data_Compound7b _audit_creation_method SHELXL-97 # 1. submission details _publ_contact_author_name 'Linda H. Doerrer' _publ_contact_author_address ; barnard college, chemistry department 3009 broadway new york, ny, 10027 ; _publ_contact_author_phone ' 212-854-2074 ' _publ_contact_author_fax ' 212-854-2310 ' _publ_contact_author_email ' ldoerrer@barnard.edu ' _publ_requested_journal 'Inorganic Chemistry' _publ_requested_coeditor_name ' Prof James Mayer ' #============================================================================== # 3. title and author list _publ_section_title ; homoleptic cobalt and copper phenolate A2[M(OAr)4] Compounds the effect of phenoxide fluorination ; # the loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address _publ_author_footnote 'buzzeo, marisa c.' #<--'Last name, first name' ; barnard college, chemistry department 3009 broadway new york, ny, 10027 ; 'iqbal, amber h.' ; barnard college, chemistry department 3009 broadway new york, ny, 10027 ; 'long, charli m.' ; barnard college, chemistry department 3009 broadway new york, ny, 10027 ; 'millar, david' ; barnard college, chemistry department 3009 broadway new york, ny, 10027 ; 'patel, sonal' ; barnard college, chemistry department 3009 broadway new york, ny, 10027 ; 'pellow, matthew a.' ; barnard college, chemistry department 3009 broadway new york, ny, 10027 ; 'saddoughi, sahar a.' ; barnard college, chemistry department 3009 broadway new york, ny, 10027 ; 'smenton, abigail l.' ; barnard college, chemistry department 3009 broadway new york, ny, 10027 ; 'turner, john f. c.' ; department of chemistry 408 buehler hall university of tennessee knoxville, tn 37996 ; 'wadhawan, jay d.' ; physical and theoretical chemistry Laboratory university of oxford oxford ox1 3qz, uk ; 'compton, richard g.' ; physical and theoretical chemistry Laboratory university of oxford oxford ox1 3qz, uk ; 'golen, james a.' ; department of chemistry and biochemistry mc 0358 university of california, san diego 9500 gilman drive la jolla, ca 92093 ; ; permanent address is the department of Chemistry & Biochemistry, University of massachusetts dartmouth, north dartmouth MA 02747 ; 'rheingold, arnold l.' ; department of chemistry and biochemistry mc 0358 university of california, san diego 9500 gilman drive la jolla, ca 92093 ; #============================================================================== _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'c56 h60 co f24 k2 o16' _chemical_formula_weight 1582.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'c' 'c' 0.0033 0.0016 'international tables vol c tables 4.2.6.8 and 6.1.1.4' 'h' 'h' 0.0000 0.0000 'international tables vol c tables 4.2.6.8 and 6.1.1.4' 'o' 'o' 0.0106 0.0060 'international tables vol c tables 4.2.6.8 and 6.1.1.4' 'k' 'k' 0.2009 0.2494 'international tables vol c tables 4.2.6.8 and 6.1.1.4' 'co' 'co' 0.3494 0.9721 'international tables vol c tables 4.2.6.8 and 6.1.1.4' 'f' 'f' 0.0171 0.0103 