data_Compound7a _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 h64 co f20 k2 o18' _chemical_formula_weight 1542.20 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' 'f' 'f' 0.0171 0.0103 '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' _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 22.0161(10) _cell_length_b 16.0513(7) _cell_length_c 19.1081(9) _cell_angle_alpha 90.00 _cell_angle_beta 101.7300(10) _cell_angle_gamma 90.00 _cell_volume 6611.5(5) _cell_formula_units_z 4 _cell_measurement_temperature 218(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.549 _exptl_crystal_density_method 'not measured' _exptl_crystal_f_000 3156 _exptl_absorpt_coefficient_mu 0.509 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_t_min 0.8623 _exptl_absorpt_correction_t_max 0.9051 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21480 _diffrn_reflns_av_r_equivalents 0.0358 _diffrn_reflns_av_sigmai/neti 0.0380 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6485 _reflns_number_gt 4961 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 four h atoms at the two c atoms (C18 and C19) bonded to the disordered o atoms (o6 and o6') have not been taken into consideration in the refenement. ; _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^)+(0.0800p)^2^+12.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6485 _refine_ls_number_parameters 443 _refine_ls_number_restraints 0 _refine_ls_r_factor_all 0.0821 _refine_ls_r_factor_gt 0.0635 _refine_ls_wr_factor_ref 0.1721 _refine_ls_wr_factor_gt 0.1601 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_s_all 1.054 _refine_ls_shift/su_max 0.004 _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 0.27588(4) 0.7500 0.03925(19) Uani 1 2 d S . . k1 k 0.09702(3) 0.28313(5) 0.93026(4) 0.0433(2) Uani 1 1 d . . . f2 f -0.02865(12) 0.46977(18) 0.66885(15) 0.0801(8) Uani 1 1 d . A . f3 f -0.07750(17) 0.62071(18) 0.6849(2) 0.1158(12) Uani 1 1 d . . . f4 f -0.17943(17) 0.63526(17) 0.7450(2) 0.1093(11) Uani 1 1 d . A . f5 f -0.22929(12) 0.49595(18) 0.79044(15) 0.0813(8) Uani 1 1 d . . . f6 f -0.18076(10) 0.34584(14) 0.77593(13) 0.0639(6) Uani 1 1 d . A . f8 f 0.05856(15) 0.0600(2) 0.68701(16) 0.0930(8) Uani 1 1 d . A . f9 f 0.16405(15) 0.02282(19) 0.64382(18) 0.1062(11) Uani 1 1 d . . . f10 f 0.22160(14) 0.1383(3) 0.57595(19) 0.1168(12) Uani 1 1 d . A . f11 f 0.17080(19) 0.2927(2) 0.5531(2) 0.1236(12) Uani 1 1 d . . . f12 f 0.06625(16) 0.33101(18) 0.59844(19) 0.1104(12) Uani 1 1 d . A . o1 o -0.07914(10) 0.32876(15) 0.71310(13) 0.0516(6) Uani 1 1 d . . . o2 o 0.00651(12) 0.2167(2) 0.66382(16) 0.0800(10) Uani 1 1 d . . . o3 o 0.0684(2) 0.4132(3) 1.0207(3) 0.1236(16) Uani 1 1 d . A . o4 o 0.04020(19) 0.2437(3) 1.0486(2) 0.1009(12) Uani 1 1 d . A . o5 o 0.08425(19) 0.1186(2) 0.97519(18) 0.0933(11) Uani 1 1 d . A . o6 o 0.16320(18) 0.1342(3) 0.8924(2) 0.0601(17) Uani 0.718(12) 1 d P A 1 o6' o 0.1419(5) 0.1575(7) 0.8490(7) 0.059(4) Uiso 0.282(12) 1 d P A 2 o7 o 0.21414(11) 0.29637(18) 0.89003(14) 0.0577(7) Uani 1 1 d . A . o8 o 0.18639(15) 0.41153(17) 0.98570(16) 0.0711(8) Uani 1 1 d . A . c1 c -0.10204(15) 0.4023(2) 0.72236(17) 0.0427(8) Uani 1 1 d . . . c2 c -0.07835(17) 0.4752(2) 0.6994(2) 0.0525(9) Uani 1 1 d . . . c3 c -0.1036(2) 0.5529(3) 0.7071(3) 0.0701(12) Uani 1 1 d . A . c4 c -0.1545(2) 0.5601(3) 0.7369(2) 0.0673(11) Uani 1 1 d . . . c5 c -0.17953(17) 0.4898(3) 0.7599(2) 0.0552(9) Uani 1 1 d . A . c6 c -0.15396(16) 0.4131(2) 0.75303(18) 0.0451(8) Uani 1 1 d . . . c7 c 0.05809(18) 0.1972(3) 0.6439(2) 0.0611(11) Uani 1 1 d . A . c8 c 0.08585(19) 0.1192(3) 0.6540(2) 0.0621(11) Uani 1 1 d . . . c9 c 0.1398(2) 0.1002(3) 0.6314(2) 0.0678(12) Uani 1 1 d . A . c10 c 0.1687(2) 0.1578(4) 0.5979(3) 0.0743(13) Uani 1 1 d . . . c11 c 0.1427(2) 0.2348(3) 0.5861(3) 0.0778(13) Uani 1 1 d . A . c12 c 0.0897(2) 0.2539(3) 0.6094(3) 0.0714(13) Uani 1 1 d . . . c13 c 0.0249(5) 0.3839(6) 1.0650(5) 0.165(4) Uani 1 1 d . . . h13a h 0.0242 0.4250 1.1027 0.198 Uiso 1 1 calc R A . h13b h -0.0169 0.3821 1.0349 0.198 Uiso 1 1 calc R . . c14 c 0.0377(4) 0.3060(7) 1.0970(4) 0.141(3) Uani 1 1 d . A . h14a h 0.0776 0.3087 1.1309 0.170 Uiso 1 1 calc R . . h14b h 0.0057 0.2925 1.1240 0.170 Uiso 1 1 calc R . . c15 c 0.0507(3) 0.1632(6) 1.0752(4) 0.122(3) Uani 1 1 d . . . h15a h 0.0198 0.1504 1.1040 0.147 Uiso 1 1 calc R A . h15b h 0.0916 0.1614 1.1071 0.147 Uiso 1 1 calc R . . c16 c 0.0482(3) 0.1007(4) 1.0228(4) 0.100(2) Uani 1 1 d . A . h16a h 0.0617 0.0477 1.0464 0.120 Uiso 1 1 calc R . . h16b h 0.0051 0.0939 0.9972 0.120 Uiso 1 1 calc R . . c17 c 0.0935(2) 0.0537(3) 0.9277(4) 0.100(2) Uani 1 1 d . . . h17a h 0.1209 0.0116 0.9547 0.120 Uiso 1 1 calc R A . h17b h 0.0535 0.0269 0.9089 0.120 Uiso 1 1 calc R . . c18 c 0.1190(5) 0.0804(4) 0.8705(4) 0.125(3) Uani 1 1 d . A . c19 c 0.1877(2) 0.1700(3) 0.8287(3) 0.0794(14) Uani 1 1 d . . . c20 c 0.23859(19) 0.2242(3) 0.8629(2) 0.0697(13) Uani 1 1 d . A . h20a h 0.2655 0.1942 0.9019 0.084 Uiso 1 1 calc R . . h20b h 0.2635 0.2405 0.8280 0.084 Uiso 1 1 calc R . . c21 c 0.25965(18) 0.3505(4) 0.9288(3) 0.0772(14) Uani 1 1 d . . . h21a h 0.2912 