#------------------------------------------------------------------------------ #$Date: 2026-06-26 23:55:25 +0100 (Fri, 26 Jun 2026) $ #$Revision: 306664 $ #$URL: svn://www.crystallography.net/cod/cif/1/57/74/1577444.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_1577444 loop_ _publ_author_name 'Koshelev, Ivan V.' 'Selikhov, Alexander N.' 'Cherkasov, Anton' 'Aysin, Rinat R.' 'Trifonov, Alexander A.' _publ_section_title ; Highly regio- and E-stereoselective C=C bond transposition catalyzed by tris(benzhydryl) sodium calciate. Proof of synergy: one metal is good, but two are better ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D6SC03562K _journal_year 2026 _chemical_formula_moiety 'C63 H81 Ca Na' _chemical_formula_sum 'C63 H81 Ca Na' _chemical_formula_weight 901.34 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2019/3 _audit_update_record ; 2025-07-02 deposited with the CCDC. 2026-06-26 downloaded from the CCDC. ; _cell_angle_alpha 63.424(3) _cell_angle_beta 77.319(3) _cell_angle_gamma 69.659(3) _cell_formula_units_Z 2 _cell_length_a 11.8319(3) _cell_length_b 16.0165(5) _cell_length_c 16.8588(5) _cell_measurement_reflns_used 10323 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 25.67 _cell_measurement_theta_min 2.22 _cell_volume 2671.28(16) _computing_cell_refinement 'CAP 42.101a' _computing_data_collection 'CAP 42.101a' _computing_data_reduction 'CAP 42.101a' _computing_structure_refinement 'SHELXL 2019/2' _computing_structure_solution 'SHELXT 2018/2' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Rigaku OD Xcalibur E' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0792 _diffrn_reflns_av_unetI/netI 0.0722 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 55996 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.681 _diffrn_reflns_theta_min 1.963 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 0.163 _exptl_absorpt_correction_T_max 0.978 _exptl_absorpt_correction_T_min 0.931 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details 'CAP 42.101a' _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.121 _exptl_crystal_description plate _exptl_crystal_F_000 980 _exptl_crystal_size_max 0.590 _exptl_crystal_size_mid 0.430 _exptl_crystal_size_min 0.140 _refine_diff_density_max 0.349 _refine_diff_density_min -0.467 _refine_diff_density_rms 0.058 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 624 _refine_ls_number_reflns 10147 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.022 _refine_ls_R_factor_all 0.1026 _refine_ls_R_factor_gt 0.0554 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0598P)^2^+1.2084P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1189 _refine_ls_wR_factor_ref 0.1419 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6639 _reflns_number_total 10147 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6sc03562k2.cif _cod_data_source_block canacph2 _cod_original_cell_volume 2671.27(17) _cod_database_code 1577444 _shelx_shelxl_version_number 2019/3 _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_min 0.910 _shelx_estimated_absorpt_t_max 0.977 _shelx_res_file ; TITL canacph2 [P-1] canacph2.res created by SHELXL-2019/3 at 16:23:34 on 02-Jul-2025 CELL 0.71073 11.831861 16.016501 16.858770 63.4240 77.3191 69.6589 ZERR 2.00 0.000335 0.000544 0.000506 0.0032 0.0025 0.0029 LATT 1 SFAC C H CA NA UNIT 126 162 2 2 SIZE 0.14 0.43 0.59 TEMP -173.15 L.S. 20 BOND $H LIST 4 FMAP 2 PLAN 50 OMIT 1 0 4 OMIT 0 -3 1 OMIT 0 -2 2 OMIT -1 3 0 OMIT 3 6 5 OMIT 0 -1 3 OMIT 1 -2 1 OMIT -1 1 4 OMIT -2 6 3 OMIT 2 4 8 ACTA WGHT 0.059800 1.208400 FVAR 0.43406 CA1 3 0.492519 0.374082 0.232210 11.00000 0.02350 0.02252 = 0.02408 -0.00614 -0.00230 -0.00810 NA1 4 0.268266 0.593422 0.290782 11.00000 0.02521 0.02038 = 0.02113 -0.00660 -0.00043 -0.01009 C1 1 0.178694 0.458896 0.296304 11.00000 0.02833 0.02576 = 0.01780 -0.00576 -0.00246 -0.00964 H1A 2 0.181735 0.436275 0.358777 11.00000 0.01387 C2 1 0.249510 0.390639 0.260144 11.00000 0.01767 0.02486 = 0.02671 -0.00825 0.00022 -0.01145 C3 1 0.310934 0.294566 0.319481 11.00000 0.02705 0.02294 = 0.02104 -0.00496 0.00129 -0.01290 AFIX 43 H3A 2 0.298224 0.278327 0.381639 11.00000 -1.20000 AFIX 0 C4 1 0.387200 0.225059 0.290561 11.00000 0.02649 0.01980 = 0.02818 -0.00370 -0.00206 -0.00931 AFIX 43 H4A 2 0.425404 0.163065 0.333480 11.00000 -1.20000 AFIX 0 C5 1 0.411172 0.241911 0.199721 11.00000 0.02125 0.02185 = 0.02604 -0.00859 0.00090 -0.00836 C6 1 0.352439 0.335429 0.140388 11.00000 0.02075 0.02333 = 0.02299 -0.00629 -0.00289 -0.00925 AFIX 43 H6A 2 0.365600 0.350569 0.078424 11.00000 -1.20000 AFIX 0 C7 1 0.275768 0.406852 0.168552 11.00000 0.02094 0.01815 = 0.02685 -0.00431 -0.00596 -0.00763 AFIX 43 H7A 2 0.239358 0.469019 0.125010 11.00000 -1.20000 AFIX 0 C8 1 0.490724 0.159902 0.171064 11.00000 0.02735 0.02115 = 0.03029 -0.00876 0.00108 -0.00656 C9 1 0.621025 0.131450 0.195321 11.00000 0.02824 0.03238 = 0.07143 -0.02976 0.00231 -0.00590 AFIX 137 H9A 2 0.654405 0.186819 0.161280 11.00000 -1.50000 H9B 2 0.670830 0.075954 0.181035 11.00000 -1.50000 H9C 2 0.620727 0.113477 0.259078 11.00000 -1.50000 AFIX 0 C10 1 0.490848 0.190370 0.072271 11.00000 0.06723 0.04009 = 0.04010 -0.02429 -0.00385 0.00611 AFIX 137 H10A 2 0.407771 0.209907 0.056577 11.00000 -1.50000 H10B 2 0.539699 0.135596 0.056651 11.00000 -1.50000 H10C 2 0.525156 0.245361 0.039527 11.00000 -1.50000 AFIX 0 C11 1 0.441535 0.071176 0.221573 11.00000 0.03847 0.02811 = 0.05813 -0.02230 0.00825 -0.01318 AFIX 137 H11A 2 0.356061 0.090385 0.211292 11.00000 -1.50000 H11B 2 0.449715 0.046399 0.285359 11.00000 -1.50000 H11C 2 0.487437 0.020119 0.200302 11.00000 -1.50000 AFIX 0 C12 1 0.078485 0.544008 0.262173 11.00000 0.02182 0.02170 = 0.02553 -0.00833 -0.00055 -0.00990 C13 1 0.019401 0.596348 0.316126 11.00000 0.02809 0.02573 = 0.02670 -0.01056 -0.00201 -0.00959 