) 0.064(2) Uani 1 1 d . . . C32 C 0.5481(4) 0.5843(8) 0.1488(4) 0.079(3) Uani 1 1 d . . . H321 H 0.5290 0.5961 0.1872 0.119 Uiso 1 1 calc R . . H322 H 0.5772 0.6354 0.1457 0.119 Uiso 1 1 calc R . . H323 H 0.5621 0.5113 0.1481 0.119 Uiso 1 1 calc R . . C33 C 0.5951(5) -0.1579(10) 0.2293(5) 0.094(4) Uani 1 1 d . . . H331 H 0.5990 -0.0823 0.2186 0.141 Uiso 1 1 calc R . . H332 H 0.5577 -0.1747 0.2348 0.141 Uiso 1 1 calc R . . H333 H 0.6097 -0.2021 0.1964 0.141 Uiso 1 1 calc R . . C34 C 0.6245(4) -0.1805(7) 0.2884(4) 0.065(2) Uani 1 1 d . . . C35 C 0.6679(4) -0.2445(8) 0.2862(5) 0.074(3) Uani 1 1 d . . . H35 H 0.6796 -0.2717 0.2478 0.089 Uiso 1 1 calc R . . P1A P 0.8065(3) 0.2134(6) 0.0605(3) 0.1453(17) Uani 0.317(6) 1 d PDU A 1 F1A F 0.7879(5) 0.1989(11) 0.1298(4) 0.144(3) Uani 0.317(6) 1 d PDU A 1 F2A F 0.8251(5) 0.2279(11) -0.0088(4) 0.148(2) Uani 0.317(6) 1 d PDU A 1 F3A F 0.7606(4) 0.1356(10) 0.0385(6) 0.148(2) Uani 0.317(6) 1 d PDU A 1 F4A F 0.8525(4) 0.2912(10) 0.0826(6) 0.148(2) Uani 0.317(6) 1 d PDU A 1 F5A F 0.7680(4) 0.3131(9) 0.0534(6) 0.150(2) Uani 0.317(6) 1 d PDU A 1 F6A F 0.8451(5) 0.1136(9) 0.0676(6) 0.149(2) Uani 0.317(6) 1 d PDU A 1 P1B P 0.80628(14) 0.1944(4) 0.05476(18) 0.1432(16) Uani 0.683(6) 1 d PDU A 2 F1B F 0.7931(3) 0.2408(6) 0.1210(3) 0.145(2) Uani 0.683(6) 1 d PDU A 2 F2B F 0.8195(3) 0.1479(6) -0.0115(3) 0.149(2) Uani 0.683(6) 1 d PDU A 2 F3B F 0.7829(3) 0.0814(5) 0.0745(3) 0.156(2) Uani 0.683(6) 1 d PDU A 2 F4B F 0.8297(3) 0.3074(5) 0.0350(3) 0.148(2) Uani 0.683(6) 1 d PDU A 2 F5B F 0.7495(2) 0.2302(7) 0.0312(3) 0.146(2) Uani 0.683(6) 1 d PDU A 2 F6B F 0.8630(2) 0.1586(6) 0.0783(3) 0.147(2) Uani 0.683(6) 1 d PDU A 2 C37 C 0.7500 0.0000 0.2124(11) 0.140(5) Uani 1 2 d SDU B 1 H371 H 0.7810 0.0454 0.2060 0.168 Uiso 0.50 1 calc PR B 1 H372 H 0.7355 -0.0212 0.1726 0.168 Uiso 0.50 1 calc PR B 1 H373 H 0.7602 -0.0639 0.2354 0.168 Uiso 0.50 1 calc PR B 1 C38 C 0.7105(10) 0.059(2) 0.2466(13) 0.135(5) Uani 0.50 1 d PDU B 1 N39 N 0.6809(8) 0.1034(19) 0.2763(13) 0.134(5) Uani 0.50 1 d PDU B 1 N40 N 0.6711(9) 0.121(2) 0.3304(13) 0.136(5) Uani 0.50 1 d PDU C 2 C41 C 0.6997(10) 0.076(2) 0.3616(14) 0.137(5) Uani 0.50 1 d PDU C 2 C42 C 0.7362(10) 0.024(3) 0.4030(12) 0.138(6) Uani 0.50 1 d PDU C 2 H421 H 0.7669 0.0699 0.4095 0.166 Uiso 0.50 1 calc PR C 2 H422 H 0.7476 -0.0442 0.3852 0.166 Uiso 0.50 1 calc PR C 2 H423 H 0.7188 0.0106 0.4424 0.166 Uiso 0.50 1 calc PR C 2 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 Os1 0.0456(3) 0.0483(3) 0.0550(3) 0.000 0.0078(2) 0.000 O1 0.102(6) 0.091(6) 0.105(6) -0.005(5) -0.012(5) 0.021(5) O2 0.105(6) 0.071(4) 0.063(4) 0.007(3) -0.018(4) 0.014(4) N1 0.062(4) 0.054(4) 0.046(4) 0.001(3) -0.002(3) -0.016(3) N2 0.052(4) 0.052(4) 0.059(4) -0.015(3) 0.014(3) -0.006(3) N3 0.048(4) 0.044(4) 0.069(4) -0.004(3) -0.001(3) 0.009(3) C1 0.115(10) 0.139(13) 0.117(10) -0.009(9) -0.027(8) 0.051(9) C2 0.079(7) 0.051(6) 0.077(7) 0.001(5) -0.004(5) -0.001(5) C3 0.093(7) 0.056(6) 0.067(6) 0.015(5) -0.024(5) -0.009(5) C4 0.072(6) 0.049(5) 0.058(5) 0.009(4) -0.001(4) -0.014(4) C5 0.095(7) 0.087(8) 0.056(5) 0.002(5) -0.013(5) -0.004(6) C6 0.079(6) 0.042(5) 0.057(5) 0.010(4) -0.005(4) -0.014(4) C7 0.053(5) 0.043(5) 0.049(4) 0.000(4) -0.001(4) -0.007(4) C8 0.074(6) 0.046(5) 0.050(5) -0.005(4) 0.000(4) -0.014(4) C9 0.087(6) 0.065(6) 0.052(5) 0.009(4) -0.013(5) -0.019(5) C10 0.064(6) 0.087(8) 0.058(5) 0.003(5) 0.003(5) -0.028(6) C11 0.073(6) 0.061(6) 0.047(5) -0.005(4) 0.007(4) -0.022(5) C12 0.051(5) 0.080(6) 0.054(5) 0.001(5) 0.008(4) -0.022(5) C13 0.059(6) 0.124(10) 0.069(6) 0.006(6) 0.009(5) -0.006(6) C14 0.056(6) 0.153(12) 0.091(8) 0.015(8) 0.027(6) -0.017(7) C15 0.065(6) 0.114(9) 0.075(7) 0.010(6) 0.016(5) 0.021(6) C16 0.083(9) 0.209(18) 0.110(10) 0.021(12) 0.032(8) 0.011(11) C17 0.081(8) 0.120(11) 0.142(12) -0.019(9) 0.001(8) 0.034(8) C18 0.059(6) 0.087(7) 0.076(6) -0.015(6) 0.004(5) 0.022(5) C19 0.073(6) 0.063(6) 0.082(6) -0.011(5) -0.007(5) 0.030(5) C20 0.066(5) 0.049(5) 0.072(5) -0.011(5) -0.009(5) 0.007(4) C21 0.052(5) 0.046(5) 0.059(5) -0.002(4) -0.006(4) 0.008(4) C22 0.049(5) 0.066(6) 0.074(6) -0.018(5) 0.005(4) 0.007(4) C23 0.045(5) 0.072(6) 0.073(6) -0.013(5) 0.013(4) -0.003(5) C24 0.068(6) 0.037(5) 0.077(6) -0.009(4) -0.011(5) 0.013(4) C25 0.069(6) 0.055(6) 0.076(6) -0.008(5) -0.016(5) 0.021(5) C26 0.074(6) 0.082(7) 0.086(7) -0.008(6) -0.020(5) 0.015(6) C27 0.077(6) 0.069(6) 0.068(6) -0.006(5) -0.024(5) 0.022(5) C28 0.083(6) 0.051(5) 0.059(5) -0.006(4) -0.014(5) 0.019(5) C29 0.106(9) 0.075(7) 0.080(7) 0.014(6) -0.021(6) -0.016(6) C30 0.076(6) 0.049(5) 0.066(5) -0.005(4) -0.015(5) 0.011(5) C31 0.087(7) 0.036(4) 0.068(5) -0.004(4) -0.014(5) 0.012(4) C32 0.095(7) 0.060(6) 0.083(7) 0.015(5) -0.034(6) -0.018(5) C33 0.138(11) 0.083(8) 0.061(5) -0.009(6) -0.021(6) 0.022(7) C34 0.090(7) 0.041(5) 0.062(6) -0.003(4) -0.005(5) -0.008(5) C35 0.102(8) 0.048(5) 0.072(6) -0.004(5) -0.001(6) 0.001(6) P1A 0.090(2) 0.238(5) 0.108(2) 0.043(3) 0.007(2) -0.019(3) F1A 0.093(4) 0.237(6) 0.102(4) 0.042(4) 0.009(4) -0.021(4) F2A 0.095(3) 0.238(5) 0.111(3) 0.042(4) 0.007(3) -0.019(3) F3A 0.092(3) 0.239(5) 0.113(3) 0.043(4) 0.004(3) -0.021(3) F4A 0.093(4) 0.237(6) 0.114(4) 0.041(4) 0.006(3) -0.021(4) F5A 0.097(4) 0.237(6) 0.115(4) 0.042(4) 0.007(3) -0.019(4) F6A 0.094(3) 0.239(5) 0.115(3) 0.043(4) 0.004(3) -0.017(3) P1B 0.087(2) 0.236(5) 0.106(2) 0.045(3) 0.0078(19) -0.018(2) F1B 0.094(3) 0.238(5) 0.102(3) 0.039(4) 0.007(3) -0.019(4) F2B 0.100(4) 0.235(6) 0.112(4) 0.037(4) 0.009(3) -0.018(4) F3B 0.105(3) 0.241(6) 0.123(3) 0.043(4) 0.006(3) -0.023(4) F4B 0.095(3) 0.235(5) 0.114(3) 0.041(3) 0.008(3) -0.019(3) F5B 0.088(3) 0.238(5) 0.112(3) 0.041(4) 0.002(3) -0.020(3) F6B 0.091(3) 0.238(5) 0.113(3) 0.044(4) 0.002(3) -0.017(3) C37 0.111(10) 0.131(11) 0.177(13) 0.000 0.000 -0.022(9) C38 0.106(10) 0.124(11) 0.176(13) 0.002(5) -0.001(5) -0.025(8) N39 0.104(10) 0.121(10) 0.177(13) 0.002(6) -0.001(6) -0.028(8) N40 0.104(10) 0.121(10) 0.181(13) -0.003(7) -0.002(7) -0.031(8) C41 0.105(11) 0.120(11) 0.185(14) -0.004(8) -0.003(8) -0.033(9) C42 0.107(12) 0.120(12) 0.188(14) -0.006(9) -0.001(9) -0.033(9) _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 Os1 N2 1.980(6) . ? Os1 N3 2.077(6) . ? Os1 N1 2.088(7) . ? O1 C2 1.372(12) . ? O1 C1 1.415(12) . ? O2 C28 1.361(12) . ? O2 C29 1.441(12) . ? N1 C7 1.324(10) . ? N1 C11 1.377(10) . ? N2 C12 1.327(11) . ? N2 C23 1.347(11) . ? N3 C21 1.341(10) . ? N3 C22 1.398(10) . ? C1 H11 0.9800 . ? C1 H12 0.9800 . ? C1 H13 0.9800 . ? C2 C3 1.345(13) . ? C2 C35 1.389(13) . ? C3 C4 1.428(13) . ? C3 H3 0.9500 . ? C4 C6 1.377(11) . ? C4 C5 1.495(12) . ? C5 H51 0.9800 . ? C5 H52 0.9800 . ? C5 H53 0.9800 . ? C6 C34 1.418(12) . ? C6 C8 1.483(13) . ? C7 C8 1.412(11) . ? C7 H7 0.9500 . ? C8 C9 1.387(12) . ? C9 C10 1.365(14) . ? C9 H9 0.9500 . ? C10 C11 1.396(13) . ? C10 H10 0.9500 . ? C11 C12 1.450(13) . ? C12 C13 1.398(12) . ? C13 C14 1.371(16) . ? C13 H131 0.9500 . ? C14 C15 1.376(16) . ? C14 H14 0.9500 . ? C15 C23 1.393(12) . ? C15 C16 1.481(19) . ? C16 C17 1.380(19) . ? C16 H16 0.9500 . ? C17 C18 1.468(16) . ? C17 H17 0.9500 . ? C18 C22 1.389(13) . ? C18 C19 1.394(14) . ? C19 C20 1.380(12) . ? C19 H19 0.9500 . ? C20 C21 1.400(11) . ? C20 C24 1.488(13) . ? C21 H21 0.9500 . ? C22 C23 1.432(13) . ? C24 C31 1.379(12) . ? C24 C25 1.412(12) . ? C25 C27 1.388(13) . ? C25 C26 1.493(13) . ? C26 H261 0.9800 . ? C26 H262 0.9800 . ? C26 H263 0.9800 . ? C27 C28 1.385(13) . ? C27 H27 0.9500 . ? C28 C30 1.399(12) . ? C29 H291 0.9800 . ? C29 H292 0.9800 . ? C29 H293 0.9800 . ? C30 C31 1.393(13) . ? C30 H30 0.9500 . ? C31 C32 1.518(12) . ? C32 H321 0.9800 . ? C32 H322 0.9800 . ? C32 H323 0.9800 . ? C33 C34 1.516(13) . ? C33 H331 0.9800 . ? C33 H332 0.9800 . ? C33 H333 0.9800 . ? C34 C35 1.365(13) . ? C35 H35 0.9500 . ? P1A F2A 1.594(4) . ? P1A F4A 1.594(4) . ? P1A F6A 1.594(4) . ? P1A F3A 1.594(4) . ? P1A F5A 1.594(4) . ? P1A F1A 1.594(4) . ? P1B F4B 1.594(4) . ? P1B F2B 1.594(4) . ? P1B F6B 1.594(4) . ? P1B F1B 1.594(4) . ? P1B F3B 1.594(4) . ? P1B F5B 1.594(4) . ? C37 C38 1.451(5) . ? C37 H371 0.9800 . ? C37 H372 0.9800 . ? C37 H373 0.9800 . ? C38 N39 1.139(5) . ? N40 C41 1.140(5) . ? C41 C42 1.451(5) . ? C42 H421 0.9800 . ? C42 H422 0.9800 . ? C42 H423 0.9800 . ? 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 N2 Os1 N2 178.6(4) . 4_655 ? N2 Os1 N3 101.0(3) . 4_655 ? N2 Os1 N3 80.0(3) . . ? N2 Os1 N3 101.0(3) 4_655 . ? N3 Os1 N3 85.0(4) . 4_655 ? N2 Os1 N1 101.6(3) . 4_655 ? N3 Os1 N1 99.9(3) . 4_655 ? N2 Os1 N1 77.4(3) . . ? N3 Os1 N1 157.4(3) . . ? N1 Os1 N1 84.0(4) . 4_655 ? C2 O1 C1 117.0(9) . . ? C28 O2 C29 117.0(8) . . ? C7 N1 C11 120.0(7) . . ? C7 N1 Os1 126.2(5) . . ? C11 N1 Os1 113.4(6) . . ? C12 N2 C23 121.6(7) . . ? C12 N2 Os1 121.2(6) . . ? C23 N2 Os1 117.2(6) . . ? C21 N3 C22 117.0(7) . . ? C21 N3 Os1 130.9(5) . . ? C22 N3 Os1 111.6(6) . . ? O1 C1 H11 109.5 . . ? O1 C1 H12 109.5 . . ? H11 C1 H12 109.5 . . ? O1 C1 H13 109.5 . . ? H11 C1 H13 109.5 . . ? H12 C1 H13 109.5 . . ? C3 C2 O1 124.4(9) . . ? C3 C2 C35 120.6(9) . . ? O1 C2 C35 115.0(9) . . ? C2 C3 C4 120.6(9) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C6 C4 C3 118.3(8) . . ? C6 C4 C5 122.8(9) . . ? C3 C4 C5 118.7(8) . . ? C4 C5 H51 109.5 . . ? C4 C5 H52 109.5 . . ? H51 C5 H52 109.5 . . ? C4 C5 H53 109.5 . . ? H51 C5 H53 109.5 . . ? H52 C5 H53 109.5 . . ? C4 C6 C34 120.4(9) . . ? C4 C6 C8 120.0(8) . . ? C34 C6 C8 119.6(8) . . ? N1 C7 C8 123.6(8) . . ? N1 C7 H7 118.2 . . ? C8 C7 H7 118.2 . . ? C9 C8 C7 115.3(9) . . ? C9 C8 C6 123.5(8) . . ? C7 C8 C6 121.2(8) . . ? C10 C9 C8 122.2(9) . . ? C10 C9 H9 118.9 . . ? C8 C9 H9 118.9 . . ? C9 C10 C11 119.7(9) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? N1 C11 C10 119.1(9) . . ? N1 C11 C12 115.4(8) . . ? C10 C11 C12 125.5(8) . . ? N2 C12 C13 120.8(9) . . ? N2 C12 C11 112.2(7) . . ? C13 C12 C11 127.0(9) . . ? C14 C13 C12 117.6(10) . . ? C14 C13 H131 121.2 . . ? C12 C13 H131 121.2 . . ? C13 C14 C15 121.7(10) . . ? C13 C14 H14 119.2 . . ? C15 C14 H14 119.2 . . ? C14 C15 C23 117.9(10) . . ? C14 C15 C16 128.6(10) . . ? C23 C15 C16 113.1(10) . . ? C17 C16 C15 121.8(11) . . ? C17 C16 H16 119.1 . . ? C15 C16 H16 119.1 . . ? C16 C17 C18 123.5(13) . . ? C16 C17 H17 118.3 . . ? C18 C17 H17 118.3 . . ? C22 C18 C19 118.6(8) . . ? C22 C18 C17 114.1(11) . . ? C19 C18 C17 127.3(11) . . ? C20 C19 C18 120.4(9) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C19 C20 C21 117.9(9) . . ? C19 C20 C24 122.5(8) . . ? C21 C20 C24 119.6(8) . . ? N3 C21 C20 124.0(8) . . ? N3 C21 H21 118.0 . . ? C20 C21 H21 118.0 . . ? C18 C22 N3 122.0(9) . . ? C18 C22 C23 122.5(8) . . ? N3 C22 C23 115.5(8) . . ? N2 C23 C15 120.2(9) . . ? N2 C23 C22 115.1(7) . . ? C15 C23 C22 124.6(9) . . ? C31 C24 C25 119.8(9) . . ? C31 C24 C20 120.3(8) . . ? C25 C24 C20 119.8(8) . . ? C27 C25 C24 118.6(9) . . ? C27 C25 C26 117.9(8) . . ? C24 C25 C26 123.5(9) . . ? C25 C26 H261 109.5 . . ? C25 C26 H262 109.5 . . ? H261 C26 H262 109.5 . . ? C25 C26 H263 109.5 . . ? H261 C26 H263 109.5 . . ? H262 C26 H263 109.5 . . ? C28 C27 C25 121.6(9) . . ? C28 C27 H27 119.2 . . ? C25 C27 H27 119.2 . . ? O2 C28 C27 116.4(8) . . ? O2 C28 C30 124.2(9) . . ? C27 C28 C30 119.4(9) . . ? O2 C29 H291 109.5 . . ? O2 C29 H292 109.5 . . ? H291 C29 H292 109.5 . . ? O2 C29 H293 109.5 . . ? H291 C29 H293 109.5 . . ? H292 C29 H293 109.5 . . ? C31 C30 C28 119.4(9) . . ? C31 C30 H30 120.3 . . ? C28 C30 H30 120.3 . . ? C24 C31 C30 121.0(8) . . ? C24 C31 C32 122.9(8) . . ? C30 C31 C32 116.1(8) . . ? C31 C32 H321 109.5 . . ? C31 C32 H322 109.5 . . ? H321 C32 H322 109.5 . . ? C31 C32 H323 109.5 . . ? H321 C32 H323 109.5 . . ? H322 C32 H323 109.5 . . ? C34 C33 H331 109.5 . . ? C34 C33 H332 109.5 . . ? H331 C33 H332 109.5 . . ? C34 C33 H333 109.5 . . ? H331 C33 H333 109.5 . . ? H332 C33 H333 109.5 . . ? C35 C34 C6 119.2(9) . . ? C35 C34 C33 118.4(9) . . ? C6 C34 C33 122.4(9) . . ? C34 C35 C2 120.8(10) . . ? C34 C35 H35 119.6 . . ? C2 C35 H35 119.6 . . ? F2A P1A F4A 90.00(4) . . ? F2A P1A F6A 90.01(4) . . ? F4A P1A F6A 90.00(4) . . ? F2A P1A F3A 90.00(4) . . ? F4A P1A F3A 179.99(7) . . ? F6A P1A F3A 90.00(4) . . ? F2A P1A F5A 90.00(4) . . ? F4A P1A F5A 90.00(4) . . ? F6A P1A F5A 179.99(7) . . ? F3A P1A F5A 90.00(4) . . ? F2A P1A F1A 180.00(7) . . ? F4A P1A F1A 90.00(4) . . ? F6A P1A F1A 90.00(4) . . ? F3A P1A F1A 89.99(4) . . ? F5A P1A F1A 90.00(4) . . ? F4B P1B F2B 90.01(4) . . ? F4B P1B F6B 90.00(4) . . ? F2B P1B F6B 90.01(4) . . ? F4B P1B F1B 90.01(4) . . ? F2B P1B F1B 179.99(7) . . ? F6B P1B F1B 90.00(4) . . ? F4B P1B F3B 179.99(7) . . ? F2B P1B F3B 89.99(4) . . ? F6B P1B F3B 90.01(4) . . ? F1B P1B F3B 89.99(4) . . ? F4B P1B F5B 90.00(4) . . ? F2B P1B F5B 90.00(4) . . ? F6B P1B F5B 179.99(7) . . ? F1B P1B F5B 89.99(4) . . ? F3B P1B F5B 90.00(4) . . ? N39 C38 C37 176(4) . . ? N40 C41 C42 177(4) . . ? C41 C42 H421 109.5 . . ? C41 C42 H422 109.5 . . ? H421 C42 H422 109.5 . . ? C41 C42 H423 109.5 . . ? H421 C42 H423 109.5 . . ? H422 C42 H423 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 N2 Os1 N1 C7 178.4(7) . . . . ? N2 Os1 N1 C7 -0.7(7) 4_655 . . . ? N3 Os1 N1 C7 -82.5(7) 4_655 . . . ? N3 Os1 N1 C7 176.5(6) . . . . ? N1 Os1 N1 C7 75.0(6) 4_655 . . . ? N2 Os1 N1 C11 5.6(5) . . . . ? N2 Os1 N1 C11 -173.5(5) 4_655 . . . ? N3 Os1 N1 C11 104.8(5) 4_655 . . . ? N3 Os1 N1 C11 3.8(10) . . . . ? N1 Os1 N1 C11 -97.7(6) 4_655 . . . ? N3 Os1 N2 C12 -101.8(6) 4_655 . . . ? N3 Os1 N2 C12 175.4(7) . . . . ? N1 Os1 N2 C12 77.2(7) 4_655 . . . ? N1 Os1 N2 C12 -3.9(6) . . . . ? N3 Os1 N2 C23 79.3(6) 4_655 . . . ? N3 Os1 N2 C23 -3.6(6) . . . . ? N1 Os1 N2 C23 -101.8(6) 4_655 . . . ? N1 Os1 N2 C23 177.1(7) . . . . ? N2 Os1 N3 C21 177.8(7) . . . . ? N2 Os1 N3 C21 -3.1(7) 4_655 . . . ? N3 Os1 N3 C21 75.7(7) 4_655 . . . ? N1 Os1 N3 C21 -82.0(7) 4_655 . . . ? N1 Os1 N3 C21 179.6(6) . . . . ? N2 Os1 N3 C22 6.2(5) . . . . ? N2 Os1 N3 C22 -174.7(6) 4_655 . . . ? N3 Os1 N3 C22 -96.0(6) 4_655 . . . ? N1 Os1 N3 C22 106.3(6) 4_655 . . . ? N1 Os1 N3 C22 8.0(10) . . . . ? C1 O1 C2 C3 -8.9(16) . . . . ? C1 O1 C2 C35 171.4(10) . . . . ? O1 C2 C3 C4 -177.9(9) . . . . ? C35 C2 C3 C4 1.8(14) . . . . ? C2 C3 C4 C6 -0.3(13) . . . . ? C2 C3 C4 C5 -176.2(9) . . . . ? C3 C4 C6 C34 -0.6(12) . . . . ? C5 C4 C6 C34 175.1(8) . . . . ? C3 C4 C6 C8 179.1(8) . . . . ? C5 C4 C6 C8 -5.2(13) . . . . ? C11 N1 C7 C8 4.2(11) . . . . ? Os1 N1 C7 C8 -168.1(6) . . . . ? N1 C7 C8 C9 -4.5(11) . . . . ? N1 C7 C8 C6 176.0(7) . . . . ? C4 C6 C8 C9 -56.2(12) . . . . ? C34 C6 C8 C9 123.5(9) . . . . ? C4 C6 C8 C7 123.2(9) . . . . ? C34 C6 C8 C7 -57.1(11) . . . . ? C7 C8 C9 C10 2.3(12) . . . . ? C6 C8 C9 C10 -178.3(8) . . . . ? C8 C9 C10 C11 0.1(13) . . . . ? C7 N1 C11 C10 -1.4(11) . . . . ? Os1 N1 C11 C10 171.8(6) . . . . ? C7 N1 C11 C12 -180.0(7) . . . . ? Os1 N1 C11 C12 -6.7(9) . . . . ? C9 C10 C11 N1 -0.7(12) . . . . ? C9 C10 C11 C12 177.7(8) . . . . ? C23 N2 C12 C13 1.1(13) . . . . ? Os1 N2 C12 C13 -177.8(7) . . . . ? C23 N2 C12 C11 -179.7(7) . . . . ? Os1 N2 C12 C11 1.4(10) . . . . ? N1 C11 C12 N2 3.7(11) . . . . ? C10 C11 C12 N2 -174.7(8) . . . . ? N1 C11 C12 C13 -177.1(8) . . . . ? C10 C11 C12 C13 4.4(15) . . . . ? N2 C12 C13 C14 -3.9(15) . . . . ? C11 C12 C13 C14 177.0(10) . . . . ? C12 C13 C14 C15 4.4(18) . . . . ? C13 C14 C15 C23 -2.0(19) . . . . ? C13 C14 C15 C16 -175.2(13) . . . . ? C14 C15 C16 C17 -179.7(14) . . . . ? C23 C15 C16 C17 7(2) . . . . ? C15 C16 C17 C18 -4(2) . . . . ? C16 C17 C18 C22 0.7(19) . . . . ? C16 C17 C18 C19 -178.2(13) . . . . ? C22 C18 C19 C20 3.0(15) . . . . ? C17 C18 C19 C20 -178.2(11) . . . . ? C18 C19 C20 C21 -1.0(13) . . . . ? C18 C19 C20 C24 179.4(9) . . . . ? C22 N3 C21 C20 1.4(12) . . . . ? Os1 N3 C21 C20 -169.8(6) . . . . ? C19 C20 C21 N3 -1.3(13) . . . . ? C24 C20 C21 N3 178.3(7) . . . . ? C19 C18 C22 N3 -2.9(14) . . . . ? C17 C18 C22 N3 178.1(9) . . . . ? C19 C18 C22 C23 178.8(9) . . . . ? C17 C18 C22 C23 -0.2(15) . . . . ? C21 N3 C22 C18 0.7(12) . . . . ? Os1 N3 C22 C18 173.6(7) . . . . ? C21 N3 C22 C23 179.2(7) . . . . ? Os1 N3 C22 C23 -7.9(9) . . . . ? C12 N2 C23 C15 1.4(13) . . . . ? Os1 N2 C23 C15 -179.6(7) . . . . ? C12 N2 C23 C22 -178.7(8) . . . . ? Os1 N2 C23 C22 0.3(10) . . . . ? C14 C15 C23 N2 -0.9(16) . . . . ? C16 C15 C23 N2 173.3(10) . . . . ? C14 C15 C23 C22 179.1(10) . . . . ? C16 C15 C23 C22 -6.6(16) . . . . ? C18 C22 C23 N2 -176.2(8) . . . . ? N3 C22 C23 N2 5.3(12) . . . . ? C18 C22 C23 C15 3.7(15) . . . . ? N3 C22 C23 C15 -174.8(9) . . . . ? C19 C20 C24 C31 124.5(9) . . . . ? C21 C20 C24 C31 -55.1(11) . . . . ? C19 C20 C24 C25 -58.4(12) . . . . ? C21 C20 C24 C25 122.0(9) . . . . ? C31 C24 C25 C27 -2.5(12) . . . . ? C20 C24 C25 C27 -179.6(8) . . . . ? C31 C24 C25 C26 176.7(8) . . . . ? C20 C24 C25 C26 -0.5(13) . . . . ? C24 C25 C27 C28 0.0(13) . . . . ? C26 C25 C27 C28 -179.2(8) . . . . ? C29 O2 C28 C27 -173.8(9) . . . . ? C29 O2 C28 C30 4.3(13) . . . . ? C25 C27 C28 O2 -178.9(8) . . . . ? C25 C27 C28 C30 2.9(13) . . . . ? O2 C28 C30 C31 178.7(8) . . . . ? C27 C28 C30 C31 -3.3(13) . . . . ? C25 C24 C31 C30 2.1(12) . . . . ? C20 C24 C31 C30 179.2(8) . . . . ? C25 C24 C31 C32 -179.3(8) . . . . ? C20 C24 C31 C32 -2.2(13) . . . . ? C28 C30 C31 C24 0.8(13) . . . . ? C28 C30 C31 C32 -177.9(8) . . . . ? C4 C6 C34 C35 0.1(13) . . . . ? C8 C6 C34 C35 -179.6(8) . . . . ? C4 C6 C34 C33 179.5(9) . . . . ? C8 C6 C34 C33 -0.2(13) . . . . ? C6 C34 C35 C2 1.4(14) . . . . ? C33 C34 C35 C2 -178.1(9) . . . . ? C3 C2 C35 C34 -2.3(15) . . . . ? O1 C2 C35 C34 177.4(9) . . . . ? #===END data_7a' _database_code_depnum_ccdc_archive 'CCDC 735256' # SG0708 _audit_creation_method SHELXL-97 _audit_creation_date 07-03-06 _chemical_name_systematic ; bis{8-(4-methoxy-2,6-dimethylphenyl)-2-[5-(4-methoxy-2,6- dimethylphenyl)-pyridin-2-yl]-1,10-phenanthroline}zinc(II) hexafluorophosphate di-acetonitrile solvate ; _chemical_name_common ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_moiety 'C70 H62 N6 O4 Zn 2+, 2(F6 P -), 2(C2 H3 N)' _chemical_formula_sum 'C74 H68 F12 N8 O4 P2 Zn' _chemical_formula_weight 1488.71 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 296 0.0033 0.0016 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; H H 272 0.0000 0.0000 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; F F 48 0.0171 0.0103 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; N N 32 0.0061 0.0033 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; O O 16 0.0106 0.0060 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; P P 8 0.1023 0.0942 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; Zn Zn 4 0.2839 1.4301 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c c a ' _symmetry_space_group_name_Hall ? _symmetry_Int_Tables_number 54 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' 'x+1/2, -y, -z+1/2' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' '-x-1/2, y, z-1/2' 'x, -y, z-1/2' _cell_length_a 24.974(1) _cell_length_b 12.912(1) _cell_length_c 22.066(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7115.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 160(1) _cell_measurement_reflns_used 32979 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.390 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3072 _exptl_absorpt_coefficient_mu 0.477 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; Solvent used: MeCN / diethyl ether Cooling Device: Oxford Cryosystems Cryostream Crystal mount: in oil on a loop Mosaicity (deg.): Frames collected: 180 Seconds exposure per frame: 1 Degrees rotation per frame: 1 Crystal-Detector distance (mm): 80 ; _diffrn_ambient_temperature 160(1) _diffrn_radiation_wavelength 0.71000 _diffrn_radiation_type X-ray _diffrn_radiation_source synchrotron _diffrn_radiation_monochromator ? _diffrn_detector 'CCD detector' _diffrn_measurement_device_type 'MarResearch 225 CCD detector' _diffrn_measurement_method '\f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 32979 _diffrn_reflns_av_R_equivalents 0.051 _diffrn_reflns_av_sigmaI/netI 0.0286 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 27.44 _diffrn_measured_fraction_theta_max 0.763 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.763 _reflns_number_total 6231 _reflns_number_gt 4786 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'SLS software' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN and SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'SHELXL97 and PLATON (Spek, 2009)' _refine_special_details ; All measurements were made at the SLS synchrotron (beamline PX) using radiation of wavelength \l = 0.710 \%A and a MarResearch 225 detector 80 mm from the crystal. Mosaicity = 0.56\%, 180 frames at 1\% \f rotation per frame and 1 second exposure per frame. The dataset completeness is low because the detector cannot be swung in theta, nor can it be brought closer than 80 mm from the crystal - it is a protein beamline. The structure was solved by using the model from the structure of the Ru-analogue and replacing Ru by Zn. Test refinements with 1%, 2% and 4% Ru did not improve the refinement results and degraded them insignificantly, so 100% Zn was assumed for the final refinement. The asymmetric unit contains one half of a cation with the Zn-atom on a two-fold axis, one anion and two closely adjacent sites in general positions which represent two equally occupied disordered positions for an acetonitrile molecule. In the cation, the two central CH groups of the phenanthroline moiety are disordered over two sites which effectively complete six-membered rings between all pyridine rings, thereby indicating that the ligand must be disordered through a 180\% rotation about the central N-atom. The site occupation factor for the major conformation refined to 0.75(1). The PF6- anion is highly disordered. Three sets of P- and F-atoms were defined for this anion and refinement of the site occupation factors of each set led to values of 0.488(4), 0.251(5) and 0.261(6). The P-F and F...F distances were restrained tightly, so as to maintain octahedral geometry and uniform P-F bond lengths and the atomic displacement parameters of the P- and F-atoms were given light pseudo-isotropic restraints. The bond lengths within the disordered MeCN molecule were also restrained to logical values. Validation reports some short contacts as A alerts. These are mostly between different disordered components of anions where the sums of the SOF of the relevant atoms is < 1.0, so that one can conceive that the "conflicting" sites are never occupied simultanously for adjacent moieties. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1159P)^2^+2.4637P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom & difmap' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6230 _refine_ls_number_parameters 637 _refine_ls_number_restraints 951 _refine_ls_R_factor_all 0.0747 _refine_ls_R_factor_gt 0.0601 _refine_ls_wR_factor_ref 0.1903 _refine_ls_wR_factor_gt 0.1800 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.524 _refine_diff_density_min -0.286 _refine_diff_density_rms 0.048 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 Zn Zn 1.0000 0.28508(3) 0.2500 0.0609(2) Uani 1 2 d S . . O1 O 1.23403(15) 0.8305(3) 0.33512(18) 0.1282(12) Uani 1 1 d . . . O2 O 1.00437(11) -0.2360(2) -0.05044(13) 0.0869(8) Uani 1 1 d . A . N1 N 1.01214(11) 0.41026(18) 0.31661(11) 0.0647(7) Uani 1 1 d . . . N2 N 0.93126(11) 0.28631(19) 0.29952(12) 0.0683(7) Uani 1 1 d . A . N3 N 0.95268(10) 0.16112(18) 0.20748(12) 0.0656(7) Uani 1 1 d . . . C1 C 1.2699(3) 0.8439(6) 0.3857(3) 0.169(3) Uani 1 1 d . . . H11 H 1.2491 0.8549 0.4227 0.254 Uiso 1 1 calc R . . H12 H 1.2929 0.9041 0.3784 0.254 Uiso 1 1 calc R . . H13 H 1.2921 0.7818 0.3902 0.254 Uiso 1 1 calc R . . C2 C 1.1913(2) 0.7640(3) 0.3433(2) 0.0958(13) Uani 1 1 d . . . C3 C 1.1757(2) 0.7244(3) 0.3979(2) 0.0964(13) Uani 1 1 d . . . H3 H 1.1953 0.7411 0.4335 0.116 Uiso 1 1 calc R . . C4 C 1.13125(18) 0.6596(3) 0.40206(17) 0.0861(11) Uani 1 1 d . . . C5 C 1.1167(2) 0.6120(4) 0.46304(18) 0.1075(14) Uani 1 1 d . . . H51 H 1.0858 0.6485 0.4801 0.161 Uiso 1 1 calc R . . H52 H 1.1472 0.6182 0.4908 0.161 Uiso 1 1 calc R . . H53 H 1.1078 0.5387 0.4575 0.161 Uiso 1 1 calc R . . C6 C 1.10178(17) 0.6352(2) 0.34955(15) 0.0780(10) Uani 1 1 d . . . C7 C 1.05397(15) 0.4735(2) 0.31904(13) 0.0670(8) Uani 1 1 d . . . H7 H 1.0851 0.4554 0.2967 0.080 Uiso 1 1 calc R . . C8 C 1.05471(16) 0.5656(2) 0.35273(14) 0.0732(9) Uani 1 1 d . . . C9 C 1.00880(19) 0.5862(3) 0.38621(16) 0.0863(12) Uani 1 1 d . A . H9 H 1.0070 0.6474 0.4100 0.104 Uiso 1 1 calc R . . C10 C 0.96631(18) 0.5201(3) 0.38553(15) 0.0838(11) Uani 1 1 d D . . H10 H 0.9356 0.5342 0.4096 0.101 Uiso 0.754(8) 1 calc PR A 1 C11 C 0.96816(15) 0.4318(2) 0.34931(13) 0.0701(9) Uani 1 1 d . A . C12 C 0.92354(15) 0.3588(3) 0.34208(15) 0.0769(9) Uani 1 1 d . . . C13 C 0.8761(2) 0.3569(5) 0.3757(2) 0.1102(16) Uani 1 1 d D A . H131 H 0.8694 0.4087 0.4052 0.132 Uiso 0.754(8) 1 calc PR A 1 C14 C 0.8394(2) 0.2797(6) 0.3656(3) 0.139(2) Uani 1 1 d . . . H14 H 0.8072 0.2787 0.3887 0.166 Uiso 1 1 calc R A . C15 C 0.84838(18) 0.2018(4) 0.3218(2) 0.1176(17) Uani 1 1 d D A . H15 H 0.8242 0.1460 0.3156 0.141 Uiso 0.246(8) 1 calc PR A 2 C16A C 0.8159(2) 0.1100(6) 0.3095(3) 0.119(2) Uani 0.754(8) 1 d PD A 1 H161 H 0.7856 0.0964 0.3343 0.143 Uiso 0.754(8) 1 calc PR A 1 C17A C 0.8276(2) 0.0445(6) 0.2643(3) 0.109(2) Uani 0.754(8) 1 d PD A 1 H171 H 0.8044 -0.0123 0.2569 0.131 Uiso 0.754(8) 1 calc PR A 1 C16B C 0.9113(4) 0.5321(15) 0.4057(8) 0.128(10) Uani 0.246(8) 1 d PD A 2 H162 H 0.9023 0.5948 0.4258 0.154 Uiso 0.246(8) 1 calc PR A 2 C17B C 0.8724(9) 0.4626(11) 0.3984(11) 0.157(13) Uani 0.246(8) 1 d PD A 2 H172 H 0.8375 0.4850 0.4094 0.188 Uiso 0.246(8) 1 calc PR A 2 C18 C 0.87453(15) 0.0574(3) 0.2263(2) 0.0939(12) Uani 1 1 d D . . H18 H 0.8429 0.0447 0.2491 0.113 Uiso 0.246(8) 1 calc PR A 2 C19 C 0.88916(16) -0.0076(3) 0.1788(2) 0.0926(11) Uani 1 1 d . A . H19 H 0.8674 -0.0656 0.1692 0.111 Uiso 1 1 calc R . . C20 C 0.93509(14) 0.0112(2) 0.14537(16) 0.0737(9) Uani 1 1 d . . . C21 C 0.96517(13) 0.0982(2) 0.16248(15) 0.0678(8) Uani 1 1 d . A . H21 H 0.9967 0.1130 0.1401 0.081 Uiso 1 1 calc R . . C22 C 0.90756(14) 0.1418(3) 0.23961(17) 0.0749(9) Uani 1 1 d . A . C23 C 0.89536(15) 0.2130(3) 0.28849(18) 0.0810(10) Uani 1 1 d . . . C24 C 0.95358(14) -0.0546(2) 0.09450(16) 0.0726(9) Uani 1 1 d . A . C25 C 0.92177(15) -0.0681(3) 0.04201(19) 0.0831(10) Uani 1 1 d . . . C26 C 0.86888(18) -0.0161(4) 0.0347(2) 0.1149(15) Uani 1 1 d . A . H261 H 0.8555 -0.0278 -0.0065 0.172 Uiso 1 1 calc R . . H262 H 0.8730 0.0584 0.0417 0.172 Uiso 1 1 calc R . . H263 H 0.8434 -0.0447 0.0640 0.172 Uiso 1 1 calc R . . C27 C 0.94110(16) -0.1291(3) -0.00483(18) 0.0843(10) Uani 1 1 d . A . H27 H 0.9198 -0.1385 -0.0401 0.101 Uiso 1 1 calc R . . C28 C 0.99023(15) -0.1765(3) -0.00159(17) 0.0735(9) Uani 1 1 d . . . C29 C 1.05581(18) -0.2801(3) -0.04963(19) 0.0921(12) Uani 1 1 d . . . H291 H 1.0827 -0.2251 -0.0459 0.138 Uiso 1 1 calc R A . H292 H 1.0618 -0.3185 -0.0873 0.138 Uiso 1 1 calc R . . H293 H 1.0589 -0.3274 -0.0151 0.138 Uiso 1 1 calc R . . C30 C 1.02194(15) -0.1622(2) 0.04883(16) 0.0715(8) Uani 1 1 d . A . H30 H 1.0563 -0.1936 0.0507 0.086 Uiso 1 1 calc R . . C31 C 1.00395(14) -0.1024(2) 0.09663(17) 0.0727(9) Uani 1 1 d . . . C32 C 1.04087(19) -0.0898(3) 0.15138(18) 0.1018(14) Uani 1 1 d . A . H321 H 1.0669 -0.1465 0.1521 0.153 Uiso 1 1 calc R . . H322 H 1.0195 -0.0913 0.1887 0.153 Uiso 1 1 calc R . . H323 H 1.0598 -0.0235 0.1485 0.153 Uiso 1 1 calc R . . C33 C 1.0893(2) 0.6548(4) 0.23651(19) 0.1090(16) Uani 1 1 d . . . H331 H 1.1037 0.6985 0.2040 0.163 Uiso 1 1 calc R . . H332 H 1.0512 0.6700 0.2422 0.163 Uiso 1 1 calc R . . H333 H 1.0937 0.5817 0.2256 0.163 Uiso 1 1 calc R . . C34 C 1.11904(18) 0.6765(2) 0.29440(17) 0.0828(10) Uani 1 1 d . . . C35 C 1.1632(2) 0.7395(3) 0.2920(2) 0.0982(13) Uani 1 1 d . . . H35 H 1.1745 0.7667 0.2541 0.118 Uiso 1 1 calc R . . P1A P 0.81197(10) 0.3106(3) -0.05886(17) 0.0809(17) Uani 0.488(4) 1 d PD B 1 F1A F 0.75402(16) 0.2918(8) -0.0348(3) 0.151(4) Uani 0.488(4) 1 d PDU B 1 F2A F 0.86988(17) 0.3286(7) -0.0829(3) 0.146(4) Uani 0.488(4) 1 d PDU B 1 F3A F 0.7945(4) 0.4188(5) -0.0831(4) 0.240(6) Uani 0.488(4) 1 d PDU B 1 F4A F 0.8296(3) 0.2025(3) -0.0344(3) 0.133(3) Uani 0.488(4) 1 d PDU B 1 F5A F 0.7953(3) 0.2619(7) -0.1207(2) 0.119(3) Uani 0.488(4) 1 d PDU B 1 F6A F 0.8279(3) 0.3608(5) 0.0028(3) 0.140(3) Uani 0.488(4) 1 d PDU B 1 P1B P 0.8040(2) 0.2267(6) -0.0670(3) 0.113(3) Uani 0.251(5) 1 d PDU C 2 F1B F 0.7506(4) 0.1861(13) -0.0393(6) 0.182(8) Uani 0.251(5) 1 d PDU C 2 F2B F 0.8572(4) 0.2679(13) -0.0951(8) 0.172(11) Uani 0.251(5) 1 d PDU C 2 F3B F 0.7847(7) 0.3405(8) -0.0579(9) 0.210(11) Uani 0.251(5) 1 d PDU C 2 F4B F 0.8238(7) 0.1134(8) -0.0768(8) 0.295(13) Uani 0.251(5) 1 d PDU C 2 F5B F 0.7780(6) 0.2252(16) -0.1313(4) 0.274(17) Uani 0.251(5) 1 d PDU C 2 F6B F 0.8302(6) 0.2269(15) -0.0029(5) 0.169(9) Uani 0.251(5) 1 d PDU C 2 P1C P 0.8112(3) 0.3048(6) -0.0634(4) 0.131(7) Uani 0.261(6) 1 d PDU D 3 F1C F 0.7569(3) 0.3546(11) -0.0439(7) 0.120(6) Uani 0.261(6) 1 d PDU D 3 F2C F 0.8651(4) 0.2544(13) -0.0834(7) 0.158(9) Uani 0.261(6) 1 d PDU D 3 F3C F 0.7920(5) 0.3077(11) -0.1306(4) 0.108(5) Uani 0.261(6) 1 d PDU D 3 F4C F 0.8296(5) 0.3029(13) 0.0041(4) 0.135(6) Uani 0.261(6) 1 d PDU D 3 F5C F 0.7861(7) 0.1950(7) -0.0558(7) 0.184(9) Uani 0.261(6) 1 d PDU D 3 F6C F 0.8364(6) 0.4145(8) -0.0705(7) 0.183(7) Uani 0.261(6) 1 d PDU D 3 C37 C 0.7547(17) 0.514(4) 0.2877(6) 0.201(14) Uani 0.50 1 d PD E 1 H371 H 0.7697 0.5619 0.3174 0.302 Uiso 0.50 1 d PR E 1 H372 H 0.7830 0.4915 0.2597 0.302 Uiso 0.50 1 d PR E 1 H373 H 0.7402 0.4529 0.3087 0.302 Uiso 0.50 1 d PR E 1 C38 C 0.7124(7) 0.5643(13) 0.2540(8) 0.155(7) Uani 0.50 1 d PD E 1 N39 N 0.6798(5) 0.6021(12) 0.2254(10) 0.159(5) Uani 0.50 1 d PD E 1 N40 N 0.6775(9) 0.618(2) 0.1648(11) 0.232(10) Uani 0.50 1 d PD F 2 C41 C 0.6971(16) 0.575(2) 0.1255(19) 0.40(3) Uani 0.50 1 d PD F 2 C42 C 0.7390(9) 0.513(2) 0.0982(12) 0.45(4) Uani 0.50 1 d PD F 2 H421 H 0.7374 0.4425 0.1147 0.669 Uiso 0.50 1 d PR F 2 H422 H 0.7740 0.5436 0.1074 0.669 Uiso 0.50 1 d PR F 2 H423 H 0.7338 0.5106 0.0542 0.669 Uiso 0.50 1 d PR F 2 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 Zn 0.0714(4) 0.0430(3) 0.0684(4) 0.000 0.0169(2) 0.000 O1 0.138(3) 0.102(2) 0.145(3) -0.003(2) -0.039(2) -0.025(2) O2 0.100(2) 0.0816(16) 0.0790(17) -0.0146(14) -0.0163(13) -0.0108(13) N1 0.0903(18) 0.0463(13) 0.0575(15) 0.0043(11) 0.0062(13) 0.0110(12) N2 0.0746(17) 0.0588(14) 0.0714(17) 0.0075(12) 0.0133(13) 0.0082(12) N3 0.0686(15) 0.0497(13) 0.0786(17) 0.0024(12) 0.0140(13) -0.0054(11) C1 0.128(5) 0.209(7) 0.170(6) -0.005(5) -0.048(4) -0.054(5) C2 0.119(3) 0.060(2) 0.108(3) 0.000(2) -0.024(3) 0.000(2) C3 0.128(4) 0.066(2) 0.095(3) -0.020(2) -0.031(3) 0.009(2) C4 0.124(3) 0.0581(18) 0.076(2) -0.0107(17) -0.021(2) 0.022(2) C5 0.153(4) 0.103(3) 0.067(2) -0.008(2) -0.023(2) 0.019(3) C6 0.123(3) 0.0445(15) 0.067(2) -0.0074(14) -0.0169(19) 0.0116(17) C7 0.097(2) 0.0473(15) 0.0572(17) 0.0020(13) 0.0018(15) 0.0075(15) C8 0.117(3) 0.0493(15) 0.0532(18) -0.0004(13) -0.0084(18) 0.0197(17) C9 0.140(4) 0.058(2) 0.061(2) -0.0085(16) -0.005(2) 0.027(2) C10 0.115(3) 0.076(2) 0.0604(19) -0.0034(17) 0.0099(19) 0.035(2) C11 0.092(2) 0.0628(17) 0.0554(18) 0.0064(14) 0.0056(16) 0.0233(17) C12 0.085(2) 0.083(2) 0.0626(19) 0.0031(17) 0.0109(17) 0.0278(19) C13 0.093(3) 0.149(4) 0.089(3) -0.030(3) 0.016(2) 0.031(3) C14 0.078(3) 0.218(7) 0.120(4) -0.047(4) 0.035(3) -0.002(4) C15 0.078(3) 0.161(5) 0.114(4) -0.025(3) 0.032(3) -0.020(3) C16A 0.071(3) 0.164(6) 0.122(5) 0.000(5) 0.031(3) -0.022(4) C17A 0.073(3) 0.126(5) 0.128(5) -0.009(4) 0.018(3) -0.031(3) C16B 0.17(2) 0.142(19) 0.070(11) -0.002(11) 0.033(13) 0.100(17) C17B 0.105(17) 0.24(4) 0.124(19) 0.03(2) 0.052(15) 0.021(18) C18 0.076(2) 0.095(3) 0.110(3) 0.003(2) 0.014(2) -0.024(2) C19 0.087(2) 0.082(2) 0.108(3) -0.003(2) 0.000(2) -0.031(2) C20 0.077(2) 0.0559(16) 0.088(2) 0.0028(16) -0.0027(17) -0.0107(15) C21 0.0725(19) 0.0494(15) 0.081(2) 0.0015(15) 0.0089(16) -0.0057(14) C22 0.067(2) 0.0694(19) 0.089(2) 0.0067(17) 0.0118(17) -0.0044(16) C23 0.070(2) 0.090(2) 0.083(2) 0.0105(19) 0.0158(18) 0.0033(19) C24 0.086(2) 0.0479(15) 0.084(2) 0.0012(15) -0.0079(18) -0.0141(15) C25 0.080(2) 0.070(2) 0.099(3) 0.002(2) -0.015(2) -0.0157(17) C26 0.091(3) 0.119(3) 0.134(4) -0.012(3) -0.023(3) 0.005(3) C27 0.092(3) 0.078(2) 0.084(2) -0.0016(19) -0.021(2) -0.020(2) C28 0.091(2) 0.0535(17) 0.077(2) 0.0001(16) -0.0167(18) -0.0173(16) C29 0.111(3) 0.080(2) 0.085(3) -0.0163(19) -0.017(2) 0.001(2) C30 0.092(2) 0.0446(15) 0.079(2) 0.0012(15) -0.0140(18) -0.0055(15) C31 0.093(2) 0.0470(15) 0.078(2) 0.0002(15) -0.0161(17) -0.0047(15) C32 0.127(3) 0.089(3) 0.089(3) -0.019(2) -0.036(2) 0.029(2) C33 0.164(5) 0.087(3) 0.076(3) 0.018(2) -0.023(3) -0.031(3) C34 0.127(3) 0.0471(16) 0.075(2) 0.0019(15) -0.018(2) -0.0046(18) C35 0.141(4) 0.0560(18) 0.098(3) 0.0027(19) -0.027(3) -0.004(2) P1A 0.0497(18) 0.109(4) 0.084(2) 0.024(2) -0.0142(16) -0.0034(19) F1A 0.065(4) 0.270(13) 0.116(5) -0.005(8) 0.001(3) 0.030(6) F2A 0.096(5) 0.189(9) 0.152(6) 0.067(6) -0.018(4) -0.059(6) F3A 0.231(11) 0.206(9) 0.283(12) 0.115(9) -0.055(10) 0.052(9) F4A 0.121(6) 0.129(5) 0.149(7) 0.018(5) -0.061(6) -0.005(4) F5A 0.089(4) 0.198(9) 0.071(4) 0.014(5) -0.011(3) 0.004(6) F6A 0.146(6) 0.123(6) 0.152(7) -0.025(5) -0.048(5) 0.012(5) P1B 0.082(4) 0.123(6) 0.135(6) 0.033(4) -0.022(4) -0.004(4) F1B 0.153(12) 0.236(15) 0.157(12) 0.065(12) 0.010(10) -0.029(12) F2B 0.146(16) 0.181(16) 0.188(16) 0.057(14) 0.006(13) -0.002(13) F3B 0.23(2) 0.139(13) 0.26(2) 0.043(14) 0.046(16) 0.049(15) F4B 0.32(2) 0.271(19) 0.30(2) 0.033(17) -0.042(17) 0.056(17) F5B 0.24(2) 0.33(2) 0.25(2) -0.036(17) -0.036(16) -0.019(17) F6B 0.130(11) 0.231(19) 0.147(14) 0.009(12) -0.066(10) 0.005(12) P1C 0.133(10) 0.129(9) 0.131(9) -0.025(6) -0.017(7) 0.029(7) F1C 0.073(7) 0.154(11) 0.132(11) -0.048(9) -0.039(7) 0.048(7) F2C 0.097(11) 0.227(17) 0.150(13) 0.007(12) 0.001(9) 0.097(12) F3C 0.077(7) 0.153(11) 0.092(8) 0.034(7) -0.028(5) 0.002(7) F4C 0.125(10) 0.170(15) 0.108(9) 0.036(9) -0.002(8) -0.001(11) F5C 0.194(18) 0.139(12) 0.218(16) 0.073(11) 0.044(14) 0.009(12) F6C 0.174(13) 0.126(10) 0.248(16) 0.000(10) 0.037(12) -0.076(10) C37 0.184(19) 0.27(3) 0.151(12) -0.08(3) 0.02(2) -0.03(2) C38 0.133(13) 0.171(16) 0.160(16) -0.041(12) 0.036(10) -0.063(13) N39 0.111(8) 0.169(12) 0.196(14) -0.063(11) -0.003(9) -0.019(8) N40 0.240(17) 0.23(2) 0.23(2) 0.039(16) -0.060(15) -0.155(17) C41 0.58(9) 0.14(2) 0.47(6) 0.11(3) -0.25(6) -0.21(4) C42 0.49(5) 0.34(4) 0.51(5) 0.33(4) -0.43(4) -0.34(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 Zn N2 2.035(3) . ? Zn N3 2.200(3) . ? Zn N1 2.206(3) . ? O1 C2 1.383(6) . ? O1 C1 1.441(6) . ? O2 C28 1.371(5) . ? O2 C29 1.405(5) . ? N1 C7 1.327(4) . ? N1 C11 1.343(4) . ? N2 C23 1.326(5) . ? N2 C12 1.339(4) . ? N3 C21 1.320(4) . ? N3 C22 1.354(4) . ? C1 H11 0.9800 . ? C1 H12 0.9800 . ? C1 H13 0.9800 . ? C2 C3 1.366(6) . ? C2 C35 1.369(6) . ? C3 C4 1.392(6) . ? C3 H3 0.9500 . ? C4 C6 1.408(5) . ? C4 C5 1.523(6) . ? C5 H51 0.9800 . ? C5 H52 0.9800 . ? C5 H53 0.9800 . ? C6 C34 1.397(5) . ? C6 C8 1.481(5) . ? C7 C8 1.403(4) . ? C7 H7 0.9500 . ? C8 C9 1.389(5) . ? C9 C10 1.361(6) . ? C9 H9 0.9500 . ? C10 C11 1.393(5) . ? C10 C16B 1.453(9) . ? C10 H10 0.9500 . ? C11 C12 1.469(5) . ? C12 C13 1.397(6) . ? C13 C14 1.372(8) . ? C13 C17B 1.456(9) . ? C13 H131 0.9500 . ? C14 C15 1.414(7) . ? C14 H14 0.9500 . ? C15 C23 1.392(5) . ? C15 C16A 1.462(7) . ? C15 H15 0.9500 . ? C16A C17A 1.340(9) . ? C16A H161 0.9500 . ? C17A C18 1.450(6) . ? C17A H171 0.9500 . ? C16B C17B 1.333(13) . ? C16B H162 0.9500 . ? C17B H172 0.9500 . ? C18 C19 1.392(6) . ? C18 C22 1.399(5) . ? C18 H18 0.9500 . ? C19 C20 1.385(5) . ? C19 H19 0.9500 . ? C20 C21 1.404(4) . ? C20 C24 1.482(5) . ? C21 H21 0.9500 . ? C22 C23 1.450(5) . ? C24 C31 1.402(5) . ? C24 C25 1.415(5) . ? C25 C27 1.386(5) . ? C25 C26 1.491(6) . ? C26 H261 0.9800 . ? C26 H262 0.9800 . ? C26 H263 0.9800 . ? C27 C28 1.373(5) . ? C27 H27 0.9500 . ? C28 C30 1.378(5) . ? C29 H291 0.9800 . ? C29 H292 0.9800 . ? C29 H293 0.9800 . ? C30 C31 1.383(5) . ? C30 H30 0.9500 . ? C31 C32 1.528(5) . ? C32 H321 0.9800 . ? C32 H322 0.9800 . ? C32 H323 0.9800 . ? C33 C34 1.504(5) . ? C33 H331 0.9800 . ? C33 H332 0.9800 . ? C33 H333 0.9800 . ? C34 C35 1.371(6) . ? C35 H35 0.9500 . ? P1A F2A 1.558(3) . ? P1A F6A 1.559(3) . ? P1A F3A 1.559(3) . ? P1A F5A 1.559(3) . ? P1A F4A 1.559(3) . ? P1A F1A 1.560(3) . ? P1B F6B 1.558(3) . ? P1B F1B 1.558(3) . ? P1B F4B 1.559(3) . ? P1B F3B 1.559(3) . ? P1B F5B 1.559(3) . ? P1B F2B 1.559(3) . ? P1C F6C 1.559(3) . ? P1C F4C 1.559(3) . ? P1C F2C 1.559(3) . ? P1C F3C 1.559(3) . ? P1C F5C 1.559(3) . ? P1C F1C 1.560(3) . ? C37 C38 1.450(5) . ? C37 H371 0.9800 . ? C37 H372 0.9800 . ? C37 H373 0.9800 . ? C38 N39 1.139(5) . ? N40 C41 1.139(5) . ? C41 C42 1.451(5) . ? C42 H421 0.9800 . ? C42 H422 0.9800 . ? C42 H423 0.9800 . ? 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 N2 Zn N2 179.10(14) . 4_755 ? N2 Zn N3 77.38(10) . . ? N2 Zn N3 103.30(10) . 4_755 ? N3 Zn N3 86.62(14) . 4_755 ? N2 Zn N1 75.67(11) . . ? N3 Zn N1 153.04(10) . . ? N2 Zn N1 103.66(10) . 4_755 ? N3 Zn N1 100.09(9) . 4_755 ? N1 Zn N1 85.75(13) . 