#------------------------------------------------------------------------------ #$Date: 2020-08-11 04:02:57 +0300 (Tue, 11 Aug 2020) $ #$Revision: 255226 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/88/1558819.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1558819 loop_ _publ_author_name 'Zhou, Zheng' 'Wei, Zheng' 'Schaub, Tobias A.' 'Jasti, Ramesh' 'Petrukhina, Marina A.' _publ_section_title ; Structural deformation and host--guest properties of doubly-reduced cycloparaphenylenes, [n]CPPs2− (n = 6, 8, 10, and 12) ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D0SC03072D _journal_year 2020 _chemical_formula_moiety 'C48 H32, 2(C16 H32 K O7) ' _chemical_formula_sum 'C80 H96 K2 O14' _chemical_formula_weight 1359.76 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_date 2019-04-09 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2020-05-23 deposited with the CCDC. 2020-07-27 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 100.403(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 10.0128(19) _cell_length_b 19.991(4) _cell_length_c 18.021(3) _cell_measurement_reflns_used 9905 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 26.40 _cell_measurement_theta_min 2.90 _cell_volume 3547.9(11) _computing_cell_refinement 'SAINT V8.38A (bruker, 2016)' _computing_data_reduction 'SAINT V8.38A (bruker, 2016)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker D8 Venture PHOTON 100 CMOS' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0809 _diffrn_reflns_av_unetI/netI 0.0408 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 78253 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.425 _diffrn_reflns_theta_min 2.904 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.199 _exptl_absorpt_correction_T_max 0.6629 _exptl_absorpt_correction_T_min 0.6029 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0808 before and 0.0684 after correction. The Ratio of minimum to maximum transmission is 0.9095. The \l/2 correction factor is Not present.' _exptl_crystal_colour 'dark green' _exptl_crystal_colour_modifier dark _exptl_crystal_colour_primary green _exptl_crystal_density_diffrn 1.273 _exptl_crystal_description block _exptl_crystal_F_000 1452 _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _refine_diff_density_max 0.356 _refine_diff_density_min -0.343 _refine_diff_density_rms 0.052 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 479 _refine_ls_number_reflns 7296 _refine_ls_number_restraints 220 _refine_ls_restrained_S_all 1.067 _refine_ls_R_factor_all 0.0891 _refine_ls_R_factor_gt 0.0541 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0285P)^2^+3.0208P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0971 _refine_ls_wR_factor_ref 0.1099 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5216 _reflns_number_total 7296 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0sc03072d2.cif _cod_data_source_block 1 _cod_original_cell_volume 3548.0(12) _cod_database_code 1558819 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.988 _shelx_estimated_absorpt_t_min 0.969 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups 2. Restrained distances O7-C37 \\sim O7A-C37A with sigma of 0.02 O7-C40 \\sim O7A-C40A with sigma of 0.02 C37-C38 \\sim C37A-C38A with sigma of 0.02 C38-C39 \\sim C38A-C39A with sigma of 0.02 C39-C40 \\sim C39A-C40A with sigma of 0.02 O7-C38 \\sim O7A-C38A with sigma of 0.04 O7-C39 \\sim O7A-C39A with sigma of 0.04 C37-C39 \\sim C37A-C39A with sigma of 0.04 C37-C40 \\sim C37A-C40A with sigma of 0.04 C38-C40 \\sim C38A-C40A with sigma of 0.04 3. Uiso/Uaniso restraints and constraints O7 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim O7A \\sim C37A \\sim C38A \\sim C39A \\sim C40A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 4. Rigid body (RIGU) restrains O7, C37, C38, C39, C40, O7A, C37A, C38A, C39A, C40A with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 5. Others Sof(O7A)=Sof(C37A)=Sof(H37C)=Sof(H37D)=Sof(C38A)=Sof(H38C)=Sof(H38D)= Sof(C39A)=Sof(H39C)=Sof(H39D)=Sof(C40A)=Sof(H40C)=Sof(H40D)=1-FVAR(1) Sof(O7)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(C39)= Sof(H39A)=Sof(H39B)=Sof(C40)=Sof(H40A)=Sof(H40B)=FVAR(1) 6.a Ternary CH refined with riding coordinates: C17(H17), C18(H18) 6.b Secondary CH2 refined with riding coordinates: C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A, H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C37A(H37C,H37D), C38A(H38C,H38D), C39A(H39C, H39D), C40A(H40C,H40D) 