Supplementary Material (ESI) for Chemical Communications This journal is (C) The Royal Society of Chemistry 2001 data_ha170 _database_code_CSD 169279 _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Michael J. Zaworotko' _publ_contact_author_name 'Michael J. Zaworotko' _publ_contact_author_address ; Michael J. Zaworotko Department of Chemistry The University of Winnipeg Winnipeg Manitoba, R3B 2E9 Canada ; _publ_contact_author_email 'mike.zaworotko@uwinnipeg.ca' _publ_section_title ; Hydroxylated Nanoballs: Synthesis, Crystal Structure, Solubility and Crystallization on Surfaces ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C200 H72 Cu24 O206.40 S4' _chemical_formula_weight 7430.18 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' 'S' 'S' 0.1246 0.1234 '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 Tetragonal _symmetry_space_group_name_H-M I4/mmm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' '-x, y, -z' 'x, -y, -z' 'y, x, -z' '-y, -x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'y+1/2, x+1/2, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' 'x, -y, z' '-x, y, z' '-y, -x, z' 'y, x, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, x+1/2, z+1/2' _cell_length_a 31.111(4) _cell_length_b 31.111(4) _cell_length_c 35.999(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 34844(8) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour blue-green _exptl_crystal_size_max .2 _exptl_crystal_size_mid .3 _exptl_crystal_size_min .3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.708 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7366 _exptl_absorpt_coefficient_mu 0.778 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 49928 _diffrn_reflns_av_R_equivalents 0.0800 _diffrn_reflns_av_sigmaI/netI 0.0462 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 0.87 _diffrn_reflns_theta_max 21.04 _reflns_number_total 5170 _reflns_number_gt 2724 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.2000P)^2^+0.0000P] 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 5170 _refine_ls_number_parameters 296 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2128 _refine_ls_R_factor_gt 0.1531 _refine_ls_wR_factor_ref 0.4702 _refine_ls_wR_factor_gt 0.4259 _refine_ls_goodness_of_fit_ref 1.679 _refine_ls_restrained_S_all 1.679 _refine_ls_shift/su_max 0.002 _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 0.25604(10) 1.0000 1.0000 0.0965(13) Uani 1 4 d S . . Cu2 Cu 0.34134(11) 1.0000 1.0000 0.1172(16) Uani 1 4 d S . . Cu3 Cu 0.17093(6) 0.82907(6) 0.79193(8) 0.1126(13) Uani 1 2 d S . . Cu4 Cu 0.12862(6) 0.87138(6) 