H13A 2 0.053181 0.573748 0.375062 11.00000 0.02521 C14 1 -0.083429 0.674254 0.292967 11.00000 0.02866 0.02549 = 0.03554 -0.01768 0.00275 -0.00884 AFIX 43 H14A 2 -0.119244 0.706313 0.331911 11.00000 -1.20000 AFIX 0 C15 1 -0.136348 0.707311 0.213915 11.00000 0.02615 0.02116 = 0.03112 -0.00767 -0.00111 -0.01059 C16 1 -0.076750 0.658686 0.159447 11.00000 0.02586 0.02833 = 0.02626 -0.00971 -0.00264 -0.00885 AFIX 43 H16A 2 -0.109118 0.679553 0.104628 11.00000 -1.20000 AFIX 0 C17 1 0.026759 0.581826 0.180476 11.00000 0.02282 0.02623 = 0.02676 -0.01174 0.00023 -0.00660 AFIX 43 H17A 2 0.064566 0.553347 0.139029 11.00000 -1.20000 AFIX 0 C18 1 -0.253977 0.790960 0.192133 11.00000 0.02361 0.02731 = 0.04147 -0.01584 -0.00357 -0.00291 C19 1 -0.231131 0.884078 0.179897 11.00000 0.03662 0.02746 = 0.08154 -0.02101 -0.01464 -0.00095 AFIX 137 H19A 2 -0.206103 0.875293 0.235478 11.00000 -1.50000 H19B 2 -0.305469 0.938058 0.164008 11.00000 -1.50000 H19C 2 -0.167125 0.898789 0.132334 11.00000 -1.50000 AFIX 0 C20 1 -0.301395 0.810989 0.106172 11.00000 0.03315 0.03613 = 0.05144 -0.01548 -0.01003 -0.00341 AFIX 137 H20A 2 -0.315726 0.751986 0.111361 11.00000 -1.50000 H20B 2 -0.241597 0.830058 0.056282 11.00000 -1.50000 H20C 2 -0.377282 0.863772 0.095730 11.00000 -1.50000 AFIX 0 C21 1 -0.351619 0.765068 0.268283 11.00000 0.02939 0.05428 = 0.05089 -0.02060 -0.00304 -0.00624 AFIX 137 H21A 2 -0.324537 0.754930 0.323667 11.00000 -1.50000 H21B 2 -0.365811 0.705310 0.275265 11.00000 -1.50000 H21C 2 -0.426793 0.818449 0.254490 11.00000 -1.50000 AFIX 0 C22 1 0.498689 0.535720 0.102829 11.00000 0.02227 0.02355 = 0.01889 -0.00792 -0.00209 -0.01076 H22A 2 0.458223 0.519539 0.073354 11.00000 0.01548 C23 1 0.625657 0.484333 0.106103 11.00000 0.02394 0.01879 = 0.01224 -0.00217 0.00101 -0.00883 C24 1 0.665972 0.397691 0.091198 11.00000 0.02052 0.02433 = 0.01876 -0.00784 -0.00086 -0.00938 H24A 2 0.608899 0.383268 0.071767 11.00000 0.02015 C25 1 0.784429 0.338569 0.098377 11.00000 0.02494 0.01845 = 0.01781 -0.00641 0.00158 -0.00620 AFIX 43 H25A 2 0.805687 0.282238 0.086318 11.00000 -1.20000 AFIX 0 C26 1 0.872939 0.359569 0.122767 11.00000 0.02044 0.01853 = 0.01241 -0.00076 0.00080 -0.00634 C27 1 0.835054 0.444528 0.137534 11.00000 0.02461 0.02213 = 0.01915 -0.00693 0.00233 -0.01285 AFIX 43 H27A 2 0.892957 0.461830 0.153727 11.00000 -1.20000 AFIX 0 C28 1 0.718171 0.504750 0.129910 11.00000 0.02261 0.01788 = 0.01975 -0.00658 0.00190 -0.00779 AFIX 43 H28A 2 0.698772 0.561596 0.140875 11.00000 -1.20000 AFIX 0 C29 1 1.005549 0.297566 0.129299 11.00000 0.01959 0.02301 = 0.02138 -0.00736 -0.00023 -0.00554 C30 1 1.083817 0.358786 0.058190 11.00000 0.02043 0.02854 = 0.02843 -0.01152 0.00115 -0.00560 AFIX 137 H30A 2 1.054508 0.383109 -0.000419 11.00000 -1.50000 H30B 2 1.167949 0.318442 0.058565 11.00000 -1.50000 H30C 2 1.079047 0.413960 0.070948 11.00000 -1.50000 AFIX 0 C31 1 1.047115 0.265658 0.221407 11.00000 0.02239 0.03318 = 0.02762 -0.00774 -0.00269 -0.00491 AFIX 137 H31A 2 1.041106 0.323367 0.230567 11.00000 -1.50000 H31B 2 1.131185 0.224742 0.224852 11.00000 -1.50000 H31C 2 0.995542 0.228533 0.267501 11.00000 -1.50000 AFIX 0 C32 1 1.025464 0.205868 0.114150 11.00000 0.02362 0.02469 = 0.03933 -0.01071 -0.00167 -0.00367 AFIX 137 H32A 2 1.003972 0.224668 0.054318 11.00000 -1.50000 H32B 2 0.974555 0.166642 0.158392 11.00000 -1.50000 H32C 2 1.110607 0.167626 0.120047 11.00000 -1.50000 AFIX 0 C33 1 0.428652 0.617354 0.123612 11.00000 0.02411 0.01926 = 0.01466 -0.00185 -0.00106 -0.00821 C34 1 0.305347 0.661556 0.102065 11.00000 0.02336 0.02438 = 0.02333 -0.00869 -0.00391 -0.00769 AFIX 43 H34A 2 0.272406 0.634430 0.075795 11.00000 -1.20000 AFIX 0 C35 1 0.232369 0.741615 0.117711 11.00000 0.01846 0.02406 = 0.02756 -0.00583 -0.00504 -0.00400 AFIX 43 H35A 2 0.151122 0.767229 0.102047 11.00000 -1.20000 AFIX 0 C36 1 0.272993 0.787104 0.155908 11.00000 0.02424 0.02213 = 0.02674 -0.00867 0.00128 -0.00923 C37 1 0.391602 0.741874 0.181193 11.00000 0.02447 0.02595 = 0.02896 -0.01252 -0.00196 -0.01054 AFIX 43 H37A 2 0.422654 0.768055 0.209532 11.00000 -1.20000 AFIX 0 C38 1 0.466117 0.660342 0.166737 11.00000 0.01815 0.02436 = 0.02648 -0.00755 -0.00346 -0.00602 AFIX 43 H38A 2 0.545310 0.632394 0.186599 11.00000 -1.20000 AFIX 0 C39 1 0.192959 0.879412 0.166710 11.00000 0.02796 0.02048 = 0.03730 -0.01283 -0.00234 -0.00350 C40 1 0.154827 0.958828 0.074957 11.00000 0.07655 0.02614 = 0.04794 -0.01306 -0.01211 0.00283 AFIX 137 H40A 2 0.112725 0.935820 0.048284 11.00000 -1.50000 H40B 2 0.226739 0.973422 0.036417 11.00000 -1.50000 H40C 2 0.100699 1.017891 0.081652 11.00000 -1.50000 AFIX 0 C41 1 0.255793 0.916639 0.208669 11.00000 0.03699 0.03973 = 0.08346 -0.04055 -0.00474 -0.00600 AFIX 137 H41A 2 0.278923 0.866706 0.267710 11.00000 -1.50000 H41B 2 0.200582 0.975961 0.214294 11.00000 -1.50000 H41C 2 0.328258 0.931176 0.170970 11.00000 -1.50000 AFIX 0 C42 1 0.079399 0.859542 0.227166 11.00000 0.03529 0.04526 = 0.05887 -0.03350 0.00543 -0.00780 AFIX 137 H42A 2 0.102539 0.811821 0.286911 11.00000 -1.50000 H42B 2 0.037919 0.833785 0.202814 11.00000 -1.50000 H42C 2 0.025163 0.920322 0.230412 11.00000 -1.50000 AFIX 0 C43 1 0.525427 0.408056 0.362153 11.00000 0.02436 0.02167 = 0.01875 -0.00380 0.00010 -0.00706 H43A 2 0.578093 0.448807 0.321601 11.00000 0.02176 C44 1 0.581758 0.304527 0.390507 11.00000 0.02088 0.02482 = 0.01849 -0.00532 -0.00325 -0.00793 C45 1 0.679380 0.271320 0.335485 11.00000 0.02266 0.02106 = 0.01730 -0.00352 -0.00156 -0.00870 AFIX 43 H45A 2 0.705462 0.318419 0.282353 11.00000 -1.20000 AFIX 0 C46 1 0.738445 0.173496 0.355570 11.00000 0.01829 0.02603 = 0.02300 -0.01042 0.00094 -0.00709 AFIX 43 H46A 2 0.803204 0.156189 0.315992 11.00000 -1.20000 AFIX 0 C47 1 0.705685 0.100099 0.431851 11.00000 0.01906 0.02238 = 0.02379 -0.00355 -0.00382 -0.00430 C48 1 0.609249 0.131769 