6.c Aromatic/amide H refined with riding coordinates: C1(H1), C2(H2), C4(H4), C5(H5), C8(H8), C9(H9), C11(H11), C12(H12), C14(H14), C15(H15), C20(H20), C21(H21), C23(H23), C24(H24) ; _shelx_res_file ; TITL final_a.res in P2(1)/c final_a.res created by SHELXL-2018/3 at 11:06:26 on 09-Apr-2019 CELL 0.71073 10.0128 19.9913 18.0214 90 100.403 90 ZERR 2 0.0019 0.0038 0.0034 0 0.002 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H K O UNIT 160 192 4 28 SADI O7 C37 O7A C37A SADI O7 C40 O7A C40A SADI C37 C38 C37A C38A SADI C38 C39 C38A C39A SADI C39 C40 C39A C40A SADI 0.04 O7 C38 O7A C38A SADI 0.04 O7 C39 O7A C39A SADI 0.04 C37 C39 C37A C39A SADI 0.04 C37 C40 C37A C40A SADI 0.04 C38 C40 C38A C40A SIMU 0.01 0.02 2 O7 C37 C38 C39 C40 O7A C37A C38A C39A C40A RIGU O7 C37 C38 C39 C40 O7A C37A C38A C39A C40A L.S. 20 PLAN 20 SIZE 0.06 0.12 0.16 TEMP -173(2) LIST 4 BOND $H fmap 2 acta OMIT -1 0 2 OMIT 0 1 3 REM REM REM WGHT 0.028500 3.020800 FVAR 0.27508 0.54760 K1 3 0.355283 0.507257 0.716464 11.00000 0.02920 0.01708 = 0.01883 0.00055 0.00493 0.00081 O1 4 0.532875 0.515301 0.858158 11.00000 0.03277 0.03061 = 0.02488 0.00281 0.00186 0.00075 O2 4 0.397757 0.628812 0.788628 11.00000 0.02536 0.02133 = 0.02437 -0.00145 0.00256 -0.00423 O3 4 0.272814 0.624439 0.633837 11.00000 0.02432 0.01947 = 0.02625 -0.00116 0.00163 0.00201 O4 4 0.177542 0.499631 0.572920 11.00000 0.02834 0.02105 = 0.02287 -0.00048 0.00439 -0.00048 O5 4 0.294301 0.383067 0.646092 11.00000 0.02883 0.01898 = 0.03077 0.00046 0.00697 -0.00284 O6 4 0.416740 0.392920 0.800638 11.00000 0.02907 0.02155 = 0.02859 0.00387 0.00496 0.00498 PART 1 O7 4 0.190507 0.507740 0.821306 21.00000 0.03845 0.01537 = 0.04808 -0.00748 0.02414 -0.00496 PART 0 C1 1 0.864063 0.200098 0.485080 11.00000 0.02611 0.01482 = 0.03471 0.00101 -0.00687 -0.00427 AFIX 43 H1 2 0.770619 0.193054 0.465207 11.00000 -1.20000 AFIX 0 C2 1 0.956204 0.194673 0.438356 11.00000 0.03817 0.01496 = 0.02847 -0.00643 -0.01051 0.00437 AFIX 43 H2 2 0.924978 0.183624 0.386876 11.00000 -1.20000 AFIX 0 C3 1 1.098446 0.205027 0.464041 11.00000 0.02760 0.01456 = 0.03314 -0.00817 -0.00606 0.00711 C4 1 1.137565 0.200691 0.543782 11.00000 0.02685 0.01547 = 0.03420 0.00104 -0.01073 0.00297 AFIX 43 H4 2 1.230524 0.193970 0.565054 11.00000 -1.20000 AFIX 0 C5 1 1.044962 0.205939 0.590504 11.00000 0.03159 0.01880 = 0.02822 0.00918 -0.00800 -0.00417 AFIX 43 H5 2 1.075708 0.202740 0.643428 11.00000 -1.20000 AFIX 0 C6 1 0.903905 0.216037 0.562901 11.00000 0.03153 0.01671 = 0.02888 0.01033 -0.00724 -0.00800 C7 1 0.819264 0.254058 0.603768 11.00000 0.02808 0.02893 = 0.02336 0.01131 0.00047 -0.01037 C8 1 0.873630 0.286049 0.672782 11.00000 0.02719 0.04044 = 0.02301 0.01348 -0.00326 -0.00757 AFIX 43 H8 2 0.953613 0.268156 0.702589 11.00000 -1.20000 AFIX 0 C9 1 0.816265 0.341425 0.698381 11.00000 0.02827 0.04750 = 0.01860 0.00518 0.00139 -0.00892 AFIX 43 H9 2 0.858100 0.360755 0.744962 11.00000 -1.20000 AFIX 0 C10 1 0.696289 0.371074 0.657765 11.00000 0.02115 0.04443 = 0.01938 0.00621 0.00505 -0.00782 C11 1 0.627418 0.331044 0.597428 11.00000 0.01897 0.04853 = 0.02291 0.00714 0.00195 -0.00850 AFIX 43 H11 2 0.537883 0.343107 0.574098 11.00000 -1.20000 AFIX 0 C12 1 0.686018 0.275703 0.571905 11.00000 0.02317 0.03852 = 0.02234 0.00571 -0.00212 -0.01123 AFIX 43 H12 2 0.635648 0.250840 0.531348 11.00000 -1.20000 AFIX 0 C13 1 0.663573 0.440709 0.667765 11.00000 0.02080 0.04877 = 0.01948 0.00127 0.00695 -0.00434 C14 1 0.734422 0.480681 0.727076 11.00000 0.02897 0.05416 = 0.01711 0.00217 0.00230 0.00000 AFIX 43 H14 2 0.785126 0.459081 0.770071 11.00000 -1.20000 AFIX 0 C15 1 0.732743 0.548953 0.724916 11.00000 0.02989 0.05181 = 0.01871 -0.00619 0.00314 0.00180 AFIX 43 H15 2 0.782011 0.572920 0.766563 11.00000 -1.20000 AFIX 0 C16 1 0.660787 0.585368 0.663326 11.00000 0.01955 0.05007 = 0.01790 -0.00479 0.00580 0.00566 C17 1 0.572361 0.545780 0.610192 11.00000 0.02078 0.05087 = 0.01726 0.00058 0.00718 0.00428 AFIX 13 H17 2 0.535397 0.567049 0.560500 11.00000 -1.20000 AFIX 0 C18 1 0.573658 0.477210 0.612422 11.00000 0.01708 0.05158 = 0.02087 -0.00211 0.00569 -0.00132 AFIX 13 H18 2 0.539808 0.453619 0.563726 11.00000 -1.20000 AFIX 0 C19 1 0.692101 0.654058 0.647790 11.00000 0.02318 0.04667 = 0.01984 -0.00788 0.00560 0.00882 C20 1 0.814159 0.684985 0.684708 11.00000 0.02888 0.04392 = 0.01875 -0.01022 -0.00053 0.00927 AFIX 43 H20 2 0.856996 0.668469 0.732540 11.00000 -1.20000 AFIX 0 C21 1 0.871885 0.737533 0.653847 11.00000 0.02805 0.03692 = 0.02428 -0.01398 -0.00162 0.00601 AFIX 43 H21 2 0.952606 0.756791 0.681353 11.00000 -1.20000 AFIX 0 C22 1 0.815716 0.764366 0.582275 11.00000 0.02862 0.02544 = 0.02523 -0.01231 -0.00219 0.01052 C23 1 0.680123 0.743134 0.554040 11.00000 0.02553 0.03721 = 0.02378 -0.00764 -0.00196 0.01331 AFIX 43 H23 2 0.628596 0.766013 0.512239 11.00000 -1.20000 AFIX 0 C24 1 0.622170 0.690870 0.585335 11.00000 0.02170 0.04287 = 0.02626 -0.00890 -0.00081 0.00956 AFIX 43 H24 2 0.531455 0.678670 0.564476 11.00000 -1.20000 AFIX 0 C25 1 0.518330 0.575731 0.897708 11.00000 0.03518 0.04216 = 0.02590 -0.00845 -0.00142 -0.00079 AFIX 23 H25A 2 0.595202 0.580682 0.940391 11.00000 -1.20000 H25B 2 0.433151 0.574433 0.918300 11.00000 -1.20000 AFIX 0 C26 1 0.515413 0.633747 0.845136 11.00000 0.02467 0.03410 = 0.03096 -0.01169 0.00122 -0.00387 AFIX 23 H26A 2 0.513984 0.676202 0.873261 11.00000 -1.20000 H26B 2 0.597599 0.633360 0.821751 11.00000 -1.20000 AFIX 0 C27 1 0.381233 0.686071 0.740779 11.00000 0.03081 0.01580 = 0.03322 -0.00196 0.01053 -0.00217 AFIX 23 H27A 2 0.461072 0.690932 0.715847 11.00000 -1.20000 H27B 2 0.374275 0.726791 0.771112 11.00000 -1.20000 AFIX 0 C28 1 0.256109 0.678365 0.682845 11.00000 0.03493 0.01666 = 0.03117 0.00045 0.00844 0.00347 AFIX 23 H28A 2 0.177533 0.669472 0.707774 11.00000 -1.20000 H28B 2 0.238105 0.720219 0.653372 11.00000 -1.20000 AFIX 0 C29 1 0.160418 0.618053 0.573351 11.00000 0.02713 0.02430 = 0.03013 0.00542 -0.00130 0.00381 AFIX 23 H29A 2 0.152574 0.658584 0.541292 11.00000 -1.20000 H29B 2 0.075321 0.612995 0.593515 11.00000 -1.20000 AFIX 0 C30 1 0.182546 0.557689 0.527617 11.00000 0.02541 0.02768 = 0.02131 0.00606 0.00024 0.00175 AFIX 23 H30A 2 0.111239 0.555219 0.481839 11.00000 -1.20000 H30B 2 0.271950 0.560657 0.511687 11.00000 -1.20000 AFIX 0 C31 1 0.194437 0.439509 0.533490 11.00000 0.02462 0.02999 = 0.02483 -0.00789 0.00231 -0.00248 AFIX 23 H31A 2 0.284666 0.439119 0.518326 11.00000 -1.20000 H31B 2 0.124026 0.436413 0.487368 11.00000 -1.20000 AFIX 0 C32 1 0.182359 0.381462 0.584339 11.00000 0.02651 0.02401 = 0.03292 -0.00746 0.00355 -0.00563 AFIX 23 H32A 2 0.095772 0.384249 0.603389 11.00000 -1.20000 H32B 2 0.183110 0.339010 0.556131 11.00000 -1.20000 AFIX 0 C33 1 0.285768 0.331312 0.699517 11.00000 0.04012 0.01612 = 0.03753 0.00085 0.01730 -0.00399 AFIX 23 H33A 2 0.277203 0.287377 0.673746 11.00000 -1.20000 H33B 2 0.204323 0.338188 0.722630 11.00000 -1.20000 AFIX 0 C34 1 0.409914 0.332012 0.759274 11.00000 0.03743 0.02017 = 0.03818 0.00647 0.01697 0.00795 AFIX 23 H34A 2 0.407658 0.293709 0.793845 11.00000 -1.20000 H34B 2 0.491606 0.327471 0.735855 11.00000 -1.20000 AFIX 0 C35 1 0.532556 0.395991 0.858655 11.00000 0.03451 0.03414 = 0.03683 0.01479 -0.00027 0.00692 AFIX 23 H35A 2 0.616009 0.396394 0.836404 11.00000 -1.20000 H35B 2 0.535489 0.356207 0.891622 11.00000 -1.20000 AFIX 0 C36 1 0.525586 0.458267 0.903964 11.00000 0.04174 0.04745 = 0.02452 0.01047 -0.00262 0.00259 AFIX 23 H36A 2 0.439502 0.458986 0.923685 11.00000 -1.20000 H36B 2 0.601778 0.458908 0.947437 11.00000 -1.20000 AFIX 0 PART 1 C37 1 0.120536 0.449066 0.839155 21.00000 0.03909 0.02241 = 0.05193 -0.00507 0.02445 -0.00340 AFIX 23 H37A 2 0.184599 0.411295 0.851633 21.00000 -1.20000 H37B 2 0.049348 0.435967 0.796050 21.00000 -1.20000 AFIX 0 C38 1 0.057601 0.467981 0.907013 21.00000 0.04717 0.02570 = 0.05015 0.00251 0.02336 -0.00382 AFIX 23 H38A 2 -0.028411 0.443419 0.906515 21.00000 -1.20000 H38B 2 0.120566 0.457897 0.954667 21.00000 -1.20000 AFIX 0 C39 1 0.033056 0.539399 0.899117 21.00000 0.02401 0.02777 = 0.04030 0.00326 0.01264 0.00613 AFIX 23 H39A 2 0.064115 0.562418 0.947815 21.00000 -1.20000 H39B 2 -0.064999 0.548409 0.882449 21.00000 -1.20000 AFIX 0 C40 1 0.113659 0.563743 0.839900 21.00000 0.03740 0.02114 = 0.04931 0.00253 0.02318 0.00561 AFIX 23 H40A 2 0.051355 0.579997 0.794490 21.00000 -1.20000 H40B 2 0.175045 0.600773 0.860383 21.00000 -1.20000 AFIX 0 PART 0 PART 2 O7A 4 0.174965 0.497337 0.813719 -21.00000 0.04636 0.02026 = 0.04666 0.00285 0.02499 0.00083 C37A 1 0.133600 0.441854 0.854569 -21.00000 0.03754 0.01975 = 0.04582 0.00885 0.01612 -0.00089 AFIX 23 H37C 2 0.205762 0.407419 0.863706 -21.00000 -1.20000 H37D 2 0.049736 0.421275 0.826246 -21.00000 -1.20000 AFIX 0 C38A 1 0.108743 0.470884 0.927889 -21.00000 0.03486 0.02766 = 0.04015 0.00554 0.01130 0.00456 AFIX 23 H38C 2 0.030842 0.448452 0.944287 -21.00000 -1.20000 H38D 2 0.189968 0.465428 0.967833 -21.00000 -1.20000 AFIX 0 C39A 1 0.079938 0.540702 0.913168 -21.00000 0.05206 0.02810 = 0.05337 -0.00098 0.02725 0.00060 AFIX 23 H39C 2 0.139182 0.568710 0.950804 -21.00000 -1.20000 H39D 2 -0.015885 0.550544 0.916068 -21.00000 -1.20000 AFIX 0 C40A 1 0.106925 0.555484 0.833483 -21.00000 0.04066 0.02086 = 0.05233 0.00552 0.01908 0.00112 AFIX 23 H40C 2 0.020711 0.562689 0.797737 -21.00000 -1.20000 H40D 2 0.164769 0.595655 0.833559 -21.00000 -1.20000 AFIX 0 HKLF 4 REM final_a.res in P2(1)/c REM wR2 = 0.1099, GooF = S = 1.077, Restrained GooF = 1.067 for all data REM R1 = 0.0541 for 5216 Fo > 4sig(Fo) and 0.0891 for all 7296 data REM 479 parameters refined using 220 restraints END WGHT 0.0285 3.0211 REM Highest difference peak 0.356, deepest hole -0.343, 1-sigma level 0.052 Q1 1 0.4975 0.4505 0.5850 11.00000 0.05 0.36 Q2 1 0.4782 0.5630 0.5716 11.00000 0.05 0.27 Q3 1 0.6518 0.2758 0.5252 11.00000 0.05 0.22 Q4 1 0.0187 0.5167 0.7166 11.00000 0.05 0.20 Q5 1 0.5946 0.4513 0.6590 11.00000 0.05 0.19 Q6 1 0.1455 0.5350 0.9451 11.00000 0.05 0.19 Q7 1 0.6436 0.4035 0.6792 11.00000 0.05 0.19 Q8 1 0.0869 0.5020 0.5947 11.00000 0.05 0.19 Q9 1 0.3146 0.5059 0.8242 11.00000 0.05 0.19 Q10 1 0.7644 0.7375 0.5612 11.00000 0.05 0.19 Q11 1 0.9934 0.2827 0.6995 11.00000 0.05 0.19 Q12 1 0.0498 0.4275 0.9549 11.00000 0.05 0.18 Q13 1 0.8795 0.6320 0.7319 11.00000 0.05 0.18 Q14 1 0.1095 0.5186 0.7964 11.00000 0.05 0.18 Q15 1 0.2620 0.4422 0.4956 11.00000 0.05 0.18 Q16 1 0.3644 0.5004 0.7675 11.00000 0.05 0.18 Q17 1 0.7444 0.2548 0.5992 11.00000 0.05 0.18 Q18 1 0.3062 0.4729 0.4773 11.00000 0.05 0.18 Q19 1 0.0564 0.4743 0.7799 11.00000 0.05 0.18 Q20 1 -0.0534 0.4712 0.7023 11.00000 0.05 0.18 ; _shelx_res_checksum 71634 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group K1 K 0.35528(5) 0.50726(2) 0.71646(3) 0.02163(12) Uani 1 1 d . . . . . O1 O 0.53287(16) 0.51530(8) 0.85816(9) 0.0298(4) Uani 1 1 d . . . . . O2 O 0.39776(15) 0.62881(7) 0.78863(8) 0.0239(3) Uani 1 1 d . . . . . O3 O 0.27281(14) 0.62444(7) 0.63384(8) 0.0237(3) Uani 1 1 d . . . . . O4 O 0.17754(15) 0.49963(7) 0.57292(8) 0.0241(3) Uani 1 1 d . . . . . O5 O 0.29430(15) 0.38307(7) 0.64609(9) 0.0260(4) Uani 1 1 d . . . . . O6 O 0.41674(15) 0.39292(7) 0.80064(9) 0.0264(4) Uani 1 1 d . . . . . O7 O 0.1905(13) 0.5077(6) 0.8213(7) 0.0319(15) Uani 0.548(15) 1 d D U P A 1 C1 C 0.8641(2) 0.20010(10) 0.48508(13) 0.0268(5) Uani 1 1 d . . . . . H1 H 0.770619 0.193054 0.465207 0.032 Uiso 1 1 calc R . . . . C2 C 0.9562(2) 0.19467(11) 0.43836(13) 0.0293(6) Uani 1 1 d . . . . . H2 H 0.924978 0.183624 0.386876 0.035 Uiso 1 1 calc R . . . . C3 C 1.0984(2) 0.20503(10) 0.46404(13) 0.0265(5) Uani 1 1 d . . . . . C4 C 1.1376(2) 0.20069(11) 0.54378(13) 0.0275(5) Uani 1 1 d . . . . . H4 H 1.230524 0.193970 0.565054 0.033 Uiso 1 1 calc R . . . . C5 C 1.0450(2) 0.20594(11) 0.59050(13) 0.0279(5) Uani 1 1 d . . . . . H5 H 1.075708 0.202740 0.643428 0.033 Uiso 1 1 calc R . . . . C6 C 0.9039(2) 0.21604(11) 0.56290(13) 0.0273(5) Uani 1 1 d . . . . . C7 C 0.8193(2) 0.25406(12) 0.60377(13) 0.0273(5) Uani 1 1 d . . . . . C8 C 0.8736(2) 0.28605(13) 0.67278(13) 0.0312(6) Uani 1 1 d . . . . . H8 H 0.953613 0.268156 0.702589 0.037 Uiso 1 1 calc R . . . . C9 C 0.8163(2) 0.34142(13) 0.69838(13) 0.0318(6) Uani 1 1 d . . . . . H9 H 0.858100 0.360755 0.744962 0.038 Uiso 1 1 calc R . . . . C10 C 0.6963(2) 0.37107(12) 0.65776(12) 0.0281(5) Uani 1 1 d . . . . . C11 C 0.6274(2) 0.33104(13) 0.59743(13) 0.0304(6) Uani 1 1 d . . . . . H11 H 0.537883 0.343107 0.574098 0.036 Uiso 1 1 calc R . . . . C12 C 0.6860(2) 0.27570(12) 0.57191(13) 0.0288(5) Uani 1 1 d . . . . . H12 H 0.635648 0.250840 0.531348 0.035 Uiso 1 1 calc R . . . . C13 C 0.6636(2) 0.44071(13) 0.66777(12) 0.0293(5) Uani 1 1 d . . . . . C14 C 0.7344(2) 0.48068(13) 0.72708(13) 0.0336(6) Uani 1 1 d . . . . . H14 H 0.785126 0.459081 0.770071 0.040 Uiso 1 1 calc R . . . . C15 C 0.7327(2) 0.54895(14) 0.72492(13) 0.0336(6) Uani 1 1 d . . . . . H15 H 0.782011 0.572920 0.766563 0.040 Uiso 1 1 calc R . . . . C16 C 0.6608(2) 0.58537(13) 0.66333(12) 0.0289(5) Uani 1 1 d . . . . . C17 C 0.5724(2) 0.54578(13) 0.61019(12) 0.0292(5) Uani 1 1 d . . . . . H17 H 0.535397 0.567049 0.560500 0.035 Uiso 1 1 calc R . . . . C18 C 0.5737(2) 0.47721(13) 0.61242(13) 0.0296(6) Uani 1 1 d . . . . . H18 H 0.539808 0.453619 0.563726 0.035 Uiso 1 1 calc R . . . . C19 C 0.6921(2) 0.65406(13) 0.64779(12) 