# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # 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_C3-YZ6 _database_code_depnum_ccdc_archive 'CCDC 814641' #TrackingRef 'C3.cif' _audit_creation_date 2012-10-08T11:05:49-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C84 H72 Gd4 O42' _chemical_formula_sum 'C84 H72 Gd4 O42' _chemical_formula_weight 2382.42 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 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 59.6523(11) _cell_length_b 8.20640(10) _cell_length_c 16.9558(2) _cell_angle_alpha 90 _cell_angle_beta 95.4470(10) _cell_angle_gamma 90 _cell_volume 8262.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 41584 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour white _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.915 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4672 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 3.271 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; 'P. Coppens in Crystallographic Computing ed F.R. Ahmed, S.R. Hall and C.P. Huber, Copenhagen, Munksgaard, (1970) pp 255-270' ; _exptl_absorpt_correction_T_min 0.814 _exptl_absorpt_correction_T_max 0.937 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type 'KappaCCD, Nonius' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0668 _diffrn_reflns_av_unetI/netI 0.062 _diffrn_reflns_number 43753 _diffrn_reflns_limit_h_min -77 _diffrn_reflns_limit_h_max 77 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 27.47 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 9450 _reflns_number_gt 6937 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ; WinGX publication routines (Farrugia, 1999), CRYSCAL (T. Roisnel, local program) ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0345P)^2^+17.6141P] 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_number_reflns 9450 _refine_ls_number_parameters 587 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0653 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.0792 _refine_ls_wR_factor_gt 0.0696 _refine_ls_goodness_of_fit_ref 0.964 _refine_ls_restrained_S_all 0.964 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.84 _refine_diff_density_min -0.821 _refine_diff_density_rms 0.147 _iucr_refine_instructions_details ; .res file for SHELXL : job.res ................................................................. TITL import in C 2/c CELL 0.71073 59.6523 8.2064 16.9558 90.000 95.447 90.000 ZERR 4.00 0.0011 0.0001 0.0002 0.000 0.001 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H O GD UNIT 336 288 168 16 MERG 2 FMAP 2 PLAN 20 SIZE 0.02 0.03 0.06 ACTA BOND $H L.S. 4 WGHT 0.034500 17.614100 FVAR 0.03694 MOLE 1 GD1 4 0.500395 1.193773 1.116673 11.00000 0.01651 0.02897 = 0.02175 -0.00021 0.00316 0.00020 GD2 4 0.739534 0.975145 1.094100 11.00000 0.01731 0.02638 = 0.02293 -0.00002 0.00133 0.00008 O101 3 0.500000 1.053015 1.250000 10.50000 0.02512 0.03145 = 0.02708 0.00000 0.00863 0.00000 O54 3 0.724950 0.764632 1.168905 11.00000 0.01747 0.03577 = 0.03589 0.00641 0.00224 0.00188 O12 3 0.528355 0.697918 0.702347 11.00000 0.02500 0.03693 = 0.02934 -0.00208 -0.00370 0.00351 O14 3 0.733298 0.725816 0.896152 11.00000 0.01741 0.04167 = 0.02979 0.00134 0.00143 0.00661 O15 3 0.716653 0.841615 0.993724 11.00000 0.02217 0.04814 = 0.02943 -0.00808 0.00161 -0.00587 O102 3 0.499840 1.495609 1.104508 11.00000 0.04601 0.03481 = 0.03578 -0.00076 0.00159 -0.00073 O11 3 0.533772 0.725911 0.833641 11.00000 0.02263 0.05007 = 0.02835 0.00258 0.00610 0.00671 O203 3 0.757930 1.001299 0.969490 11.00000 0.04245 0.03463 = 0.03652 -0.00550 0.01189 -0.00732 O34 3 0.719132 1.207974 1.030188 11.00000 0.01951 0.03586 = 0.03641 0.00865 0.00498 0.00133 O35 3 0.701664 1.071733 1.116290 11.00000 0.03201 0.03787 = 0.03097 0.00993 0.00609 0.01008 O33 3 0.618111 1.305121 0.883955 11.00000 0.01810 0.08860 = 0.04281 0.03003 0.00103 -0.00691 O52 3 0.528891 0.982926 1.119358 11.00000 0.02859 0.05072 = 0.03170 0.00460 0.00164 0.01685 O202 3 0.767521 1.181878 1.106936 11.00000 0.03438 0.04942 = 0.02823 -0.00117 0.00195 -0.01557 O31 3 0.521644 1.243166 1.008810 11.00000 0.03710 0.03687 = 0.03949 -0.00262 0.02073 0.00126 O13 3 0.634018 0.759265 0.730834 11.00000 0.01344 0.10905 = 0.03333 -0.00320 0.00087 -0.00278 O51 3 0.533919 0.861194 1.236542 11.00000 0.03047 0.05591 = 0.03236 0.00472 0.00688 0.01461 O55 3 0.711685 0.857682 1.278610 11.00000 0.02739 0.05474 = 0.03165 0.00471 0.00000 -0.00396 O103 3 0.474505 1.288424 1.001228 11.00000 0.04260 0.07167 = 0.03102 0.00625 -0.01012 -0.00867 O201 3 0.745333 1.059620 1.232633 11.00000 0.04880 0.06080 = 0.03000 -0.01039 0.00660 -0.02428 O32 3 0.520618 1.031326 0.927485 11.00000 0.02750 0.04025 = 0.04449 -0.00625 0.00927 -0.01363 C15 1 0.611923 0.751482 0.748567 11.00000 0.01675 0.04577 = 0.03465 -0.00608 -0.00020 -0.00210 C51 1 0.539954 0.894163 1.169393 11.00000 0.02122 0.03403 = 0.03428 -0.00960 0.00044 0.00197 C11 1 0.541100 0.714777 0.766677 11.00000 0.02393 0.02203 = 0.03283 -0.00004 0.00478 0.00227 C13 1 0.573925 0.769206 0.689867 11.00000 0.02285 0.04800 = 0.02269 0.00476 0.00163 0.00632 AFIX 43 H13 2 0.563835 0.787271 0.645473 11.00000 -1.20000 AFIX 0 C22 1 0.715860 0.778276 0.925805 11.00000 0.01899 0.02836 = 0.02864 0.00125 0.00246 -0.00190 C52 1 0.561709 0.822262 1.147078 11.00000 0.01879 0.03316 = 0.03048 -0.00067 0.00100 0.00021 C21 1 0.693754 0.764642 0.877940 11.00000 0.02044 0.02989 = 0.02262 -0.00202 0.00000 -0.00344 O53 3 0.621319 0.629053 1.080767 11.00000 0.01860 0.07497 = 0.07024 -0.04049 0.00098 0.00951 C16 1 0.604513 0.702299 0.819628 11.00000 0.02159 0.04476 = 0.02753 -0.00007 -0.00469 0.00262 AFIX 43 H16 2 0.614715 0.675810 0.862626 11.00000 -1.20000 AFIX 0 C32 1 0.553790 1.192802 0.941455 11.00000 0.01977 0.03064 = 0.02420 0.00248 -0.00140 0.00003 C42 1 0.700718 1.164233 1.058089 11.00000 0.01984 0.02551 = 0.03070 -0.00306 0.00212 0.00050 C14 1 0.596812 0.786563 0.684338 11.00000 0.02363 0.05710 = 0.02682 0.00621 0.00308 -0.00120 AFIX 43 H14 2 0.601978 0.821946 0.637200 11.00000 -1.20000 AFIX 0 C43 1 0.658869 1.153210 1.043333 11.00000 0.02430 0.04002 = 0.03075 0.00795 0.00510 0.00044 AFIX 43 H43 2 0.659521 1.091815 1.089596 11.00000 -1.20000 AFIX 0 C18 1 0.652731 0.757111 0.785315 11.00000 0.01632 0.04992 = 0.03377 0.00403 -0.00270 -0.00515 C60 1 0.681785 0.651707 1.111780 11.00000 0.02757 0.03756 = 0.03658 -0.00318 0.00774 0.00284 AFIX 43 H60 2 0.693961 0.613409 1.086758 11.00000 -1.20000 AFIX 0 C31 1 0.530339 1.151809 0.960222 11.00000 0.02480 0.03186 = 0.02370 0.00867 0.00172 0.00062 C33 1 0.564597 1.093314 0.890993 11.00000 0.02727 0.03295 = 0.03052 -0.00534 0.00391 -0.00047 AFIX 43 H33 2 0.557192 1.002621 0.868295 11.00000 -1.20000 AFIX 0 C12 1 0.565884 0.724984 0.761233 11.00000 0.01603 0.02746 = 0.02752 -0.00374 0.00184 0.00104 C62 1 0.708605 0.791228 1.211658 11.00000 0.02305 0.02578 = 0.03207 0.01219 -0.00310 -0.00025 C55 1 0.601819 0.696945 1.106279 11.00000 0.01730 0.04132 = 0.05104 -0.02115 -0.00010 0.00529 C44 1 0.638267 1.184592 1.001463 11.00000 0.01768 0.05189 = 0.03848 0.00779 0.00657 -0.00464 AFIX 43 H44 2 0.625059 1.145404 1.019617 11.00000 -1.20000 AFIX 0 C59 1 0.660074 0.613962 1.081162 11.00000 0.02422 0.04182 = 0.04025 -0.01487 0.00641 0.00405 AFIX 43 H59 2 0.657673 0.549378 1.036081 11.00000 -1.20000 AFIX 0 C63 1 0.667170 0.804087 1.214737 11.00000 0.02899 0.04732 = 0.03039 -0.00626 0.00556 -0.00027 AFIX 43 H63 2 0.669547 0.868499 1.259884 11.00000 -1.20000 AFIX 0 C57 1 0.573141 0.707204 1.194580 11.00000 0.03282 0.03906 = 0.03761 0.00565 0.00442 0.00459 AFIX 43 H57 2 0.567247 0.671737 1.240441 11.00000 -1.20000 AFIX 0 C36 1 0.587024 1.360826 0.960227 11.00000 0.03366 0.04372 = 0.03608 0.00027 -0.00123 -0.01389 AFIX 43 H36 2 0.594724 1.449298 0.983954 11.00000 -1.20000 AFIX 0 C61 1 0.685484 0.745941 1.179295 11.00000 0.02185 0.03154 = 0.02890 0.00674 0.00698 0.00031 C54 1 0.590859 0.813623 1.057915 11.00000 0.03066 0.04567 = 0.04329 -0.00284 0.01032 -0.00279 AFIX 43 H54 2 0.596945 0.849926 1.012561 11.00000 -1.20000 AFIX 0 C58 1 0.642080 0.672181 1.117559 11.00000 0.01491 0.03954 = 0.04587 -0.00409 -0.00276 0.00388 C37 1 0.565183 1.325995 0.976488 11.00000 0.03737 0.03259 = 0.03282 -0.00470 0.00663 -0.00418 AFIX 43 H37 2 0.558105 1.392233 1.011086 11.00000 -1.20000 AFIX 0 C35 1 0.597126 1.261514 0.908078 11.00000 0.01645 0.05598 = 0.03569 0.01585 -0.00395 -0.00049 C19 1 0.671475 0.682267 0.758999 11.00000 0.02410 0.06470 = 0.02981 -0.01531 0.00194 -0.00143 AFIX 43 H19 2 0.670345 0.628540 0.710491 11.00000 -1.20000 AFIX 0 C34 1 0.586459 1.128174 0.874041 11.00000 0.02480 0.04378 = 0.03816 -0.00065 0.00846 0.00419 AFIX 43 H34 2 0.593703 1.061636 0.840024 11.00000 -1.20000 AFIX 0 C38 1 0.637508 1.274621 0.932493 11.00000 0.01686 0.04499 = 0.02899 -0.00135 -0.00109 -0.00126 C39 1 0.656867 1.337994 0.906338 11.00000 0.02673 0.03701 = 0.03119 0.00799 0.00375 -0.00174 AFIX 43 H39 2 0.656085 1.401299 0.860667 11.00000 -1.20000 AFIX 0 C53 1 0.570619 0.874989 1.078678 11.00000 0.02881 0.04319 = 0.03800 0.00629 0.00757 0.00821 AFIX 43 H53 2 0.562898 0.952342 1.046510 11.00000 -1.20000 AFIX 0 C20 1 0.691871 0.687786 0.805163 11.00000 0.02047 0.05745 = 0.03315 -0.00982 0.00189 0.00667 AFIX 43 H20 2 0.704479 0.639093 0.786940 11.00000 -1.20000 AFIX 0 C17 1 0.581346 0.693344 0.825302 11.00000 0.02616 0.03476 = 0.02655 -0.00094 0.00424 0.00255 AFIX 43 H17 2 0.576183 0.665302 0.873550 11.00000 -1.20000 AFIX 0 C23 1 0.674760 0.836849 0.904262 11.00000 0.02145 0.04104 = 0.03309 -0.01140 0.00343 -0.00325 AFIX 43 H23 2 0.675820 0.887205 0.953612 11.00000 -1.20000 AFIX 0 C24 1 0.654190 0.835226 0.858181 11.00000 0.02253 0.05174 = 0.04201 -0.01227 0.00416 0.00467 AFIX 43 H24 2 0.641635 0.885617 0.875902 11.00000 -1.20000 AFIX 0 C64 1 0.645384 0.768584 1.184537 11.00000 0.02225 0.06107 = 0.04670 -0.01913 0.00864 -0.00046 AFIX 43 H64 2 0.633179 0.808761 1.208797 11.00000 -1.20000 AFIX 0 C41 1 0.678653 1.213165 1.016511 11.00000 0.02021 0.03115 = 0.03040 -0.00102 0.00623 0.00298 C40 1 0.677405 1.307270 0.948084 11.00000 0.02121 0.03965 = 0.03183 0.00244 0.00586 0.00072 AFIX 43 H40 2 0.690486 1.349718 0.930372 11.00000 -1.20000 AFIX 0 C56 1 0.593281 0.644417 1.174417 11.00000 0.03724 0.04047 = 0.05038 0.00556 -0.00069 0.01481 AFIX 43 H56 2 0.601020 0.567221 1.206632 11.00000 -1.20000 AFIX 0 MOLE 2 OW1 3 0.500000 0.639049 0.250000 10.50000 0.07181 0.03160 = 0.04859 0.00000 0.02034 0.00000 HKLF 4 REM import in C 2/c REM R1 = 0.0355 for 6937 Fo > 4sig(Fo) and 0.0653 for all 9450 data REM 587 parameters refined using 0 restraints END WGHT 0.0325 6.4510 REM Highest difference peak 0.84, deepest hole -0.82, 1-sigma level 0.15 Q1 1 0.5230 1.3156 0.9307 11.00000 0.05 0.84 Q2 1 0.7610 1.0924 0.9099 11.00000 0.05 0.83 Q3 1 0.7604 0.8645 0.9027 11.00000 0.05 0.77 Q4 1 0.4999 1.1571 0.8825 11.00000 0.05 0.72 Q5 1 0.7701 1.0628 0.9558 11.00000 0.05 0.72 Q6 1 0.5026 1.5616 1.1447 11.00000 0.05 0.72 Q7 1 0.7545 1.1244 1.2514 11.00000 0.05 0.69 Q8 1 0.7388 1.0184 0.8618 11.00000 0.05 0.69 Q9 1 0.5144 1.0028 1.2430 11.00000 0.05 0.66 Q10 1 0.7791 1.2220 