0.84396(8) 0.1051(12) Uani 1 2 d S . . O1 O 0.1899(9) 1.0000 1.0000 0.210(13) Uani 1 4 d S . . O2 O 0.4085(9) 1.0000 1.0000 0.195(13) Uani 1 4 d S . . O3 O 0.2049(3) 0.7951(3) 0.7501(5) 0.158(6) Uani 1 2 d S . . O4 O 0.0941(4) 0.9059(4) 0.8858(7) 0.224(11) Uani 1 2 d S . . O11 O 0.3353(4) 0.9562(4) 0.9620(3) 0.134(4) Uani 1 1 d . . . O12 O 0.2633(3) 0.9558(3) 0.9617(3) 0.114(3) Uani 1 1 d . . . O13 O 0.2217(4) 0.8416(4) 0.8216(3) 0.119(4) Uani 1 1 d . . . O14 O 0.1855(4) 0.8784(3) 0.8666(3) 0.121(4) Uani 1 1 d . . . O15 O 0.3748(5) 0.8569(8) 0.8591(6) 0.279(12) Uani 1 1 d . . . O21 O 0.0780(3) 0.8601(4) 0.8137(3) 0.117(4) Uani 1 1 d . . . O22 O 0.1138(4) 0.8235(4) 0.7690(3) 0.128(4) Uani 1 1 d . . . O23 O 0.0000 0.7837(14) 0.6782(7) 0.33(2) Uani 1 2 d S . . S1 S 0.2033(2) 0.7967(2) 0.7137(3) 0.165(8) Uani 0.50 2 d SP . . C11 C 0.2993(7) 0.9136(6) 0.9172(5) 0.119(6) Uani 1 1 d . . . C12 C 0.2601(6) 0.9010(5) 0.9011(5) 0.109(5) Uani 1 1 d . . . H12 H 0.2337 0.9106 0.9115 0.131 Uiso 1 1 calc R . . C13 C 0.2599(6) 0.8748(5) 0.8705(5) 0.116(5) Uani 1 1 d . . . C14 C 0.3001(8) 0.8574(6) 0.8584(6) 0.148(7) Uani 1 1 d . . . H14 H 0.3008 0.8365 0.8392 0.177 Uiso 1 1 calc R . . C15 C 0.3381(7) 0.8714(9) 0.8748(8) 0.172(9) Uani 1 1 d . . . C16 C 0.3369(7) 0.9007(7) 0.9051(6) 0.153(8) Uani 1 1 d . . . H16 H 0.3627 0.9107 0.9162 0.184 Uiso 1 1 calc R . . C17 C 0.2997(6) 0.9457(6) 0.9493(4) 0.107(5) Uani 1 1 d . . . C18 C 0.2178(6) 0.8641(6) 0.8516(5) 0.109(5) Uani 1 1 d . . . C21 C 0.0000 0.8390(7) 0.7827(7) 0.101(6) Uani 1 2 d S . . H21 H 0.0000 0.8520 0.8066 0.121 Uiso 1 2 calc SR . . C22 C 0.0374(6) 0.8290(5) 0.7643(5) 0.121(5) Uani 1 1 d . . . C23 C 0.0387(7) 0.8080(8) 0.7298(6) 0.168(9) Uani 1 1 d . . . H23 H 0.0652 0.8002 0.7185 0.201 Uiso 1 1 calc R . . C24 C 0.0000 0.7992(10) 0.7131(10) 0.162(11) Uani 1 2 d S . . C25 C 0.0815(6) 0.8382(6) 0.7848(5) 0.109(5) Uani 1 1 d . . . C111 C 0.2380(8) 0.7620(8) 0.6898(9) 0.15(2) Uani 0.50 2 d SP . . C211 C 0.4394(19) 1.0000 0.9726(16) 0.149(18) Uiso 0.50 2 d SP . . O551 O 0.1584(15) 0.0000 0.8999(14) 0.194(16) Uiso 0.50 2 d SP . . O552 O 0.3957(9) 0.7832(10) 0.7846(8) 0.169(10) Uiso 0.50 1 d P . . O553 O 0.3114(11) 0.9784(9) 0.8219(9) 0.196(13) Uiso 0.50 1 d P . . O554 O 0.0808(16) 0.7668(16) 0.6115(16) 0.162(19) Uiso 0.25 1 d P . . O555 O 0.3322(16) 1.0000 0.7898(14) 0.157(16) Uiso 0.40 2 d SP . . O556 O 0.2368(15) 0.7632(15) 0.561(2) 0.24(3) Uiso 0.40 2 d SP . . O557 O 0.4088(15) 0.8260(15) 0.7721(14) 0.141(16) Uiso 0.25 1 d P . . O558 O 0.3841(16) 0.7873(16) 0.7389(15) 0.155(17) Uiso 0.25 1 d P . . O559 O 0.288(2) 1.0000 