#------------------------------------------------------------------------------ #$Date: 2019-05-17 04:32:53 +0300 (Fri, 17 May 2019) $ #$Revision: 215227 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/00/7700003.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_7700003 loop_ _publ_author_name 'Santra, Biswajit' 'Narayanan, Suriya' 'Kalita, Pankaj' 'Kumar, Vierandra' 'Mandal, Debdeep' 'Gupta, Vivek' 'Zimmer, Michael' 'Huch, Volker' 'Chandrasekhar, Vadapalli' 'Scheschkewitz, David' 'Schulzke, Carola' 'Jana, Anukul' _publ_section_title ; Modulation of the Nuclearity of Molecular Mg(II)-Phosphates: Solid-State Structural Change Involving Coordinating Solvents ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/C9DT00687G _journal_year 2019 _chemical_formula_moiety 'C144 H164 Mg4 O32 P4, 4(C3 H7 N O), 2(C H Cl3), 8(H2O)' _chemical_formula_sum 'C158 H210 Cl6 Mg4 N4 O44 P4' _chemical_formula_weight 3303.11 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2019-04-29 deposited with the CCDC. 2019-05-16 downloaded from the CCDC. ; _cell_angle_alpha 87.4830(10) _cell_angle_beta 76.5730(10) _cell_angle_gamma 83.5070(10) _cell_formula_units_Z 1 _cell_length_a 10.49570(10) _cell_length_b 20.6949(3) _cell_length_c 21.1795(3) _cell_measurement_reflns_used 29539 _cell_measurement_temperature 148(2) _cell_measurement_theta_max 28.8630 _cell_measurement_theta_min 2.9610 _cell_volume 4445.16(10) _computing_cell_refinement 'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)' _computing_data_collection 'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)' _computing_data_reduction 'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 148(2) _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.870 _diffrn_measurement_device_type 'XtaLAB AFC12 (RINC): Kappa single' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0406 _diffrn_reflns_av_unetI/netI 0.0389 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.870 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 100352 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.870 _diffrn_reflns_theta_full 25.000 _diffrn_reflns_theta_max 29.114 _diffrn_reflns_theta_min 2.474 _diffrn_source 'fine-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 0.221 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.95672 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.234 _exptl_crystal_description block _exptl_crystal_F_000 1748 _exptl_crystal_size_max 0.230 _exptl_crystal_size_mid 0.180 _exptl_crystal_size_min 0.120 _platon_squeeze_details ; The SQUEEZE/PLATON procedure yielded total void volume and electron count of 405\%A^3^ and 105 e, respectively. This falls slightly short of equalling two further molecules chloroform per formula (116 e). Alternatively one chloroform (58 e) plus one DMF (40 e) or ten water molecules (10 e) might be responsible. The fraction of solvent was treated as a diffuse contribution to the overall scattering without specific atom positions. ; _refine_diff_density_max 0.468 _refine_diff_density_min -0.334 _refine_diff_density_rms 0.050 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 1254 _refine_ls_number_reflns 20783 _refine_ls_number_restraints 627 _refine_ls_restrained_S_all 1.089 _refine_ls_R_factor_all 0.0555 _refine_ls_R_factor_gt 0.0412 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0544P)^2^+1.0031P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1057 _refine_ls_wR_factor_ref 0.1115 _reflns_Friedel_coverage 0.000 _reflns_number_gt 16087 _reflns_number_total 20783 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9dt00687g2.cif _cod_data_source_block aj0477 _cod_database_code 7700003 _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_min 0.951 _shelx_estimated_absorpt_t_max 0.974 _shelx_res_file ; TITL aj0477 in P-1 shelx.res created by SHELXL-2018/3 at 16:56:21 on 17-Aug-2018 CELL 0.71073 10.4957 20.6949 21.1795 87.483 76.573 83.507 ZERR 1.00 0.0001 0.0003 0.0003 0.001 0.001 0.001 LATT 1 SFAC C H CL MG N O P UNIT 158 210 6 4 4 44 4 MERG 2 OMIT -4 -10 1 OMIT 1 6 3 OMIT -4 1 3 OMIT -2 1 4 OMIT 0 10 4 OMIT 1 5 5 OMIT 1 -6 6 OMIT 2 1 8 OMIT 0 8 8 OMIT -4 -4 9 OMIT -4 -5 4 OMIT 0 1 10 SADI C56 C57 C56 C58 C56 C59 C56 C57' C56 C58' C56 C59' DELU 0.010 0.010 C56 C57 C58 C59 C57' C58' C59' SIMU 0.010 0.010 2.900 C56 C57 C58 C59 C57' C58' C59' DELU 0.010 0.010 C20 C21 C22 C23 C20' C21' C22' C23' SIMU 0.010 0.020 2.900 C20 C21 C22 C23 C20' C21' C22' C23' DELU 0.010 0.010 C44 C45 C46 C47 C48 C49 C44' C45' C46' C47' C48' C49' SIMU 0.010 0.020 2.900 C44 C45 C46 C47 C48 C49 C44' C45' C46' C47' SIMU 0.010 0.020 2.900 C47' C48' C49' EQIV $2 x-1, y, z EQIV $1 -x+2, -y+1, -z+1 EQIV $3 x+1, y, z EQIV $4 -x+1, -y+1, -z+1 HTAB C75 O6_$2 HTAB O9 O22 HTAB O9 O8 HTAB O10 O21_$3 HTAB O11 O21_$3 HTAB O11 O2 HTAB O12 O15 HTAB O12 O20 HTAB O13 O4_$1 HTAB O14 O12_$1 HTAB O14 O6 HTAB O14 O11 HTAB O15 O19_$4 HTAB O15 O18 HTAB O16 O17 HTAB O17 O18 HTAB O17 O20_$4 HTAB O18 O8 HTAB O18 O19 HTAB O19 O21 HTAB O19 O22 HTAB O20 O22 HTAB O20 O4 FMAP 2 PLAN -5 SIZE 0.120 0.180 0.230 ACTA 50 BOND $H L.S. 24 TEMP -125.00 WGHT 0.054400 1.003100 FVAR 7.06366 0.82913 0.46985 0.48137 0.64460 MOLE 1 MG1 4 0.889825 0.662816 0.488851 11.00000 0.01998 0.01597 = 0.01234 -0.00188 -0.00559 -0.00154 MG2 4 0.892782 0.472635 0.350345 11.00000 0.01952 0.01481 = 0.01444 -0.00076 -0.00482 -0.00183 P1 7 0.916902 0.659769 0.637231 11.00000 0.01777 0.01250 = 0.01107 -0.00148 -0.00350 -0.00205 P2 7 0.834147 0.631899 0.347167 11.00000 0.01663 0.01472 = 0.01088 -0.00035 -0.00426 -0.00206 O1 6 0.957781 0.717431 0.676624 11.00000 0.01784 0.01329 = 0.01256 -0.00247 -0.00351 -0.00204 O2 6 1.046689 0.617311 0.617867 11.00000 0.02084 0.01521 = 0.01414 -0.00006 -0.00288 -0.00097 O3 6 0.867278 0.689850 0.580292 11.00000 0.02217 0.01654 = 0.01425 -0.00198 -0.00588 -0.00055 O4 6 0.811749 0.626291 0.684680 11.00000 0.02072 0.01853 = 0.01567 -0.00182 -0.00288 -0.00554 O5 6 0.910140 0.674831 0.286344 11.00000 0.01570 0.01734 = 0.01258 0.00107 -0.00454 -0.00163 O6 6 0.916492 0.635258 0.396716 11.00000 0.01916 0.01979 = 0.01291 -0.00165 -0.00569 -0.00063 O7 6 0.839081 0.563948 0.323283 11.00000 0.02390 0.01584 = 0.01580 -0.00004 -0.00725 -0.00298 O8 6 0.694554 0.664428 0.369718 11.00000 0.01679 0.01987 = 0.01694 0.00015 -0.00357 -0.00235 O9 6 0.704132 0.708008 0.485429 11.00000 0.02374 0.02760 = 0.01715 -0.00520 -0.00689 0.00247 O10 6 0.989014 0.746319 0.455674 11.00000 0.03974 0.02106 = 0.02483 0.00289 -0.00906 -0.00885 O11 6 1.076809 0.613850 0.487312 11.00000 0.01910 0.02547 = 0.01474 -0.00058 -0.00388 -0.00401 O12 6 0.817298 0.570074 0.522435 11.00000 0.02206 0.01984 = 0.01642 -0.00283 -0.00369 -0.00458 O13 6 1.046700 0.464528 0.266614 11.00000 0.02979 0.02045 = 0.01773 0.00262 -0.00244 -0.00240 O14 6 1.021034 0.508806 0.398652 11.00000 0.02834 0.01653 = 0.02741 -0.00260 -0.01508 0.00000 O15 6 0.736731 0.481415 0.433103 11.00000 0.02181 0.02125 = 0.01997 0.00192 -0.00257 -0.00142 O16 6 0.775452 0.433353 0.296304 11.00000 0.02871 0.02689 = 0.02502 -0.00278 -0.01048 -0.00558 C1 1 0.865785 0.765870 0.709003 11.00000 0.01861 0.01312 = 0.01470 -0.00251 -0.00372 -0.00227 C2 1 0.804142 0.756379 0.774141 11.00000 0.02280 0.01472 = 0.01595 -0.00020 -0.00444 -0.00494 C3 1 0.720092 0.807696 0.806134 11.00000 0.03467 0.01848 = 0.01299 0.00057 0.00298 -0.00168 AFIX 43 H3 2 0.675179 0.801216 0.849976 11.00000 -1.20000 AFIX 0 C4 1 0.699165 0.868157 0.776484 11.00000 0.04857 0.01672 = 0.02356 -0.00132 0.00740 0.00463 C5 1 0.762095 0.875188 0.711415 11.00000 0.04256 0.01318 = 0.02183 0.00279 0.00155 0.00083 AFIX 43 H5 2 0.747357 0.915533 0.689709 11.00000 -1.20000 AFIX 0 C6 1 0.845881 0.825152 0.677045 11.00000 0.02530 0.01664 = 0.01434 0.00076 -0.00231 -0.00484 C7 1 0.831276 0.693110 0.810098 11.00000 0.02075 0.01434 = 0.01175 -0.00033 -0.00294 -0.00219 AFIX 13 H7 2 0.865234 0.659236 0.776298 11.00000 -1.20000 AFIX 0 C8 1 0.703986 0.671387 0.852676 11.00000 0.01943 0.01166 = 0.01783 0.00070 -0.00275 -0.00067 C9 1 0.607865 0.653470 0.823221 11.00000 0.02494 0.03075 = 0.02164 -0.00170 -0.00739 -0.00294 AFIX 43 H9 2 0.623009 0.654378 0.777207 11.00000 -1.20000 AFIX 0 C10 1 0.491008 0.634430 0.859933 11.00000 0.02127 0.03905 = 0.03835 -0.00298 -0.00923 -0.00800 AFIX 43 H10 2 0.426526 0.622588 0.838945 11.00000 -1.20000 AFIX 0 C11 1 0.466810 0.632415 0.927006 11.00000 0.01962 0.02733 = 0.03695 0.00291 0.00258 -0.00454 AFIX 43 H11 2 0.386103 0.619469 0.952172 11.00000 -1.20000 AFIX 0 C12 1 0.561363 0.649439 0.956754 11.00000 0.02935 0.03406 = 0.02010 0.00469 0.00106 -0.00491 AFIX 43 H12 2 0.545960 0.647965 1.002777 11.00000 -1.20000 AFIX 0 C13 1 0.679337 0.668792 0.919982 11.00000 0.02519 0.02874 = 0.01776 0.00156 -0.00377 -0.00634 AFIX 43 H13 2 0.743723 0.680356 0.941182 11.00000 -1.20000 AFIX 0 C14 1 0.937238 0.694566 0.848207 11.00000 0.01687 0.02273 = 0.01352 0.00057 -0.00016 -0.00377 C15 1 1.012433 0.636731 0.857501 11.00000 0.02294 0.02603 = 0.02294 -0.00020 -0.00254 -0.00187 AFIX 43 H15 2 1.001838 0.598420 0.836980 11.00000 -1.20000 AFIX 0 C16 1 1.102813 0.634185 0.896363 11.00000 0.02449 0.03836 = 0.03598 0.00436 -0.00866 0.00495 AFIX 43 H16 2 1.153266 0.594237 0.902303 11.00000 -1.20000 AFIX 0 C17 1 1.119581 0.688988 0.926175 11.00000 0.02635 0.05668 = 0.03965 -0.00424 -0.01819 -0.00275 AFIX 43 H17 2 1.180627 0.687145 0.953201 11.00000 -1.20000 AFIX 0 C18 1 1.047139 0.746725 0.916590 11.00000 0.03568 0.04507 = 0.04602 -0.01415 -0.02070 -0.00367 AFIX 43 H18 2 1.059149 0.784930 0.936846 11.00000 -1.20000 AFIX 0 C19 1 0.956800 0.749914 0.877751 11.00000 0.02858 0.02688 = 0.03177 -0.00674 -0.01065 -0.00157 AFIX 43 H19 2 0.908059 0.790250 0.871358 11.00000 -1.20000 AFIX 0 PART 1 SAME C20' > C23' C20 1 0.583851 0.921699 0.810041 31.00000 0.01966 0.02084 = 0.02557 -0.00383 0.00173 0.01018 C21 1 0.597981 0.926045 0.879558 31.00000 0.05740 0.03647 = 0.03687 -0.01373 -0.00613 0.01592 AFIX 137 H21A 2 0.536626 0.961919 0.901183 31.00000 -1.50000 H21B 2 0.688421 0.933878 0.879376 31.00000 -1.50000 H21C 2 0.577998 0.885136 0.902902 31.00000 -1.50000 AFIX 0 C22 1 0.446943 0.905910 0.810786 31.00000 0.02759 0.05059 = 0.07200 -0.03442 -0.00704 0.01333 AFIX 137 H22A 2 0.434867 0.906698 0.766235 31.00000 -1.50000 H22B 2 0.382228 0.938207 0.836398 31.00000 -1.50000 H22C 2 0.434623 0.862547 0.830212 31.00000 -1.50000 AFIX 0 C23 1 0.604460 0.988417 0.778308 31.00000 0.06726 0.02815 = 0.05466 0.00203 0.00949 0.01862 AFIX 137 H23A 2 0.585089 0.989439 0.735163 31.00000 -1.50000 H23B 2 0.696082 0.996864 0.774154 31.00000 -1.50000 H23C 2 0.545462 1.021844 0.805204 31.00000 -1.50000 AFIX 0 PART 2 C20' 1 0.631119 0.924891 0.818706 -31.00000 0.03074 0.02197 = 0.02857 0.00073 -0.00096 0.00786 C21' 1 0.647381 0.921419 0.888917 -31.00000 0.05977 0.02823 = 0.02779 -0.01168 -0.00238 0.00711 AFIX 33 H21D 2 0.739854 0.924237 0.889142 -31.00000 -1.50000 H21E 2 0.592228 0.957656 0.913255 -31.00000 -1.50000 H21F 2 0.620455 0.880143 0.909226 -31.00000 -1.50000 AFIX 0 C22' 1 0.487401 0.920355 0.821084 -31.00000 0.05109 0.03152 = 0.04096 -0.00355 -0.00554 0.01038 AFIX 33 H22D 2 0.433351 0.955445 0.847660 -31.00000 -1.50000 H22E 2 0.472756 0.924433 0.776973 -31.00000 -1.50000 H22F 2 0.462881 0.878247 0.840163 -31.00000 -1.50000 AFIX 0 C23' 1 0.667328 0.990496 0.788675 -31.00000 0.06314 0.01647 = 0.03930 -0.00471 0.00684 0.01305 AFIX 33 H23D 2 0.760433 0.994073 0.786842 -31.00000 -1.50000 H23E 2 0.652148 0.994157 0.744655 -31.00000 -1.50000 H23F 2 0.612696 1.025459 0.815209 -31.00000 -1.50000 AFIX 0 PART 0 C24 1 0.923678 0.835314 0.607233 11.00000 0.02506 0.01363 = 0.01354 0.00046 -0.00123 -0.00319 AFIX 13 H24 2 0.938836 0.791839 0.586367 11.00000 -1.20000 AFIX 0 C25 1 1.059133 0.855175 0.606448 11.00000 0.02796 0.01607 = 0.01616 0.00547 -0.00626 -0.00336 C26 1 1.077927 0.901802 0.647790 11.00000 0.03703 0.03268 = 0.02722 -0.00381 -0.00308 -0.01367 AFIX 43 H26 2 1.004326 0.922293 0.677819 11.00000 -1.20000 AFIX 0 C27 1 1.203212 0.918696 0.645601 11.00000 0.05264 0.04592 = 0.03427 -0.00201 -0.01264 -0.02744 AFIX 43 H27 2 1.214321 0.950864 0.673952 11.00000 -1.20000 AFIX 0 C28 1 1.311505 0.889382 0.602837 11.00000 0.03398 0.04127 = 0.03800 0.01467 -0.01531 -0.01869 AFIX 43 H28 2 1.397082 0.900879 0.601793 11.00000 -1.20000 AFIX 0 C29 1 1.294152 0.842906 0.561337 11.00000 0.02571 0.03264 = 0.03724 0.01062 -0.00483 -0.00156 AFIX 43 H29 2 1.368237 0.822435 0.531588 11.00000 -1.20000 AFIX 0 C30 1 1.169103 0.826102 0.563002 11.00000 0.02958 0.02152 = 0.02553 0.00201 -0.00567 -0.00161 AFIX 43 H30 2 1.158370 0.794350 0.534127 11.00000 -1.20000 AFIX 0 C31 1 0.845528 0.880213 0.567684 11.00000 0.02160 0.01841 = 0.01346 0.00139 -0.00046 -0.00212 C32 1 0.875309 0.942586 0.546603 11.00000 0.02152 0.01990 = 0.02885 0.00441 -0.00246 -0.00351 AFIX 43 H32 2 0.947544 0.959556 0.557639 11.00000 -1.20000 AFIX 0 C33 1 0.800439 0.980377 0.509533 11.00000 0.02676 0.02288 = 0.03799 0.01167 -0.00092 0.00046 AFIX 43 H33 2 0.821997 1.022836 0.495493 11.00000 -1.20000 AFIX 0 C34 1 0.695035 0.956515 0.493049 11.00000 0.02708 0.03752 = 0.02691 0.01027 -0.00519 0.00452 AFIX 43 H34 2 0.643204 0.982595 0.468325 11.00000 -1.20000 AFIX 0 C35 1 0.665600 0.894050 0.512971 11.00000 0.02511 0.03938 = 0.02395 -0.00089 -0.00595 -0.00533 AFIX 43 H35 2 0.594061 0.877046 0.501290 11.00000 -1.20000 AFIX 0 C36 1 0.739845 0.856498 0.549700 11.00000 0.02867 0.02457 = 0.02037 0.00159 -0.00392 -0.00769 AFIX 43 H36 2 0.718683 0.813805 0.562964 11.00000 -1.20000 AFIX 0 C37 1 0.847389 0.708556 0.242089 11.00000 0.01321 0.01620 = 0.01302 0.00184 -0.00362 -0.00225 C38 1 0.794986 0.773018 0.254446 11.00000 0.01643 0.01672 = 0.01536 -0.00205 -0.00335 -0.00348 C39 1 0.739666 0.807456 0.207768 11.00000 0.02181 0.01406 = 0.02162 -0.00159 -0.00537 0.00144 AFIX 43 H39 2 0.703376 0.851270 0.215993 11.00000 -1.20000 AFIX 0 C40 1 0.735410 0.780251 0.149525 11.00000 0.02105 0.02039 = 0.01763 0.00182 -0.00592 -0.00032 C41 1 0.791803 0.716345 0.138341 11.00000 0.02024 0.02225 = 0.01400 -0.00200 -0.00555 -0.00086 AFIX 43 H41 2 0.791777 0.697069 0.098455 11.00000 -1.20000 AFIX 0 C42 1 0.848249 0.679679 0.183561 11.00000 0.01413 0.01531 = 0.01343 -0.00057 -0.00129 -0.00125 C43 1 0.804164 0.805660 0.316323 11.00000 0.02011 0.01630 = 0.01878 -0.00435 -0.00637 -0.00160 AFIX 13 H43 2 0.795320 0.772103 0.352075 11.00000 -1.20000 AFIX 0 PART 1 SAME C44' > C49' C44 1 0.686770 0.859331 0.334625 41.00000 0.02004 0.02744 = 0.02295 -0.01390 -0.00953 0.00060 C45 1 0.567760 0.843546 0.371704 41.00000 0.02966 0.03103 = 0.02074 -0.00589 -0.00915 0.00227 AFIX 43 H45 2 0.561330 0.800011 0.387288 41.00000 -1.20000 AFIX 0 C46 1 0.457510 0.887987 0.387263 41.00000 0.02689 0.03628 = 0.02803 -0.00564 -0.01253 0.00747 AFIX 43 H46 2 0.377239 0.875567 0.413421 41.00000 -1.20000 AFIX 0 C47 1 0.466996 0.951775 0.363529 41.00000 0.02512 0.03552 = 0.03139 -0.01008 -0.01257 0.00996 AFIX 43 H47 2 0.392659 0.983388 0.373861 41.00000 -1.20000 AFIX 0 C48 1 0.584985 0.969173 0.324796 41.00000 0.02897 0.03108 = 0.03669 -0.01402 -0.01582 0.00668 AFIX 43 H48 2 0.590871 1.012623 0.308861 41.00000 -1.20000 AFIX 0 C49 1 0.694501 0.923064 0.309319 41.00000 0.02729 0.02363 = 0.02526 -0.01044 -0.01438 0.00378 AFIX 43 H49 2 0.774067 0.934682 0.281766 41.00000 -1.20000 AFIX 0 PART 2 C44' 1 0.680065 0.849976 0.342022 -41.00000 0.02578 0.02230 = 0.02547 -0.01122 -0.01195 0.00580 C45' 1 0.567617 0.820772 0.371369 -41.00000 0.02304 0.03066 = 0.02045 -0.00654 -0.00847 0.00624 AFIX 43 H45' 2 0.573469 0.774941 0.378053 -41.00000 -1.20000 AFIX 0 C46' 1 0.447386 0.857540 0.390957 -41.00000 0.02697 0.03817 = 0.03040 -0.00983 -0.00752 0.00647 AFIX 43 H46' 2 0.370228 0.837097 0.409277 -41.00000 -1.20000 AFIX 0 C47' 1 0.440904 0.924382 0.383546 -41.00000 0.03168 0.03475 = 0.03719 -0.01388 -0.01234 0.01061 AFIX 43 H47' 2 0.358707 0.949876 0.397532 -41.00000 -1.20000 AFIX 0 C48' 1 0.551052 0.954638 0.356345 -41.00000 0.03965 0.02944 = 0.05050 -0.02232 -0.01891 0.01274 AFIX 43 H48' 2 0.544864 1.000652 0.351374 -41.00000 -1.20000 AFIX 0 C49' 1 0.673345 0.917117 0.335832 -41.00000 0.02972 0.02559 = 0.03287 -0.01317 -0.01626 0.00475 AFIX 43 H49' 2 0.750535 0.937679 0.317909 -41.00000 -1.20000 AFIX 0 PART 0 C50 1 0.935908 0.833229 0.309998 11.00000 0.02263 0.01640 = 0.02502 0.00092 -0.00999 -0.00372 C51 1 0.954685 0.870168 0.360158 11.00000 0.03174 0.02052 = 0.03156 -0.00294 -0.01554 -0.00336 AFIX 43 H51 2 0.883550 0.880533 0.396314 11.00000 -1.20000 AFIX 0 C52 1 1.076149 0.891851 0.357683 11.00000 0.04312 0.02830 = 0.04559 0.00172 -0.02844 -0.01091 AFIX 43 H52 2 1.087401 0.917076 0.392020 11.00000 -1.20000 AFIX 0 C53 1 1.180549 0.877029 0.305740 11.00000 0.03035 0.04452 = 0.05751 0.00857 -0.02082 -0.02102 AFIX 43 H53 2 1.263660 0.891839 0.304225 11.00000 -1.20000 AFIX 0 C54 1 1.163561 0.840722 0.256229 11.00000 0.02771 0.06391 = 0.05264 -0.00678 -0.00169 -0.01383 AFIX 43 H54 2 1.235406 0.830148 0.220454 11.00000 -1.20000 AFIX 0 C55 1 1.041836 0.819308 0.258091 11.00000 0.02687 0.04452 = 0.03639 -0.00863 -0.00568 -0.01166 AFIX 43 H55 2 1.031208 0.794726 0.223169 11.00000 -1.20000 AFIX 0 C56 1 0.666806 0.819483 0.101502 11.00000 0.03557 0.02735 = 0.02755 0.00161 -0.01621 0.00410 PART 1 C57 1 0.715848 0.886835 0.088644 21.00000 0.06376 0.03945 = 0.05230 0.02507 -0.03305 -0.00783 AFIX 137 H57A 2 0.809749 0.882091 0.067302 21.00000 -1.50000 H57B 2 0.702885 0.909089 0.129909 21.00000 -1.50000 H57C 2 0.666289 0.912421 0.060494 21.00000 -1.50000 AFIX 0 C58 1 0.517059 0.831107 0.134293 21.00000 0.03419 0.04798 = 0.04355 0.00162 -0.01787 0.01074 AFIX 137 H58A 2 0.471916 0.859702 0.106370 21.00000 -1.50000 H58B 2 0.505574 0.851543 0.176400 21.00000 -1.50000 H58C 2 0.479598 0.789381 0.140711 21.00000 -1.50000 AFIX 0 C59 1 0.680745 0.785517 0.039024 21.00000 0.05902 0.05128 = 0.02765 -0.00235 -0.02369 0.02132 AFIX 137 H59A 2 0.774389 0.775903 0.018403 21.00000 -1.50000 H59B 2 0.637321 0.813554 0.010028 21.00000 -1.50000 H59C 2 0.639661 0.744830 0.047686 21.00000 -1.50000 AFIX 0 PART 2 C59' 1 0.769071 0.814837 0.033994 -21.00000 0.05639 0.04472 = 0.03611 0.01492 -0.01985 0.01311 AFIX 33 H59D 2 0.801520 0.769147 0.024816 -21.00000 -1.50000 H59E 2 0.726174 0.833246 -0.000190 -21.00000 -1.50000 H59F 2 0.843136 0.839228 0.035360 -21.00000 -1.50000 AFIX 0 C57' 1 0.611977 0.886141 0.119930 -21.00000 0.05687 0.04319 = 0.04323 0.00611 -0.02371 0.01374 AFIX 33 H57D 2 0.570688 0.906625 0.085995 -21.00000 -1.50000 H57E 2 0.545860 0.885222 0.161022 -21.00000 -1.50000 H57F 2 0.682737 0.911127 0.125089 -21.00000 -1.50000 AFIX 0 C58' 1 0.556743 0.778468 0.091795 -21.00000 0.04867 0.05003 = 0.04519 0.00383 -0.02646 0.00601 AFIX 33 H58D 2 0.595474 0.734181 0.079526 -21.00000 -1.50000 H58E 2 0.489370 0.776923 0.132383 -21.00000 -1.50000 H58F 2 0.516399 0.798593 0.057393 -21.00000 -1.50000 AFIX 0 PART 0 C60 1 0.914825 0.610678 0.169100 11.00000 0.01800 0.01633 = 0.01178 -0.00106 -0.00278 -0.00064 AFIX 13 H60 2 0.900927 0.586374 0.211591 11.00000 -1.20000 AFIX 0 C61 1 0.847704 0.576060 0.126129 11.00000 0.01781 0.01448 = 0.01879 -0.00411 -0.00497 0.00331 C62 1 0.732692 0.548615 0.154824 11.00000 0.02126 0.02088 = 0.02395 -0.00065 -0.00439 0.00024 AFIX 43 H62 2 0.701866 0.549087 0.200687 11.00000 -1.20000 AFIX 0 C63 1 0.662315 0.520501 0.117177 11.00000 0.02159 0.02326 = 0.04498 0.00013 -0.01381 -0.00218 AFIX 43 H63 2 0.583488 0.502203 0.137305 11.00000 -1.20000 AFIX 0 C64 1 0.707084 0.519155 0.050317 11.00000 0.03435 0.02417 = 0.04114 -0.00816 -0.02551 0.00221 AFIX 43 H64 2 0.658638 0.500309 0.024494 11.00000 -1.20000 AFIX 0 C65 1 0.822292 0.545272 0.021308 11.00000 0.03731 0.02666 = 0.02254 -0.00821 -0.01388 0.00437 AFIX 43 H65 2 0.853603 0.543869 -0.024504 11.00000 -1.20000 AFIX 0 C66 1 0.892822 0.573656 0.058842 11.00000 0.02485 0.02377 = 0.01894 -0.00339 -0.00512 0.00016 AFIX 43 H66 2 0.972085 0.591479 0.038524 11.00000 -1.20000 AFIX 0 C67 1 1.063557 0.608459 0.143235 11.00000 0.01813 0.02178 = 0.01016 -0.00211 -0.00306 0.00116 C68 1 1.128429 0.663863 0.127279 11.00000 0.02210 0.02397 = 0.02518 0.00311 -0.00354 -0.00159 AFIX 43 H68 2 1.078976 0.705425 0.129615 11.00000 -1.20000 AFIX 0 C69 1 1.266114 0.659056 0.107769 11.00000 0.02277 0.03908 = 0.03351 0.00823 -0.00200 -0.00902 AFIX 43 H69 2 1.309647 0.697227 0.096926 11.00000 -1.20000 AFIX 0 C70 1 1.338873 0.598423 0.104300 11.00000 0.01666 0.05048 = 0.02804 0.01012 0.00042 0.00230 AFIX 43 H70 2 1.432354 0.595082 0.092238 11.00000 -1.20000 AFIX 0 C71 1 1.274875 0.542998 0.118443 11.00000 0.02552 0.03521 = 0.02003 0.00322 -0.00060 0.00968 AFIX 43 H71 2 1.324214 0.501383 0.115389 11.00000 -1.20000 AFIX 0 C72 1 1.138888 0.548158 0.137055 11.00000 0.02516 0.02247 = 0.01592 0.00122 -0.00317 0.00195 AFIX 43 H72 2 1.095777 0.509689 0.145839 11.00000 -1.20000 AFIX 0 C73 1 0.350143 0.692335 0.362084 11.00000 0.02656 0.04120 = 0.03700 0.00938 -0.00699 -0.01015 AFIX 43 H73 2 0.431779 0.705968 0.365354 11.00000 -1.20000 AFIX 0 C74 1 0.459749 0.665461 0.251936 11.00000 0.03353 0.07455 = 0.03828 0.00711 0.00193 -0.00038 AFIX 137 H74A 2 0.534393 0.680238 0.265702 11.00000 -1.50000 H74B 2 0.441217 0.692640 0.215387 11.00000 -1.50000 H74C 2 0.481376 0.620065 0.238494 11.00000 -1.50000 AFIX 0 C75 1 0.225010 0.647710 0.295783 11.00000 0.04124 0.12509 = 0.04129 -0.01441 -0.00775 -0.02637 AFIX 137 H75A 2 0.237021 0.600180 0.293035 11.00000 -1.50000 H75B 2 0.205979 0.666685 0.255329 11.00000 -1.50000 H75C 2 0.151399 0.660807 0.332235 11.00000 -1.50000 AFIX 0 C76 1 0.360079 0.706027 0.639049 11.00000 0.02792 0.03097 = 0.03449 0.00554 -0.01030 -0.00208 AFIX 43 H76 2 0.278451 0.692016 0.636285 11.00000 -1.20000 AFIX 0 C77 1 0.241507 0.753089 0.739830 11.00000 0.06402 0.05389 = 0.03856 0.00017 0.00632 0.01055 AFIX 137 H77A 2 0.170165 0.732690 0.728494 11.00000 -1.50000 H77B 2 0.218584 0.800305 0.741974 11.00000 -1.50000 H77C 2 0.254229 0.736173 0.782128 11.00000 -1.50000 AFIX 0 C78 1 0.481932 0.763573 0.697568 11.00000 0.06853 0.05079 = 0.04831 -0.00243 -0.03160 -0.01046 AFIX 137 H78A 2 0.558063 0.741271 0.667637 11.00000 -1.50000 H78B 2 0.491845 0.756158 0.742276 11.00000 -1.50000 H78C 2 0.476528 0.810336 0.687488 11.00000 -1.50000 AFIX 0 H9P 2 0.636018 0.705799 0.516771 11.00000 0.04027 H9Q 2 0.687742 0.698466 0.449834 11.00000 0.06363 H10O 2 0.955346 0.775459 0.439776 11.00000 0.07428 H10P 2 1.068719 0.740149 0.432397 11.00000 0.08910 H11O 2 1.141876 0.631868 0.462794 11.00000 0.06804 H11P 2 1.090434 0.612272 0.525476 11.00000 0.04398 H12O 2 0.797814 0.547805 0.498075 11.00000 0.05141 H12P 2 0.746103 0.574550 0.554540 11.00000 0.04102 H13O 2 1.119920 0.436167 0.277105 11.00000 0.06987 H13P 2 1.082237 0.499829 0.256002 11.00000 0.06088 H14O 2 1.056815 0.487337 0.425670 11.00000 0.04295 H14P 2 1.013706 0.547404 0.404957 11.00000 0.04922 H15O 2 0.710834 0.443008 0.450396 11.00000 0.03720 H15P 2 0.665827 0.505583 0.427330 11.00000 0.06791 H16O 2 0.687390 0.456430 0.299702 11.00000 0.07849 H16P 2 0.820144 0.427894 0.258931 11.00000 0.06746 MOLE 2 O17 6 0.536229 0.496652 0.299690 11.00000 0.02892 0.04126 = 0.03204 0.00501 -0.00687 -0.01188 H17O 2 0.527714 0.525544 0.336290 11.00000 0.08677 H17P 2 0.478454 0.467816 0.319109 11.00000 0.07330 MOLE 3 O18 6 0.543968 0.567926 0.406607 11.00000 0.01916 0.02497 = 0.03607 0.00012 -0.00112 -0.00557 H18O 2 0.586920 0.599056 0.391614 11.00000 0.04536 H18P 2 0.484326 0.582571 0.441773 11.00000 0.05626 MOLE 4 O19 6 0.364242 0.630380 0.508051 11.00000 0.02642 0.03247 = 0.02650 0.00206 -0.00643 -0.00580 H19O 2 0.328854 0.663198 0.484600 11.00000 0.05925 H19P 2 0.395509 0.652215 0.538353 11.00000 0.04398 MOLE 5 O20 6 0.628672 0.590154 0.632849 11.00000 0.02037 0.03184 = 0.02599 -0.00206 -0.00570 -0.00658 H20O 2 0.581622 0.623148 0.622995 11.00000 0.04498 H20P 2 0.685118 0.604234 0.651667 11.00000 0.04782 MOLE 6 N1 5 0.344236 0.670569 0.305766 11.00000 0.02500 0.04922 = 0.03016 0.00657 -0.00329 -0.00356 O21 6 0.258466 0.696885 0.412008 11.00000 0.03142 0.04355 = 0.02985 0.00618 -0.00339 -0.00735 MOLE 7 N2 5 0.362708 0.738373 0.690620 11.00000 0.04365 0.03499 = 0.02846 0.00128 -0.00775 0.00090 O22 6 0.457567 0.692403 0.593351 11.00000 0.02781 0.03934 = 0.02971 -0.00084 -0.00748 0.00054 MOLE 8 PART 1 SAME C79' > Cl3' C79 1 0.242431 0.864644 0.001202 51.00000 0.03633 0.04440 = 0.03853 0.00401 -0.01413 0.00002 AFIX 13 H79 2 0.202286 0.878588 -0.036314 51.00000 -1.20000 AFIX 0 CL1 3 0.357534 0.798339 -0.025883 51.00000 0.04567 0.03103 = 0.06020 -0.00801 -0.00291 -0.00144 CL2 3 0.317321 0.930887 0.017351 51.00000 0.04725 0.03417 = 0.06267 -0.00931 -0.01355 -0.00457 CL3 3 0.112376 0.842075 0.063404 51.00000 0.06320 0.06304 = 0.05687 0.00475 -0.00067 -0.00345 PART 2 C79' 1 0.223256 0.864650 0.005630 -51.00000 0.04111 0.03254 = 0.07953 0.00048 -0.02842 -0.01085 AFIX 13 H79' 2 0.160408 0.876409 -0.023047 -51.00000 -1.20000 AFIX 0 CL1' 3 0.338095 0.799632 -0.024881 -51.00000 0.06105 0.08079 = 0.08187 -0.02411 -0.01531 -0.01768 CL2' 3 0.295626 0.931977 0.021303 -51.00000 0.05586 0.09480 = 0.20514 -0.07879 -0.00325 -0.01992 CL3' 3 0.141295 0.842536 0.083751 -51.00000 0.08130 0.06581 = 0.08230 0.02472 0.02853 0.00493 HKLF 4 REM aj0477 in P-1 REM wR2 = 0.1115, GooF = S = 1.090, Restrained GooF = 1.089 for all data REM R1 = 0.0412 for 16087 Fo > 4sig(Fo) and 0.0555 for all 20783 data REM 1254 parameters refined using 627 restraints END WGHT 0.0540 1.0577 REM Highest difference peak 0.468, deepest hole -0.334, 1-sigma level 0.050 Q1 1 0.1609 0.5949 0.2875 11.00000 0.05 0.47 Q2 1 0.5066 0.7086 0.2945 11.00000 0.05 0.35 Q3 1 1.1941 0.6609 0.1192 11.00000 0.05 0.32 Q4 1 0.8948 0.6489 0.1728 11.00000 0.05 0.31 Q5 1 0.8814 0.5881 0.1434 11.00000 0.05 0.31 ; _shelx_res_checksum 81536 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 Mg1 Mg 0.88982(5) 0.66282(2) 0.48885(2) 0.01576(11) Uani 1 1 d . . . . . Mg2 Mg 0.89278(5) 0.47263(2) 0.35035(2) 0.01609(11) Uani 1 1 d . . . . . P1 P 0.91690(4) 0.65977(2) 0.63723(2) 0.01367(8) Uani 1 1 d . . . . . P2 P 0.83415(4) 0.63190(2) 0.34717(2) 0.01386(8) Uani 1 1 d . . . . . O1 O 0.95778(9) 0.71743(5) 0.67662(4) 0.0145(2) Uani 1 1 d . . . . . O2 O 1.04669(10) 0.61731(5) 0.61787(5) 0.0170(2) Uani 1 1 d . . . . . O3 O 0.86728(10) 0.68985(5) 0.58029(5) 0.0174(2) Uani 1 1 d . . . . . O4 O 0.81175(10) 0.62629(5) 0.68468(5) 0.0182(2) Uani 1 1 d . . . . . O5 O 0.91014(9) 0.67483(5) 0.28634(5) 0.0150(2) Uani 1 1 d . . . . . O6 O 0.91649(10) 0.63526(5) 0.39672(5) 0.0170(2) Uani 1 1 d . . . . . O7 O 0.83908(10) 0.56395(5) 0.32328(5) 0.0180(2) Uani 1 1 d . . . . . O8 O 0.69455(10) 0.66443(5) 0.36972(5) 0.0179(2) Uani 1 1 d . . . . . O9 O 0.70413(12) 0.70801(6) 0.48543(6) 0.0227(2) Uani 1 1 d . . . . . O10 O 0.98901(15) 0.74632(6) 0.45567(6) 0.0279(3) Uani 1 1 d . . . . . O11 O 1.07681(11) 0.61385(5) 0.48731(6) 0.0196(2) Uani 1 1 d . . . . . O12 O 0.81730(11) 0.57007(5) 0.52244(6) 0.0193(2) Uani 1 1 d . . . . . O13 O 1.04670(12) 0.46453(6) 0.26661(5) 0.0233(2) Uani 1 1 d . . . . . O14 O 1.02103(11) 0.50881(6) 0.39865(6) 0.0228(2) Uani 1 1 d . . . . . O15 O 0.73673(11) 0.48141(6) 0.43310(5) 0.0215(2) Uani 1 1 d . . . . . O16 O 0.77545(13) 0.43335(6) 0.29630(6) 0.0259(3) Uani 1 1 d . . . . . C1 C 0.86579(14) 0.76587(7) 0.70900(7) 0.0154(3) Uani 1 1 d . . . . . C2 C 0.80414(15) 0.75638(7) 0.77414(7) 0.0176(3) Uani 1 1 d . . . . . C3 C 0.72009(16) 0.80770(7) 0.80613(7) 0.0235(3) Uani 1 1 d . . . . . H3 H 0.675179 0.801216 0.849976 0.028 Uiso 1 1 calc R U . . . C4 C 0.69916(19) 0.86816(8) 0.77648(8) 0.0328(4) Uani 1 1 d . . . . . C5 C 0.76210(18) 0.87519(8) 0.71142(8) 0.0277(4) Uani 1 1 d . . . . . H5 H 0.747357 0.915533 0.689709 0.033 Uiso 1 1 calc R U . . . C6 C 0.84588(15) 0.82515(7) 0.67704(7) 0.0190(3) Uani 1 1 d . . . . . C7 C 0.83128(14) 0.69311(7) 0.81010(7) 0.0157(3) Uani 1 1 d . . . . . H7 H 0.865234 0.659236 0.776298 0.019 Uiso 1 1 calc R U . . . C8 C 0.70399(14) 0.67139(7) 0.85268(7) 0.0167(3) Uani 1 1 d . . . . . C9 C 0.60786(16) 0.65347(8) 0.82322(8) 0.0254(3) Uani 1 1 d . . . . . H9 H 0.623009 0.654378 0.777207 0.030 Uiso 1 1 calc R U . . . C10 C 0.49101(17) 0.63443(9) 0.85993(9) 0.0321(4) Uani 1 1 d . . . . . H10 H 0.426526 0.622588 0.838945 0.038 Uiso 1 1 calc R U . . . C11 C 0.46681(16) 0.63242(8) 0.92701(9) 0.0294(4) Uani 1 1 d . . . . . H11 H 0.386103 0.619469 0.952172 0.035 Uiso 1 1 calc R U . . . C12 C 0.56136(17) 0.64944(9) 0.95675(8) 0.0290(4) Uani 1 1 d . . . . . H12 H 0.545960 0.647965 1.002777 0.035 Uiso 1 1 calc R U . . . C13 C 0.67934(16) 0.66879(8) 0.91998(7) 0.0239(3) Uani 1 1 d . . . . . H13 H 0.743723 0.680356 0.941182 0.029 Uiso 1 1 calc R U . . . C14 C 0.93724(14) 0.69457(7) 0.84821(7) 0.0181(3) Uani 1 1 d . . . . . C15 C 1.01243(16) 0.63673(8) 0.85750(8) 0.0245(3) Uani 1 1 d . . . . . H15 H 1.001838 0.598420 0.836980 0.029 Uiso 1 1 calc R U . . . C16 C 1.10281(17) 0.63418(9) 0.89636(9) 0.0335(4) Uani 1 1 d . . . . . H16 H 1.153266 0.594237 0.902303 0.040 Uiso 1 1 calc R U . . . C17 C 1.11958(18) 0.68899(10) 0.92618(10) 0.0392(5) Uani 1 1 d . . . . . H17 H 1.180627 0.687145 0.953201 0.047 Uiso 1 1 calc R U . . . C18 C 1.04714(19) 0.74673(10) 0.91659(10) 0.0400(5) Uani 1 1 d . . . . . H18 H 1.059149 0.784930 0.936846 0.048 Uiso 1 1 calc R U . . . C19 C 0.95680(17) 0.74991(8) 0.87775(8) 0.0284(4) Uani 1 1 d . . . . . H19 H 0.908059 0.790250 0.871358 0.034 Uiso 1 1 calc R U . . . C20 C 0.5839(9) 0.9217(3) 0.8100(3) 0.0240(14) Uani 0.470(15) 1 d D U P A 1 C21 C 0.5980(10) 0.9260(4) 0.8796(4) 0.0456(17) Uani 0.470(15) 1 d D U P A 1 H21A H 0.536626 0.961919 0.901183 0.068 Uiso 0.470(15) 1 calc R U P A 1 H21B H 0.688421 0.933878 0.879376 0.068 Uiso 0.470(15) 1 calc R U P A 1 H21C H 0.577998 0.885136 0.902902 0.068 Uiso 0.470(15) 1 calc R U P A 1 C22 C 0.4469(8) 0.9059(4) 0.8108(4) 0.0511(18) Uani 0.470(15) 1 d D U P A 1 H22A H 0.434867 0.906698 0.766235 0.077 Uiso 0.470(15) 1 calc R U P A 1 H22B H 0.382228 0.938207 0.836398 0.077 Uiso 0.470(15) 1 calc R U P A 1 H22C H 0.434623 0.862547 0.830212 0.077 Uiso 0.470(15) 1 calc R U P A 1 C23 C 0.6045(12) 0.9884(3) 0.7783(4) 0.056(2) Uani 0.470(15) 1 d D U P A 1 H23A H 0.585089 0.989439 0.735163 0.084 Uiso 0.470(15) 1 calc R U P A 1 H23B H 0.696082 0.996864 0.774154 0.084 Uiso 0.470(15) 1 calc R U P A 1 H23C H 0.545462 1.021844 0.805204 0.084 Uiso 0.470(15) 1 calc R U P A 1 C20' C 0.6311(9) 0.9249(3) 0.8187(3) 0.0289(13) Uani 0.530(15) 1 d D U P A 2 C21' C 0.6474(9) 0.9214(3) 0.8889(3) 0.0404(15) Uani 0.530(15) 1 d D U P A 2 H21D H 0.739854 0.924237 0.889142 0.061 Uiso 0.530(15) 1 calc R U P A 2 H21E H 0.592228 0.957656 0.913255 0.061 Uiso 0.530(15) 1 calc R U P A 2 H21F H 0.620455 0.880143 0.909226 0.061 Uiso 0.530(15) 1 calc R U P A 2 C22' C 0.4874(9) 0.9204(3) 0.8211(3) 0.0431(16) Uani 0.530(15) 1 d D U P A 2 H22D H 0.433351 0.955445 0.847660 0.065 Uiso 0.530(15) 1 calc R U P A 2 H22E H 0.472756 0.924433 0.776973 0.065 Uiso 0.530(15) 1 calc R U P A 2 H22F H 0.462881 0.878247 0.840163 0.065 Uiso 0.530(15) 1 calc R U P A 2 C23' C 0.6673(9) 0.9905(2) 0.7887(3) 0.0439(16) Uani 0.530(15) 1 d D U P A 2 H23D H 0.760433 0.994073 0.786842 0.066 Uiso 0.530(15) 1 calc R U P A 2 H23E H 0.652148 0.994157 0.744655 0.066 Uiso 0.530(15) 1 calc R U P A 2 H23F H 0.612696 1.025459 0.815209 0.066 Uiso 0.530(15) 1 calc R U P A 2 C24 C 0.92368(15) 0.83531(7) 0.60723(7) 0.0179(3) Uani 1 1 d . . . . . H24 H 0.938836 0.791839 0.586367 0.021 Uiso 1 1 calc R U . . . C25 C 1.05913(16) 0.85518(7) 0.60645(7) 0.0200(3) Uani 1 1 d . . . . . C26 C 1.07793(19) 0.90180(9) 0.64779(9) 0.0321(4) Uani 1 1 d . . . . . H26 H 1.004326 0.922293 0.677819 0.039 Uiso 1 1 calc R U . . . C27 C 1.2032(2) 0.91870(10) 0.64560(10) 0.0420(5) Uani 1 1 d . . . . . H27 H 1.214321 0.950864 0.673952 0.050 Uiso 1 1 calc R U . . . C28 C 1.31150(19) 0.88938(9) 0.60284(9) 0.0359(4) Uani 1 1 d . . . . . H28 H 1.397082 0.900879 0.601793 0.043 Uiso 1 1 calc R U . . . C29 C 1.29415(17) 0.84291(9) 0.56134(9) 0.0327(4) Uani 1 1 d . . . . . H29 H 1.368237 0.822435 0.531588 0.039 Uiso 1 1 calc R U . . . C30 C 1.16910(16) 0.82610(8) 0.56300(8) 0.0258(3) Uani 1 1 d . . . . . H30 H 1.158370 0.794350 0.534127 0.031 Uiso 1 1 calc R U . . . C31 C 0.84553(15) 0.88021(7) 0.56768(7) 0.0185(3) Uani 1 1 d . . . . . C32 C 0.87531(16) 0.94259(8) 0.54660(8) 0.0240(3) Uani 1 1 d . . . . . H32 H 0.947544 0.959556 0.557639 0.029 Uiso 1 1 calc R U . . . C33 C 0.80044(17) 0.98038(8) 0.50953(9) 0.0309(4) Uani 1 1 d . . . . . H33 H 0.821997 1.022836 0.495493 0.037 Uiso 1 1 calc R U . . . C34 C 0.69503(17) 0.95652(9) 0.49305(8) 0.0316(4) Uani 1 1 d . . . . . H34 H 0.643204 0.982595 0.468325 0.038 Uiso 1 1 calc R U . . . C35 C 0.66560(17) 0.89405(9) 0.51297(8) 0.0293(4) Uani 1 1 d . . . . . H35 H 0.594061 0.877046 0.501290 0.035 Uiso 1 1 calc R U . . . C36 C 0.73984(16) 0.85650(8) 0.54970(8) 0.0245(3) Uani 1 1 d . . . . . H36 H 0.718683 0.813805 0.562964 0.029 Uiso 1 1 calc R U . . . C37 C 0.84739(13) 0.70856(7) 0.24209(7) 0.0141(3) Uani 1 1 d . . . . . C38 C 0.79499(14) 0.77302(7) 0.25445(7) 0.0160(3) Uani 1 1 d . . . . . C39 C 0.73967(15) 0.80746(7) 0.20777(7) 0.0193(3) Uani 1 1 d . . . . . H39 H 0.703376 0.851270 0.215993 0.023 Uiso 1 1 calc R U . . . C40 C 0.73541(15) 0.78025(7) 0.14952(7) 0.0197(3) Uani 1 1 d . . . . . C41 C 0.79180(14) 0.71634(7) 0.13834(7) 0.0186(3) Uani 1 1 d . . . . . H41 H 0.791777 0.697069 0.098455 0.022 Uiso 1 1 calc R U . . . C42 C 0.84825(13) 0.67968(7) 0.18356(7) 0.0146(3) Uani 1 1 d . . . . . C43 C 0.80416(14) 0.80566(7) 0.31632(7) 0.0180(3) Uani 1 1 d . . . . . H43 H 0.795320 0.772103 0.352075 0.022 Uiso 1 1 calc R U . B 1 C44 C 0.6868(11) 0.8593(4) 0.3346(7) 0.0226(14) Uani 0.481(7) 1 d D U P C 1 C45 C 0.5678(7) 0.8435(3) 0.3717(4) 0.0269(12) Uani 0.481(7) 1 d D U P C 1 H45 H 0.561330 0.800011 0.387288 0.032 Uiso 0.481(7) 1 calc R U P C 1 C46 C 0.4575(5) 0.8880(4) 0.3873(2) 0.0301(11) Uani 0.481(7) 1 d D U P C 1 H46 H 0.377239 0.875567 0.413421 0.036 Uiso 0.481(7) 1 calc R U P C 1 C47 C 0.4670(6) 0.9518(3) 0.3635(3) 0.0304(11) Uani 0.481(7) 1 d D U P C 1 H47 H 0.392659 0.983388 0.373861 0.036 Uiso 0.481(7) 1 calc R U P C 1 C48 C 0.5850(5) 0.9692(2) 0.3248(3) 0.0312(10) Uani 0.481(7) 1 d D U P C 1 H48 H 0.590871 1.012623 0.308861 0.037 Uiso 0.481(7) 1 calc R U P C 1 C49 C 0.6945(5) 0.9231(3) 0.3093(3) 0.0242(10) Uani 0.481(7) 1 d D U P C 1 H49 H 0.774067 0.934682 0.281766 0.029 Uiso 0.481(7) 1 calc R U P C 1 C44' C 0.6801(10) 0.8500(4) 0.3420(7) 0.0238(13) Uani 0.519(7) 1 d D U P C 2 C45' C 0.5676(6) 0.8208(3) 0.3714(3) 0.0247(10) Uani 0.519(7) 1 d D U P C 2 H45' H 0.573469 0.774941 0.378053 0.030 Uiso 0.519(7) 1 calc R U P C 2 C46' C 0.4474(5) 0.8575(3) 0.3910(2) 0.0322(10) Uani 0.519(7) 1 d D U P C 2 H46' H 0.370228 0.837097 0.409277 0.039 Uiso 0.519(7) 1 calc R U P C 2 C47' C 0.4409(5) 0.9244(4) 0.3835(3) 0.0345(11) Uani 0.519(7) 1 d D U P C 2 H47' H 0.358707 0.949876 0.397532 0.041 Uiso 0.519(7) 1 calc R U P C 2 C48' C 0.5511(6) 0.9546(2) 0.3563(3) 0.0391(12) Uani 0.519(7) 1 d D U P C 2 H48' H 0.544864 1.000652 0.351374 0.047 Uiso 0.519(7) 1 calc R U P C 2 C49' C 0.6733(5) 0.9171(3) 0.3358(3) 0.0281(11) Uani 0.519(7) 1 d D U P C 2 H49' H 0.750535 0.937679 0.317909 0.034 Uiso 0.519(7) 1 calc R U P C 2 C50 C 0.93591(15) 0.83323(7) 0.31000(8) 0.0205(3) Uani 1 1 d . . . . . C51 C 0.95468(17) 0.87017(8) 0.36016(8) 0.0265(3) Uani 1 1 d . . . . . H51 H 0.883550 0.880533 0.396314 0.032 Uiso 1 1 calc R U . . . C52 C 1.07615(19) 0.89185(9) 0.35768(10) 0.0355(4) Uani 1 1 d . . . . . H52 H 1.087401 0.917076 0.392020 0.043 Uiso 1 1 calc R U . . . C53 C 1.18055(19) 0.87703(10) 0.30574(11) 0.0413(5) Uani 1 1 d . . . . . H53 H 1.263660 0.891839 0.304225 0.050 Uiso 1 1 calc R U . . . C54 C 1.1636(2) 0.84072(12) 0.25623(11) 0.0484(5) Uani 1 1 d . . . . . H54 H 1.235406 0.830148 0.220454 0.058 Uiso 1 1 calc R U . . . C55 C 1.04184(17) 0.81931(10) 0.25809(9) 0.0353(4) Uani 1 1 d . . . . . H55 H 1.031208 0.794726 0.223169 0.042 Uiso 1 1 calc R U . . . C56 C 0.66681(18) 0.81948(8) 0.10150(8) 0.0293(4) Uani 1 1 d D U . . . C57 C 0.7158(3) 0.88683(12) 0.08864(14) 0.0492(7) Uani 0.829(3) 1 d D U P D 1 H57A H 0.809749 0.882091 0.067302 0.074 Uiso 0.829(3) 1 calc R U P D 1 H57B H 0.702885 0.909089 0.129909 0.074 Uiso 0.829(3) 1 calc R U P D 1 H57C H 0.666289 0.912421 0.060494 0.074 Uiso 0.829(3) 1 calc R U P D 1 C58 C 0.5171(2) 0.83111(13) 0.13429(12) 0.0417(6) Uani 0.829(3) 1 d D U P D 1 H58A H 0.471916 0.859702 0.106370 0.063 Uiso 0.829(3) 1 calc R U P D 1 H58B H 0.505574 0.851543 0.176400 0.063 Uiso 0.829(3) 1 calc R U P D 1 H58C H 0.479598 0.789381 0.140711 0.063 Uiso 0.829(3) 1 calc R U P D 1 C59 C 0.6807(3) 0.78552(13) 0.03902(11) 0.0458(7) Uani 0.829(3) 1 d D U P D 1 H59A H 0.774389 0.775903 0.018403 0.069 Uiso 0.829(3) 1 calc R U P D 1 H59B H 0.637321 0.813554 0.010028 0.069 Uiso 0.829(3) 1 calc R U P D 1 H59C H 0.639661 0.744830 0.047686 0.069 Uiso 0.829(3) 1 calc R U P D 1 C59' C 0.7691(13) 0.8148(7) 0.0340(5) 0.046(2) Uani 0.171(3) 1 d D U P D 2 H59D H 0.801520 0.769147 0.024816 0.069 Uiso 0.171(3) 1 calc R U P D 2 H59E H 0.726174 0.833246 -0.000190 0.069 Uiso 0.171(3) 1 calc R U P D 2 H59F H 0.843136 0.839228 0.035360 0.069 Uiso 0.171(3) 1 calc R U P D 2 C57' C 0.6120(14) 0.8861(5) 0.1199(6) 0.047(2) Uani 0.171(3) 1 d D U P D 2 H57D H 0.570688 0.906625 0.085995 0.071 Uiso 0.171(3) 1 calc R U P D 2 H57E H 0.545860 0.885222 0.161022 0.071 Uiso 0.171(3) 1 calc R U P D 2 H57F H 0.682737 0.911127 0.125089 0.071 Uiso 0.171(3) 1 calc R U P D 2 C58' C 0.5567(12) 0.7785(6) 0.0918(6) 0.046(2) Uani 0.171(3) 1 d D U P D 2 H58D H 0.595474 0.734181 0.079526 0.070 Uiso 0.171(3) 1 calc R U P D 2 H58E H 0.489370 0.776923 0.132383 0.070 Uiso 0.171(3) 1 calc R U P D 2 H58F H 0.516399 0.798593 0.057393 0.070 Uiso 0.171(3) 1 calc R U P D 2 C60 C 0.91483(14) 0.61068(7) 0.16910(7) 0.0155(3) Uani 1 1 d . . . . . H60 H 0.900927 0.586374 0.211591 0.019 Uiso 1 1 calc R U . . . C61 C 0.84770(14) 0.57606(7) 0.12613(7) 0.0172(3) Uani 1 1 d . . . . . C62 C 0.73269(15) 0.54862(7) 0.15482(8) 0.0223(3) Uani 1 1 d . . . . . H62 H 0.701866 0.549087 0.200687 0.027 Uiso 1 1 calc R U . . . C63 C 0.66232(16) 0.52050(8) 0.11718(9) 0.0290(4) Uani 1 1 d . . . . . H63 H 0.583488 0.502203 0.137305 0.035 Uiso 1 1 calc R U . . . C64 C 0.70708(18) 0.51915(8) 0.05032(9) 0.0306(4) Uani 1 1 d . . . . . H64 H 0.658638 0.500309 0.024494 0.037 Uiso 1 1 calc R U . . . C65 C 0.82229(17) 0.54527(8) 0.02131(8) 0.0281(4) Uani 1 1 d . . . . . H65 H 0.853603 0.543869 -0.024504 0.034 Uiso 1 1 calc R U . . . C66 C 0.89282(16) 0.57366(8) 0.05884(7) 0.0226(3) Uani 1 1 d . . . . . H66 H 0.972085 0.591479 0.038524 0.027 Uiso 1 1 calc R U . . . C67 C 1.06356(14) 0.60846(7) 0.14324(7) 0.0169(3) Uani 1 1 d . . . . . C68 C 1.12843(16) 0.66386(8) 0.12728(8) 0.0242(3) Uani 1 1 d . . . . . H68 H 1.078976 0.705425 0.129615 0.029 Uiso 1 1 calc R U . . . C69 C 1.26611(17) 0.65906(9) 0.10777(9) 0.0323(4) Uani 1 1 d . . . . . H69 H 1.309647 0.697227 0.096926 0.039 Uiso 1 1 calc R U . . . C70 C 1.33887(16) 0.59842(10) 0.10430(8) 0.0334(4) Uani 1 1 d . . . . . H70 H 1.432354 0.595082 0.092238 0.040 Uiso 1 1 calc R U . . . C71 C 1.27488(16) 0.54300(9) 0.11844(8) 0.0288(4) Uani 1 1 d . . . . . H71 H 1.324214 0.501383 0.115389 0.035 Uiso 1 1 calc R U . . . C72 C 1.13889(15) 0.54816(8) 0.13706(7) 0.0218(3) Uani 1 1 d . . . . . H72 H 1.095777 0.509689 0.145839 0.026 Uiso 1 1 calc R U . . . C73 C 0.35014(18) 0.69234(9) 0.36208(9) 0.0348(4) Uani 1 1 d . . . . . H73 H 0.431779 0.705968 0.365354 0.042 Uiso 1 1 calc R U . . . C74 C 0.4597(2) 0.66546(13) 0.25194(10) 0.0511(6) Uani 1 1 d . . . . . H74A H 0.534393 0.680238 0.265702 0.077 Uiso 1 1 calc R U . . . H74B H 0.441217 0.692640 0.215387 0.077 Uiso 1 1 calc R U . . . H74C H 0.481376 0.620065 0.238494 0.077 Uiso 1 1 calc R U . . . C75 C 0.2250(2) 0.64771(17) 0.29578(12) 0.0677(8) Uani 1 1 d . . . . . H75A H 0.237021 0.600180 0.293035 0.102 Uiso 1 1 calc R U . . . H75B H 0.205979 0.666685 0.255329 0.102 Uiso 1 1 calc R U . . . H75C H 0.151399 0.660807 0.332235 0.102 Uiso 1 1 calc R U . . . C76 C 0.36008(18) 0.70603(9) 0.63905(9) 0.0309(4) Uani 1 1 d . . . . . H76 H 0.278451 0.692016 0.636285 0.037 Uiso 1 1 calc R U . . . C77 C 0.2415(2) 0.75309(12) 0.73983(11) 0.0565(6) Uani 1 1 d . . . . . H77A H 0.170165 0.732690 0.728494 0.085 Uiso 1 1 calc R U . . . H77B H 0.218584 0.800305 0.741974 0.085 Uiso 1 1 calc R U . . . H77C H 0.254229 0.736173 0.782128 0.085 Uiso 1 1 calc R U . . . C78 C 0.4819(2) 0.76357(12) 0.69757(12) 0.0525(6) Uani 1 1 d . . . . . H78A H 0.558063 0.741271 0.667637 0.079 Uiso 1 1 calc R U . . . H78B H 0.491845 0.756158 0.742276 0.079 Uiso 1 1 calc R U . . . H78C H 0.476528 0.810336 0.687488 0.079 Uiso 1 1 calc R U . . . H9P H 0.636(2) 0.7058(10) 0.5168(11) 0.040(6) Uiso 1 1 d . . . . . H9Q H 0.688(3) 0.6985(13) 0.4498(14) 0.064(8) Uiso 1 1 d . . . . . H10O H 0.955(3) 0.7755(15) 0.4398(15) 0.074(10) Uiso 1 1 d . . . . . H10P H 1.069(4) 0.7401(16) 0.4324(16) 0.089(11) Uiso 1 1 d . . . . . H11O H 1.142(3) 0.6319(13) 0.4628(14) 0.068(8) Uiso 1 1 d . . . . . H11P H 1.090(2) 0.6123(11) 0.5255(12) 0.044(6) Uiso 1 1 d . . . . . H12O H 0.798(2) 0.5478(12) 0.4981(12) 0.051(7) Uiso 1 1 d . . . . . H12P H 0.746(2) 0.5745(10) 0.5545(11) 0.041(6) Uiso 1 1 d . . . . . H13O H 1.120(3) 0.4362(14) 0.2771(13) 0.070(8) Uiso 1 1 d . . . . . H13P H 1.082(3) 0.4998(14) 0.2560(12) 0.061(8) Uiso 1 1 d . . . . . H14O H 1.057(2) 0.4873(11) 0.4257(11) 0.043(6) Uiso 1 1 d . . . . . H14P H 1.014(2) 0.5474(13) 0.4050(11) 0.049(7) Uiso 1 1 d . . . . . H15O H 0.711(2) 0.4430(11) 0.4504(10) 0.037(5) Uiso 1 1 d . . . . . H15P H 0.666(3) 0.5056(14) 0.4273(13) 0.068(8) Uiso 1 1 d . . . . . H16O H 0.687(3) 0.4564(14) 0.2997(14) 0.078(9) Uiso 1 1 d . . . . . H16P H 0.820(3) 0.4279(13) 0.2589(14) 0.067(8) Uiso 1 1 d . . . . . O17 O 0.53623(12) 0.49665(7) 0.29969(6) 0.0336(3) Uani 1 1 d . . . . . H17O H 0.528(3) 0.5255(16) 0.3363(16) 0.087(10) Uiso 1 1 d . . . . . H17P H 0.478(3) 0.4678(14) 0.3191(14) 0.073(8) Uiso 1 1 d . . . . . O18 O 0.54397(12) 0.56793(6) 0.40661(6) 0.0274(3) Uani 1 1 d . . . . . H18O H 0.587(2) 0.5991(12) 0.3916(11) 0.045(6) Uiso 1 1 d . . . . . H18P H 0.484(3) 0.5826(12) 0.4418(13) 0.056(7) Uiso 1 1 d . . . . . O19 O 0.36424(12) 0.63038(6) 0.50805(6) 0.0283(3) Uani 1 1 d . . . . . H19O H 0.329(2) 0.6632(13) 0.4846(13) 0.059(7) Uiso 1 1 d . . . . . H19P H 0.396(2) 0.6522(11) 0.5384(11) 0.044(6) Uiso 1 1 d . . . . . O20 O 0.62867(12) 0.59015(6) 0.63285(6) 0.0257(2) Uani 1 1 d . . . . . H20O H 0.582(2) 0.6231(12) 0.6230(11) 0.045(7) Uiso 1 1 d . . . . . H20P H 0.685(2) 0.6042(11) 0.6517(11) 0.048(6) Uiso 1 1 d . . . . . N1 N 0.34424(14) 0.67057(8) 0.30577(7) 0.0355(4) Uani 1 1 d . . . . . O21 O 0.25847(12) 0.69689(6) 0.41201(6) 0.0355(3) Uani 1 1 d . . . . . N2 N 0.36271(16) 0.73837(8) 0.69062(7) 0.0362(4) Uani 1 1 d . . . . . O22 O 0.45757(12) 0.69240(6) 0.59335(6) 0.0325(3) Uani 1 1 d . . . . . C79 C 0.2424(9) 0.8646(4) 0.0012(4) 0.039(2) Uani 0.645(18) 1 d D . P E 1 H79 H 0.202286 0.878588 -0.036314 0.047 Uiso 0.645(18) 1 calc R U P E 1 Cl1 Cl 0.3575(6) 0.79834(13) -0.0259(2) 0.0471(7) Uani 0.645(18) 1 d D . P E 1 Cl2 Cl 0.3173(3) 0.93089(9) 0.01735(10) 0.0476(8) Uani 0.645(18) 1 d D . P E 1 Cl3 Cl 0.1124(3) 0.84208(18) 0.0634(2) 0.0636(6) Uani 0.645(18) 1 d D . P E 1 C79' C 0.2233(18) 0.8646(6) 0.0056(8) 0.048(5) Uani 0.355(18) 1 d D . P E 2 H79' H 0.160408 0.876409 -0.023047 0.058 Uiso 0.355(18) 1 calc R U P E 2 Cl1' Cl 0.3381(12) 0.7996(4) -0.0249(5) 0.073(2) Uani 0.355(18) 1 d D . P E 2 Cl2' Cl 0.2956(9) 0.9320(3) 0.0213(4) 0.120(4) Uani 0.355(18) 1 d D . P E 2 Cl3' Cl 0.1413(12) 0.8425(3) 0.0838(7) 0.086(3) Uani 0.355(18) 1 d D . P E 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 Mg1 0.0200(2) 0.0160(2) 0.0123(2) -0.00188(18) -0.00559(19) -0.00154(19) Mg2 0.0195(2) 0.0148(2) 0.0144(2) -0.00076(18) -0.00482(19) -0.00183(19) P1 0.01777(18) 0.01250(17) 0.01107(17) -0.00148(13) -0.00350(13) -0.00205(14) P2 0.01663(18) 0.01472(18) 0.01088(17) -0.00035(13) -0.00426(13) -0.00206(14) O1 0.0178(5) 0.0133(5) 0.0126(5) -0.0025(4) -0.0035(4) -0.0020(4) O2 0.0208(5) 0.0152(5) 0.0141(5) -0.0001(4) -0.0029(4) -0.0010(4) O3 0.0222(5) 0.0165(5) 0.0142(5) -0.0020(4) -0.0059(4) -0.0005(4) O4 0.0207(5) 0.0185(5) 0.0157(5) -0.0018(4) -0.0029(4) -0.0055(4) O5 0.0157(5) 0.0173(5) 0.0126(5) 0.0011(4) -0.0045(4) -0.0016(4) O6 0.0192(5) 0.0198(5) 0.0129(5) -0.0017(4) -0.0057(4) -0.0006(4) O7 0.0239(5) 0.0158(5) 0.0158(5) 0.0000(4) -0.0072(4) -0.0030(4) O8 0.0168(5) 0.0199(5) 0.0169(5) 0.0002(4) -0.0036(4) -0.0024(4) O9 0.0237(6) 0.0276(6) 0.0171(6) -0.0052(5) -0.0069(5) 0.0025(5) O10 0.0397(8) 0.0211(6) 0.0248(6) 0.0029(5) -0.0091(6) -0.0089(6) O11 0.0191(6) 0.0255(6) 0.0147(5) -0.0006(4) -0.0039(4) -0.0040(4) O12 0.0221(6) 0.0198(6) 0.0164(5) -0.0028(4) -0.0037(5) -0.0046(4) O13 0.0298(6) 0.0205(6) 0.0177(5) 0.0026(4) -0.0024(5) -0.0024(5) O14 0.0283(6) 0.0165(6) 0.0274(6) -0.0026(5) -0.0151(5) 0.0000(5) O15 0.0218(6) 0.0212(6) 0.0200(5) 0.0019(4) -0.0026(4) -0.0014(5) O16 0.0287(7) 0.0269(6) 0.0250(6) -0.0028(5) -0.0105(5) -0.0056(5) C1 0.0186(7) 0.0131(7) 0.0147(7) -0.0025(5) -0.0037(5) -0.0023(5) C2 0.0228(8) 0.0147(7) 0.0160(7) -0.0002(6) -0.0044(6) -0.0049(6) C3 0.0347(9) 0.0185(7) 0.0130(7) 0.0006(6) 0.0030(6) -0.0017(7) C4 0.0486(11) 0.0167(8) 0.0236(8) -0.0013(7) 0.0074(8) 0.0046(7) C5 0.0426(10) 0.0132(7) 0.0218(8) 0.0028(6) 0.0016(7) 0.0008(7) C6 0.0253(8) 0.0166(7) 0.0143(7) 0.0008(6) -0.0023(6) -0.0048(6) C7 0.0207(7) 0.0143(7) 0.0117(6) -0.0003(5) -0.0029(5) -0.0022(6) C8 0.0194(7) 0.0117(7) 0.0178(7) 0.0007(5) -0.0028(6) -0.0007(5) C9 0.0249(8) 0.0307(9) 0.0216(8) -0.0017(7) -0.0074(6) -0.0029(7) C10 0.0213(8) 0.0391(10) 0.0384(10) -0.0030(8) -0.0092(7) -0.0080(7) C11 0.0196(8) 0.0273(9) 0.0370(10) 0.0029(7) 0.0026(7) -0.0045(7) C12 0.0294(9) 0.0341(9) 0.0201(8) 0.0047(7) 0.0011(7) -0.0049(7) C13 0.0252(8) 0.0287(8) 0.0178(7) 0.0016(6) -0.0038(6) -0.0063(7) C14 0.0169(7) 0.0227(8) 0.0135(7) 0.0006(6) -0.0002(5) -0.0038(6) C15 0.0229(8) 0.0260(8) 0.0229(8) -0.0002(6) -0.0025(6) -0.0019(7) C16 0.0245(9) 0.0384(10) 0.0360(10) 0.0044(8) -0.0087(7) 0.0049(7) C17 0.0263(9) 0.0567(13) 0.0396(11) -0.0042(9) -0.0182(8) -0.0028(9) C18 0.0357(10) 0.0451(11) 0.0460(11) -0.0141(9) -0.0207(9) -0.0037(9) C19 0.0286(9) 0.0269(9) 0.0318(9) -0.0067(7) -0.0106(7) -0.0016(7) C20 0.020(3) 0.0208(19) 0.026(2) -0.0038(16) 0.002(2) 0.010(2) C21 0.057(4) 0.036(3) 0.037(3) -0.014(2) -0.006(3) 0.016(3) C22 0.028(3) 0.051(3) 0.072(4) -0.034(3) -0.007(2) 0.013(2) C23 0.067(5) 0.028(2) 0.055(3) 0.002(2) 0.009(3) 0.019(3) C20' 0.031(3) 0.0220(18) 0.029(2) 0.0007(15) -0.001(2) 0.008(2) C21' 0.060(4) 0.028(2) 0.028(2) -0.0117(17) -0.002(2) 0.007(3) C22' 0.051(4) 0.032(3) 0.041(3) -0.0036(19) -0.006(2) 0.010(2) C23' 0.063(4) 0.0165(18) 0.039(2) -0.0047(15) 0.007(2) 0.013(2) C24 0.0251(8) 0.0136(7) 0.0135(7) 0.0005(5) -0.0012(6) -0.0032(6) C25 0.0280(8) 0.0161(7) 0.0162(7) 0.0055(6) -0.0063(6) -0.0034(6) C26 0.0370(10) 0.0327(9) 0.0272(9) -0.0038(7) -0.0031(7) -0.0137(8) C27 0.0526(12) 0.0459(12) 0.0343(10) -0.0020(9) -0.0126(9) -0.0274(10) C28 0.0340(10) 0.0413(11) 0.0380(10) 0.0147(8) -0.0153(8) -0.0187(8) C29 0.0257(9) 0.0326(9) 0.0372(10) 0.0106(8) -0.0048(7) -0.0016(7) C30 0.0296(9) 0.0215(8) 0.0255(8) 0.0020(6) -0.0057(7) -0.0016(7) C31 0.0216(7) 0.0184(7) 0.0135(7) 0.0014(6) -0.0005(6) -0.0021(6) C32 0.0215(8) 0.0199(8) 0.0288(8) 0.0044(6) -0.0025(6) -0.0035(6) C33 0.0268(9) 0.0229(8) 0.0380(10) 0.0117(7) -0.0009(7) 0.0005(7) C34 0.0271(9) 0.0375(10) 0.0269(9) 0.0103(7) -0.0052(7) 0.0045(7) C35 0.0251(9) 0.0394(10) 0.0239(8) -0.0009(7) -0.0059(7) -0.0053(7) C36 0.0287(9) 0.0246(8) 0.0204(8) 0.0016(6) -0.0039(6) -0.0077(7) C37 0.0132(7) 0.0162(7) 0.0130(7) 0.0018(5) -0.0036(5) -0.0022(5) C38 0.0164(7) 0.0167(7) 0.0154(7) -0.0020(5) -0.0034(5) -0.0035(6) C39 0.0218(8) 0.0141(7) 0.0216(7) -0.0016(6) -0.0054(6) 0.0014(6) C40 0.0210(8) 0.0204(7) 0.0176(7) 0.0018(6) -0.0059(6) -0.0003(6) C41 0.0202(7) 0.0223(8) 0.0140(7) -0.0020(6) -0.0055(6) -0.0009(6) C42 0.0141(7) 0.0153(7) 0.0134(7) -0.0006(5) -0.0013(5) -0.0012(5) C43 0.0201(7) 0.0163(7) 0.0188(7) -0.0044(6) -0.0064(6) -0.0016(6) C44 0.020(2) 0.027(3) 0.023(3) -0.014(2) -0.0095(18) 0.001(2) C45 0.030(2) 0.031(3) 0.0207(18) -0.006(2) -0.0092(14) 0.002(2) C46 0.0269(19) 0.036(3) 0.0280(18) -0.006(3) -0.0125(14) 0.007(2) C47 0.025(2) 0.036(2) 0.031(2) -0.0101(18) -0.0126(17) 0.0100(19) C48 0.029(2) 0.031(2) 0.037(2) -0.0140(18) -0.0158(18) 0.0067(16) C49 0.0273(19) 0.0236(19) 0.025(2) -0.010(2) -0.0144(18) 0.0038(15) C44' 0.026(2) 0.022(2) 0.025(3) -0.0112(19) -0.0120(18) 0.0058(19) C45' 0.0230(16) 0.031(2) 0.0204(17) -0.007(2) -0.0085(13) 0.0062(19) C46' 0.0270(18) 0.038(2) 0.0304(18) -0.010(2) -0.0075(14) 0.006(2) C47' 0.0317(18) 0.035(2) 0.037(2) -0.014(2) -0.0123(16) 0.011(2) C48' 0.040(3) 0.029(2) 0.050(3) -0.022(2) -0.019(3) 0.013(2) C49' 0.030(2) 0.026(2) 0.033(3) -0.013(2) -0.016(2) 0.0047(16) C50 0.0226(8) 0.0164(7) 0.0250(8) 0.0009(6) -0.0100(6) -0.0037(6) C51 0.0317(9) 0.0205(8) 0.0316(9) -0.0029(7) -0.0155(7) -0.0034(7) C52 0.0431(11) 0.0283(9) 0.0456(11) 0.0017(8) -0.0284(9) -0.0109(8) C53 0.0304(10) 0.0445(11) 0.0575(13) 0.0086(10) -0.0208(9) -0.0210(9) C54 0.0277(10) 0.0639(14) 0.0526(13) -0.0068(11) -0.0017(9) -0.0138(10) C55 0.0269(9) 0.0445(11) 0.0364(10) -0.0086(8) -0.0057(7) -0.0117(8) C56 0.0356(9) 0.0273(9) 0.0276(8) 0.0016(7) -0.0162(7) 0.0041(7) C57 0.0638(17) 0.0395(13) 0.0523(15) 0.0251(11) -0.0330(13) -0.0078(12) C58 0.0342(12) 0.0480(14) 0.0435(13) 0.0016(11) -0.0179(10) 0.0107(10) C59 0.0590(16) 0.0513(14) 0.0277(11) -0.0023(10) -0.0237(11) 0.0213(12) C59' 0.056(4) 0.045(4) 0.036(4) 0.015(3) -0.020(3) 0.013(4) C57' 0.057(4) 0.043(3) 0.043(4) 0.006(3) -0.024(3) 0.014(3) C58' 0.049(4) 0.050(4) 0.045(4) 0.004(4) -0.026(3) 0.006(3) C60 0.0180(7) 0.0163(7) 0.0118(6) -0.0011(5) -0.0028(5) -0.0006(6) C61 0.0178(7) 0.0145(7) 0.0188(7) -0.0041(6) -0.0050(6) 0.0033(6) C62 0.0213(8) 0.0209(8) 0.0239(8) -0.0007(6) -0.0044(6) 0.0002(6) C63 0.0216(8) 0.0233(8) 0.0450(11) 0.0001(7) -0.0138(7) -0.0022(7) C64 0.0344(10) 0.0242(8) 0.0411(10) -0.0082(7) -0.0255(8) 0.0022(7) C65 0.0373(10) 0.0267(9) 0.0225(8) -0.0082(7) -0.0139(7) 0.0044(7) C66 0.0248(8) 0.0238(8) 0.0189(7) -0.0034(6) -0.0051(6) 0.0002(6) C67 0.0181(7) 0.0218(7) 0.0102(6) -0.0021(5) -0.0031(5) 0.0012(6) C68 0.0221(8) 0.0240(8) 0.0252(8) 0.0031(6) -0.0035(6) -0.0016(6) C69 0.0228(9) 0.0391(10) 0.0335(9) 0.0082(8) -0.0020(7) -0.0090(7) C70 0.0167(8) 0.0505(11) 0.0280(9) 0.0101(8) 0.0004(7) 0.0023(8) C71 0.0255(9) 0.0352(9) 0.0200(8) 0.0032(7) -0.0006(6) 0.0097(7) C72 0.0252(8) 0.0225(8) 0.0159(7) 0.0012(6) -0.0032(6) 0.0020(6) C73 0.0266(9) 0.0412(11) 0.0370(10) 0.0094(8) -0.0070(8) -0.0101(8) C74 0.0335(11) 0.0745(16) 0.0383(11) 0.0071(11) 0.0019(9) -0.0004(10) C75 0.0412(13) 0.125(3) 0.0413(13) -0.0144(14) -0.0077(10) -0.0264(14) C76 0.0279(9) 0.0310(9) 0.0345(10) 0.0055(8) -0.0103(7) -0.0021(7) C77 0.0640(15) 0.0539(14) 0.0386(12) 0.0002(10) 0.0063(11) 0.0105(12) C78 0.0685(15) 0.0508(13) 0.0483(13) -0.0024(10) -0.0316(11) -0.0105(11) O17 0.0289(7) 0.0413(8) 0.0320(7) 0.0050(6) -0.0069(5) -0.0119(6) O18 0.0192(6) 0.0250(6) 0.0361(7) 0.0001(5) -0.0011(5) -0.0056(5) O19 0.0264(6) 0.0325(7) 0.0265(6) 0.0021(5) -0.0064(5) -0.0058(5) O20 0.0204(6) 0.0318(7) 0.0260(6) -0.0021(5) -0.0057(5) -0.0066(5) N1 0.0250(8) 0.0492(10) 0.0302(8) 0.0066(7) -0.0033(6) -0.0036(7) O21 0.0314(7) 0.0435(8) 0.0299(7) 0.0062(6) -0.0034(5) -0.0074(6) N2 0.0437(9) 0.0350(9) 0.0285(8) 0.0013(7) -0.0078(7) 0.0009(7) O22 0.0278(6) 0.0393(7) 0.0297(6) -0.0008(5) -0.0075(5) 0.0005(5) C79 0.036(3) 0.044(5) 0.039(3) 0.004(3) -0.014(2) 0.000(2) Cl1 0.0457(11) 0.0310(11) 0.0602(13) -0.0080(8) -0.0029(7) -0.0014(7) Cl2 0.0473(9) 0.0342(9) 0.0627(14) -0.0093(7) -0.0136(6) -0.0046(5) Cl3 0.0632(10) 0.0630(9) 0.0569(12) 0.0047(8) -0.0007(8) -0.0034(7) C79' 0.041(7) 0.033(7) 0.080(11) 0.000(6) -0.028(6) -0.011(5) Cl1' 0.061(4) 0.081(4) 0.082(3) -0.024(2) -0.015(2) -0.018(2) Cl2' 0.056(2) 0.095(4) 0.205(8) -0.079(5) -0.003(2) -0.0199(18) Cl3' 0.081(4) 0.0658(18) 0.082(4) 0.025(2) 0.029(3) 0.005(2) 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' Cl Cl 0.1484 0.1585 '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' N N 0.0061 0.0033 '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' P P 0.1023 0.0942 '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 O3 Mg1 O6 178.83(5) . . O3 Mg1 O9 91.37(5) . . O6 Mg1 O9 89.75(5) . . O3 Mg1 O11 92.00(5) . . O6 Mg1 O11 86.89(5) . . O9 Mg1 O11 176.44(5) . . O3 Mg1 O10 89.79(5) . . O6 Mg1 O10 89.78(5) . . O9 Mg1 O10 94.75(6) . . O11 Mg1 O10 86.41(6) . . O3 Mg1 O12 90.53(5) . . O6 Mg1 O12 89.74(5) . . O9 Mg1 O12 93.73(5) . . O11 Mg1 O12 85.10(5) . . O10 Mg1 O12 171.50(6) . . O7 Mg2 O2 176.07(5) . 2_766 O7 Mg2 O14 89.15(5) . . O2 Mg2 O14 87.02(5) 2_766 . O7 Mg2 O15 89.60(5) . . O2 Mg2 O15 89.68(5) 2_766 . O14 Mg2 O15 92.12(5) . . O7 Mg2 O13 89.74(5) . . O2 Mg2 O13 91.03(5) 2_766 . O14 Mg2 O13 88.57(5) . . O15 Mg2 O13 179.04(5) . . O7 Mg2 O16 92.14(5) . . O2 Mg2 O16 91.75(5) 2_766 . O14 Mg2 O16 175.76(6) . . O15 Mg2 O16 91.93(5) . . O13 Mg2 O16 87.40(5) . . O3 P1 O2 113.53(6) . . O3 P1 O4 111.93(6) . . O2 P1 O4 113.22(6) . . O3 P1 O1 108.68(5) . . O2 P1 O1 101.54(5) . . O4 P1 O1 107.12(5) . . O7 P2 O6 112.58(6) . . O7 P2 O8 112.99(6) . . O6 P2 O8 112.83(6) . . O7 P2 O5 107.19(5) . . O6 P2 O5 102.49(5) . . O8 P2 O5 107.96(5) . . C1 O1 P1 122.57(9) . . P1 O2 Mg2 131.27(6) . 2_766 P1 O3 Mg1 133.32(6) . . C37 O5 P2 123.37(8) . . P2 O6 Mg1 137.94(6) . . P2 O7 Mg2 137.86(6) . . Mg1 O9 H9P 123.1(15) . . Mg1 O9 H9Q 108.0(18) . . H9P O9 H9Q 111(2) . . Mg1 O10 H10O 121(2) . . Mg1 O10 H10P 118(2) . . H10O O10 H10P 106(3) . . Mg1 O11 H11O 114.9(18) . . Mg1 O11 H11P 109.5(15) . . H11O O11 H11P 106(2) . . Mg1 O12 H12O 119.7(18) . . Mg1 O12 H12P 112.3(14) . . H12O O12 H12P 104(2) . . Mg2 O13 H13O 108.1(16) . . Mg2 O13 H13P 113.3(17) . . H13O O13 H13P 101(2) . . Mg2 O14 H14O 124.4(15) . . Mg2 O14 H14P 118.7(17) . . H14O O14 H14P 112(2) . . Mg2 O15 H15O 114.1(13) . . Mg2 O15 H15P 114.6(18) . . H15O O15 H15P 107(2) . . Mg2 O16 H16O 115.3(16) . . Mg2 O16 H16P 107.6(19) . . H16O O16 H16P 115(3) . . O1 C1 C6 118.80(12) . . O1 C1 C2 119.71(12) . . C6 C1 C2 121.25(13) . . C3 C2 C1 118.00(13) . . C3 C2 C7 120.59(13) . . C1 C2 C7 121.38(13) . . C2 C3 C4 122.69(14) . . C2 C3 H3 118.7 . . C4 C3 H3 118.7 . . C5 C4 C3 117.20(15) . . C5 C4 C20' 123.3(2) . . C3 C4 C20' 118.6(3) . . C5 C4 C20 120.2(3) . . C3 C4 C20 121.2(3) . . C4 C5 C6 122.29(15) . . C4 C5 H5 118.9 . . C6 C5 H5 118.9 . . C5 C6 C1 118.52(13) . . C5 C6 C24 121.75(13) . . C1 C6 C24 119.58(13) . . C2 C7 C14 113.82(12) . . C2 C7 C8 111.06(12) . . C14 C7 C8 111.81(11) . . C2 C7 H7 106.5 . . C14 C7 H7 106.5 . . C8 C7 H7 106.5 . . C13 C8 C9 118.05(14) . . C13 C8 C7 122.78(13) . . C9 C8 C7 119.17(13) . . C10 C9 C8 120.94(15) . . C10 C9 H9 119.5 . . C8 C9 H9 119.5 . . C9 C10 C11 120.65(16) . . C9 C10 H10 119.7 . . C11 C10 H10 119.7 . . C12 C11 C10 119.04(15) . . C12 C11 H11 120.5 . . C10 C11 H11 120.5 . . C11 C12 C13 120.56(16) . . C11 C12 H12 119.7 . . C13 C12 H12 119.7 . . C8 C13 C12 120.75(15) . . C8 C13 H13 119.6 . . C12 C13 H13 119.6 . . C19 C14 C15 118.19(14) . . C19 C14 C7 123.17(14) . . C15 C14 C7 118.50(13) . . C16 C15 C14 120.90(16) . . C16 C15 H15 119.5 . . C14 C15 H15 119.5 . . C17 C16 C15 120.32(17) . . C17 C16 H16 119.8 . . C15 C16 H16 119.8 . . C16 C17 C18 119.33(17) . . C16 C17 H17 120.3 . . C18 C17 H17 120.3 . . C17 C18 C19 120.88(17) . . C17 C18 H18 119.6 . . C19 C18 H18 119.6 . . C14 C19 C18 120.36(17) . . C14 C19 H19 119.8 . . C18 C19 H19 119.8 . . C22 C20 C21 109.1(5) . . C22 C20 C23 109.6(5) . . C21 C20 C23 106.8(6) . . C22 C20 C4 114.6(5) . . C21 C20 C4 105.7(5) . . C23 C20 C4 110.7(4) . . C20 C21 H21A 109.5 . . C20 C21 H21B 109.5 . . H21A C21 H21B 109.5 . . C20 C21 H21C 109.5 . . H21A C21 H21C 109.5 . . H21B C21 H21C 109.5 . . C20 C22 H22A 109.5 . . C20 C22 H22B 109.5 . . H22A C22 H22B 109.5 . . C20 C22 H22C 109.5 . . H22A C22 H22C 109.5 . . H22B C22 H22C 109.5 . . C20 C23 H23A 109.5 . . C20 C23 H23B 109.5 . . H23A C23 H23B 109.5 . . C20 C23 H23C 109.5 . . H23A C23 H23C 109.5 . . H23B C23 H23C 109.5 . . C22' C20' C4 102.5(4) . . C22' C20' C23' 108.6(4) . . C4 C20' C23' 112.9(4) . . C22' C20' C21' 107.3(4) . . C4 C20' C21' 115.9(4) . . C23' C20' C21' 109.0(5) . . C20' C21' H21D 109.5 . . C20' C21' H21E 109.5 . . H21D C21' H21E 109.5 . . C20' C21' H21F 109.5 . . H21D C21' H21F 109.5 . . H21E C21' H21F 109.5 . . C20' C22' H22D 109.5 . . C20' C22' H22E 109.5 . . H22D C22' H22E 109.5 . . C20' C22' H22F 109.5 . . H22D C22' H22F 109.5 . . H22E C22' H22F 109.5 . . C20' C23' H23D 109.5 . . C20' C23' H23E 109.5 . . H23D C23' H23E 109.5 . . C20' C23' H23F 109.5 . . H23D C23' H23F 109.5 . . H23E C23' H23F 109.5 . . C25 C24 C31 114.19(12) . . C25 C24 C6 110.76(12) . . C31 C24 C6 112.31(12) . . C25 C24 H24 106.3 . . C31 C24 H24 106.3 . . C6 C24 H24 106.3 . . C26 C25 C30 118.22(15) . . C26 C25 C24 122.31(14) . . C30 C25 C24 119.47(14) . . C27 C26 C25 120.64(17) . . C27 C26 H26 119.7 . . C25 C26 H26 119.7 . . C28 C27 C26 120.77(17) . . C28 C27 H27 119.6 . . C26 C27 H27 119.6 . . C27 C28 C29 119.17(17) . . C27 C28 H28 120.4 . . C29 C28 H28 120.4 . . C28 C29 C30 120.33(17) . . C28 C29 H29 119.8 . . C30 C29 H29 119.8 . . C29 C30 C25 120.86(16) . . C29 C30 H30 119.6 . . C25 C30 H30 119.6 . . C32 C31 C36 118.02(14) . . C32 C31 C24 124.12(14) . . C36 C31 C24 117.83(13) . . C31 C32 C33 120.77(15) . . C31 C32 H32 119.6 . . C33 C32 H32 119.6 . . C34 C33 C32 120.42(15) . . C34 C33 H33 119.8 . . C32 C33 H33 119.8 . . C33 C34 C35 119.33(16) . . C33 C34 H34 120.3 . . C35 C34 H34 120.3 . . C36 C35 C34 120.30(16) . . C36 C35 H35 119.8 . . C34 C35 H35 119.8 . . C35 C36 C31 121.14(15) . . C35 C36 H36 119.4 . . C31 C36 H36 119.4 . . O5 C37 C38 118.97(12) . . O5 C37 C42 119.62(12) . . C38 C37 C42 121.14(13) . . C39 C38 C37 118.32(13) . . C39 C38 C43 120.99(13) . . C37 C38 C43 120.63(13) . . C40 C39 C38 122.54(14) . . C40 C39 H39 118.7 . . C38 C39 H39 118.7 . . C39 C40 C41 117.35(13) . . C39 C40 C56 120.13(14) . . C41 C40 C56 122.49(13) . . C40 C41 C42 122.36(13) . . C40 C41 H41 118.8 . . C42 C41 H41 118.8 . . C41 C42 C37 118.25(13) . . C41 C42 C60 121.48(12) . . C37 C42 C60 120.22(12) . . C44' C43 C38 110.4(6) . . C44' C43 C50 117.5(5) . . C38 C43 C50 112.68(12) . . C38 C43 C44 108.9(6) . . C50 C43 C44 111.3(4) . . C38 C43 H43 107.9 . . C50 C43 H43 107.9 . . C44 C43 H43 107.9 . . C45 C44 C49 118.3(7) . . C45 C44 C43 119.9(6) . . C49 C44 C43 121.5(6) . . C44 C45 C46 123.1(6) . . C44 C45 H45 118.5 . . C46 C45 H45 118.5 . . C45 C46 C47 118.2(5) . . C45 C46 H46 120.9 . . C47 C46 H46 120.9 . . C48 C47 C46 120.3(4) . . C48 C47 H47 119.9 . . C46 C47 H47 119.9 . . C47 C48 C49 120.2(5) . . C47 C48 H48 119.9 . . C49 C48 H48 119.9 . . C48 C49 C44 119.8(6) . . C48 C49 H49 120.1 . . C44 C49 H49 120.1 . . C49' C44' C45' 119.6(7) . . C49' C44' C43 123.1(6) . . C45' C44' C43 117.3(6) . . C46' C45' C44' 120.9(5) . . C46' C45' H45' 119.6 . . C44' C45' H45' 119.6 . . C47' C46' C45' 119.1(5) . . C47' C46' H46' 120.4 . . C45' C46' H46' 120.4 . . C48' C47' C46' 121.2(4) . . C48' C47' H47' 119.4 . . C46' C47' H47' 119.4 . . C47' C48' C49' 119.7(5) . . C47' C48' H48' 120.2 . . C49' C48' H48' 120.2 . . C44' C49' C48' 119.4(6) . . C44' C49' H49' 120.3 . . C48' C49' H49' 120.3 . . C55 C50 C51 117.91(15) . . C55 C50 C43 122.36(14) . . C51 C50 C43 119.57(14) . . C52 C51 C50 120.69(17) . . C52 C51 H51 119.7 . . C50 C51 H51 119.7 . . C53 C52 C51 120.43(17) . . C53 C52 H52 119.8 . . C51 C52 H52 119.8 . . C54 C53 C52 119.50(17) . . C54 C53 H53 120.2 . . C52 C53 H53 120.2 . . C53 C54 C55 120.40(19) . . C53 C54 H54 119.8 . . C55 C54 H54 119.8 . . C50 C55 C54 121.06(17) . . C50 C55 H55 119.5 . . C54 C55 H55 119.5 . . C59 C56 C57 110.5(2) . . C57' C56 C40 116.3(5) . . C59 C56 C40 113.45(15) . . C57 C56 C40 110.55(15) . . C59 C56 C58 107.93(18) . . C57 C56 C58 106.40(19) . . C40 C56 C58 107.68(15) . . C57' C56 C58' 110.8(8) . . C40 C56 C58' 105.8(5) . . C57' C56 C59' 113.9(8) . . C40 C56 C59' 105.6(4) . . C58' C56 C59' 103.3(8) . . C56 C57 H57A 109.5 . . C56 C57 H57B 109.5 . . H57A C57 H57B 109.5 . . C56 C57 H57C 109.5 . . H57A C57 H57C 109.5 . . H57B C57 H57C 109.5 . . C56 C58 H58A 109.5 . . C56 C58 H58B 109.5 . . H58A C58 H58B 109.5 . . C56 C58 H58C 109.5 . . H58A C58 H58C 109.5 . . H58B C58 H58C 109.5 . . C56 C59 H59A 109.5 . . C56 C59 H59B 109.5 . . H59A C59 H59B 109.5 . . C56 C59 H59C 109.5 . . H59A C59 H59C 109.5 . . H59B C59 H59C 109.5 . . C56 C59' H59D 109.5 . . C56 C59' H59E 109.5 . . H59D C59' H59E 109.5 . . C56 C59' H59F 109.5 . . H59D C59' H59F 109.5 . . H59E C59' H59F 109.5 . . C56 C57' H57D 109.5 . . C56 C57' H57E 109.5 . . H57D C57' H57E 109.5 . . C56 C57' H57F 109.5 . . H57D C57' H57F 109.5 . . H57E C57' H57F 109.5 . . C56 C58' H58D 109.5 . . C56 C58' H58E 109.5 . . H58D C58' H58E 109.5 . . C56 C58' H58F 109.5 . . H58D C58' H58F 109.5 . . H58E C58' H58F 109.5 . . C61 C60 C67 113.18(11) . . C61 C60 C42 111.11(12) . . C67 C60 C42 112.80(12) . . C61 C60 H60 106.4 . . C67 C60 H60 106.4 . . C42 C60 H60 106.4 . . C62 C61 C66 118.75(14) . . C62 C61 C60 118.46(13) . . C66 C61 C60 122.70(13) . . C63 C62 C61 120.75(15) . . C63 C62 H62 119.6 . . C61 C62 H62 119.6 . . C64 C63 C62 120.01(16) . . C64 C63 H63 120.0 . . C62 C63 H63 120.0 . . C65 C64 C63 119.81(15) . . C65 C64 H64 120.1 . . C63 C64 H64 120.1 . . C64 C65 C66 120.33(16) . . C64 C65 H65 119.8 . . C66 C65 H65 119.8 . . C65 C66 C61 120.33(15) . . C65 C66 H66 119.8 . . C61 C66 H66 119.8 . . C68 C67 C72 118.14(14) . . C68 C67 C60 123.14(13) . . C72 C67 C60 118.70(13) . . C67 C68 C69 120.63(15) . . C67 C68 H68 119.7 . . C69 C68 H68 119.7 . . C70 C69 C68 119.92(16) . . C70 C69 H69 120.0 . . C68 C69 H69 120.0 . . C71 C70 C69 119.77(16) . . C71 C70 H70 120.1 . . C69 C70 H70 120.1 . . C70 C71 C72 119.91(16) . . C70 C71 H71 120.0 . . C72 C71 H71 120.0 . . C71 C72 C67 121.57(15) . . C71 C72 H72 119.2 . . C67 C72 H72 119.2 . . O21 C73 N1 126.24(17) . . O21 C73 H73 116.9 . . N1 C73 H73 116.9 . . N1 C74 H74A 109.5 . . N1 C74 H74B 109.5 . . H74A C74 H74B 109.5 . . N1 C74 H74C 109.5 . . H74A C74 H74C 109.5 . . H74B C74 H74C 109.5 . . N1 C75 H75A 109.5 . . N1 C75 H75B 109.5 . . H75A C75 H75B 109.5 . . N1 C75 H75C 109.5 . . H75A C75 H75C 109.5 . . H75B C75 H75C 109.5 . . O22 C76 N2 124.51(17) . . O22 C76 H76 117.7 . . N2 C76 H76 117.7 . . N2 C77 H77A 109.5 . . N2 C77 H77B 109.5 . . H77A C77 H77B 109.5 . . N2 C77 H77C 109.5 . . H77A C77 H77C 109.5 . . H77B C77 H77C 109.5 . . N2 C78 H78A 109.5 . . N2 C78 H78B 109.5 . . H78A C78 H78B 109.5 . . N2 C78 H78C 109.5 . . H78A C78 H78C 109.5 . . H78B C78 H78C 109.5 . . H17O O17 H17P 99(2) . . H18O O18 H18P 107(2) . . H19O O19 H19P 104(2) . . H20O O20 H20P 107(2) . . C73 N1 C75 121.37(16) . . C73 N1 C74 120.90(17) . . C75 N1 C74 117.66(17) . . C76 N2 C78 121.30(17) . . C76 N2 C77 119.47(18) . . C78 N2 C77 119.10(18) . . Cl2 C79 Cl1 111.8(5) . . Cl2 C79 Cl3 115.5(4) . . Cl1 C79 Cl3 111.7(5) . . Cl2 C79 H79 105.6 . . Cl1 C79 H79 105.6 . . Cl3 C79 H79 105.6 . . Cl2' C79' Cl1' 112.9(10) . . Cl2' C79' Cl3' 101.3(10) . . Cl1' C79' Cl3' 107.5(9) . . Cl2' C79' H79' 111.5 . . Cl1' C79' H79' 111.5 . . Cl3' C79' H79' 111.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Mg1 O3 1.9930(10) . Mg1 O6 2.0048(10) . Mg1 O9 2.0799(12) . Mg1 O11 2.0983(12) . Mg1 O10 2.1270(13) . Mg1 O12 2.1744(12) . Mg2 O7 2.0078(11) . Mg2 O2 2.0354(11) 2_766 Mg2 O14 2.0866(12) . Mg2 O15 2.1012(12) . Mg2 O13 2.1017(12) . Mg2 O16 2.1095(12) . P1 O3 1.5052(10) . P1 O2 1.5157(11) . P1 O4 1.5181(10) . P1 O1 1.6351(10) . P2 O7 1.5066(10) . P2 O6 1.5147(10) . P2 O8 1.5192(11) . P2 O5 1.6333(10) . O1 C1 1.3934(17) . O5 C37 1.3873(17) . O9 H9P 0.86(2) . O9 H9Q 0.85(3) . O10 H10O 0.77(3) . O10 H10P 0.87(4) . O11 H11O 0.87(3) . O11 H11P 0.85(2) . O12 H12O 0.78(3) . O12 H12P 0.88(2) . O13 H13O 0.97(3) . O13 H13P 0.86(3) . O14 H14O 0.84(3) . O14 H14P 0.81(3) . O15 H15O 0.90(2) . O15 H15P 0.88(3) . O16 H16O 0.98(3) . O16 H16P 0.83(3) . C1 C6 1.393(2) . C1 C2 1.397(2) . C2 C3 1.392(2) . C2 C7 1.518(2) . C3 C4 1.393(2) . C3 H3 0.9500 . C4 C5 1.392(2) . C4 C20' 1.515(6) . C4 C20 1.601(7) . C5 C6 1.392(2) . C5 H5 0.9500 . C6 C24 1.532(2) . C7 C14 1.522(2) . C7 C8 1.530(2) . C7 H7 1.0000 . C8 C13 1.388(2) . C8 C9 1.393(2) . C9 C10 1.380(2) . C9 H9 0.9500 . C10 C11 1.383(3) . C10 H10 0.9500 . C11 C12 1.377(3) . C11 H11 0.9500 . C12 C13 1.392(2) . C12 H12 0.9500 . C13 H13 0.9500 . C14 C19 1.386(2) . C14 C15 1.390(2) . C15 C16 1.388(2) . C15 H15 0.9500 . C16 C17 1.370(3) . C16 H16 0.9500 . C17 C18 1.375(3) . C17 H17 0.9500 . C18 C19 1.387(2) . C18 H18 0.9500 . C19 H19 0.9500 . C20 C22 1.506(7) . C20 C21 1.521(8) . C20 C23 1.524(8) . C21 H21A 0.9800 . C21 H21B 0.9800 . C21 H21C 0.9800 . C22 H22A 0.9800 . C22 H22B 0.9800 . C22 H22C 0.9800 . C23 H23A 0.9800 . C23 H23B 0.9800 . C23 H23C 0.9800 . C20' C22' 1.511(7) . C20' C23' 1.523(7) . C20' C21' 1.533(7) . C21' H21D 0.9800 . C21' H21E 0.9800 . C21' H21F 0.9800 . C22' H22D 0.9800 . C22' H22E 0.9800 . C22' H22F 0.9800 . C23' H23D 0.9800 . C23' H23E 0.9800 . C23' H23F 0.9800 . C24 C25 1.520(2) . C24 C31 1.522(2) . C24 H24 1.0000 . C25 C26 1.391(2) . C25 C30 1.393(2) . C26 C27 1.388(3) . C26 H26 0.9500 . C27 C28 1.376(3) . C27 H27 0.9500 . C28 C29 1.385(3) . C28 H28 0.9500 . C29 C30 1.388(2) . C29 H29 0.9500 . C30 H30 0.9500 . C31 C32 1.392(2) . C31 C36 1.397(2) . C32 C33 1.393(2) . C32 H32 0.9500 . C33 C34 1.381(3) . C33 H33 0.9500 . C34 C35 1.388(3) . C34 H34 0.9500 . C35 C36 1.381(2) . C35 H35 0.9500 . C36 H36 0.9500 . C37 C38 1.396(2) . C37 C42 1.3973(19) . C38 C39 1.391(2) . C38 C43 1.5278(19) . C39 C40 1.390(2) . C39 H39 0.9500 . C40 C41 1.393(2) . C40 C56 1.532(2) . C41 C42 1.394(2) . C41 H41 0.9500 . C42 C60 1.528(2) . C43 C44' 1.509(9) . C43 C50 1.530(2) . C43 C44 1.552(10) . C43 H43 1.0000 . C44 C45 1.378(9) . C44 C49 1.405(9) . C45 C46 1.379(8) . C45 H45 0.9500 . C46 C47 1.398(7) . C46 H46 0.9500 . C47 C48 1.393(7) . C47 H47 0.9500 . C48 C49 1.394(6) . C48 H48 0.9500 . C49 H49 0.9500 . C44' C49' 1.385(8) . C44' C45' 1.390(9) . C45' C46' 1.382(7) . C45' H45' 0.9500 . C46' C47' 1.381(7) . C46' H46' 0.9500 . C47' C48' 1.372(7) . C47' H47' 0.9500 . C48' C49' 1.409(6) . C48' H48' 0.9500 . C49' H49' 0.9500 . C50 C55 1.384(2) . C50 C51 1.398(2) . C51 C52 1.388(2) . C51 H51 0.9500 . C52 C53 1.378(3) . C52 H52 0.9500 . C53 C54 1.372(3) . C53 H53 0.9500 . C54 C55 1.390(3) . C54 H54 0.9500 . C55 H55 0.9500 . C56 C57' 1.466(10) . C56 C59 1.495(3) . C56 C57 1.532(3) . C56 C58 1.560(3) . C56 C58' 1.564(10) . C56 C59' 1.575(10) . C57 H57A 0.9800 . C57 H57B 0.9800 . C57 H57C 0.9800 . C58 H58A 0.9800 . C58 H58B 0.9800 . C58 H58C 0.9800 . C59 H59A 0.9800 . C59 H59B 0.9800 . C59 H59C 0.9800 . C59' H59D 0.9800 . C59' H59E 0.9800 . C59' H59F 0.9800 . C57' H57D 0.9800 . C57' H57E 0.9800 . C57' H57F 0.9800 . C58' H58D 0.9800 . C58' H58E 0.9800 . C58' H58F 0.9800 . C60 C61 1.5189(19) . C60 C67 1.526(2) . C60 H60 1.0000 . C61 C62 1.390(2) . C61 C66 1.395(2) . C62 C63 1.390(2) . C62 H62 0.9500 . C63 C64 1.385(3) . C63 H63 0.9500 . C64 C65 1.380(3) . C64 H64 0.9500 . C65 C66 1.392(2) . C65 H65 0.9500 . C66 H66 0.9500 . C67 C68 1.389(2) . C67 C72 1.394(2) . C68 C69 1.401(2) . C68 H68 0.9500 . C69 C70 1.389(3) . C69 H69 0.9500 . C70 C71 1.381(3) . C70 H70 0.9500 . C71 C72 1.383(2) . C71 H71 0.9500 . C72 H72 0.9500 . C73 O21 1.252(2) . C73 N1 1.310(2) . C73 H73 0.9500 . C74 N1 1.456(2) . C74 H74A 0.9800 . C74 H74B 0.9800 . C74 H74C 0.9800 . C75 N1 1.449(3) . C75 H75A 0.9800 . C75 H75B 0.9800 . C75 H75C 0.9800 . C76 O22 1.250(2) . C76 N2 1.313(2) . C76 H76 0.9500 . C77 N2 1.457(3) . C77 H77A 0.9800 . C77 H77B 0.9800 . C77 H77C 0.9800 . C78 N2 1.449(3) . C78 H78A 0.9800 . C78 H78B 0.9800 . C78 H78C 0.9800 . O17 H17O 0.98(3) . O17 H17P 0.92(3) . O18 H18O 0.84(3) . O18 H18P 0.89(3) . O19 H19O 0.92(3) . O19 H19P 0.94(2) . O20 H20O 0.84(3) . O20 H20P 0.87(3) . C79 Cl2 1.739(7) . C79 Cl1 1.745(8) . C79 Cl3 1.753(7) . C79 H79 1.0000 . C79' Cl2' 1.739(13) . C79' Cl1' 1.740(13) . C79' Cl3' 1.746(14) . C79' H79' 1.0000 . loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag C75 H75C O6 0.98 2.63 3.471(3) 144.6 1_455 yes O9 H9P O22 0.86(2) 2.21(2) 3.0664(17) 175(2) . yes O9 H9Q O8 0.85(3) 1.85(3) 2.6755(15) 165(3) . yes O10 H10P O21 0.87(4) 2.05(4) 2.849(2) 154(3) 1_655 yes O11 H11O O21 0.87(3) 2.02(3) 2.8670(17) 164(3) 1_655 yes O11 H11P O2 0.85(2) 1.91(2) 2.7124(15) 157(2) . yes O12 H12O O15 0.78(3) 2.23(3) 3.0100(16) 177(2) . yes O12 H12P O20 0.88(2) 1.84(2) 2.7037(16) 165(2) . yes O13 H13O O4 0.97(3) 1.68(3) 2.5911(16) 155(2) 2_766 yes O14 H14O O12 0.84(3) 2.14(3) 2.9645(17) 168(2) 2_766 yes O14 H14P O6 0.81(3) 2.00(3) 2.7232(16) 148(2) . yes O14 H14P O11 0.81(3) 2.51(2) 3.1227(15) 133(2) . yes O15 H15O O19 0.90(2) 1.88(2) 2.7780(17) 172.3(19) 2_666 yes O15 H15P O18 0.88(3) 1.83(3) 2.6895(17) 168(3) . yes O16 H16O O17 0.98(3) 1.71(3) 2.6844(18) 176(3) . yes O17 H17O O18 0.98(3) 1.81(3) 2.7777(19) 167(3) . yes O17 H17P O20 0.92(3) 1.85(3) 2.7556(18) 173(3) 2_666 yes O18 H18O O8 0.84(3) 1.84(3) 2.6646(16) 171(2) . yes O18 H18P O19 0.89(3) 1.89(3) 2.7668(18) 168(2) . yes O19 H19O O21 0.92(3) 1.93(3) 2.7788(18) 153(2) . yes O19 H19P O22 0.94(2) 1.74(2) 2.6797(18) 179(2) . yes O20 H20O O22 0.84(3) 2.01(3) 2.8435(19) 172(2) . yes O20 H20P O4 0.87(3) 1.75(3) 2.6141(16) 174(2) . yes