'international tables vol c tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_h-m C2/c 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 23.3983(13) _cell_length_b 12.7964(6) _cell_length_c 24.0070(13) _cell_angle_alpha 90.00 _cell_angle_beta 109.109(2) _cell_angle_gamma 90.00 _cell_volume 6792.0(6) _cell_formula_units_z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9816 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 28.21 _exptl_crystal_description Block _exptl_crystal_colour Blue _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.547 _exptl_crystal_density_method 'not measured' _exptl_crystal_f_000 3220 _exptl_absorpt_coefficient_mu 0.503 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_t_min 0.864 _exptl_absorpt_correction_t_max 1.000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21302 _diffrn_reflns_av_r_equivalents 0.0288 _diffrn_reflns_av_sigmai/neti 0.0361 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 28.31 _reflns_number_total 7978 _reflns_number_gt 6377 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; refinement of f^2^ against all reflections. The weighted R-factor wR and goodness of fit s are based on f^2^, conventional R-factors R are based on f, with f set to zero for negative F^2^. The threshold expression of f^2^ > 2sigma(f^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on f^2^ are statistically about twice as large as those based on F, and R- factors based on all data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(fo^2^)+(0.1049p)^2^+41.7239P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7978 _refine_ls_number_parameters 450 _refine_ls_number_restraints 0 _refine_ls_r_factor_all 0.0995 _refine_ls_r_factor_gt 0.0836 _refine_ls_wr_factor_ref 0.2250 _refine_ls_wr_factor_gt 0.2121 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_s_all 1.026 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_u_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group co1 co 0.0000 0.10668(5) 0.2500 0.02488(19) Uani 1 2 d S . . k1 k -0.08492(4) 0.17689(7) 0.10024(3) 0.0312(2) Uani 1 1 d . . . o1 o -0.06350(13) 0.0287(2) 0.19198(11) 0.0341(6) Uani 1 1 d . . . o2 o 0.02161(12) 0.1934(2) 0.19360(12) 0.0342(6) Uani 1 1 d . . . o3 o -0.11871(14) 0.2950(2) 0.17938(13) 0.0415(7) Uani 1 1 d . . . o4 o -0.21201(14) 0.1933(2) 0.09254(13) 0.0405(7) Uani 1 1 d . . . o5 o -0.17579(14) 0.0506(2) 0.02033(13) 0.0419(7) Uani 1 1 d . . . o6 o -0.06141(16) 0.0684(3) 0.00453(14) 0.0506(8) Uani 1 1 d . . . o7 o -0.06077(16) 0.2888(3) 0.00585(15) 0.0513(8) Uani 1 1 d . . . o8 o -0.06416(16) 0.3995(2) 0.10486(15) 0.0480(8) Uani 1 1 d . . . c1 c -0.08353(17) -0.0665(3) 0.19319(16) 0.0279(7) Uani 1 1 d . . . c2 c -0.06999(18) -0.1274(3) 0.24432(16) 0.0297(8) Uani 1 1 d . . . h2a h -0.0456 -0.0989 0.2809 0.036 Uiso 1 1 calc R . . c3 c -0.09150(19) -0.2283(3) 0.24235(17) 0.0330(8) Uani 1 1 d . . . c4 c -0.12734(19) -0.2739(3) 0.18987(18) 0.0352(9) Uani 1 1 d . . . h4a h -0.1421 -0.3433 0.1888 