data_Compound11 _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 'c62 h82 cl4 co2 k2 o18' _chemical_formula_weight 1453.14 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' 'cl' 'cl' 0.1484 0.1585 'international tables vol c tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_h-m P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.487(4) _cell_length_b 15.672(4) _cell_length_c 16.844(4) _cell_angle_alpha 90.00 _cell_angle_beta 105.970(6) _cell_angle_gamma 90.00 _cell_volume 3422.9(15) _cell_formula_units_z 2 _cell_measurement_temperature 218(2) _cell_measurement_reflns_used 4120 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 23.22 _exptl_crystal_description CHUNKS _exptl_crystal_colour GREEN _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'none' _exptl_crystal_density_diffrn 1.410 _exptl_crystal_density_method 'not measured' _exptl_crystal_f_000 1516 _exptl_absorpt_coefficient_mu 0.829 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_t_min 0.664 _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 18579 _diffrn_reflns_av_r_equivalents 0.0888 _diffrn_reflns_av_sigmai/neti 0.1116 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 24.00 _reflns_number_total 5378 _reflns_number_gt 3748 _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^)+(0.0487p)^2^+0.7361P] 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 5378 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_r_factor_all 0.1042 _refine_ls_r_factor_gt 0.0680 _refine_ls_wr_factor_ref 0.1664 _refine_ls_wr_factor_gt 0.1509 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_s_all 1.104 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_u_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group k1 k -0.01151(9) 0.28275(8) 0.34227(7) 0.0401(3) Uani 1 1 d . . . co1 co 0.03455(6) 0.04468(5) 0.08272(4) 0.0347(2) Uani 1 1 d . . . cl1 cl 0.12681(15) 0.52322(12) 0.08324(11) 0.0741(6) Uani 1 1 d . . . cl2 cl 0.31363(18) 0.42512(15) 0.11290(14) 0.1003(7) Uani 1 1 d . . . o1 o -0.0118(3) -0.0685(2) 0.03759(19) 0.0365(9) Uani 1 1 d . . . o2 o 0.1719(3) 0.0547(2) 0.1531(2) 0.0439(10) Uani 1 1 d . . . o3 o -0.0636(3) 0.1141(2) 0.1146(2) 0.0453(10) Uani 1 1 d . . . o4 o 0.1902(3) 0.2230(3) 0.3642(3) 0.0535(11) Uani 1 1 d . . . o5 o 0.0872(3) 0.3203(3) 0.2229(2) 0.0483(10) Uani 1 1 d . . . o6 o -0.1208(3) 0.3700(2) 0.2012(2) 0.0413(9) Uani 1 1 d . . . o7 o -0.1834(3) 0.3803(2) 0.3445(2) 0.0444(10) Uani 1 1 d . . . o8 o -0.0944(3) 