# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Prof. Mino R Caira' _publ_contact_author_address ; Department of Chemistry University of Cape Town Rondebosch 7701 South Africa ; _publ_contact_author_email xraymino@science.uct.ac.za _publ_contact_author_fax '+27 21 689 7499' _publ_contact_author_phone '+27 21 650 3071' loop_ _publ_author_name _publ_author_address M.R.Caira ; Department of Chemistry, University of Cape Town, Rondebosch 7701, South Africa ; S.A.Bourne ; Department of Chemistry, University of Cape Town, Rondebosch 7701, South Africa ; W.T.Mhlongo ; Department of Chemistry, University of Cape Town, Rondebosch 7701, South Africa ; P.M.Dean ; Department of Chemistry, University of Cape Town, Rondebosch 7701, South Africa ; _publ_section_title ; New Crystalline Forms of Permethylated Beta-Cyclodextrin ; #=============================================================================== data_c:\backup\attchdoc\atentmb _database_code_depnum_ccdc_archive 'CCDC 239740' #=============================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; heptakis(2,3,6-tri-O-methyl)-beta-cyclodextrin trihydrate ; _chemical_name_common 'heptakis(2,3,6-tri-O-methyl)-beta-cyclodextrin trihydrate' _chemical_melting_point 'DSC onset 147.7 C, peak 150.9 C ' _chemical_formula_moiety 'C63 H112 O35.3H2O' _chemical_formula_sum 'C63 H118 O38' _chemical_formula_weight 1483.57 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 16.2051(1) _cell_length_b 16.2870(1) _cell_length_c 30.0989(3) _cell_angle_alpha 90.000 _cell_angle_beta 90.000 _cell_angle_gamma 90.000 _cell_volume 7944.1(1) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 19957 _cell_measurement_theta_min 2.98 _cell_measurement_theta_max 27.46 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.65 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas - _exptl_crystal_density_diffrn 1.240 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3200 _exptl_absorpt_coefficient_mu 0.102 _exptl_absorpt_correction_type none _exptl_absorpt_process_details none _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 'Nonius Kappa CCD diffractometer' _diffrn_measurement_method '1.0 deg. phi- and omega-scans' _diffrn_reflns_number 42815 _diffrn_reflns_av_R_equivalents 0.0330 _diffrn_reflns_av_sigmaI/netI 0.0426 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 27.46 _reflns_number_total 17741 _reflns_number_gt 13791 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT 2000' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 1990)' _refine_special_details ; HOST DISORDER: This was of 3 types: (a) twofold disorder of the C6-C9 methoxyl residue attached to C6G1 and twofold disorder of the C6-C9 methoxyl residue attached to C6G3, (b) twofold disorder of methyl atom C9 attached to O6G7, (c) twofold disorder of methyl atom C7 attached to O2G6. In each case, one component of the disordered residue was assigned an s.o.f. (x) based on relative peak heights and the other an sof of (1-x) and the value of x was optimised in the LS process. Disordered atoms were treated with Uiso values fixed or refined at the values listed below. WATER DISORDER: After refinement of the host molecule, remaining peaks with electron densities > 1 eA-3 which were within hydrogen bonding distance of each other and/or host oxygen atoms, were assigned as water O atoms. These were located in 5 sites. A fixed Uiso value of 0.12A**2 (equal to the mean Uiso of the host O6 atoms) was assigned to each of the 5 peaks and their sof's were permitted to refine. The sum of the refined sof's was 2.86, in reasonable agreement with the composition TRIMEB.3H2O deduced from thermo- gravimetric data. 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^)+(0.0962P)^2^+2.5164P] 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 none _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.5(7) _refine_ls_number_reflns 17741 _refine_ls_number_parameters 896 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0820 _refine_ls_R_factor_gt 0.0632 _refine_ls_wR_factor_ref 0.1760 _refine_ls_wR_factor_gt 0.1621 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.015 _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 O61A O 0.0814(3) 0.6800(3) 0.64967(15) 0.090 Uiso 0.748(4) 1 d P A 5 O64A O 0.25963(19) 0.29973(19) 0.42376(10) 0.070 Uiso 0.892(4) 1 d P B 7 C76A C 0.1353(7) 0.8699(7) 0.2434(4) 0.080 Uiso 0.408(7) 1 d P C 1 H71A H 0.0876 0.8330 0.2450 0.120 Uiso 0.408(7) 1 calc PR C 1 H71B H 0.1507 0.8783 0.2123 0.120 Uiso 0.408(7) 1 calc PR C 1 H71C H 0.1210 0.9228 0.2569 0.120 Uiso 0.408(7) 1 calc PR C 1 C91A C 0.0117(4) 0.6276(4) 0.6540(2) 0.090 Uiso 0.748(4) 1 d P A 5 H91A H -0.0347 0.6504 0.6372 0.135 Uiso 0.748(4) 1 calc PR A 5 H91B H -0.0035 0.6231 0.6854 0.135 Uiso 0.748(4) 1 calc PR A 5 H91C H 0.0253 0.5730 0.6424 0.135 Uiso 0.748(4) 1 calc PR A 5 C94A C 0.1886(3) 0.3000(3) 0.39584(15) 0.070 Uiso 0.892(4) 1 d P B 7 H94A H 0.1804 0.2451 0.3833 0.105 Uiso 0.892(4) 1 calc PR B 7 H94B H 0.1965 0.3397 0.3717 0.105 Uiso 0.892(4) 1 calc PR B 7 H94C H 0.1400 0.3155 0.4133 0.105 Uiso 0.892(4) 1 calc PR B 7 C97A C -0.0721(6) 0.8692(7) 0.5292(4) 0.120 Uiso 0.693(10) 1 d P D 3 H97A H -0.1070 0.9127 0.5169 0.180 Uiso 0.693(10) 1 calc PR D 3 H97B H -0.0609 0.8806 0.5606 0.180 Uiso 0.693(10) 1 calc PR D 3 H97C H -0.1005 0.8163 0.5265 0.180 Uiso 0.693(10) 1 calc PR D 3 O61B O 0.0430(8) 0.7041(9) 0.5870(4) 0.090 Uiso 0.252(4) 1 d P A 6 O64B O 0.2068(16) 0.3967(16) 0.4628(8) 0.070 Uiso 0.108(4) 1 d P B 8 C76B C 0.1601(5) 0.8074(5) 0.2286(3) 0.080 Uiso 0.592(7) 1 d P C 2 H71D H 0.1608 0.7473 0.2269 0.120 Uiso 0.592(7) 1 calc PR C 2 H71E H 0.1865 0.8302 0.2020 0.120 Uiso 0.592(7) 1 calc PR C 2 H71F H 0.1030 0.8268 0.2303 0.120 Uiso 0.592(7) 1 calc PR C 2 C91B C -0.0272(13) 0.6498(13) 0.5971(7) 0.090 Uiso 0.252(4) 1 d P A 6 H91D H -0.0579 0.6382 0.5698 0.135 Uiso 0.252(4) 1 calc PR A 6 H91E H -0.0637 0.6769 0.6185 0.135 Uiso 0.252(4) 1 calc PR A 6 H91F H -0.0067 0.5983 0.6098 0.135 Uiso 0.252(4) 1 calc PR A 6 C94B C 0.135(2) 0.388(2) 0.4376(13) 0.070 Uiso 0.108(4) 1 d P B 8 H94D H 0.0867 0.4032 0.4557 0.105 Uiso 0.108(4) 1 calc PR B 8 H94E H 0.1291 0.3309 0.4278 0.105 Uiso 0.108(4) 1 calc PR B 8 H94F H 0.1375 0.4241 0.4116 0.105 Uiso 0.108(4) 1 calc PR B 8 C97B C -0.0765(7) 0.8624(15) 0.4924(8) 0.120 Uiso 0.307(10) 1 d PD D 4 H97D H -0.0864 0.8109 0.4764 0.180 Uiso 0.307(10) 1 calc PR D 4 H97E H -0.0891 0.9090 0.4730 0.180 Uiso 0.307(10) 1 calc PR D 4 H97F H -0.1119 0.8645 0.5188 0.180 Uiso 0.307(10) 1 calc PR D 4 C1G1 C 0.20940(18) 0.88564(19) 0.60629(11) 0.0486(7) Uani 1 1 d . . . H071 H 0.1834 0.9403 0.6119 0.058 Uiso 1 1 calc R . . O2G1 O 0.34352(14) 0.93131(13) 0.63395(8) 0.0562(5) Uani 1 1 d . . . C2G1 C 0.27891(18) 0.87260(18) 0.63918(10) 0.0455(6) Uani 1 1 d . . . H060 H 0.2561 0.8777 0.6699 0.055 Uiso 1 1 calc R . . O3G1 O 0.37489(13) 0.77591(15) 0.66826(8) 0.0580(6) Uani 1 1 d . . . C3G1 C 0.31629(18) 0.78735(18) 0.63395(11) 0.0469(6) Uani 1 1 d . . . H052 H 0.3442 0.7831 0.6044 0.056 Uiso 1 1 calc R . . O4G1 O 0.24135(14) 0.88417(13) 0.56281(7) 0.0523(5) Uani 1 1 d . . . C4G1 C 0.24943(18) 0.72298(17) 0.63725(10) 0.0450(6) Uani 1 1 d . . . H046 H 0.2266 0.7229 0.6681 0.054 Uiso 1 1 calc R . . O5G1 O 0.14977(13) 0.82345(13) 0.61261(8) 0.0555(5) Uani 1 1 d . . . C5G1 C 0.17982(19) 0.74157(19) 0.60452(12) 0.0513(7) Uani 1 1 d . A . H070 H 0.2023 0.7389 0.5736 0.062 Uiso 1 1 calc R . . C6G1 C 0.1075(3) 0.6843(3) 0.60794(13) 0.0689(9) Uiso 1 1 d . . . C7G1 C 0.3246(3) 1.0076(2) 0.65303(19) 0.0802(13) Uani 1 1 d . . . H08I H 0.2696 1.0250 0.6433 0.120 Uiso 1 1 calc R . . H08J H 0.3655 1.0483 0.6436 0.120 Uiso 1 1 calc R . . H08K H 0.3254 1.0027 0.6855 0.120 Uiso 1 1 calc R . . C8G1 C 0.4570(2) 0.7644(3) 0.65289(18) 0.0804(12) Uani 1 1 d . . . H4 H 0.4604 0.7129 0.6361 0.121 Uiso 1 1 calc R . . H5 H 0.4946 0.7619 0.6783 0.121 Uiso 1 1 calc R . . H6 H 0.4726 0.8103 0.6336 0.121 Uiso 1 1 calc R . . C1G2 C 0.26751(18) 0.58008(18) 0.65793(10) 0.0447(6) Uani 1 1 d . . . H059 H 0.2402 0.6035 0.6849 0.054 Uiso 1 1 calc R . . O2G2 O 0.40631(14) 0.58762(15) 0.69108(7) 0.0549(5) Uani 1 1 d . . . C2G2 C 0.34551(18) 0.53546(18) 0.67217(10) 0.0450(6) Uani 1 1 d . . . H061 H 0.3300 0.4933 0.6949 0.054 Uiso 1 1 calc R . . O3G2 O 0.45175(12) 0.44168(13) 0.64937(7) 0.0500(5) Uani 1 1 d . . . C3G2 C 0.38607(16) 0.49163(18) 0.63339(9) 0.0414(6) Uani 1 1 d . . . H039 H 0.4086 0.5333 0.6122 0.050 Uiso 1 1 calc R . . O4G2 O 0.28673(12) 0.64477(12) 0.62845(7) 0.0451(5) Uani 1 1 d . . . C4G2 C 0.32448(16) 0.43694(17) 0.60914(9) 0.0385(6) Uani 1 1 d . . . H020 H 0.3104 0.3889 0.6284 0.046 Uiso 1 1 calc R . . O5G2 O 0.21373(11) 0.52220(12) 0.63823(7) 0.0452(4) Uani 1 1 d . . . C5G2 C 0.24569(17) 0.48480(17) 0.59858(9) 0.0410(6) Uani 1 1 d . . . H023 H 0.2577 0.5281 0.5759 0.049 Uiso 1 1 calc R . . O6G2 O 0.10875(13) 0.47547(14) 0.56991(9) 0.0598(6) Uani 1 1 d . . . C6G2 C 0.17787(17) 0.42860(18) 0.58179(11) 0.0474(7) Uani 1 1 d . . . H05A H 0.1978 0.3974 0.5557 0.057 Uiso 1 1 calc R . . H05B H 0.1626 0.3889 0.6053 0.057 Uiso 1 1 calc R . . C7G2 C 0.3829(3) 0.6209(3) 0.73315(11) 0.0648(9) Uani 1 1 d . . . H07G H 0.3445 0.6667 0.7286 0.097 Uiso 1 1 calc R . . H07H H 0.4321 0.6408 0.7487 0.097 Uiso 1 1 calc R . . H07I H 0.3560 0.5783 0.7510 0.097 Uiso 1 1 calc R . . C8G2 C 0.5294(2) 0.4605(3) 0.6313(2) 0.0988(17) Uani 1 1 d . . . H08L H 0.5281 0.4520 0.5991 0.148 Uiso 1 1 calc R . . H08M H 0.5713 0.4247 0.6446 0.148 Uiso 1 1 calc R . . H08N H 0.5429 0.5179 0.6377 0.148 Uiso 1 1 calc R . . C9G2 C 0.0447(2) 0.4257(3) 0.55440(18) 0.0808(12) Uani 1 1 d . . . H08F H 0.0620 0.3984 0.5269 0.121 Uiso 1 1 calc R . . H08G H -0.0041 0.4595 0.5485 0.121 Uiso 1 1 calc R . . H08H H 0.0313 0.3842 0.5769 0.121 Uiso 1 1 calc R . . C1G3 C 0.34766(18) 0.32794(17) 0.55569(10) 0.0445(6) Uani 1 1 d . . . H047 H 0.3165 0.2987 0.5796 0.053 Uiso 1 1 calc R . . O2G3 O 0.48213(15) 0.28098(15) 0.58360(7) 0.0621(6) Uani 1 1 d . . . C2G3 C 0.42879(19) 0.28192(18) 0.54660(10) 0.0481(7) Uani 1 1 d . . . H053 H 0.4152 0.2239 0.5386 0.058 Uiso 1 1 calc R . . O3G3 O 0.54560(12) 0.27346(12) 0.49723(7) 0.0485(5) Uani 1 1 d . . . C3G3 C 0.47402(16) 0.32128(17) 0.50738(9) 0.0398(6) Uani 1 1 d . . . H036 H 0.4912 0.3783 0.5156 0.048 Uiso 1 1 calc R . . O4G3 O 0.36513(11) 0.40848(12) 0.56984(7) 0.0422(4) Uani 1 1 d . . . C4G3 C 0.41841(17) 0.32459(16) 0.46742(10) 0.0402(6) Uani 1 1 d . . . H034 H 0.4048 0.2675 0.4576 0.048 Uiso 1 1 calc R . . O5G3 O 0.30057(12) 0.32734(13) 0.51629(7) 0.0490(5) Uani 1 1 d . . . C5G3 C 0.33868(16) 0.37027(18) 0.47957(10) 0.0425(6) Uani 1 1 d . B . H035 H 0.3534 0.4270 0.4895 0.051 Uiso 1 1 calc R . . C6G3 C 0.27471(19) 0.3765(2) 0.44312(12) 0.0541(7) Uani 1 1 d . . . C7G3 C 0.4569(3) 0.2283(3) 0.61813(17) 0.0938(14) Uiso 1 1 d . . . H1 H 0.4114 0.2537 0.6345 0.141 Uiso 1 1 calc R . . H2 H 0.5034 0.2186 0.6383 0.141 Uiso 1 1 calc R . . H3 H 0.4386 0.1759 0.6055 0.141 Uiso 1 1 calc R . . C8G3 C 0.62022(18) 0.3113(2) 0.51189(12) 0.0587(8) Uani 1 1 d . . . H06E H 0.6276 0.3637 0.4964 0.088 Uiso 1 1 calc R . . H06F H 0.6670 0.2751 0.5053 0.088 Uiso 1 1 calc R . . H06G H 0.6173 0.3210 0.5440 0.088 Uiso 1 1 calc R . . C1G4 C 0.49774(17) 0.31451(16) 0.40077(9) 0.0404(6) Uani 1 1 d . . . H040 H 0.5226 0.2669 0.4169 0.048 Uiso 1 1 calc R . . O2G4 O 0.62838(12) 0.38905(13) 0.40533(7) 0.0465(5) Uani 1 1 d . . . C2G4 C 0.56561(17) 0.36076(18) 0.37610(10) 0.0429(6) Uani 1 1 d . . . H032 H 0.5918 0.3214 0.3549 0.052 Uiso 1 1 calc R . . O3G4 O 0.60210(15) 0.45517(16) 0.32278(9) 0.0644(6) Uani 1 1 d . . . C3G4 C 0.53216(18) 0.43132(18) 0.34926(10) 0.0443(6) Uani 1 1 d . . . H044 H 0.5153 0.4773 0.3693 0.053 Uiso 1 1 calc R . . O4G4 O 0.45863(11) 0.36760(11) 0.43194(6) 0.0390(4) Uani 1 1 d . . . C4G4 C 0.45950(17) 0.40519(16) 0.31988(9) 0.0400(6) Uani 1 1 d . . . H024 H 0.4817 0.3770 0.2929 0.048 Uiso 1 1 calc R . . O5G4 O 0.44204(13) 0.28509(12) 0.36874(7) 0.0485(5) Uani 1 1 d . . . C5G4 C 0.39912(18) 0.34669(18) 0.34365(10) 0.0445(6) Uani 1 1 d . . . H056 H 0.3644 0.3797 0.3645 0.053 Uiso 1 1 calc R . . O6G4 O 0.39052(19) 0.27046(17) 0.27616(9) 0.0770(8) Uani 1 1 d . . . C6G4 C 0.3428(2) 0.2994(2) 0.31311(11) 0.0564(8) Uani 1 1 d . . . H06A H 0.3181 0.2525 0.3292 0.068 Uiso 1 1 calc R . . H06B H 0.2977 0.3354 0.3025 0.068 Uiso 1 1 calc R . . C7G4 C 0.6959(2) 0.3335(2) 0.40822(13) 0.0578(8) Uani 1 1 d . . . H07D H 0.6778 0.2828 0.4227 0.087 Uiso 1 1 calc R . . H07E H 0.7404 0.3586 0.4256 0.087 Uiso 1 1 calc R . . H07F H 0.7161 0.3210 0.3783 0.087 Uiso 1 1 calc R . . C8G4 C 0.5981(2) 0.5298(3) 0.30173(14) 0.0811(14) Uani 1 1 d . . . H07A H 0.5568 0.5273 0.2780 0.122 Uiso 1 1 calc R . . H07B H 0.6522 0.5430 0.2890 0.122 Uiso 1 1 calc R . . H07C H 0.5824 0.5723 0.3232 0.122 Uiso 1 1 calc R . . C9G4 C 0.3525(4) 0.2096(3) 0.25240(15) 0.0873(13) Uani 1 1 d . . . H09G H 0.3506 0.1593 0.2702 0.131 Uiso 1 1 calc R . . H09H H 0.3834 0.1993 0.2250 0.131 Uiso 1 1 calc R . . H09I H 0.2961 0.2266 0.2450 0.131 Uiso 1 1 calc R . . C1G5 C 0.36327(17) 0.47859(19) 0.27150(9) 0.0439(6) Uani 1 1 d . . . H042 H 0.3727 0.4282 0.2533 0.053 Uiso 1 1 calc R . . O2G5 O 0.45696(13) 0.55422(16) 0.22683(6) 0.0545(6) Uani 1 1 d . . . C2G5 C 0.37454(17) 0.5539(2) 0.24222(9) 0.0452(7) Uani 1 1 d . . . H048 H 0.3370 0.5488 0.2160 0.054 Uiso 1 1 calc R . . O3G5 O 0.35299(15) 0.69841(15) 0.23633(8) 0.0609(6) Uani 1 1 d . . . C3G5 C 0.35291(18) 0.63189(19) 0.26701(10) 0.0455(6) Uani 1 1 d . . . H050 H 0.3954 0.6422 0.2904 0.055 Uiso 1 1 calc R . . O4G5 O 0.42105(12) 0.48036(12) 0.30648(6) 0.0429(4) Uani 1 1 d . . . C4G5 C 0.26876(17) 0.62480(17) 0.28867(9) 0.0420(6) Uani 1 1 d . . . H031 H 0.2253 0.6231 0.2651 0.050 Uiso 1 1 calc R . . O5G5 O 0.28135(12) 0.47721(12) 0.28824(7) 0.0473(5) Uani 1 1 d . . . C5G5 C 0.26385(18) 0.54630(17) 0.31660(10) 0.0437(6) Uani 1 1 d . . . H045 H 0.3077 0.5490 0.3399 0.052 Uiso 1 1 calc R . . O6G5 O 0.11643(14) 0.53673(16) 0.30852(9) 0.0672(7) Uani 1 1 d . . . C6G5 C 0.1827(2) 0.5298(2) 0.33918(12) 0.0546(8) Uani 1 1 d . . . H06C H 0.1832 0.4739 0.3521 0.066 Uiso 1 1 calc R . . H06D H 0.1747 0.5696 0.3637 0.066 Uiso 1 1 calc R . . C7G5 C 0.4704(3) 0.5883(3) 0.18402(13) 0.0819(13) Uani 1 1 d . . . H08R H 0.4317 0.5639 0.1628 0.123 Uiso 1 1 calc R . . H08S H 0.5271 0.5769 0.1745 0.123 Uiso 1 1 calc R . . H08T H 0.4617 0.6479 0.1852 0.123 Uiso 1 1 calc R . . C8G5 C 0.3945(3) 0.7696(3) 0.25247(18) 0.0869(14) Uani 1 1 d . . . H08C H 0.3694 0.7869 0.2806 0.130 Uiso 1 1 calc R . . H08D H 0.3896 0.8139 0.2306 0.130 Uiso 1 1 calc R . . H08E H 0.4529 0.7568 0.2573 0.130 Uiso 1 1 calc R . . C9G5 C 0.0407(3) 0.5143(3) 0.3286(2) 0.0998(17) Uani 1 1 d . . . H09M H 0.0394 0.4548 0.3331 0.150 Uiso 1 1 calc R . . H09N H -0.0051 0.5306 0.3093 0.150 Uiso 1 1 calc R . . H09O H 0.0355 0.5422 0.3573 0.150 Uiso 1 1 calc R . . C1G6 C 0.17675(18) 0.72579(18) 0.32098(10) 0.0453(6) Uani 1 1 d . . . H055 H 0.1393 0.6957 0.3002 0.054 Uiso 1 1 calc R . . O2G6 O 0.20430(18) 0.83365(15) 0.26730(8) 0.0659(7) Uani 1 1 d . . . C2G6 C 0.1731(2) 0.81700(19) 0.31034(11) 0.0500(7) Uani 1 1 d . C . H057 H 0.1139 0.8343 0.3111 0.060 Uiso 1 1 calc R . . O3G6 O 0.20849(15) 0.95267(13) 0.33624(8) 0.0573(6) Uani 1 1 d . C . C3G6 C 0.21978(18) 0.86772(17) 0.34452(10) 0.0463(6) Uani 1 1 d . . . H049 H 0.2799 0.8545 0.3424 0.056 Uiso 1 1 calc R C . O4G6 O 0.25793(12) 0.69677(12) 0.31496(7) 0.0450(4) Uani 1 1 d . . . C4G6 C 0.18934(19) 0.84636(17) 0.39079(11) 0.0470(7) Uani 1 1 d . C . H043 H 0.1297 0.8614 0.3936 0.056 Uiso 1 1 calc R . . O5G6 O 0.14948(13) 0.71285(12) 0.36489(7) 0.0488(5) Uani 1 1 d . C . C5G6 C 0.1997(2) 0.75331(17) 0.39722(10) 0.0473(7) Uani 1 1 d . . . H041 H 0.2588 0.7384 0.3919 0.057 Uiso 1 1 calc R C . O6G6 O 0.1905(2) 0.63669(14) 0.44390(9) 0.0867(10) Uani 1 1 d . . . C6G6 C 0.1743(3) 0.72217(19) 0.44176(12) 0.0674(10) Uani 1 1 d . C . H08A H 0.2054 0.7511 0.4653 0.081 Uiso 1 1 calc R . . H08B H 0.1147 0.7324 0.4465 0.081 Uiso 1 1 calc R . . C8G6 C 0.2730(3) 0.9904(3) 0.31191(18) 0.0899(14) Uani 1 1 d . . . H09D H 0.3237 0.9897 0.3296 0.135 Uiso 1 1 calc R C . H09E H 0.2579 1.0473 0.3051 0.135 Uiso 1 1 calc R . . H09F H 0.2820 0.9603 0.2841 0.135 Uiso 1 1 calc R . . C9G6 C 0.1694(4) 0.6024(4) 0.48543(18) 0.0985(15) Uiso 1 1 d . C . H09J H 0.2076 0.6226 0.5082 0.148 Uiso 1 1 calc R . . H09K H 0.1731 0.5424 0.4837 0.148 Uiso 1 1 calc R . . H09L H 0.1129 0.6183 0.4932 0.148 Uiso 1 1 calc R . . C1G7 C 0.20274(18) 0.96535(18) 0.43687(11) 0.0490(7) Uani 1 1 d . C . H066 H 0.1884 0.9971 0.4095 0.059 Uiso 1 1 calc R . . O2G7 O 0.33885(15) 1.02709(15) 0.43624(9) 0.0653(6) Uani 1 1 d . . . C2G7 C 0.26724(19) 1.01215(19) 0.46275(11) 0.0517(7) Uani 1 1 d . . . H072 H 0.2433 1.0662 0.4719 0.062 Uiso 1 1 calc R . . O3G7 O 0.34515(18) 1.0145(2) 0.53012(10) 0.0862(9) Uani 1 1 d . . . C3G7 C 0.29082(19) 0.9656(2) 0.50382(11) 0.0529(7) Uani 1 1 d . . . H063 H 0.3194 0.9135 0.4952 0.064 Uiso 1 1 calc R . . C4G7 C 0.21484(19) 0.94515(18) 0.53176(11) 0.0484(7) Uani 1 1 d . . . H054 H 0.1965 0.9953 0.5482 0.058 Uiso 1 1 calc R . . O5G7 O 0.13100(12) 0.95726(14) 0.46369(7) 0.0515(5) Uani 1 1 d . . . C5G7 C 0.14319(18) 0.91200(19) 0.50385(11) 0.0491(7) Uani 1 1 d . . . H073 H 0.1546 0.8534 0.4962 0.059 Uiso 1 1 calc R . . O6G7 O 0.00439(19) 0.8662(3) 0.50516(16) 0.1228(14) Uani 1 1 d D . . C6G7 C 0.0611(2) 0.9168(3) 0.52826(15) 0.0728(11) Uani 1 1 d . D . O4G7 O 0.23625(12) 0.88833(12) 0.42428(7) 0.0467(5) Uani 1 1 d . . . C7G7 C 0.3332(3) 1.1024(3) 0.41283(17) 0.0829(12) Uani 1 1 d . . . H08O H 0.2894 1.0986 0.3905 0.124 Uiso 1 1 calc R . . H08P H 0.3859 1.1138 0.3981 0.124 Uiso 1 1 calc R . . H08Q H 0.3205 1.1468 0.4337 0.124 Uiso 1 1 calc R . . C8G7 C 0.4223(2) 0.9787(4) 0.53939(18) 0.1060(19) Uani 1 1 d . . . H09A H 0.4147 0.9315 0.5592 0.159 Uiso 1 1 calc R . . H09B H 0.4580 1.0193 0.5538 0.159 Uiso 1 1 calc R . . H09C H 0.4479 0.9603 0.5116 0.159 Uiso 1 1 calc R . . OW1 O 0.1222(4) 1.1480(4) 0.25440(19) 0.120 Uiso 0.775(9) 1 d P . . OW2 O 0.2174(5) 0.7166(5) 0.1815(2) 0.120 Uiso 0.601(9) 1 d P . . OW3 O 0.0716(6) 0.9898(6) 0.2735(3) 0.120 Uiso 0.484(9) 1 d P . . OW4A O 0.0557(4) 0.6262(5) 0.2331(2) 0.120 Uiso 0.658(9) 1 d P . . OW4B O 0.0583(8) 0.6825(10) 0.2170(5) 0.120 Uiso 0.342(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 C1G1 0.0408(15) 0.0435(15) 0.0616(17) -0.0042(13) 0.0039(13) 0.0054(12) O2G1 0.0486(12) 0.0427(11) 0.0774(15) -0.0030(10) 0.0063(11) -0.0050(9) C2G1 0.0411(15) 0.0431(15) 0.0521(15) -0.0035(12) 0.0058(12) -0.0011(12) O3G1 0.0443(11) 0.0553(13) 0.0743(14) -0.0045(11) -0.0111(11) 0.0033(10) C3G1 0.0371(14) 0.0462(15) 0.0574(17) -0.0049(13) -0.0010(12) 0.0024(12) O4G1 0.0548(12) 0.0491(11) 0.0531(11) -0.0018(9) 0.0022(10) 0.0114(10) C4G1 0.0389(14) 0.0412(14) 0.0548(16) -0.0049(13) 0.0083(12) 0.0043(12) O5G1 0.0415(11) 0.0452(11) 0.0798(15) -0.0047(11) 0.0022(10) 0.0016(9) C5G1 0.0436(15) 0.0436(16) 0.0667(19) -0.0053(14) -0.0046(14) 0.0023(13) C7G1 0.060(2) 0.0417(18) 0.139(4) -0.014(2) -0.014(2) 0.0015(16) C8G1 0.0332(16) 0.073(2) 0.136(4) 0.010(2) -0.005(2) -0.0007(16) C1G2 0.0458(15) 0.0409(14) 0.0473(15) -0.0035(12) 0.0108(12) -0.0037(12) O2G2 0.0546(12) 0.0604(13) 0.0496(11) -0.0075(10) 0.0011(10) -0.0089(11) C2G2 0.0433(15) 0.0445(15) 0.0472(15) 0.0025(12) 0.0057(12) -0.0067(12) O3G2 0.0381(10) 0.0526(12) 0.0594(12) 0.0059(10) 0.0007(9) 0.0016(9) C3G2 0.0334(13) 0.0434(14) 0.0475(15) 0.0034(12) 0.0051(11) -0.0053(11) O4G2 0.0421(10) 0.0414(10) 0.0517(11) -0.0012(9) 0.0123(8) -0.0008(8) C4G2 0.0301(12) 0.0388(13) 0.0467(14) 0.0016(11) 0.0113(11) -0.0012(10) O5G2 0.0349(9) 0.0466(10) 0.0540(11) -0.0049(9) 0.0120(8) -0.0039(8) C5G2 0.0372(13) 0.0402(14) 0.0457(14) 0.0004(11) 0.0076(11) -0.0017(11) O6G2 0.0405(11) 0.0478(12) 0.0912(16) 0.0013(12) -0.0071(11) 0.0026(10) C6G2 0.0372(14) 0.0414(15) 0.0636(18) -0.0007(13) 0.0069(13) 0.0003(12) C7G2 0.076(2) 0.072(2) 0.0473(17) -0.0075(16) -0.0015(16) -0.0098(19) C8G2 0.0356(18) 0.102(4) 0.158(5) 0.039(3) 0.009(2) -0.001(2) C9G2 0.0452(19) 0.067(2) 0.130(4) -0.004(2) -0.020(2) -0.0022(17) C1G3 0.0401(14) 0.0382(14) 0.0554(16) 0.0031(12) 0.0125(12) -0.0029(12) O2G3 0.0658(14) 0.0691(15) 0.0514(12) 0.0209(11) 0.0127(11) 0.0165(12) C2G3 0.0508(17) 0.0398(14) 0.0539(16) 0.0066(13) 0.0140(13) 0.0028(13) O3G3 0.0407(10) 0.0458(11) 0.0591(12) 0.0034(9) 0.0093(9) 0.0110(9) C3G3 0.0353(13) 0.0340(13) 0.0502(15) 0.0020(11) 0.0085(11) 0.0036(11) O4G3 0.0354(10) 0.0409(10) 0.0503(10) 0.0004(8) 0.0124(8) -0.0048(8) C4G3 0.0383(14) 0.0269(12) 0.0554(16) 0.0016(11) 0.0078(12) -0.0030(10) O5G3 0.0352(10) 0.0518(12) 0.0598(12) -0.0056(10) 0.0113(9) -0.0095(9) C5G3 0.0348(13) 0.0390(14) 0.0537(16) -0.0003(12) 0.0056(12) 0.0007(11) C6G3 0.0405(16) 0.0537(17) 0.068(2) -0.0100(15) 0.0026(14) 0.0062(14) C8G3 0.0361(15) 0.077(2) 0.0626(19) 0.0089(17) 0.0014(14) 0.0089(15) C1G4 0.0421(14) 0.0290(12) 0.0500(15) -0.0020(11) 0.0022(12) 0.0054(11) O2G4 0.0380(10) 0.0483(11) 0.0531(11) -0.0004(9) -0.0021(8) 0.0073(9) C2G4 0.0389(14) 0.0424(14) 0.0475(15) -0.0010(12) 0.0052(11) 0.0047(12) O3G4 0.0525(13) 0.0664(15) 0.0741(15) 0.0153(12) 0.0012(11) -0.0099(11) C3G4 0.0448(15) 0.0397(14) 0.0485(15) 0.0060(12) -0.0030(12) -0.0079(12) O4G4 0.0405(10) 0.0299(9) 0.0467(10) 0.0004(7) 0.0065(8) 0.0020(7) C4G4 0.0432(14) 0.0362(13) 0.0407(13) -0.0024(11) 0.0009(11) -0.0020(11) O5G4 0.0576(12) 0.0332(10) 0.0547(11) -0.0038(9) 0.0018(9) -0.0059(9) C5G4 0.0458(15) 0.0396(14) 0.0481(15) -0.0065(12) 0.0033(12) -0.0061(12) O6G4 0.0859(19) 0.0708(17) 0.0744(16) -0.0317(13) 0.0112(14) -0.0233(15) C6G4 0.064(2) 0.0476(17) 0.0575(18) -0.0048(14) -0.0010(15) -0.0138(15) C7G4 0.0419(16) 0.060(2) 0.071(2) 0.0064(16) 0.0028(15) 0.0110(15) C8G4 0.060(2) 0.106(3) 0.077(2) 0.042(2) -0.0238(19) -0.035(2) C9G4 0.124(4) 0.064(2) 0.074(2) -0.020(2) -0.013(3) -0.022(3) C1G5 0.0378(14) 0.0492(16) 0.0448(14) -0.0096(12) -0.0035(11) 0.0005(12) O2G5 0.0393(10) 0.0856(16) 0.0386(10) 0.0013(10) 0.0001(8) 0.0008(11) C2G5 0.0335(13) 0.0619(18) 0.0400(14) 0.0014(13) -0.0045(11) 0.0007(13) O3G5 0.0591(13) 0.0623(14) 0.0614(13) 0.0223(11) 0.0099(11) 0.0029(12) C3G5 0.0412(15) 0.0529(17) 0.0423(14) 0.0093(13) 0.0008(11) -0.0041(13) O4G5 0.0440(10) 0.0394(10) 0.0452(10) -0.0029(8) -0.0064(8) -0.0020(8) C4G5 0.0404(14) 0.0405(14) 0.0450(14) 0.0002(12) -0.0014(12) -0.0006(12) O5G5 0.0405(10) 0.0430(11) 0.0583(11) -0.0098(9) 0.0036(9) -0.0042(9) C5G5 0.0458(15) 0.0382(14) 0.0471(14) -0.0043(12) 0.0061(12) -0.0038(12) O6G5 0.0482(13) 0.0607(15) 0.0927(17) -0.0055(13) 0.0160(12) -0.0058(11) C6G5 0.0566(18) 0.0413(16) 0.0659(19) 0.0031(14) 0.0201(16) -0.0026(14) C7G5 0.066(2) 0.123(4) 0.057(2) 0.023(2) 0.0164(18) 0.005(2) C8G5 0.074(3) 0.062(2) 0.124(4) 0.029(2) 0.026(3) -0.016(2) C9G5 0.050(2) 0.094(3) 0.155(5) 0.013(3) 0.037(3) -0.001(2) C1G6 0.0369(14) 0.0433(15) 0.0559(16) 0.0024(13) 