0.042 Uiso 1 1 calc R . . c5 c -0.14049(18) -0.2139(3) 0.13964(17) 0.0328(8) Uani 1 1 d . . . c6 c -0.12012(17) -0.1127(3) 0.14024(16) 0.0300(8) Uani 1 1 d . . . h6a h -0.1308 -0.0738 0.1046 0.036 Uiso 1 1 calc R . . c7 c -0.0760(3) -0.2911(4) 0.2982(2) 0.0478(11) Uani 1 1 d . . . c8 c -0.1769(2) -0.2586(4) 0.0810(2) 0.0461(11) Uani 1 1 d . . . c9 c 0.07325(17) 0.1986(3) 0.18374(16) 0.0298(8) Uani 1 1 d . . . c10 c 0.11671(18) 0.1179(3) 0.19965(17) 0.0329(8) Uani 1 1 d . . . h10a h 0.1088 0.0567 0.2184 0.039 Uiso 1 1 calc R . . c11 c 0.1708(2) 0.1272(3) 0.18814(19) 0.0380(9) Uani 1 1 d . . . c12 c 0.1845(2) 0.2150(4) 0.16111(19) 0.0402(9) Uani 1 1 d . . . h12a h 0.2215 0.2202 0.1530 0.048 Uiso 1 1 calc R . . c13 c 0.1423(2) 0.2946(3) 0.14631(18) 0.0385(9) Uani 1 1 d . . . c14 c 0.08766(18) 0.2878(3) 0.15696(17) 0.0332(8) Uani 1 1 d . . . h14a h 0.0597 0.3440 0.1460 0.040 Uiso 1 1 calc R . . c15 c 0.2149(2) 0.0389(4) 0.2054(2) 0.0517(12) Uani 1 1 d . . . c16 c 0.1549(2) 0.3896(4) 0.1162(2) 0.0496(11) Uani 1 1 d . . . c17 c -0.1805(2) 0.3092(4) 0.1740(2) 0.0514(12) Uani 1 1 d . . . h17a h -0.1980 0.3675 0.1466 0.062 Uiso 1 1 calc R . . h17b h -0.1842 0.3262 0.2129 0.062 Uiso 1 1 calc R . . c18 c -0.2132(2) 0.2106(5) 0.1511(2) 0.0541(13) Uani 1 1 d . . . h18a h -0.1937 0.1514 0.1768 0.065 Uiso 1 1 calc R . . h18b h -0.2556 0.2157 0.1506 0.065 Uiso 1 1 calc R . . c19 c -0.2449(2) 0.1024(4) 0.0679(3) 0.0533(13) Uani 1 1 d . . . h19a h -0.2883 0.1130 0.0626 0.064 Uiso 1 1 calc R . . h19b h -0.2302 0.0427 0.0950 0.064 Uiso 1 1 calc R . . c20 c -0.2375(2) 0.0786(4) 0.0100(2) 0.0533(13) Uani 1 1 d . . . h20a h -0.2644 0.0202 -0.0094 0.064 Uiso 1 1 calc R . . h20b h -0.2482 0.1406 -0.0161 0.064 Uiso 1 1 calc R . . c21 c -0.1665(3) 0.0137(4) -0.0316(2) 0.0571(14) Uani 1 1 d . . . h21a h -0.1765 0.0692 -0.0621 0.068 Uiso 1 1 calc R . . h21b h -0.1929 -0.0473 -0.0474 0.068 Uiso 1 1 calc R . . c22 c -0.1015(3) -0.0170(4) -0.0164(2) 0.0577(14) Uani 1 1 d . . . h22a h -0.0922 -0.0722 0.0142 0.069 Uiso 1 1 calc R . . h22b h -0.0947 -0.0467 -0.0518 0.069 Uiso 1 1 calc R . . c23 c -0.0541(3) 0.1295(5) -0.0421(2) 0.0631(15) Uani 1 1 d . . . h23a h -0.0941 0.1453 -0.0713 0.076 Uiso 1 1 calc R . . h23b h -0.0300 0.0904 -0.0622 0.076 Uiso 1 1 calc R . . c24 c -0.0226(3) 0.2283(5) -0.0173(2) 0.0606(14) Uani 1 1 d . . . h24a h 0.0158 0.2124 0.0144 0.073 Uiso 1 1 calc R . . h24b h -0.0131 0.2681 -0.0485 0.073 Uiso 1 1 calc R . . c25 c -0.0402(2) 0.3942(4) 0.0170(2) 0.0540(13) Uani 1 1 d . . . h25a h -0.0455 0.4303 -0.0208 0.065 Uiso 1 1 calc R . . h25b h 0.0034 0.3949 0.0403 0.065 Uiso 1 1 calc R . . c26 c -0.0747(2) 0.4495(4) 0.0496(2) 0.0553(13) Uani 1 1 d . . . h26a h -0.0617 0.5234 0.0557 0.066 Uiso 1 1 calc R . . h26b h -0.1184 0.4478 0.0268 0.066 Uiso 1 1 calc R . . c27 c -0.0888(3) 0.4552(4) 0.1428(2) 0.0546(13) Uani 1 1 d . . . h27a h -0.1318 0.4722 0.1220 0.066 Uiso 1 1 calc R . . h27b h -0.0664 0.5214 0.1556 0.066 Uiso 1 1 calc R . . c28 c -0.0834(2) 