4_755 ? C2 O1 C1 117.0(4) . . ? C28 O2 C29 116.9(3) . . ? C7 N1 C11 119.6(3) . . ? C7 N1 Zn 125.9(2) . . ? C11 N1 Zn 113.4(2) . . ? C23 N2 C12 122.0(3) . . ? C23 N2 Zn 117.8(2) . . ? C12 N2 Zn 120.2(2) . . ? C21 N3 C22 118.5(3) . . ? C21 N3 Zn 129.9(2) . . ? C22 N3 Zn 110.9(2) . . ? O1 C1 H11 109.5 . . ? O1 C1 H12 109.5 . . ? H11 C1 H12 109.5 . . ? O1 C1 H13 109.5 . . ? H11 C1 H13 109.5 . . ? H12 C1 H13 109.5 . . ? C3 C2 C35 119.9(4) . . ? C3 C2 O1 124.6(4) . . ? C35 C2 O1 115.5(4) . . ? C2 C3 C4 120.6(4) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C3 C4 C6 119.8(4) . . ? C3 C4 C5 119.3(4) . . ? C6 C4 C5 120.8(4) . . ? C4 C5 H51 109.5 . . ? C4 C5 H52 109.5 . . ? H51 C5 H52 109.5 . . ? C4 C5 H53 109.5 . . ? H51 C5 H53 109.5 . . ? H52 C5 H53 109.5 . . ? C34 C6 C4 118.0(4) . . ? C34 C6 C8 121.2(3) . . ? C4 C6 C8 120.8(3) . . ? N1 C7 C8 123.6(3) . . ? N1 C7 H7 118.2 . . ? C8 C7 H7 118.2 . . ? C9 C8 C7 115.6(4) . . ? C9 C8 C6 124.3(3) . . ? C7 C8 C6 120.0(3) . . ? C10 C9 C8 121.2(3) . . ? C10 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? C9 C10 C11 119.5(3) . . ? C9 C10 C16B 131.9(8) . . ? C11 C10 C16B 107.1(8) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? N1 C11 C10 120.3(4) . . ? N1 C11 C12 115.4(3) . . ? C10 C11 C12 124.3(3) . . ? N2 C12 C13 118.8(4) . . ? N2 C12 C11 114.6(3) . . ? C13 C12 C11 126.6(4) . . ? C14 C13 C12 119.6(4) . . ? C14 C13 C17B 133.8(9) . . ? C12 C13 C17B 102.8(9) . . ? C14 C13 H131 120.2 . . ? C12 C13 H131 120.2 . . ? C13 C14 C15 121.4(4) . . ? C13 C14 H14 119.3 . . ? C15 C14 H14 119.3 . . ? C23 C15 C14 114.9(4) . . ? C23 C15 C16A 117.0(5) . . ? C14 C15 C16A 128.0(5) . . ? C23 C15 H15 122.5 . . ? C14 C15 H15 122.5 . . ? C17A C16A C15 121.9(5) . . ? C17A C16A H161 119.0 . . ? C15 C16A H161 119.0 . . ? C16A C17A C18 122.3(5) . . ? C16A C17A H171 118.9 . . ? C18 C17A H171 118.9 . . ? C17B C16B C10 125.5(16) . . ? C17B C16B H162 117.3 . . ? C10 C16B H162 117.3 . . ? C16B C17B C13 128.7(17) . . ? C16B C17B H172 115.6 . . ? C13 C17B H172 115.6 . . ? C19 C18 C22 118.2(3) . . ? C19 C18 C17A 125.3(4) . . ? C22 C18 C17A 116.4(4) . . ? C19 C18 H18 120.9 . . ? C22 C18 H18 120.9 . . ? C20 C19 C18 120.9(3) . . ? C20 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? C19 C20 C21 116.1(3) . . ? C19 C20 C24 124.2(3) . . ? C21 C20 C24 119.7(3) . . ? N3 C21 C20 124.6(3) . . ? N3 C21 H21 117.7 . . ? C20 C21 H21 117.7 . . ? N3 C22 C18 121.6(3) . . ? N3 C22 C23 116.6(3) . . ? C18 C22 C23 121.8(3) . . ? N2 C23 C15 123.2(4) . . ? N2 C23 C22 116.5(3) . . ? C15 C23 C22 120.3(4) . . ? C31 C24 C25 118.5(3) . . ? C31 C24 C20 120.4(3) . . ? C25 C24 C20 121.0(3) . . ? C27 C25 C24 119.0(3) . . ? C27 C25 C26 118.9(4) . . ? C24 C25 C26 122.1(4) . . ? C25 C26 H261 109.5 . . ? C25 C26 H262 109.5 . . ? H261 C26 H262 109.5 . . ? C25 C26 H263 109.5 . . ? H261 C26 H263 109.5 . . ? H262 C26 H263 109.5 . . ? C28 C27 C25 121.7(3) . . ? C28 C27 H27 119.2 . . ? C25 C27 H27 119.2 . . ? O2 C28 C27 116.1(3) . . ? O2 C28 C30 124.2(3) . . ? C27 C28 C30 119.8(4) . . ? O2 C29 H291 109.5 . . ? O2 C29 H292 109.5 . . ? H291 C29 H292 109.5 . . ? O2 C29 H293 109.5 . . ? H291 C29 H293 109.5 . . ? H292 C29 H293 109.5 . . ? C28 C30 C31 120.3(3) . . ? C28 C30 H30 119.9 . . ? C31 C30 H30 119.9 . . ? C30 C31 C24 120.8(3) . . ? C30 C31 C32 117.8(3) . . ? C24 C31 C32 121.4(3) . . ? C31 C32 H321 109.5 . . ? C31 C32 H322 109.5 . . ? H321 C32 H322 109.5 . . ? C31 C32 H323 109.5 . . ? H321 C32 H323 109.5 . . ? H322 C32 H323 109.5 . . ? C34 C33 H331 109.5 . . ? C34 C33 H332 109.5 . . ? H331 C33 H332 109.5 . . ? C34 C33 H333 109.5 . . ? H331 C33 H333 109.5 . . ? H332 C33 H333 109.5 . . ? C35 C34 C6 120.6(4) . . ? C35 C34 C33 118.3(4) . . ? C6 C34 C33 121.1(4) . . ? C2 C35 C34 121.1(4) . . ? C2 C35 H35 119.5 . . ? C34 C35 H35 119.5 . . ? F2A P1A F6A 89.9(3) . . ? F2A P1A F3A 90.5(3) . . ? F6A P1A F3A 89.9(3) . . ? F2A P1A F5A 90.6(3) . . ? F6A P1A F5A 178.9(3) . . ? F3A P1A F5A 89.2(3) . . ? F2A P1A F4A 89.4(3) . . ? F6A P1A F4A 89.9(3) . . ? F3A P1A F4A 179.8(4) . . ? F5A P1A F4A 91.0(3) . . ? F2A P1A F1A 179.7(4) . . ? F6A P1A F1A 90.2(3) . . ? F3A P1A F1A 89.8(3) . . ? F5A P1A F1A 89.2(3) . . ? F4A P1A F1A 90.3(3) . . ? F6B P1B F1B 90.2(3) . . ? F6B P1B F4B 89.6(3) . . ? F1B P1B F4B 90.5(3) . . ? F6B P1B F3B 90.6(3) . . ? F1B P1B F3B 90.1(3) . . ? F4B P1B F3B 179.3(4) . . ? F6B P1B F5B 179.3(4) . . ? F1B P1B F5B 89.8(3) . . ? F4B P1B F5B 89.7(3) . . ? F3B P1B F5B 90.1(3) . . ? F6B P1B F2B 90.1(3) . . ? F1B P1B F2B 179.6(4) . . ? F4B P1B F2B 89.7(3) . . ? F3B P1B F2B 89.6(3) . . ? F5B P1B F2B 89.9(3) . . ? F6C P1C F4C 89.5(3) . . ? F6C P1C F2C 90.1(3) . . ? F4C P1C F2C 90.6(3) . . ? F6C P1C F3C 90.4(3) . . ? F4C P1C F3C 179.1(4) . . ? F2C P1C F3C 90.3(3) . . ? F6C P1C F5C 179.6(4) . . ? F4C P1C F5C 90.1(3) . . ? F2C P1C F5C 89.9(3) . . ? F3C P1C F5C 90.0(3) . . ? F6C P1C F1C 90.2(3) . . ? F4C P1C F1C 90.0(3) . . ? F2C P1C F1C 179.4(4) . . ? F3C P1C F1C 89.2(3) . . ? F5C P1C F1C 89.8(3) . . ? C38 C37 H371 109.5 . . ? C38 C37 H372 109.5 . . ? H371 C37 H372 109.5 . . ? C38 C37 H373 109.4 . . ? H371 C37 H373 109.5 . . ? H372 C37 H373 109.5 . . ? N39 C38 C37 177.1(19) . . ? N40 C41 C42 154(6) . . ? C41 C42 H421 109.5 . . ? C41 C42 H422 109.5 . . ? H421 C42 H422 109.5 . . ? C41 C42 H423 109.5 . . ? H421 C42 H423 109.5 . . ? H422 C42 H423 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 N2 Zn N1 C7 -175.6(3) . . . . ? N2 Zn N1 C7 3.8(3) 4_755 . . . ? N3 Zn N1 C7 -174.3(2) . . . . ? N3 Zn N1 C7 83.1(2) 4_755 . . . ? N1 Zn N1 C7 -70.3(2) 4_755 . . . ? N2 Zn N1 C11 -7.54(19) . . . . ? N2 Zn N1 C11 171.9(2) 4_755 . . . ? N3 Zn N1 C11 -6.2(3) . . . . ? N3 Zn N1 C11 -108.8(2) 4_755 . . . ? N1 Zn N1 C11 97.7(2) 4_755 . . . ? N3 Zn N2 C23 5.8(2) . . . . ? N3 Zn N2 C23 -77.6(3) 4_755 . . . ? N1 Zn N2 C23 -174.8(3) . . . . ? N1 Zn N2 C23 103.3(3) 4_755 . . . ? N3 Zn N2 C12 -174.9(3) . . . . ? N3 Zn N2 C12 101.7(2) 4_755 . . . ? N1 Zn N2 C12 4.5(2) . . . . ? N1 Zn N2 C12 -77.4(2) 4_755 . . . ? N2 Zn N3 C21 -178.1(3) . . . . ? N2 Zn N3 C21 2.6(3) 4_755 . . . ? N3 Zn N3 C21 -73.6(3) 4_755 . . . ? N1 Zn N3 C21 -179.4(2) . . . . ? N1 Zn N3 C21 80.1(3) 4_755 . . . ? N2 Zn N3 C22 -7.6(2) . . . . ? N2 Zn N3 C22 173.0(2) 4_755 . . . ? N3 Zn N3 C22 96.8(2) 4_755 . . . ? N1 Zn N3 C22 -8.9(3) . . . . ? N1 Zn N3 C22 -109.5(2) 4_755 . . . ? C1 O1 C2 C3 11.5(7) . . . . ? C1 O1 C2 C35 -169.6(5) . . . . ? C35 C2 C3 C4 -0.3(6) . . . . ? O1 C2 C3 C4 178.5(4) . . . . ? C2 C3 C4 C6 -0.5(6) . . . . ? C2 C3 C4 C5 176.7(4) . . . . ? C3 C4 C6 C34 0.9(5) . . . . ? C5 C4 C6 C34 -176.3(3) . . . . ? C3 C4 C6 C8 179.4(3) . . . . ? C5 C4 C6 C8 2.2(5) . . . . ? C11 N1 C7 C8 -2.3(4) . . . . ? Zn N1 C7 C8 165.0(2) . . . . ? N1 C7 C8 C9 2.3(4) . . . . ? N1 C7 C8 C6 -175.8(3) . . . . ? C34 C6 C8 C9 -120.0(4) . . . . ? C4 C6 C8 C9 61.6(4) . . . . ? C34 C6 C8 C7 58.0(4) . . . . ? C4 C6 C8 C7 -120.4(3) . . . . ? C7 C8 C9 C10 -0.2(5) . . . . ? C6 C8 C9 C10 177.9(3) . . . . ? C8 C9 C10 C11 -1.8(5) . . . . ? C8 C9 C10 C16B -166.0(10) . . . . ? C7 N1 C11 C10 0.1(4) . . . . ? Zn N1 C11 C10 -168.7(2) . . . . ? C7 N1 C11 C12 178.3(3) . . . . ? Zn N1 C11 C12 9.4(3) . . . . ? C9 C10 C11 N1 1.9(5) . . . . ? C16B C10 C11 N1 169.6(8) . . . . ? C9 C10 C11 C12 -176.0(3) . . . . ? C16B C10 C11 C12 -8.3(9) . . . . ? C23 N2 C12 C13 -0.1(5) . . . . ? Zn N2 C12 C13 -179.4(3) . . . . ? C23 N2 C12 C11 178.3(3) . . . . ? Zn N2 C12 C11 -1.0(4) . . . . ? N1 C11 C12 N2 -6.0(4) . . . . ? C10 C11 C12 N2 172.1(3) . . . . ? N1 C11 C12 C13 172.3(4) . . . . ? C10 C11 C12 C13 -9.7(6) . . . . ? N2 C12 C13 C14 1.9(7) . . . . ? C11 C12 C13 C14 -176.3(5) . . . . ? N2 C12 C13 C17B -159.1(11) . . . . ? C11 C12 C13 C17B 22.7(12) . . . . ? C12 C13 C14 C15 -0.2(9) . . . . ? C17B C13 C14 C15 153.6(15) . . . . ? C13 C14 C15 C23 -3.0(9) . . . . ? C13 C14 C15 C16A 174.0(6) . . . . ? C23 C15 C16A C17A -6.4(10) . . . . ? C14 C15 C16A C17A 176.6(7) . . . . ? C15 C16A C17A C18 2.9(11) . . . . ? C9 C10 C16B C17B 175.0(18) . . . . ? C11 C10 C16B C17B 9(2) . . . . ? C10 C16B C17B C13 8(4) . . . . ? C14 C13 C17B C16B -179.2(19) . . . . ? C12 C13 C17B C16B -22(3) . . . . ? C16A C17A C18 C19 179.9(6) . . . . ? C16A C17A C18 C22 0.5(9) . . . . ? C22 C18 C19 C20 -0.3(6) . . . . ? C17A C18 C19 C20 -179.6(5) . . . . ? C18 C19 C20 C21 0.1(6) . . . . ? C18 C19 C20 C24 179.5(4) . . . . ? C22 N3 C21 C20 -0.5(5) . . . . ? Zn N3 C21 C20 169.3(2) . . . . ? C19 C20 C21 N3 0.3(5) . . . . ? C24 C20 C21 N3 -179.1(3) . . . . ? C21 N3 C22 C18 0.3(5) . . . . ? Zn N3 C22 C18 -171.4(3) . . . . ? C21 N3 C22 C23 -179.8(3) . . . . ? Zn N3 C22 C23 8.5(4) . . . . ? C19 C18 C22 N3 0.1(6) . . . . ? C17A C18 C22 N3 179.5(4) . . . . ? C19 C18 C22 C23 -179.8(4) . . . . ? C17A C18 C22 C23 -0.4(7) . . . . ? C12 N2 C23 C15 -3.4(6) . . . . ? Zn N2 C23 C15 175.9(4) . . . . ? C12 N2 C23 C22 177.6(3) . . . . ? Zn N2 C23 C22 -3.1(4) . . . . ? C14 C15 C23 N2 4.8(7) . . . . ? C16A C15 C23 N2 -172.5(5) . . . . ? C14 C15 C23 C22 -176.2(5) . . . . ? C16A C15 C23 C22 6.4(7) . . . . ? N3 C22 C23 N2 -4.1(5) . . . . ? C18 C22 C23 N2 175.7(4) . . . . ? N3 C22 C23 C15 176.8(4) . . . . ? C18 C22 C23 C15 -3.3(6) . . . . ? C19 C20 C24 C31 -120.7(4) . . . . ? C21 C20 C24 C31 58.8(4) . . . . ? C19 C20 C24 C25 61.4(5) . . . . ? C21 C20 C24 C25 -119.2(4) . . . . ? C31 C24 C25 C27 1.0(5) . . . . ? C20 C24 C25 C27 179.0(3) . . . . ? C31 C24 C25 C26 -177.0(4) . . . . ? C20 C24 C25 C26 1.0(5) . . . . ? C24 C25 C27 C28 -0.2(5) . . . . ? C26 C25 C27 C28 178.0(4) . . . . ? C29 O2 C28 C27 176.3(3) . . . . ? C29 O2 C28 C30 -3.6(5) . . . . ? C25 C27 C28 O2 179.0(3) . . . . ? C25 C27 C28 C30 -1.1(5) . . . . ? O2 C28 C30 C31 -178.7(3) . . . . ? C27 C28 C30 C31 1.4(5) . . . . ? C28 C30 C31 C24 -0.5(5) . . . . ? C28 C30 C31 C32 179.8(3) . . . . ? C25 C24 C31 C30 -0.7(5) . . . . ? C20 C24 C31 C30 -178.7(3) . . . . ? C25 C24 C31 C32 179.0(3) . . . . ? C20 C24 C31 C32 0.9(5) . . . . ? C4 C6 C34 C35 -0.5(5) . . . . ? C8 C6 C34 C35 -179.0(3) . . . . ? C4 C6 C34 C33 -179.4(4) . . . . ? C8 C6 C34 C33 2.1(5) . . . . ? C3 C2 C35 C34 0.7(7) . . . . ? O1 C2 C35 C34 -178.2(4) . . . . ? C6 C34 C35 C2 -0.3(6) . . . . ? C33 C34 C35 C2 178.6(4) . . . . ? #===END data_3b _database_code_depnum_ccdc_archive 'CCDC 735257' # SG0403 _audit_creation_method SHELXL-97 _audit_creation_date 04-02-26 _chemical_name_systematic ; bis[5,5"-bis-(4-methoxy-2,6-dimethylphenyl)- [2,2':6,2"]terpyridine]iron(II) hexafluorophosphate hexa-acetonitrile solvate ; _chemical_name_common ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_moiety 'C66 H62 Fe N6 O4 2+, 2(F6 P 1-), 6(C2 H3 N)' _chemical_formula_sum 'C78 H80 F12 Fe N12 O4 P2' _chemical_formula_weight 1595.33 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 312 0.0033 0.0016 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; H H 320 0.0000 0.0000 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; F F 48 0.0171 0.0103 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; Fe Fe 4 0.3463 0.8444 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; N N 48 0.0061 0.0033 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; O O 16 0.0106 0.0060 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; P P 8 0.1023 0.0942 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall ? _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 29.7492(10) _cell_length_b 11.4106(4) _cell_length_c 22.7396(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.062(2) _cell_angle_gamma 90.00 _cell_volume 7719.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 160(1) _cell_measurement_reflns_used 140202 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.373 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3312 _exptl_absorpt_coefficient_mu 0.323 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Blessing, 1995)' _exptl_absorpt_correction_T_min 0.743 _exptl_absorpt_correction_T_max 0.994 _exptl_special_details ; Solvent used: MeCN / diethylether Cooling Device: Oxford Cryosystems Cryostream 700 Crystal mount: glued on a glass fibre Mosaicity (deg.): 1.378(1) Frames collected: 512 Seconds exposure per frame: 48 Degrees rotation per frame: 0.8 Crystal-Detector distance (mm): 34.3 ; _diffrn_ambient_temperature 160(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Nonius FR590 sealed tube generator' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_detector '65 mm CCD camera on \k goniostat' _diffrn_measurement_device_type 'Nonius KappaCCD area-detector diffractometer' _diffrn_measurement_method '\f and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 43088 _diffrn_reflns_av_R_equivalents 0.0676 _diffrn_reflns_av_sigmaI/netI 0.0426 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 25.01 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.997 _reflns_number_total 6783 _reflns_number_gt 5116 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'COLLECT (Nonius, 2000)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN and SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'SHELXL97 and PLATON (Spek, 2009)' _refine_special_details ; The asymmetric unit contains one half of a cation with the Fe-atom on a two-fold axis, one anion and three acetonitrile molecules. The PF6- anion is disordered. Two sets of P- and F-atoms were defined for this anion and refinement of the site occupation factors led to a value of 0.654(7), for the major orientation. The P-F and F...F distances were restrained tightly, so as to maintain octahedral geometry and uniform P-F bond lengths and neighbouring atoms within and between each disordered orientation were restrained to have similar atomic displacement parameters. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0486P)^2^+15.9333P] 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 SHELXL _refine_ls_extinction_coef 0.00065(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6782 _refine_ls_number_parameters 566 _refine_ls_number_restraints 543 _refine_ls_R_factor_all 0.0769 _refine_ls_R_factor_gt 0.0497 _refine_ls_wR_factor_ref 0.1255 _refine_ls_wR_factor_gt 0.1108 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.103 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.482 _refine_diff_density_min -0.464 _refine_diff_density_rms 0.068 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 Fe Fe 0.5000 0.19560(5) 0.7500 0.02361(17) Uani 1 2 d S . . O1 O 0.49328(7) 0.7626(2) 1.04869(8) 0.0404(5) Uani 1 1 d . . . O2 O 0.27623(7) -0.3576(2) 0.66466(12) 0.0571(7) Uani 1 1 d . . . N1 N 0.53500(7) 0.32062(19) 0.78892(9) 0.0254(5) Uani 1 1 d . . . N2 N 0.55099(7) 0.19523(19) 0.70137(9) 0.0243(5) Uani 1 1 d . . . N3 N 0.48153(7) 0.07097(19) 0.69501(9) 0.0244(5) Uani 1 1 d . . . C1 C 0.44908(11) 0.8096(3) 1.05099(14) 0.0443(8) Uani 1 1 d . . . H11 H 0.4441 0.8607 1.0169 0.067 Uiso 1 1 calc R . . H12 H 0.4454 0.8550 1.0872 0.067 Uiso 1 1 calc R . . H13 H 0.4272 0.7455 1.0503 0.067 Uiso 1 1 calc R . . C2 C 0.50308(10) 0.6912(2) 1.00173(12) 0.0315(7) Uani 1 1 d . . . C3 C 0.54608(10) 0.6450(3) 1.00076(12) 0.0340(7) Uani 1 1 d . . . H3 H 0.5662 0.6626 1.0320 0.041 Uiso 1 1 calc R . . C4 C 0.56042(9) 0.5738(3) 0.95541(12) 0.0320(7) Uani 1 1 d . . . C5 C 0.60679(10) 0.5211(3) 0.95942(14) 0.0401(7) Uani 1 1 d . . . H51 H 0.6282 0.5712 0.9385 0.060 Uiso 1 1 calc R . . H52 H 0.6066 0.4429 0.9416 0.060 Uiso 1 1 calc R . . H53 H 0.6157 0.5149 1.0008 0.060 Uiso 1 1 calc R . . C6 C 0.53057(9) 0.5499(2) 0.90818(12) 0.0288(6) Uani 1 1 d . . . C7 C 0.52308(9) 0.3833(2) 0.83638(12) 0.0275(6) Uani 1 1 d . . . H7 H 0.4971 0.3595 0.8574 0.033 Uiso 1 1 calc R . . C8 C 0.54634(9) 0.4808(2) 0.85671(12) 0.0292(6) Uani 1 1 d . . . C9 C 0.58495(9) 0.5127(3) 0.82530(13) 0.0328(7) Uani 1 1 d . . . H9 H 0.6018 0.5794 0.8370 0.039 Uiso 1 1 calc R . . C10 C 0.59863(9) 0.4475(3) 0.77739(13) 0.0319(7) Uani 1 1 d . . . H10 H 0.6251 0.4683 0.7566 0.038 Uiso 1 1 calc R . . C11 C 0.57344(9) 0.3518(2) 0.75991(12) 0.0269(6) Uani 1 1 d . . . C12 C 0.58375(9) 0.2751(2) 0.70998(12) 0.0280(6) Uani 1 1 d . . . C13 C 0.62160(9) 0.2773(3) 0.67399(13) 0.0347(7) Uani 1 1 d . . . H131 H 0.6446 0.3339 0.6797 0.042 Uiso 1 1 calc R . . C14 C 0.62467(10) 0.1941(3) 0.62948(13) 0.0374(7) Uani 1 1 d . . . H14 H 0.6500 0.1945 0.6041 0.045 Uiso 1 1 calc R . . C15 C 0.59149(9) 0.1110(3) 0.62153(13) 0.0341(7) Uani 1 1 d . . . H15 H 0.5941 0.0533 0.5916 0.041 Uiso 1 1 calc R . . C16 C 0.55431(9) 0.1136(2) 0.65820(12) 0.0275(6) Uani 1 1 d . . . C17 C 0.51470(9) 0.0374(2) 0.65661(11) 0.0266(6) Uani 1 1 d . . . C18 C 0.50958(9) -0.0599(3) 0.62090(12) 0.0308(7) Uani 1 1 d . . . H18 H 0.5332 -0.0837 0.5955 0.037 Uiso 1 1 calc R . . C19 C 0.46963(9) -0.1222(3) 0.62263(12) 0.0307(7) Uani 1 1 d . . . H19 H 0.4661 -0.1899 0.5987 0.037 Uiso 1 1 calc R . . C20 C 0.43479(9) -0.0866(2) 0.65904(12) 0.0272(6) Uani 1 1 d . . . C21 C 0.44270(8) 0.0108(2) 0.69461(11) 0.0255(6) Uani 1 1 d . . . H21 H 0.4193 0.0361 0.7200 0.031 Uiso 1 1 calc R . . C22 C 0.39115(9) -0.1509(2) 0.66057(12) 0.0284(6) Uani 1 1 d . . . C23 C 0.36603(9) -0.1642(3) 0.60876(13) 0.0330(7) Uani 1 1 d . . . C24 C 0.37876(11) -0.1060(3) 0.55187(14) 0.0438(8) Uani 1 1 d . . . H241 H 0.3839 -0.0222 0.5587 0.066 Uiso 1 1 calc R . . H242 H 0.3544 -0.1160 0.5232 0.066 Uiso 1 1 calc R . . H243 H 0.4063 -0.1418 0.5366 0.066 Uiso 1 1 calc R . . C25 C 0.32684(10) -0.2321(3) 0.60977(14) 0.0388(8) Uani 1 1 d . . . H25 H 0.3097 -0.2415 0.5748 0.047 Uiso 1 1 calc R . . C26 C 0.31275(10) -0.2854(3) 0.66097(15) 0.0399(8) Uani 1 1 d . . . C27 C 0.25267(13) -0.3825(4) 0.6109(2) 0.0731(13) Uani 1 1 d . . . H271 H 0.2387 -0.3106 0.5960 0.110 Uiso 1 1 calc R . . H272 H 0.2293 -0.4413 0.6183 0.110 Uiso 1 1 calc R . . H273 H 0.2739 -0.4127 0.5816 0.110 Uiso 1 1 calc R . . C28 C 0.33688(10) -0.2695(3) 0.71259(14) 0.0390(7) Uani 1 1 d . . . H28 H 0.3266 -0.3044 0.7480 0.047 Uiso 1 1 calc R . . C29 C 0.37601(9) -0.2029(3) 0.71279(13) 0.0323(7) Uani 1 1 d . . . C30 C 0.40209(11) -0.1935(3) 0.76989(14) 0.0460(8) Uani 1 1 d . . . H301 H 0.3977 -0.1154 0.7869 0.069 Uiso 1 1 calc R . . H302 H 0.4341 -0.2060 0.7622 0.069 Uiso 1 1 calc R . . H303 H 0.3913 -0.2530 0.7976 0.069 Uiso 1 1 calc R . . C31 C 0.45232(10) 0.5714(3) 0.86277(14) 0.0418(8) Uani 1 1 d . . . H311 H 0.4398 0.4926 0.8677 0.063 Uiso 1 1 calc R . . H312 H 0.4667 0.5774 0.8241 0.063 Uiso 1 1 calc R . . H313 H 0.4281 0.6294 0.8656 0.063 Uiso 1 1 calc R . . C32 C 0.48666(9) 0.5943(2) 0.91020(12) 0.0290(6) Uani 1 1 d . . . C33 C 0.47320(9) 0.6650(2) 0.95705(12) 0.0297(6) Uani 1 1 d . . . H33 H 0.4434 0.6951 0.9582 0.036 Uiso 1 1 calc R . . C34 C 0.20890(13) 0.5097(4) 0.7527(2) 0.0733(12) Uani 1 1 d . . . H341 H 0.2123 0.5933 0.7440 0.110 Uiso 1 1 calc R . . H342 H 0.1890 0.4999 0.7867 0.110 Uiso 1 1 calc R . . H343 H 0.1959 0.4696 0.7186 0.110 Uiso 1 1 calc R . . C35 C 0.25221(15) 0.4601(5) 0.76582(19) 0.0744(13) Uani 1 1 d . . . N36 N 0.28618(15) 0.4225(5) 0.7755(2) 0.128(2) Uani 1 1 d . . . C37 C 0.19463(13) 0.8306(4) 0.8812(2) 0.0686(12) Uani 1 1 d . . . H371 H 0.2253 0.8118 0.8687 0.103 Uiso 1 1 calc R . . H372 H 0.1931 0.8312 0.9242 0.103 Uiso 1 1 calc R . . H373 H 0.1862 0.9079 0.8660 0.103 Uiso 1 1 calc R . . C38 C 0.16403(12) 0.7432(4) 0.85843(17) 0.0531(9) Uani 1 1 d . . . N39 N 0.14013(13) 0.6759(4) 0.84039(18) 0.0792(11) Uani 1 1 d . . . C40 C 0.24792(15) 0.5277(4) 0.9291(2) 0.0809(14) Uani 1 1 d . . . H401 H 0.2630 0.5789 0.9008 0.121 Uiso 1 1 calc R . . H402 H 0.2398 0.5731 0.9641 0.121 Uiso 1 1 calc R . . H403 H 0.2207 0.4950 0.9113 0.121 Uiso 1 1 calc R . . C41 C 0.27783(15) 0.4335(4) 0.9458(2) 0.0712(12) Uani 1 1 d . . . N42 N 0.30074(15) 0.3579(4) 0.9580(2) 0.0972(14) Uani 1 1 d . . . P1A P 0.33508(7) 0.81661(16) 0.93634(9) 0.0375(6) Uani 0.654(7) 1 d PDU A 1 F1A F 0.38482(9) 0.8397(3) 0.91458(16) 0.0644(16) Uani 0.654(7) 1 d PDU A 1 F2A F 0.28539(8) 0.7937(3) 0.95820(17) 0.0601(12) Uani 0.654(7) 1 d PDU A 1 F3A F 0.31850(12) 0.8110(5) 0.87032(11) 0.0776(14) Uani 0.654(7) 1 d PDU A 1 F4A F 0.35168(12) 0.8224(4) 1.00244(10) 0.0681(12) Uani 0.654(7) 1 d PDU A 1 F5A F 0.32605(14) 0.95331(19) 0.9373(2) 0.0695(13) Uani 0.654(7) 1 d PDU A 1 F6A F 0.34419(12) 0.68010(18) 0.9355(3) 0.0778(13) Uani 0.654(7) 1 d PDU A 1 P1B P 0.33658(14) 0.8168(3) 0.92851(17) 0.0436(11) Uani 0.346(7) 1 d PDU A 2 F1B F 0.38804(15) 0.8354(6) 0.9136(3) 0.047(2) Uani 0.346(7) 1 d PDU A 2 F2B F 0.28515(15) 0.7984(6) 0.9435(3) 0.064(2) Uani 0.346(7) 1 d PDU A 2 F3B F 0.3232(2) 0.8746(7) 0.8677(2) 0.066(2) Uani 0.346(7) 1 d PDU A 2 F4B F 0.3500(2) 0.7592(8) 0.9893(3) 0.075(2) Uani 0.346(7) 1 d PDU A 2 F5B F 0.3352(3) 0.9416(5) 0.9589(3) 0.067(2) Uani 0.346(7) 1 d PDU A 2 F6B F 0.3380(2) 0.6922(4) 0.8982(4) 0.072(2) Uani 0.346(7) 1 d PDU A 2 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 Fe 0.0202(3) 0.0240(3) 0.0266(3) 0.000 0.0035(2) 0.000 O1 0.0414(12) 0.0490(14) 0.0308(11) -0.0091(10) -0.0008(9) 0.0019(10) O2 0.0379(13) 0.0530(16) 0.0803(18) 0.0020(13) -0.0016(12) -0.0173(12) N1 0.0229(12) 0.0256(13) 0.0277(12) 0.0027(10) 0.0016(9) 0.0012(10) N2 0.0225(11) 0.0231(12) 0.0271(12) 0.0014(10) 0.0012(9) 0.0016(10) N3 0.0212(11) 0.0251(12) 0.0269(12) 0.0013(10) 0.0010(9) 0.0018(9) C1 0.0448(19) 0.052(2) 0.0363(18) -0.0100(15) 0.0024(14) 0.0046(16) C2 0.0409(17) 0.0280(16) 0.0256(14) 0.0004(12) 0.0023(12) -0.0042(13) C3 0.0376(17) 0.0352(17) 0.0294(16) 0.0018(13) -0.0051(12) -0.0069(14) C4 0.0336(16) 0.0288(16) 0.0336(16) 0.0032(13) -0.0015(12) -0.0029(13) C5 0.0386(17) 0.0397(19) 0.0421(18) -0.0014(15) -0.0041(14) -0.0011(14) C6 0.0339(15) 0.0224(15) 0.0300(15) 0.0003(12) 0.0012(12) -0.0053(12) C7 0.0249(14) 0.0267(15) 0.0307(15) 0.0024(12) 0.0010(11) 0.0002(12) C8 0.0295(15) 0.0267(16) 0.0315(15) 0.0020(12) -0.0027(12) -0.0007(12) C9 0.0312(15) 0.0281(16) 0.0391(17) 0.0016(13) -0.0009(13) -0.0052(13) C10 0.0263(15) 0.0317(17) 0.0378(17) 0.0017(13) 0.0057(12) -0.0038(13) C11 0.0231(14) 0.0288(15) 0.0287(15) 0.0033(12) 0.0029(11) 0.0002(12) C12 0.0247(14) 0.0271(16) 0.0322(15) 0.0034(12) 0.0005(11) 0.0009(12) C13 0.0251(15) 0.0388(18) 0.0403(17) 0.0002(14) 0.0075(12) -0.0035(13) C14 0.0266(15) 0.0441(19) 0.0415(17) -0.0043(15) 0.0130(13) -0.0002(14) C15 0.0280(15) 0.0381(18) 0.0363(17) -0.0048(13) 0.0103(12) 0.0023(13) C16 0.0243(14) 0.0285(16) 0.0298(15) 0.0029(12) 0.0014(11) 0.0028(12) C17 0.0247(14) 0.0292(16) 0.0260(14) 0.0013(12) 0.0004(11) 0.0047(12) C18 0.0263(15) 0.0357(17) 0.0306(15) -0.0037(13) 0.0077(12) 0.0038(13) C19 0.0310(15) 0.0309(16) 0.0302(15) -0.0054(12) 0.0013(12) 0.0020(13) C20 0.0270(14) 0.0260(15) 0.0284(15) 0.0025(12) -0.0012(11) -0.0002(12) C21 0.0214(14) 0.0269(15) 0.0282(14) 0.0016(12) 0.0025(11) 0.0027(11) C22 0.0267(14) 0.0232(15) 0.0352(16) -0.0034(12) 0.0035(12) 0.0010(12) C23 0.0306(16) 0.0294(17) 0.0390(17) -0.0034(13) -0.0015(13) 0.0032(13) C24 0.0420(18) 0.047(2) 0.0425(19) 0.0013(15) -0.0058(14) -0.0044(15) C25 0.0311(16) 0.0349(18) 0.0504(19) -0.0054(15) -0.0094(14) 0.0006(14) C26 0.0254(15) 0.0326(18) 0.062(2) 0.0000(15) 0.0026(14) -0.0039(13) C27 0.046(2) 0.063(3) 0.111(4) 0.014(2) -0.029(2) -0.019(2) C28 0.0349(17) 0.0347(18) 0.0474(19) 0.0011(14) 0.0093(14) -0.0003(14) C29 0.0299(15) 0.0301(16) 0.0367(16) -0.0022(13) 0.0054(12) 0.0016(13) C30 0.048(2) 0.052(2) 0.0376(18) 0.0056(15) 0.0023(14) -0.0087(16) C31 0.0368(17) 0.049(2) 0.0400(18) -0.0081(15) -0.0062(14) 0.0083(15) C32 0.0320(15) 0.0267(15) 0.0284(15) 0.0012(12) -0.0007(12) -0.0032(12) C33 0.0317(15) 0.0276(16) 0.0297(15) 0.0023(12) 0.0032(12) -0.0012(12) C34 0.046(2) 0.076(3) 0.098(3) 0.007(3) 0.011(2) 0.003(2) C35 0.051(2) 0.097(4) 0.075(3) 0.016(3) 0.013(2) 0.011(2) N36 0.070(3) 0.192(6) 0.121(4) 0.064(4) 0.022(3) 0.050(3) C37 0.052(2) 0.071(3) 0.083(3) -0.004(2) -0.009(2) -0.009(2) C38 0.042(2) 0.054(2) 0.063(2) 0.002(2) -0.0035(18) 0.0037(19) N39 0.063(2) 0.076(3) 0.099(3) -0.010(2) -0.012(2) -0.013(2) C40 0.068(3) 0.066(3) 0.109(4) -0.018(3) 0.013(3) -0.008(2) C41 0.056(3) 0.069(3) 0.089(3) -0.027(3) 0.004(2) -0.010(2) N42 0.085(3) 0.091(3) 0.116(4) -0.033(3) -0.018(3) 0.009(3) P1A 0.0267(10) 0.0451(11) 0.0407(10) 0.0052(9) 0.0008(8) -0.0035(9) F1A 0.038(3) 0.075(3) 0.080(3) 0.018(3) 0.005(3) -0.007(3) F2A 0.037(2) 0.088(3) 0.056(2) -0.0051(19) 0.0125(15) -0.014(2) F3A 0.056(2) 0.135(4) 0.0419(19) -0.003(2) -0.0061(16) -0.006(3) F4A 0.059(2) 0.099(3) 0.0467(19) -0.002(2) -0.0131(16) -0.007(2) F5A 0.053(2) 0.057(2) 0.099(3) 0.015(2) -0.006(2) 0.0115(17) F6A 0.066(2) 0.047(2) 0.121(4) -0.002(2) 0.010(3) -0.0005(17) P1B 0.033(2) 0.055(2) 0.0426(18) -0.0044(17) -0.0006(16) 0.0017(19) F1B 0.019(4) 0.061(5) 0.060(4) 0.015(4) 0.004(4) 0.005(4) F2B 0.033(4) 0.089(5) 0.071(4) -0.001(4) 0.003(3) -0.009(4) F3B 0.055(4) 0.090(5) 0.053(4) 0.028(3) -0.005(3) 0.019(4) F4B 0.063(3) 0.097(5) 0.064(4) 0.036(3) -0.006(3) -0.008(4) F5B 0.069(4) 0.068(4) 0.064(4) -0.032(3) 0.006(3) -0.009(3) F6B 0.071(4) 0.057(3) 0.089(4) -0.019(3) 0.026(4) -0.014(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 Fe N2 1.878(2) . ? Fe N3 1.971(2) . ? Fe N1 1.975(2) . ? O1 C2 1.375(3) . ? O1 C1 1.421(4) . ? O2 C26 1.366(4) . ? O2 C27 1.438(5) . ? N1 C7 1.343(3) . ? N1 C11 1.368(3) . ? N2 C12 1.348(3) . ? N2 C16 1.357(3) . ? N3 C21 1.344(3) . ? N3 C17 1.373(3) . ? C1 H11 0.9800 . ? C1 H12 0.9800 . ? C1 H13 0.9800 . ? C2 C33 1.382(4) . ? C2 C3 1.384(4) . ? C3 C4 1.381(4) . ? C3 H3 0.9500 . ? C4 C6 1.419(4) . ? C4 C5 1.508(4) . ? C5 H51 0.9800 . ? C5 H52 0.9800 . ? C5 H53 0.9800 . ? C6 C32 1.402(4) . ? C6 C8 1.487(4) . ? C7 C8 1.389(4) . ? C7 H7 0.9500 . ? C8 C9 1.401(4) . ? C9 C10 1.381(4) . ? C9 H9 0.9500 . ? C10 C11 1.382(4) . ? C10 H10 0.9500 . ? C11 C12 1.466(4) . ? C12 C13 1.393(4) . ? C13 C14 1.391(4) . ? C13 H131 0.9500 . ? C14 C15 1.381(4) . ? C14 H14 0.9500 . ? C15 C16 1.386(4) . ? C15 H15 0.9500 . ? C16 C17 1.465(4) . ? C17 C18 1.383(4) . ? C18 C19 1.386(4) . ? C18 H18 0.9500 . ? C19 C20 1.388(4) . ? C19 H19 0.9500 . ? C20 C21 1.394(4) . ? C20 C22 1.492(4) . ? C21 H21 0.9500 . ? C22 C29 1.402(4) . ? C22 C23 1.403(4) . ? C23 C25 1.400(4) . ? C23 C24 1.503(4) . ? C24 H241 0.9800 . ? C24 H242 0.9800 . ? C24 H243 0.9800 . ? C25 C26 1.380(5) . ? C25 H25 0.9500 . ? C26 C28 1.387(4) . ? C27 H271 0.9800 . ? C27 H272 0.9800 . ? C27 H273 0.9800 . ? C28 C29 1.390(4) . ? C28 H28 0.9500 . ? C29 C30 1.516(4) . ? C30 H301 0.9800 . ? C30 H302 0.9800 . ? C30 H303 0.9800 . ? C31 C32 1.508(4) . ? C31 H311 0.9800 . ? C31 H312 0.9800 . ? C31 H313 0.9800 . ? C32 C33 1.395(4) . ? C33 H33 0.9500 . ? C34 C35 1.438(6) . ? C34 H341 0.9800 . ? C34 H342 0.9800 . ? C34 H343 0.9800 . ? C35 N36 1.119(5) . ? C37 C38 1.445(5) . ? C37 H371 0.9800 . ? C37 H372 0.9800 . ? C37 H373 0.9800 . ? C38 N39 1.124(5) . ? C40 C41 1.445(7) . ? C40 H401 0.9800 . ? C40 H402 0.9800 . ? C40 H403 0.9800 . ? C41 N42 1.134(6) . ? P1A F3A 1.5812(12) . ? P1A F6A 1.5812(12) . ? P1A F2A 1.5817(12) . ? P1A F4A 1.5829(12) . ? P1A F5A 1.5829(12) . ? P1A F1A 1.5830(12) . ? P1B F6B 1.5817(12) . ? P1B F2B 1.5819(12) . ? P1B F4B 1.5821(12) . ? P1B F3B 1.5821(12) . ? P1B F5B 1.5825(12) . ? P1B F1B 1.5826(12) . ? 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 N2 Fe N2 179.75(14) . 2_656 ? N2 Fe N3 98.45(9) . 2_656 ? N2 Fe N3 81.36(9) . . ? N3 Fe N3 87.66(13) 2_656 . ? N2 Fe N1 80.77(9) . . ? N3 Fe N1 162.12(8) . . ? N2 Fe N1 99.42(9) . 2_656 ? N3 Fe N1 95.19(9) . 2_656 ? N1 Fe N1 87.51(13) . 2_656 ? C2 O1 C1 116.7(2) . . ? C26 O2 C27 117.0(3) . . ? C7 N1 C11 118.1(2) . . ? C7 N1 Fe 127.26(18) . . ? C11 N1 Fe 114.37(18) . . ? C12 N2 C16 121.1(2) . . ? C12 N2 Fe 119.80(18) . . ? C16 N2 Fe 119.13(18) . . ? C21 N3 C17 118.1(2) . . ? C21 N3 Fe 127.72(18) . . ? C17 N3 Fe 113.88(17) . . ? O1 C1 H11 109.5 . . ? O1 C1 H12 109.5 . . ? H11 C1 H12 109.5 . . ? O1 C1 H13 109.5 . . ? H11 C1 H13 109.5 . . ? H12 C1 H13 109.5 . . ? O1 C2 C33 124.2(3) . . ? O1 C2 C3 115.8(3) . . ? C33 C2 C3 120.0(3) . . ? C4 C3 C2 121.5(3) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C3 C4 C6 119.0(3) . . ? C3 C4 C5 118.2(3) . . ? C6 C4 C5 122.7(3) . . ? C4 C5 H51 109.5 . . ? C4 C5 H52 109.5 . . ? H51 C5 H52 109.5 . . ? C4 C5 H53 109.5 . . ? H51 C5 H53 109.5 . . ? H52 C5 H53 109.5 . . ? C32 C6 C4 119.2(3) . . ? C32 C6 C8 120.8(2) . . ? C4 C6 C8 120.0(2) . . ? N1 C7 C8 124.2(2) . . ? N1 C7 H7 117.9 . . ? C8 C7 H7 117.9 . . ? C7 C8 C9 116.5(3) . . ? C7 C8 C6 121.9(2) . . ? C9 C8 C6 121.6(3) . . ? C10 C9 C8 120.3(3) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C9 C10 C11 119.5(3) . . ? C9 C10 H10 120.3 . . ? C11 C10 H10 120.3 . . ? N1 C11 C10 121.3(3) . . ? N1 C11 C12 113.2(2) . . ? C10 C11 C12 125.5(2) . . ? N2 C12 C13 120.8(3) . . ? N2 C12 C11 111.4(2) . . ? C13 C12 C11 127.9(3) . . ? C14 C13 C12 118.0(3) . . ? C14 C13 H131 121.0 . . ? C12 C13 H131 121.0 . . ? C15 C14 C13 121.1(3) . . ? C15 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? C14 C15 C16 118.5(3) . . ? C14 C15 H15 120.7 . . ? C16 C15 H15 120.7 . . ? N2 C16 C15 120.6(3) . . ? N2 C16 C17 111.5(2) . . ? C15 C16 C17 127.9(3) . . ? N3 C17 C18 121.2(2) . . ? N3 C17 C16 113.4(2) . . ? C18 C17 C16 125.4(2) . . ? C17 C18 C19 119.3(2) . . ? C17 C18 H18 120.4 . . ? C19 C18 H18 120.4 . . ? C18 C19 C20 120.5(3) . . ? C18 C19 H19 119.8 . . ? C20 C19 H19 119.8 . . ? C19 C20 C21 117.0(2) . . ? C19 C20 C22 121.4(2) . . ? C21 C20 C22 121.6(2) . . ? N3 C21 C20 123.7(2) . . ? N3 C21 H21 118.1 . . ? C20 C21 H21 118.1 . . ? C29 C22 C23 119.6(3) . . ? C29 C22 C20 120.6(2) . . ? C23 C22 C20 119.8(2) . . ? C25 C23 C22 119.3(3) . . ? C25 C23 C24 118.0(3) . . ? C22 C23 C24 122.7(3) . . ? C23 C24 H241 109.5 . . ? C23 C24 H242 109.5 . . ? H241 C24 H242 109.5 . . ? C23 C24 H243 109.5 . . ? H241 C24 H243 109.5 . . ? H242 C24 H243 109.5 . . ? C26 C25 C23 120.8(3) . . ? C26 C25 H25 119.6 . . ? C23 C25 H25 119.6 . . ? O2 C26 C25 124.1(3) . . ? O2 C26 C28 116.0(3) . . ? C25 C26 C28 119.9(3) . . ? O2 C27 H271 109.5 . . ? O2 C27 H272 109.5 . . ? H271 C27 H272 109.5 . . ? O2 C27 H273 109.5 . . ? H271 C27 H273 109.5 . . ? H272 C27 H273 109.5 . . ? C26 C28 C29 120.5(3) . . ? C26 C28 H28 119.8 . . ? C29 C28 H28 119.8 . . ? C28 C29 C22 119.9(3) . . ? C28 C29 C30 118.0(3) . . ? C22 C29 C30 122.1(3) . . ? C29 C30 H301 109.5 . . ? C29 C30 H302 109.5 . . ? H301 C30 H302 109.5 . . ? C29 C30 H303 109.5 . . ? H301 C30 H303 109.5 . . ? H302 C30 H303 109.5 . . ? C32 C31 H311 109.5 . . ? C32 C31 H312 109.5 . . ? H311 C31 H312 109.5 . . ? C32 C31 H313 109.5 . . ? H311 C31 H313 109.5 . . ? H312 C31 H313 109.5 . . ? C33 C32 C6 120.1(3) . . ? C33 C32 C31 116.9(3) . . ? C6 C32 C31 123.0(2) . . ? C2 C33 C32 120.1(3) . . ? C2 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? C35 C34 H341 109.5 . . ? C35 C34 H342 109.5 . . ? H341 C34 H342 109.5 . . ? C35 C34 H343 109.5 . . ? H341 C34 H343 109.5 . . ? H342 C34 H343 109.5 . . ? N36 C35 C34 179.1(6) . . ? C38 C37 H371 109.5 . . ? C38 C37 H372 109.5 . . ? H371 C37 H372 109.5 . . ? C38 C37 H373 109.5 . . ? H371 C37 H373 109.5 . . ? H372 C37 H373 109.5 . . ? N39 C38 C37 179.5(5) . . ? C41 C40 H401 109.5 . . ? C41 C40 H402 109.5 . . ? H401 C40 H402 109.5 . . ? C41 C40 H403 109.5 . . ? H401 C40 H403 109.5 . . ? H402 C40 H403 109.5 . . ? N42 C41 C40 178.4(5) . . ? F3A P1A F6A 90.08(4) . . ? F3A P1A F2A 90.06(4) . . ? F6A P1A F2A 90.08(4) . . ? F3A P1A F4A 179.92(7) . . ? F6A P1A F4A 90.00(4) . . ? F2A P1A F4A 89.96(4) . . ? F3A P1A F5A 90.00(4) . . ? F6A P1A F5A 179.88(7) . . ? F2A P1A F5A 90.00(4) . . ? F4A P1A F5A 89.92(4) . . ? F3A P1A F1A 90.04(4) . . ? F6A P1A F1A 90.00(4) . . ? F2A P1A F1A 179.88(7) . . ? F4A P1A F1A 89.94(4) . . ? F5A P1A F1A 89.93(4) . . ? F6B P1B F2B 90.04(4) . . ? F6B P1B F4B 90.02(4) . . ? F2B P1B F4B 90.01(4) . . ? F6B P1B F3B 90.02(4) . . ? F2B P1B F3B 90.01(4) . . ? F4B P1B F3B 179.95(8) . . ? F6B P1B F5B 179.96(8) . . ? F2B P1B F5B 90.00(4) . . ? F4B P1B F5B 89.99(4) . . ? F3B P1B F5B 89.97(4) . . ? F6B P1B F1B 90.00(4) . . ? F2B P1B F1B 179.96(8) . . ? F4B P1B F1B 89.98(4) . . ? F3B P1B F1B 89.99(4) . . ? F5B P1B F1B 89.96(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Fe N1 C7 180.0(2) . . . . ? N2 Fe N1 C7 -0.2(2) 2_656 . . . ? N3 Fe N1 C7 -82.3(2) 2_656 . . . ? N3 Fe N1 C7 179.2(3) . . . . ? N1 Fe N1 C7 80.0(2) 2_656 . . . ? N2 Fe N1 C11 6.53(18) . . . . ? N2 Fe N1 C11 -173.64(18) 2_656 . . . ? N3 Fe N1 C11 104.28(19) 2_656 . . . ? N3 Fe N1 C11 5.8(4) . . . . ? N1 Fe N1 C11 -93.43(19) 2_656 . . . ? N3 Fe N2 C12 -98.1(2) 2_656 . . . ? N3 Fe N2 C12 175.5(2) . . . . ? N1 Fe N2 C12 -4.2(2) . . . . ? N1 Fe N2 C12 81.7(2) 2_656 . . . ? N3 Fe N2 C16 81.4(2) 2_656 . . . ? N3 Fe N2 C16 -4.87(19) . . . . ? N1 Fe N2 C16 175.4(2) . . . . ? N1 Fe N2 C16 -98.7(2) 2_656 . . . ? N2 Fe N3 C21 -178.4(2) . . . . ? N2 Fe N3 C21 1.8(2) 2_656 . . . ? N3 Fe N3 C21 82.7(2) 2_656 . . . ? N1 Fe N3 C21 -177.6(3) . . . . ? N1 Fe N3 C21 -79.6(2) 2_656 . . . ? N2 Fe N3 C17 7.76(18) . . . . ? N2 Fe N3 C17 -172.07(18) 2_656 . . . ? N3 Fe N3 C17 -91.16(19) 2_656 . . . ? N1 Fe N3 C17 8.5(4) . . . . ? N1 Fe N3 C17 106.52(18) 2_656 . . . ? C1 O1 C2 C33 1.3(4) . . . . ? C1 O1 C2 C3 -179.1(3) . . . . ? O1 C2 C3 C4 -178.7(3) . . . . ? C33 C2 C3 C4 0.9(4) . . . . ? C2 C3 C4 C6 1.4(4) . . . . ? C2 C3 C4 C5 -176.4(3) . . . . ? C3 C4 C6 C32 -3.1(4) . . . . ? C5 C4 C6 C32 174.6(3) . . . . ? C3 C4 C6 C8 175.4(3) . . . . ? C5 C4 C6 C8 -6.9(4) . . . . ? C11 N1 C7 C8 2.6(4) . . . . ? Fe N1 C7 C8 -170.6(2) . . . . ? N1 C7 C8 C9 -1.0(4) . . . . ? N1 C7 C8 C6 177.5(2) . . . . ? C32 C6 C8 C7 -53.5(4) . . . . ? C4 C6 C8 C7 128.0(3) . . . . ? C32 C6 C8 C9 124.9(3) . . . . ? C4 C6 C8 C9 -53.6(4) . . . . ? C7 C8 C9 C10 -1.0(4) . . . . ? C6 C8 C9 C10 -179.5(3) . . . . ? C8 C9 C10 C11 1.3(4) . . . . ? C7 N1 C11 C10 -2.2(4) . . . . ? Fe N1 C11 C10 171.8(2) . . . . ? C7 N1 C11 C12 178.3(2) . . . . ? Fe N1 C11 C12 -7.6(3) . . . . ? C9 C10 C11 N1 0.4(4) . . . . ? C9 C10 C11 C12 179.8(3) . . . . ? C16 N2 C12 C13 1.2(4) . . . . ? Fe N2 C12 C13 -179.2(2) . . . . ? C16 N2 C12 C11 -178.4(2) . . . . ? Fe N2 C12 C11 1.2(3) . . . . ? N1 C11 C12 N2 4.3(3) . . . . ? C10 C11 C12 N2 -175.1(3) . . . . ? N1 C11 C12 C13 -175.2(3) . . . . ? C10 C11 C12 C13 5.3(5) . . . . ? N2 C12 C13 C14 -0.6(4) . . . . ? C11 C12 C13 C14 178.9(3) . . . . ? C12 C13 C14 C15 -0.7(5) . . . . ? C13 C14 C15 C16 1.4(5) . . . . ? C12 N2 C16 C15 -0.5(4) . . . . ? Fe N2 C16 C15 180.0(2) . . . . ? C12 N2 C16 C17 -179.3(2) . . . . ? Fe N2 C16 C17 1.1(3) . . . . ? C14 C15 C16 N2 -0.8(4) . . . . ? C14 C15 C16 C17 177.8(3) . . . . ? C21 N3 C17 C18 -3.9(4) . . . . ? Fe N3 C17 C18 170.7(2) . . . . ? C21 N3 C17 C16 176.3(2) . . . . ? Fe N3 C17 C16 -9.2(3) . . . . ? N2 C16 C17 N3 5.4(3) . . . . ? C15 C16 C17 N3 -173.3(3) . . . . ? N2 C16 C17 C18 -174.5(3) . . . . ? C15 C16 C17 C18 6.8(5) . . . . ? N3 C17 C18 C19 2.1(4) . . . . ? C16 C17 C18 C19 -178.0(3) . . . . ? C17 C18 C19 C20 1.0(4) . . . . ? C18 C19 C20 C21 -2.3(4) . . . . ? C18 C19 C20 C22 178.6(3) . . . . ? C17 N3 C21 C20 2.6(4) . . . . ? Fe N3 C21 C20 -171.1(2) . . . . ? C19 C20 C21 N3 0.4(4) . . . . ? C22 C20 C21 N3 179.6(2) . . . . ? C19 C20 C22 C29 119.1(3) . . . . ? C21 C20 C22 C29 -60.0(4) . . . . ? C19 C20 C22 C23 -57.9(4) . . . . ? C21 C20 C22 C23 123.0(3) . . . . ? C29 C22 C23 C25 -1.8(4) . . . . ? C20 C22 C23 C25 175.2(3) . . . . ? C29 C22 C23 C24 176.7(3) . . . . ? C20 C22 C23 C24 -6.2(4) . . . . ? C22 C23 C25 C26 0.2(4) . . . . ? C24 C23 C25 C26 -178.4(3) . . . . ? C27 O2 C26 C25 2.9(5) . . . . ? C27 O2 C26 C28 -175.4(3) . . . . ? C23 C25 C26 O2 -176.5(3) . . . . ? C23 C25 C26 C28 1.7(5) . . . . ? O2 C26 C28 C29 176.4(3) . . . . ? C25 C26 C28 C29 -1.9(5) . . . . ? C26 C28 C29 C22 0.3(4) . . . . ? C26 C28 C29 C30 -177.1(3) . . . . ? C23 C22 C29 C28 1.5(4) . . . . ? C20 C22 C29 C28 -175.5(3) . . . . ? C23 C22 C29 C30 178.9(3) . . . . ? C20 C22 C29 C30 1.9(4) . . . . ? C4 C6 C32 C33 2.5(4) . . . . ? C8 C6 C32 C33 -176.0(3) . . . . ? C4 C6 C32 C31 -178.7(3) . . . . ? C8 C6 C32 C31 2.8(4) . . . . ? O1 C2 C33 C32 178.0(3) . . . . ? C3 C2 C33 C32 -1.6(4) . . . . ? C6 C32 C33 C2 -0.2(4) . . . . ? C31 C32 C33 C2 -179.1(3) . . . . ? #===END data_4b _database_code_depnum_ccdc_archive 'CCDC 735258' # SG0417 _audit_creation_method SHELXL-97 _audit_creation_date 04-06-30 _chemical_name_systematic ; bis[5,5"-bis-(4-methoxy-2,6-dimethylphenyl)- [2,2':6,2"]terpyridine]cobalt(II) hexafluorophosphate hexa-acetonitrile solvate ; _chemical_name_common ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_moiety 'C66 H62 Co N6 O4 2+, 2(F6 P 1-), 6(C2 H3 N)' _chemical_formula_sum 'C78 H80 Co F12 N12 O4 P2' _chemical_formula_weight 1598.43 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 312 0.0033 0.0016 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; H H 320 0.0000 0.0000 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; Co Co 4 0.3494 0.9721 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; F F 48 0.0171 0.0103 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; N N 48 0.0061 0.0033 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; O O 16 0.0106 0.0060 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; P P 8 0.1023 0.0942 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall ? _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 29.5268(4) _cell_length_b 11.7893(3) _cell_length_c 22.4187(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.8473(15) _cell_angle_gamma 90.00 _cell_volume 7803.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 160(1) _cell_measurement_reflns_used 34748 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.361 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3316 _exptl_absorpt_coefficient_mu 0.347 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Blessing, 1995)' _exptl_absorpt_correction_T_min 0.819 _exptl_absorpt_correction_T_max 0.937 _exptl_special_details ; Solvent used: MeCN / diethylether Cooling Device: Oxford Cryosystems Cryostream 700 Crystal mount: glued on a glass fibre Mosaicity (deg.): 0.440(1) Frames collected: 314 Seconds exposure per frame: 20 Degrees rotation per frame: 1.7 Crystal-Detector distance (mm): 33.6 ; _diffrn_ambient_temperature 160(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Nonius FR590 sealed tube generator' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_detector '65 mm CCD camera on \k goniostat' _diffrn_measurement_device_type 'Nonius KappaCCD area-detector diffractometer' _diffrn_measurement_method '\f and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 62530 _diffrn_reflns_av_R_equivalents 0.0937 _diffrn_reflns_av_sigmaI/netI 0.0495 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 25.03 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.999 _reflns_number_total 6889 _reflns_number_gt 4796 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'COLLECT (Nonius, 2000)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN and SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'SHELXL97 and PLATON (Spek, 2009)' _refine_special_details ; The asymmetric unit contains one half of a cation with the Co-atom on a two-fold axis, one anion and three acetonitrile molecules. The PF6- anion is disordered. Two sets of P- and F-atoms were defined for this anion and refinement of the site occupation factors led to a value of 0.804(4) for the major orientation. The P-F and F...F distances were restrained tightly, so as to maintain octahedral geometry and uniform P-F bond lengths and neighbouring atoms within and between each disordered orientation were restrained to have similar atomic displacement parameters. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0765P)^2^+6.1100P] 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 SHELXL _refine_ls_extinction_coef 0.00064(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6887 _refine_ls_number_parameters 566 _refine_ls_number_restraints 555 _refine_ls_R_factor_all 0.0839 _refine_ls_R_factor_gt 0.0506 _refine_ls_wR_factor_ref 0.1421 _refine_ls_wR_factor_gt 0.1226 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.097 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.469 _refine_diff_density_min -0.483 _refine_diff_density_rms 0.063 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 Co Co 0.5000 0.19974(4) 0.7500 0.02854(19) Uani 1 2 d S . . O1 O 0.49270(7) 0.7567(2) 1.05002(9) 0.0447(6) Uani 1 1 d . . . O2 O 0.27759(8) -0.3480(2) 0.65337(13) 0.0652(7) Uani 1 1 d . . . N1 N 0.53700(7) 0.32653(19) 0.79127(11) 0.0315(6) Uani 1 1 d . . . N2 N 0.55183(7) 0.19885(18) 0.70216(10) 0.0272(5) Uani 1 1 d . . . N3 N 0.48165(7) 0.07352(19) 0.69108(10) 0.0284(5) Uani 1 1 d . . . C1 C 0.44802(11) 0.8029(3) 1.05081(15) 0.0481(9) Uani 1 1 d . . . H11 H 0.4438 0.8542 1.0168 0.072 Uiso 1 1 calc R . . H12 H 0.4438 0.8450 1.0880 0.072 Uiso 1 1 calc R . . H13 H 0.4258 0.7413 1.0482 0.072 Uiso 1 1 calc R . . C2 C 0.50297(10) 0.6890(3) 1.00238(13) 0.0346(7) Uani 1 1 d . . . C3 C 0.54635(10) 0.6428(3) 1.00326(14) 0.0383(7) Uani 1 1 d . . . H3 H 0.5661 0.6574 1.0362 0.046 Uiso 1 1 calc R . . C4 C 0.56110(9) 0.5761(3) 0.95704(13) 0.0355(7) Uani 1 1 d . . . C5 C 0.60800(10) 0.5238(3) 0.96235(15) 0.0458(8) Uani 1 1 d . . . H51 H 0.6294 0.5686 0.9390 0.069 Uiso 1 1 calc R . . H52 H 0.6071 0.4459 0.9471 0.069 Uiso 1 1 calc R . . H53 H 0.6178 0.5232 1.0043 0.069 Uiso 1 1 calc R . . C6 C 0.53212(9) 0.5546(2) 0.90762(13) 0.0317(7) Uani 1 1 d . . . C7 C 0.52495(9) 0.3903(2) 0.83756(13) 0.0322(7) Uani 1 1 d . . . H7 H 0.4990 0.3682 0.8592 0.039 Uiso 1 1 calc R . . C8 C 0.54807(9) 0.4871(2) 0.85610(13) 0.0320(7) Uani 1 1 d . . . C9 C 0.58636(9) 0.5155(3) 0.82368(13) 0.0356(7) Uani 1 1 d . . . H9 H 0.6033 0.5811 0.8343 0.043 Uiso 1 1 calc R . . C10 C 0.59996(9) 0.4497(3) 0.77636(13) 0.0346(7) Uani 1 1 d . . . H10 H 0.6263 0.4692 0.7548 0.042 Uiso 1 1 calc R . . C11 C 0.57480(9) 0.3546(2) 0.76050(13) 0.0304(7) Uani 1 1 d . . . C12 C 0.58467(9) 0.2765(2) 0.71135(13) 0.0305(7) Uani 1 1 d . . . C13 C 0.62330(9) 0.2770(3) 0.67638(14) 0.0378(7) Uani 1 1 d . . . H131 H 0.6462 0.3327 0.6822 0.045 Uiso 1 1 calc R . . C14 C 0.62752(10) 0.1943(3) 0.63298(14) 0.0404(8) Uani 1 1 d . . . H14 H 0.6536 0.1933 0.6087 0.048 Uiso 1 1 calc R . . C15 C 0.59417(9) 0.1131(3) 0.62461(13) 0.0353(7) Uani 1 1 d . . . H15 H 0.5974 0.0554 0.5954 0.042 Uiso 1 1 calc R . . C16 C 0.55602(9) 0.1178(2) 0.65974(12) 0.0302(7) Uani 1 1 d . . . C17 C 0.51639(8) 0.0414(2) 0.65552(12) 0.0283(6) Uani 1 1 d . . . C18 C 0.51313(9) -0.0542(3) 0.62018(13) 0.0339(7) Uani 1 1 d . . . H18 H 0.5379 -0.0772 0.5965 0.041 Uiso 1 1 calc R . . C19 C 0.47328(9) -0.1164(2) 0.61963(13) 0.0333(7) Uani 1 1 d . . . H19 H 0.4708 -0.1827 0.5957 0.040 Uiso 1 1 calc R . . C20 C 0.43681(9) -0.0823(2) 0.65402(12) 0.0295(6) Uani 1 1 d . . . C21 C 0.44313(9) 0.0135(2) 0.68896(12) 0.0291(6) Uani 1 1 d . . . H21 H 0.4187 0.0381 0.7128 0.035 Uiso 1 1 calc R . . C22 C 0.39314(9) -0.1467(2) 0.65358(13) 0.0326(7) Uani 1 1 d . . . C23 C 0.36920(10) -0.1622(3) 0.59986(14) 0.0377(7) Uani 1 1 d . . . C24 C 0.38318(11) -0.1085(3) 0.54191(15) 0.0470(8) Uani 1 1 d . . . H241 H 0.3889 -0.0275 0.5482 0.071 Uiso 1 1 calc R . . H242 H 0.3589 -0.1180 0.5121 0.071 Uiso 1 1 calc R . . H243 H 0.4108 -0.1451 0.5278 0.071 Uiso 1 1 calc R . . C25 C 0.32982(10) -0.2287(3) 0.59925(16) 0.0431(8) Uani 1 1 d . . . H25 H 0.3135 -0.2398 0.5629 0.052 Uiso 1 1 calc R . . C26 C 0.31457(10) -0.2779(3) 0.65070(17) 0.0459(9) Uani 1 1 d . . . C27 C 0.25742(12) -0.3817(4) 0.5974(2) 0.0718(12) Uani 1 1 d . . . H271 H 0.2439 -0.3153 0.5777 0.108 Uiso 1 1 calc R . . H272 H 0.2339 -0.4385 0.6044 0.108 Uiso 1 1 calc R . . H273 H 0.2807 -0.4142 0.5718 0.108 Uiso 1 1 calc R . . C28 C 0.33732(10) -0.2587(3) 0.70446(16) 0.0453(8) Uani 1 1 d . . . H28 H 0.3258 -0.2900 0.7402 0.054 Uiso 1 1 calc R . . C29 C 0.37692(10) -0.1941(3) 0.70652(14) 0.0362(7) Uani 1 1 d . . . C30 C 0.40152(11) -0.1811(3) 0.76516(15) 0.0514(9) Uani 1 1 d . . . H301 H 0.3971 -0.1039 0.7803 0.077 Uiso 1 1 calc R . . H302 H 0.4339 -0.1951 0.7597 0.077 Uiso 1 1 calc R . . H303 H 0.3896 -0.2358 0.7939 0.077 Uiso 1 1 calc R . . C31 C 0.45413(10) 0.5781(3) 0.85777(14) 0.0452(8) Uani 1 1 d . . . H311 H 0.4406 0.5027 0.8622 0.068 Uiso 1 1 calc R . . H312 H 0.4696 0.5826 0.8195 0.068 Uiso 1 1 calc R . . H313 H 0.4303 0.6359 0.8591 0.068 Uiso 1 1 calc R . . C32 C 0.48794(9) 0.5983(2) 0.90800(12) 0.0317(7) Uani 1 1 d . . . C33 C 0.47390(9) 0.6653(2) 0.95551(13) 0.0328(7) Uani 1 1 d . . . H33 H 0.4440 0.6949 0.9555 0.039 Uiso 1 1 calc R . . C34 C 0.20824(12) 0.5113(4) 0.7403(2) 0.0777(13) Uani 1 1 d . . . H341 H 0.2114 0.5903 0.7273 0.117 Uiso 1 1 calc R . . H342 H 0.1882 0.5079 0.7746 0.117 Uiso 1 1 calc R . . H343 H 0.1953 0.4661 0.7075 0.117 Uiso 1 1 calc R . . C35 C 0.25182(14) 0.4669(4) 0.75672(19) 0.0757(13) Uani 1 1 d . . . N36 N 0.28620(14) 0.4354(5) 0.7700(2) 0.1222(19) Uani 1 1 d . . . C37 C 0.19321(13) 0.8289(4) 0.88429(19) 0.0673(11) Uani 1 1 d . . . H371 H 0.2253 0.8135 0.8769 0.101 Uiso 1 1 calc R . . H372 H 0.1879 0.8285 0.9273 0.101 Uiso 1 1 calc R . . H373 H 0.1851 0.9034 0.8678 0.101 Uiso 1 1 calc R . . C38 C 0.16586(12) 0.7431(4) 0.85610(18) 0.0578(10) Uani 1 1 d . . . N39 N 0.14432(12) 0.6761(3) 0.83359(19) 0.0834(11) Uani 1 1 d . . . C40 C 0.24646(14) 0.5331(4) 0.9205(2) 0.0797(13) Uani 1 1 d . . . H401 H 0.2619 0.5888 0.8956 0.120 Uiso 1 1 calc R . . H402 H 0.2371 0.5693 0.9577 0.120 Uiso 1 1 calc R . . H403 H 0.2197 0.5042 0.8991 0.120 Uiso 1 1 calc R . . C41 C 0.27681(14) 0.4404(4) 0.9340(2) 0.0675(11) Uani 1 1 d . . . N42 N 0.30013(14) 0.3665(4) 0.9447(2) 0.0908(13) Uani 1 1 d . . . P1A P 0.33489(4) 0.81502(10) 0.93646(5) 0.0383(4) Uani 0.804(4) 1 d PDU A 1 F1A F 0.38470(6) 0.8354(2) 0.91355(10) 0.0701(11) Uani 0.804(4) 1 d PDU A 1 F2A F 0.28518(5) 0.7948(2) 0.95949(10) 0.0738(10) Uani 0.804(4) 1 d PDU A 1 F3A F 0.31856(8) 0.7869(3) 0.87064(8) 0.0778(11) Uani 0.804(4) 1 d PDU A 1 F4A F 0.35127(7) 0.8433(3) 1.00238(7) 0.0723(9) Uani 0.804(4) 1 d PDU A 1 F5A F 0.32360(8) 0.94473(14) 0.92578(14) 0.0882(11) Uani 0.804(4) 1 d PDU A 1 F6A F 0.34635(8) 0.68554(13) 0.94726(15) 0.0801(10) Uani 0.804(4) 1 d PDU A 1 P1B P 0.33534(18) 0.8168(4) 0.9299(2) 0.0572(15) Uani 0.196(4) 1 d PDU A 2 F1B F 0.3860(2) 0.8443(8) 0.9132(4) 0.055(3) Uani 0.196(4) 1 d PDU A 2 F2B F 0.28464(19) 0.7893(8) 0.9466(4) 0.067(3) Uani 0.196(4) 1 d PDU A 2 F3B F 0.3188(3) 0.8630(9) 0.8671(3) 0.072(3) Uani 0.196(4) 1 d PDU A 2 F4B F 0.3519(3) 0.7706(9) 0.9928(3) 0.068(2) Uani 0.196(4) 1 d PDU A 2 F5B F 0.3302(3) 0.9397(6) 0.9573(4) 0.071(3) Uani 0.196(4) 1 d PDU A 2 F6B F 0.3405(3) 0.6938(5) 0.9026(5) 0.073(2) Uani 0.196(4) 1 d PDU A 2 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 Co 0.0268(3) 0.0247(3) 0.0340(3) 0.000 -0.0024(2) 0.000 O1 0.0456(12) 0.0552(15) 0.0332(12) -0.0085(11) -0.0027(9) 0.0024(11) O2 0.0434(14) 0.0547(16) 0.098(2) -0.0040(15) 0.0048(13) -0.0197(12) N1 0.0254(12) 0.0248(13) 0.0443(15) 0.0030(11) 0.0020(10) -0.0007(10) N2 0.0239(11) 0.0211(12) 0.0365(13) 0.0024(11) -0.0019(9) 0.0013(9) N3 0.0307(12) 0.0259(13) 0.0285(13) 0.0012(10) 0.0031(10) 0.0027(10) C1 0.050(2) 0.055(2) 0.0395(19) -0.0111(16) -0.0002(15) 0.0059(16) C2 0.0395(17) 0.0337(18) 0.0307(16) 0.0023(13) 0.0020(13) -0.0047(13) C3 0.0382(17) 0.0385(19) 0.0379(18) 0.0057(15) -0.0064(13) -0.0053(14) C4 0.0333(16) 0.0336(17) 0.0397(18) 0.0073(14) -0.0020(13) -0.0039(13) C5 0.0372(17) 0.046(2) 0.054(2) 0.0017(16) -0.0075(15) 0.0005(15) C6 0.0332(15) 0.0266(16) 0.0355(17) 0.0039(13) 0.0017(12) -0.0042(12) C7 0.0258(14) 0.0293(16) 0.0415(18) 0.0053(14) 0.0038(12) 0.0014(12) C8 0.0300(15) 0.0279(16) 0.0379(17) 0.0016(13) -0.0028(12) 0.0003(12) C9 0.0331(16) 0.0283(17) 0.0453(18) 0.0020(14) -0.0005(13) -0.0071(13) C10 0.0272(15) 0.0326(17) 0.0442(18) 0.0024(14) 0.0035(13) -0.0059(12) C11 0.0232(14) 0.0287(16) 0.0395(17) 0.0057(13) 0.0003(12) -0.0014(12) C12 0.0279(15) 0.0269(16) 0.0368(17) 0.0030(13) -0.0022(12) 0.0013(12) C13 0.0247(14) 0.0407(19) 0.0481(19) 0.0011(15) 0.0021(13) -0.0041(13) C14 0.0307(16) 0.046(2) 0.0443(19) -0.0025(16) 0.0086(13) -0.0006(14) C15 0.0317(16) 0.0400(19) 0.0344(17) -0.0032(14) 0.0055(12) 0.0014(13) C16 0.0324(15) 0.0279(16) 0.0303(16) 0.0027(13) -0.0001(12) 0.0011(12) C17 0.0256(14) 0.0297(16) 0.0297(15) 0.0022(13) 0.0014(11) 0.0057(12) C18 0.0305(15) 0.0362(18) 0.0352(17) -0.0056(14) 0.0066(12) 0.0039(13) C19 0.0330(15) 0.0299(16) 0.0371(17) -0.0079(13) -0.0007(12) 0.0022(13) C20 0.0314(15) 0.0252(16) 0.0318(16) 0.0012(13) 0.0013(12) 0.0016(12) C21 0.0286(15) 0.0271(16) 0.0318(16) 0.0024(13) 0.0066(11) 0.0046(12) C22 0.0267(15) 0.0249(16) 0.0464(19) -0.0007(14) 0.0047(13) 0.0030(12) C23 0.0340(16) 0.0305(17) 0.048(2) -0.0038(15) -0.0019(14) 0.0024(13) C24 0.0461(19) 0.048(2) 0.047(2) 0.0039(16) -0.0058(15) -0.0040(16) C25 0.0323(16) 0.0382(19) 0.058(2) -0.0047(16) -0.0063(15) 0.0004(14) C26 0.0268(16) 0.0358(19) 0.075(3) -0.0040(17) 0.0041(16) -0.0039(13) C27 0.044(2) 0.058(3) 0.113(4) -0.005(2) -0.013(2) -0.0172(18) C28 0.0383(18) 0.0349(19) 0.063(2) 0.0028(17) 0.0163(16) -0.0007(14) C29 0.0373(16) 0.0303(17) 0.0413(18) 0.0010(14) 0.0074(13) 0.0039(13) C30 0.052(2) 0.055(2) 0.047(2) 0.0073(17) 0.0087(16) -0.0042(17) C31 0.0388(17) 0.052(2) 0.0444(19) -0.0107(16) -0.0093(14) 0.0110(15) C32 0.0335(15) 0.0284(16) 0.0332(16) 0.0038(13) 0.0004(12) -0.0020(12) C33 0.0317(15) 0.0306(17) 0.0361(17) 0.0043(13) 0.0025(12) -0.0002(12) C34 0.048(2) 0.085(3) 0.100(3) 0.007(3) 0.003(2) 0.007(2) C35 0.054(2) 0.109(4) 0.065(3) 0.015(3) 0.009(2) 0.020(2) N36 0.067(3) 0.194(5) 0.106(3) 0.048(4) 0.016(2) 0.049(3) C37 0.052(2) 0.071(3) 0.078(3) -0.003(2) -0.011(2) -0.002(2) C38 0.041(2) 0.061(3) 0.071(3) 0.005(2) -0.0060(18) 0.0044(19) N39 0.064(2) 0.078(3) 0.107(3) -0.009(2) -0.017(2) -0.008(2) C40 0.070(3) 0.063(3) 0.106(4) -0.008(3) 0.009(2) 0.005(2) C41 0.055(2) 0.065(3) 0.082(3) -0.022(2) -0.002(2) -0.004(2) N42 0.077(3) 0.081(3) 0.114(3) -0.027(3) -0.018(2) 0.009(2) P1A 0.0261(7) 0.0440(8) 0.0446(7) 0.0078(6) 0.0009(6) -0.0012(6) F1A 0.0345(19) 0.091(2) 0.085(2) 0.024(2) 0.0085(18) 0.0003(18) F2A 0.0353(16) 0.121(3) 0.0653(19) -0.0022(18) 0.0082(13) -0.0157(17) F3A 0.0609(16) 0.128(3) 0.0442(15) -0.0014(17) -0.0066(12) -0.0112(19) F4A 0.0573(16) 0.098(3) 0.0615(17) -0.0156(17) -0.0104(13) -0.0092(17) F5A 0.0698(18) 0.0647(19) 0.130(3) 0.0211(19) -0.016(2) 0.0188(15) F6A 0.0828(19) 0.0441(17) 0.113(3) 0.0167(17) -0.0010(19) 0.0010(14) P1B 0.041(3) 0.067(3) 0.063(3) 0.004(3) -0.004(2) 0.000(3) F1B 0.028(5) 0.067(5) 0.071(6) 0.023(5) 0.008(5) -0.019(5) F2B 0.032(5) 0.095(6) 0.072(5) 0.004(5) 0.005(4) -0.012(5) F3B 0.055(5) 0.096(6) 0.065(5) 0.026(5) -0.011(4) 0.015(5) F4B 0.061(4) 0.078(5) 0.066(5) 0.032(4) -0.008(4) -0.003(4) F5B 0.067(5) 0.066(5) 0.079(5) -0.019(4) -0.005(4) 0.000(4) F6B 0.075(4) 0.064(5) 0.082(5) -0.001(5) 0.019(4) -0.002(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 Co N2 1.882(2) . ? Co N3 2.057(2) . ? Co N1 2.063(2) . ? O1 C2 1.371(4) . ? O1 C1 1.428(4) . ? O2 C26 1.371(4) . ? O2 C27 1.438(5) . ? N1 C7 1.334(4) . ? N1 C11 1.362(3) . ? N2 C12 1.347(3) . ? N2 C16 1.355(4) . ? N3 C21 1.340(3) . ? N3 C17 1.362(3) . ? C1 H11 0.9800 . ? C1 H12 0.9800 . ? C1 H13 0.9800 . ? C2 C33 1.376(4) . ? C2 C3 1.392(4) . ? C3 C4 1.377(4) . ? C3 H3 0.9500 . ? C4 C6 1.413(4) . ? C4 C5 1.519(4) . ? C5 H51 0.9800 . ? C5 H52 0.9800 . ? C5 H53 0.9800 . ? C6 C32 1.403(4) . ? C6 C8 1.485(4) . ? C7 C8 1.391(4) . ? C7 H7 0.9500 . ? C8 C9 1.394(4) . ? C9 C10 1.379(4) . ? C9 H9 0.9500 . ? C10 C11 1.388(4) . ? C10 H10 0.9500 . ? C11 C12 1.468(4) . ? C12 C13 1.394(4) . ? C13 C14 1.384(4) . ? C13 H131 0.9500 . ? C14 C15 1.384(4) . ? C14 H14 0.9500 . ? C15 C16 1.385(4) . ? C15 H15 0.9500 . ? C16 C17 1.479(4) . ? C17 C18 1.380(4) . ? C18 C19 1.386(4) . ? C18 H18 0.9500 . ? C19 C20 1.393(4) . ? C19 H19 0.9500 . ? C20 C21 1.385(4) . ? C20 C22 1.496(4) . ? C21 H21 0.9500 . ? C22 C23 1.399(4) . ? C22 C29 1.403(4) . ? C23 C25 1.402(4) . ? C23 C24 1.508(4) . ? C24 H241 0.9800 . ? C24 H242 0.9800 . ? C24 H243 0.9800 . ? C25 C26 1.373(5) . ? C25 H25 0.9500 . ? C26 C28 1.390(5) . ? C27 H271 0.9800 . ? C27 H272 0.9800 . ? C27 H273 0.9800 . ? C28 C29 1.396(4) . ? C28 H28 0.9500 . ? C29 C30 1.500(4) . ? C30 H301 0.9800 . ? C30 H302 0.9800 . ? C30 H303 0.9800 . ? C31 C32 1.513(4) . ? C31 H311 0.9800 . ? C31 H312 0.9800 . ? C31 H313 0.9800 . ? C32 C33 1.394(4) . ? C33 H33 0.9500 . ? C34 C35 1.432(5) . ? C34 H341 0.9800 . ? C34 H342 0.9800 . ? C34 H343 0.9800 . ? C35 N36 1.118(5) . ? C37 C38 1.436(6) . ? C37 H371 0.9800 . ? C37 H372 0.9800 . ? C37 H373 0.9800 . ? C38 N39 1.128(5) . ? C40 C41 1.442(6) . ? C40 H401 0.9800 . ? C40 H402 0.9800 . ? C40 H403 0.9800 . ? C41 N42 1.135(5) . ? P1A F3A 1.5808(11) . ? P1A F2A 1.5813(11) . ? P1A F6A 1.5813(11) . ? P1A F5A 1.5827(11) . ? P1A F1A 1.5834(11) . ? P1A F4A 1.5835(11) . ? P1B F6B 1.5820(11) . ? P1B F2B 1.5820(11) . ? P1B F3B 1.5821(11) . ? P1B F4B 1.5823(11) . ? P1B F5B 1.5824(11) . ? P1B F1B 1.5825(11) . ? 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 N2 Co N2 179.36(14) . 2_656 ? N2 Co N3 80.72(9) . . ? N2 Co N3 98.81(9) . 2_656 ? N3 Co N3 87.33(13) . 2_656 ? N2 Co N1 80.21(9) . . ? N3 Co N1 160.92(9) . . ? N2 Co N1 100.27(9) . 2_656 ? N3 Co N1 95.94(9) . 2_656 ? N1 Co N1 87.11(13) . 2_656 ? C2 O1 C1 116.6(2) . . ? C26 O2 C27 116.6(3) . . ? C7 N1 C11 119.2(2) . . ? C7 N1 Co 127.72(18) . . ? C11 N1 Co 112.42(19) . . ? C12 N2 C16 120.9(2) . . ? C12 N2 Co 119.91(19) . . ? C16 N2 Co 119.17(18) . . ? C21 N3 C17 118.6(2) . . ? C21 N3 Co 128.35(18) . . ? C17 N3 Co 112.54(17) . . ? O1 C1 H11 109.5 . . ? O1 C1 H12 109.5 . . ? H11 C1 H12 109.5 . . ? O1 C1 H13 109.5 . . ? H11 C1 H13 109.5 . . ? H12 C1 H13 109.5 . . ? O1 C2 C33 124.8(3) . . ? O1 C2 C3 115.5(3) . . ? C33 C2 C3 119.7(3) . . ? C4 C3 C2 120.9(3) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C3 C4 C6 119.9(3) . . ? C3 C4 C5 118.1(3) . . ? C6 C4 C5 122.0(3) . . ? C4 C5 H51 109.5 . . ? C4 C5 H52 109.5 . . ? H51 C5 H52 109.5 . . ? C4 C5 H53 109.5 . . ? H51 C5 H53 109.5 . . ? H52 C5 H53 109.5 . . ? C32 C6 C4 118.8(3) . . ? C32 C6 C8 120.5(3) . . ? C4 C6 C8 120.7(2) . . ? N1 C7 C8 124.0(3) . . ? N1 C7 H7 118.0 . . ? C8 C7 H7 118.0 . . ? C7 C8 C9 116.1(3) . . ? C7 C8 C6 120.8(2) . . ? C9 C8 C6 123.1(3) . . ? C10 C9 C8 120.9(3) . . ? C10 C9 H9 119.5 . . ? C8 C9 H9 119.5 . . ? C9 C10 C11 119.4(3) . . ? C9 C10 H10 120.3 . . ? C11 C10 H10 120.3 . . ? N1 C11 C10 120.4(3) . . ? N1 C11 C12 113.7(2) . . ? C10 C11 C12 125.9(3) . . ? N2 C12 C13 120.7(3) . . ? N2 C12 C11 113.0(2) . . ? C13 C12 C11 126.3(3) . . ? C14 C13 C12 118.4(3) . . ? C14 C13 H131 120.8 . . ? C12 C13 H131 120.8 . . ? C13 C14 C15 120.7(3) . . ? C13 C14 H14 119.6 . . ? C15 C14 H14 119.6 . . ? C14 C15 C16 118.6(3) . . ? C14 C15 H15 120.7 . . ? C16 C15 H15 120.7 . . ? N2 C16 C15 120.7(3) . . ? N2 C16 C17 113.2(2) . . ? C15 C16 C17 126.1(3) . . ? N3 C17 C18 121.1(2) . . ? N3 C17 C16 113.3(2) . . ? C18 C17 C16 125.6(2) . . ? C17 C18 C19 119.3(2) . . ? C17 C18 H18 120.4 . . ? C19 C18 H18 120.4 . . ? C18 C19 C20 120.4(3) . . ? C18 C19 H19 119.8 . . ? C20 C19 H19 119.8 . . ? C21 C20 C19 116.7(2) . . ? C21 C20 C22 121.8(2) . . ? C19 C20 C22 121.5(3) . . ? N3 C21 C20 123.9(2) . . ? N3 C21 H21 118.0 . . ? C20 C21 H21 118.0 . . ? C23 C22 C29 120.1(3) . . ? C23 C22 C20 119.7(3) . . ? C29 C22 C20 120.1(3) . . ? C22 C23 C25 119.3(3) . . ? C22 C23 C24 123.0(3) . . ? C25 C23 C24 117.6(3) . . ? C23 C24 H241 109.5 . . ? C23 C24 H242 109.5 . . ? H241 C24 H242 109.5 . . ? C23 C24 H243 109.5 . . ? H241 C24 H243 109.5 . . ? H242 C24 H243 109.5 . . ? C26 C25 C23 120.7(3) . . ? C26 C25 H25 119.7 . . ? C23 C25 H25 119.7 . . ? O2 C26 C25 124.2(3) . . ? O2 C26 C28 115.8(3) . . ? C25 C26 C28 120.0(3) . . ? O2 C27 H271 109.5 . . ? O2 C27 H272 109.5 . . ? H271 C27 H272 109.5 . . ? O2 C27 H273 109.5 . . ? H271 C27 H273 109.5 . . ? H272 C27 H273 109.5 . . ? C26 C28 C29 120.8(3) . . ? C26 C28 H28 119.6 . . ? C29 C28 H28 119.6 . . ? C28 C29 C22 119.1(3) . . ? C28 C29 C30 118.7(3) . . ? C22 C29 C30 122.2(3) . . ? C29 C30 H301 109.5 . . ? C29 C30 H302 109.5 . . ? H301 C30 H302 109.5 . . ? C29 C30 H303 109.5 . . ? H301 C30 H303 109.5 . . ? H302 C30 H303 109.5 . . ? C32 C31 H311 109.5 . . ? C32 C31 H312 109.5 . . ? H311 C31 H312 109.5 . . ? C32 C31 H313 109.5 . . ? H311 C31 H313 109.5 . . ? H312 C31 H313 109.5 . . ? C33 C32 C6 120.0(3) . . ? C33 C32 C31 117.2(3) . . ? C6 C32 C31 122.8(3) . . ? C2 C33 C32 120.6(3) . . ? C2 C33 H33 119.7 . . ? C32 C33 H33 119.7 . . ? C35 C34 H341 109.5 . . ? C35 C34 H342 109.5 . . ? H341 C34 H342 109.5 . . ? C35 C34 H343 109.5 . . ? H341 C34 H343 109.5 . . ? H342 C34 H343 109.5 . . ? N36 C35 C34 178.0(6) . . ? C38 C37 H371 109.5 . . ? C38 C37 H372 109.5 . . ? H371 C37 H372 109.5 . . ? C38 C37 H373 109.5 . . ? H371 C37 H373 109.5 . . ? H372 C37 H373 109.5 . . ? N39 C38 C37 179.5(5) . . ? C41 C40 H401 109.5 . . ? C41 C40 H402 109.5 . . ? H401 C40 H402 109.5 . . ? C41 C40 H403 109.5 . . ? H401 C40 H403 109.5 . . ? H402 C40 H403 109.5 . . ? N42 C41 C40 179.0(5) . . ? F3A P1A F2A 90.07(4) . . ? F3A P1A F6A 90.11(4) . . ? F2A P1A F6A 90.11(4) . . ? F3A P1A F5A 90.05(4) . . ? F2A P1A F5A 90.04(4) . . ? F6A P1A F5A 179.79(7) . . ? F3A P1A F1A 90.06(4) . . ? F2A P1A F1A 179.86(6) . . ? F6A P1A F1A 89.94(4) . . ? F5A P1A F1A 89.92(4) . . ? F3A P1A F4A 179.95(7) . . ? F2A P1A F4A 89.95(4) . . ? F6A P1A F4A 89.94(4) . . ? F5A P1A F4A 89.91(4) . . ? F1A P1A F4A 89.91(4) . . ? F6B P1B F2B 90.02(5) . . ? F6B P1B F3B 90.01(4) . . ? F2B P1B F3B 90.01(4) . . ? F6B P1B F4B 90.01(4) . . ? F2B P1B F4B 90.01(4) . . ? F3B P1B F4B 179.97(8) . . ? F6B P1B F5B 179.98(8) . . ? F2B P1B F5B 90.00(4) . . ? F3B P1B F5B 89.99(4) . . ? F4B P1B F5B 89.99(4) . . ? F6B P1B F1B 90.00(4) . . ? F2B P1B F1B 179.98(8) . . ? F3B P1B F1B 90.00(5) . . ? F4B P1B F1B 89.98(4) . . ? F5B P1B F1B 89.98(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 N2 Co N1 C7 178.2(2) . . . . ? N2 Co N1 C7 -2.2(3) 2_656 . . . ? N3 Co N1 C7 177.1(2) . . . . ? N3 Co N1 C7 -83.8(2) 2_656 . . . ? N1 Co N1 C7 77.3(2) 2_656 . . . ? N2 Co N1 C11 7.92(18) . . . . ? N2 Co N1 C11 -172.52(18) 2_656 . . . ? N3 Co N1 C11 6.8(4) . . . . ? N3 Co N1 C11 105.88(19) 2_656 . . . ? N1 Co N1 C11 -93.0(2) 2_656 . . . ? N2 Co N2 C12 -141.8(2) 2_656 . . . ? N3 Co N2 C12 175.1(2) . . . . ? N3 Co N2 C12 -99.0(2) 2_656 . . . ? N1 Co N2 C12 -4.5(2) . . . . ? N1 Co N2 C12 80.7(2) 2_656 . . . ? N2 Co N2 C16 36.5(2) 2_656 . . . ? N3 Co N2 C16 -6.5(2) . . . . ? N3 Co N2 C16 79.3(2) 2_656 . . . ? N1 Co N2 C16 173.9(2) . . . . ? N1 Co N2 C16 -100.9(2) 2_656 . . . ? N2 Co N3 C21 -179.1(2) . . . . ? N2 Co N3 C21 1.4(2) 2_656 . . . ? N3 Co N3 C21 81.6(2) 2_656 . . . ? N1 Co N3 C21 -178.0(2) . . . . ? N1 Co N3 C21 -79.6(2) 2_656 . . . ? N2 Co N3 C17 9.43(18) . . . . ? N2 Co N3 C17 -170.13(18) 2_656 . . . ? N3 Co N3 C17 -89.95(19) 2_656 . . . ? N1 Co N3 C17 10.5(4) . . . . ? N1 Co N3 C17 108.90(19) 2_656 . . . ? C1 O1 C2 C33 1.5(4) . . . . ? C1 O1 C2 C3 -178.6(3) . . . . ? O1 C2 C3 C4 -178.1(3) . . . . ? C33 C2 C3 C4 1.8(5) . . . . ? C2 C3 C4 C6 0.5(5) . . . . ? C2 C3 C4 C5 -177.1(3) . . . . ? C3 C4 C6 C32 -2.6(4) . . . . ? C5 C4 C6 C32 174.9(3) . . . . ? C3 C4 C6 C8 177.3(3) . . . . ? C5 C4 C6 C8 -5.2(4) . . . . ? C11 N1 C7 C8 1.8(4) . . . . ? Co N1 C7 C8 -167.9(2) . . . . ? N1 C7 C8 C9 -1.0(4) . . . . ? N1 C7 C8 C6 179.1(3) . . . . ? C32 C6 C8 C7 -56.5(4) . . . . ? C4 C6 C8 C7 123.6(3) . . . . ? C32 C6 C8 C9 123.6(3) . . . . ? C4 C6 C8 C9 -56.3(4) . . . . ? C7 C8 C9 C10 -0.3(4) . . . . ? C6 C8 C9 C10 179.6(3) . . . . ? C8 C9 C10 C11 0.7(4) . . . . ? C7 N1 C11 C10 -1.3(4) . . . . ? Co N1 C11 C10 169.9(2) . . . . ? C7 N1 C11 C12 179.0(2) . . . . ? Co N1 C11 C12 -9.8(3) . . . . ? C9 C10 C11 N1 0.1(4) . . . . ? C9 C10 C11 C12 179.8(3) . . . . ? C16 N2 C12 C13 1.6(4) . . . . ? Co N2 C12 C13 179.9(2) . . . . ? C16 N2 C12 C11 -177.9(2) . . . . ? Co N2 C12 C11 0.4(3) . . . . ? N1 C11 C12 N2 6.6(3) . . . . ? C10 C11 C12 N2 -173.2(3) . . . . ? N1 C11 C12 C13 -172.9(3) . . . . ? C10 C11 C12 C13 7.4(5) . . . . ? N2 C12 C13 C14 -1.4(4) . . . . ? C11 C12 C13 C14 178.0(3) . . . . ? C12 C13 C14 C15 -0.1(5) . . . . ? C13 C14 C15 C16 1.4(5) . . . . ? C12 N2 C16 C15 -0.2(4) . . . . ? Co N2 C16 C15 -178.6(2) . . . . ? C12 N2 C16 C17 -179.1(2) . . . . ? Co N2 C16 C17 2.6(3) . . . . ? C14 C15 C16 N2 -1.2(4) . . . . ? C14 C15 C16 C17 177.5(3) . . . . ? C21 N3 C17 C18 -3.3(4) . . . . ? Co N3 C17 C18 169.1(2) . . . . ? C21 N3 C17 C16 177.1(2) . . . . ? Co N3 C17 C16 -10.5(3) . . . . ? N2 C16 C17 N3 5.8(3) . . . . ? C15 C16 C17 N3 -173.0(3) . . . . ? N2 C16 C17 C18 -173.9(3) . . . . ? C15 C16 C17 C18 7.3(5) . . . . ? N3 C17 C18 C19 2.0(4) . . . . ? C16 C17 C18 C19 -178.4(3) . . . . ? C17 C18 C19 C20 0.5(4) . . . . ? C18 C19 C20 C21 -1.5(4) . . . . ? C18 C19 C20 C22 179.0(3) . . . . ? C17 N3 C21 C20 2.2(4) . . . . ? Co N3 C21 C20 -168.8(2) . . . . ? C19 C20 C21 N3 0.2(4) . . . . ? C22 C20 C21 N3 179.6(3) . . . . ? C21 C20 C22 C23 122.3(3) . . . . ? C19 C20 C22 C23 -58.3(4) . . . . ? C21 C20 C22 C29 -59.6(4) . . . . ? C19 C20 C22 C29 119.9(3) . . . . ? C29 C22 C23 C25 -2.2(4) . . . . ? C20 C22 C23 C25 176.0(3) . . . . ? C29 C22 C23 C24 176.6(3) . . . . ? C20 C22 C23 C24 -5.3(4) . . . . ? C22 C23 C25 C26 0.3(5) . . . . ? C24 C23 C25 C26 -178.5(3) . . . . ? C27 O2 C26 C25 7.8(5) . . . . ? C27 O2 C26 C28 -171.5(3) . . . . ? C23 C25 C26 O2 -177.0(3) . . . . ? C23 C25 C26 C28 2.3(5) . . . . ? O2 C26 C28 C29 176.3(3) . . . . ? C25 C26 C28 C29 -3.1(5) . . . . ? C26 C28 C29 C22 1.2(5) . . . . ? C26 C28 C29 C30 -176.8(3) . . . . ? C23 C22 C29 C28 1.4(4) . . . . ? C20 C22 C29 C28 -176.8(3) . . . . ? C23 C22 C29 C30 179.4(3) . . . . ? C20 C22 C29 C30 1.2(4) . . . . ? C4 C6 C32 C33 2.4(4) . . . . ? C8 C6 C32 C33 -177.5(3) . . . . ? C4 C6 C32 C31 -178.8(3) . . . . ? C8 C6 C32 C31 1.3(4) . . . . ? O1 C2 C33 C32 177.9(3) . . . . ? C3 C2 C33 C32 -2.0(4) . . . . ? C6 C32 C33 C2 -0.1(4) . . . . ? C31 C32 C33 C2 -179.0(3) . . . . ? #===END data_5b _database_code_depnum_ccdc_archive 'CCDC 735259' # SG0508 _audit_creation_method SHELXL-97 _audit_creation_date 05-05-19 _chemical_name_systematic ; bis[5,5"-bis-(4-methoxy-2,6-dimethylphenyl)- [2,2':6,2"]terpyridine]nickel(II) hexafluorophosphate tri-acetonitrile solvate ; _chemical_name_common ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_moiety 'C66 H72 N6 Ni O4 2+, 2(F6 P 1-), 3(C2 H3 N)' _chemical_formula_sum 'C72 H71 F12 N9 Ni O4 P2' _chemical_formula_weight 1475.04 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 576 0.0033 0.0016 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; H H 568 0.0000 0.0000 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; F F 96 0.0171 0.0103 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; N N 72 0.0061 0.0033 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; Ni Ni 8 0.3393 1.1124 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; O O 32 0.0106 0.0060 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; P P 16 0.1023 0.0942 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n n a ' _symmetry_space_group_name_Hall ? _symmetry_Int_Tables_number 52 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' 'x, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' '-x, y-1/2, z-1/2' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 22.0069(3) _cell_length_b 25.2020(5) _cell_length_c 24.8731(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 13795.1(4) _cell_formula_units_Z 8 _cell_measurement_temperature 160(1) _cell_measurement_reflns_used 158471 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.420 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6112 _exptl_absorpt_coefficient_mu 0.417 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Blessing, 1995)' _exptl_absorpt_correction_T_min 0.707 _exptl_absorpt_correction_T_max 0.893 _exptl_special_details ; Solvent used: MeCN / diethylether Cooling Device: Oxford Cryosystems Cryostream 700 Crystal mount: glued on a glass fibre Mosaicity (deg.): 0.675(1) Frames collected: 340 Seconds exposure per frame: 22 Degrees rotation per frame: 1.1 Crystal-Detector distance (mm): 37.8 ; _diffrn_ambient_temperature 160(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Nonius FR590 sealed tube generator' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_detector '65 mm CCD camera on \k goniostat' _diffrn_measurement_device_type 'Nonius KappaCCD area-detector diffractometer' _diffrn_measurement_method '\f and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 128129 _diffrn_reflns_av_R_equivalents 0.1055 _diffrn_reflns_av_sigmaI/netI 0.0579 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 25.01 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _reflns_number_total 12152 _reflns_number_gt 7907 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'COLLECT (Nonius, 2000)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN and SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'SHELXL97 and PLATON (Spek, 2009)' _refine_special_details ; The asymmetric unit contains two half-cations with each Ni-atom on a crystallographic two-fold axis, two disordered PF6- anions, and six different sites for partially occupied and disordered MeCN molecules. One site for a MeCN molecule is close to a two-fold axis, so the molecule is disordered about the axis and has a site occupation of 0.5. The second MeCN molecule sits exactly on a two-fold axis. The remaining four MeCN sites are close to one another and two of the sites cannot be occupied simultaneously with the other two. Thus two sites were constrained to have identical site occupation factors [value refined to 0.733(5)], while the other two sites were restrained to be occupied to the extent that the first two sites were not. All of the MeCN molecules were further restrained to have similar geometry. By using these restrictions, the best estimate for the ratio of MeCN molecules Ni-complex cations is approximately 3:1. Each symmetry-independent PF6- anion is disordered over two orientations. Two orientations were defined for the F-atoms of each anion and refinement of the site occupation factors led to values of 0.70(2) and 0.57(3) for the major orientations. The P-F and F...F distances were restrained tightly, so as to maintain octahedral geometry and uniform P-F bond lengths and neighbouring atoms within and between each disordered orientation were restrained to have similar atomic displacement parameters. One methoxy group in each ligand of each symmetry-independent cation is disordered. Two conformations for these groups were defined in each case and refinement of the site occupation factors led to a values of 0.63(2) and 0.694(6) for the major conformations. Similarity restraints were applied to the chemically equivalent bond lengths and angles involving all disordered atoms in each cation, while neighbouring disordered atoms were restrained to have similar atomic displacement parameters. The non-hydrogen atoms were refined anisotropically, except for the atoms of one minor disordered position for a MeCN molecule, which were refined only isotropically. The H-atoms of the MeCN molecule that sits on a two-fold axis were not included in the model. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0513P)^2^+21.7030P] 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 SHELXL _refine_ls_extinction_coef 0.00026(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 12148 _refine_ls_number_parameters 1125 _refine_ls_number_restraints 1091 _refine_ls_R_factor_all 0.1059 _refine_ls_R_factor_gt 0.0563 _refine_ls_wR_factor_ref 0.1440 _refine_ls_wR_factor_gt 0.1196 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.110 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.599 _refine_diff_density_min -0.569 _refine_diff_density_rms 0.074 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 Ni1 Ni 0.2500 0.0000 0.09388(2) 0.02696(18) Uani 1 2 d S . . O1 O -0.04213(12) -0.00274(12) 0.36862(11) 0.0450(7) Uani 1 1 d . . . O2A O 0.3379(12) -0.2579(12) -0.1692(19) 0.061(3) Uani 0.37(2) 1 d PDU A 1 C27A C 0.3884(8) -0.2949(8) -0.1646(10) 0.063(3) Uani 0.37(2) 1 d PDU A 1 H271 H 0.4257 -0.2777 -0.1773 0.094 Uiso 0.37(2) 1 calc PR A 1 H272 H 0.3802 -0.3264 -0.1864 0.094 Uiso 0.37(2) 1 calc PR A 1 H273 H 0.3934 -0.3053 -0.1269 0.094 Uiso 0.37(2) 1 calc PR A 1 O2B O 0.3357(7) -0.2527(7) -0.1759(11) 0.059(3) Uani 0.63(2) 1 d PDU A 2 C27B C 0.3917(4) -0.2791(5) -0.1915(6) 0.064(3) Uani 0.63(2) 1 d PDU A 2 H274 H 0.4192 -0.2534 -0.2083 0.096 Uiso 0.63(2) 1 calc PR A 2 H275 H 0.3825 -0.3075 -0.2171 0.096 Uiso 0.63(2) 1 calc PR A 2 H276 H 0.4112 -0.2943 -0.1595 0.096 Uiso 0.63(2) 1 calc PR A 2 N1 N 0.21236(14) 0.04702(12) 0.15550(11) 0.0311(7) Uani 1 1 d . . . N2 N 0.30266(13) 0.06440(12) 0.09172(11) 0.0295(7) Uani 1 1 d . . . N3 N 0.31153(13) -0.01969(11) 0.03176(11) 0.0267(7) Uani 1 1 d . . . C1 C -0.04318(19) -0.05527(17) 0.39058(17) 0.0479(11) Uani 1 1 d . . . H11 H -0.0408 -0.0812 0.3613 0.072 Uiso 1 1 calc R . . H12 H -0.0810 -0.0605 0.4107 0.072 Uiso 1 1 calc R . . H13 H -0.0084 -0.0600 0.4148 0.072 Uiso 1 1 calc R . . C2 C 0.00653(17) 0.00964(16) 0.33627(15) 0.0361(10) Uani 1 1 d . . . C3 C 0.00412(18) 0.05933(17) 0.31219(15) 0.0405(10) Uani 1 1 d . . . H3 H -0.0300 0.0816 0.3186 0.049 Uiso 1 1 calc R . . C4 C 0.05018(18) 0.07703(16) 0.27913(15) 0.0386(10) Uani 1 1 d . . . C5 C 0.0435(2) 0.13015(17) 0.25270(17) 0.0499(11) Uani 1 1 d . . . H51 H 0.0678 0.1564 0.2722 0.075 Uiso 1 1 calc R . . H52 H 0.0007 0.1408 0.2532 0.075 Uiso 1 1 calc R . . H53 H 0.0576 0.1279 0.2154 0.075 Uiso 1 1 calc R . . C6 C 0.10070(17) 0.04395(16) 0.26986(14) 0.0348(9) Uani 1 1 d . . . C7 C 0.16755(17) 0.03338(15) 0.18898(14) 0.0331(9) Uani 1 1 d . . . H7 H 0.1454 0.0020 0.1812 0.040 Uiso 1 1 calc R . . C8 C 0.15125(18) 0.06216(15) 0.23442(15) 0.0368(9) Uani 1 1 d . . . C9 C 0.18401(19) 0.10836(17) 0.24376(16) 0.0450(11) Uani 1 1 d . . . H9 H 0.1746 0.1296 0.2742 0.054 Uiso 1 1 calc R . . C10 C 0.23012(19) 0.12383(17) 0.20940(16) 0.0434(10) Uani 1 1 d . . . H10 H 0.2521 0.1556 0.2159 0.052 Uiso 1 1 calc R . . C11 C 0.24377(17) 0.09224(15) 0.16525(14) 0.0337(9) Uani 1 1 d . . . C12 C 0.29311(17) 0.10383(15) 0.12668(14) 0.0329(9) Uani 1 1 d . . . C13 C 0.32681(19) 0.15008(16) 0.12384(17) 0.0430(10) Uani 1 1 d . . . H131 H 0.3203 0.1780 0.1488 0.052 Uiso 1 1 calc R . . C14 C 0.37004(19) 0.15474(16) 0.08396(17) 0.0448(11) Uani 1 1 d . . . H14 H 0.3937 0.1862 0.0815 0.054 Uiso 1 1 calc R . . C15 C 0.37923(17) 0.11415(15) 0.04760(16) 0.0369(9) Uani 1 1 d . . . H15 H 0.4086 0.1175 0.0198 0.044 Uiso 1 1 calc R . . C16 C 0.34471(15) 0.06856(14) 0.05251(14) 0.0292(8) Uani 1 1 d . . . C17 C 0.34784(15) 0.02127(14) 0.01678(14) 0.0274(8) Uani 1 1 d . . . C18 C 0.38329(16) 0.01856(15) -0.02906(15) 0.0325(9) Uani 1 1 d . . . H18 H 0.4083 0.0476 -0.0392 0.039 Uiso 1 1 calc R . . C19 C 0.38186(16) -0.02698(15) -0.05992(15) 0.0340(9) Uani 1 1 d . . . H19 H 0.4056 -0.0289 -0.0918 0.041 Uiso 1 1 calc R . . C20 C 0.34626(15) -0.07001(14) -0.04507(14) 0.0285(8) Uani 1 1 d . . . C21 C 0.31206(15) -0.06401(14) 0.00170(14) 0.0268(8) Uani 1 1 d . . . H21 H 0.2876 -0.0930 0.0130 0.032 Uiso 1 1 calc R . . C22 C 0.34427(16) -0.11989(14) -0.07725(14) 0.0288(8) Uani 1 1 d . A . C23 C 0.39816(16) -0.14756(15) -0.08814(14) 0.0317(9) Uani 1 1 d . . . C24 C 0.45858(17) -0.13211(16) -0.06393(16) 0.0399(10) Uani 1 1 d . . . H241 H 0.4871 -0.1618 -0.0672 0.060 Uiso 1 1 calc R . . H242 H 0.4530 -0.1233 -0.0259 0.060 Uiso 1 1 calc R . . H243 H 0.4748 -0.1012 -0.0830 0.060 Uiso 1 1 calc R . . C25 C 0.39629(18) -0.19301(15) -0.11998(15) 0.0369(9) Uani 1 1 d . A . H25 H 0.4327 -0.2118 -0.1275 0.044 Uiso 1 1 calc R . . C26 C 0.34193(19) -0.21093(16) -0.14061(16) 0.0416(10) Uani 1 1 d D . . C28 C 0.28844(17) -0.18453(16) -0.12957(15) 0.0357(9) Uani 1 1 d . A . H28 H 0.2512 -0.1975 -0.1437 0.043 Uiso 1 1 calc R . . C29 C 0.28871(16) -0.13914(15) -0.09789(14) 0.0315(9) Uani 1 1 d . . . C30 C 0.22951(17) -0.11109(18) -0.08776(18) 0.0474(11) Uani 1 1 d . A . H301 H 0.1987 -0.1241 -0.1130 0.071 Uiso 1 1 calc R . . H302 H 0.2350 -0.0728 -0.0928 0.071 Uiso 1 1 calc R . . H303 H 0.2161 -0.1180 -0.0508 0.071 Uiso 1 1 calc R . . C31 C 0.1552(2) -0.04437(19) 0.28580(18) 0.0558(13) Uani 1 1 d . . . H311 H 0.1566 -0.0697 0.3157 0.084 Uiso 1 1 calc R . . H312 H 0.1934 -0.0244 0.2844 0.084 Uiso 1 1 calc R . . H313 H 0.1495 -0.0637 0.2520 0.084 Uiso 1 1 calc R . . C32 C 0.10292(17) -0.00639(16) 0.29397(15) 0.0362(9) Uani 1 1 d . . . C33 C 0.05544(17) -0.02338(16) 0.32697(15) 0.0364(9) Uani 1 1 d . . . H33 H 0.0568 -0.0576 0.3430 0.044 Uiso 1 1 calc R . . Ni41 Ni 0.7500 0.0000 0.38432(2) 0.02507(17) Uani 1 2 d S . . O41 O 0.44129(11) -0.02186(11) 0.11504(11) 0.0428(7) Uani 1 1 d . . . O42A O 0.8734(5) -0.2207(5) 0.6703(5) 0.059(2) Uani 0.306(6) 1 d PDU B 1 C67A C 0.8215(6) -0.2496(7) 0.6880(7) 0.060(2) Uani 0.306(6) 1 d PDU B 1 H671 H 0.7942 -0.2258 0.7077 0.091 Uiso 0.306(6) 1 calc PR B 1 H672 H 0.8345 -0.2785 0.7118 0.091 Uiso 0.306(6) 1 calc PR B 1 H673 H 0.8002 -0.2644 0.6569 0.091 Uiso 0.306(6) 1 calc PR B 1 O42B O 0.8421(2) -0.2265(2) 0.6673(2) 0.0563(15) Uani 0.694(6) 1 d PDU B 2 C67B C 0.8908(3) -0.2637(3) 0.6699(3) 0.0620(17) Uani 0.694(6) 1 d PDU B 2 H674 H 0.9007 -0.2761 0.6336 0.093 Uiso 0.694(6) 1 calc PR B 2 H675 H 0.8787 -0.2940 0.6921 0.093 Uiso 0.694(6) 1 calc PR B 2 H676 H 0.9266 -0.2467 0.6858 0.093 Uiso 0.694(6) 1 calc PR B 2 N41 N 0.70113(13) 0.04098(11) 0.32360(11) 0.0280(7) Uani 1 1 d . . . N42 N 0.79200(13) 0.06962(12) 0.38344(11) 0.0285(7) Uani 1 1 d . . . N43 N 0.81440(12) -0.00934(11) 0.44663(11) 0.0270(7) Uani 1 1 d . . . C41 C 0.44116(19) -0.07417(18) 0.09356(18) 0.0507(12) Uani 1 1 d . . . H411 H 0.4764 -0.0788 0.0699 0.076 Uiso 1 1 calc R . . H412 H 0.4038 -0.0798 0.0730 0.076 Uiso 1 1 calc R . . H413 H 0.4433 -0.0999 0.1230 0.076 Uiso 1 1 calc R . . C42 C 0.48811(16) -0.00849(15) 0.14866(14) 0.0332(9) Uani 1 1 d . . . C43 C 0.48547(17) 0.04172(16) 0.17118(15) 0.0351(9) Uani 1 1 d . . . H43 H 0.4517 0.0639 0.1635 0.042 Uiso 1 1 calc R . . C44 C 0.53100(17) 0.06017(15) 0.20462(14) 0.0330(9) Uani 1 1 d . . . C45 C 0.52298(19) 0.11431(15) 0.22957(16) 0.0420(10) Uani 1 1 d . . . H451 H 0.5447 0.1408 0.2080 0.063 Uiso 1 1 calc R . . H452 H 0.5394 0.1140 0.2662 0.063 Uiso 1 1 calc R . . H453 H 0.4797 0.1232 0.2307 0.063 Uiso 1 1 calc R . . C46 C 0.58142(16) 0.02727(15) 0.21553(14) 0.0306(9) Uani 1 1 d . . . C47 C 0.65504(16) 0.02294(14) 0.29374(14) 0.0292(8) Uani 1 1 d . . . H47 H 0.6356 -0.0090 0.3046 0.035 Uiso 1 1 calc R . . C48 C 0.63379(16) 0.04827(14) 0.24749(14) 0.0301(8) Uani 1 1 d . . . C49 C 0.66349(17) 0.09463(15) 0.23282(15) 0.0360(9) Uani 1 1 d . . . H49 H 0.6518 0.1126 0.2009 0.043 Uiso 1 1 calc R . . C50 C 0.70989(17) 0.11498(15) 0.26404(15) 0.0361(9) Uani 1 1 d . . . H50 H 0.7296 0.1471 0.2542 0.043 Uiso 1 1 calc R . . C51 C 0.72722(16) 0.08784(14) 0.30986(14) 0.0307(9) Uani 1 1 d . . . C52 C 0.77483(17) 0.10640(14) 0.34755(15) 0.0331(9) Uani 1 1 d . . . C53 C 0.7991(2) 0.15675(17) 0.34884(19) 0.0566(13) Uani 1 1 d . . . H531 H 0.7866 0.1829 0.3237 0.068 Uiso 1 1 calc R . . C54 C 0.8424(2) 0.16827(18) 0.3878(2) 0.0676(15) Uani 1 1 d . . . H54 H 0.8601 0.2026 0.3892 0.081 Uiso 1 1 calc R . . C55 C 0.8598(2) 0.13036(17) 0.42426(19) 0.0502(12) Uani 1 1 d . . . H55 H 0.8891 0.1383 0.4511 0.060 Uiso 1 1 calc R . . C56 C 0.83403(16) 0.08046(15) 0.42118(15) 0.0334(9) Uani 1 1 d . . . C57 C 0.84579(15) 0.03581(15) 0.45806(14) 0.0295(8) Uani 1 1 d . . . C58 C 0.88350(16) 0.03848(16) 0.50256(15) 0.0368(9) Uani 1 1 d . . . H58 H 0.9069 0.0695 0.5092 0.044 Uiso 1 1 calc R . . C59 C 0.88683(17) -0.00412(17) 