0.0015(12) -0.0022(12) O2G6 0.0934(19) 0.0546(14) 0.0498(12) 0.0065(10) -0.0060(12) 0.0041(13) C2G6 0.0476(16) 0.0443(16) 0.0580(17) 0.0075(14) -0.0054(14) 0.0020(13) O3G6 0.0637(14) 0.0385(11) 0.0697(14) 0.0112(10) 0.0072(11) -0.0038(10) C3G6 0.0383(14) 0.0364(14) 0.0642(18) 0.0047(13) 0.0035(13) 0.0061(12) O4G6 0.0382(10) 0.0413(10) 0.0554(11) -0.0005(9) -0.0006(9) -0.0039(8) C4G6 0.0422(15) 0.0372(14) 0.0616(18) 0.0018(13) -0.0025(13) 0.0020(12) O5G6 0.0456(11) 0.0396(10) 0.0612(12) 0.0022(9) 0.0064(9) -0.0034(9) C5G6 0.0519(16) 0.0340(14) 0.0561(17) 0.0025(12) 0.0018(14) 0.0042(12) O6G6 0.164(3) 0.0380(12) 0.0580(14) 0.0077(10) 0.0161(17) 0.0093(16) C6G6 0.100(3) 0.0364(15) 0.066(2) 0.0026(15) 0.014(2) 0.0057(18) C8G6 0.099(3) 0.058(2) 0.113(3) 0.005(2) 0.039(3) -0.023(2) C1G7 0.0413(15) 0.0377(14) 0.0679(19) 0.0014(13) -0.0032(13) 0.0066(12) O2G7 0.0572(14) 0.0533(13) 0.0855(16) 0.0130(12) 0.0063(12) -0.0049(11) C2G7 0.0474(16) 0.0392(14) 0.0686(19) -0.0001(14) -0.0019(15) 0.0016(13) O3G7 0.0727(17) 0.093(2) 0.0926(19) 0.0031(16) -0.0283(15) -0.0346(16) C3G7 0.0430(15) 0.0483(17) 0.0675(19) -0.0020(15) -0.0075(14) -0.0050(13) C4G7 0.0460(16) 0.0391(14) 0.0602(17) -0.0040(13) -0.0032(13) 0.0047(12) O5G7 0.0358(10) 0.0513(12) 0.0673(13) 0.0003(10) -0.0047(9) 0.0071(9) C5G7 0.0394(15) 0.0430(15) 0.0650(18) 0.0009(14) 0.0025(13) 0.0057(12) O6G7 0.0469(16) 0.165(4) 0.157(3) 0.015(3) -0.0044(19) -0.029(2) C6G7 0.0364(17) 0.088(3) 0.094(3) 0.009(2) 0.0065(17) 0.0017(17) O4G7 0.0419(10) 0.0382(10) 0.0599(12) -0.0022(9) -0.0055(9) 0.0056(8) C7G7 0.083(3) 0.062(2) 0.104(3) 0.022(2) -0.001(2) -0.021(2) C8G7 0.044(2) 0.181(6) 0.093(3) 0.022(4) -0.010(2) -0.031(3) _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 O61A C6G1 1.327(6) . ? O61A C91A 1.422(8) . ? O64A C6G3 1.400(4) . ? O64A C94A 1.426(5) . ? C76A O2G6 1.454(12) . ? C97A O6G7 1.436(10) . ? O61B C6G1 1.263(14) . ? O61B C91B 1.47(2) . ? O64B C6G3 1.29(3) . ? O64B C94B 1.40(4) . ? C76B O2G6 1.433(8) . ? C97B O6G7 1.367(9) . ? C1G1 O4G1 1.408(4) . ? C1G1 O5G1 1.413(4) . ? C1G1 C2G1 1.515(4) . ? O2G1 C7G1 1.403(4) . ? O2G1 C2G1 1.427(4) . ? C2G1 C3G1 1.523(4) . ? O3G1 C3G1 1.415(4) . ? O3G1 C8G1 1.421(4) . ? C3G1 C4G1 1.511(4) . ? O4G1 C4G7 1.430(4) . ? C4G1 O4G2 1.435(3) . ? C4G1 C5G1 1.528(4) . ? O5G1 C5G1 1.440(4) . ? C5G1 C6G1 1.502(5) . ? C1G2 O4G2 1.412(3) . ? C1G2 O5G2 1.414(3) . ? C1G2 C2G2 1.520(4) . ? O2G2 C2G2 1.420(4) . ? O2G2 C7G2 1.429(4) . ? C2G2 C3G2 1.518(4) . ? O3G2 C8G2 1.404(4) . ? O3G2 C3G2 1.423(3) . ? C3G2 C4G2 1.524(4) . ? C4G2 O4G3 1.431(3) . ? C4G2 C5G2 1.529(4) . ? O5G2 C5G2 1.436(3) . ? C5G2 C6G2 1.517(4) . ? O6G2 C9G2 1.398(4) . ? O6G2 C6G2 1.402(4) . ? C1G3 O4G3 1.408(3) . ? C1G3 O5G3 1.410(4) . ? C1G3 C2G3 1.538(4) . ? O2G3 C7G3 1.408(6) . ? O2G3 C2G3 1.410(4) . ? C2G3 C3G3 1.530(4) . ? O3G3 C8G3 1.427(4) . ? O3G3 C3G3 1.430(3) . ? C3G3 C4G3 1.504(4) . ? C4G3 O4G4 1.434(3) . ? C4G3 C5G3 1.535(4) . ? O5G3 C5G3 1.446(3) . ? C5G3 C6G3 1.513(4) . ? C1G4 O5G4 1.405(3) . ? C1G4 O4G4 1.425(3) . ? C1G4 C2G4 1.526(4) . ? O2G4 C2G4 1.422(4) . ? O2G4 C7G4 1.423(4) . ? C2G4 C3G4 1.506(4) . ? O3G4 C8G4 1.372(5) . ? O3G4 C3G4 1.439(4) . ? C3G4 C4G4 1.533(4) . ? C4G4 O4G5 1.432(3) . ? C4G4 C5G4 1.542(4) . ? O5G4 C5G4 1.435(4) . ? C5G4 C6G4 1.506(4) . ? O6G4 C9G4 1.369(5) . ? O6G4 C6G4 1.434(4) . ? C1G5 O4G5 1.409(3) . ? C1G5 O5G5 1.420(3) . ? C1G5 C2G5 1.521(4) . ? O2G5 C2G5 1.414(4) . ? O2G5 C7G5 1.420(4) . ? C2G5 C3G5 1.515(5) . ? O3G5 C3G5 1.424(4) . ? O3G5 C8G5 1.425(5) . ? C3G5 C4G5 1.516(4) . ? C4G5 O4G6 1.425(3) . ? C4G5 C5G5 1.532(4) . ? O5G5 C5G5 1.441(3) . ? C5G5 C6G5 1.505(4) . ? O6G5 C9G5 1.416(5) . ? O6G5 C6G5 1.420(4) . ? C1G6 O5G6 1.409(4) . ? C1G6 O4G6 1.409(3) . ? C1G6 C2G6 1.521(4) . ? O2G6 C2G6 1.417(4) . ? C2G6 C3G6 1.521(4) . ? O3G6 C8G6 1.417(5) . ? O3G6 C3G6 1.418(4) . ? C3G6 C4G6 1.518(4) . ? C4G6 O4G7 1.436(4) . ? C4G6 C5G6 1.537(4) . ? O5G6 C5G6 1.430(4) . ? C5G6 C6G6 1.491(5) . ? O6G6 C9G6 1.411(6) . ? O6G6 C6G6 1.418(4) . ? C1G7 O4G7 1.418(3) . ? C1G7 O5G7 1.421(4) . ? C1G7 C2G7 1.510(4) . ? O2G7 C7G7 1.417(5) . ? O2G7 C2G7 1.429(4) . ? C2G7 C3G7 1.500(5) . ? O3G7 C8G7 1.407(6) . ? O3G7 C3G7 1.427(4) . ? C3G7 C4G7 1.528(5) . ? C4G7 C5G7 1.531(4) . ? O5G7 C5G7 1.429(4) . ? C5G7 C6G7 1.523(5) . ? O6G7 C6G7 1.417(6) . ? OW4A OW4B 1.038(14) . ? 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 C6G1 O61A C91A 111.8(5) . . ? C6G3 O64A C94A 112.5(3) . . ? C6G1 O61B C91B 112.5(13) . . ? C6G3 O64B C94B 116(2) . . ? O4G1 C1G1 O5G1 111.4(3) . . ? O4G1 C1G1 C2G1 109.4(2) . . ? O5G1 C1G1 C2G1 108.7(2) . . ? C7G1 O2G1 C2G1 112.8(3) . . ? O2G1 C2G1 C1G1 112.3(3) . . ? O2G1 C2G1 C3G1 107.9(2) . . ? C1G1 C2G1 C3G1 110.9(2) . . ? C3G1 O3G1 C8G1 114.1(3) . . ? O3G1 C3G1 C4G1 110.0(3) . . ? O3G1 C3G1 C2G1 108.1(2) . . ? C4G1 C3G1 C2G1 109.9(2) . . ? C1G1 O4G1 C4G7 119.0(2) . . ? O4G2 C4G1 C3G1 107.6(2) . . ? O4G2 C4G1 C5G1 111.6(2) . . ? C3G1 C4G1 C5G1 110.5(3) . . ? C1G1 O5G1 C5G1 114.2(2) . . ? O5G1 C5G1 C6G1 107.5(3) . . ? O5G1 C5G1 C4G1 108.9(2) . . ? C6G1 C5G1 C4G1 114.1(3) . . ? O61B C6G1 O61A 102.8(7) . . ? O61B C6G1 C5G1 116.9(7) . . ? O61A C6G1 C5G1 110.3(4) . . ? O4G2 C1G2 O5G2 111.7(2) . . ? O4G2 C1G2 C2G2 110.5(2) . . ? O5G2 C1G2 C2G2 108.2(2) . . ? C2G2 O2G2 C7G2 113.5(3) . . ? O2G2 C2G2 C3G2 106.8(2) . . ? O2G2 C2G2 C1G2 113.8(2) . . ? C3G2 C2G2 C1G2 111.6(2) . . ? C8G2 O3G2 C3G2 114.5(3) . . ? O3G2 C3G2 C2G2 109.4(2) . . ? O3G2 C3G2 C4G2 108.5(2) . . ? C2G2 C3G2 C4G2 111.1(2) . . ? C1G2 O4G2 C4G1 117.0(2) . . ? O4G3 C4G2 C3G2 106.5(2) . . ? O4G3 C4G2 C5G2 112.2(2) . . ? C3G2 C4G2 C5G2 110.4(2) . . ? C1G2 O5G2 C5G2 114.1(2) . . ? O5G2 C5G2 C6G2 105.8(2) . . ? O5G2 C5G2 C4G2 110.2(2) . . ? C6G2 C5G2 C4G2 111.5(2) . . ? C9G2 O6G2 C6G2 111.3(3) . . ? O6G2 C6G2 C5G2 109.6(2) . . ? O4G3 C1G3 O5G3 111.7(2) . . ? O4G3 C1G3 C2G3 109.6(2) . . ? O5G3 C1G3 C2G3 108.0(2) . . ? C7G3 O2G3 C2G3 114.3(3) . . ? O2G3 C2G3 C3G3 108.7(2) . . ? O2G3 C2G3 C1G3 112.9(2) . . ? C3G3 C2G3 C1G3 110.0(2) . . ? C8G3 O3G3 C3G3 112.7(2) . . ? O3G3 C3G3 C4G3 109.6(2) . . ? O3G3 C3G3 C2G3 109.0(2) . . ? C4G3 C3G3 C2G3 110.2(2) . . ? C1G3 O4G3 C4G2 117.3(2) . . ? O4G4 C4G3 C3G3 109.9(2) . . ? O4G4 C4G3 C5G3 108.9(2) . . ? C3G3 C4G3 C5G3 109.3(2) . . ? C1G3 O5G3 C5G3 114.1(2) . . ? O5G3 C5G3 C6G3 107.1(2) . . ? O5G3 C5G3 C4G3 107.9(2) . . ? C6G3 C5G3 C4G3 115.9(2) . . ? O64B C6G3 O64A 105.6(12) . . ? O64B C6G3 C5G3 105.5(11) . . ? O64A C6G3 C5G3 111.2(3) . . ? O5G4 C1G4 O4G4 111.9(2) . . ? O5G4 C1G4 C2G4 107.3(2) . . ? O4G4 C1G4 C2G4 110.0(2) . . ? C2G4 O2G4 C7G4 112.5(2) . . ? O2G4 C2G4 C3G4 110.0(2) . . ? O2G4 C2G4 C1G4 112.0(2) . . ? C3G4 C2G4 C1G4 112.2(2) . . ? C8G4 O3G4 C3G4 117.2(3) . . ? O3G4 C3G4 C2G4 102.7(2) . . ? O3G4 C3G4 C4G4 111.1(2) . . ? C2G4 C3G4 C4G4 112.0(2) . . ? C1G4 O4G4 C4G3 113.34(19) . . ? O4G5 C4G4 C3G4 105.0(2) . . ? O4G5 C4G4 C5G4 112.5(2) . . ? C3G4 C4G4 C5G4 113.0(2) . . ? C1G4 O5G4 C5G4 115.7(2) . . ? O5G4 C5G4 C6G4 104.9(2) . . ? O5G4 C5G4 C4G4 111.6(2) . . ? C6G4 C5G4 C4G4 114.6(2) . . ? C9G4 O6G4 C6G4 113.6(3) . . ? O6G4 C6G4 C5G4 108.4(3) . . ? O4G5 C1G5 O5G5 110.9(2) . . ? O4G5 C1G5 C2G5 109.7(2) . . ? O5G5 C1G5 C2G5 109.3(2) . . ? C2G5 O2G5 C7G5 116.4(3) . . ? O2G5 C2G5 C3G5 112.1(3) . . ? O2G5 C2G5 C1G5 107.9(2) . . ? C3G5 C2G5 C1G5 111.3(2) . . ? C3G5 O3G5 C8G5 113.5(3) . . ? O3G5 C3G5 C2G5 108.6(2) . . ? O3G5 C3G5 C4G5 109.7(2) . . ? C2G5 C3G5 C4G5 110.9(2) . . ? C1G5 O4G5 C4G4 118.8(2) . . ? O4G6 C4G5 C3G5 106.7(2) . . ? O4G6 C4G5 C5G5 112.0(2) . . ? C3G5 C4G5 C5G5 110.3(2) . . ? C1G5 O5G5 C5G5 112.5(2) . . ? O5G5 C5G5 C6G5 107.5(2) . . ? O5G5 C5G5 C4G5 108.5(2) . . ? C6G5 C5G5 C4G5 116.2(3) . . ? C9G5 O6G5 C6G5 110.9(3) . . ? O6G5 C6G5 C5G5 110.7(3) . . ? O5G6 C1G6 O4G6 111.3(2) . . ? O5G6 C1G6 C2G6 109.3(2) . . ? O4G6 C1G6 C2G6 109.7(2) . . ? C2G6 O2G6 C76B 120.6(4) . . ? C2G6 O2G6 C76A 104.8(5) . . ? C76B O2G6 C76A 48.3(5) . . ? O2G6 C2G6 C1G6 111.4(3) . . ? O2G6 C2G6 C3G6 109.7(3) . . ? C1G6 C2G6 C3G6 111.6(2) . . ? C8G6 O3G6 C3G6 114.8(3) . . ? O3G6 C3G6 C4G6 110.1(2) . . ? O3G6 C3G6 C2G6 110.3(2) . . ? C4G6 C3G6 C2G6 109.5(2) . . ? C1G6 O4G6 C4G5 117.5(2) . . ? O4G7 C4G6 C3G6 111.3(2) . . ? O4G7 C4G6 C5G6 108.8(2) . . ? C3G6 C4G6 C5G6 107.8(2) . . ? C1G6 O5G6 C5G6 113.0(2) . . ? O5G6 C5G6 C6G6 107.3(3) . . ? O5G6 C5G6 C4G6 107.8(2) . . ? C6G6 C5G6 C4G6 114.7(3) . . ? C9G6 O6G6 C6G6 112.6(3) . . ? O6G6 C6G6 C5G6 108.9(3) . . ? O4G7 C1G7 O5G7 112.5(2) . . ? O4G7 C1G7 C2G7 108.6(2) . . ? O5G7 C1G7 C2G7 108.7(3) . . ? C7G7 O2G7 C2G7 111.9(3) . . ? O2G7 C2G7 C3G7 109.8(3) . . ? O2G7 C2G7 C1G7 111.1(3) . . ? C3G7 C2G7 C1G7 110.2(3) . . ? C8G7 O3G7 C3G7 115.3(4) . . ? O3G7 C3G7 C2G7 109.4(3) . . ? O3G7 C3G7 C4G7 108.3(3) . . ? C2G7 C3G7 C4G7 111.0(3) . . ? O4G1 C4G7 C3G7 105.6(2) . . ? O4G1 C4G7 C5G7 110.0(2) . . ? C3G7 C4G7 C5G7 112.7(3) . . ? C1G7 O5G7 C5G7 114.5(2) . . ? O5G7 C5G7 C6G7 105.1(3) . . ? O5G7 C5G7 C4G7 112.8(3) . . ? C6G7 C5G7 C4G7 112.3(3) . . ? C97B O6G7 C6G7 141.7(11) . . ? C97B O6G7 C97A 46.8(10) . . ? C6G7 O6G7 C97A 107.0(6) . . ? O6G7 C6G7 C5G7 107.4(4) . . ? C1G7 O4G7 C4G6 114.0(2) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.610 _refine_diff_density_min -0.433 _refine_diff_density_rms 0.052 data_tbbuc _database_code_depnum_ccdc_archive 'CCDC 239741' #=============================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; heptakis(2,3,6-tri-O-methyl)-beta-cyclodextrin ; _chemical_name_common heptakis(2,3,6-tri-O-methyl)-beta-cyclodextrin _chemical_melting_point 'HSM 147-149C' _chemical_formula_moiety 'C63 H112 O35' _chemical_formula_sum 'C63 H112 O35' _chemical_formula_weight 1429.53 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 15.9509(1) _cell_length_b 16.5772(1) _cell_length_c 28.9413(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7652.69(9) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 37345 _cell_measurement_theta_min 3.61 _cell_measurement_theta_max 25.70 _exptl_crystal_description prismatic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas - _exptl_crystal_density_diffrn 1.241 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3080 _exptl_absorpt_coefficient_mu 0.101 _exptl_absorpt_correction_type none _exptl_absorpt_process_details none _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Nonius Kappa CCD diffractometer' _diffrn_measurement_method '1.0 deg. phi- and omega-scans' _diffrn_reflns_number 56677 _diffrn_reflns_av_R_equivalents 0.0562 _diffrn_reflns_av_sigmaI/netI 0.0380 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 3.61 _diffrn_reflns_theta_max 25.70 _reflns_number_total 14499 _reflns_number_gt 13091 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT 2000' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 1990)' _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^)+(0.0516P)^2^+6.2614P] 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 none _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.5(7) _refine_ls_number_reflns 14499 _refine_ls_number_parameters 899 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0609 _refine_ls_R_factor_gt 0.0531 _refine_ls_wR_factor_ref 0.1304 _refine_ls_wR_factor_gt 0.1269 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.107 _refine_ls_shift/su_max 0.040 _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 O2G1 O 0.36293(15) 0.94574(12) 0.62734(8) 0.0352(5) Uani 1 1 d . . . O3G1 O 0.38830(13) 0.79485(13) 0.66575(8) 0.0339(5) Uani 1 1 d . . . O4G1 O 0.29004(12) 0.66995(11) 0.62982(7) 0.0260(4) Uani 1 1 d . . . O5G1 O 0.15726(14) 0.85089(13) 0.61442(8) 0.0329(5) Uani 1 1 d . . . O6G1 O 0.04617(19) 0.7269(2) 0.58204(12) 0.0632(8) Uani 1 1 d . . . C1G1 C 0.2192(2) 0.90902(18) 0.60504(10) 0.0287(6) Uani 1 1 d . . . H1G1 H 0.1959 0.9638 0.6117 0.034 Uiso 1 1 calc R . . C2G1 C 0.2951(2) 0.89393(17) 0.63654(11) 0.0289(6) Uani 1 1 d . . . H2G1 H 0.2771 0.9025 0.6693 0.035 Uiso 1 1 calc R . . C3G1 C 0.32599(18) 0.80815(17) 0.63184(10) 0.0270(6) Uani 1 1 d . . . H3G1 H 0.3508 0.8003 0.6004 0.032 Uiso 1 1 calc R . . C4G1 C 0.25575(19) 0.74821(17) 0.63902(11) 0.0261(6) Uani 1 1 d . . . H4G1 H 0.2367 0.7506 0.6719 0.031 Uiso 1 1 calc R . . C5G1 C 0.1818(2) 0.76855(18) 0.60720(12) 0.0318(7) Uani 1 1 d . . . H5G1 H 0.1986 0.7606 0.5742 0.038 Uiso 1 1 calc R . . C6G1 C 0.1036(2) 0.7182(2) 0.61781(17) 0.0511(10) Uani 1 1 d . . . H6A1 H 0.1192 0.6607 0.6212 0.061 Uiso 1 1 calc R . . H6B1 H 0.0782 0.7364 0.6472 0.061 Uiso 1 1 calc R . . C7G1 C 0.3517(3) 1.0245(2) 0.64455(14) 0.0484(9) Uani 1 1 d . . . H7A1 H 0.3363 1.0219 0.6773 0.073 Uiso 1 1 calc R . . H7B1 H 0.3070 1.0514 0.6272 0.073 Uiso 1 1 calc R . . H7C1 H 0.4040 1.0549 0.6412 0.073 Uiso 1 1 calc R . . C8G1 C 0.4678(2) 0.7732(2) 0.64761(15) 0.0456(9) Uani 1 1 d . . . H8B1 H 0.5059 0.7601 0.6731 0.068 Uiso 1 1 calc R . . H8A1 H 0.4906 0.8184 0.6298 0.068 Uiso 1 1 calc R . . H8C1 H 0.4616 0.7261 0.6274 0.068 Uiso 1 1 calc R . . C9G1 C -0.0278(3) 0.6812(3) 0.5900(2) 0.0796(16) Uani 1 1 d . . . H9B1 H -0.0448 0.6869 0.6224 0.119 Uiso 1 1 calc R . . H9C1 H -0.0169 0.6243 0.5832 0.119 Uiso 1 1 calc R . . H9A1 H -0.0728 0.7010 0.5699 0.119 Uiso 1 1 calc R . . O2G2 O 0.41189(13) 0.60581(12) 0.69103(7) 0.0298(5) Uani 1 1 d . . . O3G2 O 0.43598(13) 0.44962(13) 0.65327(7) 0.0313(5) Uani 1 1 d . . . O4G2 O 0.34639(13) 0.42745(12) 0.56961(7) 0.0261(4) Uani 1 1 d . . . O5G2 O 0.20816(12) 0.55521(12) 0.64029(7) 0.0265(4) Uani 1 1 d . . . O6G2 O 0.13713(13) 0.41356(13) 0.60649(8) 0.0321(5) Uani 1 1 d . . . C1G2 C 0.26780(18) 0.60748(17) 0.66051(10) 0.0254(6) Uani 1 1 d . . . H1G2 H 0.2427 0.6320 0.6889 0.031 Uiso 1 1 calc R . . C2G2 C 0.34496(18) 0.55804(17) 0.67458(10) 0.0257(6) Uani 1 1 d . . . H2G2 H 0.3278 0.5206 0.7000 0.031 Uiso 1 1 calc R . . C3G2 C 0.37931(18) 0.50739(18) 0.63512(10) 0.0249(6) Uani 1 1 d . . . H3G2 H 0.4093 0.5430 0.6126 0.030 Uiso 1 1 calc R . . C4G2 C 0.30943(18) 0.46156(17) 0.61022(10) 0.0247(6) Uani 1 1 d . . . H4G2 H 0.2884 0.4172 0.6306 0.030 Uiso 1 1 calc R . . C5G2 C 0.23754(18) 0.51788(17) 0.59832(10) 0.0261(6) Uani 1 1 d . . . H5G2 H 0.2583 0.5607 0.5768 0.031 Uiso 1 1 calc R . . C6G2 C 0.16268(19) 0.47714(18) 0.57702(11) 0.0286(6) Uani 1 1 d . . . H6B2 H 0.1164 0.5164 0.5732 0.034 Uiso 1 1 calc R . . H6A2 H 0.1775 0.4555 0.5462 0.034 Uiso 1 1 calc R . . C7G2 C 0.3939(2) 0.6434(2) 0.73452(11) 0.0350(7) Uani 1 1 d . . . H7A2 H 0.4454 0.6671 0.7471 0.052 Uiso 1 1 calc R . . H7C2 H 0.3722 0.6029 0.7561 0.052 Uiso 1 1 calc R . . H7B2 H 0.3519 0.6858 0.7301 0.052 Uiso 1 1 calc R . . C8G2 C 0.5211(2) 0.4624(3) 0.64056(16) 0.0517(10) Uani 1 1 d . . . H8A2 H 0.5559 0.4192 0.6534 0.078 Uiso 1 1 calc R . . H8B2 H 0.5401 0.5145 0.6527 0.078 Uiso 1 1 calc R . . H8C2 H 0.5260 0.4623 0.6068 0.078 Uiso 1 1 calc R . . C9G2 C 0.0599(2) 0.3788(2) 0.59323(14) 0.0445(9) Uani 1 1 d . . . H9B2 H 0.0421 0.3398 0.6167 0.067 Uiso 1 1 calc R . . H9A2 H 0.0666 0.3512 0.5635 0.067 Uiso 1 1 calc R . . H9C2 H 0.0174 0.4212 0.5903 0.067 Uiso 1 1 calc R . . O2G3 O 0.45594(15) 0.29504(14) 0.58437(7) 0.0347(5) Uani 1 1 d . . . O3G3 O 0.51247(13) 0.27600(12) 0.49383(7) 0.0278(4) Uani 1 1 d . . . O4G3 O 0.42944(12) 0.37465(11) 0.42650(6) 0.0239(4) Uani 1 1 d . . . O5G3 O 0.27028(13) 0.35025(13) 0.51668(7) 0.0294(4) Uani 1 1 d . . . O6G3 O 0.22455(14) 