0.486680 11.00000 0.02251 0.02334 = 0.02414 -0.00074 -0.00209 -0.00674 AFIX 43 H48A 2 0.584335 0.083928 0.539760 11.00000 -1.20000 AFIX 0 C49 1 0.548547 0.228524 0.467832 11.00000 0.02043 0.03242 = 0.02151 -0.00890 0.00151 -0.00724 AFIX 43 H49A 2 0.483020 0.244762 0.507439 11.00000 -1.20000 AFIX 0 C50 1 0.769544 -0.008546 0.457135 11.00000 0.02711 0.02186 = 0.03186 -0.00362 -0.00317 -0.00221 C51 1 0.822695 -0.052781 0.547418 11.00000 0.03497 0.03224 = 0.03097 0.00036 -0.00911 0.00446 AFIX 137 H51A 2 0.757499 -0.044455 0.592870 11.00000 -1.50000 H51B 2 0.881023 -0.019759 0.543273 11.00000 -1.50000 H51C 2 0.863473 -0.122351 0.563709 11.00000 -1.50000 AFIX 0 C52 1 0.679469 -0.060553 0.462588 11.00000 0.04278 0.01864 = 0.04270 -0.00174 -0.00310 -0.00721 AFIX 137 H52A 2 0.644980 -0.031348 0.405083 11.00000 -1.50000 H52B 2 0.614580 -0.053841 0.508686 11.00000 -1.50000 H52C 2 0.721188 -0.129762 0.477485 11.00000 -1.50000 AFIX 0 C53 1 0.873322 -0.025921 0.388469 11.00000 0.03540 0.02396 = 0.03844 -0.00904 -0.00312 0.00455 AFIX 137 H53A 2 0.841516 0.001837 0.330169 11.00000 -1.50000 H53B 2 0.911393 -0.096082 0.406579 11.00000 -1.50000 H53C 2 0.933375 0.005381 0.384779 11.00000 -1.50000 AFIX 0 C54 1 0.434483 0.459490 0.410702 11.00000 0.02348 0.02272 = 0.01725 -0.00437 -0.00295 -0.00397 C55 1 0.436356 0.552348 0.398463 11.00000 0.02406 0.02780 = 0.02132 -0.00787 -0.00241 -0.00774 AFIX 43 H55A 2 0.503209 0.575314 0.364665 11.00000 -1.20000 AFIX 0 C56 1 0.345033 0.611261 0.433576 11.00000 0.02721 0.02383 = 0.01861 -0.00760 -0.00535 -0.00463 AFIX 43 H56A 2 0.350605 0.673469 0.422145 11.00000 -1.20000 AFIX 0 C57 1 0.244806 0.581785 0.485399 11.00000 0.02205 0.02564 = 0.02019 -0.00903 -0.00523 -0.00225 C58 1 0.244973 0.488139 0.501380 11.00000 0.02338 0.02862 = 0.01952 -0.00595 -0.00123 -0.00955 AFIX 43 H58A 2 0.180298 0.464053 0.538240 11.00000 -1.20000 AFIX 0 C59 1 0.334892 0.429172 0.465991 11.00000 0.02732 0.02112 = 0.02157 -0.00585 -0.00243 -0.00645 AFIX 43 H59A 2 0.329760 0.366338 0.479153 11.00000 -1.20000 AFIX 0 C60 1 0.143500 0.642530 0.529115 11.00000 0.02574 0.03059 = 0.02510 -0.01357 -0.00142 -0.00541 C61 1 0.148800 0.588919 0.630350 11.00000 0.03265 0.03774 = 0.02709 -0.01594 0.00020 -0.00662 AFIX 137 H61A 2 0.228518 0.579479 0.646283 11.00000 -1.50000 H61B 2 0.134983 0.525395 0.650286 11.00000 -1.50000 H61C 2 0.086286 0.627627 0.659167 11.00000 -1.50000 AFIX 0 C62 1 0.019371 0.655579 0.504238 11.00000 0.02595 0.03783 = 0.03407 -0.02101 -0.00113 -0.00377 AFIX 137 H62A 2 -0.044117 0.692444 0.534222 11.00000 -1.50000 H62B 2 0.007814 0.591510 0.522913 11.00000 -1.50000 H62C 2 0.015150 0.691117 0.439695 11.00000 -1.50000 AFIX 0 C63 1 0.156955 0.744490 0.500178 11.00000 0.03012 0.03370 = 0.03247 -0.01825 -0.00502 -0.00232 AFIX 137 H63A 2 0.235375 0.738285 0.515835 11.00000 -1.50000 H63B 2 0.092008 0.780007 0.530557 11.00000 -1.50000 H63C 2 0.152060 0.780166 0.435698 11.00000 -1.50000 AFIX 0 HKLF 4 REM canacph2 [P-1] REM wR2 = 0.1419, GooF = S = 1.022, Restrained GooF = 1.022 for all data REM R1 = 0.0554 for 6639 Fo > 4sig(Fo) and 0.1026 for all 10147 data REM 624 parameters refined using 0 restraints END WGHT 0.0598 1.2078 REM Highest difference peak 0.349, deepest hole -0.467, 1-sigma level 0.058 Q1 1 -0.2774 0.8360 0.2950 11.00000 0.05 0.35 Q2 1 0.4550 0.2004 0.1887 11.00000 0.05 0.33 Q3 1 -0.3317 0.7692 0.1939 11.00000 0.05 0.30 Q4 1 0.8473 0.3505 0.0972 11.00000 0.05 0.30 Q5 1 0.2508 0.6312 0.3067 11.00000 0.05 0.29 Q6 1 1.0162 0.2606 0.1121 11.00000 0.05 0.28 Q7 1 0.6609 0.4914 0.1414 11.00000 0.05 0.28 Q8 1 0.4216 0.1730 0.0748 11.00000 0.05 0.28 Q9 1 -0.2161 0.8805 0.1079 11.00000 0.05 0.27 Q10 1 0.2216 0.7668 0.5189 11.00000 0.05 0.27 Q11 1 -0.1825 0.7558 0.1895 11.00000 0.05 0.27 Q12 1 0.1964 0.6134 0.5009 11.00000 0.05 0.26 Q13 1 0.9410 0.3252 0.1309 11.00000 0.05 0.26 Q14 1 0.0744 0.5908 0.2743 11.00000 0.05 0.25 Q15 1 0.4777 0.3241 0.2105 11.00000 0.05 0.25 Q16 1 0.7305 0.0461 0.4507 11.00000 0.05 0.24 Q17 1 1.0379 0.2923 0.1706 11.00000 0.05 0.24 Q18 1 0.1047 0.6855 0.4985 11.00000 0.05 0.24 Q19 1 0.8672 0.4068 0.1041 11.00000 0.05 0.24 Q20 1 0.2931 0.5671 0.3091 11.00000 0.05 0.24 Q21 1 0.0316 0.5452 0.2992 11.00000 0.05 0.24 Q22 1 0.4401 0.4238 0.2656 11.00000 0.05 0.24 Q23 1 0.5623 0.5333 0.0966 11.00000 0.05 0.23 Q24 1 0.4484 0.1290 0.1459 11.00000 0.05 0.23 Q25 1 0.2325 0.8311 0.1601 11.00000 0.05 0.23 Q26 1 0.2590 0.7667 0.1382 11.00000 0.05 0.23 Q27 1 0.6245 0.1718 0.1246 11.00000 0.05 0.23 Q28 1 0.3628 0.5824 0.3988 11.00000 0.05 0.22 Q29 1 0.6253 0.4333 0.1220 11.00000 0.05 0.22 Q30 1 0.4138 0.5164 0.3800 11.00000 0.05 0.22 Q31 1 0.2209 0.5563 0.4688 11.00000 0.05 0.22 Q32 1 0.5650 0.3598 0.3882 11.00000 0.05 0.22 Q33 1 -0.2774 0.8331 0.2346 11.00000 0.05 0.22 Q34 1 0.2169 0.5846 0.3060 11.00000 0.05 0.22 Q35 1 0.3982 0.3752 0.2591 11.00000 0.05 0.22 Q36 1 1.0377 0.3256 0.0979 11.00000 0.05 0.22 Q37 1 0.6817 0.1164 0.4671 11.00000 0.05 0.22 Q38 1 0.1519 0.8729 0.2003 11.00000 0.05 0.22 Q39 1 0.1565 0.5370 0.2518 11.00000 0.05 0.21 Q40 1 0.2742 0.6119 0.2526 11.00000 0.05 0.21 Q41 1 0.5702 0.1808 0.4511 11.00000 0.05 0.21 Q42 1 0.3158 0.4624 0.4873 11.00000 0.05 0.21 Q43 1 0.0813 0.9272 0.0822 11.00000 0.05 0.21 Q44 1 0.7764 0.4462 0.1631 11.00000 0.05 0.21 Q45 1 0.5765 0.4806 0.1470 11.00000 0.05 0.21 Q46 1 0.8151 0.4793 0.1028 11.00000 0.05 0.21 Q47 1 0.4516 0.4940 0.4214 11.00000 0.05 0.21 Q48 1 0.7823 -0.0250 0.5878 11.00000 0.05 0.20 Q49 1 0.2674 0.3595 0.1672 11.00000 0.05 0.20 Q50 1 0.0488 0.5494 0.2329 11.00000 0.05 0.20 ; _shelx_res_checksum 36599 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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 Ca1 Ca 0.49252(5) 0.37408(4) 0.23221(4) 0.02414(15) Uani 1 1 d . . . . . Na1 Na 0.26827(9) 0.59342(7) 0.29078(6) 0.0222(2) Uani 1 1 d . . . . . C1 C 0.1787(2) 0.4589(2) 0.29630(18) 0.0245(6) Uani 1 1 d . . . . . H1A H 0.182(2) 0.4363(17) 0.3588(17) 0.014(6) Uiso 1 1 d . . . . . C2 C 0.2495(2) 0.39064(19) 0.26014(18) 0.0227(6) Uani 1 1 d . . . . . C3 C 0.3109(2) 0.29457(19) 0.31948(18) 0.0241(6) Uani 1 1 d . . . . . H3A H 0.298224 0.278327 0.381639 0.029 Uiso 1 1 calc R U . . . C4 C 0.3872(2) 0.22506(19) 0.29056(18) 0.0264(6) Uani 1 1 d . . . . . H4A H 0.425404 0.163065 0.333480 0.032 Uiso 1 1 calc R U . . . C5 C 0.4112(2) 0.24191(19) 0.19972(18) 0.0233(6) Uani 1 1 d . . . . . C6 C 0.3524(2) 0.33543(18) 0.14039(18) 0.0225(6) Uani 1 1 d . . . . . H6A H 0.365600 0.350569 0.078424 0.027 Uiso 1 1 calc R U . . . C7 C 0.2758(2) 0.40685(19) 0.16855(18) 0.0225(6) Uani 1 1 d . . . . . H7A H 0.239358 0.469019 0.125010 0.027 Uiso 1 1 calc R U . . . C8 C 0.4907(2) 0.15990(19) 0.17106(18) 0.0276(6) Uani 1 1 d . . . . . C9 C 0.6210(3) 0.1314(2) 0.1953(2) 0.0425(8) Uani 1 1 d . . . . . H9A H 0.654405 0.186819 0.161280 0.064 Uiso 1 1 calc R U . . . H9B H 0.670830 0.075954 0.181035 0.064 Uiso 1 1 calc R U . . . H9C H 0.620727 0.113477 0.259078 0.064 Uiso 1 1 calc R U . . . C10 C 0.4908(3) 0.1904(2) 0.0723(2) 0.0522(10) Uani 1 1 d . . . . . H10A H 0.407771 0.209907 0.056577 0.078 Uiso 1 1 calc R U . . . H10B H 0.539699 0.135596 0.056651 0.078 Uiso 1 1 calc R U . . . H10C H 0.525156 0.245361 0.039527 0.078 Uiso 1 1 calc R U . . . C11 C 0.4415(3) 0.0712(2) 0.2216(2) 0.0407(8) Uani 1 1 d . . . . . H11A H 0.356061 0.090385 0.211292 0.061 Uiso 1 1 calc R U . . . H11B H 0.449715 0.046399 0.285359 0.061 Uiso 1 1 calc R U . . . H11C H 0.487437 0.020119 0.200302 0.061 Uiso 1 1 calc R U . . . C12 C 0.0785(2) 0.54401(19) 0.26217(17) 0.0227(6) Uani 1 1 d . . . . . C13 C 0.0194(2) 0.5963(2) 0.31613(19) 0.0263(6) Uani 1 1 d . . . . . H13A H 0.053(2) 0.5737(19) 0.3751(18) 0.025(7) Uiso 1 1 d . . . . . C14 C -0.0834(2) 0.6743(2) 0.29297(19) 0.0284(6) Uani 1 1 d . . . . . H14A H -0.119244 0.706313 0.331911 0.034 Uiso 1 1 calc R U . . . C15 C -0.1363(2) 0.70731(19) 0.21392(18) 0.0264(6) Uani 1 1 d . . . . . C16 C -0.0767(2) 0.6587(2) 0.15945(18) 0.0269(6) Uani 1 1 d . . . . . H16A H -0.109118 0.679553 0.104628 0.032 Uiso 1 1 calc R U . . . C17 C 0.0268(2) 0.58183(19) 0.18048(18) 0.0254(6) Uani 1 1 d . . . . . H17A H 0.064566 0.553347 0.139029 0.030 Uiso 1 1 calc R U . . . C18 C -0.2540(2) 0.7910(2) 0.1921(2) 0.0311(7) Uani 1 1 d . . . . . C19 C -0.2311(3) 0.8841(2) 0.1799(3) 0.0496(9) Uani 1 1 d . . . . . H19A H -0.206103 0.875293 0.235478 0.074 Uiso 1 1 calc R U . . . H19B H -0.305469 0.938058 0.164008 0.074 Uiso 1 1 calc R U . . . H19C H -0.167125 0.898789 0.132334 0.074 Uiso 1 1 calc R U . . . C20 C -0.3014(3) 0.8110(2) 0.1062(2) 0.0418(8) Uani 1 1 d . . . . . H20A H -0.315726 0.751986 0.111361 0.063 Uiso 1 1 calc R U . . . H20B H -0.241597 0.830058 0.056282 0.063 Uiso 1 1 calc R U . . . H20C H -0.377282 0.863772 0.095730 0.063 Uiso 1 1 calc R U . . . C21 C -0.3516(3) 0.7651(3) 0.2683(2) 0.0468(9) Uani 1 1 d . . . . . H21A H -0.324537 0.754930 0.323667 0.070 Uiso 1 1 calc R U . . . H21B H -0.365811 0.705310 0.275265 0.070 Uiso 1 1 calc R U . . . H21C H -0.426793 0.818449 0.254490 0.070 Uiso 1 1 calc R U . . . C22 C 0.4987(2) 0.53572(19) 0.10283(17) 0.0205(6) Uani 1 1 d . . . . . H22A H 0.458(2) 0.5195(17) 0.0734(16) 0.015(6) Uiso 1 1 d . . . . . C23 C 0.6257(2) 0.48433(18) 0.10610(16) 0.0196(6) Uani 1 1 d . . . . . C24 C 0.6660(2) 0.39769(19) 0.09120(17) 0.0208(6) Uani 1 1 d . . . . . H24A H 0.609(2) 0.3833(18) 0.0718(17) 0.020(7) Uiso 1 1 d . . . . . C25 C 0.7844(2) 0.33857(18) 0.09838(16) 0.0213(6) Uani 1 1 d . . . . . H25A H 0.805687 0.282238 0.086318 0.026 Uiso 1 1 calc R U . . . C26 C 0.8729(2) 0.35957(18) 0.12277(16) 0.0194(5) Uani 1 1 d . . . . . C27 C 0.8351(2) 0.44453(18) 0.13753(17) 0.0214(6) Uani 1 1 d . . . . . H27A H 0.892957 0.461830 0.153727 0.026 Uiso 1 1 calc R U . . . C28 C 0.7182(2) 0.50475(18) 0.12991(16) 0.0205(6) Uani 1 1 d . . . . . H28A H 0.698772 0.561596 0.140875 0.025 Uiso 1 1 calc R U . . . C29 C 1.0055(2) 0.29757(19) 0.12930(17) 0.0224(6) Uani 1 1 d . . . . . C30 C 1.0838(2) 0.3588(2) 0.05819(18) 0.0267(6) Uani 1 1 d . . . . . H30A H 1.054508 0.383109 -0.000419 0.040 Uiso 1 1 calc R U . . . H30B H 1.167949 0.318442 0.058565 0.040 Uiso 1 1 calc R U . . . H30C H 1.079047 0.413960 0.070948 0.040 Uiso 1 1 calc R U . . . C31 C 1.0471(2) 0.2657(2) 0.22141(18) 0.0303(7) Uani 1 1 d . . . . . H31A H 1.041106 0.323367 0.230567 0.045 Uiso 1 1 calc R U . . . H31B H 1.131185 0.224742 0.224852 0.045 Uiso 1 1 calc R U . . . H31C H 0.995542 0.228533 0.267501 0.045 Uiso 1 1 calc R U . . . C32 C 1.0255(3) 0.2059(2) 0.1141(2) 0.0312(7) Uani 1 1 d . . . . . H32A H 1.003972 0.224668 0.054318 0.047 Uiso 1 1 calc R U . . . H32B H 0.974555 0.166642 0.158392 0.047 Uiso 1 1 calc R U . . . H32C H 1.110607 0.167626 0.120047 0.047 Uiso 1 1 calc R U . . . C33 C 0.4287(2) 0.61735(18) 0.12361(16) 0.0208(6) Uani 1 1 d . . . . . C34 C 0.3053(2) 0.66156(19) 0.10207(17) 0.0234(6) Uani 1 1 d . . . . . H34A H 0.272406 0.634430 0.075795 0.028 Uiso 1 1 calc R U . . . C35 C 0.2324(2) 0.74161(19) 0.11771(18) 0.0252(6) Uani 1 1 d . . . . . H35A H 0.151122 0.767229 0.102047 0.030 Uiso 1 1 calc R U . . . C36 C 0.2730(2) 0.78710(19) 0.15591(18) 0.0247(6) Uani 1 1 d . . . . . C37 C 0.3916(2) 0.74187(19) 0.18119(18) 0.0250(6) Uani 1 1 d . . . . . H37A H 0.422654 0.768055 0.209532 0.030 Uiso 1 1 calc R U . . . C38 C 0.4661(2) 0.66034(19) 0.16674(17) 0.0238(6) Uani 1 1 d . . . . . H38A H 0.545310 0.632394 0.186599 0.029 Uiso 1 1 calc R U . . . C39 C 0.1930(3) 0.8794(2) 0.16671(19) 0.0292(7) Uani 1 1 d . . . . . C40 C 0.1548(4) 0.9588(2) 0.0750(2) 0.0547(10) Uani 1 1 d . . . . . H40A H 0.112725 0.935820 0.048284 0.082 Uiso 1 1 calc R U . . . H40B H 0.226739 0.973422 0.036417 0.082 Uiso 1 1 