# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 182/1404 data_global #=========================================================================== # 1. SUBMISSION DETAILS _publ_contact_autor ; Prof. Fausto Calderazzo Dipartimento di Chimica e Chimica Industriale Universita' di Pisa Via del Risorgimento 35 I-56126 Pisa Italy ; _publ_contact_author_phone '+39 50 918218' _publ_contact_author_fax '+39 50 20237' _publ_contact_author_email facal@dcci.unipi.it _publ_requested_journal ' J. Chem. Soc., Chem. Comm.' _publ_requested_coeditor_name ? _publ_contact_letter ; ; #=========================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Isotypical N,N-dialkylcarbamato lanthanide complexes covering a range of 11 atomic numbers: direct experimental assessment of the lanthanide contraction in trivalent molecular compounds ; loop_ _publ_author_names _publ_author_address ' Abram, Ulrich' ; Forschungszentrum Rossendorf, Institute of Radiochemistry c/o Dresden University of Technology Institute of Analytical Chemistry 01062 Dresden Germany ; ' Belli Del'Amico, Daniela' ; Dipartimento di Chimica e Chimica Industriale Universita' di Pisa Via del Risorgimento 35 I-56126 Pisa Italy ; ' Calderazzo, Fausto' ; Dipartimento di Chimica e Chimica Industriale Universita' di Pisa Via del Risorgimento 35 I-56126 Pisa Italy ; ' Della Porta, Cinzia' ; Dipartimento di Chimica e Chimica Industriale Universita' di Pisa Via del Risorgimento 35 I-56126 Pisa Italy ; ' Englert, Ulli' ; Institut fYr Anorganische Chemie der RWTH Professor-Pirlet-Strasse 1 D-52074 Aachen Germany ; ' Marchetti, Fabio' ; Dipartimento di Ingegneria Chimica, dei Materiali, delle Materie Prime e Metallurgia Universita' "La Sapienza" di Roma via del Castro Laurenziano, 7 I-00195 Roma Italy; ; ' Merigo, Alessandra' ; Dipartimento di Chimica e Chimica Industriale Universita' di Pisa Via del Risorgimento 35 I-56126 Pisa Italy ; #=========================================================================== data_DB4271093 # 5. CRYSTAL DATA _chemical_compound_source 'see paper' _exptl_crystal_description ? _exptl_crystal_colour 'light blue' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _chemical_name_common ; Dodecakis(N,N-diisopropylcarbamato)tetraneodimium(iii) ; _chemical_formula_sum 'C100 H194 N12 Nd4 O24' _chemical_formula_weight 2525.69 _symmetry_cell_setting monoclinic _symmetry_space_group_name_h-m 'C2/c' 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 28.97(1) _cell_length_b 20.064(8) _cell_length_c 23.549(9) _cell_angle_alpha 90.00 _cell_angle_beta 107.44(4) _cell_angle_gamma 90.00 _cell_volume 1306(1) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 9 _cell_measurement_theta_max 13 _cell_formula_units_z 4.00 _exptl_crystal_density_diffrn 1.28 _exptl_crystal_density_meas none _diffrn_radiation_type Mo-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 1.630 _cell_measurement_temperature 253 _exptl_crystal_F_000 5240 # 6. DATA COLLECTION _diffrn_ambient_temperature 253 _diffrn_measurement_device Enraf_Nonius_CAD4 _diffrn_measurement_method \w _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.863 _exptl_absorpt_correction_T_max 1.000 _diffrn_reflns_number 7909 _reflns_number_total 7430 _reflns_number_observed 3686 _reflns_observed_criterion >2sigma(I) _diffrn_reflns_av_R_equivalents 0.107 _diffrn_reflns_theta_min 3.1 _diffrn_reflns_theta_max 23.0 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_max 24 _diffrn_standards_number 3 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0.00 _computing_data_collection CAD4_(Enraf-Nonius,_1977) _computing_cell_refinement CAD4_(Enraf-Nonius,_1977) _computing_data_reduction PROCESS_MolEN_(Fair,_1990) _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' # 7. REFINEMENT DATA loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Nd' 'Nd' -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 12 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0951P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7418 _refine_ls_number_parameters 611 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1879 _refine_ls_R_factor_obs 0.0668 _refine_ls_wR_factor_all 0.1792 _refine_ls_wR_factor_obs 0.1563 _refine_ls_goodness_of_fit_all 0.896 _refine_ls_goodness_of_fit_obs 1.200 _refine_ls_restrained_S_all 0.942 _refine_ls_restrained_S_obs 1.219 _refine_ls_shift/esd_max -1.517 _refine_ls_shift/esd_mean 0.009 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Nd1 Nd 0.07377(2) 0.69001(4) 0.20765(2) 0.0412(2) Uani 1 d . . Nd2 Nd 0.07575(2) 0.80550(4) 0.34597(2) 0.0419(2) Uani 1 d . . O11 O 0.0636(2) 0.6892(4) 0.3076(3) 0.042(2) Uani 1 d . . O12 O -0.0003(2) 0.6328(4) 0.3156(3) 0.046(2) Uani 1 d . . O21 O 0.1198(3) 0.8679(5) 0.4310(4) 0.073(3) Uani 1 d . . O22 O 0.1018(4) 0.9191(4) 0.3467(5) 0.086(3) Uani 1 d . . O31 O 0.1532(3) 0.7202(4) 0.2621(4) 0.057(3) Uani 1 d . . O32 O 0.1539(3) 0.7743(4) 0.3450(4) 0.061(3) Uani 1 d . . O41 O -0.0406(3) 0.7588(4) 0.0866(4) 0.066(3) Uani 1 d . . O42 O 0.0379(3) 0.7391(4) 0.1155(4) 0.071(3) Uani 1 d . . O51 O 0.1134(3) 0.6230(5) 0.1500(4) 0.082(3) Uani 1 d . . O52 O 0.1031(3) 0.5785(4) 0.2307(4) 0.071(3) Uani 1 d . . O61 O 0.0633(2) 0.8066(4) 0.2374(3) 0.049(2) Uani 1 d . . O62 O -0.0019(3) 0.8624(4) 0.1827(3) 0.051(2) Uani 1 d . . N1 N 0.0746(3) 0.5953(5) 0.3649(4) 0.047(3) Uani 1 d . . N2 N 0.1378(4) 0.9795(7) 0.4298(7) 0.126(6) Uani 1 d . . N3 N 0.2242(3) 0.7436(6) 0.3313(5) 0.065(3) Uani 1 d . . N4 N -0.0026(4) 0.7471(7) 0.0180(4) 0.080(4) Uani 1 d . . N5 N 0.1412(4) 0.5165(7) 0.1779(6) 0.108(5) Uani 1 d . . N6 N 0.0729(3) 0.8995(4) 0.1883(4) 0.047(3) Uani 1 d . . C1 C 0.0447(4) 0.6392(6) 0.3288(4) 0.036(3) Uani 1 d . . C2 C 0.1202(5) 0.9218(8) 0.4025(7) 0.079(5) Uani 1 d . . C3 C 0.1755(4) 0.7451(6) 0.3116(6) 0.055(4) Uani 1 d . . C4 C -0.0019(5) 0.7468(7) 0.0738(6) 0.061(4) Uani 1 d . . C5 C 0.1182(5) 0.5774(8) 0.1872(7) 0.076(5) Uani 1 d . . C6 C 0.0428(4) 0.8550(6) 0.2019(5) 0.049(4) Uani 1 d . . C11 C 0.1260(4) 0.6034(6) 0.3808(5) 0.052(4) Uani 1 d . . H11 H 0.1328(4) 0.6366(6) 0.3539(5) 0.068 Uiso 1 calc R . C12 C 0.1460(5) 0.6293(8) 0.4430(6) 0.083(5) Uani 1 d . . H12A H 0.1441(28) 0.6780(8) 0.4427(7) 0.109 Uiso 1 calc R . H12B H 0.1798(10) 0.6154(36) 0.4593(15) 0.109 Uiso 1 calc R . H12C H 0.1271(20) 0.6112(34) 0.4678(11) 0.109 Uiso 1 calc R . C13 C 0.1525(5) 0.5383(8) 0.3740(8) 0.106(6) Uani 1 d . . H13A H 0.1402(27) 0.5223(29) 0.3328(13) 0.138 Uiso 1 calc R . H13B H 0.1469(31) 0.5043(18) 0.4010(34) 0.138 Uiso 1 calc R . H13C H 0.1873(7) 0.5470(14) 0.3836(45) 0.138 Uiso 1 calc R . C14 C 0.0525(4) 0.5395(6) 0.3881(5) 0.052(4) Uani 1 d . . H14 H 0.0797(4) 0.5140(6) 0.4137(5) 0.068 Uiso 1 calc R . C15 C 0.0249(7) 0.4903(8) 0.3389(8) 0.123(7) Uani 1 d . . H15A H 0.0175(39) 0.4495(25) 0.3573(8) 0.160 Uiso 1 calc R . H15B H 0.0450(18) 0.4794(46) 0.3133(33) 0.160 Uiso 1 calc R . H15C H -0.0053(21) 0.5110(24) 0.3149(34) 0.160 Uiso 1 calc R . C16 C 0.0224(5) 0.5608(7) 0.4280(6) 0.077(5) Uani 1 d . . H16A H 0.0229(25) 0.5254(18) 0.4569(24) 0.099 Uiso 1 calc R . H16B H -0.0110(8) 0.5690(40) 0.4037(7) 0.099 Uiso 1 calc R . H16C H 0.0360(18) 0.6017(24) 0.4493(28) 0.099 Uiso 1 calc R . C21 C 0.1268(9) 1.0454(9) 0.3859(12) 0.164(11) Uani 1 d . . H21 H 0.1056(9) 1.0326(9) 0.3466(12) 0.213 Uiso 1 calc R . C22 C 0.1770(9) 1.0545(13) 0.3830(12) 0.213(13) Uani 1 d . . H22A H 0.1767(13) 1.0852(82) 0.3505(61) 0.276 Uiso 1 calc R . H22B H 0.1900(29) 1.0113(20) 0.3758(94) 0.276 Uiso 1 calc R . H22C H 0.1973(20) 1.0729(100) 0.4208(36) 0.276 Uiso 1 calc R . C23 C 0.1021(9) 1.0907(13) 0.4126(13) 0.255(17) Uani 1 d . . H23A H 0.1146(65) 1.0868(90) 0.4560(13) 0.331 Uiso 1 calc R . H23B H 0.0674(15) 1.0805(81) 0.3995(90) 0.331 Uiso 1 calc R . H23C H 0.1072(76) 1.1363(16) 0.4007(91) 0.331 Uiso 1 calc R . C24 C 0.1623(8) 0.9873(13) 0.4847(12) 0.223(13) Uani 1 d . . H24 H 0.1690(8) 1.0352(13) 0.4890(12) 0.289 Uiso 1 calc R . C25 C 0.1349(10) 0.9724(15) 0.5278(10) 0.248(16) Uani 1 d . . H25A H 0.1017(29) 0.9891(111) 0.5120(52) 0.323 Uiso 1 calc R . H25B H 0.1508(53) 0.9941(105) 0.5659(36) 0.323 Uiso 1 calc R . H25C H 0.1342(77) 0.9241(18) 0.5337(85) 0.323 Uiso 1 calc R . C26 C 0.2112(8) 0.9547(11) 0.5050(12) 0.209(14) Uani 1 d . . H26A H 0.2311(26) 0.9709(76) 0.4808(59) 0.271 Uiso 1 calc R . H26B H 0.2074(10) 0.9063(13) 0.5006(85) 0.271 Uiso 1 calc R . H26C H 0.2269(31) 0.9657(82) 0.5469(27) 0.271 Uiso 1 calc R . C31 C 0.2513(5) 0.7115(9) 0.2976(8) 0.110(7) Uani 1 d . . H31 H 0.2836(5) 0.7189(9) 0.3255(8) 0.144 Uiso 1 calc R . C32 C 0.2574(9) 0.7484(12) 