0.792(2) 0.13(2) Uiso 0.25 2 d SP . . O561 O 0.2712(13) 0.7288(13) 0.5856(17) 0.122(19) Uiso 0.25 2 d SP . . O562 O 0.3675(16) 0.8177(16) 0.7968(14) 0.141(16) Uiso 0.25 1 d P . . O563 O 0.1819(14) 0.8750(14) 0.9672(13) 0.139(15) Uiso 0.25 1 d P . . O564 O 0.277(4) 1.0000 0.829(3) 0.20(4) Uiso 0.25 2 d SP . . O565 O 0.373(3) 0.829(3) 0.0000 0.19(3) Uiso 0.25 2 d SP . . O566 O 0.0000 0.941(2) 0.8267(18) 0.14(2) Uiso 0.25 2 d SP . . O567 O 0.2722(13) 0.7278(13) 0.5123(19) 0.15(3) Uiso 0.25 2 d SP . . O568 O 0.1274(9) 0.0000 0.9223(8) 0.106(9) Uiso 0.50 2 d SP . . 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 0.074(2) 0.142(3) 0.074(2) 0.000 0.000 0.000 Cu2 0.075(3) 0.193(4) 0.083(3) 0.000 0.000 0.000 Cu3 0.1213(16) 0.1213(16) 0.095(2) -0.0264(11) 0.0264(11) 0.0173(16) Cu4 0.1103(15) 0.1103(15) 0.095(2) -0.0285(11) 0.0285(11) 0.0060(15) O1 0.14(2) 0.29(4) 0.21(3) 0.000 0.000 0.000 O2 0.12(2) 0.34(4) 0.13(2) 0.000 0.000 0.000 O3 0.175(10) 0.175(10) 0.124(14) -0.019(8) 0.019(8) 0.071(12) O4 0.220(13) 0.220(13) 0.23(2) -0.092(12) 0.092(12) 0.064(17) O11 0.063(7) 0.214(12) 0.126(9) -0.013(9) 0.008(7) 0.015(7) O12 0.089(8) 0.151(9) 0.102(7) 0.002(7) -0.004(6) -0.007(6) O13 0.136(9) 0.127(8) 0.094(7) -0.043(7) 0.027(7) 0.014(6) O14 0.106(8) 0.146(10) 0.112(8) -0.032(7) 0.032(7) 0.019(7) O15 0.114(12) 0.46(3) 0.26(2) -0.19(2) 0.017(12) 0.076(14) O21 0.111(8) 0.138(9) 0.104(8) -0.032(7) 0.015(7) 0.001(6) O22 0.120(9) 0.156(10) 0.107(8) -0.029(7) 0.031(7) 0.017(7) O23 0.20(2) 0.63(6) 0.147(19) -0.20(3) 0.000 0.000 S1 0.228(13) 0.228(13) 0.040(6) -0.020(4) 0.020(4) 0.174(14) C11 0.104(14) 0.165(16) 0.087(12) 0.000(11) 0.011(12) 0.033(13) C12 0.110(14) 0.139(14) 0.079(11) -0.017(11) 0.021(10) 0.021(10) C13 0.127(16) 0.122(13) 0.101(13) -0.016(11) 0.050(12) 0.004(11) C14 0.149(19) 0.162(17) 0.131(16) -0.037(13) 0.020(16) 0.032(15) C15 0.084(14) 0.26(3) 0.17(2) -0.02(2) -0.009(15) 0.037(16) C16 0.130(18) 0.21(2) 0.116(16) -0.053(16) 0.012(13) 0.016(15) C17 0.067(12) 0.171(16) 0.084(12) 0.011(11) 0.015(10) 0.020(11) C18 0.107(14) 0.111(13) 0.109(15) 0.005(11) 0.004(12) -0.004(11) C21 0.094(16) 0.099(16) 0.110(18) 0.007(13) 0.000 0.000 C22 0.144(17) 0.121(13) 0.097(13) -0.005(11) 0.008(12) 0.002(11) C23 0.153(19) 0.23(2) 0.120(16) -0.064(17) -0.026(15) 0.008(16) C24 0.17(3) 0.19(3) 0.13(3) -0.03(2) 0.000 0.000 C25 0.092(13) 0.134(14) 0.099(13) -0.013(11) 0.015(11) -0.014(10) C111 0.21(3) 0.21(3) 0.03(2) -0.046(14) 0.046(14) 0.14(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 Cu1 O12 1.960(11) 6_577 ? Cu1 O12 1.960(11) 21_575 ? Cu1 O12 1.960(11) 18_557 ? Cu1 O12 1.960(11) . ? Cu1 O1 2.06(3) . ? Cu1 Cu2 2.654(5) . ? Cu2 O11 1.941(13) 21_575 ? Cu2 O11 1.941(13) . ? Cu2 O11 1.941(13) 6_577 ? Cu2 O11 1.941(13) 18_557 ? Cu2 O2 2.09(3) . ? Cu3 O13 1.946(12) . ? Cu3 O13 1.946(12) 23_665 ? Cu3 O22 1.966(12) . ? Cu3 O22 1.966(12) 23_665 ? Cu3 O3 2.121(16) . ? Cu3 Cu4 2.641(3) . ? Cu4 O21 1.946(11) . ? Cu4 O21 1.946(11) 23_665 ? Cu4 O14 1.960(12) 23_665 ? Cu4 O14 1.960(12) . ? Cu4 O4 2.138(16) . ? O2 C211 1.38(6) 18_557 ? O2 C211 1.38(6) . ? O3 S1 1.312(19) . ? O11 C17 1.239(17) . ? O12 C17 1.258(16) . ? O13 C18 1.293(19) . ? O14 C18 1.224(18) . ? O15 C15 1.35(2) . ? O21 C25 1.249(19) . ? O22 C25 1.242(18) . ? O23 C24 1.35(3) . ? S1 C111 1.75(3) . ? C11 C16 1.31(2) . ? C11 C12 1.41(2) . ? C11 C17 1.53(2) . ? C12 C13 1.37(2) . ? C13 C14 1.43(2) . ? C13 C18 1.51(2) . ? C14 C15 1.39(3) . ? C15 C16 1.42(3) . ? C21 C22 1.38(2) . ? C21 C22 1.38(2) 22 ? C22 C23 1.40(2) . ? C22 C25 1.58(2) . ? C23 C24 1.38(2) . ? C24 C23 1.38(2) 22 ? C211 C211 1.98(12) 18_557 ? O551 O568 1.26(5) . ? O552 O562 1.45(5) . ? O552 O557 1.46(5) . ? O552 O558 1.69(6) . ? O553 O564 1.29(9) . ? O553 O553 1.34(6) 21_575 ? O553 O559 1.48(6) . ? O553 O555 1.48(4) . ? O555 O559 1.38(7) . ? O555 O553 1.48(4) 21_575 ? O556 O561 1.75(8) . ? O557 O562 1.58(6) . ? O559 O564 1.41(12) . ? O559 O553 1.48(6) 21_575 ? O564 O553 1.29(9) 21_575 ? O567 O567 0.89(13) 18_556 ? 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 O12 Cu1 O12 89.3(6) 6_577 21_575 ? O12 Cu1 O12 89.2(6) 6_577 18_557 ? O12 Cu1 O12 166.8(7) 21_575 18_557 ? O12 Cu1 O12 166.8(7) 6_577 . ? O12 Cu1 O12 89.2(6) 21_575 . ? O12 Cu1 O12 89.3(6) 18_557 . ? O12 Cu1 O1 96.6(3) 6_577 . ? O12 Cu1 O1 96.6(3) 21_575 . ? O12 Cu1 O1 96.6(3) 18_557 . ? O12 Cu1 O1 96.6(3) . . ? O12 Cu1 Cu2 83.4(3) 6_577 . ? O12 Cu1 Cu2 83.4(3) 21_575 . ? O12 Cu1 Cu2 83.4(3) 18_557 . ? O12 Cu1 Cu2 83.4(3) . . ? O1 Cu1 Cu2 180.000(3) . . ? O11 Cu2 O11 89.2(7) 21_575 . ? O11 Cu2 O11 89.7(7) 21_575 6_577 ? O11 Cu2 O11 168.8(7) . 6_577 ? O11 Cu2 O11 168.8(7) 21_575 18_557 ? O11 Cu2 O11 89.7(7) . 18_557 ? O11 Cu2 O11 89.2(7) 6_577 18_557 ? O11 Cu2 O2 95.6(3) 21_575 . ? O11 Cu2 O2 95.6(3) . . ? O11 Cu2 O2 95.6(3) 6_577 . ? O11 Cu2 O2 95.6(3) 18_557 . ? O11 Cu2 Cu1 84.4(3) 21_575 . ? O11 Cu2 Cu1 84.4(3) . . ? O11 Cu2 Cu1 84.4(3) 6_577 . ? O11 Cu2 Cu1 84.4(3) 18_557 . ? O2 Cu2 Cu1 180.000(3) . . ? O13 Cu3 O13 91.3(7) . 23_665 ? O13 Cu3 O22 168.8(5) . . ? O13 Cu3 O22 88.7(5) 23_665 . ? O13 Cu3 O22 88.7(5) . 23_665 ? O13 Cu3 O22 168.8(5) 23_665 23_665 ? O22 Cu3 O22 89.1(7) . 