0.3876(4) 0.1953(2) 0.0522(12) Uani 1 1 d . . . h28a h -0.0405 0.3683 0.2145 0.063 Uiso 1 1 calc R . . h28b h -0.0968 0.4276 0.2241 0.063 Uiso 1 1 calc R . . f1 f -0.1075(4) -0.2642(7) 0.3330(4) 0.063(2) Uiso 0.514(16) 1 d P . . f2 f -0.0164(3) -0.2769(6) 0.3337(3) 0.052(2) Uiso 0.514(16) 1 d P . . f3 f -0.0876(4) -0.3926(5) 0.2895(3) 0.054(2) Uiso 0.514(16) 1 d P . . f1a f -0.1225(5) -0.2924(9) 0.3203(5) 0.077(3) Uiso 0.486(16) 1 d P . . f2a f -0.0318(4) -0.2496(7) 0.3422(3) 0.059(2) Uiso 0.486(16) 1 d P . . f3a f -0.0589(5) -0.3906(5) 0.2919(3) 0.055(2) Uiso 0.486(16) 1 d P . . f4 f -0.1369(3) -0.3080(6) 0.0562(3) 0.058(2) Uiso 0.521(12) 1 d P . . f5 f -0.2039(3) -0.1924(5) 0.0415(3) 0.056(2) Uiso 0.521(12) 1 d P . . f6 f -0.2151(3) -0.3364(5) 0.0866(3) 0.0477(17) Uiso 0.521(12) 1 d P . . f4a f -0.1509(4) -0.2619(8) 0.0430(4) 0.071(3) Uiso 0.479(12) 1 d P . . f5a f -0.2272(3) -0.1948(5) 0.0555(3) 0.050(2) Uiso 0.479(12) 1 d P . . f6a f -0.1964(4) -0.3537(6) 0.0828(3) 0.0514(19) Uiso 0.479(12) 1 d P . . f7 f 0.1848(4) -0.0573(7) 0.1811(4) 0.0359(19) Uiso 0.33 1 d P . . f8 f 0.2391(4) 0.0258(7) 0.2595(3) 0.0416(17) Uiso 0.33 1 d P . . f9 f 0.2589(4) 0.0468(7) 0.1773(5) 0.0330(18) Uiso 0.33 1 d P . . f7a f 0.2151(4) -0.0102(6) 0.2581(3) 0.0354(15) Uiso 0.33 1 d P . . f8a f 0.2690(5) 0.0528(9) 0.2089(6) 0.067(3) Uiso 0.33 1 d P . . f9a f 0.1972(6) -0.0466(10) 0.1699(5) 0.063(3) Uiso 0.33 1 d P . . f7b f 0.2008(7) -0.0405(13) 0.2200(8) 0.103(4) Uiso 0.33 1 d P . . f8b f 0.2663(5) 0.0765(9) 0.2527(5) 0.067(3) Uiso 0.33 1 d P . . f9b f 0.2436(7) 0.0255(11) 0.1672(6) 0.074(4) Uiso 0.33 1 d P . . f10 f 0.2128(3) 0.4181(6) 0.1367(4) 0.059(2) Uiso 0.534(17) 1 d P . . f11 f 0.1215(4) 0.4760(5) 0.1215(4) 0.056(2) Uiso 0.534(17) 1 d P . . f12 f 0.1411(5) 0.3780(6) 0.0592(3) 0.062(2) Uiso 0.534(17) 1 d P . . f10a f 0.2129(4) 0.3891(8) 0.1143(5) 0.070(3) Uiso 0.466(17) 1 d P . . f11a f 0.1463(5) 0.4755(6) 0.1399(5) 0.062(3) Uiso 0.466(17) 1 d P . . f12a f 0.1206(5) 0.3891(7) 0.0571(4) 0.056(2) Uiso 0.466(17) 1 d P . . 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 co1 0.0295(4) 0.0216(3) 0.0200(3) 0.000 0.0032(3) 0.000 k1 0.0327(4) 0.0319(4) 0.0245(4) 0.0037(3) 0.0032(3) -0.0031(3) o1 0.0430(16) 0.0258(13) 0.0250(12) 0.0000(10) -0.0007(11) -0.0076(11) o2 0.0248(13) 0.0399(15) 0.0342(14) 0.0127(12) 0.0048(11) 0.0003(11) o3 0.0447(17) 0.0396(16) 0.0348(15) -0.0002(12) 0.0058(13) 0.0058(13) o4 0.0398(16) 0.0427(17) 0.0356(15) 0.0064(13) 0.0077(13) -0.0064(13) o5 0.0416(16) 0.0424(17) 0.0334(15) 0.0006(13) 0.0010(13) -0.0074(13) o6 0.059(2) 0.060(2) 0.0344(16) -0.0012(15) 0.0183(15) -0.0055(17) o7 0.0497(19) 0.058(2) 0.0448(18) 0.0122(16) 0.0136(15) -0.0128(16) o8 0.0505(19) 0.0359(16) 0.0501(19) 0.0106(14) 0.0062(15) 0.0022(14) c1 0.0305(18) 0.0242(17) 0.0264(17) -0.0024(13) 0.0058(14) 0.0008(14) c2 0.0351(19) 0.0275(18) 0.0254(17) -0.0050(14) 0.0082(15) -0.0023(15) c3 0.042(2) 0.0300(19) 0.0282(18) 0.0009(15) 0.0125(16) -0.0021(16) c4 