0.31804(14) 0.42164(8) 0.0369(5) Uani 1 1 d . . . C1G3 C 0.32121(19) 0.34951(18) 0.55720(10) 0.0280(6) Uani 1 1 d . . . H1G3 H 0.2887 0.3252 0.5832 0.034 Uiso 1 1 calc R . . C2G3 C 0.3986(2) 0.29720(18) 0.54740(10) 0.0278(6) Uani 1 1 d . . . H2G3 H 0.3796 0.2409 0.5408 0.033 Uiso 1 1 calc R . . C3G3 C 0.44589(18) 0.32907(17) 0.50529(9) 0.0234(6) Uani 1 1 d . . . H3G3 H 0.4693 0.3836 0.5125 0.028 Uiso 1 1 calc R . . C4G3 C 0.38700(18) 0.33575(17) 0.46415(9) 0.0235(6) Uani 1 1 d . . . H4G3 H 0.3685 0.2807 0.4544 0.028 Uiso 1 1 calc R . . C5G3 C 0.31050(18) 0.38623(18) 0.47750(10) 0.0268(6) Uani 1 1 d . . . H5G3 H 0.3301 0.4414 0.4864 0.032 Uiso 1 1 calc R . . C6G3 C 0.2443(2) 0.3947(2) 0.44068(11) 0.0330(7) Uani 1 1 d . . . H6A3 H 0.1932 0.4190 0.4542 0.040 Uiso 1 1 calc R . . H6B3 H 0.2649 0.4309 0.4160 0.040 Uiso 1 1 calc R . . C7G3 C 0.4242(3) 0.2564(2) 0.62423(12) 0.0456(9) Uani 1 1 d . . . H25A H 0.4708 0.2416 0.6446 0.068 Uiso 1 1 calc R . . H25B H 0.3935 0.2077 0.6152 0.068 Uiso 1 1 calc R . . H25C H 0.3863 0.2932 0.6406 0.068 Uiso 1 1 calc R . . C8G3 C 0.5922(2) 0.3036(2) 0.50903(11) 0.0355(7) Uani 1 1 d . . . H8A3 H 0.5896 0.3163 0.5421 0.053 Uiso 1 1 calc R . . H8B3 H 0.6078 0.3521 0.4917 0.053 Uiso 1 1 calc R . . H8C3 H 0.6342 0.2614 0.5038 0.053 Uiso 1 1 calc R . . C9G3 C 0.1505(2) 0.3196(3) 0.39465(13) 0.0463(9) Uani 1 1 d . . . H9C3 H 0.1039 0.3399 0.4134 0.069 Uiso 1 1 calc R . . H9B3 H 0.1376 0.2650 0.3839 0.069 Uiso 1 1 calc R . . H9A3 H 0.1588 0.3551 0.3680 0.069 Uiso 1 1 calc R . . O2G4 O 0.60449(13) 0.37906(13) 0.40247(7) 0.0300(5) Uani 1 1 d . . . O3G4 O 0.58652(13) 0.45380(12) 0.31735(7) 0.0282(4) Uani 1 1 d . . . O4G4 O 0.40955(12) 0.48941(11) 0.29682(6) 0.0219(4) Uani 1 1 d . . . O5G4 O 0.40763(13) 0.29525(11) 0.36034(7) 0.0251(4) Uani 1 1 d . . . O6G4 O 0.34455(15) 0.28986(13) 0.26061(7) 0.0339(5) Uani 1 1 d . . . C1G4 C 0.46515(18) 0.31995(17) 0.39504(9) 0.0240(6) Uani 1 1 d . . . H1G4 H 0.4845 0.2712 0.4124 0.029 Uiso 1 1 calc R . . C2G4 C 0.54013(18) 0.35756(18) 0.37069(9) 0.0248(6) Uani 1 1 d . . . H2G4 H 0.5635 0.3167 0.3488 0.030 Uiso 1 1 calc R . . C3G4 C 0.51420(18) 0.43087(17) 0.34301(10) 0.0238(6) Uani 1 1 d . . . H3G4 H 0.4983 0.4755 0.3645 0.029 Uiso 1 1 calc R . . C4G4 C 0.44022(18) 0.41176(16) 0.31100(10) 0.0237(6) Uani 1 1 d . . . H4G4 H 0.4613 0.3820 0.2833 0.028 Uiso 1 1 calc R . . C5G4 C 0.37170(18) 0.36132(17) 0.33469(9) 0.0239(6) Uani 1 1 d . . . H5G4 H 0.3403 0.3968 0.3566 0.029 Uiso 1 1 calc R . . C6G4 C 0.3092(2) 0.32255(18) 0.30159(10) 0.0292(6) Uani 1 1 d . . . H6B4 H 0.2795 0.2789 0.3182 0.035 Uiso 1 1 calc R . . H6A4 H 0.2670 0.3635 0.2928 0.035 Uiso 1 1 calc R . . C7G4 C 0.6751(2) 0.3287(2) 0.40008(14) 0.0395(8) Uani 1 1 d . . . H7B4 H 0.7174 0.3473 0.4222 0.059 Uiso 1 1 calc R . . H7A4 H 0.6984 0.3304 0.3688 0.059 Uiso 1 1 calc R . . H7C4 H 0.6587 0.2733 0.4076 0.059 Uiso 1 1 calc R . . C8G4 C 0.5899(2) 0.53604(18) 0.30338(11) 0.0311(7) Uani 1 1 d . . . H8B4 H 0.5713 0.5705 0.3289 0.047 Uiso 1 1 calc R . . H8C4 H 0.5531 0.5442 0.2766 0.047 Uiso 1 1 calc R . . H8A4 H 0.6476 0.5501 0.2950 0.047 Uiso 1 1 calc R . . C9G4 C 0.3749(3) 0.2101(2) 0.26516(13) 0.0452(9) Uani 1 1 d . . . H9C4 H 0.4194 0.2087 0.2885 0.068 Uiso 1 1 calc R . . H9B4 H 0.3974 0.1918 0.2354 0.068 Uiso 1 1 calc R . . H9A4 H 0.3290 0.1745 0.2747 0.068 Uiso 1 1 calc R . . O2G5 O 0.46242(12) 0.57167(13) 0.21564(7) 0.0268(4) Uani 1 1 d . . . O3G5 O 0.37006(14) 0.71220(12) 0.22920(7) 0.0311(5) Uani 1 1 d . . . O4G5 O 0.26226(12) 0.70897(12) 0.30731(7) 0.0258(4) Uani 1 1 d . . . O5G5 O 0.27108(12) 0.49577(11) 0.27122(7) 0.0244(4) Uani 1 1 d . . . O6G5 O 0.11006(14) 0.56360(15) 0.27556(9) 0.0440(6) Uani 1 1 d . . . C1G5 C 0.35676(17) 0.49310(17) 0.25774(10) 0.0228(6) Uani 1 1 d . . . H1G5 H 0.3664 0.4443 0.2381 0.027 Uiso 1 1 calc R . . C2G5 C 0.37731(17) 0.56888(17) 0.22950(10) 0.0237(6) Uani 1 1 d . . . H2G5 H 0.3411 0.5697 0.2013 0.028 Uiso 1 1 calc R . . C3G5 C 0.35955(18) 0.64369(17) 0.25788(10) 0.0237(6) Uani 1 1 d . . . H3G5 H 0.4001 0.6466 0.2842 0.028 Uiso 1 1 calc R . . C4G5 C 0.27032(17) 0.64077(16) 0.27676(9) 0.0225(6) Uani 1 1 d . . . H4G5 H 0.2300 0.6471 0.2506 0.027 Uiso 1 1 calc R . . C5G5 C 0.25155(18) 0.56189(17) 0.30189(10) 0.0250(6) Uani 1 1 d . . . H5G5 H 0.2873 0.5581 0.3302 0.030 Uiso 1 1 calc R . . C6G5 C 0.1602(2) 0.54982(19) 0.31503(12) 0.0360(7) Uani 1 1 d . . . H6A5 H 0.1514 0.4942 0.3265 0.043 Uiso 1 1 calc R . . H6B5 H 0.1444 0.5879 0.3399 0.043 Uiso 1 1 calc R . . C7G5 C 0.4872(2) 0.5048(2) 0.18807(11) 0.0310(7) Uani 1 1 d . . . H7A5 H 0.4984 0.4583 0.2080 0.046 Uiso 1 1 calc R . . H7C5 H 0.5380 0.5187 0.1708 0.046 Uiso 1 1 calc R . . H7B5 H 0.4421 0.4914 0.1664 0.046 Uiso 1 1 calc R . . C8G5 C 0.4045(2) 0.78031(18) 0.25236(13) 0.0371(7) Uani 1 1 d . . . H8A5 H 0.4642 0.7709 0.2584 0.056 Uiso 1 1 calc R . . H8C5 H 0.3751 0.7886 0.2817 0.056 Uiso 1 1 calc R . . H8B5 H 0.3981 0.8283 0.2329 0.056 Uiso 1 1 calc R . . C9G5 C 0.0245(2) 0.5436(3) 0.2825(2) 0.0640(13) Uani 1 1 d . . . H9C5 H 0.0019 0.5759 0.3080 0.096 Uiso 1 1 calc R . . H9B5 H 0.0198 0.4862 0.2902 0.096 Uiso 1 1 calc R . . H9A5 H -0.0072 0.5549 0.2543 0.096 Uiso 1 1 calc R . . O2G6 O 0.20671(14) 0.84105(13) 0.25654(7) 0.0306(5) Uani 1 1 d . . . O3G6 O 0.20294(14) 0.96434(12) 0.32525(7) 0.0296(5) Uani 1 1 d . . . O4G6 O 0.24241(13) 0.91017(12) 0.41677(7) 0.0282(4) Uani 1 1 d . . . O5G6 O 0.15833(13) 0.72879(12) 0.36165(7) 0.0266(4) Uani 1 1 d . . . O6G6 O 0.2113(2) 0.66046(14) 0.44264(8) 0.0511(7) Uani 1 1 d . . . C1G6 C 0.18051(18) 0.73828(17) 0.31483(10) 0.0235(6) Uani 1 1 d . . . H1G6 H 0.1404 0.7068 0.2953 0.028 Uiso 1 1 calc R . . C2G6 C 0.17469(19) 0.82748(17) 0.30157(10) 0.0256(6) Uani 1 1 d . . . H2G6 H 0.1143 0.8436 0.3019 0.031 Uiso 1 1 calc R . . C3G6 C 0.22197(18) 0.88187(17) 0.33477(10) 0.0246(6) Uani 1 1 d . . . H3G6 H 0.2836 0.8727 0.3314 0.030 Uiso 1 1 calc R . . C4G6 C 0.19499(19) 0.86288(17) 0.38435(9) 0.0244(6) Uani 1 1 d . . . H4G6 H 0.1338 0.8745 0.3881 0.029 Uiso 1 1 calc R . . C5G6 C 0.21143(19) 0.77312(17) 0.39252(10) 0.0263(6) Uani 1 1 d . . . H5G6 H 0.2714 0.7608 0.3853 0.032 Uiso 1 1 calc R . . C6G6 C 0.1914(2) 0.74381(18) 0.44070(10) 0.0336(7) Uani 1 1 d . . . H6A6 H 0.2248 0.7740 0.4638 0.040 Uiso 1 1 calc R . . H6B6 H 0.1312 0.7521 0.4475 0.040 Uiso 1 1 calc R . . C7G6 C 0.1539(3) 0.8113(2) 0.22070(11) 0.0412(8) Uani 1 1 d . . . H7B6 H 0.1475 0.7528 0.2240 0.062 Uiso 1 1 calc R . . H7C6 H 0.1791 0.8236 0.1906 0.062 Uiso 1 1 calc R . . H7A6 H 0.0988 0.8372 0.2228 0.062 Uiso 1 1 calc R . . C8G6 C 0.2576(3) 1.0011(2) 0.29231(13) 0.0452(9) Uani 1 1 d . . . H8B6 H 0.3157 0.9967 0.3030 0.068 Uiso 1 1 calc R . . H8C6 H 0.2428 1.0582 0.2888 0.068 Uiso 1 1 calc R . . H8A6 H 0.2518 0.9738 0.2625 0.068 Uiso 1 1 calc R . . C9G6 C 0.1896(4) 0.6273(2) 0.48531(16) 0.0716(14) Uani 1 1 d . . . H9B6 H 0.2202 0.6552 0.5099 0.107 Uiso 1 1 calc R . . H9A6 H 0.2042 0.5699 0.4857 0.107 Uiso 1 1 calc R . . H9C6 H 0.1292 0.6334 0.4903 0.107 Uiso 1 1 calc R . . O2G7 O 0.33704(14) 1.05506(13) 0.42924(8) 0.0348(5) Uani 1 1 d . . . O3G7 O 0.33583(15) 1.04903(15) 0.52814(8) 0.0412(6) Uani 1 1 d . . . O4G7 O 0.24612(14) 0.90649(13) 0.55910(7) 0.0325(5) Uani 1 1 d . . . O5G7 O 0.13065(13) 0.97277(13) 0.45605(7) 0.0300(5) Uani 1 1 d . . . O6G7 O 0.00766(18) 0.8766(2) 0.49450(12) 0.0670(9) Uani 1 1 d . . . C1G7 C 0.20217(19) 0.98390(18) 0.42848(10) 0.0279(6) Uani 1 1 d . . . H1G7 H 0.1858 1.0126 0.3995 0.034 Uiso 1 1 calc R . . C2G7 C 0.26448(19) 1.03598(18) 0.45526(11) 0.0297(6) Uani 1 1 d . . . H2G7 H 0.2359 1.0877 0.4635 0.036 Uiso 1 1 calc R . . C3G7 C 0.2902(2) 0.99443(19) 0.49974(11) 0.0304(7) Uani 1 1 d . . . H3G7 H 0.3265 0.9470 0.4922 0.037 Uiso 1 1 calc R . . C4G7 C 0.2146(2) 0.96601(19) 0.52736(10) 0.0304(6) Uani 1 1 d . . . H4G7 H 0.1913 1.0125 0.5453 0.036 Uiso 1 1 calc R . . C5G7 C 0.14450(19) 0.92864(19) 0.49805(10) 0.0293(6) Uani 1 1 d . . . H5G7 H 0.1611 0.8723 0.4898 0.035 Uiso 1 1 calc R . . C6G7 C 0.0611(2) 0.9258(2) 0.52209(13) 0.0445(8) Uani 1 1 d . . . H6A7 H 0.0673 0.9024 0.5534 0.053 Uiso 1 1 calc R . . H6B7 H 0.0375 0.9808 0.5251 0.053 Uiso 1 1 calc R . . C7G7 C 0.3234(2) 1.1194(2) 0.39793(13) 0.0406(8) Uani 1 1 d . . . H7A7 H 0.3023 1.1665 0.4148 0.061 Uiso 1 1 calc R . . H7C7 H 0.2822 1.1030 0.3747 0.061 Uiso 1 1 calc R . . H7B7 H 0.3763 1.1333 0.3827 0.061 Uiso 1 1 calc R . . C8G7 C 0.4244(2) 1.0374(3) 0.52716(15) 0.0589(11) Uani 1 1 d . . . H8C7 H 0.4509 1.0726 0.5501 0.088 Uiso 1 1 calc R . . H8A7 H 0.4458 1.0506 0.4963 0.088 Uiso 1 1 calc R . . H8B7 H 0.4373 0.9810 0.5344 0.088 Uiso 1 1 calc R . . C9G7 C -0.0738(4) 0.8721(4) 0.5132(2) 0.0935(18) Uiso 1 1 d . . . H9B7 H -0.0704 0.8575 0.5459 0.140 Uiso 1 1 calc R . . H9A7 H -0.1060 0.8310 0.4965 0.140 Uiso 1 1 calc R . . H9C7 H -0.1016 0.9245 0.5100 0.140 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 O2G1 0.0462(13) 0.0205(10) 0.0387(12) -0.0018(9) -0.0050(10) -0.0057(9) O3G1 0.0291(11) 0.0271(11) 0.0457(13) 0.0006(10) -0.0097(10) -0.0012(9) O4G1 0.0280(10) 0.0189(9) 0.0312(11) -0.0027(8) 0.0065(9) -0.0003(8) O5G1 0.0320(11) 0.0259(10) 0.0407(12) -0.0092(9) -0.0014(9) 0.0070(9) O6G1 0.0508(17) 0.0637(19) 0.075(2) 0.0045(16) -0.0203(15) -0.0083(15) C1G1 0.0347(16) 0.0241(14) 0.0273(14) -0.0055(12) -0.0003(13) 0.0071(12) C2G1 0.0363(16) 0.0229(14) 0.0276(15) -0.0032(12) -0.0033(13) 0.0014(13) C3G1 0.0289(15) 0.0240(14) 0.0280(15) -0.0022(11) -0.0036(12) 0.0015(12) C4G1 0.0262(14) 0.0213(14) 0.0309(15) -0.0053(12) 0.0027(12) 0.0028(11) C5G1 0.0300(15) 0.0246(14) 0.0406(17) -0.0082(13) -0.0031(14) 0.0050(13) C6G1 0.0338(18) 0.0287(17) 0.091(3) -0.0010(18) -0.0189(19) -0.0031(15) C7G1 0.068(2) 0.0212(15) 0.056(2) -0.0060(15) -0.020(2) 0.0011(17) C8G1 0.0248(16) 0.0385(19) 0.073(3) 0.0101(18) -0.0030(16) -0.0008(15) C9G1 0.044(2) 0.073(3) 0.122(5) 0.005(3) -0.028(3) -0.013(2) O2G2 0.0308(11) 0.0298(11) 0.0289(11) -0.0065(9) -0.0009(9) -0.0064(9) O3G2 0.0250(10) 0.0339(11) 0.0350(11) -0.0010(9) 0.0017(9) 0.0012(9) O4G2 0.0315(10) 0.0235(10) 0.0233(10) -0.0036(8) 0.0103(8) -0.0059(9) O5G2 0.0245(10) 0.0260(10) 0.0290(10) -0.0051(8) 0.0053(8) -0.0037(8) O6G2 0.0302(11) 0.0258(11) 0.0404(12) -0.0016(9) 0.0004(10) -0.0086(9) C1G2 0.0274(14) 0.0225(13) 0.0264(14) -0.0022(11) 0.0082(12) -0.0062(12) C2G2 0.0283(14) 0.0242(14) 0.0247(14) 0.0007(11) 0.0034(11) -0.0044(12) C3G2 0.0255(14) 0.0255(14) 0.0238(14) -0.0016(11) 0.0043(11) -0.0031(12) C4G2 0.0257(14) 0.0240(13) 0.0243(14) 0.0005(11) 0.0066(12) -0.0048(12) C5G2 0.0291(15) 0.0235(14) 0.0258(14) -0.0018(11) 0.0045(12) -0.0044(12) C6G2 0.0313(15) 0.0245(14) 0.0300(15) -0.0025(12) 0.0016(12) 0.0004(12) C7G2 0.0443(19) 0.0338(16) 0.0269(15) -0.0067(13) -0.0018(14) -0.0045(15) C8G2 0.0279(17) 0.054(2) 0.073(3) 0.003(2) 0.0031(17) 0.0023(17) C9G2 0.0381(18) 0.0377(19) 0.058(2) -0.0141(17) 0.0000(16) -0.0150(16) O2G3 0.0434(13) 0.0365(12) 0.0242(10) 0.0064(9) 0.0081(9) 0.0026(10) O3G3 0.0302(11) 0.0278(11) 0.0254(10) 0.0010(8) 0.0033(8) 0.0059(9) O4G3 0.0299(10) 0.0212(9) 0.0207(9) 0.0012(8) 0.0057(8) 0.0030(8) O5G3 0.0273(10) 0.0311(11) 0.0298(11) -0.0040(9) 0.0067(9) -0.0054(9) O6G3 0.0313(11) 0.0409(12) 0.0386(12) -0.0042(10) -0.0046(10) -0.0030(10) C1G3 0.0312(15) 0.0236(14) 0.0291(15) -0.0007(12) 0.0064(12) -0.0071(12) C2G3 0.0373(16) 0.0231(14) 0.0232(14) 0.0011(11) 0.0081(12) -0.0010(13) C3G3 0.0275(14) 0.0219(13) 0.0209(13) 0.0008(11) 0.0056(11) -0.0009(12) C4G3 0.0308(15) 0.0192(13) 0.0204(13) -0.0007(10) 0.0040(11) -0.0029(11) C5G3 0.0276(14) 0.0265(14) 0.0262(14) -0.0031(12) 0.0052(12) -0.0006(12) C6G3 0.0279(15) 0.0360(17) 0.0352(16) -0.0039(13) 0.0038(13) 0.0051(13) C7G3 0.067(2) 0.0423(19) 0.0276(17) 0.0116(15) 0.0131(17) 0.0077(18) C8G3 0.0298(16) 0.0461(19) 0.0306(16) 0.0041(14) 0.0005(13) 0.0083(15) C9G3 0.0367(18) 0.060(2) 0.0419(19) 0.0058(17) -0.0078(16) -0.0082(18) O2G4 0.0287(11) 0.0321(11) 0.0293(11) -0.0015(9) -0.0034(9) 0.0075(9) O3G4 0.0289(10) 0.0270(10) 0.0286(10) 0.0022(8) 0.0055(9) -0.0023(9) O4G4 0.0287(10) 0.0175(9) 0.0195(9) 0.0001(7) -0.0031(8) 0.0018(8) O5G4 0.0346(11) 0.0182(9) 0.0225(9) 0.0010(8) 0.0011(8) 0.0016(9) O6G4 0.0509(13) 0.0261(10) 0.0247(10) -0.0034(9) -0.0011(10) -0.0045(10) C1G4 0.0316(15) 0.0211(13) 0.0194(13) 0.0001(11) 0.0015(11) 0.0073(12) C2G4 0.0301(15) 0.0255(14) 0.0187(13) 0.0006(11) 0.0002(11) 0.0055(12) C3G4 0.0265(14) 0.0220(14) 0.0228(13) -0.0011(11) 0.0045(11) 0.0009(12) C4G4 0.0284(14) 0.0173(13) 0.0254(14) -0.0019(11) 0.0013(12) 0.0048(11) C5G4 0.0305(14) 0.0205(13) 0.0206(13) -0.0005(11) 0.0011(12) 0.0021(12) C6G4 0.0361(16) 0.0220(13) 0.0294(15) -0.0006(12) -0.0005(13) -0.0043(13) C7G4 0.0259(16) 0.0374(17) 0.055(2) -0.0061(16) 0.0009(15) 0.0054(14) C8G4 0.0325(16) 0.0292(15) 0.0315(16) 0.0037(13) -0.0074(13) -0.0064(13) C9G4 0.064(2) 0.0274(16) 0.044(2) -0.0053(15) 0.0086(18) 0.0012(17) O2G5 0.0246(10) 0.0303(11) 0.0253(10) 0.0007(8) 0.0018(8) 0.0004(9) O3G5 0.0415(12) 0.0225(10) 0.0294(11) 0.0062(9) 0.0062(9) 0.0000(9) O4G5 0.0250(10) 0.0206(9) 0.0319(10) -0.0056(8) -0.0010(8) 0.0001(8) O5G5 0.0227(10) 0.0195(9) 0.0309(10) -0.0041(8) 0.0023(8) 0.0007(8) O6G5 0.0264(11) 0.0434(14) 0.0623(16) -0.0118(12) -0.0002(11) -0.0012(10) C1G5 0.0227(13) 0.0218(13) 0.0239(14) -0.0003(11) -0.0032(11) 0.0007(11) C2G5 0.0214(13) 0.0268(14) 0.0229(13) 0.0028(11) -0.0024(11) 0.0018(11) C3G5 0.0260(14) 0.0196(13) 0.0256(14) 0.0039(11) -0.0008(11) -0.0016(11) C4G5 0.0247(14) 0.0199(13) 0.0230(13) -0.0015(11) 0.0004(11) -0.0011(11) C5G5 0.0289(14) 0.0192(13) 0.0268(14) -0.0022(11) 0.0008(12) 0.0004(12) C6G5 0.0390(17) 0.0235(15) 0.0455(19) -0.0001(13) 0.0143(15) -0.0035(13) C7G5 0.0297(15) 0.0347(16) 0.0284(15) -0.0023(13) 0.0003(13) 0.0034(13) C8G5 0.0368(17) 0.0222(15) 0.052(2) 0.0027(14) 0.0081(15) -0.0044(14) C9G5 0.0318(19) 0.055(2) 0.105(4) -0.024(3) 0.009(2) -0.0046(18) O2G6 0.0412(12) 0.0304(11) 0.0201(10) -0.0014(8) -0.0001(9) -0.0024(10) O3G6 0.0363(11) 0.0208(10) 0.0315(11) 0.0034(8) 0.0020(9) -0.0009(9) O4G6 0.0318(11) 0.0227(10) 0.0303(10) -0.0054(8) -0.0066(9) 0.0062(8) O5G6 0.0289(10) 0.0237(10) 0.0272(10) -0.0013(8) 0.0036(8) -0.0007(9) O6G6 0.095(2) 0.0267(12) 0.0315(12) 0.0039(10) 0.0053(13) 0.0133(13) C1G6 0.0246(14) 0.0232(13) 0.0227(14) -0.0020(11) 0.0003(11) 0.0007(11) C2G6 0.0273(14) 0.0280(14) 0.0216(14) -0.0011(11) -0.0006(11) 0.0012(12) C3G6 0.0279(14) 0.0211(13) 0.0249(14) 0.0005(11) -0.0005(12) 0.0020(12) C4G6 0.0277(14) 0.0232(14) 0.0223(14) -0.0009(11) -0.0049(11) 0.0001(12) C5G6 0.0314(15) 0.0250(14) 0.0224(14) -0.0026(11) -0.0025(12) 0.0035(12) C6G6 0.053(2) 0.0234(14) 0.0247(15) -0.0006(12) 0.0004(14) 0.0101(14) C7G6 0.066(2) 0.0341(17) 0.0234(16) 0.0031(13) -0.0109(16) -0.0042(17) C8G6 0.059(2) 0.0336(17) 0.0434(19) 0.0048(15) 0.0083(17) -0.0128(17) C9G6 0.124(4) 0.033(2) 0.057(3) 0.0167(19) 0.016(3) 0.012(3) O2G7 0.0343(11) 0.0301(11) 0.0400(12) 0.0031(9) -0.0013(10) -0.0004(10) O3G7 0.0418(13) 0.0459(14) 0.0359(12) -0.0089(11) -0.0108(10) -0.0057(11) O4G7 0.0411(12) 0.0314(11) 0.0251(10) -0.0033(9) -0.0016(9) 0.0124(10) O5G7 0.0296(11) 0.0288(11) 0.0316(11) -0.0028(9) -0.0050(9) 0.0053(9) O6G7 0.0384(14) 0.073(2) 0.089(2) 0.0174(18) -0.0104(15) -0.0179(15) C1G7 0.0308(15) 0.0256(14) 0.0275(15) -0.0032(12) -0.0038(12) 0.0081(12) C2G7 0.0308(15) 0.0239(14) 0.0343(16) -0.0026(12) -0.0007(13) 0.0041(12) C3G7 0.0304(15) 0.0294(15) 0.0315(16) -0.0077(12) -0.0071(13) 0.0001(13) C4G7 0.0358(16) 0.0273(15) 0.0280(15) -0.0044(12) -0.0030(13) 0.0088(13) C5G7 0.0304(15) 0.0267(15) 0.0309(15) -0.0015(12) -0.0030(12) 0.0084(13) C6G7 0.0330(17) 0.050(2) 0.051(2) 0.0104(17) 0.0006(16) 0.0065(16) C7G7 0.047(2) 0.0293(16) 0.0456(19) 0.0035(14) -0.0033(16) -0.0060(15) C8G7 0.040(2) 0.085(3) 0.051(2) -0.009(2) -0.0085(18) -0.020(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 O2G1 C2G1 1.407(4) . ? O2G1 C7G1 1.409(4) . ? O3G1 C3G1 1.414(4) . ? O3G1 C8G1 1.418(4) . ? O4G1 C1G2 1.410(3) . ? O4G1 C4G1 1.433(3) . ? O5G1 C1G1 1.406(4) . ? O5G1 C5G1 1.435(4) . ? O6G1 C6G1 1.389(5) . ? O6G1 C9G1 1.421(6) . ? C1G1 O4G7 1.398(4) . ? C1G1 C2G1 1.537(4) . ? C2G1 C3G1 1.511(4) . ? C3G1 C4G1 1.512(4) . ? C4G1 C5G1 1.534(4) . ? C5G1 C6G1 1.532(5) . ? O2G2 C2G2 1.412(4) . ? O2G2 C7G2 1.433(4) . ? O3G2 C3G2 1.418(4) . ? O3G2 C8G2 1.423(4) . ? O4G2 C1G3 1.400(3) . ? O4G2 C4G2 1.431(3) . ? O5G2 C1G2 1.414(3) . ? O5G2 C5G2 1.441(3) . ? O6G2 C9G2 1.414(4) . ? O6G2 C6G2 1.416(4) . ? C1G2 C2G2 1.534(4) . ? C2G2 C3G2 1.520(4) . ? C3G2 C4G2 1.529(4) . ? C4G2 C5G2 1.518(4) . ? C5G2 C6G2 1.504(4) . ? O2G3 C2G3 1.408(4) . ? O2G3 C7G3 1.413(4) . ? O3G3 C3G3 1.418(3) . ? O3G3 C8G3 1.422(4) . ? O4G3 C1G4 1.405(3) . ? O4G3 C4G3 1.436(3) . ? O5G3 C1G3 1.427(4) . ? O5G3 C5G3 1.433(3) . ? O6G3 C9G3 1.416(4) . ? O6G3 C6G3 1.420(4) . ? C1G3 C2G3 1.535(4) . ? C2G3 C3G3 1.528(4) . ? C3G3 C4G3 1.521(4) . ? C4G3 C5G3 1.529(4) . ? C5G3 C6G3 1.507(4) . ? O2G4 C7G4 1.403(4) . ? O2G4 C2G4 1.424(4) . ? O3G4 C8G4 1.423(4) . ? O3G4 C3G4 1.424(3) . ? O4G4 C1G5 1.411(3) . ? O4G4 C4G4 1.437(3) . ? O5G4 C1G4 1.421(4) . ? O5G4 C5G4 1.442(3) . ? O6G4 C9G4 1.414(4) . ? O6G4 C6G4 1.420(4) . ? C1G4 C2G4 1.522(4) . ? C2G4 C3G4 1.513(4) . ? C3G4 C4G4 1.533(4) . ? C4G4 C5G4 1.537(4) . ? C5G4 C6G4 1.524(4) . ? O2G5 C2G5 1.416(3) . ? O2G5 C7G5 1.421(4) . ? O3G5 C3G5 1.417(3) . ? O3G5 C8G5 1.424(4) . ? O4G5 C1G6 1.408(3) . ? O4G5 C4G5 1.441(3) . ? O5G5 C1G5 1.422(3) . ? O5G5 C5G5 1.444(3) . ? O6G5 C6G5 1.413(4) . ? O6G5 C9G5 1.419(5) . ? C1G5 C2G5 1.534(4) . ? C2G5 C3G5 1.514(4) . ? C3G5 C4G5 1.525(4) . ? C4G5 C5G5 1.526(4) . ? C5G5 C6G5 1.520(4) . ? O2G6 C2G6 1.418(3) . ? O2G6 C7G6 1.424(4) . ? O3G6 C3G6 1.427(3) . ? O3G6 C8G6 1.429(4) . ? O4G6 C1G7 1.421(3) . ? O4G6 C4G6 1.438(3) . ? O5G6 C1G6 1.409(3) . ? O5G6 C5G6 1.434(3) . ? O6G6 C9G6 1.396(5) . ? O6G6 C6G6 1.419(4) . ? C1G6 C2G6 1.530(4) . ? C2G6 C3G6 1.518(4) . ? C3G6 C4G6 1.531(4) . ? C4G6 C5G6 1.529(4) . ? C5G6 C6G6 1.511(4) . ? O2G7 C7G7 1.416(4) . ? O2G7 C2G7 1.416(4) . ? O3G7 C3G7 1.423(4) . ? O3G7 C8G7 1.426(5) . ? O4G7 C4G7 1.439(4) . ? O5G7 C1G7 1.404(4) . ? O5G7 C5G7 1.436(4) . ? O6G7 C9G7 1.409(7) . ? O6G7 C6G7 1.424(5) . ? C1G7 C2G7 1.528(4) . ? C2G7 C3G7 1.516(4) . ? C3G7 C4G7 1.522(5) . ? C4G7 C5G7 1.534(4) . ? C5G7 C6G7 1.502(5) . ? 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 C2G1 O2G1 C7G1 113.6(3) . . ? C3G1 O3G1 C8G1 114.3(3) . . ? C1G2 O4G1 C4G1 116.9(2) . . ? C1G1 O5G1 C5G1 115.6(2) . . ? C6G1 O6G1 C9G1 111.8(4) . . ? O4G7 C1G1 O5G1 112.3(2) . . ? O4G7 C1G1 C2G1 108.5(2) . . ? O5G1 C1G1 C2G1 109.1(2) . . ? O2G1 C2G1 C3G1 107.9(2) . . ? O2G1 C2G1 C1G1 113.2(2) . . ? C3G1 C2G1 C1G1 110.9(2) . . ? O3G1 C3G1 C2G1 108.3(2) . . ? O3G1 C3G1 C4G1 108.9(2) . . ? C2G1 C3G1 C4G1 111.4(2) . . ? O4G1 C4G1 C3G1 106.7(2) . . ? O4G1 C4G1 C5G1 112.4(2) . . ? C3G1 C4G1 C5G1 110.1(2) . . ? O5G1 C5G1 C6G1 105.5(3) . . ? O5G1 C5G1 C4G1 109.3(2) . . ? C6G1 C5G1 C4G1 112.7(3) . . ? O6G1 C6G1 C5G1 109.3(3) . . ? C2G2 O2G2 C7G2 112.9(2) . . ? C3G2 O3G2 C8G2 114.3(3) . . ? C1G3 O4G2 C4G2 117.2(2) . . ? C1G2 O5G2 C5G2 113.2(2) . . ? C9G2 O6G2 C6G2 113.0(3) . . ? O4G1 C1G2 O5G2 111.0(2) . . ? O4G1 C1G2 C2G2 111.0(2) . . ? O5G2 C1G2 C2G2 108.8(2) . . ? O2G2 C2G2 C3G2 106.9(2) . . ? O2G2 C2G2 C1G2 113.4(2) . . ? C3G2 C2G2 C1G2 112.6(2) . . ? O3G2 C3G2 C2G2 108.9(2) . . ? O3G2 C3G2 C4G2 107.7(2) . . ? C2G2 C3G2 C4G2 111.5(2) . . ? O4G2 C4G2 C5G2 111.6(2) . . ? O4G2 C4G2 C3G2 106.4(2) . . ? C5G2 C4G2 C3G2 110.6(2) . . ? O5G2 C5G2 C6G2 106.3(2) . . ? O5G2 C5G2 C4G2 108.6(2) . . ? C6G2 C5G2 C4G2 114.6(2) . . ? O6G2 C6G2 C5G2 108.4(2) . . ? C2G3 O2G3 C7G3 113.5(3) . . ? C3G3 O3G3 C8G3 113.4(2) . . ? C1G4 O4G3 C4G3 113.1(2) . . ? C1G3 O5G3 C5G3 113.5(2) . . ? C9G3 O6G3 C6G3 112.5(3) . . ? O4G2 C1G3 O5G3 111.5(2) . . ? O4G2 C1G3 C2G3 109.8(2) . . ? O5G3 C1G3 C2G3 108.1(2) . . ? O2G3 C2G3 C3G3 107.1(2) . . ? O2G3 C2G3 C1G3 113.3(2) . . ? C3G3 C2G3 C1G3 110.4(2) . . ? O3G3 C3G3 C4G3 108.9(2) . . ? O3G3 C3G3 C2G3 110.0(2) . . ? C4G3 C3G3 C2G3 110.2(2) . . ? O4G3 C4G3 C3G3 109.6(2) . . ? O4G3 C4G3 C5G3 108.8(2) . . ? C3G3 C4G3 C5G3 109.6(2) . . ? O5G3 C5G3 C6G3 106.5(2) . . ? O5G3 C5G3 C4G3 109.2(2) . . ? C6G3 C5G3 C4G3 115.6(2) . . ? O6G3 C6G3 C5G3 110.3(3) . . ? C7G4 O2G4 C2G4 113.4(2) . . ? C8G4 O3G4 C3G4 115.8(2) . . ? C1G5 O4G4 C4G4 118.1(2) . . ? C1G4 O5G4 C5G4 113.7(2) . . ? C9G4 O6G4 C6G4 114.5(2) . . ? O4G3 C1G4 O5G4 112.5(2) . . ? O4G3 C1G4 C2G4 110.7(2) . . ? O5G4 C1G4 C2G4 107.3(2) . . ? O2G4 C2G4 C3G4 109.8(2) . . ? O2G4 C2G4 C1G4 111.7(2) . . ? C3G4 C2G4 C1G4 111.1(2) . . ? O3G4 C3G4 C2G4 105.6(2) . . ? O3G4 C3G4 C4G4 111.3(2) . . ? C2G4 C3G4 C4G4 111.4(2) . . ? O4G4 C4G4 C3G4 104.5(2) . . ? O4G4 C4G4 C5G4 111.9(2) . . ? C3G4 C4G4 C5G4 113.0(2) . . ? O5G4 C5G4 C6G4 105.2(2) . . ? O5G4 C5G4 C4G4 111.1(2) . . ? C6G4 C5G4 C4G4 114.4(2) . . ? O6G4 C6G4 C5G4 115.2(3) . . ? C2G5 O2G5 C7G5 113.6(2) . . ? C3G5 O3G5 C8G5 113.9(2) . . ? C1G6 O4G5 C4G5 116.6(2) . . ? C1G5 O5G5 C5G5 113.5(2) . . ? C6G5 O6G5 C9G5 113.0(3) . . ? O4G4 C1G5 O5G5 110.8(2) . . ? O4G4 C1G5 C2G5 109.6(2) . . ? O5G5 C1G5 C2G5 109.0(2) . . ? O2G5 C2G5 C3G5 107.8(2) . . ? O2G5 C2G5 C1G5 112.5(2) . . ? C3G5 C2G5 C1G5 110.0(2) . . ? O3G5 C3G5 C2G5 108.5(2) . . ? O3G5 C3G5 C4G5 110.2(2) . . ? C2G5 C3G5 C4G5 110.1(2) . . ? O4G5 C4G5 C3G5 106.2(2) . . ? O4G5 C4G5 C5G5 111.3(2) . . ? C3G5 C4G5 C5G5 112.4(2) . . ? O5G5 C5G5 C6G5 105.1(2) . . ? O5G5 C5G5 C4G5 108.4(2) . . ? C6G5 C5G5 C4G5 114.9(2) . . ? O6G5 C6G5 C5G5 108.6(3) . . ? C2G6 O2G6 C7G6 113.7(2) . . ? C3G6 O3G6 C8G6 114.1(2) . . ? C1G7 O4G6 C4G6 112.8(2) . . ? C1G6 O5G6 C5G6 113.2(2) . . ? C9G6 O6G6 C6G6 111.3(3) . . ? O4G5 C1G6 O5G6 110.0(2) . . ? O4G5 C1G6 C2G6 110.5(2) . . ? O5G6 C1G6 C2G6 109.5(2) . . ? O2G6 C2G6 C3G6 108.0(2) . . ? O2G6 C2G6 C1G6 111.2(2) . . ? C3G6 C2G6 C1G6 112.6(2) . . ? O3G6 C3G6 C2G6 109.9(2) . . ? O3G6 C3G6 C4G6 108.6(2) . . ? C2G6 C3G6 C4G6 109.4(2) . . ? O4G6 C4G6 C5G6 109.8(2) . . ? O4G6 C4G6 C3G6 110.6(2) . . ? C5G6 C4G6 C3G6 107.3(2) . . ? O5G6 C5G6 C6G6 106.6(2) . . ? O5G6 C5G6 C4G6 107.5(2) . . ? C6G6 C5G6 C4G6 114.8(2) . . ? O6G6 C6G6 C5G6 107.6(2) . . ? C7G7 O2G7 C2G7 112.5(2) . . ? C3G7 O3G7 C8G7 114.2(3) . . ? C1G1 O4G7 C4G7 118.6(2) . . ? C1G7 O5G7 C5G7 115.0(2) . . ? C9G7 O6G7 C6G7 111.6(4) . . ? O5G7 C1G7 O4G6 112.9(2) . . ? O5G7 C1G7 C2G7 108.3(2) . . ? O4G6 C1G7 C2G7 108.2(2) . . ? O2G7 C2G7 C3G7 109.4(2) . . ? O2G7 C2G7 C1G7 112.8(2) . . ? C3G7 C2G7 C1G7 110.5(3) . . ? O3G7 C3G7 C2G7 109.9(3) . . ? O3G7 C3G7 C4G7 107.4(2) . . ? C2G7 C3G7 C4G7 111.9(2) . . ? O4G7 C4G7 C3G7 105.7(2) . . ? O4G7 C4G7 C5G7 109.3(2) . . ? C3G7 C4G7 C5G7 114.3(2) . . ? O5G7 C5G7 C6G7 105.8(3) . . ? O5G7 C5G7 C4G7 112.0(3) . . ? C6G7 C5G7 C4G7 113.7(3) . . ? O6G7 C6G7 C5G7 106.7(3) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.70 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.402 _refine_diff_density_min -0.486 _refine_diff_density_rms 0.068