0.3621 0.9006 0.093 Uiso 1 1 calc R A . h21b h 0.2801 0.3236 0.9734 0.093 Uiso 1 1 calc R . . c22 c 0.2312(2) 0.4285(3) 0.9449(3) 0.0784(14) Uani 1 1 d . A . h22a h 0.2630 0.4657 0.9715 0.094 Uiso 1 1 calc R . . h22b h 0.2117 0.4564 0.9003 0.094 Uiso 1 1 calc R . . c23 c 0.1589(3) 0.4842(3) 1.0094(3) 0.103(2) Uani 1 1 d . . . h23a h 0.1357 0.5147 0.9681 0.123 Uiso 1 1 calc R A . h23b h 0.1915 0.5210 1.0351 0.123 Uiso 1 1 calc R . . c24 c 0.1166(4) 0.4606(4) 1.0571(3) 0.115(2) Uani 1 1 d . A . h24a h 0.1395 0.4288 1.0978 0.138 Uiso 1 1 calc R . . h24b h 0.1001 0.5109 1.0755 0.138 Uiso 1 1 calc R . . o9 o 0.0789(2) -0.1404(3) 0.8501(3) 0.1129(13) Uani 1 1 d . . . c25 c 0.1314(6) -0.1759(5) 0.8937(4) 0.160(4) Uani 1 1 d . . . h25a h 0.1243 -0.2346 0.9035 0.191 Uiso 1 1 calc R . . h25b h 0.1428 -0.1459 0.9392 0.191 Uiso 1 1 calc R . . c26 c 0.1819(4) -0.1665(6) 0.8491(6) 0.157(4) Uani 1 1 d . . . h26a h 0.2098 -0.1201 0.8668 0.189 Uiso 1 1 calc R . . h26b h 0.2064 -0.2177 0.8509 0.189 Uiso 1 1 calc R . . c27 c 0.1495(4) -0.1508(5) 0.7790(5) 0.131(3) Uani 1 1 d . . . h27a h 0.1630 -0.0979 0.7615 0.157 Uiso 1 1 calc R . . h27b h 0.1566 -0.1956 0.7468 0.157 Uiso 1 1 calc R . . c28 c 0.0870(3) -0.1470(4) 0.7828(4) 0.1086(19) Uani 1 1 d . . . h28b h 0.0679 -0.0989 0.7552 0.130 Uiso 1 1 calc R . . h28a h 0.0660 -0.1973 0.7611 0.130 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 co1 0.0339(3) 0.0383(4) 0.0439(4) 0.000 0.0039(2) 0.000 k1 0.0420(4) 0.0469(4) 0.0427(4) -0.0046(3) 0.0124(3) -0.0035(3) f2 0.0649(14) 0.0960(19) 0.0909(19) 0.0118(15) 0.0432(13) 0.0025(14) f3 0.129(3) 0.0623(18) 0.170(3) 0.0264(19) 0.064(2) -0.0083(18) f4 0.135(3) 0.0529(16) 0.150(3) -0.0101(17) 0.052(2) 0.0302(17) f5 0.0725(15) 0.0937(19) 0.0895(19) -0.0083(15) 0.0444(14) 0.0245(14) f6 0.0591(13) 0.0636(14) 0.0730(15) 0.0133(12) 0.0228(11) 0.0035(11) f8 0.098(2) 0.099(2) 0.0808(19) 0.0032(16) 0.0153(16) 0.0091(18) f9 0.104(2) 0.089(2) 0.117(2) -0.0142(18) 0.0044(18) 0.0550(18) f10 0.0771(19) 0.159(3) 0.123(3) -0.047(2) 0.0417(18) 0.014(2) f11 0.133(3) 0.116(3) 0.123(3) -0.006(2) 0.027(2) -0.031(2) f12 0.121(2) 0.0611(17) 0.129(3) -0.0144(17) -0.021(2) 0.0279(17) o1 0.0377(12) 0.0537(15) 0.0596(15) -0.0119(12) 0.0008(10) 0.0132(11) o2 0.0448(14) 0.108(3) 0.079(2) -0.0503(18) -0.0065(13) 0.0221(15) o3 0.145(4) 0.113(3) 0.120(3) -0.059(3) 0.045(3) 0.013(3) o4 0.100(3) 0.139(4) 0.076(2) -0.012(3) 0.046(2) -0.012(3) o5 0.136(3) 0.073(2) 0.069(2) 0.0183(18) 0.014(2) -0.027(2) o6 0.060(2) 0.065(3) 0.051(3) -0.006(2) 0.0017(19) 0.006(2) o7 