0.043(2) 0.0261(18) 0.039(2) -0.0041(15) 0.0166(18) -0.0082(16) c5 0.034(2) 0.0309(19) 0.0313(19) -0.0057(15) 0.0080(16) -0.0023(15) c6 0.0331(19) 0.0279(18) 0.0245(17) -0.0003(14) 0.0032(14) -0.0010(15) c7 0.075(3) 0.034(2) 0.038(2) 0.0023(18) 0.023(2) -0.007(2) c8 0.061(3) 0.037(2) 0.034(2) -0.0085(18) 0.008(2) -0.017(2) c9 0.0299(18) 0.0335(19) 0.0208(16) 0.0017(14) 0.0013(14) -0.0024(15) c10 0.037(2) 0.0307(19) 0.0292(18) 0.0022(15) 0.0084(16) -0.0010(16) c11 0.040(2) 0.040(2) 0.033(2) -0.0003(17) 0.0111(17) 0.0034(18) c12 0.036(2) 0.047(2) 0.038(2) -0.0003(18) 0.0145(18) -0.0038(18) c13 0.040(2) 0.042(2) 0.032(2) 0.0037(17) 0.0108(17) -0.0067(18) c14 0.035(2) 0.034(2) 0.0266(18) 0.0049(15) 0.0045(15) 0.0009(16) c15 0.051(3) 0.055(3) 0.054(3) 0.006(2) 0.024(2) 0.013(2) c16 0.049(3) 0.054(3) 0.051(3) 0.008(2) 0.023(2) -0.007(2) c17 0.051(3) 0.068(3) 0.034(2) 0.000(2) 0.013(2) 0.015(2) c18 0.046(3) 0.077(4) 0.041(2) 0.013(2) 0.017(2) -0.002(2) c19 0.035(2) 0.047(3) 0.074(4) 0.004(2) 0.013(2) -0.009(2) c20 0.040(3) 0.042(2) 0.058(3) -0.003(2) -0.011(2) -0.006(2) c21 0.071(4) 0.056(3) 0.037(2) -0.012(2) 0.008(2) -0.025(3) c22 0.083(4) 0.048(3) 0.046(3) -0.011(2) 0.026(3) -0.008(3) c23 0.073(4) 0.082(4) 0.038(3) -0.001(3) 0.024(3) -0.013(3) c24 0.063(3) 0.083(4) 0.044(3) 0.001(3) 0.027(3) -0.016(3) c25 0.047(3) 0.054(3) 0.054(3) 0.025(2) 0.007(2) -0.012(2) c26 0.048(3) 0.043(3) 0.063(3) 0.026(2) 0.004(2) -0.002(2) c27 0.058(3) 0.033(2) 0.064(3) -0.001(2) 0.008(3) 0.001(2) c28 0.056(3) 0.044(3) 0.043(2) -0.009(2) -0.002(2) 0.004(2) _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 co1 o2 1.941(3) 2 ? co1 o2 1.941(3) . ? co1 o1 1.947(3) . ? co1 o1 1.947(3) 2 ? co1 k1 3.6060(8) 2 ? co1 k1 3.6060(8) . ? k1 o3 2.739(3) . ? k1 o2 2.761(3) . ? k1 o1 2.824(3) . ? k1 o5 2.854(3) . ? k1 o8 2.886(3) . ? k1 o6 2.888(3) . ? k1 o7 2.889(3) . ? k1 o4 2.926(3) . ? k1 c28 3.524(5) . ? o1 c1 1.309(4) . ? o2 c9 1.307(5) . ? o3 c17 1.421(6) . ? o3 c28 1.423(6) . ? o4 c19 1.413(6) . ? o4 c18 1.432(6) . ? o5 c21 1.415(6) . ? o5 c20 1.428(6) . ? o6 c22 1.420(6) . ? o6 c23 1.422(6) . ? o7 c24 1.424(7) . ? o7 c25 1.427(6) . ? o8 c26 1.419(6) . ? o8 c27 1.419(7) . ? c1 c2 1.400(5) . ? c1 c6 1.409(5) . ? c2 c3 1.381(5) . ? c3 c4 1.392(6) . ? c3 c7 1.501(6) . ? c4 c5 1.377(6) . ? c5 c6 1.378(5) . ? c5 c8 1.501(6) . ? c7 f2a 1.324(9) . ? c7 f1 1.328(9) . ? c7 f3 1.329(8) . ? c7 f3a 1.358(8) . ? c7 f1a 1.358(11) . ? c7 f2 1.389(9) . ? c8 f4a 1.253(9) . ? c8 f5 1.274(8) . ? c8 f6a 1.305(8) . ? c8 f6 1.374(8) . ? c8 f5a 1.397(9) . ? c8 f4 1.412(9) . ? c9 c14 1.404(5) . ? c9 c10 1.412(5) . ? c10 c11 1.386(6) . ? c11 c12 1.386(6) . ? c11 c15 1.494(7) . ? c12 c13 1.382(6) . ? c13 c14 1.386(6) . ? c13 c16 1.493(6) . ? c15 f7b 1.157(16) . ? c15 f8 1.247(9) . ? c15 f8a 1.254(12) . ? c15 f9b 1.315(15) . ? c15 f9a 1.366(13) . ? c15 f9 1.408(10) . ? c15 f7a 1.411(9) . ? c15 f8b 1.439(12) . ? c15 f7 1.444(11) . ? c16 f11a 1.284(9) . ? c16 f12 1.307(9) . ? c16 f10 1.332(8) . ? c16 f10a 1.371(10) . ? c16 f12a 1.383(10) . ? c16 f11 1.384(9) . ? c17 c18 1.485(8) . ? c19 c20 1.487(8) . ? c21 c22 1.498(8) . ? c23 c24 1.485(8) . ? c25 c26 1.477(8) . ? c27 c28 1.499(7) . ? f1 f1a 0.524(12) . ? f1 f2a 1.721(11) . ? f2 f2a 0.586(8) . ? f3 f3a 0.655(8) . ? f4 f4a 0.698(9) . ? f5 f5a 0.730(7) . ? f5 f4a 1.517(11) . ? f6 f6a 0.525(8) . ? f7 f7b 0.909(17) . ? f8 f7a 0.719(9) . ? f8 f8b 0.960(12) . ? f8 f7b 1.37(2) . ? f8 f8a 1.627(16) . ? f9 f8a 0.721(12) . ? f7a f7b 0.948(17) . ? f7a f8b 1.669(13) . ? f8a f9b 1.043(18) . ? f8a f8b 1.116(15) . ? f9a f7b 1.18(2) . ? f9a f9b 1.445(19) . ? f10 f10a 0.653(9) . ? f10 f11a 1.745(11) . ? f11 f11a 0.605(9) . ? f12 f10a 1.771(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 o2 co1 o2 110.27(18) 2 . ? o2 co1 o1 118.69(12) 2 . ? o2 co1 o1 96.10(12) . . ? o2 co1 o1 96.10(12) 2 2 ? o2 co1 o1 118.69(12) . 2 ? o1 co1 o1 118.29(16) . 2 ? o2 co1 k1 49.20(8) 2 2 ? o2 co1 k1 111.63(9) . 2 ? o1 co1 k1 152.07(8) . 2 ? o1 co1 k1 51.10(8) 2 2 ? o2 co1 k1 111.63(9) 2 . ? o2 co1 k1 49.20(8) . . ? o1 co1 k1 51.10(8) . . ? o1 co1 k1 152.07(8) 2 . ? k1 co1 k1 151.15(3) 2 . ? o3 k1 o2 77.50(9) . . ? o3 k1 o1 81.24(9) . . ? o2 k1 o1 62.35(8) . . ? o3 k1 o5 117.27(10) . . ? o2 k1 o5 149.90(9) . . ? o1 k1 o5 92.68(8) . . ? o3 k1 o8 60.77(10) . . ? o2 k1 o8 78.31(9) . . ? o1 k1 o8 130.42(9) . . ? o5 k1 o8 131.59(10) . . ? o3 k1 o6 172.19(10) . . ? o2 k1 o6 109.04(10) . . ? o1 k1 o6 105.43(9) . . ? o5 k1 o6 59.12(10) . . ? o8 k1 o6 115.59(11) . . ? o3 k1 o7 116.45(11) . . ? o2 k1 o7 104.03(9) . . ? o1 k1 o7 156.12(10) . . ? o5 k1 o7 92.72(10) . . ? o8 k1 o7 57.79(11) . . ? o6 k1 o7 58.47(11) . . ? o3 k1 o4 59.08(9) . . ? o2 k1 o4 132.42(9) . . ? o1 k1 o4 90.84(9) . . ? o5 k1 o4 58.66(9) . . ? o8 k1 o4 94.96(10) . . ? o6 k1 o4 116.01(10) . . ? o7 k1 o4 111.75(10) . . ? o3 k1 c28 22.01(12) . . ? o2 k1 c28 66.47(11) . . ? o1 k1 c28 92.71(10) . . ? o5 k1 c28 135.71(12) . . ? o8 k1 c28 41.77(12) . . ? o6 k1 c28 156.76(12) . . ? o7 k1 c28 99.53(12) . . ? o4 k1 c28 77.33(11) . . ? o3 k1 co1 68.65(6) . . ? o2 k1 co1 32.16(6) . . ? o1 k1 co1 32.44(5) . . ? o5 k1 co1 125.12(7) . . ? o8 k1 co1 100.18(7) . . ? o6 k1 co1 119.16(8) . . ? o7 k1 co1 136.07(7) . . ? o4 k1 co1 107.32(6) . . ? c28 k1 co1 70.10(8) . . ? c1 o1 co1 131.0(2) . . ? c1 o1 k1 132.0(2) . . ? co1 o1 k1 96.46(10) . . ? c9 o2 co1 128.5(2) . . ? c9 o2 k1 120.0(2) . . ? co1 o2 k1 98.64(10) . . ? c17 o3 c28 113.8(4) . . ? c17 o3 k1 121.6(3) . . ? c28 o3 k1 111.8(3) . . ? c19 o4 c18 110.8(4) . . ? c19 o4 k1 111.7(3) . . ? c18 o4 k1 107.2(3) . . ? c21 o5 c20 111.6(4) . . ? c21 o5 k1 119.1(3) . . ? c20 o5 k1 117.6(3) . . ? c22 o6 c23 112.4(4) . . ? c22 o6 k1 112.1(3) . . ? c23 o6 k1 117.7(3) . . ? c24 o7 c25 111.8(4) . . ? c24 o7 k1 110.2(3) . . ? c25 o7 k1 117.5(3) . . ? c26 o8 c27 113.0(4) . . ? c26 o8 k1 115.7(3) . . ? c27 o8 k1 115.0(3) . . ? o1 c1 c2 123.9(3) . . ? o1 c1 c6 119.1(3) . . ? c2 c1 c6 117.0(3) . . ? c3 c2 c1 121.0(3) . . ? c2 