# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 loop_ _publ_author_name _publ_author_address K.Murray ; School of Chemistry, Monash University, PO Box 23, VIC 3800, Australia ; N.Chilton ; School of Chemistry, Monash University, PO Box 23, VIC 3800, Australia ; S.Langley ; School of Chemistry, Monash University, PO Box 23, VIC 3800, Australia ; B.Moubaraki ; School of Chemistry, Monash University, PO Box 23, VIC 3800, Australia ; _publ_contact_author_name 'Murray, Keith' _publ_contact_author_email keith.murray@monash.edu _publ_section_title ; Synthesis, structural and magnetic studies of an isostructural family of mixed 3d/4f tetranuclear 'star' clusters ; _publ_contact_author_address ; School of Chemistry, 171 Monash university, Vic 3800, Australia ; _publ_contact_author_fax +61-3-9905-4597 _publ_contact_author_phone +61-3-9905-4512 _publ_contact_letter ; ; _publ_requested_category ? # Attachment '- 1 Mn3Gdfinal.CIF' #========================================================================== data_1_Mn3Gdfinal _database_code_depnum_ccdc_archive 'CCDC 784701' #TrackingRef '- 1 Mn3Gdfinal.CIF' #========================================================================== _audit_creation_method SHELXL-97 _audit_creation_date '9 November 2005' _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_exptl_prep ; ; _publ_section_exptl_refinement ; The compound was solved via direct methods. The asymmetric unit contains two unique Manganese ions and one Gd ion. All non H-atoms were refined anisotropically. All H-atoms were placed in calculated positions. ; _publ_section_references ;Bruker (1997) SMART (Version 5.054) and SAINT-Plus (Version 6.45). Bruker AXS Inc., Madison, Wisconsin, USA. Bruker (2001) XCIF (Version 6.12). Bruker AXS Inc., Madison, Wisconsin, USA. Bruno, I. J., Cole, J. C., Edgington, P. R., Kessler, M., Macrae, C. F., McCabe, P., Pearson, J. and Taylor, R. (2002) Acta Cryst., B58, 389--397. Farrugia, L. J. (1997) J. Appl. Cryst., 30, 565--565. Sheldrick, G. M. (1990) Acta Cryst., A46, 467--473. Sheldrick, G. M. (1997) SHELXL97., University of Gottingen, Germany. Sheldrick, G. M. (1996) SADABS., University of Gottingen, Germany. ; _publ_section_figure_captions ; ; _publ_section_table_legends ; ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C42 H66 Gd Mn3 N2 O18, C15 H21 Mn O6 ; _chemical_formula_sum 'C57 H87 Gd Mn4 N2 O24' _chemical_formula_weight 1561.30 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' Mn Mn 0.3368 0.7283 '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 Trigonal _symmetry_space_group_name_H-M P-31c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'y, x, z-1/2' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' _cell_length_a 15.9802(3) _cell_length_b 15.9802(3) _cell_length_c 15.4016(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3406.13(18) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 3047 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 26.13 _exptl_crystal_description hexagonal _exptl_crystal_colour brown _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.522 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1598 _exptl_absorpt_coefficient_mu 1.756 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.596 _exptl_absorpt_correction_T_max 0.839 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'APEX X8 Apex CCD' _diffrn_measurement_method 'scans in phi and omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 15439 _diffrn_reflns_av_R_equivalents 0.0558 _diffrn_reflns_av_sigmaI/netI 0.0491 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 30.56 _reflns_number_total 3432 _reflns_number_gt 2867 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex2 V2.0' _computing_cell_refinement 'Bruker Apex2 V2.0' _computing_data_reduction 'Bruker Apex2 V2.0' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-SEED _computing_publication_material 'XCIF V6.12 (BrukerAXS, 2001).' _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 compound was solved via direct methods. The asymmetric unit contains two unique Manganese ions and one Gd ion. All non H-atoms were refined anisotropically. All H-atoms were placed in calculated positions. ; _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^)+(0.0542P)^2^+4.5602P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3432 _refine_ls_number_parameters 138 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0580 _refine_ls_R_factor_gt 0.0443 _refine_ls_wR_factor_ref 0.1136 _refine_ls_wR_factor_gt 0.1061 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 Gd1 Gd 0.3333 0.6667 0.7500 0.01674(11) Uani 1 6 d S . . Mn1 Mn 0.58190(5) 0.79095(2) 0.7500 0.02097(17) Uani 1 2 d S . . Mn2 Mn 0.3333 0.6667 0.2500 0.0349(3) Uani 1 6 d S . . O1 O 0.47845(16) 0.68950(17) 0.68848(17) 0.0259(5) Uani 1 1 d . . . O2 O 0.59945(18) 0.90406(19) 0.65938(18) 0.0338(6) Uani 1 1 d . . . O3 O 0.68079(16) 0.78508(18) 0.68153(17) 0.0295(5) Uani 1 1 d . . . O4 O 0.4352(3) 0.7673(3) 0.3244(2) 0.0549(9) Uani 1 1 d . . . N1 N 0.3333 0.6667 0.5746(3) 0.0226(9) Uani 1 3 d S . . C1 C 0.4309(3) 0.6948(4) 0.5451(3) 0.0447(10) Uani 1 1 d . . . H1A H 0.4682 0.7647 0.5406 0.054 Uiso 1 1 calc R . . H1B H 0.4269 0.6684 0.4875 0.054 Uiso 1 1 calc R . . C2 C 0.4821(3) 0.6621(3) 0.6025(3) 0.0416(10) Uani 1 1 d . . . H2A H 0.4525 0.5924 0.5990 0.050 Uiso 1 1 calc R . . H2B H 0.5489 0.6905 0.5841 0.050 Uiso 1 1 calc R . . C3 C 0.6925(4) 1.0533(3) 0.5878(4) 0.0595(14) Uani 1 1 d . . . H4A H 0.6344 1.0417 0.5592 0.089 Uiso 1 1 calc R . . H4B H 0.7451 1.0797 0.5471 0.089 Uiso 1 1 calc R . . H4C H 0.7068 1.0981 0.6346 0.089 Uiso 1 1 calc R . . C4 C 0.6791(3) 0.9594(3) 0.6233(3) 0.0431(10) Uani 1 1 d . . . C5 C 0.7556(3) 0.9388(3) 0.6150(3) 0.0462(10) Uani 1 1 d . . . H5 H 0.8126 0.9858 0.5894 0.055 Uiso 1 1 calc R . . C6 C 0.7520(3) 0.8548(3) 0.6419(3) 0.0386(9) Uani 1 1 d . . . C7 C 0.8356(3) 0.8376(4) 0.6267(4) 0.0540(12) Uani 1 1 d . . . H7A H 0.8555 0.8236 0.6810 0.081 Uiso 1 1 calc R . . H7B H 0.8886 0.8944 0.6015 0.081 Uiso 1 1 calc R . . H7C H 0.8158 0.7839 0.5879 0.081 Uiso 1 1 calc R . . C8 C 0.4510(3) 0.9020(5) 0.2500 0.085(3) Uani 1 2 d S . . H8 H 0.4846 0.9692 0.2500 0.102 Uiso 1 2 calc SR . . C9 C 0.4757(4) 0.8559(4) 0.3147(3) 0.0577(13) Uani 1 1 d . . . C10 C 0.5529(5) 0.9152(5) 0.3799(5) 0.108(3) Uani 1 1 d . . . H10A H 0.5244 0.9287 0.4288 0.162 Uiso 1 1 calc R . . H10B H 0.6001 0.9748 0.3536 0.162 Uiso 1 1 calc R . . H10C H 0.5837 0.8799 0.3988 0.162 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.01391(12) 0.01391(12) 0.0224(2) 0.000 0.000 0.00696(6) Mn1 0.0141(3) 0.0207(2) 0.0259(4) 0.0017(2) 0.000 0.00703(14) Mn2 0.0389(5) 0.0389(5) 0.0269(7) 0.000 0.000 0.0194(2) O1 0.0191(10) 0.0273(11) 0.0310(13) -0.0081(10) -0.0008(9) 0.0114(9) O2 0.0284(12) 0.0310(13) 0.0413(15) 0.0076(11) -0.0034(11) 0.0142(11) O3 0.0191(11) 0.0317(12) 0.0364(14) 0.0045(10) 0.0052(10) 0.0116(10) O4 0.067(2) 0.0477(18) 0.0396(18) -0.0031(15) 0.0040(16) 0.0204(17) N1 0.0239(13) 0.0239(13) 0.020(2) 0.000 0.000 0.0119(7) C1 0.045(2) 0.072(3) 0.023(2) 0.0000(19) 0.0071(17) 0.033(2) C2 0.0331(19) 0.064(3) 0.039(2) -0.023(2) -0.0053(16) 0.033(2) C3 0.064(3) 0.036(2) 0.066(3) 0.022(2) -0.007(3) 0.016(2) C4 0.040(2) 0.035(2) 0.042(2) 0.0121(18) -0.0075(18) 0.0096(17) C5 0.0292(19) 0.041(2) 0.051(3) 0.013(2) 0.0025(18) 0.0044(17) C6 0.0272(17) 0.045(2) 0.037(2) 0.0023(17) 0.0020(15) 0.0129(16) C7 0.0252(19) 0.075(3) 0.059(3) 0.000(3) 0.011(2) 0.023(2) C8 0.124(7) 0.027(3) 0.071(6) 0.000 0.009(5) 0.0134(16) C9 0.052(3) 0.046(3) 0.049(3) -0.002(2) 0.019(2) 0.005(2) C10 0.076(4) 0.079(5) 0.088(5) -0.009(4) 0.000(4) -0.023(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 2.358(2) 2_665 ? Gd1 O1 2.358(2) 5_556 ? Gd1 O1 2.358(2) 6_566 ? Gd1 O1 2.358(2) 3_565 ? Gd1 O1 2.358(2) . ? Gd1 O1 2.358(2) 4_666 ? Gd1 N1 2.701(5) 4_666 ? Gd1 N1 2.701(5) . ? Gd1 Mn1 3.4400(6) 2_665 ? Gd1 Mn1 3.4400(6) 3_565 ? Gd1 Mn1 3.4400(6) . ? Mn1 O1 1.892(2) 6_566 ? Mn1 O1 1.892(2) . ? Mn1 O3 1.941(2) 6_566 ? Mn1 O3 1.941(2) . ? Mn1 O2 2.188(3) . ? Mn1 O2 2.188(3) 6_566 ? Mn2 O4 1.982(4) 2_665 ? Mn2 O4 1.982(4) 5 ? Mn2 O4 1.982(4) . ? Mn2 O4 1.982(4) 4_665 ? Mn2 O4 1.982(4) 6_565 ? Mn2 O4 1.982(4) 3_565 ? O1 C2 1.406(5) . ? O2 C4 1.259(5) . ? O3 C6 1.281(4) . ? O4 C9 1.237(6) . ? N1 C1 1.463(4) 2_665 ? N1 C1 1.463(4) 3_565 ? N1 C1 1.463(4) . ? C1 C2 1.466(6) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.509(6) . ? C3 H4A 0.9600 . ? C3 H4B 0.9600 . ? C3 H4C 0.9600 . ? C4 C5 1.421(6) . ? C5 C6 1.379(6) . ? C5 H5 0.9300 . ? C6 C7 1.510(5) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 C9 1.408(7) 5 ? C8 C9 1.408(7) . ? C8 H8 0.9300 . ? C9 C10 1.503(8) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? 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 O1 63.24(11) 2_665 5_556 ? O1 Gd1 O1 88.29(12) 2_665 6_566 ? O1 Gd1 O1 104.95(7) 5_556 6_566 ? O1 Gd1 O1 104.95(7) 2_665 3_565 ? O1 Gd1 O1 88.29(12) 5_556 3_565 ? O1 Gd1 O1 164.60(11) 6_566 3_565 ? O1 Gd1 O1 104.95(7) 2_665 . ? O1 Gd1 O1 164.60(11) 5_556 . ? O1 Gd1 O1 63.24(11) 6_566 . ? O1 Gd1 O1 104.95(7) 3_565 . ? O1 Gd1 O1 164.60(11) 2_665 4_666 ? O1 Gd1 O1 104.95(7) 5_556 4_666 ? O1 Gd1 O1 104.95(7) 6_566 4_666 ? O1 Gd1 O1 63.24(11) 3_565 4_666 ? O1 Gd1 O1 88.29(12) . 4_666 ? O1 Gd1 N1 113.69(6) 2_665 4_666 ? O1 Gd1 N1 66.31(6) 5_556 4_666 ? O1 Gd1 N1 66.31(6) 6_566 4_666 ? O1 Gd1 N1 113.69(6) 3_565 4_666 ? O1 Gd1 N1 113.69(6) . 4_666 ? O1 Gd1 N1 66.31(6) 4_666 4_666 ? O1 Gd1 N1 66.31(6) 2_665 . ? O1 Gd1 N1 113.69(6) 5_556 . ? O1 Gd1 N1 113.69(6) 6_566 . ? O1 Gd1 N1 66.31(6) 3_565 . ? O1 Gd1 N1 66.31(6) . . ? O1 Gd1 N1 113.69(6) 4_666 . ? N1 Gd1 N1 180.000(1) 4_666 . ? O1 Gd1 Mn1 31.62(6) 2_665 2_665 ? O1 Gd1 Mn1 31.62(6) 5_556 2_665 ? O1 Gd1 Mn1 97.70(6) 6_566 2_665 ? O1 Gd1 Mn1 97.70(6) 3_565 2_665 ? O1 Gd1 Mn1 135.85(6) . 2_665 ? O1 Gd1 Mn1 135.85(6) 4_666 2_665 ? N1 Gd1 Mn1 90.0 4_666 2_665 ? N1 Gd1 Mn1 90.0 . 2_665 ? O1 Gd1 Mn1 135.85(6) 2_665 3_565 ? O1 Gd1 Mn1 97.70(6) 5_556 3_565 ? O1 Gd1 Mn1 135.85(6) 6_566 3_565 ? O1 Gd1 Mn1 31.62(6) 3_565 3_565 ? O1 Gd1 Mn1 97.70(6) . 3_565 ? O1 Gd1 Mn1 31.62(6) 4_666 3_565 ? N1 Gd1 Mn1 90.000(1) 4_666 3_565 ? N1 Gd1 Mn1 90.000(1) . 3_565 ? Mn1 Gd1 Mn1 120.0 2_665 3_565 ? O1 Gd1 Mn1 97.70(6) 2_665 . ? O1 Gd1 Mn1 135.85(6) 5_556 . ? O1 Gd1 Mn1 31.62(6) 6_566 . ? O1 Gd1 Mn1 135.85(6) 3_565 . ? O1 Gd1 Mn1 31.62(6) . . ? O1 Gd1 Mn1 97.70(6) 4_666 . ? N1 Gd1 Mn1 90.000(1) 4_666 . ? N1 Gd1 Mn1 90.000(1) . . ? Mn1 Gd1 Mn1 120.0 2_665 . ? Mn1 Gd1 Mn1 120.0 3_565 . ? O1 Mn1 O1 81.63(14) 6_566 . ? O1 Mn1 O3 94.03(10) 6_566 6_566 ? O1 Mn1 O3 175.66(10) . 6_566 ? O1 Mn1 O3 175.66(10) 6_566 . ? O1 Mn1 O3 94.03(10) . . ? O3 Mn1 O3 90.31(15) 6_566 . ? O1 Mn1 O2 94.78(11) 6_566 . ? O1 Mn1 O2 94.86(11) . . ? O3 Mn1 O2 85.48(10) 6_566 . ? O3 Mn1 O2 85.54(10) . . ? O1 Mn1 O2 94.85(11) 6_566 6_566 ? O1 Mn1 O2 94.78(11) . 6_566 ? O3 Mn1 O2 85.54(10) 6_566 6_566 ? O3 Mn1 O2 85.48(10) . 6_566 ? O2 Mn1 O2 167.25(14) . 6_566 ? O1 Mn1 Gd1 40.82(7) 6_566 . ? O1 Mn1 Gd1 40.82(7) . . ? O3 Mn1 Gd1 134.84(7) 6_566 . ? O3 Mn1 Gd1 134.84(8) . . ? O2 Mn1 Gd1 96.37(7) . . ? O2 Mn1 Gd1 96.37(7) 6_566 . ? O4 Mn2 O4 89.4(2) 2_665 5 ? O4 Mn2 O4 89.93(14) 2_665 . ? O4 Mn2 O4 90.8(2) 5 . ? O4 Mn2 O4 90.8(2) 2_665 4_665 ? O4 Mn2 O4 89.93(14) 5 4_665 ? O4 Mn2 O4 179.0(2) . 4_665 ? O4 Mn2 O4 179.0(2) 2_665 6_565 ? O4 Mn2 O4 89.93(14) 5 6_565 ? O4 Mn2 O4 89.4(2) . 6_565 ? O4 Mn2 O4 89.93(14) 4_665 6_565 ? O4 Mn2 O4 89.93(14) 2_665 3_565 ? O4 Mn2 O4 179.0(2) 5 3_565 ? O4 Mn2 O4 89.93(14) . 3_565 ? O4 Mn2 O4 89.4(2) 4_665 3_565 ? O4 Mn2 O4 90.8(2) 6_565 3_565 ? C2 O1 Mn1 125.7(2) . . ? C2 O1 Gd1 121.4(2) . . ? Mn1 O1 Gd1 107.56(10) . . ? C4 O2 Mn1 121.9(3) . . ? C6 O3 Mn1 127.4(3) . . ? C9 O4 Mn2 127.3(4) . . ? C1 N1 C1 110.8(2) 2_665 3_565 ? C1 N1 C1 110.8(2) 2_665 . ? C1 N1 C1 110.8(2) 3_565 . ? C1 N1 Gd1 108.1(2) 2_665 . ? C1 N1 Gd1 108.1(2) 3_565 . ? C1 N1 Gd1 108.1(2) . . ? N1 C1 C2 113.7(4) . . ? N1 C1 H1A 108.8 . . ? C2 C1 H1A 108.8 . . ? N1 C1 H1B 108.8 . . ? C2 C1 H1B 108.8 . . ? H1A C1 H1B 107.7 . . ? O1 C2 C1 109.8(3) . . ? O1 C2 H2A 109.7 . . ? C1 C2 H2A 109.7 . . ? O1 C2 H2B 109.7 . . ? C1 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? C4 C3 H4A 109.5 . . ? C4 C3 H4B 109.5 . . ? H4A C3 H4B 109.5 . . ? C4 C3 H4C 109.5 . . ? H4A C3 H4C 109.5 . . ? H4B C3 H4C 109.5 . . ? O2 C4 C5 124.2(4) . . ? O2 C4 C3 116.7(4) . . ? C5 C4 C3 119.1(4) . . ? C6 C5 C4 125.2(4) . . ? C6 C5 H5 117.4 . . ? C4 C5 H5 117.4 . . ? O3 C6 C5 125.2(4) . . ? O3 C6 C7 113.5(4) . . ? C5 C6 C7 121.4(4) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C9 126.1(7) 5 . ? C9 C8 H8 117.0 5 . ? C9 C8 H8 117.0 . . ? O4 C9 C8 124.2(5) . . ? O4 C9 C10 115.8(6) . . ? C8 C9 C10 120.0(6) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 30.56 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.271 _refine_diff_density_min -0.695 _refine_diff_density_rms 0.104 # Attachment '- 2 Mn3Dyfinal.CIF' #========================================================================== data_2_Mn3Dyfinal _database_code_depnum_ccdc_archive 'CCDC 784702' #TrackingRef '- 2 Mn3Dyfinal.CIF' #========================================================================== _audit_creation_method SHELXL-97 _audit_creation_date '9 November 2005' _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_exptl_prep ; ; _publ_section_exptl_refinement ; The data was collected on the Australian synchrotron in which only a wavelength of 0.77 A and a resolution of ~0.9 A was possible. We were also restricted to one 360 degree phi scan. The compound was solved via direct methods. The asymmetric unit contains two unique Manganese ions and one Gd ion. All non H-atoms were refined anisotropically. All H-atoms were placed in calculated positions. ; _publ_section_references ;Bruker (1997) SMART (Version 5.054) and SAINT-Plus (Version 6.45). Bruker AXS Inc., Madison, Wisconsin, USA. Bruker (2001) XCIF (Version 6.12). Bruker AXS Inc., Madison, Wisconsin, USA. Bruno, I. J., Cole, J. C., Edgington, P. R., Kessler, M., Macrae, C. F., McCabe, P., Pearson, J. and Taylor, R. (2002) Acta Cryst., B58, 389--397. Farrugia, L. J. (1997) J. Appl. Cryst., 30, 565--565. Sheldrick, G. M. (1990) Acta Cryst., A46, 467--473. Sheldrick, G. M. (1997) SHELXL97., University of Gottingen, Germany. Sheldrick, G. M. (1996) SADABS., University of Gottingen, Germany. ; _publ_section_figure_captions ; ; _publ_section_table_legends ; ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C42 H66 Dy Mn3 N2 O18, C15 H21 Mn O6 ; _chemical_formula_sum 'C57 H87 Dy Mn4 N2 O24' _chemical_formula_weight 1566.55 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' Mn Mn 0.3368 0.7283 '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 trigonal _symmetry_space_group_name_H-M P-31c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'y, x, z-1/2' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' _cell_length_a 16.036(2) _cell_length_b 16.036(2) _cell_length_c 15.368(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3422.5(9) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 37598 _cell_measurement_theta_min 1.60 _cell_measurement_theta_max 26.59 _exptl_crystal_description hexagonal _exptl_crystal_colour brown _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.520 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1602 _exptl_absorpt_coefficient_mu 1.871 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.786 _exptl_absorpt_correction_T_max 0.876 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.77501 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Australian synchrotron MX1' _diffrn_radiation_monochromator silicon _diffrn_measurement_device_type 'ADSC Quantum 210r' _diffrn_measurement_method 'scans in phi' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37598 _diffrn_reflns_av_R_equivalents 0.0420 _diffrn_reflns_av_sigmaI/netI 0.0134 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 26.59 _reflns_number_total 1851 _reflns_number_gt 1821 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Blu-Ice (McPhillips et al, 2002)' _computing_cell_refinement 'XDS (Kabsch, 1993)' _computing_data_reduction 'XDS (Kabsch, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-SEED _computing_publication_material 'XCIF V6.12 (BrukerAXS, 2001).' _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 data was collected on the Australian synchrotron in which only a wavelength of 0.77 A and a resolution of ~0.9 A was possible. We were also restricted to one 360 degree phi scan. The compound was solved via direct methods. The asymmetric unit contains two unique Manganese ions and one Gd ion. All non H-atoms were refined anisotropically. All H-atoms were placed in calculated positions. ; _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^)+(0.0400P)^2^+8.0170P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1851 _refine_ls_number_parameters 138 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0276 _refine_ls_R_factor_gt 0.0273 _refine_ls_wR_factor_ref 0.0716 _refine_ls_wR_factor_gt 0.0715 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.100 _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 0.3333 0.6667 0.7500 0.00451(13) Uani 1 6 d S . . Mn1 Mn 0.58007(4) 0.79003(2) 0.7500 0.00977(17) Uani 1 2 d S . . Mn2 Mn 0.6667 1.3333 0.7500 0.0218(3) Uani 1 6 d S . . O1 O 0.47665(14) 0.78957(14) 0.68983(14) 0.0121(4) Uani 1 1 d . . . O2 O 0.67875(14) 0.89489(15) 0.68153(15) 0.0189(5) Uani 1 1 d . . . O3 O 0.59839(15) 0.69553(16) 0.65779(15) 0.0217(5) Uani 1 1 d . . . O4 O 0.6675(2) 1.2322(2) 0.67563(18) 0.0368(7) Uani 1 1 d . . . N1 N 0.3333 0.6667 0.5741(3) 0.0147(10) Uani 1 3 d S . . C1 C 0.4320(2) 0.7359(3) 0.5437(2) 0.0222(7) Uani 1 1 d . . . H1A H 0.4291 0.7573 0.4840 0.027 Uiso 1 1 calc R . . H1B H 0.4711 0.7038 0.5422 0.027 Uiso 1 1 calc R . . C2 C 0.4790(2) 0.8219(2) 0.6031(2) 0.0211(7) Uani 1 1 d . . . H2A H 0.5465 0.8651 0.5849 0.025 Uiso 1 1 calc R . . H2B H 0.4442 0.8584 0.6000 0.025 Uiso 1 1 calc R . . C3 C 0.8343(3) 0.9988(3) 0.6280(3) 0.0419(11) Uani 1 1 d . . . H3A H 0.8134 1.0343 0.5904 0.063 Uiso 1 1 calc R . . H3B H 0.8875 0.9955 0.6000 0.063 Uiso 1 1 calc R . . H3C H 0.8560 1.0319 0.6840 0.063 Uiso 1 1 calc R . . C4 C 0.7510(2) 0.8978(3) 0.6426(2) 0.0296(8) Uani 1 1 d . . . C5 C 0.7550(3) 0.8176(3) 0.6145(3) 0.0340(9) Uani 1 1 d . . . H5 H 0.8131 0.8281 0.5881 0.041 Uiso 1 1 calc R . . C6 C 0.6788(3) 0.7208(3) 0.6225(3) 0.0321(9) Uani 1 1 d . . . C7 C 0.6932(3) 0.6405(3) 0.5866(3) 0.0418(10) Uani 1 1 d . . . H7A H 0.7127 0.6127 0.6338 0.063 Uiso 1 1 calc R . . H7B H 0.7435 0.6666 0.5418 0.063 Uiso 1 1 calc R . . H7C H 0.6328 0.5904 0.5610 0.063 Uiso 1 1 calc R . . C8 C 0.5486(2) 1.0973(4) 0.7500 0.057(2) Uani 1 2 d S . . H8 H 0.5144 1.0289 0.7500 0.068 Uiso 1 2 calc SR . . C9 C 0.6186(3) 1.1431(3) 0.6857(3) 0.0359(9) Uani 1 1 d . . . C10 C 0.6375(5) 1.0849(4) 0.6196(4) 0.0718(18) Uani 1 1 d . . . H10A H 0.5873 1.0613 0.5747 0.108 Uiso 