1.1449 11.00000 0.05 0.65 Q11 1 0.4992 1.5405 1.0767 11.00000 0.05 0.65 Q12 1 0.7705 1.2375 1.0628 11.00000 0.05 0.63 Q13 1 0.4808 1.2933 1.0099 11.00000 0.05 0.62 Q14 1 0.7384 1.1189 1.2234 11.00000 0.05 0.59 Q15 1 0.4882 1.5920 1.1012 11.00000 0.05 0.58 Q16 1 0.5973 0.8806 0.9807 11.00000 0.05 0.58 Q17 1 0.7534 1.0264 0.9743 11.00000 0.05 0.57 Q18 1 0.4669 1.3120 0.9588 11.00000 0.05 0.57 Q19 1 0.7566 0.9574 0.9317 11.00000 0.05 0.57 Q20 1 0.7086 0.4859 1.0198 11.00000 0.05 0.56 ; #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Gd1 Gd 0.500395(4) 1.19377(3) 1.116673(12) 0.02232(7) Uani 1 1 d . . . Gd2 Gd 0.739534(4) 0.97514(3) 1.094100(12) 0.02225(7) Uani 1 1 d . . . O101 O 0.5 1.0530(5) 1.25 0.0275(10) Uani 1 2 d S . . O54 O 0.72495(5) 0.7646(4) 1.16891(18) 0.0297(7) Uani 1 1 d . . . O12 O 0.52835(5) 0.6979(4) 0.70235(18) 0.0308(8) Uani 1 1 d . . . O14 O 0.73330(5) 0.7258(4) 0.89615(17) 0.0297(7) Uani 1 1 d . . . O15 O 0.71665(5) 0.8416(4) 0.99372(18) 0.0333(8) Uani 1 1 d . . . O102 O 0.49984(6) 1.4956(4) 1.1045(2) 0.0390(9) Uani 1 1 d . . . O11 O 0.53377(5) 0.7259(4) 0.83364(18) 0.0334(8) Uani 1 1 d . . . O203 O 0.75793(6) 1.0013(4) 0.96949(19) 0.0373(8) Uani 1 1 d . . . O34 O 0.71913(5) 1.2080(4) 1.03019(18) 0.0304(8) Uani 1 1 d . . . O35 O 0.70166(5) 1.0717(4) 1.11629(18) 0.0334(8) Uani 1 1 d . . . O33 O 0.61811(6) 1.3051(5) 0.8840(2) 0.0500(11) Uani 1 1 d . . . O52 O 0.52889(6) 0.9829(4) 1.11936(19) 0.0371(8) Uani 1 1 d . . . O202 O 0.76752(6) 1.1819(4) 1.10694(18) 0.0374(9) Uani 1 1 d . . . O31 O 0.52164(6) 1.2432(4) 1.00881(19) 0.0367(8) Uani 1 1 d . . . O13 O 0.63402(6) 0.7593(6) 0.7308(2) 0.0520(11) Uani 1 1 d . . . O51 O 0.53392(6) 0.8612(4) 1.23654(19) 0.0393(9) Uani 1 1 d . . . O55 O 0.71169(5) 0.8577(4) 1.27861(19) 0.0381(8) Uani 1 1 d . . . O103 O 0.47450(6) 1.2884(5) 1.00123(19) 0.0493(10) Uani 1 1 d . . . O201 O 0.74533(6) 1.0596(5) 1.23263(19) 0.0464(10) Uani 1 1 d . . . O32 O 0.52062(6) 1.0313(4) 0.9275(2) 0.0370(8) Uani 1 1 d . . . C15 C 0.61192(8) 0.7515(6) 0.7486(3) 0.0326(11) Uani 1 1 d . . . C51 C 0.53995(8) 0.8942(6) 1.1694(3) 0.0300(11) Uani 1 1 d . . . C11 C 0.54110(8) 0.7148(5) 0.7667(3) 0.0261(10) Uani 1 1 d . . . C13 C 0.57393(8) 0.7692(6) 0.6899(3) 0.0312(11) Uani 1 1 d . . . H13 H 0.5638 0.7873 0.6455 0.037 Uiso 1 1 calc R . . C22 C 0.71586(7) 0.7783(5) 0.9258(3) 0.0253(10) Uani 1 1 d . . . C52 C 0.56171(7) 0.8223(6) 1.1471(3) 0.0276(10) Uani 1 1 d . . . C21 C 0.69375(7) 0.7646(6) 0.8779(2) 0.0244(10) Uani 1 1 d . . . O53 O 0.62132(6) 0.6291(5) 1.0808(2) 0.0548(11) Uani 1 1 d . . . C16 C 0.60451(8) 0.7023(6) 0.8196(3) 0.0317(11) Uani 1 1 d . . . H16 H 0.6147 0.6758 0.8626 0.038 Uiso 1 1 calc R . . C32 C 0.55379(7) 1.1928(5) 0.9415(2) 0.0251(10) Uani 1 1 d . . . C42 C 0.70072(8) 1.1642(5) 1.0581(3) 0.0254(10) Uani 1 1 d . . . C14 C 0.59681(8) 0.7866(6) 0.6843(3) 0.0358(12) Uani 1 1 d . . . H14 H 0.602 0.8219 0.6372 0.043 Uiso 1 1 calc R . . C43 C 0.65887(8) 1.1532(6) 1.0433(3) 0.0315(11) Uani 1 1 d . . . H43 H 0.6595 1.0918 1.0896 0.038 Uiso 1 1 calc R . . C18 C 0.65273(8) 0.7571(7) 0.7853(3) 0.0337(11) Uani 1 1 d . . . C60 C 0.68178(8) 0.6517(6) 1.1118(3) 0.0336(11) Uani 1 1 d . . . H60 H 0.694 0.6134 1.0868 0.04 Uiso 1 1 calc R . . C31 C 0.53034(8) 1.1518(6) 0.9602(3) 0.0268(10) Uani 1 1 d . . . C33 C 0.56460(8) 1.0933(6) 0.8910(3) 0.0302(11) Uani 1 1 d . . . H33 H 0.5572 1.0026 0.8683 0.036 Uiso 1 1 calc R . . C12 C 0.56588(7) 0.7250(5) 0.7612(2) 0.0237(10) Uani 1 1 d . . . C62 C 0.70860(8) 0.7912(5) 1.2117(3) 0.0273(11) Uani 1 1 d . . . C55 C 0.60182(8) 0.6969(6) 1.1063(3) 0.0368(13) Uani 1 1 d . . . C44 C 0.63827(8) 1.1846(6) 1.0015(3) 0.0358(12) Uani 1 1 d . . . H44 H 0.6251 1.1454 1.0196 0.043 Uiso 1 1 calc R . . C59 C 0.66007(8) 0.6140(6) 1.0812(3) 0.0352(12) Uani 1 1 d . . . H59 H 0.6577 0.5494 1.0361 0.042 Uiso 1 1 calc R . . C63 C 0.66717(8) 0.8041(6) 1.2147(3) 0.0354(12) Uani 1 1 d . . . H63 H 0.6695 0.8685 1.2599 0.042 Uiso 1 1 calc R . . C57 C 0.57314(9) 0.7072(6) 1.1946(3) 0.0364(12) Uani 1 1 d . . . H57 H 0.5672 0.6717 1.2404 0.044 Uiso 1 1 calc R . . C36 C 0.58702(9) 1.3608(7) 0.9602(3) 0.0381(12) Uani 1 1 d . . . H36 H 0.5947 1.4493 0.984 0.046 Uiso 1 1 calc R . . C61 C 0.68548(8) 0.7459(6) 1.1793(3) 0.0271(10) Uani 1 1 d . . . C54 C 0.59086(9) 0.8136(6) 1.0579(3) 0.0394(13) Uani 1 1 d . . . H54 H 0.5969 0.8499 1.0126 0.047 Uiso 1 1 calc R . . C58 C 0.64208(8) 0.6722(6) 1.1176(3) 0.0338(12) Uani 1 1 d . . . C37 C 0.56518(9) 1.3260(6) 0.9765(3) 0.0340(12) Uani 1 1 d . . . H37 H 0.5581 1.3922 1.0111 0.041 Uiso 1 1 calc R . . C35 C 0.59713(8) 1.2615(7) 0.9081(3) 0.0364(12) Uani 1 1 d . . . C19 C 0.67147(8) 0.6823(7) 0.7590(3) 0.0396(13) Uani 1 1 d . . . H19 H 0.6703 0.6285 0.7105 0.047 Uiso 1 1 calc R . . C34 C 0.58646(8) 1.1282(6) 0.8740(3) 0.0352(12) Uani 1 1 d . . . H34 H 0.5937 1.0616 0.84 0.042 Uiso 1 1 calc R . . C38 C 0.63751(8) 1.2746(6) 0.9325(3) 0.0305(11) Uani 1 1 d . . . C39 C 0.65687(8) 1.3380(6) 0.9063(3) 0.0316(11) Uani 1 1 d . . . H39 H 0.6561 1.4013 0.8607 0.038 Uiso 1 1 calc R . . C53 C 0.57062(8) 0.8750(6) 1.0787(3) 0.0364(12) Uani 1 1 d . . . H53 H 0.5629 0.9523 1.0465 0.044 Uiso 1 1 calc R . . C20 C 0.69187(8) 0.6878(6) 0.8052(3) 0.0371(13) Uani 1 1 d . . . H20 H 0.7045 0.6391 0.7869 0.044 Uiso 1 1 calc R . . C17 C 0.58135(8) 0.6933(6) 0.8253(3) 0.0290(11) Uani 1 1 d . . . H17 H 0.5762 0.6653 0.8736 0.035 Uiso 1 1 calc R . . C23 C 0.67476(8) 0.8368(6) 0.9043(3) 0.0318(11) Uani 1 1 d . . . H23 H 0.6758 0.8872 0.9536 0.038 Uiso 1 1 calc R . . C24 C 0.65419(8) 0.8352(7) 0.8582(3) 0.0387(13) Uani 1 1 d . . . H24 H 0.6416 0.8856 0.8759 0.046 Uiso 1 1 calc R . . C64 C 0.64538(9) 0.7686(7) 1.1845(3) 0.0430(14) Uani 1 1 d . . . H64 H 0.6332 0.8088 1.2088 0.052 Uiso 1 1 calc R . . C41 C 0.67865(8) 1.2132(6) 1.0165(3) 0.0270(10) Uani 1 1 d . . . C40 C 0.67741(8) 1.3073(6) 0.9481(3) 0.0307(11) Uani 1 1 d . . . H40 H 0.6905 1.3497 0.9304 0.037 Uiso 1 1 calc R . . C56 C 0.59328(9) 0.6444(7) 1.1744(3) 0.0430(13) Uani 1 1 d . . . H56 H 0.601 0.5672 1.2066 0.052 Uiso 1 1 calc R . . OW1 O 0.5 0.6390(6) 0.25 0.0497(14) Uani 1 2 d S . . 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 Gd1 0.01651(12) 0.02897(13) 0.02175(11) -0.00021(9) 0.00316(8) 0.00020(9) Gd2 0.01731(12) 0.02638(13) 0.02293(12) -0.00002(9) 0.00133(9) 0.00008(9) O101 0.025(3) 0.031(3) 0.027(2) 0 0.0086(19) 0 O54 0.0175(17) 0.0358(19) 0.0359(18) 0.0064(14) 0.0022(14) 0.0019(14) O12 0.0250(18) 0.037(2) 0.0293(17) -0.0021(14) -0.0037(14) 0.0035(15) O14 0.0174(17) 0.042(2) 0.0298(17) 0.0013(14) 0.0014(13) 0.0066(15) O15 0.0222(18) 0.048(2) 0.0294(18) -0.0081(15) 0.0016(14) -0.0059(16) O102 0.046(2) 0.035(2) 0.0358(18) -0.0008(14) 0.0016(16) -0.0007(17) O11 0.0226(18) 0.050(2) 0.0283(18) 0.0026(15) 0.0061(14) 0.0067(16) O203 0.042(2) 0.035(2) 0.0365(19) -0.0055(14) 0.0119(16) -0.0073(16) O34 0.0195(17) 0.036(2) 0.0364(18) 0.0086(14) 0.0050(14) 0.0013(15) O35 0.032(2) 0.038(2) 0.0310(18) 0.0099(15) 0.0061(14) 0.0101(16) O33 0.0181(19) 0.089(3) 0.043(2) 0.0300(19) 0.0010(16) -0.0069(19) O52 0.029(2) 0.051(2) 0.0317(18) 0.0046(16) 0.0016(15) 0.0168(17) O202 0.034(2) 0.049(2) 0.0282(17) -0.0012(15) 0.0019(15) -0.0156(17) O31 0.037(2) 0.037(2) 0.0395(19) -0.0026(16) 0.0207(16) 0.0013(17) O13 0.0134(18) 0.109(3) 0.0333(19) -0.003(2) 0.0009(15) -0.003(2) O51 0.030(2) 0.056(2) 0.0324(19) 0.0047(16) 0.0069(15) 0.0146(18) O55 0.027(2) 0.055(2) 0.0317(18) 0.0047(16) 0.0000(15) -0.0040(17) O103 0.043(2) 0.072(3) 0.0310(19) 0.0063(17) -0.0101(16) -0.009(2) O201 0.049(2) 0.061(3) 0.0300(18) -0.0104(17) 0.0066(16) -0.024(2) O32 0.028(2) 0.040(2) 0.044(2) -0.0062(16) 0.0093(16) -0.0136(17) C15 0.017(2) 0.046(3) 0.035(3) -0.006(2) 0.000(2) -0.002(2) C51 0.021(3) 0.034(3) 0.034(3) -0.010(2) 0.000(2) 0.002(2) C11 0.024(3) 0.022(3) 0.033(3) 0.0000(19) 0.005(2) 0.002(2) C13 0.023(3) 0.048(3) 0.023(2) 0.005(2) 0.0016(19) 0.006(2) C22 0.019(2) 0.028(3) 0.029(2) 0.0012(19) 0.0025(19) -0.002(2) C52 0.019(2) 0.033(3) 0.030(2) -0.001(2) 0.0010(19) 0.000(2) C21 0.020(2) 0.030(3) 0.023(2) -0.0020(18) 0.0000(18) -0.003(2) O53 0.0186(19) 0.075(3) 0.070(3) -0.040(2) 0.0010(18) 0.0095(19) C16 0.022(3) 0.045(3) 0.028(2) 0.000(2) -0.005(2) 0.003(2) C32 0.020(2) 0.031(3) 0.024(2) 0.0025(18) -0.0014(18) 0.000(2) C42 0.020(2) 0.026(3) 0.031(2) -0.0031(19) 0.0021(19) 0.000(2) C14 0.024(3) 0.057(4) 0.027(2) 0.006(2) 0.003(2) -0.001(2) C43 0.024(3) 0.040(3) 0.031(3) 0.008(2) 0.005(2) 0.000(2) C18 0.016(3) 0.050(3) 0.034(3) 0.004(2) -0.003(2) -0.005(2) C60 0.028(3) 0.038(3) 0.037(3) -0.003(2) 0.008(2) 0.003(2) C31 0.025(3) 0.032(3) 0.024(2) 0.009(2) 0.0017(19) 0.001(2) C33 0.027(3) 0.033(3) 0.031(2) -0.005(2) 0.004(2) 0.000(2) C12 0.016(2) 0.027(3) 0.028(2) -0.0037(18) 0.0018(18) 0.0010(19) C62 0.023(3) 0.026(3) 0.032(3) 0.012(2) -0.003(2) 0.000(2) C55 0.017(3) 0.041(3) 0.051(3) -0.021(2) 0.000(2) 0.005(2) C44 0.018(3) 0.052(3) 0.038(3) 0.008(2) 0.007(2) -0.005(2) C59 0.024(3) 0.042(3) 0.040(3) -0.015(2) 0.006(2) 0.004(2) C63 0.029(3) 0.047(3) 0.030(3) -0.006(2) 0.006(2) 0.000(2) C57 0.033(3) 0.039(3) 0.038(3) 0.006(2) 0.004(2) 0.005(2) C36 0.034(3) 0.044(3) 0.036(3) 0.000(2) -0.001(2) -0.014(3) C61 0.022(3) 0.032(3) 0.029(2) 0.007(2) 0.007(2) 0.000(2) C54 0.031(3) 0.046(3) 0.043(3) -0.003(2) 0.010(2) -0.003(3) C58 0.015(2) 0.040(3) 0.046(3) -0.004(2) -0.003(2) 0.004(2) C37 0.037(3) 0.033(3) 0.033(3) -0.005(2) 0.007(2) -0.004(2) C35 0.016(3) 0.056(4) 0.036(3) 0.016(2) -0.004(2) 0.000(2) C19 0.024(3) 0.065(4) 0.030(3) -0.015(2) 0.002(2) -0.001(3) C34 0.025(3) 0.044(3) 0.038(3) -0.001(2) 0.008(2) 0.004(2) C38 0.017(2) 0.045(3) 0.029(3) -0.001(2) -0.0011(19) -0.001(2) C39 0.027(3) 0.037(3) 0.031(3) 0.008(2) 0.004(2) -0.002(2) C53 0.029(3) 0.043(3) 0.038(3) 0.006(2) 0.008(2) 0.008(2) C20 0.020(3) 0.057(4) 0.033(3) -0.010(2) 0.002(2) 0.007(2) C17 0.026(3) 0.035(3) 0.027(2) -0.0009(19) 0.004(2) 0.003(2) C23 0.021(3) 0.041(3) 0.033(3) -0.011(2) 0.003(2) -0.003(2) C24 0.023(3) 0.052(4) 0.042(3) -0.012(2) 0.004(2) 0.005(2) C64 0.022(3) 0.061(4) 0.047(3) -0.019(3) 0.009(2) 0.000(3) C41 0.020(2) 0.031(3) 0.030(2) -0.0010(19) 0.0062(19) 0.003(2) C40 0.021(3) 0.040(3) 0.032(3) 0.002(2) 0.006(2) 0.001(2) C56 0.037(3) 0.040(3) 0.050(3) 0.006(3) -0.001(3) 0.015(3) OW1 0.072(4) 0.032(3) 0.049(3) 0 0.020(3) 0 #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Gd1 O12 2.285(3) 6_576 ? Gd1 O32 2.316(3) 5_677 ? Gd1 O31 2.357(3) . ? Gd1 O11 2.372(3) 5_677 ? Gd1 O52 2.423(3) . ? Gd1 O102 2.486(3) . ? Gd1 O103 2.499(3) . ? Gd1 O101 2.541(2) . ? Gd2 O14 2.307(3) 7_667 ? Gd2 O15 2.349(3) . ? Gd2 O54 2.358(3) . ? Gd2 O202 2.376(3) . ? Gd2 O201 2.442(3) . ? Gd2 O35 2.457(3) . ? Gd2 O34 2.461(3) . ? Gd2 O203 2.481(3) . ? Gd2 C42 2.806(4) . ? O101 Gd1 2.5407(19) 2_657 ? O54 C62 1.288(5) . ? O12 C11 1.277(5) . ? O12 Gd1 2.285(3) 6_575 ? O14 C22 1.273(5) . ? O14 Gd2 2.307(3) 7_667 ? O15 C22 1.260(5) . ? O11 C11 1.258(5) . ? O11 Gd1 2.372(3) 5_677 ? O34 C42 1.288(5) . ? O35 C42 1.242(5) . ? O33 C38 1.378(6) . ? O33 C35 1.400(6) . ? O52 C51 1.257(6) . ? O31 C31 1.261(5) . ? O13 C18 1.380(6) . ? O13 C15 1.381(5) . ? O51 C51 1.256(5) . ? O55 C62 1.257(5) . ? O32 C31 1.249(5) . ? O32 Gd1 2.317(3) 5_677 ? C15 C14 1.377(7) . ? C15 C16 1.382(6) . ? C51 C52 1.506(6) . ? C11 C12 1.492(6) . ? C13 C14 1.385(6) . ? C13 C12 1.391(6) . ? C13 H13 0.93 . ? C22 C21 1.486(6) . ? C52 C57 1.379(7) . ? C52 C53 1.390(6) . ? C21 C20 1.381(6) . ? C21 C23 1.389(6) . ? O53 C58 1.379(6) . ? O53 C55 1.395(5) . ? C16 C17 1.396(6) . ? C16 H16 0.93 . ? C32 C33 1.385(6) . ? C32 C37 1.390(6) . ? C32 C31 1.502(6) . ? C42 C41 1.488(6) . ? C14 H14 0.93 . ? C43 C44 1.384(7) . ? C43 C41 1.394(6) . ? C43 H43 0.93 . ? C18 C19 1.386(7) . ? C18 C24 1.387(7) . ? C60 C61 1.382(6) . ? C60 C59 1.384(7) . ? C60 H60 0.93 . ? C33 C34 1.391(6) . ? C33 H33 0.93 . ? C12 C17 1.381(6) . ? C62 C61 1.482(6) . ? C55 C56 1.375(7) . ? C55 C54 1.384(7) . ? C44 C38 1.380(6) . ? C44 H44 0.93 . ? C59 C58 1.374(6) . ? C59 H59 0.93 . ? C63 C61 1.381(6) . ? C63 C64 1.382(7) . ? C63 H63 0.93 . ? C57 C56 1.380(7) . ? C57 H57 0.93 . ? C36 C35 1.382(7) . ? C36 C37 1.387(7) . ? C36 H36 0.93 . ? C54 C53 1.384(7) . ? C54 H54 0.93 . ? C58 C64 1.383(7) . ? C37 H37 0.93 . ? C35 C34 1.366(7) . ? C19 C20 1.384(7) . ? C19 H19 0.93 . ? C34 H34 0.93 . ? C38 C39 1.378(6) . ? C39 C40 1.379(6) . ? C39 H39 0.93 . ? C53 H53 0.93 . ? C20 H20 0.93 . ? C17 H17 0.93 . ? C23 C24 1.391(7) . ? C23 H23 0.93 . ? C24 H24 0.93 . ? C64 H64 0.93 . ? C41 C40 1.390(6) . ? C40 H40 0.93 . ? C56 H56 0.93 . ? 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 O12 Gd1 O32 148.81(12) 6_576 5_677 ? O12 Gd1 O31 90.72(12) 6_576 . ? O32 Gd1 O31 101.57(11) 5_677 . ? O12 Gd1 O11 105.44(11) 6_576 5_677 ? O32 Gd1 O11 83.08(12) 5_677 5_677 ? O31 Gd1 O11 140.48(11) . 5_677 ? O12 Gd1 O52 78.31(12) 6_576 . ? O32 Gd1 O52 78.09(12) 5_677 . ? O31 Gd1 O52 73.11(11) . . ? O11 Gd1 O52 144.77(11) 5_677 . ? O12 Gd1 O102 70.63(11) 6_576 . ? O32 Gd1 O102 139.94(12) 5_677 . ? O31 Gd1 O102 76.59(11) . . ? O11 Gd1 O102 75.37(12) 5_677 . ? O52 Gd1 O102 135.81(12) . . ? O12 Gd1 O103 137.43(12) 6_576 . ? O32 Gd1 O103 73.71(13) 5_677 . ? O31 Gd1 O103 71.14(12) . . ? O11 Gd1 O103 72.77(11) 5_677 . ? O52 Gd1 O103 128.09(12) . . ? O102 Gd1 O103 67.85(12) . . ? O12 Gd1 O101 71.28(9) 6_576 . ? O32 Gd1 O101 82.80(11) 5_677 . ? O31 Gd1 O101 145.05(9) . . ? O11 Gd1 O101 74.30(9) 5_677 . ? O52 Gd1 O101 74.00(10) . . ? O102 Gd1 O101 121.72(12) . . ? O103 Gd1 O101 141.35(8) . . ? O14 Gd2 O15 94.26(11) 7_667 . ? O14 Gd2 O54 74.35(11) 7_667 . ? O15 Gd2 O54 80.17(11) . . ? O14 Gd2 O202 91.21(12) 7_667 . ? O15 Gd2 O202 138.97(11) . . ? O54 Gd2 O202 139.99(11) . . ? O14 Gd2 O201 95.72(12) 7_667 . ? O15 Gd2 O201 148.08(11) . . ? O54 Gd2 O201 73.52(11) . . ? O202 Gd2 O201 71.03(11) . . ? O14 Gd2 O35 150.41(11) 7_667 . ? O15 Gd2 O35 77.41(11) . . ? O54 Gd2 O35 76.25(10) . . ? O202 Gd2 O35 113.83(12) . . ? O201 Gd2 O35 79.01(12) . . ? O14 Gd2 O34 154.32(10) 7_667 . ? O15 Gd2 O34 79.29(11) . . ? O54 Gd2 O34 127.84(10) . . ? O202 Gd2 O34 78.45(11) . . ? O201 Gd2 O34 102.84(12) . . ? O35 Gd2 O34 52.65(10) . . ? O14 Gd2 O203 76.02(11) 7_667 . ? O15 Gd2 O203 72.36(11) . . ? O54 Gd2 O203 137.49(11) . . ? O202 Gd2 O203 69.66(11) . . ? O201 Gd2 O203 139.55(11) . . ? O35 Gd2 O203 126.16(11) . . ? O34 Gd2 O203 78.35(11) . . ? O14 Gd2 C42 166.03(12) 7_667 . ? O15 Gd2 C42 71.92(12) . . ? O54 Gd2 C42 100.56(12) . . ? O202 Gd2 C42 100.56(13) . . ? O201 Gd2 C42 95.22(13) . . ? O35 Gd2 C42 26.24(11) . . ? O34 Gd2 C42 27.30(11) . . ? O203 Gd2 C42 100.92(12) . . ? Gd1 O101 Gd1 125.92(17) 2_657 . ? C62 O54 Gd2 121.1(3) . . ? C11 O12 Gd1 147.2(3) . 6_575 ? C22 O14 Gd2 144.0(3) . 7_667 ? C22 O15 Gd2 145.4(3) . . ? C11 O11 Gd1 136.4(3) . 5_677 ? C42 O34 Gd2 91.4(3) . . ? C42 O35 Gd2 92.8(3) . . ? C38 O33 C35 120.2(4) . . ? C51 O52 Gd1 138.5(3) . . ? C31 O31 Gd1 133.6(3) . . ? C18 O13 C15 125.6(4) . . ? C31 O32 Gd1 171.4(3) . 5_677 ? C14 C15 O13 112.6(4) . . ? C14 C15 C16 120.7(4) . . ? O13 C15 C16 126.4(4) . . ? O51 C51 O52 124.0(4) . . ? O51 C51 C52 118.1(4) . . ? O52 C51 C52 117.9(4) . . ? O11 C11 O12 123.3(4) . . ? O11 C11 C12 118.9(4) . . ? O12 C11 C12 117.8(4) . . ? C14 C13 C12 120.6(4) . . ? C14 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? O15 C22 O14 122.6(4) . . ? O15 C22 C21 119.0(4) . . ? O14 C22 C21 118.4(4) . . ? C57 C52 C53 119.6(4) . . ? C57 C52 C51 120.8(4) . . ? C53 C52 C51 119.6(4) . . ? C20 C21 C23 118.8(4) . . ? C20 C21 C22 121.0(4) . . ? C23 C21 C22 120.1(4) . . ? C58 O53 C55 119.8(4) . . ? C15 C16 C17 118.4(4) . . ? C15 C16 H16 120.8 . . ? C17 C16 H16 120.8 . . ? C33 C32 C37 119.3(4) . . ? C33 C32 C31 119.8(4) . . ? C37 C32 C31 120.9(4) . . ? O35 C42 O34 119.1(4) . . ? O35 C42 C41 120.8(4) . . ? O34 C42 C41 119.9(4) . . ? O35 C42 Gd2 61.0(2) . . ? O34 C42 Gd2 61.2(2) . . ? C41 C42 Gd2 157.9(3) . . ? C15 C14 C13 120.0(4) . . ? C15 C14 H14 120 . . ? C13 C14 H14 120 . . ? C44 C43 C41 120.3(4) . . ? C44 C43 H43 119.8 . . ? C41 C43 H43 119.8 . . ? O13 C18 C19 114.6(4) . . ? O13 C18 C24 124.7(5) . . ? C19 C18 C24 120.5(4) . . ? C61 C60 C59 120.4(4) . . ? C61 C60 H60 119.8 . . ? C59 C60 H60 119.8 . . ? O32 C31 O31 123.9(4) . . ? O32 C31 C32 119.0(4) . . ? O31 C31 C32 117.0(4) . . ? C32 C33 C34 120.4(5) . . ? C32 C33 H33 119.8 . . ? C34 C33 H33 119.8 . . ? C17 C12 C13 118.3(4) . . ? C17 C12 C11 122.2(4) . . ? C13 C12 C11 119.6(4) . . ? O55 C62 O54 121.9(4) . . ? O55 C62 C61 119.6(4) . . ? O54 C62 C61 118.5(4) . . ? C56 C55 C54 121.5(5) . . ? C56 C55 O53 121.4(5) . . ? C54 C55 O53 117.0(5) . . ? C38 C44 C43 119.4(4) . . ? C38 C44 H44 120.3 . . ? C43 C44 H44 120.3 . . ? C58 C59 C60 119.8(5) . . ? C58 C59 H59 120.1 . . ? C60 C59 H59 120.1 . . ? C61 C63 C64 121.4(5) . . ? C61 C63 H63 119.3 . . ? C64 C63 H63 119.3 . . ? C52 C57 C56 120.3(5) . . ? C52 C57 H57 119.8 . . ? C56 C57 H57 119.8 . . ? C35 C36 C37 118.7(5) . . ? C35 C36 H36 120.6 . . ? C37 C36 H36 120.6 . . ? C63 C61 C60 118.9(4) . . ? C63 C61 C62 119.9(4) . . ? C60 C61 C62 121.1(4) . . ? C55 C54 C53 118.4(5) . . ? C55 C54 H54 120.8 . . ? C53 C54 H54 120.8 . . ? C59 C58 O53 114.5(4) . . ? C59 C58 C64 120.8(5) . . ? O53 C58 C64 124.8(4) . . ? C36 C37 C32 120.5(5) . . ? C36 C37 H37 119.8 . . ? C32 C37 H37 119.8 . . ? C34 C35 C36 121.9(5) . . ? C34 C35 O33 118.4(5) . . ? C36 C35 O33 119.5(5) . . ? C20 C19 C18 119.8(4) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C35 C34 C33 119.0(5) . . ? C35 C34 H34 120.5 . . ? C33 C34 H34 120.5 . . ? C39 C38 O33 114.9(4) . . ? C39 C38 C44 120.9(4) . . ? O33 C38 C44 124.2(4) . . ? C38 C39 C40 119.8(4) . . ? C38 C39 H39 120.1 . . ? C40 C39 H39 120.1 . . ? C54 C53 C52 120.7(5) . . ? C54 C53 H53 119.6 . . ? C52 C53 H53 119.6 . . ? C21 C20 C19 120.9(4) . . ? C21 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? C12 C17 C16 121.8(4) . . ? C12 C17 H17 119.1 . . ? C16 C17 H17 119.1 . . ? C21 C23 C24 121.2(4) . . ? C21 C23 H23 119.4 . . ? C24 C23 H23 119.4 . . ? C18 C24 C23 118.8(4) . . ? C18 C24 H24 120.6 . . ? C23 C24 H24 120.6 . . ? C63 C64 C58 118.7(5) . . ? C63 C64 H64 120.6 . . ? C58 C64 H64 120.6 . . ? C40 C41 C43 119.2(4) . . ? C40 C41 C42 121.4(4) . . ? C43 C41 C42 119.2(4) . . ? C39 C40 C41 120.3(4) . . ? C39 C40 H40 119.8 . . ? C41 C40 H40 119.8 . . ? C55 C56 C57 119.5(5) . . ? C55 C56 H56 120.3 . . ? C57 C56 H56 120.3 . . ? data_C2-2009-48 _database_code_depnum_ccdc_archive 'CCDC 814642' #TrackingRef 'C2.cif' _audit_creation_date 2012-10-08T10:32:15-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C42 H42 Gd2 O24' _chemical_formula_sum 'C42 H42 Gd2 O24' _chemical_formula_weight 1245.26 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/a 1' _symmetry_space_group_name_Hall '-P 2yab' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 9.94740(10) _cell_length_b 15.6416(2) _cell_length_c 28.7511(4) _cell_angle_alpha 90 _cell_angle_beta 95.1170(10) _cell_angle_gamma 90 _cell_volume 4455.65(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 44729 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 30.03 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 1.856 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2456 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 3.042 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; 'P. Coppens in Crystallographic Computing ed F.R. Ahmed, S.R. Hall and C.P. Huber, Copenhagen, Munksgaard, (1970) pp 255-270' ; _exptl_absorpt_correction_T_min 0.507 _exptl_absorpt_correction_T_max 0.913 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type 'KappaCCD, Nonius' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0569 _diffrn_reflns_av_unetI/netI 0.0472 _diffrn_reflns_number 45415 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 30.03 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.988 _reflns_number_total 12839 _reflns_number_gt 10447 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ; WinGX publication routines (Farrugia, 1999), CRYSCAL (T. Roisnel, local program) ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0532P)^2^+5.8335P] 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_number_reflns 12839 _refine_ls_number_parameters 613 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0549 _refine_ls_R_factor_gt 0.0404 _refine_ls_wR_factor_ref 0.1057 _refine_ls_wR_factor_gt 0.0985 _refine_ls_goodness_of_fit_ref 1.04 _refine_ls_restrained_S_all 1.04 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.123 _refine_diff_density_min -1.889 _refine_diff_density_rms 0.2 _iucr_refine_instructions_details ; .res file for SHELXL : job.res ................................................................. TITL import in P 21/a CELL 0.71073 9.9474 15.6416 28.7511 90.000 95.117 90.000 ZERR 4.00 0.0001 0.0002 0.0004 0.000 0.001 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, - Z SFAC C H O GD UNIT 168 168 96 8 MERG 2 FMAP 2 PLAN 20 SIZE 0.03 0.10 0.22 ACTA BOND $H L.S. 5 WGHT 0.053200 5.833500 FVAR 0.18273 GD1 4 0.994015 0.744248 0.488141 11.00000 0.02105 0.03293 = 0.01625 0.00068 -0.00028 0.00112 GD2 4 1.055639 0.688887 0.993769 11.00000 0.02322 0.02528 = 0.01754 -0.00077 0.00277 -0.00093 O201 3 1.152004 0.549543 0.976858 11.00000 0.04548 0.02804 = 0.04185 -0.00360 0.00517 0.00231 O202 3 1.163430 0.827142 1.011690 11.00000 0.03547 0.03303 = 0.03286 -0.00074 0.00263 -0.00548 O203 3 1.242293 0.659930 1.050596 11.00000 0.03102 0.03684 = 0.03634 0.00333 -0.00562 -0.00648 O35 3 1.468451 0.903087 0.055288 11.00000 0.03664 0.02911 = 0.02904 0.00136 0.00908 -0.00173 O34 3 1.459072 0.764451 0.064932 11.00000 0.03249 0.02827 = 0.02638 0.00042 0.00650 -0.00277 O52 3 0.837885 0.789632 0.536436 11.00000 0.03321 0.06942 = 0.01897 -0.00049 0.00679 0.01230 O51 3 1.129573 0.709445 0.557575 11.00000 0.02524 0.05521 = 0.02565 -0.00029 -0.00208 0.00607 O11 3 0.885260 0.858998 0.441727 11.00000 0.03114 0.03978 = 0.03041 0.01161 0.00017 0.00352 O102 3 0.887350 0.616531 0.522666 11.00000 0.04098 0.05026 = 0.06042 0.00778 0.00479 -0.00843 O14 3 0.611450 1.113920 0.051530 11.00000 0.04407 0.03765 = 0.02884 0.00824 -0.00314 0.00761 O32 3 1.151214 0.779476 0.436965 11.00000 0.04143 0.05097 = 0.02290 0.00692 0.01067 0.00730 O54 3 0.901311 0.790735 0.961551 11.00000 0.03689 0.03594 = 0.02237 0.00356 -0.00216 0.00379 O101 3 1.095949 0.883087 0.517094 11.00000 0.03356 0.04056 = 0.04291 -0.00811 -0.00227 0.00054 O31 3 0.859498 0.677626 0.427344 11.00000 0.03520 0.04789 = 0.03530 -0.00856 -0.01137 0.00466 O103 3 1.123638 0.613781 0.470209 11.00000 0.03355 0.03949 = 0.04177 -0.00758 -0.00085 0.00572 O55 3 0.686592 0.785533 0.932057 11.00000 0.02861 0.04202 = 0.02826 -0.00296 0.00635 -0.00001 C31 1 1.237902 0.809539 0.412331 11.00000 0.03107 0.03000 = 0.01956 -0.00032 0.00076 0.00544 O15 3 0.772819 1.015758 0.060374 11.00000 0.03290 0.04547 = 0.04016 -0.00480 0.00119 0.00298 O12 3 1.013150 0.975195 0.437275 11.00000 0.03887 0.04887 = 0.03670 0.00248 -0.00536 -0.01108 O33 3 1.086823 0.878742 0.221985 11.00000 0.04541 0.12137 = 0.01802 0.01267 0.00952 0.02880 C51 1 0.754640 0.795194 0.566831 11.00000 0.02768 0.02845 = 0.01696 -0.00034 0.00041 0.00003 C33 1 1.067948 0.812299 0.342119 11.00000 0.02633 0.05759 = 0.02230 0.00414 0.00481 0.00067 AFIX 43 H33 2 1.004007 0.789185 0.360212 11.00000 -1.20000 AFIX 0 O53 3 0.991325 0.848366 0.749952 11.00000 0.03661 0.11077 = 0.01696 -0.00284 0.00089 -0.02315 C58 1 0.934788 0.838235 0.791636 11.00000 0.02837 0.04532 = 0.01805 0.00023 -0.00091 -0.00030 C12 1 0.833083 0.952982 0.378162 11.00000 0.03471 0.04104 = 0.02337 0.00804 0.00239 -0.00054 O13 3 0.570515 1.025915 0.264443 11.00000 0.04890 0.14476 = 0.03333 0.03940 -0.00033 0.01453 C22 1 0.680542 1.059102 0.076000 11.00000 0.03155 0.02669 = 0.03166 0.00122 -0.00804 -0.00728 C21 1 0.650934 1.047176 0.125446 11.00000 0.03009 0.02872 = 0.03112 0.00415 -0.00784 -0.00393 C62 1 0.810853 0.795687 0.927826 11.00000 0.03201 0.02474 = 0.02144 0.00056 0.00472 0.00381 C54 1 0.805576 0.875940 0.691517 11.00000 0.05249 0.05790 = 0.02361 -0.01197 0.00369 0.00516 AFIX 43 H54 2 0.766843 0.914638 0.710935 11.00000 -1.20000 AFIX 0 C60 1 0.977981 0.849915 0.874689 11.00000 0.02286 0.03693 = 0.02019 -0.00075 -0.00033 -0.00236 AFIX 43 H60 2 1.035099 0.865125 0.900750 11.00000 -1.20000 AFIX 0 OW1 3 0.203044 0.510001 0.546607 11.00000 0.12329 0.04523 = 0.08656 0.00592 -0.04175 0.00232 C63 1 0.768370 0.791914 0.840902 11.00000 0.02479 0.04612 = 0.02387 -0.00109 0.00060 -0.00758 AFIX 43 H63 2 0.683280 0.769600 0.844532 11.00000 -1.20000 AFIX 0 C61 1 0.851982 0.813920 0.880169 11.00000 0.02246 0.02846 = 0.02010 -0.00048 0.00230 0.00269 C59 1 1.017428 0.862838 0.830353 11.00000 0.02556 0.04214 = 0.02441 0.00204 0.00019 -0.00681 AFIX 43 H59 2 1.100260 0.888298 0.826610 11.00000 -1.20000 AFIX 0 C11 1 0.918084 0.927354 0.421748 11.00000 0.02830 0.03651 = 0.02481 0.00234 0.00134 0.00306 C55 1 0.920477 0.831274 0.707444 11.00000 0.03072 0.06212 = 0.01805 -0.00191 0.00198 -0.01253 C32 1 1.197326 0.830704 0.362414 11.00000 0.02543 0.03692 = 0.02110 0.00095 0.00390 0.00463 C64 1 0.808680 0.802405 0.796136 11.00000 0.02858 0.05879 = 0.01932 -0.00460 -0.00296 -0.00952 AFIX 43 H64 2 0.752903 0.785933 0.769991 11.00000 -1.20000 AFIX 0 C41 1 1.352418 0.850915 0.119101 11.00000 0.03498 0.03263 = 0.01937 -0.00256 0.00503 -0.00044 C43 1 1.298226 0.929748 0.128501 11.00000 0.06871 0.04350 = 0.03452 0.00538 0.02579 0.01266 AFIX 43 H43 2 1.319432 0.977073 0.110989 11.00000 -1.20000 AFIX 0 C20 1 0.552414 1.095359 0.144575 11.00000 0.04241 0.05058 = 0.02749 0.01089 -0.00442 0.01085 AFIX 43 H20 2 0.501077 1.133687 0.125713 11.00000 -1.20000 AFIX 0 C56 1 0.978659 0.774000 0.678688 11.00000 0.03508 0.07794 = 0.02734 0.00201 -0.00724 0.01254 AFIX 43 H56 2 1.054118 0.742676 0.689944 11.00000 -1.20000 AFIX 0 C23 1 0.724907 0.989901 0.154631 11.00000 0.04289 0.03954 = 0.03856 0.00763 -0.00965 0.00525 AFIX 43 H23 2 0.790920 0.956510 0.142568 11.00000 -1.20000 AFIX 0 C44 1 1.212578 0.939276 0.163719 11.00000 0.07849 0.06286 = 0.03564 0.00816 0.02841 0.03346 AFIX 43 H44 2 1.175833 0.992476 0.169533 11.00000 -1.20000 AFIX 0 C18 1 0.604298 1.030591 0.219018 11.00000 0.04026 0.07102 = 0.02847 0.02096 -0.00397 -0.00278 C19 1 0.528953 1.087581 0.191113 11.00000 0.04551 0.07248 = 0.03087 0.01499 0.00180 0.01311 AFIX 43 H19 2 0.462868 1.120573 0.203410 11.00000 -1.20000 AFIX 0 C52 1 0.809425 0.807613 0.616230 11.00000 0.02403 0.03944 = 0.01762 -0.00198 0.00102 -0.00292 C39 1 1.238804 0.790878 0.182269 11.00000 0.08620 0.06300 = 0.03984 0.01134 0.03413 0.00410 AFIX 43 H39 2 1.220014 0.744510 0.200874 11.00000 -1.20000 AFIX 0 C38 1 1.182796 0.870190 0.189667 11.00000 0.03990 0.07928 = 0.01894 0.00406 0.00731 0.01104 C17 1 0.734829 0.897477 0.358882 11.00000 0.04775 0.04918 = 0.03445 0.01123 -0.00806 -0.00652 AFIX 43 H17 2 0.724226 0.844575 0.372860 11.00000 -1.20000 AFIX 0 C24 1 0.702410 0.981658 0.200938 11.00000 0.05199 0.05256 = 0.04151 0.02396 -0.01257 0.00625 AFIX 43 H24 2 0.753152 0.943259 0.219943 11.00000 -1.20000 AFIX 0 C35 1 1.128512 0.862081 0.268438 11.00000 0.04218 0.06271 = 0.01816 0.00460 0.00876 0.01469 C36 1 1.257559 0.881420 0.287875 11.00000 0.03557 0.07437 = 0.02992 0.01056 0.00966 0.00001 AFIX 43 H36 2 1.320838 0.904680 0.269563 11.00000 -1.20000 AFIX 0 C42 1 1.432301 0.839020 0.078435 11.00000 0.02637 0.02910 = 0.01785 -0.00077 -0.00025 -0.00240 OW3 3 0.547983 0.528377 0.047010 11.00000 0.06912 0.11539 = 0.17967 0.08275 0.00308 -0.02154 OW2 3 0.990536 0.514686 0.592700 11.00000 0.13279 0.11938 = 0.11497 0.00976 -0.01426 -0.02177 C53 1 0.748597 0.862503 0.646307 11.00000 0.03585 0.05189 = 0.02354 -0.00376 -0.00017 0.01103 AFIX 43 H53 2 0.668952 0.890406 0.635939 11.00000 -1.20000 AFIX 0 C40 1 1.323764 0.781374 0.146568 11.00000 0.07638 0.04135 = 0.03258 0.00459 0.02138 0.01055 AFIX 43 H40 2 1.361372 0.728264 0.141134 11.00000 -1.20000 AFIX 0 C16 1 0.652478 0.918735 0.319522 11.00000 0.04240 0.07323 = 0.03556 0.00987 -0.00410 -0.00873 AFIX 43 H16 2 0.588521 0.880292 0.306452 11.00000 -1.20000 AFIX 0 C15 1 0.666946 0.998078 0.299985 11.00000 0.04058 0.09460 = 0.03219 0.02221 -0.00165 0.00166 C57 1 0.924349 0.763399 0.633123 11.00000 0.03427 0.06081 = 0.02602 -0.00419 0.00286 0.01265 AFIX 43 H57 2 0.965416 0.726127 0.613537 11.00000 -1.20000 AFIX 0 C37 1 1.290859 0.865759 0.334629 11.00000 0.03039 0.05455 = 0.02780 0.00480 0.00433 -0.00209 AFIX 43 H37 2 1.377175 0.878811 0.347835 11.00000 -1.20000 AFIX 0 C14 1 0.767218 1.054104 0.317205 11.00000 0.07450 0.08693 = 0.06667 0.05366 -0.01433 -0.01460 AFIX 43 H14 2 0.779054 1.106350 0.302679 11.00000 -1.20000 AFIX 0 C34 1 1.034394 0.828242 0.295293 11.00000 0.02699 0.07780 = 0.02287 0.00125 -0.00180 0.00448 AFIX 43 H34 2 0.947914 0.816031 0.281945 11.00000 -1.20000 AFIX 0 C13 1 0.849363 1.030569 0.356509 11.00000 0.05436 0.06453 = 0.05339 0.02905 -0.01086 -0.01864 AFIX 43 H13 2 0.916737 1.067703 0.368543 11.00000 -1.20000 HKLF 4 REM import in P 21/a REM R1 = 0.0404 for 10447 Fo > 4sig(Fo) and 0.0549 for all 12839 data REM 613 parameters refined using 0 restraints END WGHT 0.0531 5.8376 REM Highest difference peak 1.12, deepest hole -1.89, 1-sigma level 0.20 Q1 1 0.1121 0.5093 0.5600 11.00000 0.05 1.12 Q2 1 1.0834 0.6795 1.0206 11.00000 0.05 0.90 Q3 1 1.0156 0.6921 0.9646 11.00000 0.05 0.88 Q4 1 1.0271 0.7432 0.5176 11.00000 0.05 0.88 Q5 1 0.9705 0.7403 0.4608 11.00000 0.05 0.82 Q6 1 1.1939 0.5212 0.9978 11.00000 0.05 0.80 Q7 1 1.0791 0.9179 0.5397 11.00000 0.05 0.79 Q8 1 1.0763 0.6487 0.9599 11.00000 0.05 0.77 Q9 1 1.0795 0.5245 0.9522 11.00000 0.05 0.74 Q10 1 1.3132 0.6883 1.0488 11.00000 0.05 0.74 Q11 1 0.6121 0.8116 0.9486 11.00000 0.05 0.73 Q12 1 0.5628 0.5691 -0.0043 11.00000 0.05 0.73 Q13 1 1.1707 0.5818 0.5015 11.00000 0.05 0.71 Q14 1 1.1158 0.4999 0.9715 11.00000 0.05 0.70 Q15 1 1.0809 0.9229 0.4894 11.00000 0.05 0.68 Q16 1 0.4874 0.4915 0.0483 11.00000 0.05 0.68 Q17 1 0.4994 0.5369 0.0193 11.00000 0.05 0.65 Q18 1 1.0187 0.8851 0.5318 11.00000 0.05 0.64 Q19 1 0.9625 0.7883 0.5206 11.00000 0.05 0.63 Q20 1 1.4910 0.8096 0.0385 11.00000 0.05 0.63 ; #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Gd1 Gd 0.994015(17) 0.744248(12) 0.488141(6) 0.02353(6) Uani 1 1 d . . . Gd2 Gd 1.055639(17) 0.688887(12) 0.993769(6) 0.02196(5) Uani 1 1 d . . . O201 O 1.1520(3) 0.54954(19) 0.97686(11) 0.0384(7) Uani 1 1 d . . . O202 O 1.1634(3) 0.82714(19) 1.01169(11) 0.0338(6) Uani 1 1 d . . . O203 O 1.2423(3) 0.6599(2) 1.05060(11) 0.0352(7) Uani 1 1 d . . . O35 O 1.4685(3) 0.90309(18) 0.05529(10) 0.0312(6) Uani 1 1 d . . . O34 O 1.4591(3) 0.76445(18) 0.06493(10) 0.0288(6) Uani 1 1 d . . . O52 O 0.8379(3) 0.7896(2) 0.53644(10) 0.0403(8) Uani 1 1 d . . . O51 O 1.1296(3) 0.7094(2) 0.55757(10) 0.0356(7) Uani 1 1 d . . . O11 O 0.8853(3) 0.8590(2) 0.44173(10) 0.0339(6) Uani 1 1 d . . . O102 O 0.8873(3) 0.6165(2) 0.52267(14) 0.0505(9) Uani 1 1 d . . . O14 O 0.6115(3) 1.1139(2) 0.05153(10) 0.0372(7) Uani 1 1 d . . . O32 O 1.1512(3) 0.7795(2) 0.43696(10) 0.0380(7) Uani 1 1 d . . . O54 O 0.9013(3) 0.79073(19) 0.96155(10) 0.0320(6) Uani 1 1 d . . . O101 O 1.0959(3) 0.8831(2) 0.51709(12) 0.0394(7) Uani 1 1 d . . . O31 O 0.8595(3) 0.6776(2) 0.42734(11) 0.0403(7) Uani 1 1 d . . . O103 O 1.1236(3) 0.6138(2) 0.47021(11) 0.0385(7) Uani 1 1 d . . . O55 O 0.6866(3) 0.7855(2) 0.93206(10) 0.0327(6) Uani 1 1 d . . . C31 C 1.2379(4) 0.8095(3) 0.41233(13) 0.0270(8) Uani 1 1 d . . . O15 O 0.7728(3) 1.0158(2) 0.06037(11) 0.0396(7) Uani 1 1 d . . . O12 O 1.0131(3) 0.9752(2) 0.43727(11) 0.0420(8) Uani 1 1 d . . . O33 O 1.0868(3) 0.8787(3) 0.22198(11) 0.0612(12) Uani 1 1 d . . . C51 C 0.7546(4) 0.7952(2) 0.56683(13) 0.0245(7) Uani 1 1 d . . . C33 C 1.0679(4) 0.8123(3) 0.34212(15) 0.0352(10) Uani 1 1 d . . . H33 H 1.004 0.7892 0.3602 0.042 Uiso 1 1 calc R . . O53 O 0.9913(3) 0.8484(3) 0.74995(11) 0.0549(10) Uani 1 1 d . . . C58 C 0.9348(4) 0.8382(3) 0.79164(13) 0.0308(8) Uani 1 1 d . . . C12 C 0.8331(4) 0.9530(3) 0.37816(14) 0.0331(9) Uani 1 1 d . . . O13 O 0.5705(4) 1.0259(4) 0.26444(13) 0.0759(15) Uani 1 1 d . . . C22 C 0.6805(4) 1.0591(3) 0.07600(15) 0.0306(8) Uani 1 1 d . . . C21 C 0.6509(4) 1.0472(3) 0.12545(15) 0.0306(8) Uani 1 1 d . . . C62 C 0.8109(4) 0.7957(2) 0.92783(13) 0.0259(7) Uani 1 1 d . . . C54 C 0.8056(5) 0.8759(3) 0.69152(16) 0.0446(11) Uani 1 1 d . . . H54 H 0.7668 0.9146 0.7109 0.054 Uiso 1 1 calc R . . C60 C 0.9780(4) 0.8499(3) 0.87469(13) 0.0268(8) Uani 1 1 d . . . H60 H 1.0351 0.8651 0.9008 0.032 Uiso 1 1 calc R . . OW1 O 0.2030(6) 0.5100(3) 0.54661(18) 0.0881(16) Uani 1 1 d . . . C63 C 0.7684(4) 0.7919(3) 0.84090(14) 0.0317(9) Uani 1 1 d . . . H63 H 0.6833 0.7696 0.8445 0.038 Uiso 1 1 calc R . . C61 C 0.8520(4) 0.8139(2) 0.88017(13) 0.0237(7) Uani 1 1 d . . . C59 C 1.0174(4) 0.8628(3) 0.83035(14) 0.0308(8) Uani 1 1 d . . . H59 H 1.1003 0.8883 0.8266 0.037 Uiso 1 1 calc R . . C11 C 0.9181(4) 0.9274(3) 0.42175(14) 0.0299(8) Uani 1 1 d . . . C55 C 0.9205(4) 0.8313(3) 0.70744(14) 0.0370(10) Uani 1 1 d . . . C32 C 1.1973(4) 0.8307(3) 0.36241(13) 0.0277(8) Uani 1 1 d . . . C64 C 0.8087(4) 0.8024(3) 0.79614(14) 0.0359(10) Uani 1 1 d . . . H64 H 0.7529 0.7859 0.77 0.043 Uiso 1 1 calc R . . C41 C 1.3524(4) 0.8509(3) 0.11910(13) 0.0288(8) Uani 1 1 d . . . C43 C 1.2982(6) 0.9297(3) 0.12850(17) 0.0476(12) Uani 1 1 d . . . H43 H 1.3194 0.9771 0.111 0.057 Uiso 1 1 calc R . . C20 C 0.5524(5) 1.0954(3) 0.14458(15) 0.0406(10) Uani 1 1 d . . . H20 H 0.5011 1.1337 0.1257 0.049 Uiso 1 1 calc R . . C56 C 0.9787(5) 0.7740(4) 0.67869(17) 0.0474(12) Uani 1 1 d . . . H56 H 1.0541 0.7427 0.6899 0.057 Uiso 1 1 calc R . . C23 C 0.7249(5) 0.9899(3) 0.15463(16) 0.0411(10) Uani 1 1 d . . . H23 H 0.7909 0.9565 0.1426 0.049 Uiso 1 1 calc R . . C44 C 1.2126(6) 0.9393(4) 0.16372(18) 0.0576(16) Uani 1 1 d . . . H44 H 1.1758 0.9925 0.1695 0.069 Uiso 1 1 calc R . . C18 C 0.6043(5) 1.0306(4) 0.21902(16) 0.0470(12) Uani 1 1 d . . . C19 C 0.5290(5) 1.0876(4) 0.19111(17) 0.0497(13) Uani 1 1 d . . . H19 H 0.4629 1.1206 0.2034 0.06 Uiso 1 1 calc R . . C52 C 0.8094(4) 0.8076(3) 0.61623(13) 0.0271(8) Uani 1 1 d . . . C39 C 1.2388(7) 0.7909(4) 0.1823(2) 0.0613(16) Uani 1 1 d . . . H39 H 1.22 0.7445 0.2009 0.074 Uiso 1 1 calc R . . C38 C 1.1828(5) 0.8702(4) 0.18967(15) 0.0458(12) Uani 1 1 d . . . C17 C 0.7348(5) 0.8975(3) 0.35888(17) 0.0445(11) Uani 1 1 d . . . H17 H 0.7242 0.8446 0.3729 0.053 Uiso 1 1 calc R . . C24 C 0.7024(5) 0.9817(4) 0.20094(18) 0.0497(13) Uani 1 1 d . . . H24 H 0.7532 0.9433 0.2199 0.06 Uiso 1 1 calc R . . C35 C 1.1285(5) 0.8621(3) 0.26844(14) 0.0407(11) Uani 1 1 d . . . C36 C 1.2576(5) 0.8814(4) 0.28788(16) 0.0462(12) Uani 1 1 d . . . H36 H 1.3208 0.9047 0.2696 0.055 Uiso 1 1 calc R . . C42 C 1.4323(4) 0.8390(3) 0.07844(13) 0.0246(7) Uani 1 1 d . . . OW3 O 0.5480(5) 0.5284(4) 0.0470(3) 0.122(2) Uani 1 1 d . . . OW2 O 0.9905(7) 0.5147(4) 0.5927(2) 0.124(2) Uani 1 1 d . . . C53 C 0.7486(4) 0.8625(3) 0.64631(15) 0.0373(10) Uani 1 1 d . . . H53 H 0.669 0.8904 0.6359 0.045 Uiso 1 1 calc R . . C40 C 1.3238(6) 0.7814(3) 0.14657(17) 0.0491(13) Uani 1 1 d . . . H40 H 1.3614 0.7283 0.1411 0.059 Uiso 1 1 calc R . . C16 C 0.6525(5) 0.9187(4) 0.31952(18) 0.0509(13) Uani 1 1 d . . . H16 H 0.5885 0.8803 0.3065 0.061 Uiso 1 1 calc R . . C15 C 0.6669(5) 0.9981(4) 0.29998(17) 0.0561(15) Uani 1 1 d . . . C57 C 0.9243(5) 0.7634(3) 0.63312(16) 0.0404(11) Uani 1 1 d . . . H57 H 0.9654 0.7261 0.6135 0.048 Uiso 1 1 calc R . . C37 C 1.2909(4) 0.8658(3) 0.33463(15) 0.0375(10) Uani 1 1 d . . . H37 H 1.3772 0.8788 0.3478 0.045 Uiso 1 1 calc R . . C14 C 0.7672(7) 1.0541(5) 0.3172(2) 0.077(2) Uani 1 1 d . . . H14 H 0.7791 1.1064 0.3027 0.093 Uiso 1 1 calc R . . C34 C 1.0344(4) 0.8282(4) 0.29529(15) 0.0428(11) Uani 1 1 d . . . H34 H 0.9479 0.816 0.2819 0.051 Uiso 1 1 calc R . . C13 C 0.8494(6) 1.0306(4) 0.3565(2) 0.0584(15) Uani 1 1 d . . . H13 H 0.9167 1.0677 0.3685 0.07 Uiso 1 1 calc R . . 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 Gd1 0.02105(9) 0.03293(11) 0.01625(9) 0.00068(7) -0.00028(6) 0.00112(6) Gd2 0.02322(9) 0.02528(10) 0.01754(9) -0.00077(6) 0.00277(6) -0.00093(6) O201 0.0455(17) 0.0280(16) 0.0418(18) -0.0036(13) 0.0052(14) 0.0023(12) O202 0.0355(15) 0.0330(16) 0.0329(16) -0.0007(12) 0.0026(12) -0.0055(12) O203 0.0310(14) 0.0368(17) 0.0363(17) 0.0033(13) -0.0056(12) -0.0065(12) O35 0.0366(15) 0.0291(15) 0.0290(15) 0.0014(12) 0.0091(12) -0.0017(11) O34 0.0325(14) 0.0283(15) 0.0264(14) 0.0004(11) 0.0065(12) -0.0028(11) O52 0.0332(15) 0.069(2) 0.0190(14) -0.0005(14) 0.0068(12) 0.0123(15) O51 0.0252(13) 0.055(2) 0.0256(15) -0.0003(14) -0.0021(11) 0.0061(13) O11 0.0311(14) 0.0398(17) 0.0304(15) 0.0116(13) 0.0002(12) 0.0035(12) O102 0.0410(18) 0.050(2) 0.060(2) 0.0078(18) 0.0048(16) -0.0084(15) O14 0.0441(17) 0.0376(17) 0.0288(15) 0.0082(13) -0.0031(13) 0.0076(13) O32 0.0414(17) 0.0510(19) 0.0229(14) 0.0069(14) 0.0107(13) 0.0073(14) O54 0.0369(15) 0.0359(16) 0.0224(14) 0.0036(12) -0.0022(11) 0.0038(12) O101 0.0336(15) 0.0406(18) 0.0429(18) -0.0081(14) -0.0023(13) 0.0005(13) O31 0.0352(16) 0.048(2) 0.0353(17) -0.0086(14) -0.0114(13) 0.0047(13) O103 0.0335(15) 0.0395(18) 0.0418(18) -0.0076(14) -0.0009(13) 0.0057(12) O55 0.0286(14) 0.0420(17) 0.0283(15) -0.0030(13) 0.0063(11) 0.0000(12) C31 0.0311(18) 0.030(2) 0.0196(17) -0.0003(14) 0.0008(14) 0.0054(15) O15 0.0329(15) 0.0455(19) 0.0402(17) -0.0048(15) 0.0012(13) 0.0030(13) O12 0.0389(16) 0.049(2) 0.0367(17) 0.0025(15) -0.0054(13) -0.0111(14) O33 0.0454(19) 0.121(4) 0.0180(15) 0.0127(19) 0.0095(14) 0.029(2) C51 0.0277(17) 0.0284(19) 0.0170(16) -0.0003(14) 0.0004(13) 0.0000(14) C33 0.0263(18) 0.058(3) 0.0223(19) 0.0041(18) 0.0048(15) 0.0007(17) O53 0.0366(17) 0.111(3) 0.0170(14) -0.0028(17) 0.0009(12) -0.0232(19) C58 0.0284(18) 0.045(2) 0.0181(17) 0.0002(16) -0.0009(14) -0.0003(16) C12 0.035(2) 0.041(2) 0.0234(19) 0.0080(17) 0.0024(16) -0.0005(17) O13 0.049(2) 0.145(4) 0.0333(19) 0.039(2) -0.0003(17) 0.015(2) C22 0.0315(19) 0.027(2) 0.032(2) 0.0012(16) -0.0080(16) -0.0073(15) C21 0.0301(18) 0.029(2) 0.031(2) 0.0041(16) -0.0078(16) -0.0039(15) C62 0.0320(19) 0.0247(19) 0.0214(17) 0.0006(14) 0.0047(15) 0.0038(14) C54 0.052(3) 0.058(3) 0.024(2) -0.012(2) 0.0037(19) 0.005(2) C60 0.0229(16) 0.037(2) 0.0202(17) -0.0007(15) -0.0003(13) -0.0024(15) OW1 0.123(4) 0.045(3) 0.087(3) 0.006(2) -0.042(3) 0.002(3) C63 0.0248(18) 0.046(2) 0.0239(19) -0.0011(17) 0.0006(15) -0.0076(16) C61 0.0225(16) 0.0285(19) 0.0201(17) -0.0005(14) 0.0023(13) 0.0027(13) C59 0.0256(17) 0.042(2) 0.0244(19) 0.0020(17) 0.0002(14) -0.0068(16) C11 0.0283(18) 0.037(2) 0.0248(19) 0.0023(16) 0.0013(15) 0.0031(16) C55 0.031(2) 0.062(3) 0.0180(18) -0.0019(18) 0.0020(15) -0.0125(19) C32 0.0254(17) 0.037(2) 0.0211(18) 0.0010(15) 0.0039(14) 0.0046(15) C64 0.0286(19) 0.059(3) 0.0193(18) -0.0046(18) -0.0030(15) -0.0095(18) C41 0.0350(19) 0.033(2) 0.0194(17) -0.0026(15) 0.0050(15) -0.0004(16) C43 0.069(3) 0.044(3) 0.035(2) 0.005(2) 0.026(2) 0.013(2) C20 0.042(2) 0.051(3) 0.027(2) 0.011(2) -0.0044(18) 0.011(2) C56 0.035(2) 0.078(4) 0.027(2) 0.002(2) -0.0072(18) 0.013(2) C23 0.043(2) 0.040(3) 0.039(2) 0.008(2) -0.0097(19) 0.0053(19) C44 0.078(4) 0.063(4) 0.036(3) 0.008(2) 0.028(3) 0.033(3) C18 0.040(2) 0.071(4) 0.028(2) 0.021(2) -0.0040(19) -0.003(2) C19 0.046(3) 0.072(4) 0.031(2) 0.015(2) 0.002(2) 0.013(2) C52 0.0240(17) 0.039(2) 0.0176(17) -0.0020(15) 0.0010(13) -0.0029(15) C39 0.086(4) 0.063(4) 0.040(3) 0.011(3) 0.034(3) 0.004(3) C38 0.040(2) 0.079(4) 0.0189(19) 0.004(2) 0.0073(17) 0.011(2) C17 0.048(3) 0.049(3) 0.034(2) 0.011(2) -0.008(2) -0.007(2) C24 0.052(3) 0.053(3) 0.042(3) 0.024(2) -0.013(2) 0.006(2) C35 0.042(2) 0.063(3) 0.0182(18) 0.0046(19) 0.0088(17) 0.015(2) C36 0.036(2) 0.074(4) 0.030(2) 0.011(2) 0.0097(18) 0.000(2) C42 0.0264(17) 0.0291(19) 0.0178(16) -0.0008(14) -0.0002(13) -0.0024(14) OW3 0.069(3) 0.115(5) 0.180(6) 0.083(5) 0.003(4) -0.022(3) OW2 0.133(5) 0.119(5) 0.115(5) 0.010(4) -0.014(4) -0.022(4) C53 0.036(2) 0.052(3) 0.0235(19) -0.0038(19) -0.0002(16) 0.0110(19) C40 0.076(4) 0.041(3) 0.033(2) 0.005(2) 0.021(2) 0.011(3) C16 0.042(3) 0.073(4) 0.036(3) 0.010(3) -0.004(2) -0.009(2) C15 0.041(3) 0.095(5) 0.032(2) 0.022(3) -0.002(2) 0.002(3) C57 0.034(2) 0.061(3) 0.026(2) -0.004(2) 0.0029(17) 0.013(2) C37 0.030(2) 0.055(3) 0.028(2) 0.005(2) 0.0043(16) -0.0021(19) C14 0.075(4) 0.087(5) 0.067(4) 0.054(4) -0.014(3) -0.015(4) C34 0.027(2) 0.078(4) 0.023(2) 0.001(2) -0.0018(16) 0.004(2) C13 0.054(3) 0.065(4) 0.053(3) 0.029(3) -0.011(3) -0.019(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Gd1 O52 2.287(3) . ? Gd1 O32 2.307(3) . ? Gd1 O31 2.348(3) . ? Gd1 O51 2.371(3) . ? Gd1 O11 2.432(3) . ? Gd1 O103 2.492(3) . ? Gd1 O101 2.507(3) . ? Gd1 O102 2.508(3) . ? Gd2 O55 2.327(3) 4_675 ? Gd2 O14 2.334(3) 2_646 ? Gd2 O54 2.345(3) . ? Gd2 O203 2.404(3) . ? Gd2 O201 2.447(3) . ? Gd2 O34 2.448(3) 4_576 ? Gd2 O202 2.448(3) . ? Gd2 O35 2.495(3) 4_576 ? Gd2 C42 2.856(4) 4_576 ? O35 C42 1.272(5) . ? O35 Gd2 2.495(3) 4_674 ? O34 C42 1.265(5) . ? O34 Gd2 2.448(3) 4_674 ? O52 C51 1.259(5) . ? O51 C51 1.251(5) 4_675 ? O11 C11 1.270(5) . ? O14 C22 1.271(5) . ? O14 Gd2 2.334(3) 2_656 ? O32 C31 1.255(5) . ? O54 C62 1.265(5) . ? O31 C31 1.264(5) 4_575 ? O55 C62 1.263(5) . ? O55 Gd2 2.327(3) 4_575 ? C31 O31 1.264(5) 4_675 ? C31 C32 1.493(5) . ? O15 C22 1.256(5) . ? O12 C11 1.256(5) . ? O33 C35 1.387(5) . ? O33 C38 1.397(5) . ? C51 O51 1.251(5) 4_575 ? C51 C52 1.488(5) . ? C33 C34 1.381(6) . ? C33 C32 1.395(6) . ? C33 H33 0.93 . ? O53 C58 1.378(5) . ? O53 C55 1.381(5) . ? C58 C59 1.378(5) . ? C58 C64 1.390(6) . ? C12 C13 1.380(7) . ? C12 C17 1.386(6) . ? C12 C11 1.502(6) . ? O13 C18 1.379(6) . ? O13 C15 1.407(6) . ? C22 C21 1.489(6) . ? C21 C20 1.388(6) . ? C21 C23 1.392(6) . ? C62 C61 1.492(5) . ? C54 C55 1.382(7) . ? C54 C53 1.387(6) . ? C54 H54 0.93 . ? C60 C59 1.382(5) . ? C60 C61 1.396(5) . ? C60 H60 0.93 . ? C63 C61 1.385(5) . ? C63 C64 1.392(6) . ? C63 H63 0.93 . ? C59 H59 0.93 . ? C55 C56 1.381(7) . ? C32 C37 1.392(6) . ? C64 H64 0.93 . ? C41 C43 1.382(6) . ? C41 C40 1.389(6) . ? C41 C42 1.483(5) . ? C43 C44 1.388(6) . ? C43 H43 0.93 . ? C20 C19 1.384(6) . ? C20 H20 0.93 . ? C56 C57 1.382(6) . ? C56 H56 0.93 . ? C23 C24 1.376(7) . ? C23 H23 0.93 . ? C44 C38 1.361(8) . ? C44 H44 0.93 . ? C18 C19 1.376(7) . ? C18 C24 1.378(8) . ? C19 H19 0.93 . ? C52 C57 1.386(6) . ? C52 C53 1.394(6) . ? C39 C38 1.384(8) . ? C39 C40 1.395(7) . ? C39 H39 0.93 . ? C17 C16 1.377(6) . ? C17 H17 0.93 . ? C24 H24 0.93 . ? C35 C34 1.372(6) . ? C35 C36 1.387(7) . ? C36 C37 1.377(6) . ? C36 H36 0.93 . ? C42 Gd2 2.856(4) 4_674 ? C53 H53 0.93 . ? C40 H40 0.93 . ? C16 C15 1.375(8) . ? C16 H16 0.93 . ? C15 C14 1.386(9) . ? C57 H57 0.93 . ? C37 H37 0.93 . ? C14 C13 1.384(7) . ? C14 H14 0.93 . ? C34 H34 0.93 . ? C13 H13 0.93 . ? 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 O52 Gd1 O32 148.07(13) . . ? O52 Gd1 O31 102.53(12) . . ? O32 Gd1 O31 90.28(12) . . ? O52 Gd1 O51 85.76(10) . . ? O32 Gd1 O51 103.00(11) . . ? O31 Gd1 O51 140.22(12) . . ? O52 Gd1 O11 79.11(11) . . ? O32 Gd1 O11 76.55(10) . . ? O31 Gd1 O11 73.92(11) . . ? O51 Gd1 O11 145.42(11) . . ? O52 Gd1 O103 140.51(12) . . ? O32 Gd1 O103 70.80(11) . . ? O31 Gd1 O103 75.74(10) . . ? O51 Gd1 O103 73.75(11) . . ? O11 Gd1 O103 134.73(10) . . ? O52 Gd1 O101 78.81(12) . . ? O32 Gd1 O101 74.21(12) . . ? O31 Gd1 O101 144.90(11) . . ? O51 Gd1 O101 74.72(11) . . ? O11 Gd1 O101 71.93(10) . . ? O103 Gd1 O101 125.21(10) . . ? O52 Gd1 O102 70.90(13) . . ? O32 Gd1 O102 141.01(12) . . ? O31 Gd1 O102 73.03(12) . . ? O51 Gd1 O102 73.31(12) . . ? O11 Gd1 O102 128.45(11) . . ? O103 Gd1 O102 71.01(11) . . ? O101 Gd1 O102 137.00(12) . . ? O55 Gd2 O14 94.60(11) 4_675 2_646 ? O55 Gd2 O54 88.47(10) 4_675 . ? O14 Gd2 O54 73.28(11) 2_646 . ? O55 Gd2 O203 95.72(10) 4_675 . ? O14 Gd2 O203 138.84(11) 2_646 . ? O54 Gd2 O203 146.62(11) . . ? O55 Gd2 O201 75.28(11) 4_675 . ? O14 Gd2 O201 73.37(11) 2_646 . ? O54 Gd2 O201 141.33(11) . . ? O203 Gd2 O201 71.02(11) . . ? O55 Gd2 O34 150.92(11) 4_675 4_576 ? O14 Gd2 O34 107.65(10) 2_646 4_576 ? O54 Gd2 O34 80.55(10) . 4_576 ? O203 Gd2 O34 79.92(10) . 4_576 ? O201 Gd2 O34 128.42(10) . 4_576 ? O55 Gd2 O202 75.18(11) 4_675 . ? O14 Gd2 O202 146.93(11) 2_646 . ? O54 Gd2 O202 75.05(10) . . ? O203 Gd2 O202 74.11(10) . . ? O201 Gd2 O202 131.04(10) . . ? O34 Gd2 O202 75.99(10) 4_576 . ? O55 Gd2 O35 153.28(10) 4_675 4_576 ? O14 Gd2 O35 80.25(10) 2_646 4_576 ? O54 Gd2 O35 114.52(10) . 4_576 ? O203 Gd2 O35 72.89(10) . 4_576 ? O201 Gd2 O35 78.14(10) . 4_576 ? O34 Gd2 O35 52.57(9) 4_576 4_576 ? O202 Gd2 O35 122.25(10) . 4_576 ? O55 Gd2 C42 171.24(10) 4_675 4_576 ? O14 Gd2 C42 93.45(11) 2_646 4_576 ? O54 Gd2 C42 97.16(10) . 4_576 ? O203 Gd2 C42 75.90(10) . 4_576 ? O201 Gd2 C42 103.82(11) . 4_576 ? O34 Gd2 C42 26.18(10) 4_576 4_576 ? O202 Gd2 C42 99.73(11) . 4_576 ? O35 Gd2 C42 26.43(10) 4_576 4_576 ? C42 O35 Gd2 92.8(2) . 4_674 ? C42 O34 Gd2 95.2(2) . 4_674 ? C51 O52 Gd1 165.3(3) . . ? C51 O51 Gd1 132.3(3) 4_675 . ? C11 O11 Gd1 138.6(3) . . ? C22 O14 Gd2 166.1(3) . 2_656 ? C31 O32 Gd1 171.2(3) . . ? C62 O54 Gd2 137.8(3) . . ? C31 O31 Gd1 130.4(3) 4_575 . ? C62 O55 Gd2 132.1(3) . 4_575 ? O32 C31 O31 123.5(4) . 4_675 ? O32 C31 C32 119.0(4) . . ? O31 C31 C32 117.5(4) 4_675 . ? C35 O33 C38 117.3(4) . . ? O51 C51 O52 123.5(4) 4_575 . ? O51 C51 C52 118.9(3) 4_575 . ? O52 C51 C52 117.6(3) . . ? C34 C33 C32 120.3(4) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? C58 O53 C55 122.1(3) . . ? O53 C58 C59 114.2(4) . . ? O53 C58 C64 124.7(4) . . ? C59 C58 C64 121.0(4) . . ? C13 C12 C17 118.5(4) . . ? C13 C12 C11 122.1(4) . . ? C17 C12 C11 119.4(4) . . ? C18 O13 C15 119.8(4) . . ? O15 C22 O14 122.8(4) . . ? O15 C22 C21 119.1(4) . . ? O14 C22 C21 118.0(4) . . ? C20 C21 C23 117.7(4) . . ? C20 C21 C22 121.1(4) . . ? C23 C21 C22 121.1(4) . . ? O55 C62 O54 123.6(4) . . ? O55 C62 C61 117.6(3) . . ? O54 C62 C61 118.8(3) . . ? C55 C54 C53 119.4(4) . . ? C55 C54 H54 120.3 . . ? C53 C54 H54 120.3 . . ? C59 C60 C61 119.7(3) . . ? C59 C60 H60 120.2 . . ? C61 C60 H60 120.2 . . ? C61 C63 C64 121.5(4) . . ? C61 C63 H63 119.2 . . ? C64 C63 H63 119.2 . . ? C63 C61 C60 119.2(3) . . ? C63 C61 C62 120.5(3) . . ? C60 C61 C62 120.2(3) . . ? C58 C59 C60 120.4(4) . . ? C58 C59 H59 119.8 . . ? C60 C59 H59 119.8 . . ? O12 C11 O11 123.8(4) . . ? O12 C11 C12 119.2(4) . . ? O11 C11 C12 117.0(4) . . ? C56 C55 O53 116.6(4) . . ? C56 C55 C54 120.5(4) . . ? O53 C55 C54 122.5(4) . . ? C37 C32 C33 118.7(4) . . ? C37 C32 C31 120.1(4) . . ? C33 C32 C31 121.1(4) . . ? C58 C64 C63 118.1(4) . . ? C58 C64 H64 121 . . ? C63 C64 H64 121 . . ? C43 C41 C40 119.0(4) . . ? C43 C41 C42 120.8(4) . . ? C40 C41 C42 120.1(4) . . ? C41 C43 C44 120.9(5) . . ? C41 C43 H43 119.5 . . ? C44 C43 H43 119.5 . . ? C19 C20 C21 121.4(4) . . ? C19 C20 H20 119.3 . . ? C21 C20 H20 119.3 . . ? C55 C56 C57 119.8(4) . . ? C55 C56 H56 120.1 . . ? C57 C56 H56 120.1 . . ? C24 C23 C21 121.4(5) . . ? C24 C23 H23 119.3 . . ? C21 C23 H23 119.3 . . ? C38 C44 C43 119.5(5) . . ? C38 C44 H44 120.2 . . ? C43 C44 H44 120.2 . . ? C19 C18 C24 120.5(4) . . ? C19 C18 O13 114.9(5) . . ? C24 C18 O13 124.6(4) . . ? C18 C19 C20 119.4(5) . . ? C18 C19 H19 120.3 . . ? C20 C19 H19 120.3 . . ? C57 C52 C53 118.7(4) . . ? C57 C52 C51 119.3(4) . . ? C53 C52 C51 122.0(4) . . ? C38 C39 C40 119.2(5) . . ? C38 C39 H39 120.4 . . ? C40 C39 H39 120.4 . . ? C44 C38 C39 121.1(4) . . ? C44 C38 O33 118.9(5) . . ? C39 C38 O33 119.8(5) . . ? C16 C17 C12 121.6(5) . . ? C16 C17 H17 119.2 . . ? C12 C17 H17 119.2 . . ? C23 C24 C18 119.7(4) . . ? C23 C24 H24 120.2 . . ? C18 C24 H24 120.2 . . ? C34 C35 C36 120.7(4) . . ? C34 C35 O33 117.0(4) . . ? C36 C35 O33 122.2(4) . . ? C37 C36 C35 119.2(4) . . ? C37 C36 H36 120.4 . . ? C35 C36 H36 120.4 . . ? O34 C42 O35 119.2(3) . . ? O34 C42 C41 120.0(3) . . ? O35 C42 C41 120.7(4) . . ? O34 C42 Gd2 58.62(19) . 4_674 ? O35 C42 Gd2 60.76(19) . 4_674 ? C41 C42 Gd2 173.0(3) . 4_674 ? C54 C53 C52 120.7(4) . . ? C54 C53 H53 119.6 . . ? C52 C53 H53 119.6 . . ? C41 C40 C39 120.2(5) . . ? C41 C40 H40 119.9 . . ? C39 C40 H40 119.9 . . ? C15 C16 C17 118.5(5) . . ? C15 C16 H16 120.7 . . ? C17 C16 H16 120.7 . . ? C16 C15 C14 121.5(5) . . ? C16 C15 O13 119.1(5) . . ? C14 C15 O13 119.1(6) . . ? C56 C57 C52 120.8(4) . . ? C56 C57 H57 119.6 . . ? C52 C57 H57 119.6 . . ? C36 C37 C32 121.0(4) . . ? C36 C37 H37 119.5 . . ? C32 C37 H37 119.5 . . ? C13 C14 C15 118.5(5) . . ? C13 C14 H14 120.7 . . ? C15 C14 H14 120.7 . . ? C35 C34 C33 120.1(4) . . ? C35 C34 H34 120 . . ? C33 C34 H34 120 . . ? C12 C13 C14 121.2(5) . . ? C12 C13 H13 119.4 . . ? C14 C13 H13 119.4 . . ? data_C1-YZ1 _database_code_depnum_ccdc_archive 'CCDC 815115' #TrackingRef 'C1.cif' _audit_creation_date 2012-10-08T09:53:43-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C42 H36 La2 O21' _chemical_formula_sum 'C42 H36 La2 O21' _chemical_formula_weight 1154.53 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 2/n 1' _symmetry_space_group_name_Hall '-P 2yac' _symmetry_Int_Tables_number 13 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 23.662(4) _cell_length_b 6.0657(10) _cell_length_c 29.414(6) _cell_angle_alpha 90 _cell_angle_beta 102.03(7) _cell_angle_gamma 90 _cell_volume 4129.0(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 30219 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 1.857 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2280 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.130 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; 'P. Coppens in Crystallographic Computing ed F.R. Ahmed, S.R. Hall and C.P. Huber, Copenhagen, Munksgaard, (1970) pp 255-270' ; _exptl_absorpt_correction_T_min 0.817 _exptl_absorpt_correction_T_max 0.880 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type 'KappaCCD, Nonius' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0595 _diffrn_reflns_av_unetI/netI 0.0532 _diffrn_reflns_number 36748 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.46 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 9422 _reflns_number_gt 7466 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ; WinGX publication routines (Farrugia, 1999), CRYSCAL (T. Roisnel, local program) ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0472P)^2^+0.0000P] 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 SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.00050(8) _refine_ls_number_reflns 9422 _refine_ls_number_parameters 587 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0532 _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_ref 0.0886 _refine_ls_wR_factor_gt 0.0812 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.502 _refine_diff_density_min -1.05 _refine_diff_density_rms 0.125 _iucr_refine_instructions_details ; .res file for SHELXL : job.res ................................................................. TITL import in P 2/n CELL 0.71069 23.6622 6.0657 29.4141 90.000 102.034 90.000 ZERR 4.00 0.0040 0.0010 0.0060 0.000 0.000 0.000 LATT 1 SYMM 1/2 - X, Y, 1/2 - Z SFAC C H O LA UNIT 168 144 84 8 MERG 2 FMAP 2 PLAN 20 SIZE 0.06 0.06 0.09 ACTA BOND $H LIST 1 L.S. 5 WGHT 0.047200 EXTI 0.000498 FVAR 0.12473 LA1 4 -0.110528 0.393281 -0.016888 11.00000 0.02423 0.01931 = 0.01436 0.00066 0.00446 0.00053 LA2 4 0.173933 0.486026 0.520291 11.00000 0.02323 0.01960 = 0.01613 -0.00107 0.00380 -0.00150 O35 3 0.227296 0.344132 0.465501 11.00000 0.03988 0.03773 = 0.02011 -0.00870 0.01328 -0.00597 O101 3 -0.152509 0.724233 0.020122 11.00000 0.03966 0.02542 = 0.02506 -0.00389 0.00901 0.00063 O203 3 0.092839 0.435112 0.564672 11.00000 0.03004 0.03698 = 0.04176 0.00183 0.01224 -0.00022 O15 3 0.098377 0.654330 0.461049 11.00000 0.03518 0.04360 = 0.02721 -0.00292 -0.00351 0.00305 O51 3 0.161879 0.805266 0.567224 11.00000 0.05104 0.02726 = 0.03524 -0.01114 0.02111 -0.01171 O12 3 0.047757 0.719949 0.071196 11.00000 0.02709 0.03335 = 0.02631 -0.00175 0.00890 -0.00491 O202 3 0.218951 0.825943 0.487734 11.00000 0.04013 0.03118 = 0.03106 0.01037 0.00631 0.00057 O32 3 0.147806 -0.030718 0.050890 11.00000 0.03424 0.02196 = 0.01863 -0.00024 0.00490 -0.00046 O34 3 0.290029 0.526109 0.432734 11.00000 0.03591 0.03857 = 0.02334 0.00243 0.00211 -0.01315 O55 3 0.161375 0.744705 0.957393 11.00000 0.03412 0.03371 = 0.02146 0.00687 0.01316 0.00454 C51 1 0.178422 0.991444 0.583050 11.00000 0.02293 0.02548 = 0.02090 0.00150 0.00410 0.00356 O31 3 0.097496 0.268110 0.061106 11.00000 0.04620 0.02995 = 0.02844 0.00858 0.01206 0.00986 O11 3 -0.033909 0.548278 0.041829 11.00000 0.04056 0.04705 = 0.01973 0.00221 -0.00115 -0.01213 O33 3 0.162594 -0.099222 0.268053 11.00000 0.07450 0.03857 = 0.01506 -0.00562 0.00403 -0.01245 O201 3 0.106805 0.173182 0.478961 11.00000 0.03767 0.03357 = 0.04642 -0.00962 0.00318 -0.00644 O52 3 0.200785 1.132277 0.560129 11.00000 0.03461 0.02604 = 0.02406 0.00330 0.00910 -0.00089 O53 3 0.155266 1.216718 0.764431 11.00000 0.07882 0.03161 = 0.01996 0.00510 0.01756 0.01081 O14 3 0.010490 0.797575 0.449214 11.00000 0.03476 0.03456 = 0.03129 -0.00813 0.00892 0.00408 OW1 3 -0.014075 0.233595 0.456564 11.00000 0.04086 0.03894 = 0.04071 0.00109 0.00937 0.00619 C24 1 -0.020698 0.619315 0.308491 11.00000 0.05509 0.08294 = 0.02192 0.00113 -0.00659 0.02065 AFIX 43 H24 2 -0.050413 0.681502 0.286518 11.00000 -1.20000 AFIX 0 C31 1 0.127970 0.101767 0.077205 11.00000 0.02815 0.01846 = 0.01914 -0.00193 0.00681 -0.00498 O54 3 0.226225 0.537054 0.931969 11.00000 0.03009 0.03144 = 0.01941 0.00160 0.00191 0.00811 C61 1 0.179580 0.823886 0.882869 11.00000 0.02067 0.02634 = 0.01703 0.00278 0.00441 -0.00123 C11 1 0.003639 0.613286 0.076048 11.00000 0.02383 0.02566 = 0.01760 -0.00230 0.00176 0.00094 C12 1 -0.004073 0.559846 0.124015 11.00000 0.01970 0.03218 = 0.02141 -0.00508 0.00491 -0.00017 O102 3 -0.044175 0.076709 0.027770 11.00000 0.05435 0.03920 = 0.04363 0.01037 0.00676 0.01959 C33 1 0.169744 -0.127087 0.146540 11.00000 0.04082 0.02577 = 0.01862 -0.00143 0.00216 0.00452 AFIX 43 H33 2 0.184241 -0.223078 0.127114 11.00000 -1.20000 AFIX 0 C42 1 0.249046 0.389799 0.430845 11.00000 0.02321 0.02939 = 0.01974 -0.00006 0.00282 0.00085 O13 3 -0.008075 0.330685 0.255610 11.00000 0.09368 0.05803 = 0.01566 -0.00260 0.01123 -0.02532 C59 1 0.192838 0.875977 0.804241 11.00000 0.04636 0.04280 = 0.01784 0.00284 0.01327 0.01125 AFIX 43 H59 2 0.207266 0.826226 0.778992 11.00000 -1.20000 AFIX 0 C41 1 0.224834 0.273263 0.386468 11.00000 0.02333 0.02843 = 0.01980 -0.00304 0.00414 -0.00012 C15 1 -0.008043 0.426568 0.213359 11.00000 0.03839 0.04751 = 0.01838 -0.00467 0.01117 -0.00485 C13 1 0.024726 0.679087 0.162232 11.00000 0.03367 0.03484 = 0.02777 -0.00248 0.00694 -0.00541 AFIX 43 H13 2 0.045624 0.803932 0.157582 11.00000 -1.20000 AFIX 0 C38 1 0.181715 0.038928 0.305201 11.00000 0.03531 0.03508 = 0.01518 -0.00524 0.00176 0.00279 C35 1 0.157262 -0.029458 0.222320 11.00000 0.03716 0.03756 = 0.01568 -0.00506 0.00374 -0.00832 C34 1 0.178213 -0.171956 0.193346 11.00000 0.04192 0.03391 = 0.02134 0.00001 0.00248 0.00426 AFIX 43 H34 2 0.198067 -0.298393 0.205385 11.00000 -1.20000 AFIX 0 C17 1 -0.036471 0.376674 0.131682 11.00000 0.02830 0.04648 = 0.01956 -0.00651 0.00361 -0.01160 AFIX 43 H17 2 -0.057481 0.298967 0.106487 11.00000 -1.20000 AFIX 0 C43 1 0.192799 0.079681 0.387367 11.00000 0.03979 0.03282 = 0.01466 0.00370 0.00644 -0.00175 AFIX 43 H43 2 0.185313 0.029707 0.415416 11.00000 -1.20000 AFIX 0 C21 1 0.037981 0.617230 0.386143 11.00000 0.02741 0.03736 = 0.02246 0.00083 0.00625 0.00151 C18 1 0.009652 0.441724 0.297217 11.00000 0.05158 0.04936 = 0.01989 -0.00047 0.00985 -0.00767 C22 1 0.049564 0.694059 0.435080 11.00000 0.02696 0.02482 = 0.02254 0.00142 0.00058 0.00150 C62 1 0.189627 0.693732 0.926662 11.00000 0.02327 0.02606 = 0.01409 -0.00134 0.00247 -0.00485 C63 1 0.149116 1.023666 0.879667 11.00000 0.03347 0.02795 = 0.01826 -0.00254 0.00904 0.00028 AFIX 43 H63 2 0.134127 1.072719 0.904690 11.00000 -1.20000 AFIX 0 C40 1 0.233183 0.348145 0.344069 11.00000 0.03457 0.03575 = 0.02094 0.00158 0.00742 -0.01041 AFIX 43 H40 2 0.253963 0.477413 0.342890 11.00000 -1.20000 AFIX 0 C57 1 0.142942 0.904958 0.655668 11.00000 0.03768 0.02775 = 0.02571 -0.00080 0.00707 -0.00475 AFIX 43 H57 2 0.127466 0.774162 0.641941 11.00000 -1.20000 AFIX 0 C60 1 0.200892 0.753640 0.845189 11.00000 0.03432 0.03314 = 0.02089 0.00382 0.00688 0.01300 AFIX 43 H60 2 0.221142 0.621397 0.847122 11.00000 -1.20000 AFIX 0 C32 1 0.139775 0.060058 0.128065 11.00000 0.02411 0.02454 = 0.01765 -0.00125 0.00364 -0.00411 C20 1 0.069503 0.443548 0.372757 11.00000 0.04375 0.06167 = 0.02710 -0.00188 0.00544 0.02118 AFIX 43 H20 2 0.100851 0.385933 0.393833 11.00000 -1.20000 AFIX 0 C58 1 0.162652 1.074792 0.801923 11.00000 0.03752 0.02910 = 0.01794 0.00530 0.00432 0.00005 C53 1 0.194533 1.241720 0.652217 11.00000 0.04532 0.02781 = 0.02319 0.00027 0.00806 -0.00769 AFIX 43 H53 2 0.213697 1.338832 0.636163 11.00000 -1.20000 AFIX 0 C54 1 0.189255 1.292157 0.696719 11.00000 0.05741 0.02771 = 0.01920 -0.00251 0.00880 -0.00677 AFIX 43 H54 2 0.204385 1.423463 0.710427 11.00000 -1.20000 AFIX 0 C52 1 0.171548 1.046976 0.630831 11.00000 0.03399 0.02103 = 0.01741 0.00165 0.00324 0.00121 C44 1 0.172313 -0.037213 0.347335 11.00000 0.04828 0.03129 = 0.02168 -0.00184 0.00827 -0.01142 AFIX 43 H44 2 0.152083 -0.167789 0.348555 11.00000 -1.20000 AFIX 0 C56 1 0.137144 0.954355 0.700055 11.00000 0.04871 0.03147 = 0.02617 0.00595 0.01005 -0.00557 AFIX 43 H56 2 0.117164 0.859615 0.715961 11.00000 -1.20000 AFIX 0 C16 1 -0.037624 0.310396 0.175841 11.00000 0.04459 0.04491 = 0.02505 0.00054 0.00957 -0.01791 AFIX 43 H16 2 -0.058587 0.185761 0.180515 11.00000 -1.20000 AFIX 0 C37 1 0.119697 0.202694 0.157970 11.00000 0.03165 0.03046 = 0.02208 -0.00370 0.00311 0.00305 AFIX 43 H37 2 0.099998 0.329802 0.146158 11.00000 -1.20000 AFIX 0 C36 1 0.128473 0.159114 0.205069 11.00000 0.04264 0.03826 = 0.02218 -0.01157 0.00738 0.00364 AFIX 43 H36 2 0.115028 0.256423 0.224839 11.00000 -1.20000 AFIX 0 C64 1 0.141333 1.147565 0.839498 11.00000 0.04025 0.02665 = 0.02062 -0.00110 0.00723 0.00356 AFIX 43 H64 2 0.121599 1.280914 0.837744 11.00000 -1.20000 AFIX 0 C39 1 0.211340 0.235341 0.303154 11.00000 0.04332 0.04329 = 0.01609 0.00203 0.00912 -0.00997 AFIX 43 H39 2 0.216444 0.290326 0.274770 11.00000 -1.20000 AFIX 0 C14 1 0.022874 0.615458 0.207063 11.00000 0.04268 0.04803 = 0.02232 -0.00646 0.00478 -0.00927 AFIX 43 H14 2 0.041870 0.697094 0.232450 11.00000 -1.20000 AFIX 0 C23 1 -0.006492 0.703449 0.352648 11.00000 0.04819 0.06342 = 0.02506 -0.00219 -0.00238 0.02702 AFIX 43 H23 2 -0.027415 0.822443 0.360388 11.00000 -1.20000 AFIX 0 C55 1 0.161538 1.148080 0.721006 11.00000 0.04480 0.03319 = 0.01681 0.00336 0.00686 0.00835 C19 1 0.054767 0.356967 0.328894 11.00000 0.06901 0.06255 = 0.02583 -0.00786 0.01162 0.02642 AFIX 43 H19 2 0.075730 0.239268 0.320641 11.00000 -1.20000 HKLF 4 REM import in P 2/n REM R1 = 0.0353 for 7466 Fo > 4sig(Fo) and 0.0532 for all 9422 data REM 587 parameters refined using 0 restraints END WGHT 0.0425 0.3768 REM Highest difference peak 1.50, deepest hole -1.05, 1-sigma level 0.12 Q1 1 -0.1103 0.6086 -0.0176 11.00000 0.05 1.50 Q2 1 0.1752 0.7342 0.5216 11.00000 0.05 0.91 Q3 1 0.2605 0.6059 0.4768 11.00000 0.05 0.90 Q4 1 0.1057 0.5339 0.9448 11.00000 0.05 0.90 Q5 1 0.0400 0.3944 0.4440 11.00000 0.05 0.82 Q6 1 0.0463 0.4830 0.5171 11.00000 0.05 0.81 Q7 1 0.2609 0.4161 0.4758 11.00000 0.05 0.77 Q8 1 -0.1601 0.8398 0.0010 11.00000 0.05 0.73 Q9 1 -0.0514 -0.0561 0.0239 11.00000 0.05 0.72 Q10 1 0.1107 0.0344 0.4738 11.00000 0.05 0.72 Q11 1 0.1751 0.2976 0.5257 11.00000 0.05 0.72 Q12 1 -0.1834 0.6910 0.0320 11.00000 0.05 0.69 Q13 1 -0.0173 0.0856 0.4503 11.00000 0.05 0.63 Q14 1 0.2194 0.9382 0.5080 11.00000 0.05 0.57 Q15 1 0.2435 0.7883 0.4688 11.00000 0.05 0.57 Q16 1 0.0684 0.3176 0.5662 11.00000 0.05 0.55 Q17 1 -0.1074 0.7409 0.0498 11.00000 0.05 0.53 Q18 1 0.0493 0.3073 0.5136 11.00000 0.05 0.53 Q19 1 0.1191 0.4778 0.5171 11.00000 0.05 0.52 Q20 1 -0.1512 0.4805 -0.0209 11.00000 0.05 0.52 ; #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' 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 -0.110528(8) 0.39328(3) -0.016888(7) 0.01923(7) Uani 1 1 d . . . La2 La 0.173933(8) 0.48603(3) 0.520291(8) 0.01970(7) Uani 1 1 d . . . O35 O 0.22730(11) 0.3441(4) 0.46550(10) 0.0316(6) Uani 1 1 d . . . O101 O -0.15251(11) 0.7242(4) 0.02012(10) 0.0297(6) Uani 1 1 d . . . O203 O 0.09284(11) 0.4351(4) 0.56467(11) 0.0356(7) Uani 1 1 d . . . O15 O 0.09838(12) 0.6543(4) 0.46105(11) 0.0368(7) Uani 1 1 d . . . O51 O 0.16188(12) 0.8053(4) 0.56722(10) 0.0361(7) Uani 1 1 d . . . O12 O 0.04776(10) 0.7199(4) 0.07120(10) 0.0284(6) Uani 1 1 d . . . O202 O 0.21895(11) 0.8259(4) 0.48773(10) 0.0343(7) Uani 1 1 d . . . O32 O 0.14781(11) -0.0307(4) 0.05089(9) 0.0250(6) Uani 1 1 d . . . O34 O 0.29003(12) 0.5261(4) 0.43273(10) 0.0332(7) Uani 1 1 d . . . O55 O 0.16138(11) 0.7447(4) 0.95739(9) 0.0287(6) Uani 1 1 d . . . C51 C 0.17842(15) 0.9914(5) 0.58305(14) 0.0232(8) Uani 1 1 d . . . O31 O 0.09750(11) 0.2681(4) 0.06111(10) 0.0342(7) Uani 1 1 d . . . O11 O -0.03391(12) 0.5483(5) 0.04183(10) 0.0369(7) Uani 1 1 d . . . O33 O 0.16259(14) -0.0992(4) 0.26805(10) 0.0435(8) Uani 1 1 d . . . O201 O 0.10680(11) 0.1732(4) 0.47896(11) 0.0400(7) Uani 1 1 d . . . O52 O 0.20079(11) 1.1323(4) 0.56013(10) 0.0278(6) Uani 1 1 d . . . O53 O 0.15527(14) 1.2167(4) 0.76443(10) 0.0424(7) Uani 1 1 d . . . O14 O 0.01049(11) 0.7976(4) 0.44921(10) 0.0332(6) Uani 1 1 d . . . OW1 O -0.01407(12) 0.2336(4) 0.45656(11) 0.0400(7) Uani 1 1 d . . . C24 C -0.0207(2) 0.6193(9) 0.30849(18) 0.0554(14) Uani 1 1 d . . . H24 H -0.0504 0.6815 0.2865 0.067 Uiso 1 1 calc R . . C31 C 0.12797(15) 0.1018(5) 0.07721(13) 0.0216(8) Uani 1 1 d . . . O54 O 0.22622(11) 0.5371(4) 0.93197(9) 0.0275(6) Uani 1 1 d . . . C61 C 0.17958(14) 0.8239(5) 0.88287(13) 0.0213(7) Uani 1 1 d . . . C11 C 0.00364(15) 0.6133(5) 0.07605(13) 0.0227(8) Uani 1 1 d . . . C12 C -0.00407(15) 0.5598(6) 0.12402(14) 0.0243(8) Uani 1 1 d . . . O102 O -0.04417(13) 0.0767(5) 0.02777(12) 0.0462(8) Uani 1 1 d . . . C33 C 0.16974(17) -0.1271(6) 0.14654(14) 0.0290(9) Uani 1 1 d . . . H33 H 0.1842 -0.2231 0.1271 0.035 Uiso 1 1 calc R . . C42 C 0.24905(15) 0.3898(5) 0.43085(14) 0.0244(8) Uani 1 1 d . . . O13 O -0.00807(16) 0.3307(5) 0.25561(11) 0.0558(9) Uani 1 1 d . . . C59 C 0.19284(18) 0.8760(6) 0.80424(15) 0.0347(10) Uani 1 1 d . . . H59 H 0.2073 0.8262 0.779 0.042 Uiso 1 1 calc R . . C41 C 0.22483(15) 0.2733(6) 0.38647(13) 0.0239(8) Uani 1 1 d . . . C15 C -0.00804(18) 0.4266(7) 0.21336(15) 0.0340(9) Uani 1 1 d . . . C13 C 0.02473(16) 0.6791(6) 0.16223(15) 0.0320(9) Uani 1 1 d . . . H13 H 0.0456 0.8039 0.1576 0.038 Uiso 1 1 calc R . . C38 C 0.18171(17) 0.0389(6) 0.30520(14) 0.0290(9) Uani 1 1 d . . . C35 C 0.15726(18) -0.0295(6) 0.22232(14) 0.0304(9) Uani 1 1 d . . . C34 C 0.17821(17) -0.1720(6) 0.19335(15) 0.0330(9) Uani 1 1 d . . . H34 H 0.1981 -0.2984 0.2054 0.04 Uiso 1 1 calc R . . C17 C -0.03647(16) 0.3767(6) 0.13168(15) 0.0316(9) Uani 1 1 d . . . H17 H -0.0575 0.299 0.1065 0.038 Uiso 1 1 calc R . . C43 C 0.19280(17) 0.0797(6) 0.38737(14) 0.0290(9) Uani 1 1 d . . . H43 H 0.1853 0.0297 0.4154 0.035 Uiso 1 1 calc R . . C21 C 0.03798(16) 0.6172(6) 0.38614(15) 0.0289(9) Uani 1 1 d . . . C18 C 0.0097(2) 0.4417(7) 0.29722(16) 0.0399(10) Uani 1 1 d . . . C22 C 0.04956(15) 0.6941(6) 0.43508(14) 0.0254(8) Uani 1 1 d . . . C62 C 0.18963(14) 0.6937(5) 0.92666(13) 0.0213(7) Uani 1 1 d . . . C63 C 0.14912(16) 1.0237(5) 0.87967(14) 0.0260(8) Uani 1 1 d . . . H63 H 0.1341 1.0727 0.9047 0.031 Uiso 1 1 calc R . . C40 C 0.23318(16) 0.3481(6) 0.34407(14) 0.0302(9) Uani 1 1 d . . . H40 H 0.254 0.4774 0.3429 0.036 Uiso 1 1 calc R . . C57 C 0.14294(17) 0.9050(6) 0.65567(15) 0.0303(9) Uani 1 1 d . . . H57 H 0.1275 0.7742 0.6419 0.036 Uiso 1 1 calc R . . C60 C 0.20089(16) 0.7536(6) 0.84519(14) 0.0293(9) Uani 1 1 d . . . H60 H 0.2211 0.6214 0.8471 0.035 Uiso 1 1 calc R . . C32 C 0.13977(15) 0.0601(5) 0.12806(13) 0.0222(8) Uani 1 1 d . . . C20 C 0.0695(2) 0.4435(8) 0.37276(17) 0.0445(11) Uani 1 1 d . . . H20 H 0.1009 0.3859 0.3938 0.053 Uiso 1 1 calc R . . C58 C 0.16265(17) 1.0748(6) 0.80192(14) 0.0284(8) Uani 1 1 d . . . C53 C 0.19453(17) 1.2417(6) 0.65222(15) 0.0320(9) Uani 1 1 d . . . H53 H 0.2137 1.3388 0.6362 0.038 Uiso 1 1 calc R . . C54 C 0.18925(18) 1.2922(6) 0.69672(15) 0.0347(10) Uani 1 1 d . . . H54 H 0.2044 1.4235 0.7104 0.042 Uiso 1 1 calc R . . C52 C 0.17155(16) 1.0470(5) 0.63083(14) 0.0245(8) Uani 1 1 d . . . C44 C 0.17231(18) -0.0372(6) 0.34734(15) 0.0336(10) Uani 1 1 d . . . H44 H 0.1521 -0.1678 0.3486 0.04 Uiso 1 1 calc R . . C56 C 0.13714(19) 0.9544(6) 0.70005(16) 0.0351(10) Uani 1 1 d . . . H56 H 0.1172 0.8596 0.716 0.042 Uiso 1 1 calc R . . C16 C -0.03762(18) 0.3104(7) 0.17584(15) 0.0379(10) Uani 1 1 d . . . H16 H -0.0586 0.1858 0.1805 0.045 Uiso 1 1 calc R . . C37 C 0.11970(16) 0.2027(6) 0.15797(14) 0.0284(8) Uani 1 1 d . . . H37 H 0.1 0.3298 0.1462 0.034 Uiso 1 1 calc R . . C36 C 0.12847(17) 0.1591(6) 0.20507(15) 0.0343(9) Uani 1 1 d . . . H36 H 0.115 0.2564 0.2248 0.041 Uiso 1 1 calc R . . C64 C 0.14133(17) 1.1476(6) 0.83950(14) 0.0290(9) Uani 1 1 d . . . H64 H 0.1216 1.2809 0.8377 0.035 Uiso 1 1 calc R . . C39 C 0.21134(17) 0.2353(6) 0.30315(15) 0.0338(9) Uani 1 1 d . . . H39 H 0.2164 0.2903 0.2748 0.041 Uiso 1 1 calc R . . C14 C 0.02287(18) 0.6155(7) 0.20706(16) 0.0380(10) Uani 1 1 d . . . H14 H 0.0419 0.6971 0.2325 0.046 Uiso 1 1 calc R . . C23 C -0.00649(19) 0.7034(8) 0.35265(16) 0.0470(12) Uani 1 1 d . . . H23 H -0.0274 0.8224 0.3604 0.056 Uiso 1 1 calc R . . C55 C 0.16154(17) 1.1481(6) 0.72101(14) 0.0315(9) Uani 1 1 d . . . C19 C 0.0548(2) 0.3570(8) 0.32889(17) 0.0522(13) Uani 1 1 d . . . H19 H 0.0757 0.2393 0.3206 0.063 Uiso 1 1 calc R . . 