# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_[K(L-H)] _database_code_depnum_ccdc_archive 'CCDC 917258' #TrackingRef '16474_web_deposit_cif_file_0_YongHuang_1356657153.[K(L-H)].cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C100 H104 K2 O6, 2(C7 H8)' _chemical_formula_sum 'C114 H122 K2 O6' _chemical_formula_weight 1666.32 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.889(3) _cell_length_b 11.600(2) _cell_length_c 27.630(6) _cell_angle_alpha 90.00 _cell_angle_beta 100.77(3) _cell_angle_gamma 90.00 _cell_volume 4687.9(16) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 10946 _cell_measurement_theta_min 5.097 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.180 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1784 _exptl_absorpt_coefficient_mu 0.157 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.972 _exptl_absorpt_correction_T_max 0.981 _exptl_absorpt_process_details 'SADABS, Sheldrick (1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16533 _diffrn_reflns_av_R_equivalents 0.0429 _diffrn_reflns_av_sigmaI/netI 0.0646 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 5.14 _diffrn_reflns_theta_max 25.50 _reflns_number_total 8617 _reflns_number_gt 5596 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _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^)+(0.0650P)^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 SHELXL _refine_ls_extinction_coef 0.0062(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8617 _refine_ls_number_parameters 555 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0875 _refine_ls_R_factor_gt 0.0465 _refine_ls_wR_factor_ref 0.1238 _refine_ls_wR_factor_gt 0.1122 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _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 K K 0.65450(3) 0.36326(4) 0.509782(18) 0.03466(15) Uani 1 1 d . . . O1 O 0.60661(8) 0.52398(11) 0.44080(5) 0.0268(3) Uani 1 1 d . . . O2 O 0.65940(8) 0.58104(11) 0.55351(5) 0.0251(3) Uani 1 1 d . . . O3 O 0.53511(9) 0.36499(11) 0.56891(5) 0.0278(3) Uani 1 1 d . . . H2A H 0.468(2) 0.411(2) 0.5642(11) 0.084(9) Uiso 1 1 d . . . C1 C 0.68465(12) 0.58512(16) 0.44402(7) 0.0235(4) Uani 1 1 d . . . C2 C 0.74078(12) 0.57054(16) 0.40847(7) 0.0250(4) Uani 1 1 d . . . C3 C 0.82017(12) 0.63568(16) 0.41349(7) 0.0268(5) Uani 1 1 d . . . H3A H 0.8572 0.6267 0.3901 0.032 Uiso 1 1 calc R . . C4 C 0.84732(12) 0.71384(16) 0.45179(7) 0.0243(4) Uani 1 1 d . . . C5 C 0.79228(12) 0.72391(16) 0.48659(7) 0.0247(4) Uani 1 1 d . . . H5A H 0.8095 0.7738 0.5130 0.030 Uiso 1 1 calc R . . C6 C 0.71154(12) 0.66120(16) 0.48312(7) 0.0231(4) Uani 1 1 d . . . C7 C 0.65266(12) 0.67799(16) 0.52085(7) 0.0247(4) Uani 1 1 d . . . H7A H 0.6715 0.7473 0.5397 0.030 Uiso 1 1 calc R . . H7B H 0.5896 0.6878 0.5045 0.030 Uiso 1 1 calc R . . C8 C 0.59636(12) 0.59461(17) 0.58673(7) 0.0247(4) Uani 1 1 d . . . H8A H 0.5341 0.5891 0.5686 0.030 Uiso 1 1 calc R . . H8B H 0.6043 0.6700 0.6021 0.030 Uiso 1 1 calc R . . C9 C 0.61294(12) 0.50309(16) 0.62540(7) 0.0249(4) Uani 1 1 d . . . C10 C 0.66000(12) 0.52948(17) 0.67219(8) 0.0286(5) Uani 1 1 d . . . H10A H 0.6807 0.6045 0.6788 0.034 Uiso 1 1 calc R . . C11 C 0.67749(13) 0.44849(18) 0.70958(7) 0.0295(5) Uani 1 1 d . . . C12 C 0.64597(13) 0.33682(19) 0.69806(8) 0.0330(5) Uani 1 1 d . . . H12A H 0.6574 0.2807 0.7225 0.040 Uiso 1 1 calc R . . C13 C 0.59808(13) 0.30520(17) 0.65163(8) 0.0299(5) Uani 1 1 d . . . C14 C 0.58089(12) 0.39030(17) 0.61449(7) 0.0261(5) Uani 1 1 d . . . C15 C 0.71148(13) 0.48786(17) 0.36459(8) 0.0296(5) Uani 1 1 d . . . C16 C 0.78642(15) 0.47268(19) 0.33371(8) 0.0378(5) Uani 1 1 d . . . H16A H 0.7654 0.4208 0.3069 0.057 Uiso 1 1 calc R . . H16B H 0.8404 0.4417 0.3540 0.057 Uiso 1 1 calc R . . H16C H 0.8003 0.5461 0.3209 0.057 Uiso 1 1 calc R . . C17 C 0.62766(14) 0.53865(19) 0.33035(8) 0.0374(5) Uani 1 1 d . . . H17A H 0.6089 0.4877 0.3029 0.056 Uiso 1 1 calc R . . H17B H 0.6431 0.6125 0.3185 0.056 Uiso 1 1 calc R . . H17C H 0.5786 0.5474 0.3482 0.056 Uiso 1 1 calc R . . C18 C 0.69247(13) 0.36807(17) 0.38394(8) 0.0295(5) Uani 1 1 d . . . C19 C 0.76149(14) 0.31203(18) 0.41625(8) 0.0342(5) Uani 1 1 d . . . H19A H 0.8241 0.3406 0.4189 0.041 Uiso 1 1 calc R . . C20 C 0.74953(15) 0.20251(19) 0.43352(9) 0.0418(6) Uani 1 1 d . . . H20A H 0.8038 0.1568 0.4471 0.050 Uiso 1 1 calc R . . C21 C 0.66708(16) 0.1460(2) 0.41859(9) 0.0444(6) Uani 1 1 d . . . H21A H 0.6587 0.0719 0.4298 0.053 Uiso 1 1 calc R . . C22 C 0.59782(16) 0.2006(2) 0.38697(9) 0.0437(6) Uani 1 1 d . . . H22A H 0.5421 0.1634 0.3770 0.052 Uiso 1 1 calc R . . C23 C 0.61049(13) 0.31025(19) 0.36995(8) 0.0364(5) Uani 1 1 d . . . H23A H 0.5629 0.3460 0.3486 0.044 Uiso 1 1 calc R . . C24 C 0.93163(12) 0.79014(17) 0.45193(8) 0.0273(5) Uani 1 1 d . . . C25 C 0.96866(14) 0.8412(2) 0.50311(8) 0.0406(6) Uani 1 1 d . . . H25A H 1.0211 0.8882 0.5016 0.061 Uiso 1 1 calc R . . H25B H 0.9858 0.7798 0.5263 0.061 Uiso 1 1 calc R . . H25C H 0.9222 0.8874 0.5134 0.061 Uiso 1 1 calc R . . C26 C 0.90195(14) 0.89093(18) 0.41691(9) 0.0398(6) Uani 1 1 d . . . H26A H 0.8784 0.8618 0.3845 0.060 Uiso 1 1 calc R . . H26B H 0.9536 0.9398 0.4158 0.060 Uiso 1 1 calc R . . H26C H 0.8553 0.9344 0.4284 0.060 Uiso 1 1 calc R . . C27 C 1.00744(12) 0.71807(17) 0.43638(8) 0.0283(5) Uani 1 1 d . . . C28 C 1.03780(14) 0.7369(2) 0.39276(9) 0.0378(6) Uani 1 1 d . . . H28A H 1.0126 0.7966 0.3722 0.045 Uiso 1 1 calc R . . C29 C 1.10521(15) 0.6682(2) 0.37912(11) 0.0535(7) Uani 1 1 d . . . H29A H 1.1237 0.6814 0.3493 0.064 Uiso 1 1 calc R . . C30 C 1.14435(16) 0.5820(3) 0.40896(14) 0.0629(9) Uani 1 1 d . . . H30A H 1.1901 0.5369 0.3998 0.076 Uiso 1 1 calc R . . C31 C 1.11593(16) 0.5615(2) 0.45313(13) 0.0612(9) Uani 1 1 d . . . H31A H 1.1426 0.5027 0.4738 0.073 Uiso 1 1 calc R . . C32 C 1.04720(14) 0.62927(19) 0.46637(9) 0.0410(6) Uani 1 1 d . . . H32A H 1.0277 0.6146 0.4958 0.049 Uiso 1 1 calc R . . C33 C 0.72519(14) 0.4855(2) 0.76117(8) 0.0364(5) Uani 1 1 d . . . C34 C 0.75718(16) 0.3822(2) 0.79515(9) 0.0480(6) Uani 1 1 d . . . H34A H 0.7054 0.3356 0.7984 0.072 Uiso 1 1 calc R . . H34B H 0.7861 0.4099 0.8270 0.072 Uiso 1 1 calc R . . H34C H 0.7999 0.3369 0.7812 0.072 Uiso 1 1 calc R . . C35 C 0.65657(17) 0.5528(3) 0.78475(9) 0.0587(7) Uani 1 1 d . . . H35A H 0.6350 0.6181 0.7645 0.088 Uiso 1 1 calc R . . H35B H 0.6857 0.5789 0.8168 0.088 Uiso 1 1 calc R . . H35C H 0.6059 0.5038 0.7877 0.088 Uiso 1 1 calc R . . C36 C 0.81016(14) 0.55697(19) 0.75713(8) 0.0338(5) Uani 1 1 d . . . C37 C 0.82598(17) 0.6668(2) 0.77576(9) 0.0481(6) Uani 1 1 d . . . H37A H 0.7827 0.7020 0.7911 0.058 Uiso 1 1 calc R . . C38 C 0.9050(2) 0.7256(2) 0.77199(10) 0.0613(8) Uani 1 1 d . . . H38A H 0.9144 0.7993 0.7852 0.074 Uiso 1 1 calc R . . C39 C 0.96896(19) 0.6778(3) 0.74939(10) 0.0608(8) Uani 1 1 d . . . H39A H 1.0219 0.7182 0.7470 0.073 Uiso 1 1 calc R . . C40 C 0.95486(16) 0.5691(3) 0.73007(9) 0.0539(7) Uani 1 1 d . . . H40A H 0.9985 0.5353 0.7145 0.065 Uiso 1 1 calc R . . C41 C 0.87577(14) 0.5096(2) 0.73363(8) 0.0399(6) Uani 1 1 d . . . H41A H 0.8666 0.4363 0.7200 0.048 Uiso 1 1 calc R . . C42 C 0.56471(13) 0.18158(18) 0.64035(8) 0.0347(5) Uani 1 1 d . . . C43 C 0.45898(14) 0.1806(2) 0.62461(10) 0.0450(6) Uani 1 1 d . . . H43A H 0.4413 0.2286 0.5961 0.068 Uiso 1 1 calc R . . H43B H 0.4318 0.2095 0.6511 0.068 Uiso 1 1 calc R . . H43C H 0.4384 0.1032 0.6169 0.068 Uiso 1 1 calc R . . C44 C 0.58780(16) 0.1037(2) 0.68581(9) 0.0460(6) Uani 1 1 d . . . H44A H 0.6529 0.1016 0.6968 0.069 Uiso 1 1 calc R . . H44B H 0.5657 0.0271 0.6774 0.069 Uiso 1 1 calc R . . H44C H 0.5592 0.1335 0.7116 0.069 Uiso 1 1 calc R . . C45 C 0.61175(13) 0.12853(17) 0.60109(8) 0.0334(5) Uani 1 1 d . . . C46 C 0.57015(15) 0.04527(19) 0.56834(9) 0.0414(6) Uani 1 1 d . . . H46A H 0.5094 0.0259 0.5680 0.050 Uiso 1 1 calc R . . C47 C 0.61697(17) -0.0095(2) 0.53619(10) 0.0479(6) Uani 1 1 d . . . H47A H 0.5873 -0.0648 0.5145 0.057 Uiso 1 1 calc R . . C48 C 0.70723(16) 0.0169(2) 0.53591(9) 0.0464(6) Uani 1 1 d . . . H48A H 0.7390 -0.0208 0.5146 0.056 Uiso 1 1 calc R . . C49 C 0.74899(15) 0.0998(2) 0.56763(10) 0.0457(6) Uani 1 1 d . . . H49A H 0.8097 0.1189 0.5676 0.055 Uiso 1 1 calc R . . C50 C 0.70229(14) 0.15547(19) 0.59961(9) 0.0395(6) Uani 1 1 d . . . H50A H 0.7396 0.1807 0.6309 0.047 Uiso 1 1 calc R . . C51 C 0.74184(18) 0.8650(2) 0.66117(13) 0.0741(9) Uani 1 1 d . . . H51A H 0.7018 0.8019 0.6498 0.111 Uiso 1 1 calc R . . H51B H 0.7182 0.9344 0.6445 0.111 Uiso 1 1 calc R . . H51C H 0.7458 0.8746 0.6960 0.111 Uiso 1 1 calc R . . C52 C 0.83436(16) 0.8408(2) 0.65058(10) 0.0521(7) Uani 1 1 d . . . C53 C 0.85465(18) 0.7398(2) 0.62853(9) 0.0522(7) Uani 1 1 d . . . H53A H 0.8089 0.6855 0.6189 0.063 Uiso 1 1 calc R . . C54 C 0.94154(19) 0.7182(2) 0.62053(9) 0.0540(7) Uani 1 1 d . . . H54A H 0.9541 0.6496 0.6057 0.065 Uiso 1 1 calc R . . C55 C 1.01013(19) 0.7983(2) 0.63440(9) 0.0552(7) Uani 1 1 d . . . H55A H 1.0691 0.7838 0.6293 0.066 Uiso 1 1 calc R . . C56 C 0.99034(18) 0.8992(2) 0.65583(9) 0.0534(7) Uani 1 1 d . . . H56A H 1.0360 0.9538 0.6651 0.064 Uiso 1 1 calc R . . C57 C 0.90361(19) 0.9204(2) 0.66375(10) 0.0563(7) Uani 1 1 d . . . H57A H 0.8912 0.9895 0.6782 0.068 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 K 0.0340(3) 0.0322(3) 0.0399(3) -0.0003(2) 0.0120(2) 0.0031(2) O1 0.0207(7) 0.0282(7) 0.0317(8) -0.0022(6) 0.0055(6) -0.0034(6) O2 0.0252(7) 0.0251(7) 0.0270(8) 0.0028(6) 0.0098(6) 0.0023(6) O3 0.0229(7) 0.0290(7) 0.0315(8) 0.0000(6) 0.0052(6) -0.0011(6) C1 0.0205(10) 0.0241(10) 0.0254(11) 0.0014(9) 0.0030(8) -0.0018(8) C2 0.0236(10) 0.0241(10) 0.0274(11) -0.0025(9) 0.0049(8) -0.0014(8) C3 0.0260(10) 0.0293(11) 0.0266(11) -0.0021(9) 0.0089(8) -0.0017(8) C4 0.0220(9) 0.0257(10) 0.0258(11) 0.0009(9) 0.0058(8) -0.0012(8) C5 0.0275(10) 0.0227(10) 0.0229(11) -0.0012(9) 0.0024(8) -0.0009(8) C6 0.0234(10) 0.0219(10) 0.0240(11) 0.0019(8) 0.0047(8) 0.0016(8) C7 0.0267(10) 0.0223(10) 0.0255(11) 0.0001(9) 0.0060(8) -0.0001(8) C8 0.0208(9) 0.0267(10) 0.0283(12) -0.0014(9) 0.0090(8) -0.0016(8) C9 0.0187(9) 0.0283(11) 0.0296(12) 0.0022(9) 0.0090(8) 0.0020(8) C10 0.0241(10) 0.0292(11) 0.0338(13) 0.0003(10) 0.0090(9) 0.0004(8) C11 0.0257(10) 0.0370(12) 0.0271(12) 0.0028(10) 0.0081(9) 0.0033(9) C12 0.0296(11) 0.0387(13) 0.0327(13) 0.0101(10) 0.0108(9) 0.0047(9) C13 0.0258(10) 0.0296(11) 0.0364(13) 0.0043(10) 0.0112(9) 0.0010(9) C14 0.0190(9) 0.0306(11) 0.0300(12) 0.0019(9) 0.0077(9) 0.0001(8) C15 0.0276(10) 0.0332(11) 0.0284(12) -0.0076(9) 0.0065(9) -0.0038(9) C16 0.0433(12) 0.0394(13) 0.0344(13) -0.0135(10) 0.0165(10) -0.0076(10) C17 0.0407(12) 0.0410(13) 0.0295(13) -0.0035(10) 0.0037(10) -0.0049(10) C18 0.0289(11) 0.0301(11) 0.0318(12) -0.0099(10) 