0.0297(5) Uani 1 1 d . . . . . C20 C 0.8142(2) 0.68498(13) 0.68471(13) 0.0311(6) Uani 1 1 d . . . . . H20 H 0.856996 0.668469 0.732540 0.037 Uiso 1 1 calc R . . . . C21 C 0.8719(2) 0.73753(12) 0.65385(13) 0.0305(6) Uani 1 1 d . . . . . H21 H 0.952606 0.756791 0.681353 0.037 Uiso 1 1 calc R . . . . C22 C 0.8157(2) 0.76437(11) 0.58228(13) 0.0273(5) Uani 1 1 d . . . . . C23 C 0.6801(2) 0.74313(12) 0.55404(13) 0.0296(5) Uani 1 1 d . . . . . H23 H 0.628596 0.766013 0.512239 0.036 Uiso 1 1 calc R . . . . C24 C 0.6222(2) 0.69087(13) 0.58534(13) 0.0309(6) Uani 1 1 d . . . . . H24 H 0.531455 0.678670 0.564476 0.037 Uiso 1 1 calc R . . . . C25 C 0.5183(3) 0.57573(13) 0.89771(14) 0.0353(6) Uani 1 1 d . . . . . H25A H 0.595202 0.580682 0.940391 0.042 Uiso 1 1 calc R . . . . H25B H 0.433151 0.574433 0.918300 0.042 Uiso 1 1 calc R . . . . C26 C 0.5154(2) 0.63375(12) 0.84514(13) 0.0304(5) Uani 1 1 d . . . . . H26A H 0.513984 0.676202 0.873261 0.036 Uiso 1 1 calc R . . . . H26B H 0.597599 0.633360 0.821751 0.036 Uiso 1 1 calc R . . . . C27 C 0.3812(2) 0.68607(11) 0.74078(13) 0.0260(5) Uani 1 1 d . . . . . H27A H 0.461072 0.690932 0.715847 0.031 Uiso 1 1 calc R . . . . H27B H 0.374275 0.726791 0.771112 0.031 Uiso 1 1 calc R . . . . C28 C 0.2561(2) 0.67837(11) 0.68284(13) 0.0273(5) Uani 1 1 d . . . . . H28A H 0.177533 0.669472 0.707774 0.033 Uiso 1 1 calc R . . . . H28B H 0.238105 0.720219 0.653372 0.033 Uiso 1 1 calc R . . . . C29 C 0.1604(2) 0.61805(11) 0.57335(13) 0.0280(5) Uani 1 1 d . . . . . H29A H 0.152574 0.658584 0.541292 0.034 Uiso 1 1 calc R . . . . H29B H 0.075321 0.612995 0.593515 0.034 Uiso 1 1 calc R . . . . C30 C 0.1825(2) 0.55769(11) 0.52762(12) 0.0253(5) Uani 1 1 d . . . . . H30A H 0.111239 0.555219 0.481839 0.030 Uiso 1 1 calc R . . . . H30B H 0.271950 0.560657 0.511687 0.030 Uiso 1 1 calc R . . . . C31 C 0.1944(2) 0.43951(11) 0.53349(13) 0.0267(5) Uani 1 1 d . . . . . H31A H 0.284666 0.439119 0.518326 0.032 Uiso 1 1 calc R . . . . H31B H 0.124026 0.436413 0.487368 0.032 Uiso 1 1 calc R . . . . C32 C 0.1824(2) 0.38146(11) 0.58434(13) 0.0280(5) Uani 1 1 d . . . . . H32A H 0.095772 0.384249 0.603389 0.034 Uiso 1 1 calc R . . . . H32B H 0.183110 0.339010 0.556131 0.034 Uiso 1 1 calc R . . . . C33 C 0.2858(2) 0.33131(11) 0.69952(13) 0.0300(6) Uani 1 1 d . . . . . H33A H 0.277203 0.287377 0.673746 0.036 Uiso 1 1 calc R . . . . H33B H 0.204323 0.338188 0.722630 0.036 Uiso 1 1 calc R . . . . C34 C 0.4099(2) 0.33201(11) 0.75927(14) 0.0307(6) Uani 1 1 d . . . . . H34A H 0.407658 0.293709 0.793845 0.037 Uiso 1 1 calc R . . . . H34B H 0.491606 0.327471 0.735855 0.037 Uiso 1 1 calc R . . . . C35 C 0.5326(3) 0.39599(13) 0.85866(14) 0.0360(6) Uani 1 1 d . . . . . H35A H 0.616009 0.396394 0.836404 0.043 Uiso 1 1 calc R . . . . H35B H 0.535489 0.356207 0.891622 0.043 Uiso 1 1 calc R . . . . C36 C 0.5256(3) 0.45827(13) 0.90396(14) 0.0390(6) Uani 1 1 d . . . . . H36A H 0.439502 0.458986 0.923685 0.047 Uiso 1 1 calc R . . . . H36B H 0.601778 0.458908 0.947437 0.047 Uiso 1 1 calc R . . . . C37 C 0.1205(14) 0.4491(5) 0.8392(6) 0.0358(18) Uani 0.548(15) 1 d D U P A 1 H37A H 0.184599 0.411295 0.851633 0.043 Uiso 0.548(15) 1 calc R . P A 1 H37B H 0.049348 0.435967 0.796050 0.043 Uiso 0.548(15) 1 calc R . P A 1 C38 C 0.0576(11) 0.4680(4) 0.9070(5) 0.0392(16) Uani 0.548(15) 1 d D U P A 1 H38A H -0.028411 0.443419 0.906515 0.047 Uiso 0.548(15) 1 calc R . P A 1 H38B H 0.120566 0.457897 0.954667 0.047 Uiso 0.548(15) 1 calc R . P A 1 C39 C 0.0331(8) 0.5394(4) 0.8991(5) 0.0298(14) Uani 0.548(15) 1 d D U P A 1 H39A H 0.064115 0.562418 0.947815 0.036 Uiso 0.548(15) 1 calc R . P A 1 H39B H -0.064999 0.548409 0.882449 0.036 Uiso 0.548(15) 1 calc R . P A 1 C40 C 0.114(2) 0.5637(6) 0.8399(8) 0.0340(17) Uani 0.548(15) 1 d D U P A 1 H40A H 0.051355 0.579997 0.794490 0.041 Uiso 0.548(15) 1 calc R . P A 1 H40B H 0.175045 0.600773 0.860383 0.041 Uiso 0.548(15) 1 calc R . P A 1 O7A O 0.1750(17) 0.4973(7) 0.8137(9) 0.0357(19) Uani 0.452(15) 1 d D U P A 2 C37A C 0.1336(18) 0.4419(6) 0.8546(7) 0.0333(19) Uani 0.452(15) 1 d D U P A 2 H37C H 0.205762 0.407419 0.863706 0.040 Uiso 0.452(15) 1 calc R . P A 2 H37D H 0.049736 0.421275 0.826246 0.040 Uiso 0.452(15) 1 calc R . P A 2 C38A C 0.1087(11) 0.4709(5) 0.9279(5) 0.0337(16) Uani 0.452(15) 1 d D U P A 2 H38C H 0.030842 0.448452 0.944287 0.040 Uiso 0.452(15) 1 calc R . P A 2 H38D H 0.189968 0.465428 0.967833 0.040 Uiso 0.452(15) 1 calc R . P A 2 C39A C 0.0799(14) 