0.0349(12) 0.0803(19) 0.0583(15) 0.0022(14) 0.0104(11) 0.0030(12) o8 0.089(2) 0.0507(16) 0.0687(18) -0.0037(14) 0.0047(16) -0.0128(15) c1 0.0416(17) 0.050(2) 0.0348(16) -0.0046(14) 0.0029(13) 0.0074(15) c2 0.0488(19) 0.059(2) 0.054(2) -0.0009(18) 0.0196(16) 0.0020(17) c3 0.085(3) 0.051(2) 0.079(3) 0.009(2) 0.027(2) -0.005(2) c4 0.079(3) 0.045(2) 0.080(3) -0.007(2) 0.023(2) 0.018(2) c5 0.053(2) 0.066(3) 0.049(2) -0.0060(18) 0.0186(17) 0.0147(19) c6 0.0478(18) 0.049(2) 0.0398(18) -0.0006(15) 0.0116(14) 0.0033(16) c7 0.047(2) 0.073(3) 0.054(2) -0.032(2) -0.0120(17) 0.018(2) c8 0.062(2) 0.070(3) 0.049(2) -0.012(2) -0.0007(18) 0.009(2) c9 0.065(3) 0.071(3) 0.061(3) -0.021(2) -0.002(2) 0.033(2) c10 0.061(3) 0.094(4) 0.067(3) -0.030(3) 0.009(2) 0.012(3) c11 0.082(3) 0.079(3) 0.068(3) -0.019(3) 0.005(2) -0.009(3) c12 0.071(3) 0.060(3) 0.072(3) -0.023(2) -0.013(2) 0.017(2) c13 0.182(8) 0.187(9) 0.163(8) -0.067(7) 0.123(7) 0.022(7) c14 0.156(7) 0.197(9) 0.091(5) 0.007(6) 0.071(5) 0.049(7) c15 0.104(5) 0.186(8) 0.087(4) 0.065(5) 0.042(4) 0.004(5) c16 0.080(3) 0.115(5) 0.097(4) 0.038(4) -0.002(3) -0.038(3) c17 0.076(3) 0.050(3) 0.154(6) -0.022(3) -0.026(3) -0.011(2) c18 0.233(9) 0.057(3) 0.087(4) -0.012(3) 0.038(5) -0.024(4) c19 0.074(3) 0.083(3) 0.083(3) -0.028(3) 0.020(2) 0.022(3) c20 0.055(2) 0.094(3) 0.068(3) 0.022(2) 0.030(2) 0.030(2) c21 0.039(2) 0.119(4) 0.071(3) 0.015(3) 0.0066(18) -0.021(2) c22 0.076(3) 0.075(3) 0.074(3) 0.011(2) -0.009(2) -0.036(3) c23 0.165(6) 0.041(3) 0.087(4) -0.017(2) -0.009(4) 0.000(3) c24 0.169(7) 0.092(4) 0.084(4) -0.038(4) 0.020(4) 0.029(4) o9 0.124(3) 0.131(4) 0.097(3) 0.003(3) 0.052(3) 0.004(3) c25 0.268(12) 0.106(5) 0.086(5) 0.016(4) -0.007(7) -0.023(7) c26 0.095(5) 0.174(9) 0.187(10) 0.046(8) -0.007(6) 0.010(5) c27 0.134(6) 0.108(5) 0.172(8) -0.011(5) 0.082(6) 0.000(5) c28 0.116(5) 0.113(5) 0.098(5) -0.007(4) 0.026(4) -0.015(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 co1 o2 1.932(3) . ? co1 o2 1.932(3) 2_556 ? co1 o1 1.938(2) 2_556 ? co1 o1 1.938(2) . ? co1 k1 3.6673(7) . ? co1 k1 3.6673(7) 2_556 ? k1 o1 2.785(3) 2_556 ? k1 o5 2.808(3) . ? k1 o2 2.811(3) 2_556 ? k1 o6' 2.842(10) . ? k1 o7 2.844(2) . ? k1 o3 2.861(4) . ? k1 o4 2.868(4) . ? k1 o8 2.897(3) . ? k1 o6 2.965(4) . ? k1 c1 3.508(3) 2_556 ? f2 c2 1.344(4) . ? f3 c3 1.339(5) . ? f4 c4 1.348(4) . ? f5 c5 1.346(4) . ? f6 c6 1.345(4) . ? f8 c8 1.346(5) . ? f9 c9 1.354(5) . ? f10 c10 1.353(5) . ? f11 c11 1.343(6) . ? f12 c12 1.341(5) . ? o1 c1 1.310(4) . ? o1 k1 2.785(3) 2_556 ? o2 c7 1.307(5) . ? o2 k1 2.811(3) 2_556 ? o3 