0.0112(9) -0.0028(9) C19 0.0292(11) 0.0343(12) 0.0406(13) -0.0069(10) 0.0101(10) -0.0003(9) C20 0.0451(13) 0.0351(13) 0.0460(15) -0.0018(11) 0.0107(11) 0.0082(10) C21 0.0550(15) 0.0290(12) 0.0518(16) -0.0039(11) 0.0170(12) -0.0078(11) C22 0.0420(13) 0.0402(14) 0.0509(16) -0.0092(12) 0.0142(12) -0.0134(11) C23 0.0309(11) 0.0377(13) 0.0413(14) -0.0100(11) 0.0083(10) -0.0050(9) C24 0.0247(10) 0.0263(11) 0.0318(12) -0.0004(9) 0.0076(9) -0.0045(8) C25 0.0368(12) 0.0456(14) 0.0407(14) -0.0141(11) 0.0102(10) -0.0169(10) C26 0.0346(12) 0.0308(12) 0.0546(16) 0.0085(11) 0.0098(11) -0.0005(9) C27 0.0217(10) 0.0282(11) 0.0343(12) -0.0047(10) 0.0036(9) -0.0056(8) C28 0.0292(11) 0.0457(14) 0.0391(14) -0.0081(11) 0.0082(10) -0.0083(10) C29 0.0344(13) 0.0671(18) 0.0620(18) -0.0268(15) 0.0172(12) -0.0091(13) C30 0.0268(13) 0.0560(18) 0.107(3) -0.0368(18) 0.0154(15) -0.0044(12) C31 0.0327(13) 0.0337(14) 0.106(3) -0.0029(15) -0.0144(15) 0.0004(11) C32 0.0303(11) 0.0352(13) 0.0543(16) 0.0029(12) -0.0008(11) -0.0046(10) C33 0.0350(11) 0.0512(14) 0.0241(12) 0.0013(11) 0.0084(9) 0.0045(10) C34 0.0508(14) 0.0640(17) 0.0281(13) 0.0133(12) 0.0048(11) -0.0048(12) C35 0.0508(15) 0.090(2) 0.0373(15) -0.0116(14) 0.0139(12) 0.0124(14) C36 0.0358(11) 0.0428(13) 0.0202(11) 0.0013(10) -0.0013(9) 0.0030(10) C37 0.0585(15) 0.0484(15) 0.0326(14) -0.0027(12) -0.0037(12) 0.0043(12) C38 0.079(2) 0.0509(17) 0.0442(17) 0.0040(14) -0.0139(16) -0.0152(15) C39 0.0571(17) 0.076(2) 0.0405(16) 0.0202(15) -0.0137(14) -0.0268(16) C40 0.0409(14) 0.080(2) 0.0395(15) 0.0165(15) 0.0041(11) -0.0009(14) C41 0.0366(12) 0.0495(14) 0.0341(13) 0.0022(11) 0.0079(10) -0.0006(11) C42 0.0327(11) 0.0284(11) 0.0434(14) 0.0080(10) 0.0082(10) -0.0033(9) C43 0.0349(12) 0.0353(13) 0.0678(18) 0.0067(12) 0.0169(12) -0.0061(10) C44 0.0525(14) 0.0355(13) 0.0514(16) 0.0128(12) 0.0135(12) -0.0013(11) C45 0.0311(11) 0.0239(11) 0.0440(14) 0.0086(10) 0.0034(10) 0.0012(9) C46 0.0355(12) 0.0348(13) 0.0507(16) 0.0025(12) -0.0002(11) -0.0001(10) C47 0.0527(15) 0.0345(13) 0.0504(16) -0.0030(12) -0.0061(12) 0.0046(11) C48 0.0505(15) 0.0382(14) 0.0487(16) -0.0013(12) 0.0049(12) 0.0134(11) C49 0.0365(12) 0.0402(13) 0.0611(17) -0.0018(13) 0.0113(12) 0.0042(10) C50 0.0321(12) 0.0364(13) 0.0490(15) -0.0009(11) 0.0053(11) 0.0010(10) C51 0.0622(19) 0.0494(17) 0.099(3) 0.0084(17) -0.0140(17) -0.0017(14) C52 0.0501(15) 0.0453(16) 0.0522(17) 0.0166(13) -0.0127(12) -0.0008(12) C53 0.0590(17) 0.0495(16) 0.0396(15) 0.0081(12) -0.0126(13) -0.0210(13) C54 0.0670(18) 0.0577(17) 0.0360(15) -0.0027(13) 0.0061(13) -0.0177(14) C55 0.0632(16) 0.0697(19) 0.0327(14) 0.0021(14) 0.0094(12) -0.0169(14) C56 0.0603(17) 0.0567(17) 0.0378(15) 0.0086(13) -0.0042(12) -0.0183(13) C57 0.0703(18) 0.0399(15) 0.0499(17) 0.0089(13) -0.0110(14) -0.0065(13) _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 K O3 2.6293(16) . ? K O1 2.6662(15) . ? K O2 2.7954(14) . ? K C1 3.230(2) . ? K C14 3.294(2) . ? K C20 3.322(2) . ? K C19 3.333(2) . ? K C50 3.437(2) . ? K C30 3.450(3) 3_766 ? K C31 3.491(2) 3_766 ? O1 C1 1.350(2) . ? O2 C7 1.433(2) . ? O2 C8 1.439(2) . ? O3 C14 1.348(2) . ? O3 H2A 1.12(3) . ? C1 C6 1.394(3) . ? C1 C2 1.414(3) . ? C2 C3 1.388(3) . ? C2 C15 1.543(3) . ? C3 C4 1.395(3) . ? C3 H3A 0.9300 . ? C4 C5 1.380(3) . ? C4 C24 1.535(3) . ? C5 C6 1.393(3) . ? C5 H5A 0.9300 . ? C6 C7 1.495(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.494(3) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.385(3) . ? C9 C14 1.406(3) . ? C10 C11 1.385(3) . ? C10 H10A 0.9300 . ? C11 C12 1.394(3) . ? C11 C33 1.530(3) . ? C12 C13 1.395(3) . ? C12 H12A 0.9300 . ? C13 C14 1.412(3) . ? C13 C42 1.530(3) . ? C15 C18 1.534(3) . ? C15 C16 1.536(3) . ? C15 C17 1.536(3) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C23 1.383(3) . ? C18 C19 1.390(3) . ? C19 C20 1.380(3) . ? C19 H19A 0.9800 . ? C20 C21 1.385(3) . ? C20 H20A 0.9800 . ? C21 C22 1.375(3) . ? C21 H21A 0.9300 . ? C22 C23 1.381(3) . ? C22 H22A 0.9300 . ? C23 H23A 0.9300 . ? C24 C26 1.529(3) . ? C24 C27 1.529(3) . ? C24 C25 1.537(3) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C28 1.381(3) . ? C27 C32 1.384(3) . ? C28 C29 1.387(3) . ? C28 H28A 0.9300 . ? C29 C30 1.356(4) . ? C29 H29A 0.9300 . ? C30 C31 1.385(4) . ? C30 K 3.450(3) 3_766 ? C30 H30A 0.9300 . ? C31 C32 1.393(4) . ? C31 K 3.491(2) 3_766 ? C31 H31A 0.9300 . ? C32 H32A 0.9300 . ? C33 C35 1.526(3) . ? C33 C36 1.534(3) . ? C33 C34 1.541(3) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 C37 1.378(3) . ? C36 C41 1.384(3) . ? C37 C38 1.381(4) . ? C37 H37A 0.9300 . ? C38 C39 1.351(4) . ? C38 H38A 0.9300 . ? C39 C40 1.370(4) . ? C39 H39A 0.9300 . ? C40 C41 1.384(3) . ? C40 H40A 0.9300 . ? C41 H41A 0.9300 . ? C42 C45 1.526(3) . ? C42 C44 1.533(3) . ? C42 C43 1.553(3) . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 C46 1.388(3) . ? C45 C50 1.392(3) . ? C46 C47 1.382(3) . ? C46 H46A 0.9300 . ? C47 C48 1.380(3) . ? C47 H47A 0.9300 . ? C48 C49 1.370(3) . ? C48 H48A 0.9300 . ? C49 C50 1.382(3) . ? C49 H49A 0.9300 . ? C50 H50A 0.9800 . ? C51 C52 1.488(4) . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 C53 1.380(4) . ? C52 C57 1.381(3) . ? C53 C54 1.376(4) . ? C53 H53A 0.9300 . ? C54 C55 1.380(3) . ? C54 H54A 0.9300 . ? C55 C56 1.368(4) . ? C55 H55A 0.9300 . ? C56 C57 1.372(4) . ? C56 H56A 0.9300 . ? C57 H57A 0.9300 . ? 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 O3 K O1 108.50(4) . . ? O3 K O2 71.98(4) . . ? O1 K O2 70.06(4) . . ? O3 K C1 121.64(5) . . ? O1 K C1 24.13(4) . . ? O2 K C1 61.83(5) . . ? O3 K C14 22.97(4) . . ? O1 K C14 118.21(5) . . ? O2 K C14 61.35(4) . . ? C1 K C14 121.48(5) . . ? O3 K C20 144.68(5) . . ? O1 K C20 91.59(5) . . ? O2 K C20 143.29(5) . . ? C1 K C20 88.28(6) . . ? C14 K C20 149.49(6) . . ? O3 K C19 163.67(5) . . ? O1 K C19 70.92(5) . . ? O2 K C19 121.24(5) . . ? C1 K C19 64.47(5) . . ? C14 K C19 169.58(5) . . ? C20 K C19 23.94(5) . . ? O3 K C50 68.26(5) . . ? O1 K C50 176.44(5) . . ? O2 K C50 109.66(5) . . ? C1 K C50 158.93(5) . . ? C14 K C50 59.38(5) . . ? C20 K C50 90.52(6) . . ? C19 K C50 111.74(6) . . ? O3 K C30 101.52(7) . 3_766 ? O1 K C30 114.85(7) . 3_766 ? O2 K C30 66.61(5) . 3_766 ? C1 K C30 91.40(7) . 3_766 ? C14 K C30 78.57(7) . 3_766 ? C20 K C30 95.46(6) . 3_766 ? C19 K C30 93.14(7) . 3_766 ? C50 K C30 67.77(7) . 3_766 ? O3 K C31 123.66(7) . 3_766 ? O1 K C31 98.71(6) . 3_766 ? O2 K C31 72.66(5) . 3_766 ? C1 K C31 74.60(6) . 3_766 ? C14 K C31 100.75(7) . 3_766 ? C20 K C31 79.45(7) . 3_766 ? C19 K C31 71.86(7) . 3_766 ? C50 K C31 84.50(7) . 3_766 ? C30 K C31 23.01(7) 3_766 3_766 ? C1 O1 K 102.02(10) . . ? C7 O2 C8 109.78(13) . . ? C7 O2 K 116.35(11) . . ? C8 O2 K 114.02(10) . . ? C14 O3 K 107.44(10) . . ? C14 O3 H2A 106.8(15) . . ? K O3 H2A 128.7(15) . . ? O1 C1 C6 120.18(17) . . ? O1 C1 C2 120.31(17) . . ? C6 C1 C2 119.50(16) . . ? O1 C1 K 53.85(9) . . ? C6 C1 K 96.81(12) . . ? C2 C1 K 117.25(12) . . ? C3 C2 C1 117.93(17) . . ? C3 C2 C15 121.82(17) . . ? C1 C2 C15 120.20(16) . . ? C2 C3 C4 123.40(18) . . ? C2 C3 H3A 118.3 . . ? C4 C3 H3A 118.3 . . ? C5 C4 C3 117.26(17) . . ? C5 C4 C24 122.76(17) . . ? C3 C4 C24 119.84(17) . . ? C4 C5 C6 121.67(18) . . ? C4 C5 H5A 119.2 . . ? C6 C5 H5A 119.2 . . ? C5 C6 C1 120.21(17) . . ? C5 C6 C7 119.66(17) . . ? C1 C6 C7 120.11(16) . . ? O2 C7 C6 110.82(15) . . ? O2 C7 H7A 109.5 . . ? C6 C7 H7A 109.5 . . ? O2 C7 H7B 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 108.1 . . ? O2 C8 C9 109.77(14) . . ? O2 C8 H8A 109.7 . . ? C9 C8 H8A 109.7 . . ? O2 C8 H8B 109.7 . . ? C9 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? C10 C9 C14 119.89(18) . . ? C10 C9 C8 119.86(17) . . ? C14 C9 C8 120.25(18) . . ? C11 C10 C9 122.57(19) . . ? C11 C10 H10A 118.7 . . ? C9 C10 H10A 118.7 . . ? C10 C11 C12 116.86(19) . . ? C10 C11 C33 119.65(19) . . ? C12 C11 C33 123.42(19) . . ? C11 C12 C13 123.12(19) . . ? C11 C12 H12A 118.4 . . ? C13 C12 H12A 118.4 . . ? C12 C13 C14 118.45(19) . . ? C12 C13 C42 121.61(18) . . ? C14 C13 C42 119.95(18) . . ? O3 C14 C9 119.70(17) . . ? O3 C14 C13 121.20(17) . . ? C9 C14 C13 119.10(18) . . ? O3 C14 K 49.59(9) . . ? C9 C14 K 96.99(12) . . ? C13 C14 K 121.78(13) . . ? C18 C15 C16 106.87(16) . . ? C18 C15 C17 112.36(16) . . ? C16 C15 C17 107.03(17) . . ? C18 C15 C2 109.42(16) . . ? C16 C15 C2 112.30(15) . . ? C17 C15 C2 108.87(16) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C23 C18 C19 117.4(2) . . ? C23 C18 C15 123.54(19) . . ? C19 C18 C15 119.01(17) . . ? C20 C19 C18 121.65(19) . . ? C20 C19 K 77.57(13) . . ? C18 C19 K 90.65(12) . . ? C20 C19 H19A 117.9 . . ? C18 C19 H19A 117.9 . . ? K C19 H19A 117.9 . . ? C19 C20 C21 119.8(2) . . ? C19 C20 K 78.49(13) . . ? C21 C20 K 89.76(14) . . ? C19 C20 H20A 118.6 . . ? C21 C20 H20A 118.6 . . ? K C20 H20A 118.6 . . ? C22 C21 C20 119.3(2) . . ? C22 C21 H21A 120.4 . . ? C20 C21 H21A 120.4 . . ? C21 C22 C23 120.4(2) . . ? C21 C22 H22A 119.8 . . ? C23 C22 H22A 119.8 . . ? C22 C23 C18 121.4(2) . . ? C22 C23 H23A 119.3 . . ? C18 C23 H23A 119.3 . . ? C26 C24 C27 112.42(17) . . ? C26 C24 C4 107.43(15) . . ? C27 C24 C4 109.28(15) . . ? C26 C24 C25 107.40(18) . . ? C27 C24 C25 108.20(16) . . ? C4 C24 C25 112.15(16) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C32 117.8(2) . . ? C28 C27 C24 122.54(19) . . ? C32 C27 C24 119.63(19) . . ? C27 C28 C29 121.2(2) . . ? C27 C28 H28A 119.4 . . ? C29 C28 H28A 119.4 . . ? C30 C29 C28 120.6(3) . . ? C30 C29 H29A 119.7 . . ? C28 C29 H29A 119.7 . . ? C29 C30 C31 119.7(2) . . ? C29 C30 K 118.83(17) . 3_766 ? C31 C30 K 80.16(17) . 3_766 ? C29 C30 H30A 120.2 . . ? C31 C30 H30A 120.2 . . ? K C30 H30A 71.9 3_766 . ? C30 C31 C32 119.6(3) . . ? C30 C31 K 76.83(15) . 3_766 ? C32 C31 K 120.59(15) . 3_766 ? C30 C31 H31A 120.2 . . ? C32 C31 H31A 120.2 . . ? K C31 H31A 73.8 3_766 . ? C27 C32 C31 121.1(3) . . ? C27 C32 H32A 119.5 . . ? C31 C32 H32A 119.5 . . ? C35 C33 C11 108.06(17) . . ? C35 C33 C36 112.4(2) . . ? C11 C33 C36 109.22(17) . . ? C35 C33 C34 107.0(2) . . ? C11 C33 C34 112.74(19) . . ? C36 C33 C34 107.41(17) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C37 C36 C41 117.1(2) . . ? C37 C36 C33 124.0(2) . . ? C41 C36 C33 118.9(2) . . ? C36 C37 C38 121.1(3) . . ? C36 C37 H37A 119.4 . . ? C38 C37 H37A 119.4 . . ? C39 C38 C37 121.1(3) . . ? C39 C38 H38A 119.5 . . ? C37 C38 H38A 119.5 . . ? C38 C39 C40 119.2(3) . . ? C38 C39 H39A 120.4 . . ? C40 C39 H39A 120.4 . . ? C39 C40 C41 120.1(3) . . ? C39 C40 H40A 119.9 . . ? C41 C40 H40A 119.9 . . ? C40 C41 C36 121.3(2) . . ? C40 C41 H41A 119.4 . . ? C36 C41 H41A 119.4 . . ? C45 C42 C13 110.34(16) . . ? C45 C42 C44 106.38(17) . . ? C13 C42 C44 111.78(19) . . ? C45 C42 C43 111.95(19) . . ? C13 C42 C43 109.71(17) . . ? C44 C42 C43 106.60(18) . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C46 C45 C50 117.0(2) . . ? C46 C45 C42 122.40(19) . . ? C50 C45 C42 120.4(2) . . ? C47 C46 C45 121.5(2) . . ? C47 C46 H46A 119.3 . . ? C45 C46 H46A 119.3 . . ? C46 C47 C48 120.7(2) . . ? C46 C47 H47A 119.7 . . ? C48 C47 H47A 119.7 . . ? C49 C48 C47 118.6(2) . . ? C49 C48 H48A 120.7 . . ? C47 C48 H48A 120.7 . . ? C48 C49 C50 121.0(2) . . ? C48 C49 H49A 119.5 . . ? C50 C49 H49A 119.5 . . ? C49 C50 C45 121.3(2) . . ? C49 C50 K 85.82(15) . . ? C45 C50 K 96.18(13) . . ? C49 C50 H50A 115.7 . . ? C45 C50 H50A 115.7 . . ? K C50 H50A 115.7 . . ? C52 C51 H51A 109.5 . . ? C52 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C52 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C53 C52 C57 118.0(3) . . ? C53 C52 C51 122.3(2) . . ? C57 C52 C51 119.7(3) . . ? C54 C53 C52 121.0(2) . . ? C54 C53 H53A 119.5 . . ? C52 C53 H53A 119.5 . . ? C53 C54 C55 120.2(3) . . ? C53 C54 H54A 119.9 . . ? C55 C54 H54A 119.9 . . ? C56 C55 C54 119.2(3) . . ? C56 C55 H55A 120.4 . . ? C54 C55 H55A 120.4 . . ? C55 C56 C57 120.5(2) . . ? C55 C56 H56A 119.7 . . ? C57 C56 H56A 119.7 . . ? C56 C57 C52 121.1(3) . . ? C56 C57 H57A 119.4 . . ? C52 C57 H57A 119.4 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.387 _refine_diff_density_min -0.316 _refine_diff_density_rms 0.043 data_[K(L-H)(THF)] _database_code_depnum_ccdc_archive 'CCDC 917259' #TrackingRef '16475_web_deposit_cif_file_1_YongHuang_1356657153.[K(L-H)(THF)].cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C108 H122 K2 O8, 2(C4 H8 O))' _chemical_formula_sum 'C116 H138 K2 O10' _chemical_formula_weight 1770.46 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.543(3) _cell_length_b 13.946(3) _cell_length_c 15.444(3) _cell_angle_alpha 104.72(3) _cell_angle_beta 108.69(3) _cell_angle_gamma 105.77(3) _cell_volume 2465.8(14) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 10612 _cell_measurement_theta_min 5.097 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.192 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 0.156 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.978 _exptl_absorpt_correction_T_max 0.985 _exptl_absorpt_process_details 'SADABS, Sheldrick (1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16726 _diffrn_reflns_av_R_equivalents 0.0239 _diffrn_reflns_av_sigmaI/netI 0.0402 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 5.12 _diffrn_reflns_theta_max 25.50 _reflns_number_total 9101 _reflns_number_gt 7076 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _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^)+(0.1000P)^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 9101 _refine_ls_number_parameters 569 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0660 _refine_ls_R_factor_gt 0.0480 _refine_ls_wR_factor_ref 0.1510 _refine_ls_wR_factor_gt 0.1406 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _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 K K 0.47040(3) 0.52186(3) 0.17377(3) 0.02864(13) Uani 1 1 d . . . O1 O 0.34831(9) 0.35429(9) 0.00165(9) 0.0221(3) Uani 1 1 d . . . O2 O 0.60659(9) 0.41314(9) 0.11905(8) 0.0230(3) Uani 1 1 d . . . O3 O 0.63492(9) 0.65545(9) 0.15345(9) 0.0225(3) Uani 1 1 d . . . O4 O 0.54486(12) 0.46379(12) 0.32753(12) 0.0447(4) Uani 1 1 d . . . O5 O 0.23907(14) 0.27753(13) 0.36264(12) 0.0532(4) Uani 1 1 d . . . C1 C 0.34905(13) 0.26856(13) 0.02504(12) 0.0204(4) Uani 1 1 d . . . C2 C 0.25182(14) 0.20072(13) 0.02860(12) 0.0215(4) Uani 1 1 d . . . C3 C 0.25625(14) 0.11184(13) 0.05214(12) 0.0232(4) Uani 1 1 d . . . H3A H 0.1920 0.0667 0.0529 0.028 Uiso 1 1 calc R . . C4 C 0.35248(14) 0.08651(13) 0.07488(12) 0.0235(4) Uani 1 1 d . . . C5 C 0.44709(14) 0.15536(13) 0.07370(12) 0.0229(4) Uani 1 1 d . . . H5A H 0.5130 0.1420 0.0903 0.028 Uiso 1 1 calc R . . C6 C 0.44619(13) 0.24429(13) 0.04819(12) 0.0211(4) Uani 1 1 d . . . C7 C 0.54768(13) 0.31057(13) 0.03921(12) 0.0222(4) Uani 1 1 d . . . H7A H 0.5981 0.2727 0.0394 0.027 Uiso 1 1 calc R . . H7B H 0.5237 0.3209 -0.0229 0.027 Uiso 1 1 calc R . . C8 C 0.69795(13) 0.47744(13) 0.10502(13) 0.0225(4) Uani 1 1 d . . . H8A H 0.6684 0.4971 0.0491 0.027 Uiso 1 1 calc R . . H8B H 0.7427 0.4367 0.0915 0.027 Uiso 1 1 calc R . . C9 C 0.77056(14) 0.57688(13) 0.19612(12) 0.0216(4) Uani 1 1 d . . . C10 C 0.87310(14) 0.58341(14) 0.26102(13) 0.0233(4) Uani 1 1 d . . . H10A H 0.8959 0.5265 0.2458 0.028 Uiso 1 1 calc R . . C11 C 0.94219(14) 0.67153(14) 0.34733(13) 0.0231(4) Uani 1 1 d . . . C12 C 0.90411(14) 0.75518(14) 0.36774(13) 0.0244(4) Uani 1 1 d . . . H12A H 0.9491 0.8151 0.4258 0.029 Uiso 1 1 calc R . . C13 C 0.80217(13) 0.75301(13) 0.30535(12) 0.0214(4) Uani 1 1 d . . . C14 C 0.73399(13) 0.66146(13) 0.21693(12) 0.0208(4) Uani 1 1 d . . . C15 C 0.14267(13) 0.22273(14) -0.00074(13) 0.0233(4) Uani 1 1 d . . . C16 C 0.05138(15) 0.14821(15) 0.01739(15) 0.0305(4) Uani 1 1 d . . . H16A H 0.0782 0.1604 0.0863 0.046 Uiso 1 1 calc R . . H16B H 0.0348 0.0747 -0.0196 0.046 Uiso 1 1 calc R . . H16C H -0.0159 0.1629 -0.0033 0.046 Uiso 1 1 calc R . . C17 C 0.09399(14) 0.19918(16) -0.11160(14) 0.0302(4) Uani 1 1 d . . . H17A H 0.1485 0.2441 -0.1265 0.045 Uiso 1 1 calc R . . H17B H 0.0264 0.2136 -0.1305 0.045 Uiso 1 1 calc R . . H17C H 0.0766 0.1251 -0.1473 0.045 Uiso 1 1 calc R . . C18 C 0.16521(13) 0.33817(14) 0.06087(13) 0.0250(4) Uani 1 1 d . . . C19 C 0.21539(15) 0.37383(16) 0.16348(14) 0.0316(4) Uani 1 1 d . . . H19A H 0.2140 0.3191 0.1927 0.038 Uiso 1 1 calc R . . C20 C 0.23064(18) 0.47468(17) 0.22251(17) 0.0431(5) Uani 1 1 d . . . H20A H 0.2405 0.4872 0.2907 0.052 Uiso 1 1 calc R . . C21 C 0.19609(18) 0.54228(17) 0.17979(18) 0.0463(6) Uani 1 1 d . . . H21A H 0.2051 0.6096 0.2190 0.056 Uiso 1 1 calc R . . C22 C 0.14835(19) 0.50960(17) 0.07907(19) 0.0452(5) Uani 1 1 d . . . H22A H 0.1265 0.5557 0.0502 0.054 Uiso 1 1 calc R . . C23 C 0.13234(16) 0.40809(16) 0.01973(16) 0.0343(4) Uani 1 1 d . . . H23A H 0.0991 0.3869 -0.0485 0.041 Uiso 1 1 calc R . . C24 C 0.34624(15) -0.01877(15) 0.09121(14) 0.0279(4) Uani 1 1 d . . . C25 C 0.46113(16) -0.02859(16) 0.12291(15) 0.0342(4) Uani 1 1 d . . . H25A H 0.5135 0.0293 0.1843 0.051 Uiso 1 1 calc R . . H25B H 0.4889 -0.0253 0.0734 0.051 Uiso 1 1 calc R . . H25C H 0.4531 -0.0959 0.1310 0.051 Uiso 1 1 calc R . . C26 C 0.3051(2) -0.02385(18) 0.17258(17) 0.0437(5) Uani 1 1 d . . . H26A H 0.3566 0.0363 0.2326 0.065 Uiso 1 1 calc R . . H26B H 0.3019 -0.0895 0.1829 0.065 Uiso 1 1 calc R . . H26C H 0.2313 -0.0215 0.1530 0.065 Uiso 1 1 calc R . . C27 C 0.26573(10) -0.11509(8) -0.00823(8) 0.0293(4) Uani 1 1 d G . . C28 C 0.19619(12) -0.21114(10) -0.01157(10) 0.0436(5) Uani 1 1 d G . . H28A H 0.1939 -0.2180 0.0462 0.052 Uiso 1 1 calc R . . C29 C 0.13013(11) -0.29700(8) -0.10121(13) 0.0581(7) Uani 1 1 d GU . . H29A H 0.0836 -0.3613 -0.1034 0.070 Uiso 1 1 calc R . . C30 C 0.13361(12) -0.28681(9) -0.18752(10) 0.0608(8) Uani 1 1 d GU . . H30A H 0.0894 -0.3443 -0.2475 0.073 Uiso 1 1 calc R . . C31 C 0.20315(13) -0.19076(12) -0.18418(8) 0.0529(6) Uani 1 1 d G . . H31A H 0.2055 -0.1839 -0.2419 0.063 Uiso 1 1 calc R . . C32 C 0.26921(11) -0.10490(9) -0.09454(9) 0.0365(5) Uani 1 1 d G . . H32A H 0.3157 -0.0406 -0.0923 0.044 Uiso 1 1 calc R . . C33 C 1.05463(14) 0.67947(14) 0.42187(13) 0.0248(4) Uani 1 1 d . . . C34 C 1.08076(16) 0.57955(15) 0.38674(15) 0.0336(5) Uani 1 1 d . . . H34A H 1.0205 0.5166 0.3768 0.050 Uiso 1 1 calc R . . H34B H 1.1502 0.5865 0.4356 0.050 Uiso 1 1 calc R . . H34C H 1.0879 0.5731 0.3259 0.050 Uiso 1 1 calc R . . C35 C 1.04347(16) 0.68611(18) 0.51868(15) 0.0367(5) Uani 1 1 d . . . H35A H 1.0273 0.7480 0.5425 0.055 Uiso 1 1 calc R . . H35B H 1.1129 0.6920 0.5667 0.055 Uiso 1 1 calc R . . H35C H 0.9832 0.6225 0.5075 0.055 Uiso 1 1 calc R . . C36 C 1.15362(14) 0.77681(14) 0.43648(13) 0.0259(4) Uani 1 1 d . . . C37 C 1.25245(16) 0.82591(16) 0.52355(16) 0.0371(5) Uani 1 1 d . . . H37A H 1.2569 0.8009 0.5745 0.044 Uiso 1 1 calc R . . C38 C 1.34427(17) 0.91124(18) 0.5358(2) 0.0511(6) Uani 1 1 d . . . H38A H 1.4092 0.9427 0.5945 0.061 Uiso 1 1 calc R . . C39 C 1.33959(18) 0.94900(19) 0.4621(2) 0.0523(7) Uani 1 1 d . . . H39A H 1.4007 1.0067 0.4706 0.063 Uiso 1 1 calc R . . C40 C 1.24385(19) 0.9013(2) 0.3749(2) 0.0501(6) Uani 1 1 d . . . H40A H 1.2407 0.9263 0.3240 0.060 Uiso 1 1 calc R . . C41 C 1.15171(17) 0.81558(18) 0.36247(16) 0.0379(5) Uani 1 1 d . . . H41A H 1.0876 0.7839 0.3031 0.045 Uiso 1 1 calc R . . C42 C 0.76129(14) 0.84494(14) 0.33012(13) 0.0244(4) Uani 1 1 d . . . C43 C 0.84590(15) 0.93614(15) 0.42945(14) 0.0317(4) Uani 1 1 d . . . H43A H 0.8562 0.9082 0.4810 0.048 Uiso 1 1 calc R . . H43B H 0.8172 0.9914 0.4428 0.048 Uiso 1 1 calc R . . H43C H 0.9170 0.9656 0.4265 0.048 Uiso 1 1 calc R . . C44 C 0.75001(16) 0.89607(15) 0.25212(15) 0.0319(4) Uani 1 1 d . . . H44A H 0.6978 0.8423 0.1884 0.048 Uiso 1 1 calc R . . H44B H 0.8225 0.9259 0.2516 0.048 Uiso 1 1 calc R . . H44C H 0.7227 0.9520 0.2677 0.048 Uiso 1 1 calc R . . C45 C 0.65016(14) 0.80125(14) 0.34022(13) 0.0245(4) Uani 1 1 d . . . C46 C 0.55395(16) 0.81637(17) 0.29127(16) 0.0372(5) Uani 1 1 d . . . H46A H 0.5533 0.8489 0.2456 0.045 Uiso 1 1 calc R . . C47 C 0.45839(17) 0.7839(2) 0.30891(19) 0.0488(6) Uani 1 1 d . . . H47A H 0.3949 0.7953 0.2752 0.059 Uiso 1 1 calc R . . C48 C 0.45645(17) 0.73536(18) 0.37549(17) 0.0431(5) Uani 1 1 d . . . H48A H 0.3929 0.7152 0.3883 0.052 Uiso 1 1 calc R . . C49 C 0.55024(18) 0.71688(17) 0.42315(16) 0.0397(5) Uani 1 1 d . . . H49A H 0.5496 0.6822 0.4672 0.048 Uiso 1 1 calc R . . C50 C 0.64576(16) 0.74999(16) 0.40542(14) 0.0331(4) Uani 1 1 d . . . H50A H 0.7086 0.7373 0.4384 0.040 Uiso 1 1 calc R . . C51 C 0.66308(19) 0.4896(2) 0.37155(18) 0.0488(6) Uani 1 1 d . . . H51A H 0.6940 0.5276 0.4423 0.059 Uiso 1 1 calc R . . H51B H 0.7018 0.5340 0.3440 0.059 Uiso 1 1 calc R . . C52 C 0.6751(2) 0.3841(2) 0.3483(2) 0.0595(7) Uani 1 1 d . . . H52A H 0.7456 0.3890 0.3955 0.071 Uiso 1 1 calc R . . H52B H 0.6716 0.3581 0.2825 0.071 Uiso 1 1 calc R . . C53 C 0.5753(2) 0.3131(2) 0.3561(2) 0.0639(7) Uani 1 1 d . . . H53A H 0.5511 0.2386 0.3144 0.077 Uiso 1 1 calc R . . H53B H 0.5926 0.3184 0.4236 0.077 Uiso 1 1 calc R . . C54 C 0.4882(2) 0.3567(2) 0.3214(2) 0.0592(7) Uani 1 1 d . . . H54A H 0.4351 0.3113 0.2539 0.071 Uiso 1 1 calc R . . H54B H 0.4467 0.3589 0.3622 0.071 Uiso 1 1 calc R . . C55 C 0.23896(19) 0.17571(18) 0.31767(17) 0.0454(5) Uani 1 1 d . . . H55A H 0.2992 0.1638 0.3624 0.054 Uiso 1 1 calc R . . H55B H 0.2509 0.1718 0.2584 0.054 Uiso 1 1 calc R . . C56 C 0.1267(2) 0.0923(2) 0.2926(2) 0.0569(6) Uani 1 1 d . . . H56A H 0.0966 0.0396 0.2263 0.068 Uiso 1 1 calc R . . H56B H 0.1334 0.0557 0.3385 0.068 Uiso 1 1 calc R . . C57 C 0.0537(2) 0.1526(3) 0.3001(3) 0.0808(10) Uani 1 1 d . . . H57A H -0.0045 0.1348 0.2356 0.097 Uiso 1 1 calc R . . H57B H 0.0178 0.1359 0.3426 0.097 Uiso 1 1 calc R . . C58 C 0.1281(2) 0.2664(2) 0.3421(3) 0.0738(9) Uani 1 1 d . . . H58A H 0.1042 0.3001 0.2958 0.089 Uiso 1 1 calc R . . H58B H 0.1230 0.3023 0.4022 0.089 Uiso 1 1 calc R . . H2A H 0.636(3) 0.648(3) 0.076(3) 0.098(11) Uiso 1 1 d . . . 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 K 0.0270(2) 0.0283(2) 0.0287(2) 0.00950(17) 0.01218(17) 0.00845(17) O1 0.0225(6) 0.0201(6) 0.0247(6) 0.0104(5) 0.0096(5) 0.0080(5) O2 0.0210(6) 0.0181(6) 0.0246(6) 0.0038(5) 0.0100(5) 0.0032(5) O3 0.0194(6) 0.0248(6) 0.0224(6) 0.0099(5) 0.0064(5) 0.0093(5) O4 0.0441(8) 0.0497(9) 0.0544(10) 0.0303(8) 0.0231(7) 0.0251(7) O5 0.0522(9) 0.0450(9) 0.0554(10) 0.0084(8) 0.0194(8) 0.0220(8) C1 0.0222(8) 0.0194(8) 0.0164(8) 0.0055(7) 0.0067(7) 0.0065(7) C2 0.0222(8) 0.0220(8) 0.0196(8) 0.0069(7) 0.0094(7) 0.0074(7) C3 0.0234(8) 0.0220(9) 0.0250(9) 0.0089(7) 0.0122(7) 0.0073(7) C4 0.0301(9) 0.0220(9) 0.0210(9) 0.0083(7) 0.0121(7) 0.0117(7) C5 0.0232(8) 0.0232(9) 0.0217(9) 0.0066(7) 0.0083(7) 0.0110(7) C6 0.0198(8) 0.0199(8) 0.0194(8) 0.0044(7) 0.0072(7) 0.0057(7) C7 0.0195(8) 0.0198(8) 0.0214(9) 0.0028(7) 0.0072(7) 0.0056(7) C8 0.0222(8) 0.0217(8) 0.0244(9) 0.0090(7) 0.0109(7) 0.0079(7) C9 0.0217(8) 0.0200(8) 0.0232(9) 0.0088(7) 0.0101(7) 0.0067(7) C10 0.0242(8) 0.0213(8) 0.0271(9) 0.0093(7) 0.0127(7) 0.0102(7) C11 0.0213(8) 0.0240(9) 0.0240(9) 0.0097(7) 0.0084(7) 0.0094(7) C12 0.0231(8) 0.0222(9) 0.0227(9) 0.0050(7) 0.0075(7) 0.0071(7) C13 0.0211(8) 0.0198(8) 0.0241(9) 0.0091(7) 0.0095(7) 0.0082(7) C14 0.0188(8) 0.0220(8) 0.0222(9) 0.0106(7) 0.0095(7) 0.0057(7) C15 0.0203(8) 0.0235(9) 0.0259(9) 0.0103(7) 0.0100(7) 0.0069(7) C16 0.0235(9) 0.0292(10) 0.0422(11) 0.0157(9) 0.0162(8) 0.0098(8) C17 0.0216(8) 0.0335(10) 0.0313(10) 0.0125(8) 0.0067(8) 0.0091(8) C18 0.0195(8) 0.0250(9) 0.0319(10) 0.0109(8) 0.0121(7) 0.0086(7) C19 0.0328(10) 0.0319(10) 0.0324(10) 0.0114(8) 0.0156(8) 0.0142(8) C20 0.0440(12) 0.0404(12) 0.0399(12) 0.0056(10) 0.0189(10) 0.0163(10) C21 0.0444(12) 0.0307(11) 0.0606(16) 0.0062(11) 0.0249(11) 0.0166(10) C22 0.0465(12) 0.0332(11) 0.0647(16) 0.0224(11) 0.0242(11) 0.0234(10) C23 0.0324(10) 0.0343(11) 0.0389(11) 0.0171(9) 0.0135(9) 0.0152(9) C24 0.0354(10) 0.0267(9) 0.0313(10) 0.0149(8) 0.0182(8) 0.0172(8) C25 0.0381(10) 0.0318(10) 0.0341(11) 0.0161(9) 0.0097(9) 0.0184(9) C26 0.0698(15) 0.0450(12) 0.0474(13) 0.0320(11) 0.0394(12) 0.0355(11) C27 0.0261(9) 0.0234(9) 0.0460(12) 0.0146(8) 0.0180(8) 0.0153(8) C28 0.0399(11) 0.0285(11) 0.0749(16) 0.0237(11) 0.0307(11) 0.0189(9) C29 0.0359(12) 0.0204(11) 0.103(2) 0.0126(12) 0.0197(13) 0.0093(9) C30 0.0442(13) 0.0284(12) 0.0730(18) -0.0033(12) -0.0033(12) 0.0152(10) C31 0.0553(14) 0.0410(13) 0.0439(13) 0.0021(11) 0.0061(11) 0.0225(11) C32 0.0369(10) 0.0303(10) 0.0388(11) 0.0092(9) 0.0130(9) 0.0146(9) C33 0.0229(8) 0.0269(9) 0.0238(9) 0.0081(7) 0.0080(7) 0.0120(7) C34 0.0293(9) 0.0301(10) 0.0361(11) 0.0103(9) 0.0051(8) 0.0163(8) C35 0.0332(10) 0.0516(13) 0.0332(11) 0.0202(10) 0.0152(9) 0.0220(9) C36 0.0219(8) 0.0266(9) 0.0299(10) 0.0072(8) 0.0102(7) 0.0144(7) C37 0.0300(10) 0.0338(11) 0.0394(11) 0.0109(9) 0.0052(9) 0.0145(9) C38 0.0254(10) 0.0375(12) 0.0712(17) 0.0107(12) 0.0063(11) 0.0103(9) C39 0.0294(11) 0.0405(13) 0.091(2) 0.0256(13) 0.0287(12) 0.0134(10) C40 0.0467(13) 0.0570(14) 0.0732(17) 0.0396(14) 0.0402(13) 0.0262(11) C41 0.0304(10) 0.0494(13) 0.0383(11) 0.0201(10) 0.0168(9) 0.0155(9) C42 0.0221(8) 0.0203(8) 0.0256(9) 0.0058(7) 0.0060(7) 0.0080(7) C43 0.0267(9) 0.0245(9) 0.0340(10) 0.0012(8) 0.0066(8) 0.0119(8) C44 0.0367(10) 0.0240(9) 0.0399(11) 0.0142(8) 0.0182(9) 0.0141(8) C45 0.0258(9) 0.0208(8) 0.0224(9) 0.0030(7) 0.0075(7) 0.0103(7) C46 0.0276(9) 0.0410(11) 0.0452(12) 0.0228(10) 0.0107(9) 0.0156(9) C47 0.0263(10) 0.0560(14) 0.0656(16) 0.0258(13) 0.0160(10) 0.0191(10) C48 0.0330(11) 0.0402(12) 0.0523(13) 0.0095(10) 0.0237(10) 0.0092(9) C49 0.0471(12) 0.0405(12) 0.0352(11) 0.0150(9) 0.0227(10) 0.0150(10) C50 0.0336(10) 0.0371(11) 0.0316(10) 0.0154(9) 0.0122(8) 0.0176(9) C51 0.0428(12) 0.0554(14) 0.0437(13) 0.0236(11) 0.0141(10) 0.0123(11) C52 0.0621(15) 0.089(2) 0.0502(15) 0.0383(15) 0.0219(12) 0.0516(15) C53 0.0749(18) 0.0519(15) 0.0617(17) 0.0307(13) 0.0159(14) 0.0264(14) C54 0.0532(14) 0.0627(17) 0.0691(17) 0.0396(14) 0.0245(13) 0.0206(13) C55 0.0432(12) 0.0485(13) 0.0417(12) 0.0107(10) 0.0145(10) 0.0235(10) C56 0.0620(15) 0.0486(14) 0.0654(17) 0.0167(13) 0.0364(13) 0.0216(12) C57 0.0567(16) 0.075(2) 0.123(3) 0.035(2) 0.0468(18) 0.0329(15) C58 0.0710(18) 0.0598(17) 0.119(3) 0.0325(18) 0.0670(19) 0.0350(15) _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 K O3 2.6501(15) . ? K O1 2.681(2) . ? K O4 2.6830(17) . ? K O2 2.8780(14) . ? K C1 3.280(2) . ? K C14 3.319(2) . ? K C19 3.438(2) . ? K C20 3.493(2) . ? O1 C1 1.336(2) . ? O2 C8 1.432(2) . ? O2 C7 1.434(2) . ? O3 C14 1.350(2) . ? O3 H2A 1.18(4) . ? O4 C51 1.421(3) . ? O4 C54 1.445(3) . ? O5 C58 1.388(3) . ? O5 C55 1.413(3) . ? C1 C6 1.405(2) . ? C1 C2 1.424(2) . ? C2 C3 1.388(2) . ? C2 C15 1.540(2) . ? C3 C4 1.402(2) . ? C3 H3A 0.9300 . ? C4 C5 1.385(2) . ? C4 C24 1.537(2) . ? C5 C6 1.395(2) . ? C5 H5A 0.9300 . ? C6 C7 1.503(2) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.500(2) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.391(2) . ? C9 C14 1.402(2) . ? C10 C11 1.380(3) . ? C10 H10A 0.9300 . ? C11 C12 1.404(3) . ? C11 C33 1.542(2) . ? C12 C13 1.395(2) . ? C12 H12A 0.9300 . ? C13 C14 1.419(2) . ? C13 C42 1.539(2) . ? C15 C17 1.532(3) . ? C15 C18 1.536(3) . ? C15 C16 1.536(2) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C23 1.386(3) . ? C18 C19 1.395(3) . ? C19 C20 1.386(3) . ? C19 H19A 0.9800 . ? C20 C21 1.379(3) . ? C20 H20A 0.9800 . ? C21 C22 1.371(3) . ? C21 H21A 0.9300 . ? C22 C23 1.392(3) . ? C22 H22A 0.9300 . ? C23 H23A 0.9300 . ? C24 C25 1.530(3) . ? C24 C26 1.538(3) . ? C24 C27 1.560(2) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C28 1.3900 . ? C27 C32 1.3900 . ? C28 C29 1.3900 . ? C28 H28A 0.9300 . ? C29 C30 1.3900 . ? C29 H29A 0.9300 . ? C30 C31 1.3900 . ? C30 H30A 0.9300 . ? C31 C32 1.3900 . ? C31 H31A 0.9300 . ? C32 H32A 0.9300 . ? C33 C35 1.533(3) . ? C33 C36 1.534(3) . ? C33 C34 1.539(3) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 C41 1.379(3) . ? C36 C37 1.396(3) . ? C37 C38 1.389(3) . ? C37 H37A 0.9300 . ? C38 C39 1.361(4) . ? C38 H38A 0.9300 . ? C39 C40 1.377(4) . ? C39 H39A 0.9300 . ? C40 C41 1.394(3) . ? C40 H40A 0.9300 . ? C41 H41A 0.9300 . ? C42 C44 1.536(3) . ? C42 C45 1.536(2) . ? C42 C43 1.541(3) . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 C50 1.382(3) . ? C45 C46 1.383(3) . ? C46 C47 1.387(3) . ? C46 H46A 0.9300 . ? C47 C48 1.371(3) . ? C47 H47A 0.9300 . ? C48 C49 1.377(3) . ? C48 H48A 0.9300 . ? C49 C50 1.389(3) . ? C49 H49A 0.9300 . ? C50 H50A 0.9300 . ? C51 C52 1.488(4) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 C53 1.503(4) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C53 C54 1.484(4) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C55 C56 1.498(3) . ? C55 H55A 0.9700 . ? C55 H55B 0.9700 . ? C56 C57 1.475(4) . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? C57 C58 1.464(4) . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? C58 H58A 0.9700 . ? C58 H58B 0.9700 . ? 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 O3 K O1 107.60(5) . . ? O3 K O4 113.28(5) . . ? O1 K O4 113.17(5) . . ? O3 K O2 70.05(4) . . ? O1 K O2 68.50(4) . . ? O4 K O2 78.70(5) . . ? O3 K C1 119.43(5) . . ? O1 K C1 23.23(4) . . ? O4 K C1 89.95(6) . . ? O2 K C1 60.64(4) . . ? O3 K C14 22.80(4) . . ? O1 K C14 116.55(5) . . ? O4 K C14 90.71(5) . . ? O2 K C14 59.75(4) . . ? C1 K C14 118.92(6) . . ? O3 K C19 165.37(5) . . ? O1 K C19 68.88(6) . . ? O4 K C19 80.58(6) . . ? O2 K C19 119.29(5) . . ? C1 K C19 62.99(5) . . ? C14 K C19 171.16(5) . . ? O3 K C20 148.92(5) . . ? O1 K C20 88.88(6) . . ? O4 K C20 82.08(6) . . ? O2 K C20 140.99(5) . . ? C1 K C20 85.90(6) . . ? C14 K C20 154.26(5) . . ? C19 K C20 23.06(5) . . ? C1 O1 K 104.44(9) . . ? C8 O2 C7 109.69(13) . . ? C8 O2 K 114.96(9) . . ? C7 O2 K 116.76(9) . . ? C14 O3 K 107.66(10) . . ? C14 O3 H2A 110.5(16) . . ? K O3 H2A 122.7(16) . . ? C51 O4 C54 107.66(18) . . ? C51 O4 K 116.09(13) . . ? C54 O4 K 120.15(14) . . ? C58 O5 C55 108.25(19) . . ? O1 C1 C6 120.82(15) . . ? O1 C1 C2 120.61(15) . . ? C6 C1 C2 118.57(15) . . ? O1 C1 K 52.33(8) . . ? C6 C1 K 97.53(10) . . ? C2 C1 K 118.80(11) . . ? C3 C2 C1 118.47(15) . . ? C3 C2 C15 121.80(15) . . ? C1 C2 C15 119.58(15) . . ? C2 C3 C4 123.45(16) . . ? C2 C3 H3A 118.3 . . ? C4 C3 H3A 118.3 . . ? C5 C4 C3 117.04(16) . . ? C5 C4 C24 123.07(16) . . ? C3 C4 C24 119.68(15) . . ? C4 C5 C6 121.75(16) . . ? C4 C5 H5A 119.1 . . ? C6 C5 H5A 119.1 . . ? C5 C6 C1 120.67(15) . . ? C5 C6 C7 119.52(15) . . ? C1 C6 C7 119.70(15) . . ? O2 C7 C6 110.82(14) . . ? O2 C7 H7A 109.5 . . ? C6 C7 H7A 109.5 . . ? O2 C7 H7B 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 108.1 . . ? O2 C8 C9 109.46(14) . . ? O2 C8 H8A 109.8 . . ? C9 C8 H8A 109.8 . . ? O2 C8 H8B 109.8 . . ? C9 C8 H8B 109.8 . . ? H8A C8 H8B 108.2 . . ? C10 C9 C14 120.27(16) . . ? C10 C9 C8 119.47(16) . . ? C14 C9 C8 120.24(15) . . ? C11 C10 C9 122.19(16) . . ? C11 C10 H10A 118.9 . . ? C9 C10 H10A 118.9 . . ? C10 C11 C12 116.97(15) . . ? C10 C11 C33 123.23(16) . . ? C12 C11 C33 119.77(15) . . ? C13 C12 C11 123.30(16) . . ? C13 C12 H12A 118.4 . . ? C11 C12 H12A 118.4 . . ? C12 C13 C14 118.04(16) . . ? C12 C13 C42 122.35(15) . . ? C14 C13 C42 119.60(14) . . ? O3 C14 C9 120.22(15) . . ? O3 C14 C13 120.55(15) . . ? C9 C14 C13 119.23(15) . . ? O3 C14 K 49.53(8) . . ? C9 C14 K 99.40(10) . . ? C13 C14 K 119.43(11) . . ? C17 C15 C18 112.36(15) . . ? C17 C15 C16 106.48(15) . . ? C18 C15 C16 106.52(14) . . ? C17 C15 C2 108.83(15) . . ? C18 C15 C2 110.78(14) . . ? C16 C15 C2 111.81(15) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C23 C18 C19 117.47(18) . . ? C23 C18 C15 123.18(17) . . ? C19 C18 C15 119.24(17) . . ? C20 C19 C18 121.5(2) . . ? C20 C19 K 80.69(13) . . ? C18 C19 K 91.64(12) . . ? C20 C19 H19A 117.4 . . ? C18 C19 H19A 117.4 . . ? K C19 H19A 117.4 . . ? C21 C20 C19 119.9(2) . . ? C21 C20 K 93.41(14) . . ? C19 C20 K 76.25(12) . . ? C21 C20 H20A 118.4 . . ? C19 C20 H20A 118.4 . . ? K C20 H20A 118.4 . . ? C22 C21 C20 119.6(2) . . ? C22 C21 H21A 120.2 . . ? C20 C21 H21A 120.2 . . ? C21 C22 C23 120.6(2) . . ? C21 C22 H22A 119.7 . . ? C23 C22 H22A 119.7 . . ? C18 C23 C22 120.9(2) . . ? C18 C23 H23A 119.5 . . ? C22 C23 H23A 119.5 . . ? C25 C24 C4 112.24(15) . . ? C25 C24 C26 107.79(16) . . ? C4 C24 C26 109.70(15) . . ? C25 C24 C27 106.72(14) . . ? C4 C24 C27 108.75(14) . . ? C26 C24 C27 111.65(15) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C32 120.0 . . ? C28 C27 C24 121.79(10) . . ? C32 C27 C24 118.12(10) . . ? C29 C28 C27 120.0 . . ? C29 C28 H28A 120.0 . . ? C27 C28 H28A 120.0 . . ? C28 C29 C30 120.0 . . ? C28 C29 H29A 120.0 . . ? C30 C29 H29A 120.0 . . ? C31 C30 C29 120.0 . . ? C31 C30 H30A 120.0 . . ? C29 C30 H30A 120.0 . . ? C30 C31 C32 120.0 . . ? C30 C31 H31A 120.0 . . ? C32 C31 H31A 120.0 . . ? C31 C32 C27 120.0 . . ? C31 C32 H32A 120.0 . . ? C27 C32 H32A 120.0 . . ? C35 C33 C36 111.73(15) . . ? C35 C33 C34 107.61(16) . . ? C36 C33 C34 106.94(15) . . ? C35 C33 C11 107.86(15) . . ? C36 C33 C11 110.85(15) . . ? C34 C33 C11 111.85(15) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C41 C36 C37 117.12(18) . . ? C41 C36 C33 121.66(16) . . ? C37 C36 C33 121.12(18) . . ? C38 C37 C36 121.5(2) . . ? C38 C37 H37A 119.3 . . ? C36 C37 H37A 119.3 . . ? C39 C38 C37 120.2(2) . . ? C39 C38 H38A 119.9 . . ? C37 C38 H38A 119.9 . . ? C38 C39 C40 119.6(2) . . ? C38 C39 H39A 120.2 . . ? C40 C39 H39A 120.2 . . ? C39 C40 C41 120.2(2) . . ? C39 C40 H40A 119.9 . . ? C41 C40 H40A 119.9 . . ? C36 C41 C40 121.3(2) . . ? C36 C41 H41A 119.3 . . ? C40 C41 H41A 119.3 . . ? C44 C42 C45 112.79(14) . . ? C44 C42 C43 106.11(15) . . ? C45 C42 C43 106.71(15) . . ? C44 C42 C13 110.45(15) . . ? C45 C42 C13 108.87(14) . . ? C43 C42 C13 111.87(14) . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C50 C45 C46 117.05(17) . . ? C50 C45 C42 119.73(16) . . ? C46 C45 C42 123.09(17) . . ? C45 C46 C47 121.3(2) . . ? C45 C46 H46A 119.3 . . ? C47 C46 H46A 119.3 . . ? C48 C47 C46 120.8(2) . . ? C48 C47 H47A 119.6 . . ? C46 C47 H47A 119.6 . . ? C47 C48 C49 118.89(19) . . ? C47 C48 H48A 120.6 . . ? C49 C48 H48A 120.6 . . ? C48 C49 C50 120.0(2) . . ? C48 C49 H49A 120.0 . . ? C50 C49 H49A 120.0 . . ? C45 C50 C49 121.92(18) . . ? C45 C50 H50A 119.0 . . ? C49 C50 H50A 119.0 . . ? O4 C51 C52 104.99(19) . . ? O4 C51 H51A 110.7 . . ? C52 C51 H51A 110.7 . . ? O4 C51 H51B 110.7 . . ? C52 C51 H51B 110.7 . . ? H51A C51 H51B 108.8 . . ? C51 C52 C53 102.7(2) . . ? C51 C52 H52A 111.2 . . ? C53 C52 H52A 111.2 . . ? C51 C52 H52B 111.2 . . ? C53 C52 H52B 111.2 . . ? H52A C52 H52B 109.1 . . ? C54 C53 C52 102.7(2) . . ? C54 C53 H53A 111.2 . . ? C52 C53 H53A 111.2 . . ? C54 C53 H53B 111.2 . . ? C52 C53 H53B 111.2 . . ? H53A C53 H53B 109.1 . . ? O4 C54 C53 108.0(2) . . ? O4 C54 H54A 110.1 . . ? C53 C54 H54A 110.1 . . ? O4 C54 H54B 110.1 . . ? C53 C54 H54B 110.1 . . ? H54A C54 H54B 108.4 . . ? O5 C55 C56 107.95(19) . . ? O5 C55 H55A 110.1 . . ? C56 C55 H55A 110.1 . . ? O5 C55 H55B 110.1 . . ? C56 C55 H55B 110.1 . . ? H55A C55 H55B 108.4 . . ? C57 C56 C55 104.8(2) . . ? C57 C56 H56A 110.8 . . ? C55 C56 H56A 110.8 . . ? C57 C56 H56B 110.8 . . ? C55 C56 H56B 110.8 . . ? H56A C56 H56B 108.9 . . ? C58 C57 C56 105.9(2) . . ? C58 C57 H57A 110.6 . . ? C56 C57 H57A 110.6 . . ? C58 C57 H57B 110.6 . . ? C56 C57 H57B 110.6 . . ? H57A C57 H57B 108.7 . . ? O5 C58 C57 110.4(2) . . ? O5 C58 H58A 109.6 . . ? C57 C58 H58A 109.6 . . ? O5 C58 H58B 109.6 . . ? C57 C58 H58B 109.6 . . ? H58A C58 H58B 108.1 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.601 _refine_diff_density_min -0.330 _refine_diff_density_rms 0.047 data_[Zn2L2] _database_code_depnum_ccdc_archive 'CCDC 917260' #TrackingRef '16476_web_deposit_cif_file_2_YongHuang_1356657153.[Zn2L2].cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C100 H104 O6 Zn2,2(C7 H8)' _chemical_formula_sum 'C114 H120 O6 Zn2' _chemical_formula_weight 1716.84 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.0407(9) _cell_length_b 13.5075(9) _cell_length_c 16.6604(11) _cell_angle_alpha 102.9950(10) _cell_angle_beta 99.0350(10) _cell_angle_gamma 118.2450(10) _cell_volume 2397.5(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4121 _cell_measurement_theta_min 2.190 _cell_measurement_theta_max 25.963 _exptl_crystal_description parallelpiped _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.189 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 912 _exptl_absorpt_coefficient_mu 0.555 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.843 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details 'SADABS, Sheldrick (1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 12969 _diffrn_reflns_av_R_equivalents 0.0139 _diffrn_reflns_av_sigmaI/netI 0.0222 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 25.50 _reflns_number_total 8762 _reflns_number_gt 7624 _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^)+(0.1250P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef none _refine_ls_number_reflns 8762 _refine_ls_number_parameters 538 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0502 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_ref 0.1515 _refine_ls_wR_factor_gt 0.1447 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.007 _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 Zn Zn 0.60730(2) 0.56635(2) 0.576970(14) 0.03829(12) Uani 1 1 d . . . O1 O 0.74706(15) 0.69148(13) 0.66353(10) 0.0483(4) Uani 1 1 d . . . O3 O 0.56574(13) 0.48364(13) 0.45176(9) 0.0380(3) Uani 1 1 d . . . O2 O 0.61135(13) 0.42712(12) 0.60723(9) 0.0378(3) Uani 1 1 d . . . C1 C 0.76684(18) 0.67611(18) 0.74008(13) 0.0389(4) Uani 1 1 d . . . C2 C 0.79177(19) 0.76426(19) 0.81766(14) 0.0430(5) Uani 1 1 d . . . C3 C 0.8101(2) 0.7417(2) 0.89520(14) 0.0484(5) Uani 1 1 d . . . H3A H 0.8274 0.7996 0.9465 0.058 Uiso 1 1 calc R . . C4 C 0.8039(2) 0.6373(2) 0.89948(14) 0.0501(5) Uani 1 1 d . . . C5 C 0.7782(2) 0.5525(2) 0.82271(14) 0.0481(5) Uani 1 1 d . . . H5A H 0.7727 0.4816 0.8237 0.058 Uiso 1 1 calc R . . C6 C 0.76041(19) 0.57027(18) 0.74409(13) 0.0398(4) Uani 1 1 d . . . C7 C 0.7340(2) 0.4747(2) 0.66297(14) 0.0447(5) Uani 1 1 d . . . H7A H 0.7936 0.5081 0.6333 0.054 Uiso 1 1 calc R . . H7B H 0.7392 0.4111 0.6774 0.054 Uiso 1 1 calc R . . C8 C 0.5699(2) 0.32320(18) 0.53113(13) 0.0414(5) Uani 1 1 d . . . H8A H 0.4832 0.2869 0.5034 0.050 Uiso 1 1 calc R . . H8B H 0.5806 0.2647 0.5497 0.050 Uiso 1 1 calc R . . C9 C 0.63688(19) 0.35319(18) 0.46611(13) 0.0387(4) Uani 1 1 d . . . C10 C 0.7033(2) 0.30157(19) 0.44414(14) 0.0453(5) Uani 1 1 d . . . H10A H 0.7088 0.2507 0.4717 0.054 Uiso 1 1 calc R . . C11 C 0.7617(2) 0.3244(2) 0.38197(15) 0.0455(5) Uani 1 1 d . . . C12 C 0.7532(2) 0.4030(2) 0.34385(15) 0.0457(5) Uani 1 1 d . . . H12A H 0.7932 0.4196 0.3026 0.055 Uiso 1 1 calc R . . C13 C 0.68869(19) 0.45856(18) 0.36331(13) 0.0394(4) Uani 1 1 d . . . C14 C 0.62901(18) 0.43143(17) 0.42644(13) 0.0361(4) Uani 1 1 d . . . C15 C 0.8007(2) 0.8812(2) 0.81602(16) 0.0505(5) Uani 1 1 d . . . C16 C 0.6781(3) 0.8539(3) 0.7593(2) 0.0811(9) Uani 1 1 d . . . H16A H 0.6586 0.8027 0.7017 0.122 Uiso 1 1 calc R . . H16B H 0.6854 0.9274 0.7574 0.122 Uiso 1 1 calc R . . H16C H 0.6143 0.8147 0.7836 0.122 Uiso 1 1 calc R . . C17 C 0.8268(3) 0.9644(2) 0.9075(2) 0.0708(8) Uani 1 1 d . . . H17A H 0.9021 0.9832 0.9451 0.106 Uiso 1 1 calc R . . H17B H 0.7612 0.9247 0.9302 0.106 Uiso 1 1 calc R . . H17C H 0.8332 1.0370 0.9038 0.106 Uiso 1 1 calc R . . C18 C 0.9093(3) 0.9513(2) 0.78537(15) 0.0535(6) Uani 1 1 d . . . C19 C 0.9067(4) 1.0183(3) 0.7337(2) 0.0895(12) Uani 1 1 d . . . H19A H 0.8360 1.0181 0.7137 0.107 Uiso 1 1 calc R . . C20 C 1.0121(6) 1.0862(3) 0.7119(3) 0.1139(18) Uani 1 1 d . . . H20A H 1.0101 1.1314 0.6778 0.137 Uiso 1 1 calc R . . C21 C 1.1150(5) 1.0878(3) 0.7387(3) 0.119(2) Uani 1 1 d . . . H21A H 1.1827 1.1318 0.7221 0.143 Uiso 1 1 calc R . . C22 C 1.1200(4) 1.0233(3) 0.7915(3) 0.1039(14) Uani 1 1 d . . . H22A H 1.1916 1.0250 0.8117 0.125 Uiso 1 1 calc R . . C23 C 1.0170(3) 0.9562(3) 0.8140(2) 0.0741(9) Uani 1 1 d . . . H23A H 1.0209 0.9131 0.8495 0.089 Uiso 1 1 calc R . . C24 C 0.8271(3) 0.6136(3) 0.98526(16) 0.0642(7) Uani 1 1 d . . . C25 C 0.8397(4) 0.7096(3) 1.06245(18) 0.0941(13) Uani 1 1 d . . . H25A H 0.8536 0.6916 1.1142 0.141 Uiso 1 1 calc R . . H25B H 0.7659 0.7110 1.0529 0.141 Uiso 1 1 calc R . . H25C H 0.9074 0.7864 1.0687 0.141 Uiso 1 1 calc R . . C26 C 0.9462(4) 0.6145(5) 1.0006(3) 0.1148(16) Uani 1 1 d . . . H26A H 0.9628 0.5999 1.0535 0.172 Uiso 1 1 calc R . . H26B H 1.0120 0.6911 1.0046 0.172 Uiso 1 1 calc R . . H26C H 0.9385 0.5532 0.9533 0.172 Uiso 1 1 calc R . . C27 C 0.7186(3) 0.4940(2) 0.97836(16) 0.0625(7) Uani 1 1 d . . . C28 C 0.7335(5) 0.4206(4) 1.0184(3) 0.1097(14) Uani 1 1 d . . . H28A H 0.8111 0.4403 1.0475 0.132 Uiso 1 1 calc R . . C29 C 0.6258(8) 0.3126(5) 1.0142(4) 0.158(3) Uani 1 1 d . . . H29A H 0.6346 0.2631 1.0418 0.190 Uiso 1 1 calc R . . C30 C 0.5146(7) 0.2828(5) 0.9717(5) 0.150(3) Uani 1 1 d . . . H30A H 0.4466 0.2121 0.9687 0.180 Uiso 1 1 calc R . . C31 C 0.5000(5) 0.3548(4) 0.9327(4) 0.1258(17) Uani 1 1 d . . . H31A H 0.4220 0.3339 0.9031 0.151 Uiso 1 1 calc R . . C32 C 0.6003(4) 0.4585(3) 0.9371(3) 0.0926(11) Uani 1 1 d . . . H32A H 0.5882 0.5077 0.9109 0.111 Uiso 1 1 calc R . . C33 C 0.8371(2) 0.2702(2) 0.35467(18) 0.0566(6) Uani 1 1 d . . . C34 C 0.9732(3) 0.3701(3) 0.3908(3) 0.0962(13) Uani 1 1 d . . . H34A H 1.0218 0.3381 0.3745 0.144 Uiso 1 1 calc R . . H34B H 0.9961 0.4020 0.4527 0.144 Uiso 1 1 calc R . . H34C H 0.9866 0.4327 0.3676 0.144 Uiso 1 1 calc R . . C35 C 0.8201(4) 0.1706(3) 0.3896(2) 0.0781(9) Uani 1 1 d . . . H35A H 0.7359 0.1063 0.3668 0.117 Uiso 1 1 calc R . . H35B H 0.8431 0.2008 0.4516 0.117 Uiso 1 1 calc R . . H35C H 0.8706 0.1416 0.3724 0.117 Uiso 1 1 calc R . . C36 C 0.7928(3) 0.2155(2) 0.25580(19) 0.0596(7) Uani 1 1 d . . . C37 C 0.6692(3) 0.1331(3) 0.2123(2) 0.0796(9) Uani 1 1 d . . . H37A H 0.6137 0.1161 0.2438 0.095 Uiso 1 1 calc R . . C38 C 0.6264(5) 0.0756(5) 0.1235(3) 0.1172(16) Uani 1 1 d . . . H38A H 0.5430 0.0213 0.0968 0.141 Uiso 1 1 calc R . . C39 C 0.6997(8) 0.0956(7) 0.0763(3) 0.138(2) Uani 1 1 d . . . H39A H 0.6690 0.0538 0.0171 0.166 Uiso 1 1 calc R . . C40 C 0.8203(7) 0.1772(6) 0.1137(4) 0.135(2) Uani 1 1 d . . . H40A H 0.8717 0.1941 0.0792 0.162 Uiso 1 1 calc R . . C41 C 0.8712(4) 0.2386(4) 0.2059(3) 0.0969(13) Uani 1 1 d . . . H41A H 0.9549 0.2925 0.2313 0.116 Uiso 1 1 calc R . . C42 C 0.6785(2) 0.5402(2) 0.31646(14) 0.0458(5) Uani 1 1 d . . . C43 C 0.5480(3) 0.4712(3) 0.25356(17) 0.0643(7) Uani 1 1 d . . . H43A H 0.4902 0.4499 0.2854 0.096 Uiso 1 1 calc R . . H43B H 0.5335 0.4000 0.2125 0.096 Uiso 1 1 calc R . . H43C H 0.5387 0.5208 0.2235 0.096 Uiso 1 1 calc R . . C44 C 0.7673(3) 0.5725(3) 0.2620(2) 0.0703(8) Uani 1 1 d . . . H44A H 0.8500 0.6156 0.2994 0.105 Uiso 1 1 calc R . . H44B H 0.7562 0.6214 0.2321 0.105 Uiso 1 1 calc R . . H44C H 0.7508 0.5005 0.2206 0.105 Uiso 1 1 calc R . . C45 C 0.7128(2) 0.6608(2) 0.38021(15) 0.0480(5) Uani 1 1 d . . . C46 C 0.8062(3) 0.7147(3) 0.4573(2) 0.0761(9) Uani 1 1 d . . . H46A H 0.8434 0.6744 0.4720 0.091 Uiso 1 1 calc R . . C47 C 0.8457(4) 0.8276(3) 0.5133(3) 0.1039(14) Uani 1 1 d . . . H47A H 0.9082 0.8618 0.5651 0.125 Uiso 1 1 calc R . . C48 C 0.7922(4) 0.8889(3) 0.4921(3) 0.0961(12) Uani 1 1 d . . . H48A H 0.8183 0.9647 0.5291 0.115 Uiso 1 1 calc R . . C49 C 0.7007(4) 0.8369(3) 0.4163(3) 0.0798(10) Uani 1 1 d . . . H49A H 0.6648 0.8781 0.4011 0.096 Uiso 1 1 calc R . . C50 C 0.6602(3) 0.7238(2) 0.36158(19) 0.0589(6) Uani 1 1 d . . . H50A H 0.5958 0.6893 0.3109 0.071 Uiso 1 1 calc R . . C53 C 0.7651(10) 1.1720(9) 0.6343(4) 0.236(7) Uani 1 1 d GU . . H53A H 0.8158 1.1841 0.5993 0.284 Uiso 1 1 calc R . . C57 C 0.8103(7) 1.2490(6) 0.7193(5) 0.196(4) Uani 1 1 d GU . . C52 C 0.7345(9) 1.2308(7) 0.7716(3) 0.197(4) Uani 1 1 d GU . . H52A H 0.7647 1.2824 0.8285 0.236 Uiso 1 1 calc R . . C56 C 0.6137(9) 1.1355(9) 0.7389(7) 0.322(9) Uani 1 1 d G . . H56A H 0.5630 1.1234 0.7739 0.386 Uiso 1 1 calc R . . C55 C 0.5685(7) 1.0585(7) 0.6539(8) 0.291(8) Uani 1 1 d G . . H55A H 0.4877 0.9948 0.6320 0.349 Uiso 1 1 calc R . . C54 C 0.6443(11) 1.0767(8) 0.6016(4) 0.295(9) Uani 1 1 d G . . H54A H 0.6141 1.0251 0.5447 0.354 Uiso 1 1 calc R . . C51 C 0.9178(9) 1.3426(13) 0.7432(10) 0.322(9) Uani 1 1 d . . . H51A H 0.9550 1.3382 0.6982 0.483 Uiso 1 1 calc R . . H51B H 0.9665 1.3472 0.7951 0.483 Uiso 1 1 calc R . . H51C H 0.9122 1.4125 0.7541 0.483 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 Zn 0.03958(17) 0.04349(17) 0.03346(16) 0.00796(11) 0.00960(11) 0.02592(13) O1 0.0523(9) 0.0406(8) 0.0415(8) 0.0155(6) 0.0078(7) 0.0182(7) O3 0.0398(7) 0.0489(8) 0.0343(7) 0.0114(6) 0.0164(6) 0.0298(7) O2 0.0392(7) 0.0420(7) 0.0331(7) 0.0086(6) 0.0136(6) 0.0232(6) C1 0.0369(10) 0.0393(10) 0.0359(10) 0.0124(8) 0.0083(8) 0.0178(9) C2 0.0386(11) 0.0394(10) 0.0458(12) 0.0108(9) 0.0113(9) 0.0189(9) C3 0.0520(13) 0.0444(11) 0.0372(11) 0.0073(9) 0.0121(10) 0.0203(10) C4 0.0556(13) 0.0505(12) 0.0384(11) 0.0155(10) 0.0111(10) 0.0246(11) C5 0.0548(13) 0.0474(12) 0.0443(12) 0.0157(10) 0.0104(10) 0.0300(11) C6 0.0385(10) 0.0422(11) 0.0370(10) 0.0101(9) 0.0095(8) 0.0222(9) C7 0.0448(12) 0.0512(12) 0.0438(12) 0.0124(10) 0.0131(9) 0.0313(10) C8 0.0486(12) 0.0350(10) 0.0399(11) 0.0095(8) 0.0185(9) 0.0216(9) C9 0.0415(11) 0.0375(10) 0.0372(10) 0.0085(8) 0.0153(9) 0.0219(9) C10 0.0537(13) 0.0424(11) 0.0461(12) 0.0108(9) 0.0175(10) 0.0313(10) C11 0.0457(12) 0.0448(11) 0.0499(12) 0.0066(9) 0.0185(10) 0.0297(10) C12 0.0456(12) 0.0495(12) 0.0486(12) 0.0132(10) 0.0265(10) 0.0280(10) C13 0.0399(11) 0.0425(10) 0.0390(10) 0.0110(8) 0.0184(9) 0.0236(9) C14 0.0352(10) 0.0385(10) 0.0364(10) 0.0077(8) 0.0137(8) 0.0222(8) C15 0.0541(13) 0.0417(11) 0.0540(13) 0.0105(10) 0.0165(11) 0.0269(10) C16 0.0715(19) 0.0611(17) 0.108(3) 0.0206(17) 0.0079(18) 0.0421(15) C17 0.092(2) 0.0507(14) 0.0756(19) 0.0145(13) 0.0418(17) 0.0403(15) C18 0.0714(16) 0.0350(11) 0.0445(12) 0.0065(9) 0.0189(11) 0.0239(11) C19 0.115(3) 0.0488(15) 0.0651(18) 0.0231(14) 0.0059(18) 0.0193(17) C20 0.167(5) 0.057(2) 0.068(2) 0.0262(17) 0.044(3) 0.019(3) C21 0.156(5) 0.0480(18) 0.133(4) 0.020(2) 0.108(4) 0.025(2) C22 0.094(3) 0.0585(18) 0.165(4) 0.028(2) 0.082(3) 0.0358(18) C23 0.0767(19) 0.0554(15) 0.109(2) 0.0344(16) 0.0532(19) 0.0384(15) C24 0.0747(18) 0.0712(17) 0.0391(12) 0.0221(12) 0.0106(12) 0.0337(15) C25 0.134(3) 0.0650(18) 0.0422(15) 0.0142(13) 0.0208(18) 0.027(2) C26 0.094(3) 0.183(5) 0.083(3) 0.076(3) 0.014(2) 0.075(3) C27 0.091(2) 0.0590(15) 0.0458(13) 0.0223(11) 0.0244(14) 0.0428(15) C28 0.154(4) 0.087(3) 0.106(3) 0.053(2) 0.032(3) 0.071(3) C29 0.227(8) 0.097(4) 0.170(6) 0.092(4) 0.067(6) 0.078(5) C30 0.181(6) 0.080(3) 0.163(6) 0.057(4) 0.070(5) 0.038(4) C31 0.107(3) 0.099(3) 0.139(4) 0.049(3) 0.047(3) 0.025(3) C32 0.085(2) 0.088(2) 0.103(3) 0.053(2) 0.035(2) 0.035(2) C33 0.0559(14) 0.0592(14) 0.0655(16) 0.0111(12) 0.0253(12) 0.0407(12) C34 0.0535(17) 0.083(2) 0.138(3) 0.003(2) 0.0226(19) 0.0427(17) C35 0.113(3) 0.099(2) 0.0743(19) 0.0308(17) 0.0425(18) 0.089(2) C36 0.0799(18) 0.0612(15) 0.0680(16) 0.0234(13) 0.0414(15) 0.0535(15) C37 0.084(2) 0.077(2) 0.0716(19) 0.0079(16) 0.0214(17) 0.0461(18) C38 0.144(4) 0.127(4) 0.076(3) -0.002(2) 0.008(3) 0.093(3) C39 0.226(7) 0.195(6) 0.077(3) 0.041(3) 0.052(4) 0.172(6) C40 0.231(7) 0.212(6) 0.113(4) 0.100(4) 0.127(5) 0.186(6) C41 0.131(3) 0.133(3) 0.113(3) 0.072(3) 0.090(3) 0.105(3) C42 0.0540(13) 0.0500(12) 0.0418(11) 0.0174(10) 0.0239(10) 0.0303(11) C43 0.0708(17) 0.0688(16) 0.0458(13) 0.0180(12) 0.0070(12) 0.0355(14) C44 0.100(2) 0.0748(18) 0.0721(18) 0.0414(15) 0.0600(17) 0.0552(17) C45 0.0575(13) 0.0465(12) 0.0511(13) 0.0216(10) 0.0277(11) 0.0304(11) C46 0.088(2) 0.0524(15) 0.0729(19) 0.0084(13) 0.0028(16) 0.0377(15) C47 0.130(3) 0.0601(19) 0.082(2) -0.0022(17) -0.005(2) 0.044(2) C48 0.141(4) 0.0558(17) 0.084(2) 0.0136(17) 0.038(2) 0.050(2) C49 0.111(3) 0.0653(18) 0.111(3) 0.0521(19) 0.068(2) 0.0627(19) C50 0.0700(17) 0.0614(15) 0.0671(16) 0.0347(13) 0.0360(14) 0.0409(14) C53 0.46(2) 0.318(14) 0.111(5) 0.084(7) 0.062(8) 0.337(16) C57 0.250(11) 0.217(9) 0.240(9) 0.134(8) 0.082(9) 0.184(9) C52 0.366(14) 0.221(9) 0.188(7) 0.144(7) 0.161(9) 0.235(10) C56 0.37(2) 0.171(10) 0.375(19) 0.122(12) 0.023(17) 0.124(12) C55 0.273(16) 0.319(18) 0.222(13) 0.081(13) 0.027(13) 0.133(14) C54 0.39(2) 0.270(17) 0.280(15) 0.094(12) -0.018(16) 0.245(18) C51 0.149(8) 0.41(2) 0.48(2) 0.231(19) 0.078(11) 0.172(11) _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 Zn O1 1.8495(15) . ? Zn O3 1.9622(14) 2_666 ? Zn O3 1.9792(13) . ? Zn O2 2.0750(15) . ? Zn Zn 2.9245(5) 2_666 ? O1 C1 1.343(2) . ? O3 C14 1.372(2) . ? O3 Zn 1.9622(14) 2_666 ? O2 C7 1.459(3) . ? O2 C8 1.462(2) . ? C1 C6 1.409(3) . ? C1 C2 1.415(3) . ? C2 C3 1.403(3) . ? C2 C15 1.534(3) . ? C3 C4 1.392(3) . ? C3 H3A 0.9300 . ? C4 C5 1.380(3) . ? C4 C24 1.549(3) . ? C5 C6 1.388(3) . ? C5 H5A 0.9300 . ? C6 C7 1.504(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.504(3) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.389(3) . ? C9 C14 1.400(3) . ? C10 C11 1.384(3) . ? C10 H10A 0.9300 . ? C11 C12 1.390(3) . ? C11 C33 1.544(3) . ? C12 C13 1.397(3) . ? C12 H12A 0.9300 . ? C13 C14 1.417(3) . ? C13 C42 1.528(3) . ? C15 C18 1.529(4) . ? C15 C16 1.549(4) . ? C15 C17 1.552(4) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C23 1.376(4) . ? C18 C19 1.389(4) . ? C19 C20 1.405(6) . ? C19 H19A 0.9300 . ? C20 C21 1.333(7) . ? C20 H20A 0.9300 . ? C21 C22 1.384(7) . ? C21 H21A 0.9300 . ? C22 C23 1.387(4) . ? C22 H22A 0.9300 . ? C23 H23A 0.9300 . ? C24 C27 1.526(4) . ? C24 C26 1.526(5) . ? C24 C25 1.532(4) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C32 1.378(5) . ? C27 C28 1.380(4) . ? C28 C29 1.445(8) . ? C28 H28A 0.9300 . ? C29 C30 1.328(9) . ? C29 H29A 0.9300 . ? C30 C31 1.350(8) . ? C30 H30A 0.9300 . ? C31 C32 1.368(5) . ? C31 H31A 0.9300 . ? C32 H32A 0.9300 . ? C33 C35 1.519(4) . ? C33 C36 1.531(4) . ? C33 C34 1.538(4) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 C41 1.384(4) . ? C36 C37 1.391(5) . ? C37 C38 1.385(5) . ? C37 H37A 0.9300 . ? C38 C39 1.300(8) . ? C38 H38A 0.9300 . ? C39 C40 1.349(8) . ? C39 H39A 0.9300 . ? C40 C41 1.440(7) . ? C40 H40A 0.9300 . ? C41 H41A 0.9300 . ? C42 C45 1.537(3) . ? C42 C43 1.537(4) . ? C42 C44 1.544(3) . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 C50 1.378(4) . ? C45 C46 1.383(4) . ? C46 C47 1.387(4) . ? C46 H46A 0.9300 . ? C47 C48 1.378(6) . ? C47 H47A 0.9300 . ? C48 C49 1.358(6) . ? C48 H48A 0.9300 . ? C49 C50 1.379(4) . ? C49 H49A 0.9300 . ? C50 H50A 0.9300 . ? C53 C57 1.3900 . ? C53 C54 1.3900 . ? C53 H53A 0.9300 . ? C57 C51 1.282(11) . ? C57 C52 1.3900 . ? C52 C56 1.3900 . ? C52 H52A 0.9300 . ? C56 C55 1.3900 . ? C56 H56A 0.9300 . ? C55 C54 1.3900 . ? C55 H55A 0.9300 . ? C54 H54A 0.9300 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn O3 133.72(7) . 2_666 ? O1 Zn O3 135.53(7) . . ? O3 Zn O3 84.20(6) 2_666 . ? O1 Zn O2 97.69(6) . . ? O3 Zn O2 104.58(6) 2_666 . ? O3 Zn O2 91.80(6) . . ? O1 Zn Zn 161.20(5) . 2_666 ? O3 Zn Zn 42.32(4) 2_666 2_666 ? O3 Zn Zn 41.87(4) . 2_666 ? O2 Zn Zn 100.96(4) . 2_666 ? C1 O1 Zn 116.05(13) . . ? C14 O3 Zn 134.91(12) . 2_666 ? C14 O3 Zn 117.97(12) . . ? Zn O3 Zn 95.80(6) 2_666 . ? C7 O2 C8 113.30(16) . . ? C7 O2 Zn 108.06(12) . . ? C8 O2 Zn 113.36(12) . . ? O1 C1 C6 120.26(19) . . ? O1 C1 C2 120.81(19) . . ? C6 C1 C2 118.92(19) . . ? C3 C2 C1 117.8(2) . . ? C3 C2 C15 121.8(2) . . ? C1 C2 C15 120.4(2) . . ? C4 C3 C2 123.5(2) . . ? C4 C3 H3A 118.2 . . ? C2 C3 H3A 118.2 . . ? C5 C4 C3 117.4(2) . . ? C5 C4 C24 119.0(2) . . ? C3 C4 C24 123.6(2) . . ? C4 C5 C6 121.7(2) . . ? C4 C5 H5A 119.2 . . ? C6 C5 H5A 119.2 . . ? C5 C6 C1 120.70(19) . . ? C5 C6 C7 118.9(2) . . ? C1 C6 C7 120.38(19) . . ? O2 C7 C6 108.54(17) . . ? O2 C7 H7A 110.0 . . ? C6 C7 H7A 110.0 . . ? O2 C7 H7B 110.0 . . ? C6 C7 H7B 110.0 . . ? H7A C7 H7B 108.4 . . ? O2 C8 C9 113.37(16) . . ? O2 C8 H8A 108.9 . . ? C9 C8 H8A 108.9 . . ? O2 C8 H8B 108.9 . . ? C9 C8 H8B 108.9 . . ? H8A C8 H8B 107.7 . . ? C10 C9 C14 120.41(19) . . ? C10 C9 C8 120.3(2) . . ? C14 C9 C8 119.23(18) . . ? C11 C10 C9 121.2(2) . . ? C11 C10 H10A 119.4 . . ? C9 C10 H10A 119.4 . . ? C10 C11 C12 117.4(2) . . ? C10 C11 C33 123.8(2) . . ? C12 C11 C33 118.8(2) . . ? C11 C12 C13 124.4(2) . . ? C11 C12 H12A 117.8 . . ? C13 C12 H12A 117.8 . . ? C12 C13 C14 116.4(2) . . ? C12 C13 C42 121.89(18) . . ? C14 C13 C42 121.68(18) . . ? O3 C14 C9 118.75(17) . . ? O3 C14 C13 120.96(18) . . ? C9 C14 C13 120.26(18) . . ? C18 C15 C2 109.11(19) . . ? C18 C15 C16 113.0(2) . . ? C2 C15 C16 110.1(2) . . ? C18 C15 C17 105.8(2) . . ? C2 C15 C17 112.1(2) . . ? C16 C15 C17 106.7(2) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C23 C18 C19 117.7(3) . . ? C23 C18 C15 119.8(2) . . ? C19 C18 C15 122.3(3) . . ? C18 C19 C20 119.4(4) . . ? C18 C19 H19A 120.3 . . ? C20 C19 H19A 120.3 . . ? C21 C20 C19 122.1(4) . . ? C21 C20 H20A 119.0 . . ? C19 C20 H20A 119.0 . . ? C20 C21 C22 119.4(4) . . ? C20 C21 H21A 120.3 . . ? C22 C21 H21A 120.3 . . ? C21 C22 C23 119.3(4) . . ? C21 C22 H22A 120.3 . . ? C23 C22 H22A 120.3 . . ? C18 C23 C22 122.1(4) . . ? C18 C23 H23A 119.0 . . ? C22 C23 H23A 119.0 . . ? C27 C24 C26 112.1(3) . . ? C27 C24 C25 107.2(2) . . ? C26 C24 C25 108.8(3) . . ? C27 C24 C4 109.1(2) . . ? C26 C24 C4 107.7(2) . . ? C25 C24 C4 112.0(3) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C32 C27 C28 117.0(4) . . ? C32 C27 C24 121.3(3) . . ? C28 C27 C24 121.6(3) . . ? C27 C28 C29 118.6(5) . . ? C27 C28 H28A 120.7 . . ? C29 C28 H28A 120.7 . . ? C30 C29 C28 121.2(5) . . ? C30 C29 H29A 119.4 . . ? C28 C29 H29A 119.4 . . ? C29 C30 C31 120.3(5) . . ? C29 C30 H30A 119.9 . . ? C31 C30 H30A 119.9 . . ? C30 C31 C32 119.6(6) . . ? C30 C31 H31A 120.2 . . ? C32 C31 H31A 120.2 . . ? C31 C32 C27 123.4(4) . . ? C31 C32 H32A 118.3 . . ? C27 C32 H32A 118.3 . . ? C35 C33 C36 107.2(2) . . ? C35 C33 C34 108.1(3) . . ? C36 C33 C34 112.7(3) . . ? C35 C33 C11 112.7(2) . . ? C36 C33 C11 108.0(2) . . ? C34 C33 C11 108.2(2) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C41 C36 C37 116.8(3) . . ? C41 C36 C33 123.1(3) . . ? C37 C36 C33 120.0(3) . . ? C38 C37 C36 121.8(4) . . ? C38 C37 H37A 119.1 . . ? C36 C37 H37A 119.1 . . ? C39 C38 C37 121.8(5) . . ? C39 C38 H38A 119.1 . . ? C37 C38 H38A 119.1 . . ? C38 C39 C40 119.8(5) . . ? C38 C39 H39A 120.1 . . ? C40 C39 H39A 120.1 . . ? C39 C40 C41 121.3(5) . . ? C39 C40 H40A 119.4 . . ? C41 C40 H40A 119.4 . . ? C36 C41 C40 118.6(5) . . ? C36 C41 H41A 120.7 . . ? C40 C41 H41A 120.7 . . ? C13 C42 C45 111.88(18) . . ? C13 C42 C43 107.66(19) . . ? C45 C42 C43 112.9(2) . . ? C13 C42 C44 112.0(2) . . ? C45 C42 C44 105.2(2) . . ? C43 C42 C44 107.2(2) . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C50 C45 C46 117.0(3) . . ? C50 C45 C42 122.7(2) . . ? C46 C45 C42 120.1(2) . . ? C45 C46 C47 121.6(3) . . ? C45 C46 H46A 119.2 . . ? C47 C46 H46A 119.2 . . ? C48 C47 C46 119.9(4) . . ? C48 C47 H47A 120.1 . . ? C46 C47 H47A 120.1 . . ? C49 C48 C47 119.0(3) . . ? C49 C48 H48A 120.5 . . ? C47 C48 H48A 120.5 . . ? C48 C49 C50 120.9(3) . . ? C48 C49 H49A 119.5 . . ? C50 C49 H49A 119.5 . . ? C49 C50 C45 121.6(3) . . ? C49 C50 H50A 119.2 . . ? C45 C50 H50A 119.2 . . ? C57 C53 C54 120.0 . . ? C57 C53 H53A 120.0 . . ? C54 C53 H53A 120.0 . . ? C51 C57 C53 117.3(9) . . ? C51 C57 C52 122.3(9) . . ? C53 C57 C52 120.0 . . ? C56 C52 C57 120.0 . . ? C56 C52 H52A 120.0 . . ? C57 C52 H52A 120.0 . . ? C52 C56 C55 120.0 . . ? C52 C56 H56A 120.0 . . ? C55 C56 H56A 120.0 . . ? C56 C55 C54 120.0 . . ? C56 C55 H55A 120.0 . . ? C54 C55 H55A 120.0 . . ? C55 C54 C53 120.0 . . ? C55 C54 H54A 120.0 . . ? C53 C54 H54A 120.0 . . ? C57 C51 H51A 109.5 . . ? C57 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C57 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.655 _refine_diff_density_min -0.420 _refine_diff_density_rms 0.058 data_[Mg2L2] _database_code_depnum_ccdc_archive 'CCDC 917261' #TrackingRef '16477_web_deposit_cif_file_3_YongHuang_1356657153.[Mg2L2].cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C100 H104 Mg2 O6' _chemical_formula_sum 'C100 H104 Mg2 O6' _chemical_formula_weight 1450.45 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' Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.498(3) _cell_length_b 13.382(3) _cell_length_c 15.071(3) _cell_angle_alpha 65.05(3) _cell_angle_beta 68.00(3) _cell_angle_gamma 65.58(3) _cell_volume 2018.9(7) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8857 _cell_measurement_theta_min 5.097 _cell_measurement_theta_max 27.485 _exptl_crystal_description parallelpiped _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.193 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 776 _exptl_absorpt_coefficient_mu 0.086 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.988 _exptl_absorpt_correction_T_max 0.994 _exptl_absorpt_process_details 'SADABS, Sheldrick (1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13724 _diffrn_reflns_av_R_equivalents 0.0738 _diffrn_reflns_av_sigmaI/netI 0.1254 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 5.10 _diffrn_reflns_theta_max 25.50 _reflns_number_total 7442 _reflns_number_gt 3987 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _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^)+(0.0350P)^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 7442 _refine_ls_number_parameters 487 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1303 _refine_ls_R_factor_gt 0.0507 _refine_ls_wR_factor_ref 0.1116 _refine_ls_wR_factor_gt 0.0922 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.001 _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 Mg1 Mg 0.97874(7) 0.58160(7) 0.40150(6) 0.0243(2) Uani 1 1 d . . . O1 O 0.91028(13) 0.66495(13) 0.28858(11) 0.0257(4) Uani 1 1 d . . . O2 O 1.06682(13) 0.69586(13) 0.36981(11) 0.0246(4) Uani 1 1 d . . . O3 O 0.91929(13) 0.57474(13) 0.54664(11) 0.0231(4) Uani 1 1 d . . . C1 C 0.97781(19) 0.7128(2) 0.19924(17) 0.0227(6) Uani 1 1 d . . . C2 C 0.97775(19) 0.7062(2) 0.10842(17) 0.0233(6) Uani 1 1 d . . . C3 C 1.05734(19) 0.7509(2) 0.01979(18) 0.0265(6) Uani 1 1 d . . . H3A H 1.0579 0.7457 -0.0400 0.032 Uiso 1 1 calc R . . C4 C 1.13589(19) 0.8030(2) 0.01610(17) 0.0251(6) Uani 1 1 d . . . C5 C 1.1290(2) 0.8140(2) 0.10561(18) 0.0268(6) Uani 1 1 d . . . H5A H 1.1782 0.8507 0.1053 0.032 Uiso 1 1 calc R . . C6 C 1.0512(2) 0.7720(2) 0.19566(17) 0.0236(6) Uani 1 1 d . . . C7 C 1.0355(2) 0.8004(2) 0.28631(17) 0.0284(6) Uani 1 1 d . . . H7A H 1.0867 0.8472 0.2694 0.034 Uiso 1 1 calc R . . H7B H 0.9521 0.8452 0.3068 0.034 Uiso 1 1 calc R . . C8 C 1.0566(2) 0.7229(2) 0.45738(17) 0.0270(6) Uani 1 1 d . . . H8A H 1.0926 0.7838 0.4356 0.032 Uiso 1 1 calc R . . H8B H 1.1009 0.6550 0.5026 0.032 Uiso 1 1 calc R . . C9 C 0.9264(2) 0.7612(2) 0.51260(17) 0.0242(6) Uani 1 1 d . . . C10 C 0.8700(2) 0.8736(2) 0.51761(17) 0.0279(6) Uani 1 1 d . . . H10A H 0.9137 0.9265 0.4849 0.034 Uiso 1 1 calc R . . C11 C 0.7507(2) 0.9087(2) 0.57007(18) 0.0281(6) Uani 1 1 d . . . C12 C 0.6899(2) 0.8249(2) 0.61852(18) 0.0263(6) Uani 1 1 d . . . H12A H 0.6105 0.8461 0.6558 0.032 Uiso 1 1 calc R . . C13 C 0.74042(19) 0.7122(2) 0.61453(17) 0.0227(6) Uani 1 1 d . . . C14 C 0.8620(2) 0.6808(2) 0.55989(17) 0.0222(6) Uani 1 1 d . . . C15 C 0.8868(2) 0.6578(2) 0.10673(18) 0.0268(6) Uani 1 1 d . . . C16 C 0.7593(2) 0.7384(2) 0.1373(2) 0.0366(7) Uani 1 1 d . . . H16A H 0.7466 0.7410 0.2033 0.055 Uiso 1 1 calc R . . H16B H 0.6999 0.7097 0.1381 0.055 Uiso 1 1 calc R . . H16C H 0.7516 0.8148 0.0896 0.055 Uiso 1 1 calc R . . C17 C 0.9039(2) 0.6569(2) 0.00043(19) 0.0382(7) Uani 1 1 d . . . H17A H 0.9829 0.6067 -0.0203 0.057 Uiso 1 1 calc R . . H17B H 0.8960 0.7339 -0.0461 0.057 Uiso 1 1 calc R . . H17C H 0.8433 0.6297 0.0014 0.057 Uiso 1 1 calc R . . C18 C 0.9015(2) 0.5322(2) 0.17486(17) 0.0268(6) Uani 1 1 d . . . C19 C 0.8079(2) 0.4837(2) 0.21247(19) 0.0344(7) Uani 1 1 d . . . H19A H 0.7316 0.5306 0.2018 0.041 Uiso 1 1 calc R . . C20 C 0.8259(2) 0.3668(2) 0.26550(19) 0.0381(7) Uani 1 1 d . . . H20A H 0.7620 0.3363 0.2894 0.046 Uiso 1 1 calc R . . C21 C 0.9376(3) 0.2961(2) 0.28288(19) 0.0387(7) Uani 1 1 d . . . H21A H 0.9493 0.2179 0.3192 0.046 Uiso 1 1 calc R . . C22 C 1.0323(2) 0.3419(2) 0.24602(19) 0.0355(7) Uani 1 1 d . . . H22A H 1.1083 0.2946 0.2572 0.043 Uiso 1 1 calc R . . C23 C 1.0138(2) 0.4582(2) 0.19243(18) 0.0307(6) Uani 1 1 d . . . H23A H 1.0786 0.4877 0.1673 0.037 Uiso 1 1 calc R . . C24 C 1.2239(2) 0.8516(2) -0.08064(18) 0.0287(6) Uani 1 1 d . . . C25 C 1.2276(2) 0.8233(3) -0.17051(18) 0.0432(8) Uani 1 1 d . . . H25A H 1.2545 0.7409 -0.1559 0.065 Uiso 1 1 calc R . . H25B H 1.2826 0.8565 -0.2294 0.065 Uiso 1 1 calc R . . H25C H 1.1481 0.8547 -0.1824 0.065 Uiso 1 1 calc R . . C26 C 1.1809(2) 0.9841(2) -0.1065(2) 0.0515(8) Uani 1 1 d . . . H26A H 1.1008 1.0146 -0.1172 0.077 Uiso 1 1 calc R . . H26B H 1.2351 1.0165 -0.1667 0.077 Uiso 1 1 calc R . . H26C H 1.1799 1.0037 -0.0518 0.077 Uiso 1 1 calc R . . C27 C 1.3514(2) 0.7978(2) -0.06305(18) 0.0289(6) Uani 1 1 d . . . C28 C 1.3914(2) 0.6820(2) -0.01009(19) 0.0365(7) Uani 1 1 d . . . H28A H 1.3391 0.6378 0.0155 0.044 Uiso 1 1 calc R . . C29 C 1.5065(2) 0.6296(3) 0.0062(2) 0.0501(8) Uani 1 1 d . . . H29A H 1.5297 0.5519 0.0440 0.060 Uiso 1 1 calc R . . C30 C 1.5867(3) 0.6919(3) -0.0335(2) 0.0548(9) Uani 1 1 d . . . H30A H 1.6647 0.6565 -0.0236 0.066 Uiso 1 1 calc R . . C31 C 1.5513(3) 0.8062(3) -0.0874(2) 0.0561(9) Uani 1 1 d . . . H31A H 1.6056 0.8487 -0.1146 0.067 Uiso 1 1 calc R . . C32 C 1.4341(2) 0.8602(3) -0.1024(2) 0.0416(7) Uani 1 1 d . . . H32A H 1.4109 0.9384 -0.1388 0.050 Uiso 1 1 calc R . . C33 C 0.6856(2) 1.0327(2) 0.57582(19) 0.0334(6) Uani 1 1 d . . . C34 C 0.7549(3) 1.1165(2) 0.4947(2) 0.0517(8) Uani 1 1 d . . . H34A H 0.8343 1.0925 0.5050 0.078 Uiso 1 1 calc R . . H34B H 0.7119 1.1931 0.4993 0.078 Uiso 1 1 calc R . . H34C H 0.7618 1.1162 0.4292 0.078 Uiso 1 1 calc R . . C35 C 0.5596(3) 1.0749(2) 0.5564(2) 0.0549(9) Uani 1 1 d . . . H35A H 0.5188 1.1522 0.5598 0.082 Uiso 1 1 calc R . . H35B H 0.5134 1.0247 0.6065 0.082 Uiso 1 1 calc R . . H35C H 0.5678 1.0743 0.4907 0.082 Uiso 1 1 calc R . . C36 C 0.6781(2) 1.0364(2) 0.67891(19) 0.0301(6) Uani 1 1 d . . . C37 C 0.7804(2) 0.9797(2) 0.71787(19) 0.0337(6) Uani 1 1 d . . . H37A H 0.8508 0.9378 0.6825 0.040 Uiso 1 1 calc R . . C38 C 0.7793(3) 0.9843(2) 0.8085(2) 0.0410(7) Uani 1 1 d . . . H38A H 0.8486 0.9460 0.8332 0.049 Uiso 1 1 calc R . . C39 C 0.6755(3) 1.0458(3) 0.8618(2) 0.0473(8) Uani 1 1 d . . . H39A H 0.6743 1.0488 0.9228 0.057 Uiso 1 1 calc R . . C40 C 0.5749(3) 1.1020(3) 0.8247(2) 0.0528(8) Uani 1 1 d . . . H40A H 0.5049 1.1437 0.8605 0.063 Uiso 1 1 calc R . . C41 C 0.5753(2) 1.0980(2) 0.7340(2) 0.0441(7) Uani 1 1 d . . . H41A H 0.5056 1.1371 0.7098 0.053 Uiso 1 1 calc R . . C42 C 0.6693(2) 0.6243(2) 0.67135(17) 0.0238(6) Uani 1 1 d . . . C43 C 0.7243(2) 0.5360(2) 0.76126(18) 0.0324(6) Uani 1 1 d . . . H43A H 0.8085 0.4990 0.7368 0.049 Uiso 1 1 calc R . . H43B H 0.6824 0.4789 0.7979 0.049 Uiso 1 1 calc R . . H43C H 0.7162 0.5753 0.8051 0.049 Uiso 1 1 calc R . . C44 C 0.5347(2) 0.6809(2) 0.71596(19) 0.0341(7) Uani 1 1 d . . . H44A H 0.4969 0.7368 0.6623 0.051 Uiso 1 1 calc R . . H44B H 0.5291 0.7187 0.7601 0.051 Uiso 1 1 calc R . . H44C H 0.4945 0.6225 0.7533 0.051 Uiso 1 1 calc R . . C45 C 0.66984(19) 0.5643(2) 0.60361(18) 0.0252(6) Uani 1 1 d . . . C46 C 0.6430(2) 0.4599(2) 0.6461(2) 0.0343(7) Uani 1 1 d . . . H46A H 0.6319 0.4231 0.7153 0.041 Uiso 1 1 calc R . . C47 C 0.6327(2) 0.4102(2) 0.5868(2) 0.0384(7) Uani 1 1 d . . . H47A H 0.6141 0.3409 0.6168 0.046 Uiso 1 1 calc R . . C48 C 0.6495(2) 0.4619(3) 0.4846(2) 0.0404(7) Uani 1 1 d . . . H48A H 0.6422 0.4282 0.4453 0.049 Uiso 1 1 calc R . . C49 C 0.6773(2) 0.5644(2) 0.4407(2) 0.0378(7) Uani 1 1 d . . . H49A H 0.6909 0.5992 0.3712 0.045 Uiso 1 1 calc R . . C50 C 0.6852(2) 0.6156(2) 0.50021(18) 0.0292(6) Uani 1 1 d . . . H50A H 0.7013 0.6862 0.4699 0.035 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 Mg1 0.0285(4) 0.0217(5) 0.0225(5) -0.0087(4) -0.0059(4) -0.0061(4) O1 0.0268(9) 0.0268(10) 0.0207(10) -0.0041(8) -0.0040(7) -0.0105(8) O2 0.0292(9) 0.0250(10) 0.0197(9) -0.0082(8) -0.0045(7) -0.0084(8) O3 0.0262(9) 0.0190(9) 0.0238(9) -0.0097(8) -0.0041(7) -0.0053(7) C1 0.0217(13) 0.0206(14) 0.0206(14) -0.0042(11) -0.0040(11) -0.0051(11) C2 0.0233(13) 0.0192(14) 0.0239(15) -0.0054(12) -0.0067(11) -0.0037(11) C3 0.0260(13) 0.0259(15) 0.0240(15) -0.0089(12) -0.0084(11) -0.0014(12) C4 0.0220(13) 0.0228(15) 0.0243(15) -0.0058(12) -0.0036(11) -0.0046(11) C5 0.0279(14) 0.0254(15) 0.0283(15) -0.0085(12) -0.0069(11) -0.0092(12) C6 0.0255(13) 0.0197(14) 0.0239(15) -0.0064(12) -0.0056(11) -0.0062(11) C7 0.0368(15) 0.0247(16) 0.0232(15) -0.0056(13) -0.0031(12) -0.0144(12) C8 0.0310(14) 0.0347(16) 0.0234(14) -0.0127(13) -0.0047(11) -0.0154(13) C9 0.0297(14) 0.0265(16) 0.0211(14) -0.0089(12) -0.0071(11) -0.0106(12) C10 0.0388(15) 0.0261(16) 0.0240(15) -0.0083(12) -0.0057(12) -0.0160(13) C11 0.0364(15) 0.0234(15) 0.0267(15) -0.0098(12) -0.0100(12) -0.0070(13) C12 0.0263(13) 0.0250(15) 0.0259(15) -0.0119(12) -0.0051(11) -0.0032(12) C13 0.0235(13) 0.0221(15) 0.0216(14) -0.0087(12) -0.0030(10) -0.0064(11) C14 0.0285(14) 0.0197(14) 0.0198(14) -0.0073(11) -0.0076(11) -0.0059(12) C15 0.0272(13) 0.0312(16) 0.0249(15) -0.0070(12) -0.0087(11) -0.0112(12) C16 0.0321(15) 0.0353(17) 0.0439(18) -0.0096(14) -0.0149(13) -0.0096(13) C17 0.0461(16) 0.0417(18) 0.0335(17) -0.0068(14) -0.0156(13) -0.0195(14) C18 0.0320(15) 0.0319(16) 0.0217(14) -0.0120(12) -0.0062(11) -0.0111(13) C19 0.0335(15) 0.0361(18) 0.0374(17) -0.0146(14) -0.0077(13) -0.0118(13) C20 0.0465(17) 0.0385(19) 0.0361(17) -0.0143(15) -0.0021(14) -0.0236(15) C21 0.0584(19) 0.0284(17) 0.0305(17) -0.0053(13) -0.0105(14) -0.0186(16) C22 0.0443(16) 0.0316(17) 0.0345(17) -0.0106(14) -0.0169(13) -0.0085(14) C23 0.0365(15) 0.0297(17) 0.0302(16) -0.0073(13) -0.0108(12) -0.0138(13) C24 0.0273(14) 0.0280(16) 0.0218(14) -0.0048(12) -0.0022(11) -0.0066(12) C25 0.0332(15) 0.068(2) 0.0250(16) -0.0141(15) -0.0011(12) -0.0183(15) C26 0.0495(18) 0.0338(18) 0.0421(19) -0.0005(15) 0.0040(15) -0.0111(15) C27 0.0332(15) 0.0365(17) 0.0204(14) -0.0127(13) 0.0009(11) -0.0167(13) C28 0.0302(15) 0.0397(19) 0.0357(17) -0.0084(15) -0.0077(12) -0.0110(14) C29 0.0391(18) 0.055(2) 0.0414(19) -0.0114(16) -0.0108(14) -0.0035(16) C30 0.0336(18) 0.083(3) 0.055(2) -0.031(2) -0.0131(16) -0.0140(19) C31 0.0407(19) 0.083(3) 0.066(2) -0.036(2) 0.0013(16) -0.038(2) C32 0.0452(18) 0.0428(19) 0.0423(18) -0.0193(15) 0.0002(14) -0.0221(15) C33 0.0444(16) 0.0202(15) 0.0354(16) -0.0097(13) -0.0138(13) -0.0052(13) C34 0.083(2) 0.0221(17) 0.0406(19) -0.0083(14) -0.0065(17) -0.0168(16) C35 0.068(2) 0.0348(19) 0.070(2) -0.0243(17) -0.0408(18) 0.0067(16) C36 0.0363(15) 0.0197(15) 0.0359(17) -0.0116(13) -0.0060(13) -0.0096(13) C37 0.0367(16) 0.0288(16) 0.0357(17) -0.0151(14) -0.0044(13) -0.0089(13) C38 0.0480(18) 0.0379(18) 0.0460(19) -0.0110(15) -0.0170(15) -0.0185(15) C39 0.060(2) 0.057(2) 0.0397(19) -0.0251(17) -0.0036(16) -0.0280(18) C40 0.0475(19) 0.059(2) 0.058(2) -0.0404(19) -0.0001(16) -0.0106(17) C41 0.0395(16) 0.0388(19) 0.057(2) -0.0260(16) -0.0097(14) -0.0051(14) C42 0.0255(13) 0.0229(15) 0.0198(14) -0.0085(12) -0.0007(10) -0.0070(11) C43 0.0352(15) 0.0344(17) 0.0264(15) -0.0079(13) -0.0040(12) -0.0145(13) C44 0.0286(14) 0.0359(17) 0.0345(16) -0.0149(13) 0.0014(12) -0.0109(13) C45 0.0208(13) 0.0240(15) 0.0296(15) -0.0102(12) -0.0041(11) -0.0058(11) C46 0.0381(16) 0.0334(17) 0.0321(16) -0.0092(14) -0.0054(12) -0.0156(14) C47 0.0360(16) 0.0342(17) 0.051(2) -0.0191(15) -0.0054(14) -0.0151(14) C48 0.0379(16) 0.049(2) 0.050(2) -0.0273(17) -0.0103(14) -0.0151(15) C49 0.0361(16) 0.049(2) 0.0350(17) -0.0183(15) -0.0095(13) -0.0134(15) C50 0.0321(14) 0.0284(16) 0.0301(16) -0.0096(13) -0.0086(12) -0.0106(12) _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 Mg1 O1 1.8901(18) . ? Mg1 O3 1.9428(19) 2_766 ? Mg1 O3 2.0037(17) . ? Mg1 O2 2.0396(17) . ? Mg1 C1 2.805(3) . ? Mg1 C14 2.838(3) . ? Mg1 Mg1 2.936(2) 2_766 ? O1 C1 1.343(3) . ? O2 C7 1.457(3) . ? O2 C8 1.459(3) . ? O3 C14 1.363(3) . ? O3 Mg1 1.9428(19) 2_766 ? C1 C2 1.408(3) . ? C1 C6 1.415(3) . ? C2 C3 1.398(3) . ? C2 C15 1.535(3) . ? C3 C4 1.395(3) . ? C3 H3A 0.9300 . ? C4 C5 1.385(3) . ? C4 C24 1.532(3) . ? C5 C6 1.386(3) . ? C5 H5A 0.9300 . ? C6 C7 1.491(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.503(3) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.394(3) . ? C9 C14 1.398(3) . ? C10 C11 1.386(3) . ? C10 H10A 0.9300 . ? C11 C12 1.401(3) . ? C11 C33 1.541(3) . ? C12 C13 1.392(3) . ? C12 H12A 0.9300 . ? C13 C14 1.411(3) . ? C13 C42 1.534(3) . ? C15 C18 1.530(3) . ? C15 C16 1.538(3) . ? C15 C17 1.540(3) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C23 1.389(3) . ? C18 C19 1.390(3) . ? C19 C20 1.387(4) . ? C19 H19A 0.9300 . ? C20 C21 1.373(3) . ? C20 H20A 0.9300 . ? C21 C22 1.380(3) . ? C21 H21A 0.9300 . ? C22 C23 1.382(3) . ? C22 H22A 0.9300 . ? C23 H23A 0.9300 . ? C24 C27 1.528(3) . ? C24 C25 1.533(3) . ? C24 C26 1.540(3) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C28 1.380(3) . ? C27 C32 1.398(3) . ? C28 C29 1.381(3) . ? C28 H28A 0.9300 . ? C29 C30 1.372(4) . ? C29 H29A 0.9300 . ? C30 C31 1.363(4) . ? C30 H30A 0.9300 . ? C31 C32 1.397(4) . ? C31 H31A 0.9300 . ? C32 H32A 0.9300 . ? C33 C35 1.534(3) . ? C33 C34 1.535(3) . ? C33 C36 1.542(3) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 C41 1.387(3) . ? C36 C37 1.392(3) . ? C37 C38 1.388(3) . ? C37 H37A 0.9300 . ? C38 C39 1.378(4) . ? C38 H38A 0.9300 . ? C39 C40 1.360(4) . ? C39 H39A 0.9300 . ? C40 C41 1.389(4) . ? C40 H40A 0.9300 . ? C41 H41A 0.9300 . ? C42 C45 1.539(3) . ? C42 C43 1.543(3) . ? C42 C44 1.544(3) . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 C50 1.385(3) . ? C45 C46 1.395(3) . ? C46 C47 1.384(3) . ? C46 H46A 0.9300 . ? C47 C48 1.369(4) . ? C47 H47A 0.9300 . ? C48 C49 1.376(4) . ? C48 H48A 0.9300 . ? C49 C50 1.387(3) . ? C49 H49A 0.9300 . ? C50 H50A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mg1 O3 135.51(8) . 2_766 ? O1 Mg1 O3 134.02(8) . . ? O3 Mg1 O3 83.88(8) 2_766 . ? O1 Mg1 O2 94.87(8) . . ? O3 Mg1 O2 109.09(7) 2_766 . ? O3 Mg1 O2 90.71(7) . . ? O1 Mg1 C1 24.64(6) . . ? O3 Mg1 C1 127.59(8) 2_766 . ? O3 Mg1 C1 148.31(7) . . ? O2 Mg1 C1 76.41(7) . . ? O1 Mg1 C14 113.52(8) . . ? O3 Mg1 C14 108.69(8) 2_766 . ? O3 Mg1 C14 26.14(6) . . ? O2 Mg1 C14 75.15(7) . . ? C1 Mg1 C14 122.51(7) . . ? O1 Mg1 Mg1 161.15(7) . 2_766 ? O3 Mg1 Mg1 42.74(6) 2_766 2_766 ? O3 Mg1 Mg1 41.15(5) . 2_766 ? O2 Mg1 Mg1 102.99(6) . 2_766 ? C1 Mg1 Mg1 169.87(6) . 2_766 ? C14 Mg1 Mg1 66.38(6) . 2_766 ? C1 O1 Mg1 119.41(13) . . ? C7 O2 C8 111.61(17) . . ? C7 O2 Mg1 112.90(13) . . ? C8 O2 Mg1 114.04(13) . . ? C14 O3 Mg1 145.45(14) . 2_766 ? C14 O3 Mg1 113.50(14) . . ? Mg1 O3 Mg1 96.12(8) 2_766 . ? O1 C1 C2 122.1(2) . . ? O1 C1 C6 119.3(2) . . ? C2 C1 C6 118.7(2) . . ? O1 C1 Mg1 35.94(9) . . ? C2 C1 Mg1 142.27(17) . . ? C6 C1 Mg1 91.45(14) . . ? C3 C2 C1 118.3(2) . . ? C3 C2 C15 121.3(2) . . ? C1 C2 C15 120.3(2) . . ? C4 C3 C2 123.6(2) . . ? C4 C3 H3A 118.2 . . ? C2 C3 H3A 118.2 . . ? C5 C4 C3 116.7(2) . . ? C5 C4 C24 119.4(2) . . ? C3 C4 C24 123.9(2) . . ? C4 C5 C6 122.2(2) . . ? C4 C5 H5A 118.9 . . ? C6 C5 H5A 118.9 . . ? C5 C6 C1 120.3(2) . . ? C5 C6 C7 119.6(2) . . ? C1 C6 C7 119.8(2) . . ? O2 C7 C6 111.29(19) . . ? O2 C7 H7A 109.4 . . ? C6 C7 H7A 109.4 . . ? O2 C7 H7B 109.4 . . ? C6 C7 H7B 109.4 . . ? H7A C7 H7B 108.0 . . ? O2 C8 C9 111.11(17) . . ? O2 C8 H8A 109.4 . . ? C9 C8 H8A 109.4 . . ? O2 C8 H8B 109.4 . . ? C9 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? C10 C9 C14 120.1(2) . . ? C10 C9 C8 121.6(2) . . ? C14 C9 C8 118.3(2) . . ? C11 C10 C9 121.8(2) . . ? C11 C10 H10A 119.1 . . ? C9 C10 H10A 119.1 . . ? C10 C11 C12 116.5(2) . . ? C10 C11 C33 122.9(2) . . ? C12 C11 C33 120.6(2) . . ? C13 C12 C11 124.4(2) . . ? C13 C12 H12A 117.8 . . ? C11 C12 H12A 117.8 . . ? C12 C13 C14 117.0(2) . . ? C12 C13 C42 121.5(2) . . ? C14 C13 C42 121.4(2) . . ? O3 C14 C9 117.4(2) . . ? O3 C14 C13 122.2(2) . . ? C9 C14 C13 120.2(2) . . ? O3 C14 Mg1 40.36(10) . . ? C9 C14 Mg1 92.02(14) . . ? C13 C14 Mg1 132.96(16) . . ? C18 C15 C2 112.33(18) . . ? C18 C15 C16 112.1(2) . . ? C2 C15 C16 107.33(19) . . ? C18 C15 C17 105.6(2) . . ? C2 C15 C17 111.67(19) . . ? C16 C15 C17 107.85(19) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C23 C18 C19 116.9(2) . . ? C23 C18 C15 120.7(2) . . ? C19 C18 C15 122.0(2) . . ? C20 C19 C18 121.4(2) . . ? C20 C19 H19A 119.3 . . ? C18 C19 H19A 119.3 . . ? C21 C20 C19 120.3(3) . . ? C21 C20 H20A 119.8 . . ? C19 C20 H20A 119.8 . . ? C20 C21 C22 119.4(3) . . ? C20 C21 H21A 120.3 . . ? C22 C21 H21A 120.3 . . ? C21 C22 C23 119.9(2) . . ? C21 C22 H22A 120.1 . . ? C23 C22 H22A 120.1 . . ? C22 C23 C18 122.0(2) . . ? C22 C23 H23A 119.0 . . ? C18 C23 H23A 119.0 . . ? C27 C24 C4 108.8(2) . . ? C27 C24 C25 107.7(2) . . ? C4 C24 C25 112.5(2) . . ? C27 C24 C26 111.9(2) . . ? C4 C24 C26 107.9(2) . . ? C25 C24 C26 108.1(2) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C32 116.9(2) . . ? C28 C27 C24 120.3(2) . . ? C32 C27 C24 122.7(2) . . ? C27 C28 C29 122.2(3) . . ? C27 C28 H28A 118.9 . . ? C29 C28 H28A 118.9 . . ? C30 C29 C28 120.1(3) . . ? C30 C29 H29A 120.0 . . ? C28 C29 H29A 120.0 . . ? C31 C30 C29 119.5(3) . . ? C31 C30 H30A 120.2 . . ? C29 C30 H30A 120.2 . . ? C30 C31 C32 120.6(3) . . ? C30 C31 H31A 119.7 . . ? C32 C31 H31A 119.7 . . ? C31 C32 C27 120.7(3) . . ? C31 C32 H32A 119.7 . . ? C27 C32 H32A 119.7 . . ? C35 C33 C34 107.4(2) . . ? C35 C33 C11 109.2(2) . . ? C34 C33 C11 111.1(2) . . ? C35 C33 C36 111.7(2) . . ? C34 C33 C36 107.0(2) . . ? C11 C33 C36 110.3(2) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C41 C36 C37 117.5(2) . . ? C41 C36 C33 123.2(2) . . ? C37 C36 C33 119.3(2) . . ? C38 C37 C36 121.3(2) . . ? C38 C37 H37A 119.4 . . ? C36 C37 H37A 119.4 . . ? C39 C38 C37 120.0(3) . . ? C39 C38 H38A 120.0 . . ? C37 C38 H38A 120.0 . . ? C40 C39 C38 119.5(3) . . ? C40 C39 H39A 120.2 . . ? C38 C39 H39A 120.2 . . ? C39 C40 C41 120.9(3) . . ? C39 C40 H40A 119.5 . . ? C41 C40 H40A 119.5 . . ? C36 C41 C40 120.9(3) . . ? C36 C41 H41A 119.6 . . ? C40 C41 H41A 119.6 . . ? C13 C42 C45 112.80(19) . . ? C13 C42 C43 107.42(18) . . ? C45 C42 C43 111.55(19) . . ? C13 C42 C44 112.2(2) . . ? C45 C42 C44 106.00(19) . . ? C43 C42 C44 106.74(19) . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C50 C45 C46 117.2(2) . . ? C50 C45 C42 122.1(2) . . ? C46 C45 C42 120.4(2) . . ? C47 C46 C45 121.0(3) . . ? C47 C46 H46A 119.5 . . ? C45 C46 H46A 119.5 . . ? C48 C47 C46 120.8(3) . . ? C48 C47 H47A 119.6 . . ? C46 C47 H47A 119.6 . . ? C47 C48 C49 119.3(3) . . ? C47 C48 H48A 120.3 . . ? C49 C48 H48A 120.3 . . ? C48 C49 C50 120.0(3) . . ? C48 C49 H49A 120.0 . . ? C50 C49 H49A 120.0 . . ? C45 C50 C49 121.7(2) . . ? C45 C50 H50A 119.2 . . ? C49 C50 H50A 119.2 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.209 _refine_diff_density_min -0.210 _refine_diff_density_rms 0.049