0.5407(5) 0.9132(6) 0.0423(18) Uani 0.452(15) 1 d D U P A 2 H39C H 0.139182 0.568710 0.950804 0.051 Uiso 0.452(15) 1 calc R . P A 2 H39D H -0.015885 0.550544 0.916068 0.051 Uiso 0.452(15) 1 calc R . P A 2 C40A C 0.107(3) 0.5555(7) 0.8335(9) 0.037(2) Uani 0.452(15) 1 d D U P A 2 H40C H 0.020711 0.562689 0.797737 0.044 Uiso 0.452(15) 1 calc R . P A 2 H40D H 0.164769 0.595655 0.833559 0.044 Uiso 0.452(15) 1 calc R . P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 K1 0.0292(2) 0.0171(2) 0.0188(2) 0.00055(19) 0.00493(18) 0.0008(2) O1 0.0328(9) 0.0306(9) 0.0249(9) 0.0028(7) 0.0019(7) 0.0008(7) O2 0.0254(8) 0.0213(8) 0.0244(8) -0.0014(6) 0.0026(7) -0.0042(6) O3 0.0243(8) 0.0195(8) 0.0263(9) -0.0012(6) 0.0016(7) 0.0020(6) O4 0.0283(8) 0.0211(8) 0.0229(8) -0.0005(6) 0.0044(6) -0.0005(7) O5 0.0288(9) 0.0190(8) 0.0308(9) 0.0005(7) 0.0070(7) -0.0028(7) O6 0.0291(9) 0.0216(8) 0.0286(9) 0.0039(7) 0.0050(7) 0.0050(7) O7 0.038(3) 0.015(3) 0.048(3) -0.007(2) 0.024(2) -0.005(2) C1 0.0261(12) 0.0148(11) 0.0347(14) 0.0010(9) -0.0069(10) -0.0043(9) C2 0.0382(14) 0.0150(11) 0.0285(13) -0.0064(9) -0.0105(11) 0.0044(10) C3 0.0276(12) 0.0146(11) 0.0331(13) -0.0082(9) -0.0061(10) 0.0071(9) C4 0.0269(12) 0.0155(11) 0.0342(14) 0.0010(10) -0.0107(10) 0.0030(9) C5 0.0316(13) 0.0188(11) 0.0282(13) 0.0092(10) -0.0080(10) -0.0042(10) C6 0.0315(13) 0.0167(11) 0.0289(13) 0.0103(9) -0.0072(10) -0.0080(10) C7 0.0281(12) 0.0289(13) 0.0234(12) 0.0113(10) 0.0005(10) -0.0104(10) C8 0.0272(13) 0.0404(15) 0.0230(13) 0.0135(11) -0.0033(10) -0.0076(11) C9 0.0283(13) 0.0475(16) 0.0186(12) 0.0052(11) 0.0014(10) -0.0089(11) C10 0.0212(12) 0.0444(15) 0.0194(12) 0.0062(10) 0.0050(9) -0.0078(10) C11 0.0190(12) 0.0485(16) 0.0229(12) 0.0071(11) 0.0019(10) -0.0085(11) C12 0.0232(12) 0.0385(14) 0.0223(12) 0.0057(10) -0.0021(10) -0.0112(10) C13 0.0208(12) 0.0488(16) 0.0195(12) 0.0013(11) 0.0069(10) -0.0043(11) C14 0.0290(13) 0.0542(17) 0.0171(12) 0.0022(11) 0.0023(10) 0.0000(12) C15 0.0299(13) 0.0518(17) 0.0187(12) -0.0062(11) 0.0031(10) 0.0018(12) C16 0.0195(12) 0.0501(16) 0.0179(12) -0.0048(11) 0.0058(9) 0.0057(11) C17 0.0208(12) 0.0509(16) 0.0173(12) 0.0006(11) 0.0072(9) 0.0043(11) C18 0.0171(11) 0.0516(17) 0.0209(12) -0.0021(11) 0.0057(9) -0.0013(10) C19 0.0232(12) 0.0467(15) 0.0198(12) -0.0079(11) 0.0056(10) 0.0088(11) C20 0.0289(13) 0.0439(15) 0.0188(12) -0.0102(11) -0.0005(10) 0.0093(11) C21 0.0280(13) 0.0369(14) 0.0243(12) -0.0140(11) -0.0016(10) 0.0060(11) C22 0.0286(12) 0.0254(12) 0.0252(12) -0.0123(10) -0.0022(10) 0.0105(10) C23 0.0255(12) 0.0372(14) 0.0238(12) -0.0076(10) -0.0020(10) 0.0133(11) C24 0.0217(12) 0.0429(15) 0.0263(13) -0.0089(11) -0.0008(10) 0.0096(11) C25 0.0352(14) 0.0422(15) 0.0259(13) -0.0084(11) -0.0014(11) -0.0008(12) C26 0.0247(12) 0.0341(14) 0.0310(13) -0.0117(11) 0.0012(10) -0.0039(10) C27 0.0308(13) 0.0158(11) 0.0332(13) -0.0020(9) 0.0105(10) -0.0022(9) C28 0.0349(13) 0.0167(11) 0.0312(13) 0.0005(9) 0.0084(11) 0.0035(10) C29 0.0271(12) 0.0243(12) 0.0301(13) 0.0054(10) -0.0013(10) 0.0038(10) C30 0.0254(12) 0.0277(12) 0.0213(12) 0.0061(9) 0.0002(9) 0.0018(10) C31 0.0246(12) 0.0300(13) 0.0248(12) -0.0079(10) 0.0023(10) -0.0025(10) C32 0.0265(12) 0.0240(12) 0.0329(13) -0.0075(10) 0.0036(10) -0.0056(10) C33 0.0401(14) 0.0161(11) 0.0375(14) 0.0008(10) 0.0173(12) -0.0040(10) C34 0.0374(14) 0.0202(12) 0.0382(14) 0.0065(10) 0.0170(11) 0.0080(10) C35 0.0345(14) 0.0341(14) 0.0368(15) 0.0148(12) -0.0003(12) 0.0069(11) C36 0.0417(15) 0.0474(16) 0.0245(13) 0.0105(12) -0.0026(11) 0.0026(13) C37 0.039(3) 0.022(3) 0.052(4) -0.005(3) 0.024(3) -0.003(3) C38 0.047(4) 0.026(2) 0.050(4) 0.003(3) 0.023(3) -0.004(3) C39 0.024(3) 0.028(2) 0.040(3) 0.003(2) 0.013(2) 0.006(2) C40 0.037(3) 0.021(3) 0.049(3) 0.003(2) 0.023(3) 0.006(3) O7A 0.046(4) 0.020(4) 0.047(3) 0.003(3) 0.025(3) 0.001(3) C37A 0.038(3) 0.020(3) 0.046(4) 0.009(3) 0.016(3) -0.001(3) C38A 0.035(4) 0.028(3) 0.040(3) 0.006(3) 0.011(3) 0.005(3) C39A 0.052(4) 0.028(3) 0.053(4) -0.001(3) 0.027(3) 0.001(3) C40A 0.041(3) 0.021(3) 0.052(3) 0.006(3) 0.019(3) 0.001(3) 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' K K 0.2009 0.2494 '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' 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 K1 O4 179.57(5) . . ? O1 K1 C17 98.05(6) . . ? O1 K1 C18 98.92(6) . . ? O2 K1 O1 60.47(5) . . ? O2 K1 O3 61.40(5) . . ? O2 K1 O4 119.41(5) . . ? O2 K1 O5 176.00(5) . . ? O2 K1 C17 90.37(6) . . ? O2 K1 C18 