calc R U . . . H40C H 0.100699 1.017891 0.081652 0.082 Uiso 1 1 calc R U . . . C41 C 0.2558(3) 0.9166(2) 0.2087(3) 0.0487(9) Uani 1 1 d . . . . . H41A H 0.278923 0.866706 0.267710 0.073 Uiso 1 1 calc R U . . . H41B H 0.200582 0.975961 0.214294 0.073 Uiso 1 1 calc R U . . . H41C H 0.328258 0.931176 0.170970 0.073 Uiso 1 1 calc R U . . . C42 C 0.0794(3) 0.8595(2) 0.2272(2) 0.0443(8) Uani 1 1 d . . . . . H42A H 0.102539 0.811821 0.286911 0.066 Uiso 1 1 calc R U . . . H42B H 0.037919 0.833785 0.202814 0.066 Uiso 1 1 calc R U . . . H42C H 0.025163 0.920322 0.230412 0.066 Uiso 1 1 calc R U . . . C43 C 0.5254(2) 0.40806(19) 0.36215(18) 0.0235(6) Uani 1 1 d . . . . . H43A H 0.578(2) 0.4488(19) 0.3216(17) 0.022(7) Uiso 1 1 d . . . . . C44 C 0.5818(2) 0.30453(19) 0.39051(17) 0.0220(6) Uani 1 1 d . . . . . C45 C 0.6794(2) 0.27132(19) 0.33548(17) 0.0213(6) Uani 1 1 d . . . . . H45A H 0.705462 0.318419 0.282353 0.026 Uiso 1 1 calc R U . . . C46 C 0.7384(2) 0.17350(19) 0.35557(17) 0.0225(6) Uani 1 1 d . . . . . H46A H 0.803204 0.156189 0.315992 0.027 Uiso 1 1 calc R U . . . C47 C 0.7057(2) 0.10010(19) 0.43185(18) 0.0241(6) Uani 1 1 d . . . . . C48 C 0.6092(2) 0.13177(19) 0.48668(18) 0.0267(6) Uani 1 1 d . . . . . H48A H 0.584335 0.083928 0.539760 0.032 Uiso 1 1 calc R U . . . C49 C 0.5485(2) 0.2285(2) 0.46783(18) 0.0262(6) Uani 1 1 d . . . . . H49A H 0.483020 0.244762 0.507439 0.031 Uiso 1 1 calc R U . . . C50 C 0.7695(3) -0.0085(2) 0.45714(19) 0.0310(7) Uani 1 1 d . . . . . C51 C 0.8227(3) -0.0528(2) 0.5474(2) 0.0408(8) Uani 1 1 d . . . . . H51A H 0.757499 -0.044455 0.592870 0.061 Uiso 1 1 calc R U . . . H51B H 0.881023 -0.019759 0.543273 0.061 Uiso 1 1 calc R U . . . H51C H 0.863473 -0.122351 0.563709 0.061 Uiso 1 1 calc R U . . . C52 C 0.6795(3) -0.0606(2) 0.4626(2) 0.0394(8) Uani 1 1 d . . . . . H52A H 0.644980 -0.031348 0.405083 0.059 Uiso 1 1 calc R U . . . H52B H 0.614580 -0.053841 0.508686 0.059 Uiso 1 1 calc R U . . . H52C H 0.721188 -0.129762 0.477485 0.059 Uiso 1 1 calc R U . . . C53 C 0.8733(3) -0.0259(2) 0.3885(2) 0.0377(7) Uani 1 1 d . . . . . H53A H 0.841516 0.001837 0.330169 0.057 Uiso 1 1 calc R U . . . H53B H 0.911393 -0.096082 0.406579 0.057 Uiso 1 1 calc R U . . . H53C H 0.933375 0.005381 0.384779 0.057 Uiso 1 1 calc R U . . . C54 C 0.4345(2) 0.45949(19) 0.41070(17) 0.0231(6) Uani 1 1 d . . . . . C55 C 0.4364(2) 0.55235(19) 0.39846(17) 0.0250(6) Uani 1 1 d . . . . . H55A H 0.503209 0.575314 0.364665 0.030 Uiso 1 1 calc R U . . . C56 C 0.3450(2) 0.6113(2) 0.43358(17) 0.0238(6) Uani 1 1 d . . . . . H56A H 0.350605 0.673469 0.422145 0.029 Uiso 1 1 calc R U . . . C57 C 0.2448(2) 0.58179(19) 0.48540(17) 0.0234(6) Uani 1 1 d . . . . . C58 C 0.2450(2) 0.48814(19) 0.50138(17) 0.0248(6) Uani 1 1 d . . . . . H58A H 0.180298 0.464053 0.538240 0.030 Uiso 1 1 calc R U . . . C59 C 0.3349(2) 0.42917(19) 0.46599(17) 0.0245(6) Uani 1 1 d . . . . . H59A H 0.329760 0.366338 0.479153 0.029 Uiso 1 1 calc R U . . . C60 C 0.1435(2) 0.6425(2) 0.52911(18) 0.0271(6) Uani 1 1 d . . . . . C61 C 0.1488(3) 0.5889(2) 0.63035(18) 0.0328(7) Uani 1 1 d . . . . . H61A H 0.228518 0.579479 0.646283 0.049 Uiso 1 1 calc R U . . . H61B H 0.134983 0.525395 0.650286 0.049 Uiso 1 1 calc R U . . . H61C H 0.086286 0.627627 0.659167 0.049 Uiso 1 1 calc R U . . . C62 C 0.0194(2) 0.6556(2) 0.5042(2) 0.0319(7) Uani 1 1 d . . . . . H62A H -0.044117 0.692444 0.534222 0.048 Uiso 1 1 calc R U . . . H62B H 0.007814 0.591510 0.522913 0.048 Uiso 1 1 calc R U . . . H62C H 0.015150 0.691117 0.439695 0.048 Uiso 1 1 calc R U . . . C63 C 0.1570(3) 0.7445(2) 0.5002(2) 0.0317(7) Uani 1 1 d . . . . . H63A H 0.235375 0.738285 0.515835 0.048 Uiso 1 1 calc R U . . . H63B H 0.092008 0.780007 0.530557 0.048 Uiso 1 1 calc R U . . . H63C H 0.152060 0.780166 0.435698 0.048 Uiso 1 1 calc R U . . . 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 Ca1 0.0235(3) 0.0225(3) 0.0241(3) -0.0061(2) -0.0023(2) -0.0081(2) Na1 0.0252(6) 0.0204(5) 0.0211(6) -0.0066(5) -0.0004(4) -0.0101(4) C1 0.0283(16) 0.0258(15) 0.0178(15) -0.0058(13) -0.0025(12) -0.0096(12) C2 0.0177(14) 0.0249(15) 0.0267(15) -0.0083(12) 0.0002(11) -0.0114(12) C3 0.0271(15) 0.0229(14) 0.0210(15) -0.0050(12) 0.0013(11) -0.0129(12) C4 0.0265(15) 0.0198(14) 0.0282(16) -0.0037(12) -0.0021(12) -0.0093(12) C5 0.0213(14) 0.0219(14) 0.0260(15) -0.0086(12) 0.0009(11) -0.0084(12) C6 0.0208(14) 0.0233(14) 0.0230(15) -0.0063(12) -0.0029(11) -0.0093(12) C7 0.0209(14) 0.0181(14) 0.0269(15) -0.0043(12) -0.0060(11) -0.0076(11) C8 0.0274(16) 0.0212(15) 0.0303(17) -0.0088(13) 0.0011(12) -0.0066(12) C9 0.0282(17) 0.0324(18) 0.071(2) -0.0298(18) 0.0023(16) -0.0059(14) C10 0.067(3) 0.040(2) 0.040(2) -0.0243(17) -0.0039(17) 0.0061(18) C11 0.0385(19) 0.0281(17) 0.058(2) -0.0223(16) 0.0083(15) -0.0132(14) C12 0.0218(14) 0.0217(14) 0.0255(15) -0.0083(12) -0.0006(11) -0.0099(12) C13 0.0281(16) 0.0257(15) 0.0267(16) -0.0106(13) -0.0020(12) -0.0096(13) C14 0.0287(16) 0.0255(15) 0.0355(17) -0.0177(14) 0.0027(13) -0.0088(13) C15 0.0261(15) 0.0212(14) 0.0311(17) -0.0077(13) -0.0011(12) -0.0106(12) C16 0.0259(15) 0.0283(16) 0.0263(16) -0.0097(13) -0.0026(12) -0.0089(13) C17 0.0228(15) 0.0262(15) 0.0268(16) -0.0117(13) 0.0002(11) -0.0066(12) C18 0.0236(16) 0.0273(16) 0.0415(19) -0.0158(14) -0.0036(13) -0.0029(12) C19 0.037(2) 0.0275(17) 0.082(3) -0.0210(19) -0.0146(18) -0.0010(15) C20 0.0332(18) 0.0361(18) 0.051(2) -0.0155(16) -0.0100(15) -0.0034(15) C21 0.0294(18) 0.054(2) 0.051(2) -0.0206(19) -0.0030(15) -0.0062(16) C22 0.0223(14) 0.0235(14) 0.0189(14) -0.0079(12) -0.0021(11) -0.0108(12) C23 0.0239(14) 0.0188(13) 0.0122(13) -0.0022(11) 0.0010(10) -0.0088(11) C24 0.0205(14) 0.0243(15) 0.0188(14) -0.0078(12) -0.0009(11) -0.0094(12) C25 0.0249(15) 0.0184(14) 0.0178(14) -0.0064(11) 0.0016(11) -0.0062(11) C26 0.0204(14) 0.0185(13) 0.0124(13) -0.0008(11) 