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 0.02423(12) 0.01931(11) 0.01436(12) 0.00066(8) 0.00446(9) 0.00053(7) La2 0.02323(12) 0.01960(11) 0.01613(13) -0.00107(8) 0.00380(9) -0.00150(7) O35 0.0399(16) 0.0377(14) 0.0201(16) -0.0087(12) 0.0133(13) -0.0060(11) O101 0.0397(15) 0.0254(13) 0.0251(17) -0.0039(11) 0.0090(12) 0.0006(11) O203 0.0300(15) 0.0370(14) 0.042(2) 0.0018(13) 0.0122(14) -0.0002(11) O15 0.0352(16) 0.0436(15) 0.0272(18) -0.0029(13) -0.0035(13) 0.0030(12) O51 0.0510(17) 0.0273(14) 0.0352(19) -0.0111(12) 0.0211(15) -0.0117(12) O12 0.0271(14) 0.0333(14) 0.0263(17) -0.0017(12) 0.0089(12) -0.0049(11) O202 0.0401(16) 0.0312(13) 0.0311(18) 0.0104(12) 0.0063(13) 0.0006(12) O32 0.0342(14) 0.0220(12) 0.0186(15) -0.0002(10) 0.0049(12) -0.0005(10) O34 0.0359(16) 0.0386(15) 0.0233(17) 0.0024(12) 0.0021(13) -0.0132(12) O55 0.0341(14) 0.0337(14) 0.0215(16) 0.0069(11) 0.0132(12) 0.0045(11) C51 0.0229(19) 0.0255(19) 0.021(2) 0.0015(15) 0.0041(16) 0.0036(13) O31 0.0462(17) 0.0300(14) 0.0284(17) 0.0086(12) 0.0121(14) 0.0099(12) O11 0.0406(17) 0.0471(16) 0.0197(17) 0.0022(13) -0.0012(13) -0.0121(13) O33 0.075(2) 0.0386(16) 0.0151(17) -0.0056(13) 0.0040(15) -0.0125(14) O201 0.0377(16) 0.0336(14) 0.046(2) -0.0096(14) 0.0032(15) -0.0064(12) O52 0.0346(15) 0.0260(13) 0.0241(16) 0.0033(11) 0.0091(12) -0.0009(10) O53 0.079(2) 0.0316(15) 0.0200(17) 0.0051(12) 0.0176(16) 0.0108(14) O14 0.0348(15) 0.0346(14) 0.0313(18) -0.0081(12) 0.0089(13) 0.0041(11) OW1 0.0409(16) 0.0389(15) 0.041(2) 0.0011(14) 0.0094(15) 0.0062(12) C24 0.055(3) 0.083(4) 0.022(3) 0.001(2) -0.007(2) 0.021(3) C31 0.0281(19) 0.0185(17) 0.019(2) -0.0019(14) 0.0068(16) -0.0050(13) O54 0.0301(14) 0.0314(13) 0.0194(16) 0.0016(11) 0.0019(12) 0.0081(11) C61 0.0207(18) 0.0263(18) 0.017(2) 0.0028(15) 0.0044(15) -0.0012(13) C11 0.0238(19) 0.0257(18) 0.018(2) -0.0023(15) 0.0018(16) 0.0009(14) C12 0.0197(18) 0.0322(18) 0.021(2) -0.0051(16) 0.0049(16) -0.0002(14) O102 0.054(2) 0.0392(16) 0.044(2) 0.0104(14) 0.0068(16) 0.0196(14) C33 0.041(2) 0.0258(19) 0.019(2) -0.0014(15) 0.0022(18) 0.0045(15) C42 0.0232(19) 0.0294(19) 0.020(2) -0.0001(15) 0.0028(16) 0.0009(14) O13 0.094(3) 0.0580(19) 0.0157(18) -0.0026(15) 0.0112(17) -0.0253(18) C59 0.046(3) 0.043(2) 0.018(2) 0.0028(18) 0.0133(19) 0.0113(18) C41 0.0233(18) 0.0284(19) 0.020(2) -0.0030(15) 0.0041(16) -0.0001(14) C15 0.038(2) 0.048(2) 0.018(2) -0.0047(19) 0.0112(19) -0.0048(18) C13 0.034(2) 0.035(2) 0.028(3) -0.0025(18) 0.0069(19) -0.0054(16) C38 0.035(2) 0.035(2) 0.015(2) -0.0052(16) 0.0018(17) 0.0028(16) C35 0.037(2) 0.038(2) 0.016(2) -0.0051(17) 0.0037(18) -0.0083(16) C34 0.042(2) 0.034(2) 0.021(2) 0.0000(17) 0.0025(19) 0.0043(17) C17 0.028(2) 0.046(2) 0.020(2) -0.0065(18) 0.0036(17) -0.0116(16) C43 0.040(2) 0.033(2) 0.015(2) 0.0037(16) 0.0064(17) -0.0018(16) C21 0.027(2) 0.037(2) 0.022(2) 0.0008(17) 0.0062(17) 0.0015(15) C18 0.052(3) 0.049(2) 0.020(2) 0.000(2) 0.010(2) -0.008(2) C22 0.027(2) 0.0248(18) 0.023(2) 0.0014(15) 0.0006(17) 0.0015(14) C62 0.0233(18) 0.0261(18) 0.014(2) -0.0013(14) 0.0025(15) -0.0048(14) C63 0.033(2) 0.0280(19) 0.018(2) -0.0025(15) 0.0090(17) 0.0003(15) C40 0.035(2) 0.036(2) 0.021(2) 0.0016(17) 0.0074(18) -0.0104(16) C57 0.038(2) 0.028(2) 0.026(2) -0.0008(16) 0.0071(18) -0.0047(15) C60 0.034(2) 0.033(2) 0.021(2) 0.0038(16) 0.0069(17) 0.0130(16) C32 0.0241(19) 0.0245(17) 0.018(2) -0.0012(15) 0.0036(15) -0.0041(14) C20 0.044(3) 0.062(3) 0.027(3) -0.002(2) 0.005(2) 0.021(2) C58 0.038(2) 0.0291(19) 0.018(2) 0.0053(16) 0.0043(17) 0.0001(16) C53 0.045(2) 0.0278(19) 0.023(2) 0.0003(17) 0.0081(19) -0.0077(16) C54 0.057(3) 0.028(2) 0.019(2) -0.0025(16) 0.009(2) -0.0068(17) C52 0.034(2) 0.0210(17) 0.017(2) 0.0017(14) 0.0032(17) 0.0012(14) C44 0.048(3) 0.031(2) 0.022(2) -0.0018(17) 0.008(2) -0.0114(17) C56 0.049(3) 0.031(2) 0.026(3) 0.0060(18) 0.010(2) -0.0056(18) C16 0.045(2) 0.045(2) 0.025(3) 0.0005(19) 0.010(2) -0.0179(19) C37 0.032(2) 0.030(2) 0.022(2) -0.0037(16) 0.0031(17) 0.0031(15) C36 0.043(2) 0.038(2) 0.022(2) -0.0116(18) 0.0074(19) 0.0036(17) C64 0.040(2) 0.0266(18) 0.021(2) -0.0011(16) 0.0072(18) 0.0036(16) C39 0.043(2) 0.043(2) 0.016(2) 0.0020(18) 0.0091(18) -0.0100(18) C14 0.043(2) 0.048(3) 0.022(2) -0.0065(19) 0.005(2) -0.0093(18) C23 0.048(3) 0.063(3) 0.025(3) -0.002(2) -0.002(2) 0.027(2) C55 0.045(2) 0.033(2) 0.017(2) 0.0034(17) 0.0069(18) 0.0083(17) C19 0.069(3) 0.063(3) 0.026(3) -0.008(2) 0.012(3) 0.026(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 O11 2.418(3) . ? La1 O55 2.468(2) 3_566 ? La1 O31 2.484(2) 3_565 ? La1 O12 2.494(3) 3_565 ? La1 O32 2.499(2) 3 ? La1 O34 2.553(3) 4_565 ? La1 O101 2.579(2) . ? La1 O102 2.649(3) . ? La2 O35 2.404(3) . ? La2 O51 2.429(3) . ? La2 O15 2.445(3) . ? La2 O52 2.464(2) 1_545 ? La2 O54 2.503(3) 2_556 ? La2 O203 2.555(3) . ? La2 O202 2.594(3) . ? La2 O201 2.607(3) . ? O35 C42 1.265(4) . ? O15 C22 1.268(4) . ? O51 C51 1.253(4) . ? O12 C11 1.261(4) . ? O12 La1 2.494(3) 3_565 ? O32 C31 1.272(4) . ? O32 La1 2.499(2) 3 ? O34 C42 1.267(4) . ? O34 La1 2.553(3) 4_666 ? O55 C62 1.269(4) . ? O55 La1 2.467(2) 3_566 ? C51 O52 1.270(4) . ? C51 C52 1.487(5) . ? O31 C31 1.273(4) . ? O31 La1 2.484(2) 3_565 ? O11 C11 1.259(5) . ? O33 C38 1.376(5) . ? O33 C35 1.391(5) . ? O52 La2 2.464(2) 1_565 ? O53 C58 1.381(5) . ? O53 C55 1.381(5) . ? O14 C22 1.258(4) . ? C24 C18 1.373(7) . ? C24 C23 1.371(7) . ? C24 H24 0.93 . ? C31 C32 1.485(5) . ? O54 C62 1.273(4) . ? O54 La2 2.503(3) 2_556 ? C61 C60 1.377(5) . ? C61 C63 1.403(5) . ? C61 C62 1.487(5) . ? C11 C12 1.495(5) . ? C12 C17 1.395(5) . ? C12 C13 1.390(5) . ? C33 C34 1.376(6) . ? C33 C32 1.388(5) . ? C33 H33 0.93 . ? C42 C41 1.490(5) . ? O13 C15 1.372(5) . ? O13 C18 1.383(5) . ? C59 C60 1.394(5) . ? C59 C58 1.396(5) . ? C59 H59 0.93 . ? C41 C40 1.380(5) . ? C41 C43 1.401(5) . ? C15 C16 1.372(6) . ? C15 C14 1.392(6) . ? C13 C14 1.383(6) . ? C13 H13 0.93 . ? C38 C44 1.383(6) . ? C38 C39 1.390(5) . ? C35 C36 1.373(6) . ? C35 C34 1.377(6) . ? C34 H34 0.93 . ? C17 C16 1.365(6) . ? C17 H17 0.93 . ? C43 C44 1.373(6) . ? C43 H43 0.93 . ? C21 C23 1.385(6) . ? C21 C20 1.394(5) . ? C21 C22 1.483(6) . ? C18 C19 1.363(7) . ? C63 C64 1.380(5) . ? C63 H63 0.93 . ? C40 C39 1.387(6) . ? C40 H40 0.93 . ? C57 C56 1.374(6) . ? C57 C52 1.393(5) . ? C57 H57 0.93 . ? C60 H60 0.93 . ? C32 C37 1.386(5) . ? C20 C19 1.369(6) . ? C20 H20 0.93 . ? C58 C64 1.380(5) . ? C53 C54 1.375(6) . ? C53 C52 1.394(5) . ? C53 H53 0.93 . ? C54 C55 1.378(5) . ? C54 H54 0.93 . ? C44 H44 0.93 . ? C56 C55 1.395(6) . ? C56 H56 0.93 . ? C16 H16 0.93 . ? C37 C36 1.383(6) . ? C37 H37 0.93 . ? C36 H36 0.93 . ? C64 H64 0.93 . ? C39 H39 0.93 . ? C14 H14 0.93 . ? C23 H23 0.93 . ? C19 H19 0.93 . ? 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 O11 La1 O55 91.67(9) . 3_566 ? O11 La1 O31 84.03(10) . 3_565 ? O55 La1 O31 141.61(8) 3_566 3_565 ? O11 La1 O12 96.12(9) . 3_565 ? O55 La1 O12 143.56(8) 3_566 3_565 ? O31 La1 O12 74.74(8) 3_565 3_565 ? O11 La1 O32 141.02(9) . 3 ? O55 La1 O32 78.57(8) 3_566 3 ? O31 La1 O32 126.15(9) 3_565 3 ? O12 La1 O32 73.08(8) 3_565 3 ? O11 La1 O34 143.43(9) . 4_565 ? O55 La1 O34 87.13(9) 3_566 4_565 ? O31 La1 O34 74.80(9) 3_565 4_565 ? O12 La1 O34 106.32(9) 3_565 4_565 ? O32 La1 O34 74.37(8) 3 4_565 ? O11 La1 O101 72.14(9) . . ? O55 La1 O101 71.16(8) 3_566 . ? O31 La1 O101 71.23(8) 3_565 . ? O12 La1 O101 144.88(8) 3_565 . ? O32 La1 O101 135.96(8) 3 . ? O34 La1 O101 72.93(8) 4_565 . ? O11 La1 O102 69.46(10) . . ? O55 La1 O102 74.26(9) 3_566 . ? O31 La1 O102 137.17(9) 3_565 . ? O12 La1 O102 75.37(9) 3_565 . ? O32 La1 O102 71.57(9) 3 . ? O34 La1 O102 143.69(9) 4_565 . ? O101 La1 O102 126.55(10) . . ? O35 La2 O51 143.76(9) . . ? O35 La2 O15 94.58(10) . . ? O51 La2 O15 85.25(10) . . ? O35 La2 O52 83.55(9) . 1_545 ? O51 La2 O52 118.24(9) . 1_545 ? O15 La2 O52 141.30(9) . 1_545 ? O35 La2 O54 81.62(9) . 2_556 ? O51 La2 O54 77.97(9) . 2_556 ? O15 La2 O54 144.36(9) . 2_556 ? O52 La2 O54 73.81(8) 1_545 2_556 ? O35 La2 O203 148.72(9) . . ? O51 La2 O203 67.43(9) . . ? O15 La2 O203 84.21(9) . . ? O52 La2 O203 78.37(8) 1_545 . ? O54 La2 O203 116.74(9) 2_556 . ? O35 La2 O202 73.95(9) . . ? O51 La2 O202 71.46(9) . . ? O15 La2 O202 72.57(9) . . ? O52 La2 O202 141.52(8) 1_545 . ? O54 La2 O202 72.34(8) 2_556 . ? O203 La2 O202 134.01(8) . . ? O35 La2 O201 77.35(9) . . ? O51 La2 O201 135.47(9) . . ? O15 La2 O201 71.80(9) . . ? O52 La2 O201 70.09(9) 1_545 . ? O54 La2 O201 139.78(8) 2_556 . ? O203 La2 O201 72.59(9) . . ? O202 La2 O201 131.58(10) . . ? C42 O35 La2 145.2(2) . . ? C22 O15 La2 161.4(3) . . ? C51 O51 La2 149.9(2) . . ? C11 O12 La1 123.3(2) . 3_565 ? C31 O32 La1 131.0(2) . 3 ? C42 O34 La1 139.0(2) . 4_666 ? C62 O55 La1 146.0(2) . 3_566 ? O51 C51 O52 122.8(4) . . ? O51 C51 C52 117.9(3) . . ? O52 C51 C52 119.3(3) . . ? C31 O31 La1 136.7(2) . 3_565 ? C11 O11 La1 172.6(3) . . ? C38 O33 C35 122.1(3) . . ? C51 O52 La2 138.0(2) . 1_565 ? C58 O53 C55 122.1(3) . . ? C18 C24 C23 118.9(4) . . ? C18 C24 H24 120.5 . . ? C23 C24 H24 120.5 . . ? O32 C31 O31 121.8(4) . . ? O32 C31 C32 119.3(3) . . ? O31 C31 C32 118.9(3) . . ? C62 O54 La2 134.4(2) . 2_556 ? C60 C61 C63 118.8(3) . . ? C60 C61 C62 120.9(3) . . ? C63 C61 C62 120.3(3) . . ? O11 C11 O12 122.2(4) . . ? O11 C11 C12 118.8(3) . . ? O12 C11 C12 119.0(3) . . ? C17 C12 C13 118.5(4) . . ? C17 C12 C11 120.3(3) . . ? C13 C12 C11 121.0(3) . . ? C34 C33 C32 120.6(4) . . ? C34 C33 H33 119.7 . . ? C32 C33 H33 119.7 . . ? O35 C42 O34 123.0(4) . . ? O35 C42 C41 117.1(3) . . ? O34 C42 C41 119.9(3) . . ? C15 O13 C18 122.5(3) . . ? C60 C59 C58 118.6(4) . . ? C60 C59 H59 120.7 . . ? C58 C59 H59 120.7 . . ? C40 C41 C43 118.2(4) . . ? C40 C41 C42 122.3(3) . . ? C43 C41 C42 119.5(3) . . ? O13 C15 C16 114.5(4) . . ? O13 C15 C14 124.7(4) . . ? C16 C15 C14 120.6(4) . . ? C14 C13 C12 121.2(4) . . ? C14 C13 H13 119.4 . . ? C12 C13 H13 119.4 . . ? O33 C38 C44 114.9(3) . . ? O33 C38 C39 124.9(4) . . ? C44 C38 C39 120.1(4) . . ? C36 C35 C34 120.6(4) . . ? C36 C35 O33 123.3(4) . . ? C34 C35 O33 115.9(4) . . ? C35 C34 C33 119.9(4) . . ? C35 C34 H34 120 . . ? C33 C34 H34 120 . . ? C16 C17 C12 120.6(4) . . ? C16 C17 H17 119.7 . . ? C12 C17 H17 119.7 . . ? C44 C43 C41 120.8(4) . . ? C44 C43 H43 119.6 . . ? C41 C43 H43 119.6 . . ? C23 C21 C20 117.1(4) . . ? C23 C21 C22 122.1(3) . . ? C20 C21 C22 120.7(4) . . ? C19 C18 C24 120.4(4) . . ? C19 C18 O13 118.1(4) . . ? C24 C18 O13 121.2(4) . . ? O14 C22 O15 122.4(4) . . ? O14 C22 C21 118.5(3) . . ? O15 C22 C21 119.1(3) . . ? O55 C62 O54 122.7(3) . . ? O55 C62 C61 118.3(3) . . ? O54 C62 C61 119.0(3) . . ? C64 C63 C61 120.2(4) . . ? C64 C63 H63 119.9 . . ? C61 C63 H63 119.9 . . ? C41 C40 C39 121.6(3) . . ? C41 C40 H40 119.2 . . ? C39 C40 H40 119.2 . . ? C56 C57 C52 121.3(4) . . ? C56 C57 H57 119.4 . . ? C52 C57 H57 119.4 . . ? C61 C60 C59 121.6(3) . . ? C61 C60 H60 119.2 . . ? C59 C60 H60 119.2 . . ? C33 C32 C37 118.5(4) . . ? C33 C32 C31 120.5(3) . . ? C37 C32 C31 121.0(3) . . ? C19 C20 C21 120.7(4) . . ? C19 C20 H20 119.7 . . ? C21 C20 H20 119.7 . . ? O53 C58 C64 115.7(3) . . ? O53 C58 C59 123.8(4) . . ? C64 C58 C59 120.4(4) . . ? C54 C53 C52 120.9(4) . . ? C54 C53 H53 119.5 . . ? C52 C53 H53 119.5 . . ? C53 C54 C55 120.0(4) . . ? C53 C54 H54 120 . . ? C55 C54 H54 120 . . ? C57 C52 C53 118.3(4) . . ? C57 C52 C51 121.1(3) . . ? C53 C52 C51 120.6(3) . . ? C43 C44 C38 120.1(4) . . ? C43 C44 H44 119.9 . . ? C38 C44 H44 119.9 . . ? C57 C56 C55 119.3(4) . . ? C57 C56 H56 120.3 . . ? C55 C56 H56 120.3 . . ? C17 C16 C15 120.4(4) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C32 C37 C36 121.1(3) . . ? C32 C37 H37 119.4 . . ? C36 C37 H37 119.4 . . ? C35 C36 C37 119.3(4) . . ? C35 C36 H36 120.4 . . ? C37 C36 H36 120.4 . . ? C58 C64 C63 120.4(3) . . ? C58 C64 H64 119.8 . . ? C63 C64 H64 119.8 . . ? C38 C39 C40 119.0(4) . . ? C38 C39 H39 120.5 . . ? C40 C39 H39 120.5 . . ? C13 C14 C15 118.6(4) . . ? C13 C14 H14 120.7 . . ? C15 C14 H14 120.7 . . ? C24 C23 C21 122.2(4) . . ? C24 C23 H23 118.9 . . ? C21 C23 H23 118.9 . . ? C54 C55 O53 116.3(4) . . ? C54 C55 C56 120.2(4) . . ? O53 C55 C56 123.3(4) . . ? C18 C19 C20 120.6(4) . . ? C18 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ?