# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_shelxl _database_code_depnum_ccdc_archive 'CCDC 910535' #TrackingRef '15365_web_deposit_cif_file_0_ChristophJaniak_1352729919.Mn-twin5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; catena-(bis(\m~9~-(5,5',5'',5'''-((Adamantane-1,3,5,7-tetrayl)- tetra-(phen-4-yl))-tetrakistetrazolato))- bis-(\m~2~-chloro)-tetraaqua-tetrakisdimethylformamido- penta-manganese(ii) dimethylformamide and water solvate ) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; (Mn 2+)5, (Cl -)2, (C38 H28 N16 4-)2, (H2 O)7, (C3 H7 N O)11 ; # Above moiety formula is without additional guest molecules # corresponding to [Mn5Cl2(L1)2(H2O)4(DMF)4] . 3 H2O . 7 DMF. # Moiety formula with additional guest molecules included is # '2(C86.63 H70 Cl2 Mn5 N36.06 O8), 10.79(C3 N O), 2(C6 N2 O), 4(C # O), 2.21(C O), 12C' _chemical_formula_sum 'C109 H147 Cl2 Mn5 N43 O18' # Above formula sum is without guest molecules # Formula sum with additional guest molecules included is #'C235.84 H140 Cl4 Mn10 N86.92 O35' and Z = 1 _chemical_formula_weight 2693.21 # Above formula weight is without additional guest molecules. # Formula weight with guest molecules included is 5442.50. 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' N N 0.0061 0.0033 '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' Mn Mn 0.3368 0.7283 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.4047(13) _cell_length_b 26.943(2) _cell_length_c 17.9892(15) _cell_angle_alpha 90.00 _cell_angle_beta 106.941(4) _cell_angle_gamma 90.00 _cell_volume 8069.8(11) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9967 _cell_measurement_theta_min 4.66 _cell_measurement_theta_max 52.0 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.108 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2810 _exptl_absorpt_coefficient_mu 0.477 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8624 _exptl_absorpt_correction_T_max 0.9539 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'ImuS MoK\a' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Bruker APEX II QUAZAR system equipped with a multilayer monochromator ; _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18521 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0671 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 27.54 _reflns_number_total 18521 _reflns_number_gt 14213 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1664P)^2^+20.3892P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constrained _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18521 _refine_ls_number_parameters 765 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1289 _refine_ls_R_factor_gt 0.0994 _refine_ls_wR_factor_ref 0.2919 _refine_ls_wR_factor_gt 0.2659 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2527(3) 0.76386(16) 0.0726(3) 0.0133(8) Uani 1 1 d . . . C2 C 0.3410(3) 0.74837(19) 0.1061(3) 0.0165(9) Uani 1 1 d . . . H2A H 0.3626 0.7620 0.1593 0.020 Uiso 1 1 calc R . . H2B H 0.3729 0.7624 0.0736 0.020 Uiso 1 1 calc R . . C3 C 0.3495(3) 0.69138(19) 0.1088(3) 0.0163(10) Uani 1 1 d . . . C4 C 0.2984(3) 0.6695(2) 0.1586(3) 0.0177(10) Uani 1 1 d . . . H4A H 0.3034 0.6329 0.1598 0.021 Uiso 1 1 calc R . . H4B H 0.3192 0.6818 0.2125 0.021 Uiso 1 1 calc R . . C5 C 0.2092(3) 0.6838(2) 0.1258(3) 0.0182(10) Uani 1 1 d . . . C6 C 0.1787(3) 0.66476(18) 0.0417(3) 0.0181(10) Uani 1 1 d . . . H6A H 0.1218 0.6744 0.0194 0.022 Uiso 1 1 calc R . . H6B H 0.1817 0.6281 0.0417 0.022 Uiso 1 1 calc R . . C7 C 0.2283(3) 0.68580(19) -0.0094(3) 0.0152(10) Uani 1 1 d . . . C8 C 0.2214(3) 0.74245(18) -0.0100(3) 0.0138(9) Uani 1 1 d . . . H8A H 0.1645 0.7521 -0.0328 0.017 Uiso 1 1 calc R . . H8B H 0.2526 0.7566 -0.0429 0.017 Uiso 1 1 calc R . . C9 C 0.3170(3) 0.6712(2) 0.0261(3) 0.0171(10) Uani 1 1 d . . . H9A H 0.3219 0.6346 0.0269 0.020 Uiso 1 1 calc R . . H9B H 0.3492 0.6846 -0.0065 0.020 Uiso 1 1 calc R . . C10 C 0.2038(3) 0.7411(2) 0.1234(3) 0.0181(10) Uani 1 1 d . . . H11A H 0.1469 0.7512 0.1025 0.022 Uiso 1 1 calc R . . H11B H 0.2242 0.7543 0.1769 0.022 Uiso 1 1 calc R . . C11 C 0.2428(3) 0.82025(18) 0.0697(3) 0.0151(9) Uani 1 1 d . . . C12 C 0.1668(3) 0.84077(19) 0.0371(3) 0.0166(10) Uani 1 1 d . . . H12 H 0.1219 0.8193 0.0192 0.020 Uiso 1 1 calc R . . C13 C 0.1554(3) 0.89124(19) 0.0302(3) 0.0173(10) Uani 1 1 d . . . H13 H 0.1030 0.9040 0.0069 0.021 Uiso 1 1 calc R . . C14 C 0.2201(3) 0.92409(18) 0.0574(3) 0.0174(9) Uani 1 1 d . . . C15 C 0.2955(3) 0.9037(2) 0.0902(4) 0.0255(12) Uani 1 1 d . . . H15 H 0.3404 0.9252 0.1085 0.031 Uiso 1 1 calc R . . C16 C 0.3071(3) 0.8527(2) 0.0970(4) 0.0239(12) Uani 1 1 d . . . H16 H 0.3594 0.8399 0.1204 0.029 Uiso 1 1 calc R . . C17 C 0.2116(3) 0.97836(18) 0.0482(3) 0.0173(10) Uani 1 1 d . . . C18 C 0.4368(3) 0.6784(2) 0.1487(3) 0.0217(11) Uani 1 1 d . . . C19 C 0.4842(4) 0.6519(3) 0.1143(4) 0.0390(17) Uani 1 1 d . . . H19 H 0.4619 0.6399 0.0628 0.047 Uiso 1 1 calc R . . C20 C 0.5653(4) 0.6421(4) 0.1536(5) 0.050(2) Uani 1 1 d . . . H20 H 0.5970 0.6236 0.1286 0.060 Uiso 1 1 calc R . . C21 C 0.5990(4) 0.6594(3) 0.2282(4) 0.0395(17) Uani 1 1 d . . . C22 C 0.5516(3) 0.6860(2) 0.2654(4) 0.0286(13) Uani 1 1 d . . . H22 H 0.5737 0.6973 0.3173 0.034 Uiso 1 1 calc R . . C23 C 0.4720(3) 0.6955(2) 0.2252(4) 0.0268(12) Uani 1 1 d . . . H23 H 0.4402 0.7141 0.2501 0.032 Uiso 1 1 calc R . . C24 C 0.6852(4) 0.6542(3) 0.2700(4) 0.0378(15) Uani 1 1 d . . . C25 C 0.1631(3) 0.6618(2) 0.1772(3) 0.0200(11) Uani 1 1 d . . . C26 C 0.1300(5) 0.6908(3) 0.2229(5) 0.050(2) Uani 1 1 d . . . H26 H 0.1325 0.7259 0.2192 0.060 Uiso 1 1 calc R . . C27 C 0.0927(6) 0.6700(3) 0.2745(5) 0.054(2) Uani 1 1 d . . . H27 H 0.0732 0.6910 0.3074 0.065 Uiso 1 1 calc R . . C28 C 0.0841(3) 0.6196(2) 0.2781(3) 0.0241(11) Uani 1 1 d . . . C29 C 0.1181(4) 0.5902(3) 0.2334(4) 0.0366(15) Uani 1 1 d . . . H29 H 0.1146 0.5551 0.2368 0.044 Uiso 1 1 calc R . . C30 C 0.1573(4) 0.6106(2) 0.1836(4) 0.0334(14) Uani 1 1 d . . . H30 H 0.1803 0.5894 0.1536 0.040 Uiso 1 1 calc R . . C31 C 0.0416(3) 0.6006(2) 0.3319(3) 0.0213(11) Uani 1 1 d . . . C32 C 0.1931(3) 0.6645(2) -0.0916(3) 0.0201(11) Uani 1 1 d . . . C33 C 0.1579(4) 0.6947(2) -0.1549(4) 0.0309(13) Uani 1 1 d . . . H33 H 0.1604 0.7297 -0.1481 0.037 Uiso 1 1 calc R . . C34 C 0.1191(4) 0.6754(2) -0.2279(4) 0.0318(14) Uani 1 1 d . . . H34 H 0.0956 0.6970 -0.2701 0.038 Uiso 1 1 calc R . . C35 C 0.1149(3) 0.6238(2) -0.2387(3) 0.0204(10) Uani 1 1 d . . . C36 C 0.1542(4) 0.5936(2) -0.1766(4) 0.0328(14) Uani 1 1 d . . . H36 H 0.1542 0.5587 -0.1840 0.039 Uiso 1 1 calc R . . C37 C 0.1930(4) 0.6130(2) -0.1046(3) 0.0282(13) Uani 1 1 d . . . H37 H 0.2199 0.5914 -0.0634 0.034 Uiso 1 1 calc R . . C38 C 0.0673(3) 0.6056(2) -0.3148(3) 0.0231(11) Uani 1 1 d . . . C40 C 0.3544(14) 1.2252(10) 0.0253(14) 0.075(6) Uiso 0.50 1 d P . . C41 C 0.324(2) 1.3083(14) -0.026(2) 0.122(11) Uiso 0.50 1 d P . . C43 C 0.4554(4) 1.0447(3) 0.1376(4) 0.0363(15) Uani 1 1 d . . . H43 H 0.4260 1.0215 0.1003 0.044 Uiso 1 1 calc R . . C44 C 0.5440(6) 0.9761(4) 0.1965(7) 0.067(3) Uani 1 1 d . . . H44A H 0.5407 0.9622 0.2458 0.101 Uiso 1 1 calc R . . H44B H 0.5995 0.9742 0.1944 0.101 Uiso 1 1 calc R . . H44C H 0.5090 0.9572 0.1532 0.101 Uiso 1 1 calc R . . C45 C 0.5724(7) 1.0623(4) 0.2446(6) 0.082(4) Uani 1 1 d . . . H45A H 0.5511 1.0961 0.2351 0.123 Uiso 1 1 calc R . . H45B H 0.6257 1.0610 0.2366 0.123 Uiso 1 1 calc R . . H45C H 0.5766 1.0527 0.2982 0.123 Uiso 1 1 calc R . . C49 C 0.6544(11) 0.3051(7) 0.1885(11) 0.118(5) Uiso 1 1 d . . . C50 C 0.5171(14) 0.3121(9) 0.1050(14) 0.157(8) Uiso 1 1 d . . . C51 C 0.6144(15) 0.3833(9) 0.1764(16) 0.165(8) Uiso 1 1 d . . . C52 C 0.1829(16) 0.4622(11) 0.3390(17) 0.175(9) Uiso 1 1 d . . . C53 C 0.1901(15) 0.4617(10) 0.1895(16) 0.167(9) Uiso 1 1 d . . . C54 C 0.0709(15) 0.4531(9) 0.2344(15) 0.162(8) Uiso 1 1 d . . . C55 C 0.7601(12) 0.5236(8) 0.2580(12) 0.130(6) Uiso 1 1 d . . . C56 C 0.8661(11) 0.5470(7) 0.2191(12) 0.131(6) Uiso 1 1 d . . . C57 C 0.7324(16) 0.5264(10) 0.1127(15) 0.160(8) Uiso 1 1 d . . . C63 C 0.6306(19) 0.8068(13) 0.2143(19) 0.105(9) Uiso 0.50 1 d P . . C64 C 0.698(3) 0.847(2) 0.207(3) 0.182(19) Uiso 0.50 1 d P . . C65 C 0.6615(14) 0.8847(9) 0.1862(15) 0.076(6) Uiso 0.50 1 d P . . C66 C 0.690(3) 0.8106(17) 0.274(3) 0.142(14) Uiso 0.50 1 d P . . C72 C -0.0863(15) 0.7749(10) 0.2679(16) 0.033(5) Uiso 0.25 1 d P . . C73 C -0.100(2) 0.7521(16) 0.198(2) 0.065(10) Uiso 0.25 1 d P . . C74 C -0.090(4) 0.715(3) 0.139(4) 0.12(2) Uiso 0.25 1 d P . . C75 C -0.092(4) 0.663(3) 0.122(4) 0.12(2) Uiso 0.25 1 d P . . N1 N 0.1436(2) 1.00579(15) 0.0322(3) 0.0155(8) Uani 1 1 d . . . N2 N 0.1696(2) 1.05235(16) 0.0327(2) 0.0168(9) Uani 1 1 d . . . N3 N 0.2481(2) 1.05292(16) 0.0488(3) 0.0199(9) Uani 1 1 d . . . N4 N 0.2765(3) 1.00720(17) 0.0596(3) 0.0223(10) Uani 1 1 d . . . N5 N 0.7156(3) 0.6468(2) 0.3451(3) 0.0304(12) Uani 1 1 d . . . N6 N 0.7962(3) 0.6471(3) 0.3588(4) 0.0390(14) Uani 1 1 d . . . N7 N 0.8112(4) 0.6531(4) 0.2908(4) 0.064(2) Uani 1 1 d . . . N8 N 0.7429(4) 0.6586(3) 0.2360(4) 0.058(2) Uani 1 1 d . . . N9 N -0.0049(3) 0.62928(19) 0.3604(3) 0.0246(10) Uani 1 1 d . . . N10 N -0.0325(3) 0.59935(19) 0.4056(3) 0.0222(10) Uani 1 1 d . . . N11 N -0.0035(3) 0.55503(17) 0.4048(3) 0.0195(9) Uani 1 1 d . . . N12 N 0.0447(3) 0.55344(18) 0.3585(3) 0.0221(10) Uani 1 1 d . . . N13 N 0.0701(3) 0.55929(18) -0.3418(3) 0.0196(9) Uani 1 1 d . . . N14 N 0.0136(3) 0.55980(18) -0.4111(3) 0.0204(9) Uani 1 1 d . . . N15 N -0.0204(3) 0.6043(2) -0.4235(3) 0.0242(10) Uani 1 1 d . . . N16 N 0.0119(3) 0.6337(2) -0.3638(3) 0.0262(11) Uani 1 1 d . . . N40 N 0.3683(17) 1.2652(11) -0.0179(17) 0.118(8) Uiso 0.50 1 d P . . N43 N 0.5182(4) 1.0280(3) 0.1906(4) 0.0520(18) Uani 1 1 d . . . N49 N 0.5953(9) 0.3298(6) 0.1575(9) 0.120(4) Uiso 1 1 d . . . N52 N 0.1520(8) 0.4537(5) 0.2592(8) 0.107(4) Uiso 1 1 d . . . N53 N 0.7801(8) 0.5343(5) 0.1944(9) 0.112(4) Uiso 1 1 d . . . Cl1 Cl -0.20507(15) 0.65650(12) -0.4570(2) 0.0871(9) Uani 1 1 d . . . Mn1 Mn 0.32642(5) 1.12117(3) 0.05270(6) 0.0270(2) Uani 1 1 d . . . Mn2 Mn -0.11245(5) 0.62949(3) -0.52904(6) 0.0232(2) Uani 1 1 d . . . Mn3 Mn 0.0000 0.5000 0.5000 0.0125(2) Uani 1 2 d S . . O1 O 0.3836(3) 1.1907(2) 0.0409(4) 0.0501(14) Uani 1 1 d . . . O2A O -0.058(2) 0.7018(13) -0.504(3) 0.083(13) Uani 0.468(17) 1 d P . . O3 O 0.4306(2) 1.08777(17) 0.1314(3) 0.0356(10) Uani 1 1 d . . . O5 O 0.6468(10) 0.2600(7) 0.1708(11) 0.191(6) Uiso 1 1 d . . . O6 O 0.3695(3) 1.0902(2) -0.0416(3) 0.0544(15) Uani 1 1 d . . . O7 O 0.2783(16) 0.4744(10) 0.3577(16) 0.140(8) Uiso 0.50 1 d P . . O8 O 0.6620(16) 0.5146(9) 0.1111(15) 0.247(10) Uiso 1 1 d . . . O11 O 0.2722(6) 0.5320(4) 0.0734(7) 0.107(3) Uiso 1 1 d . . . O12 O 0.0000 0.5000 0.0000 0.127(10) Uiso 0.50 2 d SP . . C20A C -0.0612(12) 0.7295(9) -0.5822(13) 0.070(6) Uiso 0.532(17) 1 d P . 1 C22A C -0.064(3) 0.7987(16) -0.5052(19) 0.159(15) Uiso 0.532(17) 1 d PD . 1 N20A N -0.0521(11) 0.7789(7) -0.5720(11) 0.076(6) Uiso 0.532(17) 1 d PD . 1 O2B O -0.067(2) 0.7027(10) -0.531(2) 0.088(12) Uani 0.532(17) 1 d P . 1 C21A C -0.0522 0.8124 -0.6312 0.217(19) Uiso 0.70(2) 1 d P . 1 C46A C 0.3355(14) 0.5685(9) 0.4142(14) 0.038(6) Uiso 0.303(15) 1 d P A 2 C46B C 0.4584(19) 0.5945(15) 0.501(2) 0.056(8) Uiso 0.303(15) 1 d P A 2 O4A O 0.443(5) 0.619(3) 0.480(5) 0.21(3) Uiso 0.303(15) 1 d P A 2 C46 C 0.4061(7) 0.5611(5) 0.4659(7) 0.049(3) Uiso 0.697(15) 1 d P A 3 C47 C 0.4239(13) 0.6470(9) 0.4400(13) 0.092(6) Uiso 0.697(15) 1 d P A 3 C48 C 0.2964(10) 0.6178(7) 0.3906(10) 0.075(5) Uiso 0.697(15) 1 d P A 3 N46 N 0.3742(7) 0.6061(4) 0.4305(7) 0.058(3) Uiso 0.697(15) 1 d P A 3 O4 O 0.4746(9) 0.5590(6) 0.5083(9) 0.102(5) Uiso 0.697(15) 1 d P A 3 C42 C 0.4058 1.2480 -0.0812 0.14(3) Uiso 0.25 1 d P . . C76 C -0.060(2) 0.7529(15) 0.341(2) 0.060(9) Uiso 0.25 1 d P . . 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 C1 0.0150(19) 0.009(2) 0.013(2) -0.001(2) 0.0000(18) 0.0001(15) C2 0.0155(19) 0.020(2) 0.010(2) 0.0013(19) -0.0018(17) 0.0012(18) C3 0.020(2) 0.015(2) 0.013(2) 0.0036(19) 0.0029(18) 0.0015(17) C4 0.029(2) 0.012(2) 0.010(2) 0.0069(19) 0.0026(19) 0.0001(19) C5 0.021(2) 0.020(3) 0.015(2) 0.000(2) 0.0076(19) -0.002(2) C6 0.029(2) 0.009(2) 0.017(2) -0.003(2) 0.008(2) -0.0033(18) C7 0.022(2) 0.010(2) 0.012(2) 0.0005(19) 0.0041(18) -0.0014(18) C8 0.019(2) 0.010(2) 0.011(2) 0.0012(18) 0.0014(17) 0.0004(17) C9 0.025(2) 0.013(2) 0.014(2) 0.0013(19) 0.0062(19) 0.0022(19) C10 0.023(2) 0.016(3) 0.016(2) 0.001(2) 0.0069(19) 0.0004(19) C11 0.018(2) 0.015(2) 0.011(2) -0.001(2) 0.0017(19) -0.0014(16) C12 0.0133(19) 0.016(2) 0.019(2) 0.000(2) 0.0019(18) -0.0008(16) C13 0.015(2) 0.015(2) 0.019(3) 0.000(2) -0.0012(18) 0.0017(17) C14 0.019(2) 0.014(2) 0.018(2) -0.002(2) 0.0034(19) -0.0003(17) C15 0.016(2) 0.016(2) 0.036(3) 0.002(3) -0.005(2) -0.0009(18) C16 0.015(2) 0.017(3) 0.032(3) -0.001(2) -0.004(2) 0.0003(18) C17 0.0147(19) 0.014(2) 0.020(3) -0.009(2) 0.0004(18) -0.0005(17) C18 0.024(2) 0.016(3) 0.023(3) 0.007(2) 0.005(2) 0.005(2) C19 0.034(3) 0.061(5) 0.019(3) 0.002(3) 0.003(2) 0.017(3) C20 0.033(3) 0.085(6) 0.033(4) 0.011(4) 0.012(3) 0.025(4) C21 0.024(3) 0.054(5) 0.040(4) 0.019(3) 0.009(3) 0.015(3) C22 0.028(3) 0.029(3) 0.025(3) 0.007(2) 0.000(2) 0.004(2) C23 0.026(3) 0.021(3) 0.029(3) 0.002(2) 0.000(2) 0.005(2) C24 0.029(3) 0.048(4) 0.034(4) 0.012(3) 0.007(3) 0.005(3) C25 0.025(2) 0.018(3) 0.017(2) 0.007(2) 0.006(2) 0.000(2) C26 0.085(6) 0.021(3) 0.065(5) -0.003(3) 0.058(5) -0.011(4) C27 0.100(7) 0.021(3) 0.066(5) -0.001(4) 0.063(5) -0.006(4) C28 0.026(2) 0.026(3) 0.020(3) 0.004(2) 0.006(2) -0.005(2) C29 0.049(4) 0.029(3) 0.035(4) 0.001(3) 0.018(3) -0.010(3) C30 0.054(4) 0.022(3) 0.031(3) 0.000(3) 0.021(3) -0.001(3) C31 0.026(2) 0.015(3) 0.021(3) 0.007(2) 0.004(2) -0.001(2) C32 0.025(2) 0.019(3) 0.015(2) 0.002(2) 0.004(2) -0.001(2) C33 0.046(3) 0.017(3) 0.025(3) 0.003(2) 0.004(3) -0.005(2) C34 0.052(4) 0.019(3) 0.018(3) 0.005(2) 0.001(3) -0.004(3) C35 0.028(2) 0.018(3) 0.013(2) -0.004(2) 0.002(2) -0.003(2) C36 0.048(4) 0.019(3) 0.026(3) -0.009(3) 0.003(3) 0.004(3) C37 0.043(3) 0.018(3) 0.018(3) 0.000(2) 0.000(2) 0.008(2) C38 0.027(3) 0.024(3) 0.017(3) -0.002(2) 0.005(2) -0.006(2) C43 0.035(3) 0.029(3) 0.040(4) -0.003(3) 0.003(3) 0.000(2) C44 0.067(6) 0.044(5) 0.074(6) -0.011(5) -0.006(5) 0.011(4) C45 0.089(7) 0.063(7) 0.059(6) -0.011(5) -0.033(5) 0.023(6) N1 0.0169(17) 0.0108(19) 0.018(2) -0.0025(17) 0.0041(16) -0.0021(14) N2 0.0167(18) 0.015(2) 0.016(2) -0.0009(16) 0.0016(15) -0.0014(15) N3 0.0178(18) 0.012(2) 0.029(3) -0.0020(17) 0.0062(17) 0.0002(15) N4 0.021(2) 0.014(2) 0.029(3) 0.0022(18) 0.0031(17) 0.0012(16) N5 0.023(2) 0.029(3) 0.038(3) 0.013(2) 0.006(2) 0.005(2) N6 0.023(2) 0.052(4) 0.041(3) 0.017(3) 0.007(2) 0.007(2) N7 0.036(3) 0.111(7) 0.052(4) 0.040(5) 0.021(3) 0.019(4) N8 0.032(3) 0.085(6) 0.053(4) 0.027(4) 0.005(3) 0.011(3) N9 0.026(2) 0.020(2) 0.030(3) 0.010(2) 0.011(2) -0.0005(18) N10 0.020(2) 0.022(3) 0.023(2) 0.012(2) 0.0039(18) 0.0032(18) N11 0.023(2) 0.020(2) 0.017(2) 0.0031(18) 0.0073(17) -0.0069(18) N12 0.028(2) 0.021(3) 0.017(2) 0.0028(19) 0.0070(18) -0.0046(18) N13 0.023(2) 0.019(2) 0.014(2) -0.0046(18) 0.0030(17) -0.0040(17) N14 0.024(2) 0.021(2) 0.015(2) -0.0046(18) 0.0045(17) -0.0059(17) N15 0.025(2) 0.024(3) 0.021(2) -0.007(2) 0.0013(18) 0.0006(18) N16 0.026(2) 0.026(3) 0.024(2) -0.006(2) 0.0021(19) 0.0000(19) N43 0.040(3) 0.042(4) 0.058(4) -0.013(3) -0.010(3) 0.009(3) Cl1 0.0459(12) 0.084(2) 0.123(3) -0.0081(19) 0.0112(14) 0.0110(12) Mn1 0.0236(4) 0.0255(5) 0.0304(5) -0.0004(4) 0.0055(4) -0.0045(3) Mn2 0.0194(3) 0.0181(4) 0.0290(4) 0.0035(4) 0.0023(4) 0.0007(3) Mn3 0.0156(4) 0.0116(4) 0.0089(4) 0.0004(4) 0.0014(4) -0.0018(3) O1 0.047(3) 0.039(3) 0.059(4) 0.015(3) 0.007(3) -0.010(2) O2A 0.044(9) 0.052(18) 0.16(3) -0.07(2) 0.039(14) -0.015(9) O3 0.0277(19) 0.033(2) 0.043(3) -0.006(2) 0.0048(19) 0.0032(17) O6 0.047(3) 0.066(4) 0.054(3) -0.014(3) 0.021(3) -0.014(3) O2B 0.085(16) 0.026(11) 0.15(3) 0.019(15) 0.037(17) -0.015(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C11 1.528(6) . ? C1 C2 1.537(6) . ? C1 C8 1.538(7) . ? C1 C10 1.546(7) . ? C2 C3 1.542(7) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C18 1.520(7) . ? C3 C9 1.530(7) . ? C3 C4 1.551(7) . ? C4 C5 1.540(7) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C25 1.509(7) . ? C5 C6 1.538(7) . ? C5 C10 1.548(8) . ? C6 C7 1.541(7) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.531(7) . ? C7 C32 1.537(7) . ? C7 C9 1.540(7) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H11A 0.9900 . ? C10 H11B 0.9900 . ? C11 C16 1.392(7) . ? C11 C12 1.396(6) . ? C12 C13 1.375(7) . ? C12 H12 0.9500 . ? C13 C14 1.404(7) . ? C13 H13 0.9500 . ? C14 C15 1.386(7) . ? C14 C17 1.474(7) . ? C15 C16 1.389(8) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 N4 1.337(6) . ? C17 N1 1.353(6) . ? C18 C19 1.368(9) . ? C18 C23 1.412(8) . ? C19 C20 1.407(9) . ? C19 H19 0.9500 . ? C20 C21 1.379(12) . ? C20 H20 0.9500 . ? C21 C22 1.401(10) . ? C21 C24 1.476(9) . ? C22 C23 1.387(8) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 N5 1.313(9) . ? C24 N8 1.324(9) . ? C25 C26 1.376(9) . ? C25 C30 1.391(9) . ? C26 C27 1.395(10) . ? C26 H26 0.9500 . ? C27 C28 1.372(9) . ? C27 H27 0.9500 . ? C28 C29 1.378(9) . ? C28 C31 1.470(8) . ? C29 C30 1.388(9) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 N9 1.326(8) . ? C31 N12 1.353(7) . ? C32 C33 1.387(8) . ? C32 C37 1.408(8) . ? C33 C34 1.390(9) . ? C33 H33 0.9500 . ? C34 C35 1.403(8) . ? C34 H34 0.9500 . ? C35 C36 1.390(9) . ? C35 C38 1.461(7) . ? C36 C37 1.377(8) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C38 N16 1.336(8) . ? C38 N13 1.345(8) . ? C40 O1 1.06(3) . ? C40 N40 1.39(4) . ? C41 N40 1.38(4) . ? C43 O3 1.232(8) . ? C43 N43 1.304(9) . ? C43 H43 0.9500 . ? C44 N43 1.461(11) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 N43 1.468(12) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C49 N49 1.22(2) . ? C49 O5 1.25(2) . ? C50 N49 1.49(3) . ? C51 N49 1.50(3) . ? C52 N52 1.40(3) . ? C52 O7 1.63(3) . ? C53 N52 1.60(3) . ? C54 N52 1.35(2) . ? C55 N53 1.32(2) . ? C56 N53 1.47(2) . ? C57 O8 1.26(3) . ? C57 N53 1.48(3) . ? C63 C66 1.26(5) . ? C63 C64 1.63(6) . ? C64 C65 1.20(5) . ? C64 C66 1.58(7) . ? C72 C73 1.35(5) . ? C72 C76 1.39(5) . ? C72 C21A 2.01(3) 1_556 ? C73 C74 1.51(8) . ? C74 C75 1.44(9) . ? N1 N2 1.333(6) . ? N1 Mn3 2.401(4) 2 ? N2 N3 1.310(6) . ? N2 Mn2 2.297(4) 2_554 ? N3 N4 1.321(6) . ? N3 Mn1 2.278(4) . ? N5 N6 1.351(7) . ? N5 Mn1 2.276(6) 2_645 ? N6 N7 1.333(9) . ? N6 Mn2 2.226(6) 1_656 ? N7 N8 1.314(9) . ? N9 N10 1.330(7) . ? N10 N11 1.298(7) . ? N10 Mn2 2.221(5) 1_556 ? N11 N12 1.344(6) . ? N11 Mn3 2.253(4) . ? N13 N14 1.345(6) . ? N14 N15 1.327(7) . ? N14 Mn3 2.233(5) 1_554 ? N15 N16 1.321(7) . ? N15 Mn2 2.204(5) . ? N40 C42 1.54(3) . ? Cl1 Mn2 2.454(3) . ? Cl1 Mn1 2.492(3) 2_544 ? Mn1 O3 2.146(5) . ? Mn1 O1 2.160(5) . ? Mn1 O6 2.209(6) . ? Mn1 N5 2.276(6) 2_655 ? Mn1 Cl1 2.492(3) 2_554 ? Mn2 O2B 2.13(3) . ? Mn2 O2A 2.15(3) . ? Mn2 N10 2.221(5) 1_554 ? Mn2 N6 2.226(6) 1_454 ? Mn2 N2 2.297(4) 2_544 ? Mn3 N14 2.233(5) 1_556 ? Mn3 N14 2.233(5) 3_565 ? Mn3 N11 2.253(4) 3_566 ? Mn3 N1 2.401(4) 2_545 ? Mn3 N1 2.401(4) 4_576 ? O2A C20A 1.58(5) . ? C20A O2B 1.19(4) . ? C20A N20A 1.35(3) . ? C20A C76 1.52(5) 1_554 ? C22A N20A 1.385(19) . ? N20A C21A 1.395(19) . ? N20A C76 1.68(4) 1_554 ? C21A C76 1.67(4) 1_554 ? C21A C72 2.01(3) 1_554 ? C46B O4A 0.77(9) . ? C46 O4 1.216(18) . ? C46 N46 1.406(17) . ? C47 N46 1.38(2) . ? C48 N46 1.37(2) . ? C76 C20A 1.52(5) 1_556 ? C76 C21A 1.67(4) 1_556 ? C76 N20A 1.68(4) 1_556 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 C1 C2 111.9(4) . . ? C11 C1 C8 109.6(4) . . ? C2 C1 C8 108.1(4) . . ? C11 C1 C10 109.8(4) . . ? C2 C1 C10 108.7(4) . . ? C8 C1 C10 108.8(4) . . ? C1 C2 C3 111.0(4) . . ? C1 C2 H2A 109.4 . . ? C3 C2 H2A 109.4 . . ? C1 C2 H2B 109.4 . . ? C3 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? C18 C3 C9 114.4(4) . . ? C18 C3 C2 108.5(4) . . ? C9 C3 C2 108.6(4) . . ? C18 C3 C4 107.7(4) . . ? C9 C3 C4 108.3(4) . . ? C2 C3 C4 109.3(4) . . ? C5 C4 C3 111.6(4) . . ? C5 C4 H4A 109.3 . . ? C3 C4 H4A 109.3 . . ? C5 C4 H4B 109.3 . . ? C3 C4 H4B 109.3 . . ? H4A C4 H4B 108.0 . . ? C25 C5 C6 112.3(4) . . ? C25 C5 C4 108.9(4) . . ? C6 C5 C4 108.2(4) . . ? C25 C5 C10 111.7(4) . . ? C6 C5 C10 107.7(4) . . ? C4 C5 C10 107.8(4) . . ? C5 C6 C7 111.9(4) . . ? C5 C6 H6A 109.2 . . ? C7 C6 H6A 109.2 . . ? C5 C6 H6B 109.2 . . ? C7 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? C8 C7 C32 110.9(4) . . ? C8 C7 C9 109.0(4) . . ? C32 C7 C9 111.9(4) . . ? C8 C7 C6 108.3(4) . . ? C32 C7 C6 107.6(4) . . ? C9 C7 C6 109.0(4) . . ? C7 C8 C1 111.2(4) . . ? C7 C8 H8A 109.4 . . ? C1 C8 H8A 109.4 . . ? C7 C8 H8B 109.4 . . ? C1 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? C3 C9 C7 110.8(4) . . ? C3 C9 H9A 109.5 . . ? C7 C9 H9A 109.5 . . ? C3 C9 H9B 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? C1 C10 C5 111.9(4) . . ? C1 C10 H11A 109.2 . . ? C5 C10 H11A 109.2 . . ? C1 C10 H11B 109.2 . . ? C5 C10 H11B 109.2 . . ? H11A C10 H11B 107.9 . . ? C16 C11 C12 117.7(5) . . ? C16 C11 C1 122.9(4) . . ? C12 C11 C1 119.4(4) . . ? C13 C12 C11 121.6(4) . . ? C13 C12 H12 119.2 . . ? C11 C12 H12 119.2 . . ? C12 C13 C14 120.8(4) . . ? C12 C13 H13 119.6 . . ? C14 C13 H13 119.6 . . ? C15 C14 C13 117.6(5) . . ? C15 C14 C17 119.4(4) . . ? C13 C14 C17 122.9(4) . . ? C14 C15 C16 121.6(5) . . ? C14 C15 H15 119.2 . . ? C16 C15 H15 119.2 . . ? C15 C16 C11 120.7(4) . . ? C15 C16 H16 119.7 . . ? C11 C16 H16 119.7 . . ? N4 C17 N1 111.3(4) . . ? N4 C17 C14 120.5(4) . . ? N1 C17 C14 128.2(4) . . ? C19 C18 C23 117.6(5) . . ? C19 C18 C3 124.0(5) . . ? C23 C18 C3 118.4(5) . . ? C18 C19 C20 121.3(6) . . ? C18 C19 H19 119.4 . . ? C20 C19 H19 119.4 . . ? C21 C20 C19 120.4(7) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C20 C21 C22 119.7(6) . . ? C20 C21 C24 123.1(6) . . ? C22 C21 C24 117.1(7) . . ? C23 C22 C21 118.9(6) . . ? C23 C22 H22 120.6 . . ? C21 C22 H22 120.6 . . ? C22 C23 C18 122.1(6) . . ? C22 C23 H23 118.9 . . ? C18 C23 H23 118.9 . . ? N5 C24 N8 110.8(6) . . ? N5 C24 C21 125.7(6) . . ? N8 C24 C21 123.4(6) . . ? C26 C25 C30 117.4(5) . . ? C26 C25 C5 122.2(5) . . ? C30 C25 C5 120.3(5) . . ? C25 C26 C27 121.8(7) . . ? C25 C26 H26 119.1 . . ? C27 C26 H26 119.1 . . ? C28 C27 C26 120.6(7) . . ? C28 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? C27 C28 C29 117.9(6) . . ? C27 C28 C31 117.4(6) . . ? C29 C28 C31 124.6(6) . . ? C28 C29 C30 121.7(6) . . ? C28 C29 H29 119.1 . . ? C30 C29 H29 119.1 . . ? C29 C30 C25 120.5(6) . . ? C29 C30 H30 119.8 . . ? C25 C30 H30 119.8 . . ? N9 C31 N12 112.1(5) . . ? N9 C31 C28 122.2(5) . . ? N12 C31 C28 125.7(5) . . ? C33 C32 C37 117.6(5) . . ? C33 C32 C7 121.8(5) . . ? C37 C32 C7 120.5(5) . . ? C32 C33 C34 122.2(6) . . ? C32 C33 H33 118.9 . . ? C34 C33 H33 118.9 . . ? C33 C34 C35 119.6(6) . . ? C33 C34 H34 120.2 . . ? C35 C34 H34 120.2 . . ? C36 C35 C34 118.3(5) . . ? C36 C35 C38 124.7(5) . . ? C34 C35 C38 117.1(5) . . ? C37 C36 C35 121.8(6) . . ? C37 C36 H36 119.1 . . ? C35 C36 H36 119.1 . . ? C36 C37 C32 120.4(6) . . ? C36 C37 H37 119.8 . . ? C32 C37 H37 119.8 . . ? N16 C38 N13 112.4(5) . . ? N16 C38 C35 122.1(5) . . ? N13 C38 C35 125.4(5) . . ? O1 C40 N40 133(2) . . ? O3 C43 N43 126.1(7) . . ? O3 C43 H43 116.9 . . ? N43 C43 H43 116.9 . . ? N43 C44 H44A 109.5 . . ? N43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? N43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N43 C45 H45A 109.5 . . ? N43 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? N43 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? N49 C49 O5 113.7(19) . . ? N52 C52 O7 108(2) . . ? O8 C57 N53 109(2) . . ? C66 C63 C64 65(3) . . ? C65 C64 C66 127(5) . . ? C65 C64 C63 105(4) . . ? C66 C64 C63 46(2) . . ? C63 C66 C64 69(3) . . ? C73 C72 C76 127(3) . . ? C73 C72 C21A 172(2) . 1_556 ? C76 C72 C21A 55.4(19) . 1_556 ? C72 C73 C74 158(4) . . ? C75 C74 C73 142(6) . . ? N2 N1 C17 103.8(4) . . ? N2 N1 Mn3 113.0(3) . 2 ? C17 N1 Mn3 143.2(3) . 2 ? N3 N2 N1 110.0(4) . . ? N3 N2 Mn2 114.2(3) . 2_554 ? N1 N2 Mn2 135.1(3) . 2_554 ? N2 N3 N4 110.1(4) . . ? N2 N3 Mn1 126.3(3) . . ? N4 N3 Mn1 123.5(3) . . ? N3 N4 C17 104.8(4) . . ? C24 N5 N6 105.9(5) . . ? C24 N5 Mn1 138.4(4) . 2_645 ? N6 N5 Mn1 114.5(4) . 2_645 ? N7 N6 N5 107.7(5) . . ? N7 N6 Mn2 125.3(4) . 1_656 ? N5 N6 Mn2 126.5(4) . 1_656 ? N8 N7 N6 109.0(6) . . ? N7 N8 C24 106.6(7) . . ? C31 N9 N10 104.6(5) . . ? N11 N10 N9 109.9(5) . . ? N11 N10 Mn2 130.4(4) . 1_556 ? N9 N10 Mn2 119.7(4) . 1_556 ? N10 N11 N12 110.6(4) . . ? N10 N11 Mn3 121.4(3) . . ? N12 N11 Mn3 124.5(4) . . ? N11 N12 C31 102.8(5) . . ? N14 N13 C38 103.4(4) . . ? N15 N14 N13 109.5(4) . . ? N15 N14 Mn3 125.7(4) . 1_554 ? N13 N14 Mn3 123.6(4) . 1_554 ? N16 N15 N14 110.0(5) . . ? N16 N15 Mn2 123.1(4) . . ? N14 N15 Mn2 126.8(4) . . ? N15 N16 C38 104.6(5) . . ? C41 N40 C40 122(3) . . ? C41 N40 C42 121(3) . . ? C40 N40 C42 111(2) . . ? C43 N43 C44 123.9(7) . . ? C43 N43 C45 120.4(7) . . ? C44 N43 C45 115.5(7) . . ? C49 N49 C50 127.5(18) . . ? C49 N49 C51 108.8(18) . . ? C50 N49 C51 123.7(17) . . ? C54 N52 C52 113.2(18) . . ? C54 N52 C53 112.1(18) . . ? C52 N52 C53 131.4(17) . . ? C55 N53 C56 106.9(16) . . ? C55 N53 C57 128.0(17) . . ? C56 N53 C57 124.2(16) . . ? Mn2 Cl1 Mn1 94.41(13) . 2_544 ? O3 Mn1 O1 95.9(2) . . ? O3 Mn1 O6 86.4(2) . . ? O1 Mn1 O6 89.0(2) . . ? O3 Mn1 N5 90.17(19) . 2_655 ? O1 Mn1 N5 94.7(2) . 2_655 ? O6 Mn1 N5 175.2(2) . 2_655 ? O3 Mn1 N3 93.72(17) . . ? O1 Mn1 N3 170.28(19) . . ? O6 Mn1 N3 90.37(19) . . ? N5 Mn1 N3 86.52(18) 2_655 . ? O3 Mn1 Cl1 177.25(16) . 2_554 ? O1 Mn1 Cl1 85.60(17) . 2_554 ? O6 Mn1 Cl1 91.31(19) . 2_554 ? N5 Mn1 Cl1 91.99(17) 2_655 2_554 ? N3 Mn1 Cl1 84.72(13) . 2_554 ? O2B Mn2 O2A 12(2) . . ? O2B Mn2 N15 96.9(11) . . ? O2A Mn2 N15 86.3(13) . . ? O2B Mn2 N10 92.0(10) . 1_554 ? O2A Mn2 N10 97.8(9) . 1_554 ? N15 Mn2 N10 86.20(16) . 1_554 ? O2B Mn2 N6 87.6(11) . 1_454 ? O2A Mn2 N6 98.6(13) . 1_454 ? N15 Mn2 N6 173.9(2) . 1_454 ? N10 Mn2 N6 89.4(2) 1_554 1_454 ? O2B Mn2 N2 176.1(11) . 2_544 ? O2A Mn2 N2 169.8(13) . 2_544 ? N15 Mn2 N2 86.89(17) . 2_544 ? N10 Mn2 N2 89.26(17) 1_554 2_544 ? N6 Mn2 N2 88.7(2) 1_454 2_544 ? O2B Mn2 Cl1 92.4(10) . . ? O2A Mn2 Cl1 86.5(9) . . ? N15 Mn2 Cl1 93.47(15) . . ? N10 Mn2 Cl1 175.67(15) 1_554 . ? N6 Mn2 Cl1 90.55(17) 1_454 . ? N2 Mn2 Cl1 86.42(13) 2_544 . ? N14 Mn3 N14 180.00(17) 1_556 3_565 ? N14 Mn3 N11 92.47(17) 1_556 . ? N14 Mn3 N11 87.53(17) 3_565 . ? N14 Mn3 N11 87.53(17) 1_556 3_566 ? N14 Mn3 N11 92.47(17) 3_565 3_566 ? N11 Mn3 N11 180.00(18) . 3_566 ? N14 Mn3 N1 90.66(15) 1_556 2_545 ? N14 Mn3 N1 89.34(15) 3_565 2_545 ? N11 Mn3 N1 88.73(15) . 2_545 ? N11 Mn3 N1 91.27(15) 3_566 2_545 ? N14 Mn3 N1 89.34(15) 1_556 4_576 ? N14 Mn3 N1 90.66(15) 3_565 4_576 ? N11 Mn3 N1 91.27(15) . 4_576 ? N11 Mn3 N1 88.73(15) 3_566 4_576 ? N1 Mn3 N1 180.0 2_545 4_576 ? C40 O1 Mn1 126.0(14) . . ? C20A O2A Mn2 110(2) . . ? C43 O3 Mn1 131.4(4) . . ? O2B C20A N20A 122(3) . . ? O2B C20A C76 166(3) . 1_554 ? N20A C20A C76 71(2) . 1_554 ? O2B C20A O2A 11(3) . . ? N20A C20A O2A 112(2) . . ? C76 C20A O2A 176(3) 1_554 . ? C20A N20A C22A 117(3) . . ? C20A N20A C21A 124.1(17) . . ? C22A N20A C21A 117(2) . . ? C20A N20A C76 59.2(18) . 1_554 ? C22A N20A C76 167(3) . 1_554 ? C21A N20A C76 65.0(16) . 1_554 ? C20A O2B Mn2 134(3) . . ? N20A C21A C76 65.9(16) . 1_554 ? N20A C21A C72 107.4(11) . 1_554 ? C76 C21A C72 43.2(16) 1_554 1_554 ? O4 C46 N46 120.7(13) . . ? C48 N46 C47 111.7(15) . . ? C48 N46 C46 129.3(13) . . ? C47 N46 C46 118.8(14) . . ? C72 C76 C20A 161(3) . 1_556 ? C72 C76 C21A 81(2) . 1_556 ? C20A C76 C21A 98(2) 1_556 1_556 ? C72 C76 N20A 128(3) . 1_556 ? C20A C76 N20A 49.4(16) 1_556 1_556 ? C21A C76 N20A 49.1(13) 1_556 1_556 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 C1 C2 C3 179.8(4) . . . . ? C8 C1 C2 C3 -59.5(5) . . . . ? C10 C1 C2 C3 58.4(5) . . . . ? C1 C2 C3 C18 -175.3(4) . . . . ? C1 C2 C3 C9 59.9(5) . . . . ? C1 C2 C3 C4 -58.1(5) . . . . ? C18 C3 C4 C5 176.1(4) . . . . ? C9 C3 C4 C5 -59.8(5) . . . . ? C2 C3 C4 C5 58.4(5) . . . . ? C3 C4 C5 C25 -179.4(4) . . . . ? C3 C4 C5 C6 58.2(6) . . . . ? C3 C4 C5 C10 -58.0(5) . . . . ? C25 C5 C6 C7 -177.8(4) . . . . ? C4 C5 C6 C7 -57.5(5) . . . . ? C10 C5 C6 C7 58.8(5) . . . . ? C5 C6 C7 C8 -60.1(5) . . . . ? C5 C6 C7 C32 179.9(4) . . . . ? C5 C6 C7 C9 58.3(5) . . . . ? C32 C7 C8 C1 177.2(4) . . . . ? C9 C7 C8 C1 -59.1(5) . . . . ? C6 C7 C8 C1 59.4(5) . . . . ? C11 C1 C8 C7 -178.6(4) . . . . ? C2 C1 C8 C7 59.2(5) . . . . ? C10 C1 C8 C7 -58.6(5) . . . . ? C18 C3 C9 C7 179.7(4) . . . . ? C2 C3 C9 C7 -59.0(5) . . . . ? C4 C3 C9 C7 59.6(5) . . . . ? C8 C7 C9 C3 58.9(5) . . . . ? C32 C7 C9 C3 -178.1(4) . . . . ? C6 C7 C9 C3 -59.2(5) . . . . ? C11 C1 C10 C5 177.9(4) . . . . ? C2 C1 C10 C5 -59.4(5) . . . . ? C8 C1 C10 C5 58.0(5) . . . . ? C25 C5 C10 C1 178.5(4) . . . . ? C6 C5 C10 C1 -57.7(5) . . . . ? C4 C5 C10 C1 58.9(5) . . . . ? C2 C1 C11 C16 -1.9(8) . . . . ? C8 C1 C11 C16 -121.7(6) . . . . ? C10 C1 C11 C16 118.9(6) . . . . ? C2 C1 C11 C12 176.7(5) . . . . ? C8 C1 C11 C12 56.9(6) . . . . ? C10 C1 C11 C12 -62.5(6) . . . . ? C16 C11 C12 C13 1.4(8) . . . . ? C1 C11 C12 C13 -177.3(5) . . . . ? C11 C12 C13 C14 -1.2(8) . . . . ? C12 C13 C14 C15 0.8(8) . . . . ? C12 C13 C14 C17 177.1(5) . . . . ? C13 C14 C15 C16 -0.6(9) . . . . ? C17 C14 C15 C16 -177.1(6) . . . . ? C14 C15 C16 C11 0.9(10) . . . . ? C12 C11 C16 C15 -1.2(9) . . . . ? C1 C11 C16 C15 177.4(6) . . . . ? C15 C14 C17 N4 10.6(9) . . . . ? C13 C14 C17 N4 -165.7(5) . . . . ? C15 C14 C17 N1 -165.9(6) . . . . ? C13 C14 C17 N1 17.8(9) . . . . ? C9 C3 C18 C19 1.4(8) . . . . ? C2 C3 C18 C19 -120.0(7) . . . . ? C4 C3 C18 C19 121.8(7) . . . . ? C9 C3 C18 C23 -180.0(5) . . . . ? C2 C3 C18 C23 58.6(6) . . . . ? C4 C3 C18 C23 -59.6(6) . . . . ? C23 C18 C19 C20 -0.3(11) . . . . ? C3 C18 C19 C20 178.4(7) . . . . ? C18 C19 C20 C21 -0.2(13) . . . . ? C19 C20 C21 C22 1.2(12) . . . . ? C19 C20 C21 C24 -174.5(8) . . . . ? C20 C21 C22 C23 -1.6(11) . . . . ? C24 C21 C22 C23 174.2(6) . . . . ? C21 C22 C23 C18 1.2(10) . . . . ? C19 C18 C23 C22 -0.3(9) . . . . ? C3 C18 C23 C22 -179.0(5) . . . . ? C20 C21 C24 N5 -145.5(9) . . . . ? C22 C21 C24 N5 38.8(11) . . . . ? C20 C21 C24 N8 37.5(13) . . . . ? C22 C21 C24 N8 -138.3(8) . . . . ? C6 C5 C25 C26 -128.7(7) . . . . ? C4 C5 C25 C26 111.4(7) . . . . ? C10 C5 C25 C26 -7.6(8) . . . . ? C6 C5 C25 C30 55.4(7) . . . . ? C4 C5 C25 C30 -64.4(7) . . . . ? C10 C5 C25 C30 176.6(5) . . . . ? C30 C25 C26 C27 0.8(12) . . . . ? C5 C25 C26 C27 -175.1(8) . . . . ? C25 C26 C27 C28 -3.6(15) . . . . ? C26 C27 C28 C29 4.4(13) . . . . ? C26 C27 C28 C31 -177.9(8) . . . . ? C27 C28 C29 C30 -2.5(11) . . . . ? C31 C28 C29 C30 179.9(6) . . . . ? C28 C29 C30 C25 -0.2(11) . . . . ? C26 C25 C30 C29 1.1(10) . . . . ? C5 C25 C30 C29 177.1(6) . . . . ? C27 C28 C31 N9 17.7(9) . . . . ? C29 C28 C31 N9 -164.7(6) . . . . ? C27 C28 C31 N12 -162.0(7) . . . . ? C29 C28 C31 N12 15.6(9) . . . . ? C8 C7 C32 C33 -2.2(7) . . . . ? C9 C7 C32 C33 -124.2(6) . . . . ? C6 C7 C32 C33 116.1(6) . . . . ? C8 C7 C32 C37 -179.9(5) . . . . ? C9 C7 C32 C37 58.2(7) . . . . ? C6 C7 C32 C37 -61.6(6) . . . . ? C37 C32 C33 C34 4.0(10) . . . . ? C7 C32 C33 C34 -173.7(6) . . . . ? C32 C33 C34 C35 0.1(10) . . . . ? C33 C34 C35 C36 -3.8(10) . . . . ? C33 C34 C35 C38 174.7(6) . . . . ? C34 C35 C36 C37 3.4(10) . . . . ? C38 C35 C36 C37 -175.0(6) . . . . ? C35 C36 C37 C32 0.8(11) . . . . ? C33 C32 C37 C36 -4.5(9) . . . . ? C7 C32 C37 C36 173.3(6) . . . . ? C36 C35 C38 N16 159.2(6) . . . . ? C34 C35 C38 N16 -19.2(8) . . . . ? C36 C35 C38 N13 -16.9(9) . . . . ? C34 C35 C38 N13 164.6(6) . . . . ? C66 C63 C64 C65 -127(5) . . . . ? C65 C64 C66 C63 74(6) . . . . ? C76 C72 C73 C74 -35(13) . . . . ? C21A C72 C73 C74 72(26) 1_556 . . . ? C72 C73 C74 C75 62(16) . . . . ? N4 C17 N1 N2 1.3(6) . . . . ? C14 C17 N1 N2 178.1(5) . . . . ? N4 C17 N1 Mn3 177.9(4) . . . 2 ? C14 C17 N1 Mn3 -5.3(10) . . . 2 ? C17 N1 N2 N3 -0.8(6) . . . . ? Mn3 N1 N2 N3 -178.6(3) 2 . . . ? C17 N1 N2 Mn2 -170.4(4) . . . 2_554 ? Mn3 N1 N2 Mn2 11.9(6) 2 . . 2_554 ? N1 N2 N3 N4 0.0(6) . . . . ? Mn2 N2 N3 N4 171.9(3) 2_554 . . . ? N1 N2 N3 Mn1 177.1(3) . . . . ? Mn2 N2 N3 Mn1 -10.9(5) 2_554 . . . ? N2 N3 N4 C17 0.8(6) . . . . ? Mn1 N3 N4 C17 -176.4(4) . . . . ? N1 C17 N4 N3 -1.3(6) . . . . ? C14 C17 N4 N3 -178.4(5) . . . . ? N8 C24 N5 N6 0.6(9) . . . . ? C21 C24 N5 N6 -176.8(7) . . . . ? N8 C24 N5 Mn1 -165.3(6) . . . 2_645 ? C21 C24 N5 Mn1 17.3(13) . . . 2_645 ? C24 N5 N6 N7 -2.0(9) . . . . ? Mn1 N5 N6 N7 167.8(6) 2_645 . . . ? C24 N5 N6 Mn2 -173.5(5) . . . 1_656 ? Mn1 N5 N6 Mn2 -3.8(7) 2_645 . . 1_656 ? N5 N6 N7 N8 2.6(10) . . . . ? Mn2 N6 N7 N8 174.3(6) 1_656 . . . ? N6 N7 N8 C24 -2.3(11) . . . . ? N5 C24 N8 N7 1.0(11) . . . . ? C21 C24 N8 N7 178.5(8) . . . . ? N12 C31 N9 N10 -0.6(6) . . . . ? C28 C31 N9 N10 179.7(5) . . . . ? C31 N9 N10 N11 0.5(6) . . . . ? C31 N9 N10 Mn2 178.5(4) . . . 1_556 ? N9 N10 N11 N12 -0.2(6) . . . . ? Mn2 N10 N11 N12 -177.9(4) 1_556 . . . ? N9 N10 N11 Mn3 159.5(3) . . . . ? Mn2 N10 N11 Mn3 -18.2(6) 1_556 . . . ? N10 N11 N12 C31 -0.1(6) . . . . ? Mn3 N11 N12 C31 -159.1(4) . . . . ? N9 C31 N12 N11 0.4(6) . . . . ? C28 C31 N12 N11 -179.8(5) . . . . ? N16 C38 N13 N14 0.4(6) . . . . ? C35 C38 N13 N14 176.9(5) . . . . ? C38 N13 N14 N15 -0.2(6) . . . . ? C38 N13 N14 Mn3 167.8(4) . . . 1_554 ? N13 N14 N15 N16 -0.1(6) . . . . ? Mn3 N14 N15 N16 -167.8(4) 1_554 . . . ? N13 N14 N15 Mn2 176.5(4) . . . . ? Mn3 N14 N15 Mn2 8.9(6) 1_554 . . . ? N14 N15 N16 C38 0.4(6) . . . . ? Mn2 N15 N16 C38 -176.5(4) . . . . ? N13 C38 N16 N15 -0.5(7) . . . . ? C35 C38 N16 N15 -177.1(5) . . . . ? O1 C40 N40 C41 -176(3) . . . . ? O1 C40 N40 C42 30(4) . . . . ? O3 C43 N43 C44 178.4(9) . . . . ? O3 C43 N43 C45 -7.3(14) . . . . ? O5 C49 N49 C50 2(3) . . . . ? O5 C49 N49 C51 -174(2) . . . . ? O7 C52 N52 C54 -167.4(19) . . . . ? O7 C52 N52 C53 -10(3) . . . . ? O8 C57 N53 C55 10(3) . . . . ? O8 C57 N53 C56 178(2) . . . . ? N2 N3 Mn1 O3 154.9(4) . . . . ? N4 N3 Mn1 O3 -28.3(4) . . . . ? N2 N3 Mn1 O1 -32.4(15) . . . . ? N4 N3 Mn1 O1 144.3(12) . . . . ? N2 N3 Mn1 O6 -118.6(4) . . . . ? N4 N3 Mn1 O6 58.1(4) . . . . ? N2 N3 Mn1 N5 65.0(4) . . . 2_655 ? N4 N3 Mn1 N5 -118.3(4) . . . 2_655 ? N2 N3 Mn1 Cl1 -27.4(4) . . . 2_554 ? N4 N3 Mn1 Cl1 149.4(4) . . . 2_554 ? N16 N15 Mn2 O2B 35.4(11) . . . . ? N14 N15 Mn2 O2B -140.9(11) . . . . ? N16 N15 Mn2 O2A 28.8(10) . . . . ? N14 N15 Mn2 O2A -147.5(10) . . . . ? N16 N15 Mn2 N10 126.9(5) . . . 1_554 ? N14 N15 Mn2 N10 -49.4(5) . . . 1_554 ? N16 N15 Mn2 N6 171.7(17) . . . 1_454 ? N14 N15 Mn2 N6 -5(2) . . . 1_454 ? N16 N15 Mn2 N2 -143.7(5) . . . 2_544 ? N14 N15 Mn2 N2 40.1(5) . . . 2_544 ? N16 N15 Mn2 Cl1 -57.4(5) . . . . ? N14 N15 Mn2 Cl1 126.3(5) . . . . ? Mn1 Cl1 Mn2 O2B 125.8(11) 2_544 . . . ? Mn1 Cl1 Mn2 O2A 136.8(13) 2_544 . . . ? Mn1 Cl1 Mn2 N15 -137.14(16) 2_544 . . . ? Mn1 Cl1 Mn2 N10 -52(2) 2_544 . . 1_554 ? Mn1 Cl1 Mn2 N6 38.22(19) 2_544 . . 1_454 ? Mn1 Cl1 Mn2 N2 -50.48(14) 2_544 . . 2_544 ? N10 N11 Mn3 N14 -30.6(4) . . . 1_556 ? N12 N11 Mn3 N14 126.2(4) . . . 1_556 ? N10 N11 Mn3 N14 149.4(4) . . . 3_565 ? N12 N11 Mn3 N14 -53.8(4) . . . 3_565 ? N10 N11 Mn3 N11 -179(100) . . . 3_566 ? N12 N11 Mn3 N11 -22(100) . . . 3_566 ? N10 N11 Mn3 N1 60.0(4) . . . 2_545 ? N12 N11 Mn3 N1 -143.2(4) . . . 2_545 ? N10 N11 Mn3 N1 -120.0(4) . . . 4_576 ? N12 N11 Mn3 N1 36.8(4) . . . 4_576 ? N40 C40 O1 Mn1 -145(3) . . . . ? O3 Mn1 O1 C40 -155.4(18) . . . . ? O6 Mn1 O1 C40 118.3(18) . . . . ? N5 Mn1 O1 C40 -64.8(18) 2_655 . . . ? N3 Mn1 O1 C40 32(2) . . . . ? Cl1 Mn1 O1 C40 26.9(18) 2_554 . . . ? O2B Mn2 O2A C20A -4(6) . . . . ? N15 Mn2 O2A C20A 144.5(17) . . . . ? N10 Mn2 O2A C20A 58.8(18) 1_554 . . . ? N6 Mn2 O2A C20A -31.8(18) 1_454 . . . ? N2 Mn2 O2A C20A -168(4) 2_544 . . . ? Cl1 Mn2 O2A C20A -121.8(18) . . . . ? N43 C43 O3 Mn1 -176.5(6) . . . . ? O1 Mn1 O3 C43 -143.3(7) . . . . ? O6 Mn1 O3 C43 -54.7(7) . . . . ? N5 Mn1 O3 C43 122.0(7) 2_655 . . . ? N3 Mn1 O3 C43 35.5(7) . . . . ? Cl1 Mn1 O3 C43 -20(4) 2_554 . . . ? Mn2 O2A C20A O2B 8(13) . . . . ? Mn2 O2A C20A N20A 160.4(15) . . . . ? Mn2 O2A C20A C76 -58(34) . . . 1_554 ? O2B C20A N20A C22A -11(4) . . . . ? C76 C20A N20A C22A 166(3) 1_554 . . . ? O2A C20A N20A C22A -17(3) . . . . ? O2B C20A N20A C21A -174(2) . . . . ? C76 C20A N20A C21A 3(2) 1_554 . . . ? O2A C20A N20A C21A 179.8(18) . . . . ? O2B C20A N20A C76 -177(3) . . . 1_554 ? O2A C20A N20A C76 177(3) . . . 1_554 ? N20A C20A O2B Mn2 160(2) . . . . ? C76 C20A O2B Mn2 -8(14) 1_554 . . . ? O2A C20A O2B Mn2 -170(17) . . . . ? O2A Mn2 O2B C20A 174(11) . . . . ? N15 Mn2 O2B C20A 142(3) . . . . ? N10 Mn2 O2B C20A 55(3) 1_554 . . . ? N6 Mn2 O2B C20A -34(3) 1_454 . . . ? N2 Mn2 O2B C20A -53(17) 2_544 . . . ? Cl1 Mn2 O2B C20A -125(3) . . . . ? C20A N20A C21A C76 -3(2) . . . 1_554 ? C22A N20A C21A C76 -166(3) . . . 1_554 ? C20A N20A C21A C72 9(2) . . . 1_554 ? C22A N20A C21A C72 -154(2) . . . 1_554 ? C76 N20A C21A C72 12.0(17) 1_554 . . 1_554 ? O4 C46 N46 C48 -169.5(16) . . . . ? O4 C46 N46 C47 5(2) . . . . ? C73 C72 C76 C20A -98(11) . . . 1_556 ? C21A C72 C76 C20A 91(11) 1_556 . . 1_556 ? C73 C72 C76 C21A 171(3) . . . 1_556 ? C73 C72 C76 N20A -173(3) . . . 1_556 ? C21A C72 C76 N20A 16(2) 1_556 . . 1_556 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.212 _refine_diff_density_min -1.293 _refine_diff_density_rms 0.171 data_La_phosphonate _database_code_depnum_ccdc_archive 'CCDC 910536' #TrackingRef '15366_web_deposit_cif_file_1_ChristophJaniak_1352729919.la_phosphonate.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; catena-[{\m~5~- pentahydrogen((adamant-1,3,5,7-tetrayl)-phen-4-yl)- tetraphosphonate-O,O',O'',O''',O'''')- -triaqua-lantanum(iii)} water and methanol solvate] ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C34 H33 O12 P4)3-, La 3+, (H2O)3 ' # Above moiety formula is without guest molecules # Moiety formula with guest molecules included is # '2(C34 H27.40 La O15 P4), 2(C0.50 O0.50), 2(C0.50 O0.50), C O0.5' _chemical_formula_sum 'C34 H39 La O15 P4' # Above formula sum is without guest molecules # Formula sum with guest molecules included is #'C72.70 H55.62 La2 O35.60 P8' and Z = 4 _chemical_formula_weight 950.47 # Above formula weight is without guest molecules # Formula weight with guest molecules included is 2024.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.6358(7) _cell_length_b 19.0353(5) _cell_length_c 27.9879(11) _cell_angle_alpha 90.00 _cell_angle_beta 110.636(2) _cell_angle_gamma 90.00 _cell_volume 11285.6(6) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 4442 _cell_measurement_theta_min 4.553 _cell_measurement_theta_max 36.70 _exptl_crystal_description 'transparent block' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.119 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3840 _exptl_absorpt_coefficient_mu 0.917 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9302 _exptl_absorpt_correction_T_max 0.9730 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'APEX II QUAZAR' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38944 _diffrn_reflns_av_R_equivalents 0.0771 _diffrn_reflns_av_sigmaI/netI 0.0882 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 24.12 _reflns_number_total 8916 _reflns_number_gt 5203 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1606P)^2^+93.1631P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8916 _refine_ls_number_parameters 600 _refine_ls_number_restraints 51 _refine_ls_R_factor_all 0.1627 _refine_ls_R_factor_gt 0.0994 _refine_ls_wR_factor_ref 0.3014 _refine_ls_wR_factor_gt 0.2592 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group La1 La 0.13435(4) 0.73956(4) 0.00324(3) 0.0630(3) Uani 1 1 d . . . P1 P 0.0958(2) 0.63357(18) 0.10123(15) 0.0873(14) Uani 1 1 d . A . P2 P 0.51896(19) 0.91331(19) 0.44398(17) 0.0816(12) Uani 1 1 d . . . P3 P -0.0387(2) 0.89945(16) 0.47772(19) 0.0840(13) Uani 1 1 d . . . P4 P 0.27191(16) 0.37682(14) 0.54188(12) 0.0566(9) Uani 1 1 d . . . O1 O 0.0984(5) 0.6955(4) 0.0711(3) 0.078(3) Uani 1 1 d . . . O2 O 0.0276(6) 0.5978(6) 0.0870(4) 0.120(4) Uani 1 1 d . . . O3 O 0.1434(7) 0.5771(5) 0.0962(4) 0.121(5) Uani 1 1 d . . . O4 O 0.5694(4) 0.8657(5) 0.4663(4) 0.084(3) Uani 1 1 d . . . O5 O 0.5237(7) 0.9811(8) 0.4717(8) 0.198(9) Uani 1 1 d . . . O6 O 0.5178(5) 0.9355(8) 0.3894(5) 0.145(6) Uani 1 1 d . . . O7 O -0.0827(5) 0.8429(4) 0.4783(4) 0.089(3) Uani 1 1 d . . . O8 O -0.0717(5) 0.9631(5) 0.4464(5) 0.100(3) Uani 1 1 d . . . O9 O -0.0013(6) 0.9285(6) 0.5330(5) 0.111(4) Uani 1 1 d . . . O10 O 0.3014(5) 0.3263(4) 0.5182(4) 0.093(3) Uani 1 1 d . . . O11 O 0.3211(5) 0.3978(5) 0.5959(4) 0.083(3) Uani 1 1 d . . . O12 O 0.2138(4) 0.3517(4) 0.5506(3) 0.078(3) Uani 1 1 d . . . O13 O 0.0507(7) 0.7811(8) -0.0822(5) 0.151(6) Uani 1 1 d . . . O14 O 0.1698(5) 0.6873(5) -0.0684(4) 0.096(3) Uani 1 1 d . . . O15 O 0.2159(5) 0.7884(5) 0.0891(4) 0.087(3) Uani 1 1 d . . . O1S O 0.5609(9) 0.5737(11) 0.3978(7) 0.087(5) Uiso 0.50 1 d PD . . O2S O 0.1979(11) 0.2024(12) 0.3347(9) 0.105(7) Uiso 0.50 1 d PD . . O9S O 0.3187(12) 0.4267(13) 0.2060(9) 0.076(7) Uiso 0.35 1 d PD . . C9S C 0.313(2) 0.4798(18) 0.1723(14) 0.084(12) Uiso 0.35 1 d PD . . O4S O 0.3281(15) 0.3962(12) 0.3670(10) 0.134(9) Uani 0.50 1 d P . . O10S O 0.0561(16) 0.9307(18) 0.2383(11) 0.074(10) Uani 0.25 1 d PDU . . O6S O 0.358(2) 0.944(3) 0.144(2) 0.15(2) Uiso 0.25 1 d PD . . O7S O 0.241(3) 0.950(2) 0.2302(17) 0.099(18) Uani 0.20 1 d P . . C1 C 0.1169(7) 0.6547(5) 0.1671(5) 0.074(4) Uani 1 1 d DU . . C2 C 0.1325(10) 0.7221(8) 0.1866(7) 0.047(5) Uani 0.596(19) 1 d PDU A 1 H2 H 0.1320 0.7589 0.1636 0.057 Uiso 0.596(19) 1 calc PR A 1 C3 C 0.1484(12) 0.7380(9) 0.2371(7) 0.062(6) Uani 0.596(19) 1 d PDU A 1 H3 H 0.1525 0.7856 0.2478 0.074 Uiso 0.596(19) 1 calc PR A 1 C5 C 0.1523(14) 0.6150(8) 0.2554(8) 0.082(9) Uani 0.596(19) 1 d PDU A 1 H5 H 0.1605 0.5775 0.2793 0.098 Uiso 0.596(19) 1 calc PR A 1 C6 C 0.1340(16) 0.6009(9) 0.2032(8) 0.105(12) Uani 0.596(19) 1 d PDU A 1 H6 H 0.1333 0.5537 0.1921 0.125 Uiso 0.404(19) 1 calc PR A 1 C2D C 0.1683(16) 0.699(2) 0.1875(12) 0.088(11) Uani 0.404(19) 1 d PDU A 2 H2D H 0.1913 0.7167 0.1676 0.105 Uiso 0.404(19) 1 calc PR A 2 C3D C 0.184(2) 0.715(3) 0.2382(11) 0.11(2) Uani 0.404(19) 1 d PDU A 2 H3D H 0.2153 0.7498 0.2515 0.135 Uiso 0.404(19) 1 calc PR A 2 C5D C 0.0973(11) 0.659(2) 0.2470(12) 0.084(11) Uani 0.404(19) 1 d PDU A 2 H5D H 0.0691 0.6557 0.2652 0.100 Uiso 0.404(19) 1 calc PR A 2 C6D C 0.0746(14) 0.6373(19) 0.1914(13) 0.079(9) Uani 0.404(19) 1 d PDU A 2 H6D H 0.0357 0.6140 0.1748 0.094 Uiso 0.404(19) 1 calc PR A 2 C4 C 0.1584(6) 0.6852(5) 0.2725(5) 0.059(3) Uani 1 1 d DU . . C7 C 0.1812(6) 0.7023(6) 0.3293(4) 0.055(3) Uani 1 1 d . A . C8 C 0.2441(5) 0.7424(5) 0.3450(4) 0.050(3) Uani 1 1 d . . . H8A H 0.2760 0.7132 0.3374 0.061 Uiso 1 1 calc R A . H8B H 0.2383 0.7861 0.3247 0.061 Uiso 1 1 calc R . . C9 C 0.2682(5) 0.7606(5) 0.4019(4) 0.047(3) Uani 1 1 d . A . C10 C 0.2774(5) 0.6914(5) 0.4320(4) 0.047(3) Uani 1 1 d . . . H10A H 0.2936 0.7018 0.4690 0.057 Uiso 1 1 calc R A . H10B H 0.3092 0.6622 0.4243 0.057 Uiso 1 1 calc R . . C11 C 0.2151(5) 0.6500(5) 0.4183(4) 0.046(3) Uani 1 1 d . A . C12 C 0.1910(6) 0.6345(5) 0.3607(5) 0.057(3) Uani 1 1 d . . . H12A H 0.2220 0.6043 0.3527 0.068 Uiso 1 1 calc R A . H12B H 0.1506 0.6086 0.3511 0.068 Uiso 1 1 calc R . . C13 C 0.2183(5) 0.8038(5) 0.4135(4) 0.049(3) Uani 1 1 d . . . H13A H 0.2117 0.8486 0.3943 0.059 Uiso 1 1 calc R A . H13B H 0.2334 0.8152 0.4504 0.059 Uiso 1 1 calc R . . C14 C 0.1661(5) 0.6955(5) 0.4288(4) 0.049(3) Uani 1 1 d . . . H14A H 0.1801 0.7057 0.4658 0.059 Uiso 1 1 calc R A . H14B H 0.1257 0.6695 0.4191 0.059 Uiso 1 1 calc R . . C15 C 0.1336(6) 0.7483(5) 0.3423(5) 0.054(3) Uani 1 1 d . . . H15A H 0.1277 0.7928 0.3229 0.064 Uiso 1 1 calc R A . H15B H 0.0924 0.7239 0.3319 0.064 Uiso 1 1 calc R . . C16 C 0.1556(5) 0.7646(5) 0.3992(4) 0.047(3) Uani 1 1 d . A . C17 C 0.3313(5) 0.7997(5) 0.4162(4) 0.043(2) Uani 1 1 d . . . C18 C 0.3341(6) 0.8631(6) 0.3919(5) 0.066(3) Uani 1 1 d . A . H18 H 0.2964 0.8825 0.3683 0.079 Uiso 1 1 calc R . . C19 C 0.3897(6) 0.8976(6) 0.4013(5) 0.071(4) Uani 1 1 d . . . H19 H 0.3901 0.9404 0.3841 0.085 Uiso 1 1 calc R A . C20 C 0.4452(6) 0.8718(5) 0.4353(5) 0.054(3) Uani 1 1 d . A . C21 C 0.4411(6) 0.8125(6) 0.4624(5) 0.062(3) Uani 1 1 d . . . H21 H 0.4781 0.7952 0.4882 0.075 Uiso 1 1 calc R A . C22 C 0.3854(6) 0.7782(6) 0.4530(5) 0.062(3) Uani 1 1 d . A . H22 H 0.3844 0.7379 0.4728 0.074 Uiso 1 1 calc R . . C23 C 0.2267(5) 0.5815(5) 0.4482(4) 0.050(3) Uani 1 1 d . . . C24 C 0.2724(6) 0.5346(5) 0.4452(5) 0.061(3) Uani 1 1 d . A . H24 H 0.2948 0.5451 0.4231 0.074 Uiso 1 1 calc R . . C25 C 0.2862(5) 0.4734(5) 0.4734(4) 0.053(3) Uani 1 1 d . . . H25 H 0.3178 0.4427 0.4703 0.064 Uiso 1 1 calc R A . C26 C 0.2549(5) 0.4562(6) 0.5059(4) 0.053(3) Uani 1 1 d . A . C27 C 0.2059(5) 0.5021(6) 0.5074(5) 0.056(3) Uani 1 1 d . . . H27 H 0.1815 0.4907 0.5278 0.067 Uiso 1 1 calc R A . C28 C 0.1941(5) 0.5624(6) 0.4793(4) 0.055(3) Uani 1 1 d . A . H28 H 0.1616 0.5927 0.4812 0.067 Uiso 1 1 calc R . . C29 C 0.1051(5) 0.8067(5) 0.4128(4) 0.049(3) Uani 1 1 d . . . C30 C 0.1179(5) 0.8682(5) 0.4411(5) 0.054(3) Uani 1 1 d . A . H30 H 0.1575 0.8906 0.4477 0.064 Uiso 1 1 calc R . . C31 C 0.0744(6) 0.8987(5) 0.4603(5) 0.061(3) Uani 1 1 d . . . H31 H 0.0847 0.9409 0.4797 0.073 Uiso 1 1 calc R A . C32 C 0.0175(6) 0.8675(5) 0.4510(5) 0.058(3) Uani 1 1 d . A . C33 C 0.0034(6) 0.8076(7) 0.4212(5) 0.070(4) Uani 1 1 d . . . H33 H -0.0371 0.7868 0.4134 0.085 Uiso 1 1 calc R A . C34 C 0.0454(6) 0.7774(6) 0.4026(5) 0.066(4) Uani 1 1 d . A . H34 H 0.0339 0.7360 0.3825 0.080 Uiso 1 1 calc R . . C10S C 0.035(2) 0.893(3) 0.1952(16) 0.17(2) Uani 0.50 1 d PD . . O8S O 0.126(2) 0.078(3) 0.154(2) 0.131(17) Uiso 0.25 1 d PD . . C6S C 0.3992(18) 0.891(2) 0.1500(15) 0.043(10) Uiso 0.25 1 d PD . . C8S C 0.151(3) 0.017(3) 0.144(2) 0.079(15) Uiso 0.25 1 d PD . . C2S C 0.201(4) 0.171(4) 0.2926(19) 0.26(3) Uiso 0.50 1 d PD . . C1S C 0.539(4) 0.524(4) 0.361(3) 0.33(5) Uiso 0.50 1 d PD . . 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 La1 0.0753(5) 0.0450(4) 0.0800(6) -0.0026(4) 0.0412(4) 0.0136(3) P1 0.162(4) 0.0455(19) 0.069(3) -0.0067(17) 0.059(3) 0.016(2) P2 0.076(3) 0.055(2) 0.118(3) 0.014(2) 0.040(2) -0.0159(18) P3 0.099(3) 0.0391(17) 0.158(4) -0.001(2) 0.101(3) -0.0042(17) P4 0.078(2) 0.0327(14) 0.064(2) 0.0000(14) 0.0309(18) -0.0142(14) O1 0.131(8) 0.052(5) 0.061(6) 0.000(4) 0.043(5) 0.011(5) O2 0.169(12) 0.082(7) 0.112(9) -0.034(6) 0.054(8) -0.055(8) O3 0.251(15) 0.047(5) 0.098(8) 0.012(5) 0.104(9) 0.051(7) O4 0.069(6) 0.086(6) 0.095(7) 0.036(5) 0.025(5) -0.016(5) O5 0.162(13) 0.143(12) 0.34(2) -0.138(14) 0.146(15) -0.112(11) O6 0.100(9) 0.181(13) 0.161(11) 0.119(10) 0.053(8) 0.005(8) O7 0.115(8) 0.046(5) 0.145(9) -0.027(5) 0.094(7) -0.027(5) O8 0.083(7) 0.078(7) 0.167(10) 0.023(6) 0.080(7) 0.022(5) O9 0.143(10) 0.092(7) 0.142(10) -0.060(7) 0.106(8) -0.036(7) O10 0.147(10) 0.045(5) 0.097(7) 0.010(5) 0.056(7) 0.002(5) O11 0.095(7) 0.065(6) 0.082(7) 0.004(5) 0.021(6) -0.007(5) O12 0.099(7) 0.053(5) 0.085(6) 0.004(4) 0.037(5) -0.033(5) O13 0.139(12) 0.147(11) 0.132(11) 0.062(9) 0.005(9) -0.031(9) O14 0.111(8) 0.088(7) 0.107(8) -0.025(6) 0.059(7) -0.006(6) O15 0.101(7) 0.063(5) 0.097(7) -0.026(5) 0.036(6) 0.007(5) O4S 0.20(3) 0.084(16) 0.15(2) 0.008(15) 0.10(2) -0.019(16) O10S 0.075(19) 0.10(2) 0.045(17) -0.041(16) 0.013(15) -0.021(16) O7S 0.17(5) 0.08(3) 0.08(3) -0.04(3) 0.08(3) -0.07(3) C1 0.128(12) 0.045(6) 0.060(7) -0.010(5) 0.047(8) 0.004(6) C2 0.050(12) 0.036(7) 0.058(8) 0.005(7) 0.022(10) 0.001(8) C3 0.088(18) 0.035(8) 0.062(9) -0.010(6) 0.026(13) 0.005(10) C5 0.15(3) 0.038(7) 0.065(9) 0.004(8) 0.046(15) -0.007(12) C6 0.24(4) 0.030(8) 0.077(11) -0.008(7) 0.09(2) -0.001(14) C2D 0.09(3) 0.12(3) 0.077(16) 0.00(2) 0.06(2) -0.007(19) C3D 0.15(4) 0.13(4) 0.063(17) 0.01(2) 0.04(2) -0.08(3) C5D 0.057(15) 0.13(3) 0.082(16) 0.00(2) 0.045(14) 0.005(16) C6D 0.062(19) 0.08(2) 0.088(16) 0.004(17) 0.014(12) -0.008(16) C4 0.080(8) 0.050(6) 0.063(7) -0.008(5) 0.046(6) -0.010(6) C7 0.068(8) 0.048(6) 0.059(8) -0.008(5) 0.036(6) -0.004(5) C8 0.072(8) 0.032(5) 0.059(8) 0.008(5) 0.038(6) -0.004(5) C9 0.064(7) 0.026(5) 0.063(8) 0.004(5) 0.036(6) -0.003(5) C10 0.060(7) 0.026(5) 0.064(7) 0.006(5) 0.033(6) -0.003(4) C11 0.071(7) 0.029(5) 0.053(7) -0.003(5) 0.040(6) 0.001(5) C12 0.070(8) 0.035(6) 0.087(10) 0.008(6) 0.054(7) 0.001(5) C13 0.067(7) 0.028(5) 0.064(8) 0.002(5) 0.037(6) 0.001(5) C14 0.057(7) 0.045(6) 0.059(7) 0.007(5) 0.037(6) 0.008(5) C15 0.066(7) 0.037(6) 0.072(8) -0.002(5) 0.043(6) 0.000(5) C16 0.061(7) 0.036(5) 0.054(7) -0.003(5) 0.032(6) 0.003(5) C17 0.055(7) 0.034(5) 0.048(7) 0.007(5) 0.029(6) 0.001(5) C18 0.072(9) 0.043(6) 0.083(9) 0.011(6) 0.028(7) -0.007(6) C19 0.069(9) 0.051(7) 0.098(11) 0.028(7) 0.037(8) -0.002(6) C20 0.066(8) 0.037(6) 0.064(8) 0.003(5) 0.030(7) -0.010(5) C21 0.072(8) 0.044(6) 0.070(9) 0.016(6) 0.025(7) 0.004(6) C22 0.065(8) 0.049(7) 0.085(10) 0.021(6) 0.042(7) -0.001(6) C23 0.062(7) 0.032(5) 0.078(8) 0.001(5) 0.051(7) -0.005(5) C24 0.077(8) 0.039(6) 0.092(10) 0.006(6) 0.059(8) -0.004(5) C25 0.065(7) 0.035(6) 0.073(8) 0.001(5) 0.039(7) -0.006(5) C26 0.064(8) 0.039(6) 0.060(8) -0.001(5) 0.028(6) -0.015(5) C27 0.050(7) 0.046(6) 0.086(9) 0.002(6) 0.041(6) -0.006(5) C28 0.056(7) 0.047(6) 0.075(9) 0.008(6) 0.036(6) 0.004(5) C29 0.056(7) 0.050(6) 0.042(7) 0.007(5) 0.020(6) 0.004(5) C30 0.056(7) 0.033(5) 0.086(9) 0.007(5) 0.042(6) -0.003(5) C31 0.086(9) 0.030(5) 0.094(10) 0.008(6) 0.063(8) 0.004(5) C32 0.079(9) 0.020(5) 0.093(9) 0.003(5) 0.053(7) 0.002(5) C33 0.061(8) 0.067(8) 0.096(10) -0.001(7) 0.043(8) -0.006(6) C34 0.073(9) 0.042(6) 0.099(11) -0.009(6) 0.048(8) -0.006(6) C10S 0.11(3) 0.22(6) 0.16(4) -0.08(4) 0.02(3) -0.01(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag La1 O10 2.411(10) 4 ? La1 O7 2.436(8) 2 ? La1 O1 2.463(9) . ? La1 O4 2.484(9) 8_465 ? La1 O12 2.515(8) 6_565 ? La1 O13 2.595(12) . ? La1 O14 2.604(10) . ? La1 O15 2.630(9) . ? P1 O1 1.462(9) . ? P1 O3 1.562(11) . ? P1 O2 1.605(13) . ? P1 C1 1.779(13) . ? P2 O4 1.419(10) . ? P2 O5 1.490(13) . ? P2 O6 1.575(12) . ? P2 C20 1.784(12) . ? P3 O7 1.470(9) . ? P3 O8 1.528(10) . ? P3 O9 1.578(12) . ? P3 C32 1.793(12) . ? P4 O10 1.457(10) . ? P4 O12 1.500(9) . ? P4 O11 1.580(10) . ? P4 C26 1.781(11) . ? O4 La1 2.484(9) 8_566 ? O7 La1 2.436(8) 2 ? O10 La1 2.411(10) 4_545 ? O12 La1 2.515(8) 6_566 ? O1S C1S 1.354(14) . ? O2S C2S 1.348(14) . ? O9S C9S 1.358(19) . ? O10S C10S 1.340(19) . ? O6S C6S 1.35(2) . ? C1 C2D 1.382(19) . ? C1 C2 1.390(16) . ? C1 C6 1.394(17) . ? C1 C6D 1.397(19) . ? C2 C3 1.36(2) . ? C2 H2 0.9500 . ? C3 C4 1.372(16) . ? C3 H3 0.9500 . ? C5 C6 1.40(3) . ? C5 C4 1.409(16) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C2D C3D 1.37(3) . ? C2D H2D 0.9500 . ? C3D C4 1.400(19) . ? C3D H3D 0.9500 . ? C5D C4 1.403(19) . ? C5D C6D 1.52(4) . ? C5D H5D 0.9500 . ? C6D H6D 0.9500 . ? C4 C7 1.524(16) . ? C7 C15 1.528(15) . ? C7 C12 1.533(15) . ? C7 C8 1.537(15) . ? C8 C9 1.532(16) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C13 1.523(14) . ? C9 C17 1.533(14) . ? C9 C10 1.537(13) . ? C10 C11 1.541(14) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C14 1.515(14) . ? C11 C23 1.522(14) . ? C11 C12 1.538(16) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C16 1.526(15) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C16 1.529(14) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.524(16) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C29 1.547(14) . ? C17 C22 1.356(16) . ? C17 C18 1.398(14) . ? C18 C19 1.360(17) . ? C18 H18 0.9500 . ? C19 C20 1.372(17) . ? C19 H19 0.9500 . ? C20 C21 1.381(15) . ? C21 C22 1.361(16) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C28 1.373(14) . ? C23 C24 1.391(15) . ? C24 C25 1.380(15) . ? C24 H24 0.9500 . ? C25 C26 1.375(15) . ? C25 H25 0.9500 . ? C26 C27 1.424(15) . ? C27 C28 1.364(15) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C30 1.387(15) . ? C29 C34 1.396(16) . ? C30 C31 1.402(15) . ? C30 H30 0.9500 . ? C31 C32 1.358(16) . ? C31 H31 0.9500 . ? C32 C33 1.383(16) . ? C33 C34 1.362(17) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? O8S C8S 1.37(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O10 La1 O7 82.9(3) 4 2 ? O10 La1 O1 144.8(3) 4 . ? O7 La1 O1 78.3(3) 2 . ? O10 La1 O4 140.2(3) 4 8_465 ? O7 La1 O4 118.8(3) 2 8_465 ? O1 La1 O4 74.9(3) . 8_465 ? O10 La1 O12 102.8(3) 4 6_565 ? O7 La1 O12 138.9(3) 2 6_565 ? O1 La1 O12 74.2(3) . 6_565 ? O4 La1 O12 82.6(3) 8_465 6_565 ? O10 La1 O13 82.6(4) 4 . ? O7 La1 O13 72.6(5) 2 . ? O1 La1 O13 118.8(4) . . ? O4 La1 O13 74.3(4) 8_465 . ? O12 La1 O13 148.2(5) 6_565 . ? O10 La1 O14 72.2(3) 4 . ? O7 La1 O14 140.6(3) 2 . ? O1 La1 O14 137.6(3) . . ? O4 La1 O14 70.6(3) 8_465 . ? O12 La1 O14 77.6(3) 6_565 . ? O13 La1 O14 74.3(5) . . ? O10 La1 O15 72.2(3) 4 . ? O7 La1 O15 75.8(3) 2 . ? O1 La1 O15 74.4(3) . . ? O4 La1 O15 141.9(3) 8_465 . ? O12 La1 O15 67.8(3) 6_565 . ? O13 La1 O15 141.5(4) . . ? O14 La1 O15 122.1(3) . . ? O1 P1 O3 109.6(6) . . ? O1 P1 O2 115.4(7) . . ? O3 P1 O2 108.6(7) . . ? O1 P1 C1 111.3(5) . . ? O3 P1 C1 107.8(6) . . ? O2 P1 C1 103.7(7) . . ? O4 P2 O5 115.2(9) . . ? O4 P2 O6 109.4(7) . . ? O5 P2 O6 104.2(10) . . ? O4 P2 C20 110.3(5) . . ? O5 P2 C20 110.3(7) . . ? O6 P2 C20 107.0(6) . . ? O7 P3 O8 112.9(6) . . ? O7 P3 O9 112.2(6) . . ? O8 P3 O9 105.6(7) . . ? O7 P3 C32 109.8(5) . . ? O8 P3 C32 107.8(5) . . ? O9 P3 C32 108.3(6) . . ? O10 P4 O12 115.6(6) . . ? O10 P4 O11 108.7(6) . . ? O12 P4 O11 106.7(5) . . ? O10 P4 C26 110.2(5) . . ? O12 P4 C26 109.6(5) . . ? O11 P4 C26 105.3(5) . . ? P1 O1 La1 144.1(5) . . ? P2 O4 La1 164.7(5) . 8_566 ? P3 O7 La1 166.2(7) . 2 ? P4 O10 La1 168.1(7) . 4_545 ? P4 O12 La1 129.7(5) . 6_566 ? C2D C1 C2 38.6(18) . . ? C2D C1 C6 100(2) . . ? C2 C1 C6 115.1(15) . . ? C2D C1 C6D 124(2) . . ? C2 C1 C6D 98.5(18) . . ? C6 C1 C6D 62.3(18) . . ? C2D C1 P1 116.5(16) . . ? C2 C1 P1 123.7(11) . . ? C6 C1 P1 119.3(11) . . ? C6D C1 P1 118.1(18) . . ? C3 C2 C1 123.4(16) . . ? C3 C2 H2 118.3 . . ? C1 C2 H2 118.3 . . ? C2 C3 C4 120.1(16) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C6 C5 C4 119.6(16) . . ? C6 C5 H5 120.2 . . ? C4 C5 H5 120.2 . . ? C1 C6 C5 121.5(16) . . ? C1 C6 H6 119.3 . . ? C5 C6 H6 119.3 . . ? C3D C2D C1 116(3) . . ? C3D C2D H2D 122.1 . . ? C1 C2D H2D 122.1 . . ? C2D C3D C4 127(3) . . ? C2D C3D H3D 116.5 . . ? C4 C3D H3D 116.5 . . ? C4 C5D C6D 122(2) . . ? C4 C5D H5D 118.8 . . ? C6D C5D H5D 118.8 . . ? C1 C6D C5D 113(2) . . ? C1 C6D H6D 123.4 . . ? C5D C6D H6D 123.4 . . ? C3 C4 C3D 38(2) . . ? C3 C4 C5D 90(2) . . ? C3D C4 C5D 111(2) . . ? C3 C4 C5 118.5(15) . . ? C3D C4 C5 99(2) . . ? C5D C4 C5 62.2(18) . . ? C3 C4 C7 120.4(12) . . ? C3D C4 C7 124.0(17) . . ? C5D C4 C7 121.1(16) . . ? C5 C4 C7 120.9(13) . . ? C4 C7 C15 111.3(10) . . ? C4 C7 C12 110.2(9) . . ? C15 C7 C12 108.6(9) . . ? C4 C7 C8 110.0(9) . . ? C15 C7 C8 108.0(9) . . ? C12 C7 C8 108.8(10) . . ? C9 C8 C7 111.2(9) . . ? C9 C8 H8A 109.4 . . ? C7 C8 H8A 109.4 . . ? C9 C8 H8B 109.4 . . ? C7 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? C13 C9 C8 109.0(9) . . ? C13 C9 C17 112.1(8) . . ? C8 C9 C17 109.7(8) . . ? C13 C9 C10 108.3(8) . . ? C8 C9 C10 107.8(8) . . ? C17 C9 C10 109.9(9) . . ? C9 C10 C11 111.6(9) . . ? C9 C10 H10A 109.3 . . ? C11 C10 H10A 109.3 . . ? C9 C10 H10B 109.3 . . ? C11 C10 H10B 109.3 . . ? H10A C10 H10B 108.0 . . ? C14 C11 C23 112.3(8) . . ? C14 C11 C12 107.5(9) . . ? C23 C11 C12 110.0(8) . . ? C14 C11 C10 109.1(8) . . ? C23 C11 C10 109.6(9) . . ? C12 C11 C10 108.2(8) . . ? C7 C12 C11 111.4(9) . . ? C7 C12 H12A 109.3 . . ? C11 C12 H12A 109.3 . . ? C7 C12 H12B 109.3 . . ? C11 C12 H12B 109.3 . . ? H12A C12 H12B 108.0 . . ? C9 C13 C16 111.8(8) . . ? C9 C13 H13A 109.3 . . ? C16 C13 H13A 109.3 . . ? C9 C13 H13B 109.3 . . ? C16 C13 H13B 109.3 . . ? H13A C13 H13B 107.9 . . ? C11 C14 C16 111.8(8) . . ? C11 C14 H14A 109.3 . . ? C16 C14 H14A 109.3 . . ? C11 C14 H14B 109.3 . . ? C16 C14 H14B 109.3 . . ? H14A C14 H14B 107.9 . . ? C16 C15 C7 111.6(10) . . ? C16 C15 H15A 109.3 . . ? C7 C15 H15A 109.3 . . ? C16 C15 H15B 109.3 . . ? C7 C15 H15B 109.3 . . ? H15A C15 H15B 108.0 . . ? C15 C16 C13 107.7(9) . . ? C15 C16 C14 108.8(8) . . ? C13 C16 C14 109.0(9) . . ? C15 C16 C29 111.4(9) . . ? C13 C16 C29 112.4(8) . . ? C14 C16 C29 107.4(8) . . ? C22 C17 C18 116.5(10) . . ? C22 C17 C9 124.1(9) . . ? C18 C17 C9 119.4(10) . . ? C19 C18 C17 121.3(12) . . ? C19 C18 H18 119.3 . . ? C17 C18 H18 119.3 . . ? C18 C19 C20 121.4(11) . . ? C18 C19 H19 119.3 . . ? C20 C19 H19 119.3 . . ? C19 C20 C21 116.8(11) . . ? C19 C20 P2 121.3(8) . . ? C21 C20 P2 121.9(10) . . ? C22 C21 C20 121.5(12) . . ? C22 C21 H21 119.2 . . ? C20 C21 H21 119.2 . . ? C17 C22 C21 122.0(10) . . ? C17 C22 H22 119.0 . . ? C21 C22 H22 119.0 . . ? C28 C23 C24 116.5(10) . . ? C28 C23 C11 123.2(9) . . ? C24 C23 C11 120.3(9) . . ? C25 C24 C23 122.0(10) . . ? C25 C24 H24 119.0 . . ? C23 C24 H24 119.0 . . ? C26 C25 C24 120.9(11) . . ? C26 C25 H25 119.6 . . ? C24 C25 H25 119.6 . . ? C25 C26 C27 117.5(10) . . ? C25 C26 P4 121.1(9) . . ? C27 C26 P4 121.3(8) . . ? C28 C27 C26 119.7(10) . . ? C28 C27 H27 120.1 . . ? C26 C27 H27 120.1 . . ? C27 C28 C23 123.2(10) . . ? C27 C28 H28 118.4 . . ? C23 C28 H28 118.4 . . ? C30 C29 C34 116.5(10) . . ? C30 C29 C16 123.7(10) . . ? C34 C29 C16 119.3(10) . . ? C29 C30 C31 122.4(10) . . ? C29 C30 H30 118.8 . . ? C31 C30 H30 118.8 . . ? C32 C31 C30 119.5(11) . . ? C32 C31 H31 120.3 . . ? C30 C31 H31 120.3 . . ? C31 C32 C33 118.5(11) . . ? C31 C32 P3 122.4(9) . . ? C33 C32 P3 119.0(9) . . ? C34 C33 C32 122.4(12) . . ? C34 C33 H33 118.8 . . ? C32 C33 H33 118.8 . . ? C33 C34 C29 120.6(11) . . ? C33 C34 H34 119.7 . . ? C29 C34 H34 119.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 P1 O1 La1 15.9(13) . . . . ? O2 P1 O1 La1 -107.1(11) . . . . ? C1 P1 O1 La1 135.0(10) . . . . ? O10 La1 O1 P1 -122.9(10) 4 . . . ? O7 La1 O1 P1 178.0(11) 2 . . . ? O4 La1 O1 P1 53.5(10) 8_465 . . . ? O12 La1 O1 P1 -33.0(10) 6_565 . . . ? O13 La1 O1 P1 115.6(11) . . . . ? O14 La1 O1 P1 17.1(13) . . . . ? O15 La1 O1 P1 -103.7(11) . . . . ? O5 P2 O4 La1 128(3) . . . 8_566 ? O6 P2 O4 La1 -115(3) . . . 8_566 ? C20 P2 O4 La1 3(3) . . . 8_566 ? O8 P3 O7 La1 -163(2) . . . 2 ? O9 P3 O7 La1 -44(2) . . . 2 ? C32 P3 O7 La1 77(2) . . . 2 ? O12 P4 O10 La1 -102(3) . . . 4_545 ? O11 P4 O10 La1 17(3) . . . 4_545 ? C26 P4 O10 La1 133(3) . . . 4_545 ? O10 P4 O12 La1 -27.3(9) . . . 6_566 ? O11 P4 O12 La1 -148.4(6) . . . 6_566 ? C26 P4 O12 La1 98.0(7) . . . 6_566 ? O1 P1 C1 C2D -43(3) . . . . ? O3 P1 C1 C2D 77(3) . . . . ? O2 P1 C1 C2D -168(3) . . . . ? O1 P1 C1 C2 1.3(18) . . . . ? O3 P1 C1 C2 121.4(16) . . . . ? O2 P1 C1 C2 -123.5(16) . . . . ? O1 P1 C1 C6 -162.5(19) . . . . ? O3 P1 C1 C6 -42(2) . . . . ? O2 P1 C1 C6 73(2) . . . . ? O1 P1 C1 C6D 125.2(18) . . . . ? O3 P1 C1 C6D -114.6(19) . . . . ? O2 P1 C1 C6D 0.5(19) . . . . ? C2D C1 C2 C3 -89(3) . . . . ? C6 C1 C2 C3 -16(3) . . . . ? C6D C1 C2 C3 47(3) . . . . ? P1 C1 C2 C3 179.7(17) . . . . ? C1 C2 C3 C4 9(3) . . . . ? C2D C1 C6 C5 51(4) . . . . ? C2 C1 C6 C5 14(4) . . . . ? C6D C1 C6 C5 -73(3) . . . . ? P1 C1 C6 C5 179(2) . . . . ? C4 C5 C6 C1 -5(4) . . . . ? C2 C1 C2D C3D 68(4) . . . . ? C6 C1 C2D C3D -51(4) . . . . ? C6D C1 C2D C3D 12(6) . . . . ? P1 C1 C2D C3D 180(3) . . . . ? C1 C2D C3D C4 8(8) . . . . ? C2D C1 C6D C5D -12(4) . . . . ? C2 C1 C6D C5D -43(3) . . . . ? C6 C1 C6D C5D 71(3) . . . . ? P1 C1 C6D C5D -179(2) . . . . ? C4 C5D C6D C1 -9(5) . . . . ? C2 C3 C4 C3D 68(3) . . . . ? C2 C3 C4 C5D -58(3) . . . . ? C2 C3 C4 C5 0(3) . . . . ? C2 C3 C4 C7 175.2(17) . . . . ? C2D C3D C4 C3 -87(6) . . . . ? C2D C3D C4 C5D -26(7) . . . . ? C2D C3D C4 C5 38(6) . . . . ? C2D C3D C4 C7 176(4) . . . . ? C6D C5D C4 C3 58(3) . . . . ? C6D C5D C4 C3D 25(5) . . . . ? C6D C5D C4 C5 -65(3) . . . . ? C6D C5D C4 C7 -176(2) . . . . ? C6 C5 C4 C3 -2(3) . . . . ? C6 C5 C4 C3D -38(4) . . . . ? C6 C5 C4 C5D 71(3) . . . . ? C6 C5 C4 C7 -177(2) . . . . ? C3 C4 C7 C15 61.6(18) . . . . ? C3D C4 C7 C15 107(3) . . . . ? C5D C4 C7 C15 -50(2) . . . . ? C5 C4 C7 C15 -123.8(17) . . . . ? C3 C4 C7 C12 -177.9(16) . . . . ? C3D C4 C7 C12 -133(3) . . . . ? C5D C4 C7 C12 71(2) . . . . ? C5 C4 C7 C12 -3(2) . . . . ? C3 C4 C7 C8 -58.0(18) . . . . ? C3D C4 C7 C8 -13(4) . . . . ? C5D C4 C7 C8 -169(2) . . . . ? C5 C4 C7 C8 116.6(17) . . . . ? C4 C7 C8 C9 179.8(8) . . . . ? C15 C7 C8 C9 58.2(11) . . . . ? C12 C7 C8 C9 -59.5(11) . . . . ? C7 C8 C9 C13 -57.6(10) . . . . ? C7 C8 C9 C17 179.4(8) . . . . ? C7 C8 C9 C10 59.7(11) . . . . ? C13 C9 C10 C11 57.9(12) . . . . ? C8 C9 C10 C11 -59.9(11) . . . . ? C17 C9 C10 C11 -179.4(8) . . . . ? C9 C10 C11 C14 -57.6(12) . . . . ? C9 C10 C11 C23 179.0(8) . . . . ? C9 C10 C11 C12 59.1(11) . . . . ? C4 C7 C12 C11 179.1(9) . . . . ? C15 C7 C12 C11 -58.8(12) . . . . ? C8 C7 C12 C11 58.5(11) . . . . ? C14 C11 C12 C7 59.7(11) . . . . ? C23 C11 C12 C7 -177.8(9) . . . . ? C10 C11 C12 C7 -58.1(11) . . . . ? C8 C9 C13 C16 58.3(11) . . . . ? C17 C9 C13 C16 180.0(9) . . . . ? C10 C9 C13 C16 -58.7(12) . . . . ? C23 C11 C14 C16 179.1(9) . . . . ? C12 C11 C14 C16 -59.8(11) . . . . ? C10 C11 C14 C16 57.3(12) . . . . ? C4 C7 C15 C16 179.0(8) . . . . ? C12 C7 C15 C16 57.6(12) . . . . ? C8 C7 C15 C16 -60.2(11) . . . . ? C7 C15 C16 C13 60.4(11) . . . . ? C7 C15 C16 C14 -57.7(11) . . . . ? C7 C15 C16 C29 -175.9(9) . . . . ? C9 C13 C16 C15 -59.2(11) . . . . ? C9 C13 C16 C14 58.7(11) . . . . ? C9 C13 C16 C29 177.7(9) . . . . ? C11 C14 C16 C15 59.4(12) . . . . ? C11 C14 C16 C13 -57.9(12) . . . . ? C11 C14 C16 C29 -179.9(9) . . . . ? C13 C9 C17 C22 115.5(12) . . . . ? C8 C9 C17 C22 -123.2(11) . . . . ? C10 C9 C17 C22 -4.9(15) . . . . ? C13 C9 C17 C18 -61.8(13) . . . . ? C8 C9 C17 C18 59.5(13) . . . . ? C10 C9 C17 C18 177.8(10) . . . . ? C22 C17 C18 C19 6.1(18) . . . . ? C9 C17 C18 C19 -176.4(12) . . . . ? C17 C18 C19 C20 0(2) . . . . ? C18 C19 C20 C21 -5(2) . . . . ? C18 C19 C20 P2 175.0(11) . . . . ? O4 P2 C20 C19 -159.8(11) . . . . ? O5 P2 C20 C19 71.9(15) . . . . ? O6 P2 C20 C19 -40.9(13) . . . . ? O4 P2 C20 C21 20.3(12) . . . . ? O5 P2 C20 C21 -108.0(14) . . . . ? O6 P2 C20 C21 139.2(11) . . . . ? C19 C20 C21 C22 4.9(19) . . . . ? P2 C20 C21 C22 -175.2(10) . . . . ? C18 C17 C22 C21 -6.4(18) . . . . ? C9 C17 C22 C21 176.3(11) . . . . ? C20 C21 C22 C17 1(2) . . . . ? C14 C11 C23 C28 2.8(16) . . . . ? C12 C11 C23 C28 -116.8(12) . . . . ? C10 C11 C23 C28 124.3(12) . . . . ? C14 C11 C23 C24 -176.9(11) . . . . ? C12 C11 C23 C24 63.4(14) . . . . ? C10 C11 C23 C24 -55.4(14) . . . . ? C28 C23 C24 C25 -2.5(18) . . . . ? C11 C23 C24 C25 177.2(11) . . . . ? C23 C24 C25 C26 0.0(19) . . . . ? C24 C25 C26 C27 3.0(17) . . . . ? C24 C25 C26 P4 179.3(9) . . . . ? O10 P4 C26 C25 -21.5(11) . . . . ? O12 P4 C26 C25 -149.9(9) . . . . ? O11 P4 C26 C25 95.7(10) . . . . ? O10 P4 C26 C27 154.7(10) . . . . ? O12 P4 C26 C27 26.3(11) . . . . ? O11 P4 C26 C27 -88.1(10) . . . . ? C25 C26 C27 C28 -3.6(17) . . . . ? P4 C26 C27 C28 -179.9(9) . . . . ? C26 C27 C28 C23 1.1(18) . . . . ? C24 C23 C28 C27 1.9(18) . . . . ? C11 C23 C28 C27 -177.8(11) . . . . ? C15 C16 C29 C30 -129.5(11) . . . . ? C13 C16 C29 C30 -8.5(14) . . . . ? C14 C16 C29 C30 111.5(12) . . . . ? C15 C16 C29 C34 59.8(13) . . . . ? C13 C16 C29 C34 -179.2(10) . . . . ? C14 C16 C29 C34 -59.3(13) . . . . ? C34 C29 C30 C31 2.3(17) . . . . ? C16 C29 C30 C31 -168.7(10) . . . . ? C29 C30 C31 C32 -0.2(18) . . . . ? C30 C31 C32 C33 -2.2(18) . . . . ? C30 C31 C32 P3 175.6(9) . . . . ? O7 P3 C32 C31 -158.2(10) . . . . ? O8 P3 C32 C31 78.4(12) . . . . ? O9 P3 C32 C31 -35.4(12) . . . . ? O7 P3 C32 C33 19.7(13) . . . . ? O8 P3 C32 C33 -103.7(11) . . . . ? O9 P3 C32 C33 142.5(10) . . . . ? C31 C32 C33 C34 3(2) . . . . ? P3 C32 C33 C34 -175.3(11) . . . . ? C32 C33 C34 C29 -1(2) . . . . ? C30 C29 C34 C33 -1.9(18) . . . . ? C16 C29 C34 C33 169.5(11) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 24.12 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.960 _refine_diff_density_min -0.954 _refine_diff_density_rms 0.179 # Alert level A # PLAT601_ALERT_2_A Structure Contains Solvent Accessible VOIDS of # 383 A**3 # Answer: Not all the guest molecules in the voids were modeled because of # weak average intensities collected during the diffraction experiment # from a very small crystal.. # # Alert level B # CHEMW03_ALERT_2_B WARNING: The ratio of given/expected molecular weight # as calculated from the _atom_site* data lies outside the range 0.95 <> 1.05 # PLAT043_ALERT_1_B Check Reported Molecular Weight ...........950.47 # # Answer: The molecular weight is given only for the main residue, which # was defined as consists of molecules, directly coordinated to the metal # center (i.e. the guest molecules were not counted) # # THETM01_ALERT_3_B The value of sine(theta_max)/wavelength is less than # 0.575. Calculated sin(theta_max)/wavelength = 0.5750 # # Answer: The relatively low resolution data is explained by weakness # of diffraction on high angles from the avalaible very small crystal # # PLATPLAT430_ALERT_2_B Short Inter D...A Contact O1S .. O11 .. 2.67 Ang. # PLAT430_ALERT_2_B Short Inter D...A Contact O1S .. O9 .. 2.72 Ang. # PLAT430_ALERT_2_B Short Inter D...A Contact O4S .. O15 .. 2.75 Ang. # # Answer: The listed values are not exceptional, but rather typical for # charge assisted O-H---O bonds between phosphates/phosphonates and water.