0.53713(15) 0.0397(10) Uani 1 1 d . . . H59 H 0.9115 -0.0019 0.5684 0.048 Uiso 1 1 calc R . . C60 C 0.85439(16) -0.05051(16) 0.52677(14) 0.0333(9) Uani 1 1 d . . . C61 C 0.81943(15) -0.05073(15) 0.47962(14) 0.0303(9) Uani 1 1 d . . . H61 H 0.7981 -0.0823 0.4707 0.036 Uiso 1 1 calc R . . C62 C 0.85459(17) -0.09701(16) 0.56373(14) 0.0363(9) Uani 1 1 d . B . C63 C 0.90876(18) -0.12328(17) 0.57600(15) 0.0409(10) Uani 1 1 d . . . C64 C 0.96854(19) -0.1080(2) 0.55058(17) 0.0537(12) Uani 1 1 d . . . H641 H 0.9853 -0.0770 0.5692 0.081 Uiso 1 1 calc R . . H642 H 0.9621 -0.0994 0.5126 0.081 Uiso 1 1 calc R . . H643 H 0.9971 -0.1377 0.5535 0.081 Uiso 1 1 calc R . . C65 C 0.9070(2) -0.16637(19) 0.61081(17) 0.0534(12) Uani 1 1 d . B . H65 H 0.9437 -0.1843 0.6194 0.064 Uiso 1 1 calc R . . C66 C 0.8529(2) -0.18368(17) 0.63319(16) 0.0517(12) Uani 1 1 d D . . C68 C 0.7997(2) -0.15804(18) 0.62114(16) 0.0468(11) Uani 1 1 d . B . H68 H 0.7626 -0.1701 0.6364 0.056 Uiso 1 1 calc R . . C69 C 0.79956(18) -0.11461(17) 0.58688(15) 0.0420(10) Uani 1 1 d . . . C70 C 0.73995(19) -0.0878(2) 0.5758(2) 0.0657(15) Uani 1 1 d . B . H701 H 0.7246 -0.0991 0.5406 0.099 Uiso 1 1 calc R . . H702 H 0.7457 -0.0492 0.5759 0.099 Uiso 1 1 calc R . . H703 H 0.7106 -0.0976 0.6038 0.099 Uiso 1 1 calc R . . C71 C 0.63409(18) -0.06269(17) 0.20604(17) 0.0446(11) Uani 1 1 d . . . H711 H 0.6730 -0.0439 0.2040 0.067 Uiso 1 1 calc R . . H712 H 0.6334 -0.0913 0.1794 0.067 Uiso 1 1 calc R . . H713 H 0.6290 -0.0777 0.2421 0.067 Uiso 1 1 calc R . . C72 C 0.58287(16) -0.02424(15) 0.19465(14) 0.0307(9) Uani 1 1 d . . . C73 C 0.53599(16) -0.04212(16) 0.16109(14) 0.0327(9) Uani 1 1 d . . . H73 H 0.5370 -0.0771 0.1469 0.039 Uiso 1 1 calc R . . N74 N 0.8141(4) 0.2705(6) 0.2610(5) 0.115(6) Uani 0.50 1 d PD . . C75 C 0.8635(5) 0.2564(15) 0.2553(15) 0.098(8) Uani 0.50 1 d PD . . C76 C 0.9275(4) 0.2450(19) 0.245(2) 0.100(7) Uani 0.50 1 d PD . . H761 H 0.9406 0.2646 0.2126 0.149 Uiso 0.50 1 calc PR . . H762 H 0.9327 0.2069 0.2384 0.149 Uiso 0.50 1 calc PR . . H763 H 0.9521 0.2559 0.2755 0.149 Uiso 0.50 1 calc PR . . N77 N 0.3075(4) 0.2500 0.2500 0.174(5) Uani 1 2 d SD . . C78 C 0.3597(5) 0.2500 0.2500 0.110(3) Uani 1 2 d SD . . C79 C 0.4261(4) 0.2500 0.2500 0.172(6) Uani 1 2 d SD . . N80 N 0.1550(4) 0.3303(3) -0.0615(3) 0.109(3) Uani 0.733(5) 1 d PD C 1 C81 C 0.1227(4) 0.3017(3) -0.0393(3) 0.083(3) Uani 0.733(5) 1 d PD C 1 C82 C 0.0843(3) 0.2651(3) -0.0090(3) 0.067(2) Uani 0.733(5) 1 d PD C 1 H821 H 0.1092 0.2360 0.0050 0.100 Uiso 0.733(5) 1 calc PR C 1 H822 H 0.0527 0.2508 -0.0326 0.100 Uiso 0.733(5) 1 calc PR C 1 H823 H 0.0653 0.2841 0.0210 0.100 Uiso 0.733(5) 1 calc PR C 1 N83 N 0.1998(6) 0.1855(3) 0.0535(4) 0.115(4) Uani 0.733(5) 1 d PD C 1 C84 C 0.2322(4) 0.2165(4) 0.0351(4) 0.079(3) Uani 0.733(5) 1 d PD C 1 C85 C 0.2701(6) 0.2551(6) 0.0068(8) 0.111(7) Uani 0.733(5) 1 d PD C 1 H851 H 0.2843 0.2398 -0.0271 0.167 Uiso 0.733(5) 1 calc PR C 1 H852 H 0.3051 0.2644 0.0293 0.167 Uiso 0.733(5) 1 calc PR C 1 H853 H 0.2462 0.2871 -0.0006 0.167 Uiso 0.733(5) 1 calc PR C 1 N86 N 0.2174(8) 0.3225(6) -0.0513(6) 0.064(5) Uani 0.267(5) 1 d PD C 2 C87 C 0.2464(8) 0.2908(7) -0.0296(7) 0.055(5) Uani 0.267(5) 1 d PD C 2 C88 C 0.2856(16) 0.2586(18) 0.005(2) 0.101(18) Uani 0.267(5) 1 d PD C 2 H881 H 0.3277 0.2610 -0.0078 0.152 Uiso 0.267(5) 1 calc PR C 2 H882 H 0.2722 0.2215 0.0037 0.152 Uiso 0.267(5) 1 calc PR C 2 H883 H 0.2832 0.2717 0.0420 0.152 Uiso 0.267(5) 1 calc PR C 2 N89 N 0.1060(17) 0.2393(14) 0.0193(16) 0.22(2) Uiso 0.267(5) 1 d PD C 2 C90 C 0.1357(10) 0.2071(9) 0.0392(9) 0.074(6) Uiso 0.267(5) 1 d PD C 2 C91 C 0.178(2) 0.1709(18) 0.066(2) 0.19(3) Uiso 0.267(5) 1 d PD C 2 H911 H 0.1895 0.1857 0.1008 0.290 Uiso 0.267(5) 1 calc PR C 2 H912 H 0.2139 0.1660 0.0436 0.290 Uiso 0.267(5) 1 calc PR C 2 H913 H 0.1577 0.1365 0.0715 0.290 Uiso 0.267(5) 1 calc PR C 2 P1 P 0.43256(6) 0.18554(5) 0.39812(6) 0.0637(4) Uani 1 1 d D . . F1A F 0.4934(3) 0.1637(3) 0.4280(4) 0.103(2) Uani 0.698(17) 1 d PDU D 1 F2A F 0.3740(3) 0.2069(3) 0.3712(3) 0.092(2) Uani 0.698(17) 1 d PDU D 1 F3A F 0.4621(4) 0.1690(3) 0.3432(2) 0.079(2) Uani 0.698(17) 1 d PDU D 1 F4A F 0.4062(5) 0.1995(3) 0.4559(2) 0.126(3) Uani 0.698(17) 1 d PDU D 1 F5A F 0.4047(3) 0.12774(19) 0.4036(4) 0.085(2) Uani 0.698(17) 1 d PDU D 1 F6A F 0.4631(3) 0.24201(17) 0.3953(5) 0.105(3) Uani 0.698(17) 1 d PDU D 1 F1B F 0.5014(3) 0.1704(6) 0.4052(9) 0.114(5) Uani 0.302(17) 1 d PDU D 2 F2B F 0.3635(4) 0.2023(6) 0.3887(8) 0.078(4) Uani 0.302(17) 1 d PDU D 2 F3B F 0.4330(10) 0.1590(6) 0.3399(3) 0.103(5) Uani 0.302(17) 1 d PDU D 2 F4B F 0.4314(9) 0.2137(7) 0.4542(4) 0.126(5) Uani 0.302(17) 1 d PDU D 2 F5B F 0.4119(8) 0.1318(4) 0.4234(7) 0.086(4) Uani 0.302(17) 1 d PDU D 2 F6B F 0.4520(8) 0.2403(4) 0.3704(8) 0.121(5) Uani 0.302(17) 1 d PDU D 2 P2 P 0.94185(5) 0.19765(4) 0.09061(5) 0.0482(3) Uani 1 1 d D . . F7A F 1.0100(5) 0.1888(7) 0.0691(8) 0.078(4) Uani 0.43(3) 1 d PDU E 1 F8A F 0.8757(4) 0.2061(7) 0.1120(8) 0.074(4) Uani 0.43(3) 1 d PDU E 1 F9A F 0.9640(8) 0.1786(8) 0.1481(4) 0.055(3) Uani 0.43(3) 1 d PDU E 1 F10A F 0.9224(10) 0.2156(8) 0.0322(4) 0.123(4) Uani 0.43(3) 1 d PDU E 1 F11A F 0.9267(8) 0.1377(3) 0.0751(9) 0.062(3) Uani 0.43(3) 1 d PDU E 1 F12A F 0.9589(8) 0.2571(3) 0.1054(9) 0.077(4) Uani 0.43(3) 1 d PDU E 1 F7B F 0.9963(6) 0.1887(5) 0.0512(6) 0.101(3) Uani 0.57(3) 1 d PDU E 2 F8B F 0.8859(4) 0.2057(5) 0.1313(5) 0.058(2) Uani 0.57(3) 1 d PDU E 2 F9B F 0.9817(6) 0.1781(6) 0.1399(4) 0.050(2) Uani 0.57(3) 1 d PDU E 2 F10B F 0.8994(8) 0.2164(6) 0.0431(5) 0.117(4) Uani 0.57(3) 1 d PDU E 2 F11B F 0.9200(6) 0.1378(3) 0.0809(7) 0.060(3) Uani 0.57(3) 1 d PDU E 2 F12B F 0.9621(6) 0.2570(3) 0.1012(6) 0.073(3) Uani 0.57(3) 1 d PDU E 2 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 Ni1 0.0300(4) 0.0255(4) 0.0253(4) 0.000 0.000 -0.0043(3) O1 0.0359(15) 0.0507(18) 0.0486(17) 0.0018(14) 0.0108(13) 0.0041(14) O2A 0.055(4) 0.057(5) 0.071(7) -0.035(6) -0.002(4) 0.001(3) C27A 0.059(3) 0.058(5) 0.072(7) -0.033(5) 0.002(4) 0.003(3) O2B 0.056(3) 0.054(4) 0.069(6) -0.031(5) 0.001(3) -0.001(3) C27B 0.062(3) 0.058(4) 0.072(7) -0.034(5) 0.007(4) 0.000(3) N1 0.0361(18) 0.0294(18) 0.0279(17) -0.0005(13) 0.0008(14) -0.0038(14) N2 0.0322(17) 0.0282(17) 0.0280(17) 0.0008(14) -0.0032(14) -0.0022(14) N3 0.0265(16) 0.0264(17) 0.0274(16) 0.0029(13) -0.0028(13) -0.0014(13) C1 0.041(2) 0.055(3) 0.048(3) 0.007(2) 0.011(2) 0.001(2) C2 0.034(2) 0.046(3) 0.028(2) -0.0044(18) 0.0000(17) 0.0000(19) C3 0.039(2) 0.045(3) 0.037(2) -0.0034(19) -0.0019(19) 0.007(2) C4 0.047(2) 0.039(2) 0.030(2) -0.0031(18) -0.0024(19) 0.000(2) C5 0.061(3) 0.043(3) 0.046(3) 0.001(2) 0.002(2) 0.006(2) C6 0.038(2) 0.038(2) 0.028(2) -0.0031(18) 0.0005(17) 0.0001(19) C7 0.038(2) 0.029(2) 0.032(2) -0.0032(17) -0.0003(18) -0.0036(18) C8 0.043(2) 0.035(2) 0.032(2) -0.0004(18) -0.0007(18) 0.0039(19) C9 0.058(3) 0.043(3) 0.034(2) -0.0102(19) 0.007(2) -0.005(2) C10 0.056(3) 0.037(2) 0.037(2) -0.0106(19) 0.003(2) -0.012(2) C11 0.041(2) 0.030(2) 0.030(2) -0.0005(16) 0.0000(17) -0.0041(19) C12 0.034(2) 0.032(2) 0.032(2) -0.0027(17) -0.0042(17) -0.0027(18) C13 0.050(3) 0.034(2) 0.046(3) -0.0097(19) 0.004(2) -0.010(2) C14 0.045(3) 0.033(2) 0.056(3) -0.007(2) 0.003(2) -0.012(2) C15 0.033(2) 0.035(2) 0.043(2) 0.0027(18) 0.0017(18) -0.0078(18) C16 0.0261(19) 0.032(2) 0.030(2) 0.0040(16) -0.0042(16) -0.0003(17) C17 0.0242(19) 0.0263(19) 0.032(2) 0.0030(16) -0.0027(16) 0.0010(16) C18 0.029(2) 0.029(2) 0.040(2) 0.0041(18) 0.0028(17) -0.0057(16) C19 0.031(2) 0.037(2) 0.033(2) 0.0042(18) 0.0052(17) 0.0027(18) C20 0.0260(19) 0.029(2) 0.031(2) 0.0021(16) -0.0003(16) 0.0016(16) C21 0.0255(19) 0.025(2) 0.030(2) 0.0020(16) -0.0023(16) -0.0014(16) C22 0.033(2) 0.029(2) 0.0248(19) 0.0042(16) 0.0009(16) -0.0028(17) C23 0.028(2) 0.035(2) 0.032(2) 0.0036(17) -0.0004(16) -0.0010(17) C24 0.034(2) 0.040(2) 0.046(2) -0.0023(19) -0.0034(19) 0.0054(18) C25 0.035(2) 0.037(2) 0.039(2) -0.0041(19) 0.0010(18) 0.0049(18) C26 0.047(3) 0.038(2) 0.040(2) -0.0088(19) 0.001(2) -0.003(2) C28 0.034(2) 0.039(2) 0.034(2) -0.0001(18) -0.0047(17) -0.0070(18) C29 0.028(2) 0.036(2) 0.030(2) 0.0046(17) -0.0009(16) -0.0033(17) C30 0.032(2) 0.052(3) 0.058(3) -0.006(2) -0.008(2) 0.002(2) C31 0.055(3) 0.059(3) 0.054(3) 0.018(2) 0.019(2) 0.020(2) C32 0.037(2) 0.042(3) 0.029(2) -0.0034(18) 0.0001(17) 0.0040(19) C33 0.038(2) 0.042(2) 0.029(2) 0.0004(18) 0.0011(18) 0.0009(19) Ni41 0.0259(3) 0.0243(4) 0.0250(4) 0.000 0.000 -0.0041(3) O41 0.0330(15) 0.0463(17) 0.0490(17) -0.0074(14) -0.0124(13) 0.0074(13) O42A 0.072(5) 0.052(4) 0.052(4) 0.016(4) -0.002(4) 0.006(4) C67A 0.072(5) 0.055(4) 0.054(4) 0.016(4) 0.000(4) 0.004(4) O42B 0.065(4) 0.054(3) 0.050(2) 0.016(2) 0.008(3) 0.008(3) C67B 0.071(4) 0.056(3) 0.058(3) 0.016(3) 0.001(3) 0.011(3) N41 0.0296(16) 0.0247(17) 0.0297(17) 0.0007(13) 0.0004(14) -0.0034(14) N42 0.0282(16) 0.0299(17) 0.0274(17) -0.0019(14) 0.0024(14) -0.0016(14) N43 0.0236(15) 0.0310(19) 0.0264(16) -0.0043(13) 0.0029(12) -0.0013(13) C41 0.043(3) 0.055(3) 0.054(3) -0.014(2) -0.018(2) 0.009(2) C42 0.028(2) 0.040(3) 0.032(2) 0.0017(18) -0.0006(17) -0.0021(17) C43 0.029(2) 0.037(2) 0.040(2) 0.0049(19) 0.0012(18) 0.0061(18) C44 0.037(2) 0.032(2) 0.030(2) 0.0041(17) 0.0018(17) 0.0019(18) C45 0.045(2) 0.035(2) 0.046(3) -0.0002(19) 0.0003(19) 0.004(2) C46 0.033(2) 0.033(2) 0.026(2) 0.0019(16) 0.0015(16) -0.0004(17) C47 0.030(2) 0.027(2) 0.031(2) -0.0004(16) 0.0025(17) -0.0036(16) C48 0.033(2) 0.028(2) 0.029(2) 0.0000(16) 0.0009(16) 0.0023(17) C49 0.043(2) 0.035(2) 0.030(2) 0.0071(17) -0.0010(18) -0.0002(19) C50 0.040(2) 0.030(2) 0.038(2) 0.0081(18) -0.0001(18) -0.0077(18) C51 0.032(2) 0.027(2) 0.033(2) 0.0010(17) 0.0042(16) -0.0031(17) C52 0.035(2) 0.026(2) 0.039(2) 0.0011(17) -0.0003(17) -0.0051(17) C53 0.066(3) 0.030(2) 0.074(3) 0.015(2) -0.023(3) -0.016(2) C54 0.073(3) 0.033(3) 0.097(4) 0.009(3) -0.033(3) -0.024(2) C55 0.046(3) 0.037(3) 0.067(3) 0.000(2) -0.018(2) -0.014(2) C56 0.025(2) 0.036(2) 0.039(2) -0.0070(18) 0.0015(17) -0.0031(17) C57 0.0213(18) 0.034(2) 0.033(2) -0.0072(17) 0.0035(16) -0.0008(17) C58 0.029(2) 0.041(2) 0.041(2) -0.0068(19) -0.0056(18) -0.0088(18) C59 0.033(2) 0.053(3) 0.033(2) -0.007(2) -0.0088(17) -0.001(2) C60 0.026(2) 0.043(2) 0.031(2) -0.0035(18) -0.0007(16) 0.0029(18) C61 0.0237(19) 0.034(2) 0.033(2) -0.0002(17) 0.0007(16) -0.0024(16) C62 0.038(2) 0.045(2) 0.026(2) -0.0041(18) -0.0050(17) 0.0012(19) C63 0.040(2) 0.054(3) 0.029(2) -0.004(2) -0.0019(18) 0.010(2) C64 0.043(3) 0.073(3) 0.045(3) 0.000(2) -0.006(2) 0.017(2) C65 0.068(3) 0.059(3) 0.033(2) -0.001(2) -0.006(2) 0.028(3) C66 0.083(4) 0.043(3) 0.029(2) 0.001(2) 0.006(2) 0.007(3) C68 0.054(3) 0.053(3) 0.033(2) 0.001(2) 0.001(2) -0.005(2) C69 0.042(2) 0.051(3) 0.033(2) 0.003(2) -0.0029(19) 0.000(2) C70 0.039(3) 0.096(4) 0.062(3) 0.029(3) 0.005(2) -0.002(3) C71 0.043(2) 0.045(3) 0.046(3) -0.010(2) -0.011(2) 0.010(2) C72 0.030(2) 0.032(2) 0.031(2) 0.0003(17) 0.0010(16) 0.0009(17) C73 0.032(2) 0.034(2) 0.031(2) -0.0004(17) 0.0002(17) 0.0008(18) N74 0.086(6) 0.19(2) 0.067(11) 0.048(10) 0.008(6) 0.058(8) C75 0.083(7) 0.13(2) 0.082(13) 0.046(12) -0.004(12) 0.050(15) C76 0.058(5) 0.137(17) 0.104(18) -0.103(12) -0.028(13) 0.020(12) N77 0.117(8) 0.270(16) 0.136(9) -0.021(9) 0.000 0.000 C78 0.132(10) 0.114(9) 0.085(7) -0.003(6) 0.000 0.000 C79 0.079(8) 0.224(16) 0.211(14) 0.113(12) 0.000 0.000 N80 0.102(7) 0.082(6) 0.142(8) -0.048(5) 0.010(6) -0.018(5) C81 0.080(6) 0.073(6) 0.095(7) -0.042(5) -0.010(5) 0.002(5) C82 0.079(5) 0.048(4) 0.073(5) -0.025(4) -0.004(4) -0.001(4) N83 0.223(12) 0.036(4) 0.085(6) -0.013(4) -0.021(7) 0.007(6) C84 0.090(7) 0.062(6) 0.086(7) -0.026(5) -0.038(5) 0.031(5) C85 0.083(9) 0.093(12) 0.157(17) -0.020(11) -0.017(9) -0.001(8) N86 0.086(14) 0.045(10) 0.060(10) -0.003(8) 0.017(9) -0.013(9) C87 0.062(12) 0.039(11) 0.065(13) -0.012(9) 0.013(11) -0.012(10) C88 0.07(2) 0.11(3) 0.12(3) 0.07(3) -0.042(19) -0.05(2) P1 0.0583(8) 0.0480(8) 0.0848(10) -0.0130(7) 0.0217(7) 0.0022(6) F1A 0.087(4) 0.105(4) 0.117(6) -0.002(4) -0.021(4) 0.027(3) F2A 0.074(3) 0.107(4) 0.094(5) 0.026(4) 0.003(3) 0.003(3) F3A 0.096(5) 0.065(3) 0.076(3) 0.005(2) 0.050(3) 0.002(3) F4A 0.128(7) 0.155(6) 0.096(4) -0.053(4) 0.029(4) 0.010(5) F5A 0.093(4) 0.071(3) 0.090(5) 0.004(3) 0.025(4) -0.016(3) F6A 0.069(3) 0.045(3) 0.200(8) -0.034(3) 0.001(4) -0.001(2) F1B 0.064(6) 0.110(8) 0.167(11) -0.018(9) 0.028(7) 0.002(6) F2B 0.051(6) 0.089(7) 0.094(9) 0.019(7) 0.014(6) 0.001(5) F3B 0.156(11) 0.061(7) 0.092(7) -0.010(5) 0.062(7) -0.012(8) F4B 0.104(11) 0.163(10) 0.112(8) -0.065(7) -0.008(7) 0.028(9) F5B 0.105(7) 0.080(7) 0.072(9) 0.046(6) 0.015(7) -0.008(6) F6B 0.109(9) 0.041(6) 0.214(12) -0.030(7) 0.045(9) -0.028(6) P2 0.0537(7) 0.0338(6) 0.0570(8) -0.0009(5) -0.0051(6) 0.0089(5) F7A 0.075(5) 0.075(5) 0.083(7) -0.004(6) 0.023(5) 0.013(4) F8A 0.027(4) 0.044(4) 0.153(9) -0.016(7) -0.018(5) 0.008(3) F9A 0.053(7) 0.059(5) 0.053(4) -0.014(4) 0.001(4) 0.007(6) F10A 0.201(10) 0.070(6) 0.099(7) 0.029(6) -0.073(7) 0.009(8) F11A 0.084(7) 0.038(6) 0.065(6) -0.012(5) -0.037(6) 0.012(5) F12A 0.059(6) 0.036(6) 0.135(7) -0.006(6) 0.009(6) -0.002(6) F7B 0.139(6) 0.081(4) 0.083(6) 0.002(5) 0.066(5) 0.020(6) F8B 0.034(3) 0.052(3) 0.088(6) -0.014(4) -0.005(3) -0.003(3) F9B 0.036(4) 0.049(3) 0.066(4) -0.008(4) -0.013(3) 0.011(4) F10B 0.202(9) 0.065(4) 0.085(5) 0.005(4) -0.069(5) 0.045(6) F11B 0.073(5) 0.038(4) 0.070(5) -0.007(4) -0.025(4) 0.010(4) F12B 0.060(5) 0.033(5) 0.125(5) -0.002(4) 0.012(5) -0.001(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 Ni1 N2 1.995(3) . ? Ni1 N1 2.107(3) . ? Ni1 N3 2.114(3) . ? O1 C2 1.375(5) . ? O1 C1 1.433(5) . ? O2A C26 1.384(8) . ? O2A C27A 1.456(11) . ? C27A H271 0.9800 . ? C27A H272 0.9800 . ? C27A H273 0.9800 . ? O2B C26 1.378(7) . ? O2B C27B 1.454(10) . ? C27B H274 0.9800 . ? C27B H275 0.9800 . ? C27B H276 0.9800 . ? N1 C7 1.336(5) . ? N1 C11 1.355(5) . ? N2 C12 1.337(5) . ? N2 C16 1.349(4) . ? N3 C21 1.344(4) . ? N3 C17 1.357(4) . ? C1 H11 0.9800 . ? C1 H12 0.9800 . ? C1 H13 0.9800 . ? C2 C33 1.380(5) . ? C2 C3 1.389(6) . ? C3 C4 1.380(6) . ? C3 H3 0.9500 . ? C4 C6 1.409(5) . ? C4 C5 1.499(6) . ? C5 H51 0.9800 . ? C5 H52 0.9800 . ? C5 H53 0.9800 . ? C6 C32 1.404(5) . ? C6 C8 1.492(5) . ? C7 C8 1.390(5) . ? C7 H7 0.9500 . ? C8 C9 1.389(5) . ? C9 C10 1.383(6) . ? C9 H9 0.9500 . ? C10 C11 1.389(5) . ? C10 H10 0.9500 . ? C11 C12 1.478(5) . ? C12 C13 1.383(5) . ? C13 C14 1.379(6) . ? C13 H131 0.9500 . ? C14 C15 1.380(5) . ? C14 H14 0.9500 . ? C15 C16 1.383(5) . ? C15 H15 0.9500 . ? C16 C17 1.488(5) . ? C17 C18 1.383(5) . ? C18 C19 1.381(5) . ? C18 H18 0.9500 . ? C19 C20 1.388(5) . ? C19 H19 0.9500 . ? C20 C21 1.394(5) . ? C20 C22 1.491(5) . ? C21 H21 0.9500 . ? C22 C23 1.402(5) . ? C22 C29 1.412(5) . ? C23 C25 1.393(5) . ? C23 C24 1.511(5) . ? C24 H241 0.9800 . ? C24 H242 0.9800 . ? C24 H243 0.9800 . ? C25 C26 1.378(5) . ? C25 H25 0.9500 . ? C26 C28 1.380(5) . ? C28 C29 1.389(5) . ? C28 H28 0.9500 . ? C29 C30 1.504(5) . ? C30 H301 0.9800 . ? C30 H302 0.9800 . ? C30 H303 0.9800 . ? C31 C32 1.510(5) . ? C31 H311 0.9800 . ? C31 H312 0.9800 . ? C31 H313 0.9800 . ? C32 C33 1.396(5) . ? C33 H33 0.9500 . ? Ni41 N42 1.983(3) . ? Ni41 N43 2.113(3) . ? Ni41 N41 2.122(3) . ? O41 C42 1.369(4) . ? O41 C41 1.422(5) . ? O42A C66 1.387(8) . ? O42A C67A 1.425(8) . ? C67A H671 0.9800 . ? C67A H672 0.9800 . ? C67A H673 0.9800 . ? O42B C66 1.392(6) . ? O42B C67B 1.427(7) . ? C67B H674 0.9800 . ? C67B H675 0.9800 . ? C67B H676 0.9800 . ? N41 C47 1.337(4) . ? N41 C51 1.357(4) . ? N42 C52 1.341(5) . ? N42 C56 1.346(5) . ? N43 C61 1.332(4) . ? N43 C57 1.361(4) . ? C41 H411 0.9800 . ? C41 H412 0.9800 . ? C41 H413 0.9800 . ? C42 C43 1.385(5) . ? C42 C73 1.387(5) . ? C43 C44 1.383(5) . ? C43 H43 0.9500 . ? C44 C46 1.411(5) . ? C44 C45 1.509(5) . ? C45 H451 0.9800 . ? C45 H452 0.9800 . ? C45 H453 0.9800 . ? C46 C72 1.399(5) . ? C46 C48 1.497(5) . ? C47 C48 1.396(5) . ? C47 H47 0.9500 . ? C48 C49 1.388(5) . ? C49 C50 1.382(5) . ? C49 H49 0.9500 . ? C50 C51 1.383(5) . ? C50 H50 0.9500 . ? C51 C52 1.482(5) . ? C52 C53 1.377(5) . ? C53 C54 1.390(6) . ? C53 H531 0.9500 . ? C54 C55 1.371(6) . ? C54 H54 0.9500 . ? C55 C56 1.382(5) . ? C55 H55 0.9500 . ? C56 C57 1.475(5) . ? C57 C58 1.385(5) . ? C58 C59 1.377(6) . ? C58 H58 0.9500 . ? C59 C60 1.394(5) . ? C59 H59 0.9500 . ? C60 C61 1.403(5) . ? C60 C62 1.489(5) . ? C61 H61 0.9500 . ? C62 C63 1.397(5) . ? C62 C69 1.413(5) . ? C63 C65 1.389(6) . ? C63 C64 1.509(6) . ? C64 H641 0.9800 . ? C64 H642 0.9800 . ? C64 H643 0.9800 . ? C65 C66 1.386(6) . ? C65 H65 0.9500 . ? C66 C68 1.371(6) . ? C68 C69 1.387(6) . ? C68 H68 0.9500 . ? C69 C70 1.501(6) . ? C70 H701 0.9800 . ? C70 H702 0.9800 . ? C70 H703 0.9800 . ? C71 C72 1.513(5) . ? C71 H711 0.9800 . ? C71 H712 0.9800 . ? C71 H713 0.9800 . ? C72 C73 1.401(5) . ? C73 H73 0.9500 . ? N74 C75 1.152(8) . ? C75 C76 1.462(9) . ? C76 H761 0.9800 . ? C76 H762 0.9800 . ? C76 H763 0.9800 . ? N77 C78 1.148(7) . ? C78 C79 1.461(9) . ? N80 C81 1.153(7) . ? C81 C82 1.461(9) . ? C82 H821 0.9800 . ? C82 H822 0.9800 . ? C82 H823 0.9800 . ? N83 C84 1.153(7) . ? C84 C85 1.462(9) . ? C85 H851 0.9800 . ? C85 H852 0.9800 . ? C85 H853 0.9800 . ? N86 C87 1.155(8) . ? C87 C88 1.464(9) . ? C88 H881 0.9800 . ? C88 H882 0.9800 . ? C88 H883 0.9800 . ? N89 C90 1.154(8) . ? C90 C91 1.460(9) . ? C91 H911 0.9800 . ? C91 H912 0.9800 . ? C91 H913 0.9800 . ? P1 F2A 1.549(4) . ? P1 F5B 1.561(6) . ? P1 F4B 1.565(6) . ? P1 F3A 1.569(4) . ? P1 F1B 1.572(6) . ? P1 F6A 1.575(4) . ? P1 F5A 1.586(4) . ? P1 F4A 1.588(4) . ? P1 F2B 1.594(6) . ? P1 F3B 1.596(6) . ? P1 F6B 1.601(6) . ? P1 F1A 1.627(4) . ? P2 F8A 1.564(5) . ? P2 F7B 1.564(5) . ? P2 F10B 1.578(5) . ? P2 F10A 1.580(5) . ? P2 F12B 1.583(4) . ? P2 F9A 1.584(5) . ? P2 F9B 1.585(4) . ? P2 F12A 1.587(5) . ? P2 F11A 1.593(5) . ? P2 F11B 1.601(5) . ? P2 F8B 1.607(5) . ? P2 F7A 1.607(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ni1 N2 176.92(17) . 2 ? N2 Ni1 N1 104.40(12) . 2 ? N2 Ni1 N1 77.90(12) . . ? N1 Ni1 N1 86.66(16) 2 . ? N2 Ni1 N3 99.29(11) . 2 ? N1 Ni1 N3 98.50(11) . 2 ? N2 Ni1 N3 78.42(11) . . ? N1 Ni1 N3 156.31(11) . . ? N3 Ni1 N3 86.06(15) 2 . ? C2 O1 C1 116.4(3) . . ? C26 O2A C27A 117.2(13) . . ? C26 O2B C27B 115.8(8) . . ? O2B C27B H274 109.5 . . ? O2B C27B H275 109.5 . . ? H274 C27B H275 109.5 . . ? O2B C27B H276 109.5 . . ? H274 C27B H276 109.5 . . ? H275 C27B H276 109.5 . . ? C7 N1 C11 118.8(3) . . ? C7 N1 Ni1 126.8(2) . . ? C11 N1 Ni1 113.7(2) . . ? C12 N2 C16 121.4(3) . . ? C12 N2 Ni1 119.7(2) . . ? C16 N2 Ni1 118.8(2) . . ? C21 N3 C17 118.3(3) . . ? C21 N3 Ni1 127.4(2) . . ? C17 N3 Ni1 113.5(2) . . ? O1 C1 H11 109.5 . . ? O1 C1 H12 109.5 . . ? H11 C1 H12 109.5 . . ? O1 C1 H13 109.5 . . ? H11 C1 H13 109.5 . . ? H12 C1 H13 109.5 . . ? O1 C2 C33 124.6(4) . . ? O1 C2 C3 115.3(3) . . ? C33 C2 C3 120.1(4) . . ? C4 C3 C2 121.4(4) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C3 C4 C6 119.1(4) . . ? C3 C4 C5 118.6(4) . . ? C6 C4 C5 122.3(4) . . ? C4 C5 H51 109.5 . . ? C4 C5 H52 109.5 . . ? H51 C5 H52 109.5 . . ? C4 C5 H53 109.5 . . ? H51 C5 H53 109.5 . . ? H52 C5 H53 109.5 . . ? C32 C6 C4 119.5(4) . . ? C32 C6 C8 120.3(3) . . ? C4 C6 C8 120.2(4) . . ? N1 C7 C8 124.3(4) . . ? N1 C7 H7 117.9 . . ? C8 C7 H7 117.9 . . ? C9 C8 C7 116.1(4) . . ? C9 C8 C6 123.1(3) . . ? C7 C8 C6 120.8(3) . . ? C10 C9 C8 120.9(4) . . ? C10 C9 H9 119.5 . . ? C8 C9 H9 119.5 . . ? C9 C10 C11 119.1(4) . . ? C9 C10 H10 120.5 . . ? C11 C10 H10 120.5 . . ? N1 C11 C10 120.9(3) . . ? N1 C11 C12 115.1(3) . . ? C10 C11 C12 124.0(3) . . ? N2 C12 C13 120.6(3) . . ? N2 C12 C11 113.0(3) . . ? C13 C12 C11 126.4(3) . . ? C14 C13 C12 118.6(4) . . ? C14 C13 H131 120.7 . . ? C12 C13 H131 120.7 . . ? C13 C14 C15 120.6(4) . . ? C13 C14 H14 119.7 . . ? C15 C14 H14 119.7 . . ? C14 C15 C16 118.5(4) . . ? C14 C15 H15 120.7 . . ? C16 C15 H15 120.7 . . ? N2 C16 C15 120.4(3) . . ? N2 C16 C17 113.7(3) . . ? C15 C16 C17 126.0(3) . . ? N3 C17 C18 121.4(3) . . ? N3 C17 C16 114.7(3) . . ? C18 C17 C16 123.9(3) . . ? C19 C18 C17 119.1(3) . . ? C19 C18 H18 120.5 . . ? C17 C18 H18 120.5 . . ? C18 C19 C20 121.0(3) . . ? C18 C19 H19 119.5 . . ? C20 C19 H19 119.5 . . ? C19 C20 C21 116.2(3) . . ? C19 C20 C22 122.2(3) . . ? C21 C20 C22 121.6(3) . . ? N3 C21 C20 124.0(3) . . ? N3 C21 H21 118.0 . . ? C20 C21 H21 118.0 . . ? C23 C22 C29 119.4(3) . . ? C23 C22 C20 119.9(3) . . ? C29 C22 C20 120.7(3) . . ? C25 C23 C22 119.6(3) . . ? C25 C23 C24 117.7(3) . . ? C22 C23 C24 122.6(3) . . ? C23 C24 H241 109.5 . . ? C23 C24 H242 109.5 . . ? H241 C24 H242 109.5 . . ? C23 C24 H243 109.5 . . ? H241 C24 H243 109.5 . . ? H242 C24 H243 109.5 . . ? C26 C25 C23 120.4(4) . . ? C26 C25 H25 119.8 . . ? C23 C25 H25 119.8 . . ? O2B C26 C25 125.1(6) . . ? O2B C26 C28 114.2(6) . . ? C25 C26 C28 120.6(3) . . ? C25 C26 O2A 121.9(9) . . ? C28 C26 O2A 117.4(10) . . ? C26 C28 C29 120.4(3) . . ? C26 C28 H28 119.8 . . ? C29 C28 H28 119.8 . . ? C28 C29 C22 119.5(3) . . ? C28 C29 C30 118.6(3) . . ? C22 C29 C30 121.9(3) . . ? C29 C30 H301 109.5 . . ? C29 C30 H302 109.5 . . ? H301 C30 H302 109.5 . . ? C29 C30 H303 109.5 . . ? H301 C30 H303 109.5 . . ? H302 C30 H303 109.5 . . ? C32 C31 H311 109.5 . . ? C32 C31 H312 109.5 . . ? H311 C31 H312 109.5 . . ? C32 C31 H313 109.5 . . ? H311 C31 H313 109.5 . . ? H312 C31 H313 109.5 . . ? C33 C32 C6 120.2(4) . . ? C33 C32 C31 117.1(4) . . ? C6 C32 C31 122.8(4) . . ? C2 C33 C32 119.8(4) . . ? C2 C33 H33 120.1 . . ? C32 C33 H33 120.1 . . ? N42 Ni41 N42 178.73(17) 2_655 . ? N42 Ni41 N43 102.84(11) . 2_655 ? N42 Ni41 N43 78.12(12) . . ? N43 Ni41 N43 85.66(15) 2_655 . ? N42 Ni41 N41 78.34(11) . . ? N43 Ni41 N41 156.34(11) . . ? N42 Ni41 N41 100.75(11) . 2_655 ? N43 Ni41 N41 97.35(11) . 2_655 ? N41 Ni41 N41 89.26(16) . 2_655 ? C42 O41 C41 117.3(3) . . ? C66 O42A C67A 106.8(10) . . ? C66 O42B C67B 114.2(5) . . ? O42B C67B H674 109.5 . . ? O42B C67B H675 109.5 . . ? H674 C67B H675 109.5 . . ? O42B C67B H676 109.5 . . ? H674 C67B H676 109.5 . . ? H675 C67B H676 109.5 . . ? C47 N41 C51 118.5(3) . . ? C47 N41 Ni41 127.9(2) . . ? C51 N41 Ni41 112.8(2) . . ? C52 N42 C56 121.2(3) . . ? C52 N42 Ni41 119.2(2) . . ? C56 N42 Ni41 119.5(2) . . ? C61 N43 C57 118.9(3) . . ? C61 N43 Ni41 126.5(2) . . ? C57 N43 Ni41 113.6(2) . . ? O41 C41 H411 109.5 . . ? O41 C41 H412 109.5 . . ? H411 C41 H412 109.5 . . ? O41 C41 H413 109.5 . . ? H411 C41 H413 109.5 . . ? H412 C41 H413 109.5 . . ? O41 C42 C43 116.1(3) . . ? O41 C42 C73 123.9(3) . . ? C43 C42 C73 120.0(3) . . ? C44 C43 C42 121.3(3) . . ? C44 C43 H43 119.3 . . ? C42 C43 H43 119.3 . . ? C43 C44 C46 119.2(3) . . ? C43 C44 C45 117.8(3) . . ? C46 C44 C45 122.9(3) . . ? C44 C45 H451 109.5 . . ? C44 C45 H452 109.5 . . ? H451 C45 H452 109.5 . . ? C44 C45 H453 109.5 . . ? H451 C45 H453 109.5 . . ? H452 C45 H453 109.5 . . ? C72 C46 C44 119.5(3) . . ? C72 C46 C48 120.5(3) . . ? C44 C46 C48 120.0(3) . . ? N41 C47 C48 123.8(3) . . ? N41 C47 H47 118.1 . . ? C48 C47 H47 118.1 . . ? C49 C48 C47 116.4(3) . . ? C49 C48 C46 121.4(3) . . ? C47 C48 C46 122.3(3) . . ? C50 C49 C48 120.9(3) . . ? C50 C49 H49 119.6 . . ? C48 C49 H49 119.6 . . ? C49 C50 C51 118.9(3) . . ? C49 C50 H50 120.5 . . ? C51 C50 H50 120.5 . . ? N41 C51 C50 121.4(3) . . ? N41 C51 C52 114.5(3) . . ? C50 C51 C52 124.1(3) . . ? N42 C52 C53 120.8(4) . . ? N42 C52 C51 113.7(3) . . ? C53 C52 C51 125.4(4) . . ? C52 C53 C54 118.3(4) . . ? C52 C53 H531 120.8 . . ? C54 C53 H531 120.8 . . ? C55 C54 C53 120.5(4) . . ? C55 C54 H54 119.8 . . ? C53 C54 H54 119.8 . . ? C54 C55 C56 118.9(4) . . ? C54 C55 H55 120.6 . . ? C56 C55 H55 120.6 . . ? N42 C56 C55 120.4(4) . . ? N42 C56 C57 113.6(3) . . ? C55 C56 C57 126.0(3) . . ? N43 C57 C58 120.8(3) . . ? N43 C57 C56 114.8(3) . . ? C58 C57 C56 124.4(3) . . ? C59 C58 C57 119.5(4) . . ? C59 C58 H58 120.2 . . ? C57 C58 H58 120.2 . . ? C58 C59 C60 120.7(3) . . ? C58 C59 H59 119.6 . . ? C60 C59 H59 119.6 . . ? C59 C60 C61 116.0(4) . . ? C59 C60 C62 123.0(3) . . ? C61 C60 C62 121.0(3) . . ? N43 C61 C60 123.9(3) . . ? N43 C61 H61 118.1 . . ? C60 C61 H61 118.1 . . ? C63 C62 C69 119.6(4) . . ? C63 C62 C60 120.7(4) . . ? C69 C62 C60 119.7(3) . . ? C65 C63 C62 118.9(4) . . ? C65 C63 C64 118.9(4) . . ? C62 C63 C64 122.1(4) . . ? C63 C64 H641 109.5 . . ? C63 C64 H642 109.5 . . ? H641 C64 H642 109.5 . . ? C63 C64 H643 109.5 . . ? H641 C64 H643 109.5 . . ? H642 C64 H643 109.5 . . ? C66 C65 C63 121.3(4) . . ? C66 C65 H65 119.3 . . ? C63 C65 H65 119.3 . . ? C68 C66 C65 119.9(4) . . ? C68 C66 O42A 137.8(7) . . ? C65 C66 O42A 101.4(6) . . ? C68 C66 O42B 110.7(5) . . ? C65 C66 O42B 129.4(5) . . ? C66 C68 C69 120.5(4) . . ? C66 C68 H68 119.7 . . ? C69 C68 H68 119.7 . . ? C68 C69 C62 119.8(4) . . ? C68 C69 C70 118.0(4) . . ? C62 C69 C70 122.2(4) . . ? C69 C70 H701 109.5 . . ? C69 C70 H702 109.5 . . ? H701 C70 H702 109.5 . . ? C69 C70 H703 109.5 . . ? H701 C70 H703 109.5 . . ? H702 C70 H703 109.5 . . ? C72 C71 H711 109.5 . . ? C72 C71 H712 109.5 . . ? H711 C71 H712 109.5 . . ? C72 C71 H713 109.5 . . ? H711 C71 H713 109.5 . . ? H712 C71 H713 109.5 . . ? C46 C72 C73 120.2(3) . . ? C46 C72 C71 122.8(3) . . ? C73 C72 C71 117.0(3) . . ? C42 C73 C72 119.7(4) . . ? C42 C73 H73 120.1 . . ? C72 C73 H73 120.1 . . ? N74 C75 C76 173(4) . . ? C75 C76 H761 109.5 . . ? C75 C76 H762 109.5 . . ? H761 C76 H762 109.5 . . ? C75 C76 H763 109.5 . . ? H761 C76 H763 109.5 . . ? H762 C76 H763 109.5 . . ? N77 C78 C79 180.000(1) . . ? N80 C81 C82 176.9(10) . . ? N83 C84 C85 174.4(11) . . ? N86 C87 C88 169(2) . . ? C87 C88 H881 109.5 . . ? C87 C88 H882 109.5 . . ? H881 C88 H882 109.5 . . ? C87 C88 H883 109.5 . . ? H881 C88 H883 109.5 . . ? H882 C88 H883 109.5 . . ? N89 C90 C91 174(3) . . ? C90 C91 H911 109.5 . . ? C90 C91 H912 109.5 . . ? H911 C91 H912 109.5 . . ? C90 C91 H913 109.5 . . ? H911 C91 H913 109.5 . . ? H912 C91 H913 109.5 . . ? F5B P1 F4B 91.7(4) . . ? F2A P1 F3A 93.5(3) . . ? F5B P1 F1B 91.5(4) . . ? F4B P1 F1B 91.5(4) . . ? F2A P1 F6A 91.3(3) . . ? F3A P1 F6A 91.5(3) . . ? F2A P1 F5A 92.0(3) . . ? F3A P1 F5A 89.4(3) . . ? F6A P1 F5A 176.6(3) . . ? F2A P1 F4A 90.6(3) . . ? F3A P1 F4A 175.7(3) . . ? F6A P1 F4A 89.7(3) . . ? F5A P1 F4A 89.1(3) . . ? F5B P1 F2B 90.6(4) . . ? F4B P1 F2B 89.8(4) . . ? F1B P1 F2B 177.5(5) . . ? F5B P1 F3B 90.2(4) . . ? F4B P1 F3B 177.7(5) . . ? F1B P1 F3B 89.7(4) . . ? F2B P1 F3B 89.0(4) . . ? F5B P1 F6B 177.9(5) . . ? F4B P1 F6B 89.8(4) . . ? F1B P1 F6B 89.9(4) . . ? F2B P1 F6B 87.9(4) . . ? F3B P1 F6B 88.2(4) . . ? F2A P1 F1A 178.4(3) . . ? F3A P1 F1A 88.1(3) . . ? F6A P1 F1A 88.5(3) . . ? F5A P1 F1A 88.2(3) . . ? F4A P1 F1A 87.9(3) . . ? F7B P2 F10B 91.6(3) . . ? F8A P2 F10A 91.2(4) . . ? F7B P2 F12B 91.4(3) . . ? F10B P2 F12B 90.5(3) . . ? F8A P2 F9A 91.2(4) . . ? F10A P2 F9A 177.5(5) . . ? F7B P2 F9B 90.9(4) . . ? F10B P2 F9B 177.3(4) . . ? F12B P2 F9B 90.5(3) . . ? F8A P2 F12A 90.7(4) . . ? F10A P2 F12A 90.3(4) . . ? F9A P2 F12A 90.3(4) . . ? F8A P2 F11A 91.0(4) . . ? F10A P2 F11A 89.6(4) . . ? F9A P2 F11A 89.7(4) . . ? F12A P2 F11A 178.3(5) . . ? F7B P2 F11B 90.0(3) . . ? F10B P2 F11B 89.5(3) . . ? F12B P2 F11B 178.6(4) . . ? F9B P2 F11B 89.4(3) . . ? F7B P2 F8B 179.0(4) . . ? F10B P2 F8B 88.9(3) . . ? F12B P2 F8B 89.5(3) . . ? F9B P2 F8B 88.7(3) . . ? F11B P2 F8B 89.1(3) . . ? F8A P2 F7A 179.6(5) . . ? F10A P2 F7A 89.2(4) . . ? F9A P2 F7A 88.4(4) . . ? F12A P2 F7A 89.3(4) . . ? F11A P2 F7A 89.0(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ni1 N1 C7 -175.5(3) . . . . ? N2 Ni1 N1 C7 6.6(3) 2 . . . ? N1 Ni1 N1 C7 -70.0(3) 2 . . . ? N3 Ni1 N1 C7 86.7(3) 2 . . . ? N3 Ni1 N1 C7 -173.6(3) . . . . ? N2 Ni1 N1 C11 -5.1(2) . . . . ? N2 Ni1 N1 C11 177.0(2) 2 . . . ? N1 Ni1 N1 C11 100.4(3) 2 . . . ? N3 Ni1 N1 C11 -102.8(3) 2 . . . ? N3 Ni1 N1 C11 -3.2(4) . . . . ? N2 Ni1 N2 C12 139.9(3) 2 . . . ? N1 Ni1 N2 C12 -82.0(3) 2 . . . ? N1 Ni1 N2 C12 1.3(3) . . . . ? N3 Ni1 N2 C12 98.1(3) 2 . . . ? N3 Ni1 N2 C12 -178.0(3) . . . . ? N2 Ni1 N2 C16 -35.8(2) 2 . . . ? N1 Ni1 N2 C16 102.3(3) 2 . . . ? N1 Ni1 N2 C16 -174.4(3) . . . . ? N3 Ni1 N2 C16 -77.7(3) 2 . . . ? N3 Ni1 N2 C16 6.3(2) . . . . ? N2 Ni1 N3 C21 -178.4(3) . . . . ? N2 Ni1 N3 C21 -0.5(3) 2 . . . ? N1 Ni1 N3 C21 78.6(3) 2 . . . ? N1 Ni1 N3 C21 179.7(3) . . . . ? N3 Ni1 N3 C21 -78.0(3) 2 . . . ? N2 Ni1 N3 C17 -8.7(2) . . . . ? N2 Ni1 N3 C17 169.2(2) 2 . . . ? N1 Ni1 N3 C17 -111.8(2) 2 . . . ? N1 Ni1 N3 C17 -10.6(4) . . . . ? N3 Ni1 N3 C17 91.6(2) 2 . . . ? C1 O1 C2 C33 -4.8(5) . . . . ? C1 O1 C2 C3 175.3(3) . . . . ? O1 C2 C3 C4 179.4(3) . . . . ? C33 C2 C3 C4 -0.6(6) . . . . ? C2 C3 C4 C6 -0.2(6) . . . . ? C2 C3 C4 C5 177.6(4) . . . . ? C3 C4 C6 C32 0.6(6) . . . . ? C5 C4 C6 C32 -177.1(4) . . . . ? C3 C4 C6 C8 -179.8(3) . . . . ? C5 C4 C6 C8 2.5(6) . . . . ? C11 N1 C7 C8 -1.3(6) . . . . ? Ni1 N1 C7 C8 168.8(3) . . . . ? N1 C7 C8 C9 1.2(6) . . . . ? N1 C7 C8 C6 -179.7(3) . . . . ? C32 C6 C8 C9 -122.9(4) . . . . ? C4 C6 C8 C9 57.5(5) . . . . ? C32 C6 C8 C7 58.1(5) . . . . ? C4 C6 C8 C7 -121.5(4) . . . . ? C7 C8 C9 C10 -0.3(6) . . . . ? C6 C8 C9 C10 -179.4(4) . . . . ? C8 C9 C10 C11 -0.4(6) . . . . ? C7 N1 C11 C10 0.4(5) . . . . ? Ni1 N1 C11 C10 -170.9(3) . . . . ? C7 N1 C11 C12 179.1(3) . . . . ? Ni1 N1 C11 C12 7.8(4) . . . . ? C9 C10 C11 N1 0.4(6) . . . . ? C9 C10 C11 C12 -178.2(4) . . . . ? C16 N2 C12 C13 -0.6(5) . . . . ? Ni1 N2 C12 C13 -176.2(3) . . . . ? C16 N2 C12 C11 178.0(3) . . . . ? Ni1 N2 C12 C11 2.4(4) . . . . ? N1 C11 C12 N2 -6.8(5) . . . . ? C10 C11 C12 N2 171.8(4) . . . . ? N1 C11 C12 C13 171.7(4) . . . . ? C10 C11 C12 C13 -9.6(6) . . . . ? N2 C12 C13 C14 0.5(6) . . . . ? C11 C12 C13 C14 -178.0(4) . . . . ? C12 C13 C14 C15 0.2(6) . . . . ? C13 C14 C15 C16 -0.8(6) . . . . ? C12 N2 C16 C15 0.0(5) . . . . ? Ni1 N2 C16 C15 175.7(3) . . . . ? C12 N2 C16 C17 -178.7(3) . . . . ? Ni1 N2 C16 C17 -3.0(4) . . . . ? C14 C15 C16 N2 0.7(5) . . . . ? C14 C15 C16 C17 179.2(4) . . . . ? C21 N3 C17 C18 1.9(5) . . . . ? Ni1 N3 C17 C18 -168.7(3) . . . . ? C21 N3 C17 C16 -179.6(3) . . . . ? Ni1 N3 C17 C16 9.7(4) . . . . ? N2 C16 C17 N3 -4.8(4) . . . . ? C15 C16 C17 N3 176.6(3) . . . . ? N2 C16 C17 C18 173.6(3) . . . . ? C15 C16 C17 C18 -5.0(6) . . . . ? N3 C17 C18 C19 -0.4(5) . . . . ? C16 C17 C18 C19 -178.7(3) . . . . ? C17 C18 C19 C20 -1.0(5) . . . . ? C18 C19 C20 C21 0.9(5) . . . . ? C18 C19 C20 C22 -179.4(3) . . . . ? C17 N3 C21 C20 -2.1(5) . . . . ? Ni1 N3 C21 C20 167.1(3) . . . . ? C19 C20 C21 N3 0.7(5) . . . . ? C22 C20 C21 N3 -179.0(3) . . . . ? C19 C20 C22 C23 56.5(5) . . . . ? C21 C20 C22 C23 -123.8(4) . . . . ? C19 C20 C22 C29 -122.3(4) . . . . ? C21 C20 C22 C29 57.5(5) . . . . ? C29 C22 C23 C25 1.2(5) . . . . ? C20 C22 C23 C25 -177.5(3) . . . . ? C29 C22 C23 C24 -175.0(3) . . . . ? C20 C22 C23 C24 6.3(5) . . . . ? C22 C23 C25 C26 -0.2(6) . . . . ? C24 C23 C25 C26 176.2(4) . . . . ? C27B O2B C26 C25 0(3) . . . . ? C27B O2B C26 C28 175.8(14) . . . . ? C23 C25 C26 O2B 174.5(17) . . . . ? C23 C25 C26 C28 -0.7(6) . . . . ? C23 C25 C26 O2A -175(3) . . . . ? C27A O2A C26 C25 16(6) . . . . ? C27A O2A C26 C28 -159(3) . . . . ? O2B C26 C28 C29 -175.1(16) . . . . ? C25 C26 C28 C29 0.6(6) . . . . ? O2A C26 C28 C29 176(3) . . . . ? C26 C28 C29 C22 0.4(6) . . . . ? C26 C28 C29 C30 178.9(4) . . . . ? C23 C22 C29 C28 -1.3(5) . . . . ? C20 C22 C29 C28 177.4(3) . . . . ? C23 C22 C29 C30 -179.8(4) . . . . ? C20 C22 C29 C30 -1.0(5) . . . . ? C4 C6 C32 C33 -0.2(6) . . . . ? C8 C6 C32 C33 -179.8(3) . . . . ? C4 C6 C32 C31 179.6(4) . . . . ? C8 C6 C32 C31 0.0(6) . . . . ? O1 C2 C33 C32 -179.0(3) . . . . ? C3 C2 C33 C32 1.0(6) . . . . ? C6 C32 C33 C2 -0.6(6) . . . . ? C31 C32 C33 C2 179.6(4) . . . . ? N42 Ni41 N41 C47 -0.3(3) 2_655 . . . ? N42 Ni41 N41 C47 178.8(3) . . . . ? N43 Ni41 N41 C47 -79.5(3) 2_655 . . . ? N43 Ni41 N41 C47 -175.5(3) . . . . ? N41 Ni41 N41 C47 77.7(3) 2_655 . . . ? N42 Ni41 N41 C51 -170.2(2) 2_655 . . . ? N42 Ni41 N41 C51 9.0(2) . . . . ? N43 Ni41 N41 C51 110.6(2) 2_655 . . . ? N43 Ni41 N41 C51 14.6(4) . . . . ? N41 Ni41 N41 C51 -92.2(2) 2_655 . . . ? N42 Ni41 N42 C52 40.9(3) 2_655 . . . ? N43 Ni41 N42 C52 -97.7(3) 2_655 . . . ? N43 Ni41 N42 C52 179.6(3) . . . . ? N41 Ni41 N42 C52 -2.7(3) . . . . ? N41 Ni41 N42 C52 84.3(3) 2_655 . . . ? N42 Ni41 N42 C56 -143.8(3) 2_655 . . . ? N43 Ni41 N42 C56 77.6(3) 2_655 . . . ? N43 Ni41 N42 C56 -5.1(3) . . . . ? N41 Ni41 N42 C56 172.6(3) . . . . ? N41 Ni41 N42 C56 -100.5(3) 2_655 . . . ? N42 Ni41 N43 C61 -6.0(3) 2_655 . . . ? N42 Ni41 N43 C61 174.9(3) . . . . ? N43 Ni41 N43 C61 70.8(3) 2_655 . . . ? N41 Ni41 N43 C61 169.2(3) . . . . ? N41 Ni41 N43 C61 -85.6(3) 2_655 . . . ? N42 Ni41 N43 C57 -174.6(2) 2_655 . . . ? N42 Ni41 N43 C57 6.3(2) . . . . ? N43 Ni41 N43 C57 -97.8(2) 2_655 . . . ? N41 Ni41 N43 C57 0.6(4) . . . . ? N41 Ni41 N43 C57 105.8(2) 2_655 . . . ? C41 O41 C42 C43 -176.8(4) . . . . ? C41 O41 C42 C73 2.5(5) . . . . ? O41 C42 C43 C44 -178.2(3) . . . . ? C73 C42 C43 C44 2.4(6) . . . . ? C42 C43 C44 C46 0.6(6) . . . . ? C42 C43 C44 C45 -177.1(3) . . . . ? C43 C44 C46 C72 -3.3(5) . . . . ? C45 C44 C46 C72 174.3(3) . . . . ? C43 C44 C46 C48 174.4(3) . . . . ? C45 C44 C46 C48 -8.0(5) . . . . ? C51 N41 C47 C48 3.2(5) . . . . ? Ni41 N41 C47 C48 -166.2(3) . . . . ? N41 C47 C48 C49 0.2(5) . . . . ? N41 C47 C48 C46 -179.1(3) . . . . ? C72 C46 C48 C49 123.8(4) . . . . ? C44 C46 C48 C49 -53.9(5) . . . . ? C72 C46 C48 C47 -57.0(5) . . . . ? C44 C46 C48 C47 125.3(4) . . . . ? C47 C48 C49 C50 -2.4(5) . . . . ? C46 C48 C49 C50 176.9(3) . . . . ? C48 C49 C50 C51 1.2(6) . . . . ? C47 N41 C51 C50 -4.4(5) . . . . ? Ni41 N41 C51 C50 166.5(3) . . . . ? C47 N41 C51 C52 175.8(3) . . . . ? Ni41 N41 C51 C52 -13.3(4) . . . . ? C49 C50 C51 N41 2.3(6) . . . . ? C49 C50 C51 C52 -177.9(4) . . . . ? C56 N42 C52 C53 -1.1(6) . . . . ? Ni41 N42 C52 C53 174.1(3) . . . . ? C56 N42 C52 C51 -178.7(3) . . . . ? Ni41 N42 C52 C51 -3.5(4) . . . . ? N41 C51 C52 N42 11.4(5) . . . . ? C50 C51 C52 N42 -168.4(3) . . . . ? N41 C51 C52 C53 -166.1(4) . . . . ? C50 C51 C52 C53 14.1(6) . . . . ? N42 C52 C53 C54 0.8(7) . . . . ? C51 C52 C53 C54 178.2(4) . . . . ? C52 C53 C54 C55 -0.6(8) . . . . ? C53 C54 C55 C56 0.6(8) . . . . ? C52 N42 C56 C55 1.0(5) . . . . ? Ni41 N42 C56 C55 -174.1(3) . . . . ? C52 N42 C56 C57 178.3(3) . . . . ? Ni41 N42 C56 C57 3.1(4) . . . . ? C54 C55 C56 N42 -0.8(7) . . . . ? C54 C55 C56 C57 -177.7(4) . . . . ? C61 N43 C57 C58 1.4(5) . . . . ? Ni41 N43 C57 C58 171.0(3) . . . . ? C61 N43 C57 C56 -176.1(3) . . . . ? Ni41 N43 C57 C56 -6.6(4) . . . . ? N42 C56 C57 N43 2.6(4) . . . . ? C55 C56 C57 N43 179.6(4) . . . . ? N42 C56 C57 C58 -174.8(3) . . . . ? C55 C56 C57 C58 2.2(6) . . . . ? N43 C57 C58 C59 -3.3(5) . . . . ? C56 C57 C58 C59 174.0(3) . . . . ? C57 C58 C59 C60 2.3(6) . . . . ? C58 C59 C60 C61 0.5(5) . . . . ? C58 C59 C60 C62 -177.8(4) . . . . ? C57 N43 C61 C60 1.5(5) . . . . ? Ni41 N43 C61 C60 -166.5(3) . . . . ? C59 C60 C61 N43 -2.5(5) . . . . ? C62 C60 C61 N43 175.8(3) . . . . ? C59 C60 C62 C63 -60.3(5) . . . . ? C61 C60 C62 C63 121.6(4) . . . . ? C59 C60 C62 C69 119.4(4) . . . . ? C61 C60 C62 C69 -58.8(5) . . . . ? C69 C62 C63 C65 0.1(6) . . . . ? C60 C62 C63 C65 179.8(4) . . . . ? C69 C62 C63 C64 177.1(4) . . . . ? C60 C62 C63 C64 -3.2(6) . . . . ? C62 C63 C65 C66 0.3(6) . . . . ? C64 C63 C65 C66 -176.8(4) . . . . ? C63 C65 C66 C68 -0.1(7) . . . . ? C63 C65 C66 O42A -171.3(7) . . . . ? C63 C65 C66 O42B 178.1(5) . . . . ? C67A O42A C66 C68 23.6(19) . . . . ? C67A O42A C66 C65 -167.9(11) . . . . ? C67B O42B C66 C68 163.3(5) . . . . ? C67B O42B C66 C65 -15.1(9) . . . . ? C65 C66 C68 C69 -0.4(7) . . . . ? O42A C66 C68 C69 166.6(10) . . . . ? O42B C66 C68 C69 -178.9(4) . . . . ? C66 C68 C69 C62 0.7(6) . . . . ? C66 C68 C69 C70 -179.2(4) . . . . ? C63 C62 C69 C68 -0.6(6) . . . . ? C60 C62 C69 C68 179.7(4) . . . . ? C63 C62 C69 C70 179.3(4) . . . . ? C60 C62 C69 C70 -0.3(6) . . . . ? C44 C46 C72 C73 3.0(5) . . . . ? C48 C46 C72 C73 -174.7(3) . . . . ? C44 C46 C72 C71 -177.8(4) . . . . ? C48 C46 C72 C71 4.5(5) . . . . ? O41 C42 C73 C72 178.0(3) . . . . ? C43 C42 C73 C72 -2.7(5) . . . . ? C46 C72 C73 C42 0.0(5) . . . . ? C71 C72 C73 C42 -179.3(3) . . . . ? #===END data_6b _database_code_depnum_ccdc_archive 'CCDC 735260' # SG0413 _audit_creation_method SHELXL-97 _audit_creation_date 04-07-06 _chemical_name_systematic ; bis[5,5"-bis-(4-methoxy-2,6-dimethylphenyl)- [2,2':6,2"]terpyridine]copper(II) hexafluorophosphate 2.5-acetonitrile solvate ; _chemical_name_common ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_moiety 'C66 H62 Cu N6 O4 2+, 2(F6 P 1-), 2.5(C2 H3 N)' _chemical_formula_sum 'C71 H69.50 Cu F12 N8.50 O4 P2' _chemical_formula_weight 1459.35 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 568 0.0033 0.0016 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; H H 556 0.0000 0.0000 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; Cu Cu 8 0.3201 1.2651 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; F F 96 0.0061 0.0033 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; N N 68 0.0106 0.0060 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; O O 32 0.0171 0.0103 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; P P 16 0.1023 0.0942 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n n a ' _symmetry_space_group_name_Hall ? _symmetry_Int_Tables_number 52 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' 'x, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' '-x, y-1/2, z-1/2' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 22.0072(3) _cell_length_b 24.9787(4) _cell_length_c 25.1014(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 13798.5(3) _cell_formula_units_Z 8 _cell_measurement_temperature 160(1) _cell_measurement_reflns_used 219498 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.405 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6032 _exptl_absorpt_coefficient_mu 0.451 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Blessing, 1995)' _exptl_absorpt_correction_T_min 0.747 _exptl_absorpt_correction_T_max 0.915 _exptl_special_details ; Solvent used: acetonitrile / diethylether Cooling Device: Oxford Cryosystems Cryostream 700 Crystal mount: glued on a glass fibre Mosaicity (deg.): 0.762(1) Frames collected: 413 Seconds exposure per frame: 44 Degrees rotation per frame: 1.1 Crystal-Detector distance (mm): 37.7 ; _diffrn_ambient_temperature 160(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Nonius FR590 sealed tube generator' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_detector '65 mm CCD camera on \k goniostat' _diffrn_measurement_device_type 'Nonius KappaCCD area-detector diffractometer' _diffrn_measurement_method '\f and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 146815 _diffrn_reflns_av_R_equivalents 0.0923 _diffrn_reflns_av_sigmaI/netI 0.0519 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 25.02 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.999 _reflns_number_total 12190 _reflns_number_gt 8865 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'COLLECT (Nonius, 2000)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN and SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'DIRDIF94 (Beurskens et al., 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'SHELXL97 and PLATON (Spek, 2009)' _refine_special_details ; The asymmetric unit contains two half-cations with each Cu-atom on a crystallographic two-fold axis, two disordered PF6- anions, and two to three disordered MeCN molecules. The disorder of the MeCN molecules could not be modelled adequately, so the SQUEEZE routine of the program PLATON was employed. This procedure, which allows the disordered solvent molecules to be omitted entirely from the subsequent refinement model, gave better refinement results and there were no significant peaks of residual electron density to be found in the voids of the structure. The procedure leaves eight cavities of 133 \%A^3^ per unit cell. The electron count in the disordered region was calculated to be 55 e per cavity. Allowing for 2.5 MeCN molecules per cavity yields 55 e, and this estimate was used in the subsequent calculation of the empirical formula, formula weight, density, linear absorption coefficient and F(000), although 2.5 may be an underbound. Each symmetry-independent PF6- anion is disordered over two orientations. Two orientations were defined for each anion and refinement of the site occupation factors led to values of 0.54(2) and 0.675(7) for the major orientations. The P-F and F...F distances were restrained tightly, so as to maintain octahedral geometry and uniform P-F bond lengths and neighbouring atoms within and between each disordered orientation were restrained to have similar atomic displacement parameters and pseudo-isotropic restraints were applied to the disordered F-atoms. One methoxy group and its parent mesityl group in each ligand of each symmetry-independent cation is disordered. Two conformations for these groups were defined in each case and refinement of the site occupation factors led to a values of 0.637(9) and 0.62(2) for the major conformations. Similarity restraints were applied to the chemically equivalent bond lengths and angles involving all disordered atoms in each cation. Furthermore, neighbouring disordered atoms were restrained to have similar atomic displacement parameters and the disordered mesityl ring in one cation was restrained to be a planar group. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1066P)^2^+64.2448P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00096(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 12186 _refine_ls_number_parameters 1069 _refine_ls_number_restraints 2160 _refine_ls_R_factor_all 0.1321 _refine_ls_R_factor_gt 0.0984 _refine_ls_wR_factor_ref 0.2595 _refine_ls_wR_factor_gt 0.2407 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 0.994 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.389 _refine_diff_density_min -1.307 _refine_diff_density_rms 0.102 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 0.2500 0.0000 0.38220(3) 0.0319(3) Uani 1 2 d S . . O1 O -0.06072(18) 0.02281(16) 0.11520(17) 0.0498(11) Uani 1 1 d . . . O2A O 0.3742(6) 0.2193(5) 0.6695(6) 0.062(2) Uani 0.370(9) 1 d PDU A 1 C22A C 0.3602(10) 0.094(2) 0.562(3) 0.045(2) Uani 0.370(9) 1 d PDU A 1 C23A C 0.4173(8) 0.1150(10) 0.5750(11) 0.047(2) Uani 0.370(9) 1 d PDU A 1 C24A C 0.4748(9) 0.0932(10) 0.5492(10) 0.051(4) Uani 0.370(9) 1 d PDU A 1 H241 H 0.5104 0.1104 0.5653 0.076 Uiso 0.370(9) 1 calc PR A 1 H242 H 0.4741 0.1007 0.5109 0.076 Uiso 0.370(9) 1 calc PR A 1 H243 H 0.4771 0.0545 0.5549 0.076 Uiso 0.370(9) 1 calc PR A 1 C25A C 0.4221(7) 0.1565(8) 0.6096(9) 0.048(3) Uani 0.370(9) 1 d PDU A 1 H251 H 0.4610 0.1700 0.6189 0.058 Uiso 0.370(9) 1 calc PR A 1 C26A C 0.3696(7) 0.1794(8) 0.6316(9) 0.050(2) Uani 0.370(9) 1 d PDU A 1 C27A C 0.3227(8) 0.2492(7) 0.6843(8) 0.069(3) Uani 0.370(9) 1 d PDU A 1 H271 H 0.2983 0.2570 0.6526 0.104 Uiso 0.370(9) 1 calc PR A 1 H272 H 0.3357 0.2829 0.7009 0.104 Uiso 0.370(9) 1 calc PR A 1 H273 H 0.2984 0.2286 0.7098 0.104 Uiso 0.370(9) 1 calc PR A 1 C28A C 0.3142(7) 0.1593(9) 0.6200(11) 0.044(3) Uani 0.370(9) 1 d PDU A 1 H281 H 0.2791 0.1743 0.6362 0.053 Uiso 0.370(9) 1 calc PR A 1 C29A C 0.3082(8) 0.1174(10) 0.5849(12) 0.043(2) Uani 0.370(9) 1 d PDU A 1 C30A C 0.2448(8) 0.0975(8) 0.5719(9) 0.047(3) Uani 0.370(9) 1 d PDU A 1 H301 H 0.2163 0.1103 0.5991 0.070 Uiso 0.370(9) 1 calc PR A 1 H302 H 0.2447 0.0583 0.5714 0.070 Uiso 0.370(9) 1 calc PR A 1 H303 H 0.2325 0.1111 0.5369 0.070 Uiso 0.370(9) 1 calc PR A 1 O2B O 0.3424(4) 0.2265(3) 0.6624(4) 0.064(2) Uani 0.630(9) 1 d PDU A 2 C22B C 0.3546(6) 0.0932(13) 0.5634(16) 0.0440(19) Uani 0.630(9) 1 d PDU A 2 C23B C 0.4067(5) 0.1238(6) 0.5745(7) 0.047(2) Uani 0.630(9) 1 d PDU A 2 C24B C 0.4675(6) 0.1094(6) 0.5495(6) 0.053(3) Uani 0.630(9) 1 d PDU A 2 H244 H 0.4952 0.1400 0.5523 0.079 Uiso 0.630(9) 1 calc PR A 2 H245 H 0.4615 0.1003 0.5119 0.079 Uiso 0.630(9) 1 calc PR A 2 H246 H 0.4850 0.0786 0.5682 0.079 Uiso 0.630(9) 1 calc PR A 2 C25B C 0.4037(5) 0.1668(5) 0.6074(5) 0.048(2) Uani 0.630(9) 1 d PDU A 2 H252 H 0.4396 0.1863 0.6158 0.058 Uiso 0.630(9) 1 calc PR A 2 C26B C 0.3481(5) 0.1824(5) 0.6292(5) 0.049(2) Uani 0.630(9) 1 d PDU A 2 C27B C 0.3892(5) 0.2650(4) 0.6639(5) 0.069(3) Uani 0.630(9) 1 d PDU A 2 H274 H 0.4238 0.2508 0.6840 0.104 Uiso 0.630(9) 1 calc PR A 2 H275 H 0.3742 0.2976 0.6813 0.104 Uiso 0.630(9) 1 calc PR A 2 H276 H 0.4021 0.2735 0.6275 0.104 Uiso 0.630(9) 1 calc PR A 2 C28B C 0.2974(5) 0.1536(5) 0.6192(6) 0.044(2) Uani 0.630(9) 1 d PDU A 2 H282 H 0.2598 0.1642 0.6346 0.052 Uiso 0.630(9) 1 calc PR A 2 C29B C 0.2993(5) 0.1092(6) 0.5871(7) 0.043(2) Uani 0.630(9) 1 d PDU A 2 C30B C 0.2410(5) 0.0781(5) 0.5790(5) 0.054(3) Uani 0.630(9) 1 d PDU A 2 H304 H 0.2458 0.0418 0.5934 0.080 Uiso 0.630(9) 1 calc PR A 2 H305 H 0.2317 0.0760 0.5409 0.080 Uiso 0.630(9) 1 calc PR A 2 H306 H 0.2076 0.0962 0.5976 0.080 Uiso 0.630(9) 1 calc PR A 2 N1 N 0.1986(2) -0.04192(17) 0.32094(17) 0.0395(11) Uani 1 1 d . . . N2 N 0.29095(19) -0.06984(17) 0.38126(16) 0.0317(10) Uani 1 1 d . . . N3 N 0.31602(18) 0.00850(16) 0.44572(16) 0.0305(10) Uani 1 1 d . . . C1 C -0.0606(3) 0.0760(3) 0.0947(3) 0.0549(17) Uani 1 1 d . . . H11 H -0.0542 0.1014 0.1239 0.082 Uiso 1 1 calc R . . H12 H -0.0998 0.0834 0.0776 0.082 Uiso 1 1 calc R . . H13 H -0.0279 0.0798 0.0685 0.082 Uiso 1 1 calc R . . C2 C -0.0138(3) 0.0088(2) 0.1486(2) 0.0412(13) Uani 1 1 d . . . C3 C -0.0167(3) -0.0416(2) 0.1700(2) 0.0434(14) Uani 1 1 d . . . H3 H -0.0508 -0.0637 0.1623 0.052 Uiso 1 1 calc R . . C4 C 0.0291(3) -0.0609(2) 0.2026(2) 0.0418(14) Uani 1 1 d . . . C5 C 0.0225(3) -0.1161(2) 0.2269(3) 0.0565(17) Uani 1 1 d . . . H51 H -0.0202 -0.1272 0.2252 0.085 Uiso 1 1 calc R . . H52 H 0.0358 -0.1151 0.2641 0.085 Uiso 1 1 calc R . . H53 H 0.0475 -0.1416 0.2070 0.085 Uiso 1 1 calc R . . C6 C 0.0801(3) -0.0284(2) 0.2136(2) 0.0383(13) Uani 1 1 d . . . C7 C 0.1522(3) -0.0242(2) 0.2914(2) 0.0396(13) Uani 1 1 d . . . H7 H 0.1320 0.0074 0.3027 0.048 Uiso 1 1 calc R . . C8 C 0.1317(2) -0.04937(19) 0.2449(2) 0.0322(12) Uani 1 1 d . . . C9 C 0.1632(3) -0.0953(2) 0.2296(2) 0.0391(13) Uani 1 1 d . . . H9 H 0.1526 -0.1131 0.1975 0.047 Uiso 1 1 calc R . . C10 C 0.2100(3) -0.1149(2) 0.2609(2) 0.0396(13) Uani 1 1 d . . . H10 H 0.2310 -0.1465 0.2508 0.047 Uiso 1 1 calc R . . C11 C 0.2260(3) -0.08827(19) 0.3070(2) 0.0334(12) Uani 1 1 d . . . C12 C 0.2733(3) -0.1065(2) 0.3448(2) 0.0396(13) Uani 1 1 d . . . C13 C 0.2985(4) -0.1565(2) 0.3442(3) 0.066(2) Uani 1 1 d . . . H131 H 0.2870 -0.1821 0.3180 0.080 Uiso 1 1 calc R . . C14 C 0.3412(4) -0.1688(3) 0.3827(3) 0.076(2) Uani 1 1 d . . . H14 H 0.3588 -0.2035 0.3835 0.092 Uiso 1 1 calc R . . C15 C 0.3583(3) -0.1314(2) 0.4198(3) 0.0578(18) Uani 1 1 d . . . H15 H 0.3875 -0.1400 0.4463 0.069 Uiso 1 1 calc R . . C16 C 0.3329(3) -0.0821(2) 0.4180(2) 0.0380(13) Uani 1 1 d . . . C17 C 0.3452(2) -0.0375(2) 0.4566(2) 0.0329(12) Uani 1 1 d . . . C18 C 0.3819(2) -0.0428(2) 0.5013(2) 0.0386(13) Uani 1 1 d . . . H18 H 0.4036 -0.0751 0.5078 0.046 Uiso 1 1 calc R . . C19 C 0.3863(3) -0.0005(3) 0.5360(2) 0.0458(14) Uani 1 1 d . A . H19 H 0.4105 -0.0040 0.5672 0.055 Uiso 1 1 calc R . . C20 C 0.3561(2) 0.0471(2) 0.5263(2) 0.0386(13) Uani 1 1 d D . . C21 C 0.3219(3) 0.0494(2) 0.4790(2) 0.0374(13) Uani 1 1 d . A . H21 H 0.3019 0.0820 0.4705 0.045 Uiso 1 1 calc R . . C31 C 0.1326(3) 0.0631(2) 0.2049(2) 0.0466(15) Uani 1 1 d . . . H311 H 0.1300 0.0751 0.2420 0.070 Uiso 1 1 calc R . . H312 H 0.1289 0.0941 0.1811 0.070 Uiso 1 1 calc R . . H313 H 0.1718 0.0455 0.1989 0.070 Uiso 1 1 calc R . . C32 C 0.0816(3) 0.0240(2) 0.1935(2) 0.0375(13) Uani 1 1 d . . . C33 C 0.0341(2) 0.0423(2) 0.1610(2) 0.0367(12) Uani 1 1 d . . . H33 H 0.0348 0.0779 0.1475 0.044 Uiso 1 1 calc R . . Cu2 Cu 0.7500 0.0000 0.09376(3) 0.0349(3) Uani 1 2 d S . . O41 O 0.4590(2) 0.00046(19) 0.36706(19) 0.0595(12) Uani 1 1 d . . . O42A O 0.8349(7) 0.2642(5) -0.1610(7) 0.057(3) Uani 0.380(17) 1 d PDU B 1 C67A C 0.8863(8) 0.2986(7) -0.1620(10) 0.059(3) Uani 0.380(17) 1 d PDU B 1 H671 H 0.8908 0.3159 -0.1271 0.089 Uiso 0.380(17) 1 calc PR B 1 H672 H 0.8806 0.3260 -0.1895 0.089 Uiso 0.380(17) 1 calc PR B 1 H673 H 0.9228 0.2776 -0.1699 0.089 Uiso 0.380(17) 1 calc PR B 1 C62A C 0.8446(12) 0.1212(3) -0.0768(2) 0.035(2) Uani 0.380(17) 1 d PDU B 1 C63A C 0.8981(10) 0.1492(5) -0.0874(3) 0.039(2) Uani 0.380(17) 1 d PDU B 1 C64A C 0.9596(12) 0.1322(8) -0.0656(4) 0.042(3) Uani 0.380(17) 1 d PDU B 1 H641 H 0.9913 0.1556 -0.0800 0.063 Uiso 0.380(17) 1 calc PR B 1 H642 H 0.9679 0.0951 -0.0761 0.063 Uiso 0.380(17) 1 calc PR B 1 H643 H 0.9593 0.1348 -0.0266 0.063 Uiso 0.380(17) 1 calc PR B 1 C65A C 0.8963(8) 0.1947(4) -0.1190(3) 0.046(2) Uani 0.380(17) 1 d PDU B 1 H651 H 0.9329 0.2136 -0.1261 0.055 Uiso 0.380(17) 1 calc PR B 1 C66A C 0.8424(8) 0.2132(4) -0.1405(3) 0.049(2) Uani 0.380(17) 1 d PDU B 1 C68A C 0.7896(8) 0.1857(4) -0.1299(4) 0.042(2) Uani 0.380(17) 1 d PDU B 1 H681 H 0.7524 0.1984 -0.1444 0.050 Uiso 0.380(17) 1 calc PR B 1 C69A C 0.7893(10) 0.1399(4) -0.0986(4) 0.035(2) Uani 0.380(17) 1 d PDU B 1 C70A C 0.7285(12) 0.1171(8) -0.0819(9) 0.036(3) Uani 0.380(17) 1 d PDU B 1 H701 H 0.7206 0.1262 -0.0445 0.053 Uiso 0.380(17) 1 calc PR B 1 H702 H 0.7291 0.0780 -0.0859 0.053 Uiso 0.380(17) 1 calc PR B 1 H703 H 0.6964 0.1322 -0.1043 0.053 Uiso 0.380(17) 1 calc PR B 1 O42B O 0.8376(4) 0.2528(4) -0.1784(4) 0.053(2) Uani 0.620(17) 1 d PDU B 2 C67B C 0.8922(5) 0.2799(5) -0.1925(6) 0.064(3) Uani 0.620(17) 1 d PDU B 2 H674 H 0.9060 0.3016 -0.1623 0.096 Uiso 0.620(17) 1 calc PR B 2 H675 H 0.8845 0.3032 -0.2232 0.096 Uiso 0.620(17) 1 calc PR B 2 H676 H 0.9235 0.2537 -0.2017 0.096 Uiso 0.620(17) 1 calc PR B 2 C62B C 0.8455(7) 0.1211(2) -0.0770(2) 0.0338(17) Uani 0.620(17) 1 d PDU B 2 C63B C 0.8987(7) 0.1494(3) -0.0878(2) 0.0374(16) Uani 0.620(17) 1 d PDU B 2 C64B C 0.9604(7) 0.1332(5) -0.0656(3) 0.043(2) Uani 0.620(17) 1 d PDU B 2 H644 H 0.9550 0.1166 -0.0306 0.064 Uiso 0.620(17) 1 calc PR B 2 H645 H 0.9861 0.1650 -0.0622 0.064 Uiso 0.620(17) 1 calc PR B 2 H646 H 0.9797 0.1076 -0.0899 0.064 Uiso 0.620(17) 1 calc PR B 2 C65B C 0.8963(6) 0.1950(3) -0.1193(3) 0.0470(18) Uani 0.620(17) 1 d PDU B 2 H652 H 0.9326 0.2142 -0.1265 0.056 Uiso 0.620(17) 1 calc PR B 2 C66B C 0.8420(5) 0.2129(3) -0.1404(3) 0.0496(17) Uani 0.620(17) 1 d PDU B 2 C68B C 0.7895(5) 0.1854(3) -0.1295(3) 0.0416(18) Uani 0.620(17) 1 d PDU B 2 H682 H 0.7521 0.1979 -0.1437 0.050 Uiso 0.620(17) 1 calc PR B 2 C69B C 0.7898(7) 0.1395(3) -0.0981(3) 0.0342(15) Uani 0.620(17) 1 d PDU B 2 C70B C 0.7315(7) 0.1080(5) -0.0930(6) 0.036(3) Uani 0.620(17) 1 d PDU B 2 H704 H 0.7010 0.1227 -0.1174 0.055 Uiso 0.620(17) 1 calc PR B 2 H705 H 0.7165 0.1104 -0.0563 0.055 Uiso 0.620(17) 1 calc PR B 2 H706 H 0.7392 0.0704 -0.1020 0.055 Uiso 0.620(17) 1 calc PR B 2 N41 N 0.7131(2) -0.04912(18) 0.15680(17) 0.0399(11) Uani 1 1 d . . . N42 N 0.8028(2) -0.06388(16) 0.09118(16) 0.0337(10) Uani 1 1 d . . . N43 N 0.81255(19) 0.02072(17) 0.03081(16) 0.0308(10) Uani 1 1 d . . . C41 C 0.4574(3) 0.0539(3) 0.3882(3) 0.0583(17) Uani 1 1 d . . . H411 H 0.4893 0.0580 0.4151 0.087 Uiso 1 1 calc R . . H412 H 0.4176 0.0605 0.4046 0.087 Uiso 1 1 calc R . . H413 H 0.4640 0.0797 0.3594 0.087 Uiso 1 1 calc R . . C42 C 0.5073(3) -0.0122(2) 0.3354(2) 0.0439(14) Uani 1 1 d . . . C43 C 0.5057(3) -0.0624(3) 0.3123(3) 0.0552(17) Uani 1 1 d . . . H43 H 0.4719 -0.0851 0.3188 0.066 Uiso 1 1 calc R . . C44 C 0.5529(3) -0.0803(3) 0.2797(2) 0.0526(16) Uani 1 1 d . . . C45 C 0.5457(4) -0.1344(3) 0.2539(3) 0.073(2) Uani 1 1 d . . . H451 H 0.5670 -0.1346 0.2196 0.109 Uiso 1 1 calc R . . H452 H 0.5025 -0.1417 0.2482 0.109 Uiso 1 1 calc R . . H453 H 0.5631 -0.1619 0.2772 0.109 Uiso 1 1 calc R . . C46 C 0.6028(3) -0.0474(2) 0.2711(2) 0.0445(14) Uani 1 1 d . . . C47 C 0.6680(3) -0.0357(2) 0.1905(2) 0.0461(15) Uani 1 1 d . . . H47 H 0.6445 -0.0048 0.1828 0.055 Uiso 1 1 calc R . . C48 C 0.6543(3) -0.0649(2) 0.2355(2) 0.0470(15) Uani 1 1 d . . . C49 C 0.6882(3) -0.1111(3) 0.2444(2) 0.0535(16) Uani 1 1 d . . . H49 H 0.6798 -0.1326 0.2748 0.064 Uiso 1 1 calc R . . C50 C 0.7339(3) -0.1261(2) 0.2099(2) 0.0483(15) Uani 1 1 d . . . H50 H 0.7567 -0.1578 0.2159 0.058 Uiso 1 1 calc R . . C51 C 0.7457(3) -0.0938(2) 0.1660(2) 0.0424(14) Uani 1 1 d . . . C52 C 0.7940(3) -0.1038(2) 0.1266(2) 0.0367(13) Uani 1 1 d . . . C53 C 0.8288(3) -0.1500(2) 0.1235(2) 0.0463(15) Uani 1 1 d . . . H531 H 0.8235 -0.1781 0.1486 0.056 Uiso 1 1 calc R . . C54 C 0.8711(3) -0.1545(2) 0.0834(2) 0.0488(15) Uani 1 1 d . . . H54 H 0.8948 -0.1861 0.0807 0.059 Uiso 1 1 calc R . . C55 C 0.8796(2) -0.1139(2) 0.0472(2) 0.0383(13) Uani 1 1 d . . . H55 H 0.9089 -0.1171 0.0196 0.046 Uiso 1 1 calc R . . C56 C 0.8443(2) -0.0682(2) 0.0521(2) 0.0325(12) Uani 1 1 d . . . C57 C 0.8477(2) -0.02099(19) 0.0159(2) 0.0296(11) Uani 1 1 d . . . C58 C 0.8831(2) -0.0191(2) -0.0298(2) 0.0349(12) Uani 1 1 d . . . H58 H 0.9078 -0.0487 -0.0397 0.042 Uiso 1 1 calc R . . C59 C 0.8816(2) 0.0267(2) -0.0605(2) 0.0336(12) Uani 1 1 d . B . H59 H 0.9047 0.0280 -0.0925 0.040 Uiso 1 1 calc R . . C60 C 0.8474(2) 0.07055(18) -0.04604(19) 0.0297(11) Uani 1 1 d D . . C61 C 0.8134(2) 0.06526(19) 0.00110(19) 0.0311(11) Uani 1 1 d . B . H61 H 0.7898 0.0949 0.0125 0.037 Uiso 1 1 calc R . . C71 C 0.6572(3) 0.0413(3) 0.2873(3) 0.066(2) Uani 1 1 d . . . H711 H 0.6951 0.0209 0.2841 0.100 Uiso 1 1 calc R . . H712 H 0.6598 0.0653 0.3181 0.100 Uiso 1 1 calc R . . H713 H 0.6508 0.0624 0.2549 0.100 Uiso 1 1 calc R . . C72 C 0.6050(3) 0.0034(3) 0.2947(2) 0.0446(14) Uani 1 1 d . . . C73 C 0.5575(3) 0.0200(2) 0.3268(2) 0.0416(13) Uani 1 1 d . . . H73 H 0.5594 0.0542 0.3433 0.050 Uiso 1 1 calc R . . P1 P 0.05814(6) 0.19906(5) 0.08943(6) 0.0574(5) Uani 1 1 d D . . F1A F 0.0389(3) 0.25942(11) 0.0989(3) 0.070(4) Uani 0.570(17) 1 d PDU C 1 F2A F 0.0775(3) 0.13868(11) 0.0800(3) 0.070(4) Uani 0.570(17) 1 d PDU C 1 F3A F 0.0037(3) 0.1920(3) 0.0488(3) 0.072(2) Uani 0.570(17) 1 d PDU C 1 F4A F 0.1127(3) 0.2061(3) 0.1301(3) 0.072(2) Uani 0.570(17) 1 d PDU C 1 F5A F 0.0153(3) 0.1809(2) 0.1368(2) 0.073(2) Uani 0.570(17) 1 d PDU C 1 F6A F 0.1012(3) 0.2172(2) 0.0421(2) 0.073(2) Uani 0.570(17) 1 d PDU C 1 F1B F 0.0428(4) 0.25908(14) 0.1049(4) 0.083(6) Uani 0.430(17) 1 d PDU C 2 F2B F 0.0734(4) 0.13904(14) 0.0740(4) 0.083(6) Uani 0.430(17) 1 d PDU C 2 F3B F -0.01017(19) 0.1903(4) 0.0714(5) 0.085(3) Uani 0.430(17) 1 d PDU C 2 F4B F 0.12636(19) 0.2079(4) 0.1075(5) 0.085(3) Uani 0.430(17) 1 d PDU C 2 F5B F 0.0410(6) 0.1805(4) 0.14789(19) 0.093(4) Uani 0.430(17) 1 d PDU C 2 F6B F 0.0751(6) 0.2176(4) 0.0309(2) 0.093(4) Uani 0.430(17) 1 d PDU C 2 P2A P 0.56810(13) 0.31687(11) 0.10289(12) 0.0660(13) Uani 0.663(7) 1 d PD D 1 F7A F 0.5390(2) 0.25912(14) 0.1084(2) 0.092(2) Uani 0.663(7) 1 d PDU D 1 F8A F 0.5972(2) 0.37462(14) 0.0974(2) 0.092(2) Uani 0.663(7) 1 d PDU D 1 F9A F 0.50671(17) 0.33851(19) 0.0779(2) 0.107(2) Uani 0.663(7) 1 d PDU D 1 F10A F 0.62949(19) 0.2952(2) 0.1279(2) 0.107(2) Uani 0.663(7) 1 d PDU D 1 F11A F 0.5443(2) 0.3317(2) 0.16061(16) 0.103(2) Uani 0.663(7) 1 d PDU D 1 F12A F 0.5919(2) 0.3020(2) 0.04518(15) 0.103(2) Uani 0.663(7) 1 d PDU D 1 P2B P 0.5794(3) 0.3066(2) 0.1237(3) 0.093(4) Uani 0.337(7) 1 d PD D 2 F7B F 0.5645(5) 0.2558(3) 0.1592(5) 0.154(6) Uani 0.337(7) 1 d PDU D 2 F8B F 0.5944(5) 0.3574(4) 0.0883(5) 0.154(6) Uani 0.337(7) 1 d PDU D 2 F9B F 0.5134(3) 0.3294(4) 0.1347(5) 0.121(5) Uani 0.337(7) 1 d PDU D 2 F10B F 0.6455(3) 0.2839(4) 0.1128(5) 0.121(5) Uani 0.337(7) 1 d PDU D 2 F11B F 0.6039(6) 0.3370(4) 0.1748(4) 0.160(7) Uani 0.337(7) 1 d PDU D 2 F12B F 0.5549(6) 0.2762(5) 0.0727(4) 0.160(7) Uani 0.337(7) 1 d PDU D 2 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 0.0353(5) 0.0333(5) 0.0270(5) 0.000 0.000 -0.0013(4) O1 0.039(2) 0.048(2) 0.062(3) 0.011(2) -0.017(2) -0.0069(19) O2A 0.073(6) 0.052(4) 0.060(4) -0.013(4) -0.002(5) -0.002(5) C22A 0.043(5) 0.056(4) 0.036(4) -0.003(4) 0.004(4) -0.002(4) C23A 0.048(5) 0.053(5) 0.040(4) -0.008(4) 0.008(4) -0.005(4) C24A 0.050(6) 0.054(8) 0.048(6) -0.012(7) 0.012(6) -0.001(6) C25A 0.050(6) 0.052(5) 0.044(5) -0.011(5) 0.009(5) -0.008(5) C26A 0.054(5) 0.050(4) 0.047(4) -0.011(4) 0.009(5) -0.005(4) C27A 0.083(7) 0.058(6) 0.067(6) -0.013(5) 0.007(6) 0.000(6) C28A 0.040(5) 0.051(5) 0.041(4) -0.005(4) 0.008(5) -0.003(5) C29A 0.039(5) 0.052(5) 0.038(4) -0.002(4) 0.004(4) -0.002(4) C30A 0.040(5) 0.049(7) 0.051(5) -0.005(6) 0.011(5) 0.000(6) O2B 0.069(5) 0.058(4) 0.066(4) -0.017(3) 0.009(4) -0.003(4) C22B 0.041(4) 0.057(4) 0.034(4) -0.001(3) 0.002(4) -0.005(4) C23B 0.047(4) 0.057(4) 0.037(3) -0.011(3) 0.008(4) -0.006(4) C24B 0.054(5) 0.056(6) 0.048(4) -0.018(5) 0.010(4) -0.003(5) C25B 0.047(5) 0.051(4) 0.047(4) -0.009(4) 0.013(4) -0.009(4) C26B 0.051(5) 0.051(4) 0.043(3) -0.009(3) 0.011(4) -0.006(4) C27B 0.081(6) 0.056(5) 0.070(5) -0.010(4) 0.006(5) -0.008(5) C28B 0.037(5) 0.054(4) 0.040(4) -0.001(4) 0.005(4) -0.001(4) C29B 0.037(4) 0.053(4) 0.039(3) -0.005(4) 0.004(3) 0.001(3) C30B 0.040(5) 0.060(6) 0.061(5) -0.014(5) 0.011(4) -0.003(5) N1 0.062(3) 0.028(2) 0.028(2) 0.0007(19) -0.006(2) 0.004(2) N2 0.034(2) 0.032(2) 0.029(2) 0.0052(19) -0.0016(19) 0.0011(19) N3 0.026(2) 0.034(2) 0.031(2) 0.0025(19) 0.0004(18) 0.0016(18) C1 0.051(4) 0.052(4) 0.062(4) 0.010(3) -0.022(3) -0.007(3) C2 0.042(3) 0.040(3) 0.041(3) 0.004(3) 0.003(3) 0.002(3) C3 0.042(3) 0.036(3) 0.052(4) -0.003(3) 0.001(3) -0.008(3) C4 0.040(3) 0.035(3) 0.050(3) 0.006(3) 0.004(3) -0.002(3) C5 0.063(4) 0.037(3) 0.069(4) 0.017(3) 0.009(3) 0.000(3) C6 0.042(3) 0.042(3) 0.032(3) 0.003(2) 0.003(2) 0.003(3) C7 0.059(4) 0.026(3) 0.034(3) 0.001(2) 0.004(3) 0.011(3) C8 0.040(3) 0.022(3) 0.034(3) 0.001(2) 0.006(2) 0.000(2) C9 0.044(3) 0.039(3) 0.035(3) -0.008(2) -0.007(3) 0.002(3) C10 0.050(3) 0.026(3) 0.042(3) -0.008(2) -0.003(3) 0.007(2) C11 0.045(3) 0.021(2) 0.033(3) -0.002(2) 0.002(2) 0.001(2) C12 0.048(3) 0.027(3) 0.043(3) 0.003(2) -0.010(3) 0.000(2) C13 0.089(5) 0.032(3) 0.079(5) -0.019(3) -0.032(4) 0.020(3) C14 0.091(6) 0.036(4) 0.103(6) -0.008(4) -0.035(5) 0.018(4) C15 0.068(4) 0.038(3) 0.068(4) 0.004(3) -0.032(4) 0.013(3) C16 0.039(3) 0.035(3) 0.040(3) 0.007(2) 0.000(3) 0.003(2) C17 0.028(3) 0.038(3) 0.032(3) 0.009(2) -0.001(2) 0.000(2) C18 0.032(3) 0.043(3) 0.041(3) 0.007(3) -0.002(2) 0.009(2) C19 0.035(3) 0.067(4) 0.035(3) 0.002(3) -0.007(2) 0.004(3) C20 0.025(3) 0.057(4) 0.034(3) 0.000(3) 0.001(2) -0.002(3) C21 0.047(3) 0.035(3) 0.030(3) 0.001(2) 0.005(2) 0.006(3) C31 0.046(3) 0.041(3) 0.053(4) 0.014(3) -0.015(3) -0.010(3) C32 0.041(3) 0.037(3) 0.035(3) 0.003(2) 0.003(2) 0.003(2) C33 0.040(3) 0.035(3) 0.035(3) 0.006(2) 0.000(2) 0.002(2) Cu2 0.0477(6) 0.0297(5) 0.0274(5) 0.000 0.000 0.0003(4) O41 0.045(3) 0.064(3) 0.070(3) -0.011(2) 0.015(2) -0.006(2) O42A 0.056(4) 0.048(4) 0.066(5) 0.020(4) 0.002(5) 0.002(4) C67A 0.059(5) 0.052(6) 0.067(6) 0.024(5) 0.003(6) 0.002(5) C62A 0.035(4) 0.032(4) 0.037(4) -0.001(4) 0.000(4) 0.004(4) C63A 0.033(4) 0.036(4) 0.046(4) 0.002(3) -0.001(3) 0.002(3) C64A 0.036(5) 0.038(5) 0.052(5) 0.006(5) -0.005(5) -0.002(5) C65A 0.042(4) 0.040(4) 0.056(4) 0.009(4) 0.000(4) 0.000(4) C66A 0.049(4) 0.043(4) 0.055(4) 0.011(4) 0.000(4) 0.004(3) C68A 0.041(4) 0.039(4) 0.046(4) 0.004(4) -0.002(4) 0.006(4) C69A 0.035(4) 0.034(4) 0.037(4) -0.001(3) 0.000(3) 0.005(3) C70A 0.037(5) 0.034(5) 0.036(6) -0.006(5) -0.004(5) 0.003(5) O42B 0.056(3) 0.047(4) 0.057(4) 0.015(3) 0.009(3) 0.007(3) C67B 0.061(5) 0.058(5) 0.073(6) 0.024(5) 0.007(5) 0.002(4) C62B 0.035(3) 0.031(3) 0.036(3) -0.001(3) 0.001(3) 0.004(3) C63B 0.031(3) 0.036(3) 0.045(3) 0.002(3) 0.000(3) 0.002(3) C64B 0.036(4) 0.038(4) 0.054(4) 0.006(4) -0.007(4) -0.002(4) C65B 0.043(4) 0.040(3) 0.058(4) 0.010(3) 0.000(3) -0.001(3) C66B 0.051(3) 0.043(3) 0.055(3) 0.011(3) -0.001(3) 0.004(3) C68B 0.040(3) 0.039(3) 0.046(3) 0.003(3) -0.003(3) 0.006(3) C69B 0.034(3) 0.033(3) 0.035(3) -0.001(3) 0.001(3) 0.005(3) C70B 0.033(4) 0.034(4) 0.042(5) -0.006(4) -0.004(4) 0.006(4) N41 0.057(3) 0.033(2) 0.030(2) 0.000(2) 0.006(2) 0.007(2) N42 0.042(3) 0.028(2) 0.031(2) 0.0008(19) -0.007(2) -0.0012(19) N43 0.029(2) 0.034(2) 0.029(2) -0.0021(19) -0.0014(18) 0.0033(19) C41 0.053(4) 0.064(4) 0.058(4) -0.008(3) 0.011(3) -0.007(3) C42 0.042(3) 0.053(4) 0.036(3) -0.003(3) 0.003(3) 0.001(3) C43 0.050(4) 0.055(4) 0.061(4) -0.004(3) -0.002(3) -0.015(3) C44 0.068(4) 0.049(4) 0.041(3) -0.007(3) 0.000(3) -0.007(3) C45 0.087(5) 0.060(4) 0.071(5) -0.013(4) 0.003(4) -0.022(4) C46 0.054(4) 0.050(4) 0.029(3) -0.008(3) 0.005(3) 0.000(3) C47 0.066(4) 0.036(3) 0.036(3) -0.007(3) -0.003(3) 0.012(3) C48 0.071(4) 0.041(3) 0.029(3) -0.004(3) 0.003(3) 0.001(3) C49 0.078(5) 0.048(4) 0.035(3) 0.006(3) 0.012(3) -0.004(3) C50 0.064(4) 0.041(3) 0.041(3) 0.011(3) 0.006(3) 0.012(3) C51 0.059(4) 0.032(3) 0.036(3) 0.003(2) -0.005(3) 0.004(3) C52 0.045(3) 0.034(3) 0.031(3) 0.004(2) -0.008(2) -0.002(2) C53 0.058(4) 0.035(3) 0.046(3) 0.012(3) -0.004(3) 0.007(3) C54 0.051(4) 0.038(3) 0.057(4) 0.009(3) -0.001(3) 0.011(3) C55 0.033(3) 0.033(3) 0.049(3) 0.001(3) 0.002(3) 0.007(2) C56 0.033(3) 0.030(3) 0.034(3) 0.004(2) -0.001(2) -0.002(2) C57 0.027(3) 0.028(2) 0.034(3) -0.005(2) -0.008(2) -0.005(2) C58 0.033(3) 0.029(3) 0.043(3) -0.002(2) 0.007(2) 0.006(2) C59 0.035(3) 0.032(3) 0.034(3) -0.003(2) 0.008(2) 0.000(2) C60 0.027(3) 0.028(3) 0.034(3) -0.002(2) -0.004(2) 0.000(2) C61 0.038(3) 0.027(3) 0.028(3) -0.002(2) -0.005(2) -0.001(2) C71 0.060(4) 0.078(5) 0.061(4) -0.031(4) 0.016(4) -0.025(4) C72 0.045(3) 0.057(4) 0.032(3) 0.000(3) 0.004(3) -0.007(3) C73 0.044(3) 0.049(3) 0.032(3) -0.003(3) 0.000(3) -0.001(3) P1 0.0617(11) 0.0330(8) 0.0774(13) -0.0028(8) 0.0129(10) -0.0086(8) F1A 0.075(6) 0.031(5) 0.104(6) -0.008(3) 0.015(4) -0.005(3) F2A 0.075(6) 0.031(5) 0.104(6) -0.008(3) 0.015(4) -0.005(3) F3A 0.080(4) 0.060(3) 0.076(4) -0.003(3) -0.013(3) -0.007(3) F4A 0.080(4) 0.060(3) 0.076(4) -0.003(3) -0.013(3) -0.007(3) F5A 0.085(4) 0.053(3) 0.083(4) 0.001(3) 0.031(3) -0.015(3) F6A 0.085(4) 0.053(3) 0.083(4) 0.001(3) 0.031(3) -0.015(3) F1B 0.084(8) 0.058(8) 0.108(8) -0.008(5) 0.013(5) 0.000(5) F2B 0.084(8) 0.058(8) 0.108(8) -0.008(5) 0.013(5) 0.000(5) F3B 0.072(5) 0.068(5) 0.116(6) -0.015(5) 0.018(4) -0.001(4) F4B 0.072(5) 0.068(5) 0.116(6) -0.015(5) 0.018(4) -0.001(4) F5B 0.091(6) 0.088(5) 0.100(5) 0.011(4) 0.020(4) 0.014(4) F6B 0.091(6) 0.088(5) 0.100(5) 0.011(4) 0.020(4) 0.014(4) P2A 0.063(2) 0.0401(19) 0.095(3) -0.0047(18) 0.028(2) 0.0044(16) F7A 0.086(3) 0.055(3) 0.135(4) -0.017(3) 0.031(3) -0.008(2) F8A 0.086(3) 0.055(3) 0.135(4) -0.017(3) 0.031(3) -0.008(2) F9A 0.097(4) 0.105(4) 0.120(4) -0.014(3) -0.006(3) 0.022(3) F10A 0.097(4) 0.105(4) 0.120(4) -0.014(3) -0.006(3) 0.022(3) F11A 0.115(4) 0.107(4) 0.087(3) -0.022(3) 0.030(3) 0.012(3) F12A 0.115(4) 0.107(4) 0.087(3) -0.022(3) 0.030(3) 0.012(3) P2B 0.054(5) 0.032(4) 0.192(11) -0.045(5) 0.023(6) 0.006(3) F7B 0.161(8) 0.132(8) 0.169(8) 0.015(6) 0.020(6) -0.010(6) F8B 0.161(8) 0.132(8) 0.169(8) 0.015(6) 0.020(6) -0.010(6) F9B 0.114(7) 0.106(7) 0.143(7) -0.006(5) 0.026(5) 0.009(5) F10B 0.114(7) 0.106(7) 0.143(7) -0.006(5) 0.026(5) 0.009(5) F11B 0.170(9) 0.149(8) 0.161(8) -0.019(6) -0.016(6) 0.005(6) F12B 0.170(9) 0.149(8) 0.161(8) -0.019(6) -0.016(6) 0.005(6) _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 N2 1.964(4) . ? Cu1 N3 2.167(4) . ? Cu1 N1 2.177(4) . ? O1 C2 1.375(7) . ? O1 C1 1.425(7) . ? O2A C26A 1.383(10) . ? O2A C27A 1.406(13) . ? C22A C23A 1.402(11) . ? C22A C29A 1.411(10) . ? C22A C20 1.473(8) . ? C23A C25A 1.355(11) . ? C23A C24A 1.522(11) . ? C24A H241 0.9800 . ? C24A H242 0.9800 . ? C24A H243 0.9800 . ? C25A C26A 1.402(12) . ? C25A H251 0.9500 . ? C26A C28A 1.350(12) . ? C27A H271 0.9800 . ? C27A H272 0.9800 . ? C27A H273 0.9800 . ? C28A C29A 1.374(11) . ? C28A H281 0.9500 . ? C29A C30A 1.516(11) . ? C30A H301 0.9800 . ? C30A H302 0.9800 . ? C30A H303 0.9800 . ? O2B C26B 1.385(9) . ? O2B C27B 1.411(11) . ? C22B C23B 1.405(10) . ? C22B C29B 1.412(9) . ? C22B C20 1.481(7) . ? C23B C25B 1.358(10) . ? C23B C24B 1.521(10) . ? C24B H244 0.9800 . ? C24B H245 0.9800 . ? C24B H246 0.9800 . ? C25B C26B 1.396(12) . ? C25B H252 0.9500 . ? C26B C28B 1.352(11) . ? C27B H274 0.9800 . ? C27B H275 0.9800 . ? C27B H276 0.9800 . ? C28B C29B 1.371(10) . ? C28B H282 0.9500 . ? C29B C30B 1.516(10) . ? C30B H304 0.9800 . ? C30B H305 0.9800 . ? C30B H306 0.9800 . ? N1 C7 1.336(7) . ? N1 C11 1.351(7) . ? N2 C16 1.341(7) . ? N2 C12 1.352(7) . ? N3 C21 1.327(7) . ? N3 C17 1.344(6) . ? C1 H11 0.9800 . ? C1 H12 0.9800 . ? C1 H13 0.9800 . ? C2 C3 1.370(8) . ? C2 C33 1.382(8) . ? C3 C4 1.386(8) . ? C3 H3 0.9500 . ? C4 C6 1.414(8) . ? C4 C5 1.514(8) . ? C5 H51 0.9800 . ? C5 H52 0.9800 . ? C5 H53 0.9800 . ? C6 C32 1.404(7) . ? C6 C8 1.476(8) . ? C7 C8 1.400(7) . ? C7 H7 0.9500 . ? C8 C9 1.395(7) . ? C9 C10 1.386(7) . ? C9 H9 0.9500 . ? C10 C11 1.380(7) . ? C10 H10 0.9500 . ? C11 C12 1.481(8) . ? C12 C13 1.366(8) . ? C13 C14 1.383(10) . ? C13 H131 0.9500 . ? C14 C15 1.371(9) . ? C14 H14 0.9500 . ? C15 C16 1.353(8) . ? C15 H15 0.9500 . ? C16 C17 1.501(8) . ? C17 C18 1.390(7) . ? C18 C19 1.372(8) . ? C18 H18 0.9500 . ? C19 C20 1.385(8) . ? C19 H19 0.9500 . ? C20 C21 1.407(7) . ? C21 H21 0.9500 . ? C31 C32 1.514(8) . ? C31 H311 0.9800 . ? C31 H312 0.9800 . ? C31 H313 0.9800 . ? C32 C33 1.403(8) . ? C33 H33 0.9500 . ? Cu2 N42 1.975(4) . ? Cu2 N43 2.159(4) . ? Cu2 N41 2.161(4) . ? O41 C42 1.364(7) . ? O41 C41 1.438(8) . ? O42A C66A 1.383(9) . ? O42A C67A 1.421(11) . ? C67A H671 0.9800 . ? C67A H672 0.9800 . ? C67A H673 0.9800 . ? C62A C63A 1.396(9) . ? C62A C69A 1.412(9) . ? C62A C60 1.484(8) . ? C63A C65A 1.387(9) . ? C63A C64A 1.521(9) . ? C64A H641 0.9800 . ? C64A H642 0.9800 . ? C64A H643 0.9800 . ? C65A C66A 1.382(10) . ? C65A H651 0.9500 . ? C66A C68A 1.376(10) . ? C68A C69A 1.388(9) . ? C68A H681 0.9500 . ? C69A C70A 1.514(9) . ? C70A H701 0.9800 . ? C70A H702 0.9800 . ? C70A H703 0.9800 . ? O42B C66B 1.381(8) . ? O42B C67B 1.425(10) . ? C67B H674 0.9800 . ? C67B H675 0.9800 . ? C67B H676 0.9800 . ? C62B C63B 1.395(8) . ? C62B C69B 1.411(8) . ? C62B C60 1.483(7) . ? C63B C65B 1.388(8) . ? C63B C64B 1.521(8) . ? C64B H644 0.9800 . ? C64B H645 0.9800 . ? C64B H646 0.9800 . ? C65B C66B 1.382(9) . ? C65B H652 0.9500 . ? C66B C68B 1.372(9) . ? C68B C69B 1.390(8) . ? C68B H682 0.9500 . ? C69B C70B 1.511(9) . ? C70B H704 0.9800 . ? C70B H705 0.9800 . ? C70B H706 0.9800 . ? N41 C47 1.346(7) . ? N41 C51 1.347(7) . ? N42 C56 1.343(7) . ? N42 C52 1.350(7) . ? N43 C61 1.340(6) . ? N43 C57 1.350(6) . ? C41 H411 0.9800 . ? C41 H412 0.9800 . ? C41 H413 0.9800 . ? C42 C43 1.382(9) . ? C42 C73 1.383(8) . ? C43 C44 1.397(9) . ? C43 H43 0.9500 . ? C44 C46 1.389(9) . ? C44 C45 1.506(9) . ? C45 H451 0.9800 . ? C45 H452 0.9800 . ? C45 H453 0.9800 . ? C46 C72 1.401(8) . ? C46 C48 1.507(8) . ? C47 C48 1.380(8) . ? C47 H47 0.9500 . ? C48 C49 1.392(9) . ? C49 C50 1.380(8) . ? C49 H49 0.9500 . ? C50 C51 1.390(8) . ? C50 H50 0.9500 . ? C51 C52 1.473(8) . ? C52 C53 1.387(8) . ? C53 C54 1.375(9) . ? C53 H531 0.9500 . ? C54 C55 1.373(8) . ? C54 H54 0.9500 . ? C55 C56 1.387(7) . ? C55 H55 0.9500 . ? C56 C57 1.491(7) . ? C57 C58 1.387(7) . ? C58 C59 1.381(7) . ? C58 H58 0.9500 . ? C59 C60 1.378(7) . ? C59 H59 0.9500 . ? C60 C61 1.406(7) . ? C61 H61 0.9500 . ? C71 C72 1.499(8) . ? C71 H711 0.9800 . ? C71 H712 0.9800 . ? C71 H713 0.9800 . ? C72 C73 1.384(8) . ? C73 H73 0.9500 . ? P1 F3A 1.5833(16) . ? P1 F4B 1.5834(16) . ? P1 F1A 1.5842(16) . ? P1 F2B 1.5844(16) . ? P1 F5A 1.5845(16) . ? P1 F6A 1.5845(16) . ? P1 F5B 1.5845(16) . ? P1 F6B 1.5845(16) . ? P1 F1B 1.5847(16) . ? P1 F2A 1.5849(16) . ? P1 F3B 1.5856(16) . ? P1 F4A 1.5858(16) . ? P2A F12A 1.5844(16) . ? P2A F10A 1.5845(16) . ? P2A F7A 1.5845(16) . ? P2A F9A 1.5845(16) . ? P2A F8A 1.5845(16) . ? P2A F11A 1.5847(16) . ? P2B F10B 1.5844(16) . ? P2B F7B 1.5845(16) . ? P2B F9B 1.5845(16) . ? P2B F11B 1.5845(16) . ? P2B F12B 1.5845(16) . ? P2B F8B 1.5846(16) . ? 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 N2 Cu1 N2 178.6(2) 2 . ? N2 Cu1 N3 77.77(16) . . ? N2 Cu1 N3 103.26(16) . 2 ? N3 Cu1 N3 85.3(2) . 2 ? N2 Cu1 N1 100.38(17) . 2 ? N3 Cu1 N1 97.14(17) . 2 ? N2 Cu1 N1 78.63(17) . . ? N3 Cu1 N1 156.19(16) . . ? N1 Cu1 N1 90.1(2) 2 . ? C2 O1 C1 117.2(4) . . ? C26A O2A C27A 120.4(9) . . ? C23A C22A C29A 118.3(7) . . ? C23A C22A C20 119.7(12) . . ? C29A C22A C20 122.0(11) . . ? C25A C23A C22A 120.5(8) . . ? C25A C23A C24A 118.7(8) . . ? C22A C23A C24A 120.7(8) . . ? C23A C25A C26A 120.1(9) . . ? C23A C25A H251 120.0 . . ? C26A C25A H251 120.0 . . ? C28A C26A O2A 118.8(9) . . ? C28A C26A C25A 120.5(8) . . ? O2A C26A C25A 120.4(9) . . ? C26A C28A C29A 120.5(9) . . ? C26A C28A H281 119.8 . . ? C29A C28A H281 119.8 . . ? C28A C29A C22A 120.2(8) . . ? C28A C29A C30A 118.4(8) . . ? C22A C29A C30A 121.4(8) . . ? C26B O2B C27B 119.5(7) . . ? C23B C22B C29B 117.7(6) . . ? C23B C22B C20 121.9(8) . . ? C29B C22B C20 120.3(8) . . ? C25B C23B C22B 120.8(7) . . ? C25B C23B C24B 118.7(7) . . ? C22B C23B C24B 120.5(6) . . ? C23B C24B H244 109.5 . . ? C23B C24B H245 109.5 . . ? H244 C24B H245 109.5 . . ? C23B C24B H246 109.5 . . ? H244 C24B H246 109.5 . . ? H245 C24B H246 109.5 . . ? C23B C25B C26B 120.1(8) . . ? C23B C25B H252 120.0 . . ? C26B C25B H252 120.0 . . ? C28B C26B O2B 117.4(8) . . ? C28B C26B C25B 120.2(7) . . ? O2B C26B C25B 122.4(7) . . ? O2B C27B H274 109.5 . . ? O2B C27B H275 109.5 . . ? H274 C27B H275 109.5 . . ? O2B C27B H276 109.5 . . ? H274 C27B H276 109.5 . . ? H275 C27B H276 109.5 . . ? C26B C28B C29B 120.9(7) . . ? C26B C28B H282 119.6 . . ? C29B C28B H282 119.6 . . ? C28B C29B C22B 120.3(7) . . ? C28B C29B C30B 117.8(7) . . ? C22B C29B C30B 121.9(7) . . ? C29B C30B H304 109.5 . . ? C29B C30B H305 109.5 . . ? H304 C30B H305 109.5 . . ? C29B C30B H306 109.5 . . ? H304 C30B H306 109.5 . . ? H305 C30B H306 109.5 . . ? C7 N1 C11 118.8(5) . . ? C7 N1 Cu1 129.0(4) . . ? C11 N1 Cu1 111.3(4) . . ? C16 N2 C12 120.6(5) . . ? C16 N2 Cu1 120.7(4) . . ? C12 N2 Cu1 118.6(3) . . ? C21 N3 C17 119.0(4) . . ? C21 N3 Cu1 127.1(4) . . ? C17 N3 Cu1 112.7(3) . . ? O1 C1 H11 109.5 . . ? O1 C1 H12 109.5 . . ? H11 C1 H12 109.5 . . ? O1 C1 H13 109.5 . . ? H11 C1 H13 109.5 . . ? H12 C1 H13 109.5 . . ? C3 C2 O1 116.0(5) . . ? C3 C2 C33 120.3(5) . . ? O1 C2 C33 123.7(5) . . ? C2 C3 C4 121.2(5) . . ? C2 C3 H3 119.4 . . ? C4 C3 H3 119.4 . . ? C3 C4 C6 119.6(5) . . ? C3 C4 C5 119.0(5) . . ? C6 C4 C5 121.4(5) . . ? C4 C5 H51 109.5 . . ? C4 C5 H52 109.5 . . ? H51 C5 H52 109.5 . . ? C4 C5 H53 109.5 . . ? H51 C5 H53 109.5 . . ? H52 C5 H53 109.5 . . ? C32 C6 C4 119.0(5) . . ? C32 C6 C8 120.4(5) . . ? C4 C6 C8 120.7(5) . . ? N1 C7 C8 124.0(5) . . ? N1 C7 H7 118.0 . . ? C8 C7 H7 118.0 . . ? C9 C8 C7 116.0(5) . . ? C9 C8 C6 121.8(5) . . ? C7 C8 C6 122.1(5) . . ? C10 C9 C8 120.3(5) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C11 C10 C9 119.6(5) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? N1 C11 C10 121.1(5) . . ? N1 C11 C12 114.4(5) . . ? C10 C11 C12 124.6(5) . . ? N2 C12 C13 120.7(5) . . ? N2 C12 C11 115.3(5) . . ? C13 C12 C11 124.0(5) . . ? C12 C13 C14 118.1(6) . . ? C12 C13 H131 121.0 . . ? C14 C13 H131 121.0 . . ? C15 C14 C13 120.6(6) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C16 C15 C14 119.1(6) . . ? C16 C15 H15 120.5 . . ? C14 C15 H15 120.5 . . ? N2 C16 C15 120.9(5) . . ? N2 C16 C17 113.4(4) . . ? C15 C16 C17 125.6(5) . . ? N3 C17 C18 121.6(5) . . ? N3 C17 C16 114.7(4) . . ? C18 C17 C16 123.7(5) . . ? C19 C18 C17 118.7(5) . . ? C19 C18 H18 120.6 . . ? C17 C18 H18 120.6 . . ? C18 C19 C20 121.0(5) . . ? C18 C19 H19 119.5 . . ? C20 C19 H19 119.5 . . ? C19 C20 C21 116.2(5) . . ? C19 C20 C22A 123(3) . . ? C21 C20 C22A 121(3) . . ? C19 C20 C22B 124.6(18) . . ? C21 C20 C22B 119.1(18) . . ? N3 C21 C20 123.5(5) . . ? N3 C21 H21 118.3 . . ? C20 C21 H21 118.3 . . ? C32 C31 H311 109.5 . . ? C32 C31 H312 109.5 . . ? H311 C31 H312 109.5 . . ? C32 C31 H313 109.5 . . ? H311 C31 H313 109.5 . . ? H312 C31 H313 109.5 . . ? C33 C32 C6 119.7(5) . . ? C33 C32 C31 116.9(5) . . ? C6 C32 C31 123.4(5) . . ? C2 C33 C32 120.1(5) . . ? C2 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? N42 Cu2 N42 176.2(2) 2_655 . ? N42 Cu2 N43 78.13(16) . . ? N42 Cu2 N43 99.07(16) . 2_655 ? N43 Cu2 N43 85.9(2) . 2_655 ? N42 Cu2 N41 77.67(17) . . ? N43 Cu2 N41 155.76(16) . . ? N42 Cu2 N41 105.16(17) . 2_655 ? N43 Cu2 N41 99.22(17) . 2_655 ? N41 Cu2 N41 85.8(2) . 2_655 ? C42 O41 C41 116.7(5) . . ? C66A O42A C67A 117.9(9) . . ? C63A C62A C69A 119.2(6) . . ? C63A C62A C60 119.4(14) . . ? C69A C62A C60 121.3(14) . . ? C65A C63A C62A 119.7(6) . . ? C65A C63A C64A 117.4(7) . . ? C62A C63A C64A 122.9(7) . . ? C66A C65A C63A 121.4(7) . . ? C66A C65A H651 119.3 . . ? C63A C65A H651 119.3 . . ? C68A C66A C65A 118.9(7) . . ? C68A C66A O42A 115.5(7) . . ? C65A C66A O42A 123.8(7) . . ? C66A C68A C69A 121.7(7) . . ? C66A C68A H681 119.2 . . ? C69A C68A H681 119.2 . . ? C68A C69A C62A 119.1(6) . . ? C68A C69A C70A 118.1(7) . . ? C62A C69A C70A 122.0(7) . . ? C66B O42B C67B 117.1(7) . . ? O42B C67B H674 109.5 . . ? O42B C67B H675 109.5 . . ? H674 C67B H675 109.5 . . ? O42B C67B H676 109.5 . . ? H674 C67B H676 109.5 . . ? H675 C67B H676 109.5 . . ? C63B C62B C69B 119.4(5) . . ? C63B C62B C60 120.6(9) . . ? C69B C62B C60 120.0(9) . . ? C65B C63B C62B 119.6(6) . . ? C65B C63B C64B 117.4(6) . . ? C62B C63B C64B 122.9(6) . . ? C63B C64B H644 109.5 . . ? C63B C64B H645 109.5 . . ? H644 C64B H645 109.5 . . ? C63B C64B H646 109.5 . . ? H644 C64B H646 109.5 . . ? H645 C64B H646 109.5 . . ? C66B C65B C63B 121.2(6) . . ? C66B C65B H652 119.4 . . ? C63B C65B H652 119.4 . . ? C68B C66B O42B 116.1(6) . . ? C68B C66B C65B 119.3(6) . . ? O42B C66B C65B 124.0(6) . . ? C66B C68B C69B 121.4(6) . . ? C66B C68B H682 119.3 . . ? C69B C68B H682 119.3 . . ? C68B C69B C62B 119.1(5) . . ? C68B C69B C70B 118.2(6) . . ? C62B C69B C70B 122.4(6) . . ? C69B C70B H704 109.5 . . ? C69B C70B H705 109.5 . . ? H704 C70B H705 109.5 . . ? C69B C70B H706 109.5 . . ? H704 C70B H706 109.5 . . ? H705 C70B H706 109.5 . . ? C47 N41 C51 119.4(5) . . ? C47 N41 Cu2 126.6(4) . . ? C51 N41 Cu2 113.3(4) . . ? C56 N42 C52 121.2(5) . . ? C56 N42 Cu2 119.2(3) . . ? C52 N42 Cu2 119.4(4) . . ? C61 N43 C57 118.6(4) . . ? C61 N43 Cu2 128.0(3) . . ? C57 N43 Cu2 112.5(3) . . ? O41 C41 H411 109.5 . . ? O41 C41 H412 109.5 . . ? H411 C41 H412 109.5 . . ? O41 C41 H413 109.5 . . ? H411 C41 H413 109.5 . . ? H412 C41 H413 109.5 . . ? O41 C42 C43 115.7(6) . . ? O41 C42 C73 125.3(5) . . ? C43 C42 C73 118.9(6) . . ? C42 C43 C44 121.1(6) . . ? C42 C43 H43 119.4 . . ? C44 C43 H43 119.4 . . ? C46 C44 C43 119.3(6) . . ? C46 C44 C45 123.2(6) . . ? C43 C44 C45 117.5(6) . . ? C44 C45 H451 109.5 . . ? C44 C45 H452 109.5 . . ? H451 C45 H452 109.5 . . ? C44 C45 H453 109.5 . . ? H451 C45 H453 109.5 . . ? H452 C45 H453 109.5 . . ? C44 C46 C72 119.9(5) . . ? C44 C46 C48 120.9(5) . . ? C72 C46 C48 119.2(5) . . ? N41 C47 C48 123.0(5) . . ? N41 C47 H47 118.5 . . ? C48 C47 H47 118.5 . . ? C47 C48 C49 116.9(6) . . ? C47 C48 C46 119.7(5) . . ? C49 C48 C46 123.3(5) . . ? C50 C49 C48 121.0(5) . . ? C50 C49 H49 119.5 . . ? C48 C49 H49 119.5 . . ? C49 C50 C51 118.5(6) . . ? C49 C50 H50 120.8 . . ? C51 C50 H50 120.8 . . ? N41 C51 C50 121.1(5) . . ? N41 C51 C52 114.2(5) . . ? C50 C51 C52 124.6(5) . . ? N42 C52 C53 119.9(5) . . ? N42 C52 C51 114.9(5) . . ? C53 C52 C51 125.2(5) . . ? C54 C53 C52 118.8(5) . . ? C54 C53 H531 120.6 . . ? C52 C53 H531 120.6 . . ? C55 C54 C53 121.1(5) . . ? C55 C54 H54 119.4 . . ? C53 C54 H54 119.4 . . ? C54 C55 C56 118.2(5) . . ? C54 C55 H55 120.9 . . ? C56 C55 H55 120.9 . . ? N42 C56 C55 120.8(5) . . ? N42 C56 C57 114.5(4) . . ? C55 C56 C57 124.7(5) . . ? N43 C57 C58 121.6(5) . . ? N43 C57 C56 114.4(4) . . ? C58 C57 C56 124.0(5) . . ? C59 C58 C57 118.5(5) . . ? C59 C58 H58 120.8 . . ? C57 C58 H58 120.8 . . ? C60 C59 C58 121.6(5) . . ? C60 C59 H59 119.2 . . ? C58 C59 H59 119.2 . . ? C59 C60 C61 115.9(4) . . ? C59 C60 C62B 123.7(6) . . ? C61 C60 C62B 120.4(5) . . ? C59 C60 C62A 124.3(7) . . ? C61 C60 C62A 119.7(7) . . ? N43 C61 C60 123.7(5) . . ? N43 C61 H61 118.2 . . ? C60 C61 H61 118.2 . . ? C72 C71 H711 109.5 . . ? C72 C71 H712 109.5 . . ? H711 C71 H712 109.5 . . ? C72 C71 H713 109.5 . . ? H711 C71 H713 109.5 . . ? H712 C71 H713 109.5 . . ? C73 C72 C46 119.4(5) . . ? C73 C72 C71 117.5(6) . . ? C46 C72 C71 123.0(5) . . ? C42 C73 C72 121.3(6) . . ? C42 C73 H73 119.3 . . ? C72 C73 H73 119.3 . . ? F3A P1 F1A 90.06(4) . . ? F4B P1 F2B 90.06(4) . . ? F3A P1 F5A 90.06(4) . . ? F1A P1 F5A 90.03(4) . . ? F3A P1 F6A 90.08(4) . . ? F1A P1 F6A 90.01(4) . . ? F5A P1 F6A 179.85(6) . . ? F4B P1 F5B 90.06(4) . . ? F2B P1 F5B 90.01(4) . . ? F4B P1 F6B 90.06(4) . . ? F2B P1 F6B 90.01(4) . . ? F5B P1 F6B 179.87(6) . . ? F4B P1 F1B 90.03(4) . . ? F2B P1 F1B 179.91(6) . . ? F5B P1 F1B 89.99(4) . . ? F6B P1 F1B 89.99(4) . . ? F3A P1 F2A 90.02(4) . . ? F1A P1 F2A 179.92(7) . . ? F5A P1 F2A 89.99(4) . . ? F6A P1 F2A 89.98(4) . . ? F4B P1 F3B 179.98(7) . . ? F2B P1 F3B 89.97(4) . . ? F5B P1 F3B 89.94(4) . . ? F6B P1 F3B 89.94(4) . . ? F1B P1 F3B 89.95(4) . . ? F3A P1 F4A 179.97(7) . . ? F1A P1 F4A 89.97(4) . . ? F5A P1 F4A 89.92(4) . . ? F6A P1 F4A 89.94(4) . . ? F1B P1 F4A 84.2(5) . . ? F2A P1 F4A 89.95(4) . . ? F12A P2A F10A 90.00(4) . . ? F12A P2A F7A 90.00(5) . . ? F10A P2A F7A 89.99(4) . . ? F12A P2A F9A 90.00(4) . . ? F10A P2A F9A 179.99(7) . . ? F7A P2A F9A 90.00(4) . . ? F12A P2A F8A 90.04(8) . . ? F10A P2A F8A 90.01(4) . . ? F7A P2A F8A 179.96(9) . . ? F9A P2A F8A 90.00(4) . . ? F12A P2A F11A 179.99(9) . . ? F10A P2A F11A 90.00(4) . . ? F7A P2A F11A 89.99(5) . . ? F9A P2A F11A 89.99(4) . . ? F8A P2A F11A 89.97(5) . . ? F10B P2B F7B 90.00(4) . . ? F10B P2B F9B 180.00(7) . . ? F7B P2B F9B 90.00(4) . . ? F10B P2B F11B 90.00(4) . . ? F7B P2B F11B 90.00(5) . . ? F9B P2B F11B 90.00(4) . . ? F10B P2B F12B 90.00(4) . . ? F7B P2B F12B 90.00(5) . . ? F9B P2B F12B 90.00(4) . . ? F11B P2B F12B 179.99(9) . . ? F10B P2B F8B 90.00(4) . . ? F7B P2B F8B 179.99(8) . . ? F9B P2B F8B 89.99(4) . . ? F11B P2B F8B 90.00(5) . . ? F12B P2B F8B 90.01(8) . . ? 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 C29A C22A C23A C25A 1(8) . . . . ? C20 C22A C23A C25A -177(5) . . . . ? C29A C22A C23A C24A -177(4) . . . . ? C20 C22A C23A C24A 5(9) . . . . ? C22A C23A C25A C26A -1(6) . . . . ? C24A C23A C25A C26A 176(2) . . . . ? C27A O2A C26A C28A -18(3) . . . . ? C27A O2A C26A C25A 168(2) . . . . ? C23A C25A C26A C28A 2(4) . . . . ? C23A C25A C26A O2A 176(2) . . . . ? O2A C26A C28A C29A -176(3) . . . . ? C25A C26A C28A C29A -2(4) . . . . ? C26A C28A C29A C22A 2(6) . . . . ? C26A C28A C29A C30A -178(3) . . . . ? C23A C22A C29A C28A -1(8) . . . . ? C20 C22A C29A C28A 176(5) . . . . ? C23A C22A C29A C30A 179(5) . . . . ? C20 C22A C29A C30A -3(8) . . . . ? C29B C22B C23B C25B 1(5) . . . . ? C20 C22B C23B C25B 178(3) . . . . ? C29B C22B C23B C24B -179(2) . . . . ? C20 C22B C23B C24B -2(5) . . . . ? C22B C23B C25B C26B -3(3) . . . . ? C24B C23B C25B C26B 177.2(14) . . . . ? C27B O2B C26B C28B -164.6(13) . . . . ? C27B O2B C26B C25B 17.0(19) . . . . ? C23B C25B C26B C28B 3(2) . . . . ? C23B C25B C26B O2B -179.0(14) . . . . ? O2B C26B C28B C29B -179.5(15) . . . . ? C25B C26B C28B C29B -1(2) . . . . ? C26B C28B C29B C22B -1(3) . . . . ? C26B C28B C29B C30B 178.3(16) . . . . ? C23B C22B C29B C28B 1(5) . . . . ? C20 C22B C29B C28B -177(3) . . . . ? C23B C22B C29B C30B -178(3) . . . . ? C20 C22B C29B C30B 5(5) . . . . ? N2 Cu1 N1 C7 0.0(5) 2 . . . ? N2 Cu1 N1 C7 -179.0(5) . . . . ? N3 Cu1 N1 C7 173.3(4) . . . . ? N3 Cu1 N1 C7 78.8(5) 2 . . . ? N1 Cu1 N1 C7 -78.5(5) 2 . . . ? N2 Cu1 N1 C11 168.3(4) 2 . . . ? N2 Cu1 N1 C11 -10.7(4) . . . . ? N3 Cu1 N1 C11 -18.4(6) . . . . ? N3 Cu1 N1 C11 -112.9(4) 2 . . . ? N1 Cu1 N1 C11 89.8(4) 2 . . . ? N3 Cu1 N2 C16 4.8(4) . . . . ? N3 Cu1 N2 C16 -77.3(4) 2 . . . ? N1 Cu1 N2 C16 100.0(4) 2 . . . ? N1 Cu1 N2 C16 -172.0(4) . . . . ? N3 Cu1 N2 C12 -179.2(4) . . . . ? N3 Cu1 N2 C12 98.7(4) 2 . . . ? N1 Cu1 N2 C12 -84.0(4) 2 . . . ? N1 Cu1 N2 C12 4.0(4) . . . . ? N2 Cu1 N3 C21 6.3(5) 2 . . . ? N2 Cu1 N3 C21 -174.6(4) . . . . ? N3 Cu1 N3 C21 -69.9(4) 2 . . . ? N1 Cu1 N3 C21 86.3(4) 2 . . . ? N1 Cu1 N3 C21 -166.9(4) . . . . ? N2 Cu1 N3 C17 173.6(3) 2 . . . ? N2 Cu1 N3 C17 -7.3(3) . . . . ? N3 Cu1 N3 C17 97.4(4) 2 . . . ? N1 Cu1 N3 C17 -106.4(3) 2 . . . ? N1 Cu1 N3 C17 0.4(6) . . . . ? C1 O1 C2 C3 176.6(5) . . . . ? C1 O1 C2 C33 -3.1(8) . . . . ? O1 C2 C3 C4 177.6(5) . . . . ? C33 C2 C3 C4 -2.7(9) . . . . ? C2 C3 C4 C6 -0.6(9) . . . . ? C2 C3 C4 C5 177.7(6) . . . . ? C3 C4 C6 C32 3.4(8) . . . . ? C5 C4 C6 C32 -174.9(5) . . . . ? C3 C4 C6 C8 -175.4(5) . . . . ? C5 C4 C6 C8 6.3(8) . . . . ? C11 N1 C7 C8 -3.3(8) . . . . ? Cu1 N1 C7 C8 164.3(4) . . . . ? N1 C7 C8 C9 -0.8(8) . . . . ? N1 C7 C8 C6 179.9(5) . . . . ? C32 C6 C8 C9 -122.1(6) . . . . ? C4 C6 C8 C9 56.7(7) . . . . ? C32 C6 C8 C7 57.3(7) . . . . ? C4 C6 C8 C7 -124.0(6) . . . . ? C7 C8 C9 C10 2.9(8) . . . . ? C6 C8 C9 C10 -177.7(5) . . . . ? C8 C9 C10 C11 -1.1(8) . . . . ? C7 N1 C11 C10 5.2(8) . . . . ? Cu1 N1 C11 C10 -164.4(4) . . . . ? C7 N1 C11 C12 -175.2(5) . . . . ? Cu1 N1 C11 C12 15.1(6) . . . . ? C9 C10 C11 N1 -3.1(8) . . . . ? C9 C10 C11 C12 177.4(5) . . . . ? C16 N2 C12 C13 -1.0(9) . . . . ? Cu1 N2 C12 C13 -176.9(5) . . . . ? C16 N2 C12 C11 178.9(5) . . . . ? Cu1 N2 C12 C11 3.0(6) . . . . ? N1 C11 C12 N2 -12.7(7) . . . . ? C10 C11 C12 N2 166.9(5) . . . . ? N1 C11 C12 C13 167.2(6) . . . . ? C10 C11 C12 C13 -13.2(10) . . . . ? N2 C12 C13 C14 1.7(11) . . . . ? C11 C12 C13 C14 -178.2(7) . . . . ? C12 C13 C14 C15 -1.1(13) . . . . ? C13 C14 C15 C16 -0.2(13) . . . . ? C12 N2 C16 C15 -0.4(8) . . . . ? Cu1 N2 C16 C15 175.5(5) . . . . ? C12 N2 C16 C17 -177.7(5) . . . . ? Cu1 N2 C16 C17 -1.8(6) . . . . ? C14 C15 C16 N2 1.0(11) . . . . ? C14 C15 C16 C17 177.9(7) . . . . ? C21 N3 C17 C18 -1.0(7) . . . . ? Cu1 N3 C17 C18 -169.5(4) . . . . ? C21 N3 C17 C16 176.9(5) . . . . ? Cu1 N3 C17 C16 8.5(5) . . . . ? N2 C16 C17 N3 -4.9(7) . . . . ? C15 C16 C17 N3 177.9(6) . . . . ? N2 C16 C17 C18 173.0(5) . . . . ? C15 C16 C17 C18 -4.2(9) . . . . ? N3 C17 C18 C19 2.6(8) . . . . ? C16 C17 C18 C19 -175.2(5) . . . . ? C17 C18 C19 C20 -1.6(9) . . . . ? C18 C19 C20 C21 -0.7(8) . . . . ? C18 C19 C20 C22A -179(2) . . . . ? C18 C19 C20 C22B 175.2(13) . . . . ? C23A C22A C20 C19 55(7) . . . . ? C29A C22A C20 C19 -123(5) . . . . ? C23A C22A C20 C21 -123(5) . . . . ? C29A C22A C20 C21 59(7) . . . . ? C23B C22B C20 C19 68(4) . . . . ? C29B C22B C20 C19 -115(3) . . . . ? C23B C22B C20 C21 -116(3) . . . . ? C29B C22B C20 C21 61(4) . . . . ? C17 N3 C21 C20 -1.5(8) . . . . ? Cu1 N3 C21 C20 165.1(4) . . . . ? C19 C20 C21 N3 2.4(8) . . . . ? C22A C20 C21 N3 -179(2) . . . . ? C22B C20 C21 N3 -173.7(13) . . . . ? C4 C6 C32 C33 -2.9(8) . . . . ? C8 C6 C32 C33 176.0(5) . . . . ? C4 C6 C32 C31 177.2(5) . . . . ? C8 C6 C32 C31 -4.0(8) . . . . ? C3 C2 C33 C32 3.2(8) . . . . ? O1 C2 C33 C32 -177.1(5) . . . . ? C6 C32 C33 C2 -0.4(8) . . . . ? C31 C32 C33 C2 179.5(5) . . . . ? C69A C62A C63A C65A -0.2(4) . . . . ? C60 C62A C63A C65A 175.8(5) . . . . ? C69A C62A C63A C64A 179.9(3) . . . . ? C60 C62A C63A C64A -4.1(4) . . . . ? C62A C63A C65A C66A 0.2(6) . . . . ? C64A C63A C65A C66A -179.9(4) . . . . ? C63A C65A C66A C68A 0.1(8) . . . . ? C63A C65A C66A O42A 163.7(12) . . . . ? C67A O42A C66A C68A 166.7(14) . . . . ? C67A O42A C66A C65A 3(2) . . . . ? C65A C66A C68A C69A -0.4(8) . . . . ? O42A C66A C68A C69A -165.2(11) . . . . ? C66A C68A C69A C62A 0.3(8) . . . . ? C66A C68A C69A C70A 170.7(12) . . . . ? C63A C62A C69A C68A 0.0(6) . . . . ? C60 C62A C69A C68A -176.0(5) . . . . ? C63A C62A C69A C70A -170.0(12) . . . . ? C60 C62A C69A C70A 14.0(12) . . . . ? C69B C62B C63B C65B -0.4(7) . . . . ? C60 C62B C63B C65B 176.5(5) . . . . ? C69B C62B C63B C64B 178.5(4) . . . . ? C60 C62B C63B C64B -4.6(7) . . . . ? C62B C63B C65B C66B -0.2(7) . . . . ? C64B C63B C65B C66B -179.1(4) . . . . ? C67B O42B C66B C68B -176.7(8) . . . . ? C67B O42B C66B C65B -6.0(12) . . . . ? C63B C65B C66B C68B 0.7(8) . . . . ? C63B C65B C66B O42B -169.7(8) . . . . ? O42B C66B C68B C69B 170.4(7) . . . . ? C65B C66B C68B C69B -0.7(8) . . . . ? C66B C68B C69B C62B 0.2(7) . . . . ? C66B C68B C69B C70B -173.2(7) . . . . ? C63B C62B C69B C68B 0.4(7) . . . . ? C60 C62B C69B C68B -176.5(5) . . . . ? C63B C62B C69B C70B 173.5(8) . . . . ? C60 C62B C69B C70B -3.3(9) . . . . ? N42 Cu2 N41 C47 -6.5(5) 2_655 . . . ? N42 Cu2 N41 C47 176.1(5) . . . . ? N43 Cu2 N41 C47 172.8(4) . . . . ? N43 Cu2 N41 C47 -86.6(5) 2_655 . . . ? N41 Cu2 N41 C47 69.5(4) 2_655 . . . ? N42 Cu2 N41 C51 -177.0(4) 2_655 . . . ? N42 Cu2 N41 C51 5.5(4) . . . . ? N43 Cu2 N41 C51 2.3(7) . . . . ? N43 Cu2 N41 C51 102.9(4) 2_655 . . . ? N41 Cu2 N41 C51 -101.0(4) 2_655 . . . ? N43 Cu2 N42 C56 -7.1(4) . . . . ? N43 Cu2 N42 C56 76.7(4) 2_655 . . . ? N41 Cu2 N42 C56 174.3(4) . . . . ? N41 Cu2 N42 C56 -103.6(4) 2_655 . . . ? N43 Cu2 N42 C52 177.1(4) . . . . ? N43 Cu2 N42 C52 -99.1(4) 2_655 . . . ? N41 Cu2 N42 C52 -1.6(4) . . . . ? N41 Cu2 N42 C52 80.6(4) 2_655 . . . ? N42 Cu2 N43 C61 1.4(4) 2_655 . . . ? N42 Cu2 N43 C61 178.8(4) . . . . ? N43 Cu2 N43 C61 78.6(4) 2_655 . . . ? N41 Cu2 N43 C61 -178.0(4) . . . . ? N41 Cu2 N43 C61 -77.5(4) 2_655 . . . ? N42 Cu2 N43 C57 -167.6(3) 2_655 . . . ? N42 Cu2 N43 C57 9.9(3) . . . . ? N43 Cu2 N43 C57 -90.3(3) 2_655 . . . ? N41 Cu2 N43 C57 13.1(6) . . . . ? N41 Cu2 N43 C57 113.5(3) 2_655 . . . ? C41 O41 C42 C43 -175.4(6) . . . . ? C41 O41 C42 C73 7.4(9) . . . . ? O41 C42 C43 C44 -179.1(6) . . . . ? C73 C42 C43 C44 -1.7(10) . . . . ? C42 C43 C44 C46 1.3(10) . . . . ? C42 C43 C44 C45 -176.8(6) . . . . ? C43 C44 C46 C72 -0.7(9) . . . . ? C45 C44 C46 C72 177.3(6) . . . . ? C43 C44 C46 C48 -179.2(6) . . . . ? C45 C44 C46 C48 -1.2(10) . . . . ? C51 N41 C47 C48 2.1(9) . . . . ? Cu2 N41 C47 C48 -167.9(5) . . . . ? N41 C47 C48 C49 -2.2(9) . . . . ? N41 C47 C48 C46 -179.8(5) . . . . ? C44 C46 C48 C47 118.7(7) . . . . ? C72 C46 C48 C47 -59.7(8) . . . . ? C44 C46 C48 C49 -58.7(9) . . . . ? C72 C46 C48 C49 122.9(7) . . . . ? C47 C48 C49 C50 0.9(9) . . . . ? C46 C48 C49 C50 178.4(6) . . . . ? C48 C49 C50 C51 0.5(10) . . . . ? C47 N41 C51 C50 -0.6(9) . . . . ? Cu2 N41 C51 C50 170.7(5) . . . . ? C47 N41 C51 C52 -179.5(5) . . . . ? Cu2 N41 C51 C52 -8.3(6) . . . . ? C49 C50 C51 N41 -0.7(9) . . . . ? C49 C50 C51 C52 178.1(6) . . . . ? C56 N42 C52 C53 1.0(8) . . . . ? Cu2 N42 C52 C53 176.7(4) . . . . ? C56 N42 C52 C51 -178.1(5) . . . . ? Cu2 N42 C52 C51 -2.3(6) . . . . ? N41 C51 C52 N42 7.2(7) . . . . ? C50 C51 C52 N42 -171.7(6) . . . . ? N41 C51 C52 C53 -171.8(5) . . . . ? C50 C51 C52 C53 9.3(9) . . . . ? N42 C52 C53 C54 -1.1(9) . . . . ? C51 C52 C53 C54 177.9(6) . . . . ? C52 C53 C54 C55 0.7(9) . . . . ? C53 C54 C55 C56 -0.1(9) . . . . ? C52 N42 C56 C55 -0.3(8) . . . . ? Cu2 N42 C56 C55 -176.1(4) . . . . ? C52 N42 C56 C57 179.1(4) . . . . ? Cu2 N42 C56 C57 3.4(6) . . . . ? C54 C55 C56 N42 -0.1(8) . . . . ? C54 C55 C56 C57 -179.5(5) . . . . ? C61 N43 C57 C58 -1.7(7) . . . . ? Cu2 N43 C57 C58 168.4(4) . . . . ? C61 N43 C57 C56 179.0(4) . . . . ? Cu2 N43 C57 C56 -11.0(5) . . . . ? N42 C56 C57 N43 5.7(6) . . . . ? C55 C56 C57 N43 -174.9(5) . . . . ? N42 C56 C57 C58 -173.7(5) . . . . ? C55 C56 C57 C58 5.8(8) . . . . ? N43 C57 C58 C59 -0.4(8) . . . . ? C56 C57 C58 C59 178.9(5) . . . . ? C57 C58 C59 C60 1.9(8) . . . . ? C58 C59 C60 C61 -1.3(7) . . . . ? C58 C59 C60 C62B 178.5(8) . . . . ? C58 C59 C60 C62A 179.0(11) . . . . ? C63B C62B C60 C59 -57.2(8) . . . . ? C69B C62B C60 C59 119.6(7) . . . . ? C63B C62B C60 C61 122.6(6) . . . . ? C69B C62B C60 C61 -60.6(7) . . . . ? C63A C62A C60 C59 -57.3(9) . . . . ? C69A C62A C60 C59 118.6(8) . . . . ? C63A C62A C60 C61 123.0(6) . . . . ? C69A C62A C60 C61 -61.0(7) . . . . ? C57 N43 C61 C60 2.3(7) . . . . ? Cu2 N43 C61 C60 -166.1(4) . . . . ? C59 C60 C61 N43 -0.8(7) . . . . ? C62B C60 C61 N43 179.3(8) . . . . ? C62A C60 C61 N43 178.8(11) . . . . ? C44 C46 C72 C73 0.6(9) . . . . ? C48 C46 C72 C73 179.1(5) . . . . ? C44 C46 C72 C71 -179.8(6) . . . . ? C48 C46 C72 C71 -1.3(9) . . . . ? O41 C42 C73 C72 178.7(6) . . . . ? C43 C42 C73 C72 1.6(9) . . . . ? C46 C72 C73 C42 -1.1(9) . . . . ? C71 C72 C73 C42 179.3(6) . . . . ? #===END data_7b _database_code_depnum_ccdc_archive 'CCDC 735261' # SG0507 _audit_creation_method SHELXL-97 _audit_creation_date 05-04-29 _chemical_name_systematic ; bis[5,5"-bis-(4-methoxy-2,6-dimethylphenyl)- [2,2':6,2"]terpyridine]zinc(II) hexafluorophosphate 2.82-acetonitrile solvate ; _chemical_name_common ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_moiety 'C66 H72 N6 O4 Zn 2+, 2(F6 P 1-), 2.82(C2 H3 N)' _chemical_formula_sum 'C71.65 H70.47 F12 N8.82 O4 P2 Zn' _chemical_formula_weight 1474.46 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 573 0.0033 0.0016 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; H H 564 0.0000 0.0000 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; F F 96 0.0171 0.0103 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; N N 71 0.0061 0.0033 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; O O 32 0.0106 0.0060 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; P P 16 0.1023 0.0942 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; Zn Zn 8 0.2839 1.4301 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n n a ' _symmetry_space_group_name_Hall ? _symmetry_Int_Tables_number 52 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' 'x, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' '-x, y-1/2, z-1/2' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 22.0637(2) _cell_length_b 25.1063(4) _cell_length_c 25.1199(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 13914.9(3) _cell_formula_units_Z 8 _cell_measurement_temperature 160(1) _cell_measurement_reflns_used 77505 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 26.0 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.408 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6096.88 _exptl_absorpt_coefficient_mu 0.487 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Blessing, 1995)' _exptl_absorpt_correction_T_min 0.851 _exptl_absorpt_correction_T_max 0.951 _exptl_special_details ; Solvent used: MeCN / diethyl ether Cooling Device: Oxford Cryosystems Cryostream 700 Crystal mount: glued on a glass fibre Mosaicity (deg.): 0.421(1) Frames collected: 256 Seconds exposure per frame: 42 Degrees rotation per frame: 1.4 Crystal-Detector distance (mm): 37.8 ; _diffrn_ambient_temperature 160(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Nonius FR590 sealed tube generator' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_detector '65 mm CCD camera on \k goniostat' _diffrn_measurement_device_type 'Nonius KappaCCD area-detector diffractometer' _diffrn_measurement_method '\f and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 127617 _diffrn_reflns_av_R_equivalents 0.0954 _diffrn_reflns_av_sigmaI/netI 0.0577 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 26.02 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.999 _reflns_number_total 13714 _reflns_number_gt 8677 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'COLLECT (Nonius, 2000)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN and SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'SHELXL97 and PLATON (Spek, 2009)' _refine_special_details ; The asymmetric unit contains two half-cations with each Zn-atom on a crystallographic two-fold axis, two disordered PF6- anions, and five different sites for partially occupied and disordered MeCN molecules. One site for a MeCN molecule is close to a two-fold axis, so the molecule is disordered about the axis and has a site occupation of 0.5. The second MeCN molecule sits exactly on a two-fold axis. The remaining three MeCN sites are close to one another and one of the three cannot be occupied simultaneously with the other two. Thus two sites were constrained to have identical site occupation factors [value refined to 0.824(7)], while the third site was restrained to be occupied to the extent that the other two sites were not. All of the MeCN molecules were further restrained to have similar geometry. By using these restrictions, the best estimate for the ratio of MeCN molecules Zn-complex cations is approximately 2.82:1. Each symmetry-independent PF6- anion is disordered over two orientations. Two orientations were defined for the F-atoms of each anion and refinement of the site occupation factors led to values of 0.59(3) and 0.52(2) for the major orientations. The P-F and F...F distances were restrained tightly, so as to maintain octahedral geometry and uniform P-F bond lengths and neighbouring atoms within and between each disordered orientation were restrained to have similar atomic displacement parameters. One methoxy group in each ligand of each symmetry-independent cation is disordered. Two conformations for these groups were defined in each case and refinement of the site occupation factors led to a values of 0.66(3) and 0.637(9) for the major conformations. Similarity restraints were applied to the chemically equivalent bond lengths and angles involving all disordered atoms in each cation, while neighbouring disordered atoms were restrained to have similar atomic displacement parameters. The H-atoms of the MeCN molecule that sits on a two-fold axis were not included in the model. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0582P)^2^+26.1830P] 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_extinction_coef ? _refine_ls_number_reflns 13712 _refine_ls_number_parameters 1039 _refine_ls_number_restraints 1018 _refine_ls_R_factor_all 0.1116 _refine_ls_R_factor_gt 0.0603 _refine_ls_wR_factor_ref 0.1587 _refine_ls_wR_factor_gt 0.1338 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.444 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.839 _refine_diff_density_min -0.634 _refine_diff_density_rms 0.067 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 Zn1 Zn 0.2500 0.0000 0.09635(3) 0.0283(2) Uani 1 2 d S . . O1 O -0.04297(17) 0.00002(16) 0.36293(16) 0.0464(10) Uani 1 1 d . . . O2A O 0.3377(13) -0.2570(9) -0.1653(14) 0.052(3) Uani 0.34(3) 1 d PDU A 1 C27A C 0.3885(12) -0.2931(12) -0.1661(15) 0.053(3) Uani 0.34(3) 1 d PDU A 1 H271 H 0.4222 -0.2767 -0.1854 0.080 Uiso 0.34(3) 1 calc PR A 1 H272 H 0.3767 -0.3262 -0.1839 0.080 Uiso 0.34(3) 1 calc PR A 1 H273 H 0.4011 -0.3009 -0.1295 0.080 Uiso 0.34(3) 1 calc PR A 1 O2B O 0.3368(7) -0.2510(5) -0.1734(7) 0.049(3) Uani 0.66(3) 1 d PDU A 2 C27B C 0.3919(6) -0.2782(7) -0.1875(8) 0.054(3) Uani 0.66(3) 1 d PDU A 2 H274 H 0.4194 -0.2533 -0.2053 0.081 Uiso 0.66(3) 1 calc PR A 2 H275 H 0.3826 -0.3079 -0.2114 0.081 Uiso 0.66(3) 1 calc PR A 2 H276 H 0.4113 -0.2920 -0.1552 0.081 Uiso 0.66(3) 1 calc PR A 2 N1 N 0.2148(2) 0.05114(17) 0.15813(17) 0.0339(10) Uani 1 1 d . . . N2 N 0.30480(19) 0.06705(16) 0.09280(16) 0.0300(10) Uani 1 1 d . . . N3 N 0.31467(17) -0.01781(16) 0.03306(16) 0.0271(9) Uani 1 1 d . . . C1 C -0.0437(3) -0.0522(2) 0.3857(3) 0.0488(15) Uani 1 1 d . . . H11 H -0.0378 -0.0788 0.3576 0.073 Uiso 1 1 calc R . . H12 H -0.0828 -0.0583 0.4032 0.073 Uiso 1 1 calc R . . H13 H -0.0111 -0.0553 0.4120 0.073 Uiso 1 1 calc R . . C2 C 0.0068(2) 0.0137(2) 0.3329(2) 0.0376(14) Uani 1 1 d . . . C3 C 0.0044(3) 0.0633(2) 0.3091(2) 0.0417(14) Uani 1 1 d . . . H3 H -0.0302 0.0851 0.3143 0.050 Uiso 1 1 calc R . . C4 C 0.0518(3) 0.0817(2) 0.2779(2) 0.0435(14) Uani 1 1 d . . . C5 C 0.0450(3) 0.1349(2) 0.2512(3) 0.0566(17) Uani 1 1 d . . . H51 H 0.0672 0.1619 0.2715 0.085 Uiso 1 1 calc R . . H52 H 0.0020 0.1445 0.2497 0.085 Uiso 1 1 calc R . . H53 H 0.0614 0.1329 0.2150 0.085 Uiso 1 1 calc R . . C6 C 0.1033(3) 0.0496(2) 0.2707(2) 0.0381(13) Uani 1 1 d . . . C7 C 0.1702(2) 0.0376(2) 0.1917(2) 0.0351(13) Uani 1 1 d . . . H7 H 0.1485 0.0057 0.1849 0.042 Uiso 1 1 calc R . . C8 C 0.1539(3) 0.0676(2) 0.2358(2) 0.0390(13) Uani 1 1 d . . . C9 C 0.1866(3) 0.1142(2) 0.2440(2) 0.0491(16) Uani 1 1 d . . . H9 H 0.1771 0.1364 0.2735 0.059 Uiso 1 1 calc R . . C10 C 0.2329(3) 0.1288(2) 0.2096(2) 0.0467(15) Uani 1 1 d . . . H10 H 0.2551 0.1607 0.2154 0.056 Uiso 1 1 calc R . . C11 C 0.2464(3) 0.0963(2) 0.1667(2) 0.0350(12) Uani 1 1 d . . . C12 C 0.2949(2) 0.1071(2) 0.1275(2) 0.0337(12) Uani 1 1 d . . . C13 C 0.3288(3) 0.1535(2) 0.1242(2) 0.0436(15) Uani 1 1 d . . . H131 H 0.3232 0.1814 0.1492 0.052 Uiso 1 1 calc R . . C14 C 0.3710(3) 0.1582(2) 0.0836(2) 0.0448(15) Uani 1 1 d . . . H14 H 0.3940 0.1900 0.0803 0.054 Uiso 1 1 calc R . . C15 C 0.3799(2) 0.1169(2) 0.0481(2) 0.0365(13) Uani 1 1 d . . . H15 H 0.4089 0.1200 0.0202 0.044 Uiso 1 1 calc R . . C16 C 0.3458(2) 0.07107(19) 0.0538(2) 0.0291(11) Uani 1 1 d . . . C17 C 0.3498(2) 0.02355(19) 0.0184(2) 0.0278(11) Uani 1 1 d . . . C18 C 0.3847(2) 0.0213(2) -0.0274(2) 0.0329(12) Uani 1 1 d . . . H18 H 0.4090 0.0508 -0.0376 0.040 Uiso 1 1 calc R . . C19 C 0.3838(2) -0.0244(2) -0.0581(2) 0.0325(12) Uani 1 1 d . . . H19 H 0.4075 -0.0261 -0.0896 0.039 Uiso 1 1 calc R . . C20 C 0.3486(2) -0.06799(19) -0.0434(2) 0.0274(11) Uani 1 1 d . . . C21 C 0.3153(2) -0.06219(19) 0.0032(2) 0.0276(11) Uani 1 1 d . . . H21 H 0.2915 -0.0915 0.0147 0.033 Uiso 1 1 calc R . . C22 C 0.3464(2) -0.11799(19) -0.07557(19) 0.0281(11) Uani 1 1 d . A . C23 C 0.3995(2) -0.1460(2) -0.0865(2) 0.0305(12) Uani 1 1 d . . . C24 C 0.4603(2) -0.1302(2) -0.0632(2) 0.0370(13) Uani 1 1 d . . . H241 H 0.4872 -0.1612 -0.0627 0.056 Uiso 1 1 calc R . . H242 H 0.4545 -0.1171 -0.0268 0.056 Uiso 1 1 calc R . . H243 H 0.4784 -0.1020 -0.0850 0.056 Uiso 1 1 calc R . . C25 C 0.3974(2) -0.1918(2) -0.1181(2) 0.0346(12) Uani 1 1 d . A . H25 H 0.4336 -0.2107 -0.1257 0.042 Uiso 1 1 calc R . . C26 C 0.3429(3) -0.2096(2) -0.1381(2) 0.0374(13) Uani 1 1 d D . . C28 C 0.2899(2) -0.1826(2) -0.1261(2) 0.0342(12) Uani 1 1 d . A . H28 H 0.2524 -0.1956 -0.1394 0.041 Uiso 1 1 calc R . . C29 C 0.2904(2) -0.1370(2) -0.0952(2) 0.0306(12) Uani 1 1 d . . . C30 C 0.2310(3) -0.1091(2) -0.0844(3) 0.0473(15) Uani 1 1 d . A . H301 H 0.2002 -0.1219 -0.1094 0.071 Uiso 1 1 calc R . . H302 H 0.2362 -0.0706 -0.0889 0.071 Uiso 1 1 calc R . . H303 H 0.2179 -0.1166 -0.0479 0.071 Uiso 1 1 calc R . . C31 C 0.1593(3) -0.0375(3) 0.2898(3) 0.0610(19) Uani 1 1 d . . . H311 H 0.1596 -0.0627 0.3196 0.091 Uiso 1 1 calc R . . H312 H 0.1968 -0.0165 0.2902 0.091 Uiso 1 1 calc R . . H313 H 0.1565 -0.0571 0.2562 0.091 Uiso 1 1 calc R . . C32 C 0.1055(2) -0.0006(2) 0.2950(2) 0.0385(13) Uani 1 1 d . . . C33 C 0.0568(2) -0.0184(2) 0.3260(2) 0.0365(13) Uani 1 1 d . . . H33 H 0.0583 -0.0525 0.3422 0.044 Uiso 1 1 calc R . . Zn41 Zn 0.7500 0.0000 0.38225(3) 0.0251(2) Uani 1 2 d S . . O41 O 0.43916(16) -0.02328(15) 0.11885(16) 0.0432(10) Uani 1 1 d . . . O42A O 0.8784(6) -0.2181(6) 0.6650(6) 0.057(3) Uani 0.363(9) 1 d PDU B 1 C67A C 0.8281(7) -0.2492(8) 0.6810(8) 0.058(3) Uani 0.363(9) 1 d PDU B 1 H671 H 0.7992 -0.2266 0.7002 0.088 Uiso 0.363(9) 1 calc PR B 1 H672 H 0.8418 -0.2780 0.7043 0.088 Uiso 0.363(9) 1 calc PR B 1 H673 H 0.8083 -0.2643 0.6495 0.088 Uiso 0.363(9) 1 calc PR B 1 O42B O 0.8467(4) -0.2220(3) 0.6632(3) 0.056(2) Uani 0.637(9) 1 d PDU B 2 C67B C 0.8934(5) -0.2607(4) 0.6636(4) 0.059(2) Uani 0.637(9) 1 d PDU B 2 H674 H 0.9013 -0.2727 0.6271 0.088 Uiso 0.637(9) 1 calc PR B 2 H675 H 0.8810 -0.2911 0.6854 0.088 Uiso 0.637(9) 1 calc PR B 2 H676 H 0.9304 -0.2450 0.6784 0.088 Uiso 0.637(9) 1 calc PR B 2 N41 N 0.70024(18) 0.04372(16) 0.32097(16) 0.0279(9) Uani 1 1 d . . . N42 N 0.79210(18) 0.07328(16) 0.38078(17) 0.0285(9) Uani 1 1 d . . . N43 N 0.81687(17) -0.00507(16) 0.44541(16) 0.0265(9) Uani 1 1 d . . . C41 C 0.4396(3) -0.0755(2) 0.0970(3) 0.0501(16) Uani 1 1 d . . . H411 H 0.4736 -0.0790 0.0722 0.075 Uiso 1 1 calc R . . H412 H 0.4015 -0.0819 0.0780 0.075 Uiso 1 1 calc R . . H413 H 0.4439 -0.1016 0.1258 0.075 Uiso 1 1 calc R . . C42 C 0.4869(2) -0.0091(2) 0.1504(2) 0.0333(12) Uani 1 1 d . . . C43 C 0.4842(2) 0.0415(2) 0.1724(2) 0.0358(13) Uani 1 1 d . . . H43 H 0.4499 0.0633 0.1655 0.043 Uiso 1 1 calc R . . C44 C 0.5304(2) 0.0609(2) 0.2042(2) 0.0318(12) Uani 1 1 d . . . C45 C 0.5227(3) 0.1154(2) 0.2286(2) 0.0434(14) Uani 1 1 d . . . H451 H 0.5446 0.1417 0.2072 0.065 Uiso 1 1 calc R . . H452 H 0.5389 0.1153 0.2650 0.065 Uiso 1 1 calc R . . H453 H 0.4795 0.1247 0.2296 0.065 Uiso 1 1 calc R . . C46 C 0.5819(2) 0.0284(2) 0.2140(2) 0.0312(12) Uani 1 1 d . . . C47 C 0.6551(2) 0.0250(2) 0.2909(2) 0.0296(11) Uani 1 1 d . . . H47 H 0.6364 -0.0074 0.3013 0.036 Uiso 1 1 calc R . . C48 C 0.6338(2) 0.05021(19) 0.2453(2) 0.0281(11) Uani 1 1 d . . . C49 C 0.6636(2) 0.0966(2) 0.2305(2) 0.0354(13) Uani 1 1 d . . . H49 H 0.6523 0.1144 0.1986 0.042 Uiso 1 1 calc R . . C50 C 0.7097(2) 0.1172(2) 0.2619(2) 0.0382(13) Uani 1 1 d . . . H50 H 0.7294 0.1494 0.2521 0.046 Uiso 1 1 calc R . . C51 C 0.7266(2) 0.09037(19) 0.3074(2) 0.0291(11) Uani 1 1 d . . . C52 C 0.7733(2) 0.1097(2) 0.3454(2) 0.0340(12) Uani 1 1 d . . . C53 C 0.7951(3) 0.1610(2) 0.3474(3) 0.0572(19) Uani 1 1 d . . . H531 H 0.7816 0.1870 0.3227 0.069 Uiso 1 1 calc R . . C54 C 0.8369(3) 0.1737(3) 0.3859(3) 0.072(2) Uani 1 1 d . . . H54 H 0.8527 0.2089 0.3876 0.086 Uiso 1 1 calc R . . C55 C 0.8562(3) 0.1362(2) 0.4221(3) 0.0534(17) Uani 1 1 d . . . H55 H 0.8851 0.1450 0.4487 0.064 Uiso 1 1 calc R . . C56 C 0.8325(2) 0.0854(2) 0.4188(2) 0.0318(12) Uani 1 1 d . . . C57 C 0.8462(2) 0.0409(2) 0.4561(2) 0.0288(11) Uani 1 1 d . . . C58 C 0.8827(2) 0.0458(2) 0.5006(2) 0.0354(13) Uani 1 1 d . . . H58 H 0.9042 0.0780 0.5072 0.042 Uiso 1 1 calc R . . C59 C 0.8875(2) 0.0034(2) 0.5353(2) 0.0377(13) Uani 1 1 d . . . H59 H 0.9117 0.0068 0.5664 0.045 Uiso 1 1 calc R . . C60 C 0.8577(2) -0.0442(2) 0.5255(2) 0.0321(12) Uani 1 1 d . . . C61 C 0.8235(2) -0.0460(2) 0.4787(2) 0.0280(11) Uani 1 1 d . . . H61 H 0.8037 -0.0785 0.4701 0.034 Uiso 1 1 calc R . . C62 C 0.8584(2) -0.0905(2) 0.5626(2) 0.0355(13) Uani 1 1 d . B . C63 C 0.9131(3) -0.1167(2) 0.5744(2) 0.0411(14) Uani 1 1 d . . . C64 C 0.9725(3) -0.0998(3) 0.5497(2) 0.0522(17) Uani 1 1 d . . . H641 H 0.9875 -0.0678 0.5676 0.078 Uiso 1 1 calc R . . H642 H 0.9664 -0.0922 0.5118 0.078 Uiso 1 1 calc R . . H643 H 1.0023 -0.1286 0.5536 0.078 Uiso 1 1 calc R . . C65 C 0.9120(3) -0.1607(3) 0.6080(2) 0.0518(17) Uani 1 1 d . B . H65 H 0.9489 -0.1785 0.6162 0.062 Uiso 1 1 calc R . . C66 C 0.8587(3) -0.1790(2) 0.6296(2) 0.0505(17) Uani 1 1 d D . . C68 C 0.8051(3) -0.1536(3) 0.6181(2) 0.0489(16) Uani 1 1 d . B . H68 H 0.7683 -0.1663 0.6331 0.059 Uiso 1 1 calc R . . C69 C 0.8041(3) -0.1095(3) 0.5846(2) 0.0446(15) Uani 1 1 d . . . C70 C 0.7438(3) -0.0839(3) 0.5737(3) 0.075(2) Uani 1 1 d . B . H701 H 0.7291 -0.0950 0.5386 0.112 Uiso 1 1 calc R . . H702 H 0.7482 -0.0451 0.5744 0.112 Uiso 1 1 calc R . . H703 H 0.7146 -0.0949 0.6010 0.112 Uiso 1 1 calc R . . C71 C 0.6360(3) -0.0607(2) 0.2030(2) 0.0442(15) Uani 1 1 d . . . H711 H 0.6742 -0.0411 0.1994 0.066 Uiso 1 1 calc R . . H712 H 0.6348 -0.0897 0.1769 0.066 Uiso 1 1 calc R . . H713 H 0.6330 -0.0755 0.2390 0.066 Uiso 1 1 calc R . . C72 C 0.5835(2) -0.0233(2) 0.1933(2) 0.0311(12) Uani 1 1 d . . . C73 C 0.5357(2) -0.0416(2) 0.1616(2) 0.0317(12) Uani 1 1 d . . . H73 H 0.5369 -0.0768 0.1476 0.038 Uiso 1 1 calc R . . N74 N 0.8134(6) 0.2736(7) 0.2632(7) 0.117(8) Uani 0.50 1 d PD . . C75 C 0.8628(6) 0.2600(12) 0.2599(9) 0.074(7) Uani 0.50 1 d PD . . C76 C 0.9261(6) 0.2399(14) 0.2575(17) 0.076(10) Uani 0.50 1 d PD . . H761 H 0.9460 0.2537 0.2255 0.114 Uiso 0.50 1 calc PR . . H762 H 0.9258 0.2009 0.2563 0.114 Uiso 0.50 1 calc PR . . H763 H 0.9484 0.2518 0.2891 0.114 Uiso 0.50 1 calc PR . . N77 N 0.3071(4) 0.2500 0.2500 0.099(4) Uani 1 2 d SD . . C78 C 0.3590(5) 0.2500 0.2500 0.071(3) Uani 1 2 d SD . . C79 C 0.4264(4) 0.2500 0.2500 0.115(5) Uani 1 2 d SD . . N80 N 0.1560(6) 0.3314(4) -0.0589(4) 0.117(4) Uani 0.824(7) 1 d PD C 1 C81 C 0.1225(5) 0.3036(4) -0.0374(4) 0.088(4) Uani 0.824(7) 1 d PD C 1 C82 C 0.0826(4) 0.2665(3) -0.0073(4) 0.076(3) Uani 0.824(7) 1 d PD C 1 H821 H 0.1074 0.2390 0.0098 0.114 Uiso 0.824(7) 1 calc PR C 1 H822 H 0.0538 0.2496 -0.0317 0.114 Uiso 0.824(7) 1 calc PR C 1 H823 H 0.0603 0.2864 0.0200 0.114 Uiso 0.824(7) 1 calc PR C 1 N83 N 0.1984(5) 0.1840(3) 0.0530(4) 0.106(4) Uani 0.824(7) 1 d PD C 1 C84 C 0.2311(5) 0.2152(4) 0.0358(4) 0.081(4) Uani 0.824(7) 1 d PD C 1 C85 C 0.2700(6) 0.2572(5) 0.0116(7) 0.103(5) Uani 0.824(7) 1 d PD C 1 H851 H 0.2800 0.2473 -0.0251 0.155 Uiso 0.824(7) 1 calc PR C 1 H852 H 0.3075 0.2607 0.0323 0.155 Uiso 0.824(7) 1 calc PR C 1 H853 H 0.2482 0.2912 0.0117 0.155 Uiso 0.824(7) 1 calc PR C 1 N86 N 0.2177(14) 0.3230(12) -0.0500(12) 0.054(9) Uani 0.176(7) 1 d PD C 2 C87 C 0.2464(14) 0.2907(13) -0.0296(13) 0.045(9) Uani 0.176(7) 1 d PD C 2 C88 C 0.291(2) 0.254(2) -0.004(2) 0.073(18) Uani 0.176(7) 1 d PDU C 2 H881 H 0.3306 0.2584 -0.0212 0.110 Uiso 0.176(7) 1 calc PR C 2 H882 H 0.2773 0.2169 -0.0094 0.110 Uiso 0.176(7) 1 calc PR C 2 H883 H 0.2939 0.2616 0.0336 0.110 Uiso 0.176(7) 1 calc PR C 2 P1 P 0.43181(8) 0.18222(6) 0.39736(7) 0.0529(5) Uani 1 1 d D . . F1A F 0.4896(4) 0.1556(4) 0.4269(4) 0.082(3) Uani 0.59(3) 1 d PD D 1 F2A F 0.3746(4) 0.2074(4) 0.3724(4) 0.082(3) Uani 0.59(3) 1 d PD D 1 F3A F 0.4620(5) 0.1703(4) 0.3429(3) 0.080(3) Uani 0.59(3) 1 d PD D 1 F4A F 0.4039(5) 0.1900(5) 0.4561(3) 0.080(3) Uani 0.59(3) 1 d PD D 1 F5A F 0.4021(4) 0.1239(2) 0.3970(5) 0.064(3) Uani 0.59(3) 1 d PD D 1 F6A F 0.4635(3) 0.2378(2) 0.4018(6) 0.064(3) Uani 0.59(3) 1 d PD D 1 F1B F 0.4964(5) 0.1651(7) 0.4176(8) 0.128(8) Uani 0.41(3) 1 d PD D 2 F2B F 0.3693(5) 0.2022(7) 0.3727(7) 0.128(8) Uani 0.41(3) 1 d PD D 2 F3B F 0.4489(9) 0.1587(6) 0.3396(4) 0.098(5) Uani 0.41(3) 1 d PD D 2 F4B F 0.4164(9) 0.2098(7) 0.4509(4) 0.098(5) Uani 0.41(3) 1 d PD D 2 F5B F 0.4036(8) 0.1284(4) 0.4130(7) 0.096(5) Uani 0.41(3) 1 d PD D 2 F6B F 0.4612(7) 0.2382(4) 0.3771(9) 0.096(5) Uani 0.41(3) 1 d PD D 2 P2 P 0.94147(8) 0.19786(6) 0.08985(7) 0.0495(4) Uani 1 1 d D . . F7A F 1.0126(3) 0.1923(3) 0.0679(5) 0.080(3) Uani 0.517(15) 1 d PD E 1 F8A F 0.8783(3) 0.2040(4) 0.1120(5) 0.080(3) Uani 0.517(15) 1 d PD E 1 F9A F 0.9678(5) 0.1766(5) 0.1456(3) 0.081(3) Uani 0.517(15) 1 d PD E 1 F10A F 0.9249(6) 0.2178(3) 0.0324(3) 0.081(3) Uani 0.517(15) 1 d PD E 1 F11A F 0.9315(4) 0.1380(2) 0.0722(4) 0.060(2) Uani 0.517(15) 1 d PD E 1 F12A F 0.9606(4) 0.2569(2) 0.1083(4) 0.060(2) Uani 0.517(15) 1 d PD E 1 F7B F 0.9905(4) 0.1888(4) 0.0497(3) 0.063(3) Uani 0.483(15) 1 d PD E 2 F8B F 0.8846(4) 0.2049(4) 0.1331(4) 0.063(3) Uani 0.483(15) 1 d PD E 2 F9B F 0.9804(4) 0.1820(4) 0.1391(3) 0.052(2) Uani 0.483(15) 1 d PD E 2 F10B F 0.8911(4) 0.2137(3) 0.0456(3) 0.052(2) Uani 0.483(15) 1 d PD E 2 F11B F 0.9182(4) 0.1367(2) 0.0830(5) 0.052(2) Uani 0.483(15) 1 d PD E 2 F12B F 0.9555(4) 0.2589(2) 0.0956(5) 0.052(2) Uani 0.483(15) 1 d PD E 2 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 Zn1 0.0380(5) 0.0233(4) 0.0236(4) 0.000 0.000 -0.0060(4) O1 0.040(2) 0.051(2) 0.048(2) -0.002(2) 0.0083(19) 0.0070(19) O2A 0.058(4) 0.046(5) 0.051(6) -0.017(5) 0.001(4) 0.002(4) C27A 0.060(4) 0.046(5) 0.053(6) -0.019(5) 0.003(5) 0.003(5) O2B 0.056(3) 0.043(4) 0.049(5) -0.017(4) 0.001(3) -0.001(3) C27B 0.063(4) 0.045(5) 0.054(6) -0.020(5) 0.006(4) 0.002(4) N1 0.048(3) 0.030(2) 0.024(2) -0.0012(19) 0.000(2) -0.004(2) N2 0.038(2) 0.026(2) 0.026(2) -0.0018(18) -0.004(2) -0.0041(18) N3 0.028(2) 0.025(2) 0.028(2) 0.0039(18) -0.0028(18) -0.0022(17) C1 0.040(3) 0.055(4) 0.051(4) 0.005(3) 0.007(3) 0.000(3) C2 0.037(3) 0.050(4) 0.025(3) -0.005(2) -0.001(2) 0.003(3) C3 0.047(3) 0.043(4) 0.035(3) -0.003(3) -0.001(3) 0.011(3) C4 0.060(4) 0.040(3) 0.030(3) -0.004(3) -0.003(3) 0.005(3) C5 0.080(5) 0.046(4) 0.044(4) 0.004(3) 0.003(3) 0.013(3) C6 0.050(3) 0.043(3) 0.021(3) -0.003(2) 0.001(2) 0.002(3) C7 0.046(3) 0.032(3) 0.027(3) 0.001(2) 0.001(3) -0.003(2) C8 0.053(3) 0.039(3) 0.025(3) -0.001(2) 0.002(3) 0.002(3) C9 0.072(4) 0.045(4) 0.030(3) -0.010(3) 0.004(3) -0.002(3) C10 0.066(4) 0.037(3) 0.037(3) -0.011(3) 0.004(3) -0.013(3) C11 0.047(3) 0.030(3) 0.027(3) -0.002(2) -0.002(3) -0.006(3) C12 0.042(3) 0.027(3) 0.031(3) -0.003(2) -0.007(2) -0.006(2) C13 0.054(4) 0.035(3) 0.042(3) -0.009(3) 0.000(3) -0.009(3) C14 0.048(4) 0.032(3) 0.054(4) -0.004(3) 0.002(3) -0.011(3) C15 0.035(3) 0.034(3) 0.041(3) 0.000(3) -0.001(3) -0.008(2) C16 0.030(3) 0.026(3) 0.031(3) 0.002(2) -0.006(2) -0.001(2) C17 0.027(3) 0.026(3) 0.030(3) 0.005(2) -0.003(2) -0.001(2) C18 0.034(3) 0.028(3) 0.037(3) 0.007(2) 0.004(2) -0.006(2) C19 0.033(3) 0.034(3) 0.030(3) 0.001(2) 0.005(2) 0.000(2) C20 0.025(3) 0.028(3) 0.029(3) 0.002(2) -0.002(2) 0.003(2) C21 0.030(3) 0.025(3) 0.028(3) 0.003(2) -0.004(2) -0.003(2) C22 0.034(3) 0.026(3) 0.024(3) 0.004(2) -0.001(2) -0.002(2) C23 0.034(3) 0.031(3) 0.027(3) 0.005(2) 0.001(2) 0.001(2) C24 0.031(3) 0.037(3) 0.043(3) -0.003(3) -0.006(2) 0.002(2) C25 0.038(3) 0.032(3) 0.034(3) -0.001(2) 0.000(2) 0.005(2) C26 0.052(4) 0.030(3) 0.030(3) -0.003(2) -0.002(3) -0.002(3) C28 0.037(3) 0.035(3) 0.031(3) 0.000(2) -0.004(2) -0.007(2) C29 0.033(3) 0.033(3) 0.026(3) 0.003(2) -0.002(2) -0.005(2) C30 0.038(3) 0.048(4) 0.055(4) -0.006(3) -0.004(3) 0.000(3) C31 0.055(4) 0.065(5) 0.063(5) 0.026(4) 0.019(3) 0.019(3) C32 0.042(3) 0.047(3) 0.027(3) -0.001(3) 0.002(2) 0.006(3) C33 0.045(3) 0.037(3) 0.028(3) 0.003(2) -0.002(3) 0.004(3) Zn41 0.0301(4) 0.0230(4) 0.0220(4) 0.000 0.000 -0.0062(3) O41 0.038(2) 0.041(2) 0.051(3) -0.0053(19) -0.0124(19) 0.0065(18) O42A 0.073(7) 0.047(5) 0.051(5) 0.016(4) 0.002(6) 0.004(6) C67A 0.072(6) 0.050(5) 0.053(5) 0.017(4) 0.005(5) 0.005(5) O42B 0.069(5) 0.051(4) 0.047(4) 0.017(3) 0.011(4) 0.010(4) C67B 0.073(5) 0.049(4) 0.054(4) 0.016(4) 0.005(4) 0.008(4) N41 0.035(2) 0.024(2) 0.025(2) 0.0032(18) 0.0015(19) -0.0035(18) N42 0.028(2) 0.027(2) 0.031(2) -0.0039(19) 0.0020(19) -0.0044(18) N43 0.027(2) 0.029(2) 0.024(2) -0.0055(19) 0.0022(17) -0.0021(18) C41 0.045(3) 0.050(4) 0.055(4) -0.012(3) -0.021(3) 0.008(3) C42 0.034(3) 0.037(3) 0.029(3) 0.001(2) -0.002(2) -0.003(2) C43 0.034(3) 0.035(3) 0.038(3) 0.005(3) -0.001(2) 0.006(2) C44 0.039(3) 0.031(3) 0.026(3) 0.003(2) 0.002(2) 0.001(2) C45 0.050(3) 0.037(3) 0.043(4) -0.001(3) 0.001(3) 0.006(3) C46 0.036(3) 0.034(3) 0.024(3) 0.002(2) 0.001(2) -0.001(2) C47 0.033(3) 0.027(3) 0.029(3) 0.000(2) 0.002(2) -0.005(2) C48 0.031(3) 0.027(3) 0.026(3) -0.001(2) 0.004(2) 0.001(2) C49 0.041(3) 0.036(3) 0.029(3) 0.007(2) -0.002(2) 0.000(2) C50 0.044(3) 0.028(3) 0.043(3) 0.009(3) 0.000(3) -0.006(2) C51 0.032(3) 0.022(3) 0.033(3) 0.003(2) 0.003(2) -0.004(2) C52 0.037(3) 0.026(3) 0.039(3) 0.000(2) 0.000(2) -0.004(2) C53 0.068(4) 0.032(3) 0.072(5) 0.017(3) -0.028(4) -0.019(3) C54 0.078(5) 0.032(4) 0.106(6) 0.009(4) -0.038(5) -0.021(3) C55 0.051(4) 0.037(4) 0.073(5) 0.000(3) -0.022(3) -0.014(3) C56 0.029(3) 0.030(3) 0.036(3) -0.004(2) -0.001(2) -0.007(2) C57 0.025(3) 0.033(3) 0.029(3) -0.008(2) 0.003(2) -0.001(2) C58 0.030(3) 0.043(3) 0.034(3) -0.008(3) -0.002(2) -0.009(2) C59 0.031(3) 0.054(4) 0.028(3) -0.007(3) -0.007(2) -0.006(3) C60 0.023(3) 0.047(3) 0.026(3) -0.001(2) 0.000(2) 0.000(2) C61 0.026(3) 0.030(3) 0.028(3) -0.002(2) -0.001(2) -0.002(2) C62 0.035(3) 0.047(3) 0.024(3) -0.002(2) -0.005(2) -0.001(2) C63 0.044(3) 0.054(4) 0.025(3) -0.009(3) -0.005(3) 0.009(3) C64 0.041(3) 0.076(5) 0.039(4) 0.002(3) 0.000(3) 0.014(3) C65 0.070(4) 0.059(4) 0.027(3) 0.002(3) -0.002(3) 0.026(3) C66 0.087(5) 0.041(4) 0.024(3) 0.003(3) 0.007(3) 0.003(3) C68 0.056(4) 0.059(4) 0.031(3) 0.001(3) -0.001(3) -0.014(3) C69 0.044(3) 0.058(4) 0.032(3) 0.006(3) -0.003(3) -0.007(3) C70 0.035(4) 0.121(7) 0.068(5) 0.045(5) 0.001(3) -0.002(4) C71 0.045(3) 0.041(3) 0.047(4) -0.012(3) -0.011(3) 0.012(3) C72 0.036(3) 0.032(3) 0.026(3) -0.001(2) -0.002(2) 0.001(2) C73 0.036(3) 0.031(3) 0.029(3) 0.003(2) 0.000(2) 0.000(2) N74 0.105(11) 0.17(2) 0.079(14) 0.067(13) 0.031(10) 0.066(11) C75 0.081(9) 0.10(2) 0.038(18) 0.014(11) 0.016(9) 0.028(12) C76 0.069(8) 0.09(3) 0.07(2) -0.016(17) 0.015(11) 0.017(10) N77 0.082(7) 0.118(9) 0.098(8) -0.026(7) 0.000 0.000 C78 0.099(9) 0.049(6) 0.064(7) -0.006(5) 0.000 0.000 C79 0.062(8) 0.143(13) 0.140(13) 0.061(11) 0.000 0.000 N80 0.136(11) 0.080(7) 0.135(10) -0.050(7) 0.024(8) -0.032(7) C81 0.098(9) 0.071(8) 0.096(9) -0.047(7) -0.027(7) 0.011(6) C82 0.082(7) 0.059(6) 0.088(7) -0.031(5) 0.012(6) -0.012(5) N83 0.199(12) 0.039(5) 0.081(7) -0.016(5) -0.011(7) -0.010(6) C84 0.098(8) 0.066(7) 0.079(8) -0.025(6) -0.036(6) 0.033(6) C85 0.068(8) 0.087(10) 0.156(16) 0.008(10) -0.004(9) 0.002(7) N86 0.05(2) 0.06(2) 0.05(2) -0.021(16) 0.020(16) -0.021(17) C87 0.033(18) 0.07(3) 0.033(19) -0.020(18) 0.005(16) 0.007(18) C88 0.07(2) 0.07(2) 0.07(2) 0.004(13) 0.001(14) -0.005(13) P1 0.0580(11) 0.0408(9) 0.0598(12) -0.0059(8) 0.0162(9) 0.0028(8) F1A 0.104(8) 0.065(5) 0.078(6) -0.009(4) -0.036(5) 0.017(5) F2A 0.104(8) 0.065(5) 0.078(6) -0.009(4) -0.036(5) 