data_Compound4 _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 h72 cu f20 n2 o4' _chemical_formula_weight 1280.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'c' 'c' 0.0033 0.0016 'international tables vol c tables 4.2.6.8 and 6.1.1.4' 'h' 'h' 0.0000 0.0000 'international tables vol c tables 4.2.6.8 and 6.1.1.4' 'n' 'n' 0.0061 0.0033 'international tables vol c tables 4.2.6.8 and 6.1.1.4' 'o' 'o' 0.0106 0.0060 'international tables vol c tables 4.2.6.8 and 6.1.1.4' 'f' 'f' 0.0171 0.0103 'international tables vol c tables 4.2.6.8 and 6.1.1.4' 'cu' 'cu' 0.3201 1.2651 'international tables vol c tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_h-m Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 15.0601(9) _cell_length_b 17.5377(11) _cell_length_c 22.8468(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6034.3(7) _cell_formula_units_z 4 _cell_measurement_temperature 218(2) _cell_measurement_reflns_used 6300 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 26.49 _exptl_crystal_description Block _exptl_crystal_colour Green _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.410 _exptl_crystal_density_method 'not measured' _exptl_crystal_f_000 2652 _exptl_absorpt_coefficient_mu 0.469 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_t_min 0.825 _exptl_absorpt_correction_t_max 1.000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 218(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 36069 _diffrn_reflns_av_r_equivalents 0.0313 _diffrn_reflns_av_sigmai/neti 0.0301 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 28.32 _reflns_number_total 7277 _reflns_number_gt 4867 _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. the h atoms of the disordered ch2CH3 group in a (nBu4N)+ cation have not been taken in consideration. ; _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^)+(0.0988p)^2^+1.1784P] 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 7277 _refine_ls_number_parameters 376 _refine_ls_number_restraints 0 _refine_ls_r_factor_all 0.0763 _refine_ls_r_factor_gt 0.0505 _refine_ls_wr_factor_ref 0.1722 _refine_ls_wr_factor_gt 0.1509 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_s_all 1.030 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_u_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group cu1 cu 0.0000 0.0000 0.5000 0.04710(14) Uani 1 2 d S . . o1 o 0.10676(11) 0.03385(12) 0.46171(7) 0.0690(5) Uani 1 1 d . . . o2 o -0.07511(10) 0.03483(9) 0.43693(7) 0.0563(4) Uani 1 1 d . . . c1 c 0.11831(13) 0.03930(13) 0.40557(10) 