c3 c4 121.8(4) . . ? c2 c3 c7 119.4(4) . . ? c4 c3 c7 118.8(4) . . ? c5 c4 c3 117.1(4) . . ? c4 c5 c6 122.5(4) . . ? c4 c5 c8 120.3(4) . . ? c6 c5 c8 117.1(4) . . ? c5 c6 c1 120.6(4) . . ? f2a c7 f1 81.0(6) . . ? f2a c7 f3 125.6(6) . . ? f1 c7 f3 103.0(6) . . ? f2a c7 f3a 106.5(6) . . ? f1 c7 f3a 123.9(6) . . ? f3 c7 f3a 28.2(3) . . ? f2a c7 f1a 102.0(6) . . ? f1 c7 f1a 22.5(5) . . ? f3 c7 f1a 84.3(6) . . ? f3a c7 f1a 109.6(6) . . ? f2a c7 f2 24.8(4) . . ? f1 c7 f2 103.5(6) . . ? f3 c7 f2 109.6(6) . . ? f3a c7 f2 85.3(5) . . ? f1a c7 f2 122.2(6) . . ? f2a c7 c3 113.3(5) . . ? f1 c7 c3 113.7(5) . . ? f3 c7 c3 114.0(5) . . ? f3a c7 c3 113.3(5) . . ? f1a c7 c3 111.5(6) . . ? f2 c7 c3 112.2(4) . . ? f4a c8 f5 73.7(6) . . ? f4a c8 f6a 104.5(6) . . ? f5 c8 f6a 123.5(6) . . ? f4a c8 f6 122.3(6) . . ? f5 c8 f6 112.1(5) . . ? f6a c8 f6 22.4(4) . . ? f4a c8 f5a 104.0(6) . . ? f5 c8 f5a 31.3(3) . . ? f6a c8 f5a 107.9(6) . . ? f6 c8 f5a 89.2(5) . . ? f4a c8 f4 29.6(4) . . ? f5 c8 f4 102.6(5) . . ? f6a c8 f4 83.3(5) . . ? f6 c8 f4 105.1(5) . . ? f5a c8 f4 131.0(5) . . ? f4a c8 c5 115.7(5) . . ? f5 c8 c5 115.8(4) . . ? f6a c8 c5 114.9(5) . . ? f6 c8 c5 111.8(4) . . ? f5a c8 c5 109.0(4) . . ? f4 c8 c5 108.3(5) . . ? o2 c9 c14 120.0(4) . . ? o2 c9 c10 122.7(3) . . ? c14 c9 c10 117.3(4) . . ? c11 c10 c9 120.5(4) . . ? c12 c11 c10 121.9(4) . . ? c12 c11 c15 119.9(4) . . ? c10 c11 c15 118.2(4) . . ? c13 c12 c11 117.6(4) . . ? c12 c13 c14 122.0(4) . . ? c12 c13 c16 119.2(4) . . ? c14 c13 c16 118.8(4) . . ? c13 c14 c9 120.6(4) . . ? f7b c15 f8 69.2(10) . . ? f7b c15 f8a 119.1(10) . . ? f8 c15 f8a 81.2(8) . . ? f7b c15 f9b 111.0(12) . . ? f8 c15 f9b 123.3(8) . . ? f8a c15 f9b 47.8(8) . . ? f7b c15 f9a 55.0(10) . . ? f8 c15 f9a 118.9(8) . . ? f8a c15 f9a 104.4(9) . . ? f9b c15 f9a 65.2(9) . . ? f7b c15 f9 122.3(10) . . ? f8 c15 f9 110.9(7) . . ? f8a c15 f9 30.8(6) . . ? f9b c15 f9 18.7(7) . . ? f9a c15 f9 83.0(8) . . ? f7b c15 f7a 41.9(9) . . ? f8 c15 f7a 30.6(4) . . ? f8a c15 f7a 107.3(8) . . ? f9b c15 f7a 135.7(8) . . ? f9a c15 f7a 96.5(7) . . ? f9 c15 f7a 132.4(6) . . ? f7b c15 f8b 107.7(11) . . ? f8 c15 f8b 41.1(5) . . ? f8a c15 f8b 48.4(7) . . ? f9b c15 f8b 96.2(8) . . ? f9a c15 f8b 139.9(8) . . ? f9 c15 f8b 78.5(7) . . ? f7a c15 f8b 71.7(6) . . ? f7b c15 f7 39.0(9) . . ? f8 c15 f7 107.5(7) . . ? f8a c15 f7 119.7(8) . . ? f9b c15 f7 84.3(8) . . ? f9a c15 f7 19.2(6) . . ? f9 c15 f7 101.7(7) . . ? f7a c15 f7 80.8(6) . . ? f8b c15 f7 140.8(7) . . ? f7b c15 c11 120.5(9) . . ? f8 c15 c11 115.3(5) . . ? f8a c15 c11 120.1(7) . . ? f9b c15 c11 111.7(7) . . ? f9a c15 c11 113.0(7) . . ? f9 c15 c11 111.1(5) . . ? f7a c15 c11 112.6(5) . . ? f8b c15 c11 106.8(6) . . ? f7 c15 c11 109.4(5) . . ? f11a c16 f12 122.7(7) . . ? f11a c16 f10 83.7(6) . . ? f12 c16 f10 106.9(6) . . ? f11a c16 f10a 108.6(7) . . ? f12 c16 f10a 82.7(6) . . ? f10 c16 f10a 27.9(4) . . ? f11a c16 f12a 109.6(7) . . ? f12 c16 f12a 20.7(4) . . ? f10 c16 f12a 124.1(6) . . ? f10a c16 f12a 102.5(6) . . ? f11a c16 f11 25.9(4) . . ? f12 c16 f11 103.5(6) . . ? f10 c16 f11 106.5(6) . . ? f10a c16 f11 127.0(6) . . ? f12a c16 f11 86.6(6) . . ? f11a c16 c13 113.4(5) . . ? f12 c16 c13 113.2(5) . . ? f10 c16 c13 112.5(5) . . ? f10a c16 c13 111.5(5) . . ? f12a c16 c13 110.7(5) . . ? f11 c16 c13 113.5(4) . . ? o3 c17 c18 108.1(4) . . ? o4 c18 c17 108.8(4) . . ? o4 c19 c20 110.2(4) . . ? o5 c20 c19 108.0(4) . . ? o5 c21 c22 108.0(4) . . ? o6 c22 c21 112.6(4) . . ? o6 c23 c24 108.9(4) . . ? o7 c24 c23 109.1(5) . . ? o7 c25 c26 110.0(4) . . ? o8 c26 c25 108.8(4) . . ? o8 c27 c28 108.0(4) . . ? o3 c28 c27 111.9(4) . . ? o3 c28 k1 46.2(2) . . ? c27 c28 k1 85.3(3) . . ? f1a f1 c7 82.0(17) . . ? f1a f1 f2a 127.8(19) . . ? c7 f1 f2a 49.4(4) . . ? f2a f2 c7 71.4(11) . . ? f3a f3 c7 78.3(10) . . ? f1 f1a c7 75.5(17) . . ? f2 f2a c7 83.8(12) . . ? f2 f2a f1 128.1(13) . . ? c7 f2a f1 49.6(4) . . ? f3 f3a c7 73.5(10) . . ? f4a f4 c8 62.5(10) . . ? f5a f5 c8 83.7(9) . . ? f5a f5 f4a 133.9(10) . . ? c8 f5 f4a 52.5(5) . . ? f6a f6 c8 71.4(12) . . ? f4 f4a c8 87.9(11) . . ? f4 f4a f5 139.8(13) . . ? c8 f4a f5 53.8(5) . . ? f5 f5a c8 65.0(8) . . ? f6 f6a c8 86.2(13) . . ? f7b f7 c15 53.2(11) . . ? f7a f8 f8b 167.6(16) . . ? f7a f8 c15 87.4(11) . . ? f8b f8 c15 80.2(9) . . ? f7a f8 f7b 40.8(10) . . ? f8b f8 f7b 128.4(13) . . ? c15 f8 f7b 52.3(8) . . ? f7a f8 f8a 128.3(12) . . ? f8b f8 f8a 42.0(8) . . ? c15 f8 f8a 49.6(6) . . ? f7b f8 f8a 87.5(9) . . ? f8a f9 c15 62.7(12) . . ? f8 f7a f7b 109.5(16) . . ? f8 f7a c15 62.0(9) . . ? f7b f7a c15 54.6(11) . . ? f8 f7a f8b 7.1(9) . . ? f7b f7a f8b 103.5(13) . . ? c15 f7a f8b 54.9(5) . . ? f9 f8a f9b 21.0(13) . . ? f9 f8a f8b 157.0(18) . . ? f9b f8a f8b 143.7(15) . . ? f9 f8a c15 86.5(14) . . ? f9b f8a c15 69.2(10) . . ? f8b f8a c15 74.5(10) . . ? f9 f8a f8 133.7(16) . . ? f9b f8a f8 113.4(13) . . ? f8b f8a f8 35.1(7) . . ? c15 f8a f8 49.3(6) . . ? f7b f9a c15 53.5(10) . . ? f7b f9a f9b 101.5(14) . . ? c15 f9a f9b 55.7(8) . . ? f7 f7b f7a 169(2) . . ? f7 f7b c15 87.8(15) . . ? f7a f7b c15 83.5(14) . . ? f7 f7b f9a 21.8(10) . . ? f7a f7b f9a 154(2) . . ? c15 f7b f9a 71.6(11) . . ? f7 f7b f8 144.6(19) . . ? f7a f7b f8 29.7(8) . . ? c15 f7b f8 58.5(9) . . ? f9a f7b f8 124.2(15) . . ? f8 f8b f8a 102.9(13) . . ? f8 f8b c15 58.7(8) . . ? f8a f8b c15 57.1(8) . . ? f8 f8b f7a 5.3(7) . . ? f8a f8b f7a 99.0(10) . . ? c15 f8b f7a 53.4(5) . . ? f8a f9b c15 63.0(10) . . ? f8a f9b f9a 111.8(15) . . ? c15 f9b f9a 59.1(8) . . ? f10a f10 c16 79.4(11) . . ? f10a f10 f11a 121.2(13) . . ? c16 f10 f11a 47.0(4) . . ? f11a f11 c16 67.8(11) . . ? c16 f12 f10a 50.2(5) . . ? f10 f10a c16 72.7(12) . . ? f10 f10a f12 113.8(13) . . ? c16 f10a f12 47.1(4) . . ? f11 f11a c16 86.3(13) . . ? f11 f11a f10 129.0(14) . . ? c16 f11a f10 49.3(4) . . ? _diffrn_measured_fraction_theta_max 0.944 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.944 _refine_diff_density_max 1.462 _refine_diff_density_min -0.834 _refine_diff_density_rms 0.100 #===end