0.0008(10) -0.0063(11) C27 0.0246(15) 0.0221(14) 0.0192(14) -0.0069(12) 0.0023(11) -0.0128(12) C28 0.0226(14) 0.0179(13) 0.0197(14) -0.0066(11) 0.0019(11) -0.0078(11) C29 0.0196(14) 0.0230(14) 0.0214(15) -0.0074(12) -0.0002(11) -0.0055(11) C30 0.0204(14) 0.0285(15) 0.0284(16) -0.0115(13) 0.0011(12) -0.0056(12) C31 0.0224(15) 0.0332(16) 0.0276(16) -0.0077(14) -0.0027(12) -0.0049(13) C32 0.0236(16) 0.0247(15) 0.0393(18) -0.0107(14) -0.0017(13) -0.0037(12) C33 0.0241(15) 0.0193(14) 0.0147(13) -0.0018(11) -0.0011(11) -0.0082(11) C34 0.0234(15) 0.0244(15) 0.0233(15) -0.0087(12) -0.0039(11) -0.0077(12) C35 0.0185(14) 0.0241(15) 0.0276(16) -0.0058(13) -0.0050(11) -0.0040(12) C36 0.0242(15) 0.0221(14) 0.0267(16) -0.0087(13) 0.0013(12) -0.0092(12) C37 0.0245(15) 0.0260(15) 0.0290(16) -0.0125(13) -0.0020(12) -0.0105(12) C38 0.0181(14) 0.0244(15) 0.0265(15) -0.0075(12) -0.0035(11) -0.0060(12) C39 0.0280(16) 0.0205(15) 0.0373(18) -0.0128(14) -0.0023(13) -0.0035(12) C40 0.077(3) 0.0261(18) 0.048(2) -0.0131(17) -0.0121(19) 0.0028(18) C41 0.037(2) 0.0397(19) 0.083(3) -0.041(2) -0.0047(18) -0.0060(16) C42 0.0353(19) 0.045(2) 0.059(2) -0.0335(19) 0.0054(16) -0.0078(16) C43 0.0244(15) 0.0217(14) 0.0188(14) -0.0038(12) 0.0001(11) -0.0071(12) C44 0.0209(14) 0.0248(14) 0.0185(14) -0.0053(12) -0.0032(11) -0.0079(12) C45 0.0227(14) 0.0211(14) 0.0173(14) -0.0035(11) -0.0016(11) -0.0087(11) C46 0.0183(14) 0.0260(15) 0.0230(15) -0.0104(12) 0.0009(11) -0.0071(12) C47 0.0191(14) 0.0224(14) 0.0238(15) -0.0036(12) -0.0038(11) -0.0043(11) C48 0.0225(15) 0.0233(15) 0.0241(15) -0.0007(12) -0.0021(11) -0.0067(12) C49 0.0204(14) 0.0324(16) 0.0215(15) -0.0089(13) 0.0015(11) -0.0072(12) C50 0.0271(16) 0.0219(15) 0.0319(17) -0.0036(13) -0.0032(12) -0.0022(12) C51 0.0350(18) 0.0322(17) 0.0310(18) 0.0004(14) -0.0091(14) 0.0045(14) C52 0.0428(19) 0.0186(15) 0.043(2) -0.0017(14) -0.0031(15) -0.0072(14) C53 0.0354(18) 0.0240(16) 0.0384(19) -0.0090(14) -0.0031(14) 0.0045(13) C54 0.0235(15) 0.0227(14) 0.0172(14) -0.0044(12) -0.0029(11) -0.0040(12) C55 0.0241(15) 0.0278(15) 0.0213(15) -0.0079(13) -0.0024(11) -0.0077(12) C56 0.0272(15) 0.0238(14) 0.0186(14) -0.0076(12) -0.0054(11) -0.0046(12) C57 0.0220(14) 0.0256(15) 0.0202(14) -0.0090(12) -0.0052(11) -0.0023(12) C58 0.0234(15) 0.0286(15) 0.0195(15) -0.0059(12) -0.0012(11) -0.0095(12) C59 0.0273(15) 0.0211(14) 0.0216(15) -0.0059(12) -0.0024(11) -0.0065(12) C60 0.0257(15) 0.0306(16) 0.0251(16) -0.0136(13) -0.0014(12) -0.0054(13) C61 0.0327(17) 0.0377(18) 0.0271(17) -0.0159(14) 0.0002(13) -0.0066(14) C62 0.0259(16) 0.0378(17) 0.0341(17) -0.0210(15) -0.0011(13) -0.0038(13) C63 0.0301(16) 0.0337(17) 0.0325(17) -0.0183(14) -0.0050(13) -0.0023(13) 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' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 '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 C22 Ca1 C43 99.71(8) . . ? C22 Ca1 C23 31.80(8) . . ? C43 Ca1 C23 96.19(8) . . ? C22 Ca1 C45 119.40(8) . . ? C43 Ca1 C45 55.33(8) . . ? C23 Ca1 C45 91.25(8) . . ? C22 Ca1 C44 125.66(8) . . ? C43 Ca1 C44 31.55(8) . . ? C23 Ca1 C44 108.90(8) . . ? C45 Ca1 C44 30.66(8) . . ? C22 Ca1 C3 132.55(8) . . ? C43 Ca1 C3 95.57(8) . . ? C23 Ca1 C3 162.36(8) . . ? C45 Ca1 C3 106.25(8) . . ? C44 Ca1 C3 87.86(8) . . ? C22 Ca1 C2 102.06(8) . . ? C43 Ca1 C2 101.40(8) . . ? C23 Ca1 C2 133.23(8) . . ? C45 Ca1 C2 134.07(8) . . ? C44 Ca1 C2 108.60(8) . . ? C3 Ca1 C2 30.59(8) . . ? C22 Ca1 C24 54.96(8) . . ? C43 Ca1 C24 116.25(8) . . ? C23 Ca1 C24 30.20(7) . . ? C45 Ca1 C24 85.60(8) . . ? C44 Ca1 C24 113.58(8) . . ? C3 Ca1 C24 146.59(8) . . ? C2 Ca1 C24 137.67(8) . . ? C22 Ca1 C4 141.64(9) . . ? C43 Ca1 C4 112.81(9) . . ? C23 Ca1 C4 149.02(8) . . ? C45 Ca1 C4 96.32(8) . . ? C44 Ca1 C4 92.06(8) . . ? C3 Ca1 C4 29.11(8) . . ? C2 Ca1 C4 53.22(8) . . ? C24 Ca1 C4 120.48(8) . . ? C22 Ca1 C7 84.55(8) . . ? C43 Ca1 C7 128.63(8) . . ? C23 Ca1 C7 110.62(8) . . ? C45 Ca1 C7 155.77(8) . . ? C44 Ca1 C7 137.85(8) . . ? C3 Ca1 C7 51.79(8) . . ? C2 Ca1 C7 29.86(8) . . ? C24 Ca1 C7 107.89(8) . . ? C4 Ca1 C7 59.57(8) . . ? C22 Ca1 C6 92.16(8) . . ? C43 Ca1 C6 153.06(8) . . ? C23 Ca1 C6 106.31(8) . . ? C45 Ca1 C6 136.54(8) . . ? C44 Ca1 C6 141.94(8) . . ? C3 Ca1 C6 59.32(8) . . ? C2 Ca1 C6 52.19(7) . . ? C24 Ca1 C6 90.37(8) . . ? C4 Ca1 C6 49.88(8) . . ? C7 Ca1 C6 28.41(7) . . ? C22 Ca1 C5 117.40(8) . . ? C43 Ca1 C5 141.32(8) . . ? C23 Ca1 C5 120.90(7) . . ? C45 Ca1 C5 109.14(8) . . ? C44 Ca1 C5 116.43(8) . . ? C3 Ca1 C5 51.70(8) . . ? C2 Ca1 C5 62.21(7) . . ? C24 Ca1 C5 95.00(7) . . ? C4 Ca1 C5 28.74(7) . . ? C7 Ca1 C5 51.03(7) . . ? C6 Ca1 C5 28.16(7) . . ? C22 Ca1 H22A 20.3(5) . . ? C43 Ca1 H22A 118.6(5) . . ? C23 Ca1 H22A 43.9(5) . . ? C45 Ca1 H22A 135.1(5) . . ? C44 Ca1 H22A 146.0(5) . . ? C3 Ca1 H22A 118.6(5) . . ? C2 Ca1 H22A 90.2(5) . . ? C24 Ca1 H22A 55.8(5) . . ? C4 Ca1 H22A 121.6(5) . . ? C7 Ca1 H22A 67.3(5) . . ? C6 Ca1 H22A 71.9(5) . . ? C5 Ca1 H22A 97.3(5) . . ? C22 Ca1 H24A 58.2(5) . . ? C43 Ca1 H24A 136.0(6) . . ? C23 Ca1 H24A 44.0(5) . . ? C45 Ca1 H24A 100.0(6) . . ? C44 Ca1 H24A 130.1(6) . . ? C3 Ca1 H24A 127.8(6) . . ? C2 Ca1 H24A 119.3(6) . . ? C24 Ca1 H24A 19.8(5) . . ? C4 Ca1 H24A 105.0(5) . . ? C7 Ca1 H24A 89.5(6) . . ? C6 Ca1 H24A 70.5(6) . . ? C5 Ca1 H24A 77.4(5) . . ? H22A Ca1 H24A 50.7(7) . . ? C1 Na1 C55 122.98(9) . . ? C1 Na1 C54 93.33(8) . . ? C55 Na1 C54 30.16(8) . . ? C1 Na1 C12 30.21(8) . . ? C55 Na1 C12 148.04(9) . . ? C54 Na1 C12 121.37(8) . . ? C1 Na1 C35 104.67(8) . . ? C55 Na1 C35 127.31(9) . . ? C54 Na1 C35 145.75(8) . . ? C12 Na1 C35 84.59(8) . . ? C1 Na1 C34 89.86(8) . . ? C55 Na1 C34 124.51(8) . . ? C54 Na1 C34 126.42(8) . . ? C12 Na1 C34 81.94(8) . . ? C35 Na1 C34 28.06(7) . . ? C1 Na1 C13 52.37(8) . . ? C55 Na1 C13 135.05(9) . . ? C54 Na1 C13 123.14(9) . . ? C12 Na1 C13 28.88(7) . . ? C35 Na1 C13 90.58(8) . . ? C34 Na1 C13 100.37(8) . . ? C1 Na1 C56 129.95(9) . . ? C55 Na1 C56 28.28(7) . . ? C54 Na1 C56 51.55(8) . . ? C12 Na1 C56 138.01(8) . . ? C35 Na1 C56 124.46(8) . . ? C34 Na1 C56 138.38(8) . . ? C13 Na1 C56 113.13(8) . . ? C1 Na1 C37 146.20(9) . . ? C55 Na1 C37 78.69(8) . . ? C54 Na1 C37 101.97(8) . . ? C12 Na1 C37 133.21(8) . . ? C35 Na1 C37 48.63(8) . . ? C34 Na1 C37 56.81(7) . . ? C13 Na1 C37 132.42(9) . . ? C56 Na1 C37 82.00(8) . . ? C1 Na1 C36 132.60(9) . . ? C55 Na1 C36 102.49(8) . . ? C54 Na1 C36 128.96(8) . . ? C12 Na1 C36 108.89(8) . . ? C35 Na1 C36 28.24(7) . . ? C34 Na1 C36 50.01(7) . . ? C13 Na1 C36 104.82(8) . . ? C56 Na1 C36 96.25(8) . . ? C37 Na1 C36 27.71(7) . . ? C1 Na1 C38 125.41(8) . . ? C55 Na1 C38 76.36(8) . . ? C54 Na1 C38 88.74(8) . . ? C12 Na1 C38 129.74(8) . . ? C35 Na1 C38 57.06(8) . . ? C34 Na1 C38 48.64(7) . . ? C13 Na1 C38 147.16(9) . . ? C56 Na1 C38 92.18(8) . . ? C37 Na1 C38 27.51(7) . . ? C36 Na1 C38 49.47(7) . . ? C1 Na1 C33 98.92(8) . . ? C55 Na1 C33 97.83(8) . . ? C54 Na1 C33 98.92(8) . . ? C12 Na1 C33 103.23(8) . . ? C35 Na1 C33 50.17(7) . . ? C34 Na1 C33 28.29(7) . . ? C13 Na1 C33 126.81(8) . . ? C56 Na1 C33 118.60(8) . . ? C37 Na1 C33 49.31(7) . . ? C36 Na1 C33 59.11(7) . . ? C38 Na1 C33 27.67(7) . . ? C1 Na1 H13A 58.2(5) . . ? C55 Na1 H13A 114.3(6) . . ? C54 Na1 H13A 105.3(6) . . ? C12 Na1 H13A 44.8(6) . . ? C35 Na1 H13A 108.9(6) . . ? C34 Na1 H13A 121.1(6) . . ? C13 Na1 H13A 20.7(6) . . ? C56 Na1 H13A 94.1(6) . . ? C37 Na1 H13A 141.3(5) . . ? C36 Na1 H13A 116.7(6) . . ? C38 Na1 H13A 165.5(6) . . ? C33 Na1 H13A 147.1(6) . . ? C2 C1 C12 130.5(2) . . ? C2 C1 Na1 119.93(18) . . ? C12 C1 Na1 80.61(15) . . ? C2 C1 H1A 114.6(14) . . ? C12 C1 H1A 112.3(14) . . ? Na1 C1 H1A 82.6(14) . . ? C1 C2 C7 127.7(2) . . ? C1 C2 C3 118.6(2) . . ? C7 C2 C3 113.5(2) . . ? C1 C2 Ca1 115.06(17) . . ? C7 C2 Ca1 76.66(14) . . ? C3 C2 Ca1 72.54(14) . . ? C4 C3 C2 123.0(2) . . ? C4 C3 Ca1 78.45(15) . . ? C2 C3 Ca1 76.87(14) . . ? C4 C3 H3A 118.5 . . ? C2 C3 H3A 118.5 . . ? Ca1 C3 H3A 116.6 . . ? C3 C4 C5 122.7(3) . . ? C3 C4 Ca1 72.44(15) . . ? C5 C4 Ca1 80.83(15) . . ? C3 C4 H4A 118.6 . . ? C5 C4 H4A 118.6 . . ? Ca1 C4 H4A 118.8 . . ? C6 C5 C4 115.3(2) . . ? C6 C5 C8 123.9(2) . . ? C4 C5 C8 120.7(2) . . ? C6 C5 Ca1 74.76(14) . . ? C4 C5 Ca1 70.43(14) . . ? C8 C5 Ca1 126.67(17) . . ? C7 C6 C5 122.7(2) . . ? C7 C6 Ca1 72.61(14) . . ? C5 C6 Ca1 77.08(15) . . ? C7 C6 H6A 118.7 . . ? C5 C6 H6A 118.7 . . ? Ca1 C6 H6A 123.0 . . ? C6 C7 C2 122.7(2) . . ? C6 C7 Ca1 78.98(15) . . ? C2 C7 Ca1 73.48(14) . . ? C6 C7 H7A 118.6 . . ? C2 C7 H7A 118.6 . . ? Ca1 C7 H7A 119.7 . . ? C10 C8 C5 111.6(2) . . ? C10 C8 C11 109.0(3) . . ? C5 C8 C11 108.6(2) . . ? C10 C8 C9 109.4(3) . . ? C5 C8 C9 109.2(2) . . ? C11 C8 C9 109.0(2) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C17 C12 C13 114.2(2) . . ? C17 C12 C1 127.7(2) . . ? C13 C12 C1 118.1(2) . . ? C17 C12 Na1 126.15(18) . . ? C13 C12 Na1 77.42(15) . . ? C1 C12 Na1 69.18(14) . . ? C14 C13 C12 122.8(3) . . ? C14 C13 Na1 130.00(19) . . ? C12 C13 Na1 73.70(15) . . ? C14 C13 H13A 119.1(14) . . ? C12 C13 H13A 118.1(14) . . ? Na1 C13 H13A 68.9(15) . . ? C13 C14 C15 121.9(2) . . ? C13 C14 H14A 119.0 . . ? C15 C14 H14A 119.0 . . ? C16 C15 C14 115.6(3) . . ? C16 C15 C18 123.7(2) . . ? C14 C15 C18 120.7(2) . . ? C17 C16 C15 123.5(3) . . ? C17 C16 H16A 118.2 . . ? C15 C16 H16A 118.2 . . ? C16 C17 C12 121.8(2) . . ? C16 C17 H17A 119.1 . . ? C12 C17 H17A 119.1 . . ? C19 C18 C20 107.3(3) . . ? C19 C18 C15 109.4(2) . . ? C20 C18 C15 112.4(2) . . ? C19 C18 C21 110.3(3) . . ? C20 C18 C21 108.1(2) . . ? C15 C18 C21 109.4(2) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C33 C22 C23 131.8(2) . . ? C33 C22 Ca1 112.27(17) . . ? C23 C22 Ca1 79.59(15) . . ? C33 C22 H22A 114.0(15) . . ? C23 C22 H22A 113.3(15) . . ? Ca1 C22 H22A 86.1(15) . . ? C24 C23 C28 113.7(2) . . ? C24 C23 C22 118.2(2) . . ? C28 C23 C22 128.0(2) . . ? C24 C23 Ca1 77.59(14) . . ? C28 C23 Ca1 120.36(16) . . ? C22 C23 Ca1 68.61(14) . . ? C25 C24 C23 123.5(2) . . ? C25 C24 Ca1 123.12(18) . . ? C23 C24 Ca1 72.21(14) . . ? C25 C24 H24A 119.8(15) . . ? C23 C24 H24A 116.6(15) . . ? Ca1 C24 H24A 77.7(15) . . ? C24 C25 C26 121.8(2) . . ? C24 C25 H25A 119.1 . . ? C26 C25 H25A 119.1 . . ? C25 C26 C27 115.6(2) . . ? C25 C26 C29 123.5(2) . . ? C27 C26 C29 120.9(2) . . ? C28 C27 C26 123.6(2) . . ? C28 C27 H27A 118.2 . . ? C26 C27 H27A 118.2 . . ? C27 C28 C23 122.0(2) . . ? C27 C28 H28A 119.0 . . ? C23 C28 H28A 119.0 . . ? C32 C29 C30 108.5(2) . . ? C32 C29 C26 111.9(2) . . ? C30 C29 C26 108.7(2) . . ? C32 C29 C31 108.1(2) . . ? C30 C29 C31 108.9(2) . . ? C26 C29 C31 110.7(2) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C38 C33 C34 113.7(2) . . ? C38 C33 C22 127.3(2) . . ? C34 C33 C22 119.0(2) . . ? C38 C33 Na1 74.23(14) . . ? C34 C33 Na1 70.76(14) . . ? C22 C33 Na1 121.63(16) . . ? C35 C34 C33 122.9(2) . . ? C35 C34 Na1 74.94(15) . . ? C33 C34 Na1 80.94(15) . . ? C35 C34 H34A 118.6 . . ? C33 C34 H34A 118.6 . . ? Na1 C34 H34A 115.9 . . ? C34 C35 C36 122.7(2) . . ? C34 C35 Na1 77.00(16) . . ? C36 C35 Na1 79.84(16) . . ? C34 C35 H35A 118.6 . . ? C36 C35 H35A 118.6 . . ? Na1 C35 H35A 114.8 . . ? C37 C36 C35 115.0(2) . . ? C37 C36 C39 123.5(2) . . ? C35 C36 C39 121.5(2) . . ? C37 C36 Na1 75.76(15) . . ? C35 C36 Na1 71.92(15) . . ? C39 C36 Na1 121.95(17) . . ? C38 C37 C36 123.0(2) . . ? C38 C37 Na1 76.91(15) . . ? C36 C37 Na1 76.52(15) . . ? C38 C37 H37A 118.5 . . ? C36 C37 H37A 118.5 . . ? Na1 C37 H37A 118.8 . . ? C37 C38 C33 122.6(2) . . ? C37 C38 Na1 75.58(15) . . ? C33 C38 Na1 78.10(14) . . ? C37 C38 H38A 118.7 . . ? C33 C38 H38A 118.7 . . ? Na1 C38 H38A 118.3 . . ? C36 C39 C41 112.6(2) . . ? C36 C39 C42 109.7(2) . . ? C41 C39 C42 107.4(2) . . ? C36 C39 C40 109.0(2) . . ? C41 C39 C40 109.1(3) . . ? C42 C39 C40 108.9(3) . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C39 C41 H41A 109.5 . . ? C39 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C39 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C39 C42 H42A 109.5 . . ? C39 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C39 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44 C43 C54 128.5(2) . . ? C44 C43 Ca1 77.12(14) . . ? C54 C43 Ca1 127.11(18) . . ? C44 C43 H43A 114.4(15) . . ? C54 C43 H43A 110.3(14) . . ? Ca1 C43 H43A 90.5(14) . . ? C45 C44 C49 114.1(2) . . ? C45 C44 C43 118.5(2) . . ? C49 C44 C43 127.4(2) . . ? C45 C44 Ca1 74.58(14) . . ? C49 C44 Ca1 123.18(17) . . ? C43 C44 Ca1 71.33(14) . . ? C46 C45 C44 123.2(2) . . ? C46 C45 Ca1 123.73(17) . . ? C44 C45 Ca1 74.76(14) . . ? C46 C45 H45A 118.4 . . ? C44 C45 H45A 118.4 . . ? Ca1 C45 H45A 72.1 . . ? C45 C46 C47 122.0(2) . . ? C45 C46 H46A 119.0 . . ? C47 C46 H46A 119.0 . . ? C46 C47 C48 115.4(2) . . ? C46 C47 C50 123.6(2) . . ? C48 C47 C50 120.9(2) . . ? C49 C48 C47 123.7(3) . . ? C49 C48 H48A 118.2 . . ? C47 C48 H48A 118.2 . . ? C48 C49 C44 121.6(2) . . ? C48 C49 H49A 119.2 . . ? C44 C49 H49A 119.2 . . ? C52 C50 C47 109.8(2) . . ? C52 C50 C53 107.9(2) . . ? C47 C50 C53 111.8(2) . . ? C52 C50 C51 109.9(2) . . ? C47 C50 C51 109.4(2) . . ? C53 C50 C51 108.0(2) . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C50 C52 H52A 109.5 . . ? C50 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C50 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C50 C53 H53A 109.5 . . ? C50 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C50 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C55 C54 C59 114.5(2) . . ? C55 C54 C43 119.3(2) . . ? C59 C54 C43 126.0(2) . . ? C55 C54 Na1 73.50(15) . . ? C59 C54 Na1 85.57(16) . . ? C43 C54 Na1 104.99(17) . . ? C56 C55 C54 122.9(3) . . ? C56 C55 Na1 84.23(16) . . ? C54 C55 Na1 76.35(15) . . ? C56 C55 H55A 118.5 . . ? C54 C55 H55A 118.5 . . ? Na1 C55 H55A 110.6 . . ? C55 C56 C57 121.9(2) . . ? C55 C56 Na1 67.48(14) . . ? C57 C56 Na1 86.83(15) . . ? C55 C56 H56A 119.1 . . ? C57 C56 H56A 119.1 . . ? Na1 C56 H56A 116.8 . . ? C56 C57 C58 115.6(2) . . ? C56 C57 C60 124.0(2) . . ? C58 C57 C60 120.2(2) . . ? C59 C58 C57 123.0(2) . . ? C59 C58 H58A 118.5 . . ? C57 C58 H58A 118.5 . . ? C58 C59 C54 122.0(2) . . ? C58 C59 Na1 84.85(16) . . ? C54 C59 Na1 66.18(15) . . ? C58 C59 H59A 119.0 . . ? C54 C59 H59A 119.0 . . ? Na1 C59 H59A 120.6 . . ? C61 C60 C62 109.3(2) . . ? C61 C60 C63 108.5(2) . . ? C62 C60 C63 107.8(2) . . ? C61 C60 C57 108.4(2) . . ? C62 C60 C57 110.6(2) . . ? C63 C60 C57 112.1(2) . . ? C60 C61 H61A 109.5 . . ? C60 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C60 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C60 C62 H62A 109.5 . . ? C60 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C60 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C60 C63 H63A 109.5 . . ? C60 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C60 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? 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 Ca1 C22 2.544(3) . ? Ca1 C43 2.614(3) . ? Ca1 C23 2.688(2) . ? Ca1 C45 2.688(3) . ? Ca1 C44 2.690(3) . ? Ca1 C3 2.691(3) . ? Ca1 C2 2.747(2) . ? Ca1 C24 2.757(3) . ? Ca1 C4 2.765(3) . ? Ca1 C7 2.788(3) . ? Ca1 C6 2.868(2) . ? Ca1 C5 2.897(3) . ? Ca1 H22A 2.65(2) . ? Ca1 H24A 2.72(2) . ? Na1 C1 2.672(3) . ? Na1 C55 2.700(3) . ? Na1 C54 2.737(3) . ? Na1 C12 2.820(3) . ? Na1 C35 2.824(3) . ? Na1 C34 2.849(3) . ? Na1 C13 2.868(3) . ? Na1 C56 2.908(3) . ? Na1 C37 2.914(3) . ? Na1 C36 2.924(3) . ? Na1 C38 2.931(3) . ? Na1 C33 2.980(3) . ? Na1 H13A 2.68(3) . ? C1 C2 1.416(4) . ? C1 C12 1.438(4) . ? C1 H1A 0.95(2) . ? C2 C7 1.427(4) . ? C2 C3 1.436(4) . ? C3 C4 1.373(4) . ? C3 H3A 0.9500 . ? C4 C5 1.411(4) . ? C4 H4A 0.9500 . ? C5 C6 1.403(4) . ? C5 C8 1.534(4) . ? C6 C7 1.390(4) . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? C8 C10 1.511(4) . ? C8 C11 1.536(4) . ? C8 C9 1.541(4) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C17 1.416(4) . ? C12 C13 1.419(4) . ? C13 C14 1.381(4) . ? C13 H13A 1.01(3) . ? C14 C15 1.398(4) . ? C14 H14A 0.9500 . ? C15 C16 1.386(4) . ? C15 C18 1.534(4) . ? C16 C17 1.376(4) . ? C16 H16A 0.9500 . ? C17 H17A 0.9500 . ? C18 C19 1.523(4) . ? C18 C20 1.528(4) . ? C18 C21 1.536(4) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C33 1.431(4) . ? C22 C23 1.440(4) . ? C22 H22A 0.92(2) . ? C23 C24 1.420(3) . ? C23 C28 1.423(3) . ? C24 C25 1.387(4) . ? C24 H24A 0.94(3) . ? C25 C26 1.392(3) . ? C25 H25A 0.9500 . ? C26 C27 1.394(3) . ? C26 C29 1.535(3) . ? C27 C28 1.378(4) . ? C27 H27A 0.9500 . ? C28 H28A 0.9500 . ? C29 C32 1.532(4) . ? C29 C30 1.532(4) . ? C29 C31 1.538(4) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C38 1.414(3) . ? C33 C34 1.430(4) . ? C34 C35 1.376(4) . ? C34 H34A 0.9500 . ? C35 C36 1.406(4) . ? C35 H35A 0.9500 . ? C36 C37 1.398(4) . ? C36 C39 1.519(4) . ? C37 C38 1.390(4) . ? C37 H37A 0.9500 . ? C38 H38A 0.9500 . ? C39 C41 1.525(4) . ? C39 C42 1.533(4) . ? C39 C40 1.537(4) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.444(4) . ? C43 C54 1.451(4) . ? C43 H43A 0.99(3) . ? C44 C45 1.422(4) . ? C44 C49 1.422(4) . ? C45 C46 1.388(4) . ? C45 H45A 0.9500 . ? C46 C47 1.390(4) . ? C46 H46A 0.9500 . ? C47 C48 1.403(4) . ? C47 C50 1.531(4) . ? C48 C49 1.380(4) . ? C48 H48A 0.9500 . ? C49 H49A 0.9500 . ? C50 C52 1.531(4) . ? C50 C53 1.534(4) . ? C50 C51 1.536(4) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 C55 1.415(4) . ? C54 C59 1.416(4) . ? C55 C56 1.385(4) . ? C55 H55A 0.9500 . ? C56 C57 1.399(4) . ? C56 H56A 0.9500 . ? C57 C58 1.400(4) . ? C57 C60 1.539(4) . ? C58 C59 1.381(4) . ? C58 H58A 0.9500 . ? C59 H59A 0.9500 . ? C60 C61 1.534(4) . ? C60 C62 1.535(4) . ? C60 C63 1.538(4) . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ?