# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Annie Powell' _publ_contact_author_email ANNIE.POWELL@KIT.EDU _publ_section_title ; Synthesis, Structures and Magnetic Properties of a Series of 3d-4f Tetranuclear CoII2LnIII2 Cubanes ; loop_ _publ_author_name 'Annie Powell' 'Christopher E. Anson' 'Peng Cheng.' 'Yanhua Lan.' 'Bin Zhao.' ; Xiao-Qing Zhao ; # Attachment 'co2ln2_a1.cif' data_zhao416 _database_code_depnum_ccdc_archive 'CCDC 756450' #TrackingRef 'co2ln2_a1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C58 H86 Co2 Y2 N4 O20, 4(C2 H3 N)' _chemical_formula_sum 'C66 H98 Co2 N8 O20 Y2' _chemical_formula_weight 1619.20 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.6311(7) _cell_length_b 18.8516(8) _cell_length_c 26.8450(12) _cell_angle_alpha 90.00 _cell_angle_beta 100.565(4) _cell_angle_gamma 90.00 _cell_volume 7776.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 54904 _cell_measurement_theta_min 1.54 _cell_measurement_theta_max 28.40 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.383 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3368 _exptl_absorpt_coefficient_mu 1.967 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.540 _exptl_absorpt_correction_T_max 0.674 _exptl_absorpt_process_details ; XPREP in SHELXTL 6.14 (BrukerAXS Inc., 2003) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean 6.667 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 56085 _diffrn_reflns_av_R_equivalents 0.0465 _diffrn_reflns_av_sigmaI/netI 0.0366 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 26.73 _reflns_number_total 16475 _reflns_number_gt 13361 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'WinXpose 1.6.8 (Stoe & Cie GmbH, 2004)' _computing_cell_refinement 'X-Area 1.38 (Stoe & Cie GmbH, 2006)' _computing_data_reduction 'X-Area 1.38 (Stoe & Cie GmbH, 2006)' _computing_structure_solution 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_structure_refinement 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_molecular_graphics 'Diamond 2.1 (Crystal Impact, 1998)' _computing_publication_material 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _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. Several pivalate t-butyl groups and lattice MeCN molecules were disordered, and were refined using partial C or N atoms with appropriate geometrical restraints. ; _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^)+(0.0944P)^2^+10.6739P] 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 16475 _refine_ls_number_parameters 900 _refine_ls_number_restraints 40 _refine_ls_R_factor_all 0.0814 _refine_ls_R_factor_gt 0.0652 _refine_ls_wR_factor_ref 0.1696 _refine_ls_wR_factor_gt 0.1607 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.083 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 0.41905(2) 0.190932(19) 0.290507(14) 0.02538(10) Uani 1 1 d . . . Y2 Y 0.61526(3) 0.20525(2) 0.214276(15) 0.02816(11) Uani 1 1 d . . . Co1 Co 0.43301(3) 0.30883(3) 0.19887(2) 0.02567(13) Uani 1 1 d . . . Co2 Co 0.57531(4) 0.32099(3) 0.30276(2) 0.02663(13) Uani 1 1 d . . . N1 N 0.3883(2) 0.41744(18) 0.21028(14) 0.0319(7) Uani 1 1 d . . . C1 C 0.3646(3) 0.4236(2) 0.25534(17) 0.0310(9) Uani 1 1 d . . . C2 C 0.3239(3) 0.4836(2) 0.2697(2) 0.0433(11) Uani 1 1 d . . . H2A H 0.3081 0.4859 0.3022 0.052 Uiso 1 1 calc R . . C3 C 0.3065(3) 0.5400(3) 0.2363(2) 0.0492(12) Uani 1 1 d . . . H3A H 0.2792 0.5819 0.2454 0.059 Uiso 1 1 calc R . . C4 C 0.3301(4) 0.5335(3) 0.1893(2) 0.0496(13) Uani 1 1 d . . . H4A H 0.3179 0.5709 0.1653 0.059 Uiso 1 1 calc R . . C5 C 0.3712(3) 0.4729(2) 0.17717(19) 0.0416(11) Uani 1 1 d . . . C6 C 0.3798(3) 0.3608(2) 0.29083(16) 0.0309(9) Uani 1 1 d . . . H6A H 0.4056 0.3779 0.3252 0.037 Uiso 1 1 calc R . . H6B H 0.3229 0.3388 0.2927 0.037 Uiso 1 1 calc R . . O1 O 0.43442(19) 0.30906(13) 0.27619(10) 0.0281(6) Uani 1 1 d . . . C7 C 0.3956(5) 0.4653(3) 0.1261(2) 0.0606(16) Uani 1 1 d . . . H7A H 0.3975 0.5128 0.1107 0.073 Uiso 1 1 calc R . . H7B H 0.4545 0.4442 0.1300 0.073 Uiso 1 1 calc R . . O2 O 0.3352(4) 0.4216(3) 0.09320(16) 0.0738(14) Uani 1 1 d D . . H2 H 0.354(6) 0.376(2) 0.098(3) 0.111 Uiso 1 1 d D . . N2 N 0.5876(2) 0.43506(18) 0.28841(14) 0.0337(8) Uani 1 1 d . . . C8 C 0.6007(3) 0.4456(2) 0.24114(18) 0.0353(9) Uani 1 1 d . . . C9 C 0.6099(4) 0.5127(3) 0.2219(2) 0.0568(15) Uani 1 1 d . . . H9A H 0.6174 0.5187 0.1878 0.068 Uiso 1 1 calc R . . C10 C 0.6080(6) 0.5712(3) 0.2534(3) 0.076(2) Uani 1 1 d . . . H10A H 0.6145 0.6179 0.2412 0.092 Uiso 1 1 calc R . . C11 C 0.5965(5) 0.5603(3) 0.3025(2) 0.0593(15) Uani 1 1 d . . . H11A H 0.5957 0.5994 0.3248 0.071 Uiso 1 1 calc R . . C12 C 0.5861(3) 0.4917(2) 0.3191(2) 0.0428(11) Uani 1 1 d . . . C13 C 0.6097(3) 0.3811(2) 0.20903(17) 0.0354(9) Uani 1 1 d . . . H13A H 0.5818 0.3912 0.1736 0.043 Uiso 1 1 calc R . . H13B H 0.6722 0.3722 0.2095 0.043 Uiso 1 1 calc R . . O3 O 0.57255(19) 0.32011(14) 0.22520(11) 0.0296(6) Uani 1 1 d . . . C14 C 0.5774(5) 0.4791(3) 0.3728(2) 0.0606(16) Uani 1 1 d . . . H14A H 0.5666 0.5249 0.3887 0.073 Uiso 1 1 calc R . . H14B H 0.5267 0.4480 0.3736 0.073 Uiso 1 1 calc R . . O4 O 0.6531(4) 0.4473(2) 0.40121(17) 0.0838(16) Uani 1 1 d D . . H4 H 0.657(6) 0.397(2) 0.400(4) 0.126 Uiso 1 1 d D . . N3 N 0.4209(2) 0.07446(18) 0.24760(14) 0.0329(8) Uani 1 1 d . . . C15 C 0.4191(3) 0.0742(2) 0.19744(18) 0.0371(10) Uani 1 1 d . . . C16 C 0.4166(4) 0.0108(3) 0.1703(2) 0.0467(12) Uani 1 1 d . . . H16A H 0.4146 0.0112 0.1347 0.056 Uiso 1 1 calc R . . C17 C 0.4172(4) -0.0536(3) 0.1967(2) 0.0609(16) Uani 1 1 d . . . H17A H 0.4152 -0.0974 0.1791 0.073 Uiso 1 1 calc R . . C18 C 0.4206(4) -0.0529(3) 0.2480(2) 0.0571(15) Uani 1 1 d . . . H18A H 0.4224 -0.0961 0.2665 0.068 Uiso 1 1 calc R . . C19 C 0.4215(3) 0.0126(2) 0.2729(2) 0.0409(10) Uani 1 1 d . . . C20 C 0.4227(3) 0.1454(2) 0.17250(16) 0.0308(8) Uani 1 1 d . . . H20A H 0.4559 0.1414 0.1445 0.037 Uiso 1 1 calc R . . H20B H 0.3630 0.1614 0.1580 0.037 Uiso 1 1 calc R . . O5 O 0.46265(18) 0.19482(13) 0.20781(10) 0.0245(5) Uani 1 1 d . . . C21 C 0.4217(4) 0.0179(2) 0.3282(2) 0.0452(11) Uani 1 1 d . . . H21A H 0.3662 -0.0006 0.3356 0.054 Uiso 1 1 calc R . . H21B H 0.4697 -0.0112 0.3470 0.054 Uiso 1 1 calc R . . O6 O 0.4326(2) 0.08934(16) 0.34408(13) 0.0405(7) Uani 1 1 d D . . H6 H 0.391(3) 0.100(3) 0.3655(19) 0.049 Uiso 1 1 d D . . N4 N 0.6405(2) 0.0922(2) 0.26170(16) 0.0371(8) Uani 1 1 d . . . C22 C 0.6421(3) 0.0929(2) 0.31135(19) 0.0380(10) Uani 1 1 d . . . C23 C 0.6605(4) 0.0325(3) 0.3414(2) 0.0564(14) Uani 1 1 d . . . H23A H 0.6620 0.0343 0.3769 0.068 Uiso 1 1 calc R . . C24 C 0.6768(5) -0.0304(3) 0.3177(3) 0.0694(18) Uani 1 1 d . . . H24A H 0.6896 -0.0724 0.3371 0.083 Uiso 1 1 calc R . . C25 C 0.6743(4) -0.0316(3) 0.2666(2) 0.0574(15) Uani 1 1 d . . . H25A H 0.6851 -0.0744 0.2500 0.069 Uiso 1 1 calc R . . C26 C 0.6558(3) 0.0306(3) 0.2394(2) 0.0443(11) Uani 1 1 d . . . C27 C 0.6211(3) 0.1626(2) 0.33357(16) 0.0335(9) Uani 1 1 d . . . H27A H 0.5891 0.1539 0.3616 0.040 Uiso 1 1 calc R . . H27B H 0.6758 0.1876 0.3477 0.040 Uiso 1 1 calc R . . O7 O 0.57117(17) 0.20474(14) 0.29722(10) 0.0243(5) Uani 1 1 d . . . C28 C 0.6510(4) 0.0336(3) 0.1833(2) 0.0488(12) Uani 1 1 d . . . H28A H 0.7091 0.0230 0.1753 0.059 Uiso 1 1 calc R . . H28B H 0.6099 -0.0030 0.1669 0.059 Uiso 1 1 calc R . . O8 O 0.6231(2) 0.10138(18) 0.16372(14) 0.0455(8) Uani 1 1 d D . . H8 H 0.657(3) 0.111(3) 0.1372(18) 0.055 Uiso 1 1 d D . . O9 O 0.30204(19) 0.28935(17) 0.17769(12) 0.0356(7) Uani 1 1 d . . . O10 O 0.29090(19) 0.20048(16) 0.23146(11) 0.0334(6) Uani 1 1 d . . . C29 C 0.2594(3) 0.2415(2) 0.19568(15) 0.0297(8) Uani 1 1 d . . . C30 C 0.1631(3) 0.2335(3) 0.17221(19) 0.0481(13) Uani 1 1 d . . . C31 C 0.1105(4) 0.2289(5) 0.2146(3) 0.076(2) Uani 1 1 d . . . H31A H 0.1155 0.2737 0.2335 0.115 Uiso 1 1 calc R . . H31B H 0.1328 0.1900 0.2376 0.115 Uiso 1 1 calc R . . H31C H 0.0492 0.2200 0.2000 0.115 Uiso 1 1 calc R . . C32 C 0.1328(4) 0.2956(4) 0.1367(2) 0.072(2) Uani 1 1 d . . . H32A H 0.1372 0.3398 0.1563 0.108 Uiso 1 1 calc R . . H32B H 0.0721 0.2881 0.1202 0.108 Uiso 1 1 calc R . . H32C H 0.1695 0.2988 0.1109 0.108 Uiso 1 1 calc R . . C33 C 0.1552(5) 0.1640(4) 0.1411(3) 0.085(2) Uani 1 1 d . . . H33A H 0.0943 0.1565 0.1253 0.128 Uiso 1 1 calc R . . H33B H 0.1754 0.1241 0.1636 0.128 Uiso 1 1 calc R . . H33C H 0.1909 0.1675 0.1148 0.128 Uiso 1 1 calc R . . O11 O 0.4440(2) 0.30966(17) 0.12478(11) 0.0366(7) Uani 1 1 d . . . O12 O 0.5580(2) 0.23736(18) 0.12983(11) 0.0380(7) Uani 1 1 d . . . C34 C 0.4932(3) 0.2685(2) 0.10499(16) 0.0329(9) Uani 1 1 d . . . C35 C 0.4703(3) 0.2589(3) 0.04734(18) 0.0457(12) Uani 1 1 d . . . C36 C 0.5228(4) 0.1980(4) 0.0304(2) 0.0622(16) Uani 1 1 d . . . H36A H 0.5082 0.1930 -0.0065 0.093 Uiso 1 1 calc R . . H36B H 0.5089 0.1538 0.0464 0.093 Uiso 1 1 calc R . . H36C H 0.5851 0.2080 0.0405 0.093 Uiso 1 1 calc R . . C37 C 0.4952(5) 0.3289(4) 0.0241(2) 0.0650(17) Uani 1 1 d . . . H37A H 0.4615 0.3679 0.0350 0.097 Uiso 1 1 calc R . . H37B H 0.4825 0.3254 -0.0129 0.097 Uiso 1 1 calc R . . H37C H 0.5574 0.3380 0.0355 0.097 Uiso 1 1 calc R . . C38 C 0.3721(4) 0.2459(5) 0.0319(2) 0.075(2) Uani 1 1 d . . . H38A H 0.3403 0.2861 0.0428 0.112 Uiso 1 1 calc R . . H38B H 0.3563 0.2024 0.0480 0.112 Uiso 1 1 calc R . . H38C H 0.3569 0.2409 -0.0050 0.112 Uiso 1 1 calc R . . O13 O 0.5668(2) 0.32009(16) 0.37667(12) 0.0370(7) Uani 1 1 d . . . O14 O 0.47042(19) 0.23213(16) 0.37422(11) 0.0331(6) Uani 1 1 d . . . C39 C 0.5280(3) 0.2716(2) 0.39792(16) 0.0330(9) Uani 1 1 d . . . C40 C 0.5549(3) 0.2636(3) 0.45547(16) 0.0388(10) Uani 1 1 d . . . C41 C 0.5153(4) 0.1973(3) 0.47412(19) 0.0519(13) Uani 1 1 d . . . H41A H 0.4517 0.2000 0.4654 0.078 Uiso 1 1 calc R . . H41B H 0.5331 0.1936 0.5110 0.078 Uiso 1 1 calc R . . H41C H 0.5356 0.1554 0.4580 0.078 Uiso 1 1 calc R . . C42 C 0.5234(4) 0.3294(3) 0.47979(19) 0.0563(14) Uani 1 1 d . . . H42A H 0.4597 0.3313 0.4721 0.084 Uiso 1 1 calc R . . H42B H 0.5473 0.3719 0.4664 0.084 Uiso 1 1 calc R . . H42C H 0.5431 0.3274 0.5166 0.084 Uiso 1 1 calc R . . C43 C 0.6545(4) 0.2601(4) 0.4684(2) 0.0677(19) Uani 1 1 d . . . H43A H 0.6730 0.2554 0.5052 0.102 Uiso 1 1 calc R . . H43B H 0.6791 0.3036 0.4569 0.102 Uiso 1 1 calc R . . H43C H 0.6749 0.2190 0.4516 0.102 Uiso 1 1 calc R . . O15 O 0.7104(2) 0.32251(17) 0.32356(12) 0.0382(7) Uani 1 1 d . . . O16 O 0.7375(2) 0.23504(18) 0.27227(12) 0.0392(7) Uani 1 1 d . . . C44 C 0.7603(3) 0.2774(2) 0.30864(17) 0.0344(9) Uani 1 1 d . . . C45 C 0.8560(3) 0.2742(3) 0.33598(18) 0.0388(10) Uani 1 1 d . . . C46 C 0.8765(4) 0.3332(3) 0.3749(2) 0.0540(14) Uani 1 1 d . . . H46A H 0.8671 0.3793 0.3579 0.081 Uiso 1 1 calc R . . H46B H 0.9373 0.3294 0.3921 0.081 Uiso 1 1 calc R . . H46C H 0.8382 0.3290 0.3999 0.081 Uiso 1 1 calc R . . C47 C 0.8693(4) 0.2017(3) 0.3627(2) 0.0504(13) Uani 1 1 d . . . H47A H 0.8574 0.1637 0.3375 0.076 Uiso 1 1 calc R . . H47B H 0.8294 0.1974 0.3868 0.076 Uiso 1 1 calc R . . H47C H 0.9294 0.1978 0.3810 0.076 Uiso 1 1 calc R . . C48 C 0.9147(3) 0.2796(3) 0.2961(2) 0.0498(12) Uani 1 1 d . . . H48A H 0.9001 0.2415 0.2712 0.075 Uiso 1 1 calc R . . H48B H 0.9758 0.2751 0.3127 0.075 Uiso 1 1 calc R . . H48C H 0.9058 0.3256 0.2790 0.075 Uiso 1 1 calc R . . O17 O 0.3014(2) 0.20172(17) 0.33183(11) 0.0361(7) Uani 1 1 d . . . O18 O 0.3218(2) 0.12634(17) 0.39692(13) 0.0431(8) Uani 1 1 d . . . C49 C 0.2864(3) 0.1807(2) 0.37426(16) 0.0325(9) Uani 1 1 d . A . C50 C 0.2218(3) 0.2239(3) 0.39869(17) 0.0386(10) Uani 1 1 d D . . C51A C 0.1957(7) 0.1804(5) 0.4416(3) 0.064(2) Uani 0.71 1 d P A 1 H51A H 0.2476 0.1696 0.4669 0.097 Uiso 0.71 1 calc PR A 1 H51B H 0.1683 0.1361 0.4278 0.097 Uiso 0.71 1 calc PR A 1 H51C H 0.1545 0.2076 0.4574 0.097 Uiso 0.71 1 calc PR A 1 C52A C 0.1424(5) 0.2403(5) 0.3591(3) 0.055(2) Uani 0.71 1 d P A 1 H52A H 0.1138 0.1959 0.3464 0.082 Uiso 0.71 1 calc PR A 1 H52B H 0.1600 0.2663 0.3310 0.082 Uiso 0.71 1 calc PR A 1 H52C H 0.1018 0.2693 0.3742 0.082 Uiso 0.71 1 calc PR A 1 C53A C 0.2686(6) 0.2915(5) 0.4185(4) 0.066(3) Uani 0.71 1 d P A 1 H53A H 0.3189 0.2797 0.4448 0.099 Uiso 0.71 1 calc PR A 1 H53B H 0.2288 0.3222 0.4329 0.099 Uiso 0.71 1 calc PR A 1 H53C H 0.2885 0.3163 0.3906 0.099 Uiso 0.71 1 calc PR A 1 C51B C 0.147(2) 0.184(2) 0.4143(14) 0.135(15) Uiso 0.29 1 d PD A 2 H51D H 0.1092 0.2171 0.4283 0.203 Uiso 0.29 1 calc PR A 2 H51E H 0.1695 0.1483 0.4400 0.203 Uiso 0.29 1 calc PR A 2 H51F H 0.1128 0.1600 0.3846 0.203 Uiso 0.29 1 calc PR A 2 C52B C 0.177(3) 0.2852(18) 0.3672(16) 0.159(19) Uiso 0.29 1 d PD A 2 H52D H 0.1369 0.3089 0.3860 0.239 Uiso 0.29 1 calc PR A 2 H52E H 0.1440 0.2668 0.3351 0.239 Uiso 0.29 1 calc PR A 2 H52F H 0.2206 0.3191 0.3602 0.239 Uiso 0.29 1 calc PR A 2 C53B C 0.266(3) 0.260(2) 0.4475(12) 0.147(18) Uiso 0.29 1 d PD A 2 H53D H 0.2227 0.2864 0.4620 0.220 Uiso 0.29 1 calc PR A 2 H53E H 0.3112 0.2919 0.4402 0.220 Uiso 0.29 1 calc PR A 2 H53F H 0.2923 0.2234 0.4717 0.220 Uiso 0.29 1 calc PR A 2 O19 O 0.7293(2) 0.2274(2) 0.17274(12) 0.0446(8) Uani 1 1 d . . . O20 O 0.7290(3) 0.1472(2) 0.11156(15) 0.0549(10) Uani 1 1 d . . . C54 C 0.7534(3) 0.2062(3) 0.13269(18) 0.0425(11) Uani 1 1 d . . . C55 C 0.8122(3) 0.2554(3) 0.10862(19) 0.0465(12) Uani 1 1 d . . . C56 C 0.7542(4) 0.3151(3) 0.0836(2) 0.0590(15) Uani 1 1 d . . . H56A H 0.7268 0.3390 0.1091 0.089 Uiso 1 1 calc R . . H56B H 0.7091 0.2954 0.0570 0.089 Uiso 1 1 calc R . . H56C H 0.7894 0.3493 0.0687 0.089 Uiso 1 1 calc R . . C57 C 0.8828(4) 0.2855(4) 0.1504(2) 0.0700(19) Uani 1 1 d . . . H57A H 0.9200 0.2468 0.1663 0.105 Uiso 1 1 calc R . . H57B H 0.8554 0.3091 0.1760 0.105 Uiso 1 1 calc R . . H57C H 0.9181 0.3199 0.1357 0.105 Uiso 1 1 calc R . . C58 C 0.8552(6) 0.2143(4) 0.0706(3) 0.097(3) Uani 1 1 d . . . H58A H 0.8922 0.1768 0.0883 0.145 Uiso 1 1 calc R . . H58B H 0.8907 0.2467 0.0544 0.145 Uiso 1 1 calc R . . H58C H 0.8101 0.1930 0.0447 0.145 Uiso 1 1 calc R . . N61A N 0.4286(10) 0.4685(8) -0.0838(6) 0.084(4) Uiso 0.50 1 d P B 1 N61B N 0.3932(12) 0.4944(10) -0.0919(7) 0.099(5) Uiso 0.50 1 d P B 2 C61 C 0.3844(6) 0.4932(5) -0.0554(3) 0.090(3) Uani 1 1 d . . . C62A C 0.3319(13) 0.4991(10) -0.0180(8) 0.087(5) Uiso 0.50 1 d P B 1 C62B C 0.3590(10) 0.5188(8) -0.0070(6) 0.062(3) Uiso 0.50 1 d P B 2 N62 N 0.4023(7) 0.0239(7) 0.5488(3) 0.153(4) Uani 1 1 d D . . C63 C 0.3874(6) 0.0043(5) 0.5076(4) 0.094(3) Uani 1 1 d D . . C64 C 0.3699(6) -0.0239(4) 0.4559(3) 0.085(2) Uani 1 1 d D . . H64A H 0.4247 -0.0386 0.4462 0.128 Uiso 1 1 calc R . . H64B H 0.3424 0.0130 0.4326 0.128 Uiso 1 1 calc R . . H64C H 0.3308 -0.0648 0.4543 0.128 Uiso 1 1 calc R . . N63A N 0.413(4) 0.506(4) 0.4010(17) 0.46(4) Uiso 0.50 1 d PD C 1 C65A C 0.3854(11) 0.4945(8) 0.4353(6) 0.070(4) Uiso 0.50 1 d PD C 1 C66A C 0.326(2) 0.496(2) 0.4735(13) 0.201(15) Uiso 0.50 1 d PD C 1 N63B N 0.3501(11) 0.4770(8) 0.4005(5) 0.098(4) Uiso 0.50 1 d PD D 2 C65B C 0.3447(10) 0.4743(7) 0.4405(5) 0.062(3) Uiso 0.50 1 d PD D 2 C66B C 0.3468(11) 0.4673(9) 0.4957(5) 0.076(4) Uiso 0.50 1 d PD D 2 N64A N 0.5904(12) 0.0528(10) -0.0451(7) 0.118(6) Uiso 0.50 1 d PD E 1 C67A C 0.6075(11) 0.0287(10) -0.0046(6) 0.079(4) Uiso 0.50 1 d PD E 1 C68A C 0.6409(14) 0.0132(11) 0.0488(6) 0.077(6) Uiso 0.50 1 d PD E 1 N64B N 0.5902(18) -0.0024(16) -0.0451(9) 0.183(11) Uiso 0.50 1 d PD F 2 C67B C 0.615(2) -0.0094(17) -0.0021(9) 0.151(11) Uiso 0.50 1 d PD F 2 C68B C 0.6268(17) -0.0043(14) 0.0525(8) 0.101(8) Uiso 0.50 1 d PD F 2 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 Y1 0.02763(19) 0.02472(18) 0.02368(19) 0.00193(13) 0.00439(14) -0.00008(14) Y2 0.02690(19) 0.0318(2) 0.0253(2) -0.00020(15) 0.00346(14) 0.00013(15) Co1 0.0256(3) 0.0287(3) 0.0226(3) 0.0027(2) 0.0039(2) 0.0003(2) Co2 0.0281(3) 0.0282(3) 0.0230(3) 0.0000(2) 0.0029(2) -0.0007(2) N1 0.0303(18) 0.0286(17) 0.038(2) 0.0076(14) 0.0079(15) 0.0052(14) C1 0.027(2) 0.0287(19) 0.037(2) 0.0015(17) 0.0044(17) 0.0014(15) C2 0.043(3) 0.036(2) 0.052(3) 0.004(2) 0.013(2) 0.009(2) C3 0.046(3) 0.037(2) 0.067(4) 0.004(2) 0.014(3) 0.012(2) C4 0.048(3) 0.038(2) 0.062(3) 0.016(2) 0.009(2) 0.013(2) C5 0.044(3) 0.036(2) 0.045(3) 0.013(2) 0.009(2) 0.0082(19) C6 0.033(2) 0.030(2) 0.031(2) 0.0000(16) 0.0101(17) 0.0105(16) O1 0.0353(15) 0.0193(12) 0.0245(14) -0.0022(10) -0.0085(11) 0.0070(11) C7 0.083(4) 0.052(3) 0.050(3) 0.023(3) 0.020(3) 0.022(3) O2 0.103(4) 0.071(3) 0.040(2) 0.011(2) -0.005(2) 0.034(3) N2 0.0360(19) 0.0279(17) 0.037(2) -0.0010(14) 0.0055(15) -0.0056(14) C8 0.038(2) 0.030(2) 0.038(2) 0.0004(17) 0.0075(18) -0.0055(17) C9 0.087(4) 0.036(3) 0.052(3) 0.006(2) 0.025(3) -0.002(3) C10 0.134(7) 0.028(3) 0.076(4) 0.001(3) 0.043(4) -0.011(3) C11 0.091(5) 0.033(3) 0.058(4) -0.008(2) 0.024(3) -0.007(3) C12 0.050(3) 0.031(2) 0.047(3) -0.005(2) 0.009(2) -0.003(2) C13 0.042(2) 0.029(2) 0.036(2) 0.0013(17) 0.0098(19) -0.0133(18) O3 0.0362(15) 0.0209(12) 0.0255(14) 0.0050(10) -0.0112(12) -0.0096(11) C14 0.097(5) 0.042(3) 0.044(3) -0.014(2) 0.015(3) -0.010(3) O4 0.136(5) 0.050(2) 0.050(2) -0.008(2) -0.022(3) -0.016(3) N3 0.0351(19) 0.0267(17) 0.037(2) -0.0023(14) 0.0080(15) -0.0006(14) C15 0.034(2) 0.033(2) 0.045(3) -0.0089(19) 0.0076(19) -0.0043(17) C16 0.056(3) 0.036(2) 0.051(3) -0.014(2) 0.014(2) -0.006(2) C17 0.083(4) 0.032(3) 0.071(4) -0.014(2) 0.021(3) -0.010(3) C18 0.079(4) 0.027(2) 0.070(4) -0.005(2) 0.026(3) 0.003(2) C19 0.041(3) 0.030(2) 0.053(3) 0.003(2) 0.012(2) 0.0005(18) C20 0.031(2) 0.034(2) 0.027(2) -0.0065(16) 0.0041(16) -0.0043(16) O5 0.0291(14) 0.0237(12) 0.0220(13) 0.0025(10) 0.0078(10) 0.0040(10) C21 0.055(3) 0.030(2) 0.054(3) 0.004(2) 0.019(2) 0.000(2) O6 0.057(2) 0.0299(15) 0.0379(18) 0.0068(13) 0.0175(15) 0.0030(14) N4 0.0266(18) 0.0350(19) 0.049(2) -0.0007(16) 0.0044(16) 0.0057(14) C22 0.030(2) 0.040(2) 0.044(3) 0.010(2) 0.0062(19) 0.0075(18) C23 0.062(3) 0.048(3) 0.058(3) 0.017(3) 0.006(3) 0.019(3) C24 0.086(5) 0.043(3) 0.078(5) 0.022(3) 0.010(4) 0.026(3) C25 0.060(3) 0.039(3) 0.071(4) 0.004(3) 0.006(3) 0.021(2) C26 0.039(3) 0.038(2) 0.056(3) -0.002(2) 0.008(2) 0.006(2) C27 0.029(2) 0.039(2) 0.031(2) 0.0101(17) 0.0008(17) 0.0058(17) O7 0.0242(13) 0.0258(13) 0.0231(13) -0.0017(10) 0.0045(10) -0.0023(10) C28 0.054(3) 0.039(2) 0.057(3) -0.003(2) 0.018(3) 0.007(2) O8 0.058(2) 0.0376(17) 0.0437(19) -0.0040(15) 0.0161(16) 0.0048(15) O9 0.0289(15) 0.0406(16) 0.0359(17) 0.0071(13) 0.0022(13) 0.0018(12) O10 0.0276(14) 0.0432(17) 0.0281(15) 0.0054(12) 0.0016(12) -0.0017(12) C29 0.0231(19) 0.041(2) 0.0243(19) -0.0021(16) 0.0034(15) -0.0018(16) C30 0.026(2) 0.078(4) 0.036(3) 0.017(2) -0.0061(19) -0.006(2) C31 0.031(3) 0.135(7) 0.065(4) 0.045(4) 0.015(3) 0.002(3) C32 0.035(3) 0.120(6) 0.057(4) 0.043(4) -0.002(3) 0.006(3) C33 0.083(5) 0.107(6) 0.053(4) -0.009(4) -0.017(3) -0.047(4) O11 0.0401(17) 0.0451(17) 0.0247(15) 0.0069(13) 0.0063(13) 0.0063(14) O12 0.0383(17) 0.0532(19) 0.0229(15) 0.0003(13) 0.0062(13) 0.0037(14) C34 0.032(2) 0.042(2) 0.025(2) 0.0018(17) 0.0080(17) -0.0025(18) C35 0.037(3) 0.073(3) 0.026(2) -0.001(2) 0.0019(19) 0.003(2) C36 0.066(4) 0.083(4) 0.037(3) -0.018(3) 0.007(3) 0.010(3) C37 0.080(4) 0.088(4) 0.029(3) 0.017(3) 0.017(3) 0.012(4) C38 0.041(3) 0.134(7) 0.044(3) -0.024(4) -0.009(2) -0.003(4) O13 0.0447(18) 0.0376(16) 0.0288(16) -0.0041(12) 0.0067(13) -0.0074(13) O14 0.0332(15) 0.0438(16) 0.0222(14) 0.0020(12) 0.0050(12) -0.0045(13) C39 0.032(2) 0.044(2) 0.023(2) 0.0000(17) 0.0042(16) 0.0017(18) C40 0.035(2) 0.059(3) 0.021(2) 0.0018(19) 0.0011(17) 0.001(2) C41 0.062(3) 0.064(3) 0.027(2) 0.008(2) 0.002(2) 0.001(3) C42 0.073(4) 0.070(4) 0.026(2) -0.013(2) 0.010(2) -0.011(3) C43 0.038(3) 0.123(6) 0.037(3) 0.010(3) -0.007(2) -0.001(3) O15 0.0325(16) 0.0414(17) 0.0388(18) -0.0023(14) 0.0019(13) -0.0005(13) O16 0.0288(15) 0.0540(19) 0.0332(17) -0.0054(14) 0.0012(13) -0.0037(14) C44 0.027(2) 0.044(2) 0.031(2) 0.0041(18) 0.0016(17) -0.0045(18) C45 0.026(2) 0.044(2) 0.042(3) 0.004(2) -0.0045(18) -0.0018(18) C46 0.046(3) 0.057(3) 0.051(3) -0.005(3) -0.013(2) -0.001(2) C47 