112.38(6) . . ? O3 K1 O1 120.27(5) . . ? O3 K1 O4 59.51(4) . . ? O3 K1 C17 69.74(6) . . ? O3 K1 C18 90.72(6) . . ? O4 K1 C17 81.52(5) . . ? O4 K1 C18 80.74(5) . . ? O5 K1 O1 120.43(5) . . ? O5 K1 O3 118.54(5) . . ? O5 K1 O4 59.73(4) . . ? O5 K1 C17 93.31(6) . . ? O5 K1 C18 71.54(6) . . ? O6 K1 O1 60.65(5) . . ? O6 K1 O2 118.22(5) . . ? O6 K1 O3 175.59(5) . . ? O6 K1 O4 119.60(5) . . ? O6 K1 O5 61.48(5) . . ? O6 K1 C17 114.61(6) . . ? O6 K1 C18 93.38(6) . . ? O7 K1 O1 74.7(3) . . ? O7 K1 O2 74.4(2) . . ? O7 K1 O3 102.0(3) . . ? O7 K1 O4 105.7(3) . . ? O7 K1 O5 102.0(2) . . ? O7 K1 O6 74.0(3) . . ? O7 K1 C17 164.7(2) . . ? O7 K1 C18 167.3(3) . . ? C18 K1 C17 24.64(6) . . ? O7A K1 O1 78.9(4) . . ? O7A K1 O2 79.9(3) . . ? O7A K1 O3 103.5(4) . . ? O7A K1 O4 101.5(4) . . ? O7A K1 O5 96.3(3) . . ? O7A K1 O6 72.2(4) . . ? O7A K1 C17 170.1(3) . . ? O7A K1 C18 164.7(3) . . ? C25 O1 K1 113.21(13) . . ? C36 O1 K1 112.85(13) . . ? C36 O1 C25 111.74(18) . . ? C26 O2 K1 116.05(13) . . ? C26 O2 C27 111.73(17) . . ? C27 O2 K1 115.61(12) . . ? C28 O3 K1 110.98(12) . . ? C28 O3 C29 112.20(16) . . ? C29 O3 K1 116.46(12) . . ? C30 O4 K1 113.16(12) . . ? C31 O4 K1 112.67(12) . . ? C31 O4 C30 112.49(16) . . ? C32 O5 K1 116.60(12) . . ? C33 O5 K1 111.81(12) . . ? C33 O5 C32 112.02(17) . . ? C34 O6 K1 115.94(13) . . ? C35 O6 K1 116.30(13) . . ? C35 O6 C34 112.30(17) . . ? C37 O7 K1 122.3(7) . . ? C40 O7 K1 125.7(7) . . ? C40 O7 C37 106.4(8) . . ? C2 C1 H1 119.1 . . ? C2 C1 C6 121.8(2) . . ? C6 C1 H1 119.1 . . ? C1 C2 H2 118.8 . . ? C1 C2 C3 122.3(2) . . ? C3 C2 H2 118.8 . . ? C2 C3 C22 122.5(2) . 3_766 ? C4 C3 C2 113.2(2) . . ? C4 C3 C22 121.9(2) . 3_766 ? C3 C4 H4 119.2 . . ? C5 C4 C3 121.7(2) . . ? C5 C4 H4 119.2 . . ? C4 C5 H5 118.8 . . ? C4 C5 C6 122.5(2) . . ? C6 C5 H5 118.8 . . ? C1 C6 C5 113.3(2) . . ? C1 C6 C7 122.5(2) . . ? C5 C6 C7 122.4(2) . . ? C8 C7 C6 121.3(2) . . ? C8 C7 C12 113.6(2) . . ? C12 C7 C6 123.5(2) . . ? C7 C8 H8 118.5 . . ? C9 C8 C7 123.0(2) . . ? C9 C8 H8 118.5 . . ? C8 C9 H9 118.9 . . ? C8 C9 C10 122.2(2) . . ? C10 C9 H9 118.9 . . ? C9 C10 C11 114.0(2) . . ? C9 C10 C13 121.8(2) . . ? C11 C10 C13 123.1(2) . . ? C10 C11 H11 118.9 . . ? C12 C11 C10 122.2(2) . . ? C12 C11 H11 118.9 . . ? C7 C12 H12 118.7 . . ? C11 C12 C7 122.5(2) . . ? C11 C12 H12 118.7 . . ? C14 C13 C10 122.8(2) . . ? C14 C13 C18 114.1(2) . . ? C18 C13 C10 122.4(2) . . ? C13 C14 H14 118.7 . . ? C15 C14 C13 122.7(2) . . ? C15 C14 H14 118.7 . . ? C14 C15 H15 118.7 . . ? C14 C15 C16 122.7(2) . . ? C16 C15 H15 118.7 . . ? C15 C16 C17 114.2(2) . . ? C15 C16 C19 123.0(2) . . ? C17 C16 C19 121.9(2) . . ? K1 C17 H17 116.8 . . ? C16 C17 K1 97.87(13) . . ? C16 C17 H17 116.8 . . ? C18 C17 K1 75.45(13) . . ? C18 C17 C16 122.4(2) . . ? C18 C17 H17 116.8 . . ? K1 C18 H18 116.5 . . ? C13 C18 K1 95.69(13) . . ? C13 C18 H18 116.5 . . ? C17 C18 K1 79.91(13) . . ? C17 C18 C13 122.4(2) . . ? C17 C18 H18 116.5 . . ? C20 C19 C16 121.3(2) . . ? C24 C19 C16 123.5(2) . . ? C24 C19 C20 113.9(2) . . ? C19 C20 H20 118.8 . . ? C21 C20 C19 122.3(2) . . ? C21 C20 H20 118.8 . . ? C20 C21 H21 118.8 . . ? C20 C21 C22 122.3(2) . . ? C22 C21 H21 118.8 . . ? C21 C22 C3 120.6(2) . 3_766 ? C21 C22 C23 114.1(2) . . ? C23 C22 C3 123.4(2) . 3_766 ? C22 C23 H23 119.0 . . ? C24 C23 C22 121.9(2) . . ? C24 C23 H23 119.0 . . ? C19 C24 H24 118.7 . . ? C23 C24 C19 122.6(2) . . ? C23 C24 H24 118.7 . . ? O1 C25 H25A 109.8 . . ? O1 C25 H25B 109.8 . . ? O1 C25 C26 109.47(19) . . ? H25A C25 H25B 108.2 . . ? C26 C25 H25A 109.8 . . ? C26 C25 H25B 109.8 . . ? O2 C26 C25 108.70(19) . . ? O2 C26 H26A 109.9 . . ? O2 C26 H26B 109.9 . . ? C25 C26 H26A 109.9 . . ? C25 C26 H26B 109.9 . . ? H26A C26 H26B 108.3 . . ? O2 C27 H27A 109.8 . . ? O2 C27 H27B 109.8 . . ? O2 C27 C28 109.44(18) . . ? H27A C27 H27B 108.2 . . ? C28 C27 H27A 109.8 . . ? C28 C27 H27B 109.8 . . ? O3 C28 C27 109.62(18) . . ? O3 C28 H28A 109.7 . . ? O3 C28 H28B 109.7 . . ? C27 C28 H28A 109.7 . . ? C27 C28 H28B 109.7 . . ? H28A C28 H28B 108.2 . . ? O3 C29 H29A 110.0 . . ? O3 C29 H29B 110.0 . . ? O3 C29 C30 108.54(18) . . ? H29A C29 H29B 108.4 . . ? C30 C29 H29A 110.0 . . ? C30 C29 H29B 110.0 . . ? O4 C30 C29 108.45(18) . . ? O4 C30 H30A 110.0 . . ? O4 C30 H30B 110.0 . . ? C29 C30 H30A 110.0 . . ? C29 C30 H30B 110.0 . . ? H30A C30 H30B 108.4 . . ? O4 C31 H31A 110.0 . . ? O4 C31 H31B 110.0 . . ? O4 C31 C32 108.62(18) . . ? H31A C31 H31B 108.3 . . ? C32 C31 H31A 110.0 . . ? C32 C31 H31B 110.0 . . ? O5 C32 