0.2723(3) 0.4779(2) 0.0520(11) Uani 1 1 d . . . o9 o 0.1123(3) 0.2327(3) 0.5004(2) 0.0546(11) Uani 1 1 d . . . c1 c -0.0176(4) -0.1426(4) 0.0759(3) 0.0340(13) Uani 1 1 d . . . c2 c -0.0563(5) -0.2150(3) 0.0305(3) 0.0413(15) Uani 1 1 d . . . h2a h -0.0777 -0.2124 -0.0275 0.050 Uiso 1 1 calc R . . c3 c -0.0635(5) -0.2898(4) 0.0695(4) 0.0534(17) Uani 1 1 d . . . h3a h -0.0895 -0.3381 0.0375 0.064 Uiso 1 1 calc R . . c4 c -0.0347(5) -0.2972(4) 0.1525(4) 0.0542(17) Uani 1 1 d . . . h4a h -0.0400 -0.3497 0.1781 0.065 Uiso 1 1 calc R . . c5 c 0.0022(5) -0.2264(5) 0.1981(4) 0.0576(18) Uani 1 1 d . . . h5a h 0.0214 -0.2300 0.2560 0.069 Uiso 1 1 calc R . . c6 c 0.0118(4) -0.1498(4) 0.1610(3) 0.0429(14) Uani 1 1 d . . . h6a h 0.0385 -0.1021 0.1938 0.052 Uiso 1 1 calc R . . c7 c 0.2567(5) 0.0300(3) 0.1354(3) 0.0389(14) Uani 1 1 d . . . c8 c 0.2576(5) -0.0260(3) 0.0722(3) 0.0441(14) Uani 1 1 d . . . h8a h 0.1947 -0.0478 0.0394 0.053 Uiso 1 1 calc R . . c9 c 0.3482(5) -0.0508(4) 0.0558(4) 0.0559(17) Uani 1 1 d . . . h9a h 0.3465 -0.0893 0.0126 0.067 Uiso 1 1 calc R . . c10 c 0.4403(5) -0.0195(4) 0.1024(4) 0.0510(16) Uani 1 1 d . . . h10a h 0.5025 -0.0364 0.0922 0.061 Uiso 1 1 calc R . . c11 c 0.4401(5) 0.0370(4) 0.1642(3) 0.0499(16) Uani 1 1 d . . . h11a h 0.5030 0.0594 0.1962 0.060 Uiso 1 1 calc R . . c12 c 0.3509(4) 0.0615(4) 0.1807(3) 0.0418(14) Uani 1 1 d . . . h12a h 0.3535 0.1006 0.2235 0.050 Uiso 1 1 calc R . . c13 c -0.0911(5) 0.1120(3) 0.1837(3) 0.0401(14) Uani 1 1 d . . . c14 c -0.1849(5) 0.1451(4) 0.1861(4) 0.0528(17) Uani 1 1 d . . . h14a h -0.2298 0.1679 0.1379 0.063 Uiso 1 1 calc R . . c15 c -0.2134(6) 0.1448(4) 0.2590(5) 0.063(2) Uani 1 1 d . . . h15a h -0.2845 0.1616 0.2582 0.076 Uiso 1 1 calc R . . c16 c -0.1497(7) 0.1115(4) 0.3294(4) 0.067(2) Uani 1 1 d . . . h16a h -0.1786 0.0968 0.3757 0.080 Uiso 1 1 calc R . . c17 c -0.0569(6) 0.0788(4) 0.3286(4) 0.0591(19) Uani 1 1 d . . . h17a h -0.0198 0.0409 0.3742 0.071 Uiso 1 1 calc R . . c18 c -0.0289(5) 0.0790(4) 0.2555(3) 0.0444(15) Uani 1 1 d . . . h18a h 0.0354 0.0495 0.2539 0.053 Uiso 1 1 calc R . . c19 c 0.2387(5) 0.2575(4) 0.3064(5) 0.066(2) Uani 1 1 d . . . h19a h 0.2987 0.2227 0.3052 0.079 Uiso 1 1 calc R . . h19b h 0.2625 0.3156 0.3225 0.079 Uiso 1 1 calc R . . c20 c 0.1639(6) 0.2582(4) 0.2240(4) 0.064(2) Uani 1 1 d . . . h20a h 0.1992 0.2718 0.1819 0.077 Uiso 1 1 calc R . . h20b h 0.1320 0.2018 0.2116 0.077 Uiso 1 1 calc R . . c21 c 0.0136(5) 0.3296(4) 0.1438(3) 0.0495(16) Uani 1 1 d . . . h21a h -0.0244 0.2762 0.1275 0.059 Uiso 1 1 calc R . . h21b h 0.0486 0.3444 0.1018 0.059 Uiso 1 1 calc R . . c22 c -0.0577(5) 0.3986(4) 0.1518(3) 0.0464(16) Uani 1 1 d . . . h22a h -0.0182 0.4488 0.1773 0.056 Uiso 1 1 calc R . . h22b h -0.1008 0.4149 0.0970 0.056 Uiso 1 1 calc R . . c23 c -0.1904(5) 0.4325(4) 0.2118(3) 0.0471(15) Uani 1 1 d . . . h23a h -0.2372 0.4480 0.1581 0.056 Uiso 1 1 calc R . . h23b h -0.1527 0.4838 0.2363 0.056 Uiso 1 1 calc R . . c24 c -0.2498(4) 0.3994(4) 0.2658(3) 0.0492(16) Uani 1 1 d . . . h24a h -0.3008 0.4419 0.2713 0.059 Uiso 1 1 calc R . . h24b h -0.2868 0.3477 0.2415 0.059 Uiso 1 1 calc R . . c25 c -0.2392(4) 0.3490(5) 0.3991(3) 0.0565(18) Uani 1 1 d . . . h25a h -0.2729 0.2950 0.3782 0.068 Uiso 1 1 calc R . . h25b h -0.2926 0.3901 0.4026 0.068 Uiso 1 1 calc R . . c26 c -0.1664(5) 0.3360(4) 0.4820(3) 0.0565(18) Uani 1 1 d . . . h26a h -0.1302 0.3895 0.5014 0.068 Uiso 1 1 calc R . . h26b h -0.2046 0.3191 0.5212 0.068 Uiso 1 1 calc R . . c27 c -0.0258(6) 0.2591(5) 0.5559(4) 0.064(2) Uani 1 1 d . . . h27a h -0.0634 0.2375 0.5940 0.077 Uiso 1 1 calc R . . h27b h 0.0069 0.3133 0.5778 0.077 Uiso 1 1 calc R . . c28 c 0.0541(6) 0.1967(5) 0.5493(4) 0.072(2) Uani 1 1 d . . . h28a h 0.0988 0.1832 0.6043 0.087 Uiso 1 1 calc R . . h28b h 0.0214 0.1438 0.5240 0.087 Uiso 1 1 calc R . . c29 c 0.2017(5) 0.1842(4) 0.5014(4) 0.0647(19) Uani 1 1 d . . . h29a h 0.1822 0.1259 0.4824 0.078 Uiso 1 1 calc R . . h29b h 0.2476 0.1815 0.5577 0.078 Uiso 1 1 calc R . . c30 c 0.2547(5) 0.2268(4) 0.4458(4) 0.0644(19) Uani 1 1 d . . . h30a h 0.2695 0.2864 0.4625 0.077 Uiso 1 1 calc R . . h30b h 0.3202 0.1979 0.4491 0.077 Uiso 1 1 calc R . . c31 c 0.2353(6) 0.4880(5) 0.1557(4) 0.076(2) Uani 1 1 d . . . h31a h 0.2145 0.4548 0.1978 0.091 Uiso 1 1 calc R . . h31b h 0.2749 0.5374 0.1829 0.091 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 k1 0.0366(8) 0.0497(8) 0.0344(7) 0.0028(5) 0.0105(5) 0.0043(6) co1 0.0361(5) 0.0407(5) 0.0279(4) -0.0048(3) 0.0096(3) 0.0013(4) cl1 0.0707(13) 0.0725(13) 0.0748(12) 0.0231(9) 0.0124(10) -0.0074(10) cl2 0.0983(18) 0.0959(18) 0.1116(17) -0.0192(13) 0.0371(14) 0.0136(13) o1 0.043(2) 0.036(2) 0.0310(19) -0.0036(16) 0.0112(17) -0.0012(18) o2 0.038(2) 0.055(3) 0.037(2) -0.0073(18) 0.0076(18) 0.0049(19) o3 0.052(3) 0.050(3) 0.040(2) 0.0002(17) 0.0226(19) 0.009(2) o4 0.032(2) 0.060(3) 0.066(3) -0.008(2) 0.008(2) -0.001(2) o5 0.052(3) 0.051(3) 0.049(2) -0.0112(19) 0.025(2) 0.002(2) o6 0.046(3) 0.041(2) 0.038(2) 0.0009(17) 0.0130(18) 0.0001(19) o7 0.028(2) 0.065(3) 0.040(2) -0.0091(19) 0.0089(18) -0.0022(19) o8 0.059(3) 0.064(3) 0.032(2) -0.0049(19) 0.012(2) -0.006(2) o9 0.054(3) 0.051(3) 0.050(2) 0.0078(19) 0.000(2) 0.014(2) c1 0.025(3) 0.044(4) 0.036(3) 0.004(3) 0.014(2) 0.009(3) c2 0.062(4) 0.039(4) 0.031(3) 0.000(2) 0.027(3) 0.001(3) c3 0.072(5) 0.041(4) 0.057(4) -0.006(3) 0.034(4) -0.002(3) c4 0.057(4) 0.050(5) 0.063(4) 0.019(3) 0.029(4) 0.013(3) c5 0.052(4) 0.077(5) 0.045(4) 0.026(4) 0.016(3) 0.021(4) c6 0.037(4) 0.051(4) 0.038(3) -0.001(3) 0.005(3) 0.002(3) c7 0.047(4) 0.033(3) 0.033(3) 0.008(2) 0.005(3) 0.004(3) c8 0.044(4) 0.035(4) 0.051(4) -0.002(3) 0.010(3) -0.003(3) c9 0.060(5) 0.047(4) 0.063(4) -0.005(3) 0.021(4) 0.006(3) c10 0.045(4) 0.044(4) 0.064(4) 0.013(3) 0.015(3) 0.013(3) c11 0.040(4) 0.059(4) 0.043(3) 0.014(3) -0.002(3) 0.004(3) c12 0.040(4) 0.051(4) 0.028(3) 0.000(3) -0.002(3) 0.003(3) c13 0.045(4) 0.034(3) 0.046(3) -0.008(3) 0.019(3) -0.005(3) c14 0.063(5) 0.043(4) 0.061(4) -0.007(3) 0.031(4) 0.004(3) c15 0.059(5) 0.049(5) 0.098(6) -0.018(4) 0.051(5) -0.015(4) c16 0.089(6) 0.059(5) 0.067(5) -0.023(4) 0.046(5) -0.030(4) c17 0.078(5) 0.062(5) 0.039(3) -0.014(3) 0.019(3) -0.019(4) c18 0.050(4) 0.044(4) 0.039(3) -0.014(3) 0.012(3) -0.003(3) c19 0.040(4) 0.061(5) 0.104(6) -0.012(4) 0.034(4) -0.002(3) c20 0.071(5) 0.050(4) 0.094(6) -0.012(4) 0.059(5) -0.002(4) c21 0.074(5) 0.042(4) 0.041(3) -0.010(3) 0.030(3) -0.012(3) c22 0.063(4) 0.047(4) 0.028(3) 0.005(3) 0.012(3) -0.018(3) c23 0.042(4) 0.044(4) 0.052(4) 0.002(3) 0.005(3) 0.001(3) c24 0.032(4) 0.060(4) 0.048(4) -0.001(3) 0.000(3) 0.009(3) c25 0.033(4) 0.095(5) 0.043(3) -0.013(3) 0.014(3) -0.002(3) c26 0.051(4) 0.080(5) 0.047(4) -0.018(3) 0.028(3) 0.000(4) c27 0.084(6) 0.072(5) 0.035(4) 0.002(3) 0.015(4) 0.001(4) c28 0.097(6) 0.071(5) 0.039(4) 0.015(3) 0.003(4) 0.004(5) c29 0.063(5) 0.051(5) 0.066(4) 0.001(3) -0.006(4) 0.020(4) c30 0.035(4) 0.059(5) 0.086(5) -0.017(4) -0.006(4) 0.016(3) c31 0.077(6) 0.075(5) 0.062(4) -0.018(4) -0.004(4) 0.006(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 k1 o5 2.762(4) . ? k1 o7 2.786(4) . ? k1 o6 2.786(4) . ? k1 o4 2.804(4) . ? k1 o8 2.811(4) . ? k1 o9 2.838(4) . ? k1 c16 3.240(6) . ? k1 c17 3.251(7) . ? k1 c10 3.302(6) 2 ? k1 c15 3.458(7) . ? k1 c18 3.493(5) . ? k1 c20 3.509(6) . ? co1 o3 1.901(3) . ? co1 o2 1.911(4) . ? co1 o1 1.962(3) . ? co1 o1 2.000(3) 3 ? cl1 c31 1.718(7) . ? cl2 c31 1.739(7) . ? o1 c1 1.341(6) . ? o1 co1 2.000(3) 3 ? o2 c7 1.318(6) . ? o3 c13 1.315(6) . ? o4 c30 1.410(7) . ? o4 c19 1.421(7) . ? o5 c20 1.417(7) . ? o5 c21 1.434(7) . ? o6 c23 1.401(6) . ? o6 c22 1.417(6) . ? o7 c24 1.412(6) . ? o7 c25 1.425(6) . ? o8 c27 1.398(7) . ? o8 c26 1.408(7) . ? o9 c28 1.402(7) . ? o9 c29 1.421(7) . ? c1 c6 1.384(7) . ? c1 c2 1.389(7) . ? c2 c3 1.360(7) . ? c3 c4 1.348(8) . ? c4 c5 1.364(9) . ? c5 c6 1.375(8) . ? c7 c12 1.381(7) . ? c7 c8 1.383(7) . ? c8 c9 1.380(8) . ? c9 c10 1.366(8) . ? c9 k1 3.539(6) 2_545 ? c10 c11 1.367(8) . ? c10 k1 3.302(6) 2_545 ? c11 c12 1.361(8) . ? c13 c18 1.370(7) . ? c13 c14 1.377(8) . ? c14 c15 1.386(8) . ? c15 c16 1.361(9) . ? c16 c17 1.357(10) . ? c17 c18 1.383(7) . ? c19 c20 1.474(9) . ? c21 c22 1.477(8) . ? c23 c24 1.463(7) . ? c25 c26 1.483(8) . ? c27 c28 1.482(9) . ? c29 c30 1.485(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 o5 k1 o7 117.54(12) . . ? o5 k1 o6 61.49(11) . . ? o7 k1 o6 59.68(10) . . ? o5 k1 o4 61.50(12) . . ? o7 k1 o4 164.23(12) . . ? o6 k1 o4 122.89(12) . . ? o5 k1 o8 169.38(12) . . ? o7 k1 o8 60.17(12) . . ? o6 k1 o8 119.11(12) . . ? o4 k1 o8 117.49(13) . . ? o5 k1 o9 117.72(13) . . ? o7 k1 o9 114.58(11) . . ? o6 k1 o9 166.65(12) . . ? o4 k1 o9 58.99(12) . . ? o8 k1 o9 58.91(12) . . ? o5 k1 c16 120.73(14) . . ? o7 k1 c16 89.40(17) . . ? o6 k1 c16 100.93(18) . . ? o4 k1 c16 104.58(18) . . ? o8 k1 c16 69.89(14) . . ? o9 k1 c16 90.75(18) . . ? o5 k1 c17 106.06(13) . . ? o7 k1 c17 113.53(16) . . ? o6 k1 c17 112.15(14) . . ? o4 k1 c17 80.68(16) . . ? o8 k1 c17 83.75(13) . . ? o9 k1 c17 81.11(14) . . ? c16 k1 c17 24.13(17) . . ? o5 k1 c10 81.06(13) . 2 ? o7 k1 c10 70.12(14) . 2 ? o6 k1 c10 79.89(14) . 2 ? o4 k1 c10 94.57(15) . 2 ? o8 k1 c10 88.58(13) . 2 ? o9 k1 c10 86.81(14) . 2 ? c16 k1 c10 155.99(16) . 2 ? c17 k1 c10 167.79(16) . 2 ? o5 k1 c15 108.76(14) . . ? o7 k1 c15 77.45(14) . . ? o6 k1 c15 77.78(16) . . ? o4 k1 c15 118.18(15) . . ? o8 k1 c15 81.26(14) . . ? o9 k1 c15 113.71(16) . . ? c16 k1 c15 23.16(16) . . ? c17 k1 c15 40.93(18) . . ? c10 k1 c15 146.80(17) 2 . ? o5 k1 c18 83.15(12) . . ? o7 k1 c18 123.14(13) . . ? o6 k1 c18 97.65(13) . . ? o4 k1 c18 72.62(13) . . ? o8 k1 c18 106.90(13) . . ? o9 k1 c18 95.42(13) . . ? c16 k1 c18 40.84(15) . . ? c17 k1 c18 23.30(13) . . ? c10 k1 c18 163.15(15) 2 . ? c15 k1 c18 45.88(15) . . ? o5 k1 c20 22.31(14) . . ? o7 k1 c20 139.60(15) . . ? o6 k1 c20 81.41(15) . . ? o4 k1 c20 42.00(15) . . ? o8 k1 c20 159.43(16) . . ? o9 k1 c20 100.85(16) . . ? c16 k1 c20 109.66(16) . . ? c17 k1 c20 89.72(16) . . ? c10 k1 c20 94.24(16) 2 . ? c15 k1 c20 106.27(16) . . ? c18 k1 c20 68.93(14) . . ? o3 co1 o2 114.12(16) . . ? o3 co1 o1 117.00(16) . . ? o2 co1 o1 117.76(15) . . ? o3 co1 o1 104.80(15) . 3 ? o2 co1 o1 117.75(15) . 3 ? o1 co1 o1 80.33(15) . 3 ? c1 o1 co1 130.6(3) . . ? c1 o1 co1 129.5(3) . 3 ? co1 o1 co1 99.67(15) . 3 ? c7 o2 co1 126.1(3) . . ? c13 o3 co1 128.6(4) . . ? c30 o4 c19 112.0(5) . . ? c30 o4 k1 115.6(3) . . ? c19 o4 k1 113.3(4) . . ? c20 o5 c21 113.5(4) . . ? c20 o5 k1 110.0(3) . . ? c21 o5 k1 110.4(3) . . ? c23 o6 c22 112.7(4) . . ? c23 o6 k1 116.7(3) . . ? c22 o6 k1 113.2(3) . . ? c24 o7 c25 111.6(4) . . ? c24 o7 k1 114.8(3) . . ? c25 o7 k1 114.2(3) . . ? c27 o8 c26 110.2(4) . . ? c27 o8 k1 117.7(4) . . ? c26 o8 k1 115.6(3) . . ? c28 o9 c29 112.9(5) . . ? c28 o9 k1 112.5(4) . . ? c29 o9 k1 115.9(3) . . ? o1 c1 c6 122.1(5) . . ? o1 c1 c2 120.4(4) . . ? c6 c1 c2 117.4(5) . . ? c3 c2 c1 120.3(5) . . ? c4 c3 c2 122.5(6) . . ? c3 c4 c5 118.0(6) . . ? c4 c5 c6 121.3(6) . . ? c5 c6 c1 120.4(6) . . ? o2 c7 c12 119.6(5) . . ? o2 c7 c8 123.6(5) . . ? c12 c7 c8 116.8(5) . . ? c9 c8 c7 121.9(6) . . ? c10 c9 c8 120.0(6) . . ? c10 c9 k1 68.9(4) . 2_545 ? c8 c9 k1 125.3(4) . 2_545 ? c9 c10 c11 118.6(6) . . ? c9 c10 k1 88.4(4) . 2_545 ? c11 c10 k1 117.0(4) . 2_545 ? c12 c11 c10 121.7(6) . . ? c11 c12 c7 121.1(5) . . ? o3 c13 c18 122.5(5) . . ? o3 c13 c14 120.1(5) . . ? c18 c13 c14 117.4(5) . . ? c13 c14 c15 120.4(6) . . ? c16 c15 c14 120.7(7) . . ? c16 c15 k1 69.4(4) . . ? c14 c15 k1 88.7(4) . . ? c17 c16 c15 120.0(6) . . ? c17 c16 k1 78.4(4) . . ? c15 c16 k1 87.4(4) . . ? c16 c17 c18 119.1(7) . . ? c16 c17 k1 77.5(4) . . ? c18 c17 k1 88.2(4) . . ? c13 c18 c17 122.5(6) . . ? c13 c18 k1 88.8(3) . . ? c17 c18 k1 68.5(3) . . ? o4 c19 c20 108.9(5) . . ? o5 c20 c19 109.0(5) . . ? o5 c20 k1 47.7(2) . . ? c19 c20 k1 81.9(3) . . ? o5 c21 c22 107.0(4) . . ? o5 c21 k1 47.2(2) . . ? c22 c21 k1 80.3(3) . . ? o6 c22 c21 109.5(4) . . ? o6 c23 c24 109.4(5) . . ? o7 c24 c23 110.2(5) . . ? o7 c25 c26 108.9(5) . . ? o8 c26 c25 109.8(4) . . ? o8 c27 c28 109.5(5) . . ? o9 c28 c27 108.4(5) . . ? o9 c29 c30 107.9(5) . . ? o4 c30 c29 108.7(5) . . ? cl1 c31 cl2 112.6(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.521 _refine_diff_density_min -0.347 _refine_diff_density_rms 0.074 #===end