0.017(5) F3A 0.119(6) 0.057(5) 0.063(4) -0.007(3) 0.043(4) 0.001(4) F4A 0.119(6) 0.057(5) 0.063(4) -0.007(3) 0.043(4) 0.001(4) F5A 0.067(4) 0.041(3) 0.083(6) -0.013(3) 0.015(3) -0.007(3) F6A 0.067(4) 0.041(3) 0.083(6) -0.013(3) 0.015(3) -0.007(3) F1B 0.058(9) 0.112(13) 0.215(19) 0.014(11) 0.016(10) 0.026(8) F2B 0.058(9) 0.112(13) 0.215(19) 0.014(11) 0.016(10) 0.026(8) F3B 0.181(13) 0.044(7) 0.069(7) -0.003(4) 0.033(7) 0.009(7) F4B 0.181(13) 0.044(7) 0.069(7) -0.003(4) 0.033(7) 0.009(7) F5B 0.151(11) 0.068(7) 0.069(9) 0.006(5) 0.042(7) -0.027(6) F6B 0.151(11) 0.068(7) 0.069(9) 0.006(5) 0.042(7) -0.027(6) P2 0.0584(10) 0.0301(8) 0.0600(11) -0.0037(7) -0.0111(9) 0.0083(7) F7A 0.037(3) 0.055(4) 0.148(9) -0.025(5) -0.002(4) 0.000(3) F8A 0.037(3) 0.055(4) 0.148(9) -0.025(5) -0.002(4) 0.000(3) F9A 0.099(7) 0.063(5) 0.081(5) 0.016(4) -0.032(4) -0.022(4) F10A 0.099(7) 0.063(5) 0.081(5) 0.016(4) -0.032(4) -0.022(4) F11A 0.073(5) 0.037(5) 0.072(5) -0.009(3) -0.019(4) 0.003(3) F12A 0.073(5) 0.037(5) 0.072(5) -0.009(3) -0.019(4) 0.003(3) F7B 0.071(5) 0.056(4) 0.061(5) -0.007(3) 0.022(4) -0.001(4) F8B 0.071(5) 0.056(4) 0.061(5) -0.007(3) 0.022(4) -0.001(4) F9B 0.057(4) 0.042(4) 0.056(4) -0.004(3) -0.016(3) 0.013(3) F10B 0.057(4) 0.042(4) 0.056(4) -0.004(3) -0.016(3) 0.013(3) F11B 0.059(4) 0.027(4) 0.071(5) 0.000(3) -0.010(3) 0.004(3) F12B 0.059(4) 0.027(4) 0.071(5) 0.000(3) -0.010(3) 0.004(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 Zn1 N2 2.074(4) . ? Zn1 N1 2.159(4) . ? Zn1 N3 2.183(4) . ? O1 C2 1.376(7) . ? O1 C1 1.431(7) . ? O2A C26 1.377(12) . ? O2A C27A 1.440(10) . ? C27A H271 0.9800 . ? C27A H272 0.9800 . ? C27A H273 0.9800 . ? O2B C26 1.373(8) . ? O2B C27B 1.440(9) . ? C27B H274 0.9800 . ? C27B H275 0.9800 . ? C27B H276 0.9800 . ? N1 C7 1.339(7) . ? N1 C11 1.348(6) . ? N2 C16 1.337(6) . ? N2 C12 1.348(6) . ? N3 C21 1.343(6) . ? N3 C17 1.347(6) . ? C1 H11 0.9800 . ? C1 H12 0.9800 . ? C1 H13 0.9800 . ? C2 C33 1.377(7) . ? C2 C3 1.382(8) . ? C3 C4 1.387(8) . ? C3 H3 0.9500 . ? C4 C6 1.405(8) . ? C4 C5 1.500(8) . ? C5 H51 0.9800 . ? C5 H52 0.9800 . ? C5 H53 0.9800 . ? C6 C32 1.402(8) . ? C6 C8 1.489(8) . ? C7 C8 1.388(7) . ? C7 H7 0.9500 . ? C8 C9 1.390(8) . ? C9 C10 1.387(8) . ? C9 H9 0.9500 . ? C10 C11 1.385(7) . ? C10 H10 0.9500 . ? C11 C12 1.480(8) . ? C12 C13 1.388(7) . ? C13 C14 1.385(8) . ? C13 H131 0.9500 . ? C14 C15 1.382(8) . ? C14 H14 0.9500 . ? C15 C16 1.384(7) . ? C15 H15 0.9500 . ? C16 C17 1.491(7) . ? C17 C18 1.384(7) . ? C18 C19 1.382(7) . ? C18 H18 0.9500 . ? C19 C20 1.392(7) . ? C19 H19 0.9500 . ? C20 C21 1.389(7) . ? C20 C22 1.493(7) . ? C21 H21 0.9500 . ? C22 C23 1.394(7) . ? C22 C29 1.413(7) . ? C23 C25 1.398(7) . ? C23 C24 1.516(7) . ? C24 H241 0.9800 . ? C24 H242 0.9800 . ? C24 H243 0.9800 . ? C25 C26 1.379(7) . ? C25 H25 0.9500 . ? C26 C28 1.385(8) . ? C28 C29 1.383(7) . ? C28 H28 0.9500 . ? C29 C30 1.511(7) . ? C30 H301 0.9800 . ? C30 H302 0.9800 . ? C30 H303 0.9800 . ? C31 C32 1.511(8) . ? C31 H311 0.9800 . ? C31 H312 0.9800 . ? C31 H313 0.9800 . ? C32 C33 1.399(8) . ? C33 H33 0.9500 . ? Zn41 N42 2.061(4) . ? Zn41 N43 2.170(4) . ? Zn41 N41 2.186(4) . ? O41 C42 1.366(6) . ? O41 C41 1.421(7) . ? O42A C66 1.393(11) . ? O42A C67A 1.415(11) . ? C67A H671 0.9800 . ? C67A H672 0.9800 . ? C67A H673 0.9800 . ? O42B C66 1.397(9) . ? O42B C67B 1.416(10) . ? C67B H674 0.9800 . ? C67B H675 0.9800 . ? C67B H676 0.9800 . ? N41 C47 1.335(6) . ? N41 C51 1.351(6) . ? N42 C52 1.341(7) . ? N42 C56 1.343(6) . ? N43 C61 1.334(6) . ? N43 C57 1.350(6) . ? C41 H411 0.9800 . ? C41 H412 0.9800 . ? C41 H413 0.9800 . ? C42 C73 1.380(7) . ? C42 C43 1.387(7) . ? C43 C44 1.382(7) . ? C43 H43 0.9500 . ? C44 C46 1.420(7) . ? C44 C45 1.511(7) . ? C45 H451 0.9800 . ? C45 H452 0.9800 . ? C45 H453 0.9800 . ? C46 C72 1.399(7) . ? C46 C48 1.494(7) . ? C47 C48 1.390(7) . ? C47 H47 0.9500 . ? C48 C49 1.389(7) . ? C49 C50 1.387(7) . ? C49 H49 0.9500 . ? C50 C51 1.380(7) . ? C50 H50 0.9500 . ? C51 C52 1.487(7) . ? C52 C53 1.373(7) . ? C53 C54 1.374(9) . ? C53 H531 0.9500 . ? C54 C55 1.377(9) . ? C54 H54 0.9500 . ? C55 C56 1.379(7) . ? C55 H55 0.9500 . ? C56 C57 1.490(7) . ? C57 C58 1.383(7) . ? C58 C59 1.381(8) . ? C58 H58 0.9500 . ? C59 C60 1.385(7) . ? C59 H59 0.9500 . ? C60 C61 1.398(7) . ? C60 C62 1.489(7) . ? C61 H61 0.9500 . ? C62 C69 1.404(8) . ? C62 C63 1.407(7) . ? C63 C65 1.390(8) . ? C63 C64 1.511(8) . ? C64 H641 0.9800 . ? C64 H642 0.9800 . ? C64 H643 0.9800 . ? C65 C66 1.375(9) . ? C65 H65 0.9500 . ? C66 C68 1.375(9) . ? C68 C69 1.391(8) . ? C68 H68 0.9500 . ? C69 C70 1.503(9) . ? C70 H701 0.9800 . ? C70 H702 0.9800 . ? C70 H703 0.9800 . ? C71 C72 1.512(7) . ? C71 H711 0.9800 . ? C71 H712 0.9800 . ? C71 H713 0.9800 . ? C72 C73 1.399(7) . ? C73 H73 0.9500 . ? N74 C75 1.146(9) . ? C75 C76 1.487(11) . ? C76 H761 0.9800 . ? C76 H762 0.9800 . ? C76 H763 0.9800 . ? N77 C78 1.145(8) . ? C78 C79 1.488(10) . ? N80 C81 1.150(8) . ? C81 C82 1.488(10) . ? C82 H821 0.9800 . ? C82 H822 0.9800 . ? C82 H823 0.9800 . ? N83 C84 1.151(8) . ? C84 C85 1.489(10) . ? C85 H851 0.9800 . ? C85 H852 0.9800 . ? C85 H853 0.9800 . ? N86 C87 1.150(9) . ? C87 C88 1.490(11) . ? C88 H881 0.9800 . ? C88 H882 0.9800 . ? C88 H883 0.9800 . ? P1 F5B 1.537(7) . ? P1 F2A 1.544(6) . ? P1 F3A 1.549(5) . ? P1 F4B 1.551(6) . ? P1 F6A 1.565(5) . ? P1 F1B 1.572(7) . ? P1 F2B 1.593(7) . ? P1 F5A 1.605(5) . ? P1 F4A 1.611(5) . ? P1 F3B 1.611(6) . ? P1 F1A 1.619(5) . ? P1 F6B 1.630(6) . ? P2 F7B 1.497(6) . ? P2 F8A 1.508(6) . ? P2 F9B 1.557(5) . ? P2 F12B 1.569(5) . ? P2 F10A 1.570(5) . ? P2 F11A 1.582(5) . ? P2 F9A 1.608(6) . ? P2 F12A 1.609(5) . ? P2 F10B 1.622(5) . ? P2 F11B 1.628(5) . ? P2 F8B 1.668(6) . ? P2 F7A 1.669(6) . ? 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 N2 Zn1 N2 175.1(2) . 2 ? N2 Zn1 N1 107.69(16) . 2 ? N2 Zn1 N1 76.00(16) . . ? N1 Zn1 N1 88.1(2) 2 . ? N2 Zn1 N3 75.75(16) . . ? N1 Zn1 N3 151.73(15) . . ? N2 Zn1 N3 100.58(15) . 2 ? N1 Zn1 N3 99.59(15) . 2 ? N3 Zn1 N3 86.5(2) . 2 ? C2 O1 C1 117.2(4) . . ? C26 O2A C27A 119.1(19) . . ? C26 O2B C27B 115.7(10) . . ? O2B C27B H274 109.5 . . ? O2B C27B H275 109.5 . . ? H274 C27B H275 109.5 . . ? O2B C27B H276 109.5 . . ? H274 C27B H276 109.5 . . ? H275 C27B H276 109.5 . . ? C7 N1 C11 119.5(5) . . ? C7 N1 Zn1 124.5(3) . . ? C11 N1 Zn1 115.4(4) . . ? C16 N2 C12 121.8(4) . . ? C16 N2 Zn1 119.1(3) . . ? C12 N2 Zn1 118.8(3) . . ? C21 N3 C17 118.7(4) . . ? C21 N3 Zn1 125.7(3) . . ? C17 N3 Zn1 114.7(3) . . ? O1 C1 H11 109.5 . . ? O1 C1 H12 109.5 . . ? H11 C1 H12 109.5 . . ? O1 C1 H13 109.5 . . ? H11 C1 H13 109.5 . . ? H12 C1 H13 109.5 . . ? O1 C2 C33 124.3(5) . . ? O1 C2 C3 115.5(5) . . ? C33 C2 C3 120.2(5) . . ? C2 C3 C4 121.1(5) . . ? C2 C3 H3 119.4 . . ? C4 C3 H3 119.4 . . ? C3 C4 C6 119.3(5) . . ? C3 C4 C5 118.3(5) . . ? C6 C4 C5 122.3(6) . . ? C4 C5 H51 109.5 . . ? C4 C5 H52 109.5 . . ? H51 C5 H52 109.5 . . ? C4 C5 H53 109.5 . . ? H51 C5 H53 109.5 . . ? H52 C5 H53 109.5 . . ? C32 C6 C4 119.3(5) . . ? C32 C6 C8 120.2(5) . . ? C4 C6 C8 120.4(5) . . ? N1 C7 C8 123.8(5) . . ? N1 C7 H7 118.1 . . ? C8 C7 H7 118.1 . . ? C7 C8 C9 116.1(5) . . ? C7 C8 C6 120.0(5) . . ? C9 C8 C6 123.9(5) . . ? C10 C9 C8 120.9(5) . . ? C10 C9 H9 119.6 . . ? C8 C9 H9 119.6 . . ? C11 C10 C9 119.1(5) . . ? C11 C10 H10 120.4 . . ? C9 C10 H10 120.4 . . ? N1 C11 C10 120.6(5) . . ? N1 C11 C12 114.9(4) . . ? C10 C11 C12 124.5(5) . . ? N2 C12 C13 120.0(5) . . ? N2 C12 C11 114.3(4) . . ? C13 C12 C11 125.7(5) . . ? C14 C13 C12 118.6(5) . . ? C14 C13 H131 120.7 . . ? C12 C13 H131 120.7 . . ? C15 C14 C13 120.5(5) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C14 C15 C16 118.6(5) . . ? C14 C15 H15 120.7 . . ? C16 C15 H15 120.7 . . ? N2 C16 C15 120.5(5) . . ? N2 C16 C17 114.7(4) . . ? C15 C16 C17 124.8(5) . . ? N3 C17 C18 121.0(5) . . ? N3 C17 C16 114.8(4) . . ? C18 C17 C16 124.2(4) . . ? C19 C18 C17 119.3(5) . . ? C19 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? C18 C19 C20 120.8(5) . . ? C18 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? C21 C20 C19 115.8(5) . . ? C21 C20 C22 121.8(4) . . ? C19 C20 C22 122.4(4) . . ? N3 C21 C20 124.3(4) . . ? N3 C21 H21 117.9 . . ? C20 C21 H21 117.9 . . ? C23 C22 C29 119.7(5) . . ? C23 C22 C20 120.2(4) . . ? C29 C22 C20 120.0(4) . . ? C22 C23 C25 119.9(5) . . ? C22 C23 C24 122.4(5) . . ? C25 C23 C24 117.6(5) . . ? C23 C24 H241 109.5 . . ? C23 C24 H242 109.5 . . ? H241 C24 H242 109.5 . . ? C23 C24 H243 109.5 . . ? H241 C24 H243 109.5 . . ? H242 C24 H243 109.5 . . ? C26 C25 C23 120.2(5) . . ? C26 C25 H25 119.9 . . ? C23 C25 H25 119.9 . . ? O2B C26 C25 124.6(8) . . ? O2A C26 C25 122.3(13) . . ? O2B C26 C28 115.4(7) . . ? O2A C26 C28 117.5(13) . . ? C25 C26 C28 119.9(5) . . ? C29 C28 C26 121.4(5) . . ? C29 C28 H28 119.3 . . ? C26 C28 H28 119.3 . . ? C28 C29 C22 118.8(5) . . ? C28 C29 C30 118.5(5) . . ? C22 C29 C30 122.6(5) . . ? C29 C30 H301 109.5 . . ? C29 C30 H302 109.5 . . ? H301 C30 H302 109.5 . . ? C29 C30 H303 109.5 . . ? H301 C30 H303 109.5 . . ? H302 C30 H303 109.5 . . ? C32 C31 H311 109.5 . . ? C32 C31 H312 109.5 . . ? H311 C31 H312 109.5 . . ? C32 C31 H313 109.5 . . ? H311 C31 H313 109.5 . . ? H312 C31 H313 109.5 . . ? C33 C32 C6 120.1(5) . . ? C33 C32 C31 117.2(5) . . ? C6 C32 C31 122.7(5) . . ? C2 C33 C32 120.0(5) . . ? C2 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? N42 Zn41 N42 177.9(2) . 2_655 ? N42 Zn41 N43 105.50(15) . 2_655 ? N42 Zn41 N43 76.06(16) . . ? N43 Zn41 N43 86.1(2) 2_655 . ? N42 Zn41 N41 102.07(15) . 2_655 ? N43 Zn41 N41 98.28(14) . 2_655 ? N42 Zn41 N41 76.44(16) . . ? N43 Zn41 N41 152.32(15) . . ? N41 Zn41 N41 90.5(2) 2_655 . ? C42 O41 C41 117.3(4) . . ? C66 O42A C67A 108.9(12) . . ? C66 O42B C67B 113.2(7) . . ? O42B C67B H674 109.5 . . ? O42B C67B H675 109.5 . . ? H674 C67B H675 109.5 . . ? O42B C67B H676 109.5 . . ? H674 C67B H676 109.5 . . ? H675 C67B H676 109.5 . . ? C47 N41 C51 118.9(4) . . ? C47 N41 Zn41 126.6(3) . . ? C51 N41 Zn41 113.4(3) . . ? C52 N42 C56 121.4(4) . . ? C52 N42 Zn41 118.8(3) . . ? C56 N42 Zn41 119.3(3) . . ? C61 N43 C57 118.7(4) . . ? C61 N43 Zn41 125.3(3) . . ? C57 N43 Zn41 115.0(3) . . ? O41 C41 H411 109.5 . . ? O41 C41 H412 109.5 . . ? H411 C41 H412 109.5 . . ? O41 C41 H413 109.5 . . ? H411 C41 H413 109.5 . . ? H412 C41 H413 109.5 . . ? O41 C42 C73 124.5(5) . . ? O41 C42 C43 115.9(5) . . ? C73 C42 C43 119.6(5) . . ? C44 C43 C42 121.4(5) . . ? C44 C43 H43 119.3 . . ? C42 C43 H43 119.3 . . ? C43 C44 C46 119.2(5) . . ? C43 C44 C45 118.1(5) . . ? C46 C44 C45 122.7(5) . . ? C44 C45 H451 109.5 . . ? C44 C45 H452 109.5 . . ? H451 C45 H452 109.5 . . ? C44 C45 H453 109.5 . . ? H451 C45 H453 109.5 . . ? H452 C45 H453 109.5 . . ? C72 C46 C44 119.2(5) . . ? C72 C46 C48 121.1(4) . . ? C44 C46 C48 119.7(5) . . ? N41 C47 C48 123.9(5) . . ? N41 C47 H47 118.0 . . ? C48 C47 H47 118.0 . . ? C49 C48 C47 116.3(5) . . ? C49 C48 C46 121.9(5) . . ? C47 C48 C46 121.8(4) . . ? C50 C49 C48 120.5(5) . . ? C50 C49 H49 119.8 . . ? C48 C49 H49 119.8 . . ? C51 C50 C49 119.2(5) . . ? C51 C50 H50 120.4 . . ? C49 C50 H50 120.4 . . ? N41 C51 C50 121.1(5) . . ? N41 C51 C52 114.9(4) . . ? C50 C51 C52 124.0(5) . . ? N42 C52 C53 120.4(5) . . ? N42 C52 C51 114.6(4) . . ? C53 C52 C51 124.9(5) . . ? C52 C53 C54 118.6(6) . . ? C52 C53 H531 120.7 . . ? C54 C53 H531 120.7 . . ? C53 C54 C55 120.8(6) . . ? C53 C54 H54 119.6 . . ? C55 C54 H54 119.6 . . ? C54 C55 C56 118.5(6) . . ? C54 C55 H55 120.8 . . ? C56 C55 H55 120.8 . . ? N42 C56 C55 120.2(5) . . ? N42 C56 C57 114.3(4) . . ? C55 C56 C57 125.4(5) . . ? N43 C57 C58 121.1(5) . . ? N43 C57 C56 114.7(4) . . ? C58 C57 C56 124.0(5) . . ? C59 C58 C57 119.0(5) . . ? C59 C58 H58 120.5 . . ? C57 C58 H58 120.5 . . ? C58 C59 C60 121.1(5) . . ? C58 C59 H59 119.4 . . ? C60 C59 H59 119.4 . . ? C59 C60 C61 115.8(5) . . ? C59 C60 C62 123.9(5) . . ? C61 C60 C62 120.3(5) . . ? N43 C61 C60 124.1(5) . . ? N43 C61 H61 117.9 . . ? C60 C61 H61 117.9 . . ? C69 C62 C63 119.3(5) . . ? C69 C62 C60 120.1(5) . . ? C63 C62 C60 120.5(5) . . ? C65 C63 C62 119.1(6) . . ? C65 C63 C64 119.2(5) . . ? C62 C63 C64 121.7(5) . . ? C63 C64 H641 109.5 . . ? C63 C64 H642 109.5 . . ? H641 C64 H642 109.5 . . ? C63 C64 H643 109.5 . . ? H641 C64 H643 109.5 . . ? H642 C64 H643 109.5 . . ? C66 C65 C63 121.4(6) . . ? C66 C65 H65 119.3 . . ? C63 C65 H65 119.3 . . ? C68 C66 C65 119.8(6) . . ? C68 C66 O42A 136.9(8) . . ? C65 C66 O42A 102.7(8) . . ? C68 C66 O42B 108.8(6) . . ? C65 C66 O42B 131.3(7) . . ? C66 C68 C69 120.7(6) . . ? C66 C68 H68 119.7 . . ? C69 C68 H68 119.7 . . ? C68 C69 C62 119.7(6) . . ? C68 C69 C70 117.6(5) . . ? C62 C69 C70 122.6(5) . . ? C69 C70 H701 109.5 . . ? C69 C70 H702 109.5 . . ? H701 C70 H702 109.5 . . ? C69 C70 H703 109.5 . . ? H701 C70 H703 109.5 . . ? H702 C70 H703 109.5 . . ? C72 C71 H711 109.5 . . ? C72 C71 H712 109.5 . . ? H711 C71 H712 109.5 . . ? C72 C71 H713 109.5 . . ? H711 C71 H713 109.5 . . ? H712 C71 H713 109.5 . . ? C73 C72 C46 119.9(5) . . ? C73 C72 C71 117.7(5) . . ? C46 C72 C71 122.4(5) . . ? C42 C73 C72 120.6(5) . . ? C42 C73 H73 119.7 . . ? C72 C73 H73 119.7 . . ? N74 C75 C76 177(3) . . ? C75 C76 H761 109.5 . . ? C75 C76 H762 109.5 . . ? H761 C76 H762 109.5 . . ? C75 C76 H763 109.5 . . ? H761 C76 H763 109.5 . . ? H762 C76 H763 109.5 . . ? N77 C78 C79 180.00 . . ? N80 C81 C82 176.1(14) . . ? N83 C84 C85 176.1(12) . . ? N86 C87 C88 172(4) . . ? C87 C88 H881 109.5 . . ? C87 C88 H882 109.5 . . ? H881 C88 H882 109.5 . . ? C87 C88 H883 109.5 . . ? H881 C88 H883 109.5 . . ? H882 C88 H883 109.5 . . ? F2A P1 F3A 94.1(4) . . ? F5B P1 F4B 94.7(5) . . ? F2A P1 F6A 91.7(4) . . ? F3A P1 F6A 92.5(4) . . ? F5B P1 F1B 92.5(5) . . ? F4B P1 F1B 92.4(5) . . ? F5B P1 F2B 91.5(5) . . ? F4B P1 F2B 90.3(5) . . ? F1B P1 F2B 175.0(6) . . ? F2A P1 F5A 92.1(3) . . ? F3A P1 F5A 89.7(3) . . ? F6A P1 F5A 175.4(4) . . ? F2A P1 F4A 90.5(4) . . ? F3A P1 F4A 174.7(5) . . ? F6A P1 F4A 89.8(3) . . ? F5A P1 F4A 87.7(4) . . ? F5B P1 F3B 90.2(4) . . ? F4B P1 F3B 174.9(5) . . ? F1B P1 F3B 88.8(5) . . ? F2B P1 F3B 88.2(5) . . ? F2A P1 F1A 176.5(4) . . ? F3A P1 F1A 89.2(4) . . ? F6A P1 F1A 89.0(3) . . ? F5A P1 F1A 87.0(4) . . ? F4A P1 F1A 86.1(4) . . ? F5B P1 F6B 176.6(5) . . ? F4B P1 F6B 88.5(4) . . ? F1B P1 F6B 88.6(5) . . ? F2B P1 F6B 87.2(5) . . ? F3B P1 F6B 86.6(5) . . ? F7B P2 F9B 95.6(4) . . ? F7B P2 F12B 93.9(4) . . ? F9B P2 F12B 93.9(4) . . ? F8A P2 F10A 95.3(4) . . ? F8A P2 F11A 94.1(4) . . ? F10A P2 F11A 90.7(4) . . ? F8A P2 F9A 92.6(4) . . ? F10A P2 F9A 172.1(5) . . ? F11A P2 F9A 88.8(4) . . ? F8A P2 F12A 92.4(4) . . ? F10A P2 F12A 91.9(4) . . ? F11A P2 F12A 172.7(5) . . ? F9A P2 F12A 87.6(4) . . ? F7B P2 F10B 94.1(3) . . ? F9B P2 F10B 170.1(5) . . ? F12B P2 F10B 87.6(3) . . ? F7B P2 F11B 90.7(4) . . ? F9B P2 F11B 90.9(4) . . ? F12B P2 F11B 173.0(5) . . ? F10B P2 F11B 86.8(4) . . ? F7B P2 F8B 176.6(4) . . ? F9B P2 F8B 85.7(4) . . ? F12B P2 F8B 89.2(4) . . ? F10B P2 F8B 84.6(4) . . ? F11B P2 F8B 86.1(4) . . ? F8A P2 F7A 177.3(4) . . ? F10A P2 F7A 86.7(4) . . ? F11A P2 F7A 87.6(4) . . ? F9A P2 F7A 85.4(4) . . ? F12A P2 F7A 85.8(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Zn1 N1 C7 -175.9(4) . . . . ? N2 Zn1 N1 C7 7.5(5) 2 . . . ? N1 Zn1 N1 C7 -67.2(4) 2 . . . ? N3 Zn1 N1 C7 -174.0(4) . . . . ? N3 Zn1 N1 C7 85.5(4) 2 . . . ? N2 Zn1 N1 C11 -5.1(4) . . . . ? N2 Zn1 N1 C11 178.3(4) 2 . . . ? N1 Zn1 N1 C11 103.6(4) 2 . . . ? N3 Zn1 N1 C11 -3.2(6) . . . . ? N3 Zn1 N1 C11 -103.7(4) 2 . . . ? N2 Zn1 N2 C16 -35.4(4) 2 . . . ? N1 Zn1 N2 C16 102.5(4) 2 . . . ? N1 Zn1 N2 C16 -174.1(4) . . . . ? N3 Zn1 N2 C16 6.8(4) . . . . ? N3 Zn1 N2 C16 -76.8(4) 2 . . . ? N2 Zn1 N2 C12 139.7(4) 2 . . . ? N1 Zn1 N2 C12 -82.5(4) 2 . . . ? N1 Zn1 N2 C12 0.9(4) . . . . ? N3 Zn1 N2 C12 -178.2(4) . . . . ? N3 Zn1 N2 C12 98.3(4) 2 . . . ? N2 Zn1 N3 C21 -178.0(4) . . . . ? N2 Zn1 N3 C21 -1.3(4) 2 . . . ? N1 Zn1 N3 C21 76.1(4) 2 . . . ? N1 Zn1 N3 C21 -179.9(4) . . . . ? N3 Zn1 N3 C21 -76.1(4) 2 . . . ? N2 Zn1 N3 C17 -9.1(3) . . . . ? N2 Zn1 N3 C17 167.6(3) 2 . . . ? N1 Zn1 N3 C17 -115.0(3) 2 . . . ? N1 Zn1 N3 C17 -11.0(5) . . . . ? N3 Zn1 N3 C17 92.8(3) 2 . . . ? C1 O1 C2 C33 -3.7(8) . . . . ? C1 O1 C2 C3 176.6(5) . . . . ? O1 C2 C3 C4 179.9(5) . . . . ? C33 C2 C3 C4 0.2(8) . . . . ? C2 C3 C4 C6 -0.5(8) . . . . ? C2 C3 C4 C5 177.2(5) . . . . ? C3 C4 C6 C32 0.3(8) . . . . ? C5 C4 C6 C32 -177.3(5) . . . . ? C3 C4 C6 C8 177.9(5) . . . . ? C5 C4 C6 C8 0.3(8) . . . . ? C11 N1 C7 C8 0.0(8) . . . . ? Zn1 N1 C7 C8 170.4(4) . . . . ? N1 C7 C8 C9 0.5(8) . . . . ? N1 C7 C8 C6 179.5(5) . . . . ? C32 C6 C8 C7 57.8(7) . . . . ? C4 C6 C8 C7 -119.8(6) . . . . ? C32 C6 C8 C9 -123.3(6) . . . . ? C4 C6 C8 C9 59.2(8) . . . . ? C7 C8 C9 C10 -0.5(9) . . . . ? C6 C8 C9 C10 -179.5(6) . . . . ? C8 C9 C10 C11 0.0(9) . . . . ? C7 N1 C11 C10 -0.5(8) . . . . ? Zn1 N1 C11 C10 -171.8(4) . . . . ? C7 N1 C11 C12 179.6(5) . . . . ? Zn1 N1 C11 C12 8.3(6) . . . . ? C9 C10 C11 N1 0.5(9) . . . . ? C9 C10 C11 C12 -179.6(5) . . . . ? C16 N2 C12 C13 -1.8(8) . . . . ? Zn1 N2 C12 C13 -176.7(4) . . . . ? C16 N2 C12 C11 178.0(4) . . . . ? Zn1 N2 C12 C11 3.1(6) . . . . ? N1 C11 C12 N2 -7.5(7) . . . . ? C10 C11 C12 N2 172.5(5) . . . . ? N1 C11 C12 C13 172.2(5) . . . . ? C10 C11 C12 C13 -7.7(9) . . . . ? N2 C12 C13 C14 2.3(8) . . . . ? C11 C12 C13 C14 -177.5(5) . . . . ? C12 C13 C14 C15 -1.4(9) . . . . ? C13 C14 C15 C16 0.1(9) . . . . ? C12 N2 C16 C15 0.4(7) . . . . ? Zn1 N2 C16 C15 175.3(4) . . . . ? C12 N2 C16 C17 -178.6(4) . . . . ? Zn1 N2 C16 C17 -3.7(6) . . . . ? C14 C15 C16 N2 0.4(8) . . . . ? C14 C15 C16 C17 179.4(5) . . . . ? C21 N3 C17 C18 1.8(7) . . . . ? Zn1 N3 C17 C18 -167.9(4) . . . . ? C21 N3 C17 C16 179.7(4) . . . . ? Zn1 N3 C17 C16 10.0(5) . . . . ? N2 C16 C17 N3 -4.5(6) . . . . ? C15 C16 C17 N3 176.5(5) . . . . ? N2 C16 C17 C18 173.4(5) . . . . ? C15 C16 C17 C18 -5.6(8) . . . . ? N3 C17 C18 C19 -0.6(7) . . . . ? C16 C17 C18 C19 -178.3(5) . . . . ? C17 C18 C19 C20 -0.3(8) . . . . ? C18 C19 C20 C21 0.0(7) . . . . ? C18 C19 C20 C22 180.0(5) . . . . ? C17 N3 C21 C20 -2.2(7) . . . . ? Zn1 N3 C21 C20 166.3(4) . . . . ? C19 C20 C21 N3 1.4(7) . . . . ? C22 C20 C21 N3 -178.7(4) . . . . ? C21 C20 C22 C23 -122.8(5) . . . . ? C19 C20 C22 C23 57.2(7) . . . . ? C21 C20 C22 C29 57.5(7) . . . . ? C19 C20 C22 C29 -122.5(5) . . . . ? C29 C22 C23 C25 1.8(7) . . . . ? C20 C22 C23 C25 -177.9(5) . . . . ? C29 C22 C23 C24 -175.2(5) . . . . ? C20 C22 C23 C24 5.1(7) . . . . ? C22 C23 C25 C26 -0.5(8) . . . . ? C24 C23 C25 C26 176.7(5) . . . . ? C27B O2B C26 C25 3.1(18) . . . . ? C27B O2B C26 C28 178.0(11) . . . . ? C27A O2A C26 C25 10(4) . . . . ? C27A O2A C26 C28 -163(3) . . . . ? C23 C25 C26 O2B 173.6(12) . . . . ? C23 C25 C26 O2A -174(2) . . . . ? C23 C25 C26 C28 -1.2(8) . . . . ? O2B C26 C28 C29 -173.7(11) . . . . ? O2A C26 C28 C29 175(2) . . . . ? C25 C26 C28 C29 1.5(8) . . . . ? C26 C28 C29 C22 -0.2(8) . . . . ? C26 C28 C29 C30 179.1(5) . . . . ? C23 C22 C29 C28 -1.5(7) . . . . ? C20 C22 C29 C28 178.3(5) . . . . ? C23 C22 C29 C30 179.3(5) . . . . ? C20 C22 C29 C30 -1.0(7) . . . . ? C4 C6 C32 C33 0.2(8) . . . . ? C8 C6 C32 C33 -177.4(5) . . . . ? C4 C6 C32 C31 -179.4(6) . . . . ? C8 C6 C32 C31 3.0(8) . . . . ? O1 C2 C33 C32 -179.4(5) . . . . ? C3 C2 C33 C32 0.3(8) . . . . ? C6 C32 C33 C2 -0.5(8) . . . . ? C31 C32 C33 C2 179.1(5) . . . . ? N42 Zn41 N41 C47 177.5(4) . . . . ? N42 Zn41 N41 C47 -1.0(4) 2_655 . . . ? N43 Zn41 N41 C47 -78.4(4) 2_655 . . . ? N43 Zn41 N41 C47 -175.8(4) . . . . ? N41 Zn41 N41 C47 75.2(4) 2_655 . . . ? N42 Zn41 N41 C51 9.9(3) . . . . ? N42 Zn41 N41 C51 -168.6(3) 2_655 . . . ? N43 Zn41 N41 C51 114.0(3) 2_655 . . . ? N43 Zn41 N41 C51 16.6(5) . . . . ? N41 Zn41 N41 C51 -92.4(3) 2_655 . . . ? N42 Zn41 N42 C52 41.7(4) 2_655 . . . ? N43 Zn41 N42 C52 -97.2(4) 2_655 . . . ? N43 Zn41 N42 C52 -179.0(4) . . . . ? N41 Zn41 N42 C52 85.3(4) 2_655 . . . ? N41 Zn41 N42 C52 -2.2(4) . . . . ? N42 Zn41 N42 C56 -145.8(4) 2_655 . . . ? N43 Zn41 N42 C56 75.3(4) 2_655 . . . ? N43 Zn41 N42 C56 -6.5(4) . . . . ? N41 Zn41 N42 C56 -102.2(4) 2_655 . . . ? N41 Zn41 N42 C56 170.3(4) . . . . ? N42 Zn41 N43 C61 175.5(4) . . . . ? N42 Zn41 N43 C61 -5.9(4) 2_655 . . . ? N43 Zn41 N43 C61 68.4(4) 2_655 . . . ? N41 Zn41 N43 C61 -84.1(4) 2_655 . . . ? N41 Zn41 N43 C61 168.7(4) . . . . ? N42 Zn41 N43 C57 6.9(3) . . . . ? N42 Zn41 N43 C57 -174.5(3) 2_655 . . . ? N43 Zn41 N43 C57 -100.1(3) 2_655 . . . ? N41 Zn41 N43 C57 107.4(3) 2_655 . . . ? N41 Zn41 N43 C57 0.2(5) . . . . ? C41 O41 C42 C73 1.3(8) . . . . ? C41 O41 C42 C43 -178.0(5) . . . . ? O41 C42 C43 C44 -178.7(5) . . . . ? C73 C42 C43 C44 2.0(8) . . . . ? C42 C43 C44 C46 0.7(8) . . . . ? C42 C43 C44 C45 -177.3(5) . . . . ? C43 C44 C46 C72 -3.0(7) . . . . ? C45 C44 C46 C72 174.9(5) . . . . ? C43 C44 C46 C48 176.0(5) . . . . ? C45 C44 C46 C48 -6.0(7) . . . . ? C51 N41 C47 C48 1.3(7) . . . . ? Zn41 N41 C47 C48 -165.7(4) . . . . ? N41 C47 C48 C49 2.0(7) . . . . ? N41 C47 C48 C46 -178.1(5) . . . . ? C72 C46 C48 C49 122.9(6) . . . . ? C44 C46 C48 C49 -56.2(7) . . . . ? C72 C46 C48 C47 -57.0(7) . . . . ? C44 C46 C48 C47 124.0(5) . . . . ? C47 C48 C49 C50 -3.3(7) . . . . ? C46 C48 C49 C50 176.8(5) . . . . ? C48 C49 C50 C51 1.5(8) . . . . ? C47 N41 C51 C50 -3.3(7) . . . . ? Zn41 N41 C51 C50 165.3(4) . . . . ? C47 N41 C51 C52 175.8(4) . . . . ? Zn41 N41 C51 C52 -15.5(5) . . . . ? C49 C50 C51 N41 2.0(8) . . . . ? C49 C50 C51 C52 -177.1(5) . . . . ? C56 N42 C52 C53 -0.2(8) . . . . ? Zn41 N42 C52 C53 172.1(5) . . . . ? C56 N42 C52 C51 -177.5(4) . . . . ? Zn41 N42 C52 C51 -5.2(6) . . . . ? N41 C51 C52 N42 14.0(7) . . . . ? C50 C51 C52 N42 -166.8(5) . . . . ? N41 C51 C52 C53 -163.1(6) . . . . ? C50 C51 C52 C53 16.0(9) . . . . ? N42 C52 C53 C54 0.8(10) . . . . ? C51 C52 C53 C54 177.8(6) . . . . ? C52 C53 C54 C55 -0.6(12) . . . . ? C53 C54 C55 C56 -0.1(12) . . . . ? C52 N42 C56 C55 -0.5(8) . . . . ? Zn41 N42 C56 C55 -172.8(4) . . . . ? C52 N42 C56 C57 177.4(4) . . . . ? Zn41 N42 C56 C57 5.1(6) . . . . ? C54 C55 C56 N42 0.6(10) . . . . ? C54 C55 C56 C57 -177.1(6) . . . . ? C61 N43 C57 C58 0.1(7) . . . . ? Zn41 N43 C57 C58 169.5(4) . . . . ? C61 N43 C57 C56 -175.8(4) . . . . ? Zn41 N43 C57 C56 -6.4(5) . . . . ? N42 C56 C57 N43 1.2(6) . . . . ? C55 C56 C57 N43 179.0(5) . . . . ? N42 C56 C57 C58 -174.6(5) . . . . ? C55 C56 C57 C58 3.2(9) . . . . ? N43 C57 C58 C59 -1.9(8) . . . . ? C56 C57 C58 C59 173.6(5) . . . . ? C57 C58 C59 C60 1.6(8) . . . . ? C58 C59 C60 C61 0.5(8) . . . . ? C58 C59 C60 C62 -176.8(5) . . . . ? C57 N43 C61 C60 2.1(7) . . . . ? Zn41 N43 C61 C60 -166.1(4) . . . . ? C59 C60 C61 N43 -2.4(7) . . . . ? C62 C60 C61 N43 175.0(5) . . . . ? C59 C60 C62 C69 119.1(6) . . . . ? C61 C60 C62 C69 -58.1(7) . . . . ? C59 C60 C62 C63 -63.0(7) . . . . ? C61 C60 C62 C63 119.8(6) . . . . ? C69 C62 C63 C65 -0.4(8) . . . . ? C60 C62 C63 C65 -178.3(5) . . . . ? C69 C62 C63 C64 176.8(5) . . . . ? C60 C62 C63 C64 -1.1(8) . . . . ? C62 C63 C65 C66 0.1(9) . . . . ? C64 C63 C65 C66 -177.1(6) . . . . ? C63 C65 C66 C68 0.0(9) . . . . ? C63 C65 C66 O42A -172.9(9) . . . . ? C63 C65 C66 O42B 179.1(7) . . . . ? C67A O42A C66 C68 23(2) . . . . ? C67A O42A C66 C65 -166.3(13) . . . . ? C67B O42B C66 C68 160.2(8) . . . . ? C67B O42B C66 C65 -18.9(13) . . . . ? C65 C66 C68 C69 0.1(9) . . . . ? O42A C66 C68 C69 170.0(12) . . . . ? O42B C66 C68 C69 -179.2(7) . . . . ? C66 C68 C69 C62 -0.4(9) . . . . ? C66 C68 C69 C70 179.9(6) . . . . ? C63 C62 C69 C68 0.5(8) . . . . ? C60 C62 C69 C68 178.4(5) . . . . ? C63 C62 C69 C70 -179.8(6) . . . . ? C60 C62 C69 C70 -1.9(9) . . . . ? C44 C46 C72 C73 2.7(7) . . . . ? C48 C46 C72 C73 -176.4(5) . . . . ? C44 C46 C72 C71 -178.5(5) . . . . ? C48 C46 C72 C71 2.4(8) . . . . ? O41 C42 C73 C72 178.4(5) . . . . ? C43 C42 C73 C72 -2.3(8) . . . . ? C46 C72 C73 C42 0.0(8) . . . . ? C71 C72 C73 C42 -178.8(5) . . . . ? #===END data_8b _database_code_depnum_ccdc_archive 'CCDC 735262' # SG0404 _audit_creation_method SHELXL-97 _audit_creation_date 04-02-27 _chemical_name_systematic ; bis[5,5"-bis-(4-methoxy-2,6-dimethylphenyl)- [2,2':6,2"]terpyridine]ruthenium(II) hexafluorophosphate hexa-acetonitrile solvate ; _chemical_name_common ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_moiety 'C66 H62 N6 O4 Ru 2+, 2(F6 P 1-), 6(C2 H3 N)' _chemical_formula_sum 'C78 H80 F12 N12 O4 P2 Ru' _chemical_formula_weight 1640.49 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 312 0.0033 0.0016 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; H H 320 0.0000 0.0000 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; F F 48 0.0171 0.0103 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; N N 48 0.0061 0.0033 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; O O 16 0.0106 0.0060 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; P P 8 0.1023 0.0942 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; Ru Ru 4 -1.2594 0.8363 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall ? _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 29.4883(4) _cell_length_b 11.8087(1) _cell_length_c 22.4060(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.9353(6) _cell_angle_gamma 90.00 _cell_volume 7801.14(16) _cell_formula_units_Z 4 _cell_measurement_temperature 160(1) _cell_measurement_reflns_used 103846 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 30.0 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.397 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3384 _exptl_absorpt_coefficient_mu 0.328 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Blessing, 1995)' _exptl_absorpt_correction_T_min 0.614 _exptl_absorpt_correction_T_max 0.885 _exptl_special_details ; Solvent used: MeCN / diethylether Cooling Device: Oxford Cryosystems Cryostream 700 Crystal mount: glued on a glass fibre Mosaicity (deg.): 0.554(1) Frames collected: 650 Seconds exposure per frame: 14 Degrees rotation per frame: 1.2 Crystal-Detector distance (mm): 33.6 ; _diffrn_ambient_temperature 160(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Nonius FR590 sealed tube generator' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_detector '65 mm CCD camera on \k goniostat' _diffrn_measurement_device_type 'Nonius KappaCCD area-detector diffractometer' _diffrn_measurement_method '\f and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 94623 _diffrn_reflns_av_R_equivalents 0.0843 _diffrn_reflns_av_sigmaI/netI 0.0449 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 30.04 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.04 _diffrn_measured_fraction_theta_full 0.999 _reflns_number_total 11431 _reflns_number_gt 8995 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'COLLECT (Nonius, 2000)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN and SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'SHELXL97 and PLATON (Spek, 2009)' _refine_special_details ; The asymmetric unit contains one half of a cation with the Ru-atom on a two-fold axis, one anion and three acetonitrile molecules. The PF6- anion is disordered. Two sets of P- and F-atoms were defined for this anion and refinement of the site occupation factors led to a value of 0.846(3), for the major orientation. The P-F and F...F distances were restrained tightly, so as to maintain octahedral geometry and uniform P-F bond lengths and neighbouring atoms within and between each disordered orientation were restrained to have similar atomic displacement parameters. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0549P)^2^+9.1532P] 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_extinction_coef ? _refine_ls_number_reflns 11428 _refine_ls_number_parameters 565 _refine_ls_number_restraints 561 _refine_ls_R_factor_all 0.0648 _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_ref 0.1174 _refine_ls_wR_factor_gt 0.1056 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.594 _refine_diff_density_min -0.823 _refine_diff_density_rms 0.075 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 Ru Ru 0.5000 0.202213(17) 0.7500 0.02080(7) Uani 1 2 d S . . O1 O 0.49286(6) 0.75101(15) 1.05108(7) 0.0384(4) Uani 1 1 d . . . O2 O 0.27827(7) -0.34480(17) 0.65531(10) 0.0585(5) Uani 1 1 d . . . N1 N 0.53789(5) 0.32917(13) 0.78941(7) 0.0233(3) Uani 1 1 d . . . N2 N 0.55419(5) 0.20125(13) 0.69956(7) 0.0224(3) Uani 1 1 d . . . N3 N 0.48283(5) 0.07517(13) 0.69084(7) 0.0223(3) Uani 1 1 d . . . C1 C 0.44840(9) 0.7971(2) 1.05146(11) 0.0425(5) Uani 1 1 d . . . H11 H 0.4444 0.8487 1.0175 0.064 Uiso 1 1 calc R . . H12 H 0.4440 0.8388 1.0887 0.064 Uiso 1 1 calc R . . H13 H 0.4261 0.7357 1.0484 0.064 Uiso 1 1 calc R . . C2 C 0.50384(8) 0.68552(17) 1.00286(9) 0.0299(4) Uani 1 1 d . . . C3 C 0.54710(8) 0.63980(18) 1.00389(9) 0.0323(4) Uani 1 1 d . . . H3 H 0.5665 0.6532 1.0374 0.039 Uiso 1 1 calc R . . C4 C 0.56254(7) 0.57486(17) 0.95689(9) 0.0305(4) Uani 1 1 d . . . C5 C 0.60931(8) 0.5233(2) 0.96258(11) 0.0392(5) Uani 1 1 d . . . H51 H 0.6309 0.5694 0.9403 0.059 Uiso 1 1 calc R . . H52 H 0.6088 0.4462 0.9463 0.059 Uiso 1 1 calc R . . H53 H 0.6186 0.5208 1.0048 0.059 Uiso 1 1 calc R . . C6 C 0.53376(7) 0.55562(16) 0.90696(9) 0.0277(4) Uani 1 1 d . . . C7 C 0.52590(7) 0.39307(16) 0.83612(9) 0.0250(4) Uani 1 1 d . . . H7 H 0.4995 0.3724 0.8572 0.030 Uiso 1 1 calc R . . C8 C 0.55003(7) 0.48808(16) 0.85532(9) 0.0270(4) Uani 1 1 d . . . C9 C 0.58888(7) 0.51540(18) 0.82367(10) 0.0324(4) Uani 1 1 d . . . H9 H 0.6063 0.5799 0.8349 0.039 Uiso 1 1 calc R . . C10 C 0.60224(7) 0.44936(18) 0.77621(10) 0.0313(4) Uani 1 1 d . . . H10 H 0.6290 0.4678 0.7553 0.038 Uiso 1 1 calc R . . C11 C 0.57649(7) 0.35590(17) 0.75912(9) 0.0263(4) Uani 1 1 d . . . C12 C 0.58699(7) 0.27922(17) 0.70927(9) 0.0266(4) Uani 1 1 d . . . C13 C 0.62540(7) 0.27966(19) 0.67406(10) 0.0339(5) Uani 1 1 d . . . H131 H 0.6485 0.3348 0.6800 0.041 Uiso 1 1 calc R . . C14 C 0.62914(7) 0.1975(2) 0.63006(11) 0.0374(5) Uani 1 1 d . . . H14 H 0.6551 0.1969 0.6054 0.045 Uiso 1 1 calc R . . C15 C 0.59555(7) 0.11625(19) 0.62153(10) 0.0325(4) Uani 1 1 d . . . H15 H 0.5987 0.0591 0.5920 0.039 Uiso 1 1 calc R . . C16 C 0.55746(6) 0.12011(17) 0.65683(9) 0.0254(4) Uani 1 1 d . . . C17 C 0.51746(6) 0.04583(17) 0.65353(8) 0.0249(4) Uani 1 1 d . . . C18 C 0.51319(7) -0.04805(18) 0.61687(9) 0.0302(4) Uani 1 1 d . . . H18 H 0.5374 -0.0693 0.5918 0.036 Uiso 1 1 calc R . . C19 C 0.47353(7) -0.11118(18) 0.61671(9) 0.0310(4) Uani 1 1 d . . . H19 H 0.4709 -0.1762 0.5920 0.037 Uiso 1 1 calc R . . C20 C 0.43765(7) -0.07958(16) 0.65264(9) 0.0259(4) Uani 1 1 d . . . C21 C 0.44417(6) 0.01486(16) 0.68899(8) 0.0235(4) Uani 1 1 d . . . H21 H 0.4200 0.0379 0.7138 0.028 Uiso 1 1 calc R . . C22 C 0.39398(7) -0.14399(16) 0.65318(9) 0.0275(4) Uani 1 1 d . . . C23 C 0.36943(7) -0.16085(18) 0.59983(10) 0.0331(4) Uani 1 1 d . . . C24 C 0.38301(9) -0.1080(2) 0.54144(11) 0.0435(6) Uani 1 1 d . . . H241 H 0.3932 -0.0301 0.5485 0.065 Uiso 1 1 calc R . . H242 H 0.3569 -0.1075 0.5138 0.065 Uiso 1 1 calc R . . H243 H 0.4077 -0.1521 0.5241 0.065 Uiso 1 1 calc R . . C25 C 0.33008(8) -0.22663(19) 0.59973(12) 0.0387(5) Uani 1 1 d . . . H25 H 0.3135 -0.2382 0.5635 0.046 Uiso 1 1 calc R . . C26 C 0.31515(8) -0.2748(2) 0.65189(13) 0.0419(6) Uani 1 1 d . . . C27 C 0.25778(10) -0.3802(3) 0.59952(17) 0.0645(9) Uani 1 1 d . . . H271 H 0.2443 -0.3145 0.5792 0.097 Uiso 1 1 calc R . . H272 H 0.2341 -0.4364 0.6072 0.097 Uiso 1 1 calc R . . H273 H 0.2810 -0.4138 0.5742 0.097 Uiso 1 1 calc R . . C28 C 0.33836(8) -0.2551(2) 0.70535(12) 0.0402(5) Uani 1 1 d . . . H28 H 0.3271 -0.2858 0.7414 0.048 Uiso 1 1 calc R . . C29 C 0.37791(8) -0.19088(17) 0.70680(10) 0.0334(5) Uani 1 1 d . . . C30 C 0.40316(10) -0.1776(2) 0.76532(11) 0.0463(6) Uani 1 1 d . . . H301 H 0.3986 -0.1008 0.7807 0.070 Uiso 1 1 calc R . . H302 H 0.4356 -0.1907 0.7593 0.070 Uiso 1 1 calc R . . H303 H 0.3917 -0.2328 0.7941 0.070 Uiso 1 1 calc R . . C31 C 0.45609(8) 0.5821(2) 0.85588(11) 0.0419(6) Uani 1 1 d . . . H311 H 0.4415 0.5080 0.8599 0.063 Uiso 1 1 calc R . . H312 H 0.4721 0.5853 0.8179 0.063 Uiso 1 1 calc R . . H313 H 0.4330 0.6418 0.8567 0.063 Uiso 1 1 calc R . . C32 C 0.48950(7) 0.59926(17) 0.90686(9) 0.0286(4) Uani 1 1 d . . . C33 C 0.47496(7) 0.66428(18) 0.95484(9) 0.0289(4) Uani 1 1 d . . . H33 H 0.4451 0.6942 0.9546 0.035 Uiso 1 1 calc R . . C34 C 0.20659(11) 0.5147(3) 0.73969(18) 0.0749(10) Uani 1 1 d . . . H341 H 0.2100 0.5943 0.7284 0.112 Uiso 1 1 calc R . . H342 H 0.1859 0.5089 0.7734 0.112 Uiso 1 1 calc R . . H343 H 0.1941 0.4719 0.7057 0.112 Uiso 1 1 calc R . . C35 C 0.24999(12) 0.4691(4) 0.75660(16) 0.0745(10) Uani 1 1 d . . . N36 N 0.28400(13) 0.4341(5) 0.76968(18) 0.1240(17) Uani 1 1 d . . . C37 C 0.19399(11) 0.8259(3) 0.88432(16) 0.0637(8) Uani 1 1 d . . . H371 H 0.2257 0.8085 0.8758 0.096 Uiso 1 1 calc R . . H372 H 0.1896 0.8255 0.9276 0.096 Uiso 1 1 calc R . . H373 H 0.1863 0.9007 0.8683 0.096 Uiso 1 1 calc R . . C38 C 0.16499(10) 0.7414(3) 0.85670(14) 0.0522(7) Uani 1 1 d . . . N39 N 0.14230(11) 0.6766(3) 0.83485(16) 0.0764(8) Uani 1 1 d . . . C40 C 0.24578(13) 0.5350(3) 0.92107(19) 0.0784(10) Uani 1 1 d . . . H401 H 0.2622 0.5895 0.8966 0.118 Uiso 1 1 calc R . . H402 H 0.2360 0.5719 0.9579 0.118 Uiso 1 1 calc R . . H403 H 0.2191 0.5074 0.8988 0.118 Uiso 1 1 calc R . . C41 C 0.27510(11) 0.4410(3) 0.93577(16) 0.0625(8) Uani 1 1 d . . . N42 N 0.29778(11) 0.3668(3) 0.94781(17) 0.0856(10) Uani 1 1 d . . . P1A P 0.33532(3) 0.81477(7) 0.93595(4) 0.0362(2) Uani 0.846(3) 1 d PDU A 1 F1A F 0.38495(5) 0.83861(17) 0.91313(8) 0.0719(10) Uani 0.846(3) 1 d PDU A 1 F2A F 0.28577(4) 0.79134(16) 0.95902(8) 0.0694(7) Uani 0.846(3) 1 d PDU A 1 F3A F 0.31885(6) 0.7893(2) 0.86984(6) 0.0813(8) Uani 0.846(3) 1 d PDU A 1 F4A F 0.35178(6) 0.84049(19) 1.00228(6) 0.0742(7) Uani 0.846(3) 1 d PDU A 1 F5A F 0.32308(6) 0.94436(11) 0.92718(10) 0.0865(9) Uani 0.846(3) 1 d PDU A 1 F6A F 0.34772(6) 0.68557(11) 0.94497(11) 0.0869(9) Uani 0.846(3) 1 d PDU A 1 P1B P 0.33623(18) 0.8144(4) 0.9279(2) 0.0564(15) Uani 0.154(3) 1 d PDU A 2 F1B F 0.3876(2) 0.8408(7) 0.9141(4) 0.041(3) Uani 0.154(3) 1 d PDU A 2 F2B F 0.28484(19) 0.7881(8) 0.9417(4) 0.069(3) Uani 0.154(3) 1 d PDU A 2 F3B F 0.3214(3) 0.8713(9) 0.8667(3) 0.078(3) Uani 0.154(3) 1 d PDU A 2 F4B F 0.3511(3) 0.7576(9) 0.9891(3) 0.072(2) Uani 0.154(3) 1 d PDU A 2 F5B F 0.3319(3) 0.9329(6) 0.9604(4) 0.075(3) Uani 0.154(3) 1 d PDU A 2 F6B F 0.3405(3) 0.6960(6) 0.8955(5) 0.079(3) Uani 0.154(3) 1 d PDU A 2 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 Ru 0.01745(11) 0.02182(11) 0.02322(11) 0.000 0.00365(7) 0.000 O1 0.0414(9) 0.0450(9) 0.0287(8) -0.0070(7) -0.0027(7) -0.0005(7) O2 0.0408(11) 0.0511(11) 0.0838(15) -0.0044(10) 0.0052(10) -0.0197(9) N1 0.0202(8) 0.0225(7) 0.0271(8) 0.0025(6) 0.0012(6) -0.0011(6) N2 0.0191(7) 0.0234(7) 0.0247(7) 0.0031(6) 0.0041(6) 0.0018(6) N3 0.0200(8) 0.0235(7) 0.0235(7) 0.0009(6) 0.0024(6) 0.0028(6) C1 0.0444(14) 0.0470(14) 0.0361(12) -0.0098(10) -0.0003(10) 0.0026(11) C2 0.0371(11) 0.0281(10) 0.0246(9) 0.0011(7) 0.0011(8) -0.0069(8) C3 0.0351(11) 0.0335(11) 0.0281(10) 0.0004(8) -0.0073(8) -0.0071(9) C4 0.0299(11) 0.0281(10) 0.0335(10) 0.0032(8) -0.0041(8) -0.0057(8) C5 0.0317(12) 0.0425(13) 0.0431(13) -0.0015(10) -0.0072(10) -0.0014(9) C6 0.0298(10) 0.0227(9) 0.0306(10) 0.0007(7) -0.0021(8) -0.0044(7) C7 0.0224(9) 0.0246(9) 0.0280(9) 0.0018(7) 0.0020(7) -0.0010(7) C8 0.0271(10) 0.0246(9) 0.0291(10) 0.0009(7) -0.0028(8) -0.0003(7) C9 0.0299(11) 0.0280(10) 0.0393(11) 0.0019(8) -0.0016(9) -0.0084(8) C10 0.0233(10) 0.0330(10) 0.0376(11) 0.0025(9) 0.0031(8) -0.0057(8) C11 0.0204(9) 0.0280(9) 0.0304(10) 0.0037(8) 0.0028(7) -0.0018(7) C12 0.0202(9) 0.0303(10) 0.0294(9) 0.0048(8) 0.0021(7) -0.0004(7) C13 0.0212(10) 0.0419(12) 0.0390(11) 0.0016(9) 0.0076(8) -0.0036(8) C14 0.0235(10) 0.0493(13) 0.0398(12) 0.0007(10) 0.0120(9) -0.0004(9) C15 0.0252(10) 0.0402(12) 0.0324(10) -0.0027(9) 0.0081(8) 0.0035(8) C16 0.0214(9) 0.0298(10) 0.0251(9) 0.0007(7) 0.0030(7) 0.0044(7) C17 0.0214(9) 0.0288(9) 0.0247(9) -0.0002(7) 0.0023(7) 0.0039(7) C18 0.0256(10) 0.0349(11) 0.0301(10) -0.0060(8) 0.0051(8) 0.0058(8) C19 0.0302(11) 0.0300(10) 0.0328(10) -0.0087(8) 0.0022(8) 0.0041(8) C20 0.0265(10) 0.0241(9) 0.0270(9) -0.0012(7) -0.0003(8) 0.0017(7) C21 0.0214(9) 0.0241(9) 0.0251(9) 0.0003(7) 0.0020(7) 0.0018(7) C22 0.0261(10) 0.0225(9) 0.0340(10) -0.0036(8) 0.0026(8) 0.0019(7) C23 0.0294(11) 0.0281(10) 0.0416(12) -0.0047(9) -0.0025(9) 0.0014(8) C24 0.0440(14) 0.0471(14) 0.0392(12) 0.0000(10) -0.0083(10) -0.0023(11) C25 0.0326(12) 0.0337(11) 0.0495(14) -0.0082(10) -0.0070(10) -0.0017(9) C26 0.0281(11) 0.0316(11) 0.0659(16) -0.0084(11) 0.0042(11) -0.0039(9) C27 0.0402(15) 0.0529(17) 0.100(3) -0.0024(16) -0.0144(16) -0.0140(13) C28 0.0368(13) 0.0324(11) 0.0517(14) -0.0003(10) 0.0147(11) -0.0015(9) C29 0.0336(11) 0.0274(10) 0.0395(11) -0.0027(8) 0.0068(9) 0.0016(8) C30 0.0528(16) 0.0501(15) 0.0363(12) 0.0063(11) 0.0053(11) -0.0076(12) C31 0.0377(13) 0.0482(14) 0.0393(12) -0.0127(10) -0.0133(10) 0.0112(10) C32 0.0328(11) 0.0243(9) 0.0287(10) -0.0002(8) -0.0035(8) -0.0025(8) C33 0.0295(10) 0.0283(9) 0.0290(10) 0.0008(8) -0.0008(8) -0.0016(8) C34 0.0444(18) 0.085(3) 0.096(3) 0.009(2) 0.0037(17) 0.0057(16) C35 0.053(2) 0.107(3) 0.065(2) 0.015(2) 0.0130(16) 0.0165(19) N36 0.069(2) 0.202(5) 0.101(3) 0.055(3) 0.020(2) 0.056(3) C37 0.0475(17) 0.068(2) 0.075(2) -0.0015(16) -0.0099(15) -0.0014(14) C38 0.0384(15) 0.0558(17) 0.0622(17) 0.0062(14) -0.0044(13) 0.0049(13) N39 0.0604(18) 0.0724(19) 0.096(2) -0.0033(16) -0.0161(16) -0.0132(15) C40 0.070(2) 0.061(2) 0.105(3) -0.008(2) 0.008(2) 0.0018(17) C41 0.0509(18) 0.0584(19) 0.078(2) -0.0192(16) -0.0003(16) -0.0025(15) N42 0.069(2) 0.079(2) 0.107(3) -0.0239(19) -0.0149(18) 0.0102(17) P1A 0.0244(4) 0.0419(5) 0.0422(5) 0.0079(4) -0.0003(3) -0.0019(4) F1A 0.0339(13) 0.095(2) 0.0871(19) 0.0267(16) 0.0057(13) -0.0054(14) F2A 0.0342(11) 0.115(2) 0.0595(14) 0.0003(13) 0.0077(9) -0.0177(12) F3A 0.0577(14) 0.140(3) 0.0462(12) -0.0081(14) -0.0039(10) -0.0131(15) F4A 0.0534(13) 0.113(2) 0.0559(12) -0.0092(13) -0.0119(10) -0.0080(13) F5A 0.0655(15) 0.0566(13) 0.137(2) 0.0243(14) -0.0142(16) 0.0167(11) F6A 0.0817(17) 0.0482(13) 0.131(2) 0.0164(14) -0.0014(17) 0.0031(11) P1B 0.042(3) 0.068(3) 0.059(2) -0.001(2) -0.003(2) -0.002(2) F1B 0.025(4) 0.048(4) 0.050(4) 0.009(4) 0.001(4) -0.003(4) F2B 0.042(5) 0.098(5) 0.068(5) 0.014(5) 0.000(4) -0.009(5) F3B 0.061(5) 0.100(6) 0.074(5) 0.020(5) -0.010(4) 0.014(5) F4B 0.060(4) 0.083(5) 0.073(5) 0.031(4) -0.006(4) -0.002(4) F5B 0.066(5) 0.073(5) 0.085(5) -0.017(4) -0.001(4) -0.005(4) F6B 0.074(5) 0.076(5) 0.087(5) -0.003(4) 0.015(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 Ru N2 1.9724(15) . ? Ru N3 2.0596(16) . ? Ru N1 2.0599(16) . ? O1 C2 1.372(3) . ? O1 C1 1.420(3) . ? O2 C26 1.369(3) . ? O2 C27 1.442(4) . ? N1 C7 1.342(2) . ? N1 C11 1.371(2) . ? N2 C12 1.350(2) . ? N2 C16 1.359(2) . ? N3 C21 1.344(2) . ? N3 C17 1.375(2) . ? C1 H11 0.9800 . ? C1 H12 0.9800 . ? C1 H13 0.9800 . ? C2 C33 1.384(3) . ? C2 C3 1.385(3) . ? C3 C4 1.386(3) . ? C3 H3 0.9500 . ? C4 C6 1.412(3) . ? C4 C5 1.511(3) . ? C5 H51 0.9800 . ? C5 H52 0.9800 . ? C5 H53 0.9800 . ? C6 C32 1.403(3) . ? C6 C8 1.491(3) . ? C7 C8 1.393(3) . ? C7 H7 0.9500 . ? C8 C9 1.395(3) . ? C9 C10 1.381(3) . ? C9 H9 0.9500 . ? C10 C11 1.390(3) . ? C10 H10 0.9500 . ? C11 C12 1.475(3) . ? C12 C13 1.391(3) . ? C13 C14 1.389(3) . ? C13 H131 0.9500 . ? C14 C15 1.390(3) . ? C14 H14 0.9500 . ? C15 C16 1.385(3) . ? C15 H15 0.9500 . ? C16 C17 1.471(3) . ? C17 C18 1.384(3) . ? C18 C19 1.387(3) . ? C18 H18 0.9500 . ? C19 C20 1.391(3) . ? C19 H19 0.9500 . ? C20 C21 1.392(3) . ? C20 C22 1.496(3) . ? C21 H21 0.9500 . ? C22 C23 1.402(3) . ? C22 C29 1.412(3) . ? C23 C25 1.396(3) . ? C23 C24 1.509(3) . ? C24 H241 0.9800 . ? C24 H242 0.9800 . ? C24 H243 0.9800 . ? C25 C26 1.378(4) . ? C25 H25 0.9500 . ? C26 C28 1.389(4) . ? C27 H271 0.9800 . ? C27 H272 0.9800 . ? C27 H273 0.9800 . ? C28 C29 1.391(3) . ? C28 H28 0.9500 . ? C29 C30 1.505(3) . ? C30 H301 0.9800 . ? C30 H302 0.9800 . ? C30 H303 0.9800 . ? C31 C32 1.510(3) . ? C31 H311 0.9800 . ? C31 H312 0.9800 . ? C31 H313 0.9800 . ? C32 C33 1.394(3) . ? C33 H33 0.9500 . ? C34 C35 1.434(5) . ? C34 H341 0.9800 . ? C34 H342 0.9800 . ? C34 H343 0.9800 . ? C35 N36 1.120(4) . ? C37 C38 1.446(4) . ? C37 H371 0.9800 . ? C37 H372 0.9800 . ? C37 H373 0.9800 . ? C38 N39 1.124(4) . ? C40 C41 1.442(5) . ? C40 H401 0.9800 . ? C40 H402 0.9800 . ? C40 H403 0.9800 . ? C41 N42 1.132(4) . ? P1A F3A 1.5802(10) . ? P1A F6A 1.5811(10) . ? P1A F2A 1.5823(10) . ? P1A F1A 1.5835(10) . ? P1A F5A 1.5838(10) . ? P1A F4A 1.5852(10) . ? P1B F6B 1.5824(10) . ? P1B F2B 1.5826(10) . ? P1B F3B 1.5826(10) . ? P1B F4B 1.5827(10) . ? P1B F1B 1.5829(10) . ? P1B F5B 1.5829(10) . ? 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 N2 Ru N2 179.34(9) 2_656 . ? N2 Ru N3 99.88(6) . 2_656 ? N2 Ru N3 79.63(6) . . ? N3 Ru N3 86.50(9) 2_656 . ? N2 Ru N1 101.39(6) . 2_656 ? N3 Ru N1 97.37(6) . 2_656 ? N2 Ru N1 79.10(6) . . ? N3 Ru N1 158.73(6) . . ? N1 Ru N1 86.60(9) 2_656 . ? C2 O1 C1 116.79(18) . . ? C26 O2 C27 116.7(2) . . ? C7 N1 C11 119.19(17) . . ? C7 N1 Ru 126.54(13) . . ? C11 N1 Ru 113.84(13) . . ? C12 N2 C16 122.37(17) . . ? C12 N2 Ru 119.24(13) . . ? C16 N2 Ru 118.38(13) . . ? C21 N3 C17 119.06(16) . . ? C21 N3 Ru 127.25(13) . . ? C17 N3 Ru 113.43(12) . . ? O1 C1 H11 109.5 . . ? O1 C1 H12 109.5 . . ? H11 C1 H12 109.5 . . ? O1 C1 H13 109.5 . . ? H11 C1 H13 109.5 . . ? H12 C1 H13 109.5 . . ? O1 C2 C33 124.4(2) . . ? O1 C2 C3 115.82(19) . . ? C33 C2 C3 119.81(19) . . ? C2 C3 C4 121.13(19) . . ? C2 C3 H3 119.4 . . ? C4 C3 H3 119.4 . . ? C3 C4 C6 119.4(2) . . ? C3 C4 C5 118.02(19) . . ? C6 C4 C5 122.6(2) . . ? C4 C5 H51 109.5 . . ? C4 C5 H52 109.5 . . ? H51 C5 H52 109.5 . . ? C4 C5 H53 109.5 . . ? H51 C5 H53 109.5 . . ? H52 C5 H53 109.5 . . ? C32 C6 C4 119.30(19) . . ? C32 C6 C8 120.42(18) . . ? C4 C6 C8 120.28(19) . . ? N1 C7 C8 123.64(18) . . ? N1 C7 H7 118.2 . . ? C8 C7 H7 118.2 . . ? C7 C8 C9 116.67(19) . . ? C7 C8 C6 120.09(18) . . ? C9 C8 C6 123.23(18) . . ? C10 C9 C8 120.51(19) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C9 C10 C11 119.93(19) . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? N1 C11 C10 120.04(19) . . ? N1 C11 C12 114.82(17) . . ? C10 C11 C12 125.15(18) . . ? N2 C12 C13 119.92(19) . . ? N2 C12 C11 112.46(17) . . ? C13 C12 C11 127.61(19) . . ? C14 C13 C12 118.4(2) . . ? C14 C13 H131 120.8 . . ? C12 C13 H131 120.8 . . ? C13 C14 C15 121.01(19) . . ? C13 C14 H14 119.5 . . ? C15 C14 H14 119.5 . . ? C16 C15 C14 118.8(2) . . ? C16 C15 H15 120.6 . . ? C14 C15 H15 120.6 . . ? N2 C16 C15 119.54(19) . . ? N2 C16 C17 112.93(16) . . ? C15 C16 C17 127.51(19) . . ? N3 C17 C18 120.09(18) . . ? N3 C17 C16 114.98(17) . . ? C18 C17 C16 124.92(18) . . ? C17 C18 C19 120.03(18) . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? C18 C19 C20 120.25(19) . . ? C18 C19 H19 119.9 . . ? C20 C19 H19 119.9 . . ? C19 C20 C21 117.02(18) . . ? C19 C20 C22 122.10(18) . . ? C21 C20 C22 120.88(17) . . ? N3 C21 C20 123.46(17) . . ? N3 C21 H21 118.3 . . ? C20 C21 H21 118.3 . . ? C23 C22 C29 119.6(2) . . ? C23 C22 C20 119.88(19) . . ? C29 C22 C20 120.48(19) . . ? C25 C23 C22 119.9(2) . . ? C25 C23 C24 117.4(2) . . ? C22 C23 C24 122.7(2) . . ? C23 C24 H241 109.5 . . ? C23 C24 H242 109.5 . . ? H241 C24 H242 109.5 . . ? C23 C24 H243 109.5 . . ? H241 C24 H243 109.5 . . ? H242 C24 H243 109.5 . . ? C26 C25 C23 120.3(2) . . ? C26 C25 H25 119.8 . . ? C23 C25 H25 119.8 . . ? O2 C26 C25 124.2(2) . . ? O2 C26 C28 115.7(2) . . ? C25 C26 C28 120.1(2) . . ? O2 C27 H271 109.5 . . ? O2 C27 H272 109.5 . . ? H271 C27 H272 109.5 . . ? O2 C27 H273 109.5 . . ? H271 C27 H273 109.5 . . ? H272 C27 H273 109.5 . . ? C26 C28 C29 120.8(2) . . ? C26 C28 H28 119.6 . . ? C29 C28 H28 119.6 . . ? C28 C29 C22 119.1(2) . . ? C28 C29 C30 118.7(2) . . ? C22 C29 C30 122.2(2) . . ? C29 C30 H301 109.5 . . ? C29 C30 H302 109.5 . . ? H301 C30 H302 109.5 . . ? C29 C30 H303 109.5 . . ? H301 C30 H303 109.5 . . ? H302 C30 H303 109.5 . . ? C32 C31 H311 109.5 . . ? C32 C31 H312 109.5 . . ? H311 C31 H312 109.5 . . ? C32 C31 H313 109.5 . . ? H311 C31 H313 109.5 . . ? H312 C31 H313 109.5 . . ? C33 C32 C6 119.92(19) . . ? C33 C32 C31 116.88(19) . . ? C6 C32 C31 123.19(19) . . ? C2 C33 C32 120.4(2) . . ? C2 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C35 C34 H341 109.5 . . ? C35 C34 H342 109.5 . . ? H341 C34 H342 109.5 . . ? C35 C34 H343 109.5 . . ? H341 C34 H343 109.5 . . ? H342 C34 H343 109.5 . . ? N36 C35 C34 179.6(5) . . ? C38 C37 H371 109.5 . . ? C38 C37 H372 109.5 . . ? H371 C37 H372 109.5 . . ? C38 C37 H373 109.5 . . ? H371 C37 H373 109.5 . . ? H372 C37 H373 109.5 . . ? N39 C38 C37 179.3(4) . . ? C41 C40 H401 109.5 . . ? C41 C40 H402 109.5 . . ? H401 C40 H402 109.5 . . ? C41 C40 H403 109.5 . . ? H401 C40 H403 109.5 . . ? H402 C40 H403 109.5 . . ? N42 C41 C40 179.2(5) . . ? F3A P1A F6A 90.18(4) . . ? F3A P1A F2A 90.09(4) . . ? F6A P1A F2A 90.14(4) . . ? F3A P1A F1A 90.16(4) . . ? F6A P1A F1A 89.98(4) . . ? F2A P1A F1A 179.72(6) . . ? F3A P1A F5A 90.09(4) . . ? F6A P1A F5A 179.70(6) . . ? F2A P1A F5A 89.99(4) . . ? F1A P1A F5A 89.89(4) . . ? F3A P1A F4A 179.90(6) . . ? F6A P1A F4A 89.91(4) . . ? F2A P1A F4A 89.86(4) . . ? F1A P1A F4A 89.89(4) . . ? F5A P1A F4A 89.82(4) . . ? F6B P1B F2B 90.02(4) . . ? F6B P1B F3B 90.02(4) . . ? F2B P1B F3B 90.01(4) . . ? F6B P1B F4B 90.01(4) . . ? F2B P1B F4B 90.00(4) . . ? F3B P1B F4B 179.98(8) . . ? F6B P1B F1B 90.01(4) . . ? F2B P1B F1B 179.97(8) . . ? F3B P1B F1B 90.00(4) . . ? F4B P1B F1B 89.99(4) . . ? F6B P1B F5B 179.99(8) . . ? F2B P1B F5B 89.99(4) . . ? F3B P1B F5B 89.99(4) . . ? F4B P1B F5B 89.99(4) . . ? F1B P1B F5B 89.98(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ru N1 C7 -1.69(17) 2_656 . . . ? N2 Ru N1 C7 178.77(17) . . . . ? N3 Ru N1 C7 -82.53(16) 2_656 . . . ? N3 Ru N1 C7 178.11(16) . . . . ? N1 Ru N1 C7 76.47(15) 2_656 . . . ? N2 Ru N1 C11 -174.01(13) 2_656 . . . ? N2 Ru N1 C11 6.44(13) . . . . ? N3 Ru N1 C11 105.14(13) 2_656 . . . ? N3 Ru N1 C11 5.8(3) . . . . ? N1 Ru N1 C11 -95.85(14) 2_656 . . . ? N3 Ru N2 C12 -99.45(14) 2_656 . . . ? N3 Ru N2 C12 175.99(15) . . . . ? N1 Ru N2 C12 80.47(15) 2_656 . . . ? N1 Ru N2 C12 -3.77(14) . . . . ? N3 Ru N2 C16 79.28(14) 2_656 . . . ? N3 Ru N2 C16 -5.27(14) . . . . ? N1 Ru N2 C16 -100.79(14) 2_656 . . . ? N1 Ru N2 C16 174.97(15) . . . . ? N2 Ru N3 C21 1.79(16) 2_656 . . . ? N2 Ru N3 C21 -178.66(16) . . . . ? N3 Ru N3 C21 80.62(15) 2_656 . . . ? N1 Ru N3 C21 -78.37(16) 2_656 . . . ? N1 Ru N3 C21 -178.01(16) . . . . ? N2 Ru N3 C17 -172.26(13) 2_656 . . . ? N2 Ru N3 C17 7.29(13) . . . . ? N3 Ru N3 C17 -93.43(13) 2_656 . . . ? N1 Ru N3 C17 107.58(13) 2_656 . . . ? N1 Ru N3 C17 7.9(2) . . . . ? C1 O1 C2 C33 1.5(3) . . . . ? C1 O1 C2 C3 -178.9(2) . . . . ? O1 C2 C3 C4 -178.13(19) . . . . ? C33 C2 C3 C4 1.5(3) . . . . ? C2 C3 C4 C6 0.4(3) . . . . ? C2 C3 C4 C5 -177.2(2) . . . . ? C3 C4 C6 C32 -2.3(3) . . . . ? C5 C4 C6 C32 175.2(2) . . . . ? C3 C4 C6 C8 178.69(19) . . . . ? C5 C4 C6 C8 -3.9(3) . . . . ? C11 N1 C7 C8 1.5(3) . . . . ? Ru N1 C7 C8 -170.42(14) . . . . ? N1 C7 C8 C9 -0.6(3) . . . . ? N1 C7 C8 C6 178.79(18) . . . . ? C32 C6 C8 C7 -54.9(3) . . . . ? C4 C6 C8 C7 124.1(2) . . . . ? C32 C6 C8 C9 124.5(2) . . . . ? C4 C6 C8 C9 -56.5(3) . . . . ? C7 C8 C9 C10 -0.6(3) . . . . ? C6 C8 C9 C10 180.0(2) . . . . ? C8 C9 C10 C11 1.0(3) . . . . ? C7 N1 C11 C10 -1.1(3) . . . . ? Ru N1 C11 C10 171.80(15) . . . . ? C7 N1 C11 C12 178.98(17) . . . . ? Ru N1 C11 C12 -8.1(2) . . . . ? C9 C10 C11 N1 -0.1(3) . . . . ? C9 C10 C11 C12 179.8(2) . . . . ? C16 N2 C12 C13 1.3(3) . . . . ? Ru N2 C12 C13 -179.98(15) . . . . ? C16 N2 C12 C11 -178.15(17) . . . . ? Ru N2 C12 C11 0.5(2) . . . . ? N1 C11 C12 N2 5.1(2) . . . . ? C10 C11 C12 N2 -174.76(19) . . . . ? N1 C11 C12 C13 -174.3(2) . . . . ? C10 C11 C12 C13 5.8(3) . . . . ? N2 C12 C13 C14 -1.0(3) . . . . ? C11 C12 C13 C14 178.4(2) . . . . ? C12 C13 C14 C15 -0.4(3) . . . . ? C13 C14 C15 C16 1.6(3) . . . . ? C12 N2 C16 C15 -0.1(3) . . . . ? Ru N2 C16 C15 -178.82(15) . . . . ? C12 N2 C16 C17 -178.96(17) . . . . ? Ru N2 C16 C17 2.3(2) . . . . ? C14 C15 C16 N2 -1.3(3) . . . . ? C14 C15 C16 C17 177.3(2) . . . . ? C21 N3 C17 C18 -3.2(3) . . . . ? Ru N3 C17 C18 171.36(15) . . . . ? C21 N3 C17 C16 177.20(16) . . . . ? Ru N3 C17 C16 -8.2(2) . . . . ? N2 C16 C17 N3 4.1(2) . . . . ? C15 C16 C17 N3 -174.63(19) . . . . ? N2 C16 C17 C18 -175.46(19) . . . . ? C15 C16 C17 C18 5.8(3) . . . . ? N3 C17 C18 C19 1.5(3) . . . . ? C16 C17 C18 C19 -178.96(19) . . . . ? C17 C18 C19 C20 1.0(3) . . . . ? C18 C19 C20 C21 -1.6(3) . . . . ? C18 C19 C20 C22 179.00(19) . . . . ? C17 N3 C21 C20 2.6(3) . . . . ? Ru N3 C21 C20 -171.17(14) . . . . ? C19 C20 C21 N3 -0.2(3) . . . . ? C22 C20 C21 N3 179.24(18) . . . . ? C19 C20 C22 C23 -56.1(3) . . . . ? C21 C20 C22 C23 124.5(2) . . . . ? C19 C20 C22 C29 122.0(2) . . . . ? C21 C20 C22 C29 -57.4(3) . . . . ? C29 C22 C23 C25 -1.9(3) . . . . ? C20 C22 C23 C25 176.21(19) . . . . ? C29 C22 C23 C24 176.5(2) . . . . ? C20 C22 C23 C24 -5.4(3) . . . . ? C22 C23 C25 C26 0.2(3) . . . . ? C24 C23 C25 C26 -178.3(2) . . . . ? C27 O2 C26 C25 8.0(4) . . . . ? C27 O2 C26 C28 -170.9(2) . . . . ? C23 C25 C26 O2 -176.7(2) . . . . ? C23 C25 C26 C28 2.1(4) . . . . ? O2 C26 C28 C29 176.1(2) . . . . ? C25 C26 C28 C29 -2.8(4) . . . . ? C26 C28 C29 C22 1.0(3) . . . . ? C26 C28 C29 C30 -176.6(2) . . . . ? C23 C22 C29 C28 1.3(3) . . . . ? C20 C22 C29 C28 -176.84(19) . . . . ? C23 C22 C29 C30 178.9(2) . . . . ? C20 C22 C29 C30 0.7(3) . . . . ? C4 C6 C32 C33 2.3(3) . . . . ? C8 C6 C32 C33 -178.67(18) . . . . ? C4 C6 C32 C31 -179.3(2) . . . . ? C8 C6 C32 C31 -0.3(3) . . . . ? O1 C2 C33 C32 178.12(19) . . . . ? C3 C2 C33 C32 -1.5(3) . . . . ? C6 C32 C33 C2 -0.4(3) . . . . ? C31 C32 C33 C2 -178.9(2) . . . . ? #===END data_9b _database_code_depnum_ccdc_archive 'CCDC 735263' # SG0523 _audit_creation_method SHELXL-97 _audit_creation_date 05-09-14 _chemical_name_systematic ; bis[5,5"-bis-(4-methoxy-2,6-dimethylphenyl)- [2,2':6,2"]terpyridine]osmium(II) hexafluorophosphate hexa-acetonitrile solvate ; _chemical_name_common ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_moiety 'C66 H62 N6 O4 Os 2+, 2(F6 P 1-), 6(C2 H3 N)' _chemical_formula_sum 'C78 H80 F12 N12 O4 Os P2' _chemical_formula_weight 1729.69 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 312 0.0033 0.0016 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; H H 320 0.0000 0.0000 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; F F 48 0.0171 0.0103 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; N N 48 0.0061 0.0033 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; O O 16 0.0106 0.0060 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; Os Os 4 -1.2165 7.6030 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; P P 8 0.1023 0.0942 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall ? _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 29.4529(4) _cell_length_b 11.8271(1) _cell_length_c 22.4142(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.9746(7) _cell_angle_gamma 90.00 _cell_volume 7806.69(14) _cell_formula_units_Z 4 _cell_measurement_temperature 160(1) _cell_measurement_reflns_used 159774 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 27.9 _exptl_crystal_description tablet _exptl_crystal_colour brown _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.472 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3512 _exptl_absorpt_coefficient_mu 1.759 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Blessing, 1995)' _exptl_absorpt_correction_T_min 0.584 _exptl_absorpt_correction_T_max 0.773 _exptl_special_details ; Solvent used: MeCN / dichloromethane Cooling Device: Oxford Cryosystems Cryostream 700 Crystal mount: glued on a glass fibre Mosaicity (deg.): 0.786(1) Frames collected: 828 Seconds exposure per frame: 10 Degrees rotation per frame: 1.0 Crystal-Detector distance (mm): 38.0 ; _diffrn_ambient_temperature 160(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Nonius FR590 sealed tube generator' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_detector '65 mm CCD camera on \k goniostat' _diffrn_measurement_device_type 'Nonius KappaCCD area-detector diffractometer' _diffrn_measurement_method '\f and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 81476 _diffrn_reflns_av_R_equivalents 0.0566 _diffrn_reflns_av_sigmaI/netI 0.0291 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 27.87 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 0.999 _reflns_number_total 9306 _reflns_number_gt 8424 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'COLLECT (Nonius, 2000)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN and SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'SHELXL97 and PLATON (Spek, 2009)' _refine_special_details ; The asymmetric unit contains one half of a cation with the Os-atom on a two-fold axis, one anion and three acetonitrile molecules. In the PF6- anion, four of the six F-atoms, all of which are in the same plane, are disordered. Two sets of positions were defined for these F-atoms and the site occupation factor of the major orientation of the PF6- anion refined to 0.55(1). The P-F and F...F distances involving the disordered F-atoms were restrained, so as to maintain octahedral geometry and uniform P-F bond lengths, while neighbouring atoms within and between each disordered orientation were restrained to have similar atomic displacement parameters. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0375P)^2^+16.4115P] 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_extinction_coef ? _refine_ls_number_reflns 9302 _refine_ls_number_parameters 538 _refine_ls_number_restraints 415 _refine_ls_R_factor_all 0.0385 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0767 _refine_ls_wR_factor_gt 0.0729 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.091 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.762 _refine_diff_density_min -1.184 _refine_diff_density_rms 0.089 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 Os Os 0.5000 0.203090(11) 0.7500 0.02246(5) Uani 1 2 d S . . O1 O 0.49301(8) 0.7495(2) 1.05120(9) 0.0400(5) Uani 1 1 d . . . O2 O 0.27869(9) -0.3440(2) 0.65710(14) 0.0632(7) Uani 1 1 d . . . N1 N 0.53811(7) 0.33011(18) 0.78868(10) 0.0248(4) Uani 1 1 d . . . N2 N 0.55451(7) 0.20216(17) 0.69921(10) 0.0237(4) Uani 1 1 d . . . N3 N 0.48332(7) 0.07573(17) 0.69073(9) 0.0230(4) Uani 1 1 d . . . C1 C 0.44941(12) 0.7957(3) 1.05204(14) 0.0414(7) Uani 1 1 d . . . H11 H 0.4455 0.8483 1.0186 0.062 Uiso 1 1 calc R . . H12 H 0.4452 0.8362 1.0897 0.062 Uiso 1 1 calc R . . H13 H 0.4269 0.7350 1.0485 0.062 Uiso 1 1 calc R . . C2 C 0.50408(10) 0.6846(2) 1.00293(12) 0.0316(6) Uani 1 1 d . . . C3 C 0.54749(10) 0.6388(2) 1.00377(13) 0.0345(6) Uani 1 1 d . . . H3 H 0.5669 0.6518 1.0373 0.041 Uiso 1 1 calc R . . C4 C 0.56300(10) 0.5745(2) 0.95651(13) 0.0327(6) Uani 1 1 d . . . C5 C 0.60967(11) 0.5230(3) 0.96231(15) 0.0424(7) Uani 1 1 d . . . H51 H 0.6314 0.5692 0.9404 0.064 Uiso 1 1 calc R . . H52 H 0.6092 0.4463 0.9458 0.064 Uiso 1 1 calc R . . H53 H 0.6188 0.5200 1.0045 0.064 Uiso 1 1 calc R . . C6 C 0.53391(9) 0.5553(2) 0.90684(12) 0.0288(5) Uani 1 1 d . . . C7 C 0.52610(9) 0.3937(2) 0.83569(11) 0.0257(5) Uani 1 1 d . . . H7 H 0.4997 0.3729 0.8568 0.031 Uiso 1 1 calc R . . C8 C 0.55032(9) 0.4883(2) 0.85496(12) 0.0288(5) Uani 1 1 d . . . C9 C 0.58927(10) 0.5161(3) 0.82346(13) 0.0347(6) Uani 1 1 d . . . H9 H 0.6067 0.5806 0.8347 0.042 Uiso 1 1 calc R . . C10 C 0.60254(9) 0.4501(2) 0.77600(13) 0.0340(6) Uani 1 1 d . . . H10 H 0.6293 0.4687 0.7551 0.041 Uiso 1 1 calc R . . C11 C 0.57690(9) 0.3566(2) 0.75864(12) 0.0278(5) Uani 1 1 d . . . C12 C 0.58744(9) 0.2810(2) 0.70865(12) 0.0280(5) Uani 1 1 d . . . C13 C 0.62564(10) 0.2813(3) 0.67321(14) 0.0361(6) Uani 1 1 d . . . H131 H 0.6488 0.3364 0.6789 0.043 Uiso 1 1 calc R . . C14 C 0.62933(10) 0.1991(3) 0.62918(14) 0.0393(7) Uani 1 1 d . . . H14 H 0.6552 0.1983 0.6045 0.047 Uiso 1 1 calc R . . C15 C 0.59568(9) 0.1182(3) 0.62078(13) 0.0345(6) Uani 1 1 d . . . H15 H 0.5987 0.0614 0.5912 0.041 Uiso 1 1 calc R . . C16 C 0.55772(9) 0.1212(2) 0.65599(11) 0.0266(5) Uani 1 1 d . . . C17 C 0.51791(9) 0.0467(2) 0.65303(11) 0.0262(5) Uani 1 1 d . . . C18 C 0.51338(9) -0.0471(2) 0.61638(12) 0.0316(6) Uani 1 1 d . . . H18 H 0.5375 -0.0682 0.5910 0.038 Uiso 1 1 calc R . . C19 C 0.47389(10) -0.1098(2) 0.61673(12) 0.0326(6) Uani 1 1 d . . . H19 H 0.4712 -0.1748 0.5920 0.039 Uiso 1 1 calc R . . C20 C 0.43800(9) -0.0789(2) 0.65298(11) 0.0266(5) Uani 1 1 d . . . C21 C 0.44459(9) 0.0150(2) 0.68924(11) 0.0245(5) Uani 1 1 d . . . H21 H 0.4206 0.0376 0.7143 0.029 Uiso 1 1 calc R . . C22 C 0.39453(9) -0.1439(2) 0.65394(12) 0.0290(5) Uani 1 1 d . . . C23 C 0.36956(10) -0.1604(2) 0.60083(14) 0.0352(6) Uani 1 1 d . . . C24 C 0.38297(12) -0.1085(3) 0.54236(14) 0.0446(7) Uani 1 1 d . . . H241 H 0.3938 -0.0312 0.5492 0.067 Uiso 1 1 calc R . . H242 H 0.3566 -0.1070 0.5151 0.067 Uiso 1 1 calc R . . H243 H 0.4072 -0.1536 0.5247 0.067 Uiso 1 1 calc R . . C25 C 0.33019(11) -0.2265(3) 0.60102(16) 0.0427(7) Uani 1 1 d . . . H25 H 0.3135 -0.2385 0.5650 0.051 Uiso 1 1 calc R . . C26 C 0.31564(11) -0.2742(3) 0.65338(18) 0.0451(8) Uani 1 1 d . . . C27 C 0.25766(14) -0.3795(4) 0.6017(2) 0.0691(12) Uani 1 1 d . . . H271 H 0.2444 -0.3137 0.5814 0.104 Uiso 1 1 calc R . . H272 H 0.2338 -0.4348 0.6099 0.104 Uiso 1 1 calc R . . H273 H 0.2806 -0.4140 0.5763 0.104 Uiso 1 1 calc R . . C28 C 0.33900(11) -0.2544(3) 0.70664(16) 0.0433(7) Uani 1 1 d . . . H28 H 0.3278 -0.2849 0.7428 0.052 Uiso 1 1 calc R . . C29 C 0.37871(10) -0.1901(2) 0.70768(14) 0.0345(6) Uani 1 1 d . . . C30 C 0.40419(13) -0.1761(3) 0.76609(15) 0.0486(8) Uani 1 1 d . . . H301 H 0.3989 -0.1000 0.7818 0.073 Uiso 1 1 calc R . . H302 H 0.4367 -0.1867 0.7597 0.073 Uiso 1 1 calc R . . H303 H 0.3935 -0.2323 0.7947 0.073 Uiso 1 1 calc R . . C31 C 0.45616(11) 0.5821(3) 0.85568(14) 0.0441(8) Uani 1 1 d . . . H311 H 0.4417 0.5079 0.8596 0.066 Uiso 1 1 calc R . . H312 H 0.4721 0.5859 0.8177 0.066 Uiso 1 1 calc R . . H313 H 0.4329 0.6413 0.8567 0.066 Uiso 1 1 calc R . . C32 C 0.48975(9) 0.5995(2) 0.90678(12) 0.0297(6) Uani 1 1 d . . . C33 C 0.47494(10) 0.6637(2) 0.95486(12) 0.0312(6) Uani 1 1 d . . . H33 H 0.4449 0.6931 0.9547 0.037 Uiso 1 1 calc R . . C34 C 0.20615(15) 0.5159(5) 0.7405(2) 0.0801(14) Uani 1 1 d . . . H341 H 0.2103 0.5939 0.7268 0.120 Uiso 1 1 calc R . . H342 H 0.1859 0.5152 0.7748 0.120 Uiso 1 1 calc R . . H343 H 0.1928 0.4706 0.7081 0.120 Uiso 1 1 calc R . . C35 C 0.24942(16) 0.4691(5) 0.7578(2) 0.0791(14) Uani 1 1 d . . . N36 N 0.28362(17) 0.4344(6) 0.7705(3) 0.140(3) Uani 1 1 d . . . C37 C 0.19435(15) 0.8246(4) 0.8842(2) 0.0687(12) Uani 1 1 d . . . H371 H 0.2255 0.8126 0.8710 0.103 Uiso 1 1 calc R . . H372 H 0.1933 0.8172 0.9277 0.103 Uiso 1 1 calc R . . H373 H 0.1843 0.9005 0.8725 0.103 Uiso 1 1 calc R . . C38 C 0.16465(13) 0.7408(4) 0.85658(19) 0.0554(9) Uani 1 1 d . . . N39 N 0.14135(14) 0.6782(3) 0.8348(2) 0.0793(12) Uani 1 1 d . . . C40 C 0.24534(18) 0.5343(4) 0.9215(3) 0.0832(14) Uani 1 1 d . . . H401 H 0.2612 0.5854 0.8945 0.125 Uiso 1 1 calc R . . H402 H 0.2370 0.5755 0.9577 0.125 Uiso 1 1 calc R . . H403 H 0.2178 0.5054 0.9016 0.125 Uiso 1 1 calc R . . C41 C 0.27465(15) 0.4412(4) 0.9374(2) 0.0697(12) Uani 1 1 d . . . N42 N 0.29711(16) 0.3658(4) 0.9499(2) 0.0943(14) Uani 1 1 d . . . P1 P 0.33567(2) 0.81553(7) 0.93519(3) 0.04143(19) Uani 1 1 d DU . . F1 F 0.38552(5) 0.84072(15) 0.91356(7) 0.0708(7) Uani 1 1 d DU A . F2 F 0.28587(5) 0.79045(15) 0.95691(8) 0.0787(8) Uani 1 1 d DU A . F3A F 0.32198(9) 0.7736(6) 0.87039(10) 0.0779(17) Uani 0.550(12) 1 d PDU A 1 F4A F 0.34939(9) 0.8575(6) 1.00007(10) 0.0705(16) Uani 0.550(12) 1 d PDU A 1 F5A F 0.32102(8) 0.9400(2) 0.9178(3) 0.092(2) Uani 0.550(12) 1 d PDU A 1 F6A F 0.35038(8) 0.6911(2) 0.9527(3) 0.0751(17) Uani 0.550(12) 1 d PDU A 1 F3B F 0.31760(8) 0.8215(7) 0.86843(7) 0.084(2) Uani 0.450(12) 1 d PDU A 2 F4B F 0.35375(7) 0.8097(7) 1.00199(7) 0.076(2) Uani 0.450(12) 1 d PDU A 2 F5B F 0.32695(11) 0.94679(12) 0.9424(4) 0.0708(19) Uani 0.450(12) 1 d PDU A 2 F6B F 0.34443(12) 0.68438(12) 0.9280(4) 0.103(2) Uani 0.450(12) 1 d PDU A 2 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 Os 0.02009(7) 0.02174(7) 0.02568(8) 0.000 0.00431(5) 0.000 O1 0.0480(13) 0.0420(12) 0.0297(10) -0.0060(9) -0.0022(9) -0.0025(10) O2 0.0448(14) 0.0522(15) 0.093(2) -0.0051(15) 0.0068(14) -0.0205(13) N1 0.0243(10) 0.0221(10) 0.0278(11) 0.0022(8) 0.0000(8) -0.0013(8) N2 0.0183(9) 0.0259(10) 0.0272(11) 0.0037(8) 0.0048(8) 0.0026(8) N3 0.0234(10) 0.0215(10) 0.0241(10) -0.0001(8) 0.0023(8) 0.0025(8) C1 0.0527(19) 0.0384(16) 0.0335(15) -0.0088(13) 0.0072(13) -0.0009(14) C2 0.0403(15) 0.0278(14) 0.0268(13) 0.0019(10) 0.0000(11) -0.0104(11) C3 0.0385(15) 0.0334(15) 0.0315(14) 0.0030(11) -0.0083(12) -0.0090(12) C4 0.0343(15) 0.0278(13) 0.0358(15) 0.0049(11) -0.0034(11) -0.0086(11) C5 0.0367(16) 0.0417(17) 0.0485(18) 0.0005(14) -0.0099(13) -0.0024(14) C6 0.0329(14) 0.0215(12) 0.0321(14) 0.0019(10) -0.0020(11) -0.0054(11) C7 0.0249(12) 0.0245(12) 0.0277(13) 0.0012(10) 0.0003(10) -0.0015(10) C8 0.0289(13) 0.0240(12) 0.0333(14) 0.0016(10) -0.0045(11) -0.0020(10) C9 0.0326(15) 0.0317(14) 0.0396(16) 0.0040(12) -0.0013(12) -0.0085(12) C10 0.0246(13) 0.0358(15) 0.0416(16) 0.0054(12) 0.0030(11) -0.0066(11) C11 0.0232(12) 0.0292(13) 0.0311(13) 0.0050(11) 0.0021(10) -0.0018(10) C12 0.0216(12) 0.0309(14) 0.0316(13) 0.0054(11) 0.0026(10) -0.0010(10) C13 0.0245(13) 0.0431(17) 0.0408(16) 0.0036(13) 0.0079(11) -0.0039(12) C14 0.0268(14) 0.0510(19) 0.0404(16) 0.0027(14) 0.0130(12) 0.0016(13) C15 0.0295(14) 0.0414(16) 0.0329(14) -0.0015(12) 0.0086(11) 0.0046(12) C16 0.0257(12) 0.0289(13) 0.0254(12) 0.0020(10) 0.0040(10) 0.0062(10) C17 0.0251(12) 0.0287(13) 0.0250(12) 0.0005(10) 0.0046(10) 0.0060(10) C18 0.0295(14) 0.0342(14) 0.0312(14) -0.0058(11) 0.0070(11) 0.0062(11) C19 0.0334(14) 0.0310(14) 0.0337(14) -0.0072(11) 0.0029(11) 0.0049(12) C20 0.0284(13) 0.0240(12) 0.0274(13) -0.0014(10) -0.0001(10) 0.0026(10) C21 0.0247(12) 0.0226(12) 0.0262(12) -0.0005(10) 0.0027(9) 0.0020(10) C22 0.0295(13) 0.0209(12) 0.0365(14) -0.0044(10) 0.0027(11) 0.0017(10) C23 0.0304(14) 0.0276(13) 0.0473(17) -0.0061(12) -0.0026(12) 0.0025(12) C24 0.0459(18) 0.0470(18) 0.0407(17) 0.0001(14) -0.0098(14) -0.0016(15) C25 0.0371(16) 0.0347(16) 0.056(2) -0.0077(14) -0.0051(14) 0.0000(13) C26 0.0316(15) 0.0305(15) 0.073(2) -0.0086(15) 0.0045(15) -0.0028(12) C27 0.044(2) 0.054(2) 0.109(4) -0.003(2) -0.011(2) -0.0159(18) C28 0.0441(18) 0.0299(15) 0.057(2) -0.0008(14) 0.0164(15) -0.0010(14) C29 0.0368(15) 0.0272(14) 0.0398(16) -0.0033(11) 0.0072(12) 0.0023(12) C30 0.058(2) 0.0478(19) 0.0402(18) 0.0075(14) 0.0067(15) -0.0074(16) C31 0.0423(17) 0.0472(18) 0.0422(17) -0.0143(14) -0.0139(14) 0.0134(15) C32 0.0337(14) 0.0243(12) 0.0311(14) -0.0009(10) -0.0034(11) -0.0042(11) C33 0.0336(14) 0.0260(13) 0.0340(14) 0.0028(11) -0.0011(11) -0.0033(11) C34 0.052(3) 0.089(4) 0.099(4) 0.008(3) 0.007(2) 0.004(2) C35 0.048(2) 0.108(4) 0.082(3) 0.015(3) 0.013(2) 0.015(3) N36 0.070(3) 0.228(7) 0.121(4) 0.068(5) 0.026(3) 0.057(4) C37 0.050(2) 0.074(3) 0.081(3) -0.002(2) -0.010(2) -0.005(2) C38 0.043(2) 0.056(2) 0.066(2) 0.0085(19) -0.0060(17) 0.0055(18) N39 0.064(2) 0.071(3) 0.102(3) -0.002(2) -0.018(2) -0.013(2) C40 0.076(3) 0.064(3) 0.110(4) -0.007(3) 0.009(3) 0.005(3) C41 0.054(2) 0.065(3) 0.089(3) -0.026(2) -0.001(2) -0.005(2) N42 0.079(3) 0.083(3) 0.121(4) -0.027(3) -0.021(3) 0.012(3) P1 0.0294(4) 0.0453(5) 0.0495(5) 0.0065(4) -0.0009(3) -0.0019(3) F1 0.0358(11) 0.0913(17) 0.0855(17) 0.0266(14) 0.0065(11) -0.0057(12) F2 0.0399(12) 0.118(2) 0.0788(17) -0.0014(14) 0.0101(11) -0.0175(13) F3A 0.065(3) 0.118(5) 0.050(3) -0.009(2) -0.004(2) -0.010(3) F4A 0.056(3) 0.078(4) 0.077(3) -0.026(2) -0.013(2) 0.006(2) F5A 0.069(3) 0.062(3) 0.144(5) 0.031(3) -0.032(3) 0.015(2) F6A 0.076(3) 0.047(3) 0.101(4) 0.020(2) -0.019(3) -0.003(2) F3B 0.054(3) 0.152(6) 0.046(3) -0.010(3) -0.008(3) 0.023(3) F4B 0.055(3) 0.112(5) 0.059(3) 0.037(3) -0.008(3) 0.012(3) F5B 0.064(3) 0.052(3) 0.095(5) -0.006(3) -0.019(3) 0.007(3) F6B 0.097(5) 0.064(4) 0.148(6) -0.003(4) 0.001(4) 0.010(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 Os N2 1.984(2) . ? Os N1 2.058(2) . ? Os N3 2.062(2) . ? O1 C2 1.371(4) . ? O1 C1 1.396(4) . ? O2 C26 1.370(4) . ? O2 C27 1.440(5) . ? N1 C7 1.347(3) . ? N1 C11 1.372(3) . ? N2 C12 1.360(3) . ? N2 C16 1.366(3) . ? N3 C21 1.348(3) . ? N3 C17 1.378(3) . ? C1 H11 0.9800 . ? C1 H12 0.9800 . ? C1 H13 0.9800 . ? C2 C3 1.388(4) . ? C2 C33 1.388(4) . ? C3 C4 1.388(4) . ? C3 H3 0.9500 . ? C4 C6 1.411(4) . ? C4 C5 1.507(4) . ? C5 H51 0.9800 . ? C5 H52 0.9800 . ? C5 H53 0.9800 . ? C6 C32 1.401(4) . ? C6 C8 1.494(4) . ? C7 C8 1.391(4) . ? C7 H7 0.9500 . ? C8 C9 1.397(4) . ? C9 C10 1.381(4) . ? C9 H9 0.9500 . ? C10 C11 1.391(4) . ? C10 H10 0.9500 . ? C11 C12 1.471(4) . ? C12 C13 1.388(4) . ? C13 C14 1.391(4) . ? C13 H131 0.9500 . ? C14 C15 1.388(4) . ? C14 H14 0.9500 . ? C15 C16 1.380(4) . ? C15 H15 0.9500 . ? C16 C17 1.468(4) . ? C17 C18 1.385(4) . ? C18 C19 1.380(4) . ? C18 H18 0.9500 . ? C19 C20 1.393(4) . ? C19 H19 0.9500 . ? C20 C21 1.388(3) . ? C20 C22 1.493(4) . ? C21 H21 0.9500 . ? C22 C23 1.402(4) . ? C22 C29 1.409(4) . ? C23 C25 1.399(4) . ? C23 C24 1.506(5) . ? C24 H241 0.9800 . ? C24 H242 0.9800 . ? C24 H243 0.9800 . ? C25 C26 1.377(5) . ? C25 H25 0.9500 . ? C26 C28 1.388(5) . ? C27 H271 0.9800 . ? C27 H272 0.9800 . ? C27 H273 0.9800 . ? C28 C29 1.395(4) . ? C28 H28 0.9500 . ? C29 C30 1.507(5) . ? C30 H301 0.9800 . ? C30 H302 0.9800 . ? C30 H303 0.9800 . ? C31 C32 1.515(4) . ? C31 H311 0.9800 . ? C31 H312 0.9800 . ? C31 H313 0.9800 . ? C32 C33 1.395(4) . ? C33 H33 0.9500 . ? C34 C35 1.437(6) . ? C34 H341 0.9800 . ? C34 H342 0.9800 . ? C34 H343 0.9800 . ? C35 N36 1.120(6) . ? C37 C38 1.453(6) . ? C37 H371 0.9800 . ? C37 H372 0.9800 . ? C37 H373 0.9800 . ? C38 N39 1.117(5) . ? C40 C41 1.440(7) . ? C40 H401 0.9800 . ? C40 H402 0.9800 . ? C40 H403 0.9800 . ? C41 N42 1.142(6) . ? P1 F3A 1.5806(12) . ? P1 F6B 1.5810(12) . ? P1 F3B 1.5811(12) . ? P1 F2 1.5813(12) . ? P1 F5A 1.5816(12) . ? P1 F6A 1.5816(12) . ? P1 F5B 1.5822(12) . ? P1 F4B 1.5822(12) . ? P1 F1 1.5825(12) . ? P1 F4A 1.5827(12) . ? 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 N2 Os N2 179.37(12) . 2_656 ? N2 Os N1 78.75(9) . . ? N2 Os N1 101.72(8) . 2_656 ? N1 Os N1 86.23(12) . 2_656 ? N2 Os N3 100.33(8) . 2_656 ? N1 Os N3 98.02(8) . 2_656 ? N2 Os N3 79.19(9) . . ? N1 Os N3 157.94(9) . . ? N3 Os N3 86.16(11) . 2_656 ? C2 O1 C1 117.5(2) . . ? C26 O2 C27 117.0(3) . . ? C7 N1 C11 119.2(2) . . ? C7 N1 Os 126.07(17) . . ? C11 N1 Os 114.38(17) . . ? C12 N2 C16 122.2(2) . . ? C12 N2 Os 119.28(18) . . ? C16 N2 Os 118.50(17) . . ? C21 N3 C17 119.1(2) . . ? C21 N3 Os 126.69(17) . . ? C17 N3 Os 114.00(17) . . ? O1 C1 H11 109.5 . . ? O1 C1 H12 109.5 . . ? H11 C1 H12 109.5 . . ? O1 C1 H13 109.5 . . ? H11 C1 H13 109.5 . . ? H12 C1 H13 109.5 . . ? O1 C2 C3 116.0(3) . . ? O1 C2 C33 124.1(3) . . ? C3 C2 C33 119.9(3) . . ? C2 C3 C4 121.2(3) . . ? C2 C3 H3 119.4 . . ? C4 C3 H3 119.4 . . ? C3 C4 C6 119.1(3) . . ? C3 C4 C5 117.9(3) . . ? C6 C4 C5 123.0(3) . . ? C4 C5 H51 109.5 . . ? C4 C5 H52 109.5 . . ? H51 C5 H52 109.5 . . ? C4 C5 H53 109.5 . . ? H51 C5 H53 109.5 . . ? H52 C5 H53 109.5 . . ? C32 C6 C4 119.5(3) . . ? C32 C6 C8 120.6(2) . . ? C4 C6 C8 119.9(3) . . ? N1 C7 C8 123.5(2) . . ? N1 C7 H7 118.2 . . ? C8 C7 H7 118.2 . . ? C7 C8 C9 117.0(3) . . ? C7 C8 C6 119.8(2) . . ? C9 C8 C6 123.2(2) . . ? C10 C9 C8 120.1(3) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C9 C10 C11 120.4(3) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? N1 C11 C10 119.8(3) . . ? N1 C11 C12 115.0(2) . . ? C10 C11 C12 125.2(2) . . ? N2 C12 C13 119.7(3) . . ? N2 C12 C11 112.1(2) . . ? C13 C12 C11 128.2(3) . . ? C12 C13 C14 118.6(3) . . ? C12 C13 H131 120.7 . . ? C14 C13 H131 120.7 . . ? C15 C14 C13 120.9(3) . . ? C15 C14 H14 119.5 . . ? C13 C14 H14 119.5 . . ? C16 C15 C14 119.2(3) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? N2 C16 C15 119.4(3) . . ? N2 C16 C17 112.8(2) . . ? C15 C16 C17 127.8(3) . . ? N3 C17 C18 119.9(2) . . ? N3 C17 C16 114.9(2) . . ? C18 C17 C16 125.2(2) . . ? C19 C18 C17 120.0(2) . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C18 C19 C20 120.7(3) . . ? C18 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? C21 C20 C19 116.8(2) . . ? C21 C20 C22 121.0(2) . . ? C19 C20 C22 122.2(2) . . ? N3 C21 C20 123.4(2) . . ? N3 C21 H21 118.3 . . ? C20 C21 H21 118.3 . . ? C23 C22 C29 119.7(3) . . ? C23 C22 C20 119.8(3) . . ? C29 C22 C20 120.5(2) . . ? C25 C23 C22 119.9(3) . . ? C25 C23 C24 117.4(3) . . ? C22 C23 C24 122.7(3) . . ? C23 C24 H241 109.5 . . ? C23 C24 H242 109.5 . . ? H241 C24 H242 109.5 . . ? C23 C24 H243 109.5 . . ? H241 C24 H243 109.5 . . ? H242 C24 H243 109.5 . . ? C26 C25 C23 120.1(3) . . ? C26 C25 H25 120.0 . . ? C23 C25 H25 120.0 . . ? O2 C26 C25 123.9(3) . . ? O2 C26 C28 115.6(3) . . ? C25 C26 C28 120.5(3) . . ? O2 C27 H271 109.5 . . ? O2 C27 H272 109.5 . . ? H271 C27 H272 109.5 . . ? O2 C27 H273 109.5 . . ? H271 C27 H273 109.5 . . ? H272 C27 H273 109.5 . . ? C26 C28 C29 120.7(3) . . ? C26 C28 H28 119.7 . . ? C29 C28 H28 119.7 . . ? C28 C29 C22 119.1(3) . . ? C28 C29 C30 118.7(3) . . ? C22 C29 C30 122.2(3) . . ? C29 C30 H301 109.5 . . ? C29 C30 H302 109.5 . . ? H301 C30 H302 109.5 . . ? C29 C30 H303 109.5 . . ? H301 C30 H303 109.5 . . ? H302 C30 H303 109.5 . . ? C32 C31 H311 109.5 . . ? C32 C31 H312 109.5 . . ? H311 C31 H312 109.5 . . ? C32 C31 H313 109.5 . . ? H311 C31 H313 109.5 . . ? H312 C31 H313 109.5 . . ? C33 C32 C6 120.3(2) . . ? C33 C32 C31 116.7(3) . . ? C6 C32 C31 123.0(3) . . ? C2 C33 C32 120.0(3) . . ? C2 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C35 C34 H341 109.5 . . ? C35 C34 H342 109.5 . . ? H341 C34 H342 109.5 . . ? C35 C34 H343 109.5 . . ? H341 C34 H343 109.5 . . ? H342 C34 H343 109.5 . . ? N36 C35 C34 178.4(6) . . ? C38 C37 H371 109.5 . . ? C38 C37 H372 109.5 . . ? H371 C37 H372 109.5 . . ? C38 C37 H373 109.5 . . ? H371 C37 H373 109.5 . . ? H372 C37 H373 109.5 . . ? N39 C38 C37 178.5(5) . . ? C41 C40 H401 109.5 . . ? C41 C40 H402 109.5 . . ? H401 C40 H402 109.5 . . ? C41 C40 H403 109.5 . . ? H401 C40 H403 109.5 . . ? H402 C40 H403 109.5 . . ? N42 C41 C40 178.5(5) . . ? F6B P1 F3B 90.05(4) . . ? F3A P1 F2 90.04(4) . . ? F6B P1 F2 90.06(4) . . ? F3B P1 F2 90.05(4) . . ? F3A P1 F5A 90.06(4) . . ? F2 P1 F5A 90.01(4) . . ? F3A P1 F6A 90.05(4) . . ? F2 P1 F6A 90.04(4) . . ? F5A P1 F6A 179.87(6) . . ? F6B P1 F5B 179.94(7) . . ? F3B P1 F5B 89.99(4) . . ? F2 P1 F5B 89.98(4) . . ? F6B P1 F4B 90.01(4) . . ? F3B P1 F4B 179.93(7) . . ? F2 P1 F4B 89.98(4) . . ? F5B P1 F4B 89.95(4) . . ? F3A P1 F1 90.05(4) . . ? F6B P1 F1 89.99(4) . . ? F3B P1 F1 90.04(4) . . ? F2 P1 F1 179.90(5) . . ? F5A P1 F1 89.97(4) . . ? F6A P1 F1 89.97(4) . . ? F5B P1 F1 89.97(4) . . ? F4B P1 F1 89.94(4) . . ? F3A P1 F4A 179.97(7) . . ? F2 P1 F4A 89.98(4) . . ? F5A P1 F4A 89.96(4) . . ? F6A P1 F4A 89.93(4) . . ? F1 P1 F4A 89.93(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Os N1 C7 -1.2(2) 2_656 . . . ? N2 Os N1 C7 179.3(2) . . . . ? N1 Os N1 C7 76.5(2) 2_656 . . . ? N3 Os N1 C7 -81.7(2) 2_656 . . . ? N3 Os N1 C7 178.6(2) . . . . ? N2 Os N1 C11 -174.39(18) 2_656 . . . ? N2 Os N1 C11 6.04(18) . . . . ? N1 Os N1 C11 -96.71(19) 2_656 . . . ? N3 Os N1 C11 105.05(18) 2_656 . . . ? N3 Os N1 C11 5.4(3) . . . . ? N2 Os N2 C12 -142.0(2) 2_656 . . . ? N1 Os N2 C12 -3.94(19) . . . . ? N1 Os N2 C12 79.8(2) 2_656 . . . ? N3 Os N2 C12 -100.16(19) 2_656 . . . ? N3 Os N2 C12 175.8(2) . . . . ? N2 Os N2 C16 37.56(19) 2_656 . . . ? N1 Os N2 C16 175.6(2) . . . . ? N1 Os N2 C16 -100.68(19) 2_656 . . . ? N3 Os N2 C16 79.40(19) 2_656 . . . ? N3 Os N2 C16 -4.63(18) . . . . ? N2 Os N3 C21 1.6(2) 2_656 . . . ? N2 Os N3 C21 -178.9(2) . . . . ? N1 Os N3 C21 -178.2(2) . . . . ? N1 Os N3 C21 -78.4(2) 2_656 . . . ? N3 Os N3 C21 79.8(2) 2_656 . . . ? N2 Os N3 C17 -172.66(17) 2_656 . . . ? N2 Os N3 C17 6.91(17) . . . . ? N1 Os N3 C17 7.5(3) . . . . ? N1 Os N3 C17 107.40(18) 2_656 . . . ? N3 Os N3 C17 -94.38(18) 2_656 . . . ? C1 O1 C2 C3 -179.3(3) . . . . ? C1 O1 C2 C33 1.0(4) . . . . ? O1 C2 C3 C4 -178.0(3) . . . . ? C33 C2 C3 C4 1.7(4) . . . . ? C2 C3 C4 C6 -0.1(4) . . . . ? C2 C3 C4 C5 -177.0(3) . . . . ? C3 C4 C6 C32 -1.4(4) . . . . ? C5 C4 C6 C32 175.3(3) . . . . ? C3 C4 C6 C8 178.7(2) . . . . ? C5 C4 C6 C8 -4.6(4) . . . . ? C11 N1 C7 C8 2.0(4) . . . . ? Os N1 C7 C8 -170.98(19) . . . . ? N1 C7 C8 C9 -0.7(4) . . . . ? N1 C7 C8 C6 178.7(2) . . . . ? C32 C6 C8 C7 -55.3(4) . . . . ? C4 C6 C8 C7 124.6(3) . . . . ? C32 C6 C8 C9 124.1(3) . . . . ? C4 C6 C8 C9 -56.1(4) . . . . ? C7 C8 C9 C10 -0.8(4) . . . . ? C6 C8 C9 C10 179.8(3) . . . . ? C8 C9 C10 C11 1.0(4) . . . . ? C7 N1 C11 C10 -1.7(4) . . . . ? Os N1 C11 C10 172.0(2) . . . . ? C7 N1 C11 C12 179.0(2) . . . . ? Os N1 C11 C12 -7.2(3) . . . . ? C9 C10 C11 N1 0.3(4) . . . . ? C9 C10 C11 C12 179.4(3) . . . . ? C16 N2 C12 C13 0.7(4) . . . . ? Os N2 C12 C13 -179.8(2) . . . . ? C16 N2 C12 C11 -178.3(2) . . . . ? Os N2 C12 C11 1.2(3) . . . . ? N1 C11 C12 N2 4.1(3) . . . . ? C10 C11 C12 N2 -175.2(3) . . . . ? N1 C11 C12 C13 -174.8(3) . . . . ? C10 C11 C12 C13 6.0(5) . . . . ? N2 C12 C13 C14 -0.8(4) . . . . ? C11 C12 C13 C14 178.0(3) . . . . ? C12 C13 C14 C15 -0.2(5) . . . . ? C13 C14 C15 C16 1.3(5) . . . . ? C12 N2 C16 C15 0.5(4) . . . . ? Os N2 C16 C15 -179.1(2) . . . . ? C12 N2 C16 C17 -178.8(2) . . . . ? Os N2 C16 C17 1.6(3) . . . . ? C14 C15 C16 N2 -1.5(4) . . . . ? C14 C15 C16 C17 177.8(3) . . . . ? C21 N3 C17 C18 -3.1(4) . . . . ? Os N3 C17 C18 171.6(2) . . . . ? C21 N3 C17 C16 177.2(2) . . . . ? Os N3 C17 C16 -8.1(3) . . . . ? N2 C16 C17 N3 4.5(3) . . . . ? C15 C16 C17 N3 -174.8(3) . . . . ? N2 C16 C17 C18 -175.3(2) . . . . ? C15 C16 C17 C18 5.4(4) . . . . ? N3 C17 C18 C19 1.4(4) . . . . ? C16 C17 C18 C19 -178.9(3) . . . . ? C17 C18 C19 C20 1.0(4) . . . . ? C18 C19 C20 C21 -1.7(4) . . . . ? C18 C19 C20 C22 179.2(3) . . . . ? C17 N3 C21 C20 2.4(4) . . . . ? Os N3 C21 C20 -171.54(19) . . . . ? C19 C20 C21 N3 0.0(4) . . . . ? C22 C20 C21 N3 179.1(2) . . . . ? C21 C20 C22 C23 124.3(3) . . . . ? C19 C20 C22 C23 -56.6(4) . . . . ? C21 C20 C22 C29 -56.6(4) . . . . ? C19 C20 C22 C29 122.5(3) . . . . ? C29 C22 C23 C25 -2.6(4) . . . . ? C20 C22 C23 C25 176.4(3) . . . . ? C29 C22 C23 C24 176.7(3) . . . . ? C20 C22 C23 C24 -4.3(4) . . . . ? C22 C23 C25 C26 0.8(5) . . . . ? C24 C23 C25 C26 -178.6(3) . . . . ? C27 O2 C26 C25 7.8(5) . . . . ? C27 O2 C26 C28 -171.3(3) . . . . ? C23 C25 C26 O2 -177.0(3) . . . . ? C23 C25 C26 C28 2.0(5) . . . . ? O2 C26 C28 C29 176.2(3) . . . . ? C25 C26 C28 C29 -2.9(5) . . . . ? C26 C28 C29 C22 1.0(4) . . . . ? C26 C28 C29 C30 -176.8(3) . . . . ? C23 C22 C29 C28 1.8(4) . . . . ? C20 C22 C29 C28 -177.3(3) . . . . ? C23 C22 C29 C30 179.5(3) . . . . ? C20 C22 C29 C30 0.4(4) . . . . ? C4 C6 C32 C33 1.3(4) . . . . ? C8 C6 C32 C33 -178.8(2) . . . . ? C4 C6 C32 C31 -179.4(3) . . . . ? C8 C6 C32 C31 0.5(4) . . . . ? O1 C2 C33 C32 177.9(3) . . . . ? C3 C2 C33 C32 -1.8(4) . . . . ? C6 C32 C33 C2 0.3(4) . . . . ? C31 C32 C33 C2 -179.0(3) . . . . ? #===END