0.2501(9) 0.184(10) Uani 1 d . . H32A H 0.2590(65) 0.7181(14) 0.2181(33) 0.239 Uiso 1 calc R . H32B H 0.2875(32) 0.7740(68) 0.2635(21) 0.239 Uiso 1 calc R . H32C H 0.2301(32) 0.7790(64) 0.2353(51) 0.239 Uiso 1 calc R . C33 C 0.2523(9) 0.6388(10) 0.2985(11) 0.210(11) Uani 1 d . . H33A H 0.2824(35) 0.6232(10) 0.2920(96) 0.273 Uiso 1 calc R . H33B H 0.2246(43) 0.6216(10) 0.2668(62) 0.273 Uiso 1 calc R . H33C H 0.2506(80) 0.6229(10) 0.3371(36) 0.273 Uiso 1 calc R . C34 C 0.2516(6) 0.7723(9) 0.3912(8) 0.107(7) Uani 1 d . . H34 H 0.2230(6) 0.7796(9) 0.4044(8) 0.140 Uiso 1 calc R . C35 C 0.2725(12) 0.7317(13) 0.4334(9) 0.256(18) Uani 1 d . . H35A H 0.3003(56) 0.7109(97) 0.4247(57) 0.332 Uiso 1 calc R . H35B H 0.2495(28) 0.6971(76) 0.4365(76) 0.332 Uiso 1 calc R . H35C H 0.2837(86) 0.7561(26) 0.4711(21) 0.332 Uiso 1 calc R . C36 C 0.2598(8) 0.8442(10) 0.3812(9) 0.144(8) Uani 1 d . . H36A H 0.2656(49) 0.8686(15) 0.4188(15) 0.187 Uiso 1 calc R . H36B H 0.2312(20) 0.8625(19) 0.3517(45) 0.187 Uiso 1 calc R . H36C H 0.2880(30) 0.8488(11) 0.3667(58) 0.187 Uiso 1 calc R . C41 C -0.0483(7) 0.7646(6) -0.0400(8) 0.134(7) Uiso 1 d D . H41A H -0.0703(7) 0.7642(6) -0.0155(8) 0.175 Uiso 0.664(10) calc PR 1 H41B H -0.0627(7) 0.7949(6) -0.0174(8) 0.175 Uiso 0.336(10) calc PR 2 C42 C -0.0747(4) 0.7012(6) -0.0760(5) 0.011(3) Uiso 0.664(10) d PD 1 H42A H -0.0722(21) 0.6638(11) -0.0485(7) 0.014 Uiso 0.664(10) calc PR 1 H42B H -0.0593(16) 0.6892(20) -0.1063(20) 0.014 Uiso 0.664(10) calc PR 1 H42C H -0.1089(7) 0.7117(12) -0.0952(24) 0.014 Uiso 0.664(10) calc PR 1 C43 C -0.0506(8) 0.8395(9) -0.0436(10) 0.093(8) Uiso 0.664(10) d PD 1 H43A H -0.0553(52) 0.8575(10) -0.0071(28) 0.121 Uiso 0.664(10) calc PR 1 H43B H -0.0777(32) 0.8530(9) -0.0779(38) 0.121 Uiso 0.664(10) calc PR 1 H43C H -0.0203(21) 0.8568(10) -0.0483(64) 0.121 Uiso 0.664(10) calc PR 1 C44 C 0.0429(7) 0.7321(6) -0.0014(8) 0.137(8) Uiso 1 d D . H44A H 0.0650(7) 0.7290(6) 0.0392(8) 0.179 Uiso 0.699(12) calc PR 3 H44B H 0.0589(7) 0.7049(6) 0.0335(8) 0.179 Uiso 0.301(12) calc PR 4 C45 C 0.0704(3) 0.8014(5) -0.0203(4) 0.000(2) Uiso 0.699(12) d PD 3 H45A H 0.1014(10) 0.7885(7) -0.0257(24) 0.000 Uiso 0.699(12) calc PR 3 H45B H 0.0760(18) 0.8346(12) 0.0116(12) 0.000 Uiso 0.699(12) calc PR 3 H45C H 0.0495(9) 0.8204(17) -0.0574(14) 0.000 Uiso 0.699(12) calc PR 3 C46 C 0.0429(9) 0.6528(10) -0.0146(11) 0.119(10) Uiso 0.699(12) d PD 3 H46A H 0.0740(24) 0.6400(18) -0.0198(74) 0.154 Uiso 0.699(12) calc PR 3 H46B H 0.0168(39) 0.6424(16) -0.0510(41) 0.154 Uiso 0.699(12) calc PR 3 H46C H 0.0379(60) 0.6281(10) 0.0189(34) 0.154 Uiso 0.699(12) calc PR 3 C42A C -0.0710(7) 0.8075(11) -0.1038(7) 0.000(5) Uiso 0.336(10) d PD 2 H42D H -0.1042(16) 0.8215(50) -0.1074(26) 0.000 Uiso 0.336(10) calc PR 2 H42E H -0.0711(39) 0.7790(22) -0.1377(8) 0.000 Uiso 0.336(10) calc PR 2 H42F H -0.0510(25) 0.8469(33) -0.1035(23) 0.000 Uiso 0.336(10) calc PR 2 C43A C -0.0860(7) 0.7106(11) -0.0428(11) 0.014(7) Uiso 0.336(10) d PD 2 H43D H -0.0805(31) 0.6909(47) -0.0033(17) 0.016 Uiso 0.336(10) calc PR 2 H43E H -0.0833(33) 0.6759(35) -0.0710(47) 0.016 Uiso 0.336(10) calc PR 2 H43F H -0.1184(8) 0.7303(17) -0.0561(58) 0.016 Uiso 0.336(10) calc PR 2 C45A C 0.0690(10) 0.6943(18) -0.0463(12) 0.048(10) Uiso 0.301(12) d PD 4 H45D H 0.0767(71) 0.6481(37) -0.0331(57) 0.058 Uiso 0.301(12) calc PR 4 H45E H 0.0989(41) 0.7178(66) -0.0453(74) 0.058 Uiso 0.301(12) calc PR 4 H45F H 0.0469(32) 0.6945(95) -0.0870(21) 0.058 Uiso 0.301(12) calc PR 4 C46A C 0.0829(7) 0.7863(11) 0.0116(12) 0.007(7) Uiso 0.301(12) d PD 4 H46D H 0.0765(29) 0.8171(43) -0.0221(30) 0.009 Uiso 0.301(12) calc PR 4 H46E H 0.1145(10) 0.7650(12) 0.0176(63) 0.009 Uiso 0.301(12) calc PR 4 H46F H 0.0830(35) 0.8109(48) 0.0476(38) 0.009 Uiso 0.301(12) calc PR 4 C51 C 0.1447(8) 0.4580(9) 0.2147(11) 0.147(9) Uani 1 d . . H51 H 0.1280(8) 0.4688(9) 0.2440(11) 0.191 Uiso 1 calc R . C52 C 0.1982(8) 0.4487(10) 0.2495(9) 0.185(11) Uani 1 d . . H52A H 0.2013(10) 0.4130(60) 0.2790(54) 0.240 Uiso 1 calc R . H52B H 0.2110(19) 0.4903(28) 0.2700(65) 0.240 Uiso 1 calc R . H52C H 0.2164(14) 0.4367(88) 0.2220(14) 0.240 Uiso 1 calc R . C53 C 0.1220(8) 0.3957(9) 0.1842(12) 0.199(14) Uani 1 d . . H53A H 0.0969(49) 0.4072(10) 0.1472(44) 0.258 Uiso 1 calc R . H53B H 0.1074(60) 0.3709(48) 0.2104(35) 0.258 Uiso 1 calc R . H53C H 0.1467(15) 0.3681(45) 0.1750(78) 0.258 Uiso 1 calc R . C54 C 0.1594(7) 0.5107(13) 0.1288(8) 0.161(10) Uani 1 d . . H54 H 0.1734(7) 0.4660(13) 0.1311(8) 0.209 Uiso 1 calc R . C55 C 0.1983(8) 0.5576(13) 0.1293(10) 0.200(12) Uani 1 d . . H55A H 0.1859(19) 0.6033(14) 0.1269(88) 0.260 Uiso 1 calc R . H55B H 0.2101(49) 0.5488(65) 0.0952(49) 0.260 Uiso 1 calc R . H55C H 0.2249(30) 0.5521(67) 0.1663(40) 0.260 Uiso 1 calc R . C56 C 0.1239(8) 0.5164(12) 0.0685(9) 0.219(12) Uani 1 d . . H56A H 0.0996(46) 0.4812(69) 0.0630(38) 0.285 Uiso 1 calc R . H56B H 0.1408(14) 0.5118(113) 0.0383(9) 0.285 Uiso 1 calc R . H56C H 0.1081(60) 0.5600(44) 0.0643(37) 0.285 Uiso 1 calc R . C61 C 0.0522(5) 0.9591(7) 0.1494(6) 0.069(4) Uani 1 d . . H61 H 0.0791(5) 0.9843(7) 0.1429(6) 0.090 Uiso 1 calc R . C62 C 0.0189(6) 0.9361(7) 0.0881(7) 0.094(6) Uani 1 d . . H62A H 0.0287(22) 0.8915(21) 0.0792(20) 0.122 Uiso 1 calc R . H62B H 0.0216(27) 0.9674(27) 0.0573(9) 0.122 Uiso 1 calc R . H62C H -0.0147(7) 0.9347(46) 0.0890(15) 0.122 Uiso 1 calc R . C63 C 0.0258(6) 1.0039(8) 0.1798(7) 0.096(6) Uani 1 d . . H63A H -0.0012(21) 0.9795(16) 0.1871(39) 0.124 Uiso 1 calc R . H63B H 0.0133(30) 1.0426(25) 0.1545(20) 0.124 Uiso 1 calc R . H63C H 0.0480(10) 1.0189(39) 0.2178(21) 0.124 Uiso 1 calc R . C64 C 0.1253(4) 0.8895(8) 0.2096(6) 0.071(5) Uani 1 d . . H64 H 0.1320(4) 0.8540(8) 0.2396(6) 0.092 Uiso 1 calc R . C65 C 0.1524(6) 0.9519(10) 0.2387(7) 0.125(8) Uani 1 d . . H65A H 0.1521(38) 0.9850(25) 0.2080(9) 0.163 Uiso 1 calc R . H65B H 0.1859(13) 0.9402(15) 0.2603(45) 0.163 Uiso 1 calc R . H65C H 0.1366(26) 0.9705(35) 0.2666(41) 0.163 Uiso 1 calc R . C66 C 0.1426(5) 0.8670(9) 0.1596(7) 0.099(6) Uani 1 d . . H66A H 0.1694(25) 0.8355(39) 0.1744(10) 0.128 Uiso 1 calc R . H66B H 0.1538(34) 0.9055(11) 0.1417(29) 0.128 Uiso 1 calc R . H66C H 0.1161(11) 0.8450(45) 0.1295(22) 0.128 Uiso 1 calc R . C70 C 0.4262(5) 0.6940(8) 0.2781(6) 0.075(4) Uiso 1 d . . C71 C 0.4232(3) 0.8079(6) 0.1590(4) 0.038(3) Uiso 1 d . . C72 C 0.5000 0.7110(49) 0.2500 0.222(41) Uiso 0.50 d SP . C73 C 0.4356(18) 0.7429(25) 0.2376(21) 0.348(25) Uiso 1 d . . C74 C 0.5000 0.7868(121) 0.2500 0.569(168) Uiso 0.50 d SP . C75 C 0.4753(27) 0.7513(41) 0.2468(34) 0.226(35) Uiso 0.50 d P . C80 C 0.2901(20) 1.1434(28) 0.5388(23) 0.389(27) Uiso 1 d . . C81 C 0.2605(16) 0.7708(21) 0.0341(16) 0.279(19) Uiso 1 d . . C82 C 0.3054(38) 0.7841(51) 0.0361(43) 0.688(74) Uiso 1 d . . C83 C 0.2373(22) 0.8226(30) 0.0586(25) 0.416(32) Uiso 1 d . . 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 Nd1 0.0433(3) 0.0432(4) 0.0386(3) -0.0031(4) 0.0144(3) 0.0038(4) Nd2 0.0463(4) 0.0408(4) 0.0376(3) -0.0056(4) 0.0111(3) -0.0030(4) O11 0.061(4) 0.032(4) 0.029(4) -0.004(4) 0.007(3) -0.013(4) O12 0.042(4) 0.052(5) 0.041(4) 0.001(4) 0.008(4) 0.004(4) O21 0.085(6) 0.070(7) 0.046(5) -0.012(5) -0.007(5) 0.000(6) O22 0.109(7) 0.028(5) 0.115(8) -0.012(6) 0.028(6) -0.016(5) O31 0.036(4) 0.069(6) 0.058(5) -0.010(4) 0.001(4) -0.009(4) O32 0.055(5) 0.067(6) 0.061(5) -0.002(5) 0.016(4) 0.010(5) O41 0.087(6) 0.054(6) 0.070(5) 0.002(5) 0.044(5) -0.006(5) O42 0.079(6) 0.072(6) 0.049(5) 0.025(5) 0.001(5) -0.011(5) O51 0.085(6) 0.122(9) 0.050(5) -0.011(5) 0.039(5) 0.028(6) O52 0.069(6) 0.060(6) 0.082(6) 0.011(5) 0.019(5) 0.015(5) O61 0.050(4) 0.057(5) 0.041(4) -0.006(5) 0.016(3) -0.013(5) O62 0.038(4) 0.064(6) 0.049(5) 0.010(4) 0.008(4) -0.010(4) N1 0.037(5) 0.064(7) 0.033(5) 0.007(5) 0.002(4) -0.005(5) N2 0.059(8) 0.114(11) 0.199(14) -0.108(11) 0.032(9) -0.014(8) N3 0.030(5) 0.085(8) 0.078(7) -0.008(7) 0.010(5) -0.001(6) N4 0.082(7) 0.141(12) 0.027(5) 0.013(6) 0.031(5) 0.011(8) N5 0.069(8) 0.122(11) 0.126(11) -0.068(9) 0.017(8) 0.037(8) N6 0.061(6) 0.029(6) 0.052(6) 0.025(5) 0.019(5) 0.017(5) C1 0.030(6) 0.048(8) 0.025(6) -0.009(6) 0.004(5) 0.000(6) C2 0.058(9) 0.069(11) 0.099(12) -0.050(10) 0.006(9) 0.004(9) C3 0.046(7) 0.047(8) 0.069(8) 0.014(7) 0.014(7) 0.005(7) C4 0.064(8) 0.053(9) 0.078(9) 0.010(7) 0.042(7) 0.013(7) C5 0.064(9) 0.078(11) 0.080(11) -0.027(10) 0.012(8) 0.003(9) C6 0.068(8) 0.042(8) 0.039(6) 0.022(6) 0.021(6) -0.014(7) C11 0.047(7) 0.041(8) 0.059(8) 0.015(7) 0.003(6) 0.001(6) C12 0.084(10) 0.092(12) 0.070(10) -0.003(9) 0.018(8) -0.003(9) C13 0.060(10) 0.120(14) 0.127(15) 0.000(12) 0.012(10) 0.040(10) C14 0.043(7) 0.039(8) 0.072(8) 0.009(7) 0.015(6) 0.003(6) C15 0.160(17) 0.073(12) 0.122(15) -0.001(11) 0.019(13) -0.054(12) C16 0.077(9) 0.094(11) 0.055(8) 0.033(8) 0.016(7) -0.011(9) C21 0.165(21) 0.056(12) 0.215(25) -0.035(14) -0.029(19) -0.031(13) C22 0.214(28) 0.198(28) 0.229(28) -0.086(22) 0.071(24) -0.049(23) C23 0.186(24) 0.196(25) 0.334(41) -0.082(27) 0.006(25) 0.118(21) C24 0.104(17) 0.257(24) 0.282(26) -0.229(21) 0.021(17) -0.048(17) C25 0.256(32) 0.361(41) 0.107(18) -0.042(23) 0.023(20) -0.164(29) C26 0.150(21) 0.141(21) 0.254(31) 0.033(20) -0.061(21) -0.061(17) C31 0.042(7) 0.177(19) 0.124(12) 0.047(13) 0.043(8) 0.009(10) C32 0.304(23) 0.176(23) 0.129(14) -0.008(15) 0.152(15) 0.024(20) C33 0.351(27) 0.122(17) 0.209(22) 0.017(17) 0.161(20) 0.126(20) C34 0.055(9) 0.114(14) 0.118(14) -0.025(12) -0.029(10) 0.007(10) C35 0.461(49) 0.181(25) 0.052(12) -0.014(15) -0.033(21) -0.088(29) C36 0.189(20) 0.129(17) 0.122(16) -0.010(14) 0.060(14) -0.059(16) C51 0.175(20) 0.074(13) 0.192(22) 0.010(14) 0.054(17) 0.059(14) C52 0.222(21) 0.162(19) 0.153(20) -0.007(15) 0.030(18) 0.145(17) C53 0.147(20) 0.066(14) 0.335(36) -0.059(18) -0.002(21) -0.019(14) C54 0.126(15) 0.270(27) 0.072(11) -0.062(15) 0.010(12) 0.087(17) C55 0.178(18) 0.267(33) 0.202(21) -0.048(21) 0.128(17) 0.053(21) C56 0.253(23) 0.277(26) 0.121(17) -0.040(18) 0.046(17) 0.186(21) C61 0.058(8) 0.061(10) 0.091(10) 0.010(8) 0.027(8) -0.002(8) C62 0.111(12) 0.071(11) 0.089(11) 0.042(9) 0.014(10) 0.002(10) C63 0.088(11) 0.068(11) 0.123(14) 0.014(10) 0.020(10) 0.006(9) C64 0.043(8) 0.095(11) 0.062(9) 0.027(8) -0.003(7) -0.020(8) C65 0.087(12) 0.176(19) 0.098(13) 0.040(13) 0.005(10) -0.049(13) C66 0.081(10) 0.130(15) 0.098(11) 0.018(11) 0.046(9) 0.021(11) _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 Nd1 O42 2.325(8) . ? Nd1 O12 2.334(7) 2 ? Nd1 O31 2.353(7) . ? Nd1 O52 2.397(9) . ? Nd1 O51 2.430(9) . ? Nd1 O11 2.458(7) . ? Nd1 O61 2.486(8) . ? Nd1 C5 2.71(2) . ? Nd1 Nd2 3.9837(14) . ? Nd2 O41 2.324(8) 2 ? Nd2 O62 2.340(7) 2 ? Nd2 O32 2.355(8) . ? Nd2 O21 2.383(8) . ? Nd2 O22 2.400(9) . ? Nd2 O61 2.473(7) . ? Nd2 O11 2.490(7) . ? Nd2 C2 2.802(15) . ? O11 C1 1.311(13) . ? O12 C1 1.254(11) . ? O12 Nd1 2.334(7) 2 ? O21 C2 1.28(2) . ? O22 C2 1.26(2) . ? O31 C3 1.255(14) . ? O32 C3 1.284(15) . ? O41 C4 1.270(14) . ? O41 Nd2 2.324(8) 2 ? O42 C4 1.279(14) . ? O51 C5 1.25(2) . ? O52 C5 1.23(2) . ? O61 C6 1.303(13) . ? O62 C6 1.246(13) . ? O62 Nd2 2.340(7) 2 ? N1 C1 1.344(13) . ? N1 C11 1.429(14) . ? N1 C14 1.474(15) . ? N2 C24 1.28(3) . ? N2 C2 1.35(2) . ? N2 C21 1.65(3) . ? N3 C3 1.347(14) . ? N3 C31 1.43(2) . ? N3 C34 1.51(2) . ? N4 C4 1.310(15) . ? N4 C44 1.55(2) . ? N4 C41 1.63(2) . ? N5 C54 1.41(2) . ? N5 C5 1.44(2) . ? N5 C51 1.44(2) . ? N6 C6 1.353(14) . ? N6 C64 1.463(15) . ? N6 C61 1.52(2) . ? C11 C12 1.50(2) . ? C11 C13 1.55(2) . ? C14 C16 1.52(2) . ? C14 C15 1.55(2) . ? C21 C23 1.41(3) . ? C21 C22 1.49(3) . ? C24 C25 1.49(3) . ? C24 C26 1.50(3) . ? C31 C32 1.40(2) . ? C31 C33 1.46(2) . ? C34 C35 1.29(3) . ? C34 C36 1.49(2) . ? C41 C43 1.51(2) . ? C41 C43A 1.53(2) . ? C41 C42 1.59(2) . ? C41 C42A 1.69(2) . ? C44 C46A 1.55(2) . ? C44 C46 1.62(2) . ? C44 C45A 1.66(2) . ? C44 C45 1.72(2) . ? C51 C53 1.49(3) . ? C51 C52 1.53(3) . ? C54 C55 1.47(3) . ? C54 C56 1.49(2) . ? C61 C63 1.49(2) . ? C61 C62 1.55(2) . ? C64 C66 1.48(2) . ? C64 C65 1.53(2) . ? C70 C73 1.45(5) . ? C72 C75 1.07(10) . ? C72 C75 1.07(10) 2_655 ? C72 C74 1.52(25) . ? C72 C73 1.91(6) 2_655 ? C72 C73 1.91(6) . ? C73 C75 1.12(8) . ? C73 C74 2.00(11) . ? C74 C75 1.00(19) 2_655 ? C74 C75 1.00(19) . ? C74 C73 2.00(11) 2_655 ? C75 C75 1.39(15) 2_655 ? C80 C82 1.53(11) 6_576 ? C80 C83 1.86(7) 6_576 ? C80 C81 1.91(7) 6_576 ? C81 C82 1.31(11) . ? C81 C83 1.45(7) . ? C81 C81 1.75(7) 7_565 ? C81 C80 1.91(7) 6_575 ? C82 C80 1.53(11) 6_575 ? C83 C80 1.86(7) 6_575 ? 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 O42 Nd1 O12 82.4(3) . 2 ? O42 Nd1 O31 119.4(3) . . ? O12 Nd1 O31 158.2(3) 2 . ? O42 Nd1 O52 129.5(3) . . ? O12 Nd1 O52 80.2(3) 2 . ? O31 Nd1 O52 84.0(3) . . ? O42 Nd1 O51 82.3(3) . . ? O12 Nd1 O51 98.4(3) 2 . ? O31 Nd1 O51 84.2(3) . . ? O52 Nd1 O51 54.2(3) . . ? O42 Nd1 O11 138.4(3) . . ? O12 Nd1 O11 81.9(2) 2 . ? O31 Nd1 O11 81.9(3) . . ? O52 Nd1 O11 85.0(3) . . ? O51 Nd1 O11 138.0(3) . . ? O42 Nd1 O61 78.8(3) . . ? O12 Nd1 O61 110.5(2) 2 . ? O31 Nd1 O61 77.6(3) . . ? O52 Nd1 O61 151.5(3) . . ? O51 Nd1 O61 142.8(3) . . ? O11 Nd1 O61 71.2(2) . . ? O42 Nd1 C5 106.9(4) . . ? O12 Nd1 C5 89.8(4) 2 . ? O31 Nd1 C5 82.7(4) . . ? O52 Nd1 C5 26.9(4) . . ? O51 Nd1 C5 27.3(4) . . ? O11 Nd1 C5 111.3(4) . . ? O61 Nd1 C5 159.6(3) . . ? O42 Nd1 Nd2 114.2(2) . . ? O12 Nd1 Nd2 105.5(2) 2 . ? O31 Nd1 Nd2 68.4(2) . . ? O52 Nd1 Nd2 116.1(2) . . ? O51 Nd1 Nd2 152.3(2) . . ? O11 Nd1 Nd2 36.6(2) . . ? O61 Nd1 Nd2 36.4(2) . . ? C5 Nd1 Nd2 137.5(3) . . ? O41 Nd2 O62 81.0(3) 2 2 ? O41 Nd2 O32 121.2(3) 2 . ? O62 Nd2 O32 157.8(3) 2 . ? O41 Nd2 O21 82.6(3) 2 . ? O62 Nd2 O21 101.5(3) 2 . ? O32 Nd2 O21 82.7(3) . . ? O41 Nd2 O22 125.4(3) 2 . ? O62 Nd2 O22 78.2(3) 2 . ? O32 Nd2 O22 87.3(3) . . ? O21 Nd2 O22 53.6(3) . . ? O41 Nd2 O61 138.8(3) 2 . ? O62 Nd2 O61 82.0(3) 2 . ? O32 Nd2 O61 80.5(3) . . ? O21 Nd2 O61 137.7(3) . . ? O22 Nd2 O61 87.0(3) . . ? O41 Nd2 O11 80.0(3) 2 . ? O62 Nd2 O11 109.6(2) 2 . ? O32 Nd2 O11 77.2(3) . . ? O21 Nd2 O11 141.2(3) . . ? O22 Nd2 O11 154.6(3) . . ? O61 Nd2 O11 70.8(2) . . ? O41 Nd2 C2 104.1(4) 2 . ? O62 Nd2 C2 88.9(3) 2 . ? O32 Nd2 C2 85.4(4) . . ? O21 Nd2 C2 27.0(4) . . ? O22 Nd2 C2 26.7(4) . . ? O61 Nd2 C2 112.8(4) . . ? O11 Nd2 C2 161.5(3) . . ? O41 Nd2 Nd1 115.0(2) 2 . ? O62 Nd2 Nd1 105.1(2) 2 . ? O32 Nd2 Nd1 67.4(2) . . ? O21 Nd2 Nd1 150.0(2) . . ? O22 Nd2 Nd1 119.1(3) . . ? O61 Nd2 Nd1 36.7(2) . . ? O11 Nd2 Nd1 36.1(2) . . ? C2 Nd2 Nd1 139.9(4) . . ? C1 O11 Nd1 123.6(6) . . ? C1 O11 Nd2 127.5(6) . . ? Nd1 O11 Nd2 107.3(3) . . ? C1 O12 Nd1 144.6(7) . 2 ? C2 O21 Nd2 95.1(8) . . ? C2 O22 Nd2 94.7(9) . . ? C3 O31 Nd1 139.1(8) . . ? C3 O32 Nd2 140.7(7) . . ? C4 O41 Nd2 146.9(8) . 2 ? C4 O42 Nd1 144.6(9) . . ? C5 O51 Nd1 89.1(9) . . ? C5 O52 Nd1 91.1(9) . . ? C6 O61 Nd2 124.5(7) . . ? C6 O61 Nd1 126.3(7) . . ? Nd2 O61 Nd1 106.9(3) . . ? C6 O62 Nd2 143.8(8) . 2 ? C1 N1 C11 121.0(10) . . ? C1 N1 C14 117.5(9) . . ? C11 N1 C14 121.5(9) . . ? C24 N2 C2 126.9(20) . . ? C24 N2 C21 118.6(17) . . ? C2 N2 C21 114.5(15) . . ? C3 N3 C31 120.8(12) . . ? C3 N3 C34 121.2(12) . . ? C31 N3 C34 117.9(11) . . ? C4 N4 C44 122.5(11) . . ? C4 N4 C41 127.3(12) . . ? C44 N4 C41 110.2(11) . . ? C54 N5 C5 119.9(17) . . ? C54 N5 C51 116.6(16) . . ? C5 N5 C51 123.4(16) . . ? C6 N6 C64 120.3(10) . . ? C6 N6 C61 119.8(10) . . ? C64 N6 C61 119.9(10) . . ? O12 C1 O11 120.4(10) . . ? O12 C1 N1 121.1(10) . . ? O11 C1 N1 118.5(9) . . ? O22 C2 O21 116.4(13) . . ? O22 C2 N2 121.0(16) . . ? O21 C2 N2 122.6(15) . . ? O22 C2 Nd2 58.6(7) . . ? O21 C2 Nd2 57.9(7) . . ? N2 C2 Nd2 175.1(10) . . ? O31 C3 O32 122.7(11) . . ? O31 C3 N3 120.4(12) . . ? O32 C3 N3 116.8(12) . . ? O41 C4 O42 119.9(12) . . ? O41 C4 N4 119.2(12) . . ? O42 C4 N4 120.7(12) . . ? O52 C5 O51 125.5(14) . . ? O52 C5 N5 116.0(15) . . ? O51 C5 N5 118.4(15) . . ? O52 C5 Nd1 62.0(8) . . ? O51 C5 Nd1 63.6(8) . . ? N5 C5 Nd1 178.0(13) . . ? O62 C6 O61 123.2(10) . . ? O62 C6 N6 120.6(10) . . ? O61 C6 N6 116.2(10) . . ? N1 C11 C12 111.3(11) . . ? N1 C11 C13 112.8(10) . . ? C12 C11 C13 109.6(11) . . ? N1 C14 C16 114.1(10) . . ? N1 C14 C15 113.1(11) . . ? C16 C14 C15 112.2(12) . . ? C23 C21 C22 124.9(20) . . ? C23 C21 N2 105.5(22) . . ? C22 C21 N2 96.8(17) . . ? N2 C24 C25 114.5(20) . . ? N2 C24 C26 116.8(21) . . ? C25 C24 C26 109.8(26) . . ? C32 C31 N3 115.4(17) . . ? C32 C31 C33 122.3(19) . . ? N3 C31 C33 117.1(15) . . ? C35 C34 C36 132.3(18) . . ? C35 C34 N3 118.2(17) . . ? C36 C34 N3 106.7(15) . . ? C43 C41 C42 139.6(15) . . ? C43 C41 N4 105.9(13) . . ? C43A C41 N4 106.0(13) . . ? C42 C41 N4 114.5(10) . . ? C43A C41 C42A 103.9(15) . . ? N4 C41 C42A 149.2(14) . . ? N4 C44 C46A 117.3(14) . . ? N4 C44 C46 107.1(14) . . ? N4 C44 C45A 150.3(16) . . ? C46A C44 C45A 89.5(18) . . ? N4 C44 C45 114.8(10) . . ? C46 C44 C45 135.7(16) . . ? N5 C51 C53 116.8(20) . . ? N5 C51 C52 107.4(18) . . ? C53 C51 C52 112.6(16) . . ? N5 C54 C55 114.5(18) . . ? N5 C54 C56 117.2(17) . . ? C55 C54 C56 105.5(21) . . ? C63 C61 N6 110.7(12) . . ? C63 C61 C62 111.2(12) . . ? N6 C61 C62 110.5(11) . . ? N6 C64 C66 109.3(11) . . ? N6 C64 C65 112.5(13) . . ? C66 C64 C65 110.9(13) . . ? C75 C72 C75 81.4(100) . 2_655 ? C75 C72 C74 40.7(59) . . ? C75 C72 C74 40.7(59) 2_655 . ? C75 C72 C73 111.1(82) . 2_655 ? C75 C72 C73 29.8(47) 2_655 2_655 ? C74 C72 C73 70.4(32) . 2_655 ? C75 C72 C73 29.8(48) . . ? C75 C72 C73 111.1(82) 2_655 . ? C74 C72 C73 70.4(32) . . ? C73 C72 C73 140.9(65) 2_655 . ? C75 C73 C70 111.1(62) . . ? C75 C73 C72 28.3(54) . . ? C70 C73 C72 92.3(33) . . ? C75 C73 C74 17.5(85) . . ? C70 C73 C74 123.5(48) . . ? C72 C73 C74 45.6(67) . . ? C75 C74 C75 88.7(100) 2_655 . ? C75 C74 C72 44.3(100) 2_655 . ? C75 C74 C72 44.3(100) . . ? C75 C74 C73 19.7(66) 2_655 2_655 ? C75 C74 C73 108.2(100) . 2_655 ? C72 C74 C73 63.9(64) . 2_655 ? C75 C74 C73 108.2(100) 2_655 . ? C75 C74 C73 19.7(66) . . ? C72 C74 C73 63.9(64) . . ? C73 C74 C73 127.9(100) 2_655 . ? C74 C75 C72 94.9(100) . . ? C74 C75 C73 142.8(100) . . ? C72 C75 C73 121.9(94) . . ? C74 C75 C75 45.7(100) . 2_655 ? C72 C75 C75 49.3(59) . 2_655 ? C73 C75 C75 170.2(74) . 2_655 ? C82 C80 C83 86.1(53) 6_576 6_576 ? C82 C80 C81 43.1(45) 6_576 6_576 ? C83 C80 C81 45.2(24) 6_576 6_576 ? C82 C81 C83 114.5(61) . . ? C82 C81 C81 101.4(60) . 7_565 ? C83 C81 C81 129.2(50) . 7_565 ? C82 C81 C80 52.7(49) . 6_575 ? C83 C81 C80 65.5(33) . 6_575 ? C81 C81 C80 120.6(40) 7_565 6_575 ? C81 C82 C80 84.2(65) . 6_575 ? C81 C83 C80 69.4(36) . 6_575 ? _refine_diff_density_max 1.732 _refine_diff_density_min -0.708 _refine_diff_density_rms 0.130 #==END data_squeeze _audit_creation_method SHELXL _chemical_name_systematic ; Dodecakis(N,N-diisopropylcarbamato)tetragadolinium(iii) ; _chemical_name_common ? _chemical_formula_moiety 'Gd4 (O2 C N i-Pr2)12 ' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C84 H168 Gd4 N12 O24' _chemical_formula_weight 1179.65 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Gd' 'Gd' -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c 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 29.041(8) _cell_length_b 19.676(2) _cell_length_c 23.170(8) _cell_angle_alpha 90.00 _cell_angle_beta 107.52(1) _cell_angle_gamma 90.00 _cell_volume 12624 _cell_formula_units_Z 4 _cell_measurement_temperature 203 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.77 _cell_measurement_theta_max 13.64 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.241 _exptl_crystal_density_method ? _exptl_crystal_F_000 4816 _exptl_absorpt_coefficient_mu 2.132 _exptl_absorpt_correction_type difabs _exptl_absorpt_correction_T_min 0.511 _exptl_absorpt_correction_T_max 1.00 _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.70930 _diffrn_radiation_type 'Mo K\a ' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device cad4 _diffrn_measurement_method omega-scan _diffrn_standards_number 3 _diffrn_standards_interval_count 300 _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% 16.6 _diffrn_reflns_number 11961 _diffrn_reflns_av_R_equivalents 0.0257 _diffrn_reflns_av_sigmaI/netI 0.0633 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 30.98 _reflns_number_total 11367 _reflns_number_observed 6713 _reflns_observed_criterion >2sigma(I) _computing_data_collection cad4 _computing_cell_refinement cad4 _computing_data_reduction cad4,sdp _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics SCHAKAL,ZORTEP _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0663P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11367 _refine_ls_number_parameters 559 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1033 _refine_ls_R_factor_obs 0.0489 _refine_ls_wR_factor_all 0.1332 _refine_ls_wR_factor_obs 0.1209 _refine_ls_goodness_of_fit_all 1.056 _refine_ls_goodness_of_fit_obs 1.267 _refine_ls_restrained_S_all 1.056 _refine_ls_restrained_S_obs 1.267 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Gd1 Gd 0.070747(9) 0.19615(2) 0.206016(12) 0.0370(2) Uani 1 d . . Gd2 Gd 0.076185(10) 0.31128(2) 0.343920(12) 0.0362(2) Uani 1 d . . O11 O 0.00061(13) 0.1378(3) 0.1843(2) 0.0404(15) Uani 1 d . . O12 O 0.06334(13) 0.1954(2) 0.3065(2) 0.0329(14) Uani 1 d . . N11 N 0.0740(2) 0.0978(3) 0.3617(2) 0.039(2) Uani 1 d . . C11 C 0.0445(2) 0.1448(4) 0.3272(2) 0.037(2) Uani 1 d . . C12 C 0.0534(2) 0.0394(4) 0.3881(3) 0.050(2) Uani 1 d . . H12 H 0.0812(2) 0.0138(4) 0.4132(3) 0.060 Uiso 1 calc R . C13 C 0.1273(2) 0.1039(4) 0.3792(3) 0.048(2) Uani 1 d . . H13 H 0.1346(2) 0.1371(4) 0.3516(3) 0.057 Uiso 1 calc R . C14 C 0.0255(3) -0.0097(5) 0.3386(4) 0.083(3) Uani 1 d . . H14A H 0.0452(3) -0.0221(5) 0.3136(4) 0.124 Uiso 1 calc R . H14B H -0.0035(3) 0.0119(5) 0.3142(4) 0.124 Uiso 1 calc R . H14C H 0.0172(3) -0.0498(5) 0.3569(4) 0.124 Uiso 1 calc R . C15 C 0.1481(2) 0.1315(5) 0.4420(3) 0.078(3) Uani 1 d . . H15A H 0.1319(2) 0.1731(5) 0.4459(3) 0.116 Uiso 1 calc R . H15B H 0.1819(2) 0.1401(5) 0.4497(3) 0.116 Uiso 1 calc R . H15C H 0.1436(2) 0.0990(5) 0.4708(3) 0.116 Uiso 1 calc R . C16 C 0.1516(3) 0.0390(5) 0.3714(4) 0.080(3) Uani 1 d . . H16A H 0.1376(3) 0.0224(5) 0.3309(4) 0.120 Uiso 1 calc R . H16B H 0.1472(3) 0.0058(5) 0.3996(4) 0.120 Uiso 1 calc R . H16C H 0.1854(3) 0.0470(5) 0.3786(4) 0.120 Uiso 1 calc R . C17 C 0.0253(3) 0.0619(5) 0.4300(3) 0.066(3) Uani 1 d . . H17A H 0.0447(3) 0.0925(5) 0.4598(3) 0.099 Uiso 1 calc R . H17B H 0.0171(3) 0.0229(5) 0.4498(3) 0.099 Uiso 1 calc R . H17C H -0.0037(3) 0.0846(5) 0.4070(3) 0.099 Uiso 1 calc R . O21 O 0.06109(14) 0.3095(2) 0.2360(2) 0.0321(13) Uani 1 d . . O22 O 0.00389(13) 0.3675(2) 0.3188(2) 0.0385(14) Uani 1 d . . N21 N 0.0692(2) 0.4053(4) 0.1841(2) 0.046(2) Uani 1 d . . C21 C 0.0419(2) 0.3601(4) 0.2008(3) 0.037(2) Uani 1 d . . C22 C 0.1222(2) 0.3947(5) 0.2012(3) 0.064(3) Uani 1 d . . H22 H 0.1304(2) 0.3602(5) 0.2332(3) 0.077 Uiso 1 calc R . C23 C 0.0489(3) 0.4627(5) 0.1459(4) 0.060(3) Uani 1 d . . H23 H 0.0764(3) 0.4873(5) 0.1396(4) 0.072 Uiso 1 calc R . C24 C 0.1506(3) 0.4597(6) 0.2278(4) 0.090(4) Uani 1 d . . H24A H 0.1402(3) 0.4758(6) 0.2610(4) 0.136 Uiso 1 calc R . H24B H 0.1447(3) 0.4941(6) 0.1971(4) 0.136 Uiso 1 calc R . H24C H 0.1845(3) 0.4496(6) 0.2419(4) 0.136 Uiso 1 calc R . C25 C 0.1368(3) 0.3664(5) 0.1485(4) 0.090(3) Uani 1 d . . H25A H 0.1183(3) 0.3262(5) 0.1335(4) 0.134 Uiso 1 calc R . H25B H 0.1705(3) 0.3553(5) 0.1617(4) 0.134 Uiso 1 calc R . H25C H 0.1307(3) 0.3998(5) 0.1169(4) 0.134 Uiso 1 calc R . C26 C 0.0162(3) 0.4429(5) 0.0822(3) 0.082(3) Uani 1 d . . H26A H 0.0329(3) 0.4112(5) 0.0642(3) 0.123 Uiso 1 calc R . H26B H 0.0082(3) 0.4828(5) 0.0574(3) 0.123 Uiso 1 calc R . H26C H -0.0129(3) 0.4223(5) 0.0855(3) 0.123 Uiso 1 calc R . C27 C 0.0236(3) 0.5120(5) 0.1751(4) 0.084(3) Uani 1 d . . H27A H 0.0445(3) 0.5238(5) 0.2146(4) 0.125 Uiso 1 calc R . H27B H -0.0054(3) 0.4917(5) 0.1789(4) 0.125 Uiso 1 calc R . H27C H 0.0156(3) 0.5523(5) 0.1507(4) 0.125 Uiso 1 calc R . O31 O 0.0474(2) 0.2645(3) 0.4174(2) 0.0514(15) Uani 1 d . . O32 O 0.0321(2) 0.2450(3) 0.1154(2) 0.053(2) Uani 1 d . . N31 N 0.0070(2) 0.2463(4) 0.4850(2) 0.061(2) Uani 1 d . . C31 C 0.0068(2) 0.2520(4) 0.4265(3) 0.048(2) Uani 1 d . . C32 C -0.0378(3) 0.2202(6) 0.4971(4) 0.092(4) Uani 1 d . . H32 H -0.0586(3) 0.2049(6) 0.4577(4) 0.110 Uiso 1 calc R . C33 C 0.0489(3) 0.2690(7) 0.5370(3) 0.089(4) Uani 1 d . . H33 H 0.0362(3) 0.2630(7) 0.5713(3) 0.107 Uiso 1 calc R . C34 C -0.0305(4) 0.1592(6) 0.5365(5) 0.114(4) Uani 1 d . . H34A H -0.0134(4) 0.1251(6) 0.5214(5) 0.171 Uiso 1 calc R . H34B H -0.0613(4) 0.1415(6) 0.5365(5) 0.171 Uiso 1 calc R . H34C H -0.0121(4) 0.1713(6) 0.5770(5) 0.171 Uiso 1 calc R . C35 C -0.0655(4) 0.2814(6) 0.5149(5) 0.118(4) Uani 1 d . . H35A H -0.0681(4) 0.3178(6) 0.4864(5) 0.176 Uiso 1 calc R . H35B H -0.0481(4) 0.2970(6) 0.5547(5) 0.176 Uiso 1 calc R . H35C H -0.0972(4) 0.2670(6) 0.5143(5) 0.176 Uiso 1 calc R . C36 C 0.0898(3) 0.2183(6) 0.5515(4) 0.102(4) Uani 1 d . . H36A H 0.0769(3) 0.1731(6) 0.5473(4) 0.153 Uiso 1 calc R . H36B H 0.1100(3) 0.2252(6) 0.5922(4) 0.153 Uiso 1 calc R . H36C H 0.1085(3) 0.2245(6) 0.5240(4) 0.153 Uiso 1 calc R . C37 C 0.0597(4) 0.3412(6) 0.5402(5) 0.114(5) Uani 1 d . . H37A H 0.0301(4) 0.3665(6) 0.5297(5) 0.171 Uiso 1 calc R . H37B H 0.0773(4) 0.3520(6) 0.5123(5) 0.171 Uiso 1 calc R . H37C H 0.0788(4) 0.3527(6) 0.5805(5) 0.171 Uiso 1 calc R . O41 O 0.15174(13) 0.2795(3) 0.3420(2) 0.0477(14) Uani 1 d . . O42 O 0.14914(14) 0.2247(3) 0.2573(2) 0.0487(14) Uani 1 d . . N41 N 0.2212(2) 0.2455(3) 0.3261(3) 0.060(2) Uani 1 d . . C41 C 0.1715(2) 0.2497(4) 0.3079(3) 0.047(2) Uani 1 d . . C42 C 0.2461(3) 0.2102(7) 0.2866(5) 0.090(4) Uani 1 d . . H42 H 0.2785(3) 0.2218(7) 0.3129(5) 0.108 Uiso 1 calc R . C43 C 0.2494(2) 0.2780(6) 0.3870(6) 0.102(4) Uani 1 d . . H43 H 0.2206(2) 0.2879(6) 0.3993(6) 0.122 Uiso 1 calc R . C44 C 0.2508(5) 0.2510(7) 0.2374(5) 0.140(5) Uani 1 d . . H44A H 0.2435(5) 0.2975(7) 0.2437(5) 0.209 Uiso 1 calc R . H44B H 0.2288(5) 0.2349(7) 0.2001(5) 0.209 Uiso 1 calc R . H44C H 0.2833(5) 0.2480(7) 0.2354(5) 0.209 Uiso 1 calc R . C45 C 0.2530(7) 0.1405(8) 0.2972(7) 0.198(9) Uani 1 d . . H45A H 0.2470(7) 0.1290(8) 0.3345(7) 0.297 Uiso 1 calc R . H45B H 0.2857(7) 0.1288(8) 0.2997(7) 0.297 Uiso 1 calc R . H45C H 0.2312(7) 0.1158(8) 0.2645(7) 0.297 Uiso 1 calc R . C46 C 0.2694(6) 0.2312(9) 0.4349(5) 0.197(8) Uani 1 d . . H46A H 0.2537(6) 0.1880(9) 0.4251(5) 0.295 Uiso 1 calc R . H46B H 0.2648(6) 0.2481(9) 0.4716(5) 0.295 Uiso 1 calc R . H46C H 0.3033(6) 0.2260(9) 0.4404(5) 0.295 Uiso 1 calc R . C47 C 0.2612(6) 0.3499(8) 0.3805(6) 0.180(8) Uani 1 d . . H47A H 0.2410(6) 0.3670(8) 0.3425(6) 0.270 Uiso 1 calc R . H47B H 0.2945(6) 0.3536(8) 0.3818(6) 0.270 Uiso 1 calc R . H47C H 0.2558(6) 0.3759(8) 0.4129(6) 0.270 Uiso 1 calc R . O51 O 0.1001(2) 0.4254(3) 0.3362(2) 0.054(2) Uani 1 d . . O52 O 0.1204(2) 0.3781(4) 0.4269(2) 0.066(2) Uani 1 d . . N51 N 0.1395(2) 0.4903(6) 0.4177(3) 0.069(3) Uani 1 d . . C51 C 0.1203(3) 0.4285(7) 0.3934(4) 0.060(3) Uani 1 d . . C52 C 0.1355(4) 0.5496(7) 0.3805(6) 0.088(4) Uani 1 d . . H52 H 0.1152(4) 0.5365(7) 0.3400(6) 0.106 Uiso 1 calc R . C53 C 0.1658(4) 0.4921(7) 0.4841(5) 0.112(4) Uani 1 d . . H53 H 0.1772(4) 0.5391(7) 0.4920(5) 0.135 Uiso 1 calc R . C54 C 0.2122(4) 0.4492(6) 0.4972(5) 0.145(6) Uani 1 d . . H54A H 0.2294(4) 0.4613(6) 0.4693(5) 0.217 Uiso 1 calc R . H54B H 0.2038(4) 0.4019(6) 0.4927(5) 0.217 Uiso 1 calc R . H54C H 0.2322(4) 0.4577(6) 0.5378(5) 0.217 Uiso 1 calc R . C55 C 0.1327(6) 0.4818(8) 0.5227(5) 0.185(8) Uani 1 d . . H55A H 0.1055(6) 0.5119(8) 0.5092(5) 0.277 Uiso 1 calc R . H55B H 0.1499(6) 0.4914(8) 0.5642(5) 0.277 Uiso 1 calc R . H55C H 0.1216(6) 0.4356(8) 0.5191(5) 0.277 Uiso 1 calc R . C56 C 0.1091(4) 0.6069(6) 0.4008(6) 0.139(5) Uani 1 d . . H56A H 0.0788(4) 0.5905(6) 0.4038(6) 0.208 Uiso 1 calc R . H56B H 0.1035(4) 0.6431(6) 0.3718(6) 0.208 Uiso 1 calc R . H56C H 0.1284(4) 0.6233(6) 0.4395(6) 0.208 Uiso 1 calc R . C57 C 0.1842(3) 0.5687(6) 0.3738(5) 0.123(5) Uani 1 d . . H57A H 0.1984(3) 0.5297(6) 0.3611(5) 0.185 Uiso 1 calc R . H57B H 0.2050(3) 0.5845(6) 0.4120(5) 0.185 Uiso 1 calc R . H57C H 0.1800(3) 0.6041(6) 0.3442(5) 0.185 Uiso 1 calc R . O61 O 0.1058(2) 0.1327(4) 0.1458(2) 0.067(2) Uani 1 d . . O62 O 0.1009(2) 0.0840(3) 0.2290(2) 0.061(2) Uani 1 d . . N61 N 0.1386(3) 0.0262(6) 0.1696(4) 0.103(4) Uani 1 d . . C61 C 0.1141(3) 0.0809(6) 0.1821(4) 0.070(3) Uani 1 d . . C62 C 0.1559(4) 0.0224(10) 0.1181(5) 0.182(10) Uani 1 d . . H62 H 0.1732(4) -0.0210(10) 0.1220(5) 0.218 Uiso 1 calc R . C63 C 0.1474(4) -0.0306(8) 0.2108(6) 0.124(5) Uani 1 d . . H63 H 0.1313(4) -0.0220(8) 0.2416(6) 0.148 Uiso 1 calc R . C64 C 0.1270(5) -0.0928(7) 0.1776(9) 0.213(10) Uani 1 d . . H64A H 0.0931(5) -0.0865(7) 0.1581(9) 0.320 Uiso 1 calc R . H64B H 0.1316(5) -0.1302(7) 0.2054(9) 0.320 Uiso 1 calc R . H64C H 0.1429(5) -0.1024(7) 0.1477(9) 0.320 Uiso 1 calc R . C65 C 0.1139(5) 0.0170(8) 0.0587(5) 0.199(9) Uani 1 d . . H65A H 0.0924(5) -0.0187(8) 0.0622(5) 0.298 Uiso 1 calc R . H65B H 0.1266(5) 0.0071(8) 0.0258(5) 0.298 Uiso 1 calc R . H65C H 0.0967(5) 0.0593(8) 0.0511(5) 0.298 Uiso 1 calc R . C66 C 0.1926(5) 0.0755(10) 0.1202(6) 0.208(10) Uani 1 d . . H66A H 0.2168(5) 0.0743(10) 0.1589(6) 0.311 Uiso 1 calc R . H66B H 0.1773(5) 0.1193(10) 0.1142(6) 0.311 Uiso 1 calc R . H66C H 0.2073(5) 0.0672(10) 0.0889(6) 0.311 Uiso 1 calc R . C67 C 0.2011(4) -0.0400(7) 0.2422(5) 0.150(6) Uani 1 d . . H67A H 0.2140(4) 0.0008(7) 0.2638(5) 0.225 Uiso 1 calc R . H67B H 0.2173(4) -0.0493(7) 0.2125(5) 0.225 Uiso 1 calc R . H67C H 0.2058(4) -0.0773(7) 0.2700(5) 0.225 Uiso 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 0.03530(14) 0.0374(5) 0.0394(2) -0.0058(2) 0.01288(11) -0.0002(2) Gd2 0.03919(15) 0.0317(5) 0.03567(15) -0.0030(2) 0.00838(11) -0.0013(2) O11 0.039(2) 0.034(5) 0.048(2) -0.011(2) 0.012(2) 0.001(2) O12 0.038(2) 0.023(5) 0.039(2) 0.004(2) 0.013(2) -0.006(2) N11 0.041(3) 0.022(6) 0.052(3) 0.010(3) 0.010(2) 0.005(3) C11 0.039(3) 0.035(8) 0.033(3) -0.006(3) 0.005(2) 0.001(4) C12 0.056(4) 0.025(8) 0.064(4) 0.008(4) 0.013(3) 0.000(4) C13 0.036(3) 0.043(8) 0.062(4) 0.009(4) 0.012(3) -0.001(4) C14 0.106(7) 0.044(10) 0.088(6) 0.003(6) 0.014(5) -0.014(6) C15 0.045(4) 0.104(10) 0.072(5) 0.003(5) 0.000(3) -0.008(5) C16 0.072(5) 0.057(10) 0.106(7) 0.009(6) 0.018(5) 0.038(5) C17 0.065(4) 0.071(9) 0.063(4) 0.022(5) 0.021(3) 0.004(5) O21 0.048(2) 0.012(5) 0.035(2) 0.006(2) 0.011(2) -0.000(2) O22 0.041(2) 0.029(5) 0.044(2) -0.004(2) 0.010(2) -0.001(2) N21 0.042(3) 0.032(6) 0.061(3) 0.015(3) 0.009(2) -0.007(3) C21 0.048(3) 0.019(7) 0.040(3) -0.005(4) 0.011(3) -0.003(4) C22 0.049(4) 0.070(9) 0.074(5) 0.020(5) 0.021(3) -0.007(4) C23 0.057(4) 0.044(9) 0.081(5) 0.019(5) 0.024(4) 0.000(4) C24 0.061(5) 0.113(12) 0.092(6) 0.008(6) 0.015(4) -0.032(6) C25 0.086(6) 0.093(11) 0.102(7) 0.032(6) 0.047(5) 0.006(6) C26 0.075(5) 0.100(10) 0.066(5) 0.031(5) 0.016(4) -0.020(6) C27 0.092(6) 0.042(10) 0.102(7) 0.010(6) 0.009(5) -0.017(6) O31 0.060(3) 0.047(5) 0.050(3) 0.004(3) 0.022(2) 0.009(3) O32 0.060(3) 0.053(5) 0.042(2) -0.003(2) 0.010(2) -0.006(3) N31 0.066(3) 0.084(7) 0.036(3) 0.003(3) 0.020(2) -0.001(4) C31 0.061(4) 0.038(9) 0.045(3) -0.003(4) 0.017(3) 0.012(4) C32 0.072(5) 0.157(12) 0.057(4) 0.023(6) 0.036(4) 0.020(6) C33 0.088(6) 0.141(14) 0.033(4) -0.005(5) 0.011(3) 0.022(7) C34 0.140(9) 0.115(13) 0.102(8) 0.016(8) 0.058(7) -0.009(8) C35 0.102(7) 0.149(13) 0.131(9) 0.022(8) 0.079(7) 0.027(8) C36 0.087(6) 0.124(11) 0.075(6) 0.014(6) -0.007(5) 0.019(7) C37 0.145(10) 0.063(14) 0.106(8) -0.007(7) -0.007(7) -0.041(9) O41 0.035(2) 0.049(5) 0.056(3) -0.008(3) 0.010(2) -0.010(2) O42 0.039(2) 0.050(5) 0.055(3) -0.012(3) 0.011(2) -0.005(2) N41 0.035(3) 0.057(7) 0.086(4) -0.010(4) 0.014(3) -0.008(3) C41 0.035(3) 0.035(8) 0.072(5) 0.007(4) 0.019(3) -0.001(3) C42 0.039(4) 0.104(13) 0.135(9) -0.005(8) 0.037(4) 0.014(5) C43 0.028(3) 0.066(12) 0.177(11) -0.039(8) -0.022(5) 0.000(4) C44 0.216(14) 0.120(15) 0.095(8) -0.015(8) 0.066(9) -0.001(10) C45 0.353(26) 0.086(17) 0.208(16) -0.019(13) 0.165(17) 0.067(16) C46 0.279(19) 0.198(19) 0.080(8) 0.018(10) 0.005(10) -0.126(17) C47 0.294(20) 0.147(18) 0.133(11) -0.077(11) 0.116(12) -0.154(16) O51 0.065(3) 0.028(5) 0.060(3) -0.002(3) 0.008(2) -0.011(3) O52 0.082(4) 0.058(7) 0.050(3) -0.017(3) 0.006(2) -0.016(3) N51 0.070(4) 0.036(10) 0.090(6) -0.022(5) 0.009(4) -0.006(5) C51 0.055(4) 0.040(12) 0.088(7) -0.021(7) 0.024(4) -0.006(5) C52 0.088(7) 0.024(13) 0.140(10) -0.019(8) 0.018(6) -0.009(6) C53 0.111(8) 0.073(12) 0.132(9) -0.061(8) 0.005(7) -0.022(8) C54 0.114(9) 0.107(14) 0.156(11) -0.024(9) -0.045(8) 0.006(8) C55 0.239(17) 0.223(19) 0.129(10) -0.113(11) 0.111(11) -0.114(14) C56 0.121(9) 0.046(13) 0.240(16) -0.037(10) 0.043(10) 0.002(8) C57 0.091(7) 0.118(13) 0.154(10) -0.003(9) 0.028(7) -0.049(7) O61 0.049(3) 0.090(7) 0.060(3) -0.025(3) 0.015(2) 0.012(3) O62 0.067(3) 0.037(5) 0.078(3) -0.011(3) 0.019(3) 0.013(3) N61 0.065(4) 0.127(13) 0.095(6) -0.059(6) -0.009(4) 0.044(6) C61 0.047(4) 0.075(12) 0.076(6) -0.030(6) -0.002(4) 0.009(5) C62 0.110(9) 0.326(27) 0.078(7) -0.097(11) -0.018(7) 0.114(12) C63 0.110(9) 0.058(15) 0.163(12) -0.041(10) -0.018(8) 0.054(8) C64 0.188(15) 0.031(16) 0.334(23) -0.069(15) -0.053(15) 0.029(10) C65 0.163(11) 0.296(21) 0.092(8) -0.106(10) -0.030(7) 0.125(12) C66 0.115(10) 0.404(30) 0.121(10) -0.050(14) 0.061(9) 0.056(15) C67 0.122(9) 0.155(15) 0.137(10) -0.048(9) -0.017(7) 0.076(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O11 2.259(4) . ? Gd1 O32 2.274(4) . ? Gd1 O42 2.298(4) . ? Gd1 O61 2.324(5) . ? Gd1 O62 2.375(6) . ? Gd1 O21 2.379(5) . ? Gd1 O12 2.401(4) . ? Gd1 C61 2.729(11) . ? Gd1 Gd2 3.8809(10) . ? Gd2 O22 2.288(4) . ? Gd2 O41 2.294(4) . ? Gd2 O31 2.304(5) . ? Gd2 O52 2.364(5) . ? Gd2 O51 2.373(5) . ? Gd2 O21 2.404(4) . ? Gd2 O12 2.427(5) . ? Gd2 C51 2.719(12) . ? O11 C11 1.263(6) 2 ? O12 C11 1.297(8) . ? N11 C11 1.347(8) . ? N11 C13 1.483(7) . ? N11 C12 1.507(9) . ? C11 O11 1.263(6) 2 ? C12 C17 1.510(10) . ? C12 C14 1.533(10) . ? C13 C16 1.496(10) . ? C13 C15 1.501(9) . ? O21 C21 1.301(8) . ? O22 C21 1.277(7) 2 ? N21 C21 1.324(8) . ? N21 C23 1.446(9) . ? N21 C22 1.486(8) . ? C21 O22 1.277(7) 2 ? C22 C25 1.512(11) . ? C22 C24 1.546(12) . ? C23 C27 1.498(11) . ? C23 C26 1.544(10) . ? O31 C31 1.282(8) . ? O32 C31 1.256(7) 2 ? N31 C31 1.357(8) . ? N31 C33 1.498(10) . ? N31 C32 1.502(10) . ? C31 O32 1.256(7) 2 ? C32 C34 1.484(13) . ? C32 C35 1.571(13) . ? C33 C37 1.452(13) . ? C33 C36 1.508(12) . ? O41 C41 1.255(8) . ? O42 C41 1.256(8) . ? N41 C41 1.378(7) . ? N41 C42 1.498(11) . ? N41 C43 1.541(11) . ? C42 C45 1.397(15) . ? C42 C44 1.434(14) . ? C43 C46 1.43(2) . ? C43 C47 1.47(2) . ? O51 C51 1.280(10) . ? O52 C51 1.259(11) . ? N51 C51 1.384(11) . ? N51 C52 1.434(12) . ? N51 C53 1.498(12) . ? C52 C56 1.513(13) . ? C52 C57 1.515(13) . ? C53 C55 1.511(15) . ? C53 C54 1.539(14) . ? O61 C61 1.296(11) . ? O62 C61 1.256(10) . ? N61 C61 1.368(12) . ? N61 C62 1.432(15) . ? N61 C63 1.44(2) . ? C62 C66 1.48(2) . ? C62 C65 1.543(13) . ? C63 C64 1.472(15) . ? C63 C67 1.519(13) . ? 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 Gd1 O32 81.3(2) . . ? O11 Gd1 O42 157.8(2) . . ? O32 Gd1 O42 120.7(2) . . ? O11 Gd1 O61 97.0(2) . . ? O32 Gd1 O61 81.7(2) . . ? O42 Gd1 O61 84.1(2) . . ? O11 Gd1 O62 79.9(2) . . ? O32 Gd1 O62 130.2(2) . . ? O42 Gd1 O62 82.5(2) . . ? O61 Gd1 O62 55.7(2) . . ? O11 Gd1 O21 111.35(15) . . ? O32 Gd1 O21 78.8(2) . . ? O42 Gd1 O21 78.8(2) . . ? O61 Gd1 O21 142.3(2) . . ? O62 Gd1 O21 150.9(2) . . ? O11 Gd1 O12 82.80(14) . . ? O32 Gd1 O12 137.2(2) . . ? O42 Gd1 O12 82.18(14) . . ? O61 Gd1 O12 139.7(2) . . ? O62 Gd1 O12 85.0(2) . . ? O21 Gd1 O12 70.67(15) . . ? O11 Gd1 C61 88.4(2) . . ? O32 Gd1 C61 107.0(2) . . ? O42 Gd1 C61 82.1(2) . . ? O61 Gd1 C61 28.3(2) . . ? O62 Gd1 C61 27.4(2) . . ? O21 Gd1 C61 160.2(2) . . ? O12 Gd1 C61 111.9(3) . . ? O11 Gd1 Gd2 106.87(10) . . ? O32 Gd1 Gd2 113.58(13) . . ? O42 Gd1 Gd2 69.09(11) . . ? O61 Gd1 Gd2 153.09(12) . . ? O62 Gd1 Gd2 115.92(13) . . ? O21 Gd1 Gd2 35.99(9) . . ? O12 Gd1 Gd2 36.74(12) . . ? C61 Gd1 Gd2 138.1(2) . . ? O22 Gd2 O41 159.4(2) . . ? O22 Gd2 O31 82.6(2) . . ? O41 Gd2 O31 117.9(2) . . ? O22 Gd2 O52 99.8(2) . . ? O41 Gd2 O52 83.0(2) . . ? O31 Gd2 O52 81.4(2) . . ? O22 Gd2 O51 77.9(2) . . ? O41 Gd2 O51 87.3(2) . . ? O31 Gd2 O51 127.8(2) . . ? O52 Gd2 O51 55.6(2) . . ? O22 Gd2 O21 82.88(14) . . ? O41 Gd2 O21 81.50(14) . . ? O31 Gd2 O21 140.3(2) . . ? O52 Gd2 O21 137.5(2) . . ? O51 Gd2 O21 84.3(2) . . ? O22 Gd2 O12 109.44(14) . . ? O41 Gd2 O12 77.4(2) . . ? O31 Gd2 O12 80.7(2) . . ? O52 Gd2 O12 143.2(2) . . ? O51 Gd2 O12 151.44(15) . . ? O21 Gd2 O12 69.81(14) . . ? O22 Gd2 C51 88.7(2) . . ? O41 Gd2 C51 84.7(2) . . ? O31 Gd2 C51 104.9(2) . . ? O52 Gd2 C51 27.6(2) . . ? O51 Gd2 C51 28.1(2) . . ? O21 Gd2 C51 111.4(3) . . ? O12 Gd2 C51 161.7(2) . . ? O22 Gd2 Gd1 105.42(10) . . ? O41 Gd2 Gd1 68.12(11) . . ? O31 Gd2 Gd1 116.24(13) . . ? O52 Gd2 Gd1 150.65(14) . . ? O51 Gd2 Gd1 115.47(12) . . ? O21 Gd2 Gd1 35.55(11) . . ? O12 Gd2 Gd1 36.28(9) . . ? C51 Gd2 Gd1 137.7(2) . . ? C11 O11 Gd1 143.1(5) 2 . ? C11 O12 Gd1 122.3(4) . . ? C11 O12 Gd2 128.7(4) . . ? Gd1 O12 Gd2 107.0(2) . . ? C11 N11 C13 122.1(6) . . ? C11 N11 C12 120.3(5) . . ? C13 N11 C12 117.4(5) . . ? O11 C11 O12 122.1(6) 2 . ? O11 C11 N11 119.0(7) 2 . ? O12 C11 N11 118.9(5) . . ? N11 C12 C17 113.2(7) . . ? N11 C12 C14 111.3(6) . . ? C17 C12 C14 113.6(7) . . ? N11 C13 C16 112.9(7) . . ? N11 C13 C15 112.1(6) . . ? C16 C13 C15 111.1(6) . . ? C21 O21 Gd1 126.8(4) . . ? C21 O21 Gd2 123.5(4) . . ? Gd1 O21 Gd2 108.5(2) . . ? C21 O22 Gd2 144.3(5) 2 . ? C21 N21 C23 122.3(6) . . ? C21 N21 C22 119.5(6) . . ? C23 N21 C22 118.1(6) . . ? O22 C21 O21 121.0(6) 2 . ? O22 C21 N21 118.0(7) 2 . ? O21 C21 N21 121.0(6) . . ? N21 C22 C25 110.8(6) . . ? N21 C22 C24 112.1(7) . . ? C25 C22 C24 112.4(7) . . ? N21 C23 C27 113.2(7) . . ? N21 C23 C26 114.0(8) . . ? C27 C23 C26 110.6(7) . . ? C31 O31 Gd2 139.0(4) . . ? C31 O32 Gd1 147.1(5) 2 . ? C31 N31 C33 122.5(6) . . ? C31 N31 C32 118.1(6) . . ? C33 N31 C32 119.4(6) . . ? O32 C31 O31 123.4(6) 2 . ? O32 C31 N31 119.7(6) 2 . ? O31 C31 N31 116.8(6) . . ? C34 C32 N31 114.9(7) . . ? C34 C32 C35 116.7(7) . . ? N31 C32 C35 109.1(9) . . ? C37 C33 N31 116.2(8) . . ? C37 C33 C36 119.5(10) . . ? N31 C33 C36 112.1(9) . . ? C41 O41 Gd2 139.6(4) . . ? C41 O42 Gd1 137.1(4) . . ? C41 N41 C42 119.7(6) . . ? C41 N41 C43 118.3(6) . . ? C42 N41 C43 122.0(6) . . ? O41 C41 O42 124.3(6) . . ? O41 C41 N41 118.1(6) . . ? O42 C41 N41 117.5(7) . . ? C45 C42 C44 130.3(11) . . ? C45 C42 N41 114.7(10) . . ? C44 C42 N41 113.9(11) . . ? C46 C43 C47 130.3(10) . . ? C46 C43 N41 115.2(10) . . ? C47 C43 N41 112.4(10) . . ? C51 O51 Gd2 91.2(6) . . ? C51 O52 Gd2 92.1(6) . . ? C51 N51 C52 121.3(10) . . ? C51 N51 C53 117.2(10) . . ? C52 N51 C53 121.4(10) . . ? O52 C51 O51 121.1(10) . . ? O52 C51 N51 121.0(9) . . ? O51 C51 N51 117.8(10) . . ? O52 C51 Gd2 60.3(6) . . ? O51 C51 Gd2 60.8(5) . . ? N51 C51 Gd2 175.8(6) . . ? N51 C52 C56 112.1(12) . . ? N51 C52 C57 110.8(9) . . ? C56 C52 C57 114.9(11) . . ? N51 C53 C55 112.6(9) . . ? N51 C53 C54 109.7(9) . . ? C55 C53 C54 118.9(13) . . ? C61 O61 Gd1 93.5(5) . . ? C61 O62 Gd1 92.2(6) . . ? C61 N61 C62 123.6(12) . . ? C61 N61 C63 118.2(10) . . ? C62 N61 C63 118.2(11) . . ? O62 C61 O61 118.6(9) . . ? O62 C61 N61 122.2(11) . . ? O61 C61 N61 119.2(10) . . ? O62 C61 Gd1 60.4(5) . . ? O61 C61 Gd1 58.2(5) . . ? N61 C61 Gd1 175.7(8) . . ? N61 C62 C66 111.4(11) . . ? N61 C62 C65 111.4(11) . . ? C66 C62 C65 116.4(16) . . ? N61 C63 C64 109.6(13) . . ? N61 C63 C67 111.3(12) . . ? C64 C63 C67 110.1(11) . . ? _refine_diff_density_max 1.071 _refine_diff_density_min -1.074 _refine_diff_density_rms 0.097 #==END data_holcar _audit_creation_method SHELXL-97 _chemical_name_systematic ; Dodecakis(N,N-diisopropylcarbamato)tetraholmium(iii) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Ho4 (O2 C N i-Pr2)12' _chemical_formula_sum 'C98 H200 Ho4 N12 O24' _chemical_formula_weight 2590.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ho' 'Ho' -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'C2/c ' 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 29.130(2) _cell_length_b 19.844(2) _cell_length_c 23.1310(10) _cell_angle_alpha 90.00 _cell_angle_beta 107.240(10) _cell_angle_gamma 90.00 _cell_volume 12770.3(17) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 36 _cell_measurement_theta_min 9.697 _cell_measurement_theta_max 25.029 _exptl_crystal_description 'Prism' _exptl_crystal_colour 'Light yellow' _exptl_crystal_size_max 0.82 _exptl_crystal_size_mid 0.48 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.347 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5328 _exptl_absorpt_coefficient_mu 2.514 _exptl_absorpt_correction_type 'integration' _exptl_absorpt_correction_T_min 0.3425 _exptl_absorpt_correction_T_max 0.4623 _exptl_absorpt_process_details ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1.00 0.00 0.00 0.1750 -1.00 0.00 0.00 0.1750 1.00 1.00 1.00 0.4000 -1.00 -1.00 -1.00 0.4000 1.00 -1.00 -1.00 0.4150 -1.00 1.00 1.00 0.4150 1.00 1.00 -1.00 0.2300 -1.00 -1.00 1.00 0.2300 1.00 -1.00 1.00 0.2400 -1.00 1.00 -1.00 0.2400 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '2\q/\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10120 _diffrn_reflns_av_R_equivalents 0.0236 _diffrn_reflns_av_sigmaI/netI 0.0313 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 23.01 _reflns_number_total 8868 _reflns_number_gt 6711 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0439P)^2^+99.2485P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8868 _refine_ls_number_parameters 467 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0640 _refine_ls_R_factor_gt 0.0392 _refine_ls_wR_factor_ref 0.1102 _refine_ls_wR_factor_gt 0.0938 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.076 _refine_ls_shift/su_mean 0.002 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 Ho1 Ho 0.069263(11) 0.802596(18) 0.705264(15) 0.04636(11) Uani 1 1 d . . . Ho2 Ho 0.075547(11) 0.689928(17) 0.841681(15) 0.04627(11) Uani 1 1 d . . . O11 O 0.06269(16) 0.8034(2) 0.8047(2) 0.0459(11) Uani 1 1 d . . . O12 O -0.00051(16) 0.8594(3) 0.8156(2) 0.0540(13) Uani 1 1 d . . . C11 C 0.0447(2) 0.8531(4) 0.8274(3) 0.0442(16) Uani 1 1 d . . . N1 N 0.0737(2) 0.8995(3) 0.8616(3) 0.0564(16) Uani 1 1 d . . . C12 C 0.1264(3) 0.8915(5) 0.8783(4) 0.071(2) Uani 1 1 d . . . H12 H 0.1333 0.8573 0.8514 0.093 Uiso 1 1 calc R . . C13 C 0.0532(3) 0.9573(5) 0.8871(4) 0.074(3) Uani 1 1 d . . . H13 H 0.0807 0.9828 0.9123 0.096 Uiso 1 1 calc R . . C14 C 0.1463(4) 0.8662(6) 0.9424(5) 0.102(3) Uiso 1 1 d . . . H14A H 0.1536 0.8190 0.9418 0.133 Uiso 1 1 calc R . . H14B H 0.1229 0.8727 0.9636 0.133 Uiso 1 1 calc R . . H14C H 0.1750 0.8906 0.9625 0.133 Uiso 1 1 calc R . . C15 C 0.1508(4) 0.9561(6) 0.8690(5) 0.107(4) Uiso 1 1 d . . . H15A H 0.1650 0.9501 0.8368 0.139 Uiso 1 1 calc R . . H15B H 0.1754 0.9674 0.9056 0.139 Uiso 1 1 calc R . . H15C H 0.1276 0.9918 0.8587 0.139 Uiso 1 1 calc R . . C16 C 0.0245(4) 0.9349(5) 0.9289(5) 0.087(3) Uiso 1 1 d . . . H16A H 0.0156 0.8885 0.9213 0.114 Uiso 1 1 calc R . . H16B H -0.0040 0.9620 0.9216 0.114 Uiso 1 1 calc R . . H16C H 0.0437 0.9402 0.9703 0.114 Uiso 1 1 calc R . . C17 C 0.0260(4) 1.0049(6) 0.8375(5) 0.105(4) Uiso 1 1 d . . . H17A H 0.0169 0.9816 0.7994 0.137 Uiso 1 1 calc R . . H17B H 0.0461 1.0425 0.8353 0.137 Uiso 1 1 calc R . . H17C H -0.0024 1.0208 0.8463 0.137 Uiso 1 1 calc R . . O21 O 0.05987(16) 0.6904(2) 0.7352(2) 0.0479(11) Uani 1 1 d . . . O22 O -0.00500(18) 0.6349(3) 0.6812(2) 0.0564(13) Uani 1 1 d . . . C21 C 0.0400(3) 0.6404(4) 0.6998(3) 0.0516(18) Uani 1 1 d . . . N2 N 0.0678(2) 0.5954(3) 0.6836(3) 0.0666(19) Uani 1 1 d . . . C22 C 0.1204(3) 0.6045(5) 0.7005(5) 0.083(3) Uani 1 1 d . . . H22 H 0.1291 0.6384 0.7327 0.108 Uiso 1 1 calc R . . C23 C 0.0460(4) 0.5377(5) 0.6437(5) 0.082(3) Uani 1 1 d . . . H23 H 0.0729 0.5127 0.6366 0.107 Uiso 1 1 calc R . . C24 C 0.1469(4) 0.5412(6) 0.7248(6) 0.114(4) Uiso 1 1 d . . . H24A H 0.1540 0.5171 0.6925 0.149 Uiso 1 1 calc R . . H24B H 0.1275 0.5137 0.7423 0.149 Uiso 1 1 calc R . . H24C H 0.1764 0.5523 0.7551 0.149 Uiso 1 1 calc R . . C25 C 0.1348(4) 0.6319(6) 0.6473(6) 0.110(4) Uiso 1 1 d . . . H25A H 0.1294 0.5981 0.6163 0.143 Uiso 1 1 calc R . . H25B H 0.1682 0.6440 0.6603 0.143 Uiso 1 1 calc R . . H25C H 0.1158 0.6711 0.6315 0.143 Uiso 1 1 calc R . . C26 C 0.0220(4) 0.4899(6) 0.6764(5) 0.108(4) Uiso 1 1 d . . . H26A H 0.0052 0.4556 0.6490 0.140 Uiso 1 1 calc R . . H26B H -0.0005 0.5143 0.6916 0.140 Uiso 1 1 calc R . . H26C H 0.0459 0.4694 0.7096 0.140 Uiso 1 1 calc R . . C27 C 0.0145(4) 0.5592(6) 0.5821(5) 0.099(3) Uiso 1 1 d . . . H27A H 0.0258 0.5386 0.5513 0.129 Uiso 1 1 calc R . . H27B H 0.0157 0.6073 0.5786 0.129 Uiso 1 1 calc R . . H27C H -0.0180 0.5454 0.5771 0.129 Uiso 1 1 calc R . . O31 O 0.14630(18) 0.7747(3) 0.7546(3) 0.0631(14) Uani 1 1 d . . . O32 O 0.15026(18) 0.7204(3) 0.8398(3) 0.0616(14) Uani 1 1 d . . . C31 C 0.1692(3) 0.7481(4) 0.8042(4) 0.059(2) Uani 1 1 d . . . N3 N 0.2181(2) 0.7512(4) 0.8201(4) 0.076(2) Uani 1 1 d . . . C32 C 0.2427(4) 0.7879(7) 0.7813(6) 0.107(4) Uani 1 1 d . . . H32 H 0.2129 0.8050 0.7529 0.140 Uiso 1 1 calc R . . C33 C 0.2471(4) 0.7179(6) 0.8782(8) 0.133(6) Uani 1 1 d . . . H33 H 0.2777 0.7261 0.8697 0.173 Uiso 1 1 calc R . . C34 C 0.2549(7) 0.7464(10) 0.7385(9) 0.192(8) Uiso 1 1 d . . . H34A H 0.2356 0.7062 0.7321 0.249 Uiso 1 1 calc R . . H34B H 0.2883 0.7344 0.7533 0.249 Uiso 1 1 calc R . . H34C H 0.2490 0.7703 0.7009 0.249 Uiso 1 1 calc R . . C35 C 0.2604(7) 0.8515(10) 0.8030(9) 0.209(9) Uiso 1 1 d . . . H35A H 0.2406 0.8858 0.7785 0.272 Uiso 1 1 calc R . . H35B H 0.2928 0.8561 0.8011 0.272 Uiso 1 1 calc R . . H35C H 0.2602 0.8563 0.8442 0.272 Uiso 1 1 calc R . . C36 C 0.2500(6) 0.6454(9) 0.8704(8) 0.169(6) Uiso 1 1 d . . . H36A H 0.2226 0.6306 0.8383 0.220 Uiso 1 1 calc R . . H36B H 0.2503 0.6230 0.9073 0.220 Uiso 1 1 calc R . . H36C H 0.2789 0.6348 0.8604 0.220 Uiso 1 1 calc R . . C37 C 0.2594(8) 0.7576(11) 0.9288(9) 0.207(9) Uiso 1 1 d . . . H37A H 0.2441 0.7409 0.9574 0.270 Uiso 1 1 calc R . . H37B H 0.2492 0.8031 0.9179 0.270 Uiso 1 1 calc R . . H37C H 0.2937 0.7566 0.9467 0.270 Uiso 1 1 calc R . . O41 O 0.0318(2) 0.7545(3) 0.6162(2) 0.0665(15) Uani 1 1 d . . . O42 O -0.0472(2) 0.7367(3) 0.5865(2) 0.0617(14) Uani 1 1 d . . . C41 C -0.0078(3) 0.7473(4) 0.5749(4) 0.061(2) Uani 1 1 d . . . N4 N -0.0088(3) 0.7510(5) 0.5166(3) 0.084(2) Uani 1 1 d . . . C42 C 0.0344(5) 0.7747(8) 0.5010(6) 0.127(5) Uani 1 1 d . . . H42 H 0.0546 0.7898 0.5408 0.165 Uiso 1 1 calc R . . C43 C -0.0518(5) 0.7295(8) 0.4665(5) 0.125(5) Uani 1 1 d . . . H43 H -0.0381 0.7387 0.4334 0.163 Uiso 1 1 calc R . . C44 C 0.0634(6) 0.7195(8) 0.4894(8) 0.154(6) Uiso 1 1 d . . . H44A H 0.0626 0.7202 0.4476 0.200 Uiso 1 1 calc R . . H44B H 0.0508 0.6775 0.4984 0.200 Uiso 1 1 calc R . . H44C H 0.0960 0.7246 0.5145 0.200 Uiso 1 1 calc R . . C45 C 0.0299(6) 0.8366(8) 0.4671(7) 0.156(6) Uiso 1 1 d . . . H45A H 0.0455 0.8317 0.4362 0.202 Uiso 1 1 calc R . . H45B H 0.0447 0.8726 0.4939 0.202 Uiso 1 1 calc R . . H45C H -0.0035 0.8466 0.4488 0.202 Uiso 1 1 calc R . . C46 C -0.0592(6) 0.6615(9) 0.4549(8) 0.172(7) Uiso 1 1 d . . . H46A H -0.0345 0.6441 0.4393 0.224 Uiso 1 1 calc R . . H46B H -0.0901 0.6547 0.4257 0.224 Uiso 1 1 calc R . . H46C H -0.0582 0.6384 0.4918 0.224 Uiso 1 1 calc R . . C47 C -0.0902(5) 0.7790(8) 0.4484(7) 0.142(5) Uiso 1 1 d . . . H47A H -0.1064 0.7744 0.4059 0.185 Uiso 1 1 calc R . . H47B H -0.0769 0.8235 0.4565 0.185 Uiso 1 1 calc R . . H47C H -0.1127 0.7717 0.4709 0.185 Uiso 1 1 calc R . . O51 O 0.1037(2) 0.8623(4) 0.6437(3) 0.083(2) Uani 1 1 d . . . O52 O 0.0996(2) 0.9120(3) 0.7269(3) 0.0759(17) Uani 1 1 d . . . C51 C 0.1131(3) 0.9128(6) 0.6795(5) 0.085(3) Uani 1 1 d . . . N5 N 0.1367(3) 0.9655(6) 0.6662(5) 0.121(4) Uani 1 1 d . . . C52 C 0.1576(6) 0.9668(11) 0.6150(7) 0.186(10) Uani 1 1 d . . . H52 H 0.1766 1.0083 0.6192 0.242 Uiso 1 1 calc R . . C53 C 0.1455(6) 1.0226(8) 0.7059(9) 0.175(9) Uani 1 1 d . . . H53 H 0.1291 1.0129 0.7363 0.227 Uiso 1 1 calc R . . C54 C 0.1907(7) 0.9115(10) 0.6175(9) 0.195(9) Uiso 1 1 d . . . H54A H 0.1744 0.8760 0.5911 0.253 Uiso 1 1 calc R . . H54B H 0.2021 0.8949 0.6583 0.253 Uiso 1 1 calc R . . H54C H 0.2174 0.9271 0.6049 0.253 Uiso 1 1 calc R . . C55 C 0.1150(6) 0.9746(9) 0.5565(8) 0.187(7) Uiso 1 1 d . . . H55A H 0.1148 0.9375 0.5299 0.243 Uiso 1 1 calc R . . H55B H 0.1184 1.0161 0.5367 0.243 Uiso 1 1 calc R . . H55C H 0.0854 0.9753 0.5668 0.243 Uiso 1 1 calc R . . C56 C 0.1983(6) 1.0322(9) 0.7411(8) 0.179(7) Uiso 1 1 d . . . H56A H 0.2159 0.9922 0.7379 0.233 Uiso 1 1 calc R . . H56B H 0.2012 1.0407 0.7829 0.233 Uiso 1 1 calc R . . H56C H 0.2111 1.0698 0.7246 0.233 Uiso 1 1 calc R . . C57 C 0.1236(8) 1.0857(12) 0.6757(11) 0.243(11) Uiso 1 1 d . . . H57A H 0.1156 1.0803 0.6326 0.316 Uiso 1 1 calc R . . H57B H 0.1461 1.1221 0.6882 0.316 Uiso 1 1 calc R . . H57C H 0.0950 1.0956 0.6866 0.316 Uiso 1 1 calc R . . O61 O 0.1008(2) 0.5790(3) 0.8359(3) 0.0743(17) Uani 1 1 d . . . O62 O 0.1184(2) 0.6274(4) 0.9250(3) 0.0804(18) Uani 1 1 d . . . C61 C 0.1194(3) 0.5756(5) 0.8930(6) 0.075(3) Uani 1 1 d . . . N6 N 0.1397(3) 0.5185(4) 0.9205(5) 0.096(3) Uani 1 1 d . . . C62 C 0.1362(5) 0.4581(6) 0.8823(8) 0.130(5) Uani 1 1 d . . . H62 H 0.1160 0.4705 0.8418 0.169 Uiso 1 1 calc R . . C63 C 0.1657(5) 0.5142(8) 0.9856(7) 0.145(6) Uani 1 1 d . . . H63 H 0.1778 0.4679 0.9917 0.188 Uiso 1 1 calc R . . C64 C 0.1111(6) 0.4003(9) 0.9029(8) 0.182(7) Uiso 1 1 d . . . H64A H 0.1068 0.3639 0.8745 0.237 Uiso 1 1 calc R . . H64B H 0.0803 0.4151 0.9052 0.237 Uiso 1 1 calc R . . H64C H 0.1302 0.3853 0.9421 0.237 Uiso 1 1 calc R . . C65 C 0.1851(6) 0.4392(8) 0.8760(7) 0.157(6) Uiso 1 1 d . . . H65A H 0.1810 0.4179 0.8375 0.204 Uiso 1 1 calc R . . H65B H 0.2010 0.4086 0.9078 0.204 Uiso 1 1 calc R . . H65C H 0.2043 0.4791 0.8786 0.204 Uiso 1 1 calc R . . C66 C 0.1330(7) 0.5202(10) 1.0239(9) 0.189(8) Uiso 1 1 d . . . H66A H 0.1058 0.4910 1.0085 0.245 Uiso 1 1 calc R . . H66B H 0.1221 0.5660 1.0233 0.245 Uiso 1 1 calc R . . H66C H 0.1499 0.5075 1.0647 0.245 Uiso 1 1 calc R . . C67 C 0.2092(6) 0.5568(9) 1.0012(8) 0.172(7) Uiso 1 1 d . . . H67A H 0.2261 0.5504 0.9717 0.224 Uiso 1 1 calc R . . H67B H 0.2297 0.5445 1.0405 0.224 Uiso 1 1 calc R . . H67C H 0.2001 0.6033 1.0015 0.224 Uiso 1 1 calc R . . C1H C 0.2714(14) 0.272(2) 0.0205(19) 0.341(19) Uiso 1 1 d . . . C2H C 0.3095(18) 0.347(2) 0.087(2) 0.41(2) Uiso 1 1 d . . . C3H C 0.2573(19) 0.321(3) 0.060(2) 0.43(3) Uiso 1 1 d . . . C8H C 0.424(3) 0.286(4) 0.222(3) 0.59(5) Uiso 1 1 d . . . C9H C 0.486(5) 0.264(3) 0.246(8) 0.56(5) Uiso 1 1 d . . . C10H C 0.446(3) 0.225(3) 0.263(3) 0.41(3) Uiso 1 1 d . . . C11H C 0.3986(19) 0.193(2) 0.271(2) 0.43(3) Uiso 1 1 d . . . 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 Ho1 0.03904(19) 0.0537(2) 0.0466(2) 0.00717(17) 0.01299(15) -0.00068(15) Ho2 0.0446(2) 0.0474(2) 0.0443(2) 0.00547(16) 0.00938(15) 0.00243(15) O11 0.050(3) 0.046(3) 0.041(3) 0.001(2) 0.014(2) 0.002(2) O12 0.042(3) 0.058(3) 0.059(3) -0.010(3) 0.011(2) 0.000(2) C11 0.047(4) 0.044(4) 0.041(4) 0.003(3) 0.013(3) 0.001(3) N1 0.048(3) 0.052(4) 0.064(4) -0.021(3) 0.008(3) -0.008(3) C12 0.049(5) 0.075(6) 0.088(7) -0.020(5) 0.016(4) -0.014(4) C13 0.069(5) 0.072(6) 0.070(6) -0.027(5) 0.004(5) -0.008(5) O21 0.048(3) 0.049(3) 0.047(3) 0.001(2) 0.015(2) 0.001(2) O22 0.053(3) 0.056(3) 0.059(3) -0.010(3) 0.015(3) 0.000(2) C21 0.054(5) 0.054(5) 0.045(4) -0.004(4) 0.013(4) 0.001(4) N2 0.057(4) 0.060(4) 0.083(5) -0.018(4) 0.021(4) 0.011(3) C22 0.053(5) 0.104(8) 0.083(7) -0.024(6) 0.007(5) 0.024(5) C23 0.087(7) 0.072(6) 0.089(7) -0.017(6) 0.028(6) 0.022(5) O31 0.043(3) 0.077(4) 0.068(4) 0.013(3) 0.015(3) 0.002(3) O32 0.045(3) 0.067(4) 0.071(4) 0.010(3) 0.014(3) 0.002(3) C31 0.040(4) 0.059(5) 0.075(6) 0.000(5) 0.013(4) 0.007(4) N3 0.039(4) 0.091(6) 0.095(6) 0.009(5) 0.012(4) 0.001(4) C32 0.051(6) 0.132(10) 0.143(11) -0.008(9) 0.035(6) -0.010(6) C33 0.049(6) 0.083(8) 0.223(17) 0.030(9) -0.028(8) 0.008(5) O41 0.068(4) 0.078(4) 0.050(3) -0.007(3) 0.012(3) -0.004(3) O42 0.065(3) 0.070(4) 0.054(3) -0.001(3) 0.024(3) 0.000(3) C41 0.074(6) 0.059(5) 0.052(5) 0.002(4) 0.024(5) 0.006(4) N4 0.078(5) 0.129(7) 0.046(4) 0.004(5) 0.019(4) 0.006(5) C42 0.115(9) 0.180(14) 0.111(10) 0.059(10) 0.073(8) 0.049(9) C43 0.129(10) 0.171(14) 0.061(7) -0.032(8) 0.006(7) 0.049(10) O51 0.064(4) 0.119(6) 0.068(4) 0.030(4) 0.021(3) -0.020(4) O52 0.067(4) 0.057(4) 0.104(5) 0.007(4) 0.026(4) -0.015(3) C51 0.047(5) 0.107(9) 0.087(8) 0.053(7) -0.004(5) -0.011(5) N5 0.091(6) 0.110(8) 0.150(10) 0.054(7) 0.019(6) -0.045(6) C52 0.143(13) 0.26(2) 0.136(13) 0.110(14) 0.012(11) -0.099(14) C53 0.129(12) 0.125(13) 0.24(2) 0.092(14) 0.012(13) -0.049(10) O61 0.068(4) 0.055(4) 0.094(5) 0.003(4) 0.015(3) 0.013(3) O62 0.092(5) 0.080(5) 0.065(4) 0.024(4) 0.016(3) 0.016(4) C61 0.056(5) 0.063(6) 0.108(9) 0.030(6) 0.026(5) 0.010(5) N6 0.081(6) 0.067(6) 0.138(9) 0.048(6) 0.027(6) 0.018(4) C62 0.105(9) 0.074(8) 0.214(17) 0.056(10) 0.052(10) 0.019(7) C63 0.105(10) 0.140(13) 0.178(15) 0.099(12) 0.026(10) 0.035(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ho1 O12 2.223(5) 2_556 ? Ho1 O41 2.239(6) . ? Ho1 O31 2.264(5) . ? Ho1 O51 2.298(6) . ? Ho1 O52 2.342(6) . ? Ho1 O11 2.364(4) . ? Ho1 O21 2.371(5) . ? Ho1 C51 2.687(10) . ? Ho1 Ho2 3.8271(5) . ? Ho2 O22 2.247(5) 2_556 ? Ho2 O42 2.262(5) 2_556 ? Ho2 O32 2.272(5) . ? Ho2 O62 2.321(6) . ? Ho2 O61 2.338(6) . ? Ho2 O21 2.367(5) . ? Ho2 O11 2.398(5) . ? Ho2 C61 2.701(9) . ? O11 C11 1.299(8) . ? O12 C11 1.271(8) . ? O12 Ho1 2.223(5) 2_556 ? C11 N1 1.338(9) . ? N1 C12 1.475(10) . ? N1 C13 1.492(10) . ? C12 C14 1.510(13) . ? C12 C15 1.513(13) . ? C13 C17 1.517(14) . ? C13 C16 1.520(13) . ? O21 C21 1.308(8) . ? O22 C21 1.258(8) . ? O22 Ho2 2.247(5) 2_556 ? C21 N2 1.331(9) . ? N2 C22 1.475(11) . ? N2 C23 1.491(11) . ? C22 C24 1.495(14) . ? C22 C25 1.514(14) . ? C23 C27 1.510(14) . ? C23 C26 1.510(14) . ? O31 C31 1.261(10) . ? O32 C31 1.246(10) . ? C31 N3 1.363(9) . ? N3 C32 1.491(13) . ? N3 C33 1.510(15) . ? C32 C35 1.40(2) . ? C32 C34 1.414(19) . ? C33 C37 1.37(2) . ? C33 C36 1.455(19) . ? O41 C41 1.270(10) . ? O42 C41 1.269(9) . ? O42 Ho2 2.262(5) 2_556 ? C41 N4 1.344(10) . ? N4 C42 1.485(14) . ? N4 C43 1.495(14) . ? C42 C45 1.441(18) . ? C42 C44 1.456(18) . ? C43 C46 1.38(2) . ? C43 C47 1.452(17) . ? O51 C51 1.278(13) . ? O52 C51 1.270(12) . ? C51 N5 1.337(12) . ? N5 C53 1.43(2) . ? N5 C52 1.48(2) . ? C52 C54 1.45(2) . ? C52 C55 1.55(2) . ? C53 C57 1.48(2) . ? C53 C56 1.52(2) . ? O61 C61 1.273(12) . ? O62 C61 1.272(12) . ? C61 N6 1.347(11) . ? N6 C63 1.473(17) . ? N6 C62 1.475(17) . ? C62 C64 1.509(18) . ? C62 C65 1.523(17) . ? C63 C67 1.476(19) . ? C63 C66 1.49(2) . ? C1H C3H 1.47(6) . ? C1H C1H 1.59(7) 7 ? C2H C3H 1.55(6) . ? C8H C10H 1.57(8) . ? C8H C9H 1.79(14) . ? C9H C9H 0.8(3) 2_655 ? C9H C10H 1.54(13) . ? C10H C11H 1.58(7) . ? 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 Ho1 O41 81.7(2) 2_556 . ? O12 Ho1 O31 158.1(2) 2_556 . ? O41 Ho1 O31 119.9(2) . . ? O12 Ho1 O51 97.8(2) 2_556 . ? O41 Ho1 O51 80.4(2) . . ? O31 Ho1 O51 83.6(2) . . ? O12 Ho1 O52 80.5(2) 2_556 . ? O41 Ho1 O52 130.0(2) . . ? O31 Ho1 O52 82.1(2) . . ? O51 Ho1 O52 56.5(3) . . ? O12 Ho1 O11 83.11(17) 2_556 . ? O41 Ho1 O11 137.75(18) . . ? O31 Ho1 O11 82.28(18) . . ? O51 Ho1 O11 140.8(2) . . ? O52 Ho1 O11 85.4(2) . . ? O12 Ho1 O21 111.38(17) 2_556 . ? O41 Ho1 O21 78.57(19) . . ? O31 Ho1 O21 78.85(18) . . ? O51 Ho1 O21 140.7(2) . . ? O52 Ho1 O21 151.2(2) . . ? O11 Ho1 O21 70.86(16) . . ? O12 Ho1 C51 89.8(3) 2_556 . ? O41 Ho1 C51 106.1(3) . . ? O31 Ho1 C51 81.1(2) . . ? O51 Ho1 C51 28.3(3) . . ? O52 Ho1 C51 28.2(3) . . ? O11 Ho1 C51 113.0(3) . . ? O21 Ho1 C51 158.8(2) . . ? O12 Ho1 Ho2 107.14(13) 2_556 . ? O41 Ho1 Ho2 113.63(15) . . ? O31 Ho1 Ho2 69.15(14) . . ? O51 Ho1 Ho2 152.68(16) . . ? O52 Ho1 Ho2 116.26(18) . . ? O11 Ho1 Ho2 36.82(11) . . ? O21 Ho1 Ho2 36.10(11) . . ? C51 Ho1 Ho2 138.5(2) . . ? O22 Ho2 O42 82.20(19) 2_556 2_556 ? O22 Ho2 O32 159.9(2) 2_556 . ? O42 Ho2 O32 117.7(2) 2_556 . ? O22 Ho2 O62 99.5(2) 2_556 . ? O42 Ho2 O62 80.4(2) 2_556 . ? O32 Ho2 O62 82.8(2) . . ? O22 Ho2 O61 79.1(2) 2_556 . ? O42 Ho2 O61 128.2(2) 2_556 . ? O32 Ho2 O61 86.0(2) . . ? O62 Ho2 O61 56.2(2) . . ? O22 Ho2 O21 82.88(17) 2_556 . ? O42 Ho2 O21 139.66(18) 2_556 . ? O32 Ho2 O21 82.51(18) . . ? O62 Ho2 O21 139.1(2) . . ? O61 Ho2 O21 84.9(2) . . ? O22 Ho2 O11 109.67(17) 2_556 . ? O42 Ho2 O11 79.89(18) 2_556 . ? O32 Ho2 O11 78.02(17) . . ? O62 Ho2 O11 141.9(2) . . ? O61 Ho2 O11 151.9(2) . . ? O21 Ho2 O11 70.34(16) . . ? O22 Ho2 C61 88.6(2) 2_556 . ? O42 Ho2 C61 104.5(3) 2_556 . ? O32 Ho2 C61 84.3(2) . . ? O62 Ho2 C61 28.1(3) . . ? O61 Ho2 C61 28.1(3) . . ? O21 Ho2 C61 112.4(3) . . ? O11 Ho2 C61 161.7(2) . . ? O22 Ho2 Ho1 105.82(13) 2_556 . ? O42 Ho2 Ho1 115.29(14) 2_556 . ? O32 Ho2 Ho1 68.94(14) . . ? O62 Ho2 Ho1 151.57(16) . . ? O61 Ho2 Ho1 116.21(17) . . ? O21 Ho2 Ho1 36.17(12) . . ? O11 Ho2 Ho1 36.21(11) . . ? C61 Ho2 Ho1 138.9(2) . . ? C11 O11 Ho1 123.9(4) . . ? C11 O11 Ho2 127.4(4) . . ? Ho1 O11 Ho2 106.97(18) . . ? C11 O12 Ho1 143.9(5) . 2_556 ? O12 C11 O11 120.2(6) . . ? O12 C11 N1 119.5(6) . . ? O11 C11 N1 120.2(6) . . ? C11 N1 C12 120.3(6) . . ? C11 N1 C13 120.4(6) . . ? C12 N1 C13 119.1(6) . . ? N1 C12 C14 111.1(8) . . ? N1 C12 C15 111.6(8) . . ? C14 C12 C15 111.2(9) . . ? N1 C13 C17 111.1(8) . . ? N1 C13 C16 112.9(8) . . ? C17 C13 C16 113.6(8) . . ? C21 O21 Ho2 124.2(4) . . ? C21 O21 Ho1 126.7(4) . . ? Ho2 O21 Ho1 107.73(19) . . ? C21 O22 Ho2 145.8(5) . 2_556 ? O22 C21 O21 120.2(7) . . ? O22 C21 N2 120.3(7) . . ? O21 C21 N2 119.5(7) . . ? C21 N2 C22 120.9(7) . . ? C21 N2 C23 120.4(7) . . ? C22 N2 C23 118.4(7) . . ? N2 C22 C24 112.2(9) . . ? N2 C22 C25 110.2(8) . . ? C24 C22 C25 111.8(9) . . ? N2 C23 C27 113.4(8) . . ? N2 C23 C26 110.3(9) . . ? C27 C23 C26 114.1(9) . . ? C31 O31 Ho1 137.7(5) . . ? C31 O32 Ho2 138.1(5) . . ? O32 C31 O31 124.6(7) . . ? O32 C31 N3 118.3(8) . . ? O31 C31 N3 117.1(8) . . ? C31 N3 C32 120.6(8) . . ? C31 N3 C33 119.0(8) . . ? C32 N3 C33 120.4(8) . . ? C35 C32 C34 129.3(15) . . ? C35 C32 N3 114.7(13) . . ? C34 C32 N3 113.7(13) . . ? C37 C33 C36 131.7(16) . . ? C37 C33 N3 116.4(13) . . ? C36 C33 N3 111.1(13) . . ? C41 O41 Ho1 145.7(5) . . ? C41 O42 Ho2 140.5(5) . 2_556 ? O42 C41 O41 122.5(7) . . ? O42 C41 N4 118.0(8) . . ? O41 C41 N4 119.5(8) . . ? C41 N4 C42 119.6(9) . . ? C41 N4 C43 121.7(9) . . ? C42 N4 C43 118.6(10) . . ? C45 C42 C44 120.3(12) . . ? C45 C42 N4 117.1(11) . . ? C44 C42 N4 112.6(13) . . ? C46 C43 C47 122.9(15) . . ? C46 C43 N4 118.3(13) . . ? C47 C43 N4 115.3(12) . . ? C51 O51 Ho1 93.0(6) . . ? C51 O52 Ho1 91.2(7) . . ? O52 C51 O51 119.2(9) . . ? O52 C51 N5 121.4(13) . . ? O51 C51 N5 119.4(12) . . ? O52 C51 Ho1 60.6(5) . . ? O51 C51 Ho1 58.7(5) . . ? N5 C51 Ho1 176.9(10) . . ? C51 N5 C53 118.5(13) . . ? C51 N5 C52 123.9(14) . . ? C53 N5 C52 117.5(11) . . ? C54 C52 N5 112.3(13) . . ? C54 C52 C55 118(2) . . ? N5 C52 C55 106.6(14) . . ? N5 C53 C57 113.3(17) . . ? N5 C53 C56 113.6(16) . . ? C57 C53 C56 111.8(15) . . ? C61 O61 Ho2 92.0(6) . . ? C61 O62 Ho2 92.8(6) . . ? O62 C61 O61 119.0(8) . . ? O62 C61 N6 119.1(11) . . ? O61 C61 N6 121.8(11) . . ? O62 C61 Ho2 59.1(4) . . ? O61 C61 Ho2 59.9(4) . . ? N6 C61 Ho2 176.8(8) . . ? C61 N6 C63 123.5(12) . . ? C61 N6 C62 117.2(11) . . ? C63 N6 C62 119.2(10) . . ? N6 C62 C64 112.5(13) . . ? N6 C62 C65 110.9(12) . . ? C64 C62 C65 113.5(12) . . ? N6 C63 C67 111.2(12) . . ? N6 C63 C66 112.2(12) . . ? C67 C63 C66 117.6(17) . . ? C3H C1H C1H 115(5) . 7 ? C1H C3H C2H 93(4) . . ? C10H C8H C9H 54(5) . . ? C9H C9H C10H 140(10) 2_655 . ? C9H C9H C8H 164(10) 2_655 . ? C10H C9H C8H 56(6) . . ? C9H C10H C8H 70(6) . . ? C9H C10H C11H 169(9) . . ? C8H C10H C11H 99(6) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 23.01 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.834 _refine_diff_density_min -0.572 _refine_diff_density_rms 0.096 #==END