0.043(3) 0.052(3) 0.051(3) 0.012(2) -0.005(2) 0.003(2) C48 0.028(2) 0.069(3) 0.052(3) 0.011(3) 0.007(2) -0.003(2) O17 0.0331(16) 0.0500(18) 0.0271(15) 0.0030(13) 0.0108(12) 0.0017(13) O18 0.051(2) 0.0399(17) 0.0415(19) 0.0059(14) 0.0171(15) -0.0019(15) C49 0.030(2) 0.040(2) 0.028(2) -0.0035(17) 0.0054(16) -0.0074(17) C50 0.034(2) 0.051(3) 0.031(2) -0.003(2) 0.0095(18) -0.003(2) C51A 0.075(6) 0.083(6) 0.048(5) 0.016(4) 0.045(5) 0.019(5) C52A 0.034(4) 0.086(6) 0.042(4) -0.013(4) -0.002(3) 0.019(4) C53A 0.051(5) 0.058(5) 0.095(7) -0.045(5) 0.030(5) -0.013(4) O19 0.0316(16) 0.071(2) 0.0333(17) -0.0062(16) 0.0121(13) -0.0053(16) O20 0.069(3) 0.052(2) 0.050(2) -0.0014(17) 0.0265(19) 0.0098(19) C54 0.040(3) 0.058(3) 0.031(2) 0.005(2) 0.0106(19) 0.015(2) C55 0.040(3) 0.065(3) 0.039(3) 0.006(2) 0.018(2) 0.005(2) C56 0.057(3) 0.065(4) 0.050(3) 0.012(3) -0.001(3) 0.000(3) C57 0.036(3) 0.114(6) 0.059(4) 0.026(4) 0.006(3) 0.002(3) C58 0.125(7) 0.087(5) 0.104(6) 0.000(5) 0.088(6) 0.008(5) C61 0.109(7) 0.104(6) 0.057(5) -0.003(4) 0.013(4) -0.025(5) N62 0.145(9) 0.247(13) 0.076(6) 0.007(7) 0.043(6) 0.033(8) C63 0.076(5) 0.121(7) 0.092(6) 0.037(6) 0.032(5) 0.022(5) C64 0.091(6) 0.092(5) 0.072(5) 0.027(4) 0.013(4) 0.011(4) _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 Y1 O1 2.280(3) . ? Y1 O10 2.322(3) . ? Y1 O17 2.325(3) . ? Y1 O7 2.366(3) . ? Y1 O14 2.374(3) . ? Y1 O6 2.381(3) . ? Y1 O5 2.440(3) . ? Y1 N3 2.482(3) . ? Y2 O3 2.300(3) . ? Y2 O16 2.301(3) . ? Y2 O19 2.307(3) . ? Y2 O12 2.359(3) . ? Y2 O5 2.368(3) . ? Y2 O8 2.399(3) . ? Y2 O7 2.449(3) . ? Y2 N4 2.477(4) . ? Co1 O11 2.028(3) . ? Co1 O9 2.055(3) . ? Co1 O1 2.072(3) . ? Co1 O3 2.177(3) . ? Co1 O5 2.202(3) . ? Co1 N1 2.203(3) . ? Co2 O13 2.013(3) . ? Co2 O3 2.075(3) . ? Co2 O15 2.083(3) . ? Co2 O7 2.197(3) . ? Co2 O1 2.198(3) . ? Co2 N2 2.199(3) . ? N1 C1 1.333(6) . ? N1 C5 1.366(6) . ? C1 C2 1.387(6) . ? C1 C6 1.511(6) . ? C2 C3 1.386(7) . ? C2 H2A 0.9500 . ? C3 C4 1.384(8) . ? C3 H3A 0.9500 . ? C4 C5 1.380(7) . ? C4 H4A 0.9500 . ? C5 C7 1.495(7) . ? C6 O1 1.399(5) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 O2 1.430(8) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? O2 H2 0.90(4) . ? N2 C8 1.337(6) . ? N2 C12 1.352(6) . ? C8 C9 1.384(6) . ? C8 C13 1.512(6) . ? C9 C10 1.395(8) . ? C9 H9A 0.9500 . ? C10 C11 1.378(9) . ? C10 H10A 0.9500 . ? C11 C12 1.388(7) . ? C11 H11A 0.9500 . ? C12 C14 1.491(8) . ? C13 O3 1.392(5) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 O4 1.418(8) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? O4 H4 0.94(4) . ? N3 C15 1.342(6) . ? N3 C19 1.349(6) . ? C15 C16 1.397(6) . ? C15 C20 1.506(6) . ? C16 C17 1.406(8) . ? C16 H16A 0.9500 . ? C17 C18 1.369(9) . ? C17 H17A 0.9500 . ? C18 C19 1.402(7) . ? C18 H18A 0.9500 . ? C19 C21 1.486(7) . ? C20 O5 1.393(5) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 O6 1.414(5) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? O6 H6 0.97(3) . ? N4 C22 1.329(6) . ? N4 C26 1.349(6) . ? C22 C23 1.395(7) . ? C22 C27 1.503(6) . ? C23 C24 1.390(9) . ? C23 H23A 0.9500 . ? C24 C25 1.367(9) . ? C24 H24A 0.9500 . ? C25 C26 1.383(7) . ? C25 H25A 0.9500 . ? C26 C28 1.494(8) . ? C27 O7 1.383(5) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 O8 1.420(6) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? O8 H8 0.99(3) . ? O9 C29 1.269(5) . ? O10 C29 1.261(5) . ? C29 C30 1.529(6) . ? C30 C31 1.524(8) . ? C30 C32 1.530(8) . ? C30 C33 1.545(10) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? O11 C34 1.275(5) . ? O12 C34 1.252(5) . ? C34 C35 1.534(6) . ? C35 C36 1.528(8) . ? C35 C38 1.536(7) . ? C35 C37 1.539(8) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? O13 C39 1.286(5) . ? O14 C39 1.249(5) . ? C39 C40 1.533(6) . ? C40 C41 1.520(7) . ? C40 C42 1.525(7) . ? C40 C43 1.533(7) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? O15 C44 1.267(6) . ? O16 C44 1.261(5) . ? C44 C45 1.543(6) . ? C45 C46 1.520(7) . ? C45 C48 1.536(7) . ? C45 C47 1.541(7) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? O17 C49 1.268(5) . ? O18 C49 1.266(6) . ? C49 C50 1.536(6) . ? C50 C52A 1.510(8) . ? C50 C53A 1.517(9) . ? C50 C51B 1.52(3) . ? C50 C53B 1.52(3) . ? C50 C52B 1.52(3) . ? C50 C51A 1.528(9) . ? C51A H51A 0.9800 . ? C51A H51B 0.9800 . ? C51A H51C 0.9800 . ? C52A H52A 0.9800 . ? C52A H52B 0.9800 . ? C52A H52C 0.9800 . ? C53A H53A 0.9800 . ? C53A H53B 0.9800 . ? C53A H53C 0.9800 . ? C51B H51D 0.9800 . ? C51B H51E 0.9800 . ? C51B H51F 0.9800 . ? C52B H52D 0.9800 . ? C52B H52E 0.9800 . ? C52B H52F 0.9800 . ? C53B H53D 0.9800 . ? C53B H53E 0.9800 . ? C53B H53F 0.9800 . ? O19 C54 1.267(6) . ? O20 C54 1.275(7) . ? C54 C55 1.530(7) . ? C55 C56 1.520(8) . ? C55 C57 1.531(8) . ? C55 C58 1.533(8) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? N61A C61 1.212(17) . ? N61B C61 1.013(18) . ? C61 C62A 1.41(2) . ? C61 C62B 1.508(17) . ? N62 C63 1.147(11) . ? C63 C64 1.464(11) . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? N63A C65A 1.111(17) . ? C65A C66A 1.509(16) . ? N63B C65B 1.092(14) . ? C65B C66B 1.483(14) . ? N64A C67A 1.162(14) . ? C67A C68A 1.462(14) . ? N64B C67B 1.156(16) . ? C67B C68B 1.446(16) . ? 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 O1 Y1 O10 85.04(10) . . ? O1 Y1 O17 96.44(11) . . ? O10 Y1 O17 70.12(11) . . ? O1 Y1 O7 76.69(10) . . ? O10 Y1 O7 140.58(10) . . ? O17 Y1 O7 145.71(10) . . ? O1 Y1 O14 79.18(10) . . ? O10 Y1 O14 136.09(11) . . ? O17 Y1 O14 71.31(11) . . ? O7 Y1 O14 74.41(10) . . ? O1 Y1 O6 152.49(11) . . ? O10 Y1 O6 116.41(12) . . ? O17 Y1 O6 76.86(11) . . ? O7 Y1 O6 93.77(11) . . ? O14 Y1 O6 73.39(11) . . ? O1 Y1 O5 76.21(10) . . ? O10 Y1 O5 74.13(10) . . ? O17 Y1 O5 144.00(10) . . ? O7 Y1 O5 67.76(9) . . ? O14 Y1 O5 138.51(10) . . ? O6 Y1 O5 124.41(10) . . ? O1 Y1 N3 140.83(11) . . ? O10 Y1 N3 80.43(12) . . ? O17 Y1 N3 112.11(12) . . ? O7 Y1 N3 92.04(11) . . ? O14 Y1 N3 134.26(11) . . ? O6 Y1 N3 63.99(12) . . ? O5 Y1 N3 64.88(10) . . ? O3 Y2 O16 84.74(11) . . ? O3 Y2 O19 99.19(12) . . ? O16 Y2 O19 70.37(12) . . ? O3 Y2 O12 79.23(11) . . ? O16 Y2 O12 135.18(12) . . ? O19 Y2 O12 71.33(12) . . ? O3 Y2 O5 77.03(9) . . ? O16 Y2 O5 140.33(10) . . ? O19 Y2 O5 146.79(11) . . ? O12 Y2 O5 75.58(10) . . ? O3 Y2 O8 152.47(11) . . ? O16 Y2 O8 117.37(12) . . ? O19 Y2 O8 75.50(13) . . ? O12 Y2 O8 73.47(12) . . ? O5 Y2 O8 92.64(11) . . ? O3 Y2 O7 75.59(10) . . ? O16 Y2 O7 73.91(10) . . ? O19 Y2 O7 144.24(10) . . ? O12 Y2 O7 138.97(10) . . ? O5 Y2 O7 67.58(9) . . ? O8 Y2 O7 124.30(11) . . ? O3 Y2 N4 140.09(12) . . ? O16 Y2 N4 80.09(12) . . ? O19 Y2 N4 109.84(13) . . ? O12 Y2 N4 135.35(12) . . ? O5 Y2 N4 91.70(10) . . ? O8 Y2 N4 64.43(13) . . ? O7 Y2 N4 64.80(11) . . ? O11 Co1 O9 89.37(13) . . ? O11 Co1 O1 174.60(13) . . ? O9 Co1 O1 96.01(12) . . ? O11 Co1 O3 93.32(12) . . ? O9 Co1 O3 174.62(11) . . ? O1 Co1 O3 81.28(12) . . ? O11 Co1 O5 93.47(11) . . ? O9 Co1 O5 91.99(11) . . ? O1 Co1 O5 85.95(10) . . ? O3 Co1 O5 83.20(10) . . ? O11 Co1 N1 102.43(13) . . ? O9 Co1 N1 83.07(13) . . ? O1 Co1 N1 78.70(12) . . ? O3 Co1 N1 100.86(12) . . ? O5 Co1 N1 163.26(12) . . ? O13 Co2 O3 175.00(13) . . ? O13 Co2 O15 89.03(13) . . ? O3 Co2 O15 95.90(12) . . ? O13 Co2 O7 92.97(11) . . ? O3 Co2 O7 85.94(10) . . ? O15 Co2 O7 92.74(11) . . ? O13 Co2 O1 94.32(12) . . ? O3 Co2 O1 80.69(11) . . ? O15 Co2 O1 173.88(11) . . ? O7 Co2 O1 81.99(10) . . ? O13 Co2 N2 101.80(13) . . ? O3 Co2 N2 79.54(12) . . ? O15 Co2 N2 85.24(13) . . ? O7 Co2 N2 165.04(12) . . ? O1 Co2 N2 99.05(12) . . ? C1 N1 C5 118.0(4) . . ? C1 N1 Co1 110.8(3) . . ? C5 N1 Co1 130.5(3) . . ? N1 C1 C2 122.8(4) . . ? N1 C1 C6 117.8(4) . . ? C2 C1 C6 119.3(4) . . ? C3 C2 C1 119.4(5) . . ? C3 C2 H2A 120.3 . . ? C1 C2 H2A 120.3 . . ? C4 C3 C2 117.9(5) . . ? C4 C3 H3A 121.0 . . ? C2 C3 H3A 121.0 . . ? C5 C4 C3 120.2(5) . . ? C5 C4 H4A 119.9 . . ? C3 C4 H4A 119.9 . . ? N1 C5 C4 121.6(5) . . ? N1 C5 C7 118.1(4) . . ? C4 C5 C7 120.3(4) . . ? O1 C6 C1 113.7(3) . . ? O1 C6 H6A 108.8 . . ? C1 C6 H6A 108.8 . . ? O1 C6 H6B 108.8 . . ? C1 C6 H6B 108.8 . . ? H6A C6 H6B 107.7 . . ? C6 O1 Co1 112.8(2) . . ? C6 O1 Co2 117.7(2) . . ? Co1 O1 Co2 98.71(13) . . ? C6 O1 Y1 123.0(3) . . ? Co1 O1 Y1 100.65(11) . . ? Co2 O1 Y1 100.10(10) . . ? O2 C7 C5 111.8(5) . . ? O2 C7 H7A 109.3 . . ? C5 C7 H7A 109.3 . . ? O2 C7 H7B 109.3 . . ? C5 C7 H7B 109.3 . . ? H7A C7 H7B 107.9 . . ? C7 O2 H2 107(6) . . ? C8 N2 C12 119.0(4) . . ? C8 N2 Co2 110.2(3) . . ? C12 N2 Co2 130.8(3) . . ? N2 C8 C9 122.3(4) . . ? N2 C8 C13 117.9(4) . . ? C9 C8 C13 119.7(4) . . ? C8 C9 C10 118.8(5) . . ? C8 C9 H9A 120.6 . . ? C10 C9 H9A 120.6 . . ? C11 C10 C9 118.9(5) . . ? C11 C10 H10A 120.6 . . ? C9 C10 H10A 120.6 . . ? C10 C11 C12 119.4(5) . . ? C10 C11 H11A 120.3 . . ? C12 C11 H11A 120.3 . . ? N2 C12 C11 121.6(5) . . ? N2 C12 C14 118.6(4) . . ? C11 C12 C14 119.7(5) . . ? O3 C13 C8 113.5(4) . . ? O3 C13 H13A 108.9 . . ? C8 C13 H13A 108.9 . . ? O3 C13 H13B 108.9 . . ? C8 C13 H13B 108.9 . . ? H13A C13 H13B 107.7 . . ? C13 O3 Co2 111.9(2) . . ? C13 O3 Co1 115.4(3) . . ? Co2 O3 Co1 99.32(13) . . ? C13 O3 Y2 126.2(3) . . ? Co2 O3 Y2 100.51(10) . . ? Co1 O3 Y2 99.42(10) . . ? O4 C14 C12 111.8(6) . . ? O4 C14 H14A 109.2 . . ? C12 C14 H14A 109.2 . . ? O4 C14 H14B 109.2 . . ? C12 C14 H14B 109.2 . . ? H14A C14 H14B 107.9 . . ? C14 O4 H4 118(6) . . ? C15 N3 C19 119.9(4) . . ? C15 N3 Y1 118.0(3) . . ? C19 N3 Y1 122.1(3) . . ? N3 C15 C16 121.4(4) . . ? N3 C15 C20 116.5(4) . . ? C16 C15 C20 122.0(4) . . ? C15 C16 C17 118.5(5) . . ? C15 C16 H16A 120.7 . . ? C17 C16 H16A 120.7 . . ? C18 C17 C16 119.7(5) . . ? C18 C17 H17A 120.2 . . ? C16 C17 H17A 120.2 . . ? C17 C18 C19 118.9(5) . . ? C17 C18 H18A 120.6 . . ? C19 C18 H18A 120.6 . . ? N3 C19 C18 121.5(5) . . ? N3 C19 C21 116.2(4) . . ? C18 C19 C21 122.2(4) . . ? O5 C20 C15 110.0(3) . . ? O5 C20 H20A 109.7 . . ? C15 C20 H20A 109.7 . . ? O5 C20 H20B 109.7 . . ? C15 C20 H20B 109.7 . . ? H20A C20 H20B 108.2 . . ? C20 O5 Co1 121.3(2) . . ? C20 O5 Y2 115.1(2) . . ? Co1 O5 Y2 96.66(10) . . ? C20 O5 Y1 115.7(2) . . ? Co1 O5 Y1 92.31(9) . . ? Y2 O5 Y1 112.43(11) . . ? O6 C21 C19 110.2(4) . . ? O6 C21 H21A 109.6 . . ? C19 C21 H21A 109.6 . . ? O6 C21 H21B 109.6 . . ? C19 C21 H21B 109.6 . . ? H21A C21 H21B 108.1 . . ? C21 O6 Y1 126.2(3) . . ? C21 O6 H6 109(3) . . ? Y1 O6 H6 101(3) . . ? C22 N4 C26 118.9(4) . . ? C22 N4 Y2 118.6(3) . . ? C26 N4 Y2 122.5(3) . . ? N4 C22 C23 122.3(5) . . ? N4 C22 C27 116.3(4) . . ? C23 C22 C27 121.4(5) . . ? C24 C23 C22 117.9(6) . . ? C24 C23 H23A 121.0 . . ? C22 C23 H23A 121.0 . . ? C25 C24 C23 120.0(5) . . ? C25 C24 H24A 120.0 . . ? C23 C24 H24A 120.0 . . ? C24 C25 C26 118.7(5) . . ? C24 C25 H25A 120.7 . . ? C26 C25 H25A 120.7 . . ? N4 C26 C25 122.2(5) . . ? N4 C26 C28 115.8(4) . . ? C25 C26 C28 122.0(5) . . ? O7 C27 C22 111.0(4) . . ? O7 C27 H27A 109.4 . . ? C22 C27 H27A 109.4 . . ? O7 C27 H27B 109.4 . . ? C22 C27 H27B 109.4 . . ? H27A C27 H27B 108.0 . . ? C27 O7 Co2 121.3(2) . . ? C27 O7 Y1 114.8(2) . . ? Co2 O7 Y1 97.57(10) . . ? C27 O7 Y2 115.3(2) . . ? Co2 O7 Y2 92.74(10) . . ? Y1 O7 Y2 112.20(10) . . ? O8 C28 C26 111.2(4) . . ? O8 C28 H28A 109.4 . . ? C26 C28 H28A 109.4 . . ? O8 C28 H28B 109.4 . . ? C26 C28 H28B 109.4 . . ? H28A C28 H28B 108.0 . . ? C28 O8 Y2 124.7(3) . . ? C28 O8 H8 106(3) . . ? Y2 O8 H8 110(3) . . ? C29 O9 Co1 126.0(3) . . ? C29 O10 Y1 137.3(3) . . ? O10 C29 O9 124.5(4) . . ? O10 C29 C30 118.1(4) . . ? O9 C29 C30 117.4(4) . . ? C31 C30 C29 108.9(4) . . ? C31 C30 C32 111.1(5) . . ? C29 C30 C32 110.5(4) . . ? C31 C30 C33 110.8(6) . . ? C29 C30 C33 106.4(5) . . ? C32 C30 C33 109.1(5) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C30 C33 H33A 109.5 . . ? C30 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C34 O11 Co1 124.8(3) . . ? C34 O12 Y2 139.5(3) . . ? O12 C34 O11 123.7(4) . . ? O12 C34 C35 119.9(4) . . ? O11 C34 C35 116.5(4) . . ? C36 C35 C34 110.5(4) . . ? C36 C35 C38 111.4(5) . . ? C34 C35 C38 109.2(4) . . ? C36 C35 C37 109.6(5) . . ? C34 C35 C37 106.1(4) . . ? C38 C35 C37 110.0(5) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C39 O13 Co2 124.4(3) . . ? C39 O14 Y1 139.8(3) . . ? O14 C39 O13 123.5(4) . . ? O14 C39 C40 119.6(4) . . ? O13 C39 C40 116.9(4) . . ? C41 C40 C42 110.2(4) . . ? C41 C40 C39 111.1(4) . . ? C42 C40 C39 107.5(4) . . ? C41 C40 C43 110.3(5) . . ? C42 C40 C43 109.4(5) . . ? C39 C40 C43 108.2(4) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C40 C43 H43A 109.5 . . ? C40 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C40 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C44 O15 Co2 123.9(3) . . ? C44 O16 Y2 139.5(3) . . ? O16 C44 O15 124.5(4) . . ? O16 C44 C45 117.1(4) . . ? O15 C44 C45 118.4(4) . . ? C46 C45 C48 110.8(4) . . ? C46 C45 C47 109.6(4) . . ? C48 C45 C47 109.7(4) . . ? C46 C45 C44 111.2(4) . . ? C48 C45 C44 108.5(4) . . ? C47 C45 C44 107.0(4) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C45 C48 H48A 109.5 . . ? C45 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C45 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C49 O17 Y1 133.9(3) . . ? O18 C49 O17 123.3(4) . . ? O18 C49 C50 119.2(4) . . ? O17 C49 C50 117.5(4) . . ? C52A C50 C53A 110.9(6) . . ? C51B C50 C53B 103.6(15) . . ? C51B C50 C52B 103.3(15) . . ? C53B C50 C52B 103.5(15) . . ? C52A C50 C51A 110.0(6) . . ? C53A C50 C51A 111.4(7) . . ? C52A C50 C49 109.2(4) . . ? C53A C50 C49 106.4(4) . . ? C51B C50 C49 117.1(17) . . ? C53B C50 C49 111.8(18) . . ? C52B C50 C49 115.9(19) . . ? C51A C50 C49 108.9(5) . . ? C50 C51A H51A 109.5 . . ? C50 C51A H51B 109.5 . . ? H51A C51A H51B 109.5 . . ? C50 C51A H51C 109.5 . . ? H51A C51A H51C 109.5 . . ? H51B C51A H51C 109.5 . . ? C50 C52A H52A 109.5 . . ? C50 C52A H52B 109.5 . . ? H52A C52A H52B 109.5 . . ? C50 C52A H52C 109.5 . . ? H52A C52A H52C 109.5 . . ? H52B C52A H52C 109.5 . . ? C50 C53A H53A 109.5 . . ? C50 C53A H53B 109.5 . . ? H53A C53A H53B 109.5 . . ? C50 C53A H53C 109.5 . . ? H53A C53A H53C 109.5 . . ? H53B C53A H53C 109.5 . . ? C50 C51B H51D 109.5 . . ? C50 C51B H51E 109.5 . . ? H51D C51B H51E 109.5 . . ? C50 C51B H51F 109.5 . . ? H51D C51B H51F 109.5 . . ? H51E C51B H51F 109.5 . . ? C50 C52B H52D 109.5 . . ? C50 C52B H52E 109.5 . . ? H52D C52B H52E 109.5 . . ? C50 C52B H52F 109.5 . . ? H52D C52B H52F 109.5 . . ? H52E C52B H52F 109.5 . . ? C50 C53B H53D 109.5 . . ? C50 C53B H53E 109.5 . . ? H53D C53B H53E 109.5 . . ? C50 C53B H53F 109.5 . . ? H53D C53B H53F 109.5 . . ? H53E C53B H53F 109.5 . . ? C54 O19 Y2 136.9(3) . . ? O19 C54 O20 122.7(5) . . ? O19 C54 C55 117.6(5) . . ? O20 C54 C55 119.7(4) . . ? C56 C55 C54 106.2(4) . . ? C56 C55 C57 109.9(5) . . ? C54 C55 C57 108.9(4) . . ? C56 C55 C58 112.3(6) . . ? C54 C55 C58 110.2(5) . . ? C57 C55 C58 109.3(6) . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C55 C57 H57A 109.5 . . ? C55 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C55 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C55 C58 H58A 109.5 . . ? C55 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C55 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? N61A C61 C62A 161.7(14) . . ? N61B C61 C62B 158.6(16) . . ? N62 C63 C64 177.4(11) . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? N63A C65A C66A 162(4) . . ? N63B C65B C66B 173.9(18) . . ? N64A C67A C68A 167(2) . . ? N64B C67B C68B 164(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2 O11 0.90(4) 1.92(6) 2.744(5) 150(8) . O4 H4 O13 0.94(4) 2.05(8) 2.771(5) 132(8) . O6 H6 O18 0.97(3) 1.57(3) 2.530(5) 174(5) . O8 H8 O20 0.99(3) 1.57(4) 2.509(5) 158(5) . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.314 _refine_diff_density_min -1.227 _refine_diff_density_rms 0.118 ########################################################## data_zhao10 _database_code_depnum_ccdc_archive 'CCDC 756451' #TrackingRef 'co2ln2_a1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C58 H86 Co2 Gd2 N4 O20, 4(C2 H3 N)' _chemical_formula_sum 'C66 H98 Co2 Gd2 N8 O20' _chemical_formula_weight 1755.88 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' Co Co 0.3494 0.9721 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.5754(5) _cell_length_b 18.7803(6) _cell_length_c 26.9225(8) _cell_angle_alpha 90.00 _cell_angle_beta 100.538(1) _cell_angle_gamma 90.00 _cell_volume 7742.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 13772 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 28.14 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.31 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.506 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3568 _exptl_absorpt_coefficient_mu 2.183 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.449 _exptl_absorpt_correction_T_max 0.558 _exptl_absorpt_process_details 'SADABS 2.10 (Bruker AXS Inc., 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART Apex' _diffrn_measurement_method 'CCD area detector' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53002 _diffrn_reflns_av_R_equivalents 0.0179 _diffrn_reflns_av_sigmaI/netI 0.0183 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 28.16 _reflns_number_total 17546 _reflns_number_gt 16409 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT 5.6 (Bruker AXS Inc., 2005)' _computing_cell_refinement 'SMART-NT 5.6 (Bruker AXS Inc., 2005)' _computing_data_reduction 'SAINT+ 6.45 (Bruker AXS Inc., 2003)' _computing_structure_solution 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_structure_refinement 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_molecular_graphics 'Diamond 2.1 (Crystal Impact, 1998)' _computing_publication_material 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _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. Two lattice MeCN were twofold disordered and refined using half-occupancy atoms with geometrical restraints. ; _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^)+(0.0303P)^2^+11.2342P] 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 17546 _refine_ls_number_parameters 901 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0310 _refine_ls_R_factor_gt 0.0284 _refine_ls_wR_factor_ref 0.0697 _refine_ls_wR_factor_gt 0.0683 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.091 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.421019(7) 0.193180(6) 0.292060(4) 0.01801(3) Uani 1 1 d . . . Gd2 Gd 0.620649(8) 0.207889(6) 0.215319(4) 0.02024(4) Uani 1 1 d . . . Co1 Co 0.43501(2) 0.311287(17) 0.199266(11) 0.01771(7) Uani 1 1 d . . . Co2 Co 0.57792(2) 0.325735(18) 0.303256(12) 0.01919(7) Uani 1 1 d . . . N1 N 0.38951(14) 0.42022(11) 0.20931(8) 0.0227(4) Uani 1 1 d . . . C1 C 0.36515(16) 0.42732(13) 0.25430(9) 0.0234(5) Uani 1 1 d . . . C2 C 0.32361(18) 0.48775(15) 0.26841(11) 0.0301(6) Uani 1 1 d . . . H2A H 0.3084 0.4910 0.3009 0.036 Uiso 1 1 calc R . . C3 C 0.3050(2) 0.54272(16) 0.23422(12) 0.0365(7) Uani 1 1 d . . . H3A H 0.2764 0.5845 0.2426 0.044 Uiso 1 1 calc R . . C4 C 0.32883(19) 0.53581(15) 0.18746(11) 0.0338(6) Uani 1 1 d . . . H4A H 0.3165 0.5730 0.1633 0.041 Uiso 1 1 calc R . . C5 C 0.37081(18) 0.47456(14) 0.17574(10) 0.0286(5) Uani 1 1 d . . . C6 C 0.38172(17) 0.36544(13) 0.29076(9) 0.0239(5) Uani 1 1 d . . . H6A H 0.4072 0.3837 0.3248 0.029 Uiso 1 1 calc R . . H6B H 0.3253 0.3425 0.2930 0.029 Uiso 1 1 calc R . . O1 O 0.43855(11) 0.31397(8) 0.27629(6) 0.0195(3) Uani 1 1 d . . . C7 C 0.3949(2) 0.46595(17) 0.12419(11) 0.0392(7) Uani 1 1 d . . . H7A H 0.3955 0.5133 0.1080 0.047 Uiso 1 1 calc R . . H7B H 0.4545 0.4457 0.1280 0.047 Uiso 1 1 calc R . . O2 O 0.33520(18) 0.42073(13) 0.09264(8) 0.0486(6) Uani 1 1 d D . . H2 H 0.352(3) 0.3791(18) 0.1002(17) 0.073 Uiso 1 1 d D . . N2 N 0.58876(14) 0.43984(11) 0.28846(8) 0.0241(4) Uani 1 1 d . . . C8 C 0.60104(17) 0.45081(14) 0.24110(10) 0.0257(5) Uani 1 1 d . . . C9 C 0.6100(2) 0.51862(16) 0.22156(12) 0.0404(7) Uani 1 1 d . . . H9A H 0.6178 0.5246 0.1876 0.048 Uiso 1 1 calc R . . C10 C 0.6072(3) 0.57693(16) 0.25262(13) 0.0483(9) Uani 1 1 d . . . H10A H 0.6128 0.6238 0.2403 0.058 Uiso 1 1 calc R . . C11 C 0.5962(2) 0.56612(16) 0.30160(12) 0.0399(7) Uani 1 1 d . . . H11A H 0.5950 0.6056 0.3235 0.048 Uiso 1 1 calc R . . C12 C 0.58706(19) 0.49737(15) 0.31891(11) 0.0309(6) Uani 1 1 d . . . C13 C 0.61070(17) 0.38582(13) 0.20912(9) 0.0228(5) Uani 1 1 d . . . H13A H 0.5828 0.3955 0.1737 0.027 Uiso 1 1 calc R . . H13B H 0.6735 0.3769 0.2098 0.027 Uiso 1 1 calc R . . O3 O 0.57292(11) 0.32470(9) 0.22601(6) 0.0200(3) Uani 1 1 d . . . C14 C 0.5797(3) 0.48436(17) 0.37305(11) 0.0456(8) Uani 1 1 d . . . H14A H 0.5697 0.5302 0.3892 0.055 Uiso 1 1 calc R . . H14B H 0.5288 0.4533 0.3742 0.055 Uiso 1 1 calc R . . O4 O 0.6558(2) 0.45197(13) 0.40053(9) 0.0632(8) Uani 1 1 d D . . H4 H 0.656(4) 0.4056(18) 0.3971(19) 0.095 Uiso 1 1 d D . . N3 N 0.42405(14) 0.07492(11) 0.24858(8) 0.0257(4) Uani 1 1 d . . . C15 C 0.42244(17) 0.07480(14) 0.19833(10) 0.0261(5) Uani 1 1 d . . . C16 C 0.4172(2) 0.01182(15) 0.17081(12) 0.0352(6) Uani 1 1 d . . . H16A H 0.4142 0.0124 0.1352 0.042 Uiso 1 1 calc R . . C17 C 0.4165(2) -0.05206(16) 0.19678(14) 0.0454(8) Uani 1 1 d . . . H17A H 0.4126 -0.0959 0.1789 0.054 Uiso 1 1 calc R . . C18 C 0.4214(2) -0.05199(16) 0.24853(13) 0.0417(7) Uani 1 1 d . . . H18A H 0.4232 -0.0955 0.2667 0.050 Uiso 1 1 calc R . . C19 C 0.42382(18) 0.01284(14) 0.27337(12) 0.0318(6) Uani 1 1 d . . . C20 C 0.42579(17) 0.14675(13) 0.17348(9) 0.0237(5) Uani 1 1 d . . . H20A H 0.4590 0.1428 0.1455 0.028 Uiso 1 1 calc R . . H20B H 0.3658 0.1625 0.1590 0.028 Uiso 1 1 calc R . . O5 O 0.46607(11) 0.19768(8) 0.20891(6) 0.0187(3) Uani 1 1 d . . . C21 C 0.4251(2) 0.01731(15) 0.32920(12) 0.0348(6) Uani 1 1 d . . . H21A H 0.3693 -0.0010 0.3367 0.042 Uiso 1 1 calc R . . H21B H 0.4729 -0.0128 0.3474 0.042 Uiso 1 1 calc R . . O6 O 0.43754(14) 0.08853(10) 0.34628(7) 0.0311(4) Uani 1 1 d D . . H6 H 0.398(2) 0.0976(18) 0.3647(12) 0.037 Uiso 1 1 d D . . N4 N 0.64449(14) 0.09422(12) 0.26496(9) 0.0284(5) Uani 1 1 d . . . C22 C 0.64513(17) 0.09648(15) 0.31472(11) 0.0304(6) Uani 1 1 d . . . C23 C 0.6615(2) 0.03640(18) 0.34523(13) 0.0434(8) Uani 1 1 d . . . H23A H 0.6622 0.0392 0.3805 0.052 Uiso 1 1 calc R . . C24 C 0.6767(3) -0.02735(19) 0.32283(16) 0.0547(10) Uani 1 1 d . . . H24A H 0.6884 -0.0692 0.3428 0.066 Uiso 1 1 calc R . . C25 C 0.6748(2) -0.03020(17) 0.27184(14) 0.0450(8) Uani 1 1 d . . . H25A H 0.6846 -0.0740 0.2561 0.054 Uiso 1 1 calc R . . C26 C 0.65842(18) 0.03174(15) 0.24343(12) 0.0334(6) Uani 1 1 d . . . C27 C 0.62581(17) 0.16741(14) 0.33588(10) 0.0258(5) Uani 1 1 d . . . H27A H 0.5940 0.1601 0.3641 0.031 Uiso 1 1 calc R . . H27B H 0.6813 0.1921 0.3494 0.031 Uiso 1 1 calc R . . O7 O 0.57503(11) 0.21026(9) 0.29844(6) 0.0197(3) Uani 1 1 d . . . C28 C 0.6553(2) 0.03233(16) 0.18723(12) 0.0381(7) Uani 1 1 d . . . H28A H 0.7135 0.0195 0.1801 0.046 Uiso 1 1 calc R . . H28B H 0.6129 -0.0038 0.1711 0.046 Uiso 1 1 calc R . . O8 O 0.63075(15) 0.10012(11) 0.16641(8) 0.0354(5) Uani 1 1 d D . . H8 H 0.666(2) 0.1115(19) 0.1441(12) 0.042 Uiso 1 1 d D . . O9 O 0.30419(12) 0.29111(10) 0.17790(7) 0.0257(4) Uani 1 1 d . . . O10 O 0.29148(12) 0.20313(10) 0.23184(7) 0.0245(4) Uani 1 1 d . . . C29 C 0.26102(16) 0.24416(14) 0.19577(9) 0.0230(5) Uani 1 1 d . . . C30 C 0.16484(18) 0.23498(19) 0.17171(11) 0.0395(7) Uani 1 1 d . . . C31 C 0.1111(2) 0.2295(3) 0.21412(15) 0.0644(13) Uani 1 1 d . . . H31A H 0.1159 0.2742 0.2332 0.097 Uiso 1 1 calc R . . H31B H 0.1335 0.1902 0.2368 0.097 Uiso 1 1 calc R . . H31C H 0.0498 0.2206 0.1994 0.097 Uiso 1 1 calc R . . C32 C 0.1338(2) 0.2970(2) 0.13599(14) 0.0558(11) Uani 1 1 d . . . H32A H 0.1380 0.3415 0.1553 0.084 Uiso 1 1 calc R . . H32B H 0.0729 0.2890 0.1197 0.084 Uiso 1 1 calc R . . H32C H 0.1705 0.3001 0.1101 0.084 Uiso 1 1 calc R . . C33 C 0.1572(3) 0.1654(2) 0.14148(15) 0.0698(14) Uani 1 1 d . . . H33A H 0.0962 0.1576 0.1255 0.105 Uiso 1 1 calc R . . H33B H 0.1773 0.1256 0.1642 0.105 Uiso 1 1 calc R . . H33C H 0.1934 0.1684 0.1153 0.105 Uiso 1 1 calc R . . O11 O 0.44594(12) 0.31066(10) 0.12526(6) 0.0249(4) Uani 1 1 d . . . O12 O 0.56155(12) 0.23979(10) 0.12973(6) 0.0269(4) Uani 1 1 d . . . C34 C 0.49629(17) 0.27040(14) 0.10554(9) 0.0238(5) Uani 1 1 d . . . C35 C 0.47346(19) 0.26114(17) 0.04762(10) 0.0322(6) Uani 1 1 d . . . C36 C 0.5260(2) 0.19975(19) 0.03069(11) 0.0412(7) Uani 1 1 d . . . H36A H 0.5114 0.1949 -0.0061 0.062 Uiso 1 1 calc R . . H36B H 0.5118 0.1554 0.0466 0.062 Uiso 1 1 calc R . . H36C H 0.5886 0.2097 0.0408 0.062 Uiso 1 1 calc R . . C37 C 0.4965(2) 0.3314(2) 0.02413(11) 0.0449(8) Uani 1 1 d . . . H37A H 0.4624 0.3702 0.0352 0.067 Uiso 1 1 calc R . . H37B H 0.4829 0.3276 -0.0128 0.067 Uiso 1 1 calc R . . H37C H 0.5589 0.3412 0.0349 0.067 Uiso 1 1 calc R . . C38 C 0.3758(2) 0.2459(2) 0.03215(13) 0.0516(9) Uani 1 1 d . . . H38A H 0.3424 0.2856 0.0427 0.077 Uiso 1 1 calc R . . H38B H 0.3614 0.2020 0.0485 0.077 Uiso 1 1 calc R . . H38C H 0.3610 0.2404 -0.0046 0.077 Uiso 1 1 calc R . . O13 O 0.56877(13) 0.32496(10) 0.37722(6) 0.0271(4) Uani 1 1 d . . . O14 O 0.47197(12) 0.23715(10) 0.37634(6) 0.0253(4) Uani 1 1 d . . . C39 C 0.53007(17) 0.27735(14) 0.39889(9) 0.0239(5) Uani 1 1 d . . . C40 C 0.55879(18) 0.27025(16) 0.45663(9) 0.0295(6) Uani 1 1 d . . . C41 C 0.5223(2) 0.20196(17) 0.47544(11) 0.0373(7) Uani 1 1 d . . . H41A H 0.4584 0.2030 0.4672 0.056 Uiso 1 1 calc R . . H41B H 0.5412 0.1982 0.5121 0.056 Uiso 1 1 calc R . . H41C H 0.5440 0.1608 0.4590 0.056 Uiso 1 1 calc R . . C42 C 0.5239(2) 0.33537(18) 0.48062(10) 0.0374(7) Uani 1 1 d . . . H42A H 0.4599 0.3358 0.4722 0.056 Uiso 1 1 calc R . . H42B H 0.5468 0.3788 0.4676 0.056 Uiso 1 1 calc R . . H42C H 0.5424 0.3333 0.5174 0.056 Uiso 1 1 calc R . . C43 C 0.6586(2) 0.2700(2) 0.46972(12) 0.0496(9) Uani 1 1 d . . . H43A H 0.6773 0.2653 0.5064 0.074 Uiso 1 1 calc R . . H43B H 0.6812 0.3146 0.4584 0.074 Uiso 1 1 calc R . . H43C H 0.6813 0.2298 0.4528 0.074 Uiso 1 1 calc R . . O15 O 0.71342(12) 0.32791(10) 0.32476(7) 0.0284(4) Uani 1 1 d . . . O16 O 0.74382(12) 0.24147(11) 0.27422(7) 0.0308(4) Uani 1 1 d . . . C44 C 0.76458(17) 0.28421(15) 0.31040(10) 0.0260(5) Uani 1 1 d . . . C45 C 0.85990(18) 0.28082(16) 0.33850(11) 0.0303(6) Uani 1 1 d . . . C46 C 0.8788(2) 0.33916(17) 0.37889(12) 0.0406(7) Uani 1 1 d . . . H46A H 0.8698 0.3860 0.3627 0.061 Uiso 1 1 calc R . . H46B H 0.9394 0.3351 0.3967 0.061 Uiso 1 1 calc R . . H46C H 0.8393 0.3337 0.4031 0.061 Uiso 1 1 calc R . . C47 C 0.8744(2) 0.20736(16) 0.36418(12) 0.0351(6) Uani 1 1 d . . . H47A H 0.8623 0.1699 0.3385 0.053 Uiso 1 1 calc R . . H47B H 0.8350 0.2020 0.3885 0.053 Uiso 1 1 calc R . . H47C H 0.9350 0.2035 0.3819 0.053 Uiso 1 1 calc R . . C48 C 0.91968(19) 0.2886(2) 0.29944(12) 0.0413(7) Uani 1 1 d . . . H48A H 0.9063 0.2510 0.2740 0.062 Uiso 1 1 calc R . . H48B H 0.9808 0.2846 0.3164 0.062 Uiso 1 1 calc R . . H48C H 0.9101 0.3352 0.2830 0.062 Uiso 1 1 calc R . . O17 O 0.30111(12) 0.19948(10) 0.33377(7) 0.0264(4) Uani 1 1 d . . . O18 O 0.32661(13) 0.12605(10) 0.39971(7) 0.0321(4) Uani 1 1 d . . . C49 C 0.28916(16) 0.17877(14) 0.37665(10) 0.0245(5) Uani 1 1 d . . . C50 C 0.22410(18) 0.22182(16) 0.40147(10) 0.0291(6) Uani 1 1 d . . . C51 C 0.1933(3) 0.1771(2) 0.44186(16) 0.0686(13) Uani 1 1 d . . . H51A H 0.1520 0.2047 0.4576 0.103 Uiso 1 1 calc R . . H51B H 0.2435 0.1636 0.4676 0.103 Uiso 1 1 calc R . . H51C H 0.1643 0.1340 0.4264 0.103 Uiso 1 1 calc R . . C52 C 0.1466(3) 0.2425(3) 0.36196(14) 0.0694(14) Uani 1 1 d . . . H52A H 0.1050 0.2695 0.3778 0.104 Uiso 1 1 calc R . . H52B H 0.1181 0.1995 0.3462 0.104 Uiso 1 1 calc R . . H52C H 0.1662 0.2720 0.3361 0.104 Uiso 1 1 calc R . . C53 C 0.2715(3) 0.2865(3) 0.4244(2) 0.0833(18) Uani 1 1 d . . . H53A H 0.2324 0.3152 0.4410 0.125 Uiso 1 1 calc R . . H53B H 0.2909 0.3147 0.3979 0.125 Uiso 1 1 calc R . . H53C H 0.3224 0.2719 0.4494 0.125 Uiso 1 1 calc R . . O19 O 0.73757(13) 0.22771(12) 0.17345(7) 0.0339(4) Uani 1 1 d . . . O20 O 0.73617(15) 0.14685(12) 0.11307(8) 0.0412(5) Uani 1 1 d . . . C54 C 0.75924(18) 0.20594(16) 0.13346(11) 0.0315(6) Uani 1 1 d . . . C55 C 0.8164(2) 0.25604(17) 0.10834(11) 0.0364(7) Uani 1 1 d . . . C56 C 0.7564(2) 0.31512(18) 0.08284(13) 0.0445(8) Uani 1 1 d . . . H56A H 0.7288 0.3392 0.1081 0.067 Uiso 1 1 calc R . . H56B H 0.7112 0.2944 0.0567 0.067 Uiso 1 1 calc R . . H56C H 0.7907 0.3496 0.0674 0.067 Uiso 1 1 calc R . . C57 C 0.8864(2) 0.2893(2) 0.14898(15) 0.0561(11) Uani 1 1 d . . . H57A H 0.9250 0.2518 0.1657 0.084 Uiso 1 1 calc R . . H57B H 0.8583 0.3137 0.1740 0.084 Uiso 1 1 calc R . . H57C H 0.9206 0.3236 0.1333 0.084 Uiso 1 1 calc R . . C58 C 0.8593(4) 0.2164(2) 0.0700(2) 0.0852(18) Uani 1 1 d . . . H58A H 0.8968 0.1785 0.0871 0.128 Uiso 1 1 calc R . . H58B H 0.8946 0.2496 0.0541 0.128 Uiso 1 1 calc R . . H58C H 0.8141 0.1954 0.0440 0.128 Uiso 1 1 calc R . . N61 N 0.4140(4) 0.4730(3) -0.08782(16) 0.109(2) Uani 1 1 d D . . C61 C 0.3848(3) 0.4887(2) -0.05513(14) 0.0610(11) Uani 1 1 d D . . C62 C 0.3497(3) 0.5111(3) -0.01195(17) 0.0736(13) Uani 1 1 d D . . H62A H 0.3922 0.5416 0.0095 0.110 Uiso 1 1 calc R . . H62B H 0.3375 0.4692 0.0073 0.110 Uiso 1 1 calc R . . H62C H 0.2956 0.5377 -0.0232 0.110 Uiso 1 1 calc R . . N62 N 0.4017(3) 0.0287(3) 0.54762(17) 0.0990(16) Uani 1 1 d . . . C63 C 0.3868(3) 0.0044(3) 0.50735(18) 0.0668(12) Uani 1 1 d . . . C64 C 0.3701(3) -0.0261(2) 0.45578(15) 0.0609(10) Uani 1 1 d . . . H64A H 0.4242 -0.0468 0.4485 0.091 Uiso 1 1 calc R . . H64B H 0.3499 0.0116 0.4312 0.091 Uiso 1 1 calc R . . H64C H 0.3253 -0.0632 0.4535 0.091 Uiso 1 1 calc R . . N63 N 0.3578(5) 0.4818(3) 0.4013(2) 0.153(3) Uani 1 1 d . . . C65 C 0.3499(4) 0.4783(3) 0.44093(17) 0.0730(13) Uani 1 1 d . . . C66 C 0.3406(4) 0.4705(3) 0.49169(18) 0.0828(15) Uani 1 1 d . . . H66A H 0.2999 0.4316 0.4944 0.124 Uiso 1 1 calc R . . H66B H 0.3178 0.5149 0.5034 0.124 Uiso 1 1 calc R . . H66C H 0.3975 0.4598 0.5125 0.124 Uiso 1 1 calc R . . N64A N 0.5879(6) 0.0413(5) -0.0468(3) 0.083(2) Uiso 0.50 1 d PD A 1 C67A C 0.6069(6) 0.0281(5) -0.0052(3) 0.055(2) Uiso 0.50 1 d PD A 1 C68A C 0.630(3) 0.012(2) 0.0483(5) 0.064(3) Uani 0.50 1 d PD A 1 H68A H 0.6939 0.0091 0.0579 0.096 Uiso 0.50 1 calc PR A 1 H68B H 0.6038 -0.0328 0.0555 0.096 Uiso 0.50 1 calc PR A 1 H68C H 0.6089 0.0506 0.0677 0.096 Uiso 0.50 1 calc PR A 1 N64B N 0.5924(6) -0.0132(6) -0.0423(3) 0.091(3) Uiso 0.50 1 d PD B 2 C67B C 0.6138(6) -0.0054(5) 0.0004(3) 0.058(2) Uiso 0.50 1 d PD B 2 C68B C 0.640(3) 0.011(2) 0.0534(5) 0.064(3) Uani 0.50 1 d PD B 2 H68D H 0.6654 0.0594 0.0569 0.096 Uiso 0.50 1 calc PR B 2 H68E H 0.6844 -0.0232 0.0690 0.096 Uiso 0.50 1 calc PR B 2 H68F H 0.5897 0.0091 0.0701 0.096 Uiso 0.50 1 calc PR B 2 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 0.01888(6) 0.01736(6) 0.01782(6) 0.00263(4) 0.00345(4) 0.00044(4) Gd2 0.01872(6) 0.02262(6) 0.01908(6) -0.00027(4) 0.00269(4) 0.00077(4) Co1 0.01909(15) 0.01845(15) 0.01536(14) 0.00170(11) 0.00253(12) 0.00022(12) Co2 0.02132(16) 0.02036(16) 0.01532(14) -0.00011(11) 0.00182(12) -0.00114(12) N1 0.0227(10) 0.0205(10) 0.0249(10) 0.0040(8) 0.0040(8) 0.0022(8) C1 0.0208(11) 0.0222(12) 0.0261(12) 0.0021(10) 0.0015(10) 0.0017(9) C2 0.0299(14) 0.0275(13) 0.0346(14) 0.0010(11) 0.0103(11) 0.0060(11) C3 0.0323(15) 0.0283(14) 0.0493(18) 0.0031(12) 0.0082(13) 0.0111(12) C4 0.0343(15) 0.0252(14) 0.0406(16) 0.0101(12) 0.0031(12) 0.0069(11) C5 0.0292(13) 0.0248(13) 0.0313(13) 0.0085(10) 0.0040(11) 0.0039(11) C6 0.0307(13) 0.0198(12) 0.0224(12) 0.0008(9) 0.0081(10) 0.0067(10) O1 0.0234(8) 0.0160(8) 0.0180(8) -0.0006(6) 0.0013(7) 0.0035(6) C7 0.0530(19) 0.0341(16) 0.0319(15) 0.0136(12) 0.0114(14) 0.0117(14) O2 0.0671(16) 0.0455(14) 0.0284(11) 0.0071(10) -0.0043(11) 0.0195(12) N2 0.0255(11) 0.0224(10) 0.0232(10) -0.0023(8) 0.0015(8) -0.0025(8) C8 0.0276(13) 0.0220(12) 0.0276(13) -0.0011(10) 0.0050(10) -0.0048(10) C9 0.061(2) 0.0266(15) 0.0355(15) 0.0028(12) 0.0150(15) -0.0055(14) C10 0.078(3) 0.0197(14) 0.0496(19) 0.0025(13) 0.0196(18) -0.0049(15) C11 0.055(2) 0.0224(14) 0.0428(17) -0.0073(12) 0.0114(15) -0.0044(13) C12 0.0373(15) 0.0243(13) 0.0306(14) -0.0048(11) 0.0048(12) -0.0033(11) C13 0.0267(12) 0.0210(12) 0.0221(11) -0.0002(9) 0.0077(10) -0.0062(10) O3 0.0241(8) 0.0170(8) 0.0162(8) 0.0019(6) -0.0033(6) -0.0062(7) C14 0.078(3) 0.0295(15) 0.0303(15) -0.0095(12) 0.0128(16) -0.0078(16) O4 0.105(2) 0.0354(13) 0.0367(13) -0.0065(10) -0.0202(14) -0.0111(14) N3 0.0245(11) 0.0208(10) 0.0330(12) -0.0007(9) 0.0084(9) -0.0013(8) C15 0.0236(12) 0.0211(12) 0.0345(14) -0.0046(10) 0.0080(10) -0.0011(10) C16 0.0374(15) 0.0269(14) 0.0427(16) -0.0110(12) 0.0105(13) -0.0041(12) C17 0.053(2) 0.0221(14) 0.065(2) -0.0106(14) 0.0203(17) -0.0039(13) C18 0.0486(19) 0.0205(14) 0.060(2) 0.0013(13) 0.0208(16) 0.0004(13) C19 0.0295(14) 0.0216(13) 0.0462(16) 0.0039(11) 0.0116(12) 0.0021(11) C20 0.0256(12) 0.0236(12) 0.0216(11) -0.0056(9) 0.0035(10) -0.0034(10) O5 0.0204(8) 0.0182(8) 0.0170(8) -0.0012(6) 0.0023(6) 0.0007(6) C21 0.0390(16) 0.0215(13) 0.0477(17) 0.0097(12) 0.0178(13) 0.0048(11) O6 0.0391(11) 0.0228(9) 0.0341(10) 0.0079(8) 0.0139(9) 0.0057(8) N4 0.0198(10) 0.0254(11) 0.0400(13) 0.0039(9) 0.0054(9) 0.0047(9) C22 0.0224(12) 0.0301(14) 0.0385(15) 0.0096(11) 0.0049(11) 0.0052(11) C23 0.0432(18) 0.0397(17) 0.0474(18) 0.0180(14) 0.0081(15) 0.0137(14) C24 0.056(2) 0.0364(18) 0.072(3) 0.0246(17) 0.0131(19) 0.0211(16) C25 0.0402(17) 0.0275(15) 0.068(2) 0.0069(15) 0.0118(16) 0.0135(13) C26 0.0248(13) 0.0260(14) 0.0495(17) 0.0008(12) 0.0068(12) 0.0051(11) C27 0.0214(12) 0.0305(13) 0.0247(12) 0.0102(10) 0.0019(10) 0.0030(10) O7 0.0186(8) 0.0218(8) 0.0181(8) 0.0026(6) 0.0015(6) 0.0011(6) C28 0.0372(16) 0.0255(14) 0.0542(19) -0.0048(13) 0.0154(14) 0.0051(12) O8 0.0438(12) 0.0279(10) 0.0366(11) -0.0038(8) 0.0134(9) 0.0031(9) O9 0.0221(9) 0.0263(9) 0.0276(9) 0.0039(7) 0.0017(7) 0.0008(7) O10 0.0209(9) 0.0300(10) 0.0220(9) 0.0024(7) 0.0020(7) -0.0016(7) C29 0.0195(11) 0.0278(13) 0.0214(11) -0.0017(9) 0.0032(9) 0.0001(10) C30 0.0204(13) 0.062(2) 0.0330(15) 0.0170(14) -0.0029(11) -0.0089(13) C31 0.0230(15) 0.114(4) 0.058(2) 0.045(2) 0.0120(15) 0.0086(19) C32 0.0239(15) 0.092(3) 0.049(2) 0.036(2) -0.0007(14) 0.0058(17) C33 0.073(3) 0.081(3) 0.044(2) 0.006(2) -0.0199(19) -0.045(2) O11 0.0283(9) 0.0291(9) 0.0175(8) 0.0018(7) 0.0049(7) 0.0024(7) O12 0.0256(9) 0.0350(10) 0.0203(8) 0.0001(7) 0.0050(7) 0.0022(8) C34 0.0238(12) 0.0286(13) 0.0192(11) 0.0010(10) 0.0044(9) -0.0056(10) C35 0.0290(14) 0.0479(17) 0.0188(12) -0.0053(11) 0.0020(10) 0.0024(12) C36 0.0411(17) 0.056(2) 0.0251(14) -0.0121(13) 0.0027(13) 0.0059(15) C37 0.053(2) 0.059(2) 0.0241(14) 0.0133(14) 0.0112(14) 0.0129(17) C38 0.0294(16) 0.087(3) 0.0346(17) -0.0204(17) -0.0042(13) -0.0004(17) O13 0.0331(10) 0.0302(10) 0.0182(8) -0.0015(7) 0.0049(7) -0.0044(8) O14 0.0256(9) 0.0310(10) 0.0191(8) 0.0027(7) 0.0034(7) -0.0016(8) C39 0.0225(12) 0.0302(13) 0.0191(11) 0.0021(10) 0.0043(9) 0.0031(10) C40 0.0246(13) 0.0448(16) 0.0178(12) 0.0032(11) 0.0001(10) -0.0007(12) C41 0.0455(18) 0.0457(18) 0.0194(13) 0.0082(11) 0.0024(12) 0.0014(14) C42 0.0440(17) 0.0476(18) 0.0205(13) -0.0062(12) 0.0057(12) -0.0097(14) C43 0.0282(15) 0.089(3) 0.0285(15) 0.0097(17) -0.0022(12) 0.0010(17) O15 0.0229(9) 0.0315(10) 0.0289(9) 0.0015(8) -0.0005(7) -0.0022(8) O16 0.0225(9) 0.0441(12) 0.0249(9) -0.0016(8) 0.0022(7) -0.0025(8) C44 0.0227(12) 0.0321(14) 0.0214(12) 0.0066(10) -0.0005(10) -0.0030(10) C45 0.0231(13) 0.0332(14) 0.0319(14) 0.0070(11) -0.0021(11) -0.0026(11) C46 0.0374(16) 0.0383(17) 0.0390(16) 0.0013(13) -0.0123(13) -0.0047(13) C47 0.0302(14) 0.0363(16) 0.0361(15) 0.0094(12) -0.0014(12) 0.0021(12) C48 0.0212(13) 0.057(2) 0.0441(17) 0.0137(15) 0.0019(12) -0.0048(13) O17 0.0218(9) 0.0359(10) 0.0221(9) 0.0024(7) 0.0055(7) 0.0014(7) O18 0.0377(11) 0.0282(10) 0.0330(10) 0.0055(8) 0.0133(9) -0.0009(8) C49 0.0185(11) 0.0304(13) 0.0246(12) -0.0026(10) 0.0042(9) -0.0060(10) C50 0.0239(13) 0.0395(15) 0.0248(13) -0.0026(11) 0.0066(10) -0.0018(11) C51 0.088(3) 0.070(3) 0.063(3) 0.008(2) 0.055(2) 0.010(2) C52 0.051(2) 0.115(4) 0.043(2) 0.000(2) 0.0109(17) 0.042(2) C53 0.044(2) 0.076(3) 0.137(5) -0.069(3) 0.035(3) -0.014(2) O19 0.0261(10) 0.0498(12) 0.0262(10) -0.0033(9) 0.0059(8) -0.0037(9) O20 0.0514(13) 0.0361(12) 0.0405(12) -0.0007(9) 0.0199(10) 0.0082(10) C54 0.0259(13) 0.0413(16) 0.0277(13) 0.0060(11) 0.0059(11) 0.0114(12) C55 0.0378(16) 0.0421(17) 0.0326(15) 0.0046(12) 0.0153(13) 0.0070(13) C56 0.0456(19) 0.0433(18) 0.0393(17) 0.0075(14) -0.0064(14) -0.0052(15) C57 0.0232(15) 0.086(3) 0.057(2) 0.030(2) 0.0022(15) -0.0028(16) C58 0.131(5) 0.057(3) 0.096(4) 0.001(2) 0.095(4) 0.007(3) N61 0.161(5) 0.116(4) 0.063(3) -0.028(3) 0.053(3) -0.071(4) C61 0.080(3) 0.066(3) 0.0367(19) 0.0014(17) 0.0095(19) -0.023(2) C62 0.095(4) 0.073(3) 0.060(3) 0.025(2) 0.034(2) 0.023(3) N62 0.115(4) 0.127(4) 0.063(3) 0.005(3) 0.038(3) 0.020(3) C63 0.054(2) 0.084(3) 0.065(3) 0.022(2) 0.019(2) 0.011(2) C64 0.066(3) 0.055(2) 0.058(2) 0.0192(19) 0.001(2) 0.001(2) N63 0.263(9) 0.133(5) 0.081(4) 0.042(3) 0.078(5) 0.090(5) C65 0.108(4) 0.064(3) 0.050(2) 0.000(2) 0.020(2) 0.022(3) C66 0.104(4) 0.087(4) 0.063(3) -0.023(3) 0.031(3) -0.005(3) C68A 0.071(10) 0.072(3) 0.046(3) -0.003(4) 0.004(4) 0.006(4) C68B 0.071(10) 0.072(3) 0.046(3) -0.003(4) 0.004(4) 0.006(4) _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 O1 2.3330(16) . ? Gd1 O17 2.3517(18) . ? Gd1 O10 2.3533(18) . ? Gd1 O7 2.3949(17) . ? Gd1 O14 2.4086(17) . ? Gd1 O6 2.4335(18) . ? Gd1 O5 2.4669(16) . ? Gd1 N3 2.515(2) . ? Gd2 O19 2.3401(19) . ? Gd2 O16 2.3408(18) . ? Gd2 O3 2.3507(17) . ? Gd2 O5 2.3898(17) . ? Gd2 O12 2.3958(18) . ? Gd2 O8 2.435(2) . ? Gd2 O7 2.4691(16) . ? Gd2 N4 2.510(2) . ? Co1 O11 2.0306(17) . ? Co1 O9 2.0488(19) . ? Co1 O1 2.0650(16) . ? Co1 O3 2.1517(17) . ? Co1 O5 2.1926(16) . ? Co1 N1 2.198(2) . ? Co2 O13 2.0223(17) . ? Co2 O3 2.0671(16) . ? Co2 O15 2.0843(19) . ? Co2 O1 2.1706(17) . ? Co2 O7 2.1725(17) . ? Co2 N2 2.192(2) . ? N1 C1 1.340(3) . ? N1 C5 1.359(3) . ? C1 C2 1.393(4) . ? C1 C6 1.513(3) . ? C2 C3 1.378(4) . ? C2 H2A 0.9500 . ? C3 C4 1.382(4) . ? C3 H3A 0.9500 . ? C4 C5 1.388(4) . ? C4 H4A 0.9500 . ? C5 C7 1.511(4) . ? C6 O1 1.413(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 O2 1.421(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? O2 H2 0.84(3) . ? N2 C8 1.339(3) . ? N2 C12 1.359(3) . ? C8 C9 1.394(4) . ? C8 C13 1.517(3) . ? C9 C10 1.383(4) . ? C9 H9A 0.9500 . ? C10 C11 1.375(5) . ? C10 H10A 0.9500 . ? C11 C12 1.389(4) . ? C11 H11A 0.9500 . ? C12 C14 1.503(4) . ? C13 O3 1.403(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 O4 1.414(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? O4 H4 0.87(3) . ? N3 C19 1.344(3) . ? N3 C15 1.348(3) . ? C15 C16 1.390(4) . ? C15 C20 1.513(4) . ? C16 C17 1.390(4) . ? C16 H16A 0.9500 . ? C17 C18 1.381(5) . ? C17 H17A 0.9500 . ? C18 C19 1.386(4) . ? C18 H18A 0.9500 . ? C19 C21 1.502(4) . ? C20 O5 1.414(3) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 O6 1.416(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? O6 H6 0.87(3) . ? N4 C22 1.339(4) . ? N4 C26 1.344(4) . ? C22 C23 1.391(4) . ? C22 C27 1.501(4) . ? C23 C24 1.380(5) . ? C23 H23A 0.9500 . ? C24 C25 1.369(5) . ? C24 H24A 0.9500 . ? C25 C26 1.390(4) . ? C25 H25A 0.9500 . ? C26 C28 1.505(4) . ? C27 O7 1.413(3) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 O8 1.415(4) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? O8 H8 0.91(3) . ? O9 C29 1.257(3) . ? O10 C29 1.262(3) . ? C29 C30 1.529(4) . ? C30 C32 1.531(4) . ? C30 C33 1.533(6) . ? C30 C31 1.537(4) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? O11 C34 1.273(3) . ? O12 C34 1.243(3) . ? C34 C35 1.545(3) . ? C35 C38 1.529(4) . ? C35 C36 1.531(4) . ? C35 C37 1.533(5) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? O13 C39 1.277(3) . ? O14 C39 1.248(3) . ? C39 C40 1.543(3) . ? C40 C41 1.526(4) . ? C40 C42 1.529(4) . ? C40 C43 1.530(4) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? O15 C44 1.253(3) . ? O16 C44 1.258(3) . ? C44 C45 1.539(4) . ? C45 C48 1.534(4) . ? C45 C46 1.534(4) . ? C45 C47 1.541(4) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? O17 C49 1.264(3) . ? O18 C49 1.254(3) . ? C49 C50 1.541(4) . ? C50 C53 1.495(5) . ? C50 C52 1.507(5) . ? C50 C51 1.520(4) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? O19 C54 1.254(3) . ? O20 C54 1.261(4) . ? C54 C55 1.535(4) . ? C55 C58 1.524(4) . ? C55 C57 1.529(5) . ? C55 C56 1.530(4) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? N61 C61 1.103(5) . ? C61 C62 1.434(5) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? N62 C63 1.160(6) . ? C63 C64 1.480(6) . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? N63 C65 1.099(6) . ? C65 C66 1.408(6) . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? N64A C67A 1.134(9) . ? C67A C68A 1.448(13) . ? C68A H68A 0.9800 . ? C68A H68B 0.9800 . ? C68A H68C 0.9800 . ? N64B C67B 1.147(9) . ? C67B C68B 1.444(14) . ? C68B H68D 0.9800 . ? C68B H68E 0.9800 . ? C68B H68F 0.9800 . ? 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 O1 Gd1 O17 99.65(6) . . ? O1 Gd1 O10 84.93(6) . . ? O17 Gd1 O10 70.69(6) . . ? O1 Gd1 O7 74.56(6) . . ? O17 Gd1 O7 146.25(6) . . ? O10 Gd1 O7 139.47(6) . . ? O1 Gd1 O14 78.97(6) . . ? O17 Gd1 O14 71.73(6) . . ? O10 Gd1 O14 135.65(6) . . ? O7 Gd1 O14 74.54(6) . . ? O1 Gd1 O6 153.04(6) . . ? O17 Gd1 O6 76.13(7) . . ? O10 Gd1 O6 117.43(7) . . ? O7 Gd1 O6 94.04(6) . . ? O14 Gd1 O6 74.42(7) . . ? O1 Gd1 O5 74.89(5) . . ? O17 Gd1 O5 144.51(6) . . ? O10 Gd1 O5 73.88(6) . . ? O7 Gd1 O5 67.24(6) . . ? O14 Gd1 O5 138.05(6) . . ? O6 Gd1 O5 123.75(6) . . ? O1 Gd1 N3 139.56(6) . . ? O17 Gd1 N3 110.54(7) . . ? O10 Gd1 N3 80.57(7) . . ? O7 Gd1 N3 92.74(6) . . ? O14 Gd1 N3 135.26(7) . . ? O6 Gd1 N3 63.71(7) . . ? O5 Gd1 N3 64.86(6) . . ? O19 Gd2 O16 70.72(7) . . ? O19 Gd2 O3 101.65(7) . . ? O16 Gd2 O3 84.49(6) . . ? O19 Gd2 O5 147.19(6) . . ? O16 Gd2 O5 139.51(6) . . ? O3 Gd2 O5 75.33(6) . . ? O19 Gd2 O12 72.12(6) . . ? O16 Gd2 O12 135.01(7) . . ? O3 Gd2 O12 79.04(6) . . ? O5 Gd2 O12 75.27(6) . . ? O19 Gd2 O8 74.86(7) . . ? O16 Gd2 O8 117.66(7) . . ? O3 Gd2 O8 153.49(6) . . ? O5 Gd2 O8 93.33(7) . . ? O12 Gd2 O8 74.89(7) . . ? O19 Gd2 O7 144.29(6) . . ? O16 Gd2 O7 73.57(6) . . ? O3 Gd2 O7 73.88(6) . . ? O5 Gd2 O7 67.28(6) . . ? O12 Gd2 O7 138.03(6) . . ? O8 Gd2 O7 124.25(6) . . ? O19 Gd2 N4 109.84(7) . . ? O16 Gd2 N4 81.10(7) . . ? O3 Gd2 N4 138.40(7) . . ? O5 Gd2 N4 91.10(6) . . ? O12 Gd2 N4 135.91(7) . . ? O8 Gd2 N4 64.10(7) . . ? O7 Gd2 N4 64.64(7) . . ? O11 Co1 O9 88.91(8) . . ? O11 Co1 O1 173.68(7) . . ? O9 Co1 O1 97.41(7) . . ? O11 Co1 O3 94.08(7) . . ? O9 Co1 O3 175.05(7) . . ? O1 Co1 O3 79.60(7) . . ? O11 Co1 O5 93.11(7) . . ? O9 Co1 O5 92.28(7) . . ? O1 Co1 O5 86.56(6) . . ? O3 Co1 O5 83.63(6) . . ? O11 Co1 N1 102.30(7) . . ? O9 Co1 N1 83.12(8) . . ? O1 Co1 N1 78.68(7) . . ? O3 Co1 N1 100.05(7) . . ? O5 Co1 N1 163.79(7) . . ? O13 Co2 O3 173.83(7) . . ? O13 Co2 O15 88.67(8) . . ? O3 Co2 O15 97.44(7) . . ? O13 Co2 O1 94.72(7) . . ? O3 Co2 O1 79.12(7) . . ? O15 Co2 O1 174.16(7) . . ? O13 Co2 O7 92.70(7) . . ? O3 Co2 O7 86.22(6) . . ? O15 Co2 O7 92.58(7) . . ? O1 Co2 O7 82.52(6) . . ? O13 Co2 N2 101.99(8) . . ? O3 Co2 N2 79.42(7) . . ? O15 Co2 N2 85.62(8) . . ? O1 Co2 N2 98.30(7) . . ? O7 Co2 N2 165.15(7) . . ? C1 N1 C5 117.7(2) . . ? C1 N1 Co1 110.78(16) . . ? C5 N1 Co1 130.67(18) . . ? N1 C1 C2 123.4(2) . . ? N1 C1 C6 117.8(2) . . ? C2 C1 C6 118.8(2) . . ? C3 C2 C1 118.6(3) . . ? C3 C2 H2A 120.7 . . ? C1 C2 H2A 120.7 . . ? C2 C3 C4 118.6(3) . . ? C2 C3 H3A 120.7 . . ? C4 C3 H3A 120.7 . . ? C3 C4 C5 120.1(3) . . ? C3 C4 H4A 120.0 . . ? C5 C4 H4A 120.0 . . ? N1 C5 C4 121.6(3) . . ? N1 C5 C7 118.1(2) . . ? C4 C5 C7 120.3(2) . . ? O1 C6 C1 112.82(19) . . ? O1 C6 H6A 109.0 . . ? C1 C6 H6A 109.0 . . ? O1 C6 H6B 109.0 . . ? C1 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? C6 O1 Co1 112.99(14) . . ? C6 O1 Co2 118.48(15) . . ? Co1 O1 Co2 100.35(7) . . ? C6 O1 Gd1 121.00(14) . . ? Co1 O1 Gd1 100.16(6) . . ? Co2 O1 Gd1 100.45(6) . . ? O2 C7 C5 111.5(3) . . ? O2 C7 H7A 109.3 . . ? C5 C7 H7A 109.3 . . ? O2 C7 H7B 109.3 . . ? C5 C7 H7B 109.3 . . ? H7A C7 H7B 108.0 . . ? C7 O2 H2 106(3) . . ? C8 N2 C12 118.3(2) . . ? C8 N2 Co2 110.65(16) . . ? C12 N2 Co2 131.06(18) . . ? N2 C8 C9 122.8(2) . . ? N2 C8 C13 117.6(2) . . ? C9 C8 C13 119.6(2) . . ? C10 C9 C8 118.6(3) . . ? C10 C9 H9A 120.7 . . ? C8 C9 H9A 120.7 . . ? C11 C10 C9 119.1(3) . . ? C11 C10 H10A 120.5 . . ? C9 C10 H10A 120.5 . . ? C10 C11 C12 119.8(3) . . ? C10 C11 H11A 120.1 . . ? C12 C11 H11A 120.1 . . ? N2 C12 C11 121.5(3) . . ? N2 C12 C14 118.0(2) . . ? C11 C12 C14 120.5(3) . . ? O3 C13 C8 112.54(19) . . ? O3 C13 H13A 109.1 . . ? C8 C13 H13A 109.1 . . ? O3 C13 H13B 109.1 . . ? C8 C13 H13B 109.1 . . ? H13A C13 H13B 107.8 . . ? C13 O3 Co2 112.17(14) . . ? C13 O3 Co1 116.07(15) . . ? Co2 O3 Co1 100.91(7) . . ? C13 O3 Gd2 124.27(15) . . ? Co2 O3 Gd2 100.22(6) . . ? Co1 O3 Gd2 99.70(6) . . ? O4 C14 C12 111.9(3) . . ? O4 C14 H14A 109.2 . . ? C12 C14 H14A 109.2 . . ? O4 C14 H14B 109.2 . . ? C12 C14 H14B 109.2 . . ? H14A C14 H14B 107.9 . . ? C14 O4 H4 113(4) . . ? C19 N3 C15 119.7(2) . . ? C19 N3 Gd1 122.20(18) . . ? C15 N3 Gd1 118.03(17) . . ? N3 C15 C16 121.6(3) . . ? N3 C15 C20 116.5(2) . . ? C16 C15 C20 121.9(2) . . ? C17 C16 C15 118.1(3) . . ? C17 C16 H16A 120.9 . . ? C15 C16 H16A 120.9 . . ? C18 C17 C16 120.2(3) . . ? C18 C17 H17A 119.9 . . ? C16 C17 H17A 119.9 . . ? C17 C18 C19 118.6(3) . . ? C17 C18 H18A 120.7 . . ? C19 C18 H18A 120.7 . . ? N3 C19 C18 121.6(3) . . ? N3 C19 C21 116.6(2) . . ? C18 C19 C21 121.7(3) . . ? O5 C20 C15 110.7(2) . . ? O5 C20 H20A 109.5 . . ? C15 C20 H20A 109.5 . . ? O5 C20 H20B 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 108.1 . . ? C20 O5 Co1 121.15(14) . . ? C20 O5 Gd2 114.83(14) . . ? Co1 O5 Gd2 97.36(6) . . ? C20 O5 Gd1 115.10(14) . . ? Co1 O5 Gd1 92.73(6) . . ? Gd2 O5 Gd1 112.78(6) . . ? O6 C21 C19 110.7(2) . . ? O6 C21 H21A 109.5 . . ? C19 C21 H21A 109.5 . . ? O6 C21 H21B 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 108.1 . . ? C21 O6 Gd1 125.09(17) . . ? C21 O6 H6 108(2) . . ? Gd1 O6 H6 100(2) . . ? C22 N4 C26 119.2(2) . . ? C22 N4 Gd2 118.64(18) . . ? C26 N4 Gd2 122.19(19) . . ? N4 C22 C23 122.2(3) . . ? N4 C22 C27 116.3(2) . . ? C23 C22 C27 121.6(3) . . ? C24 C23 C22 118.2(3) . . ? C24 C23 H23A 120.9 . . ? C22 C23 H23A 120.9 . . ? C25 C24 C23 119.9(3) . . ? C25 C24 H24A 120.1 . . ? C23 C24 H24A 120.1 . . ? C24 C25 C26 119.1(3) . . ? C24 C25 H25A 120.4 . . ? C26 C25 H25A 120.4 . . ? N4 C26 C25 121.4(3) . . ? N4 C26 C28 116.7(3) . . ? C25 C26 C28 121.9(3) . . ? O7 C27 C22 111.1(2) . . ? O7 C27 H27A 109.4 . . ? C22 C27 H27A 109.4 . . ? O7 C27 H27B 109.4 . . ? C22 C27 H27B 109.4 . . ? H27A C27 H27B 108.0 . . ? C27 O7 Co2 121.54(15) . . ? C27 O7 Gd1 113.42(14) . . ? Co2 O7 Gd1 98.48(6) . . ? C27 O7 Gd2 114.82(14) . . ? Co2 O7 Gd2 93.77(6) . . ? Gd1 O7 Gd2 112.52(6) . . ? O8 C28 C26 111.2(2) . . ? O8 C28 H28A 109.4 . . ? C26 C28 H28A 109.4 . . ? O8 C28 H28B 109.4 . . ? C26 C28 H28B 109.4 . . ? H28A C28 H28B 108.0 . . ? C28 O8 Gd2 124.97(18) . . ? C28 O8 H8 108(2) . . ? Gd2 O8 H8 105(2) . . ? C29 O9 Co1 126.62(17) . . ? C29 O10 Gd1 137.11(16) . . ? O9 C29 O10 124.8(2) . . ? O9 C29 C30 117.9(2) . . ? O10 C29 C30 117.3(2) . . ? C29 C30 C32 110.7(3) . . ? C29 C30 C33 107.2(3) . . ? C32 C30 C33 109.3(3) . . ? C29 C30 C31 108.5(2) . . ? C32 C30 C31 111.4(3) . . ? C33 C30 C31 109.7(3) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C30 C33 H33A 109.5 . . ? C30 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C34 O11 Co1 125.53(16) . . ? C34 O12 Gd2 138.85(16) . . ? O12 C34 O11 124.3(2) . . ? O12 C34 C35 119.5(2) . . ? O11 C34 C35 116.2(2) . . ? C38 C35 C36 109.8(3) . . ? C38 C35 C37 110.2(3) . . ? C36 C35 C37 110.3(3) . . ? C38 C35 C34 109.3(2) . . ? C36 C35 C34 110.4(2) . . ? C37 C35 C34 107.0(2) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C39 O13 Co2 125.37(17) . . ? C39 O14 Gd1 138.64(16) . . ? O14 C39 O13 124.2(2) . . ? O14 C39 C40 119.3(2) . . ? O13 C39 C40 116.5(2) . . ? C41 C40 C42 110.4(2) . . ? C41 C40 C43 110.2(3) . . ? C42 C40 C43 109.3(3) . . ? C41 C40 C39 110.5(2) . . ? C42 C40 C39 107.2(2) . . ? C43 C40 C39 109.1(2) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C40 C43 H43A 109.5 . . ? C40 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C40 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C44 O15 Co2 124.77(17) . . ? C44 O16 Gd2 139.39(18) . . ? O15 C44 O16 124.7(2) . . ? O15 C44 C45 119.1(2) . . ? O16 C44 C45 116.3(2) . . ? C48 C45 C46 110.9(3) . . ? C48 C45 C44 108.1(2) . . ? C46 C45 C44 111.2(2) . . ? C48 C45 C47 109.6(3) . . ? C46 C45 C47 109.1(2) . . ? C44 C45 C47 107.8(2) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C45 C48 H48A 109.5 . . ? C45 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C45 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C49 O17 Gd1 133.09(17) . . ? O18 C49 O17 124.2(2) . . ? O18 C49 C50 118.9(2) . . ? O17 C49 C50 116.9(2) . . ? C53 C50 C52 110.7(4) . . ? C53 C50 C51 110.5(3) . . ? C52 C50 C51 109.3(3) . . ? C53 C50 C49 106.9(2) . . ? C52 C50 C49 109.6(2) . . ? C51 C50 C49 109.8(3) . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C50 C52 H52A 109.5 . . ? C50 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C50 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C50 C53 H53A 109.5 . . ? C50 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C50 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C54 O19 Gd2 135.8(2) . . ? O19 C54 O20 124.1(3) . . ? O19 C54 C55 116.6(3) . . ? O20 C54 C55 119.3(3) . . ? C58 C55 C57 110.0(3) . . ? C58 C55 C56 111.0(3) . . ? C57 C55 C56 108.8(3) . . ? C58 C55 C54 111.1(3) . . ? C57 C55 C54 109.3(2) . . ? C56 C55 C54 106.6(3) . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C55 C57 H57A 109.5 . . ? C55 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C55 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C55 C58 H58A 109.5 . . ? C55 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C55 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? N61 C61 C62 177.6(5) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? N62 C63 C64 178.4(5) . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? N63 C65 C66 177.5(6) . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? N64A C67A C68A 179(2) . . ? N64B C67B C68B 175(2) . . ? C67B C68B H68D 109.5 . . ? C67B C68B H68E 109.5 . . ? H68D C68B H68E 109.5 . . ? C67B C68B H68F 109.5 . . ? H68D C68B H68F 109.5 . . ? H68E C68B H68F 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2 O11 0.84(3) 1.98(4) 2.732(3) 150(4) . O4 H4 O13 0.87(3) 2.04(4) 2.759(3) 139(5) . O6 H6 O18 0.87(3) 1.67(3) 2.542(3) 173(3) . O8 H8 O20 0.91(3) 1.63(3) 2.528(3) 167(3) . _diffrn_measured_fraction_theta_max 0.923 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.561 _refine_diff_density_min -0.789 _refine_diff_density_rms 0.084 ######################################################### data_zhao413 _database_code_depnum_ccdc_archive 'CCDC 756452' #TrackingRef 'co2ln2_a1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C58 H86 Co2 N4 O20 Tb2, 4(C2 H3 N)' _chemical_formula_sum 'C66 H98 Co2 N8 O20 Tb2' _chemical_formula_weight 1759.22 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.6306(7) _cell_length_b 18.8377(10) _cell_length_c 26.9544(11) _cell_angle_alpha 90.00 _cell_angle_beta 100.594(3) _cell_angle_gamma 90.00 _cell_volume 7801.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 59634 _cell_measurement_theta_min 1.33 _cell_measurement_theta_max 27.30 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.498 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3576 _exptl_absorpt_coefficient_mu 2.279 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.393 _exptl_absorpt_correction_T_max 0.634 _exptl_absorpt_process_details ; XPREP in SHELXTL 6.14 (BrukerAXS Inc., 2003) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean 6.667 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 51003 _diffrn_reflns_av_R_equivalents 0.0702 _diffrn_reflns_av_sigmaI/netI 0.0525 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 26.82 _reflns_number_total 16550 _reflns_number_gt 12993 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'WinXpose 1.6.8 (Stoe & Cie GmbH, 2004)' _computing_cell_refinement 'X-Area 1.38 (Stoe & Cie GmbH, 2006)' _computing_data_reduction 'X-Area 1.38 (Stoe & Cie GmbH, 2006)' _computing_structure_solution 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_structure_refinement 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_molecular_graphics 'Diamond 2.1 (Crystal Impact, 1998)' _computing_publication_material 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _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. One lattice MeCN was twofold disordered and refined using half-occupancy atoms with geometrical restraints. ; _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^)+(0.1011P)^2^+8.0505P] 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 16550 _refine_ls_number_parameters 896 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0811 _refine_ls_R_factor_gt 0.0644 _refine_ls_wR_factor_ref 0.1698 _refine_ls_wR_factor_gt 0.1595 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.419088(18) 0.191247(15) 0.290986(11) 0.03812(9) Uani 1 1 d . . . Tb2 Tb 0.617110(19) 0.205440(16) 0.214261(11) 0.04113(10) Uani 1 1 d . . . Co1 Co 0.43359(5) 0.30945(4) 0.19899(3) 0.03817(18) Uani 1 1 d . . . Co2 Co 0.57643(5) 0.32208(4) 0.30267(3) 0.03935(18) Uani 1 1 d . . . N1 N 0.3893(3) 0.4179(3) 0.2095(2) 0.0443(11) Uani 1 1 d . . . C1 C 0.3661(4) 0.4248(3) 0.2553(3) 0.0447(13) Uani 1 1 d . . . C2 C 0.3247(4) 0.4852(4) 0.2699(3) 0.0548(16) Uani 1 1 d . . . H2A H 0.3092 0.4880 0.3023 0.066 Uiso 1 1 calc R . . C3 C 0.3066(5) 0.5409(4) 0.2356(3) 0.0595(18) Uani 1 1 d . . . H3A H 0.2789 0.5829 0.2442 0.071 Uiso 1 1 calc R . . C4 C 0.3301(5) 0.5336(4) 0.1887(3) 0.0587(18) Uani 1 1 d . . . H4A H 0.3178 0.5708 0.1646 0.070 Uiso 1 1 calc R . . C5 C 0.3711(5) 0.4727(4) 0.1764(3) 0.0539(16) Uani 1 1 d . . . C6 C 0.3816(4) 0.3623(3) 0.2910(2) 0.0434(13) Uani 1 1 d . . . H6A H 0.4085 0.3797 0.3250 0.052 Uiso 1 1 calc R . . H6B H 0.3248 0.3408 0.2936 0.052 Uiso 1 1 calc R . . O1 O 0.4342(3) 0.31075(19) 0.27648(16) 0.0431(10) Uani 1 1 d . . . C7 C 0.3947(6) 0.4646(5) 0.1252(3) 0.073(2) Uani 1 1 d . . . H7A H 0.3962 0.5120 0.1094 0.088 Uiso 1 1 calc R . . H7B H 0.4535 0.4435 0.1287 0.088 Uiso 1 1 calc R . . O2 O 0.3340(5) 0.4210(4) 0.0938(2) 0.087(2) Uani 1 1 d D . . H2 H 0.363(7) 0.380(4) 0.093(5) 0.131 Uiso 1 1 d D . . N2 N 0.5883(4) 0.4362(3) 0.2882(2) 0.0467(12) Uani 1 1 d . . . C8 C 0.6011(4) 0.4465(3) 0.2407(3) 0.0472(14) Uani 1 1 d . . . C9 C 0.6104(6) 0.5144(4) 0.2218(3) 0.071(2) Uani 1 1 d . . . H9A H 0.6176 0.5211 0.1879 0.085 Uiso 1 1 calc R . . C10 C 0.6089(8) 0.5722(4) 0.2538(4) 0.088(3) Uani 1 1 d . . . H10A H 0.6159 0.6189 0.2420 0.106 Uiso 1 1 calc R . . C11 C 0.5974(6) 0.5613(4) 0.3021(3) 0.070(2) Uani 1 1 d . . . H11A H 0.5959 0.6007 0.3239 0.085 Uiso 1 1 calc R . . C12 C 0.5879(5) 0.4929(4) 0.3194(3) 0.0546(16) Uani 1 1 d . . . C13 C 0.6100(4) 0.3814(3) 0.2089(2) 0.0457(14) Uani 1 1 d . . . H13A H 0.5818 0.3913 0.1736 0.055 Uiso 1 1 calc R . . H13B H 0.6726 0.3729 0.2092 0.055 Uiso 1 1 calc R . . O3 O 0.5745(3) 0.32076(19) 0.22455(16) 0.0425(10) Uani 1 1 d . . . C14 C 0.5795(7) 0.4799(4) 0.3728(3) 0.074(2) Uani 1 1 d D . . H14A H 0.5687 0.5254 0.3889 0.089 Uiso 1 1 calc R . . H14B H 0.5291 0.4484 0.3736 0.089 Uiso 1 1 calc R . . O4 O 0.6561(6) 0.4480(3) 0.4004(2) 0.096(2) Uani 1 1 d D . . H4 H 0.636(5) 0.402(2) 0.400(5) 0.144 Uiso 1 1 d D . . N3 N 0.4212(3) 0.0740(3) 0.2473(2) 0.0456(12) Uani 1 1 d . . . C15 C 0.4202(4) 0.0739(4) 0.1982(3) 0.0517(15) Uani 1 1 d . . . C16 C 0.4169(5) 0.0114(4) 0.1704(3) 0.0586(17) Uani 1 1 d . . . H16A H 0.4151 0.0124 0.1350 0.070 Uiso 1 1 calc R . . C17 C 0.4164(6) -0.0533(4) 0.1965(4) 0.076(2) Uani 1 1 d . . . H17A H 0.4139 -0.0970 0.1787 0.092 Uiso 1 1 calc R . . C18 C 0.4195(6) -0.0531(4) 0.2472(3) 0.071(2) Uani 1 1 d . . . H18A H 0.4204 -0.0966 0.2652 0.085 Uiso 1 1 calc R . . C19 C 0.4214(5) 0.0114(4) 0.2725(3) 0.0556(16) Uani 1 1 d . . . C20 C 0.4234(4) 0.1457(3) 0.1732(2) 0.0432(13) Uani 1 1 d . . . H20A H 0.4562 0.1418 0.1452 0.052 Uiso 1 1 calc R . . H20B H 0.3636 0.1617 0.1589 0.052 Uiso 1 1 calc R . . O5 O 0.4638(3) 0.1951(2) 0.20867(15) 0.0381(8) Uani 1 1 d . . . C21 C 0.4217(5) 0.0169(4) 0.3284(3) 0.0584(17) Uani 1 1 d . . . H21A H 0.3660 -0.0014 0.3357 0.070 Uiso 1 1 calc R . . H21B H 0.4694 -0.0125 0.3471 0.070 Uiso 1 1 calc R . . O6 O 0.4329(3) 0.0874(2) 0.34443(19) 0.0547(11) Uani 1 1 d D . . H6 H 0.397(4) 0.097(4) 0.367(3) 0.066 Uiso 1 1 d D . . N4 N 0.6416(3) 0.0920(3) 0.2623(2) 0.0498(13) Uani 1 1 d . . . C22 C 0.6416(4) 0.0935(4) 0.3119(3) 0.0526(16) Uani 1 1 d . . . C23 C 0.6599(6) 0.0332(4) 0.3423(4) 0.070(2) Uani 1 1 d . . . H23A H 0.6614 0.0354 0.3776 0.085 Uiso 1 1 calc R . . C24 C 0.6760(6) -0.0304(5) 0.3190(4) 0.082(3) Uani 1 1 d . . . H24A H 0.6886 -0.0723 0.3386 0.098 Uiso 1 1 calc R . . C25 C 0.6738(6) -0.0325(4) 0.2682(4) 0.071(2) Uani 1 1 d . . . H25A H 0.6831 -0.0756 0.2518 0.085 Uiso 1 1 calc R . . C26 C 0.6573(5) 0.0306(4) 0.2411(3) 0.0585(18) Uani 1 1 d . . . C27 C 0.6220(4) 0.1634(4) 0.3335(2) 0.0487(14) Uani 1 1 d . . . H27A H 0.5898 0.1554 0.3614 0.058 Uiso 1 1 calc R . . H27B H 0.6772 0.1878 0.3475 0.058 Uiso 1 1 calc R . . O7 O 0.5727(3) 0.2060(2) 0.29694(16) 0.0390(9) Uani 1 1 d . . . C28 C 0.6545(5) 0.0324(4) 0.1848(3) 0.0630(19) Uani 1 1 d . . . H28A H 0.7131 0.0219 0.1777 0.076 Uiso 1 1 calc R . . H28B H 0.6140 -0.0046 0.1683 0.076 Uiso 1 1 calc R . . O8 O 0.6267(4) 0.0998(3) 0.16460(19) 0.0580(12) Uani 1 1 d D . . H8 H 0.661(5) 0.113(4) 0.141(2) 0.070 Uiso 1 1 d D . . O9 O 0.3024(3) 0.2896(2) 0.17761(18) 0.0488(10) Uani 1 1 d . . . O10 O 0.2905(3) 0.2013(2) 0.23156(17) 0.0459(10) Uani 1 1 d . . . C29 C 0.2604(4) 0.2427(3) 0.1956(2) 0.0427(13) Uani 1 1 d . . . C30 C 0.1632(5) 0.2347(4) 0.1720(3) 0.0603(19) Uani 1 1 d . . . C31 C 0.1115(5) 0.2306(6) 0.2142(4) 0.088(3) Uani 1 1 d . . . H31A H 0.1169 0.2755 0.2328 0.132 Uiso 1 1 calc R . . H31B H 0.1340 0.1918 0.2371 0.132 Uiso 1 1 calc R . . H31C H 0.0501 0.2218 0.1999 0.132 Uiso 1 1 calc R . . C32 C 0.1335(5) 0.2977(6) 0.1367(4) 0.083(3) Uani 1 1 d . . . H32A H 0.1381 0.3417 0.1563 0.124 Uiso 1 1 calc R . . H32B H 0.0729 0.2905 0.1200 0.124 Uiso 1 1 calc R . . H32C H 0.1706 0.3010 0.1111 0.124 Uiso 1 1 calc R . . C33 C 0.1541(7) 0.1661(6) 0.1409(4) 0.098(3) Uani 1 1 d . . . H33A H 0.0930 0.1591 0.1252 0.147 Uiso 1 1 calc R . . H33B H 0.1741 0.1257 0.1630 0.147 Uiso 1 1 calc R . . H33C H 0.1896 0.1695 0.1145 0.147 Uiso 1 1 calc R . . O11 O 0.4447(3) 0.3096(2) 0.12505(17) 0.0479(10) Uani 1 1 d . . . O12 O 0.5591(3) 0.2375(3) 0.12959(17) 0.0525(11) Uani 1 1 d . . . C34 C 0.4932(4) 0.2689(4) 0.1051(2) 0.0459(14) Uani 1 1 d . . . C35 C 0.4706(5) 0.2590(5) 0.0472(3) 0.0580(18) Uani 1 1 d . . . C36 C 0.5234(6) 0.1986(5) 0.0305(3) 0.075(2) Uani 1 1 d . . . H36A H 0.5088 0.1936 -0.0063 0.113 Uiso 1 1 calc R . . H36B H 0.5097 0.1543 0.0464 0.113 Uiso 1 1 calc R . . H36C H 0.5856 0.2089 0.0406 0.113 Uiso 1 1 calc R . . C37 C 0.4955(6) 0.3293(5) 0.0242(3) 0.077(2) Uani 1 1 d . . . H37A H 0.4618 0.3683 0.0351 0.116 Uiso 1 1 calc R . . H37B H 0.4829 0.3259 -0.0127 0.116 Uiso 1 1 calc R . . H37C H 0.5578 0.3384 0.0357 0.116 Uiso 1 1 calc R . . C38 C 0.3730(5) 0.2451(7) 0.0326(3) 0.092(3) Uani 1 1 d . . . H38A H 0.3409 0.2852 0.0434 0.138 Uiso 1 1 calc R . . H38B H 0.3583 0.2016 0.0492 0.138 Uiso 1 1 calc R . . H38C H 0.3572 0.2396 -0.0041 0.138 Uiso 1 1 calc R . . O13 O 0.5677(3) 0.3212(2) 0.37641(17) 0.0493(10) Uani 1 1 d . . . O14 O 0.4713(3) 0.2336(2) 0.37480(16) 0.0465(10) Uani 1 1 d . . . C39 C 0.5280(4) 0.2723(4) 0.3976(2) 0.0454(14) Uani 1 1 d . . . C40 C 0.5566(4) 0.2657(4) 0.4553(2) 0.0533(16) Uani 1 1 d . . . C41 C 0.5169(6) 0.1992(4) 0.4744(3) 0.066(2) Uani 1 1 d . . . H41A H 0.4533 0.2018 0.4657 0.099 Uiso 1 1 calc R . . H41B H 0.5348 0.1960 0.5112 0.099 Uiso 1 1 calc R . . H41C H 0.5373 0.1571 0.4587 0.099 Uiso 1 1 calc R . . C42 C 0.5229(6) 0.3314(5) 0.4795(3) 0.067(2) Uani 1 1 d . . . H42A H 0.4592 0.3324 0.4714 0.100 Uiso 1 1 calc R . . H42B H 0.5462 0.3744 0.4664 0.100 Uiso 1 1 calc R . . H42C H 0.5420 0.3293 0.5162 0.100 Uiso 1 1 calc R . . C43 C 0.6558(5) 0.2630(6) 0.4685(3) 0.082(3) Uani 1 1 d . . . H43A H 0.6741 0.2584 0.5051 0.123 Uiso 1 1 calc R . . H43B H 0.6800 0.3068 0.4570 0.123 Uiso 1 1 calc R . . H43C H 0.6769 0.2222 0.4517 0.123 Uiso 1 1 calc R . . O15 O 0.7122(3) 0.3230(2) 0.32353(18) 0.0510(11) Uani 1 1 d . . . O16 O 0.7403(3) 0.2367(3) 0.27302(17) 0.0532(11) Uani 1 1 d . . . C44 C 0.7619(4) 0.2791(4) 0.3087(2) 0.0464(14) Uani 1 1 d . . . C45 C 0.8572(4) 0.2759(4) 0.3368(3) 0.0519(15) Uani 1 1 d . . . C46 C 0.8761(5) 0.3342(4) 0.3759(3) 0.068(2) Uani 1 1 d . . . H46A H 0.8669 0.3805 0.3593 0.102 Uiso 1 1 calc R . . H46B H 0.9367 0.3305 0.3935 0.102 Uiso 1 1 calc R . . H46C H 0.8371 0.3293 0.4003 0.102 Uiso 1 1 calc R . . C47 C 0.8702(5) 0.2026(4) 0.3629(3) 0.0609(18) Uani 1 1 d . . . H47A H 0.8582 0.1650 0.3375 0.091 Uiso 1 1 calc R . . H47B H 0.8303 0.1980 0.3869 0.091 Uiso 1 1 calc R . . H47C H 0.9303 0.1984 0.3811 0.091 Uiso 1 1 calc R . . C48 C 0.9165(4) 0.2814(5) 0.2972(3) 0.066(2) Uani 1 1 d . . . H48A H 0.9020 0.2434 0.2722 0.099 Uiso 1 1 calc R . . H48B H 0.9775 0.2768 0.3139 0.099 Uiso 1 1 calc R . . H48C H 0.9078 0.3276 0.2802 0.099 Uiso 1 1 calc R . . O17 O 0.3011(3) 0.2003(2) 0.33248(17) 0.0472(10) Uani 1 1 d . . . O18 O 0.3219(3) 0.1257(2) 0.39765(19) 0.0562(11) Uani 1 1 d . . . C49 C 0.2860(4) 0.1799(3) 0.3745(2) 0.0450(13) Uani 1 1 d . . . C50 C 0.2221(4) 0.2223(4) 0.3993(2) 0.0496(15) Uani 1 1 d . . . C51 C 0.1930(9) 0.1799(7) 0.4409(5) 0.111(4) Uani 1 1 d . . . H51A H 0.1520 0.2082 0.4562 0.167 Uiso 1 1 calc R . . H51B H 0.2437 0.1679 0.4667 0.167 Uiso 1 1 calc R . . H51C H 0.1644 0.1362 0.4268 0.167 Uiso 1 1 calc R . . C52 C 0.1437(7) 0.2422(7) 0.3607(4) 0.107(4) Uani 1 1 d . . . H52A H 0.1028 0.2691 0.3770 0.160 Uiso 1 1 calc R . . H52B H 0.1152 0.1991 0.3455 0.160 Uiso 1 1 calc R . . H52C H 0.1619 0.2715 0.3344 0.160 Uiso 1 1 calc R . . C53 C 0.2700(7) 0.2870(6) 0.4219(6) 0.118(5) Uani 1 1 d . . . H53A H 0.2314 0.3159 0.4386 0.177 Uiso 1 1 calc R . . H53B H 0.2891 0.3148 0.3953 0.177 Uiso 1 1 calc R . . H53C H 0.3209 0.2725 0.4468 0.177 Uiso 1 1 calc R . . O19 O 0.7323(3) 0.2261(3) 0.17260(18) 0.0575(12) Uani 1 1 d . . . O20 O 0.7313(4) 0.1464(3) 0.1118(2) 0.0664(14) Uani 1 1 d . . . C54 C 0.7565(4) 0.2056(4) 0.1330(3) 0.0528(16) Uani 1 1 d . . . C55 C 0.8139(5) 0.2537(5) 0.1086(3) 0.0602(18) Uani 1 1 d . . . C56 C 0.7549(6) 0.3140(5) 0.0833(3) 0.070(2) Uani 1 1 d . . . H56A H 0.7275 0.3379 0.1087 0.105 Uiso 1 1 calc R . . H56B H 0.7097 0.2942 0.0569 0.105 Uiso 1 1 calc R . . H56C H 0.7899 0.3483 0.0684 0.105 Uiso 1 1 calc R . . C57 C 0.8848(5) 0.2853(6) 0.1496(4) 0.088(3) Uani 1 1 d . . . H57A H 0.9225 0.2472 0.1658 0.132 Uiso 1 1 calc R . . H57B H 0.8576 0.3095 0.1749 0.132 Uiso 1 1 calc R . . H57C H 0.9195 0.3194 0.1342 0.132 Uiso 1 1 calc R . . C58 C 0.8562(9) 0.2139(6) 0.0694(5) 0.114(5) Uani 1 1 d . . . H58A H 0.8937 0.1761 0.0862 0.171 Uiso 1 1 calc R . . H58B H 0.8911 0.2472 0.0535 0.171 Uiso 1 1 calc R . . H58C H 0.8107 0.1932 0.0436 0.171 Uiso 1 1 calc R . . N61 N 0.4146(11) 0.4784(8) -0.0881(5) 0.170(6) Uani 1 1 d D . . C61 C 0.3823(8) 0.4914(7) -0.0553(4) 0.099(3) Uani 1 1 d D . . C62 C 0.3463(10) 0.5093(8) -0.0123(5) 0.129(5) Uani 1 1 d D . . H62A H 0.3752 0.5520 0.0036 0.194 Uiso 1 1 calc R . . H62B H 0.3552 0.4699 0.0119 0.194 Uiso 1 1 calc R . . H62C H 0.2839 0.5185 -0.0226 0.194 Uiso 1 1 calc R . . N62 N 0.4038(10) 0.0266(9) 0.5495(5) 0.164(6) Uani 1 1 d . . . C63 C 0.3873(8) 0.0045(8) 0.5083(6) 0.109(4) Uani 1 1 d . . . C64 C 0.3689(8) -0.0244(6) 0.4551(4) 0.106(4) Uani 1 1 d . . . H64A H 0.4237 -0.0380 0.4450 0.158 Uiso 1 1 calc R . . H64B H 0.3399 0.0121 0.4321 0.158 Uiso 1 1 calc R . . H64C H 0.3310 -0.0661 0.4537 0.158 Uiso 1 1 calc R . . N63 N 0.3637(17) 0.4840(11) 0.4046(8) 0.243(11) Uani 1 1 d . . . C65 C 0.3543(13) 0.4803(9) 0.4419(6) 0.138(6) Uani 1 1 d . . . C66 C 0.3423(12) 0.4758(10) 0.4911(6) 0.176(8) Uani 1 1 d . . . H66A H 0.3650 0.4303 0.5056 0.264 Uiso 1 1 calc R . . H66B H 0.2800 0.4790 0.4921 0.264 Uiso 1 1 calc R . . H66C H 0.3733 0.5148 0.5108 0.264 Uiso 1 1 calc R . . N64A N 0.5901(16) 0.0478(14) -0.0455(8) 0.122(7) Uiso 0.50 1 d PD A 1 C67A C 0.6074(17) 0.0291(15) -0.0042(8) 0.095(7) Uiso 0.50 1 d PD A 1 C68A C 0.6458(18) 0.0123(17) 0.0468(8) 0.095(5) Uiso 0.50 1 d PD A 1 H68A H 0.6826 -0.0299 0.0472 0.143 Uiso 0.50 1 calc PR A 1 H68B H 0.5998 0.0028 0.0662 0.143 Uiso 0.50 1 calc PR A 1 H68C H 0.6813 0.0524 0.0618 0.143 Uiso 0.50 1 calc PR A 1 N64B N 0.5873(18) -0.0048(17) -0.0442(9) 0.150(10) Uiso 0.50 1 d PD B 2 C67B C 0.614(2) -0.0052(18) -0.0014(9) 0.117(9) Uiso 0.50 1 d PD B 2 C68B C 0.6244(18) 0.0012(17) 0.0520(8) 0.095(5) Uiso 0.50 1 d PD B 2 H68D H 0.6309 0.0513 0.0615 0.143 Uiso 0.50 1 calc PR B 2 H68E H 0.6763 -0.0250 0.0680 0.143 Uiso 0.50 1 calc PR B 2 H68F H 0.5731 -0.0184 0.0631 0.143 Uiso 0.50 1 calc PR B 2 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 Tb1 0.03899(16) 0.03894(15) 0.03634(16) 0.00251(10) 0.00666(11) 0.00012(10) Tb2 0.03874(16) 0.04580(16) 0.03832(17) -0.00043(11) 0.00565(12) 0.00154(11) Co1 0.0370(4) 0.0416(4) 0.0352(4) 0.0020(3) 0.0046(3) 0.0006(3) Co2 0.0397(4) 0.0419(4) 0.0352(4) 0.0002(3) 0.0036(3) -0.0006(3) N1 0.043(3) 0.041(2) 0.049(3) 0.010(2) 0.007(2) 0.005(2) C1 0.041(3) 0.038(3) 0.055(4) 0.001(3) 0.008(3) 0.002(2) C2 0.048(4) 0.055(4) 0.064(4) 0.002(3) 0.015(3) 0.013(3) C3 0.056(4) 0.041(3) 0.081(5) 0.006(3) 0.011(4) 0.018(3) C4 0.061(4) 0.047(3) 0.068(5) 0.013(3) 0.010(4) 0.010(3) C5 0.057(4) 0.050(3) 0.055(4) 0.009(3) 0.008(3) 0.003(3) C6 0.051(3) 0.038(3) 0.041(3) 0.001(2) 0.010(3) 0.009(2) O1 0.054(2) 0.0279(17) 0.038(2) -0.0024(15) -0.0145(18) 0.0106(16) C7 0.091(6) 0.066(5) 0.068(5) 0.024(4) 0.026(5) 0.026(4) O2 0.112(5) 0.089(4) 0.054(3) 0.009(3) -0.003(3) 0.034(4) N2 0.050(3) 0.040(3) 0.048(3) -0.001(2) 0.004(2) -0.008(2) C8 0.051(4) 0.040(3) 0.050(4) 0.000(3) 0.008(3) -0.008(3) C9 0.100(6) 0.050(4) 0.063(5) 0.003(3) 0.018(4) -0.007(4) C10 0.148(10) 0.044(4) 0.081(6) -0.003(4) 0.042(6) -0.020(5) C11 0.092(6) 0.053(4) 0.070(5) -0.010(4) 0.024(4) -0.006(4) C12 0.062(4) 0.048(3) 0.054(4) -0.007(3) 0.011(3) -0.001(3) C13 0.055(4) 0.038(3) 0.045(3) -0.001(2) 0.013(3) -0.012(3) O3 0.051(2) 0.0274(17) 0.038(2) 0.0062(15) -0.0201(18) -0.0090(16) C14 0.109(7) 0.051(4) 0.063(5) -0.016(4) 0.018(5) -0.017(4) O4 0.152(7) 0.061(3) 0.061(4) -0.005(3) -0.018(4) -0.018(4) N3 0.046(3) 0.041(3) 0.050(3) 0.000(2) 0.012(2) 0.000(2) C15 0.041(3) 0.052(3) 0.063(4) -0.010(3) 0.009(3) -0.003(3) C16 0.064(4) 0.051(4) 0.063(5) -0.012(3) 0.017(3) -0.006(3) C17 0.095(6) 0.046(4) 0.091(7) -0.018(4) 0.025(5) -0.006(4) C18 0.098(6) 0.040(3) 0.080(6) 0.000(3) 0.033(5) 0.000(4) C19 0.051(4) 0.052(4) 0.067(5) 0.000(3) 0.017(3) 0.002(3) C20 0.044(3) 0.047(3) 0.039(3) -0.008(2) 0.008(2) -0.001(3) O5 0.044(2) 0.0366(19) 0.036(2) 0.0004(15) 0.0125(17) 0.0022(16) C21 0.067(4) 0.047(3) 0.065(5) 0.004(3) 0.022(4) 0.001(3) O6 0.068(3) 0.044(2) 0.056(3) 0.009(2) 0.019(2) 0.004(2) N4 0.042(3) 0.049(3) 0.056(3) 0.000(2) 0.003(2) 0.008(2) C22 0.042(3) 0.050(3) 0.064(4) 0.009(3) 0.006(3) 0.006(3) C23 0.075(5) 0.057(4) 0.078(6) 0.017(4) 0.009(4) 0.019(4) C24 0.090(6) 0.062(5) 0.093(7) 0.029(5) 0.017(5) 0.027(4) C25 0.071(5) 0.056(4) 0.084(6) 0.007(4) 0.011(4) 0.017(4) C26 0.050(4) 0.052(4) 0.073(5) -0.004(3) 0.009(3) 0.005(3) C27 0.044(3) 0.055(4) 0.044(3) 0.011(3) 0.002(3) 0.006(3) O7 0.036(2) 0.043(2) 0.039(2) 0.0011(16) 0.0103(16) 0.0005(16) C28 0.063(4) 0.053(4) 0.076(5) -0.006(4) 0.020(4) 0.009(3) O8 0.072(3) 0.050(3) 0.055(3) -0.003(2) 0.019(2) 0.005(2) O9 0.039(2) 0.054(2) 0.052(3) 0.007(2) 0.0037(19) -0.0029(19) O10 0.038(2) 0.056(2) 0.042(2) 0.0061(19) 0.0049(18) -0.0017(18) C29 0.037(3) 0.052(3) 0.039(3) -0.004(3) 0.006(2) -0.002(3) C30 0.043(3) 0.081(5) 0.052(4) 0.015(4) -0.003(3) -0.010(3) C31 0.037(4) 0.139(9) 0.089(7) 0.050(6) 0.017(4) 0.005(5) C32 0.044(4) 0.121(8) 0.079(6) 0.045(5) 0.001(4) 0.006(4) C33 0.092(7) 0.118(8) 0.073(6) -0.007(6) -0.015(5) -0.040(6) O11 0.052(3) 0.054(2) 0.037(2) 0.0058(18) 0.0057(19) 0.004(2) O12 0.051(3) 0.068(3) 0.038(2) 0.002(2) 0.008(2) 0.005(2) C34 0.042(3) 0.057(4) 0.039(3) 0.000(3) 0.008(3) -0.003(3) C35 0.051(4) 0.084(5) 0.037(3) -0.004(3) 0.001(3) 0.005(4) C36 0.073(5) 0.099(6) 0.052(5) -0.020(4) 0.007(4) 0.018(5) C37 0.088(6) 0.099(6) 0.047(4) 0.021(4) 0.018(4) 0.015(5) C38 0.047(4) 0.163(10) 0.061(5) -0.030(6) -0.005(4) -0.003(5) O13 0.058(3) 0.050(2) 0.040(2) -0.0028(19) 0.008(2) -0.008(2) O14 0.045(2) 0.060(3) 0.033(2) 0.0017(19) 0.0040(18) -0.003(2) C39 0.042(3) 0.058(4) 0.035(3) 0.004(3) 0.004(2) 0.007(3) C40 0.047(3) 0.078(5) 0.034(3) 0.002(3) 0.005(3) -0.002(3) C41 0.078(5) 0.073(5) 0.047(4) 0.014(3) 0.010(4) 0.002(4) C42 0.082(5) 0.082(5) 0.039(4) -0.008(4) 0.016(3) -0.011(4) C43 0.046(4) 0.149(9) 0.047(4) 0.013(5) 0.000(3) 0.000(5) O15 0.042(2) 0.056(3) 0.052(3) -0.002(2) 0.001(2) -0.002(2) O16 0.044(2) 0.069(3) 0.044(3) -0.007(2) -0.0003(19) -0.004(2) C44 0.041(3) 0.058(4) 0.041(3) 0.008(3) 0.010(3) -0.004(3) C45 0.043(3) 0.062(4) 0.047(4) 0.006(3) -0.002(3) -0.003(3) C46 0.059(4) 0.070(5) 0.067(5) -0.002(4) -0.010(4) 0.000(4) C47 0.055(4) 0.070(5) 0.054(4) 0.012(3) 0.000(3) 0.005(3) C48 0.037(3) 0.086(5) 0.074(5) 0.014(4) 0.010(3) -0.003(3) O17 0.041(2) 0.061(3) 0.044(2) 0.0049(19) 0.0198(19) 0.0018(19) O18 0.065(3) 0.050(2) 0.057(3) 0.007(2) 0.022(2) -0.002(2) C49 0.038(3) 0.052(3) 0.046(3) -0.007(3) 0.010(3) -0.004(3) C50 0.041(3) 0.070(4) 0.039(3) -0.006(3) 0.012(3) -0.004(3) C51 0.137(11) 0.113(9) 0.105(9) 0.028(7) 0.079(8) 0.028(8) C52 0.077(6) 0.159(11) 0.081(7) -0.022(7) 0.006(5) 0.038(7) C53 0.083(7) 0.102(8) 0.174(13) -0.081(9) 0.036(8) -0.016(6) O19 0.043(2) 0.086(3) 0.048(3) -0.004(2) 0.020(2) -0.004(2) O20 0.079(4) 0.062(3) 0.064(3) -0.005(3) 0.030(3) 0.006(3) C54 0.038(3) 0.069(4) 0.050(4) 0.004(3) 0.006(3) 0.011(3) C55 0.055(4) 0.080(5) 0.051(4) 0.001(4) 0.026(3) 0.001(4) C56 0.068(5) 0.077(5) 0.061(5) 0.014(4) -0.002(4) 0.001(4) C57 0.043(4) 0.130(8) 0.087(7) 0.037(6) 0.002(4) 0.002(5) C58 0.158(12) 0.095(7) 0.119(10) 0.004(7) 0.106(9) 0.014(8) N61 0.235(16) 0.191(14) 0.101(9) -0.036(9) 0.083(10) -0.088(12) C61 0.115(9) 0.103(8) 0.080(7) 0.004(6) 0.022(6) -0.023(7) C62 0.163(13) 0.143(12) 0.094(9) 0.037(8) 0.054(9) 0.056(10) N62 0.192(15) 0.218(16) 0.092(9) -0.008(10) 0.052(9) 0.025(12) C63 0.101(8) 0.119(10) 0.116(10) 0.033(8) 0.042(8) 0.024(7) C64 0.124(9) 0.108(9) 0.082(8) 0.027(6) 0.010(7) 0.011(7) N63 0.38(3) 0.217(19) 0.168(17) 0.074(15) 0.134(19) 0.130(19) C65 0.215(18) 0.119(11) 0.089(10) 0.001(8) 0.053(11) 0.036(11) C66 0.22(2) 0.210(19) 0.116(12) -0.075(12) 0.074(12) -0.071(16) _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 Tb1 O1 2.305(4) . ? Tb1 O17 2.332(4) . ? Tb1 O10 2.336(4) . ? Tb1 O7 2.393(4) . ? Tb1 O14 2.393(4) . ? Tb1 O6 2.416(4) . ? Tb1 O5 2.446(4) . ? Tb1 N3 2.506(5) . ? Tb2 O3 2.304(4) . ? Tb2 O19 2.323(4) . ? Tb2 O16 2.333(4) . ? Tb2 O12 2.374(4) . ? Tb2 O5 2.382(4) . ? Tb2 O8 2.418(5) . ? Tb2 O7 2.453(4) . ? Tb2 N4 2.491(5) . ? Co1 O11 2.032(5) . ? Co1 O9 2.059(4) . ? Co1 O1 2.087(5) . ? Co1 N1 2.192(5) . ? Co1 O3 2.194(4) . ? Co1 O5 2.211(4) . ? Co2 O13 2.017(5) . ? Co2 O15 2.094(4) . ? Co2 O3 2.101(4) . ? Co2 O7 2.193(4) . ? Co2 N2 2.199(5) . ? Co2 O1 2.215(4) . ? N1 C1 1.355(8) . ? N1 C5 1.360(8) . ? C1 C2 1.401(9) . ? C1 C6 1.512(8) . ? C2 C3 1.393(10) . ? C2 H2A 0.9500 . ? C3 C4 1.388(11) . ? C3 H3A 0.9500 . ? C4 C5 1.384(10) . ? C4 H4A 0.9500 . ? C5 C7 1.500(11) . ? C6 O1 1.376(7) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 O2 1.414(12) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? O2 H2 0.90(4) . ? N2 C8 1.346(9) . ? N2 C12 1.359(8) . ? C8 C9 1.396(10) . ? C8 C13 1.517(9) . ? C9 C10 1.391(12) . ? C9 H9A 0.9500 . ? C10 C11 1.362(12) . ? C10 H10A 0.9500 . ? C11 C12 1.389(11) . ? C11 H11A 0.9500 . ? C12 C14 1.489(11) . ? C13 O3 1.369(7) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 O4 1.422(12) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? O4 H4 0.93(4) . ? N3 C15 1.321(9) . ? N3 C19 1.361(9) . ? C15 C16 1.391(9) . ? C15 C20 1.516(9) . ? C16 C17 1.409(11) . ? C16 H16A 0.9500 . ? C17 C18 1.358(12) . ? C17 H17A 0.9500 . ? C18 C19 1.392(10) . ? C18 H18A 0.9500 . ? C19 C21 1.508(11) . ? C20 O5 1.400(7) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 O6 1.397(8) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? O6 H6 0.91(4) . ? N4 C26 1.332(9) . ? N4 C22 1.337(9) . ? C22 C23 1.399(10) . ? C22 C27 1.493(10) . ? C23 C24 1.397(13) . ? C23 H23A 0.9500 . ? C24 C25 1.363(13) . ? C24 H24A 0.9500 . ? C25 C26 1.394(11) . ? C25 H25A 0.9500 . ? C26 C28 1.510(11) . ? C27 O7 1.388(7) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 O8 1.419(9) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? O8 H8 0.94(4) . ? O9 C29 1.251(8) . ? O10 C29 1.266(7) . ? C29 C30 1.542(9) . ? C30 C31 1.512(11) . ? C30 C33 1.534(13) . ? C30 C32 1.540(11) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? O11 C34 1.265(8) . ? O12 C34 1.264(8) . ? C34 C35 1.546(9) . ? C35 C36 1.522(11) . ? C35 C38 1.527(10) . ? C35 C37 1.542(12) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? O13 C39 1.298(8) . ? O14 C39 1.223(8) . ? C39 C40 1.543(9) . ? C40 C43 1.526(10) . ? C40 C41 1.530(11) . ? C40 C42 1.536(11) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? O15 C44 1.250(8) . ? O16 C44 1.247(8) . ? C44 C45 1.543(9) . ? C45 C46 1.514(11) . ? C45 C48 1.542(10) . ? C45 C47 1.546(10) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? O17 C49 1.260(8) . ? O18 C49 1.272(8) . ? C49 C50 1.526(9) . ? C50 C53 1.500(11) . ? C50 C52 1.502(12) . ? C50 C51 1.513(12) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? O19 C54 1.257(9) . ? O20 C54 1.281(9) . ? C54 C55 1.509(10) . ? C55 C57 1.533(12) . ? C55 C58 1.540(11) . ? C55 C56 1.541(11) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? N61 C61 1.124(13) . ? C61 C62 1.418(14) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? N62 C63 1.171(18) . ? C63 C64 1.510(19) . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? N63 C65 1.047(18) . ? C65 C66 1.38(2) . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? N64A C67A 1.152(17) . ? C67A C68A 1.430(18) . ? C68A H68A 0.9800 . ? C68A H68B 0.9800 . ? C68A H68C 0.9800 . ? N64B C67B 1.154(18) . ? C67B C68B 1.423(18) . ? C68B H68D 0.9800 . ? C68B H68E 0.9800 . ? C68B H68F 0.9800 . ? 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 O1 Tb1 O17 97.16(17) . . ? O1 Tb1 O10 84.67(14) . . ? O17 Tb1 O10 70.51(16) . . ? O1 Tb1 O7 76.40(15) . . ? O17 Tb1 O7 146.24(15) . . ? O10 Tb1 O7 139.72(15) . . ? O1 Tb1 O14 78.86(15) . . ? O17 Tb1 O14 71.66(16) . . ? O10 Tb1 O14 136.17(16) . . ? O7 Tb1 O14 74.58(14) . . ? O1 Tb1 O6 153.09(16) . . ? O17 Tb1 O6 76.41(16) . . ? O10 Tb1 O6 116.44(16) . . ? O7 Tb1 O6 94.34(16) . . ? O14 Tb1 O6 74.31(16) . . ? O1 Tb1 O5 76.23(15) . . ? O17 Tb1 O5 144.63(15) . . ? O10 Tb1 O5 74.27(15) . . ? O7 Tb1 O5 66.88(14) . . ? O14 Tb1 O5 137.87(14) . . ? O6 Tb1 O5 123.75(15) . . ? O1 Tb1 N3 140.42(17) . . ? O17 Tb1 N3 111.70(17) . . ? O10 Tb1 N3 80.39(17) . . ? O7 Tb1 N3 91.96(15) . . ? O14 Tb1 N3 134.87(17) . . ? O6 Tb1 N3 63.81(18) . . ? O5 Tb1 N3 64.49(15) . . ? O3 Tb2 O19 99.62(18) . . ? O3 Tb2 O16 84.32(15) . . ? O19 Tb2 O16 70.70(17) . . ? O3 Tb2 O12 78.95(15) . . ? O19 Tb2 O12 71.68(17) . . ? O16 Tb2 O12 135.26(17) . . ? O3 Tb2 O5 77.02(14) . . ? O19 Tb2 O5 147.51(16) . . ? O16 Tb2 O5 139.40(15) . . ? O12 Tb2 O5 75.99(15) . . ? O3 Tb2 O8 153.03(16) . . ? O19 Tb2 O8 74.79(18) . . ? O16 Tb2 O8 117.13(18) . . ? O12 Tb2 O8 74.24(17) . . ? O5 Tb2 O8 93.53(16) . . ? O3 Tb2 O7 75.55(15) . . ? O19 Tb2 O7 144.33(15) . . ? O16 Tb2 O7 73.65(15) . . ? O12 Tb2 O7 138.64(15) . . ? O5 Tb2 O7 66.93(14) . . ? O8 Tb2 O7 124.27(16) . . ? O3 Tb2 N4 140.04(18) . . ? O19 Tb2 N4 109.63(19) . . ? O16 Tb2 N4 80.49(18) . . ? O12 Tb2 N4 135.46(18) . . ? O5 Tb2 N4 91.11(15) . . ? O8 Tb2 N4 64.07(18) . . ? O7 Tb2 N4 64.76(16) . . ? O11 Co1 O9 89.18(19) . . ? O11 Co1 O1 174.87(19) . . ? O9 Co1 O1 95.95(19) . . ? O11 Co1 N1 102.22(19) . . ? O9 Co1 N1 83.30(19) . . ? O1 Co1 N1 78.65(17) . . ? O11 Co1 O3 92.65(18) . . ? O9 Co1 O3 174.80(16) . . ? O1 Co1 O3 82.22(18) . . ? N1 Co1 O3 101.05(17) . . ? O11 Co1 O5 93.56(17) . . ? O9 Co1 O5 92.07(17) . . ? O1 Co1 O5 86.07(15) . . ? N1 Co1 O5 163.44(18) . . ? O3 Co1 O5 82.97(14) . . ? O13 Co2 O15 89.1(2) . . ? O13 Co2 O3 175.23(18) . . ? O15 Co2 O3 95.52(18) . . ? O13 Co2 O7 93.16(17) . . ? O15 Co2 O7 92.31(17) . . ? O3 Co2 O7 85.55(15) . . ? O13 Co2 N2 101.9(2) . . ? O15 Co2 N2 85.68(19) . . ? O3 Co2 N2 79.66(18) . . ? O7 Co2 N2 164.79(19) . . ? O13 Co2 O1 93.86(18) . . ? O15 Co2 O1 174.13(17) . . ? O3 Co2 O1 81.43(18) . . ? O7 Co2 O1 82.49(14) . . ? N2 Co2 O1 98.64(17) . . ? C1 N1 C5 117.8(6) . . ? C1 N1 Co1 110.5(4) . . ? C5 N1 Co1 130.9(5) . . ? N1 C1 C2 123.3(6) . . ? N1 C1 C6 117.9(5) . . ? C2 C1 C6 118.8(6) . . ? C3 C2 C1 118.3(7) . . ? C3 C2 H2A 120.9 . . ? C1 C2 H2A 120.9 . . ? C4 C3 C2 118.3(6) . . ? C4 C3 H3A 120.9 . . ? C2 C3 H3A 120.9 . . ? C5 C4 C3 120.9(6) . . ? C5 C4 H4A 119.6 . . ? C3 C4 H4A 119.6 . . ? N1 C5 C4 121.5(7) . . ? N1 C5 C7 118.0(6) . . ? C4 C5 C7 120.5(6) . . ? O1 C6 C1 113.7(5) . . ? O1 C6 H6A 108.8 . . ? C1 C6 H6A 108.8 . . ? O1 C6 H6B 108.8 . . ? C1 C6 H6B 108.8 . . ? H6A C6 H6B 107.7 . . ? C6 O1 Co1 113.6(3) . . ? C6 O1 Co2 117.3(4) . . ? Co1 O1 Co2 98.1(2) . . ? C6 O1 Tb1 123.8(4) . . ? Co1 O1 Tb1 100.17(15) . . ? Co2 O1 Tb1 99.70(14) . . ? O2 C7 C5 110.9(7) . . ? O2 C7 H7A 109.5 . . ? C5 C7 H7A 109.5 . . ? O2 C7 H7B 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 108.0 . . ? C7 O2 H2 103(8) . . ? C8 N2 C12 119.6(6) . . ? C8 N2 Co2 109.9(4) . . ? C12 N2 Co2 130.4(5) . . ? N2 C8 C9 121.5(6) . . ? N2 C8 C13 117.9(5) . . ? C9 C8 C13 120.5(6) . . ? C10 C9 C8 118.4(8) . . ? C10 C9 H9A 120.8 . . ? C8 C9 H9A 120.8 . . ? C11 C10 C9 119.7(8) . . ? C11 C10 H10A 120.1 . . ? C9 C10 H10A 120.1 . . ? C10 C11 C12 120.1(7) . . ? C10 C11 H11A 119.9 . . ? C12 C11 H11A 119.9 . . ? N2 C12 C11 120.5(7) . . ? N2 C12 C14 118.6(6) . . ? C11 C12 C14 120.8(7) . . ? O3 C13 C8 114.5(5) . . ? O3 C13 H13A 108.6 . . ? C8 C13 H13A 108.6 . . ? O3 C13 H13B 108.6 . . ? C8 C13 H13B 108.6 . . ? H13A C13 H13B 107.6 . . ? C13 O3 Co2 111.5(3) . . ? C13 O3 Co1 115.1(4) . . ? Co2 O3 Co1 98.3(2) . . ? C13 O3 Tb2 127.3(4) . . ? Co2 O3 Tb2 100.41(14) . . ? Co1 O3 Tb2 99.57(14) . . ? O4 C14 C12 111.1(8) . . ? O4 C14 H14A 109.4 . . ? C12 C14 H14A 109.4 . . ? O4 C14 H14B 109.4 . . ? C12 C14 H14B 109.4 . . ? H14A C14 H14B 108.0 . . ? C14 O4 H4 98(4) . . ? C15 N3 C19 119.9(6) . . ? C15 N3 Tb1 118.2(4) . . ? C19 N3 Tb1 121.9(5) . . ? N3 C15 C16 122.2(7) . . ? N3 C15 C20 116.7(6) . . ? C16 C15 C20 121.1(7) . . ? C15 C16 C17 117.8(7) . . ? C15 C16 H16A 121.1 . . ? C17 C16 H16A 121.1 . . ? C18 C17 C16 119.9(7) . . ? C18 C17 H17A 120.1 . . ? C16 C17 H17A 120.1 . . ? C17 C18 C19 119.3(7) . . ? C17 C18 H18A 120.3 . . ? C19 C18 H18A 120.3 . . ? N3 C19 C18 120.9(7) . . ? N3 C19 C21 116.0(6) . . ? C18 C19 C21 123.1(7) . . ? O5 C20 C15 109.6(5) . . ? O5 C20 H20A 109.7 . . ? C15 C20 H20A 109.7 . . ? O5 C20 H20B 109.7 . . ? C15 C20 H20B 109.7 . . ? H20A C20 H20B 108.2 . . ? C20 O5 Co1 120.5(4) . . ? C20 O5 Tb2 114.8(3) . . ? Co1 O5 Tb2 96.76(15) . . ? C20 O5 Tb1 115.7(3) . . ? Co1 O5 Tb1 92.61(14) . . ? Tb2 O5 Tb1 113.37(16) . . ? O6 C21 C19 110.6(6) . . ? O6 C21 H21A 109.5 . . ? C19 C21 H21A 109.5 . . ? O6 C21 H21B 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 108.1 . . ? C21 O6 Tb1 126.3(4) . . ? C21 O6 H6 109(5) . . ? Tb1 O6 H6 104(5) . . ? C26 N4 C22 118.8(6) . . ? C26 N4 Tb2 123.0(5) . . ? C22 N4 Tb2 118.2(4) . . ? N4 C22 C23 122.0(7) . . ? N4 C22 C27 116.5(6) . . ? C23 C22 C27 121.5(7) . . ? C24 C23 C22 117.9(8) . . ? C24 C23 H23A 121.0 . . ? C22 C23 H23A 121.0 . . ? C25 C24 C23 120.1(8) . . ? C25 C24 H24A 119.9 . . ? C23 C24 H24A 119.9 . . ? C24 C25 C26 118.0(8) . . ? C24 C25 H25A 121.0 . . ? C26 C25 H25A 121.0 . . ? N4 C26 C25 123.1(8) . . ? N4 C26 C28 116.0(6) . . ? C25 C26 C28 120.9(7) . . ? O7 C27 C22 111.1(5) . . ? O7 C27 H27A 109.4 . . ? C22 C27 H27A 109.4 . . ? O7 C27 H27B 109.4 . . ? C22 C27 H27B 109.4 . . ? H27A C27 H27B 108.0 . . ? C27 O7 Co2 121.5(4) . . ? C27 O7 Tb1 113.6(4) . . ? Co2 O7 Tb1 97.69(15) . . ? C27 O7 Tb2 115.4(4) . . ? Co2 O7 Tb2 93.42(15) . . ? Tb1 O7 Tb2 112.75(16) . . ? O8 C28 C26 110.8(6) . . ? O8 C28 H28A 109.5 . . ? C26 C28 H28A 109.5 . . ? O8 C28 H28B 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 108.1 . . ? C28 O8 Tb2 124.8(4) . . ? C28 O8 H8 109(5) . . ? Tb2 O8 H8 105(5) . . ? C29 O9 Co1 125.9(4) . . ? C29 O10 Tb1 136.6(4) . . ? O9 C29 O10 125.8(5) . . ? O9 C29 C30 117.2(6) . . ? O10 C29 C30 117.0(6) . . ? C31 C30 C33 111.1(8) . . ? C31 C30 C32 111.2(8) . . ? C33 C30 C32 108.9(8) . . ? C31 C30 C29 108.5(6) . . ? C33 C30 C29 107.1(7) . . ? C32 C30 C29 110.0(6) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C30 C33 H33A 109.5 . . ? C30 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C34 O11 Co1 125.6(4) . . ? C34 O12 Tb2 138.7(4) . . ? O12 C34 O11 123.9(6) . . ? O12 C34 C35 118.9(6) . . ? O11 C34 C35 117.3(6) . . ? C36 C35 C38 111.4(8) . . ? C36 C35 C37 109.4(7) . . ? C38 C35 C37 111.0(8) . . ? C36 C35 C34 110.7(6) . . ? C38 C35 C34 108.2(6) . . ? C37 C35 C34 105.9(6) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C39 O13 Co2 124.3(4) . . ? C39 O14 Tb1 139.7(4) . . ? O14 C39 O13 124.3(6) . . ? O14 C39 C40 120.4(6) . . ? O13 C39 C40 115.3(6) . . ? C43 C40 C41 110.5(7) . . ? C43 C40 C42 109.9(7) . . ? C41 C40 C42 109.0(6) . . ? C43 C40 C39 109.3(6) . . ? C41 C40 C39 110.2(6) . . ? C42 C40 C39 107.8(6) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C40 C43 H43A 109.5 . . ? C40 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C40 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C44 O15 Co2 124.5(4) . . ? C44 O16 Tb2 139.2(4) . . ? O16 C44 O15 125.2(6) . . ? O16 C44 C45 116.9(6) . . ? O15 C44 C45 117.9(6) . . ? C46 C45 C48 111.6(7) . . ? C46 C45 C44 111.2(6) . . ? C48 C45 C44 107.8(6) . . ? C46 C45 C47 109.7(6) . . ? C48 C45 C47 109.3(7) . . ? C44 C45 C47 107.0(6) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C45 C48 H48A 109.5 . . ? C45 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C45 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C49 O17 Tb1 134.8(4) . . ? O17 C49 O18 123.1(6) . . ? O17 C49 C50 118.8(6) . . ? O18 C49 C50 118.1(6) . . ? C53 C50 C52 111.2(9) . . ? C53 C50 C51 108.9(9) . . ? C52 C50 C51 109.1(9) . . ? C53 C50 C49 106.5(6) . . ? C52 C50 C49 110.1(6) . . ? C51 C50 C49 111.0(7) . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C50 C52 H52A 109.5 . . ? C50 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C50 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C50 C53 H53A 109.5 . . ? C50 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C50 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C54 O19 Tb2 137.7(5) . . ? O19 C54 O20 122.0(7) . . ? O19 C54 C55 118.8(7) . . ? O20 C54 C55 119.2(7) . . ? C54 C55 C57 109.2(7) . . ? C54 C55 C58 111.8(7) . . ? C57 C55 C58 109.7(8) . . ? C54 C55 C56 106.3(6) . . ? C57 C55 C56 109.1(7) . . ? C58 C55 C56 110.7(8) . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C55 C57 H57A 109.5 . . ? C55 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C55 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C55 C58 H58A 109.5 . . ? C55 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C55 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? N61 C61 C62 176.5(16) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? N62 C63 C64 178.3(15) . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? N63 C65 C66 180(3) . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? N64A C67A C68A 168(3) . . ? N64B C67B C68B 164(4) . . ? C67B C68B H68D 109.5 . . ? C67B C68B H68E 109.5 . . ? H68D C68B H68E 109.5 . . ? C67B C68B H68F 109.5 . . ? H68D C68B H68F 109.5 . . ? H68E C68B H68F 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2 O11 0.90(4) 1.93(7) 2.752(7) 151(11) . O4 H4 O13 0.93(4) 1.90(5) 2.776(8) 158(7) . O6 H6 O18 0.91(4) 1.65(4) 2.550(7) 168(8) . O8 H8 O20 0.94(4) 1.59(4) 2.514(7) 165(8) . _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.945 _refine_diff_density_min -2.974 _refine_diff_density_rms 0.179 ######################################################## data_zhao414 _database_code_depnum_ccdc_archive 'CCDC 756453' #TrackingRef 'co2ln2_a1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C58 H86 Co2 Hod2 N4 O20, 4(C2 H3 N)' _chemical_formula_sum 'C66 H98 Co2 Ho2 N8 O20' _chemical_formula_weight 1771.24 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' Co Co 0.3494 0.9721 '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 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.5298(15) _cell_length_b 18.7934(17) _cell_length_c 26.786(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.569(2) _cell_angle_gamma 90.00 _cell_volume 7685.1(12) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 17661 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 28.13 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.531 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3592 _exptl_absorpt_coefficient_mu 2.532 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.537 _exptl_absorpt_correction_T_max 0.620 _exptl_absorpt_process_details 'SADABS 2.10 (Bruker AXS Inc., 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART Apex' _diffrn_measurement_method 'CCD area detector' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46990 _diffrn_reflns_av_R_equivalents 0.0185 _diffrn_reflns_av_sigmaI/netI 0.0203 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 28.15 _reflns_number_total 17309 _reflns_number_gt 16269 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT 5.6 (Bruker AXS Inc., 2005)' _computing_cell_refinement 'SMART-NT 5.6 (Bruker AXS Inc., 2005)' _computing_data_reduction 'SAINT+ 6.45 (Bruker AXS Inc., 2003)' _computing_structure_solution 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_structure_refinement 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_molecular_graphics 'Diamond 2.1 (Crystal Impact, 1998)' _computing_publication_material 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _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. The cubane complex appears to show a slight two-fold "whole molecule" disorder, corresponding to inversion of the molecule about its centroid, which could be modelled using "ghost" Ho and Co atoms of 1.3% occupancy. These ghost atoms formed a Co2Ho2 core with a very similar geometry to that in the primary structure. No attempt was made to locate the ligand atoms of the very minor component. Some pivalate t-butyl groups and lattice MeCN were disordered, and refined using half atoms with geoemtrical restraints as appropriate. ; _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^)+(0.0274P)^2^+12.6114P] 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 17309 _refine_ls_number_parameters 934 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0300 _refine_ls_R_factor_gt 0.0275 _refine_ls_wR_factor_ref 0.0657 _refine_ls_wR_factor_gt 0.0645 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ho1 Ho 0.421676(7) 0.191159(6) 0.291438(4) 0.01635(3) Uani 0.99 1 d D A 1 Ho2 Ho 0.618568(8) 0.206851(6) 0.215057(4) 0.01763(3) Uani 0.99 1 d D A 1 Co1 Co 0.43341(2) 0.308659(17) 0.198943(12) 0.01640(7) Uani 0.99 1 d D A 1 Co2 Co 0.57629(2) 0.323563(18) 0.302863(12) 0.01744(7) Uani 0.99 1 d D A 1 Ho1X Ho 0.4054(7) 0.3009(5) 0.2907(4) 0.0156(13) Uiso 0.01 1 d PD A 2 Ho2X Ho 0.6016(7) 0.3144(5) 0.2141(4) 0.0156(13) Uiso 0.01 1 d PD A 2 Co1X Co 0.4451(18) 0.1859(14) 0.2003(11) 0.0156(13) Uiso 0.01 1 d PD A 2 Co2X Co 0.5876(17) 0.1948(16) 0.3065(11) 0.0156(13) Uiso 0.01 1 d PD A 2 N1 N 0.38732(15) 0.41725(11) 0.20925(8) 0.0212(4) Uani 1 1 d . . . C1 C 0.36243(17) 0.42313(14) 0.25457(10) 0.0212(5) Uani 1 1 d . . . C2 C 0.31997(19) 0.48304(15) 0.26875(11) 0.0269(6) Uani 1 1 d . . . H2A H 0.3040 0.4856 0.3013 0.032 Uiso 1 1 calc R . . C3 C 0.3013(2) 0.53864(16) 0.23474(12) 0.0325(7) Uani 1 1 d . . . H3A H 0.2725 0.5802 0.2434 0.039 Uiso 1 1 calc R . . C4 C 0.3257(2) 0.53245(15) 0.18787(12) 0.0311(6) Uani 1 1 d . . . H4A H 0.3131 0.5698 0.1637 0.037 Uiso 1 1 calc R . . C5 C 0.36852(19) 0.47176(15) 0.17604(11) 0.0267(6) Uani 1 1 d . . . C6 C 0.37850(18) 0.36101(14) 0.29066(10) 0.0227(5) Uani 1 1 d . . . H6A H 0.4031 0.3788 0.3251 0.027 Uiso 1 1 calc R . . H6B H 0.3220 0.3376 0.2921 0.027 Uiso 1 1 calc R . . O1 O 0.43671(13) 0.31030(9) 0.27606(7) 0.0177(4) Uani 1 1 d . . . C7 C 0.3935(2) 0.46419(17) 0.12462(12) 0.0358(7) Uani 1 1 d . . . H7A H 0.3939 0.5118 0.1088 0.043 Uiso 1 1 calc R . . H7B H 0.4535 0.4444 0.1287 0.043 Uiso 1 1 calc R . . O2 O 0.33474(18) 0.41912(13) 0.09202(9) 0.0432(6) Uani 1 1 d D . . H2 H 0.355(3) 0.3787(18) 0.0998(17) 0.065 Uiso 1 1 d D . . N2 N 0.58644(15) 0.43735(11) 0.28790(8) 0.0214(4) Uani 1 1 d . . . C8 C 0.59935(18) 0.44798(14) 0.24037(11) 0.0242(5) Uani 1 1 d . . . C9 C 0.6075(2) 0.51560(16) 0.22044(13) 0.0373(7) Uani 1 1 d . . . H9A H 0.6150 0.5215 0.1863 0.045 Uiso 1 1 calc R . . C10 C 0.6043(3) 0.57390(17) 0.25149(14) 0.0451(9) Uani 1 1 d . . . H10A H 0.6095 0.6206 0.2389 0.054 Uiso 1 1 calc R . . C11 C 0.5936(2) 0.56365(16) 0.30060(13) 0.0374(7) Uani 1 1 d . . . H11A H 0.5926 0.6032 0.3225 0.045 Uiso 1 1 calc R . . C12 C 0.5843(2) 0.49504(15) 0.31815(11) 0.0279(6) Uani 1 1 d . . . C13 C 0.61005(18) 0.38301(13) 0.20854(10) 0.0210(5) Uani 1 1 d . . . H13A H 0.5828 0.3924 0.1728 0.025 Uiso 1 1 calc R . . H13B H 0.6732 0.3741 0.2097 0.025 Uiso 1 1 calc R . . O3 O 0.57147(13) 0.32192(9) 0.22566(7) 0.0179(4) Uani 1 1 d . . . C14 C 0.5756(3) 0.48264(17) 0.37240(12) 0.0423(8) Uani 1 1 d . . . H14A H 0.5650 0.5287 0.3882 0.051 Uiso 1 1 calc R . . H14B H 0.5244 0.4516 0.3733 0.051 Uiso 1 1 calc R . . O4 O 0.6514(2) 0.45056(14) 0.40079(10) 0.0569(8) Uani 1 1 d D . . H4 H 0.646(3) 0.4042(18) 0.3976(19) 0.085 Uiso 1 1 d D . . N3 N 0.42537(15) 0.07430(11) 0.24923(9) 0.0221(5) Uani 1 1 d . . . C15 C 0.42319(18) 0.07324(14) 0.19875(10) 0.0229(5) Uani 1 1 d . . . C16 C 0.4189(2) 0.00962(15) 0.17186(12) 0.0315(6) Uani 1 1 d . . . H16A H 0.4159 0.0096 0.1361 0.038 Uiso 1 1 calc R . . C17 C 0.4192(2) -0.05384(16) 0.19836(14) 0.0404(8) Uani 1 1 d . . . H17A H 0.4159 -0.0979 0.1807 0.048 Uiso 1 1 calc R . . C18 C 0.4243(2) -0.05297(16) 0.25027(13) 0.0368(7) Uani 1 1 d . . . H18A H 0.4267 -0.0961 0.2690 0.044 Uiso 1 1 calc R . . C19 C 0.42584(19) 0.01228(15) 0.27459(12) 0.0281(6) Uani 1 1 d . . . C20 C 0.42570(18) 0.14490(14) 0.17321(10) 0.0220(5) Uani 1 1 d . . . H20A H 0.4587 0.1409 0.1450 0.026 Uiso 1 1 calc R . . H20B H 0.3653 0.1604 0.1588 0.026 Uiso 1 1 calc R . . O5 O 0.46643(12) 0.19603(11) 0.20899(7) 0.0180(4) Uani 1 1 d . . . C21 C 0.4278(2) 0.01821(14) 0.33057(12) 0.0300(6) Uani 1 1 d . . . H21A H 0.3724 -0.0004 0.3387 0.036 Uiso 1 1 calc R . . H21B H 0.4766 -0.0108 0.3491 0.036 Uiso 1 1 calc R . . O6 O 0.43891(14) 0.09014(10) 0.34644(8) 0.0278(4) Uani 1 1 d D . . H6 H 0.400(2) 0.0970(18) 0.3664(12) 0.033 Uiso 1 1 d D . . N4 N 0.64436(15) 0.09442(12) 0.26340(9) 0.0238(5) Uani 1 1 d . . . C22 C 0.64621(18) 0.09629(15) 0.31365(11) 0.0256(6) Uani 1 1 d . . . C23 C 0.6655(2) 0.03613(17) 0.34382(13) 0.0373(7) Uani 1 1 d . . . H23A H 0.6673 0.0383 0.3794 0.045 Uiso 1 1 calc R . . C24 C 0.6819(3) -0.02705(18) 0.32074(15) 0.0466(9) Uani 1 1 d . . . H24A H 0.6959 -0.0688 0.3406 0.056 Uiso 1 1 calc R . . C25 C 0.6780(2) -0.02936(17) 0.26918(14) 0.0383(7) Uani 1 1 d . . . H25A H 0.6878 -0.0727 0.2529 0.046 Uiso 1 1 calc R . . C26 C 0.65935(19) 0.03272(15) 0.24119(12) 0.0295(6) Uani 1 1 d . . . C27 C 0.62503(18) 0.16625(14) 0.33544(10) 0.0233(5) Uani 1 1 d . . . H27A H 0.5930 0.1579 0.3636 0.028 Uiso 1 1 calc R . . H27B H 0.6800 0.1918 0.3493 0.028 Uiso 1 1 calc R . . O7 O 0.57299(13) 0.20853(11) 0.29745(8) 0.0186(4) Uani 1 1 d . . . C28 C 0.6546(2) 0.03472(15) 0.18490(12) 0.0313(6) Uani 1 1 d . . . H28A H 0.7126 0.0227 0.1769 0.038 Uiso 1 1 calc R . . H28B H 0.6120 -0.0013 0.1686 0.038 Uiso 1 1 calc R . . O8 O 0.62875(15) 0.10281(11) 0.16520(8) 0.0308(5) Uani 1 1 d D . . H8 H 0.660(2) 0.1131(19) 0.1424(12) 0.037 Uiso 1 1 d D . . O9 O 0.30219(12) 0.28778(10) 0.17808(7) 0.0238(4) Uani 1 1 d . . . O10 O 0.29294(12) 0.19866(10) 0.23194(7) 0.0226(4) Uani 1 1 d . . . C29 C 0.26078(17) 0.23938(14) 0.19590(9) 0.0208(5) Uani 1 1 d . . . C30 C 0.1646(2) 0.22787(19) 0.17140(12) 0.0335(7) Uani 1 1 d . . . C31 C 0.1104(2) 0.2212(2) 0.21345(14) 0.0505(10) Uani 1 1 d . . . H31A H 0.1145 0.2655 0.2330 0.076 Uiso 1 1 calc R . . H31B H 0.1331 0.1818 0.2360 0.076 Uiso 1 1 calc R . . H31C H 0.0491 0.2120 0.1983 0.076 Uiso 1 1 calc R . . C32 C 0.1314(2) 0.2893(2) 0.13542(13) 0.0457(9) Uani 1 1 d . . . H32A H 0.1356 0.3340 0.1546 0.069 Uiso 1 1 calc R . . H32B H 0.0702 0.2807 0.1197 0.069 Uiso 1 1 calc R . . H32C H 0.1672 0.2927 0.1090 0.069 Uiso 1 1 calc R . . C33 C 0.1599(3) 0.1579(2) 0.14105(14) 0.0556(11) Uani 1 1 d . . . H33A H 0.0992 0.1489 0.1246 0.083 Uiso 1 1 calc R . . H33B H 0.1809 0.1186 0.1641 0.083 Uiso 1 1 calc R . . H33C H 0.1967 0.1618 0.1151 0.083 Uiso 1 1 calc R . . O11 O 0.44409(13) 0.30872(10) 0.12470(7) 0.0233(4) Uani 1 1 d . . . O12 O 0.56021(13) 0.23771(10) 0.13001(7) 0.0242(4) Uani 1 1 d . . . C34 C 0.49517(17) 0.26845(14) 0.10522(10) 0.0214(5) Uani 1 1 d . . . C35 C 0.47344(19) 0.25954(17) 0.04715(10) 0.0286(6) Uani 1 1 d . . . C36 C 0.5273(2) 0.19881(19) 0.03032(12) 0.0378(7) Uani 1 1 d . . . H36A H 0.5127 0.1937 -0.0067 0.057 Uiso 1 1 calc R . . H36B H 0.5137 0.1544 0.0464 0.057 Uiso 1 1 calc R . . H36C H 0.5898 0.2094 0.0405 0.057 Uiso 1 1 calc R . . C37 C 0.4966(2) 0.3301(2) 0.02396(12) 0.0405(8) Uani 1 1 d . . . H37A H 0.4622 0.3686 0.0352 0.061 Uiso 1 1 calc R . . H37B H 0.4831 0.3267 -0.0132 0.061 Uiso 1 1 calc R . . H37C H 0.5591 0.3399 0.0350 0.061 Uiso 1 1 calc R . . C38 C 0.3757(2) 0.2438(2) 0.03081(13) 0.0478(9) Uani 1 1 d . . . H38A H 0.3416 0.2832 0.0411 0.072 Uiso 1 1 calc R . . H38B H 0.3612 0.1998 0.0470 0.072 Uiso 1 1 calc R . . H38C H 0.3618 0.2384 -0.0062 0.072 Uiso 1 1 calc R . . O13 O 0.56735(13) 0.32323(10) 0.37710(7) 0.0245(4) Uani 1 1 d . . . O14 O 0.47184(12) 0.23414(10) 0.37527(7) 0.0226(4) Uani 1 1 d . . . C39 C 0.52913(17) 0.27452(14) 0.39847(10) 0.0218(5) Uani 1 1 d . . . C40 C 0.55765(19) 0.26727(17) 0.45618(10) 0.0270(6) Uani 1 1 d . . . C41 C 0.5202(2) 0.19925(17) 0.47504(11) 0.0327(7) Uani 1 1 d . . . H41A H 0.4561 0.2007 0.4667 0.049 Uiso 1 1 calc R . . H41B H 0.5389 0.1955 0.5119 0.049 Uiso 1 1 calc R . . H41C H 0.5416 0.1579 0.4586 0.049 Uiso 1 1 calc R . . C42 C 0.5237(2) 0.33260(18) 0.48076(11) 0.0358(7) Uani 1 1 d . . . H42A H 0.4595 0.3335 0.4725 0.054 Uiso 1 1 calc R . . H42B H 0.5470 0.3759 0.4678 0.054 Uiso 1 1 calc R . . H42C H 0.5427 0.3302 0.5177 0.054 Uiso 1 1 calc R . . C43 C 0.6576(2) 0.2657(2) 0.46939(12) 0.0453(9) Uani 1 1 d . . . H43A H 0.6761 0.2610 0.5062 0.068 Uiso 1 1 calc R . . H43B H 0.6812 0.3099 0.4579 0.068 Uiso 1 1 calc R . . H43C H 0.6796 0.2251 0.4525 0.068 Uiso 1 1 calc R . . O15 O 0.71203(13) 0.32638(10) 0.32364(7) 0.0254(4) Uani 1 1 d . . . O16 O 0.74080(12) 0.23838(11) 0.27343(7) 0.0258(4) Uani 1 1 d . . . C44 C 0.76279(18) 0.28193(15) 0.30927(10) 0.0226(5) Uani 1 1 d . . . C45 C 0.85878(18) 0.27849(15) 0.33706(11) 0.0253(6) Uani 1 1 d . . . C46 C 0.8787(2) 0.33771(17) 0.37661(12) 0.0359(7) Uani 1 1 d . . . H46A H 0.8694 0.3841 0.3597 0.054 Uiso 1 1 calc R . . H46B H 0.9397 0.3339 0.3941 0.054 Uiso 1 1 calc R . . H46C H 0.8397 0.3331 0.4014 0.054 Uiso 1 1 calc R . . C47 C 0.8732(2) 0.20601(16) 0.36377(12) 0.0309(6) Uani 1 1 d . . . H47A H 0.8614 0.1679 0.3385 0.046 Uiso 1 1 calc R . . H47B H 0.8336 0.2013 0.3881 0.046 Uiso 1 1 calc R . . H47C H 0.9340 0.2025 0.3818 0.046 Uiso 1 1 calc R . . C48 C 0.9178(2) 0.28485(18) 0.29746(12) 0.0346(7) Uani 1 1 d . . . H48A H 0.9036 0.2468 0.2723 0.052 Uiso 1 1 calc R . . H48B H 0.9792 0.2807 0.3142 0.052 Uiso 1 1 calc R . . H48C H 0.9084 0.3312 0.2805 0.052 Uiso 1 1 calc R . . O17 O 0.30324(13) 0.20004(10) 0.33275(7) 0.0248(4) Uani 1 1 d . . . O18 O 0.32652(14) 0.12679(11) 0.39910(7) 0.0293(4) Uani 1 1 d . . . C49 C 0.28983(18) 0.17937(15) 0.37560(10) 0.0233(5) Uani 1 1 d . A . C50 C 0.22323(19) 0.22234(17) 0.39956(11) 0.0275(6) Uani 1 1 d D . . C51A C 0.1933(4) 0.1765(3) 0.44070(19) 0.0430(12) Uani 0.71 1 d P A 1 H51A H 0.2440 0.1646 0.4670 0.065 Uiso 0.71 1 calc PR A 1 H51B H 0.1665 0.1326 0.4254 0.065 Uiso 0.71 1 calc PR A 1 H51C H 0.1504 0.2029 0.4560 0.065 Uiso 0.71 1 calc PR A 1 C52A C 0.1461(3) 0.2417(3) 0.35930(17) 0.0422(12) Uani 0.71 1 d P A 1 H52A H 0.1157 0.1982 0.3456 0.063 Uiso 0.71 1 calc PR A 1 H52B H 0.1664 0.2676 0.3319 0.063 Uiso 0.71 1 calc PR A 1 H52C H 0.1058 0.2718 0.3741 0.063 Uiso 0.71 1 calc PR A 1 C53A C 0.2717(3) 0.2883(3) 0.4222(2) 0.0472(14) Uani 0.71 1 d P A 1 H53A H 0.3216 0.2742 0.4483 0.071 Uiso 0.71 1 calc PR A 1 H53B H 0.2320 0.3184 0.4374 0.071 Uiso 0.71 1 calc PR A 1 H53C H 0.2930 0.3149 0.3953 0.071 Uiso 0.71 1 calc PR A 1 C51B C 0.1529(12) 0.1782(10) 0.4150(7) 0.084(6) Uiso 0.29 1 d PD A 2 H51D H 0.1128 0.2090 0.4295 0.127 Uiso 0.29 1 calc PR A 2 H51E H 0.1792 0.1433 0.4405 0.127 Uiso 0.29 1 calc PR A 2 H51F H 0.1204 0.1534 0.3853 0.127 Uiso 0.29 1 calc PR A 2 C52B C 0.1759(12) 0.2815(9) 0.3646(7) 0.077(5) Uiso 0.29 1 d PD A 2 H52D H 0.1350 0.3067 0.3822 0.115 Uiso 0.29 1 calc PR A 2 H52E H 0.1435 0.2600 0.3334 0.115 Uiso 0.29 1 calc PR A 2 H52F H 0.2192 0.3151 0.3560 0.115 Uiso 0.29 1 calc PR A 2 C53B C 0.2705(12) 0.2619(9) 0.4455(6) 0.072(6) Uiso 0.29 1 d PD A 2 H53D H 0.2281 0.2893 0.4607 0.108 Uiso 0.29 1 calc PR A 2 H53E H 0.3135 0.2944 0.4353 0.108 Uiso 0.29 1 calc PR A 2 H53F H 0.3006 0.2278 0.4705 0.108 Uiso 0.29 1 calc PR A 2 O19 O 0.73336(13) 0.23064(12) 0.17349(7) 0.0291(4) Uani 1 1 d . . . O20 O 0.73558(16) 0.15000(11) 0.11332(8) 0.0359(5) Uani 1 1 d . . . C54 C 0.75758(19) 0.20855(16) 0.13392(11) 0.0282(6) Uani 1 1 d . . . C55 C 0.8166(2) 0.25901(17) 0.10985(11) 0.0307(6) Uani 1 1 d . . . C56 C 0.7568(2) 0.31713(18) 0.08253(13) 0.0398(8) Uani 1 1 d . . . H56A H 0.7282 0.3423 0.1071 0.060 Uiso 1 1 calc R . . H56B H 0.7122 0.2955 0.0563 0.060 Uiso 1 1 calc R . . H56C H 0.7918 0.3509 0.0667 0.060 Uiso 1 1 calc R . . C57 C 0.8846(2) 0.2930(2) 0.15157(13) 0.0416(8) Uani 1 1 d . . . H57A H 0.9238 0.2560 0.1687 0.062 Uiso 1 1 calc R . . H57B H 0.8548 0.3165 0.1763 0.062 Uiso 1 1 calc R . . H57C H 0.9188 0.3281 0.1365 0.062 Uiso 1 1 calc R . . C58 C 0.8638(3) 0.2188(2) 0.07334(16) 0.0598(12) Uani 1 1 d . . . H58A H 0.9006 0.1815 0.0919 0.090 Uiso 1 1 calc R . . H58B H 0.9006 0.2520 0.0583 0.090 Uiso 1 1 calc R . . H58C H 0.8206 0.1972 0.0464 0.090 Uiso 1 1 calc R . . N61 N 0.4173(4) 0.4733(3) -0.08634(17) 0.1002(19) Uani 1 1 d . . . C61 C 0.3878(3) 0.4896(2) -0.05417(15) 0.0546(10) Uani 1 1 d . . . C62 C 0.3504(3) 0.5127(2) -0.01109(17) 0.0627(12) Uani 1 1 d . . . H62A H 0.3905 0.5461 0.0095 0.094 Uiso 1 1 calc R . . H62B H 0.3411 0.4713 0.0096 0.094 Uiso 1 1 calc R . . H62C H 0.2942 0.5363 -0.0233 0.094 Uiso 1 1 calc R . . N62 N 0.4025(3) 0.0258(3) 0.54828(16) 0.0840(14) Uani 1 1 d . . . C63 C 0.3872(3) 0.0027(3) 0.50788(17) 0.0565(11) Uani 1 1 d . . . C64 C 0.3688(3) -0.0254(2) 0.45617(15) 0.0534(10) Uani 1 1 d . . . H64A H 0.4224 -0.0456 0.4477 0.080 Uiso 1 1 calc R . . H64B H 0.3477 0.0131 0.4324 0.080 Uiso 1 1 calc R . . H64C H 0.3238 -0.0625 0.4538 0.080 Uiso 1 1 calc R . . N63 N 0.3538(6) 0.4769(4) 0.4025(2) 0.160(4) Uani 1 1 d . . . C65 C 0.3505(5) 0.4753(3) 0.4414(2) 0.090(2) Uani 1 1 d . . . C66 C 0.3419(5) 0.4695(4) 0.4931(2) 0.103(2) Uani 1 1 d . . . H66A H 0.3999 0.4627 0.5142 0.154 Uiso 1 1 calc R . . H66B H 0.3046 0.4286 0.4972 0.154 Uiso 1 1 calc R . . H66C H 0.3154 0.5130 0.5035 0.154 Uiso 1 1 calc R . . N64A N 0.5852(10) 0.0403(8) -0.0466(5) 0.105(4) Uani 0.50 1 d P B 1 C67A C 0.6061(18) 0.0260(8) -0.0057(9) 0.068(4) Uani 0.50 1 d P B 1 C68A C 0.639(4) 0.014(3) 0.0467(18) 0.059(5) Uani 0.50 1 d P B 1 H68A H 0.6703 -0.0312 0.0511 0.088 Uiso 0.50 1 calc PR B 1 H68B H 0.5907 0.0137 0.0654 0.088 Uiso 0.50 1 calc PR B 1 H68C H 0.6799 0.0529 0.0598 0.088 Uiso 0.50 1 calc PR B 1 N64B N 0.5934(10) -0.0142(7) -0.0428(4) 0.105(4) Uani 0.50 1 d P C 2 C67B C 0.6140(18) -0.0042(8) 0.0000(9) 0.068(4) Uani 0.50 1 d P C 2 C68B C 0.634(4) 0.007(3) 0.0551(19) 0.059(5) Uani 0.50 1 d P C 2 H68D H 0.6334 0.0582 0.0623 0.088 Uiso 0.50 1 calc PR C 2 H68E H 0.6924 -0.0122 0.0687 0.088 Uiso 0.50 1 calc PR C 2 H68F H 0.5903 -0.0171 0.0710 0.088 Uiso 0.50 1 calc PR C 2 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 0.01747(6) 0.01602(6) 0.01586(6) 0.00193(4) 0.00381(4) -0.00007(4) Ho2 0.01688(6) 0.01904(6) 0.01711(6) -0.00064(4) 0.00345(4) 0.00056(4) Co1 0.01700(16) 0.01781(16) 0.01461(15) 0.00195(12) 0.00346(12) 0.00040(12) Co2 0.01937(17) 0.01779(16) 0.01493(16) 0.00009(12) 0.00255(13) -0.00053(13) N1 0.0208(11) 0.0197(10) 0.0230(11) 0.0040(9) 0.0039(9) 0.0022(9) C1 0.0178(12) 0.0203(12) 0.0247(13) 0.0019(10) 0.0021(10) 0.0009(10) C2 0.0268(14) 0.0233(13) 0.0322(15) -0.0002(11) 0.0094(12) 0.0054(11) C3 0.0290(16) 0.0234(14) 0.0459(18) 0.0015(13) 0.0086(13) 0.0095(12) C4 0.0299(15) 0.0240(14) 0.0393(17) 0.0111(12) 0.0062(13) 0.0074(12) C5 0.0275(14) 0.0246(13) 0.0278(14) 0.0071(11) 0.0042(11) 0.0033(11) C6 0.0278(14) 0.0211(12) 0.0211(12) -0.0008(10) 0.0092(11) 0.0050(10) O1 0.0204(9) 0.0173(9) 0.0157(9) 0.0005(7) 0.0039(8) 0.0029(7) C7 0.0463(19) 0.0306(15) 0.0328(16) 0.0134(13) 0.0132(14) 0.0100(14) O2 0.0561(16) 0.0430(14) 0.0274(11) 0.0083(10) -0.0009(11) 0.0182(12) N2 0.0229(11) 0.0187(10) 0.0222(11) -0.0025(8) 0.0028(9) -0.0025(9) C8 0.0239(14) 0.0215(13) 0.0269(14) 0.0000(10) 0.0041(11) -0.0030(10) C9 0.055(2) 0.0239(14) 0.0363(17) 0.0036(12) 0.0165(15) -0.0041(14) C10 0.072(3) 0.0192(14) 0.049(2) 0.0037(14) 0.0220(19) -0.0025(15) C11 0.051(2) 0.0212(14) 0.0423(18) -0.0067(13) 0.0143(16) -0.0015(13) C12 0.0318(15) 0.0229(13) 0.0288(14) -0.0041(11) 0.0049(12) -0.0014(11) C13 0.0253(13) 0.0172(12) 0.0218(12) 0.0002(10) 0.0074(10) -0.0054(10) O3 0.0193(10) 0.0187(9) 0.0155(9) 0.0012(7) 0.0023(7) -0.0031(7) C14 0.070(3) 0.0277(15) 0.0305(16) -0.0087(13) 0.0129(16) -0.0061(16) O4 0.091(2) 0.0328(13) 0.0363(14) -0.0052(11) -0.0158(14) -0.0114(14) N3 0.0212(11) 0.0170(10) 0.0289(12) -0.0005(9) 0.0071(9) -0.0007(8) C15 0.0200(13) 0.0212(12) 0.0285(14) -0.0045(10) 0.0067(11) -0.0010(10) C16 0.0344(16) 0.0257(14) 0.0361(16) -0.0104(12) 0.0108(13) -0.0028(12) C17 0.050(2) 0.0201(14) 0.054(2) -0.0113(14) 0.0165(17) -0.0049(13) C18 0.0424(19) 0.0180(13) 0.053(2) 0.0017(13) 0.0171(16) 0.0005(12) C19 0.0276(15) 0.0205(13) 0.0374(16) 0.0024(11) 0.0094(12) 0.0023(11) C20 0.0249(14) 0.0232(13) 0.0180(12) -0.0054(10) 0.0041(10) -0.0031(10) O5 0.0186(11) 0.0184(9) 0.0165(10) -0.0024(7) 0.0018(8) -0.0014(7) C21 0.0347(16) 0.0184(12) 0.0398(16) 0.0075(12) 0.0143(13) 0.0011(11) O6 0.0362(12) 0.0209(9) 0.0291(10) 0.0050(8) 0.0132(9) 0.0025(8) N4 0.0171(11) 0.0216(11) 0.0327(12) 0.0025(9) 0.0050(9) 0.0034(9) C22 0.0195(13) 0.0249(13) 0.0322(15) 0.0067(11) 0.0045(11) 0.0040(11) C23 0.0391(18) 0.0348(16) 0.0378(17) 0.0146(14) 0.0065(14) 0.0121(14) C24 0.049(2) 0.0284(16) 0.061(2) 0.0185(16) 0.0072(18) 0.0168(15) C25 0.0340(17) 0.0248(15) 0.056(2) 0.0026(14) 0.0068(15) 0.0073(13) C26 0.0210(14) 0.0231(13) 0.0443(17) -0.0021(12) 0.0060(12) 0.0038(11) C27 0.0215(13) 0.0256(13) 0.0219(13) 0.0085(10) 0.0016(10) 0.0025(11) O7 0.0187(10) 0.0194(11) 0.0169(10) 0.0040(7) 0.0011(8) 0.0018(7) C28 0.0303(16) 0.0224(13) 0.0430(17) -0.0059(12) 0.0115(13) 0.0028(12) O8 0.0385(12) 0.0239(10) 0.0327(11) -0.0035(8) 0.0143(9) 0.0012(9) O9 0.0202(9) 0.0267(10) 0.0240(10) 0.0040(8) 0.0027(8) -0.0002(8) O10 0.0188(9) 0.0284(10) 0.0203(9) 0.0023(7) 0.0027(7) -0.0009(7) C29 0.0175(12) 0.0280(13) 0.0170(12) -0.0015(10) 0.0037(10) 0.0014(10) C30 0.0201(14) 0.0504(19) 0.0279(15) 0.0121(14) -0.0011(11) -0.0057(13) C31 0.0205(16) 0.083(3) 0.049(2) 0.033(2) 0.0099(15) 0.0046(17) C32 0.0218(16) 0.075(3) 0.0379(19) 0.0237(18) -0.0013(13) 0.0030(16) C33 0.056(2) 0.065(3) 0.038(2) 0.0006(18) -0.0111(17) -0.031(2) O11 0.0270(10) 0.0270(10) 0.0164(9) 0.0026(7) 0.0054(8) 0.0026(8) O12 0.0231(10) 0.0322(10) 0.0178(9) 0.0000(8) 0.0054(7) 0.0018(8) C34 0.0197(13) 0.0272(13) 0.0176(12) 0.0007(10) 0.0042(10) -0.0064(10) C35 0.0246(14) 0.0449(17) 0.0154(13) -0.0039(11) 0.0011(10) 0.0021(12) C36 0.0377(18) 0.052(2) 0.0226(15) -0.0118(13) 0.0034(13) 0.0058(15) C37 0.045(2) 0.056(2) 0.0217(15) 0.0117(14) 0.0108(14) 0.0114(16) C38 0.0268(17) 0.083(3) 0.0303(17) -0.0191(17) -0.0045(13) -0.0014(17) O13 0.0303(11) 0.0258(9) 0.0174(9) -0.0008(7) 0.0047(8) -0.0035(8) O14 0.0230(10) 0.0283(10) 0.0171(9) 0.0026(7) 0.0052(7) -0.0023(8) C39 0.0202(13) 0.0269(13) 0.0188(12) 0.0003(10) 0.0051(10) 0.0040(10) C40 0.0240(14) 0.0395(16) 0.0168(13) 0.0019(11) 0.0017(10) 0.0003(12) C41 0.0407(18) 0.0376(16) 0.0190(14) 0.0076(12) 0.0030(12) 0.0010(13) C42 0.0445(19) 0.0432(18) 0.0204(14) -0.0066(13) 0.0081(13) -0.0065(15) C43 0.0252(16) 0.082(3) 0.0261(16) 0.0070(16) -0.0011(13) -0.0001(17) O15 0.0224(10) 0.0259(10) 0.0266(10) 0.0002(8) 0.0013(8) -0.0018(8) O16 0.0202(10) 0.0339(11) 0.0230(10) -0.0016(8) 0.0029(8) -0.0019(8) C44 0.0195(13) 0.0273(13) 0.0200(12) 0.0055(10) 0.0007(10) -0.0027(10) C45 0.0192(13) 0.0292(14) 0.0257(14) 0.0043(11) -0.0010(11) -0.0019(11) C46 0.0336(17) 0.0336(16) 0.0347(17) 0.0001(13) -0.0091(13) -0.0039(13) C47 0.0283(15) 0.0311(15) 0.0307(15) 0.0079(12) -0.0010(12) 0.0038(12) C48 0.0202(14) 0.0447(18) 0.0374(17) 0.0090(14) 0.0013(12) -0.0032(13) O17 0.0214(10) 0.0344(11) 0.0193(9) 0.0022(8) 0.0056(8) -0.0001(8) O18 0.0354(12) 0.0268(10) 0.0283(10) 0.0042(8) 0.0128(9) -0.0029(9) C49 0.0189(13) 0.0300(14) 0.0213(13) -0.0034(11) 0.0047(10) -0.0065(11) C50 0.0225(14) 0.0391(16) 0.0221(13) -0.0026(12) 0.0073(11) -0.0034(12) C51A 0.052(3) 0.054(3) 0.032(3) 0.009(2) 0.032(2) 0.011(2) C52A 0.029(2) 0.071(4) 0.026(2) -0.005(2) 0.0032(18) 0.023(2) C53A 0.032(3) 0.043(3) 0.071(4) -0.034(3) 0.021(3) -0.006(2) O19 0.0237(10) 0.0416(12) 0.0231(10) -0.0037(9) 0.0074(8) -0.0029(9) O20 0.0443(13) 0.0315(11) 0.0366(12) -0.0021(9) 0.0197(10) 0.0023(10) C54 0.0251(14) 0.0353(15) 0.0246(14) 0.0038(12) 0.0057(11) 0.0083(12) C55 0.0307(16) 0.0355(16) 0.0288(15) 0.0031(12) 0.0129(12) 0.0051(13) C56 0.0403(19) 0.0412(18) 0.0339(17) 0.0086(14) -0.0032(14) -0.0045(15) C57 0.0231(16) 0.059(2) 0.0417(19) 0.0136(16) 0.0038(14) -0.0030(15) C58 0.084(3) 0.051(2) 0.062(3) -0.0030(19) 0.056(3) -0.001(2) N61 0.140(5) 0.111(4) 0.062(3) -0.026(3) 0.051(3) -0.063(3) C61 0.068(3) 0.061(3) 0.035(2) 0.0007(17) 0.0081(19) -0.020(2) C62 0.073(3) 0.063(3) 0.058(3) 0.023(2) 0.031(2) 0.016(2) N62 0.079(3) 0.124(4) 0.053(2) 0.004(2) 0.023(2) 0.018(3) C63 0.041(2) 0.074(3) 0.057(3) 0.020(2) 0.0157(19) 0.011(2) C64 0.056(2) 0.051(2) 0.052(2) 0.0162(18) 0.0055(19) 0.0035(19) N63 0.268(10) 0.131(5) 0.108(5) 0.060(4) 0.102(6) 0.094(6) C65 0.149(6) 0.072(3) 0.048(3) -0.002(2) 0.017(3) 0.042(4) C66 0.131(6) 0.112(5) 0.075(4) -0.035(4) 0.042(4) -0.006(4) N64A 0.101(5) 0.171(12) 0.046(3) -0.029(8) 0.018(3) -0.008(10) C67A 0.075(6) 0.083(11) 0.049(6) -0.014(9) 0.015(4) -0.010(10) C68A 0.080(7) 0.061(9) 0.037(13) 0.001(7) 0.015(7) 0.003(4) N64B 0.101(5) 0.171(12) 0.046(3) -0.029(8) 0.018(3) -0.008(10) C67B 0.075(6) 0.083(11) 0.049(6) -0.014(9) 0.015(4) -0.010(10) C68B 0.080(7) 0.061(9) 0.037(13) 0.001(7) 0.015(7) 0.003(4) _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 O1 2.2962(18) . ? Ho1 O17 2.3199(19) . ? Ho1 O10 2.3212(19) . ? Ho1 O7 2.349(2) . ? Ho1 O14 2.3791(18) . ? Ho1 O6 2.3880(19) . ? Ho1 O5 2.435(2) . ? Ho1 N3 2.476(2) . ? Ho2 O16 2.3044(19) . ? Ho2 O19 2.3120(19) . ? Ho2 O3 2.3171(19) . ? Ho2 O5 2.3472(19) . ? Ho2 O12 2.3642(18) . ? Ho2 O8 2.389(2) . ? Ho2 O7 2.438(2) . ? Ho2 N4 2.472(2) . ? Co1 O11 2.0256(18) . ? Co1 O9 2.050(2) . ? Co1 O1 2.0570(19) . ? Co1 O3 2.147(2) . ? Co1 O5 2.183(2) . ? Co1 N1 2.197(2) . ? Co2 O13 2.0185(18) . ? Co2 O3 2.0557(19) . ? Co2 O15 2.080(2) . ? Co2 O7 2.167(2) . ? Co2 O1 2.169(2) . ? Co2 N2 2.187(2) . ? Ho1X Co1X 3.384(19) . ? Ho1X Co2X 3.423(19) . ? Ho2X Co2X 3.380(19) . ? Ho2X Co1X 3.397(18) . ? N1 C1 1.344(3) . ? N1 C5 1.353(3) . ? C1 C2 1.392(4) . ? C1 C6 1.507(4) . ? C2 C3 1.382(4) . ? C2 H2A 0.9500 . ? C3 C4 1.381(4) . ? C3 H3A 0.9500 . ? C4 C5 1.386(4) . ? C4 H4A 0.9500 . ? C5 C7 1.505(4) . ? C6 O1 1.417(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 O2 1.422(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? O2 H2 0.83(3) . ? N2 C8 1.340(3) . ? N2 C12 1.358(3) . ? C8 C9 1.393(4) . ? C8 C13 1.516(4) . ? C9 C10 1.382(5) . ? C9 H9A 0.9500 . ? C10 C11 1.370(5) . ? C10 H10A 0.9500 . ? C11 C12 1.389(4) . ? C11 H11A 0.9500 . ? C12 C14 1.502(4) . ? C13 O3 1.410(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 O4 1.414(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? O4 H4 0.88(3) . ? N3 C15 1.347(3) . ? N3 C19 1.348(3) . ? C15 C16 1.391(4) . ? C15 C20 1.514(4) . ? C16 C17 1.387(4) . ? C16 H16A 0.9500 . ? C17 C18 1.378(5) . ? C17 H17A 0.9500 . ? C18 C19 1.387(4) . ? C18 H18A 0.9500 . ? C19 C21 1.498(4) . ? C20 O5 1.421(3) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 O6 1.418(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? O6 H6 0.89(3) . ? N4 C22 1.342(4) . ? N4 C26 1.343(4) . ? C22 C23 1.390(4) . ? C22 C27 1.499(4) . ? C23 C24 1.384(5) . ? C23 H23A 0.9500 . ? C24 C25 1.372(5) . ? C24 H24A 0.9500 . ? C25 C26 1.388(4) . ? C25 H25A 0.9500 . ? C26 C28 1.497(4) . ? C27 O7 1.421(3) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 O8 1.414(4) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? O8 H8 0.87(3) . ? O9 C29 1.258(3) . ? O10 C29 1.261(3) . ? C29 C30 1.533(4) . ? C30 C31 1.529(4) . ? C30 C32 1.532(4) . ? C30 C33 1.540(5) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? O11 C34 1.275(3) . ? O12 C34 1.245(3) . ? C34 C35 1.539(4) . ? C35 C38 1.529(4) . ? C35 C36 1.531(4) . ? C35 C37 1.534(5) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? O13 C39 1.282(3) . ? O14 C39 1.245(3) . ? C39 C40 1.534(4) . ? C40 C43 1.528(4) . ? C40 C41 1.528(4) . ? C40 C42 1.532(4) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? O15 C44 1.257(3) . ? O16 C44 1.260(3) . ? C44 C45 1.541(4) . ? C45 C48 1.528(4) . ? C45 C46 1.528(4) . ? C45 C47 1.536(4) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? O17 C49 1.265(3) . ? O18 C49 1.251(3) . ? C49 C50 1.542(4) . ? C50 C51B 1.489(15) . ? C50 C52A 1.502(5) . ? C50 C53B 1.509(14) . ? C50 C53A 1.518(5) . ? C50 C51A 1.537(5) . ? C50 C52B 1.549(15) . ? C51A H51A 0.9800 . ? C51A H51B 0.9800 . ? C51A H51C 0.9800 . ? C52A H52A 0.9800 . ? C52A H52B 0.9800 . ? C52A H52C 0.9800 . ? C53A H53A 0.9800 . ? C53A H53B 0.9800 . ? C53A H53C 0.9800 . ? C51B H51D 0.9800 . ? C51B H51E 0.9800 . ? C51B H51F 0.9800 . ? C52B H52D 0.9800 . ? C52B H52E 0.9800 . ? C52B H52F 0.9800 . ? C53B H53D 0.9800 . ? C53B H53E 0.9800 . ? C53B H53F 0.9800 . ? O19 C54 1.258(3) . ? O20 C54 1.250(4) . ? C54 C55 1.540(4) . ? C55 C58 1.526(4) . ? C55 C57 1.529(5) . ? C55 C56 1.530(4) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? N61 C61 1.092(6) . ? C61 C62 1.450(6) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? N62 C63 1.149(6) . ? C63 C64 1.461(6) . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? N63 C65 1.055(7) . ? C65 C66 1.417(7) . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? N64A C67A 1.12(3) . ? C67A C68A 1.42(5) . ? C68A H68A 0.9800 . ? C68A H68B 0.9800 . ? C68A H68C 0.9800 . ? N64B C67B 1.15(3) . ? C67B C68B 1.47(6) . ? C68B H68D 0.9800 . ? C68B H68E 0.9800 . ? C68B H68F 0.9800 . ? 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 O1 Ho1 O17 97.53(7) . . ? O1 Ho1 O10 85.45(6) . . ? O17 Ho1 O10 70.42(7) . . ? O1 Ho1 O7 75.13(7) . . ? O17 Ho1 O7 145.91(7) . . ? O10 Ho1 O7 139.78(6) . . ? O1 Ho1 O14 79.15(6) . . ? O17 Ho1 O14 71.12(7) . . ? O10 Ho1 O14 135.98(7) . . ? O7 Ho1 O14 74.80(7) . . ? O1 Ho1 O6 151.93(7) . . ? O17 Ho1 O6 76.81(7) . . ? O10 Ho1 O6 117.19(7) . . ? O7 Ho1 O6 94.05(7) . . ? O14 Ho1 O6 72.98(7) . . ? O1 Ho1 O5 75.25(7) . . ? O17 Ho1 O5 144.38(7) . . ? O10 Ho1 O5 74.23(6) . . ? O7 Ho1 O5 66.96(7) . . ? O14 Ho1 O5 138.13(6) . . ? O6 Ho1 O5 124.82(7) . . ? O1 Ho1 N3 140.48(7) . . ? O17 Ho1 N3 111.62(7) . . ? O10 Ho1 N3 80.18(7) . . ? O7 Ho1 N3 92.75(8) . . ? O14 Ho1 N3 134.53(7) . . ? O6 Ho1 N3 64.35(7) . . ? O5 Ho1 N3 65.47(7) . . ? O16 Ho2 O19 70.43(7) . . ? O16 Ho2 O3 85.18(7) . . ? O19 Ho2 O3 99.62(7) . . ? O16 Ho2 O5 139.71(7) . . ? O19 Ho2 O5 147.00(7) . . ? O3 Ho2 O5 75.70(7) . . ? O16 Ho2 O12 135.49(7) . . ? O19 Ho2 O12 71.44(7) . . ? O3 Ho2 O12 79.36(6) . . ? O5 Ho2 O12 75.61(7) . . ? O16 Ho2 O8 117.32(7) . . ? O19 Ho2 O8 75.71(7) . . ? O3 Ho2 O8 152.51(7) . . ? O5 Ho2 O8 93.40(7) . . ? O12 Ho2 O8 73.45(7) . . ? O16 Ho2 O7 73.88(7) . . ? O19 Ho2 O7 144.17(7) . . ? O3 Ho2 O7 74.12(7) . . ? O5 Ho2 O7 66.93(7) . . ? O12 Ho2 O7 138.18(6) . . ? O8 Ho2 O7 125.20(7) . . ? O16 Ho2 N4 80.23(7) . . ? O19 Ho2 N4 110.63(7) . . ? O3 Ho2 N4 139.28(7) . . ? O5 Ho2 N4 91.52(7) . . ? O12 Ho2 N4 135.32(7) . . ? O8 Ho2 N4 64.68(8) . . ? O7 Ho2 N4 65.36(7) . . ? O11 Co1 O9 89.36(8) . . ? O11 Co1 O1 173.91(8) . . ? O9 Co1 O1 96.73(8) . . ? O11 Co1 O3 94.05(8) . . ? O9 Co1 O3 174.48(7) . . ? O1 Co1 O3 79.86(8) . . ? O11 Co1 O5 93.55(7) . . ? O9 Co1 O5 92.71(7) . . ? O1 Co1 O5 85.91(7) . . ? O3 Co1 O5 82.75(7) . . ? O11 Co1 N1 102.13(8) . . ? O9 Co1 N1 83.20(8) . . ? O1 Co1 N1 78.96(7) . . ? O3 Co1 N1 100.29(8) . . ? O5 Co1 N1 163.72(8) . . ? O13 Co2 O3 173.98(8) . . ? O13 Co2 O15 89.19(8) . . ? O3 Co2 O15 96.76(8) . . ? O13 Co2 O7 93.31(8) . . ? O3 Co2 O7 85.51(7) . . ? O15 Co2 O7 93.08(8) . . ? O13 Co2 O1 94.62(8) . . ? O3 Co2 O1 79.37(8) . . ? O15 Co2 O1 173.58(7) . . ? O7 Co2 O1 81.56(7) . . ? O13 Co2 N2 101.76(8) . . ? O3 Co2 N2 79.68(8) . . ? O15 Co2 N2 85.44(8) . . ? O7 Co2 N2 164.82(8) . . ? O1 Co2 N2 98.80(8) . . ? C1 N1 C5 117.9(2) . . ? C1 N1 Co1 110.13(16) . . ? C5 N1 Co1 131.04(19) . . ? N1 C1 C2 122.8(2) . . ? N1 C1 C6 118.3(2) . . ? C2 C1 C6 118.8(2) . . ? C3 C2 C1 119.0(3) . . ? C3 C2 H2A 120.5 . . ? C1 C2 H2A 120.5 . . ? C4 C3 C2 118.5(3) . . ? C4 C3 H3A 120.8 . . ? C2 C3 H3A 120.8 . . ? C3 C4 C5 120.0(3) . . ? C3 C4 H4A 120.0 . . ? C5 C4 H4A 120.0 . . ? N1 C5 C4 121.8(3) . . ? N1 C5 C7 118.0(2) . . ? C4 C5 C7 120.2(3) . . ? O1 C6 C1 112.5(2) . . ? O1 C6 H6A 109.1 . . ? C1 C6 H6A 109.1 . . ? O1 C6 H6B 109.1 . . ? C1 C6 H6B 109.1 . . ? H6A C6 H6B 107.8 . . ? C6 O1 Co1 112.80(15) . . ? C6 O1 Co2 118.73(16) . . ? Co1 O1 Co2 99.99(9) . . ? C6 O1 Ho1 121.02(16) . . ? Co1 O1 Ho1 100.42(7) . . ? Co2 O1 Ho1 100.43(7) . . ? O2 C7 C5 112.0(3) . . ? O2 C7 H7A 109.2 . . ? C5 C7 H7A 109.2 . . ? O2 C7 H7B 109.2 . . ? C5 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? C7 O2 H2 103(3) . . ? C8 N2 C12 118.2(2) . . ? C8 N2 Co2 110.39(17) . . ? C12 N2 Co2 131.39(19) . . ? N2 C8 C9 122.7(3) . . ? N2 C8 C13 117.7(2) . . ? C9 C8 C13 119.5(2) . . ? C10 C9 C8 118.5(3) . . ? C10 C9 H9A 120.8 . . ? C8 C9 H9A 120.8 . . ? C11 C10 C9 119.4(3) . . ? C11 C10 H10A 120.3 . . ? C9 C10 H10A 120.3 . . ? C10 C11 C12 119.6(3) . . ? C10 C11 H11A 120.2 . . ? C12 C11 H11A 120.2 . . ? N2 C12 C11 121.6(3) . . ? N2 C12 C14 118.0(3) . . ? C11 C12 C14 120.3(3) . . ? O3 C13 C8 112.1(2) . . ? O3 C13 H13A 109.2 . . ? C8 C13 H13A 109.2 . . ? O3 C13 H13B 109.2 . . ? C8 C13 H13B 109.2 . . ? H13A C13 H13B 107.9 . . ? C13 O3 Co2 112.08(15) . . ? C13 O3 Co1 116.36(16) . . ? Co2 O3 Co1 100.77(9) . . ? C13 O3 Ho2 123.89(17) . . ? Co2 O3 Ho2 100.56(7) . . ? Co1 O3 Ho2 99.74(7) . . ? O4 C14 C12 111.9(3) . . ? O4 C14 H14A 109.2 . . ? C12 C14 H14A 109.2 . . ? O4 C14 H14B 109.2 . . ? C12 C14 H14B 109.2 . . ? H14A C14 H14B 107.9 . . ? C14 O4 H4 108(4) . . ? C15 N3 C19 119.3(2) . . ? C15 N3 Ho1 118.24(17) . . ? C19 N3 Ho1 122.35(18) . . ? N3 C15 C16 121.5(3) . . ? N3 C15 C20 116.3(2) . . ? C16 C15 C20 122.2(3) . . ? C17 C16 C15 118.6(3) . . ? C17 C16 H16A 120.7 . . ? C15 C16 H16A 120.7 . . ? C18 C17 C16 120.0(3) . . ? C18 C17 H17A 120.0 . . ? C16 C17 H17A 120.0 . . ? C17 C18 C19 118.5(3) . . ? C17 C18 H18A 120.7 . . ? C19 C18 H18A 120.7 . . ? N3 C19 C18 122.0(3) . . ? N3 C19 C21 115.9(2) . . ? C18 C19 C21 122.1(3) . . ? O5 C20 C15 110.0(2) . . ? O5 C20 H20A 109.7 . . ? C15 C20 H20A 109.7 . . ? O5 C20 H20B 109.7 . . ? C15 C20 H20B 109.7 . . ? H20A C20 H20B 108.2 . . ? C20 O5 Co1 120.47(17) . . ? C20 O5 Ho2 115.03(15) . . ? Co1 O5 Ho2 97.77(8) . . ? C20 O5 Ho1 114.86(15) . . ? Co1 O5 Ho1 92.79(7) . . ? Ho2 O5 Ho1 113.05(8) . . ? O6 C21 C19 110.5(2) . . ? O6 C21 H21A 109.6 . . ? C19 C21 H21A 109.6 . . ? O6 C21 H21B 109.6 . . ? C19 C21 H21B 109.6 . . ? H21A C21 H21B 108.1 . . ? C21 O6 Ho1 125.39(17) . . ? C21 O6 H6 105(2) . . ? Ho1 O6 H6 104(2) . . ? C22 N4 C26 119.6(2) . . ? C22 N4 Ho2 118.34(18) . . ? C26 N4 Ho2 122.04(19) . . ? N4 C22 C23 121.7(3) . . ? N4 C22 C27 116.6(2) . . ? C23 C22 C27 121.7(3) . . ? C24 C23 C22 118.4(3) . . ? C24 C23 H23A 120.8 . . ? C22 C23 H23A 120.8 . . ? C25 C24 C23 120.0(3) . . ? C25 C24 H24A 120.0 . . ? C23 C24 H24A 120.0 . . ? C24 C25 C26 118.9(3) . . ? C24 C25 H25A 120.5 . . ? C26 C25 H25A 120.5 . . ? N4 C26 C25 121.5(3) . . ? N4 C26 C28 116.4(3) . . ? C25 C26 C28 122.2(3) . . ? O7 C27 C22 110.4(2) . . ? O7 C27 H27A 109.6 . . ? C22 C27 H27A 109.6 . . ? O7 C27 H27B 109.6 . . ? C22 C27 H27B 109.6 . . ? H27A C27 H27B 108.1 . . ? C27 O7 Co2 120.44(18) . . ? C27 O7 Ho1 113.69(15) . . ? Co2 O7 Ho1 98.88(7) . . ? C27 O7 Ho2 114.82(16) . . ? Co2 O7 Ho2 93.80(7) . . ? Ho1 O7 Ho2 112.90(8) . . ? O8 C28 C26 110.9(2) . . ? O8 C28 H28A 109.5 . . ? C26 C28 H28A 109.5 . . ? O8 C28 H28B 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 108.0 . . ? C28 O8 Ho2 125.13(18) . . ? C28 O8 H8 108(2) . . ? Ho2 O8 H8 108(2) . . ? C29 O9 Co1 125.95(17) . . ? C29 O10 Ho1 137.12(17) . . ? O9 C29 O10 124.8(2) . . ? O9 C29 C30 117.8(2) . . ? O10 C29 C30 117.4(2) . . ? C31 C30 C32 111.0(3) . . ? C31 C30 C29 108.7(2) . . ? C32 C30 C29 110.6(3) . . ? C31 C30 C33 109.9(3) . . ? C32 C30 C33 109.5(3) . . ? C29 C30 C33 107.1(3) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C30 C33 H33A 109.5 . . ? C30 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C34 O11 Co1 124.78(17) . . ? C34 O12 Ho2 139.30(17) . . ? O12 C34 O11 124.2(2) . . ? O12 C34 C35 119.7(2) . . ? O11 C34 C35 116.1(2) . . ? C38 C35 C36 109.8(3) . . ? C38 C35 C37 110.2(3) . . ? C36 C35 C37 110.1(3) . . ? C38 C35 C34 109.4(2) . . ? C36 C35 C34 110.4(2) . . ? C37 C35 C34 106.9(2) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C39 O13 Co2 124.30(17) . . ? C39 O14 Ho1 139.30(16) . . ? O14 C39 O13 124.0(2) . . ? O14 C39 C40 119.8(2) . . ? O13 C39 C40 116.2(2) . . ? C43 C40 C41 109.8(3) . . ? C43 C40 C42 109.4(3) . . ? C41 C40 C42 110.3(2) . . ? C43 C40 C39 109.2(2) . . ? C41 C40 C39 110.5(2) . . ? C42 C40 C39 107.7(2) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C40 C43 H43A 109.5 . . ? C40 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C40 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C44 O15 Co2 124.27(18) . . ? C44 O16 Ho2 139.32(18) . . ? O15 C44 O16 124.6(3) . . ? O15 C44 C45 119.0(2) . . ? O16 C44 C45 116.4(2) . . ? C48 C45 C46 110.7(3) . . ? C48 C45 C47 109.7(3) . . ? C46 C45 C47 109.2(2) . . ? C48 C45 C44 108.1(2) . . ? C46 C45 C44 111.1(2) . . ? C47 C45 C44 107.9(2) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C45 C48 H48A 109.5 . . ? C45 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C45 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C49 O17 Ho1 133.46(18) . . ? O18 C49 O17 124.3(3) . . ? O18 C49 C50 118.8(2) . . ? O17 C49 C50 116.9(2) . . ? C51B C50 C53B 108.6(9) . . ? C52A C50 C53A 111.2(4) . . ? C52A C50 C51A 110.1(4) . . ? C53A C50 C51A 111.5(4) . . ? C51B C50 C49 114.0(9) . . ? C52A C50 C49 109.6(3) . . ? C53B C50 C49 109.6(8) . . ? C53A C50 C49 105.8(3) . . ? C51A C50 C49 108.6(3) . . ? C51B C50 C52B 106.1(9) . . ? C53B C50 C52B 104.2(8) . . ? C49 C50 C52B 113.8(8) . . ? C50 C51A H51A 109.5 . . ? C50 C51A H51B 109.5 . . ? H51A C51A H51B 109.5 . . ? C50 C51A H51C 109.5 . . ? H51A C51A H51C 109.5 . . ? H51B C51A H51C 109.5 . . ? C50 C52A H52A 109.5 . . ? C50 C52A H52B 109.5 . . ? H52A C52A H52B 109.5 . . ? C50 C52A H52C 109.5 . . ? H52A C52A H52C 109.5 . . ? H52B C52A H52C 109.5 . . ? C50 C53A H53A 109.5 . . ? C50 C53A H53B 109.5 . . ? H53A C53A H53B 109.5 . . ? C50 C53A H53C 109.5 . . ? H53A C53A H53C 109.5 . . ? H53B C53A H53C 109.5 . . ? C50 C51B H51D 109.5 . . ? C50 C51B H51E 109.5 . . ? H51D C51B H51E 109.5 . . ? C50 C51B H51F 109.5 . . ? H51D C51B H51F 109.5 . . ? H51E C51B H51F 109.5 . . ? C50 C52B H52D 109.5 . . ? C50 C52B H52E 109.5 . . ? H52D C52B H52E 109.5 . . ? C50 C52B H52F 109.5 . . ? H52D C52B H52F 109.5 . . ? H52E C52B H52F 109.5 . . ? C50 C53B H53D 109.5 . . ? C50 C53B H53E 109.5 . . ? H53D C53B H53E 109.5 . . ? C50 C53B H53F 109.5 . . ? H53D C53B H53F 109.5 . . ? H53E C53B H53F 109.5 . . ? C54 O19 Ho2 135.9(2) . . ? O20 C54 O19 124.2(3) . . ? O20 C54 C55 119.5(3) . . ? O19 C54 C55 116.3(3) . . ? C58 C55 C57 109.0(3) . . ? C58 C55 C56 111.6(3) . . ? C57 C55 C56 109.2(3) . . ? C58 C55 C54 110.9(3) . . ? C57 C55 C54 109.6(2) . . ? C56 C55 C54 106.6(3) . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C55 C57 H57A 109.5 . . ? C55 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C55 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C55 C58 H58A 109.5 . . ? C55 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C55 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? N61 C61 C62 178.6(5) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? N62 C63 C64 178.9(5) . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? N63 C65 C66 176.3(10) . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? N64A C67A C68A 173(3) . . ? N64B C67B C68B 176(3) . . ? C67B C68B H68D 109.5 . . ? C67B C68B H68E 109.5 . . ? H68D C68B H68E 109.5 . . ? C67B C68B H68F 109.5 . . ? H68D C68B H68F 109.5 . . ? H68E C68B H68F 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2 O11 0.83(3) 1.94(3) 2.722(3) 157(5) . O4 H4 O13 0.88(3) 1.96(4) 2.744(3) 147(5) . O6 H6 O18 0.89(3) 1.66(3) 2.533(3) 168(3) . O8 H8 O20 0.87(3) 1.67(3) 2.513(3) 162(4) . _diffrn_measured_fraction_theta_max 0.918 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.666 _refine_diff_density_min -0.707 _refine_diff_density_rms 0.087 ######################################################## data_zhao399s _database_code_depnum_ccdc_archive 'CCDC 756454' #TrackingRef 'co2ln2_a1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C58 H86 Co2 Dy2 N4 O20, 2(C2 H3 N)' _chemical_formula_sum 'C62 H92 Co2 Dy2 N6 O20' _chemical_formula_weight 1684.28 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n n a' _symmetry_space_group_name_Hall '-P 2a 2bc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x, y-1/2, z-1/2' _cell_length_a 19.8071(12) _cell_length_b 23.3437(15) _cell_length_c 16.0781(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7434.0(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 32389 _cell_measurement_theta_min 1.54 _cell_measurement_theta_max 27.10 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.505 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3408 _exptl_absorpt_coefficient_mu 2.494 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.505 _exptl_absorpt_correction_T_max 0.607 _exptl_absorpt_process_details ; XPREP in SHELXTL 6.14 (BrukerAXS Inc., 2003) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean 6.667 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47604 _diffrn_reflns_av_R_equivalents 0.0674 _diffrn_reflns_av_sigmaI/netI 0.0262 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 26.81 _reflns_number_total 7932 _reflns_number_gt 5406 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'WinXpose 1.6.8 (Stoe & Cie GmbH, 2004)' _computing_cell_refinement 'X-Area 1.38 (Stoe & Cie GmbH, 2006)' _computing_data_reduction 'X-Area 1.38 (Stoe & Cie GmbH, 2006)' _computing_structure_solution 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_structure_refinement 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_molecular_graphics 'Diamond 2.1 (Crystal Impact, 1998)' _computing_publication_material 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _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. The lattice MeCN in the assymmetric unit (i.e. two per Co2Dy2) was badly disordered, and was treated using SQUEEZE (see below). ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.250 0.000 -0.108 224 45 ' ' 2 0.750 0.000 0.108 223 45 ' ' 3 0.250 0.500 0.134 39 5 ' ' 4 0.750 0.500 0.392 224 45 ' ' 5 0.250 0.000 0.366 39 5 ' ' 6 0.250 0.500 0.608 224 45 ' ' 7 0.750 0.000 0.634 39 5 ' ' 8 0.750 0.500 0.866 39 5 ' ' _platon_squeeze_details ; Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13 ; _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^)+(0.1078P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7932 _refine_ls_number_parameters 394 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0869 _refine_ls_R_factor_gt 0.0635 _refine_ls_wR_factor_ref 0.1613 _refine_ls_wR_factor_gt 0.1504 _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_restrained_S_all 0.997 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.638440(13) 0.188480(15) 0.336721(17) 0.05887(13) Uani 1 1 d . . . Co1 Co 0.52318(4) 0.20159(4) 0.17995(5) 0.0569(2) Uani 1 1 d . . . N1 N 0.4158(3) 0.1865(2) 0.2144(3) 0.0594(12) Uani 1 1 d . . . C1 C 0.4115(3) 0.1720(3) 0.2951(4) 0.0589(14) Uani 1 1 d . . . C2 C 0.3507(3) 0.1573(4) 0.3336(4) 0.0682(17) Uani 1 1 d . . . H2A H 0.3501 0.1469 0.3908 0.082 Uiso 1 1 calc R . . C3 C 0.2915(3) 0.1581(3) 0.2880(4) 0.0691(17) Uani 1 1 d . . . H3A H 0.2494 0.1492 0.3131 0.083 Uiso 1 1 calc R . . C4 C 0.2957(3) 0.1725(3) 0.2031(4) 0.0713(18) Uani 1 1 d . . . H4A H 0.2562 0.1725 0.1695 0.086 Uiso 1 1 calc R . . C5 C 0.3579(3) 0.1869(3) 0.1687(4) 0.0648(17) Uani 1 1 d . . . C6 C 0.4770(3) 0.1721(3) 0.3457(3) 0.0635(16) Uani 1 1 d . . . H6A H 0.4676 0.1861 0.4026 0.076 Uiso 1 1 calc R . . H6B H 0.4945 0.1325 0.3500 0.076 Uiso 1 1 calc R . . O1 O 0.52591(18) 0.20720(19) 0.3082(2) 0.0531(9) Uani 1 1 d . . . C7 C 0.3648(3) 0.2011(3) 0.0777(4) 0.0699(18) Uani 1 1 d . . . H7A H 0.3196 0.2092 0.0543 0.084 Uiso 1 1 calc R . . H7B H 0.3925 0.2361 0.0716 0.084 Uiso 1 1 calc R . . O2 O 0.3952(2) 0.1557(2) 0.0318(3) 0.0751(13) Uani 1 1 d D . . H2 H 0.438(2) 0.166(3) 0.032(5) 0.090 Uiso 1 1 d D . . N2 N 0.7468(2) 0.1784(2) 0.2622(3) 0.0543(11) Uani 1 1 d . . . C8 C 0.7445(3) 0.1710(3) 0.1802(4) 0.0551(13) Uani 1 1 d . . . C9 C 0.8025(3) 0.1581(3) 0.1346(4) 0.0632(15) Uani 1 1 d . . . H9A H 0.8003 0.1522 0.0762 0.076 Uiso 1 1 calc R . . C10 C 0.8629(3) 0.1541(3) 0.1761(5) 0.0736(18) Uani 1 1 d . . . H10A H 0.9029 0.1449 0.1465 0.088 Uiso 1 1 calc R . . C11 C 0.8657(3) 0.1634(3) 0.2608(5) 0.0646(16) Uani 1 1 d . . . H11A H 0.9074 0.1622 0.2899 0.077 Uiso 1 1 calc R . . C12 C 0.8053(3) 0.1747(3) 0.3026(4) 0.0567(14) Uani 1 1 d . . . C13 C 0.6772(3) 0.1779(3) 0.1380(4) 0.0606(15) Uani 1 1 d . . . H13A H 0.6835 0.1967 0.0834 0.073 Uiso 1 1 calc R . . H13B H 0.6567 0.1398 0.1285 0.073 Uiso 1 1 calc R . . O3 O 0.63371(18) 0.2117(2) 0.1885(2) 0.0550(9) Uani 1 1 d . . . C14 C 0.8045(3) 0.1847(3) 0.3958(4) 0.0680(17) Uani 1 1 d . . . H14A H 0.8182 0.1491 0.4248 0.082 Uiso 1 1 calc R . . H14B H 0.8374 0.2150 0.4102 0.082 Uiso 1 1 calc R . . O4 O 0.7400(2) 0.2009(2) 0.4226(3) 0.0608(10) Uani 1 1 d D . . H4 H 0.721(3) 0.178(3) 0.462(4) 0.073 Uiso 1 1 d D . . O5 O 0.5300(2) 0.1154(2) 0.1726(3) 0.0681(11) Uani 1 1 d . . . O6 O 0.6110(2) 0.1047(2) 0.2692(3) 0.0679(11) Uani 1 1 d . . . C15 C 0.5731(3) 0.0856(3) 0.2119(4) 0.0676(17) Uani 1 1 d . . . C16 C 0.5825(4) 0.0231(3) 0.1877(5) 0.080(2) Uani 1 1 d . . . C17 C 0.6556(5) 0.0097(5) 0.1843(8) 0.113(3) Uani 1 1 d . . . H17A H 0.6762 0.0180 0.2385 0.170 Uiso 1 1 calc R . . H17B H 0.6772 0.0333 0.1414 0.170 Uiso 1 1 calc R . . H17C H 0.6617 -0.0309 0.1710 0.170 Uiso 1 1 calc R . . C18 C 0.5475(6) -0.0121(4) 0.2556(7) 0.124(4) Uani 1 1 d . . . H18A H 0.5692 -0.0047 0.3093 0.186 Uiso 1 1 calc R . . H18B H 0.5511 -0.0530 0.2422 0.186 Uiso 1 1 calc R . . H18C H 0.4997 -0.0012 0.2586 0.186 Uiso 1 1 calc R . . C19 C 0.5501(7) 0.0106(4) 0.1024(7) 0.135(4) Uani 1 1 d . . . H19A H 0.5729 0.0332 0.0594 0.202 Uiso 1 1 calc R . . H19B H 0.5022 0.0208 0.1040 0.202 Uiso 1 1 calc R . . H19C H 0.5548 -0.0303 0.0896 0.202 Uiso 1 1 calc R . . O7 O 0.5188(2) 0.2063(2) 0.0544(3) 0.0691(12) Uani 1 1 d . . . O8 O 0.6004(2) 0.2720(2) 0.0362(2) 0.0698(13) Uani 1 1 d . . . C20 C 0.5622(3) 0.2336(4) 0.0104(4) 0.0697(19) Uani 1 1 d . . . C21 C 0.5654(4) 0.2169(5) -0.0826(4) 0.089(3) Uani 1 1 d . . . C22 C 0.5045(4) 0.2463(5) -0.1238(5) 0.104(3) Uani 1 1 d . . . H22A H 0.5089 0.2879 -0.1185 0.156 Uiso 1 1 calc R . . H22B H 0.4628 0.2337 -0.0965 0.156 Uiso 1 1 calc R . . H22C H 0.5029 0.2359 -0.1829 0.156 Uiso 1 1 calc R . . C23 C 0.5601(6) 0.1514(5) -0.0923(5) 0.124(4) Uani 1 1 d . . . H23A H 0.5996 0.1332 -0.0668 0.185 Uiso 1 1 calc R . . H23B H 0.5583 0.1416 -0.1515 0.185 Uiso 1 1 calc R . . H23C H 0.5190 0.1378 -0.0647 0.185 Uiso 1 1 calc R . . C24 C 0.6318(4) 0.2384(8) -0.1198(5) 0.156(6) Uani 1 1 d . . . H24A H 0.6344 0.2801 -0.1139 0.233 Uiso 1 1 calc R . . H24B H 0.6337 0.2281 -0.1788 0.233 Uiso 1 1 calc R . . H24C H 0.6698 0.2206 -0.0904 0.233 Uiso 1 1 calc R . . O9 O 0.6350(3) 0.1155(2) 0.4338(3) 0.0924(19) Uani 1 1 d . . . O10 O 0.7061(3) 0.1322(3) 0.5380(3) 0.0909(17) Uani 1 1 d . . . C25 C 0.6562(5) 0.1067(4) 0.5065(5) 0.105(3) Uani 1 1 d . . . C26 C 0.6192(7) 0.0609(7) 0.5579(7) 0.167(7) Uani 1 1 d . . . C27 C 0.6352(9) 0.0017(7) 0.5151(15) 0.238(12) Uani 1 1 d . . . H27A H 0.6834 -0.0069 0.5211 0.357 Uiso 1 1 calc R . . H27B H 0.6236 0.0037 0.4560 0.357 Uiso 1 1 calc R . . H27C H 0.6087 -0.0286 0.5418 0.357 Uiso 1 1 calc R . . C28 C 0.6404(10) 0.0640(12) 0.6460(9) 0.37(2) Uani 1 1 d . . . H28A H 0.6284 0.1016 0.6688 0.558 Uiso 1 1 calc R . . H28B H 0.6894 0.0586 0.6497 0.558 Uiso 1 1 calc R . . H28C H 0.6176 0.0339 0.6779 0.558 Uiso 1 1 calc R . . C29 C 0.5431(7) 0.0722(7) 0.5465(7) 0.184(8) Uani 1 1 d . . . H29A H 0.5310 0.1083 0.5739 0.276 Uiso 1 1 calc R . . H29B H 0.5173 0.0407 0.5713 0.276 Uiso 1 1 calc R . . H29C H 0.5326 0.0748 0.4870 0.276 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.04187(17) 0.0916(2) 0.04314(16) 0.01319(13) -0.00193(10) -0.00372(13) Co1 0.0427(4) 0.0900(6) 0.0381(3) 0.0052(3) -0.0022(3) -0.0008(4) N1 0.044(3) 0.088(4) 0.046(2) -0.002(2) 0.001(2) -0.001(2) C1 0.045(3) 0.086(4) 0.045(3) -0.003(3) 0.006(2) -0.005(3) C2 0.053(4) 0.097(5) 0.054(3) -0.005(3) 0.005(3) -0.009(3) C3 0.048(3) 0.101(5) 0.058(4) -0.003(3) 0.003(3) -0.009(3) C4 0.043(3) 0.110(5) 0.061(4) -0.013(4) 0.003(3) -0.005(3) C5 0.042(3) 0.099(5) 0.054(4) -0.009(3) -0.002(2) -0.001(3) C6 0.049(3) 0.100(5) 0.042(3) 0.011(3) 0.003(2) -0.009(3) O1 0.0364(18) 0.088(3) 0.0352(17) 0.0070(17) 0.0003(14) -0.0045(18) C7 0.052(4) 0.108(5) 0.050(3) -0.004(3) -0.005(3) 0.009(3) O2 0.054(3) 0.115(4) 0.055(2) -0.012(3) -0.005(2) 0.001(3) N2 0.041(2) 0.069(3) 0.053(3) 0.011(2) -0.002(2) 0.002(2) C8 0.049(3) 0.060(3) 0.056(3) 0.013(3) 0.006(3) -0.001(3) C9 0.053(3) 0.075(4) 0.062(3) 0.004(3) 0.004(3) 0.003(3) C10 0.051(4) 0.087(5) 0.083(5) 0.004(4) 0.011(3) 0.003(3) C11 0.039(3) 0.076(4) 0.079(4) 0.008(3) 0.000(3) 0.001(3) C12 0.050(3) 0.058(3) 0.062(3) 0.015(3) 0.000(3) -0.006(3) C13 0.050(3) 0.090(5) 0.042(3) 0.006(3) 0.009(2) 0.008(3) O3 0.041(2) 0.085(3) 0.0385(18) 0.0053(19) 0.0048(15) 0.0077(18) C14 0.052(4) 0.092(5) 0.060(4) 0.016(3) -0.003(3) -0.001(3) O4 0.043(2) 0.086(3) 0.054(2) 0.010(2) -0.0041(17) -0.008(2) O5 0.052(2) 0.091(3) 0.062(2) 0.006(2) 0.001(2) 0.002(2) O6 0.062(3) 0.093(3) 0.048(2) 0.009(2) -0.002(2) 0.004(2) C15 0.055(4) 0.092(5) 0.055(3) 0.012(3) 0.005(3) -0.006(3) C16 0.074(5) 0.084(5) 0.081(5) 0.004(4) 0.009(4) 0.004(4) C17 0.068(5) 0.117(8) 0.155(10) -0.037(7) 0.021(6) 0.004(5) C18 0.137(9) 0.084(6) 0.150(9) 0.029(6) 0.066(8) 0.009(6) C19 0.184(12) 0.099(7) 0.121(8) -0.021(6) -0.051(8) -0.002(7) O7 0.054(2) 0.109(3) 0.044(2) 0.003(2) -0.0002(19) -0.001(2) O8 0.048(2) 0.124(4) 0.0368(19) 0.012(2) -0.0036(17) -0.001(3) C20 0.045(3) 0.124(6) 0.040(3) 0.010(3) 0.000(2) 0.016(4) C21 0.056(4) 0.179(9) 0.032(3) 0.000(4) 0.000(3) 0.008(5) C22 0.082(6) 0.174(9) 0.055(4) 0.026(5) -0.020(4) -0.015(6) C23 0.118(8) 0.188(11) 0.065(5) -0.048(6) -0.005(5) 0.047(8) C24 0.069(6) 0.35(2) 0.049(4) -0.010(8) 0.015(4) -0.032(8) O9 0.100(4) 0.111(4) 0.066(3) 0.046(3) -0.039(3) -0.049(3) O10 0.081(3) 0.128(4) 0.063(3) 0.039(3) -0.029(3) -0.040(3) C25 0.098(6) 0.137(7) 0.078(5) 0.047(5) -0.043(5) -0.057(6) C26 0.154(11) 0.248(16) 0.098(7) 0.099(9) -0.071(7) -0.138(12) C27 0.185(17) 0.171(14) 0.36(3) 0.149(18) -0.115(17) -0.083(13) C28 0.35(3) 0.63(5) 0.137(11) 0.22(2) -0.150(15) -0.42(3) C29 0.158(12) 0.290(19) 0.104(8) 0.061(10) -0.011(8) -0.147(13) _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 Dy1 O6 2.302(5) . ? Dy1 O9 2.312(4) . ? Dy1 O1 2.317(4) . ? Dy1 O8 2.366(4) 4 ? Dy1 O3 2.368(5) 4 ? Dy1 O3 2.446(4) . ? Dy1 O4 2.457(4) . ? Dy1 N2 2.470(5) . ? Co1 O5 2.021(5) . ? Co1 O7 2.023(4) . ? Co1 O1 2.066(4) . ? Co1 O1 2.139(4) 4 ? Co1 O3 2.206(4) . ? Co1 N1 2.227(5) . ? N1 C1 1.343(7) . ? N1 C5 1.362(8) . ? C1 C2 1.396(8) . ? C1 C6 1.532(9) . ? C2 C3 1.384(9) . ? C2 H2A 0.9500 . ? C3 C4 1.409(9) . ? C3 H3A 0.9500 . ? C4 C5 1.391(9) . ? C4 H4A 0.9500 . ? C5 C7 1.507(9) . ? C6 O1 1.405(7) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? O1 Co1 2.138(4) 4 ? C7 O2 1.425(9) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? O2 H2 0.88(4) . ? N2 C8 1.329(8) . ? N2 C12 1.330(8) . ? C8 C9 1.397(9) . ? C8 C13 1.504(9) . ? C9 C10 1.373(10) . ? C9 H9A 0.9500 . ? C10 C11 1.380(10) . ? C10 H10A 0.9500 . ? C11 C12 1.397(9) . ? C11 H11A 0.9500 . ? C12 C14 1.517(9) . ? C13 O3 1.422(7) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? O3 Dy1 2.368(5) 4 ? C14 O4 1.400(8) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? O4 H4 0.91(4) . ? O5 C15 1.268(8) . ? O6 C15 1.269(8) . ? C15 C16 1.521(11) . ? C16 C17 1.481(11) . ? C16 C18 1.534(11) . ? C16 C19 1.542(12) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? O7 C20 1.282(8) . ? O8 C20 1.244(9) . ? O8 Dy1 2.365(4) 4 ? C20 C21 1.547(8) . ? C21 C24 1.528(12) . ? C21 C22 1.539(11) . ? C21 C23 1.541(14) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? O9 C25 1.258(9) . ? O10 C25 1.261(9) . ? C25 C26 1.538(12) . ? C26 C28 1.481(15) . ? C26 C29 1.54(2) . ? C26 C27 1.58(3) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? 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 O6 Dy1 O9 71.66(18) . . ? O6 Dy1 O1 80.77(16) . . ? O9 Dy1 O1 104.15(17) . . ? O6 Dy1 O8 131.56(17) . 4 ? O9 Dy1 O8 72.2(2) . 4 ? O1 Dy1 O8 77.93(14) . 4 ? O6 Dy1 O3 138.26(14) . 4 ? O9 Dy1 O3 147.15(19) . 4 ? O1 Dy1 O3 75.07(14) . 4 ? O8 Dy1 O3 75.61(16) 4 4 ? O6 Dy1 O3 73.70(15) . . ? O9 Dy1 O3 145.08(19) . . ? O1 Dy1 O3 74.24(12) . . ? O8 Dy1 O3 138.01(15) 4 . ? O3 Dy1 O3 67.28(18) 4 . ? O6 Dy1 O4 123.98(16) . . ? O9 Dy1 O4 74.47(15) . . ? O1 Dy1 O4 151.23(15) . . ? O8 Dy1 O4 74.32(15) 4 . ? O3 Dy1 O4 90.69(14) 4 . ? O3 Dy1 O4 123.54(13) . . ? O6 Dy1 N2 83.99(16) . . ? O9 Dy1 N2 106.4(2) . . ? O1 Dy1 N2 139.27(14) . . ? O8 Dy1 N2 137.20(16) 4 . ? O3 Dy1 N2 92.60(15) 4 . ? O3 Dy1 N2 65.26(14) . . ? O4 Dy1 N2 64.67(16) . . ? O5 Co1 O7 89.9(2) . . ? O5 Co1 O1 96.89(18) . . ? O7 Co1 O1 173.2(2) . . ? O5 Co1 O1 174.41(17) . 4 ? O7 Co1 O1 92.07(18) . 4 ? O1 Co1 O1 81.20(16) . 4 ? O5 Co1 O3 92.47(18) . . ? O7 Co1 O3 95.68(16) . . ? O1 Co1 O3 84.56(15) . . ? O1 Co1 O3 82.14(16) 4 . ? O5 Co1 N1 85.48(19) . . ? O7 Co1 N1 102.46(18) . . ? O1 Co1 N1 77.69(16) . . ? O1 Co1 N1 99.18(17) 4 . ? O3 Co1 N1 161.73(17) . . ? C1 N1 C5 118.0(5) . . ? C1 N1 Co1 109.9(4) . . ? C5 N1 Co1 132.0(4) . . ? N1 C1 C2 123.1(6) . . ? N1 C1 C6 117.3(5) . . ? C2 C1 C6 119.7(5) . . ? C3 C2 C1 119.5(6) . . ? C3 C2 H2A 120.3 . . ? C1 C2 H2A 120.3 . . ? C2 C3 C4 117.8(6) . . ? C2 C3 H3A 121.1 . . ? C4 C3 H3A 121.1 . . ? C5 C4 C3 119.7(6) . . ? C5 C4 H4A 120.2 . . ? C3 C4 H4A 120.2 . . ? N1 C5 C4 122.0(6) . . ? N1 C5 C7 116.7(5) . . ? C4 C5 C7 121.3(6) . . ? O1 C6 C1 111.0(5) . . ? O1 C6 H6A 109.4 . . ? C1 C6 H6A 109.4 . . ? O1 C6 H6B 109.4 . . ? C1 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? C6 O1 Co1 111.9(3) . . ? C6 O1 Co1 121.7(4) . 4 ? Co1 O1 Co1 98.72(16) . 4 ? C6 O1 Dy1 117.9(4) . . ? Co1 O1 Dy1 102.17(15) . . ? Co1 O1 Dy1 101.21(16) 4 . ? O2 C7 C5 112.2(6) . . ? O2 C7 H7A 109.2 . . ? C5 C7 H7A 109.2 . . ? O2 C7 H7B 109.2 . . ? C5 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? C7 O2 H2 102(5) . . ? C8 N2 C12 120.4(5) . . ? C8 N2 Dy1 117.6(4) . . ? C12 N2 Dy1 121.7(4) . . ? N2 C8 C9 121.3(6) . . ? N2 C8 C13 117.7(5) . . ? C9 C8 C13 121.0(6) . . ? C10 C9 C8 118.4(6) . . ? C10 C9 H9A 120.8 . . ? C8 C9 H9A 120.8 . . ? C9 C10 C11 120.3(6) . . ? C9 C10 H10A 119.9 . . ? C11 C10 H10A 119.9 . . ? C10 C11 C12 118.0(6) . . ? C10 C11 H11A 121.0 . . ? C12 C11 H11A 121.0 . . ? N2 C12 C11 121.5(6) . . ? N2 C12 C14 117.7(5) . . ? C11 C12 C14 120.8(6) . . ? O3 C13 C8 109.8(5) . . ? O3 C13 H13A 109.7 . . ? C8 C13 H13A 109.7 . . ? O3 C13 H13B 109.7 . . ? C8 C13 H13B 109.7 . . ? H13A C13 H13B 108.2 . . ? C13 O3 Co1 120.5(4) . . ? C13 O3 Dy1 115.1(4) . 4 ? Co1 O3 Dy1 97.68(16) . 4 ? C13 O3 Dy1 114.2(3) . . ? Co1 O3 Dy1 94.31(14) . . ? Dy1 O3 Dy1 112.53(18) 4 . ? O4 C14 C12 110.7(5) . . ? O4 C14 H14A 109.5 . . ? C12 C14 H14A 109.5 . . ? O4 C14 H14B 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? C14 O4 Dy1 122.8(4) . . ? C14 O4 H4 115(5) . . ? Dy1 O4 H4 89(5) . . ? C15 O5 Co1 124.2(5) . . ? C15 O6 Dy1 141.3(5) . . ? O5 C15 O6 124.5(7) . . ? O5 C15 C16 118.7(6) . . ? O6 C15 C16 116.7(6) . . ? C17 C16 C15 109.4(7) . . ? C17 C16 C18 110.8(8) . . ? C15 C16 C18 106.0(6) . . ? C17 C16 C19 109.5(9) . . ? C15 C16 C19 111.0(7) . . ? C18 C16 C19 110.0(9) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C20 O7 Co1 123.3(4) . . ? C20 O8 Dy1 139.7(4) . 4 ? O8 C20 O7 125.6(6) . . ? O8 C20 C21 118.5(6) . . ? O7 C20 C21 115.9(7) . . ? C24 C21 C22 111.1(8) . . ? C24 C21 C23 110.1(9) . . ? C22 C21 C23 110.2(8) . . ? C24 C21 C20 109.4(7) . . ? C22 C21 C20 105.8(6) . . ? C23 C21 C20 110.2(7) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C25 O9 Dy1 137.5(5) . . ? O9 C25 O10 123.9(7) . . ? O9 C25 C26 116.9(7) . . ? O10 C25 C26 119.2(7) . . ? C28 C26 C25 110.1(9) . . ? C28 C26 C29 112.5(16) . . ? C25 C26 C29 106.5(10) . . ? C28 C26 C27 113.8(18) . . ? C25 C26 C27 106.2(13) . . ? C29 C26 C27 107.2(10) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2 O7 0.88(4) 1.89(4) 2.742(7) 162(8) . O4 H4 O10 0.91(4) 1.65(4) 2.543(6) 166(7) . _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.807 _refine_diff_density_min -2.387 _refine_diff_density_rms 0.164