c24 1.372(8) . ? o3 c13 1.479(9) . ? o4 c14 1.371(9) . ? o4 c15 1.391(8) . ? o5 c16 1.356(7) . ? o5 c17 1.423(7) . ? o6 c18 1.305(8) . ? o6 c19 1.541(7) . ? o6' c19 1.171(11) . ? o6' c18 1.428(12) . ? o7 c21 1.416(5) . ? o7 c20 1.419(5) . ? o8 c22 1.402(6) . ? o8 c23 1.431(6) . ? c1 c2 1.388(5) . ? c1 c6 1.397(5) . ? c1 k1 3.508(3) 2_556 ? c2 c3 1.385(6) . ? c3 c4 1.361(6) . ? c4 c5 1.367(6) . ? c5 c6 1.371(5) . ? c7 c12 1.390(7) . ? c7 c8 1.391(6) . ? c8 c9 1.377(6) . ? c9 c10 1.355(7) . ? c10 c11 1.362(7) . ? c11 c12 1.364(7) . ? c13 c14 1.395(11) . ? c15 c16 1.411(10) . ? c17 c18 1.395(9) . ? c19 c20 1.463(7) . ? c21 c22 1.461(7) . ? c23 c24 1.478(9) . ? o9 c28 1.338(7) . ? o9 c25 1.401(10) . ? c25 c26 1.540(12) . ? c26 c27 1.405(11) . ? c27 c28 1.393(9) . ? 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 121.0(2) . 2_556 ? o2 co1 o1 107.98(12) . 2_556 ? o2 co1 o1 97.03(11) 2_556 2_556 ? o2 co1 o1 97.03(11) . . ? o2 co1 o1 107.98(12) 2_556 . ? o1 co1 o1 128.04(15) 2_556 . ? o2 co1 k1 133.33(8) . . ? o2 co1 k1 49.08(8) 2_556 . ? o1 co1 k1 48.34(7) 2_556 . ? o1 co1 k1 129.56(7) . . ? o2 co1 k1 49.08(8) . 2_556 ? o2 co1 k1 133.33(8) 2_556 2_556 ? o1 co1 k1 129.56(7) 2_556 2_556 ? o1 co1 k1 48.34(7) . 2_556 ? k1 co1 k1 176.36(3) . 2_556 ? o1 k1 o5 123.03(9) 2_556 . ? o1 k1 o2 62.40(7) 2_556 2_556 ? o5 k1 o2 73.74(10) . 2_556 ? o1 k1 o6' 69.2(3) 2_556 . ? o5 k1 o6' 64.4(3) . . ? o2 k1 o6' 73.0(3) 2_556 . ? o1 k1 o7 70.68(7) 2_556 . ? o5 k1 o7 107.79(11) . . ? o2 k1 o7 121.15(9) 2_556 . ? o6' k1 o7 58.0(2) . . ? o1 k1 o3 113.43(12) 2_556 . ? o5 k1 o3 116.97(14) . . ? o2 k1 o3 114.45(13) 2_556 . ? o6' k1 o3 172.5(3) . . ? o7 k1 o3 115.58(12) . . ? o1 k1 o4 146.74(10) 2_556 . ? o5 k1 o4 57.64(13) . . ? o2 k1 o4 89.62(10) 2_556 . ? o6' k1 o4 122.0(3) . . ? o7 k1 o4 142.58(10) . . ? o3 k1 o4 60.00(14) . . ? o1 k1 o8 97.02(8) 2_556 . ? o5 k1 o8 131.29(10) . . ? o2 k1 o8 154.97(9) 2_556 . ? o6' k1 o8 114.8(2) . . ? o7 k1 o8 57.33(9) . . ? o3 k1 o8 58.43(13) . . ? o4 k1 o8 103.96(11) . . ? o1 k1 o6 87.14(11) 2_556 . ? o5 k1 o6 53.22(12) . . ? o2 k1 o6 84.98(11) 2_556 . ? o6' k1 o6 18.5(2) . . ? o7 k1 o6 58.46(10) . . ? o3 k1 o6 156.26(14) . . ? o4 k1 o6 109.23(14) . . ? o8 k1 o6 109.39(10) . . ? o1 k1 c1 20.12(7) 2_556 2_556 ? o5 k1 c1 142.08(10) . 2_556 ? o2 k1 c1 80.43(8) 2_556 2_556 ? o6' k1 c1 81.9(3) . 2_556 ? o7 k1 c1 63.33(8) . 2_556 ? o3 k1 c1 98.75(12) . 2_556 ? o4 k1 c1 150.23(12) . 2_556 ? o8 k1 c1 77.42(8) . 2_556 ? o6 k1 c1 97.85(11) . 