#------------------------------------------------------------------------------ #$Date: 2019-05-17 04:32:53 +0300 (Fri, 17 May 2019) $ #$Revision: 215227 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/00/7700006.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_7700006 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_sum 'C288 H354 Cl2 Mg9 O77 P8' _chemical_formula_weight 5585.14 _space_group_crystal_system tetragonal _space_group_IT_number 85 _space_group_name_Hall '-P 4a' _space_group_name_H-M_alt 'P 4/n' _symmetry_space_group_name_Hall '-P 4a' _symmetry_space_group_name_H-M 'P 4/n :2' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2016/6 _audit_update_record ; 2019-04-29 deposited with the CCDC. 2019-05-16 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 29.2437(5) _cell_length_b 29.2437(5) _cell_length_c 22.0280(5) _cell_measurement_reflns_used 20346 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 27.0670 _cell_measurement_theta_min 2.6690 _cell_volume 18838.2(6) _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 120(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _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 0.0945 _diffrn_reflns_av_unetI/netI 0.0775 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 139116 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.500 _diffrn_reflns_theta_min 2.676 _diffrn_source 'fine-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 0.129 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.00907 _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 0.985 _exptl_crystal_description cube _exptl_crystal_F_000 5920 _exptl_crystal_size_max 0.227 _exptl_crystal_size_mid 0.196 _exptl_crystal_size_min 0.168 _refine_diff_density_max 0.614 _refine_diff_density_min -0.415 _refine_diff_density_rms 0.075 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 976 _refine_ls_number_reflns 19503 _refine_ls_number_restraints 159 _refine_ls_restrained_S_all 1.029 _refine_ls_R_factor_all 0.1184 _refine_ls_R_factor_gt 0.0829 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1034P)^2^+33.9425P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2124 _refine_ls_wR_factor_ref 0.2286 _reflns_Friedel_coverage 0.000 _reflns_number_gt 13372 _reflns_number_total 19503 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9dt00687g2.cif _cod_data_source_block aj0270 _cod_original_cell_volume 18838.2(8) _cod_database_code 7700006 _shelx_shelxl_version_number 2016/6 _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 0.971 _shelx_estimated_absorpt_t_max 0.979 _shelx_res_file ; TITL aj0270_a.res in P4/n shelx.res created by SHELXL-2016/6 at 13:10:13 on 26-Jun-2018 CELL 0.71073 29.2437 29.2437 22.0280 90.000 90.000 90.000 ZERR 2.00 0.0005 0.0005 0.0005 0.000 0.000 0.000 LATT 1 SYMM 1/2 - X, 1/2 - Y, Z SYMM 1/2 - Y, X, Z SYMM Y, 1/2 - X, Z SFAC C H CL MG O P UNIT 576 708 4 18 154 16 MERG 2 OMIT -3.00 53.00 OMIT 5 8 2 OMIT 1 3 2 OMIT 1 2 5 OMIT 3 13 3 OMIT -1 2 3 OMIT 2 11 2 OMIT -2 3 1 OMIT 3 6 2 OMIT 7 9 3 OMIT 6 7 2 OMIT 2 6 4 OMIT -10 11 1 OMIT -8 16 0 OMIT -4 18 1 OMIT -4 15 2 OMIT 4 15 2 OMIT 4 6 2 OMIT 4 8 4 OMIT 6 7 4 OMIT 7 7 4 DFIX 0.955 0.02 O5 H5O O5 H5P O6 H6O O6 H6P O7 H7O O7 H7P O8 H8O O8 H8P DFIX 0.955 0.02 O9 H9O O9 H9P O14 H14O O14 H14P O15 H15O O15 H15P DFIX 0.955 0.02 O16 H16O O16 H16P O17 H17O O17 H17P O18 H18O DFIX 0.955 0.02 O19 H19O O19 H19P O20 H20O O20 H20P DFIX 1.515 0.02 H5O H5P H6O H6P H7O H7P H8O H8P H9O H9P H14O H14P H15O H15P DFIX 1.515 0.02 H16O H16P H17O H17P H19O H19P SADI 0.02 C56 C57 C56' C57' C56 C58 C56' C58' C56 C59 C56' C59' SADI 0.02 C57 C58 C57 C59 C58 C59 C57' C58' C57' C59' C58' C59' DELU 0.010 0.010 C56 C57 C58 C59 C56' C57' C58' C59' SIMU 0.005 0.010 1.700 C56 C57 C58 C59 C56' C57' C58' C59' EQIV $1 1.5-Y,+X,+Z EQIV $2 y, -x+3/2, z HTAB O5 O1 HTAB O6 O4 HTAB O6 O11 HTAB O7 Cl1 HTAB O7 O4_$1 HTAB O8 O3_$1 HTAB O8 O4_$1 HTAB O9 O12 HTAB O9 O20_$1 HTAB O14 O11_$2 HTAB O14 O14_$2 HTAB O14 O7_$2 HTAB O15 O12_$2 HTAB O15 O20 HTAB O16 O10 HTAB O17 O17_$2 HTAB O17 Cl2 HTAB O17 O13 HTAB O17 O17_$1 HTAB O19 O2 HTAB O19 O3_$1 HTAB O20 O4 FMAP 2 PLAN -5 SIZE 0.227 0.196 0.168 ACTA BOND $H L.S. 24 TEMP -153 WGHT 0.103400 33.942501 FVAR 1.43638 0.74820 MOLE 1 MG1 4 0.891256 0.666501 0.585421 11.00000 0.02562 0.02386 = 0.01335 -0.00219 0.00045 0.00045 P1 6 0.812944 0.609106 0.516583 11.00000 0.02217 0.02045 = 0.01350 -0.00290 0.00123 0.00143 O1 5 0.850334 0.576796 0.481909 11.00000 0.02677 0.02618 = 0.01544 -0.00555 -0.00032 -0.00067 O2 5 0.839284 0.653092 0.527367 11.00000 0.02238 0.02300 = 0.01499 -0.00208 -0.00117 0.00236 O3 5 0.772701 0.613716 0.474454 11.00000 0.02502 0.02747 = 0.01456 -0.00360 -0.00001 0.00106 O4 5 0.800664 0.586562 0.576946 11.00000 0.02477 0.02268 = 0.01782 -0.00307 0.00183 0.00058 O5 5 0.925696 0.606564 0.553548 11.00000 0.03269 0.02649 = 0.02623 -0.00348 -0.00094 0.00515 H5O 2 0.937408 0.583529 0.579521 11.00000 -1.50000 H5P 2 0.906053 0.591637 0.525912 11.00000 -1.50000 O6 5 0.860866 0.628300 0.653108 11.00000 0.03216 0.02982 = 0.01438 -0.00283 -0.00116 -0.00871 H6O 2 0.834742 0.611803 0.638181 11.00000 -1.50000 H6P 2 0.851871 0.637119 0.692638 11.00000 -1.50000 O7 5 0.858113 0.728760 0.612435 11.00000 0.02401 0.02160 = 0.01925 -0.00028 0.00049 -0.00158 H7O 2 0.827374 0.731082 0.601149 11.00000 -1.50000 H7P 2 0.873871 0.754826 0.598855 11.00000 -1.50000 O8 5 0.928235 0.700078 0.519158 11.00000 0.02756 0.02656 = 0.01998 0.00005 0.00389 0.00291 H8O 2 0.919084 0.728752 0.504543 11.00000 -1.50000 H8P 2 0.941172 0.683007 0.488061 11.00000 -1.50000 O9 5 0.943957 0.677943 0.643368 11.00000 0.02544 0.03060 = 0.01624 -0.00107 -0.00006 -0.00535 H9O 2 0.938522 0.678402 0.686466 11.00000 -1.50000 H9P 2 0.963059 0.703993 0.637458 11.00000 -1.50000 C1 1 0.839235 0.549232 0.431858 11.00000 0.02372 0.02682 = 0.01796 -0.00767 -0.00010 0.00275 C2 1 0.842062 0.566862 0.374017 11.00000 0.02245 0.03554 = 0.02405 -0.01140 0.00261 0.00887 C3 1 0.832845 0.537432 0.325813 11.00000 0.02686 0.05022 = 0.01842 -0.01180 -0.00181 0.00882 AFIX 43 H3 2 0.834620 0.548823 0.285493 11.00000 -1.20000 AFIX 0 C4 1 0.821064 0.491651 0.335038 11.00000 0.02754 0.03963 = 0.02484 -0.01912 -0.00575 0.00981 C5 1 0.817279 0.475765 0.393866 11.00000 0.02727 0.03256 = 0.03432 -0.01324 0.00180 -0.00047 AFIX 43 H5 2 0.807938 0.445085 0.400741 11.00000 -1.20000 AFIX 0 C6 1 0.826840 0.503704 0.443047 11.00000 0.01842 0.03083 = 0.02092 -0.00807 0.00251 0.00122 C7 1 0.850104 0.617817 0.363480 11.00000 0.02846 0.03064 = 0.01588 0.00087 0.00341 0.00544 AFIX 13 H7 2 0.831206 0.633837 0.394772 11.00000 -1.20000 AFIX 0 C8 1 0.899212 0.635808 0.372363 11.00000 0.03304 0.03545 = 0.01120 -0.00423 0.00304 0.00693 C9 1 0.935708 0.608905 0.389844 11.00000 0.03459 0.03285 = 0.02858 -0.00129 -0.00089 0.00594 AFIX 43 H9 2 0.931494 0.577112 0.396714 11.00000 -1.20000 AFIX 0 C10 1 0.979024 0.628685 0.397422 11.00000 0.03159 0.04000 = 0.04469 -0.00215 -0.00260 0.00313 AFIX 43 H10 2 1.004313 0.610019 0.408317 11.00000 -1.20000 AFIX 0 C11 1 0.985152 0.674780 0.389223 11.00000 0.04131 0.04325 = 0.02966 -0.00365 0.00886 -0.00585 AFIX 43 H11 2 1.014456 0.687999 0.395424 11.00000 -1.20000 AFIX 0 C12 1 0.948814 0.702024 0.371970 11.00000 0.04749 0.02957 = 0.02947 -0.00205 0.00997 -0.00401 AFIX 43 H12 2 0.952895 0.733890 0.365574 11.00000 -1.20000 AFIX 0 C13 1 0.906694 0.682137 0.364254 11.00000 0.03964 0.03457 = 0.02534 0.00393 0.00207 0.00616 AFIX 43 H13 2 0.881641 0.700956 0.352874 11.00000 -1.20000 AFIX 0 C14 1 0.830930 0.633101 0.302449 11.00000 0.03105 0.03398 = 0.02318 -0.00013 0.00145 -0.00351 C15 1 0.856644 0.631335 0.248828 11.00000 0.03844 0.05989 = 0.02067 -0.00086 0.00398 0.00707 AFIX 43 H15 2 0.888077 0.623183 0.250037 11.00000 -1.20000 AFIX 0 C16 1 0.835492 0.641737 0.193274 11.00000 0.04988 0.06273 = 0.01905 0.00012 0.00703 0.00121 AFIX 43 H16 2 0.852552 0.639816 0.156662 11.00000 -1.20000 AFIX 0 C17 1 0.790909 0.654506 0.191438 11.00000 0.06427 0.05680 = 0.02527 -0.00070 -0.01633 0.00091 AFIX 43 H17 2 0.777062 0.661611 0.153582 11.00000 -1.20000 AFIX 0 C18 1 0.765304 0.657278 0.244550 11.00000 0.03708 0.04700 = 0.04151 0.00411 -0.00768 0.00568 AFIX 43 H18 2 0.734076 0.666165 0.243107 11.00000 -1.20000 AFIX 0 C19 1 0.785738 0.646983 0.299354 11.00000 0.03258 0.03936 = 0.02820 0.00075 -0.00071 -0.00117 AFIX 43 H19 2 0.768430 0.649476 0.335700 11.00000 -1.20000 AFIX 0 C20 1 0.809539 0.460514 0.280899 11.00000 0.04742 0.05530 = 0.03918 -0.03092 -0.01215 0.01047 C21 1 0.832618 0.478469 0.222132 11.00000 0.12956 0.11018 = 0.04303 -0.05577 0.00470 -0.01935 AFIX 33 H21A 2 0.822306 0.509772 0.214077 11.00000 -1.50000 H21B 2 0.865905 0.478226 0.227268 11.00000 -1.50000 H21C 2 0.824223 0.458751 0.187930 11.00000 -1.50000 AFIX 0 C22 1 0.758556 0.463352 0.268467 11.00000 0.05412 0.14524 = 0.07760 -0.07968 -0.01023 -0.00131 AFIX 33 H22A 2 0.749747 0.495404 0.262821 11.00000 -1.50000 H22B 2 0.751311 0.446001 0.231641 11.00000 -1.50000 H22C 2 0.741700 0.450483 0.302914 11.00000 -1.50000 AFIX 0 C23 1 0.826920 0.412476 0.290355 11.00000 0.19096 0.06314 = 0.05350 -0.03958 -0.03721 0.03397 AFIX 33 H23A 2 0.859909 0.413284 0.298106 11.00000 -1.50000 H23B 2 0.811266 0.398708 0.325187 11.00000 -1.50000 H23C 2 0.820878 0.394226 0.253915 11.00000 -1.50000 AFIX 0 C24 1 0.826837 0.485921 0.508368 11.00000 0.03733 0.02084 = 0.02460 -0.00807 0.00544 0.00069 AFIX 13 H24 2 0.814144 0.511303 0.533695 11.00000 -1.20000 AFIX 0 C25 1 0.794752 0.445682 0.517446 11.00000 0.04835 0.02849 = 0.03660 -0.01097 0.01425 -0.00478 C26 1 0.746840 0.454238 0.516258 11.00000 0.04477 0.04111 = 0.04217 -0.00617 -0.00009 -0.00373 AFIX 43 H26 2 0.735829 0.484406 0.509760 11.00000 -1.20000 AFIX 0 C27 1 0.716666 0.419081 0.524460 11.00000 0.05138 0.05320 = 0.06425 -0.00347 0.01166 -0.01580 AFIX 43 H27 2 0.684784 0.425307 0.524809 11.00000 -1.20000 AFIX 0 C28 1 0.731555 0.374949 0.532201 11.00000 0.07198 0.05281 = 0.13892 -0.00607 0.02592 -0.03060 AFIX 43 H28 2 0.710335 0.350470 0.535397 11.00000 -1.20000 AFIX 0 C29 1 0.778225 0.366848 0.535259 11.00000 0.07286 0.03462 = 0.21975 0.01274 0.02797 -0.00877 AFIX 43 H29 2 0.788936 0.336867 0.543837 11.00000 -1.20000 AFIX 0 C30 1 0.809246 0.401496 0.526079 11.00000 0.04984 0.03485 = 0.14520 0.00808 0.02399 -0.00647 AFIX 43 H30 2 0.841033 0.394798 0.525705 11.00000 -1.20000 AFIX 0 C31 1 0.875039 0.479086 0.529772 11.00000 0.03908 0.02156 = 0.02541 0.00095 0.00092 -0.00171 C32 1 0.889646 0.497155 0.585103 11.00000 0.05822 0.03488 = 0.02852 -0.00916 -0.00263 0.00752 AFIX 43 H32 2 0.867998 0.511655 0.610860 11.00000 -1.20000 AFIX 0 C33 1 0.934527 0.494530 0.603330 11.00000 0.07207 0.03216 = 0.03793 -0.00525 -0.02479 0.00450 AFIX 43 H33 2 0.943609 0.507104 0.641223 11.00000 -1.20000 AFIX 0 C34 1 0.966599 0.473385 0.566062 11.00000 0.05094 0.03783 = 0.05029 0.00014 -0.01539 -0.00073 AFIX 43 H34 2 0.997784 0.472133 0.578025 11.00000 -1.20000 AFIX 0 C35 1 0.952977 0.454124 0.511384 11.00000 0.04675 0.05630 = 0.03443 0.00180 -0.00364 0.01276 AFIX 43 H35 2 0.974454 0.438855 0.486163 11.00000 -1.20000 AFIX 0 C36 1 0.907760 0.457526 0.494301 11.00000 0.04544 0.04393 = 0.02523 -0.00330 0.00100 0.00638 AFIX 43 H36 2 0.898628 0.444563 0.456661 11.00000 -1.20000 AFIX 0 MOLE 2 MG2 4 0.780568 0.634246 0.806221 11.00000 0.02210 0.02599 = 0.01430 -0.00126 0.00085 -0.00122 P2 6 0.885733 0.671800 0.801482 11.00000 0.01949 0.02296 = 0.01229 -0.00097 -0.00132 0.00200 O10 5 0.900740 0.634121 0.851655 11.00000 0.02545 0.02070 = 0.01599 0.00046 -0.00244 0.00493 O11 5 0.844251 0.649171 0.772371 11.00000 0.01946 0.02892 = 0.01437 -0.00103 -0.00068 -0.00251 O12 5 0.925337 0.679244 0.759049 11.00000 0.02217 0.02755 = 0.01709 0.00098 0.00232 -0.00226 O13 5 0.872859 0.715069 0.836330 11.00000 0.02212 0.02290 = 0.01183 -0.00042 0.00001 0.00243 O14 5 0.754224 0.679126 0.734776 11.00000 0.02161 0.02792 = 0.01481 -0.00089 0.00221 0.00240 H14O 2 0.725237 0.691210 0.744399 11.00000 -1.50000 H14P 2 0.749932 0.663995 0.697547 11.00000 -1.50000 O15 5 0.770734 0.581195 0.746964 11.00000 0.03219 0.03608 = 0.02698 -0.01279 -0.00075 0.00545 H15O 2 0.740310 0.569076 0.751443 11.00000 -1.50000 H15P 2 0.788514 0.555199 0.737642 11.00000 -1.50000 O16 5 0.810144 0.589459 0.871205 11.00000 0.03330 0.04592 = 0.02546 0.01103 -0.00164 -0.00041 H16O 2 0.841149 0.582141 0.869842 11.00000 -1.50000 H16P 2 0.802546 0.592481 0.912862 11.00000 -1.50000 O17 5 0.789217 0.686609 0.865328 11.00000 0.02199 0.05309 = 0.03428 -0.02384 0.00999 -0.01204 H17O 2 0.771827 0.699666 0.894841 11.00000 -1.50000 H17P 2 0.817142 0.701499 0.861073 11.00000 -1.50000 C37 1 0.945668 0.625481 0.870237 11.00000 0.02247 0.02581 = 0.02339 0.00163 -0.00509 0.00312 C38 1 0.961779 0.646402 0.922217 11.00000 0.03144 0.03416 = 0.02038 -0.00561 -0.00398 0.00971 C39 1 1.004998 0.634394 0.942636 11.00000 0.04031 0.05900 = 0.02227 -0.02136 -0.01222 0.01704 AFIX 43 H39 2 1.016321 0.648465 0.978484 11.00000 -1.20000 AFIX 0 C40 1 1.032237 0.602990 0.913279 11.00000 0.03883 0.07065 = 0.03195 -0.01679 -0.01632 0.02733 C41 1 1.014776 0.583222 0.860344 11.00000 0.04002 0.05375 = 0.02748 -0.01690 -0.01220 0.02709 AFIX 43 H41 2 1.033160 0.562036 0.838590 11.00000 -1.20000 AFIX 0 C42 1 0.971340 0.593569 0.838477 11.00000 0.04078 0.03107 = 0.02028 -0.00425 -0.00468 0.01453 C43 1 0.930458 0.678851 0.957287 11.00000 0.03004 0.03130 = 0.02325 -0.00909 -0.00820 0.01164 AFIX 13 H43 2 0.915819 0.699140 0.926341 11.00000 -1.20000 AFIX 0 C44 1 0.891763 0.652729 0.987771 11.00000 0.03433 0.03102 = 0.01595 -0.00736 -0.00689 0.00290 C45 1 0.850615 0.675446 0.997956 11.00000 0.03479 0.03744 = 0.02235 0.00146 -0.00261 0.00201 AFIX 43 H45 2 0.847771 0.706746 0.987046 11.00000 -1.20000 AFIX 0 C46 1 0.813157 0.652518 1.024260 11.00000 0.03166 0.05175 = 0.02858 -0.00379 -0.00230 0.00534 AFIX 43 H46 2 0.785192 0.668298 1.030797 11.00000 -1.20000 AFIX 0 C47 1 0.817163 0.606694 1.040673 11.00000 0.04671 0.05280 = 0.02588 -0.00055 0.00059 -0.01296 AFIX 43 H47 2 0.792217 0.590845 1.058573 11.00000 -1.20000 AFIX 0 C48 1 0.858859 0.584583 1.030135 11.00000 0.05012 0.03676 = 0.03768 -0.00200 0.00090 -0.00058 AFIX 43 H48 2 0.862076 0.553180 1.040316 11.00000 -1.20000 AFIX 0 C49 1 0.894997 0.607598 1.005385 11.00000 0.04400 0.04310 = 0.03074 -0.00773 -0.00461 0.00535 AFIX 43 H49 2 0.923230 0.592021 1.000151 11.00000 -1.20000 AFIX 0 C50 1 0.957276 0.710283 0.999785 11.00000 0.03327 0.03207 = 0.02501 -0.00738 -0.00909 0.00851 C51 1 0.956642 0.705875 1.062295 11.00000 0.06593 0.04052 = 0.02690 -0.00526 -0.01952 0.00790 AFIX 43 H51 2 0.938027 0.683057 1.080505 11.00000 -1.20000 AFIX 0 C52 1 0.982558 0.734038 1.098359 11.00000 0.09508 0.05525 = 0.04084 -0.01849 -0.03648 0.00532 AFIX 43 H52 2 0.982330 0.730087 1.141165 11.00000 -1.20000 AFIX 0 C53 1 1.008689 0.767734 1.072982 11.00000 0.07708 0.05035 = 0.06693 -0.02148 -0.03554 -0.00305 AFIX 43 H53 2 1.025732 0.787841 1.098190 11.00000 -1.20000 AFIX 0 C54 1 1.010297 0.772536 1.010472 11.00000 0.04619 0.04456 = 0.07101 -0.01358 -0.01155 -0.00594 AFIX 43 H54 2 1.029125 0.795383 0.992719 11.00000 -1.20000 AFIX 0 C55 1 0.984716 0.744317 0.974249 11.00000 0.03319 0.04419 = 0.04241 -0.00987 -0.00637 -0.00080 AFIX 43 H55 2 0.985652 0.747929 0.931407 11.00000 -1.20000 AFIX 0 PART 1 C56 1 1.082385 0.593784 0.931685 21.00000 0.03740 0.09491 = 0.04393 -0.02298 -0.01854 0.03356 C57 1 1.095099 0.616658 0.992202 21.00000 0.04190 0.11195 = 0.05299 -0.02104 -0.02547 0.02522 AFIX 137 H57A 2 1.074223 0.606106 1.024061 21.00000 -1.50000 H57B 2 1.092619 0.649932 0.988054 21.00000 -1.50000 H57C 2 1.126559 0.608521 1.003074 21.00000 -1.50000 AFIX 0 C58 1 1.116213 0.609339 0.883501 21.00000 0.03761 0.11707 = 0.05247 -0.01311 -0.01459 0.01969 AFIX 137 H58A 2 1.147135 0.599831 0.895108 21.00000 -1.50000 H58B 2 1.115135 0.642724 0.879917 21.00000 -1.50000 H58C 2 1.108170 0.595486 0.844424 21.00000 -1.50000 AFIX 0 C59 1 1.087133 0.541689 0.940043 21.00000 0.05326 0.09649 = 0.06245 -0.00717 -0.02411 0.03298 AFIX 137 H59A 2 1.118228 0.534456 0.953567 21.00000 -1.50000 H59B 2 1.081069 0.526316 0.901340 21.00000 -1.50000 H59C 2 1.065120 0.531161 0.970537 21.00000 -1.50000 AFIX 0 PART 2 C56' 1 1.069153 0.572513 0.948880 -21.00000 0.04006 0.09498 = 0.04443 -0.01942 -0.01871 0.03451 C57' 1 1.093935 0.606237 0.991017 -21.00000 0.04198 0.10017 = 0.04928 -0.01905 -0.02188 0.02994 AFIX 33 H57D 2 1.103063 0.633351 0.967850 -21.00000 -1.50000 H57E 2 1.073385 0.615345 1.024013 -21.00000 -1.50000 H57F 2 1.121170 0.591531 1.008072 -21.00000 -1.50000 AFIX 0 C58' 1 1.103965 0.556300 0.901199 -21.00000 0.03880 0.10525 = 0.04782 -0.01549 -0.01999 0.03877 AFIX 33 H58D 2 1.113378 0.582281 0.876030 -21.00000 -1.50000 H58E 2 1.130784 0.543445 0.921702 -21.00000 -1.50000 H58F 2 1.089921 0.532840 0.875476 -21.00000 -1.50000 AFIX 0 C59' 1 1.055527 0.530686 0.987020 -21.00000 0.05525 0.09144 = 0.05315 -0.00923 -0.02449 0.03358 AFIX 33 H59D 2 1.039594 0.508506 0.961238 -21.00000 -1.50000 H59E 2 1.083042 0.516530 1.004104 -21.00000 -1.50000 H59F 2 1.035257 0.540344 1.020045 -21.00000 -1.50000 AFIX 0 PART 0 C60 1 0.950515 0.570273 0.783485 11.00000 0.03680 0.02850 = 0.02119 -0.00444 -0.00231 0.01573 AFIX 13 H60 2 0.934353 0.594790 0.760223 11.00000 -1.20000 AFIX 0 C61 1 0.986551 0.551221 0.741108 11.00000 0.03908 0.03499 = 0.01891 -0.00749 -0.00702 0.01156 C62 1 1.005250 0.579294 0.696677 11.00000 0.04401 0.02543 = 0.02706 -0.00863 -0.00209 0.00693 AFIX 43 H62 2 0.994050 0.609573 0.691879 11.00000 -1.20000 AFIX 0 C63 1 1.040208 0.563623 0.659068 11.00000 0.04394 0.04190 = 0.03259 -0.00072 0.00174 0.00531 AFIX 43 H63 2 1.053018 0.583366 0.629340 11.00000 -1.20000 AFIX 0 C64 1 1.056378 0.519110 0.664990 11.00000 0.04514 0.03729 = 0.03640 -0.01060 -0.00066 0.01111 AFIX 43 H64 2 1.079679 0.508057 0.638765 11.00000 -1.20000 AFIX 0 C65 1 1.038293 0.491284 0.709179 11.00000 0.05615 0.03262 = 0.03821 -0.00210 -0.00018 0.02320 AFIX 43 H65 2 1.049506 0.460972 0.713533 11.00000 -1.20000 AFIX 0 C66 1 1.003728 0.506779 0.747793 11.00000 0.05955 0.03578 = 0.02531 -0.00391 -0.00050 0.02266 AFIX 43 H66 2 0.991904 0.487255 0.778481 11.00000 -1.20000 AFIX 0 C67 1 0.914340 0.535351 0.800079 11.00000 0.05204 0.03077 = 0.02931 -0.00825 -0.00071 0.00797 C68 1 0.913038 0.514287 0.856181 11.00000 0.10187 0.04911 = 0.04257 0.01258 -0.00112 -0.00944 AFIX 43 H68 2 0.934765 0.522526 0.886319 11.00000 -1.20000 AFIX 0 C69 1 0.880190 0.481037 0.869154 11.00000 0.14115 0.06215 = 0.07178 0.01576 0.01526 -0.02479 AFIX 43 H69 2 0.880480 0.465725 0.907188 11.00000 -1.20000 AFIX 0 C70 1 0.846328 0.470221 0.825173 11.00000 0.09385 0.05684 = 0.09522 0.00483 0.00885 -0.01817 AFIX 43 H70 2 0.823161 0.448383 0.833748 11.00000 -1.20000 AFIX 0 C71 1 0.847841 0.492170 0.769658 11.00000 0.07199 0.05159 = 0.07211 -0.01717 -0.00509 0.00405 AFIX 43 H71 2 0.825789 0.484835 0.739524 11.00000 -1.20000 AFIX 0 C72 1 0.880439 0.524161 0.757419 11.00000 0.04766 0.03919 = 0.03741 -0.00991 0.00261 0.00298 AFIX 43 H72 2 0.880233 0.539222 0.719208 11.00000 -1.20000 AFIX 0 MOLE 3 CL1 3 0.750000 0.750000 0.575185 10.25000 0.02467 0.02467 = 0.01790 0.00000 0.00000 0.00000 MG3 4 0.750000 0.750000 0.453846 10.25000 0.02540 0.02540 = 0.01232 0.00000 0.00000 0.00000 O18 5 0.750000 0.750000 0.357112 10.25000 0.03895 0.03895 = 0.01637 0.00000 0.00000 0.00000 H18O 2 0.772787 0.766012 10.333000 10.50000 -1.50000 O19 5 0.813463 0.722254 0.452029 11.00000 0.02422 0.02325 = 0.02160 0.00057 -0.00268 -0.00043 H19P 2 0.819793 0.694443 0.472748 11.00000 -1.50000 H19O 2 0.839375 0.740936 0.460810 11.00000 -1.50000 MOLE 4 CL2 3 0.750000 0.750000 0.966923 10.25000 0.02787 0.02787 = 0.01343 0.00000 0.00000 0.00000 MOLE 5 O20 5 0.765877 0.516565 0.643412 11.00000 0.04243 0.04158 = 0.03557 0.00639 0.00695 0.00694 H20O 2 0.797770 0.516481 0.653010 11.00000 -1.50000 H20P 2 0.772438 0.538283 0.611949 11.00000 -1.50000 HKLF 4 REM aj0270_a.res in P4/n REM R1 = 0.0829 for 13372 Fo > 4sig(Fo) and 0.1184 for all 19503 data REM 976 parameters refined using 159 restraints END WGHT 0.0741 42.8967 REM Highest difference peak 0.614, deepest hole -0.415, 1-sigma level 0.075 Q1 1 0.7589 0.4352 0.3025 11.00000 0.05 0.61 Q2 1 0.7972 0.4067 0.3093 11.00000 0.05 0.46 Q3 1 0.7799 0.6133 0.5140 11.00000 0.05 0.45 Q4 1 0.9212 0.6725 0.7919 11.00000 0.05 0.44 Q5 1 0.7835 0.7523 0.5786 11.00000 0.05 0.40 ; _shelx_res_checksum 9804 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z' 'y, -x+1/2, z' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z' '-y, x-1/2, -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 0.89126(4) 0.66650(4) 0.58542(5) 0.0209(3) Uani 1 1 d . . . . . P1 P 0.81294(3) 0.60911(3) 0.51658(4) 0.0187(2) Uani 1 1 d . . . . . O1 O 0.85033(8) 0.57680(8) 0.48191(10) 0.0228(5) Uani 1 1 d . . . . . O2 O 0.83928(8) 0.65309(8) 0.52737(10) 0.0201(5) Uani 1 1 d . . . . . O3 O 0.77270(8) 0.61372(8) 0.47445(10) 0.0223(5) Uani 1 1 d . . . . . O4 O 0.80066(8) 0.58656(8) 0.57695(10) 0.0218(5) Uani 1 1 d . . . . . O5 O 0.92570(9) 0.60656(9) 0.55355(12) 0.0285(6) Uani 1 1 d D . . . . H5O H 0.9374(14) 0.5835(11) 0.5795(15) 0.043 Uiso 1 1 d D U . . . H5P H 0.9061(12) 0.5916(12) 0.5259(15) 0.043 Uiso 1 1 d D U . . . O6 O 0.86087(9) 0.62830(9) 0.65311(11) 0.0255(6) Uani 1 1 d D . . . . H6O H 0.8347(10) 0.6118(13) 0.6382(15) 0.038 Uiso 1 1 d D U . . . H6P H 0.8519(12) 0.6371(13) 0.6926(10) 0.038 Uiso 1 1 d D U . . . O7 O 0.85811(8) 0.72876(8) 0.61244(10) 0.0216(5) Uani 1 1 d D . . . . H7O H 0.8274(7) 0.7311(13) 0.6011(18) 0.032 Uiso 1 1 d D U . . . H7P H 0.8739(10) 0.7548(10) 0.5989(17) 0.032 Uiso 1 1 d D U . . . O8 O 0.92824(9) 0.70008(9) 0.51916(11) 0.0247(5) Uani 1 1 d D . . . . H8O H 0.9191(14) 0.7288(8) 0.5045(16) 0.037 Uiso 1 1 d D U . . . H8P H 0.9412(13) 0.6830(11) 0.4881(14) 0.037 Uiso 1 1 d D U . . . O9 O 0.94396(8) 0.67794(9) 0.64337(11) 0.0241(5) Uani 1 1 d D . . . . H9O H 0.9385(13) 0.6784(13) 0.6865(9) 0.036 Uiso 1 1 d D U . . . H9P H 0.9631(12) 0.7040(10) 0.6375(15) 0.036 Uiso 1 1 d D U . . . C1 C 0.83923(12) 0.54923(12) 0.43186(15) 0.0228(8) Uani 1 1 d . . . . . C2 C 0.84206(12) 0.56686(13) 0.37402(16) 0.0273(8) Uani 1 1 d . . . . . C3 C 0.83284(13) 0.53743(15) 0.32581(17) 0.0318(9) Uani 1 1 d . . . . . H3 H 0.834620 0.548823 0.285493 0.038 Uiso 1 1 calc R U . . . C4 C 0.82106(13) 0.49165(14) 0.33504(17) 0.0307(9) Uani 1 1 d . . . . . C5 C 0.81728(13) 0.47576(14) 0.39387(18) 0.0314(9) Uani 1 1 d . . . . . H5 H 0.807938 0.445085 0.400741 0.038 Uiso 1 1 calc R U . . . C6 C 0.82684(12) 0.50370(13) 0.44305(16) 0.0234(8) Uani 1 1 d . . . . . C7 C 0.85010(13) 0.61782(13) 0.36348(15) 0.0250(8) Uani 1 1 d . . . . . H7 H 0.831206 0.633837 0.394772 0.030 Uiso 1 1 calc R U . . . C8 C 0.89921(13) 0.63581(13) 0.37236(15) 0.0266(8) Uani 1 1 d . . . . . C9 C 0.93571(14) 0.60890(14) 0.38984(18) 0.0320(9) Uani 1 1 d . . . . . H9 H 0.931494 0.577112 0.396714 0.038 Uiso 1 1 calc R U . . . C10 C 0.97902(15) 0.62869(15) 0.3974(2) 0.0388(10) Uani 1 1 d . . . . . H10 H 1.004313 0.610019 0.408317 0.047 Uiso 1 1 calc R U . . . C11 C 0.98515(16) 0.67478(15) 0.38922(18) 0.0381(10) Uani 1 1 d . . . . . H11 H 1.014456 0.687999 0.395424 0.046 Uiso 1 1 calc R U . . . C12 C 0.94881(15) 0.70202(14) 0.37197(18) 0.0355(10) Uani 1 1 d . . . . . H12 H 0.952895 0.733890 0.365574 0.043 Uiso 1 1 calc R U . . . C13 C 0.90669(15) 0.68214(14) 0.36425(17) 0.0332(9) Uani 1 1 d . . . . . H13 H 0.881641 0.700956 0.352874 0.040 Uiso 1 1 calc R U . . . C14 C 0.83093(13) 0.63310(14) 0.30245(17) 0.0294(8) Uani 1 1 d . . . . . C15 C 0.85664(15) 0.63134(16) 0.24883(17) 0.0397(10) Uani 1 1 d . . . . . H15 H 0.888077 0.623183 0.250037 0.048 Uiso 1 1 calc R U . . . C16 C 0.83549(16) 0.64174(17) 0.19327(18) 0.0439(11) Uani 1 1 d . . . . . H16 H 0.852552 0.639816 0.156662 0.053 Uiso 1 1 calc R U . . . C17 C 0.79091(18) 0.65451(17) 0.1914(2) 0.0488(12) Uani 1 1 d . . . . . H17 H 0.777062 0.661611 0.153582 0.059 Uiso 1 1 calc R U . . . C18 C 0.76530(16) 0.65728(16) 0.2445(2) 0.0419(11) Uani 1 1 d . . . . . H18 H 0.734076 0.666165 0.243107 0.050 Uiso 1 1 calc R U . . . C19 C 0.78574(14) 0.64698(14) 0.29935(18) 0.0334(9) Uani 1 1 d . . . . . H19 H 0.768430 0.649476 0.335700 0.040 Uiso 1 1 calc R U . . . C20 C 0.80954(16) 0.46051(17) 0.2809(2) 0.0473(12) Uani 1 1 d . . . . . C21 C 0.8326(3) 0.4785(3) 0.2221(3) 0.094(2) Uani 1 1 d . . . . . H21A H 0.822306 0.509772 0.214077 0.141 Uiso 1 1 calc R U . . . H21B H 0.865905 0.478226 0.227268 0.141 Uiso 1 1 calc R U . . . H21C H 0.824223 0.458751 0.187930 0.141 Uiso 1 1 calc R U . . . C22 C 0.7586(2) 0.4634(3) 0.2685(3) 0.092(3) Uani 1 1 d . . . . . H22A H 0.749747 0.495404 0.262821 0.138 Uiso 1 1 calc R U . . . H22B H 0.751311 0.446001 0.231641 0.138 Uiso 1 1 calc R U . . . H22C H 0.741700 0.450483 0.302914 0.138 Uiso 1 1 calc R U . . . C23 C 0.8269(3) 0.4125(2) 0.2904(3) 0.103(3) Uani 1 1 d . . . . . H23A H 0.859909 0.413284 0.298106 0.154 Uiso 1 1 calc R U . . . H23B H 0.811266 0.398708 0.325187 0.154 Uiso 1 1 calc R U . . . H23C H 0.820878 0.394226 0.253915 0.154 Uiso 1 1 calc R U . . . C24 C 0.82684(13) 0.48592(12) 0.50837(17) 0.0276(8) Uani 1 1 d . . . . . H24 H 0.814144 0.511303 0.533695 0.033 Uiso 1 1 calc R U . . . C25 C 0.79475(16) 0.44568(14) 0.51745(19) 0.0378(10) Uani 1 1 d . . . . . C26 C 0.74684(16) 0.45424(16) 0.5163(2) 0.0427(11) Uani 1 1 d . . . . . H26 H 0.735829 0.484406 0.509760 0.051 Uiso 1 1 calc R U . . . C27 C 0.71667(19) 0.41908(18) 0.5245(2) 0.0563(13) Uani 1 1 d . . . . . H27 H 0.684784 0.425307 0.524809 0.068 Uiso 1 1 calc R U . . . C28 C 0.7316(2) 0.3749(2) 0.5322(4) 0.088(2) Uani 1 1 d . . . . . H28 H 0.710335 0.350470 0.535397 0.105 Uiso 1 1 calc R U . . . C29 C 0.7782(2) 0.3668(2) 0.5353(5) 0.109(3) Uani 1 1 d . . . . . H29 H 0.788936 0.336867 0.543837 0.131 Uiso 1 1 calc R U . . . C30 C 0.8092(2) 0.40150(18) 0.5261(3) 0.077(2) Uani 1 1 d . . . . . H30 H 0.841033 0.394798 0.525705 0.092 Uiso 1 1 calc R U . . . C31 C 0.87504(14) 0.47909(13) 0.52977(17) 0.0287(8) Uani 1 1 d . . . . . C32 C 0.88965(17) 0.49715(15) 0.58510(19) 0.0405(10) Uani 1 1 d . . . . . H32 H 0.867998 0.511655 0.610860 0.049 Uiso 1 1 calc R U . . . C33 C 0.93453(18) 0.49453(15) 0.6033(2) 0.0474(12) Uani 1 1 d . . . . . H33 H 0.943609 0.507104 0.641223 0.057 Uiso 1 1 calc R U . . . C34 C 0.96660(18) 0.47339(16) 0.5661(2) 0.0464(11) Uani 1 1 d . . . . . H34 H 0.997784 0.472133 0.578025 0.056 Uiso 1 1 calc R U . . . C35 C 0.95298(17) 0.45412(17) 0.5114(2) 0.0458(11) Uani 1 1 d . . . . . H35 H 0.974454 0.438855 0.486163 0.055 Uiso 1 1 calc R U . . . C36 C 0.90776(15) 0.45753(15) 0.49430(19) 0.0382(10) Uani 1 1 d . . . . . H36 H 0.898628 0.444563 0.456661 0.046 Uiso 1 1 calc R U . . . Mg2 Mg 0.78057(4) 0.63425(4) 0.80622(5) 0.0208(3) Uani 1 1 d . . . . . P2 P 0.88573(3) 0.67180(3) 0.80148(4) 0.0182(2) Uani 1 1 d . . . . . O10 O 0.90074(8) 0.63412(8) 0.85166(10) 0.0207(5) Uani 1 1 d . . . . . O11 O 0.84425(8) 0.64917(8) 0.77237(10) 0.0209(5) Uani 1 1 d . . . . . O12 O 0.92534(8) 0.67924(8) 0.75905(10) 0.0223(5) Uani 1 1 d . . . . . O13 O 0.87286(8) 0.71507(8) 0.83633(10) 0.0189(5) Uani 1 1 d . . . . . O14 O 0.75422(8) 0.67913(8) 0.73478(10) 0.0214(5) Uani 1 1 d D . . . . H14O H 0.7252(8) 0.6912(13) 0.7444(16) 0.032 Uiso 1 1 d D U . . . H14P H 0.7499(12) 0.6640(12) 0.6975(12) 0.032 Uiso 1 1 d D U . . . O15 O 0.77073(10) 0.58119(9) 0.74696(12) 0.0318(6) Uani 1 1 d D . . . . H15O H 0.7403(7) 0.5691(13) 0.751(2) 0.048 Uiso 1 1 d D U . . . H15P H 0.7885(11) 0.5552(10) 0.738(2) 0.048 Uiso 1 1 d D U . . . O16 O 0.81014(10) 0.58946(10) 0.87121(12) 0.0349(7) Uani 1 1 d D . . . . H16O H 0.8411(7) 0.5821(16) 0.8698(18) 0.052 Uiso 1 1 d D U . . . H16P H 0.8025(13) 0.5925(17) 0.9129(10) 0.052 Uiso 1 1 d D U . . . O17 O 0.78922(9) 0.68661(10) 0.86533(12) 0.0365(7) Uani 1 1 d D . . . . H17O H 0.7718(12) 0.6997(15) 0.8948(17) 0.055 Uiso 1 1 d D U . . . H17P H 0.8171(9) 0.7015(14) 0.861(2) 0.055 Uiso 1 1 d D U . . . C37 C 0.94567(12) 0.62548(12) 0.87024(16) 0.0239(8) Uani 1 1 d . . . . . C38 C 0.96178(13) 0.64640(13) 0.92222(16) 0.0287(8) Uani 1 1 d . . . . . C39 C 1.00500(15) 0.63439(16) 0.94264(18) 0.0405(11) Uani 1 1 d . . . . . H39 H 1.016321 0.648465 0.978484 0.049 Uiso 1 1 calc R U . . . C40 C 1.03224(16) 0.60299(18) 0.91328(19) 0.0471(12) Uani 1 1 d . . . . . C41 C 1.01478(15) 0.58322(16) 0.86034(18) 0.0404(11) Uani 1 1 d . . . . . H41 H 1.033160 0.562036 0.838590 0.048 Uiso 1 1 calc R U . . . C42 C 0.97134(14) 0.59357(13) 0.83848(16) 0.0307(9) Uani 1 1 d . . . . . C43 C 0.93046(13) 0.67885(13) 0.95729(17) 0.0282(8) Uani 1 1 d . . . . . H43 H 0.915819 0.699140 0.926341 0.034 Uiso 1 1 calc R U . . . C44 C 0.89176(13) 0.65273(13) 0.98777(16) 0.0271(8) Uani 1 1 d . . . . . C45 C 0.85061(14) 0.67545(15) 0.99796(17) 0.0315(9) Uani 1 1 d . . . . . H45 H 0.847771 0.706746 0.987046 0.038 Uiso 1 1 calc R U . . . C46 C 0.81316(15) 0.65252(16) 1.02426(18) 0.0373(10) Uani 1 1 d . . . . . H46 H 0.785192 0.668298 1.030797 0.045 Uiso 1 1 calc R U . . . C47 C 0.81716(16) 0.60669(17) 1.04067(19) 0.0418(11) Uani 1 1 d . . . . . H47 H 0.792217 0.590845 1.058573 0.050 Uiso 1 1 calc R U . . . C48 C 0.85886(16) 0.58458(16) 1.0301(2) 0.0415(10) Uani 1 1 d . . . . . H48 H 0.862076 0.553180 1.040316 0.050 Uiso 1 1 calc R U . . . C49 C 0.89500(16) 0.60760(15) 1.00539(19) 0.0393(10) Uani 1 1 d . . . . . H49 H 0.923230 0.592021 1.000151 0.047 Uiso 1 1 calc R U . . . C50 C 0.95728(14) 0.71028(14) 0.99979(17) 0.0301(9) Uani 1 1 d . . . . . C51 C 0.95664(18) 0.70587(16) 1.06229(19) 0.0445(12) Uani 1 1 d . . . . . H51 H 0.938027 0.683057 1.080505 0.053 Uiso 1 1 calc R U . . . C52 C 0.9826(2) 0.73404(19) 1.0984(2) 0.0637(16) Uani 1 1 d . . . . . H52 H 0.982330 0.730087 1.141165 0.076 Uiso 1 1 calc R U . . . C53 C 1.0087(2) 0.76773(19) 1.0730(3) 0.0648(16) Uani 1 1 d . . . . . H53 H 1.025732 0.787841 1.098190 0.078 Uiso 1 1 calc R U . . . C54 C 1.01030(17) 0.77254(17) 1.0105(3) 0.0539(13) Uani 1 1 d . . . . . H54 H 1.029125 0.795383 0.992719 0.065 Uiso 1 1 calc R U . . . C55 C 0.98472(14) 0.74432(15) 0.9742(2) 0.0399(10) Uani 1 1 d . . . . . H55 H 0.985652 0.747929 0.931407 0.048 Uiso 1 1 calc R U . . . C56 C 1.0824(2) 0.5938(3) 0.9317(3) 0.0587(17) Uani 0.748(7) 1 d D U P A 1 C57 C 1.0951(6) 0.6167(4) 0.9922(5) 0.069(2) Uani 0.748(7) 1 d D U P A 1 H57A H 1.074223 0.606106 1.024061 0.103 Uiso 0.748(7) 1 calc R U P A 1 H57B H 1.092619 0.649932 0.988054 0.103 Uiso 0.748(7) 1 calc R U P A 1 H57C H 1.126559 0.608521 1.003074 0.103 Uiso 0.748(7) 1 calc R U P A 1 C58 C 1.1162(2) 0.6093(3) 0.8835(3) 0.069(2) Uani 0.748(7) 1 d D U P A 1 H58A H 1.147135 0.599831 0.895108 0.104 Uiso 0.748(7) 1 calc R U P A 1 H58B H 1.115135 0.642724 0.879917 0.104 Uiso 0.748(7) 1 calc R U P A 1 H58C H 1.108170 0.595486 0.844424 0.104 Uiso 0.748(7) 1 calc R U P A 1 C59 C 1.0871(3) 0.5417(3) 0.9400(4) 0.071(2) Uani 0.748(7) 1 d D U P A 1 H59A H 1.118228 0.534456 0.953567 0.106 Uiso 0.748(7) 1 calc R U P A 1 H59B H 1.081069 0.526316 0.901340 0.106 Uiso 0.748(7) 1 calc R U P A 1 H59C H 1.065120 0.531161 0.970537 0.106 Uiso 0.748(7) 1 calc R U P A 1 C56' C 1.0692(7) 0.5725(7) 0.9489(8) 0.060(2) Uani 0.252(7) 1 d D U P A 2 C57' C 1.0939(16) 0.6062(11) 0.9910(13) 0.064(3) Uani 0.252(7) 1 d D U P A 2 H57D H 1.103063 0.633351 0.967850 0.096 Uiso 0.252(7) 1 calc R U P A 2 H57E H 1.073385 0.615345 1.024013 0.096 Uiso 0.252(7) 1 calc R U P A 2 H57F H 1.121170 0.591531 1.008072 0.096 Uiso 0.252(7) 1 calc R U P A 2 C58' C 1.1040(6) 0.5563(8) 0.9012(8) 0.064(3) Uani 0.252(7) 1 d D U P A 2 H58D H 1.113378 0.582281 0.876030 0.096 Uiso 0.252(7) 1 calc R U P A 2 H58E H 1.130784 0.543445 0.921702 0.096 Uiso 0.252(7) 1 calc R U P A 2 H58F H 1.089921 0.532840 0.875476 0.096 Uiso 0.252(7) 1 calc R U P A 2 C59' C 1.0555(7) 0.5307(7) 0.9870(9) 0.067(3) Uani 0.252(7) 1 d D U P A 2 H59D H 1.039594 0.508506 0.961238 0.100 Uiso 0.252(7) 1 calc R U P A 2 H59E H 1.083042 0.516530 1.004104 0.100 Uiso 0.252(7) 1 calc R U P A 2 H59F H 1.035257 0.540344 1.020045 0.100 Uiso 0.252(7) 1 calc R U P A 2 C60 C 0.95052(14) 0.57027(13) 0.78349(16) 0.0288(9) Uani 1 1 d . . . . . H60 H 0.934353 0.594790 0.760223 0.035 Uiso 1 1 calc R U . . . C61 C 0.98655(14) 0.55122(14) 0.74111(16) 0.0310(9) Uani 1 1 d . . . . . C62 C 1.00525(14) 0.57929(13) 0.69668(17) 0.0322(9) Uani 1 1 d . . . . . H62 H 0.994050 0.609573 0.691879 0.039 Uiso 1 1 calc R U . . . C63 C 1.04021(15) 0.56362(15) 0.65907(19) 0.0395(10) Uani 1 1 d . . . . . H63 H 1.053018 0.583366 0.629340 0.047 Uiso 1 1 calc R U . . . C64 C 1.05638(16) 0.51911(15) 0.66499(19) 0.0396(10) Uani 1 1 d . . . . . H64 H 1.079679 0.508057 0.638765 0.048 Uiso 1 1 calc R U . . . C65 C 1.03829(16) 0.49128(15) 0.7092(2) 0.0423(11) Uani 1 1 d . . . . . H65 H 1.049506 0.460972 0.713533 0.051 Uiso 1 1 calc R U . . . C66 C 1.00373(16) 0.50678(15) 0.74779(18) 0.0402(11) Uani 1 1 d . . . . . H66 H 0.991904 0.487255 0.778481 0.048 Uiso 1 1 calc R U . . . C67 C 0.91434(16) 0.53535(14) 0.80008(18) 0.0374(10) Uani 1 1 d . . . . . C68 C 0.9130(2) 0.51429(18) 0.8562(2) 0.0645(16) Uani 1 1 d . . . . . H68 H 0.934765 0.522526 0.886319 0.077 Uiso 1 1 calc R U . . . C69 C 0.8802(3) 0.4810(2) 0.8692(3) 0.092(2) Uani 1 1 d . . . . . H69 H 0.880480 0.465725 0.907188 0.110 Uiso 1 1 calc R U . . . C70 C 0.8463(3) 0.4702(2) 0.8252(4) 0.082(2) Uani 1 1 d . . . . . H70 H 0.823161 0.448383 0.833748 0.098 Uiso 1 1 calc R U . . . C71 C 0.8478(2) 0.49217(19) 0.7697(3) 0.0652(16) Uani 1 1 d . . . . . H71 H 0.825789 0.484835 0.739524 0.078 Uiso 1 1 calc R U . . . C72 C 0.88044(16) 0.52416(16) 0.7574(2) 0.0414(11) Uani 1 1 d . . . . . H72 H 0.880233 0.539222 0.719208 0.050 Uiso 1 1 calc R U . . . Cl1 Cl 0.750000 0.750000 0.57518(7) 0.0224(4) Uani 1 4 d S T P . . Mg3 Mg 0.750000 0.750000 0.45385(10) 0.0210(5) Uani 1 4 d S T P . . O18 O 0.750000 0.750000 0.3571(2) 0.0314(12) Uani 1 4 d DS T P . . H18O H 0.773(3) 0.766(4) 0.333000 0.047 Uiso 0.5 1 d D U P . . O19 O 0.81346(8) 0.72225(9) 0.45203(11) 0.0230(5) Uani 1 1 d D . . . . H19P H 0.8198(13) 0.6944(8) 0.4727(17) 0.035 Uiso 1 1 d D U . . . H19O H 0.8394(10) 0.7409(10) 0.4608(18) 0.035 Uiso 1 1 d D U . . . Cl2 Cl 0.750000 0.750000 0.96692(7) 0.0231(4) Uani 1 4 d S T P . . O20 O 0.76588(11) 0.51657(11) 0.64341(13) 0.0399(7) Uani 1 1 d D . . . . H20O H 0.7978(8) 0.5165(18) 0.653(2) 0.060 Uiso 1 1 d D U . . . H20P H 0.7724(18) 0.5383(14) 0.6119(17) 0.060 Uiso 1 1 d D 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 Mg1 0.0256(6) 0.0239(6) 0.0134(5) -0.0022(5) 0.0004(5) 0.0004(5) P1 0.0222(4) 0.0204(4) 0.0135(4) -0.0029(3) 0.0012(3) 0.0014(4) O1 0.0268(13) 0.0262(13) 0.0154(11) -0.0056(10) -0.0003(10) -0.0007(11) O2 0.0224(12) 0.0230(12) 0.0150(11) -0.0021(10) -0.0012(10) 0.0024(10) O3 0.0250(13) 0.0275(13) 0.0146(11) -0.0036(10) 0.0000(10) 0.0011(11) O4 0.0248(13) 0.0227(12) 0.0178(12) -0.0031(10) 0.0018(10) 0.0006(10) O5 0.0327(15) 0.0265(14) 0.0262(14) -0.0035(11) -0.0009(11) 0.0052(12) O6 0.0322(14) 0.0298(14) 0.0144(11) -0.0028(10) -0.0012(11) -0.0087(11) O7 0.0240(13) 0.0216(13) 0.0193(12) -0.0003(10) 0.0005(10) -0.0016(10) O8 0.0276(13) 0.0266(13) 0.0200(12) 0.0001(11) 0.0039(11) 0.0029(11) O9 0.0254(13) 0.0306(14) 0.0162(12) -0.0011(11) -0.0001(10) -0.0054(11) C1 0.0237(18) 0.0268(19) 0.0180(17) -0.0077(15) -0.0001(14) 0.0028(15) C2 0.0224(18) 0.036(2) 0.0241(18) -0.0114(16) 0.0026(15) 0.0089(16) C3 0.027(2) 0.050(3) 0.0184(18) -0.0118(17) -0.0018(15) 0.0088(18) C4 0.028(2) 0.040(2) 0.0248(19) -0.0191(17) -0.0057(16) 0.0098(17) C5 0.027(2) 0.033(2) 0.034(2) -0.0132(17) 0.0018(17) -0.0005(17) C6 0.0184(17) 0.031(2) 0.0209(17) -0.0081(15) 0.0025(14) 0.0012(15) C7 0.028(2) 0.031(2) 0.0159(16) 0.0009(15) 0.0034(15) 0.0054(16) C8 0.033(2) 0.035(2) 0.0112(16) -0.0042(15) 0.0030(15) 0.0069(17) C9 0.035(2) 0.033(2) 0.029(2) -0.0013(17) -0.0009(17) 0.0059(18) C10 0.032(2) 0.040(2) 0.045(2) -0.002(2) -0.0026(19) 0.0031(19) C11 0.041(2) 0.043(3) 0.030(2) -0.0037(19) 0.0089(19) -0.006(2) C12 0.047(3) 0.030(2) 0.029(2) -0.0020(17) 0.0100(19) -0.0040(19) C13 0.040(2) 0.035(2) 0.025(2) 0.0039(17) 0.0021(17) 0.0062(19) C14 0.031(2) 0.034(2) 0.0232(19) -0.0001(16) 0.0015(16) -0.0035(17) C15 0.038(2) 0.060(3) 0.0207(19) -0.0009(19) 0.0040(18) 0.007(2) C16 0.050(3) 0.063(3) 0.0190(19) 0.000(2) 0.0070(19) 0.001(2) C17 0.064(3) 0.057(3) 0.025(2) -0.001(2) -0.016(2) 0.001(3) C18 0.037(2) 0.047(3) 0.042(2) 0.004(2) -0.008(2) 0.006(2) C19 0.033(2) 0.039(2) 0.028(2) 0.0007(18) -0.0007(17) -0.0012(18) C20 0.047(3) 0.055(3) 0.039(2) -0.031(2) -0.012(2) 0.010(2) C21 0.130(6) 0.110(6) 0.043(3) -0.056(4) 0.005(4) -0.019(5) C22 0.054(4) 0.145(7) 0.078(4) -0.080(5) -0.010(3) -0.001(4) C23 0.191(9) 0.063(4) 0.053(4) -0.040(3) -0.037(5) 0.034(5) C24 0.037(2) 0.0208(18) 0.0246(18) -0.0081(15) 0.0054(16) 0.0007(16) C25 0.048(3) 0.028(2) 0.037(2) -0.0110(18) 0.014(2) -0.0048(19) C26 0.045(3) 0.041(2) 0.042(2) -0.006(2) 0.000(2) -0.004(2) C27 0.051(3) 0.053(3) 0.064(3) -0.003(3) 0.012(3) -0.016(3) C28 0.072(4) 0.053(4) 0.139(7) -0.006(4) 0.026(4) -0.031(3) C29 0.073(5) 0.035(3) 0.220(10) 0.013(4) 0.028(5) -0.009(3) C30 0.050(3) 0.035(3) 0.145(6) 0.008(3) 0.024(4) -0.006(2) C31 0.039(2) 0.0216(18) 0.0254(19) 0.0009(15) 0.0009(17) -0.0017(16) C32 0.058(3) 0.035(2) 0.029(2) -0.0092(18) -0.003(2) 0.008(2) C33 0.072(3) 0.032(2) 0.038(2) -0.005(2) -0.025(2) 0.004(2) C34 0.051(3) 0.038(2) 0.050(3) 0.000(2) -0.015(2) -0.001(2) C35 0.047(3) 0.056(3) 0.034(2) 0.002(2) -0.004(2) 0.013(2) C36 0.045(3) 0.044(3) 0.025(2) -0.0033(18) 0.0010(19) 0.006(2) Mg2 0.0221(6) 0.0260(6) 0.0143(5) -0.0013(5) 0.0008(5) -0.0012(5) P2 0.0195(4) 0.0230(4) 0.0123(4) -0.0010(3) -0.0013(3) 0.0020(4) O10 0.0255(13) 0.0207(12) 0.0160(11) 0.0005(10) -0.0024(10) 0.0049(10) O11 0.0195(12) 0.0289(13) 0.0144(11) -0.0010(10) -0.0007(9) -0.0025(10) O12 0.0222(12) 0.0276(13) 0.0171(11) 0.0010(10) 0.0023(10) -0.0023(10) O13 0.0221(12) 0.0229(12) 0.0118(11) -0.0004(9) 0.0000(9) 0.0024(10) O14 0.0216(12) 0.0279(13) 0.0148(11) -0.0009(10) 0.0022(10) 0.0024(11) O15 0.0322(15) 0.0361(15) 0.0270(14) -0.0128(12) -0.0008(12) 0.0054(12) O16 0.0333(15) 0.0459(17) 0.0255(14) 0.0110(13) -0.0016(12) -0.0004(14) O17 0.0220(14) 0.0531(18) 0.0343(15) -0.0238(14) 0.0100(12) -0.0120(13) C37 0.0225(18) 0.0258(19) 0.0234(18) 0.0016(15) -0.0051(15) 0.0031(15) C38 0.031(2) 0.034(2) 0.0204(18) -0.0056(16) -0.0040(16) 0.0097(17) C39 0.040(2) 0.059(3) 0.0223(19) -0.021(2) -0.0122(18) 0.017(2) C40 0.039(2) 0.071(3) 0.032(2) -0.017(2) -0.016(2) 0.027(2) C41 0.040(2) 0.054(3) 0.027(2) -0.0169(19) -0.0122(18) 0.027(2) C42 0.041(2) 0.031(2) 0.0203(18) -0.0043(16) -0.0047(17) 0.0145(18) C43 0.030(2) 0.031(2) 0.0233(18) -0.0091(16) -0.0082(16) 0.0116(17) C44 0.034(2) 0.031(2) 0.0159(17) -0.0074(15) -0.0069(16) 0.0029(17) C45 0.035(2) 0.037(2) 0.0224(18) 0.0015(17) -0.0026(16) 0.0020(18) C46 0.032(2) 0.052(3) 0.029(2) -0.0038(19) -0.0023(17) 0.005(2) C47 0.047(3) 0.053(3) 0.026(2) -0.001(2) 0.0006(19) -0.013(2) C48 0.050(3) 0.037(2) 0.038(2) -0.002(2) 0.001(2) -0.001(2) C49 0.044(3) 0.043(3) 0.031(2) -0.0077(19) -0.0046(19) 0.005(2) C50 0.033(2) 0.032(2) 0.0250(19) -0.0074(16) -0.0091(16) 0.0085(17) C51 0.066(3) 0.041(2) 0.027(2) -0.0053(19) -0.020(2) 0.008(2) C52 0.095(4) 0.055(3) 0.041(3) -0.018(3) -0.036(3) 0.005(3) C53 0.077(4) 0.050(3) 0.067(4) -0.021(3) -0.036(3) -0.003(3) C54 0.046(3) 0.045(3) 0.071(4) -0.014(3) -0.012(3) -0.006(2) C55 0.033(2) 0.044(3) 0.042(2) -0.010(2) -0.0064(19) -0.0008(19) C56 0.037(3) 0.095(4) 0.044(3) -0.023(3) -0.019(2) 0.034(3) C57 0.042(3) 0.112(6) 0.053(3) -0.021(4) -0.025(3) 0.025(5) C58 0.038(3) 0.117(5) 0.052(4) -0.013(4) -0.015(3) 0.020(4) C59 0.053(4) 0.096(4) 0.062(4) -0.007(4) -0.024(3) 0.033(4) C56' 0.040(4) 0.095(5) 0.044(4) -0.019(4) -0.019(4) 0.035(4) C57' 0.042(6) 0.100(6) 0.049(5) -0.019(5) -0.022(5) 0.030(6) C58' 0.039(5) 0.105(6) 0.048(5) -0.015(5) -0.020(4) 0.039(5) C59' 0.055(7) 0.091(7) 0.053(6) -0.009(6) -0.024(6) 0.034(6) C60 0.037(2) 0.029(2) 0.0212(18) -0.0044(15) -0.0023(16) 0.0157(17) C61 0.039(2) 0.035(2) 0.0189(18) -0.0075(16) -0.0070(16) 0.0116(18) C62 0.044(2) 0.0254(19) 0.027(2) -0.0086(16) -0.0021(18) 0.0069(18) C63 0.044(3) 0.042(2) 0.033(2) -0.0007(19) 0.0017(19) 0.005(2) C64 0.045(3) 0.037(2) 0.036(2) -0.011(2) -0.001(2) 0.011(2) C65 0.056(3) 0.033(2) 0.038(2) -0.0021(19) 0.000(2) 0.023(2) C66 0.060(3) 0.036(2) 0.025(2) -0.0039(18) -0.001(2) 0.023(2) C67 0.052(3) 0.031(2) 0.029(2) -0.0082(18) -0.0007(19) 