C31 108.68(18) . . ? O5 C32 H32A 110.0 . . ? O5 C32 H32B 110.0 . . ? C31 C32 H32A 110.0 . . ? C31 C32 H32B 110.0 . . ? H32A C32 H32B 108.3 . . ? O5 C33 H33A 109.7 . . ? O5 C33 H33B 109.7 . . ? O5 C33 C34 109.70(18) . . ? H33A C33 H33B 108.2 . . ? C34 C33 H33A 109.7 . . ? C34 C33 H33B 109.7 . . ? O6 C34 C33 109.97(18) . . ? O6 C34 H34A 109.7 . . ? O6 C34 H34B 109.7 . . ? C33 C34 H34A 109.7 . . ? C33 C34 H34B 109.7 . . ? H34A C34 H34B 108.2 . . ? O6 C35 H35A 109.9 . . ? O6 C35 H35B 109.9 . . ? O6 C35 C36 109.04(19) . . ? H35A C35 H35B 108.3 . . ? C36 C35 H35A 109.9 . . ? C36 C35 H35B 109.9 . . ? O1 C36 C35 109.8(2) . . ? O1 C36 H36A 109.7 . . ? O1 C36 H36B 109.7 . . ? C35 C36 H36A 109.7 . . ? C35 C36 H36B 109.7 . . ? H36A C36 H36B 108.2 . . ? O7 C37 H37A 110.6 . . ? O7 C37 H37B 110.6 . . ? O7 C37 C38 105.5(7) . . ? H37A C37 H37B 108.8 . . ? C38 C37 H37A 110.6 . . ? C38 C37 H37B 110.6 . . ? C37 C38 H38A 110.8 . . ? C37 C38 H38B 110.8 . . ? H38A C38 H38B 108.9 . . ? C39 C38 C37 104.7(6) . . ? C39 C38 H38A 110.8 . . ? C39 C38 H38B 110.8 . . ? C38 C39 H39A 110.5 . . ? C38 C39 H39B 110.5 . . ? C38 C39 C40 106.3(6) . . ? H39A C39 H39B 108.7 . . ? C40 C39 H39A 110.5 . . ? C40 C39 H39B 110.5 . . ? O7 C40 C39 106.7(7) . . ? O7 C40 H40A 110.4 . . ? O7 C40 H40B 110.4 . . ? C39 C40 H40A 110.4 . . ? C39 C40 H40B 110.4 . . ? H40A C40 H40B 108.6 . . ? C37A O7A K1 132.0(10) . . ? C40A O7A K1 120.0(9) . . ? C40A O7A C37A 107.9(9) . . ? O7A C37A H37C 110.7 . . ? O7A C37A H37D 110.7 . . ? O7A C37A C38A 105.2(9) . . ? H37C C37A H37D 108.8 . . ? C38A C37A H37C 110.7 . . ? C38A C37A H37D 110.7 . . ? C37A C38A H38C 110.6 . . ? C37A C38A H38D 110.6 . . ? H38C C38A H38D 108.7 . . ? C39A C38A C37A 105.8(7) . . ? C39A C38A H38C 110.6 . . ? C39A C38A H38D 110.6 . . ? C38A C39A H39C 110.3 . . ? C38A C39A H39D 110.3 . . ? C38A C39A C40A 107.2(8) . . ? H39C C39A H39D 108.5 . . ? C40A C39A H39C 110.3 . . ? C40A C39A H39D 110.3 . . ? O7A C40A C39A 104.4(9) . . ? O7A C40A H40C 110.9 . . ? O7A C40A H40D 110.9 . . ? C39A C40A H40C 110.9 . . ? C39A C40A H40D 110.9 . . ? H40C C40A H40D 108.9 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag K1 O1 2.8405(17) . ? K1 O2 2.7527(16) . ? K1 O3 2.8183(16) . ? K1 O4 2.8670(16) . ? K1 O5 2.8045(16) . ? K1 O6 2.7509(16) . ? K1 O7 2.724(10) . ? K1 C17 3.239(2) . ? K1 C18 3.184(2) . ? K1 O7A 2.741(12) . ? O1 C25 1.423(3) . ? O1 C36 1.417(3) . ? O2 C26 1.415(3) . ? O2 C27 1.425(3) . ? O3 C28 1.423(3) . ? O3 C29 1.424(3) . ? O4 C30 1.425(3) . ? O4 C31 1.422(3) . ? O5 C32 1.430(3) . ? O5 C33 1.426(3) . ? O6 C34 1.423(3) . ? O6 C35 1.416(3) . ? O7 C37 1.432(9) . ? O7 C40 1.432(9) . ? C1 H1 0.9500 . ? C1 C2 1.361(3) . ? C1 C6 1.423(3) . ? C2 H2 0.9500 . ? C2 C3 1.431(3) . ? C3 C4 1.422(3) . ? C3 C22 1.438(3) 3_766 ? C4 H4 0.9500 . ? C4 C5 1.364(3) . ? C5 H5 0.9500 . ? C5 C6 1.425(3) . ? C6 C7 1.437(3) . ? C7 C8 1.417(3) . ? C7 C12 1.421(3) . ? C8 H8 0.9500 . ? C8 C9 1.365(4) . ? C9 H9 0.9500 . ? C9 C10 1.419(3) . ? C10 C11 1.424(3) . ? C10 C13 1.449(4) . ? C11 H11 0.9500 . ? C11 C12 1.370(3) . ? C12 H12 0.9500 . ? C13 C14 1.418(3) . ? C13 C18 1.419(3) . ? C14 H14 0.9500 . ? C14 C15 1.365(4) . ? C15 H15 0.9500 . ? C15 C16 1.411(3) . ? C16 C17 1.422(3) . ? C16 C19 1.447(4) . ? C17 H17 1.0000 . ? C17 C18 1.371(4) . ? C18 H18 1.0000 . ? C19 C20 1.423(3) . ? C19 C24 1.419(3) . ? C20 H20 0.9500 . ? C20 C21 1.365(4) . ? C21 H21 0.9500 . ? C21 C22 1.416(3) . ? C22 C23 1.426(3) . ? C23 H23 0.9500 . ? C23 C24 1.366(3) . ? C24 H24 0.9500 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C25 C26 1.495(3) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C27 C28 1.487(3) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C29 C30 1.500(3) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C31 C32 1.497(3) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C33 C34 1.491(3) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C35 C36 1.497(4) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C37 C38 1.521(8) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C38 C39 1.451(8) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C39 C40 1.529(10) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? O7A C37A 1.433(10) . ? O7A C40A 1.425(10) . ? C37A H37C 0.9900 . ? C37A H37D 0.9900 . ? C37A C38A 1.504(10) . ? C38A H38C 0.9900 . ? C38A H38D 0.9900 . ? C38A C39A 1.440(9) . ? C39A H39C 0.9900 . ? C39A H39D 0.9900 . ? C39A C40A 1.537(12) . ? C40A H40C 0.9900 . ? C40A H40D 0.9900 . ?