2_556 ? o1 k1 co1 31.32(5) 2_556 . ? o5 k1 co1 100.48(7) . . ? o2 k1 co1 31.29(5) 2_556 . ? o6' k1 co1 70.4(3) . . ? o7 k1 co1 97.78(6) . . ? o3 k1 co1 115.64(11) . . ? o4 k1 co1 117.98(9) . . ? o8 k1 co1 126.06(6) . . ? o6 k1 co1 88.07(9) . . ? c1 k1 co1 49.25(5) 2_556 . ? c1 o1 co1 133.5(2) . . ? c1 o1 k1 112.87(19) . 2_556 ? co1 o1 k1 100.34(9) . 2_556 ? c7 o2 co1 125.8(2) . . ? c7 o2 k1 122.9(3) . 2_556 ? co1 o2 k1 99.63(10) . 2_556 ? c24 o3 c13 114.2(6) . . ? c24 o3 k1 117.9(4) . . ? c13 o3 k1 111.2(4) . . ? c14 o4 c15 117.2(6) . . ? c14 o4 k1 117.0(5) . . ? c15 o4 k1 115.3(3) . . ? c16 o5 c17 116.8(5) . . ? c16 o5 k1 120.9(4) . . ? c17 o5 k1 117.3(3) . . ? c18 o6 c19 110.6(5) . . ? c18 o6 k1 103.9(4) . . ? c19 o6 k1 99.2(3) . . ? c19 o6' c18 128.5(10) . . ? c19 o6' k1 118.6(7) . . ? c18 o6' k1 106.0(6) . . ? c21 o7 c20 114.3(3) . . ? c21 o7 k1 119.2(2) . . ? c20 o7 k1 118.0(2) . . ? c22 o8 c23 114.1(4) . . ? c22 o8 k1 115.9(2) . . ? c23 o8 k1 113.3(3) . . ? o1 c1 c2 122.5(3) . . ? o1 c1 c6 122.6(3) . . ? c2 c1 c6 114.8(3) . . ? o1 c1 k1 47.01(15) . 2_556 ? c2 c1 k1 96.9(2) . 2_556 ? c6 c1 k1 125.7(2) . 2_556 ? f2 c2 c3 119.0(4) . . ? f2 c2 c1 118.3(3) . . ? c3 c2 c1 122.8(3) . . ? f3 c3 c4 120.4(4) . . ? f3 c3 c2 119.4(4) . . ? c4 c3 c2 120.2(4) . . ? f4 c4 c3 120.9(4) . . ? f4 c4 c5 120.1(4) . . ? c3 c4 c5 119.0(4) . . ? f5 c5 c4 119.8(4) . . ? f5 c5 c6 119.5(4) . . ? c4 c5 c6 120.7(3) . . ? f6 c6 c5 118.3(3) . . ? f6 c6 c1 119.2(3) . . ? c5 c6 c1 122.5(3) . . ? o2 c7 c12 122.1(4) . . ? o2 c7 c8 123.9(5) . . ? c12 c7 c8 114.1(4) . . ? f8 c8 c9 119.1(4) . . ? f8 c8 c7 118.4(4) . . ? c9 c8 c7 122.5(5) . . ? c10 c9 f9 120.1(4) . . ? c10 c9 c8 121.0(4) . . ? f9 c9 c8 118.9(5) . . ? f10 c10 c9 120.4(5) . . ? f10 c10 c11 121.2(6) . . ? c9 c10 c11 118.4(4) . . ? f11 c11 c10 119.1(5) . . ? f11 c11 c12 120.3(5) . . ? c10 c11 c12 120.6(5) . . ? f12 c12 c11 119.0(5) . . ? f12 c12 c7 117.6(5) . . ? c11 c12 c7 123.4(4) . . ? c14 c13 o3 116.0(7) . . ? o4 c14 c13 113.0(6) . . ? o4 c15 c16 114.9(5) . . ? o5 c16 c15 112.4(5) . . ? c18 c17 o5 114.0(5) . . ? o6 c18 c17 110.2(5) . . ? o6 c18 o6' 40.0(5) . . ? c17 c18 o6' 135.5(7) . . ? o6' c19 c20 125.9(7) . . ? o6' c19 o6 37.7(7) . . ? c20 c19 o6 103.2(4) . . ? o7 c20 c19 109.6(3) . . ? o7 c21 c22 110.3(3) . . ? o8 c22 c21 109.3(4) . . ? o8 c23 c24 110.3(4) . . ? o3 c24 c23 110.4(5) . . ? c28 o9 c25 106.6(6) . . ? o9 c25 c26 103.4(6) . . ? c27 c26 c25 105.1(6) . . ? c28 c27 c26 106.0(7) . . ? o9 c28 c27 112.2(6) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.652 _refine_diff_density_min -0.305 _refine_diff_density_rms 0.060 #===end