23_665 ? O13 Cu3 O3 94.9(5) . . ? O13 Cu3 O3 94.9(5) 23_665 . ? O22 Cu3 O3 96.2(5) . . ? O22 Cu3 O3 96.2(5) 23_665 . ? O13 Cu3 Cu4 85.1(3) . . ? O13 Cu3 Cu4 85.1(3) 23_665 . ? O22 Cu3 Cu4 83.8(3) . . ? O22 Cu3 Cu4 83.8(3) 23_665 . ? O3 Cu3 Cu4 179.9(6) . . ? O21 Cu4 O21 88.8(7) . 23_665 ? O21 Cu4 O14 88.8(5) . 23_665 ? O21 Cu4 O14 169.4(5) 23_665 23_665 ? O21 Cu4 O14 169.4(5) . . ? O21 Cu4 O14 88.8(5) 23_665 . ? O14 Cu4 O14 91.6(7) 23_665 . ? O21 Cu4 O4 94.5(6) . . ? O21 Cu4 O4 94.5(6) 23_665 . ? O14 Cu4 O4 96.0(6) 23_665 . ? O14 Cu4 O4 96.0(6) . . ? O21 Cu4 Cu3 85.3(3) . . ? O21 Cu4 Cu3 85.3(3) 23_665 . ? O14 Cu4 Cu3 84.3(3) 23_665 . ? O14 Cu4 Cu3 84.3(3) . . ? O4 Cu4 Cu3 179.6(8) . . ? C211 O2 C211 92(5) 18_557 . ? C211 O2 Cu2 134(3) 18_557 . ? C211 O2 Cu2 134(3) . . ? S1 O3 Cu3 132.2(11) . . ? C17 O11 Cu2 122.1(11) . . ? C17 O12 Cu1 121.9(11) . . ? C18 O13 Cu3 119.5(11) . . ? C18 O14 Cu4 121.3(12) . . ? C25 O21 Cu4 119.5(11) . . ? C25 O22 Cu3 120.4(11) . . ? O3 S1 C111 116.4(16) . . ? C16 C11 C12 123.5(18) . . ? C16 C11 C17 116(2) . . ? C12 C11 C17 120.1(17) . . ? C13 C12 C11 120.0(16) . . ? C12 C13 C14 117.8(19) . . ? C12 C13 C18 119.7(17) . . ? C14 C13 C18 122.5(18) . . ? C15 C14 C13 119.7(19) . . ? O15 C15 C14 116(2) . . ? O15 C15 C16 124(2) . . ? C14 C15 C16 120.3(19) . . ? C11 C16 C15 118(2) . . ? O11 C17 O12 127.4(17) . . ? O11 C17 C11 117.2(16) . . ? O12 C17 C11 115.1(17) . . ? O14 C18 O13 129.7(17) . . ? O14 C18 C13 115.8(17) . . ? O13 C18 C13 114.5(17) . . ? C22 C21 C22 116(2) . 22 ? C21 C22 C23 124(2) . . ? C21 C22 C25 117.8(16) . . ? C23 C22 C25 118.2(17) . . ? C24 C23 C22 117(2) . . ? O23 C24 C23 118.7(16) . . ? O23 C24 C23 118.7(16) . 22 ? C23 C24 C23 122(3) . 22 ? O22 C25 O21 130.9(16) . . ? O22 C25 C22 114.8(16) . . ? O21 C25 C22 114.3(15) . . ? O2 C211 C211 44(3) . 18_557 ? O562 O552 O557 66(3) . . ? O562 O552 O558 96(3) . . ? O557 O552 O558 72(3) . . ? O564 O553 O553 59(3) . 21_575 ? O564 O553 O559 61(5) . . ? O553 O553 O559 63.0(17) 21_575 . ? O564 O553 O555 107(5) . . ? O553 O553 O555 63.1(15) 21_575 . ? O559 O553 O555 56(3) . . ? O559 O555 O553 62(3) . 21_575 ? O559 O555 O553 62(3) . . ? O553 O555 O553 54(3) 21_575 . ? O552 O557 O562 57(3) . . ? O555 O559 O564 106(7) . . ? O555 O559 O553 62(3) . 21_575 ? O564 O559 O553 53(4) . 21_575 ? O555 O559 O553 62(3) . . ? O564 O559 O553 53(4) . . ? O553 O559 O553 54(3) 21_575 . ? O552 O562 O557 57(3) . . ? O553 O564 O553 63(6) . 21_575 ? O553 O564 O559 66(6) . . ? O553 O564 O559 66(6) 21_575 . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 21.04 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.051 _refine_diff_density_min -0.592 _refine_diff_density_rms 0.183