# Electronic Supplementary Material (ESI) for Dalton Transactions # 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_meso-[(EBI*)CeI(THF)] _database_code_depnum_ccdc_archive 'CCDC 886148' #TrackingRef 'CrystallographicData.cif' #============================================================================== _audit_creation_date 12-06-30 _audit_creation_method CRYSTALS_ver_14.40 _oxford_structure_analysis_title 5566 _chemical_name_systematic . _chemical_melting_point 'not measured' _cell_length_a 9.2981(1) _cell_length_b 19.2885(2) _cell_length_c 35.5339(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 6372.88(12) _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a ' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x,-y+1/2,z+1/2 -x,y+1/2,-z+1/2 -x+1/2,-y,z+1/2 x+1/2,y,-z+1/2 x+1/2,-y+1/2,-z -x+1/2,y+1/2,z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Ce -0.2486 2.6331 21.1671 2.8122 19.7695 0.2268 11.8513 17.6083 3.3305 127.1130 1.8626 'International Tables Vol C 4.2.6.8 and 6.1.1.4' I -0.4742 1.8119 20.1472 4.3470 18.9949 0.3814 7.5138 27.7660 2.2735 66.8776 4.0712 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 8 # Given Formula = C64 H80 Ce2 I2 O1 # Dc = 2.92 Fooo = 3064.00 Mu = 48.30 M = 1399.39 # Found Formula = C36 H48 Ce1 I1 O1 # Dc = 1.59 FOOO = 3064.00 Mu = 24.24 M = 763.80 _chemical_formula_sum 'C36 H48 Ce1 I1 O1' _chemical_formula_moiety 'C36 H48 Ce1 I1 O1' _chemical_compound_source . _chemical_formula_weight 763.80 _cell_measurement_reflns_used 71481 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description plate _exptl_crystal_colour clear_intense_orange _exptl_crystal_size_min 0.080 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_max 0.250 _exptl_crystal_density_diffrn 1.592 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 3064.000 _exptl_absorpt_coefficient_mu 2.424 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Multi-scan from symmetry-related measurements using Sortav (Blessing 1995). ; _exptl_absorpt_correction_T_min 0.673 _exptl_absorpt_correction_T_max 0.819 _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% . _diffrn_ambient_temperature 150 _diffrn_reflns_number 51825 _reflns_number_total 7182 _diffrn_reflns_av_R_equivalents 0.088 # Number of reflections without Friedels Law is 14185 # Number of reflections with Friedels Law is 7182 # Theoretical number of reflections is about 7285 _diffrn_reflns_theta_min 5.109 _diffrn_reflns_theta_max 27.452 _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 26.629 _diffrn_measured_fraction_theta_full 0.987 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 45 _reflns_limit_h_min 0 _reflns_limit_h_max 12 _reflns_limit_k_min 0 _reflns_limit_k_max 24 _reflns_limit_l_min 0 _reflns_limit_l_max 46 _oxford_diffrn_Wilson_B_factor 2.08 _oxford_diffrn_Wilson_scale 518.08 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -1.81 _refine_diff_density_max 1.90 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-3.0\s(I) _refine_ls_number_reflns 7182 _refine_ls_number_restraints 180 _refine_ls_number_parameters 389 _oxford_refine_ls_R_factor_ref 0.0894 _refine_ls_wR_factor_ref 0.1222 _refine_ls_goodness_of_fit_ref 0.9596 _refine_ls_shift/su_max 0.0010361 _refine_ls_shift/su_mean 0.0000461 # The values computed with all filters except I/sigma _oxford_reflns_number_all 7182 _refine_ls_R_factor_all 0.0894 _refine_ls_wR_factor_all 0.1222 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 4811 _refine_ls_R_factor_gt 0.0449 _refine_ls_wR_factor_gt 0.0936 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr #undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 10.7 14.9 7.38 1.91 ; # Insert your own references if required - in alphabetical order 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Ce1 Ce 0.45626(4) 0.263496(18) 0.372581(10) 0.0222 1.0000 Uani . . . . . . I1 I 0.21292(5) 0.37050(3) 0.385893(15) 0.0391 1.0000 Uani . . . . . . O1 O 0.3075(6) 0.1671(2) 0.39848(15) 0.0467 1.0000 Uani D . . . . . C2 C 0.3466(18) 0.0941(4) 0.3959(4) 0.0471 0.414(15) Uani D . P 1 1 . C3 C 0.2897(19) 0.0626(6) 0.4318(4) 0.0461 0.414(15) Uani D . P 1 1 . C4 C 0.1405(15) 0.1008(8) 0.4329(5) 0.0518 0.414(15) Uani D . P 1 1 . C5 C 0.1944(17) 0.1740(6) 0.4268(4) 0.0508 0.414(15) Uani D . P 1 1 . C6 C 0.3312(12) 0.0924(3) 0.3963(4) 0.0523 0.586(15) Uani D . P 1 2 . C7 C 0.1928(14) 0.0610(4) 0.4107(4) 0.0565 0.586(15) Uani D . P 1 2 . C8 C 0.1632(14) 0.1136(6) 0.4436(3) 0.0523 0.586(15) Uani D . P 1 2 . C9 C 0.1816(11) 0.1794(4) 0.4218(4) 0.0519 0.586(15) Uani D . P 1 2 . C11 C 0.7372(7) 0.2702(3) 0.39134(18) 0.0258 1.0000 Uani . . . . . . C12 C 0.6958(7) 0.3394(3) 0.39925(18) 0.0247 1.0000 Uani . . . . . . C13 C 0.5986(7) 0.3422(4) 0.42937(18) 0.0267 1.0000 Uani . . . . . . C14 C 0.5847(7) 0.2721(3) 0.44336(17) 0.0238 1.0000 Uani . . . . . . C15 C 0.5033(7) 0.2454(4) 0.47420(18) 0.0298 1.0000 Uani . . . . . . C16 C 0.5241(8) 0.1768(4) 0.48446(19) 0.0319 1.0000 Uani . . . . . . C17 C 0.6145(8) 0.1327(4) 0.4622(2) 0.0333 1.0000 Uani . . . . . . C18 C 0.6823(8) 0.1557(4) 0.4301(2) 0.0305 1.0000 Uani . . . . . . C19 C 0.6722(6) 0.2281(3) 0.42024(18) 0.0239 1.0000 Uani . . . . . . C21 C 0.6310(7) 0.2588(4) 0.31054(17) 0.0250 1.0000 Uani . . . . . . C22 C 0.5301(8) 0.3119(3) 0.30225(17) 0.0246 1.0000 Uani . . . . . . C23 C 0.3905(8) 0.2838(4) 0.29706(19) 0.0292 1.0000 Uani . . . . . . C24 C 0.4043(7) 0.2096(3) 0.30073(17) 0.0232 1.0000 Uani . . . . . . C25 C 0.3002(7) 0.1560(4) 0.29809(19) 0.0287 1.0000 Uani . . . . . . C26 C 0.3458(8) 0.0880(4) 0.29944(19) 0.0298 1.0000 Uani . . . . . . C27 C 0.4959(8) 0.0713(3) 0.30301(19) 0.0280 1.0000 Uani . . . . . . C28 C 0.5991(8) 0.1225(3) 0.30658(18) 0.0261 1.0000 Uani . . . . . . C29 C 0.5534(7) 0.1937(3) 0.30720(17) 0.0230 1.0000 Uani . . . . . . C32 C 0.7634(8) 0.4033(4) 0.3822(2) 0.0361 1.0000 Uani . . . . . . C33 C 0.5473(9) 0.4092(4) 0.4461(2) 0.0392 1.0000 Uani . . . . . . C35 C 0.400(1) 0.2911(4) 0.4953(2) 0.0434 1.0000 Uani . . . . . . C36 C 0.4499(10) 0.1469(5) 0.5185(2) 0.0474 1.0000 Uani . . . . . . C37 C 0.6422(12) 0.0590(4) 0.4764(3) 0.0569 1.0000 Uani . . . . . . C38 C 0.7643(10) 0.1066(4) 0.4048(2) 0.0476 1.0000 Uani . . . . . . C42 C 0.5616(9) 0.3875(4) 0.2988(2) 0.0363 1.0000 Uani . . . . . . C43 C 0.2651(8) 0.3253(4) 0.2822(2) 0.0384 1.0000 Uani . . . . . . C45 C 0.1415(8) 0.1742(5) 0.2966(3) 0.0453 1.0000 Uani . . . . . . C46 C 0.2405(9) 0.0287(4) 0.2967(3) 0.0454 1.0000 Uani . . . . . . C47 C 0.5408(10) -0.0048(4) 0.3016(2) 0.0414 1.0000 Uani . . . . . . C48 C 0.7580(8) 0.1045(4) 0.3038(2) 0.0334 1.0000 Uani . . . . . . C51 C 0.8386(7) 0.2502(3) 0.3594(2) 0.0297 1.0000 Uani . . . . . . C52 C 0.7882(7) 0.2711(4) 0.31997(18) 0.0283 1.0000 Uani . . . . . . H21 H 0.4507 0.0915 0.3974 0.0560 0.414(15) Uiso R . P 1 1 . H22 H 0.3140 0.0713 0.3731 0.0562 0.414(15) Uiso R . P 1 1 . H31 H 0.3453 0.0725 0.4541 0.0550 0.414(15) Uiso R . P 1 1 . H32 H 0.2785 0.0129 0.4292 0.0550 0.414(15) Uiso R . P 1 1 . H42 H 0.0972 0.0966 0.4576 0.0620 0.414(15) Uiso R . P 1 1 . H41 H 0.0754 0.0821 0.4141 0.0621 0.414(15) Uiso R . P 1 1 . H51 H 0.2207 0.1987 0.4497 0.0601 0.414(15) Uiso R . P 1 1 . H52 H 0.1157 0.1978 0.4143 0.0600 0.414(15) Uiso R . P 1 1 . H62 H 0.4159 0.0770 0.4099 0.0590 0.586(15) Uiso R . P 1 2 . H61 H 0.3398 0.0798 0.3699 0.0591 0.586(15) Uiso R . P 1 2 . H71 H 0.2095 0.0149 0.4207 0.0681 0.586(15) Uiso R . P 1 2 . H72 H 0.1157 0.0594 0.3924 0.0680 0.586(15) Uiso R . P 1 2 . H81 H 0.2271 0.1075 0.4649 0.0651 0.586(15) Uiso R . P 1 2 . H82 H 0.0645 0.1090 0.4520 0.0650 0.586(15) Uiso R . P 1 2 . H91 H 0.2068 0.2153 0.4399 0.0661 0.586(15) Uiso R . P 1 2 . H92 H 0.0977 0.1937 0.4075 0.0660 0.586(15) Uiso R . P 1 2 . H321 H 0.6891 0.4340 0.3734 0.0539 1.0000 Uiso R . . . . . H322 H 0.8201 0.4263 0.4009 0.0540 1.0000 Uiso R . . . . . H323 H 0.8235 0.3906 0.3614 0.0539 1.0000 Uiso R . . . . . H331 H 0.4445 0.4088 0.4486 0.0592 1.0000 Uiso R . . . . . H332 H 0.5894 0.4156 0.4706 0.0590 1.0000 Uiso R . . . . . H333 H 0.5746 0.4474 0.4301 0.0590 1.0000 Uiso R . . . . . H352 H 0.3288 0.2625 0.5072 0.0650 1.0000 Uiso R . . . . . H351 H 0.4504 0.3173 0.5140 0.0651 1.0000 Uiso R . . . . . H353 H 0.3532 0.3224 0.4783 0.0652 1.0000 Uiso R . . . . . H362 H 0.4024 0.1046 0.5117 0.0710 1.0000 Uiso R . . . . . H361 H 0.5189 0.1377 0.5379 0.0710 1.0000 Uiso R . . . . . H363 H 0.3802 0.1794 0.5276 0.0711 1.0000 Uiso R . . . . . H371 H 0.7407 0.0470 0.4721 0.0851 1.0000 Uiso R . . . . . H373 H 0.6216 0.0566 0.5028 0.0850 1.0000 Uiso R . . . . . H372 H 0.5814 0.0272 0.4629 0.0849 1.0000 Uiso R . . . . . H381 H 0.7287 0.1103 0.3795 0.0710 1.0000 Uiso R . . . . . H383 H 0.8642 0.1186 0.4051 0.0710 1.0000 Uiso R . . . . . H382 H 0.7526 0.0599 0.4135 0.0710 1.0000 Uiso R . . . . . H421 H 0.5346 0.4033 0.2742 0.0551 1.0000 Uiso R . . . . . H422 H 0.5087 0.4130 0.3174 0.0550 1.0000 Uiso R . . . . . H423 H 0.6622 0.3963 0.3024 0.0551 1.0000 Uiso R . . . . . H431 H 0.2222 0.3017 0.2612 0.0580 1.0000 Uiso R . . . . . H432 H 0.1942 0.3308 0.3017 0.0581 1.0000 Uiso R . . . . . H433 H 0.2980 0.3703 0.2741 0.0581 1.0000 Uiso R . . . . . H451 H 0.0871 0.1385 0.3088 0.0679 1.0000 Uiso R . . . . . H452 H 0.1257 0.2178 0.3092 0.0680 1.0000 Uiso R . . . . . H453 H 0.1118 0.1780 0.2708 0.0680 1.0000 Uiso R . . . . . H462 H 0.2700 -0.0026 0.2772 0.0681 1.0000 Uiso R . . . . . H461 H 0.2373 0.0041 0.3202 0.0680 1.0000 Uiso R . . . . . H463 H 0.1463 0.0457 0.2910 0.0681 1.0000 Uiso R . . . . . H472 H 0.6424 -0.0086 0.3053 0.0622 1.0000 Uiso R . . . . . H471 H 0.4922 -0.0297 0.3213 0.0619 1.0000 Uiso R . . . . . H473 H 0.5152 -0.0242 0.2775 0.0621 1.0000 Uiso R . . . . . H481 H 0.8149 0.1456 0.3065 0.0503 1.0000 Uiso R . . . . . H483 H 0.7835 0.0727 0.3234 0.0502 1.0000 Uiso R . . . . . H482 H 0.7784 0.0840 0.2799 0.0500 1.0000 Uiso R . . . . . H511 H 0.9313 0.2714 0.3639 0.0359 1.0000 Uiso R . . . . . H512 H 0.8511 0.2005 0.3598 0.0358 1.0000 Uiso R . . . . . H521 H 0.8059 0.3204 0.3178 0.0339 1.0000 Uiso R . . . . . H522 H 0.8462 0.2469 0.3015 0.0339 1.0000 Uiso 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 Ce1 0.01917(15) 0.02490(16) 0.02259(16) 0.00009(15) 0.00000(14) -0.00122(15) I1 0.0318(2) 0.0410(3) 0.0444(3) -0.0048(2) -0.0009(2) 0.0100(2) O1 0.049(3) 0.044(3) 0.047(3) 0.007(2) 0.005(2) -0.013(2) C2 0.056(6) 0.042(5) 0.044(5) 0.004(5) 0.005(5) -0.020(5) C3 0.055(6) 0.039(6) 0.044(6) 0.004(5) 0.005(6) -0.018(5) C4 0.055(6) 0.048(6) 0.052(6) 0.005(6) 0.006(6) -0.016(5) C5 0.052(5) 0.049(5) 0.052(5) 0.007(5) 0.007(5) -0.013(5) C6 0.057(5) 0.047(4) 0.053(5) -0.002(5) 0.010(5) -0.014(4) C7 0.054(5) 0.053(5) 0.062(6) -0.002(5) 0.016(5) -0.011(5) C8 0.047(5) 0.058(5) 0.052(6) 0.002(5) 0.013(5) -0.008(5) C9 0.043(5) 0.056(5) 0.056(5) 0.005(4) 0.005(4) -0.007(5) C11 0.019(3) 0.030(3) 0.028(3) -0.001(3) -0.006(2) -0.002(3) C12 0.024(3) 0.018(3) 0.033(3) 0.006(3) -0.008(3) -0.005(3) C13 0.026(3) 0.028(3) 0.026(3) -0.003(3) -0.001(3) -0.001(3) C14 0.021(3) 0.029(4) 0.021(3) -0.004(3) -0.006(2) 0.003(3) C15 0.027(3) 0.041(4) 0.021(3) 0.001(3) -0.003(2) -0.006(3) C16 0.033(4) 0.032(4) 0.031(3) 0.002(3) 0.000(3) -0.008(3) C17 0.037(4) 0.026(3) 0.037(4) 0.005(3) 0.000(3) 0.000(3) C18 0.029(4) 0.028(3) 0.035(4) 0.001(3) -0.001(3) 0.000(3) C19 0.018(3) 0.029(3) 0.025(3) 0.003(3) -0.005(2) -0.005(3) C21 0.024(3) 0.026(3) 0.024(3) 0.000(3) -0.001(2) 0.001(3) C22 0.031(4) 0.028(3) 0.015(3) 0.002(2) 0.002(3) 0.006(3) C23 0.031(4) 0.035(4) 0.022(3) 0.002(3) -0.003(3) 0.005(3) C24 0.021(3) 0.029(3) 0.019(3) 0.000(3) -0.003(2) 0.008(3) C25 0.022(3) 0.036(4) 0.028(3) -0.002(3) -0.002(3) -0.002(3) C26 0.037(4) 0.028(4) 0.024(3) 0.001(3) -0.002(3) -0.007(3) C27 0.035(4) 0.020(3) 0.029(3) 0.002(3) 0.002(3) 0.002(3) C28 0.030(3) 0.028(3) 0.020(3) -0.001(3) 0.001(3) 0.005(3) C29 0.027(3) 0.023(3) 0.019(3) -0.001(2) -0.001(3) 0.002(3) C32 0.035(4) 0.031(4) 0.042(4) -0.002(3) -0.001(3) -0.005(3) C33 0.045(4) 0.026(4) 0.047(4) -0.011(3) -0.005(4) 0.005(3) C35 0.046(5) 0.045(5) 0.039(4) -0.004(4) 0.014(4) 0.003(4) C36 0.054(5) 0.052(5) 0.036(4) 0.011(4) 0.006(4) -0.010(4) C37 0.075(7) 0.029(4) 0.066(6) 0.016(4) 0.016(5) 0.003(4) C38 0.061(6) 0.027(4) 0.054(5) 0.004(4) 0.018(4) 0.007(4) C42 0.045(5) 0.026(4) 0.038(4) 0.003(3) 0.000(3) -0.001(3) C43 0.034(4) 0.037(4) 0.044(4) -0.004(3) -0.018(3) 0.013(3) C45 0.021(4) 0.052(5) 0.063(6) -0.001(4) -0.007(4) -0.002(3) C46 0.046(5) 0.034(4) 0.057(5) 0.002(4) -0.004(4) -0.018(4) C47 0.054(5) 0.022(3) 0.048(4) 0.003(3) 0.001(4) -0.002(4) C48 0.029(4) 0.037(4) 0.034(4) -0.009(3) -0.002(3) 0.011(3) C51 0.017(3) 0.032(4) 0.040(4) 0.004(3) 0.000(3) 0.001(2) C52 0.023(3) 0.032(4) 0.029(3) 0.000(3) 0.005(3) -0.006(3) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.063873(12) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ce1 . I1 . 3.0988(6) yes Ce1 . O1 . 2.494(4) yes Ce1 . C11 . 2.699(6) yes Ce1 . C12 . 2.829(6) yes Ce1 . C13 . 2.851(6) yes Ce1 . C14 . 2.789(6) yes Ce1 . C19 . 2.714(6) yes Ce1 . C21 . 2.740(6) yes Ce1 . C22 . 2.755(6) yes Ce1 . C23 . 2.780(7) yes Ce1 . C24 . 2.799(6) yes Ce1 . C29 . 2.833(6) yes O1 . C2 . 1.455(6) yes O1 . C5 . 1.463(6) yes O1 . C6 . 1.459(5) yes O1 . C9 . 1.454(5) yes C2 . C3 . 1.509(6) yes C2 . H21 . 0.970 no C2 . H22 . 0.972 no C3 . C4 . 1.571(6) yes C3 . H31 . 0.967 no C3 . H32 . 0.968 no C4 . C5 . 1.515(6) yes C4 . H42 . 0.968 no C4 . H41 . 0.971 no C5 . H51 . 0.971 no C5 . H52 . 0.971 no C6 . C7 . 1.511(6) yes C6 . H62 . 0.971 no C6 . H61 . 0.974 no C7 . C8 . 1.573(5) yes C7 . H71 . 0.970 no C7 . H72 . 0.969 no C8 . C9 . 1.497(6) yes C8 . H81 . 0.968 no C8 . H82 . 0.968 no C9 . H91 . 0.973 no C9 . H92 . 0.971 no C11 . C12 . 1.417(9) yes C11 . C19 . 1.442(9) yes C11 . C51 . 1.525(9) yes C12 . C13 . 1.402(9) yes C12 . C32 . 1.510(9) yes C13 . C14 . 1.447(9) yes C13 . C33 . 1.501(9) yes C14 . C15 . 1.428(9) yes C14 . C19 . 1.434(9) yes C15 . C16 . 1.385(10) yes C15 . C35 . 1.504(10) yes C16 . C17 . 1.434(10) yes C16 . C36 . 1.507(10) yes C17 . C18 . 1.376(10) yes C17 . C37 . 1.530(10) yes C18 . C19 . 1.444(9) yes C18 . C38 . 1.513(10) yes C21 . C22 . 1.421(9) yes C21 . C29 . 1.453(9) yes C21 . C52 . 1.518(9) yes C22 . C23 . 1.420(10) yes C22 . C42 . 1.492(9) yes C23 . C24 . 1.443(10) yes C23 . C43 . 1.510(9) yes C24 . C25 . 1.418(10) yes C24 . C29 . 1.438(9) yes C25 . C26 . 1.379(10) yes C25 . C45 . 1.517(10) yes C26 . C27 . 1.439(10) yes C26 . C46 . 1.510(10) yes C27 . C28 . 1.382(10) yes C27 . C47 . 1.527(10) yes C28 . C29 . 1.437(9) yes C28 . C48 . 1.522(10) yes C32 . H321 . 0.961 no C32 . H322 . 0.956 no C32 . H323 . 0.959 no C33 . H331 . 0.960 no C33 . H332 . 0.961 no C33 . H333 . 0.964 no C35 . H352 . 0.959 no C35 . H351 . 0.959 no C35 . H353 . 0.958 no C36 . H362 . 0.960 no C36 . H361 . 0.959 no C36 . H363 . 0.958 no C37 . H371 . 0.958 no C37 . H373 . 0.958 no C37 . H372 . 0.961 no C38 . H381 . 0.960 no C38 . H383 . 0.957 no C38 . H382 . 0.960 no C42 . H421 . 0.958 no C42 . H422 . 0.958 no C42 . H423 . 0.959 no C43 . H431 . 0.962 no C43 . H432 . 0.963 no C43 . H433 . 0.963 no C45 . H451 . 0.958 no C45 . H452 . 0.963 no C45 . H453 . 0.960 no C46 . H462 . 0.960 no C46 . H461 . 0.958 no C46 . H463 . 0.957 no C47 . H472 . 0.956 no C47 . H471 . 0.961 no C47 . H473 . 0.964 no C48 . H481 . 0.957 no C48 . H483 . 0.957 no C48 . H482 . 0.956 no C51 . C52 . 1.531(9) yes C51 . H511 . 0.967 no C51 . H512 . 0.967 no C52 . H521 . 0.968 no C52 . H522 . 0.970 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag I1 . Ce1 . O1 . 92.05(12) yes I1 . Ce1 . C11 . 129.56(14) yes O1 . Ce1 . C11 . 118.77(19) yes I1 . Ce1 . C12 . 100.31(13) yes O1 . Ce1 . C12 . 134.35(18) yes C11 . Ce1 . C12 . 29.59(19) yes I1 . Ce1 . C13 . 82.89(14) yes O1 . Ce1 . C13 . 113.16(19) yes C11 . Ce1 . C13 . 49.5(2) yes C12 . Ce1 . C13 . 28.58(19) yes I1 . Ce1 . C14 . 97.79(13) yes O1 . Ce1 . C14 . 87.07(19) yes C11 . Ce1 . C14 . 50.20(19) yes C12 . Ce1 . C14 . 47.94(19) yes C13 . Ce1 . C14 . 29.70(19) yes I1 . Ce1 . C19 . 127.77(14) yes O1 . Ce1 . C19 . 89.56(18) yes C11 . Ce1 . C19 . 30.90(19) yes C12 . Ce1 . C19 . 48.61(18) yes C13 . Ce1 . C19 . 49.38(19) yes I1 . Ce1 . C21 . 125.31(14) yes O1 . Ce1 . C21 . 126.92(19) yes C11 . Ce1 . C21 . 68.06(19) yes C12 . Ce1 . C21 . 79.6(2) yes C13 . Ce1 . C21 . 108.19(19) yes I1 . Ce1 . C22 . 95.43(14) yes O1 . Ce1 . C22 . 136.55(19) yes C11 . Ce1 . C22 . 88.1(2) yes C12 . Ce1 . C22 . 86.1(2) yes C13 . Ce1 . C22 . 110.2(2) yes I1 . Ce1 . C23 . 83.86(15) yes O1 . Ce1 . C23 . 109.8(2) yes C11 . Ce1 . C23 . 116.4(2) yes C12 . Ce1 . C23 . 115.1(2) yes C13 . Ce1 . C23 . 135.3(2) yes I1 . Ce1 . C24 . 105.11(13) yes O1 . Ce1 . C24 . 87.91(19) yes C11 . Ce1 . C24 . 114.22(19) yes C12 . Ce1 . C24 . 129.34(19) yes C13 . Ce1 . C24 . 157.48(19) yes I1 . Ce1 . C29 . 132.41(13) yes O1 . Ce1 . C29 . 97.17(18) yes C11 . Ce1 . C29 . 85.2(2) yes C12 . Ce1 . C29 . 105.7(2) yes C13 . Ce1 . C29 . 133.3(2) yes C14 . Ce1 . C19 . 30.17(19) yes C14 . Ce1 . C21 . 118.3(2) yes C19 . Ce1 . C21 . 93.15(19) yes C14 . Ce1 . C22 . 133.7(2) yes C19 . Ce1 . C22 . 117.8(2) yes C21 . Ce1 . C22 . 29.97(19) yes C14 . Ce1 . C23 . 163.0(2) yes C19 . Ce1 . C23 . 143.2(2) yes C21 . Ce1 . C23 . 50.1(2) yes C22 . Ce1 . C23 . 29.7(2) yes C14 . Ce1 . C24 . 156.70(18) yes C19 . Ce1 . C24 . 127.11(19) yes C21 . Ce1 . C24 . 49.92(19) yes C22 . Ce1 . C24 . 48.8(2) yes C23 . Ce1 . C24 . 30.0(2) yes C14 . Ce1 . C29 . 129.13(19) yes C19 . Ce1 . C29 . 98.99(19) yes C21 . Ce1 . C29 . 30.16(19) yes C22 . Ce1 . C29 . 48.54(19) yes C23 . Ce1 . C29 . 49.11(19) yes C24 . Ce1 . C29 . 29.59(18) yes Ce1 . O1 . C2 . 124.0(5) yes Ce1 . O1 . C5 . 125.7(5) yes C2 . O1 . C5 . 108.19(7) yes Ce1 . O1 . C6 . 129.3(4) yes Ce1 . O1 . C9 . 122.3(4) yes C6 . O1 . C9 . 108.20(7) yes O1 . C2 . C3 . 104.42(7) yes O1 . C2 . H21 . 107.3 no C3 . C2 . H21 . 106.4 no O1 . C2 . H22 . 114.4 no C3 . C2 . H22 . 114.4 no H21 . C2 . H22 . 109.4 no C2 . C3 . C4 . 98.16(7) yes C2 . C3 . H31 . 115.2 no C4 . C3 . H31 . 111.0 no C2 . C3 . H32 . 111.0 no C4 . C3 . H32 . 111.8 no H31 . C3 . H32 . 109.4 no C3 . C4 . C5 . 98.17(7) yes C3 . C4 . H42 . 110.5 no C5 . C4 . H42 . 110.1 no C3 . C4 . H41 . 111.0 no C5 . C4 . H41 . 117.1 no H42 . C4 . H41 . 109.5 no C4 . C5 . O1 . 104.44(7) yes C4 . C5 . H51 . 115.0 no O1 . C5 . H51 . 116.0 no C4 . C5 . H52 . 104.9 no O1 . C5 . H52 . 105.6 no H51 . C5 . H52 . 109.9 no O1 . C6 . C7 . 104.45(7) yes O1 . C6 . H62 . 113.5 no C7 . C6 . H62 . 113.6 no O1 . C6 . H61 . 108.0 no C7 . C6 . H61 . 107.2 no H62 . C6 . H61 . 109.7 no C6 . C7 . C8 . 98.17(7) yes C6 . C7 . H71 . 110.8 no C8 . C7 . H71 . 110.3 no C6 . C7 . H72 . 114.6 no C8 . C7 . H72 . 113.1 no H71 . C7 . H72 . 109.5 no C7 . C8 . C9 . 98.13(7) yes C7 . C8 . H81 . 113.3 no C9 . C8 . H81 . 115.9 no C7 . C8 . H82 . 109.5 no C9 . C8 . H82 . 110.1 no H81 . C8 . H82 . 109.4 no C8 . C9 . O1 . 104.41(7) yes C8 . C9 . H91 . 106.8 no O1 . C9 . H91 . 107.4 no C8 . C9 . H92 . 114.8 no O1 . C9 . H92 . 113.3 no H91 . C9 . H92 . 109.7 no Ce1 . C11 . C12 . 80.3(4) yes Ce1 . C11 . C19 . 75.1(3) yes C12 . C11 . C19 . 106.0(6) yes Ce1 . C11 . C51 . 113.7(4) yes C12 . C11 . C51 . 123.6(6) yes C19 . C11 . C51 . 130.3(6) yes C11 . C12 . Ce1 . 70.1(3) yes C11 . C12 . C13 . 111.2(6) yes Ce1 . C12 . C13 . 76.6(4) yes C11 . C12 . C32 . 125.2(6) yes Ce1 . C12 . C32 . 128.0(4) yes C13 . C12 . C32 . 122.9(6) yes C12 . C13 . Ce1 . 74.9(4) yes C12 . C13 . C14 . 106.5(6) yes Ce1 . C13 . C14 . 72.8(3) yes C12 . C13 . C33 . 122.7(6) yes Ce1 . C13 . C33 . 126.3(5) yes C14 . C13 . C33 . 129.9(6) yes C13 . C14 . Ce1 . 77.5(3) yes C13 . C14 . C15 . 130.3(6) yes Ce1 . C14 . C15 . 116.3(4) yes C13 . C14 . C19 . 107.8(6) yes Ce1 . C14 . C19 . 72.0(3) yes C15 . C14 . C19 . 121.8(6) yes C14 . C15 . C16 . 118.1(6) yes C14 . C15 . C35 . 120.7(6) yes C16 . C15 . C35 . 121.2(6) yes C15 . C16 . C17 . 120.2(6) yes C15 . C16 . C36 . 120.8(7) yes C17 . C16 . C36 . 118.9(7) yes C16 . C17 . C18 . 122.3(6) yes C16 . C17 . C37 . 118.0(7) yes C18 . C17 . C37 . 119.6(7) yes C17 . C18 . C19 . 118.9(6) yes C17 . C18 . C38 . 121.6(7) yes C19 . C18 . C38 . 119.5(6) yes Ce1 . C19 . C18 . 116.3(4) yes Ce1 . C19 . C11 . 74.0(3) yes C18 . C19 . C11 . 133.8(6) yes Ce1 . C19 . C14 . 77.8(3) yes C18 . C19 . C14 . 118.0(6) yes C11 . C19 . C14 . 108.2(6) yes Ce1 . C21 . C22 . 75.6(4) yes Ce1 . C21 . C29 . 78.5(4) yes C22 . C21 . C29 . 106.2(6) yes Ce1 . C21 . C52 . 112.8(4) yes C22 . C21 . C52 . 124.6(6) yes C29 . C21 . C52 . 129.2(6) yes Ce1 . C22 . C21 . 74.4(3) yes Ce1 . C22 . C23 . 76.1(4) yes C21 . C22 . C23 . 110.7(6) yes Ce1 . C22 . C42 . 117.1(4) yes C21 . C22 . C42 . 126.4(7) yes C23 . C22 . C42 . 122.9(6) yes Ce1 . C23 . C22 . 74.2(4) yes Ce1 . C23 . C24 . 75.7(4) yes C22 . C23 . C24 . 106.7(6) yes Ce1 . C23 . C43 . 125.6(5) yes C22 . C23 . C43 . 123.3(6) yes C24 . C23 . C43 . 128.8(7) yes C23 . C24 . Ce1 . 74.3(4) yes C23 . C24 . C25 . 131.0(6) yes Ce1 . C24 . C25 . 116.7(4) yes C23 . C24 . C29 . 108.1(6) yes Ce1 . C24 . C29 . 76.5(4) yes C25 . C24 . C29 . 120.9(6) yes C24 . C25 . C26 . 118.7(6) yes C24 . C25 . C45 . 119.8(6) yes C26 . C25 . C45 . 121.3(7) yes C25 . C26 . C27 . 120.9(6) yes C25 . C26 . C46 . 121.3(7) yes C27 . C26 . C46 . 117.7(7) yes C26 . C27 . C28 . 121.4(6) yes C26 . C27 . C47 . 118.5(6) yes C28 . C27 . C47 . 120.0(7) yes C27 . C28 . C29 . 118.6(6) yes C27 . C28 . C48 . 120.3(6) yes C29 . C28 . C48 . 120.4(6) yes C21 . C29 . C24 . 107.9(5) yes C21 . C29 . C28 . 132.8(6) yes C24 . C29 . C28 . 119.1(6) yes C21 . C29 . Ce1 . 71.4(3) yes C24 . C29 . Ce1 . 73.9(4) yes C28 . C29 . Ce1 . 124.1(4) yes C12 . C32 . H321 . 109.5 no C12 . C32 . H322 . 109.2 no H321 . C32 . H322 . 109.7 no C12 . C32 . H323 . 110.0 no H321 . C32 . H323 . 109.1 no H322 . C32 . H323 . 109.4 no C13 . C33 . H331 . 110.2 no C13 . C33 . H332 . 109.8 no H331 . C33 . H332 . 108.8 no C13 . C33 . H333 . 110.0 no H331 . C33 . H333 . 108.8 no H332 . C33 . H333 . 109.1 no C15 . C35 . H352 . 108.9 no C15 . C35 . H351 . 109.9 no H352 . C35 . H351 . 109.5 no C15 . C35 . H353 . 110.1 no H352 . C35 . H353 . 109.2 no H351 . C35 . H353 . 109.1 no C16 . C36 . H362 . 109.7 no C16 . C36 . H361 . 110.0 no H362 . C36 . H361 . 109.2 no C16 . C36 . H363 . 109.2 no H362 . C36 . H363 . 109.2 no H361 . C36 . H363 . 109.4 no C17 . C37 . H371 . 109.6 no C17 . C37 . H373 . 109.5 no H371 . C37 . H373 . 109.5 no C17 . C37 . H372 . 109.3 no H371 . C37 . H372 . 109.2 no H373 . C37 . H372 . 109.7 no C18 . C38 . H381 . 109.8 no C18 . C38 . H383 . 109.3 no H381 . C38 . H383 . 109.1 no C18 . C38 . H382 . 109.7 no H381 . C38 . H382 . 109.5 no H383 . C38 . H382 . 109.4 no C22 . C42 . H421 . 109.6 no C22 . C42 . H422 . 110.1 no H421 . C42 . H422 . 109.2 no C22 . C42 . H423 . 110.7 no H421 . C42 . H423 . 108.6 no H422 . C42 . H423 . 108.6 no C23 . C43 . H431 . 109.9 no C23 . C43 . H432 . 109.6 no H431 . C43 . H432 . 109.2 no C23 . C43 . H433 . 109.7 no H431 . C43 . H433 . 109.1 no H432 . C43 . H433 . 109.4 no C25 . C45 . H451 . 109.4 no C25 . C45 . H452 . 109.5 no H451 . C45 . H452 . 109.6 no C25 . C45 . H453 . 109.3 no H451 . C45 . H453 . 109.5 no H452 . C45 . H453 . 109.5 no C26 . C46 . H462 . 109.7 no C26 . C46 . H461 . 109.9 no H462 . C46 . H461 . 109.0 no C26 . C46 . H463 . 110.3 no H462 . C46 . H463 . 108.8 no H461 . C46 . H463 . 109.1 no C27 . C47 . H472 . 109.8 no C27 . C47 . H471 . 109.2 no H472 . C47 . H471 . 109.1 no C27 . C47 . H473 . 109.6 no H472 . C47 . H473 . 109.6 no H471 . C47 . H473 . 109.5 no C28 . C48 . H481 . 110.0 no C28 . C48 . H483 . 109.9 no H481 . C48 . H483 . 108.7 no C28 . C48 . H482 . 110.1 no H481 . C48 . H482 . 108.7 no H483 . C48 . H482 . 109.5 no C11 . C51 . C52 . 115.1(5) yes C11 . C51 . H511 . 108.6 no C52 . C51 . H511 . 108.3 no C11 . C51 . H512 . 108.3 no C52 . C51 . H512 . 108.2 no H511 . C51 . H512 . 108.1 no C51 . C52 . C21 . 117.1(5) yes C51 . C52 . H521 . 106.3 no C21 . C52 . H521 . 107.5 no C51 . C52 . H522 . 108.8 no C21 . C52 . H522 . 108.1 no H521 . C52 . H522 . 108.9 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C2 . H61 . C26 . 159.0 0.966 2.509 3.429(12) yes C6 . H61 . C26 . 161.5 0.974 2.509 3.447(12) yes C48 . H481 . C52 . 140.5 0.957 2.480 3.276(12) yes C51 . H512 . C38 . 132.7 0.967 2.544 3.278(12) yes _iucr_refine_instruction_details_constraints ; # # Punched on 30/06/12 at 14:59:51 # #LIST 12 BLOCK SCALE X'S, U'S EQUIV PART(1001,OCC) PART(1002,OCC) WEIGHT -1 PART(1002,OCC) RIDE C ( 2,X'S) H ( 21,X'S) H ( 22,X'S) RIDE C ( 3,X'S) H ( 31,X'S) H ( 32,X'S) RIDE C ( 4,X'S) H ( 42,X'S) H ( 41,X'S) RIDE C ( 5,X'S) H ( 51,X'S) H ( 52,X'S) RIDE C ( 6,X'S) H ( 62,X'S) H ( 61,X'S) RIDE C ( 7,X'S) H ( 71,X'S) H ( 72,X'S) RIDE C ( 8,X'S) H ( 81,X'S) H ( 82,X'S) RIDE C ( 9,X'S) H ( 91,X'S) H ( 92,X'S) RIDE C ( 32,X'S) H ( 321,X'S) H ( 322,X'S) H ( 323,X'S) RIDE C ( 33,X'S) H ( 331,X'S) H ( 332,X'S) H ( 333,X'S) RIDE C ( 35,X'S) H ( 352,X'S) H ( 351,X'S) H ( 353,X'S) RIDE C ( 36,X'S) H ( 362,X'S) H ( 361,X'S) H ( 363,X'S) RIDE C ( 37,X'S) H ( 371,X'S) H ( 373,X'S) H ( 372,X'S) RIDE C ( 38,X'S) H ( 381,X'S) H ( 383,X'S) H ( 382,X'S) RIDE C ( 42,X'S) H ( 421,X'S) H ( 422,X'S) H ( 423,X'S) RIDE C ( 43,X'S) H ( 431,X'S) H ( 432,X'S) H ( 433,X'S) RIDE C ( 45,X'S) H ( 451,X'S) H ( 452,X'S) H ( 453,X'S) RIDE C ( 46,X'S) H ( 462,X'S) H ( 461,X'S) H ( 463,X'S) RIDE C ( 47,X'S) H ( 472,X'S) H ( 471,X'S) H ( 473,X'S) RIDE C ( 48,X'S) H ( 481,X'S) H ( 483,X'S) H ( 482,X'S) RIDE C ( 51,X'S) H ( 511,X'S) H ( 512,X'S) RIDE C ( 52,X'S) H ( 521,X'S) H ( 522,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 30/06/12 at 14:59:51 # #LIST 16 SAME O(1) C(2) C(3) C(4) C(5) AND CONT O(1) C(5) C(4) C(3) C(2) AND CONT O(1) C(6) C(7) C(8) C(9) AND CONT O(1) C(9) C(8) C(7) C(6) DELU 0.01 O(1) C(2) C(3) C(4) C(5) AND CONT O(1) C(5) C(4) C(3) C(2) AND CONT O(1) C(6) C(7) C(8) C(9) AND CONT O(1) C(9) C(8) C(7) C(6) SIMU 0.01 O(1) C(2) C(3) C(4) C(5) AND CONT O(1) C(5) C(4) C(3) C(2) AND CONT O(1) C(6) C(7) C(8) C(9) AND CONT O(1) C(9) C(8) C(7) C(6) END ; _chemical_name_common .