0.0505(5) Uani 1 1 d . . . c2 c 0.09484(16) -0.01674(15) 0.36556(14) 0.0643(7) Uani 1 1 d . . . c3 c 0.1057(2) -0.0093(2) 0.30645(15) 0.0802(9) Uani 1 1 d . . . c4 c 0.1427(2) 0.0557(2) 0.28376(12) 0.0851(10) Uani 1 1 d . . . c5 c 0.16757(17) 0.11219(17) 0.32104(12) 0.0679(7) Uani 1 1 d . . . c6 c 0.15602(14) 0.10355(13) 0.37995(10) 0.0527(5) Uani 1 1 d . . . c7 c -0.06707(12) 0.09925(12) 0.40930(9) 0.0445(4) Uani 1 1 d . . . c8 c -0.09178(14) 0.10673(14) 0.35062(10) 0.0535(5) Uani 1 1 d . . . c9 c -0.08407(17) 0.17348(17) 0.32044(10) 0.0645(7) Uani 1 1 d . . . c10 c -0.05010(17) 0.23724(16) 0.34671(13) 0.0676(7) Uani 1 1 d . . . c11 c -0.02560(16) 0.23295(14) 0.40359(13) 0.0613(6) Uani 1 1 d . . . c12 c -0.03482(14) 0.16622(14) 0.43400(9) 0.0504(5) Uani 1 1 d . . . f1 f 0.05844(13) -0.08137(9) 0.38738(11) 0.1033(7) Uani 1 1 d . . . f2 f 0.08087(16) -0.06648(16) 0.27082(11) 0.1390(10) Uani 1 1 d . . . f3 f 0.15473(18) 0.06414(19) 0.22533(8) 0.1410(10) Uani 1 1 d . . . f4 f 0.20342(14) 0.17637(12) 0.29955(9) 0.1103(7) Uani 1 1 d . . . f5 f 0.17976(11) 0.16217(9) 0.41463(7) 0.0793(5) Uani 1 1 d . . . f6 f -0.12464(13) 0.04526(10) 0.32284(7) 0.0829(5) Uani 1 1 d . . . f7 f -0.11005(16) 0.17738(13) 0.26432(7) 0.1105(7) Uani 1 1 d . . . f8 f -0.04356(14) 0.30347(11) 0.31674(10) 0.1091(7) Uani 1 1 d . . . f9 f 0.00617(12) 0.29531(10) 0.43127(11) 0.0958(6) Uani 1 1 d . . . f10 f -0.01151(11) 0.16517(11) 0.49130(6) 0.0739(5) Uani 1 1 d . . . n1 n -0.16373(12) -0.20871(11) 0.38137(8) 0.0529(4) Uani 1 1 d . . . c13 c -0.18162(17) -0.13406(14) 0.41290(11) 0.0616(6) Uani 1 1 d . . . h13a h -0.1452 -0.0940 0.3951 0.074 Uiso 1 1 calc R . . h13b h -0.1630 -0.1393 0.4538 0.074 Uiso 1 1 calc R . . c14 c -0.2784(2) -0.1092(2) 0.41145(17) 0.0922(10) Uani 1 1 d . . . h14a h -0.2968 -0.1030 0.3706 0.111 Uiso 1 1 calc R . . h14b h -0.3150 -0.1496 0.4287 0.111 Uiso 1 1 calc R . . c15 c -0.2953(2) -0.0381(2) 0.4427(2) 0.1075(13) Uani 1 1 d . . . h15a h -0.2587 0.0023 0.4254 0.129 Uiso 1 1 calc R . . h15b h -0.2769 -0.0442 0.4836 0.129 Uiso 1 1 calc R . . c16 c -0.3905(3) -0.0136(2) 0.4412(3) 0.1272(17) Uani 1 1 d . . . h16a h -0.3970 0.0343 0.4620 0.191 Uiso 1 1 calc R . . h16b h -0.4270 -0.0522 0.4598 0.191 Uiso 1 1 calc R . . h16c h -0.4092 -0.0071 0.4009 0.191 Uiso 1 1 calc R . . c17 c -0.21637(16) -0.27274(15) 0.40918(11) 0.0604(6) Uani 1 1 d . . . h17a h -0.2091 -0.3188 0.3854 0.072 Uiso 1 1 calc R . . h17b h -0.2794 -0.2590 0.4086 0.072 Uiso 1 1 calc R . . c18 c -0.18989(18) -0.29101(17) 0.47171(12) 0.0711(7) Uani 1 1 d . . . h18a h -0.1325 -0.3174 0.4716 0.085 Uiso 1 1 calc R . . h18b h -0.1827 -0.2433 0.4935 0.085 Uiso 1 1 calc R . . c19 c -0.2570(2) -0.3397(2) 0.50198(13) 0.0842(9) Uani 1 1 d . . . h19a h -0.2689 -0.3848 0.4779 0.101 Uiso 1 1 calc R . . h19b h -0.3126 -0.3111 0.5057 0.101 Uiso 1 1 calc R . . c20 c -0.2275(3) -0.3648(2) 0.56138(15) 0.1095(13) Uani 1 1 d . . . h20a h -0.2734 -0.3959 0.5791 0.164 Uiso 1 1 calc R . . h20b h -0.2166 -0.3205 0.5857 0.164 Uiso 1 1 calc R . . h20c h -0.1733 -0.3944 0.5579 0.164 Uiso 1 1 calc R . . c21 c -0.19073(18) -0.20366(15) 0.31749(11) 0.0626(6) Uani 1 1 d . . . h21a h -0.1783 -0.2527 0.2987 0.075 Uiso 1 1 calc R . . h21b h -0.2549 -0.1950 0.3154 0.075 Uiso 1 1 calc R . . c22 c -0.1445(2) -0.1416(2) 0.28356(12) 0.0813(8) Uani 1 1 d . . . h22a h -0.1456 -0.0946 0.3067 0.098 Uiso 1 1 calc R . . h22b h -0.0821 -0.1561 0.2782 0.098 Uiso 1 1 calc R . . c23 c -0.1842(3) -0.1259(2) 0.22522(15) 0.1018(11) Uani 1 1 d . . . h23a h -0.2477 -0.1152 0.2302 0.122 Uiso 1 1 calc R . . h23b h -0.1787 -0.1716 0.2008 0.122 Uiso 1 1 calc R . . c24 c -0.1417(3) -0.0602(2) 0.19430(15) 0.1027(12) Uani 1 1 d . . . h24a h -0.1709 -0.0521 0.1570 0.154 Uiso 1 1 calc R . . h24b h -0.0794 -0.0713 0.1877 0.154 Uiso 1 1 calc R . . h24c h -0.1471 -0.0147 0.2181 0.154 Uiso 1 1 calc R . . c25 c -0.06486(15) -0.22455(14) 0.38648(10) 0.0566(6) Uani 1 1 d . . . h25a h -0.0327 -0.1821 0.3683 0.068 Uiso 1 1 calc R . . h25b h -0.0491 -0.2251 0.4281 0.068 Uiso 1 1 calc R . . c26 c -0.0325(2) -0.29796(18) 0.35925(14) 0.0757(8) Uani 1 1 d . . . h26a h -0.0383 -0.2951 0.3166 0.091 Uiso 1 1 calc R . . h26b h -0.0688 -0.3407 0.3732 0.091 Uiso 1 1 calc R . . c27 c 0.0651(2) -0.3111(2) 0.37585(19) 0.1093(13) Uani 1 1 d . . . c28 c 0.0821(5) -0.3396(5) 0.4281(4) 0.112(3) Uiso 0.572(9) 1 d P . . c28a c 0.0937(5) -0.3904(5) 0.3730(4) 0.088(3) Uiso 0.428(9) 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 cu1 0.0468(2) 0.0518(3) 0.0427(2) 0.01206(16) -0.00446(14) -0.00560(14) o1 0.0539(9) 0.1031(14) 0.0499(9) 0.0217(9) -0.0040(7) -0.0174(9) o2 0.0555(8) 0.0589(10) 0.0545(9) 0.0159(8) -0.0115(7) -0.0089(7) c1 0.0439(10) 0.0569(13) 0.0507(12) 0.0094(10) -0.0015(9) -0.0004(9) c2 0.0572(13) 0.0526(14) 0.0831(19) 0.0010(13) -0.0063(12) -0.0001(10) c3 0.0714(17) 0.091(2) 0.078(2) -0.0363(18) -0.0104(15) 0.0117(15) c4 0.0801(18) 0.132(3) 0.0435(14) -0.0017(17) 0.0044(13) 0.0263(19) c5 0.0686(14) 0.0727(17) 0.0624(16) 0.0213(14) 0.0146(12) 0.0116(13) c6 0.0513(11) 0.0528(13) 0.0539(13) 0.0018(11) 0.0063(9) -0.0004(9) c7 0.0415(9) 0.0530(12) 0.0390(10) 0.0055(9) 0.0004(8) 0.0007(8) c8 0.0586(12) 0.0605(14) 0.0413(11) -0.0046(10) -0.0036(9) 0.0057(10) c9 0.0728(15) 0.0822(19) 0.0385(12) 0.0161(12) 0.0031(10) 0.0140(13) c10 0.0625(13) 0.0613(16) 0.0789(18) 0.0286(14) 0.0145(13) 0.0094(12) c11 0.0531(11) 0.0491(14) 0.0816(18) 0.0008(13) 0.0005(12) 0.0000(10) c12 0.0494(10) 0.0594(14) 0.0423(11) -0.0014(10) -0.0038(9) 0.0001(9) f1 0.0892(12) 0.0576(10) 0.163(2) 0.0048(11) -0.0069(12) -0.0191(8) f2 0.1172(17) 0.162(2) 0.138(2) -0.0951(18) -0.0189(14) 0.0066(15) f3 0.1379(19) 0.239(3) 0.0464(10) 0.0070(14) 0.0096(11) 0.0397(19) f4 0.1174(15) 0.1023(14) 0.1112(16) 0.0564(12) 0.0349(12) -0.0001(11) f5 0.0797(10) 0.0718(10) 0.0865(11) -0.0187(9) 0.0166(8) -0.0197(8) f6 0.1075(13) 0.0813(12) 0.0599(9) -0.0160(8) -0.0278(9) 0.0005(9) f7 0.1425(17) 0.1447(19) 0.0444(9) 0.0300(10) -0.0090(10) 0.0196(14) f8 0.1075(14) 0.0867(13) 0.1330(17) 0.0630(12) 0.0163(13) 0.0083(10) f9 0.0882(12) 0.0562(10) 0.1429(18) -0.0098(11) -0.0140(10) -0.0098(8) f10 0.0860(11) 0.0859(12) 0.0499(8) -0.0112(7) -0.0196(7) -0.0032(8) n1 0.0568(10) 0.0537(11) 0.0481(10) -0.0089(8) -0.0076(8) -0.0046(8) c13 0.0714(14) 0.0582(14) 0.0553(14) -0.0146(12) -0.0026(11) -0.0009(11) c14 0.0792(19) 0.085(2) 0.112(3) -0.027(2) -0.0056(17) 0.0142(16) c15 0.082(2) 0.097(3) 0.144(3) -0.041(2) 0.002(2) 0.0107(18) c16 0.091(3) 0.099(3) 0.191(5) -0.027(3) 0.010(3) 0.023(2) c17 0.0570(12) 0.0620(14) 0.0622(15) -0.0082(12) -0.0081(11) -0.0100(10) c18 0.0731(15) 0.0787(18) 0.0615(16) 0.0034(14) -0.0112(13) -0.0212(13) c19 0.0734(18) 0.097(2) 0.082(2) 0.0117(17) -0.0089(14) -0.0281(17) c20 0.108(3) 0.136(3) 0.085(2) 0.035(2) -0.0119(19) -0.057(2) c21 0.0692(14) 0.0678(16) 0.0508(13) -0.0111(11) -0.0136(11) 0.0003(12) c22 0.097(2) 0.093(2) 0.0536(16) 0.0042(15) -0.0107(14) -0.0077(17) c23 0.138(3) 0.089(2) 0.078(2) 0.0131(19) -0.035(2) -0.002(2) c24 0.152(4) 0.092(2) 0.064(2) 0.0078(18) -0.022(2) 0.008(2) c25 0.0526(11) 0.0650(15) 0.0521(13) -0.0069(11) -0.0069(10) -0.0061(10) c26 0.0708(15) 0.078(2) 0.0781(19) -0.0077(15) -0.0042(14) 0.0092(14) c27 0.086(2) 0.120(3) 0.122(3) -0.001(2) -0.012(2) 0.038(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 cu1 o1 1.9243(16) . ? cu1 o1 1.9243(16) 5_556 ? cu1 o2 1.9311(15) . ? cu1 o2 1.9311(15) 5_556 ? o1 c1 1.298(3) . ? o2 c7 1.300(3) . ? c1 c2 1.388(4) . ? c1 c6 1.391(3) . ? c2 f1 1.354(3) . ? c2 c3 1.366(4) . ? c3 f2 1.344(3) . ? c3 c4 1.371(5) . ? c4 f3 1.355(3) . ? c4 c5 1.359(5) . ? c5 f4 1.341(3) . ? c5 c6 1.366(3) . ? c6 f5 1.346(3) . ? c7 c12 1.391(3) . ? c7 c8 1.397(3) . ? c8 f6 1.345(3) . ? c8 c9 1.364(4) . ? c9 f7 1.342(3) . ? c9 c10 1.368(4) . ? c10 f8 1.352(3) . ? c10 c11 1.353(4) . ? c11 f9 1.351(3) . ? c11 c12 1.368(3) . ? c12 f10 1.355(3) . ? n1 c17 1.514(3) . ? n1 c21 1.518(3) . ? n1 c13 1.518(3) . ? n1 c25 1.519(3) . ? c13 c14 1.522(4) . ? c14 c15 1.459(4) . ? c15 c16 1.498(5) . ? c17 c18 1.517(3) . ? c18 c19 1.493(4) . ? c19 c20 1.494(4) . ? c21 c22 1.507(4) . ? c22 c23 1.487(4) . ? c23 c24 1.496(5) . ? c25 c26 1.511(4) . ? c26 c27 1.536(5) . ? c27 c28 1.319(8) . ? c27 c28a 1.457(9) . ? c28 c28a 1.552(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 o1 cu1 o1 180.00(5) . 5_556 ? o1 cu1 o2 93.02(7) . . ? o1 cu1 o2 86.98(7) 5_556 . ? o1 cu1 o2 86.98(7) . 5_556 ? o1 cu1 o2 93.02(7) 5_556 5_556 ? o2 cu1 o2 180.00(6) . 5_556 ? c1 o1 cu1 125.73(14) . . ? c7 o2 cu1 125.65(13) . . ? o1 c1 c2 124.4(2) . . ? o1 c1 c6 122.0(2) . . ? c2 c1 c6 113.6(2) . . ? f1 c2 c3 119.5(3) . . ? f1 c2 c1 116.9(3) . . ? c3 c2 c1 123.6(3) . . ? f2 c3 c2 119.6(3) . . ? f2 c3 c4 120.3(3) . . ? c2 c3 c4 120.1(3) . . ? f3 c4 c5 120.1(4) . . ? f3 c4 c3 121.2(4) . . ? c5 c4 c3 118.8(3) . . ? f4 c5 c4 119.5(3) . . ? f4 c5 c6 120.3(3) . . ? c4 c5 c6 120.1(3) . . ? f5 c6 c5 117.5(2) . . ? f5 c6 c1 118.7(2) . . ? c5 c6 c1 123.8(2) . . ? o2 c7 c12 124.72(19) . . ? o2 c7 c8 121.5(2) . . ? c12 c7 c8 113.8(2) . . ? f6 c8 c9 118.7(2) . . ? f6 c8 c7 118.4(2) . . ? c9 c8 c7 122.9(2) . . ? f7 c9 c8 120.1(3) . . ? f7 c9 c10 119.1(3) . . ? c8 c9 c10 120.8(2) . . ? f8 c10 c11 121.0(3) . . ? f8 c10 c9 120.5(3) . . ? c11 c10 c9 118.5(2) . . ? f9 c11 c10 120.1(3) . . ? f9 c11 c12 119.4(3) . . ? c10 c11 c12 120.5(2) . . ? f10 c12 c11 118.4(2) . . ? f10 c12 c7 118.1(2) . . ? c11 c12 c7 123.5(2) . . ? c17 n1 c21 107.85(17) . . ? c17 n1 c13 110.33(19) . . ? c21 n1 c13 111.00(19) . . ? c17 n1 c25 110.19(18) . . ? c21 n1 c25 110.32(18) . . ? c13 n1 c25 107.17(17) . . ? n1 c13 c14 114.0(2) . . ? c15 c14 c13 113.6(3) . . ? c14 c15 c16 113.6(3) . . ? n1 c17 c18 114.46(18) . . ? c19 c18 c17 112.3(2) . . ? c18 c19 c20 112.8(2) . . ? c22 c21 n1 114.4(2) . . ? c23 c22 c21 114.1(3) . . ? c22 c23 c24 113.2(3) . . ? c26 c25 n1 116.1(2) . . ? c25 c26 c27 109.6(3) . . ? c28 c27 c28a 67.7(5) . . ? c28 c27 c26 117.8(5) . . ? c28a c27 c26 114.6(4) . . ? c27 c28 c28a 60.4(5) . . ? c27 c28a c28 51.9(4) . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.568 _refine_diff_density_min -0.289 _refine_diff_density_rms 0.053 #===end