0.0080(19) C68 0.102(5) 0.049(3) 0.043(3) 0.013(2) -0.001(3) -0.009(3) C69 0.141(7) 0.062(4) 0.072(4) 0.016(3) 0.015(5) -0.025(4) C70 0.094(5) 0.057(4) 0.095(5) 0.005(4) 0.009(4) -0.018(4) C71 0.072(4) 0.052(3) 0.072(4) -0.017(3) -0.005(3) 0.004(3) C72 0.048(3) 0.039(2) 0.037(2) -0.010(2) 0.003(2) 0.003(2) Cl1 0.0247(5) 0.0247(5) 0.0179(8) 0.000 0.000 0.000 Mg3 0.0254(8) 0.0254(8) 0.0123(10) 0.000 0.000 0.000 O18 0.0389(19) 0.0389(19) 0.016(2) 0.000 0.000 0.000 O19 0.0242(13) 0.0233(13) 0.0216(12) 0.0006(10) -0.0027(10) -0.0004(10) Cl2 0.0279(5) 0.0279(5) 0.0134(7) 0.000 0.000 0.000 O20 0.0424(17) 0.0416(17) 0.0356(16) 0.0064(13) 0.0069(14) 0.0069(15) 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' 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 O2 Mg1 O9 178.27(12) . . O2 Mg1 O6 91.62(11) . . O9 Mg1 O6 87.81(11) . . O2 Mg1 O8 92.22(11) . . O9 Mg1 O8 88.19(11) . . O6 Mg1 O8 173.40(12) . . O2 Mg1 O5 89.28(11) . . O9 Mg1 O5 89.08(11) . . O6 Mg1 O5 89.79(11) . . O8 Mg1 O5 84.90(11) . . O2 Mg1 O7 90.02(10) . . O9 Mg1 O7 91.64(11) . . O6 Mg1 O7 93.69(11) . . O8 Mg1 O7 91.67(11) . . O5 Mg1 O7 176.47(11) . . O3 P1 O2 114.67(14) . . O3 P1 O4 113.07(14) . . O2 P1 O4 110.42(13) . . O3 P1 O1 106.67(13) . . O2 P1 O1 102.92(13) . . O4 P1 O1 108.34(13) . . C1 O1 P1 123.0(2) . . P1 O2 Mg1 130.08(14) . . Mg1 O5 H5O 124(3) . . Mg1 O5 H5P 108(3) . . H5O O5 H5P 106(2) . . Mg1 O6 H6O 112(2) . . Mg1 O6 H6P 130(2) . . H6O O6 H6P 103(2) . . Mg1 O7 H7O 115(2) . . Mg1 O7 H7P 112(2) . . H7O O7 H7P 109(2) . . Mg1 O8 H8O 121(2) . . Mg1 O8 H8P 119(2) . . H8O O8 H8P 110(2) . . Mg1 O9 H9O 120(2) . . Mg1 O9 H9P 119(2) . . H9O O9 H9P 103(2) . . C2 C1 C6 122.3(3) . . C2 C1 O1 119.9(3) . . C6 C1 O1 117.8(3) . . C1 C2 C3 117.5(4) . . C1 C2 C7 121.0(3) . . C3 C2 C7 121.1(3) . . C2 C3 C4 121.9(4) . . C2 C3 H3 119.0 . . C4 C3 H3 119.0 . . C5 C4 C3 118.6(3) . . C5 C4 C20 120.7(4) . . C3 C4 C20 120.6(4) . . C4 C5 C6 121.3(4) . . C4 C5 H5 119.4 . . C6 C5 H5 119.4 . . C5 C6 C1 118.4(3) . . C5 C6 C24 122.3(3) . . C1 C6 C24 119.2(3) . . C14 C7 C2 111.3(3) . . C14 C7 C8 110.8(3) . . C2 C7 C8 117.2(3) . . C14 C7 H7 105.5 . . C2 C7 H7 105.5 . . C8 C7 H7 105.5 . . C9 C8 C13 118.1(4) . . C9 C8 C7 124.1(4) . . C13 C8 C7 117.7(3) . . C8 C9 C10 119.8(4) . . C8 C9 H9 120.1 . . C10 C9 H9 120.1 . . C11 C10 C9 120.5(4) . . C11 C10 H10 119.7 . . C9 C10 H10 119.7 . . C10 C11 C12 120.2(4) . . C10 C11 H11 119.9 . . C12 C11 H11 119.9 . . C13 C12 C11 118.7(4) . . C13 C12 H12 120.7 . . C11 C12 H12 120.7 . . C12 C13 C8 122.7(4) . . C12 C13 H13 118.6 . . C8 C13 H13 118.6 . . C19 C14 C15 118.8(4) . . C19 C14 C7 118.7(3) . . C15 C14 C7 122.4(4) . . C14 C15 C16 119.3(4) . . C14 C15 H15 120.3 . . C16 C15 H15 120.3 . . C17 C16 C15 120.6(4) . . C17 C16 H16 119.7 . . C15 C16 H16 119.7 . . C16 C17 C18 120.5(4) . . C16 C17 H17 119.7 . . C18 C17 H17 119.7 . . C19 C18 C17 119.3(4) . . C19 C18 H18 120.3 . . C17 C18 H18 120.3 . . C18 C19 C14 121.4(4) . . C18 C19 H19 119.3 . . C14 C19 H19 119.3 . . C23 C20 C22 114.0(6) . . C23 C20 C4 111.7(4) . . C22 C20 C4 108.8(4) . . C23 C20 C21 106.5(5) . . C22 C20 C21 105.0(5) . . C4 C20 C21 110.6(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 . . C31 C24 C25 115.9(3) . . C31 C24 C6 109.9(3) . . C25 C24 C6 112.8(3) . . C31 C24 H24 105.8 . . C25 C24 H24 105.8 . . C6 C24 H24 105.8 . . C30 C25 C26 118.2(4) . . C30 C25 C24 123.8(4) . . C26 C25 C24 118.0(4) . . C27 C26 C25 120.1(5) . . C27 C26 H26 120.0 . . C25 C26 H26 120.0 . . C26 C27 C28 121.3(5) . . C26 C27 H27 119.4 . . C28 C27 H27 119.4 . . C27 C28 C29 118.6(5) . . C27 C28 H28 120.7 . . C29 C28 H28 120.7 . . C30 C29 C28 121.1(6) . . C30 C29 H29 119.5 . . C28 C29 H29 119.5 . . C29 C30 C25 120.7(6) . . C29 C30 H30 119.7 . . C25 C30 H30 119.7 . . C36 C31 C32 116.9(4) . . C36 C31 C24 122.1(3) . . C32 C31 C24 120.8(4) . . C33 C32 C31 121.8(4) . . C33 C32 H32 119.1 . . C31 C32 H32 119.1 . . C32 C33 C34 119.7(4) . . C32 C33 H33 120.1 . . C34 C33 H33 120.1 . . C35 C34 C33 119.9(5) . . C35 C34 H34 120.0 . . C33 C34 H34 120.0 . . C36 C35 C34 118.9(4) . . C36 C35 H35 120.6 . . C34 C35 H35 120.6 . . C35 C36 C31 122.7(4) . . C35 C36 H36 118.6 . . C31 C36 H36 118.6 . . O17 Mg2 O13 89.16(11) . 4_565 O17 Mg2 O15 179.05(13) . . O13 Mg2 O15 89.90(11) 4_565 . O17 Mg2 O11 87.68(11) . . O13 Mg2 O11 173.04(11) 4_565 . O15 Mg2 O11 93.26(11) . . O17 Mg2 O16 88.98(13) . . O13 Mg2 O16 95.77(11) 4_565 . O15 Mg2 O16 91.12(12) . . O11 Mg2 O16 90.37(11) . . O17 Mg2 O14 93.03(12) . . O13 Mg2 O14 87.96(10) 4_565 . O15 Mg2 O14 86.94(11) . . O11 Mg2 O14 86.02(10) . . O16 Mg2 O14 175.80(12) . . O12 P2 O11 114.48(13) . . O12 P2 O13 112.47(14) . . O11 P2 O13 112.04(14) . . O12 P2 O10 108.28(13) . . O11 P2 O10 101.96(13) . . O13 P2 O10 106.69(12) . . C37 O10 P2 125.2(2) . . P2 O11 Mg2 131.44(14) . . P2 O13 Mg2 129.82(13) . 3_655 Mg2 O14 H14O 112(2) . . Mg2 O14 H14P 113(2) . . H14O O14 H14P 105(2) . . Mg2 O15 H15O 110(3) . . Mg2 O15 H15P 132(3) . . H15O O15 H15P 104(2) . . Mg2 O16 H16O 121(3) . . Mg2 O16 H16P 120(3) . . H16O O16 H16P 106(2) . . Mg2 O17 H17O 135(3) . . Mg2 O17 H17P 113(3) . . H17O O17 H17P 111(3) . . C38 C37 C42 122.1(3) . . C38 C37 O10 118.9(3) . . C42 C37 O10 118.8(3) . . C37 C38 C39 117.9(3) . . C37 C38 C43 119.3(3) . . C39 C38 C43 122.6(3) . . C40 C39 C38 122.9(4) . . C40 C39 H39 118.5 . . C38 C39 H39 118.5 . . C39 C40 C41 117.1(4) . . C39 C40 C56 122.8(4) . . C41 C40 C56 119.6(4) . . C39 C40 C56' 122.0(7) . . C41 C40 C56' 115.1(8) . . C42 C41 C40 122.1(4) . . C42 C41 H41 118.9 . . C40 C41 H41 118.9 . . C37 C42 C41 117.8(3) . . C37 C42 C60 119.2(3) . . C41 C42 C60 123.0(3) . . C44 C43 C38 110.9(3) . . C44 C43 C50 114.4(3) . . C38 C43 C50 112.1(3) . . C44 C43 H43 106.3 . . C38 C43 H43 106.3 . . C50 C43 H43 106.3 . . C49 C44 C45 118.1(4) . . C49 C44 C43 123.6(4) . . C45 C44 C43 118.3(3) . . C44 C45 C46 120.7(4) . . C44 C45 H45 119.6 . . C46 C45 H45 119.6 . . C47 C46 C45 119.9(4) . . C47 C46 H46 120.0 . . C45 C46 H46 120.0 . . C46 C47 C48 118.3(4) . . C46 C47 H47 120.8 . . C48 C47 H47 120.8 . . C49 C48 C47 120.8(4) . . C49 C48 H48 119.6 . . C47 C48 H48 119.6 . . C48 C49 C44 122.1(4) . . C48 C49 H49 119.0 . . C44 C49 H49 119.0 . . C51 C50 C55 118.4(4) . . C51 C50 C43 123.1(4) . . C55 C50 C43 118.5(3) . . C52 C51 C50 120.9(5) . . C52 C51 H51 119.6 . . C50 C51 H51 119.6 . . C53 C52 C51 120.3(5) . . C53 C52 H52 119.8 . . C51 C52 H52 119.8 . . C52 C53 C54 119.9(5) . . C52 C53 H53 120.0 . . C54 C53 H53 120.0 . . C55 C54 C53 120.0(5) . . C55 C54 H54 120.0 . . C53 C54 H54 120.0 . . C54 C55 C50 120.6(4) . . C54 C55 H55 119.7 . . C50 C55 H55 119.7 . . C58 C56 C57 108.5(7) . . C58 C56 C59 108.7(6) . . C57 C56 C59 107.7(6) . . C58 C56 C40 112.5(5) . . C57 C56 C40 112.4(8) . . C59 C56 C40 106.8(6) . . 