1 1 calc R . . H10B H 0.6368 1.0301 0.6485 0.108 Uiso 1 1 calc R . . H10C H 0.7005 1.1256 0.5926 0.108 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 0.00301(14) 0.00301(14) 0.00751(19) 0.000 0.000 0.00151(7) Mn1 0.0038(3) 0.0084(2) 0.0156(3) -0.0023(2) 0.000 0.00189(15) Mn2 0.0244(4) 0.0244(4) 0.0166(6) 0.000 0.000 0.0122(2) O1 0.0073(10) 0.0122(10) 0.0150(11) 0.0044(8) 0.0020(8) 0.0036(8) O2 0.0091(10) 0.0151(11) 0.0267(13) -0.0004(9) 0.0052(9) 0.0018(9) O3 0.0130(11) 0.0218(12) 0.0319(13) -0.0121(10) -0.0036(10) 0.0100(10) O4 0.0449(18) 0.0300(15) 0.0261(15) -0.0010(12) -0.0030(11) 0.0118(13) N1 0.0156(14) 0.0156(14) 0.013(2) 0.000 0.000 0.0078(7) C1 0.0234(18) 0.0294(19) 0.0097(16) 0.0058(13) 0.0068(13) 0.0102(15) C2 0.0165(16) 0.0203(17) 0.0206(17) 0.0119(14) 0.0041(13) 0.0048(15) C3 0.0136(18) 0.041(2) 0.051(3) 0.008(2) 0.0099(17) -0.0015(17) C4 0.0159(17) 0.039(2) 0.028(2) 0.0000(16) 0.0023(14) 0.0091(16) C5 0.0191(18) 0.048(2) 0.037(2) -0.0065(18) 0.0045(15) 0.0179(18) C6 0.025(2) 0.042(2) 0.035(2) -0.0206(18) -0.0100(16) 0.0214(18) C7 0.037(2) 0.052(3) 0.049(3) -0.027(2) -0.006(2) 0.033(2) C8 0.078(4) 0.016(3) 0.056(4) 0.000 0.009(3) 0.0080(14) C9 0.050(3) 0.033(2) 0.036(2) 0.0014(17) -0.0092(19) 0.029(2) C10 0.129(5) 0.057(3) 0.061(3) 0.003(3) 0.013(4) 0.069(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 Dy1 O1 2.343(2) 2_665 ? Dy1 O1 2.343(2) 5_556 ? Dy1 O1 2.343(2) 4_666 ? Dy1 O1 2.343(2) . ? Dy1 O1 2.343(2) 3_565 ? Dy1 O1 2.343(2) 6_566 ? Dy1 N1 2.703(4) 4_666 ? Dy1 N1 2.703(4) . ? Dy1 Mn1 3.4266(7) 2_665 ? Dy1 Mn1 3.4266(7) . ? Dy1 Mn1 3.4266(7) 3_565 ? Mn1 O1 1.896(2) 6_566 ? Mn1 O1 1.896(2) . ? Mn1 O2 1.944(2) 6_566 ? Mn1 O2 1.944(2) . ? Mn1 O3 2.199(2) . ? Mn1 O3 2.199(2) 6_566 ? Mn2 O4 1.989(3) 4_776 ? Mn2 O4 1.989(3) . ? Mn2 O4 1.989(3) 2_775 ? Mn2 O4 1.989(3) 5_556 ? Mn2 O4 1.989(3) 6_576 ? Mn2 O4 1.989(3) 3_575 ? O1 C2 1.424(4) . ? O2 C4 1.284(4) . ? O3 C6 1.264(4) . ? O4 C9 1.249(5) . ? N1 C1 1.482(4) 2_665 ? N1 C1 1.482(4) . ? N1 C1 1.482(4) 3_565 ? C1 C2 1.505(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.516(5) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.388(6) . ? C5 C6 1.421(6) . ? C5 H5 0.9500 . ? C6 C7 1.522(5) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.396(5) . ? C8 C9 1.396(5) 5_556 ? C8 H8 0.9500 . ? C9 C10 1.509(6) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 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 Dy1 O1 63.72(10) 2_665 5_556 ? O1 Dy1 O1 86.51(10) 2_665 4_666 ? O1 Dy1 O1 105.45(6) 5_556 4_666 ? O1 Dy1 O1 105.45(6) 2_665 . ? O1 Dy1 O1 86.51(10) 5_556 . ? O1 Dy1 O1 166.10(10) 4_666 . ? O1 Dy1 O1 105.45(6) 2_665 3_565 ? O1 Dy1 O1 166.10(10) 5_556 3_565 ? O1 Dy1 O1 63.72(10) 4_666 3_565 ? O1 Dy1 O1 105.45(6) . 3_565 ? O1 Dy1 O1 166.10(10) 2_665 6_566 ? O1 Dy1 O1 105.45(6) 5_556 6_566 ? O1 Dy1 O1 105.45(6) 4_666 6_566 ? O1 Dy1 O1 63.72(10) . 6_566 ? O1 Dy1 O1 86.51(10) 3_565 6_566 ? O1 Dy1 N1 113.24(5) 2_665 4_666 ? O1 Dy1 N1 66.76(5) 5_556 4_666 ? O1 Dy1 N1 66.76(5) 4_666 4_666 ? O1 Dy1 N1 113.24(5) . 4_666 ? O1 Dy1 N1 113.24(5) 3_565 4_666 ? O1 Dy1 N1 66.76(5) 6_566 4_666 ? O1 Dy1 N1 66.76(5) 2_665 . ? O1 Dy1 N1 113.24(5) 5_556 . ? O1 Dy1 N1 113.24(5) 4_666 . ? O1 Dy1 N1 66.76(5) . . ? O1 Dy1 N1 66.76(5) 3_565 . ? O1 Dy1 N1 113.24(5) 6_566 . ? N1 Dy1 N1 180.000(2) 4_666 . ? O1 Dy1 Mn1 31.86(5) 2_665 2_665 ? O1 Dy1 Mn1 31.86(5) 5_556 2_665 ? O1 Dy1 Mn1 96.95(5) 4_666 2_665 ? O1 Dy1 Mn1 96.95(5) . 2_665 ? O1 Dy1 Mn1 136.75(5) 3_565 2_665 ? O1 Dy1 Mn1 136.75(5) 6_566 2_665 ? N1 Dy1 Mn1 90.0 4_666 2_665 ? N1 Dy1 Mn1 90.0 . 2_665 ? O1 Dy1 Mn1 136.75(5) 2_665 . ? O1 Dy1 Mn1 96.95(5) 5_556 . ? O1 Dy1 Mn1 136.75(5) 4_666 . ? O1 Dy1 Mn1 31.86(5) . . ? O1 Dy1 Mn1 96.95(5) 3_565 . ? O1 Dy1 Mn1 31.86(5) 6_566 . ? N1 Dy1 Mn1 90.000(1) 4_666 . ? N1 Dy1 Mn1 90.000(1) . . ? Mn1 Dy1 Mn1 120.0 2_665 . ? O1 Dy1 Mn1 96.95(5) 2_665 3_565 ? O1 Dy1 Mn1 136.75(5) 5_556 3_565 ? O1 Dy1 Mn1 31.86(5) 4_666 3_565 ? O1 Dy1 Mn1 136.75(5) . 3_565 ? O1 Dy1 Mn1 31.86(5) 3_565 3_565 ? O1 Dy1 Mn1 96.95(5) 6_566 3_565 ? N1 Dy1 Mn1 90.000(1) 4_666 3_565 ? N1 Dy1 Mn1 90.000(1) . 3_565 ? Mn1 Dy1 Mn1 120.0 2_665 3_565 ? Mn1 Dy1 Mn1 120.0 . 3_565 ? O1 Mn1 O1 81.48(12) 6_566 . ? O1 Mn1 O2 94.10(9) 6_566 6_566 ? O1 Mn1 O2 175.47(9) . 6_566 ? O1 Mn1 O2 175.47(9) 6_566 . ? O1 Mn1 O2 94.10(9) . . ? O2 Mn1 O2 90.33(14) 6_566 . ? O1 Mn1 O3 94.26(9) 6_566 . ? O1 Mn1 O3 95.79(9) . . ? O2 Mn1 O3 85.47(9) 6_566 . ? O2 Mn1 O3 85.17(9) . . ? O1 Mn1 O3 95.79(9) 6_566 6_566 ? O1 Mn1 O3 94.26(9) . 6_566 ? O2 Mn1 O3 85.17(9) 6_566 6_566 ? O2 Mn1 O3 85.47(9) . 6_566 ? O3 Mn1 O3 166.71(12) . 6_566 ? O1 Mn1 Dy1 40.74(6) 6_566 . ? O1 Mn1 Dy1 40.74(6) . . ? O2 Mn1 Dy1 134.83(7) 6_566 . ? O2 Mn1 Dy1 134.83(7) . . ? O3 Mn1 Dy1 96.64(6) . . ? O3 Mn1 Dy1 96.64(6) 6_566 . ? O4 Mn2 O4 89.27(16) 4_776 . ? O4 Mn2 O4 90.17(16) 4_776 2_775 ? O4 Mn2 O4 90.28(12) . 2_775 ? O4 Mn2 O4 90.28(12) 4_776 5_556 ? O4 Mn2 O4 90.17(16) . 5_556 ? O4 Mn2 O4 179.37(16) 2_775 5_556 ? O4 Mn2 O4 90.28(12) 4_776 6_576 ? O4 Mn2 O4 179.37(16) . 6_576 ? O4 Mn2 O4 89.27(17) 2_775 6_576 ? O4 Mn2 O4 90.28(12) 5_556 6_576 ? O4 Mn2 O4 179.37(16) 4_776 3_575 ? O4 Mn2 O4 90.28(12) . 3_575 ? O4 Mn2 O4 90.28(12) 2_775 3_575 ? O4 Mn2 O4 89.27(17) 5_556 3_575 ? O4 Mn2 O4 90.17(16) 6_576 3_575 ? C2 O1 Mn1 126.29(19) . . ? C2 O1 Dy1 120.78(18) . . ? Mn1 O1 Dy1 107.40(9) . . ? C4 O2 Mn1 127.8(2) . . ? C6 O3 Mn1 121.4(2) . . ? C9 O4 Mn2 127.3(3) . . ? C1 N1 C1 110.6(2) 2_665 . ? C1 N1 C1 110.6(2) 2_665 3_565 ? C1 N1 C1 110.6(2) . 3_565 ? C1 N1 Dy1 108.3(2) 2_665 . ? C1 N1 Dy1 108.3(2) . . ? C1 N1 Dy1 108.3(2) 3_565 . ? N1 C1 C2 110.7(3) . . ? N1 C1 H1A 109.5 . . ? C2 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 108.1 . . ? O1 C2 C1 108.9(3) . . ? O1 C2 H2A 109.9 . . ? C1 C2 H2A 109.9 . . ? O1 C2 H2B 109.9 . . ? C1 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? C4 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C4 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? O2 C4 C5 124.8(3) . . ? O2 C4 C3 113.9(3) . . ? C5 C4 C3 121.3(3) . . ? C4 C5 C6 124.9(3) . . ? C4 C5 H5 117.6 . . ? C6 C5 H5 117.6 . . ? O3 C6 C5 124.7(3) . . ? O3 C6 C7 116.5(4) . . ? C5 C6 C7 118.8(3) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C9 125.8(6) . 5_556 ? C9 C8 H8 117.1 . . ? C9 C8 H8 117.1 5_556 . ? O4 C9 C8 124.7(4) . . ? O4 C9 C10 114.7(4) . . ? C8 C9 C10 120.6(4) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.59 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.095 _refine_diff_density_min -1.244 _refine_diff_density_rms 0.101 # Attachment '- Chilton3 Fe3Gdfinal new.CIF' #========================================================================== data_Chilton3_Fe3Gdfinal_new _database_code_depnum_ccdc_archive 'CCDC 784703' #TrackingRef '- Chilton3 Fe3Gdfinal new.CIF' #========================================================================== _audit_creation_method SHELXL-97 _audit_creation_date '9 November 2005' _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_exptl_prep ; ; _publ_section_exptl_refinement ; The compound was solved via direct methods. The asymmetric unit contains the entire cluster. All non H-atoms were refined anisotropically. All H-atoms were placed in calculated positions. ; _publ_section_references ;Bruker (1997) SMART (Version 5.054) and SAINT-Plus (Version 6.45). Bruker AXS Inc., Madison, Wisconsin, USA. Bruker (2001) XCIF (Version 6.12). Bruker AXS Inc., Madison, Wisconsin, USA. Bruno, I. J., Cole, J. C., Edgington, P. R., Kessler, M., Macrae, C. F., McCabe, P., Pearson, J. and Taylor, R. (2002) Acta Cryst., B58, 389--397. Farrugia, L. J. (1997) J. Appl. Cryst., 30, 565--565. Sheldrick, G. M. (1990) Acta Cryst., A46, 467--473. Sheldrick, G. M. (1997) SHELXL97., University of Gottingen, Germany. Sheldrick, G. M. (1996) SADABS., University of Gottingen, Germany. ; _publ_section_figure_captions ; ; _publ_section_table_legends ; ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C42 H66 Fe3 Gd N2 O18 ; _chemical_formula_sum 'C42 H66 Fe3 Gd N2 O18' _chemical_formula_weight 1211.77 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' Fe Fe 0.3463 0.8444 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9299(3) _cell_length_b 15.2338(5) _cell_length_c 15.9340(7) _cell_angle_alpha 80.2980(10) _cell_angle_beta 82.3470(10) _cell_angle_gamma 82.567(3) _cell_volume 2576.26(16) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3214 _cell_measurement_theta_min 2.12 _cell_measurement_theta_max 25.12 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.562 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1236 _exptl_absorpt_coefficient_mu 2.167 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.437 _exptl_absorpt_correction_T_max 0.805 _exptl_absorpt_process_details SADABS _exptl_special_details ; Although the Rint value was slightly high the most reasonable space group found statistically was P-1. The only two options found by xprep in this case were Triclinic P-1 or P1 and this compound is part of a family of an isostructural series all of which are found to be in the P-1 space group. Analysis through ADDSYM also suggest P-1 is the correct space group. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'APEX X8 Apex CCD' _diffrn_measurement_method 'scans in phi and omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 21345 _diffrn_reflns_av_R_equivalents 0.1032 _diffrn_reflns_av_sigmaI/netI 0.1220 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8855 _reflns_number_gt 5959 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex2 V2.0' _computing_cell_refinement 'Bruker Apex2 V2.0' _computing_data_reduction 'Bruker Apex2 V2.0' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-SEED _computing_publication_material 'XCIF V6.12 (BrukerAXS, 2001).' _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 compound was solved via direct methods. The asymmetric unit contains the entire cluster. All non H-atoms were refined anisotropically. All H-atoms were placed in calculated positions. ; _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^)+(0.0870P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8855 _refine_ls_number_parameters 606 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1113 _refine_ls_R_factor_gt 0.0653 _refine_ls_wR_factor_ref 0.1685 _refine_ls_wR_factor_gt 0.1423 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _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 Gd1 Gd 0.71737(4) 0.71961(3) 0.69600(3) 0.02277(15) Uani 1 1 d . . . Fe1 Fe 0.78802(11) 0.82027(8) 0.86132(8) 0.0288(3) Uani 1 1 d . . . Fe2 Fe 0.82097(10) 0.80792(8) 0.48729(8) 0.0267(3) Uani 1 1 d . . . Fe3 Fe 0.55424(11) 0.53226(8) 0.73518(9) 0.0312(3) Uani 1 1 d . . . O1 O 0.6923(5) 0.8599(4) 0.9707(4) 0.0368(15) Uani 1 1 d . . . O2 O 0.7528(5) 0.9496(4) 0.8056(4) 0.0364(15) Uani 1 1 d . . . O3 O 0.9449(5) 0.8634(4) 0.8896(4) 0.0409(16) Uani 1 1 d . . . O4 O 0.8329(5) 0.7051(4) 0.9410(4) 0.0333(15) Uani 1 1 d . . . O5 O 0.6449(5) 0.7801(3) 0.8242(4) 0.0256(13) Uani 1 1 d . . . O6 O 0.8700(5) 0.7755(4) 0.7588(4) 0.0298(14) Uani 1 1 d . . . O7 O 0.6622(5) 0.8067(4) 0.4339(4) 0.0345(15) Uani 1 1 d . . . O8 O 0.9102(5) 0.7510(4) 0.3853(4) 0.0338(15) Uani 1 1 d . . . O9 O 0.8272(5) 0.9285(4) 0.4122(4) 0.0340(15) Uani 1 1 d . . . O10 O 0.9919(5) 0.8248(4) 0.5141(4) 0.0334(15) Uani 1 1 d . . . O11 O 0.7261(5) 0.8481(3) 0.5894(4) 0.0279(14) Uani 1 1 d . . . O12 O 0.8180(5) 0.6929(3) 0.5623(3) 0.0240(13) Uani 1 1 d . . . O13 O 0.4191(6) 0.5815(4) 0.8200(4) 0.0436(18) Uani 1 1 d . . . O14 O 0.5551(6) 0.4159(4) 0.8191(5) 0.0463(18) Uani 1 1 d . . . O15 O 0.6765(5) 0.4597(4) 0.6610(4) 0.0341(15) Uani 1 1 d . . . O16 O 0.4194(5) 0.4973(4) 0.6752(4) 0.0398(17) Uani 1 1 d . . . O17 O 0.5525(5) 0.6507(3) 0.6639(4) 0.0277(14) Uani 1 1 d . . . O18 O 0.6929(5) 0.5770(3) 0.7760(4) 0.0251(13) Uani 1 1 d . . . N1 N 0.9354(6) 0.6084(4) 0.7042(5) 0.0280(17) Uani 1 1 d . . . N2 N 0.4995(5) 0.8299(4) 0.6877(4) 0.0209(15) Uani 1 1 d . . . C1 C 0.6395(9) 0.9447(7) 1.0832(6) 0.053(3) Uani 1 1 d . . . H1A H 0.5816 0.9006 1.1077 0.080 Uiso 1 1 calc R . . H1B H 0.5989 1.0051 1.0887 0.080 Uiso 1 1 calc R . . H1C H 0.7133 0.9329 1.1139 0.080 Uiso 1 1 calc R . . C2 C 0.6776(8) 0.9380(6) 0.9892(6) 0.037(2) Uani 1 1 d . . . C3 C 0.6946(8) 1.0164(6) 0.9306(6) 0.034(2) Uani 1 1 d . . . H3 H 0.6808 1.0719 0.9520 0.041 Uiso 1 1 calc R . . C4 C 0.7303(8) 1.0182(6) 0.8433(6) 0.035(2) Uani 1 1 d . . . C5 C 0.7460(9) 1.1060(6) 0.7864(7) 0.048(3) Uani 1 1 d . . . H5A H 0.8343 1.1145 0.7754 0.072 Uiso 1 1 calc R . . H5B H 0.7005 1.1548 0.8147 0.072 Uiso 1 1 calc R . . H5C H 0.7133 1.1059 0.7320 0.072 Uiso 1 1 calc R . . C6 C 1.1172(10) 0.8820(9) 0.9564(8) 0.084(4) Uani 1 1 d . . . H6A H 1.1689 0.8926 0.9013 0.126 Uiso 1 1 calc R . . H6B H 1.1683 0.8488 0.9999 0.126 Uiso 1 1 calc R . . H6C H 1.0814 0.9396 0.9736 0.126 Uiso 1 1 calc R . . C7 C 1.0125(9) 0.8274(7) 0.9477(7) 0.041(3) Uani 1 1 d . . . C8 C 1.0012(9) 0.7456(7) 1.0004(6) 0.048(3) Uani 1 1 d . . . H8 H 1.0562 0.7272 1.0430 0.058 Uiso 1 1 calc R . . C9 C 0.9129(8) 0.6888(7) 0.9938(6) 0.040(2) Uani 1 1 d . . . C10 C 0.9106(9) 0.6022(7) 1.0523(7) 0.054(3) Uani 1 1 d . . . H10A H 0.8483 0.6090 1.1017 0.080 Uiso 1 1 calc R . . H10B H 0.9925 0.5839 1.0721 0.080 Uiso 1 1 calc R . . H10C H 0.8894 0.5565 1.0217 0.080 Uiso 1 1 calc R . . C11 C 0.9996(7) 0.7438(6) 0.7437(6) 0.033(2) Uani 1 1 d . . . H11A H 1.0469 0.7659 0.7832 0.040 Uiso 1 1 calc R . . H11B H 1.0326 0.7665 0.6842 0.040 Uiso 1 1 calc R . . C12 C 1.0142(7) 0.6426(6) 0.7582(6) 0.038(2) Uani 1 1 d . . . H12A H 1.1023 0.6201 0.7437 0.045 Uiso 1 1 calc R . . H12B H 0.9898 0.6202 0.8194 0.045 Uiso 1 1 calc R . . C13 C 0.9056(7) 0.5173(5) 0.7441(6) 0.033(2) Uani 1 1 d . . . H13A H 0.9779 0.4840 0.7711 0.039 Uiso 1 1 calc R . . H13B H 0.8877 0.4843 0.6996 0.039 Uiso 1 1 calc R . . C14 C 0.7939(8) 0.5235(6) 0.8113(6) 0.035(2) Uani 1 1 d . . . H14A H 0.7703 0.4626 0.8340 0.042 Uiso 1 1 calc R . . H14B H 0.8156 0.5495 0.8595 0.042 Uiso 1 1 calc R . . C15 C 0.9981(7) 0.6068(6) 0.6159(6) 0.032(2) Uani 1 1 d . . . H15A H 1.0535 0.5503 0.6135 0.039 Uiso 1 1 calc R . . H15B H 1.0492 0.6574 0.5990 0.039 Uiso 1 1 calc R . . C16 C 0.9001(7) 0.6143(5) 0.5549(6) 0.030(2) Uani 1 1 d . . . H16A H 0.9406 0.6165 0.4953 0.036 Uiso 1 1 calc R . . H16B H 0.8534 0.5612 0.5691 0.036 Uiso 1 1 calc R . . C17 C 0.5193(7) 0.8114(6) 0.8426(6) 0.029(2) Uani 1 1 d . . . H17A H 0.5083 0.8429 0.8930 0.034 Uiso 1 1 calc R . . H17B H 0.4687 0.7604 0.8559 0.034 Uiso 1 1 calc R . . C18 C 0.4772(7) 0.8749(5) 0.7657(6) 0.030(2) Uani 1 1 d . . . H18A H 0.3876 0.8951 0.7770 0.036 Uiso 1 1 calc R . . H18B H 0.5232 0.9283 0.7556 0.036 Uiso 1 1 calc R . . C19 C 0.5099(7) 0.8974(5) 0.6098(5) 0.0257(19) Uani 1 1 d . . . H19A H 0.4490 0.9504 0.6174 0.031 Uiso 1 1 calc R . . H19B H 0.4908 0.8721 0.5604 0.031 Uiso 1 1 calc R . . C20 C 0.6416(7) 0.9259(5) 0.5920(6) 0.031(2) Uani 1 1 d . . . H20A H 0.6512 0.9665 0.5366 0.037 Uiso 1 1 calc R . . H20B H 0.6576 0.9581 0.6378 0.037 Uiso 1 1 calc R . . C21 C 0.4005(7) 0.7733(5) 0.6869(5) 0.029(2) Uani 1 1 d . . . H21A H 0.3276 0.8107 0.6642 0.035 Uiso 1 1 calc R . . H21B H 0.3742 0.7452 0.7462 0.035 Uiso 1 1 calc R . . C22 C 0.4454(7) 0.7013(5) 0.6321(6) 0.028(2) Uani 1 1 d . . . H22A H 0.3796 0.6618 0.6341 0.034 Uiso 1 1 calc R . . H22B H 0.4660 0.7288 0.5718 0.034 Uiso 1 1 calc R . . C23 C 1.1960(8) 0.8652(6) 0.5018(7) 0.047(3) Uani 1 1 d . . . H23A H 1.2129 0.9214 0.5178 0.070 Uiso 1 1 calc R . . H23B H 1.2581 0.8490 0.4551 0.070 Uiso 1 1 calc R . . H23C H 1.2000 0.8176 0.5515 0.070 Uiso 1 1 calc R . . C24 C 1.0675(8) 0.8769(6) 0.4725(6) 0.034(2) Uani 1 1 d . . . C25 C 1.0411(8) 0.9408(6) 0.4039(7) 0.041(3) Uani 1 1 d . . . H25 H 1.1071 0.9725 0.3738 0.049 Uiso 1 1 calc R . . C26 C 0.9259(9) 0.9624(5) 0.3756(6) 0.037(2) Uani 1 1 d . . . C27 C 0.9072(9) 1.0297(6) 0.2968(7) 0.056(3) Uani 1 1 d . . . H27A H 0.8686 1.0029 0.2566 0.084 Uiso 1 1 calc R . . H27B H 0.9877 1.0480 0.2696 0.084 Uiso 1 1 calc R . . H27C H 0.8531 1.0822 0.3127 0.084 Uiso 1 1 calc R . . C28 C 0.9717(9) 0.7350(7) 0.2423(6) 0.050(3) Uani 1 1 d . . . H28A H 1.0110 0.7883 0.2143 0.076 Uiso 1 1 calc R . . H28B H 0.9327 0.7114 0.2001 0.076 Uiso 1 1 calc R . . H28C H 1.0346 0.6893 0.2662 0.076 Uiso 1 1 calc R . . C29 C 0.8742(9) 0.7597(6) 0.3133(6) 0.037(2) Uani 1 1 d . . . C30 C 0.7532(8) 0.7901(6) 0.2941(6) 0.042(3) Uani 1 1 d . . . H30 H 0.7375 0.7986 0.2359 0.051 Uiso 1 1 calc R . . C31 C 0.6553(9) 0.8082(6) 0.3552(7) 0.043(3) Uani 1 1 d . . . C32 C 0.5269(9) 0.8359(7) 0.3292(7) 0.055(3) Uani 1 1 d . . . H32A H 0.5183 0.8093 0.2783 0.082 Uiso 1 1 d . . . H32B H 0.5132 0.9014 0.3151 0.082 Uiso 1 1 d . . . H32C H 0.4649 0.8151 0.3760 0.082 Uiso 1 1 d . . . C33 C 0.7700(8) 0.3504(6) 0.5772(7) 0.052(3) Uani 1 1 d . . . H33A H 0.8422 0.3844 0.5668 0.078 Uiso 1 1 calc R . . H33B H 0.7544 0.3331 0.5234 0.078 Uiso 1 1 calc R . . H33C H 0.7864 0.2964 0.6190 0.078 Uiso 1 1 calc R . . C34 C 0.6573(8) 0.4078(5) 0.6119(6) 0.034(2) Uani 1 1 d . . . C35 C 0.5424(8) 0.3975(6) 0.5892(6) 0.038(2) Uani 1 1 d . . . H35 H 0.5397 0.3563 0.5510 0.045 Uiso 1 1 calc R . . C36 C 0.4307(9) 0.4436(5) 0.6187(7) 0.042(3) Uani 1 1 d . . . C37 C 0.3120(8) 0.4320(6) 0.5882(7) 0.050(3) Uani 1 1 d . . . H37A H 0.2512 0.4155 0.6376 0.075 Uiso 1 1 calc R . . H37B H 0.3263 0.3845 0.5523 0.075 Uiso 1 1 calc R . . H37C H 0.2802 0.4882 0.5546 0.075 Uiso 1 1 calc R . . C38 C 0.5072(11) 0.2993(7) 0.9310(9) 0.084(4) Uani 1 1 d . . . H38A H 0.4700 0.2625 0.8986 0.126 Uiso 1 1 calc R . . H38B H 0.4663 0.2936 0.9900 0.126 Uiso 1 1 calc R . . H38C H 0.5960 0.2789 0.9316 0.126 Uiso 1 1 calc R . . C39 C 0.4911(10) 0.3952(7) 0.8898(8) 0.056(3) Uani 1 1 d . . . C40 C 0.4034(10) 0.4559(8) 0.9291(7) 0.063(3) Uani 1 1 d . . . H40 H 0.3618 0.4352 0.9837 0.075 Uiso 1 1 calc R . . C41 C 0.3736(8) 0.5453(7) 0.8925(7) 0.049(3) Uani 1 1 d . . . C42 C 0.2733(10) 0.6049(7) 0.9391(7) 0.066(4) Uani 1 1 d . . . H42A H 0.3042 0.6622 0.9406 0.100 Uiso 1 1 calc R . . H42B H 0.2522 0.5751 0.9978 0.100 Uiso 1 1 calc R . . H42C H 0.1992 0.6158 0.9088 0.100 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.0270(2) 0.0187(2) 0.0231(3) -0.00447(18) -0.00253(18) -0.00327(16) Fe1 0.0370(7) 0.0239(7) 0.0283(8) -0.0067(6) -0.0079(6) -0.0067(5) Fe2 0.0312(7) 0.0224(6) 0.0254(7) -0.0021(6) -0.0007(6) -0.0037(5) Fe3 0.0346(7) 0.0223(7) 0.0372(8) -0.0079(6) 0.0048(6) -0.0093(5) O1 0.049(4) 0.035(4) 0.032(4) -0.016(3) -0.006(3) -0.008(3) O2 0.049(4) 0.026(3) 0.036(4) -0.009(3) -0.010(3) -0.003(3) O3 0.040(4) 0.049(4) 0.040(4) -0.006(3) -0.015(3) -0.019(3) O4 0.048(4) 0.027(3) 0.030(4) -0.006(3) -0.015(3) -0.007(3) O5 0.031(3) 0.019(3) 0.028(4) -0.010(3) -0.002(3) 0.002(2) O6 0.031(3) 0.032(3) 0.031(4) -0.012(3) -0.006(3) -0.008(3) O7 0.030(3) 0.041(4) 0.031(4) -0.003(3) -0.002(3) -0.003(3) O8 0.037(3) 0.036(4) 0.029(4) -0.011(3) 0.002(3) -0.004(3) O9 0.044(4) 0.022(3) 0.031(4) 0.002(3) 0.006(3) -0.002(3) O10 0.042(3) 0.029(3) 0.030(4) -0.001(3) 0.001(3) -0.015(3) O11 0.030(3) 0.013(3) 0.038(4) -0.002(3) -0.001(3) 0.005(2) O12 0.030(3) 0.021(3) 0.021(3) -0.010(3) 0.000(3) 0.005(2) O13 0.052(4) 0.038(4) 0.039(4) -0.014(3) 0.020(3) -0.015(3) O14 0.053(4) 0.026(3) 0.056(5) -0.002(3) 0.009(4) -0.012(3) O15 0.036(3) 0.025(3) 0.045(4) -0.018(3) -0.001(3) -0.007(3) O16 0.032(3) 0.031(4) 0.061(5) -0.022(4) -0.003(3) -0.007(3) O17 0.030(3) 0.024(3) 0.029(4) -0.009(3) 0.001(3) -0.001(2) O18 0.030(3) 0.020(3) 0.026(3) -0.005(3) -0.005(3) -0.002(2) N1 0.031(4) 0.018(4) 0.033(5) -0.004(3) -0.003(3) 0.004(3) N2 0.022(3) 0.017(3) 0.023(4) -0.003(3) -0.004(3) 0.003(3) C1 0.064(7) 0.057(7) 0.045(7) -0.027(6) 0.001(6) -0.010(6) C2 0.033(5) 0.042(6) 0.038(6) -0.010(5) -0.012(4) -0.002(4) C3 0.047(5) 0.027(5) 0.033(6) -0.020(5) -0.004(5) 0.000(4) C4 0.037(5) 0.024(5) 0.051(7) -0.015(5) -0.020(5) 0.001(4) C5 0.059(6) 0.024(5) 0.061(8) -0.005(5) -0.009(6) -0.002(5) C6 0.075(8) 0.108(11) 0.084(10) -0.004(9) -0.041(8) -0.050(8) C7 0.048(6) 0.049(6) 0.036(6) -0.029(6) -0.001(5) -0.012(5) C8 0.047(6) 0.073(8) 0.031(6) -0.017(6) -0.009(5) -0.013(6) C9 0.040(6) 0.048(6) 0.030(6) -0.017(5) 0.001(5) 0.011(5) C10 0.061(7) 0.055(7) 0.043(7) 0.001(6) -0.022(6) 0.002(5) C11 0.022(4) 0.039(5) 0.040(6) -0.012(5) -0.003(4) -0.005(4) C12 0.027(5) 0.047(6) 0.043(6) -0.014(5) -0.012(4) -0.003(4) C13 0.036(5) 0.018(4) 0.041(6) -0.004(4) -0.006(4) 0.008(4) C14 0.048(6) 0.026(5) 0.030(6) 0.000(4) -0.002(5) -0.011(4) C15 0.029(5) 0.030(5) 0.038(6) -0.009(4) -0.005(4) 0.003(4) C16 0.039(5) 0.028(5) 0.022(5) -0.015(4) 0.010(4) -0.002(4) C17 0.018(4) 0.039(5) 0.030(5) -0.014(4) 0.001(4) -0.002(4) C18 0.026(4) 0.024(5) 0.039(6) -0.009(4) -0.003(4) 0.006(4) C19 0.036(5) 0.021(4) 0.021(5) -0.009(4) -0.010(4) 0.008(4) C20 0.044(5) 0.012(4) 0.032(6) -0.001(4) 0.002(4) 0.005(4) C21 0.023(4) 0.038(5) 0.026(5) -0.006(4) -0.001(4) -0.004(4) C22 0.028(5) 0.028(5) 0.030(5) -0.008(4) -0.005(4) -0.004(4) C23 0.042(6) 0.046(6) 0.059(7) -0.026(6) 0.003(5) -0.015(5) C24 0.046(5) 0.025(5) 0.037(6) -0.025(5) 0.009(5) -0.012(4) C25 0.041(6) 0.025(5) 0.057(7) -0.013(5) 0.007(5) -0.011(4) C26 0.054(6) 0.015(4) 0.036(6) 0.000(4) 0.008(5) 0.001(4) C27 0.056(7) 0.040(6) 0.060(8) 0.006(6) 0.011(6) 0.002(5) C28 0.069(7) 0.045(6) 0.036(7) -0.010(5) -0.004(6) 0.005(5) C29 0.051(6) 0.027(5) 0.032(6) -0.001(5) 0.003(5) -0.011(4) C30 0.042(6) 0.046(6) 0.038(6) 0.000(5) -0.003(5) -0.008(5) C31 0.048(6) 0.037(6) 0.046(7) 0.005(5) -0.022(5) -0.011(5) C32 0.053(6) 0.067(8) 0.043(7) -0.002(6) -0.016(5) -0.002(5) C33 0.042(6) 0.045(6) 0.076(9) -0.033(6) -0.002(6) 0.000(5) C34 0.042(5) 0.021(5) 0.037(6) -0.009(5) 0.007(5) -0.003(4) C35 0.038(5) 0.041(6) 0.041(6) -0.021(5) -0.006(5) -0.009(5) C36 0.054(6) 0.015(5) 0.061(7) -0.001(5) -0.006(5) -0.021(4) C37 0.042(6) 0.043(6) 0.066(8) -0.009(6) -0.008(5) -0.005(5) C38 0.072(8) 0.061(8) 0.102(11) 0.038(8) -0.002(8) -0.017(7) C39 0.058(7) 0.045(7) 0.063(8) 0.018(6) -0.010(6) -0.024(6) C40 0.067(8) 0.066(8) 0.049(8) 0.003(7) 0.022(6) -0.027(7) C41 0.036(6) 0.067(8) 0.047(7) -0.020(6) 0.010(5) -0.022(5) C42 0.083(8) 0.062(7) 0.051(8) -0.026(6) 0.034(7) -0.015(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O12 2.338(5) . ? Gd1 O17 2.351(5) . ? Gd1 O18 2.355(5) . ? Gd1 O6 2.369(5) . ? Gd1 O11 2.369(5) . ? Gd1 O5 2.380(5) . ? Gd1 N2 2.736(6) . ? Gd1 N1 2.744(6) . ? Fe1 O6 1.941(6) . ? Fe1 O5 1.946(5) . ? Fe1 O4 2.031(6) . ? Fe1 O2 2.031(6) . ? Fe1 O3 2.043(5) . ? Fe1 O1 2.050(6) . ? Fe2 O12 1.949(5) . ? Fe2 O11 1.954(5) . ? Fe2 O9 2.019(6) . ? Fe2 O10 2.028(6) . ? Fe2 O7 2.035(6) . ? Fe2 O8 2.044(6) . ? Fe3 O17 1.962(6) . ? Fe3 O18 1.965(5) . ? Fe3 O15 2.010(6) . ? Fe3 O13 2.024(6) . ? Fe3 O16 2.030(6) . ? Fe3 O14 2.033(6) . ? O1 C2 1.258(10) . ? O2 C4 1.273(9) . ? O3 C7 1.269(12) . ? O4 C9 1.266(11) . ? O5 C17 1.403(9) . ? O6 C11 1.438(9) . ? O7 C31 1.263(11) . ? O8 C29 1.243(11) . ? O9 C26 1.283(10) . ? O10 C24 1.263(9) . ? O11 C20 1.408(9) . ? O12 C16 1.413(9) . ? O13 C41 1.260(11) . ? O14 C39 1.259(12) . ? O15 C34 1.256(10) . ? O16 C36 1.300(10) . ? O17 C22 1.419(9) . ? O18 C14 1.407(10) . ? N1 C13 1.483(9) . ? N1 C15 1.483(10) . ? N1 C12 1.489(10) . ? N2 C21 1.471(9) . ? N2 C19 1.475(10) . ? N2 C18 1.495(10) . ? C1 C2 1.518(13) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.403(12) . ? C3 C4 1.391(12) . ? C3 H3 0.9500 . ? C4 C5 1.499(12) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.533(12) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.390(14) . ? C8 C9 1.401(12) . ? C8 H8 0.9500 . ? C9 C10 1.483(13) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.511(11) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.517(11) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.521(12) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.511(12) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.534(10) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.509(10) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.518(13) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.371(13) . ? C25 C26 1.376(13) . ? C25 H25 0.9500 . ? C26 C27 1.501(13) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.508(12) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.399(13) . ? C30 C31 1.381(12) . ? C30 H30 0.9500 . ? C31 C32 1.504(13) . ? C32 H32A 0.9856 . ? C32 H32B 0.9802 . ? C32 H32C 0.9787 . ? C33 C34 1.514(11) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.387(12) . ? C35 C36 1.393(12) . ? C35 H35 0.9500 . ? C36 C37 1.485(12) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C39 1.496(14) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C40 1.405(14) . ? C40 C41 1.403(15) . ? C40 H40 0.9500 . ? C41 C42 1.527(13) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 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 O12 Gd1 O17 86.59(18) . . ? O12 Gd1 O18 105.44(18) . . ? O17 Gd1 O18 65.10(19) . . ? O12 Gd1 O6 103.67(18) . . ? O17 Gd1 O6 167.77(19) . . ? O18 Gd1 O6 105.14(19) . . ? O12 Gd1 O11 65.01(18) . . ? O17 Gd1 O11 103.46(19) . . ? O18 Gd1 O11 166.34(18) . . ? O6 Gd1 O11 87.12(19) . . ? O12 Gd1 O5 164.91(16) . . ? O17 Gd1 O5 106.28(17) . . ? O18 Gd1 O5 87.46(18) . . ? O6 Gd1 O5 64.64(18) . . ? O11 Gd1 O5 103.52(18) . . ? O12 Gd1 N2 113.94(19) . . ? O17 Gd1 N2 66.18(17) . . ? O18 Gd1 N2 113.42(17) . . ? O6 Gd1 N2 114.21(18) . . ? O11 Gd1 N2 65.23(17) . . ? O5 Gd1 N2 66.16(19) . . ? O12 Gd1 N1 66.0(2) . . ? O17 Gd1 N1 113.57(18) . . ? O18 Gd1 N1 66.39(18) . . ? O6 Gd1 N1 66.02(19) . . ? O11 Gd1 N1 114.92(18) . . ? O5 Gd1 N1 113.9(2) . . ? N2 Gd1 N1 179.75(18) . . ? O6 Fe1 O5 81.6(2) . . ? O6 Fe1 O4 94.4(2) . . ? O5 Fe1 O4 95.6(2) . . ? O6 Fe1 O2 96.4(2) . . ? O5 Fe1 O2 94.9(2) . . ? O4 Fe1 O2 165.9(2) . . ? O6 Fe1 O3 94.0(2) . . ? O5 Fe1 O3 175.1(2) . . ? O4 Fe1 O3 86.7(2) . . ? O2 Fe1 O3 83.6(2) . . ? O6 Fe1 O1 175.5(2) . . ? O5 Fe1 O1 94.6(2) . . ? O4 Fe1 O1 83.6(2) . . ? O2 Fe1 O1 86.3(2) . . ? O3 Fe1 O1 89.9(2) . . ? O12 Fe2 O11 80.8(2) . . ? O12 Fe2 O9 178.1(2) . . ? O11 Fe2 O9 98.3(2) . . ? O12 Fe2 O10 93.0(2) . . ? O11 Fe2 O10 97.4(2) . . ? O9 Fe2 O10 85.5(2) . . ? O12 Fe2 O7 98.1(2) . . ? O11 Fe2 O7 91.2(2) . . ? O9 Fe2 O7 83.5(2) . . ? O10 Fe2 O7 167.0(2) . . ? O12 Fe2 O8 93.0(2) . . ? O11 Fe2 O8 172.7(2) . . ? O9 Fe2 O8 88.0(2) . . ? O10 Fe2 O8 86.6(2) . . ? O7 Fe2 O8 86.0(2) . . ? O17 Fe3 O18 80.3(2) . . ? O17 Fe3 O15 100.4(2) . . ? O18 Fe3 O15 89.6(2) . . ? O17 Fe3 O13 90.2(2) . . ? O18 Fe3 O13 96.5(2) . . ? O15 Fe3 O13 168.6(2) . . ? O17 Fe3 O16 92.2(2) . . ? O18 Fe3 O16 171.1(2) . . ? O15 Fe3 O16 87.0(2) . . ? O13 Fe3 O16 88.3(2) . . ? O17 Fe3 O14 174.4(2) . . ? O18 Fe3 O14 96.3(3) . . ? O15 Fe3 O14 84.0(2) . . ? O13 Fe3 O14 85.7(3) . . ? O16 Fe3 O14 91.5(3) . . ? C2 O1 Fe1 126.3(6) . . ? C4 O2 Fe1 126.7(6) . . ? C7 O3 Fe1 127.5(6) . . ? C9 O4 Fe1 129.0(6) . . ? C17 O5 Fe1 127.5(5) . . ? C17 O5 Gd1 120.9(5) . . ? Fe1 O5 Gd1 106.6(2) . . ? C11 O6 Fe1 125.9(5) . . ? C11 O6 Gd1 121.6(4) . . ? Fe1 O6 Gd1 107.2(2) . . ? C31 O7 Fe2 125.4(6) . . ? C29 O8 Fe2 126.1(6) . . ? C26 O9 Fe2 125.9(6) . . ? C24 O10 Fe2 128.5(6) . . ? C20 O11 Fe2 126.6(5) . . ? C20 O11 Gd1 123.2(5) . . ? Fe2 O11 Gd1 106.3(2) . . ? C16 O12 Fe2 127.3(5) . . ? C16 O12 Gd1 120.4(5) . . ? Fe2 O12 Gd1 107.7(2) . . ? C41 O13 Fe3 130.1(7) . . ? C39 O14 Fe3 131.3(7) . . ? C34 O15 Fe3 129.6(5) . . ? C36 O16 Fe3 128.3(6) . . ? C22 O17 Fe3 124.8(4) . . ? C22 O17 Gd1 121.9(4) . . ? Fe3 O17 Gd1 107.4(3) . . ? C14 O18 Fe3 125.5(5) . . ? C14 O18 Gd1 120.8(4) . . ? Fe3 O18 Gd1 107.2(2) . . ? C13 N1 C15 110.2(6) . . ? C13 N1 C12 109.6(7) . . ? C15 N1 C12 111.2(6) . . ? C13 N1 Gd1 108.5(4) . . ? C15 N1 Gd1 108.6(5) . . ? C12 N1 Gd1 108.7(5) . . ? C21 N2 C19 111.5(6) . . ? C21 N2 C18 110.6(6) . . ? C19 N2 C18 110.1(6) . . ? C21 N2 Gd1 107.3(4) . . ? C19 N2 Gd1 109.5(4) . . ? C18 N2 Gd1 107.8(4) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 125.3(9) . . ? O1 C2 C1 115.5(9) . . ? C3 C2 C1 119.2(8) . . ? C4 C3 C2 124.2(8) . . ? C4 C3 H3 117.9 . . ? C2 C3 H3 117.9 . . ? O2 C4 C3 125.1(9) . . ? O2 C4 C5 115.1(9) . . ? C3 C4 C5 119.8(8) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O3 C7 C8 126.8(8) . . ? O3 C7 C6 113.8(9) . . ? C8 C7 C6 119.4(10) . . ? C7 C8 C9 123.3(10) . . ? C7 C8 H8 118.3 . . ? C9 C8 H8 118.3 . . ? O4 C9 C8 125.2(10) . . ? O4 C9 C10 115.9(9) . . ? C8 C9 C10 118.8(10) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O6 C11 C12 108.9(6) . . ? O6 C11 H11A 109.9 . . ? C12 C11 H11A 109.9 . . ? O6 C11 H11B 109.9 . . ? C12 C11 H11B 109.9 . . ? H11A C11 H11B 108.3 . . ? N1 C12 C11 110.5(7) . . ? N1 C12 H12A 109.6 . . ? C11 C12 H12A 109.6 . . ? N1 C12 H12B 109.6 . . ? C11 C12 H12B 109.6 . . ? H12A C12 H12B 108.1 . . ? N1 C13 C14 110.1(6) . . ? N1 C13 H13A 109.6 . . ? C14 C13 H13A 109.6 . . ? N1 C13 H13B 109.6 . . ? C14 C13 H13B 109.6 . . ? H13A C13 H13B 108.2 . . ? O18 C14 C13 110.7(7) . . ? O18 C14 H14A 109.5 . . ? C13 C14 H14A 109.5 . . ? O18 C14 H14B 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? N1 C15 C16 109.0(6) . . ? N1 C15 H15A 109.9 . . ? C16 C15 H15A 109.9 . . ? N1 C15 H15B 109.9 . . ? C16 C15 H15B 109.9 . . ? H15A C15 H15B 108.3 . . ? O12 C16 C15 109.3(6) . . ? O12 C16 H16A 109.8 . . ? C15 C16 H16A 109.8 . . ? O12 C16 H16B 109.8 . . ? C15 C16 H16B 109.8 . . ? H16A C16 H16B 108.3 . . ? O5 C17 C18 109.0(6) . . ? O5 C17 H17A 109.9 . . ? C18 C17 H17A 109.9 . . ? O5 C17 H17B 109.9 . . ? C18 C17 H17B 109.9 . . ? H17A C17 H17B 108.3 . . ? N2 C18 C17 110.6(6) . . ? N2 C18 H18A 109.5 . . ? C17 C18 H18A 109.5 . . ? N2 C18 H18B 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 108.1 . . ? N2 C19 C20 110.1(7) . . ? N2 C19 H19A 109.6 . . ? C20 C19 H19A 109.6 . . ? N2 C19 H19B 109.6 . . ? C20 C19 H19B 109.6 . . ? H19A C19 H19B 108.2 . . ? O11 C20 C19 108.0(6) . . ? O11 C20 H20A 110.1 . . ? C19 C20 H20A 110.1 . . ? O11 C20 H20B 110.1 . . ? C19 C20 H20B 110.1 . . ? H20A C20 H20B 108.4 . . ? N2 C21 C22 110.5(6) . . ? N2 C21 H21A 109.5 . . ? C22 C21 H21A 109.5 . . ? N2 C21 H21B 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 108.1 . . ? O17 C22 C21 108.5(6) . . ? O17 C22 H22A 110.0 . . ? C21 C22 H22A 110.0 . . ? O17 C22 H22B 110.0 . . ? C21 C22 H22B 110.0 . . ? H22A C22 H22B 108.4 . . ? C24 C23 H23A 109.5 . . ? C24 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C24 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O10 C24 C25 124.6(9) . . ? O10 C24 C23 116.2(9) . . ? C25 C24 C23 119.3(8) . . ? C24 C25 C26 124.6(8) . . ? C24 C25 H25 117.7 . . ? C26 C25 H25 117.7 . . ? O9 C26 C25 124.6(9) . . ? O9 C26 C27 114.4(9) . . ? C25 C26 C27 120.9(8) . . ? 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 . . ? C29 C28 H28A 109.5 . . ? C29 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C29 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O8 C29 C30 125.4(9) . . ? O8 C29 C28 115.6(9) . . ? C30 C29 C28 119.0(9) . . ? C31 C30 C29 123.6(10) . . ? C31 C30 H30 118.2 . . ? C29 C30 H30 118.2 . . ? O7 C31 C30 126.1(9) . . ? O7 C31 C32 114.1(9) . . ? C30 C31 C32 119.8(9) . . ? C31 C32 H32A 109.4 . . ? C31 C32 H32B 109.8 . . ? H32A C32 H32B 109.0 . . ? C31 C32 H32C 109.9 . . ? H32A C32 H32C 109.1 . . ? H32B C32 H32C 109.6 . . ? C34 C33 H33A 109.5 . . ? C34 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C34 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O15 C34 C35 125.6(8) . . ? O15 C34 C33 116.2(8) . . ? C35 C34 C33 118.2(8) . . ? C34 C35 C36 124.3(8) . . ? C34 C35 H35 117.9 . . ? C36 C35 H35 117.9 . . ? O16 C36 C35 124.5(9) . . ? O16 C36 C37 114.4(8) . . ? C35 C36 C37 121.1(9) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C39 C38 H38A 109.5 . . ? C39 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C39 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O14 C39 C40 123.7(10) . . ? O14 C39 C38 117.0(10) . . ? C40 C39 C38 119.3(10) . . ? C41 C40 C39 123.9(9) . . ? C41 C40 H40 118.1 . . ? C39 C40 H40 118.1 . . ? O13 C41 C40 125.2(9) . . ? O13 C41 C42 114.9(10) . . ? C40 C41 C42 119.8(9) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.679 _refine_diff_density_min -1.512 _refine_diff_density_rms 0.191 # Attachment '- 4 Fe3Dyfinal.CIF' #========================================================================== data_4 _database_code_depnum_ccdc_archive 'CCDC 784704' #TrackingRef '- 4 Fe3Dyfinal.CIF' #========================================================================== _audit_creation_method SHELXL-97 _audit_creation_date '9 November 2005' _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_exptl_prep ; ; _publ_section_exptl_refinement ; The compound was solved via direct methods. The asymmetric unit contains the entire cluster. All non H-atoms were refined anisotropically. All H-atoms were placed in calculated positions. ; _publ_section_references ;Bruker (1997) SMART (Version 5.054) and SAINT-Plus (Version 6.45). Bruker AXS Inc., Madison, Wisconsin, USA. Bruker (2001) XCIF (Version 6.12). Bruker AXS Inc., Madison, Wisconsin, USA. Bruno, I. J., Cole, J. C., Edgington, P. R., Kessler, M., Macrae, C. F., McCabe, P., Pearson, J. and Taylor, R. (2002) Acta Cryst., B58, 389--397. Farrugia, L. J. (1997) J. Appl. Cryst., 30, 565--565. Sheldrick, G. M. (1990) Acta Cryst., A46, 467--473. Sheldrick, G. M. (1997) SHELXL97., University of Gottingen, Germany. Sheldrick, G. M. (1996) SADABS., University of Gottingen, Germany. ; _publ_section_figure_captions ; ; _publ_section_table_legends ; ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C42 H66 Dy Fe3 N2 O18 ; _chemical_formula_sum 'C42 H66 Dy Fe3 N2 O18' _chemical_formula_weight 1217.02 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' Fe Fe 0.3463 0.8444 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9164(16) _cell_length_b 15.200(2) _cell_length_c 15.894(3) _cell_angle_alpha 80.504(7) _cell_angle_beta 82.114(6) _cell_angle_gamma 82.359(6) _cell_volume 2560.2(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3876 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 21.74 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.579 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 2.345 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.632 _exptl_absorpt_correction_T_max 0.791 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'APEX X8 Apex CCD' _diffrn_measurement_method 'scans in phi and omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 23089 _diffrn_reflns_av_R_equivalents 0.0622 _diffrn_reflns_av_sigmaI/netI 0.1000 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9000 _reflns_number_gt 6019 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex2 V2.0' _computing_cell_refinement 'Bruker Apex2 V2.0' _computing_data_reduction 'Bruker Apex2 V2.0' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-SEED _computing_publication_material 'XCIF V6.12 (BrukerAXS, 2001).' _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 compound was solved via direct methods. The asymmetric unit contains the entire cluster. All non H-atoms were refined anisotropically. All H-atoms were placed in calculated positions. ; _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^)+(0.0665P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8362 _refine_ls_number_parameters 607 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0905 _refine_ls_R_factor_gt 0.0577 _refine_ls_wR_factor_ref 0.1313 _refine_ls_wR_factor_gt 0.1178 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.71559(3) 0.72073(2) 0.69585(2) 0.02116(13) Uani 1 1 d . . . Fe1 Fe 0.78367(9) 0.82183(7) 0.86067(6) 0.0255(3) Uani 1 1 d . . . Fe2 Fe 0.82018(8) 0.80723(7) 0.48803(6) 0.0249(3) Uani 1 1 d . . . Fe3 Fe 0.55276(9) 0.53388(7) 0.73591(7) 0.0278(3) Uani 1 1 d . . . O1 O 0.6871(4) 0.8610(3) 0.9702(3) 0.0320(13) Uani 1 1 d . . . O2 O 0.7463(4) 0.9522(3) 0.8060(3) 0.0322(13) Uani 1 1 d . . . O3 O 0.9389(4) 0.8662(3) 0.8893(3) 0.0314(13) Uani 1 1 d . . . O4 O 0.8312(4) 0.7064(3) 0.9397(3) 0.0289(12) Uani 1 1 d . . . O5 O 0.6423(4) 0.7801(3) 0.8236(3) 0.0241(12) Uani 1 1 d . . . O6 O 0.8676(4) 0.7780(3) 0.7576(3) 0.0250(12) Uani 1 1 d . . . O7 O 0.6620(4) 0.8059(3) 0.4342(3) 0.0297(12) Uani 1 1 d . . . O8 O 0.9109(4) 0.7488(3) 0.3870(3) 0.0286(12) Uani 1 1 d . . . O9 O 0.8268(4) 0.9287(3) 0.4125(3) 0.0303(12) Uani 1 1 d . . . O10 O 0.9917(4) 0.8234(3) 0.5156(3) 0.0279(12) Uani 1 1 d . . . O11 O 0.7265(4) 0.8481(3) 0.5901(3) 0.0252(12) Uani 1 1 d . . . O12 O 0.8167(4) 0.6918(3) 0.5633(3) 0.0220(11) Uani 1 1 d . . . O13 O 0.4145(4) 0.5852(4) 0.8188(3) 0.0381(14) Uani 1 1 d . . . O14 O 0.5537(5) 0.4183(4) 0.8221(4) 0.0443(15) Uani 1 1 d . . . O15 O 0.6773(4) 0.4591(3) 0.6631(3) 0.0294(12) Uani 1 1 d . . . O16 O 0.4198(4) 0.4978(3) 0.6755(3) 0.0335(13) Uani 1 1 d . . . O17 O 0.5533(4) 0.6511(3) 0.6630(3) 0.0237(11) Uani 1 1 d . . . O18 O 0.6908(4) 0.5797(3) 0.7762(3) 0.0259(12) Uani 1 1 d . . . N1 N 0.9342(5) 0.6086(4) 0.7049(4) 0.0244(14) Uani 1 1 d . . . N2 N 0.4970(5) 0.8316(4) 0.6877(4) 0.0242(15) Uani 1 1 d . . . C1 C 0.6376(8) 0.9442(6) 1.0849(5) 0.045(2) Uani 1 1 d . . . H1A H 0.5776 0.9030 1.1079 0.068 Uiso 1 1 calc R . . H1B H 0.6019 1.0041 1.0921 0.068 Uiso 1 1 calc R . . H1C H 0.7099 0.9286 1.1148 0.068 Uiso 1 1 calc R . . C2 C 0.6742(6) 0.9391(6) 0.9906(5) 0.0297(19) Uani 1 1 d . . . C3 C 0.6919(7) 1.0171(6) 0.9327(5) 0.034(2) Uani 1 1 d . . . H3 H 0.6798 1.0711 0.9547 0.041 Uiso 1 1 calc R . . C4 C 0.7260(6) 1.0207(5) 0.8450(5) 0.032(2) Uani 1 1 d . . . C5 C 0.7430(7) 1.1088(6) 0.7897(5) 0.044(2) Uani 1 1 d . . . H5A H 0.8301 1.1128 0.7725 0.066 Uiso 1 1 calc R . . H5B H 0.7088 1.1567 0.8213 0.066 Uiso 1 1 calc R . . H5C H 0.7010 1.1134 0.7396 0.066 Uiso 1 1 calc R . . C6 C 1.1124(8) 0.8863(7) 0.9535(6) 0.067(3) Uani 1 1 d . . . H6A H 1.1737 0.8836 0.9043 0.100 Uiso 1 1 calc R . . H6B H 1.1504 0.8622 1.0047 0.100 Uiso 1 1 calc R . . H6C H 1.0789 0.9477 0.9560 0.100 Uiso 1 1 calc R . . C7 C 1.0078(7) 0.8314(6) 0.9465(5) 0.036(2) Uani 1 1 d . . . C8 C 0.9952(7) 0.7515(6) 0.9990(5) 0.038(2) Uani 1 1 d . . . H8 H 1.0474 0.7356 1.0420 0.046 Uiso 1 1 calc R . . C9 C 0.9100(7) 0.6911(6) 0.9938(5) 0.034(2) Uani 1 1 d . . . C10 C 0.9105(7) 0.6038(5) 1.0517(5) 0.040(2) Uani 1 1 d . . . H10A H 0.8424 0.6072 1.0967 0.061 Uiso 1 1 calc R . . H10B H 0.9875 0.5906 1.0764 0.061 Uiso 1 1 calc R . . H10C H 0.9018 0.5573 1.0195 0.061 Uiso 1 1 calc R . . C11 C 0.9958(6) 0.7471(5) 0.7403(5) 0.0267(18) Uani 1 1 d . . . H11A H 1.0436 0.7705 0.7770 0.032 Uiso 1 1 calc R . . H11B H 1.0256 0.7681 0.6810 0.032 Uiso 1 1 calc R . . C12 C 1.0122(6) 0.6453(5) 0.7570(5) 0.0268(18) Uani 1 1 d . . . H12A H 1.0990 0.6235 0.7427 0.032 Uiso 1 1 calc R . . H12B H 0.9889 0.6248 0.8175 0.032 Uiso 1 1 calc R . . C13 C 0.9023(6) 0.5184(5) 0.7464(5) 0.0288(18) Uani 1 1 d . . . H13A H 0.9729 0.4852 0.7730 0.035 Uiso 1 1 calc R . . H13B H 0.8836 0.4853 0.7034 0.035 Uiso 1 1 calc R . . C14 C 0.7908(6) 0.5269(5) 0.8140(5) 0.0282(18) Uani 1 1 d . . . H14A H 0.7672 0.4679 0.8382 0.034 Uiso 1 1 calc R . . H14B H 0.8119 0.5548 0.8600 0.034 Uiso 1 1 calc R . . C15 C 0.9951(6) 0.6059(5) 0.6166(4) 0.0254(18) Uani 1 1 d . . . H15A H 1.0505 0.5507 0.6145 0.030 Uiso 1 1 calc R . . H15B H 1.0443 0.6559 0.5990 0.030 Uiso 1 1 calc R . . C16 C 0.8975(6) 0.6112(5) 0.5560(4) 0.0244(17) Uani 1 1 d . . . H16A H 0.9369 0.6118 0.4974 0.029 Uiso 1 1 calc R . . H16B H 0.8509 0.5597 0.5713 0.029 Uiso 1 1 calc R . . C17 C 0.5141(6) 0.8113(5) 0.8422(4) 0.0260(18) Uani 1 1 d . . . H17A H 0.5023 0.8419 0.8921 0.031 Uiso 1 1 calc R . . H17B H 0.4653 0.7609 0.8548 0.031 Uiso 1 1 calc R . . C18 C 0.4719(6) 0.8746(5) 0.7661(4) 0.0259(18) Uani 1 1 d . . . H18A H 0.3834 0.8930 0.7771 0.031 Uiso 1 1 calc R . . H18B H 0.5150 0.9278 0.7575 0.031 Uiso 1 1 calc R . . C19 C 0.5101(6) 0.8998(5) 0.6103(5) 0.0269(18) Uani 1 1 d . . . H19A H 0.4509 0.9522 0.6182 0.032 Uiso 1 1 calc R . . H19B H 0.4912 0.8758 0.5613 0.032 Uiso 1 1 calc R . . C20 C 0.6423(6) 0.9278(5) 0.5921(5) 0.0288(18) Uani 1 1 d . . . H20A H 0.6522 0.9669 0.5374 0.035 Uiso 1 1 calc R . . H20B H 0.6582 0.9599 0.6367 0.035 Uiso 1 1 calc R . . C21 C 0.3985(6) 0.7750(5) 0.6839(5) 0.0307(19) Uani 1 1 d . . . H21A H 0.3282 0.8121 0.6602 0.037 Uiso 1 1 calc R . . H21B H 0.3699 0.7474 0.7415 0.037 Uiso 1 1 calc R . . C22 C 0.4474(6) 0.7023(5) 0.6283(5) 0.0285(19) Uani 1 1 d . . . H22A H 0.3834 0.6638 0.6282 0.034 Uiso 1 1 calc R . . H22B H 0.4707 0.7295 0.5696 0.034 Uiso 1 1 calc R . . C23 C 1.1955(6) 0.8637(6) 0.5019(5) 0.035(2) Uani 1 1 d . . . H23A H 1.2026 0.8121 0.5456 0.053 Uiso 1 1 calc R . . H23B H 1.2078 0.9161 0.5248 0.053 Uiso 1 1 calc R . . H23C H 1.2575 0.8552 0.4540 0.053 Uiso 1 1 calc R . . C24 C 1.0685(6) 0.8757(5) 0.4728(5) 0.0273(18) Uani 1 1 d . . . C25 C 1.0432(7) 0.9390(5) 0.4026(5) 0.035(2) Uani 1 1 d . . . H25 H 1.1087 0.9684 0.3720 0.042 Uiso 1 1 calc R . . C26 C 0.9253(7) 0.9619(5) 0.3743(5) 0.0320(19) Uani 1 1 d . . . C27 C 0.9090(7) 1.0284(6) 0.2961(5) 0.048(2) Uani 1 1 d . . . H27A H 0.8808 1.0002 0.2536 0.072 Uiso 1 1 calc R . . H27B H 0.9871 1.0507 0.2737 0.072 Uiso 1 1 calc R . . H27C H 0.8487 1.0773 0.3102 0.072 Uiso 1 1 calc R . . C28 C 0.9743(7) 0.7335(6) 0.2414(5) 0.042(2) Uani 1 1 d . . . H28A H 1.0360 0.7747 0.2317 0.064 Uiso 1 1 calc R . . H28B H 0.9368 0.7360 0.1897 0.064 Uiso 1 1 calc R . . H28C H 1.0129 0.6737 0.2578 0.064 Uiso 1 1 calc R . . C29 C 0.8759(7) 0.7586(5) 0.3121(5) 0.0305(19) Uani 1 1 d . . . C30 C 0.7543(7) 0.7886(5) 0.2941(5) 0.038(2) Uani 1 1 d . . . H30 H 0.7388 0.7961 0.2371 0.045 Uiso 1 1 calc R . . C31 C 0.6538(7) 0.8081(5) 0.3562(5) 0.0318(19) Uani 1 1 d . . . C32 C 0.5251(7) 0.8341(6) 0.3288(5) 0.046(2) Uani 1 1 d . . . H32A H 0.4838 0.7812 0.3337 0.068 Uiso 1 1 calc R . . H32B H 0.5316 0.8633 0.2703 0.068 Uiso 1 1 calc R . . H32C H 0.4780 0.8743 0.3651 0.068 Uiso 1 1 calc R . . C33 C 0.7715(6) 0.3518(6) 0.5770(5) 0.043(2) Uani 1 1 d . . . H33A H 0.8408 0.3865 0.5661 0.064 Uiso 1 1 calc R . . H33B H 0.7562 0.3343 0.5244 0.064 Uiso 1 1 calc R . . H33C H 0.7900 0.2991 0.6177 0.064 Uiso 1 1 calc R . . C34 C 0.6583(6) 0.4069(5) 0.6129(5) 0.0288(19) Uani 1 1 d . . . C35 C 0.5425(6) 0.3995(5) 0.5876(5) 0.033(2) Uani 1 1 d . . . H35 H 0.5399 0.3618 0.5476 0.040 Uiso 1 1 calc R . . C36 C 0.4312(6) 0.4452(5) 0.6190(5) 0.0323(19) Uani 1 1 d . . . C37 C 0.3128(7) 0.4341(6) 0.5862(6) 0.043(2) Uani 1 1 d . . . H37A H 0.2576 0.4067 0.6324 0.064 Uiso 1 1 calc R . . H37B H 0.3309 0.3967 0.5419 0.064 Uiso 1 1 calc R . . H37C H 0.2740 0.4919 0.5632 0.064 Uiso 1 1 calc R . . C38 C 0.5054(9) 0.3049(7) 0.9366(7) 0.078(4) Uani 1 1 d . . . H38A H 0.4721 0.2668 0.9051 0.117 Uiso 1 1 calc R . . H38B H 0.4630 0.3007 0.9940 0.117 Uiso 1 1 calc R . . H38C H 0.5926 0.2863 0.9389 0.117 Uiso 1 1 calc R . . C39 C 0.4877(8) 0.4004(6) 0.8928(6) 0.047(2) Uani 1 1 d . . . C40 C 0.3989(8) 0.4627(7) 0.9290(6) 0.054(3) Uani 1 1 d . . . H40 H 0.3580 0.4439 0.9829 0.065 Uiso 1 1 calc R . . C41 C 0.3667(7) 0.5495(7) 0.8919(6) 0.040(2) Uani 1 1 d . . . C42 C 0.2655(8) 0.6105(7) 0.9350(6) 0.063(3) Uani 1 1 d . . . H42A H 0.2961 0.6664 0.9369 0.094 Uiso 1 1 calc R . . H42B H 0.2409 0.5824 0.9924 0.094 Uiso 1 1 calc R . . H42C H 0.1950 0.6215 0.9031 0.094 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 0.01939(18) 0.0259(2) 0.0178(2) 0.00012(17) -0.00365(13) -0.00398(14) Fe1 0.0257(5) 0.0305(7) 0.0216(6) -0.0026(5) -0.0066(4) -0.0054(5) Fe2 0.0230(5) 0.0304(7) 0.0191(6) 0.0028(5) -0.0015(4) -0.0037(5) Fe3 0.0259(5) 0.0290(7) 0.0274(7) -0.0014(6) 0.0024(4) -0.0079(5) O1 0.036(3) 0.034(3) 0.030(3) -0.010(3) -0.005(2) -0.007(2) O2 0.037(3) 0.035(3) 0.027(3) -0.003(3) -0.013(2) -0.005(2) O3 0.030(3) 0.044(3) 0.024(3) -0.002(3) -0.009(2) -0.013(2) O4 0.033(3) 0.035(3) 0.021(3) 0.001(3) -0.011(2) -0.006(2) O5 0.024(2) 0.027(3) 0.021(3) -0.003(2) -0.005(2) -0.001(2) O6 0.017(2) 0.036(3) 0.022(3) -0.003(3) -0.0008(19) -0.006(2) O7 0.025(3) 0.041(3) 0.019(3) 0.005(3) -0.003(2) -0.003(2) O8 0.028(3) 0.035(3) 0.020(3) 0.004(3) 0.000(2) -0.005(2) O9 0.029(3) 0.032(3) 0.025(3) 0.003(3) 0.001(2) 0.000(2) O10 0.028(3) 0.032(3) 0.025(3) -0.001(3) -0.003(2) -0.009(2) O11 0.024(2) 0.024(3) 0.024(3) 0.002(2) 0.000(2) -0.003(2) O12 0.022(2) 0.018(3) 0.024(3) 0.003(2) -0.003(2) 0.000(2) O13 0.039(3) 0.038(3) 0.034(4) -0.004(3) 0.013(3) -0.010(3) O14 0.045(3) 0.033(3) 0.051(4) 0.011(3) -0.004(3) -0.013(3) O15 0.022(2) 0.031(3) 0.037(3) -0.009(3) -0.004(2) -0.006(2) O16 0.023(3) 0.031(3) 0.047(4) -0.008(3) 0.004(2) -0.009(2) O17 0.020(2) 0.025(3) 0.025(3) -0.001(2) -0.003(2) -0.002(2) O18 0.029(3) 0.026(3) 0.021(3) 0.006(2) -0.003(2) -0.006(2) N1 0.023(3) 0.030(4) 0.021(4) -0.001(3) -0.009(3) -0.001(3) N2 0.020(3) 0.030(4) 0.024(4) -0.007(3) -0.007(2) -0.001(3) C1 0.053(5) 0.055(6) 0.031(5) -0.016(5) -0.005(4) -0.004(4) C2 0.018(4) 0.040(6) 0.034(5) -0.007(5) -0.010(3) -0.004(3) C3 0.039(4) 0.038(6) 0.029(5) -0.012(5) -0.010(4) -0.002(4) C4 0.025(4) 0.035(5) 0.040(6) -0.005(5) -0.014(4) -0.008(4) C5 0.043(5) 0.045(6) 0.045(6) -0.004(5) -0.010(4) -0.003(4) C6 0.059(6) 0.108(9) 0.047(6) -0.005(6) -0.026(5) -0.050(6) C7 0.035(4) 0.050(6) 0.027(5) -0.009(5) -0.002(4) -0.018(4) C8 0.030(4) 0.070(7) 0.020(5) -0.007(5) -0.011(3) -0.010(4) C9 0.030(4) 0.045(6) 0.023(5) -0.002(4) -0.004(3) 0.003(4) C10 0.050(5) 0.039(5) 0.028(5) 0.007(5) -0.010(4) -0.002(4) C11 0.016(3) 0.035(5) 0.029(5) -0.003(4) -0.004(3) -0.002(3) C12 0.020(3) 0.032(5) 0.029(5) 0.002(4) -0.011(3) -0.002(3) C13 0.037(4) 0.029(5) 0.019(4) 0.005(4) -0.010(3) -0.003(4) C14 0.038(4) 0.025(5) 0.019(4) 0.009(4) -0.007(3) -0.007(4) C15 0.023(4) 0.033(5) 0.018(4) -0.002(4) 0.000(3) -0.002(3) C16 0.024(4) 0.026(4) 0.022(4) -0.005(4) -0.002(3) 0.002(3) C17 0.020(3) 0.036(5) 0.023(4) -0.016(4) 0.000(3) 0.005(3) C18 0.020(3) 0.031(5) 0.025(4) 0.000(4) -0.004(3) -0.002(3) C19 0.026(4) 0.029(5) 0.026(5) -0.003(4) -0.011(3) 0.004(3) C20 0.029(4) 0.023(4) 0.031(5) -0.002(4) 0.002(3) -0.001(3) C21 0.026(4) 0.041(5) 0.023(5) 0.002(4) -0.005(3) -0.003(4) C22 0.032(4) 0.029(5) 0.026(5) -0.003(4) -0.010(3) -0.004(3) C23 0.031(4) 0.045(5) 0.033(5) -0.005(4) 0.000(3) -0.019(4) C24 0.034(4) 0.026(5) 0.024(5) -0.009(4) 0.003(3) -0.010(4) C25 0.032(4) 0.037(5) 0.036(5) -0.006(5) 0.008(4) -0.012(4) C26 0.046(5) 0.028(5) 0.014(4) 0.009(4) 0.005(4) -0.001(4) C27 0.044(5) 0.047(6) 0.044(6) 0.004(5) 0.008(4) 0.001(4) C28 0.055(5) 0.046(6) 0.024(5) -0.003(5) 0.006(4) -0.010(4) C29 0.040(4) 0.021(4) 0.029(5) 0.001(4) 0.003(4) -0.010(3) C30 0.039(5) 0.052(6) 0.020(5) 0.003(4) -0.012(4) -0.003(4) C31 0.038(4) 0.036(5) 0.021(5) 0.007(4) -0.012(4) -0.009(4) C32 0.036(4) 0.062(6) 0.037(5) 0.006(5) -0.014(4) -0.008(4) C33 0.028(4) 0.052(6) 0.053(6) -0.023(5) -0.002(4) -0.003(4) C34 0.027(4) 0.028(5) 0.031(5) 0.001(4) -0.006(3) -0.007(3) C35 0.037(4) 0.035(5) 0.029(5) -0.013(4) -0.006(3) 0.002(4) C36 0.032(4) 0.031(5) 0.035(5) -0.001(4) -0.006(3) -0.013(4) C37 0.032(4) 0.041(5) 0.058(6) -0.007(5) -0.012(4) -0.007(4) C38 0.057(6) 0.089(9) 0.070(8) 0.057(7) -0.009(5) -0.028(6) C39 0.035(5) 0.057(7) 0.047(6) 0.021(6) -0.008(4) -0.027(5) C40 0.053(6) 0.083(8) 0.022(5) 0.014(6) 0.005(4) -0.031(6) C41 0.038(5) 0.058(7) 0.027(5) -0.003(5) 0.003(4) -0.028(4) C42 0.049(5) 0.089(8) 0.052(6) -0.025(6) 0.021(5) -0.020(5) _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 O12 2.322(4) . ? Dy1 O18 2.336(5) . ? Dy1 O17 2.338(4) . ? Dy1 O11 2.349(5) . ? Dy1 O5 2.355(4) . ? Dy1 O6 2.363(4) . ? Dy1 N2 2.738(5) . ? Dy1 N1 2.748(5) . ? Fe1 O6 1.938(4) . ? Fe1 O5 1.941(4) . ? Fe1 O4 2.034(5) . ? Fe1 O3 2.037(5) . ? Fe1 O2 2.040(5) . ? Fe1 O1 2.041(5) . ? Fe2 O11 1.942(4) . ? Fe2 O12 1.956(5) . ? Fe2 O7 2.033(4) . ? Fe2 O9 2.034(5) . ? Fe2 O10 2.035(4) . ? Fe2 O8 2.038(5) . ? Fe3 O17 1.958(5) . ? Fe3 O18 1.963(4) . ? Fe3 O15 2.018(4) . ? Fe3 O16 2.025(5) . ? Fe3 O13 2.025(5) . ? Fe3 O14 2.042(6) . ? O1 C2 1.267(8) . ? O2 C4 1.278(8) . ? O3 C7 1.263(9) . ? O4 C9 1.271(8) . ? O5 C17 1.423(7) . ? O6 C11 1.420(7) . ? O7 C31 1.250(8) . ? O8 C29 1.278(8) . ? O9 C26 1.281(9) . ? O10 C24 1.280(9) . ? O11 C20 1.422(8) . ? O12 C16 1.422(7) . ? O13 C41 1.271(10) . ? O14 C39 1.260(10) . ? O15 C34 1.268(8) . ? O16 C36 1.281(8) . ? O17 C22 1.430(8) . ? O18 C14 1.409(8) . ? N1 C15 1.472(8) . ? N1 C12 1.481(8) . ? N1 C13 1.484(9) . ? N2 C19 1.476(9) . ? N2 C18 1.477(8) . ? N2 C21 1.477(9) . ? C1 C2 1.509(10) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.393(11) . ? C3 C4 1.387(11) . ? C3 H3 0.9300 . ? C4 C5 1.494(11) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.527(11) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C8 1.368(12) . ? C8 C9 1.410(11) . ? C8 H8 0.9300 . ? C9 C10 1.486(11) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.517(10) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.516(10) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.518(8) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.500(10) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.534(10) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.524(9) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.500(9) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 C25 1.381(11) . ? C25 C26 1.403(10) . ? C25 H25 0.9300 . ? C26 C27 1.483(11) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 C29 1.505(10) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C30 1.397(10) . ? C30 C31 1.408(10) . ? C30 H30 0.9300 . ? C31 C32 1.512(9) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 C34 1.498(9) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 C35 1.401(9) . ? C35 C36 1.389(9) . ? C35 H35 0.9300 . ? C36 C37 1.498(9) . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 C39 1.502(13) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 C40 1.397(12) . ? C40 C41 1.374(12) . ? C40 H40 0.9300 . ? C41 C42 1.510(11) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O12 Dy1 O18 105.17(16) . . ? O12 Dy1 O17 85.80(15) . . ? O18 Dy1 O17 65.11(16) . . ? O12 Dy1 O11 65.55(15) . . ? O18 Dy1 O11 166.97(15) . . ? O17 Dy1 O11 104.02(16) . . ? O12 Dy1 O5 165.91(16) . . ? O18 Dy1 O5 86.59(16) . . ? O17 Dy1 O5 106.51(15) . . ? O11 Dy1 O5 104.00(16) . . ? O12 Dy1 O6 103.64(15) . . ? O18 Dy1 O6 105.51(16) . . ? O17 Dy1 O6 168.50(16) . . ? O11 Dy1 O6 86.08(16) . . ? O5 Dy1 O6 65.05(15) . . ? O12 Dy1 N2 114.36(16) . . ? O18 Dy1 N2 113.27(17) . . ? O17 Dy1 N2 66.75(15) . . ? O11 Dy1 N2 65.67(17) . . ? O5 Dy1 N2 66.25(15) . . ? O6 Dy1 N2 113.88(15) . . ? O12 Dy1 N1 65.91(15) . . ? O18 Dy1 N1 66.34(17) . . ? O17 Dy1 N1 113.05(15) . . ? O11 Dy1 N1 114.72(17) . . ? O5 Dy1 N1 113.57(15) . . ? O6 Dy1 N1 66.24(15) . . ? N2 Dy1 N1 179.61(19) . . ? O6 Fe1 O5 81.69(18) . . ? O6 Fe1 O4 94.3(2) . . ? O5 Fe1 O4 95.49(19) . . ? O6 Fe1 O3 93.90(19) . . ? O5 Fe1 O3 175.3(2) . . ? O4 Fe1 O3 86.6(2) . . ? O6 Fe1 O2 96.6(2) . . ? O5 Fe1 O2 95.41(19) . . ? O4 Fe1 O2 165.60(18) . . ? O3 Fe1 O2 83.3(2) . . ? O6 Fe1 O1 175.9(2) . . ? O5 Fe1 O1 94.84(19) . . ? O4 Fe1 O1 83.9(2) . . ? O3 Fe1 O1 89.63(19) . . ? O2 Fe1 O1 85.9(2) . . ? O11 Fe2 O12 80.90(19) . . ? O11 Fe2 O7 91.90(18) . . ? O12 Fe2 O7 98.0(2) . . ? O11 Fe2 O9 98.2(2) . . ? O12 Fe2 O9 178.14(19) . . ? O7 Fe2 O9 83.7(2) . . ? O11 Fe2 O10 96.76(18) . . ? O12 Fe2 O10 92.74(19) . . ? O7 Fe2 O10 167.2(2) . . ? O9 Fe2 O10 85.7(2) . . ? O11 Fe2 O8 172.7(2) . . ? O12 Fe2 O8 92.37(19) . . ? O7 Fe2 O8 86.14(18) . . ? O9 Fe2 O8 88.62(19) . . ? O10 Fe2 O8 86.40(18) . . ? O17 Fe3 O18 79.79(19) . . ? O17 Fe3 O15 100.1(2) . . ? O18 Fe3 O15 89.40(18) . . ? O17 Fe3 O16 92.4(2) . . ? O18 Fe3 O16 170.7(2) . . ? O15 Fe3 O16 86.93(18) . . ? O17 Fe3 O13 90.3(2) . . ? O18 Fe3 O13 97.21(19) . . ? O15 Fe3 O13 168.5(2) . . ? O16 Fe3 O13 87.9(2) . . ? O17 Fe3 O14 174.2(2) . . ? O18 Fe3 O14 96.1(2) . . ? O15 Fe3 O14 83.9(2) . . ? O16 Fe3 O14 92.0(2) . . ? O13 Fe3 O14 86.1(2) . . ? C2 O1 Fe1 126.4(5) . . ? C4 O2 Fe1 126.4(5) . . ? C7 O3 Fe1 128.5(5) . . ? C9 O4 Fe1 129.0(5) . . ? C17 O5 Fe1 127.4(4) . . ? C17 O5 Dy1 120.7(3) . . ? Fe1 O5 Dy1 106.74(19) . . ? C11 O6 Fe1 127.4(4) . . ? C11 O6 Dy1 120.7(4) . . ? Fe1 O6 Dy1 106.52(18) . . ? C31 O7 Fe2 126.4(5) . . ? C29 O8 Fe2 125.8(4) . . ? C26 O9 Fe2 126.2(5) . . ? C24 O10 Fe2 127.9(5) . . ? C20 O11 Fe2 125.9(4) . . ? C20 O11 Dy1 123.7(4) . . ? Fe2 O11 Dy1 106.4(2) . . ? C16 O12 Fe2 128.1(4) . . ? C16 O12 Dy1 120.7(4) . . ? Fe2 O12 Dy1 107.03(18) . . ? C41 O13 Fe3 129.7(5) . . ? C39 O14 Fe3 130.1(6) . . ? C34 O15 Fe3 129.2(4) . . ? C36 O16 Fe3 129.1(4) . . ? C22 O17 Fe3 125.3(4) . . ? C22 O17 Dy1 121.3(4) . . ? Fe3 O17 Dy1 107.60(19) . . ? C14 O18 Fe3 125.8(4) . . ? C14 O18 Dy1 121.0(4) . . ? Fe3 O18 Dy1 107.5(2) . . ? C15 N1 C12 111.5(5) . . ? C15 N1 C13 110.9(5) . . ? C12 N1 C13 110.9(5) . . ? C15 N1 Dy1 107.8(4) . . ? C12 N1 Dy1 107.9(4) . . ? C13 N1 Dy1 107.7(4) . . ? C19 N2 C18 110.7(5) . . ? C19 N2 C21 111.3(5) . . ? C18 N2 C21 110.6(5) . . ? C19 N2 Dy1 108.8(4) . . ? C18 N2 Dy1 108.1(4) . . ? C21 N2 Dy1 107.2(4) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 124.5(7) . . ? O1 C2 C1 115.4(8) . . ? C3 C2 C1 120.1(7) . . ? C4 C3 C2 125.3(7) . . ? C4 C3 H3 117.4 . . ? C2 C3 H3 117.4 . . ? O2 C4 C3 124.3(8) . . ? O2 C4 C5 115.5(7) . . ? C3 C4 C5 120.2(7) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O3 C7 C8 125.4(7) . . ? O3 C7 C6 114.3(8) . . ? C8 C7 C6 120.4(8) . . ? C7 C8 C9 125.7(7) . . ? C7 C8 H8 117.1 . . ? C9 C8 H8 117.1 . . ? O4 C9 C8 123.2(8) . . ? O4 C9 C10 116.3(7) . . ? C8 C9 C10 120.4(7) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O6 C11 C12 108.9(6) . . ? O6 C11 H11A 109.9 . . ? C12 C11 H11A 109.9 . . ? O6 C11 H11B 109.9 . . ? C12 C11 H11B 109.9 . . ? H11A C11 H11B 108.3 . . ? N1 C12 C11 110.6(5) . . ? N1 C12 H12A 109.5 . . ? C11 C12 H12A 109.5 . . ? N1 C12 H12B 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 108.1 . . ? N1 C13 C14 110.3(6) . . ? N1 C13 H13A 109.6 . . ? C14 C13 H13A 109.6 . . ? N1 C13 H13B 109.6 . . ? C14 C13 H13B 109.6 . . ? H13A C13 H13B 108.1 . . ? O18 C14 C13 109.4(6) . . ? O18 C14 H14A 109.8 . . ? C13 C14 H14A 109.8 . . ? O18 C14 H14B 109.8 . . ? C13 C14 H14B 109.8 . . ? H14A C14 H14B 108.2 . . ? N1 C15 C16 109.9(5) . . ? N1 C15 H15A 109.7 . . ? C16 C15 H15A 109.7 . . ? N1 C15 H15B 109.7 . . ? C16 C15 H15B 109.7 . . ? H15A C15 H15B 108.2 . . ? O12 C16 C15 107.5(5) . . ? O12 C16 H16A 110.2 . . ? C15 C16 H16A 110.2 . . ? O12 C16 H16B 110.2 . . ? C15 C16 H16B 110.2 . . ? H16A C16 H16B 108.5 . . ? O5 C17 C18 109.2(6) . . ? O5 C17 H17A 109.8 . . ? C18 C17 H17A 109.8 . . ? O5 C17 H17B 109.8 . . ? C18 C17 H17B 109.8 . . ? H17A C17 H17B 108.3 . . ? N2 C18 C17 111.0(5) . . ? N2 C18 H18A 109.4 . . ? C17 C18 H18A 109.4 . . ? N2 C18 H18B 109.4 . . ? C17 C18 H18B 109.4 . . ? H18A C18 H18B 108.0 . . ? N2 C19 C20 111.4(5) . . ? N2 C19 H19A 109.4 . . ? C20 C19 H19A 109.4 . . ? N2 C19 H19B 109.4 . . ? C20 C19 H19B 109.4 . . ? H19A C19 H19B 108.0 . . ? O11 C20 C19 107.4(6) . . ? O11 C20 H20A 110.2 . . ? C19 C20 H20A 110.2 . . ? O11 C20 H20B 110.2 . . ? C19 C20 H20B 110.2 . . ? H20A C20 H20B 108.5 . . ? N2 C21 C22 110.5(5) . . ? N2 C21 H21A 109.5 . . ? C22 C21 H21A 109.5 . . ? N2 C21 H21B 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 108.1 . . ? O17 C22 C21 108.1(5) . . ? O17 C22 H22A 110.1 . . ? C21 C22 H22A 110.1 . . ? O17 C22 H22B 110.1 . . ? C21 C22 H22B 110.1 . . ? H22A C22 H22B 108.4 . . ? C24 C23 H23A 109.5 . . ? C24 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C24 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O10 C24 C25 124.9(7) . . ? O10 C24 C23 115.8(7) . . ? C25 C24 C23 119.3(7) . . ? C24 C25 C26 124.3(7) . . ? C24 C25 H25 117.8 . . ? C26 C25 H25 117.8 . . ? O9 C26 C25 124.0(7) . . ? O9 C26 C27 116.0(7) . . ? C25 C26 C27 120.0(7) . . ? 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 . . ? C29 C28 H28A 109.5 . . ? C29 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C29 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O8 C29 C30 124.2(7) . . ? O8 C29 C28 115.9(6) . . ? C30 C29 C28 119.9(7) . . ? C29 C30 C31 124.4(7) . . ? C29 C30 H30 117.8 . . ? C31 C30 H30 117.8 . . ? O7 C31 C30 124.9(6) . . ? O7 C31 C32 116.0(7) . . ? C30 C31 C32 119.1(7) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 H33A 109.5 . . ? C34 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C34 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O15 C34 C35 125.3(6) . . ? O15 C34 C33 115.6(6) . . ? C35 C34 C33 119.1(6) . . ? C36 C35 C34 123.9(7) . . ? C36 C35 H35 118.1 . . ? C34 C35 H35 118.1 . . ? O16 C36 C35 125.2(6) . . ? O16 C36 C37 115.3(6) . . ? C35 C36 C37 119.6(7) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C39 C38 H38A 109.5 . . ? C39 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C39 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O14 C39 C40 123.7(8) . . ? O14 C39 C38 116.0(9) . . ? C40 C39 C38 120.3(9) . . ? C41 C40 C39 125.7(8) . . ? C41 C40 H40 117.1 . . ? C39 C40 H40 117.1 . . ? O13 C41 C40 124.6(8) . . ? O13 C41 C42 113.8(8) . . ? C40 C41 C42 121.6(8) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 1.514 _refine_diff_density_min -1.738 _refine_diff_density_rms 0.170