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 . . C59' C56' C57' 107.6(12) . . C59' C56' C58' 107.4(12) . . C57' C56' C58' 107.4(12) . . C59' C56' C40 122.3(15) . . C57' C56' C40 105(2) . . C58' C56' C40 106.4(13) . . 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 . . 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 . . C67 C60 C61 112.7(3) . . C67 C60 C42 113.0(3) . . C61 C60 C42 112.2(3) . . C67 C60 H60 106.1 . . C61 C60 H60 106.1 . . C42 C60 H60 106.1 . . C62 C61 C66 118.7(4) . . C62 C61 C60 119.4(3) . . C66 C61 C60 121.7(4) . . C61 C62 C63 120.9(4) . . C61 C62 H62 119.6 . . C63 C62 H62 119.6 . . C64 C63 C62 120.1(4) . . C64 C63 H63 120.0 . . C62 C63 H63 120.0 . . C65 C64 C63 119.3(4) . . C65 C64 H64 120.3 . . C63 C64 H64 120.3 . . C64 C65 C66 121.2(4) . . C64 C65 H65 119.4 . . C66 C65 H65 119.4 . . C65 C66 C61 119.8(4) . . C65 C66 H66 120.1 . . C61 C66 H66 120.1 . . C68 C67 C72 118.4(5) . . C68 C67 C60 122.4(4) . . C72 C67 C60 119.2(4) . . C67 C68 C69 120.8(6) . . C67 C68 H68 119.6 . . C69 C68 H68 119.6 . . C68 C69 C70 119.7(6) . . C68 C69 H69 120.2 . . C70 C69 H69 120.2 . . C71 C70 C69 118.5(6) . . C71 C70 H70 120.7 . . C69 C70 H70 120.7 . . C72 C71 C70 121.1(6) . . C72 C71 H71 119.5 . . C70 C71 H71 119.5 . . C71 C72 C67 121.4(5) . . C71 C72 H72 119.3 . . C67 C72 H72 119.3 . . O19 Mg3 O19 177.74(18) 4_565 3_655 O19 Mg3 O19 89.978(4) 4_565 2_665 O19 Mg3 O19 89.978(4) 3_655 2_665 O19 Mg3 O19 89.979(4) 4_565 . O19 Mg3 O19 89.977(4) 3_655 . O19 Mg3 O19 177.74(18) 2_665 . O19 Mg3 O18 88.87(9) 4_565 . O19 Mg3 O18 88.87(9) 3_655 . O19 Mg3 O18 88.87(9) 2_665 . O19 Mg3 O18 88.87(9) . . O19 Mg3 Cl1 91.13(9) 4_565 . O19 Mg3 Cl1 91.13(9) 3_655 . O19 Mg3 Cl1 91.13(9) 2_665 . O19 Mg3 Cl1 91.13(9) . . O18 Mg3 Cl1 180.0 . . Mg3 O18 H18O 123.1(9) . . Mg3 O19 H19P 121(2) . . Mg3 O19 H19O 120(2) . . H19P O19 H19O 104(2) . . H20O O20 H20P 88(4) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Mg1 O2 2.025(3) . Mg1 O9 2.029(3) . Mg1 O6 2.064(3) . Mg1 O8 2.065(3) . Mg1 O5 2.140(3) . Mg1 O7 2.147(3) . P1 O3 1.505(2) . P1 O2 1.518(3) . P1 O4 1.527(2) . P1 O1 1.635(2) . O1 C1 1.404(4) . O5 H5O 0.948(18) . O5 H5P 0.944(18) . O6 H6O 0.962(18) . O6 H6P 0.945(18) . O7 H7O 0.935(18) . O7 H7P 0.940(18) . O8 H8O 0.937(18) . O8 H8P 0.928(18) . O9 H9O 0.963(18) . O9 H9P 0.954(18) . C1 C2 1.377(5) . C1 C6 1.402(5) . C2 C3 1.393(5) . C2 C7 1.526(5) . C3 C4 1.397(6) . C3 H3 0.9500 . C4 C5 1.381(6) . C4 C20 1.538(5) . C5 C6 1.385(5) . C5 H5 0.9500 . C6 C24 1.530(5) . C7 C14 1.524(5) . C7 C8 1.542(5) . C7 H7 1.0000 . C8 C9 1.381(5) . C8 C13 1.384(6) . C9 C10 1.403(6) . C9 H9 0.9500 . C10 C11 1.372(6) . C10 H10 0.9500 . C11 C12 1.381(6) . C11 H11 0.9500 . C12 C13 1.373(6) . C12 H12 0.9500 . C13 H13 0.9500 . C14 C19 1.384(6) . C14 C15 1.401(5) . C15 C16 1.405(6) . C15 H15 0.9500 . C16 C17 1.357(7) . C16 H16 0.9500 . C17 C18 1.391(7) . C17 H17 0.9500 . C18 C19 1.380(6) . C18 H18 0.9500 . C19 H19 0.9500 . C20 C23 1.508(8) . C20 C22 1.518(7) . C20 C21 1.551(9) . 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 . C24 C31 1.500(6) . C24 C25 1.518(6) . C24 H24 1.0000 . C25 C30 1.373(7) . C25 C26 1.424(6) . C26 C27 1.367(7) . C26 H26 0.9500 . C27 C28 1.373(8) . C27 H27 0.9500 . C28 C29 1.387(10) . C28 H28 0.9500 . C29 C30 1.375(8) . C29 H29 0.9500 . C30 H30 0.9500 . C31 C36 1.387(6) . C31 C32 1.395(6) . C32 C33 1.375(7) . C32 H32 0.9500 . C33 C34 1.391(7) . C33 H33 0.9500 . C34 C35 1.388(6) . C34 H34 0.9500 . C35 C36 1.378(6) . C35 H35 0.9500 . C36 H36 0.9500 . Mg2 O17 2.026(3) . Mg2 O13 2.038(3) 4_565 Mg2 O15 2.048(3) . Mg2 O11 2.053(3) . Mg2 O16 2.124(3) . Mg2 O14 2.189(3) . P2 O12 1.504(2) . P2 O11 1.523(2) . P2 O13 1.527(2) . P2 O10 1.621(2) . O10 C37 1.399(4) . O14 H14O 0.943(18) . O14 H14P 0.940(18) . O15 H15O 0.963(18) . O15 H15P 0.944(18) . O16 H16O 0.932(18) . O16 H16P 0.948(18) . O17 H17O 0.909(18) . O17 H17P 0.930(18) . C37 C38 1.381(5) . C37 C42 1.387(5) . C38 C39 1.387(5) . C38 C43 1.528(5) . C39 C40 1.377(6) . C39 H39 0.9500 . C40 C41 1.398(6) . C40 C56 1.545(8) . C40 C56' 1.60(2) . C41 C42 1.392(5) . C41 H41 0.9500 . C42 C60 1.517(5) . C43 C44 1.522(6) . C43 C50 1.528(5) . C43 H43 1.0000 . C44 C49 1.379(6) . C44 C45 1.393(5) . C45 C46 1.409(6) . C45 H45 0.9500 . C46 C47 1.393(6) . C46 H46 0.9500 . C47 C48 1.400(7) . C47 H47 0.9500 . C48 C49 1.366(6) . C48 H48 0.9500 . C49 H49 0.9500 . C50 C51 1.383(6) . C50 C55 1.397(6) . C51 C52 1.373(7) . C51 H51 0.9500 . C52 C53 1.367(8) . C52 H52 0.9500 . C53 C54 1.385(8) . C53 H53 0.9500 . C54 C55 1.370(6) . C54 H54 0.9500 . C55 H55 0.9500 . C56 C58 1.521(9) . C56 C57 1.537(9) . C56 C59 1.541(9) . 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 . C56' C59' 1.536(14) . C56' C57' 1.536(14) . C56' C58' 1.538(14) . C57' H57D 0.9800 . C57' H57E 0.9800 . C57' H57F 0.9800 . C58' H58D 0.9800 . C58' H58E 0.9800 . C58' H58F 0.9800 . C59' H59D 0.9800 . C59' H59E 0.9800 . C59' H59F 0.9800 . C60 C67 1.515(6) . C60 C61 1.514(5) . C60 H60 1.0000 . C61 C62 1.390(6) . C61 C66 1.401(6) . C62 C63 1.393(6) . C62 H62 0.9500 . C63 C64 1.391(6) . C63 H63 0.9500 . C64 C65 1.375(6) . C64 H64 0.9500 . C65 C66 1.397(6) . C65 H65 0.9500 . C66 H66 0.9500 . C67 C68 1.381(6) . C67 C72 1.405(6) . C68 C69 1.396(9) . C68 H68 0.9500 . C69 C70 1.421(10) . C69 H69 0.9500 . C70 C71 1.382(9) . C70 H70 0.9500 . C71 C72 1.363(8) . C71 H71 0.9500 . C72 H72 0.9500 . Cl1 Mg3 2.673(3) . Mg3 O19 2.026(2) 4_565 Mg3 O19 2.026(2) 3_655 Mg3 O19 2.026(2) 2_665 Mg3 O19 2.026(2) . Mg3 O18 2.131(5) . O18 H18O 0.97(2) . O19 H19P 0.951(18) . O19 H19O 0.954(18) . O20 H20O 0.956(19) . O20 H20P 0.959(19) . 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 O5 H5P O1 0.944(18) 1.94(2) 2.847(4) 159(4) . O6 H6O O4 0.962(18) 1.83(2) 2.721(3) 152(3) . O6 H6P O11 0.945(18) 1.805(19) 2.741(3) 170(4) . O7 H7O Cl1 0.935(18) 2.40(2) 3.325(2) 171(3) . O7 H7P O4 0.940(18) 1.835(18) 2.766(3) 170(3) 3_655 O8 H8O O3 0.937(18) 1.74(2) 2.643(3) 162(4) 3_655 O9 H9O O12 0.963(18) 1.645(18) 2.606(3) 176(4) . O9 H9P O20 0.954(18) 1.91(2) 2.819(4) 158(3) 3_655 O14 H14O O11 0.943(18) 2.53(3) 3.254(3) 134(3) 4_565 O14 H14O O14 0.943(18) 2.10(3) 2.936(3) 147(3) 4_565 O14 H14P O7 0.940(18) 2.08(2) 3.001(3) 167(3) 4_565 O15 H15O O12 0.963(18) 1.80(2) 2.696(4) 153(4) 4_565 O15 H15P O20 0.944(18) 2.45(4) 2.966(4) 114(3) . O16 H16O O10 0.932(18) 2.35(4) 2.985(4) 125(4) . O17 H17O O17 0.909(18) 2.60(4) 3.083(4) 114(3) 4_565 O17 H17O Cl2 0.909(18) 2.26(3) 3.124(3) 159(4) . O17 H17P O13 0.930(18) 1.76(2) 2.662(3) 161(4) . O17 H17P O17 0.930(18) 2.57(4) 3.083(4) 115(3) 3_655 O19 H19P O2 0.951(18) 1.80(2) 2.723(3) 163(3) . O19 H19O O3 0.954(18) 1.684(19) 2.637(3) 178(4) 3_655 O20 H20P O4 0.959(19) 1.81(3) 2.715(4) 156(5) .