# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Cameron Jones' 'Andreas Stasch' 'William D. Woodul' _publ_contact_author_name 'Cameron Jones' _publ_contact_author_email CAMERON.JONES@SCI.MONASH.EDU.AU _publ_section_title ; Gallyl Lanthanide Complexes Containing Unsupported Ln-Ga (Ln = Sm, Eu, Yb or Tm) Bonds ; # Attachment 'Ce_DAB__tmeda_I.CIF' data_[{Ce[(ArNCH)2](tmeda)(m-I)}2] _database_code_depnum_ccdc_archive 'CCDC 705275' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C82 H146 Ce2 I2 N8' _chemical_formula_weight 1778.11 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 37.609(8) _cell_length_b 8.9281(18) _cell_length_c 27.205(5) _cell_angle_alpha 90.00 _cell_angle_beta 110.41(3) _cell_angle_gamma 90.00 _cell_volume 8561(3) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.380 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3664 _exptl_absorpt_coefficient_mu 1.815 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.710 _exptl_absorpt_correction_T_max 0.930 _exptl_absorpt_process_details 'Sortav(Blessing, 1995)' _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 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17019 _diffrn_reflns_av_R_equivalents 0.0327 _diffrn_reflns_av_sigmaI/netI 0.0472 _diffrn_reflns_limit_h_min -47 _diffrn_reflns_limit_h_max 48 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 27.00 _reflns_number_total 9280 _reflns_number_gt 7146 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Amolecule of hexane was located in the asymmetric unit and found to be disordered over two sites. This disorder was successfully modelled. Another half molecule, sitting on a 2-fold rotation axis was located and refined. The largest residual electron density peak in the final difference map (1.599 e/A3) sits close to Ce(1). ; _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^)+(0.0473P)^2^+15.9824P] 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 9280 _refine_ls_number_parameters 421 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0597 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.0952 _refine_ls_wR_factor_gt 0.0847 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.329 _refine_ls_shift/su_max 0.066 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ce1 Ce 0.075346(6) 0.07875(3) 0.047602(8) 0.02132(5) Uani 1 1 d . . . I1 I 0.005994(7) -0.14552(3) 0.058225(9) 0.02749(7) Uani 1 1 d . . . N1 N 0.11310(9) 0.0599(4) 0.13356(11) 0.0234(8) Uani 1 1 d . . . C1 C 0.11762(10) -0.0944(5) 0.12685(14) 0.0250(9) Uani 1 1 d . . . H1 H 0.1180 -0.1593 0.1547 0.030 Uiso 1 1 calc R . . N2 N 0.12195(8) -0.0809(4) 0.03902(12) 0.0226(7) Uani 1 1 d . . . C2 C 0.12154(10) -0.1576(5) 0.08351(14) 0.0251(9) Uani 1 1 d . . . H2 H 0.1242 -0.2634 0.0835 0.030 Uiso 1 1 calc R . . N3 N 0.06661(9) 0.3683(4) 0.07194(12) 0.0285(8) Uani 1 1 d . . . C3 C 0.12713(11) 0.1068(5) 0.18737(14) 0.0268(10) Uani 1 1 d . . . N4 N 0.11401(10) 0.2848(4) 0.00643(14) 0.0401(9) Uani 1 1 d . . . C4 C 0.10318(12) 0.1236(5) 0.21650(15) 0.0338(11) Uani 1 1 d . . . C5 C 0.11848(13) 0.1712(6) 0.26824(16) 0.0407(13) Uani 1 1 d . . . H5 H 0.1023 0.1807 0.2883 0.049 Uiso 1 1 calc R . . C6 C 0.15631(13) 0.2050(6) 0.29122(16) 0.0416(12) Uani 1 1 d . . . H6 H 0.1661 0.2392 0.3265 0.050 Uiso 1 1 calc R . . C7 C 0.17989(13) 0.1888(5) 0.26277(16) 0.0365(11) Uani 1 1 d . . . H7 H 0.2061 0.2111 0.2788 0.044 Uiso 1 1 calc R . . C8 C 0.16604(11) 0.1404(5) 0.21079(15) 0.0277(9) Uani 1 1 d . . . C9 C 0.06146(12) 0.0838(6) 0.19376(17) 0.0440(13) Uani 1 1 d . . . H9 H 0.0541 0.0819 0.1547 0.053 Uiso 1 1 calc R . . C10 C 0.03600(13) 0.1993(8) 0.20729(18) 0.0579(17) Uani 1 1 d . . . H10A H 0.0394 0.1917 0.2446 0.087 Uiso 1 1 calc R . . H10B H 0.0094 0.1797 0.1862 0.087 Uiso 1 1 calc R . . H10C H 0.0429 0.3003 0.1997 0.087 Uiso 1 1 calc R . . C11 C 0.05423(14) -0.0717(7) 0.21119(19) 0.0571(16) Uani 1 1 d . . . H11A H 0.0702 -0.1448 0.2018 0.086 Uiso 1 1 calc R . . H11B H 0.0275 -0.0982 0.1937 0.086 Uiso 1 1 calc R . . H11C H 0.0603 -0.0724 0.2493 0.086 Uiso 1 1 calc R . . C12 C 0.19373(11) 0.1212(5) 0.18153(16) 0.0325(11) Uani 1 1 d . . . H12 H 0.1791 0.0834 0.1455 0.039 Uiso 1 1 calc R . . C13 C 0.21155(14) 0.2703(6) 0.1760(2) 0.0543(15) Uani 1 1 d . . . H13A H 0.1915 0.3444 0.1606 0.081 Uiso 1 1 calc R . . H13B H 0.2265 0.2577 0.1531 0.081 Uiso 1 1 calc R . . H13C H 0.2281 0.3049 0.2106 0.081 Uiso 1 1 calc R . . C14 C 0.22367(14) 0.0061(7) 0.20845(19) 0.0531(15) Uani 1 1 d . . . H14A H 0.2390 0.0424 0.2434 0.080 Uiso 1 1 calc R . . H14B H 0.2400 -0.0104 0.1877 0.080 Uiso 1 1 calc R . . H14C H 0.2114 -0.0882 0.2117 0.080 Uiso 1 1 calc R . . C15 C 0.13885(10) -0.1586(4) 0.00727(15) 0.0255(9) Uani 1 1 d . . . C16 C 0.11902(11) -0.1709(5) -0.04719(15) 0.0266(9) Uani 1 1 d . . . C17 C 0.13403(11) -0.2573(5) -0.07789(16) 0.0323(10) Uani 1 1 d . . . H17 H 0.1204 -0.2659 -0.1144 0.039 Uiso 1 1 calc R . . C18 C 0.16822(12) -0.3306(5) -0.05648(16) 0.0351(11) Uani 1 1 d . . . H18 H 0.1774 -0.3933 -0.0776 0.042 Uiso 1 1 calc R . . C19 C 0.18888(11) -0.3116(5) -0.00388(16) 0.0329(10) Uani 1 1 d . . . H19 H 0.2130 -0.3586 0.0105 0.039 Uiso 1 1 calc R . . C20 C 0.17550(11) -0.2255(5) 0.02867(15) 0.0283(10) Uani 1 1 d . . . C21 C 0.07993(11) -0.1038(5) -0.07199(15) 0.0284(10) Uani 1 1 d . . . H21 H 0.0786 -0.0141 -0.0507 0.034 Uiso 1 1 calc R . . C22 C 0.04998(12) -0.2125(6) -0.06893(17) 0.0372(11) Uani 1 1 d . . . H22A H 0.0512 -0.3042 -0.0881 0.056 Uiso 1 1 calc R . . H22B H 0.0248 -0.1668 -0.0846 0.056 Uiso 1 1 calc R . . H22C H 0.0545 -0.2370 -0.0321 0.056 Uiso 1 1 calc R . . C23 C 0.07070(13) -0.0504(6) -0.12890(15) 0.0375(12) Uani 1 1 d . . . H23A H 0.0922 0.0064 -0.1316 0.056 Uiso 1 1 calc R . . H23B H 0.0482 0.0138 -0.1390 0.056 Uiso 1 1 calc R . . H23C H 0.0658 -0.1373 -0.1523 0.056 Uiso 1 1 calc R . . C24 C 0.20162(11) -0.1998(5) 0.08479(15) 0.0307(10) Uani 1 1 d . . . H24 H 0.1892 -0.1256 0.1011 0.037 Uiso 1 1 calc R . . C25 C 0.20813(13) -0.3435(5) 0.11706(18) 0.0417(12) Uani 1 1 d . . . H25A H 0.1838 -0.3804 0.1180 0.063 Uiso 1 1 calc R . . H25B H 0.2253 -0.3230 0.1529 0.063 Uiso 1 1 calc R . . H25C H 0.2195 -0.4194 0.1011 0.063 Uiso 1 1 calc R . . C26 C 0.23947(12) -0.1332(6) 0.08611(19) 0.0453(13) Uani 1 1 d . . . H26A H 0.2517 -0.2020 0.0689 0.068 Uiso 1 1 calc R . . H26B H 0.2560 -0.1182 0.1226 0.068 Uiso 1 1 calc R . . H26C H 0.2349 -0.0368 0.0677 0.068 Uiso 1 1 calc R . . C27 C 0.07176(11) 0.4620(5) 0.02977(16) 0.0316(10) Uani 1 1 d . . . H27A H 0.0691 0.5689 0.0374 0.038 Uiso 1 1 calc R . . H27B H 0.0517 0.4374 -0.0040 0.038 Uiso 1 1 calc R . . C28 C 0.11024(12) 0.4372(5) 0.02497(17) 0.0334(11) Uani 1 1 d . . . H28A H 0.1140 0.5113 0.0001 0.040 Uiso 1 1 calc R . . H28B H 0.1303 0.4536 0.0596 0.040 Uiso 1 1 calc R . . C29 C 0.09267(13) 0.4199(5) 0.12373(17) 0.0384(12) Uani 1 1 d . . . H29A H 0.0897 0.5281 0.1270 0.058 Uiso 1 1 calc R . . H29B H 0.1189 0.3979 0.1269 0.058 Uiso 1 1 calc R . . H29C H 0.0867 0.3680 0.1516 0.058 Uiso 1 1 calc R . . C30 C 0.02775(11) 0.3906(6) 0.07143(17) 0.0371(12) Uani 1 1 d . . . H30A H 0.0238 0.4968 0.0771 0.056 Uiso 1 1 calc R . . H30B H 0.0239 0.3309 0.0994 0.056 Uiso 1 1 calc R . . H30C H 0.0096 0.3590 0.0374 0.056 Uiso 1 1 calc R . . C31 C 0.09909(18) 0.2880(7) -0.05132(19) 0.0861(19) Uani 1 1 d . . . H31A H 0.0721 0.3137 -0.0636 0.129 Uiso 1 1 calc R . . H31B H 0.1024 0.1892 -0.0649 0.129 Uiso 1 1 calc R . . H31C H 0.1129 0.3631 -0.0638 0.129 Uiso 1 1 calc R . . C32 C 0.15479(14) 0.2463(6) 0.0251(3) 0.0749(18) Uani 1 1 d . . . H32A H 0.1687 0.3234 0.0136 0.112 Uiso 1 1 calc R . . H32B H 0.1582 0.1492 0.0106 0.112 Uiso 1 1 calc R . . H32C H 0.1645 0.2409 0.0635 0.112 Uiso 1 1 calc R . . C33 C -0.0006(4) -0.4168(15) 0.2734(4) 0.189(6) Uiso 1 1 d D . . H33A H -0.0154 -0.5048 0.2773 0.226 Uiso 1 1 calc R . . H33B H -0.0142 -0.3259 0.2779 0.226 Uiso 1 1 calc R . . C34 C 0.0377(3) -0.421(2) 0.3164(6) 0.240(8) Uiso 1 1 d D . . H34A H 0.0388 -0.3281 0.3368 0.289 Uiso 1 1 calc R . . H34B H 0.0361 -0.5043 0.3395 0.289 Uiso 1 1 calc R . . C35 C 0.0757(3) -0.4344(14) 0.3128(4) 0.171(5) Uiso 1 1 d D . . H35A H 0.0735 -0.4730 0.2781 0.256 Uiso 1 1 calc R . . H35B H 0.0911 -0.5034 0.3399 0.256 Uiso 1 1 calc R . . H35C H 0.0879 -0.3357 0.3180 0.256 Uiso 1 1 calc R . . C36 C 0.2100(5) 0.0598(17) -0.0584(7) 0.082(5) Uiso 0.444(7) 1 d PD A 1 H36A H 0.1939 0.0047 -0.0893 0.123 Uiso 0.444(7) 1 calc PR A 1 H36B H 0.1987 0.0562 -0.0310 0.123 Uiso 0.444(7) 1 calc PR A 1 H36C H 0.2353 0.0140 -0.0453 0.123 Uiso 0.444(7) 1 calc PR A 1 C38 C 0.1923(6) 0.197(2) -0.1286(6) 0.110(7) Uiso 0.444(7) 1 d PD A 1 H38A H 0.1689 0.1439 -0.1294 0.132 Uiso 0.444(7) 1 calc PR A 1 H38B H 0.2074 0.1235 -0.1401 0.132 Uiso 0.444(7) 1 calc PR A 1 C41 C 0.1657(4) 0.3905(14) -0.2646(5) 0.050(3) Uiso 0.444(7) 1 d PD A 1 H41A H 0.1438 0.4537 -0.2675 0.076 Uiso 0.444(7) 1 calc PR A 1 H41B H 0.1627 0.3479 -0.2990 0.076 Uiso 0.444(7) 1 calc PR A 1 H41C H 0.1889 0.4510 -0.2523 0.076 Uiso 0.444(7) 1 calc PR A 1 C40 C 0.1685(4) 0.2671(16) -0.2266(5) 0.072(4) Uiso 0.444(7) 1 d PD A 1 H40A H 0.1435 0.2165 -0.2369 0.086 Uiso 0.444(7) 1 calc PR A 1 H40B H 0.1871 0.1928 -0.2298 0.086 Uiso 0.444(7) 1 calc PR A 1 C40A C 0.1696(4) 0.3774(16) -0.2020(5) 0.100(5) Uiso 0.556(7) 1 d PD A 2 H40C H 0.1971 0.4002 -0.1894 0.120 Uiso 0.556(7) 1 calc PR A 2 H40D H 0.1574 0.4454 -0.1839 0.120 Uiso 0.556(7) 1 calc PR A 2 C38A C 0.1700(4) 0.182(2) -0.1317(5) 0.128(7) Uiso 0.556(7) 1 d PD A 2 H38C H 0.1654 0.2743 -0.1145 0.154 Uiso 0.556(7) 1 calc PR A 2 H38D H 0.1510 0.1068 -0.1304 0.154 Uiso 0.556(7) 1 calc PR A 2 C39 C 0.1795(5) 0.311(2) -0.1713(5) 0.097(6) Uiso 0.444(7) 1 d PD A 1 H39A H 0.1577 0.3646 -0.1672 0.116 Uiso 0.444(7) 1 calc PR A 1 H39B H 0.2003 0.3854 -0.1645 0.116 Uiso 0.444(7) 1 calc PR A 1 C37A C 0.2062(4) 0.128(2) -0.1032(5) 0.121(6) Uiso 0.556(7) 1 d PD A 2 H37A H 0.2243 0.2004 -0.1091 0.145 Uiso 0.556(7) 1 calc PR A 2 H37B H 0.2091 0.0337 -0.1204 0.145 Uiso 0.556(7) 1 calc PR A 2 C37 C 0.2135(8) 0.224(2) -0.0735(8) 0.188(12) Uiso 0.444(7) 1 d PD A 1 H37C H 0.2008 0.2956 -0.0572 0.225 Uiso 0.444(7) 1 calc PR A 1 H37D H 0.2400 0.2557 -0.0669 0.225 Uiso 0.444(7) 1 calc PR A 1 C36A C 0.2211(4) 0.0953(14) -0.0430(4) 0.064(3) Uiso 0.556(7) 1 d PD A 2 H36D H 0.2084 0.1619 -0.0257 0.096 Uiso 0.556(7) 1 calc PR A 2 H36E H 0.2485 0.1126 -0.0286 0.096 Uiso 0.556(7) 1 calc PR A 2 H36F H 0.2157 -0.0091 -0.0371 0.096 Uiso 0.556(7) 1 calc PR A 2 C39A C 0.1637(5) 0.2176(17) -0.1891(6) 0.117(6) Uiso 0.556(7) 1 d PD A 2 H39C H 0.1810 0.1536 -0.2003 0.141 Uiso 0.556(7) 1 calc PR A 2 H39D H 0.1375 0.1884 -0.2104 0.141 Uiso 0.556(7) 1 calc PR A 2 C41A C 0.1527(4) 0.4032(16) -0.2608(5) 0.076(4) Uiso 0.556(7) 1 d PD A 2 H41D H 0.1646 0.3349 -0.2787 0.115 Uiso 0.556(7) 1 calc PR A 2 H41E H 0.1573 0.5070 -0.2687 0.115 Uiso 0.556(7) 1 calc PR A 2 H41F H 0.1253 0.3843 -0.2730 0.115 Uiso 0.556(7) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ce1 0.01905(10) 0.02374(12) 0.01947(9) -0.00030(9) 0.00456(8) 0.00006(9) I1 0.02325(12) 0.03104(15) 0.02500(12) 0.00276(11) 0.00441(10) -0.00177(11) N1 0.0224(16) 0.0258(18) 0.0181(14) 0.0004(13) 0.0021(13) -0.0005(14) C1 0.0223(18) 0.028(2) 0.0241(17) 0.0040(16) 0.0069(15) 0.0001(17) N2 0.0189(15) 0.0257(18) 0.0230(14) 0.0002(13) 0.0069(12) 0.0037(14) C2 0.0199(18) 0.025(2) 0.0278(19) 0.0018(16) 0.0046(15) -0.0017(16) N3 0.0264(17) 0.0275(19) 0.0286(17) 0.0032(14) 0.0059(14) 0.0024(15) C3 0.0258(19) 0.031(2) 0.0204(17) 0.0022(16) 0.0041(15) -0.0007(17) N4 0.050(2) 0.027(2) 0.054(2) -0.0057(17) 0.0321(17) -0.0101(18) C4 0.031(2) 0.049(3) 0.0207(18) -0.0006(18) 0.0078(16) -0.001(2) C5 0.037(2) 0.063(3) 0.0216(19) -0.004(2) 0.0091(18) -0.003(2) C6 0.039(2) 0.061(3) 0.0199(19) -0.007(2) 0.0038(18) -0.005(2) C7 0.031(2) 0.044(3) 0.025(2) -0.0029(19) -0.0025(18) -0.002(2) C8 0.0258(19) 0.027(2) 0.0286(19) 0.0004(17) 0.0068(16) -0.0005(17) C9 0.031(2) 0.076(4) 0.025(2) -0.009(2) 0.0110(18) -0.006(2) C10 0.033(2) 0.108(5) 0.032(2) -0.011(3) 0.011(2) 0.006(3) C11 0.043(3) 0.086(4) 0.045(3) -0.009(3) 0.019(2) -0.023(3) C12 0.024(2) 0.039(3) 0.031(2) -0.0035(19) 0.0058(17) -0.0013(19) C13 0.053(3) 0.061(4) 0.056(3) -0.009(3) 0.029(2) -0.019(3) C14 0.039(3) 0.071(4) 0.040(3) -0.010(3) 0.002(2) 0.014(3) C15 0.0205(18) 0.022(2) 0.034(2) 0.0016(16) 0.0102(16) -0.0042(16) C16 0.0244(18) 0.032(2) 0.0256(18) 0.0018(16) 0.0110(15) 0.0006(17) C17 0.034(2) 0.037(3) 0.0308(19) -0.0016(18) 0.0163(17) 0.0021(19) C18 0.033(2) 0.040(3) 0.036(2) -0.0054(19) 0.0168(18) 0.003(2) C19 0.027(2) 0.032(2) 0.043(2) 0.0007(19) 0.0151(18) 0.0035(18) C20 0.028(2) 0.025(2) 0.033(2) 0.0007(17) 0.0128(17) -0.0008(17) C21 0.031(2) 0.032(2) 0.0199(17) -0.0029(16) 0.0060(16) -0.0024(18) C22 0.030(2) 0.042(3) 0.038(2) 0.002(2) 0.0086(19) 0.000(2) C23 0.038(2) 0.050(3) 0.0217(19) 0.0009(19) 0.0072(18) 0.003(2) C24 0.0239(19) 0.033(2) 0.031(2) 0.0006(18) 0.0050(17) 0.0008(18) C25 0.040(3) 0.040(3) 0.041(2) 0.002(2) 0.008(2) 0.009(2) C26 0.027(2) 0.058(3) 0.048(3) -0.008(2) 0.010(2) -0.004(2) C27 0.031(2) 0.025(2) 0.035(2) 0.0013(18) 0.0059(18) 0.0017(18) C28 0.033(2) 0.029(2) 0.036(2) 0.0000(18) 0.0090(18) -0.0027(19) C29 0.037(2) 0.036(3) 0.036(2) -0.001(2) 0.004(2) 0.000(2) C30 0.023(2) 0.045(3) 0.040(2) -0.007(2) 0.0070(18) -0.0024(19) C31 0.140(4) 0.090(4) 0.054(3) -0.040(3) 0.067(3) -0.078(4) C32 0.064(3) 0.036(3) 0.157(5) 0.009(3) 0.078(3) 0.000(3) _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 Ce1 N1 2.280(3) . ? Ce1 N2 2.333(3) . ? Ce1 C1 2.679(4) . ? Ce1 C2 2.691(4) . ? Ce1 N3 2.717(4) . ? Ce1 N4 2.808(4) . ? Ce1 I1 3.3795(6) . ? Ce1 I1 3.4438(14) 5 ? I1 Ce1 3.4438(14) 5 ? N1 C1 1.408(5) . ? N1 C3 1.434(5) . ? C1 C2 1.361(5) . ? N2 C2 1.396(5) . ? N2 C15 1.419(5) . ? N3 C30 1.470(5) . ? N3 C29 1.482(5) . ? N3 C27 1.486(5) . ? C3 C4 1.400(6) . ? C3 C8 1.410(6) . ? N4 C31 1.473(6) . ? N4 C28 1.476(6) . ? N4 C32 1.478(6) . ? C4 C5 1.389(6) . ? C4 C9 1.514(6) . ? C5 C6 1.373(6) . ? C6 C7 1.373(6) . ? C7 C8 1.394(6) . ? C8 C12 1.525(6) . ? C9 C11 1.523(8) . ? C9 C10 1.537(7) . ? C12 C14 1.511(7) . ? C12 C13 1.522(7) . ? C15 C16 1.412(5) . ? C15 C20 1.427(5) . ? C16 C17 1.393(6) . ? C16 C21 1.511(6) . ? C17 C18 1.378(6) . ? C18 C19 1.380(6) . ? C19 C20 1.392(6) . ? C20 C24 1.517(5) . ? C21 C22 1.511(6) . ? C21 C23 1.540(5) . ? C24 C25 1.525(6) . ? C24 C26 1.532(6) . ? C27 C28 1.514(6) . ? C33 C33 1.29(2) 2 ? C33 C34 1.507(14) . ? C34 C35 1.472(14) . ? C36 C37 1.54(2) . ? C38 C37 1.451(19) . ? C38 C39 1.494(18) . ? C41 C40 1.489(15) . ? C40 C39 1.468(16) . ? C40A C39A 1.504(17) . ? C40A C41A 1.519(14) . ? C38A C37A 1.397(17) . ? C38A C39A 1.529(16) . ? C37A C36A 1.562(15) . ? 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 N1 Ce1 N2 80.60(11) . . ? N1 Ce1 C1 31.71(12) . . ? N2 Ce1 C1 58.14(11) . . ? N1 Ce1 C2 58.50(12) . . ? N2 Ce1 C2 31.23(11) . . ? C1 Ce1 C2 29.36(12) . . ? N1 Ce1 N3 84.56(11) . . ? N2 Ce1 N3 139.88(11) . . ? C1 Ce1 N3 116.18(11) . . ? C2 Ce1 N3 140.83(10) . . ? N1 Ce1 N4 103.50(11) . . ? N2 Ce1 N4 81.30(11) . . ? C1 Ce1 N4 117.02(11) . . ? C2 Ce1 N4 107.45(11) . . ? N3 Ce1 N4 66.26(11) . . ? N1 Ce1 I1 95.27(8) . . ? N2 Ce1 I1 106.00(8) . . ? C1 Ce1 I1 81.29(9) . . ? C2 Ce1 I1 85.65(8) . . ? N3 Ce1 I1 112.36(7) . . ? N4 Ce1 I1 160.82(8) . . ? N1 Ce1 I1 157.56(8) . 5 ? N2 Ce1 I1 120.09(7) . 5 ? C1 Ce1 I1 151.37(8) . 5 ? C2 Ce1 I1 135.40(8) . 5 ? N3 Ce1 I1 83.76(7) . 5 ? N4 Ce1 I1 89.18(8) . 5 ? I1 Ce1 I1 71.759(18) . 5 ? Ce1 I1 Ce1 108.241(18) . 5 ? C1 N1 C3 113.6(3) . . ? C1 N1 Ce1 90.0(2) . . ? C3 N1 Ce1 154.3(3) . . ? C2 C1 N1 124.9(4) . . ? C2 C1 Ce1 75.8(2) . . ? N1 C1 Ce1 58.33(18) . . ? C2 N2 C15 115.5(3) . . ? C2 N2 Ce1 88.7(2) . . ? C15 N2 Ce1 150.6(2) . . ? C1 C2 N2 125.8(4) . . ? C1 C2 Ce1 74.8(2) . . ? N2 C2 Ce1 60.08(19) . . ? C30 N3 C29 107.0(3) . . ? C30 N3 C27 108.3(3) . . ? C29 N3 C27 109.8(3) . . ? C30 N3 Ce1 109.3(3) . . ? C29 N3 Ce1 115.6(3) . . ? C27 N3 Ce1 106.7(2) . . ? C4 C3 C8 119.5(4) . . ? C4 C3 N1 121.9(3) . . ? C8 C3 N1 118.5(4) . . ? C31 N4 C28 107.5(4) . . ? C31 N4 C32 109.6(4) . . ? C28 N4 C32 108.0(4) . . ? C31 N4 Ce1 112.4(3) . . ? C28 N4 Ce1 110.1(3) . . ? C32 N4 Ce1 109.3(3) . . ? C5 C4 C3 119.1(4) . . ? C5 C4 C9 119.3(4) . . ? C3 C4 C9 121.5(4) . . ? C6 C5 C4 121.7(4) . . ? C7 C6 C5 119.4(4) . . ? C6 C7 C8 121.2(4) . . ? C7 C8 C3 119.1(4) . . ? C7 C8 C12 118.9(4) . . ? C3 C8 C12 122.0(4) . . ? C4 C9 C11 111.0(4) . . ? C4 C9 C10 112.8(4) . . ? C11 C9 C10 110.1(4) . . ? C14 C12 C13 111.3(4) . . ? C14 C12 C8 110.6(4) . . ? C13 C12 C8 111.0(4) . . ? C16 C15 N2 119.5(3) . . ? C16 C15 C20 118.5(4) . . ? N2 C15 C20 122.0(3) . . ? C17 C16 C15 119.7(4) . . ? C17 C16 C21 119.1(3) . . ? C15 C16 C21 120.9(4) . . ? C18 C17 C16 121.5(4) . . ? C19 C18 C17 119.0(4) . . ? C18 C19 C20 122.0(4) . . ? C19 C20 C15 118.9(4) . . ? C19 C20 C24 118.2(4) . . ? C15 C20 C24 122.8(4) . . ? C22 C21 C16 110.4(4) . . ? C22 C21 C23 110.1(3) . . ? C16 C21 C23 114.5(4) . . ? C20 C24 C25 111.7(4) . . ? C20 C24 C26 110.6(4) . . ? C25 C24 C26 110.6(4) . . ? N3 C27 C28 111.7(3) . . ? N4 C28 C27 111.9(4) . . ? C33 C33 C34 114.4(16) 2 . ? C35 C34 C33 129.7(13) . . ? C37 C38 C39 126.9(17) . . ? C39 C40 C41 116.1(13) . . ? C39A C40A C41A 110.4(12) . . ? C37A C38A C39A 114.4(14) . . ? C40 C39 C38 120.9(15) . . ? C38A C37A C36A 124.8(14) . . ? C38 C37 C36 92.7(15) . . ? C40A C39A C38A 116.8(14) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.599 _refine_diff_density_min -0.780 _refine_diff_density_rms 0.115 # Attachment 'cmpd5.CIF' data_compound5 _database_code_depnum_ccdc_archive 'CCDC 705276' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H104 Ga2 N8 Sm' _chemical_formula_weight 1275.34 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' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 29.344(6) _cell_length_b 13.855(3) _cell_length_c 21.633(4) _cell_angle_alpha 90.00 _cell_angle_beta 131.48(3) _cell_angle_gamma 90.00 _cell_volume 6589(2) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.286 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2672 _exptl_absorpt_coefficient_mu 1.734 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.540 _exptl_absorpt_correction_T_max 0.791 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1997)' _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 'Bruker X8 CCd' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41996 _diffrn_reflns_av_R_equivalents 0.0226 _diffrn_reflns_av_sigmaI/netI 0.0190 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 30.00 _reflns_number_total 9610 _reflns_number_gt 8436 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The carbon atoms of one isopropyl group of the molecule were found to be disordered over two sites. This disorder was successfully modelled. The largest residual electron density peak in the final difference map (1.782 e/A3) was located close to Sm(1). ; _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^)+(0.0422P)^2^+15.1112P] 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 9610 _refine_ls_number_parameters 382 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0382 _refine_ls_R_factor_gt 0.0312 _refine_ls_wR_factor_ref 0.0854 _refine_ls_wR_factor_gt 0.0802 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.038 _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 Sm1 Sm 0.0000 0.0000 0.0000 0.02206(5) Uani 1 2 d S . . Ga1 Ga 0.111816(9) 0.159860(16) 0.093408(14) 0.02187(6) Uani 1 1 d . . . N1 N 0.14848(8) 0.25395(13) 0.18047(11) 0.0256(3) Uani 1 1 d . . . C1 C 0.18876(12) 0.31387(19) 0.18549(16) 0.0386(6) Uani 1 1 d . . . H1 H 0.2108 0.3633 0.2259 0.046 Uiso 1 1 calc R . . N2 N 0.16114(9) 0.22177(14) 0.07531(12) 0.0278(4) Uani 1 1 d . . . C2 C 0.19473(13) 0.2978(2) 0.12984(17) 0.0413(6) Uani 1 1 d . . . H2 H 0.2205 0.3364 0.1279 0.050 Uiso 1 1 calc R . . N3 N 0.00390(14) -0.0014(2) 0.12825(18) 0.0553(8) Uani 1 1 d . . . C3 C 0.14434(11) 0.26141(18) 0.24224(15) 0.0323(5) Uani 1 1 d . . . N4 N 0.07439(12) -0.1462(2) 0.10754(16) 0.0534(6) Uani 1 1 d . . . C4 C 0.09589(13) 0.3118(2) 0.22542(19) 0.0462(7) Uani 1 1 d . . . C5 C 0.09179(17) 0.3145(3) 0.2865(2) 0.0628(10) Uani 1 1 d . . . H5 H 0.0592 0.3486 0.2761 0.075 Uiso 1 1 calc R . . C6 C 0.1333(2) 0.2693(3) 0.3599(2) 0.0734(13) Uani 1 1 d . . . H6 H 0.1295 0.2720 0.4001 0.088 Uiso 1 1 calc R . . C7 C 0.18082(18) 0.2199(3) 0.3767(2) 0.0594(9) Uani 1 1 d . . . H7 H 0.2094 0.1883 0.4284 0.071 Uiso 1 1 calc R . . C8 C 0.18798(14) 0.2150(2) 0.31883(16) 0.0412(6) Uani 1 1 d . . . C9 C 0.04986(12) 0.3618(3) 0.1437(2) 0.0539(8) Uani 1 1 d . . . H9 H 0.0474 0.3242 0.1021 0.065 Uiso 1 1 calc R . . C10 C -0.01441(16) 0.3658(3) 0.1128(3) 0.0822(14) Uani 1 1 d . . . H10A H -0.0294 0.3000 0.1060 0.123 Uiso 1 1 calc R . . H10B H -0.0414 0.3994 0.0596 0.123 Uiso 1 1 calc R . . H10C H -0.0137 0.4006 0.1529 0.123 Uiso 1 1 calc R . . C11 C 0.06979(18) 0.4624(4) 0.1447(3) 0.0800(12) Uani 1 1 d . . . H11A H 0.0752 0.5006 0.1873 0.120 Uiso 1 1 calc R . . H11B H 0.0388 0.4927 0.0908 0.120 Uiso 1 1 calc R . . H11C H 0.1084 0.4594 0.1568 0.120 Uiso 1 1 calc R . . C12 C 0.24071(14) 0.1593(2) 0.33759(17) 0.0463(6) Uani 1 1 d . . . H12 H 0.2477 0.1867 0.3017 0.056 Uiso 1 1 calc R . . C13 C 0.30099(19) 0.1680(3) 0.4275(2) 0.0793(13) Uani 1 1 d . . . H13A H 0.3113 0.2363 0.4421 0.119 Uiso 1 1 calc R . . H13B H 0.3334 0.1356 0.4335 0.119 Uiso 1 1 calc R . . H13C H 0.2966 0.1376 0.4642 0.119 Uiso 1 1 calc R . . C14 C 0.22499(17) 0.0528(2) 0.3152(2) 0.0579(8) Uani 1 1 d . . . H14A H 0.2154 0.0244 0.3470 0.087 Uiso 1 1 calc R . . H14B H 0.2598 0.0190 0.3282 0.087 Uiso 1 1 calc R . . H14C H 0.1897 0.0467 0.2561 0.087 Uiso 1 1 calc R . . C15 C 0.16812(9) 0.20074(15) 0.01772(13) 0.0247(4) Uani 1 1 d . A . C16 C 0.14445(13) 0.26345(17) -0.04868(16) 0.0353(5) Uani 1 1 d D . . C17 C 0.15318(12) 0.24123(18) -0.10300(15) 0.0353(5) Uani 1 1 d . A . H17 H 0.1379 0.2839 -0.1474 0.042 Uiso 1 1 calc R . . C18 C 0.18320(11) 0.15942(19) -0.09382(14) 0.0342(5) Uani 1 1 d . . . H18 H 0.1889 0.1457 -0.1313 0.041 Uiso 1 1 calc R A . C19 C 0.20512(11) 0.0969(2) -0.02968(15) 0.0365(5) Uani 1 1 d . A . H19 H 0.2252 0.0395 -0.0241 0.044 Uiso 1 1 calc R . . C20 C 0.19833(10) 0.11635(18) 0.02702(13) 0.0288(4) Uani 1 1 d . . . C21 C 0.1229(4) 0.3592(5) -0.0493(5) 0.0281(14) Uani 0.419(8) 1 d PD A 1 H21 H 0.1469 0.3822 0.0087 0.034 Uiso 0.419(8) 1 calc PR A 1 C22 C 0.1237(4) 0.4361(5) -0.0991(5) 0.0407(17) Uani 0.419(8) 1 d PD A 1 H22A H 0.1653 0.4441 -0.0772 0.061 Uiso 0.419(8) 1 calc PR A 1 H22B H 0.1092 0.4975 -0.0951 0.061 Uiso 0.419(8) 1 calc PR A 1 H22C H 0.0970 0.4161 -0.1570 0.061 Uiso 0.419(8) 1 calc PR A 1 C23A C 0.0382(2) 0.3516(4) -0.1597(4) 0.0530(16) Uani 0.581(8) 1 d PD A 2 H23A H 0.0124 0.4015 -0.1644 0.079 Uiso 0.581(8) 1 calc PR A 2 H23B H 0.0183 0.2886 -0.1733 0.079 Uiso 0.581(8) 1 calc PR A 2 H23C H 0.0444 0.3660 -0.1980 0.079 Uiso 0.581(8) 1 calc PR A 2 C24 C 0.22447(13) 0.0483(2) 0.09898(17) 0.0415(6) Uani 1 1 d . A . H24 H 0.1931 0.0415 0.1040 0.050 Uiso 1 1 calc R . . C25 C 0.28120(14) 0.0910(3) 0.18021(19) 0.0657(11) Uani 1 1 d . . . H25A H 0.2948 0.0485 0.2259 0.099 Uiso 1 1 calc R A . H25B H 0.2716 0.1549 0.1885 0.099 Uiso 1 1 calc R . . H25C H 0.3136 0.0971 0.1784 0.099 Uiso 1 1 calc R . . C26 C 0.2375(2) -0.0524(3) 0.0862(3) 0.0691(12) Uani 1 1 d . . . H26A H 0.2723 -0.0500 0.0892 0.104 Uiso 1 1 calc R A . H26B H 0.2017 -0.0765 0.0319 0.104 Uiso 1 1 calc R . . H26C H 0.2468 -0.0955 0.1292 0.104 Uiso 1 1 calc R . . C27 C 0.0247(3) -0.0990(4) 0.1628(3) 0.108(2) Uani 1 1 d . . . H27A H -0.0090 -0.1446 0.1244 0.130 Uiso 1 1 calc R . . H27B H 0.0334 -0.1010 0.2155 0.130 Uiso 1 1 calc R . . C28 C 0.0788(2) -0.1334(4) 0.1782(2) 0.0771(13) Uani 1 1 d . . . H28A H 0.1123 -0.0875 0.2166 0.093 Uiso 1 1 calc R . . H28B H 0.0907 -0.1962 0.2072 0.093 Uiso 1 1 calc R . . C29 C 0.0349(2) 0.0773(3) 0.1824(3) 0.0832(15) Uani 1 1 d . . . H29A H 0.0358 0.0701 0.2283 0.125 Uiso 1 1 calc R . . H29B H 0.0139 0.1374 0.1527 0.125 Uiso 1 1 calc R . . H29C H 0.0766 0.0794 0.2040 0.125 Uiso 1 1 calc R . . C30 C -0.0583(2) 0.0022(5) 0.0971(3) 0.129(3) Uani 1 1 d . . . H30A H -0.0572 -0.0070 0.1429 0.194 Uiso 1 1 calc R . . H30B H -0.0827 -0.0491 0.0562 0.194 Uiso 1 1 calc R . . H30C H -0.0764 0.0651 0.0712 0.194 Uiso 1 1 calc R . . C31 C 0.1343(2) -0.1364(4) 0.1326(3) 0.0923(16) Uani 1 1 d . . . H31A H 0.1609 -0.1886 0.1707 0.139 Uiso 1 1 calc R . . H31B H 0.1521 -0.0741 0.1601 0.139 Uiso 1 1 calc R . . H31C H 0.1301 -0.1398 0.0838 0.139 Uiso 1 1 calc R . . C32 C 0.0524(2) -0.2414(3) 0.0742(3) 0.103(2) Uani 1 1 d . . . H32A H 0.0827 -0.2892 0.1144 0.155 Uiso 1 1 calc R . . H32B H 0.0452 -0.2475 0.0233 0.155 Uiso 1 1 calc R . . H32C H 0.0142 -0.2526 0.0623 0.155 Uiso 1 1 calc R . . C23 C 0.0574(3) 0.3403(6) -0.0888(6) 0.063(3) Uani 0.419(8) 1 d PD A 1 H23D H 0.0363 0.3052 -0.1407 0.094 Uiso 0.419(8) 1 calc PR A 1 H23E H 0.0368 0.4019 -0.0997 0.094 Uiso 0.419(8) 1 calc PR A 1 H23F H 0.0570 0.3015 -0.0512 0.094 Uiso 0.419(8) 1 calc PR A 1 C22A C 0.1334(3) 0.4451(4) -0.0552(6) 0.0578(19) Uani 0.581(8) 1 d PD A 2 H22D H 0.1399 0.4512 -0.0940 0.087 Uiso 0.581(8) 1 calc PR A 2 H22E H 0.1728 0.4446 0.0014 0.087 Uiso 0.581(8) 1 calc PR A 2 H22F H 0.1092 0.4999 -0.0622 0.087 Uiso 0.581(8) 1 calc PR A 2 C21A C 0.0990(3) 0.3496(4) -0.0723(4) 0.0355(13) Uani 0.581(8) 1 d PD A 2 H21A H 0.0911 0.3468 -0.0339 0.043 Uiso 0.581(8) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.02051(7) 0.02668(8) 0.02058(7) -0.00365(5) 0.01429(6) -0.00786(5) Ga1 0.02028(10) 0.02370(11) 0.02398(11) -0.00556(8) 0.01564(9) -0.00724(8) N1 0.0281(8) 0.0270(9) 0.0286(8) -0.0080(7) 0.0217(7) -0.0096(7) C1 0.0510(14) 0.0373(13) 0.0445(13) -0.0224(11) 0.0388(12) -0.0277(11) N2 0.0359(9) 0.0276(9) 0.0310(9) -0.0094(7) 0.0269(8) -0.0133(7) C2 0.0563(15) 0.0409(14) 0.0511(15) -0.0235(11) 0.0459(14) -0.0309(12) N3 0.0660(17) 0.0736(19) 0.0522(15) -0.0292(13) 0.0502(14) -0.0402(14) C3 0.0385(11) 0.0346(12) 0.0364(11) -0.0165(9) 0.0302(10) -0.0183(9) N4 0.0498(14) 0.0518(15) 0.0389(12) 0.0106(11) 0.0210(11) 0.0042(11) C4 0.0408(13) 0.0599(18) 0.0509(15) -0.0256(14) 0.0359(13) -0.0173(12) C5 0.0628(19) 0.084(3) 0.075(2) -0.032(2) 0.059(2) -0.0211(18) C6 0.091(3) 0.103(3) 0.066(2) -0.037(2) 0.069(2) -0.044(2) C7 0.087(2) 0.065(2) 0.0479(16) -0.0165(15) 0.0536(18) -0.0349(18) C8 0.0602(16) 0.0373(13) 0.0372(12) -0.0112(10) 0.0370(13) -0.0216(12) C9 0.0311(12) 0.070(2) 0.0566(18) -0.0225(15) 0.0275(13) -0.0021(13) C10 0.0418(17) 0.086(3) 0.115(4) -0.020(3) 0.050(2) 0.0032(18) C11 0.0489(19) 0.101(3) 0.064(2) 0.013(2) 0.0258(18) -0.001(2) C12 0.0556(16) 0.0416(15) 0.0364(13) 0.0070(11) 0.0283(13) -0.0021(12) C13 0.061(2) 0.082(3) 0.0484(19) 0.0051(19) 0.0164(17) -0.010(2) C14 0.0603(19) 0.0493(18) 0.0577(19) 0.0048(15) 0.0363(17) 0.0001(15) C15 0.0272(9) 0.0267(10) 0.0256(9) -0.0055(7) 0.0198(8) -0.0095(8) C16 0.0551(15) 0.0247(11) 0.0405(13) 0.0010(9) 0.0378(12) -0.0016(10) C17 0.0475(13) 0.0350(12) 0.0302(11) 0.0024(9) 0.0286(11) -0.0039(10) C18 0.0351(11) 0.0480(14) 0.0273(10) -0.0010(10) 0.0240(10) -0.0016(10) C19 0.0354(11) 0.0494(15) 0.0352(12) 0.0079(10) 0.0278(10) 0.0122(10) C20 0.0250(9) 0.0391(12) 0.0265(10) 0.0031(8) 0.0188(8) 0.0010(8) C21 0.030(4) 0.029(3) 0.030(4) 0.008(3) 0.023(3) 0.006(3) C22 0.055(4) 0.028(3) 0.051(4) 0.016(3) 0.041(4) 0.014(3) C23A 0.041(3) 0.042(3) 0.065(4) 0.013(2) 0.031(3) 0.005(2) C24 0.0449(13) 0.0533(16) 0.0389(13) 0.0191(12) 0.0331(12) 0.0198(12) C25 0.0429(15) 0.114(3) 0.0348(14) 0.0273(18) 0.0236(13) 0.0188(18) C26 0.100(3) 0.068(2) 0.078(2) 0.042(2) 0.075(2) 0.051(2) C27 0.170(6) 0.105(4) 0.080(3) -0.018(3) 0.095(4) -0.061(4) C28 0.077(3) 0.101(3) 0.0379(16) 0.0149(18) 0.0311(18) -0.017(2) C29 0.118(3) 0.095(3) 0.088(3) -0.057(2) 0.091(3) -0.069(3) C30 0.097(3) 0.242(8) 0.108(4) -0.126(5) 0.093(3) -0.118(4) C31 0.064(2) 0.079(3) 0.113(4) 0.039(3) 0.049(3) 0.027(2) C32 0.106(4) 0.052(2) 0.065(3) 0.0072(19) 0.020(3) 0.025(2) C23 0.050(4) 0.062(5) 0.096(7) 0.047(5) 0.057(5) 0.031(4) C22A 0.052(3) 0.030(3) 0.091(6) -0.001(3) 0.047(4) -0.001(2) C21A 0.029(3) 0.031(2) 0.045(3) 0.003(2) 0.024(3) 0.001(2) _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 Sm1 N3 2.700(2) . ? Sm1 N3 2.700(2) 5 ? Sm1 N4 2.748(3) 5 ? Sm1 N4 2.748(3) . ? Sm1 Ga1 3.3124(9) 5 ? Sm1 Ga1 3.3124(9) . ? Ga1 N1 1.9287(18) . ? Ga1 N2 1.9326(18) . ? N1 C1 1.389(3) . ? N1 C3 1.424(3) . ? C1 C2 1.345(3) . ? N2 C2 1.390(3) . ? N2 C15 1.420(3) . ? N3 C29 1.406(4) . ? N3 C30 1.468(5) . ? N3 C27 1.469(7) . ? C3 C4 1.398(4) . ? C3 C8 1.410(4) . ? N4 C32 1.436(5) . ? N4 C28 1.458(5) . ? N4 C31 1.463(5) . ? C4 C5 1.403(4) . ? C4 C9 1.506(5) . ? C5 C6 1.355(6) . ? C6 C7 1.369(6) . ? C7 C8 1.401(4) . ? C8 C12 1.524(5) . ? C9 C11 1.507(6) . ? C9 C10 1.529(4) . ? C12 C14 1.526(4) . ? C12 C13 1.539(5) . ? C15 C20 1.399(3) . ? C15 C16 1.407(3) . ? C16 C17 1.393(3) . ? C16 C21 1.467(8) . ? C16 C21A 1.601(6) . ? C17 C18 1.367(4) . ? C18 C19 1.381(3) . ? C19 C20 1.393(3) . ? C20 C24 1.523(3) . ? C21 C23 1.522(9) . ? C21 C22 1.526(9) . ? C23A C21A 1.514(8) . ? C24 C26 1.519(5) . ? C24 C25 1.528(5) . ? C27 C28 1.467(8) . ? C22A C21A 1.553(8) . ? 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 N3 Sm1 N3 180.00(13) . 5 ? N3 Sm1 N4 110.14(10) . 5 ? N3 Sm1 N4 69.86(10) 5 5 ? N3 Sm1 N4 69.86(10) . . ? N3 Sm1 N4 110.14(10) 5 . ? N4 Sm1 N4 180.00(8) 5 . ? N3 Sm1 Ga1 88.44(6) . 5 ? N3 Sm1 Ga1 91.56(6) 5 5 ? N4 Sm1 Ga1 93.78(7) 5 5 ? N4 Sm1 Ga1 86.22(7) . 5 ? N3 Sm1 Ga1 91.56(6) . . ? N3 Sm1 Ga1 88.44(6) 5 . ? N4 Sm1 Ga1 86.22(7) 5 . ? N4 Sm1 Ga1 93.78(7) . . ? Ga1 Sm1 Ga1 180.000(9) 5 . ? N1 Ga1 N2 83.66(8) . . ? N1 Ga1 Sm1 137.23(5) . . ? N2 Ga1 Sm1 138.19(5) . . ? C1 N1 C3 118.73(18) . . ? C1 N1 Ga1 112.08(14) . . ? C3 N1 Ga1 128.80(14) . . ? C2 C1 N1 116.1(2) . . ? C2 N2 C15 117.82(17) . . ? C2 N2 Ga1 111.69(14) . . ? C15 N2 Ga1 130.49(14) . . ? C1 C2 N2 116.4(2) . . ? C29 N3 C30 106.1(3) . . ? C29 N3 C27 118.0(4) . . ? C30 N3 C27 103.7(4) . . ? C29 N3 Sm1 114.50(19) . . ? C30 N3 Sm1 109.5(2) . . ? C27 N3 Sm1 104.4(2) . . ? C4 C3 C8 120.6(2) . . ? C4 C3 N1 119.8(2) . . ? C8 C3 N1 119.6(2) . . ? C32 N4 C28 109.6(4) . . ? C32 N4 C31 107.6(4) . . ? C28 N4 C31 110.5(3) . . ? C32 N4 Sm1 114.3(2) . . ? C28 N4 Sm1 105.5(2) . . ? C31 N4 Sm1 109.3(2) . . ? C3 C4 C5 118.3(3) . . ? C3 C4 C9 120.1(2) . . ? C5 C4 C9 121.6(3) . . ? C6 C5 C4 121.3(3) . . ? C5 C6 C7 120.6(3) . . ? C6 C7 C8 121.1(4) . . ? C7 C8 C3 118.1(3) . . ? C7 C8 C12 120.9(3) . . ? C3 C8 C12 121.0(2) . . ? C4 C9 C11 111.8(3) . . ? C4 C9 C10 114.7(3) . . ? C11 C9 C10 109.1(3) . . ? C8 C12 C14 111.4(3) . . ? C8 C12 C13 114.3(3) . . ? C14 C12 C13 109.2(3) . . ? C20 C15 C16 120.0(2) . . ? C20 C15 N2 119.42(19) . . ? C16 C15 N2 120.6(2) . . ? C17 C16 C15 118.9(2) . . ? C17 C16 C21 120.8(3) . . ? C15 C16 C21 119.1(3) . . ? C17 C16 C21A 118.4(3) . . ? C15 C16 C21A 122.0(3) . . ? C21 C16 C21A 19.8(3) . . ? C18 C17 C16 121.4(2) . . ? C17 C18 C19 119.5(2) . . ? C18 C19 C20 121.4(2) . . ? C19 C20 C15 118.8(2) . . ? C19 C20 C24 120.8(2) . . ? C15 C20 C24 120.4(2) . . ? C16 C21 C23 103.0(6) . . ? C16 C21 C22 115.5(6) . . ? C23 C21 C22 109.1(6) . . ? C26 C24 C20 113.5(2) . . ? C26 C24 C25 110.6(3) . . ? C20 C24 C25 111.3(3) . . ? N3 C27 C28 116.0(4) . . ? N4 C28 C27 118.0(3) . . ? C23A C21A C22A 108.9(6) . . ? C23A C21A C16 117.1(5) . . ? C22A C21A C16 106.7(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.782 _refine_diff_density_min -0.706 _refine_diff_density_rms 0.083 # Attachment 'cmpd6.CIF' data_c:\bono\temp\import _database_code_depnum_ccdc_archive 'CCDC 705277' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H104 Eu Ga2 N8' _chemical_formula_weight 1276.95 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' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 29.408(6) _cell_length_b 14.089(3) _cell_length_c 21.746(4) _cell_angle_alpha 90.00 _cell_angle_beta 131.73(3) _cell_angle_gamma 90.00 _cell_volume 6724(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.261 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2676 _exptl_absorpt_coefficient_mu 1.758 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.762 _exptl_absorpt_correction_T_max 0.852 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30486 _diffrn_reflns_av_R_equivalents 0.0425 _diffrn_reflns_av_sigmaI/netI 0.0353 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 26.03 _reflns_number_total 6552 _reflns_number_gt 5236 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The largest residual electron density peak in the final difference map (1.656 e/A3) was located close to Eu(1). ; _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^)+(0.0915P)^2^+33.3023P] 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 6552 _refine_ls_number_parameters 354 _refine_ls_number_restraints 86 _refine_ls_R_factor_all 0.0709 _refine_ls_R_factor_gt 0.0553 _refine_ls_wR_factor_ref 0.1608 _refine_ls_wR_factor_gt 0.1474 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.096 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu 0.0000 0.0000 0.0000 0.03845(15) Uani 1 2 d S . . Ga1 Ga 0.11055(2) 0.15979(4) 0.09350(3) 0.03692(18) Uani 1 1 d . . . N1 N 0.1474(2) 0.2524(3) 0.1805(3) 0.0445(11) Uani 1 1 d . . . N2 N 0.1607(2) 0.2201(3) 0.0766(3) 0.0400(10) Uani 1 1 d . . . N3 N 0.0743(3) -0.1396(6) 0.1074(4) 0.087(2) Uani 1 1 d D . . N4 N -0.0013(3) 0.0071(5) 0.1207(5) 0.082(2) Uani 1 1 d DU . . C1 C 0.1876(3) 0.3106(5) 0.1856(4) 0.0591(18) Uani 1 1 d . . . H1 H 0.2101 0.3589 0.2262 0.071 Uiso 1 1 calc R . . C2 C 0.1932(3) 0.2952(5) 0.1300(4) 0.0586(17) Uani 1 1 d . . . H2 H 0.2183 0.3340 0.1276 0.070 Uiso 1 1 calc R . . C3 C 0.1440(3) 0.2601(5) 0.2432(5) 0.064(2) Uani 1 1 d . . . C4 C 0.1886(4) 0.2115(6) 0.3201(5) 0.083(3) Uani 1 1 d . . . C5 C 0.1851(5) 0.2184(7) 0.3811(6) 0.094(3) Uani 1 1 d U . . H5 H 0.2143 0.1890 0.4334 0.112 Uiso 1 1 calc R . . C6 C 0.1386(6) 0.2682(9) 0.3621(8) 0.113(3) Uani 1 1 d U . . H6 H 0.1352 0.2683 0.4026 0.135 Uiso 1 1 calc R . . C7 C 0.0967(5) 0.3174(9) 0.2947(8) 0.117(4) Uani 1 1 d . . . H7 H 0.0676 0.3556 0.2892 0.141 Uiso 1 1 calc R . . C8 C 0.0982(4) 0.3093(8) 0.2291(6) 0.090(3) Uani 1 1 d . . . C9 C 0.2427(5) 0.1589(6) 0.3398(5) 0.084(3) Uani 1 1 d . . . H9 H 0.2475 0.1833 0.3012 0.101 Uiso 1 1 calc R . . C10 C 0.3032(5) 0.1703(9) 0.4258(7) 0.140(5) Uani 1 1 d . . . H10A H 0.3139 0.2378 0.4372 0.210 Uiso 1 1 calc R . . H10B H 0.3345 0.1357 0.4310 0.210 Uiso 1 1 calc R . . H10C H 0.3006 0.1449 0.4654 0.210 Uiso 1 1 calc R . . C11 C 0.2283(5) 0.0514(7) 0.3223(7) 0.114(4) Uani 1 1 d . . . H11A H 0.2200 0.0262 0.3561 0.170 Uiso 1 1 calc R . . H11B H 0.2633 0.0181 0.3360 0.170 Uiso 1 1 calc R . . H11C H 0.1925 0.0420 0.2639 0.170 Uiso 1 1 calc R . . C12 C 0.0516(4) 0.3578(7) 0.1489(7) 0.100(3) Uani 1 1 d D . . H12 H 0.0477 0.3183 0.1073 0.120 Uiso 1 1 calc R . . C13 C 0.0697(6) 0.4546(9) 0.1434(9) 0.140(4) Uani 1 1 d DU . . H13A H 0.0804 0.4943 0.1885 0.210 Uiso 1 1 calc R . . H13B H 0.0356 0.4836 0.0905 0.210 Uiso 1 1 calc R . . H13C H 0.1050 0.4494 0.1477 0.210 Uiso 1 1 calc R . . C14 C -0.0129(5) 0.3646(10) 0.1174(9) 0.140(4) Uani 1 1 d U . . H14A H -0.0113 0.3948 0.1594 0.210 Uiso 1 1 calc R . . H14B H -0.0302 0.3007 0.1058 0.210 Uiso 1 1 calc R . . H14C H -0.0385 0.4025 0.0668 0.210 Uiso 1 1 calc R . . C15 C 0.1673(2) 0.1999(4) 0.0186(3) 0.0376(11) Uani 1 1 d . . . C16 C 0.1984(2) 0.1192(4) 0.0283(3) 0.0427(12) Uani 1 1 d . . . C17 C 0.2052(3) 0.1002(5) -0.0281(4) 0.0527(15) Uani 1 1 d . . . H17 H 0.2254 0.0440 -0.0227 0.063 Uiso 1 1 calc R . . C18 C 0.1826(3) 0.1625(5) -0.0917(4) 0.0508(14) Uani 1 1 d . . . H18 H 0.1886 0.1500 -0.1288 0.061 Uiso 1 1 calc R . . C19 C 0.1522(3) 0.2408(5) -0.1013(4) 0.0525(15) Uani 1 1 d . . . H19 H 0.1365 0.2826 -0.1459 0.063 Uiso 1 1 calc R . . C20 C 0.1431(3) 0.2623(4) -0.0473(4) 0.0480(13) Uani 1 1 d . . . C21 C 0.2251(3) 0.0509(4) 0.0999(4) 0.0592(17) Uani 1 1 d D . . H21 H 0.1940 0.0441 0.1053 0.071 Uiso 1 1 calc R . . C22 C 0.2379(5) -0.0485(5) 0.0870(6) 0.090(3) Uani 1 1 d D . . H22A H 0.2699 -0.0452 0.0842 0.135 Uiso 1 1 calc R . . H22B H 0.2007 -0.0748 0.0353 0.135 Uiso 1 1 calc R . . H22C H 0.2515 -0.0894 0.1330 0.135 Uiso 1 1 calc R . . C23 C 0.2819(3) 0.0940(7) 0.1804(4) 0.089(3) Uani 1 1 d D . . H23A H 0.2965 0.0521 0.2264 0.133 Uiso 1 1 calc R . . H23B H 0.2718 0.1563 0.1887 0.133 Uiso 1 1 calc R . . H23C H 0.3137 0.1011 0.1779 0.133 Uiso 1 1 calc R . . C24 C 0.1059(4) 0.3487(5) -0.0624(5) 0.081(2) Uani 1 1 d D . . H24 H 0.1055 0.3551 -0.0169 0.097 Uiso 1 1 calc R . . C25 C 0.1292(5) 0.4397(7) -0.0702(8) 0.118(4) Uani 1 1 d DU . . H25A H 0.1719 0.4492 -0.0203 0.178 Uiso 1 1 calc R . . H25B H 0.1048 0.4933 -0.0774 0.178 Uiso 1 1 calc R . . H25C H 0.1259 0.4353 -0.1181 0.178 Uiso 1 1 calc R . . C26 C 0.0405(5) 0.3433(10) -0.1454(8) 0.155(5) Uani 1 1 d DU . . H26A H 0.0317 0.3999 -0.1780 0.233 Uiso 1 1 calc R . . H26B H 0.0122 0.3401 -0.1362 0.233 Uiso 1 1 calc R . . H26C H 0.0359 0.2865 -0.1752 0.233 Uiso 1 1 calc R . . C27 C 0.0784(6) -0.1308(9) 0.1785(6) 0.126(4) Uani 1 1 d DU . . H27A H 0.1153 -0.0933 0.2216 0.151 Uiso 1 1 calc R . . H27B H 0.0843 -0.1950 0.2013 0.151 Uiso 1 1 calc R . . C28 C 0.0234(8) -0.0843(10) 0.1618(11) 0.194(7) Uani 1 1 d DU . . H28A H -0.0105 -0.1305 0.1292 0.233 Uiso 1 1 calc R . . H28B H 0.0346 -0.0783 0.2158 0.233 Uiso 1 1 calc R . . C29 C 0.1356(5) -0.1310(8) 0.1360(8) 0.119(4) Uani 1 1 d U . . H29A H 0.1602 -0.1860 0.1702 0.178 Uiso 1 1 calc R . . H29B H 0.1549 -0.0728 0.1685 0.178 Uiso 1 1 calc R . . H29C H 0.1325 -0.1284 0.0883 0.178 Uiso 1 1 calc R . . C30 C 0.0546(6) -0.2396(8) 0.0760(8) 0.136(4) Uani 1 1 d U . . H30A H 0.0870 -0.2838 0.1171 0.204 Uiso 1 1 calc R . . H30B H 0.0465 -0.2461 0.0246 0.204 Uiso 1 1 calc R . . H30C H 0.0175 -0.2541 0.0657 0.204 Uiso 1 1 calc R . . C31 C -0.0565(5) -0.0052(7) 0.0984(7) 0.101(3) Uani 1 1 d U . . H31A H -0.0795 -0.0542 0.0557 0.151 Uiso 1 1 calc R . . H31B H -0.0792 0.0547 0.0770 0.151 Uiso 1 1 calc R . . H31C H -0.0505 -0.0249 0.1466 0.151 Uiso 1 1 calc R . . C32 C 0.0321(5) 0.0818(8) 0.1795(7) 0.109(3) Uani 1 1 d U . . H32A H 0.0080 0.1403 0.1568 0.164 Uiso 1 1 calc R . . H32B H 0.0705 0.0919 0.1919 0.164 Uiso 1 1 calc R . . H32C H 0.0408 0.0645 0.2301 0.164 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 Eu1 0.0338(2) 0.0537(3) 0.0338(2) -0.00995(15) 0.02497(18) -0.01456(15) Ga1 0.0326(3) 0.0470(4) 0.0377(3) -0.0103(2) 0.0261(3) -0.0120(2) N1 0.045(3) 0.053(3) 0.048(3) -0.018(2) 0.036(2) -0.017(2) N2 0.042(2) 0.047(2) 0.042(2) -0.0137(19) 0.032(2) -0.017(2) N3 0.056(4) 0.103(5) 0.072(4) 0.006(4) 0.030(3) -0.007(4) N4 0.086(4) 0.108(5) 0.090(4) -0.044(3) 0.075(4) -0.048(3) C1 0.070(4) 0.065(4) 0.072(4) -0.035(3) 0.060(4) -0.036(3) C2 0.070(4) 0.062(4) 0.072(4) -0.028(3) 0.059(4) -0.035(3) C3 0.065(4) 0.077(5) 0.078(5) -0.043(4) 0.059(4) -0.040(4) C4 0.119(7) 0.097(6) 0.062(4) -0.024(4) 0.073(5) -0.054(5) C5 0.107(5) 0.104(5) 0.083(5) -0.010(4) 0.069(4) -0.029(4) C6 0.110(6) 0.123(6) 0.117(6) -0.021(5) 0.080(5) -0.021(5) C7 0.099(8) 0.157(10) 0.156(11) -0.046(9) 0.111(9) -0.032(7) C8 0.066(5) 0.136(8) 0.086(6) -0.057(6) 0.058(5) -0.034(5) C9 0.117(7) 0.072(5) 0.063(5) 0.018(4) 0.060(5) 0.022(5) C10 0.097(8) 0.139(11) 0.107(9) -0.029(7) 0.035(7) -0.025(7) C11 0.110(8) 0.085(7) 0.128(9) -0.008(6) 0.071(7) -0.022(6) C12 0.069(5) 0.110(7) 0.124(8) -0.038(6) 0.066(6) 0.002(5) C13 0.123(7) 0.156(7) 0.145(7) 0.011(6) 0.091(5) 0.012(6) C14 0.099(6) 0.154(7) 0.174(8) -0.017(6) 0.093(5) 0.016(5) C15 0.034(3) 0.046(3) 0.038(3) -0.009(2) 0.026(2) -0.014(2) C16 0.038(3) 0.055(3) 0.044(3) 0.004(2) 0.031(3) -0.001(2) C17 0.056(4) 0.065(4) 0.058(4) 0.006(3) 0.046(3) 0.008(3) C18 0.053(3) 0.065(4) 0.043(3) -0.007(3) 0.035(3) -0.008(3) C19 0.053(3) 0.063(4) 0.039(3) 0.004(3) 0.030(3) -0.007(3) C20 0.052(3) 0.050(3) 0.050(3) -0.002(3) 0.037(3) -0.006(3) C21 0.066(4) 0.071(4) 0.061(4) 0.020(3) 0.050(4) 0.019(3) C22 0.116(7) 0.088(6) 0.108(7) 0.045(5) 0.092(6) 0.046(5) C23 0.057(4) 0.146(8) 0.053(4) 0.038(5) 0.032(4) 0.023(5) C24 0.120(7) 0.060(4) 0.090(6) 0.024(4) 0.082(6) 0.027(4) C25 0.095(5) 0.089(5) 0.161(7) 0.006(5) 0.080(5) 0.005(4) C26 0.119(7) 0.135(7) 0.187(8) -0.003(6) 0.092(6) 0.003(5) C27 0.138(7) 0.128(6) 0.097(6) 0.021(5) 0.071(5) -0.011(5) C28 0.214(10) 0.204(10) 0.180(9) -0.008(6) 0.137(7) -0.002(7) C29 0.109(6) 0.112(6) 0.134(6) 0.033(5) 0.080(5) 0.017(5) C30 0.132(7) 0.110(6) 0.120(6) -0.005(5) 0.064(5) 0.003(5) C31 0.097(5) 0.144(7) 0.098(5) -0.045(4) 0.080(5) -0.045(4) C32 0.125(6) 0.132(6) 0.109(5) -0.036(4) 0.093(5) -0.050(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 Eu1 N4 2.651(7) . ? Eu1 N4 2.651(7) 5 ? Eu1 N3 2.703(7) 5 ? Eu1 N3 2.703(7) . ? Eu1 Ga1 3.3124(11) 5 ? Eu1 Ga1 3.3124(11) . ? Ga1 N1 1.931(4) . ? Ga1 N2 1.937(4) . ? N1 C1 1.382(7) . ? N1 C3 1.436(8) . ? N2 C2 1.380(7) . ? N2 C15 1.426(6) . ? N3 C29 1.467(13) . ? N3 C27 1.474(8) . ? N3 C30 1.504(13) . ? N4 C31 1.362(12) . ? N4 C32 1.427(11) . ? N4 C28 1.457(9) . ? C1 C2 1.340(8) . ? C3 C8 1.357(11) . ? C3 C4 1.437(12) . ? C4 C5 1.403(11) . ? C4 C9 1.533(13) . ? C5 C6 1.334(15) . ? C6 C7 1.321(15) . ? C7 C8 1.460(13) . ? C8 C12 1.485(14) . ? C9 C10 1.503(13) . ? C9 C11 1.550(13) . ? C12 C13 1.499(9) . ? C12 C14 1.532(13) . ? C15 C16 1.385(8) . ? C15 C20 1.405(8) . ? C16 C17 1.392(8) . ? C16 C21 1.530(8) . ? C17 C18 1.379(9) . ? C18 C19 1.347(9) . ? C19 C20 1.401(8) . ? C20 C24 1.520(9) . ? C21 C22 1.525(8) . ? C21 C23 1.526(8) . ? C24 C25 1.515(8) . ? C24 C26 1.530(9) . ? C27 C28 1.547(9) . ? 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 N4 Eu1 N4 180.0(3) . 5 ? N4 Eu1 N3 107.0(2) . 5 ? N4 Eu1 N3 73.0(2) 5 5 ? N4 Eu1 N3 73.0(2) . . ? N4 Eu1 N3 107.0(2) 5 . ? N3 Eu1 N3 180.0(4) 5 . ? N4 Eu1 Ga1 88.76(13) . 5 ? N4 Eu1 Ga1 91.24(13) 5 5 ? N3 Eu1 Ga1 93.74(15) 5 5 ? N3 Eu1 Ga1 86.26(15) . 5 ? N4 Eu1 Ga1 91.24(13) . . ? N4 Eu1 Ga1 88.76(13) 5 . ? N3 Eu1 Ga1 86.26(15) 5 . ? N3 Eu1 Ga1 93.74(15) . . ? Ga1 Eu1 Ga1 180.00(2) 5 . ? N1 Ga1 N2 83.57(18) . . ? N1 Ga1 Eu1 137.92(13) . . ? N2 Ga1 Eu1 137.87(12) . . ? C1 N1 C3 118.4(5) . . ? C1 N1 Ga1 111.8(4) . . ? C3 N1 Ga1 129.3(4) . . ? C2 N2 C15 118.2(4) . . ? C2 N2 Ga1 111.3(3) . . ? C15 N2 Ga1 130.4(3) . . ? C29 N3 C27 109.2(8) . . ? C29 N3 C30 105.3(9) . . ? C27 N3 C30 107.1(9) . . ? C29 N3 Eu1 111.4(6) . . ? C27 N3 Eu1 107.4(6) . . ? C30 N3 Eu1 116.3(6) . . ? C31 N4 C32 111.0(8) . . ? C31 N4 C28 95.5(9) . . ? C32 N4 C28 109.7(12) . . ? C31 N4 Eu1 116.3(6) . . ? C32 N4 Eu1 117.4(5) . . ? C28 N4 Eu1 104.2(8) . . ? C2 C1 N1 116.3(5) . . ? C1 C2 N2 116.9(5) . . ? C8 C3 N1 120.7(8) . . ? C8 C3 C4 120.4(7) . . ? N1 C3 C4 118.8(7) . . ? C5 C4 C3 118.8(10) . . ? C5 C4 C9 119.0(9) . . ? C3 C4 C9 122.0(6) . . ? C6 C5 C4 116.7(11) . . ? C7 C6 C5 128.8(12) . . ? C6 C7 C8 115.5(11) . . ? C3 C8 C7 119.4(10) . . ? C3 C8 C12 120.1(8) . . ? C7 C8 C12 120.5(9) . . ? C10 C9 C4 116.4(8) . . ? C10 C9 C11 108.3(8) . . ? C4 C9 C11 109.9(9) . . ? C8 C12 C13 114.4(9) . . ? C8 C12 C14 117.0(10) . . ? C13 C12 C14 107.9(10) . . ? C16 C15 C20 120.2(5) . . ? C16 C15 N2 119.7(5) . . ? C20 C15 N2 120.1(5) . . ? C15 C16 C17 119.4(5) . . ? C15 C16 C21 120.7(5) . . ? C17 C16 C21 119.9(5) . . ? C18 C17 C16 120.4(6) . . ? C19 C18 C17 120.2(6) . . ? C18 C19 C20 121.6(6) . . ? C19 C20 C15 118.1(5) . . ? C19 C20 C24 120.3(6) . . ? C15 C20 C24 121.6(5) . . ? C22 C21 C23 111.1(7) . . ? C22 C21 C16 114.3(5) . . ? C23 C21 C16 110.2(5) . . ? C25 C24 C20 112.8(7) . . ? C25 C24 C26 102.5(8) . . ? C20 C24 C26 112.0(8) . . ? N3 C27 C28 116.5(11) . . ? N4 C28 C27 122.3(13) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.03 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.656 _refine_diff_density_min -1.189 _refine_diff_density_rms 0.119 # Attachment 'cmpd7.CIF' data_c:\bono\temp\mon _database_code_depnum_ccdc_archive 'CCDC 705278' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H104 Ga2 N8 Yb' _chemical_formula_weight 1298.03 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' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 21.866(4) _cell_length_b 14.060(3) _cell_length_c 21.602(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.47(3) _cell_angle_gamma 90.00 _cell_volume 6611(2) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red-orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.304 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2704 _exptl_absorpt_coefficient_mu 2.254 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.601 _exptl_absorpt_correction_T_max 0.701 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _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 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24357 _diffrn_reflns_av_R_equivalents 0.0442 _diffrn_reflns_av_sigmaI/netI 0.0754 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 26.38 _reflns_number_total 13377 _reflns_number_gt 8750 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The largest residual electron density peak in the final difference map (2.348 e/A3) was located close to Yb(1). ; _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^)+(0.0583P)^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 13377 _refine_ls_number_parameters 700 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0880 _refine_ls_R_factor_gt 0.0459 _refine_ls_wR_factor_ref 0.1171 _refine_ls_wR_factor_gt 0.1029 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 0.999 _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 Yb1 Yb 0.252877(9) 0.261621(14) 0.252902(9) 0.02783(8) Uani 1 1 d . . . Ga1 Ga 0.36138(2) 0.10344(3) 0.27012(2) 0.02462(13) Uani 1 1 d . . . Ga2 Ga 0.14504(2) 0.41636(3) 0.23459(2) 0.02657(14) Uani 1 1 d . . . N1 N 0.41386(16) 0.0428(2) 0.33670(15) 0.0244(9) Uani 1 1 d . . . N2 N 0.39807(16) 0.0112(2) 0.21825(15) 0.0275(9) Uani 1 1 d . . . N3 N 0.10808(17) 0.5114(2) 0.28402(16) 0.0297(9) Uani 1 1 d . . . N4 N 0.09795(17) 0.4783(2) 0.16551(16) 0.0282(9) Uani 1 1 d . . . N5 N 0.17414(19) 0.1361(3) 0.2839(2) 0.0496(12) Uani 1 1 d . . . N6 N 0.2534(2) 0.2746(3) 0.37209(19) 0.0435(12) Uani 1 1 d . . . N7 N 0.2513(2) 0.2548(3) 0.13371(19) 0.0470(13) Uani 1 1 d . . . N8 N 0.32435(19) 0.4014(3) 0.2224(2) 0.0468(12) Uani 1 1 d . . . C1 C 0.4479(2) -0.0309(3) 0.3144(2) 0.0328(12) Uani 1 1 d . . . H1 H 0.4751 -0.0685 0.3412 0.039 Uiso 1 1 calc R . . C2 C 0.4402(2) -0.0460(3) 0.2530(2) 0.0343(12) Uani 1 1 d . . . H2 H 0.4627 -0.0938 0.2340 0.041 Uiso 1 1 calc R . . C3 C 0.42144(19) 0.0622(3) 0.40198(19) 0.0230(10) Uani 1 1 d . . . C4 C 0.4000(2) -0.0032(3) 0.4439(2) 0.0309(12) Uani 1 1 d . . . C5 C 0.4079(2) 0.0183(3) 0.5073(2) 0.0324(12) Uani 1 1 d . . . H5 H 0.3945 -0.0257 0.5365 0.039 Uiso 1 1 calc R . . C6 C 0.4346(2) 0.1020(3) 0.5279(2) 0.0311(11) Uani 1 1 d . . . H6 H 0.4389 0.1160 0.5711 0.037 Uiso 1 1 calc R . . C7 C 0.4553(2) 0.1657(3) 0.4866(2) 0.0317(12) Uani 1 1 d . . . H7 H 0.4735 0.2236 0.5015 0.038 Uiso 1 1 calc R . . C8 C 0.45006(19) 0.1466(3) 0.42292(19) 0.0253(11) Uani 1 1 d . . . C9 C 0.3673(3) -0.0945(3) 0.4219(2) 0.0438(14) Uani 1 1 d . . . H9 H 0.3872 -0.1174 0.3848 0.053 Uiso 1 1 calc R . . C10 C 0.3719(3) -0.1745(3) 0.4692(3) 0.0577(18) Uani 1 1 d . . . H10A H 0.3462 -0.1597 0.5027 0.086 Uiso 1 1 calc R . . H10B H 0.4147 -0.1817 0.4865 0.086 Uiso 1 1 calc R . . H10C H 0.3577 -0.2340 0.4489 0.086 Uiso 1 1 calc R . . C11 C 0.3021(3) -0.0733(4) 0.4006(3) 0.082(2) Uani 1 1 d . . . H11A H 0.2803 -0.0551 0.4363 0.123 Uiso 1 1 calc R . . H11B H 0.2828 -0.1299 0.3808 0.123 Uiso 1 1 calc R . . H11C H 0.3003 -0.0209 0.3705 0.123 Uiso 1 1 calc R . . C12 C 0.4758(2) 0.2160(3) 0.3774(2) 0.0340(12) Uani 1 1 d . . . H12 H 0.4441 0.2225 0.3411 0.041 Uiso 1 1 calc R . . C13 C 0.4886(3) 0.3165(3) 0.4037(2) 0.0456(14) Uani 1 1 d . . . H13A H 0.5207 0.3132 0.4385 0.068 Uiso 1 1 calc R . . H13B H 0.4510 0.3426 0.4182 0.068 Uiso 1 1 calc R . . H13C H 0.5023 0.3576 0.3710 0.068 Uiso 1 1 calc R . . C14 C 0.5337(2) 0.1754(4) 0.3525(2) 0.0479(15) Uani 1 1 d . . . H14A H 0.5663 0.1695 0.3867 0.072 Uiso 1 1 calc R . . H14B H 0.5473 0.2181 0.3207 0.072 Uiso 1 1 calc R . . H14C H 0.5246 0.1126 0.3342 0.072 Uiso 1 1 calc R . . C15 C 0.3952(2) 0.0046(3) 0.1518(2) 0.0339(13) Uani 1 1 d . . . C16 C 0.4408(3) 0.0484(4) 0.1199(2) 0.0434(14) Uani 1 1 d . . . C17 C 0.4346(3) 0.0423(4) 0.0553(3) 0.0617(19) Uani 1 1 d . . . H17 H 0.4645 0.0719 0.0325 0.074 Uiso 1 1 calc R . . C18 C 0.3871(4) -0.0049(5) 0.0240(3) 0.070(2) Uani 1 1 d . . . H18 H 0.3843 -0.0076 -0.0202 0.084 Uiso 1 1 calc R . . C19 C 0.3438(3) -0.0480(5) 0.0544(3) 0.064(2) Uani 1 1 d . . . H19 H 0.3112 -0.0814 0.0317 0.076 Uiso 1 1 calc R . . C20 C 0.3467(3) -0.0438(4) 0.1206(2) 0.0486(16) Uani 1 1 d . . . C21 C 0.4944(3) 0.1009(4) 0.1548(3) 0.0467(14) Uani 1 1 d . . . H21 H 0.5008 0.0734 0.1976 0.056 Uiso 1 1 calc R . . C22 C 0.4781(3) 0.2075(4) 0.1613(3) 0.0606(17) Uani 1 1 d . . . H22A H 0.4701 0.2358 0.1199 0.091 Uiso 1 1 calc R . . H22B H 0.5126 0.2406 0.1843 0.091 Uiso 1 1 calc R . . H22C H 0.4415 0.2134 0.1838 0.091 Uiso 1 1 calc R . . C23 C 0.5551(3) 0.0936(4) 0.1259(3) 0.079(2) Uani 1 1 d . . . H23A H 0.5670 0.0266 0.1233 0.118 Uiso 1 1 calc R . . H23B H 0.5870 0.1284 0.1516 0.118 Uiso 1 1 calc R . . H23C H 0.5504 0.1211 0.0840 0.118 Uiso 1 1 calc R . . C24 C 0.2983(3) -0.0916(4) 0.1555(3) 0.0578(18) Uani 1 1 d . . . H24 H 0.2938 -0.0516 0.1931 0.069 Uiso 1 1 calc R . . C25 C 0.3170(3) -0.1885(5) 0.1788(3) 0.081(2) Uani 1 1 d . . . H25A H 0.3306 -0.2263 0.1446 0.122 Uiso 1 1 calc R . . H25B H 0.2820 -0.2198 0.1954 0.122 Uiso 1 1 calc R . . H25C H 0.3508 -0.1827 0.2119 0.122 Uiso 1 1 calc R . . C26 C 0.2346(3) -0.0985(5) 0.1203(3) 0.092(3) Uani 1 1 d . . . H26A H 0.2210 -0.0351 0.1060 0.139 Uiso 1 1 calc R . . H26B H 0.2056 -0.1242 0.1479 0.139 Uiso 1 1 calc R . . H26C H 0.2362 -0.1406 0.0843 0.139 Uiso 1 1 calc R . . C27 C 0.0695(2) 0.5719(4) 0.2467(2) 0.0434(14) Uani 1 1 d . . . H27 H 0.0475 0.6221 0.2639 0.052 Uiso 1 1 calc R . . C28 C 0.0652(2) 0.5552(3) 0.1854(2) 0.0390(13) Uani 1 1 d . . . H28 H 0.0409 0.5942 0.1568 0.047 Uiso 1 1 calc R . . C29 C 0.1111(2) 0.5241(3) 0.3497(2) 0.0371(13) Uani 1 1 d . . . C30 C 0.0714(3) 0.4741(4) 0.3840(2) 0.0492(16) Uani 1 1 d . . . C31 C 0.0744(3) 0.4866(5) 0.4486(3) 0.070(2) Uani 1 1 d . . . H31 H 0.0471 0.4527 0.4723 0.084 Uiso 1 1 calc R . . C32 C 0.1160(4) 0.5469(7) 0.4771(3) 0.093(3) Uani 1 1 d . . . H32 H 0.1176 0.5554 0.5209 0.112 Uiso 1 1 calc R . . C33 C 0.1563(3) 0.5961(6) 0.4439(4) 0.097(3) Uani 1 1 d . . . H33 H 0.1852 0.6380 0.4651 0.117 Uiso 1 1 calc R . . C34 C 0.1553(3) 0.5854(5) 0.3786(3) 0.0579(18) Uani 1 1 d . . . C35 C 0.0235(3) 0.4084(4) 0.3527(3) 0.0647(19) Uani 1 1 d . . . H35 H 0.0366 0.3925 0.3108 0.078 Uiso 1 1 calc R . . C36 C 0.0186(3) 0.3162(5) 0.3874(4) 0.114(3) Uani 1 1 d U . . H36A H 0.0594 0.2974 0.4060 0.170 Uiso 1 1 calc R . . H36B H 0.0023 0.2667 0.3585 0.170 Uiso 1 1 calc R . . H36C H -0.0089 0.3246 0.4202 0.170 Uiso 1 1 calc R . . C37 C -0.0387(3) 0.4500(5) 0.3427(4) 0.108(3) Uani 1 1 d U . . H37A H -0.0543 0.4622 0.3831 0.163 Uiso 1 1 calc R . . H37B H -0.0662 0.4054 0.3188 0.163 Uiso 1 1 calc R . . H37C H -0.0370 0.5098 0.3197 0.163 Uiso 1 1 calc R . . C38 C 0.1998(3) 0.6378(5) 0.3420(3) 0.075(2) Uani 1 1 d . . . H38 H 0.2031 0.6010 0.3028 0.090 Uiso 1 1 calc R . . C39 C 0.2647(3) 0.6443(5) 0.3758(4) 0.105(3) Uani 1 1 d . . . H39A H 0.2637 0.6832 0.4133 0.157 Uiso 1 1 calc R . . H39B H 0.2924 0.6734 0.3482 0.157 Uiso 1 1 calc R . . H39C H 0.2794 0.5803 0.3874 0.157 Uiso 1 1 calc R . . C40 C 0.1770(3) 0.7372(6) 0.3230(4) 0.097(3) Uani 1 1 d . . . H40A H 0.1391 0.7320 0.2949 0.145 Uiso 1 1 calc R . . H40B H 0.2084 0.7701 0.3017 0.145 Uiso 1 1 calc R . . H40C H 0.1687 0.7731 0.3601 0.145 Uiso 1 1 calc R . . C41 C 0.0905(2) 0.4584(3) 0.1007(2) 0.0284(11) Uani 1 1 d . . . C42 C 0.1178(2) 0.5161(3) 0.0583(2) 0.0341(12) Uani 1 1 d . . . C43 C 0.1074(2) 0.4946(4) -0.0046(2) 0.0391(13) Uani 1 1 d . . . H43 H 0.1258 0.5330 -0.0339 0.047 Uiso 1 1 calc R . . C44 C 0.0715(2) 0.4194(4) -0.0255(2) 0.0422(14) Uani 1 1 d . . . H44 H 0.0638 0.4077 -0.0689 0.051 Uiso 1 1 calc R . . C45 C 0.0466(2) 0.3613(4) 0.0162(2) 0.0383(13) Uani 1 1 d . . . H45 H 0.0232 0.3077 0.0013 0.046 Uiso 1 1 calc R . . C46 C 0.0548(2) 0.3787(3) 0.0799(2) 0.0291(11) Uani 1 1 d . . . C47 C 0.1569(3) 0.6022(3) 0.0796(3) 0.0468(15) Uani 1 1 d . . . H47 H 0.1627 0.6024 0.1261 0.056 Uiso 1 1 calc R . . C48 C 0.2203(3) 0.6033(4) 0.0546(3) 0.079(2) Uani 1 1 d . . . H48A H 0.2154 0.6152 0.0097 0.119 Uiso 1 1 calc R . . H48B H 0.2404 0.5417 0.0627 0.119 Uiso 1 1 calc R . . H48C H 0.2455 0.6536 0.0754 0.119 Uiso 1 1 calc R . . C49 C 0.1249(3) 0.6921(4) 0.0582(3) 0.075(2) Uani 1 1 d . . . H49A H 0.1214 0.6950 0.0127 0.112 Uiso 1 1 calc R . . H49B H 0.1486 0.7469 0.0753 0.112 Uiso 1 1 calc R . . H49C H 0.0838 0.6935 0.0727 0.112 Uiso 1 1 calc R . . C50 C 0.0256(2) 0.3148(4) 0.1250(2) 0.0426(14) Uani 1 1 d . . . H50 H 0.0569 0.3057 0.1615 0.051 Uiso 1 1 calc R . . C51 C 0.0097(3) 0.2164(4) 0.0995(3) 0.0648(19) Uani 1 1 d . . . H51A H -0.0060 0.1773 0.1320 0.097 Uiso 1 1 calc R . . H51B H 0.0467 0.1865 0.0858 0.097 Uiso 1 1 calc R . . H51C H -0.0217 0.2217 0.0641 0.097 Uiso 1 1 calc R . . C52 C -0.0297(3) 0.3604(5) 0.1498(3) 0.0657(18) Uani 1 1 d . . . H52A H -0.0182 0.4228 0.1675 0.098 Uiso 1 1 calc R . . H52B H -0.0445 0.3198 0.1821 0.098 Uiso 1 1 calc R . . H52C H -0.0623 0.3683 0.1158 0.098 Uiso 1 1 calc R . . C53 C 0.1853(3) 0.1308(5) 0.3538(3) 0.0681(19) Uani 1 1 d . . . H53A H 0.2219 0.0907 0.3651 0.082 Uiso 1 1 calc R . . H53B H 0.1496 0.0995 0.3703 0.082 Uiso 1 1 calc R . . C54 C 0.1953(3) 0.2287(6) 0.3852(3) 0.089(3) Uani 1 1 d . . . H54A H 0.1607 0.2710 0.3708 0.107 Uiso 1 1 calc R . . H54B H 0.1952 0.2209 0.4308 0.107 Uiso 1 1 calc R . . C55 C 0.1095(3) 0.1591(5) 0.2672(3) 0.079(2) Uani 1 1 d . . . H55A H 0.1007 0.1572 0.2218 0.119 Uiso 1 1 calc R . . H55B H 0.1008 0.2229 0.2823 0.119 Uiso 1 1 calc R . . H55C H 0.0836 0.1126 0.2861 0.119 Uiso 1 1 calc R . . C56 C 0.1849(3) 0.0412(4) 0.2600(3) 0.0698(19) Uani 1 1 d . . . H56A H 0.1591 -0.0048 0.2795 0.105 Uiso 1 1 calc R . . H56B H 0.2283 0.0243 0.2696 0.105 Uiso 1 1 calc R . . H56C H 0.1746 0.0404 0.2148 0.105 Uiso 1 1 calc R . . C57 C 0.3049(3) 0.2345(4) 0.4081(2) 0.070(2) Uani 1 1 d . . . H57A H 0.2986 0.2383 0.4523 0.105 Uiso 1 1 calc R . . H57B H 0.3421 0.2699 0.4004 0.105 Uiso 1 1 calc R . . H57C H 0.3096 0.1678 0.3963 0.105 Uiso 1 1 calc R . . C58 C 0.2456(3) 0.3745(5) 0.3929(3) 0.099(3) Uani 1 1 d . . . H58A H 0.2397 0.3752 0.4373 0.149 Uiso 1 1 calc R . . H58B H 0.2097 0.4027 0.3692 0.149 Uiso 1 1 calc R . . H58C H 0.2824 0.4113 0.3858 0.149 Uiso 1 1 calc R . . C59 C 0.2752(3) 0.3546(5) 0.1175(3) 0.071(2) Uani 1 1 d . . . H59A H 0.2831 0.3553 0.0732 0.085 Uiso 1 1 calc R . . H59B H 0.2427 0.4020 0.1231 0.085 Uiso 1 1 calc R . . C60 C 0.3327(3) 0.3840(4) 0.1561(3) 0.0642(18) Uani 1 1 d . . . H60A H 0.3640 0.3337 0.1536 0.077 Uiso 1 1 calc R . . H60B H 0.3486 0.4428 0.1382 0.077 Uiso 1 1 calc R . . C61 C 0.1907(3) 0.2470(4) 0.1031(3) 0.069(2) Uani 1 1 d . . . H61A H 0.1922 0.2536 0.0581 0.103 Uiso 1 1 calc R . . H61B H 0.1648 0.2974 0.1180 0.103 Uiso 1 1 calc R . . H61C H 0.1734 0.1848 0.1122 0.103 Uiso 1 1 calc R . . C62 C 0.2913(3) 0.1848(4) 0.1108(2) 0.071(2) Uani 1 1 d . . . H62A H 0.2745 0.1212 0.1166 0.107 Uiso 1 1 calc R . . H62B H 0.3321 0.1896 0.1337 0.107 Uiso 1 1 calc R . . H62C H 0.2947 0.1959 0.0665 0.107 Uiso 1 1 calc R . . C63 C 0.3021(3) 0.4999(4) 0.2293(3) 0.0672(19) Uani 1 1 d . . . H63A H 0.2959 0.5118 0.2730 0.101 Uiso 1 1 calc R . . H63B H 0.2631 0.5083 0.2035 0.101 Uiso 1 1 calc R . . H63C H 0.3325 0.5447 0.2160 0.101 Uiso 1 1 calc R . . C64 C 0.3846(3) 0.3941(4) 0.2574(3) 0.071(2) Uani 1 1 d . . . H64A H 0.3980 0.3276 0.2584 0.107 Uiso 1 1 calc R . . H64B H 0.3821 0.4168 0.2999 0.107 Uiso 1 1 calc R . . H64C H 0.4142 0.4330 0.2372 0.107 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 Yb1 0.02675(13) 0.03466(14) 0.02194(11) 0.00098(9) 0.00162(8) 0.00923(10) Ga1 0.0249(3) 0.0293(3) 0.0193(2) -0.0010(2) 0.0000(2) 0.0073(2) Ga2 0.0240(3) 0.0314(3) 0.0236(3) -0.0014(2) -0.0014(2) 0.0080(2) N1 0.032(2) 0.026(2) 0.0154(18) 0.0011(15) 0.0020(16) 0.0065(17) N2 0.030(2) 0.033(2) 0.0188(19) -0.0051(16) 0.0014(17) 0.0112(18) N3 0.030(2) 0.030(2) 0.027(2) -0.0026(17) -0.0055(18) 0.0064(18) N4 0.030(2) 0.030(2) 0.024(2) -0.0016(17) -0.0004(17) 0.0079(18) N5 0.035(3) 0.058(3) 0.055(3) -0.001(2) -0.002(2) 0.000(2) N6 0.046(3) 0.056(3) 0.028(2) -0.007(2) -0.002(2) 0.025(2) N7 0.056(3) 0.056(3) 0.027(2) -0.005(2) -0.005(2) 0.033(2) N8 0.036(3) 0.050(3) 0.055(3) 0.007(2) 0.009(2) 0.006(2) C1 0.040(3) 0.032(3) 0.025(2) 0.003(2) -0.002(2) 0.011(2) C2 0.041(3) 0.036(3) 0.026(3) -0.002(2) 0.003(2) 0.016(2) C3 0.022(3) 0.027(3) 0.019(2) 0.0034(19) -0.0001(19) 0.007(2) C4 0.034(3) 0.032(3) 0.026(2) 0.003(2) 0.001(2) 0.005(2) C5 0.041(3) 0.036(3) 0.021(2) 0.009(2) 0.008(2) -0.002(2) C6 0.039(3) 0.036(3) 0.018(2) -0.003(2) 0.004(2) -0.001(2) C7 0.033(3) 0.036(3) 0.026(2) 0.000(2) -0.003(2) -0.005(2) C8 0.022(3) 0.030(3) 0.023(2) 0.003(2) -0.003(2) 0.004(2) C9 0.063(4) 0.035(3) 0.032(3) 0.003(2) 0.000(3) -0.011(3) C10 0.054(4) 0.033(3) 0.080(4) 0.017(3) -0.022(3) -0.007(3) C11 0.069(5) 0.059(4) 0.109(6) 0.015(4) -0.041(4) -0.012(4) C12 0.030(3) 0.045(3) 0.026(2) 0.002(2) 0.001(2) -0.006(2) C13 0.057(4) 0.044(3) 0.036(3) 0.002(3) 0.004(3) -0.013(3) C14 0.044(4) 0.065(4) 0.036(3) 0.009(3) 0.011(3) -0.010(3) C15 0.042(3) 0.038(3) 0.021(2) -0.005(2) -0.002(2) 0.025(2) C16 0.067(4) 0.043(3) 0.022(3) 0.005(2) 0.015(3) 0.026(3) C17 0.089(5) 0.066(4) 0.031(3) 0.014(3) 0.015(3) 0.039(4) C18 0.095(6) 0.089(5) 0.026(3) -0.006(3) 0.004(4) 0.045(5) C19 0.069(5) 0.078(5) 0.039(4) -0.024(3) -0.019(3) 0.028(4) C20 0.046(4) 0.059(4) 0.038(3) -0.017(3) -0.010(3) 0.021(3) C21 0.061(4) 0.040(3) 0.043(3) 0.009(3) 0.022(3) 0.006(3) C22 0.071(5) 0.046(4) 0.066(4) 0.001(3) 0.013(3) 0.011(3) C23 0.078(5) 0.064(4) 0.101(6) 0.013(4) 0.048(4) 0.009(4) C24 0.041(4) 0.062(4) 0.067(4) -0.026(3) -0.014(3) 0.004(3) C25 0.056(5) 0.099(6) 0.090(5) -0.001(5) 0.008(4) -0.013(4) C26 0.050(4) 0.104(6) 0.117(6) -0.043(5) -0.028(4) 0.001(4) C27 0.051(4) 0.042(3) 0.035(3) -0.008(2) -0.004(3) 0.021(3) C28 0.044(3) 0.036(3) 0.036(3) -0.003(2) -0.003(2) 0.016(3) C29 0.037(3) 0.041(3) 0.031(3) -0.008(2) -0.004(2) 0.024(3) C30 0.077(5) 0.040(3) 0.030(3) 0.003(3) 0.006(3) 0.026(3) C31 0.103(6) 0.081(5) 0.027(3) 0.006(3) 0.010(4) 0.040(4) C32 0.069(6) 0.164(9) 0.043(4) -0.030(5) -0.012(4) 0.060(6) C33 0.047(5) 0.161(8) 0.077(5) -0.070(6) -0.029(4) 0.046(5) C34 0.035(4) 0.086(5) 0.051(4) -0.030(3) -0.008(3) 0.024(3) C35 0.113(6) 0.034(3) 0.054(4) 0.006(3) 0.045(4) -0.010(4) C36 0.094(5) 0.078(4) 0.171(6) 0.038(4) 0.025(5) 0.011(4) C37 0.113(5) 0.083(5) 0.119(5) -0.001(4) -0.044(4) 0.007(4) C38 0.030(4) 0.096(5) 0.097(5) -0.062(4) -0.002(4) 0.003(4) C39 0.036(4) 0.100(6) 0.172(8) -0.070(6) -0.028(5) 0.014(4) C40 0.042(4) 0.142(8) 0.105(7) -0.021(5) 0.004(4) 0.004(5) C41 0.030(3) 0.030(3) 0.025(2) 0.002(2) -0.003(2) 0.013(2) C42 0.039(3) 0.027(3) 0.035(3) 0.006(2) -0.001(2) 0.002(2) C43 0.047(3) 0.045(3) 0.027(3) 0.009(2) 0.010(2) 0.002(3) C44 0.047(3) 0.053(3) 0.026(3) -0.003(3) -0.001(2) 0.004(3) C45 0.040(3) 0.044(3) 0.030(3) -0.002(2) -0.005(2) -0.008(2) C46 0.025(3) 0.034(3) 0.027(2) 0.006(2) -0.004(2) 0.001(2) C47 0.058(4) 0.037(3) 0.046(3) 0.003(3) 0.006(3) -0.011(3) C48 0.056(5) 0.066(4) 0.113(6) 0.006(4) -0.007(4) -0.004(4) C49 0.064(5) 0.031(3) 0.124(6) 0.008(4) -0.014(4) -0.006(3) C50 0.041(3) 0.046(3) 0.039(3) 0.007(3) -0.008(3) -0.015(3) C51 0.078(5) 0.055(4) 0.057(4) 0.019(3) -0.018(3) -0.030(4) C52 0.053(4) 0.092(5) 0.054(4) 0.020(4) 0.016(3) -0.010(4) C53 0.080(5) 0.074(5) 0.055(4) 0.017(4) 0.030(4) 0.011(4) C54 0.075(6) 0.157(8) 0.038(4) 0.007(4) 0.020(4) 0.014(5) C55 0.056(4) 0.082(5) 0.098(5) 0.046(4) -0.010(4) -0.025(4) C56 0.049(4) 0.071(5) 0.090(5) -0.010(4) 0.008(4) -0.007(3) C57 0.066(4) 0.111(5) 0.029(3) -0.020(3) -0.015(3) 0.053(4) C58 0.146(7) 0.103(6) 0.042(4) -0.015(4) -0.028(4) 0.084(5) C59 0.088(5) 0.081(5) 0.045(4) 0.016(3) 0.014(4) 0.031(4) C60 0.069(5) 0.063(4) 0.064(4) 0.019(3) 0.022(4) 0.020(3) C61 0.060(4) 0.103(6) 0.040(3) -0.023(3) -0.010(3) 0.038(4) C62 0.084(5) 0.093(5) 0.035(3) -0.011(3) 0.004(3) 0.059(4) C63 0.058(4) 0.044(4) 0.102(5) 0.002(4) 0.023(4) 0.004(3) C64 0.065(5) 0.069(4) 0.075(5) 0.022(4) -0.022(4) -0.025(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 Yb1 N7 2.574(4) . ? Yb1 N6 2.580(4) . ? Yb1 N5 2.597(5) . ? Yb1 N8 2.633(4) . ? Yb1 Ga2 3.2050(7) . ? Yb1 Ga1 3.2473(7) . ? Ga1 N2 1.937(3) . ? Ga1 N1 1.949(3) . ? Ga2 N3 1.935(4) . ? Ga2 N4 1.937(3) . ? N1 C1 1.389(5) . ? N1 C3 1.430(5) . ? N2 C2 1.388(5) . ? N2 C15 1.434(5) . ? N3 C27 1.397(5) . ? N3 C29 1.424(6) . ? N4 C28 1.387(6) . ? N4 C41 1.423(5) . ? N5 C56 1.457(7) . ? N5 C55 1.461(7) . ? N5 C53 1.510(7) . ? N6 C57 1.423(6) . ? N6 C54 1.475(8) . ? N6 C58 1.489(7) . ? N7 C61 1.428(7) . ? N7 C62 1.435(6) . ? N7 C59 1.549(7) . ? N8 C64 1.458(6) . ? N8 C63 1.481(6) . ? N8 C60 1.481(7) . ? C1 C2 1.337(6) . ? C3 C8 1.397(6) . ? C3 C4 1.402(6) . ? C4 C5 1.399(6) . ? C4 C9 1.522(6) . ? C5 C6 1.368(6) . ? C6 C7 1.372(6) . ? C7 C8 1.394(6) . ? C8 C12 1.530(6) . ? C9 C11 1.485(7) . ? C9 C10 1.518(6) . ? C12 C14 1.533(7) . ? C12 C13 1.538(7) . ? C15 C20 1.379(7) . ? C15 C16 1.407(7) . ? C16 C17 1.392(7) . ? C16 C21 1.524(7) . ? C17 C18 1.358(9) . ? C18 C19 1.348(9) . ? C19 C20 1.426(7) . ? C20 C24 1.514(8) . ? C21 C23 1.523(7) . ? C21 C22 1.549(7) . ? C24 C25 1.495(8) . ? C24 C26 1.526(7) . ? C27 C28 1.340(6) . ? C29 C30 1.386(7) . ? C29 C34 1.397(7) . ? C30 C31 1.402(7) . ? C30 C35 1.507(8) . ? C31 C32 1.350(10) . ? C32 C33 1.374(11) . ? C33 C34 1.417(9) . ? C34 C38 1.503(9) . ? C35 C37 1.476(9) . ? C35 C36 1.507(8) . ? C38 C40 1.526(9) . ? C38 C39 1.536(7) . ? C41 C42 1.398(6) . ? C41 C46 1.413(6) . ? C42 C43 1.391(6) . ? C42 C47 1.526(6) . ? C43 C44 1.368(7) . ? C44 C45 1.366(7) . ? C45 C46 1.392(6) . ? C46 C50 1.512(6) . ? C47 C49 1.496(7) . ? C47 C48 1.535(8) . ? C50 C52 1.511(8) . ? C50 C51 1.518(7) . ? C53 C54 1.541(9) . ? C59 C60 1.499(8) . ? 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 N7 Yb1 N6 178.02(13) . . ? N7 Yb1 N5 106.64(15) . . ? N6 Yb1 N5 74.39(15) . . ? N7 Yb1 N8 74.30(15) . . ? N6 Yb1 N8 104.51(15) . . ? N5 Yb1 N8 174.44(13) . . ? N7 Yb1 Ga2 87.85(9) . . ? N6 Yb1 Ga2 90.48(9) . . ? N5 Yb1 Ga2 89.71(10) . . ? N8 Yb1 Ga2 84.83(9) . . ? N7 Yb1 Ga1 91.65(9) . . ? N6 Yb1 Ga1 90.03(9) . . ? N5 Yb1 Ga1 90.01(10) . . ? N8 Yb1 Ga1 95.46(9) . . ? Ga2 Yb1 Ga1 179.338(13) . . ? N2 Ga1 N1 83.49(14) . . ? N2 Ga1 Yb1 136.94(10) . . ? N1 Ga1 Yb1 139.17(11) . . ? N3 Ga2 N4 83.99(15) . . ? N3 Ga2 Yb1 137.89(10) . . ? N4 Ga2 Yb1 136.97(11) . . ? C1 N1 C3 118.0(3) . . ? C1 N1 Ga1 111.6(3) . . ? C3 N1 Ga1 130.4(3) . . ? C2 N2 C15 117.9(4) . . ? C2 N2 Ga1 111.4(3) . . ? C15 N2 Ga1 129.9(3) . . ? C27 N3 C29 117.8(4) . . ? C27 N3 Ga2 111.3(3) . . ? C29 N3 Ga2 130.8(3) . . ? C28 N4 C41 116.3(3) . . ? C28 N4 Ga2 111.4(3) . . ? C41 N4 Ga2 132.3(3) . . ? C56 N5 C55 107.5(4) . . ? C56 N5 C53 107.0(5) . . ? C55 N5 C53 108.5(5) . . ? C56 N5 Yb1 113.4(4) . . ? C55 N5 Yb1 115.8(3) . . ? C53 N5 Yb1 104.1(3) . . ? C57 N6 C54 111.9(5) . . ? C57 N6 C58 108.4(4) . . ? C54 N6 C58 103.3(5) . . ? C57 N6 Yb1 116.4(3) . . ? C54 N6 Yb1 103.9(3) . . ? C58 N6 Yb1 112.2(3) . . ? C61 N7 C62 110.9(4) . . ? C61 N7 C59 106.4(4) . . ? C62 N7 C59 108.3(5) . . ? C61 N7 Yb1 112.9(4) . . ? C62 N7 Yb1 114.8(3) . . ? C59 N7 Yb1 102.7(3) . . ? C64 N8 C63 107.7(5) . . ? C64 N8 C60 107.5(5) . . ? C63 N8 C60 108.8(4) . . ? C64 N8 Yb1 110.3(3) . . ? C63 N8 Yb1 117.7(3) . . ? C60 N8 Yb1 104.4(3) . . ? C2 C1 N1 116.2(4) . . ? C1 C2 N2 117.3(4) . . ? C8 C3 C4 121.0(4) . . ? C8 C3 N1 119.2(4) . . ? C4 C3 N1 119.8(4) . . ? C5 C4 C3 118.2(4) . . ? C5 C4 C9 119.9(4) . . ? C3 C4 C9 121.8(4) . . ? C6 C5 C4 120.9(4) . . ? C5 C6 C7 120.4(4) . . ? C6 C7 C8 121.0(4) . . ? C7 C8 C3 118.3(4) . . ? C7 C8 C12 120.7(4) . . ? C3 C8 C12 120.9(4) . . ? C11 C9 C10 110.9(5) . . ? C11 C9 C4 109.6(4) . . ? C10 C9 C4 114.6(4) . . ? C8 C12 C14 110.8(4) . . ? C8 C12 C13 114.4(4) . . ? C14 C12 C13 110.1(4) . . ? C20 C15 C16 121.6(5) . . ? C20 C15 N2 118.6(5) . . ? C16 C15 N2 119.7(4) . . ? C17 C16 C15 117.3(6) . . ? C17 C16 C21 121.5(6) . . ? C15 C16 C21 121.2(4) . . ? C18 C17 C16 121.7(6) . . ? C19 C18 C17 121.1(6) . . ? C18 C19 C20 120.3(6) . . ? C15 C20 C19 117.9(6) . . ? C15 C20 C24 121.1(5) . . ? C19 C20 C24 120.9(5) . . ? C23 C21 C16 115.1(5) . . ? C23 C21 C22 108.6(5) . . ? C16 C21 C22 109.9(4) . . ? C25 C24 C20 112.9(5) . . ? C25 C24 C26 108.5(5) . . ? C20 C24 C26 115.4(5) . . ? C28 C27 N3 116.4(4) . . ? C27 C28 N4 116.9(4) . . ? C30 C29 C34 121.1(5) . . ? C30 C29 N3 119.8(5) . . ? C34 C29 N3 119.1(5) . . ? C29 C30 C31 119.8(6) . . ? C29 C30 C35 121.0(5) . . ? C31 C30 C35 119.2(6) . . ? C32 C31 C30 119.9(7) . . ? C31 C32 C33 121.0(7) . . ? C32 C33 C34 121.2(7) . . ? C29 C34 C33 117.0(7) . . ? C29 C34 C38 121.5(5) . . ? C33 C34 C38 121.5(6) . . ? C37 C35 C36 107.8(6) . . ? C37 C35 C30 114.4(5) . . ? C36 C35 C30 112.5(6) . . ? C34 C38 C40 112.3(5) . . ? C34 C38 C39 113.2(7) . . ? C40 C38 C39 109.7(6) . . ? C42 C41 C46 120.6(4) . . ? C42 C41 N4 120.9(4) . . ? C46 C41 N4 118.5(4) . . ? C43 C42 C41 118.2(4) . . ? C43 C42 C47 120.0(5) . . ? C41 C42 C47 121.7(4) . . ? C44 C43 C42 121.7(5) . . ? C45 C44 C43 119.7(5) . . ? C44 C45 C46 121.7(4) . . ? C45 C46 C41 117.9(4) . . ? C45 C46 C50 120.8(4) . . ? C41 C46 C50 121.3(4) . . ? C49 C47 C42 110.2(4) . . ? C49 C47 C48 107.1(5) . . ? C42 C47 C48 113.7(5) . . ? C52 C50 C46 112.1(4) . . ? C52 C50 C51 110.6(5) . . ? C46 C50 C51 113.8(5) . . ? N5 C53 C54 113.5(5) . . ? N6 C54 C53 113.3(6) . . ? C60 C59 N7 114.0(5) . . ? N8 C60 C59 114.2(5) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.38 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 2.348 _refine_diff_density_min -0.882 _refine_diff_density_rms 0.112 # Attachment 'cmpd8.CIF' data_compound8 _database_code_depnum_ccdc_archive 'CCDC 705279' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H98 Ga N6 O Tm' _chemical_formula_weight 1182.11 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' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tm Tm -0.3139 5.2483 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.791(3) _cell_length_b 19.556(4) _cell_length_c 20.300(4) _cell_angle_alpha 90.45(3) _cell_angle_beta 99.45(3) _cell_angle_gamma 90.31(3) _cell_volume 6575(2) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.194 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2480 _exptl_absorpt_coefficient_mu 1.790 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.491 _exptl_absorpt_correction_T_max 0.841 _exptl_absorpt_process_details 'SADABS (Scheldrick, 1997)' _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 'Bruker X8 CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 71431 _diffrn_reflns_av_R_equivalents 0.0715 _diffrn_reflns_av_sigmaI/netI 0.0890 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.04 _diffrn_reflns_theta_max 25.06 _reflns_number_total 22752 _reflns_number_gt 15622 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. " crystallographically independent molecules were refined in the asymmetric unit. There are no significant geometric differences between them. Four molecules of diethyl ether were located in the asymmetric unit and all atoms of these refined with 50% occupancy of their sites. The relatively poor r-factors for the complex and high residual electron density peaks in the final difference map (highest 2.823 e/A3 near Tm(1)) result from the fact that the crystal chosen for th eexperiment was a non-merohedral twin. The diffraction patterns for the components could not be deconvoluted. Despite this, the gross molecular framework of the complex is unambiguous and the geometric parameters for the complex are reliable within the esd's. resulting from the refinement. Cifcheck suggested the structure may have higher symmetry and the possible space group, P2(1)/c. This possibility was examined but discounted as no sensible structural solution could be obtained with a range of space groups other than P-1. ; _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^)+(0.0835P)^2^+91.2001P] 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 22752 _refine_ls_number_parameters 1318 _refine_ls_number_restraints 150 _refine_ls_R_factor_all 0.1273 _refine_ls_R_factor_gt 0.0853 _refine_ls_wR_factor_ref 0.2228 _refine_ls_wR_factor_gt 0.2011 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.058 _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 Tm1 Tm 0.82992(3) 0.47798(2) 0.29773(2) 0.03068(15) Uani 1 1 d . . . Ga1 Ga 0.69071(7) 0.38947(6) 0.24039(6) 0.0325(3) Uani 1 1 d . . . O1 O 0.6295(10) 0.0114(9) 0.1389(8) 0.055(4) Uiso 0.50 1 d PD . . N1 N 0.5783(5) 0.3890(5) 0.2462(5) 0.039(2) Uani 1 1 d . . . C1 C 0.5368(7) 0.3367(7) 0.2073(7) 0.050(3) Uani 1 1 d . . . H1 H 0.4801 0.3302 0.2032 0.060 Uiso 1 1 calc R . . Tm2 Tm 0.32964(3) 0.02045(2) 0.29934(3) 0.03154(15) Uani 1 1 d . . . Ga2 Ga 0.19185(7) 0.10874(6) 0.24255(6) 0.0327(3) Uani 1 1 d . . . O2 O 1.1260(14) 0.4810(12) 0.1344(12) 0.091(7) Uiso 0.50 1 d PD . . N2 N 0.6655(5) 0.3106(4) 0.1852(5) 0.039(2) Uani 1 1 d . . . C2 C 0.5839(7) 0.2962(7) 0.1761(6) 0.050(3) Uani 1 1 d . . . H2 H 0.5616 0.2590 0.1486 0.060 Uiso 1 1 calc R . . O3 O 0.566(3) 0.7934(15) 0.1637(15) 0.206(19) Uiso 0.50 1 d PD . . N3 N 0.8007(6) 0.5840(5) 0.2765(6) 0.050(3) Uani 1 1 d . . . C3 C 0.5301(6) 0.4378(6) 0.2741(6) 0.038(3) Uani 1 1 d . . . O4 O 0.064(3) -0.2708(18) 0.1485(17) 0.214(17) Uiso 0.50 1 d PDU . . N4 N 0.7927(5) 0.4988(4) 0.3934(4) 0.033(2) Uani 1 1 d . . . C4 C 0.5258(7) 0.4366(5) 0.3421(7) 0.042(3) Uani 1 1 d . . . N5 N 0.9741(6) 0.5060(5) 0.3378(5) 0.040(2) Uani 1 1 d . . . C5 C 0.4730(8) 0.4841(7) 0.3656(7) 0.055(4) Uani 1 1 d . . . H5 H 0.4682 0.4840 0.4116 0.066 Uiso 1 1 calc R . . N6 N 0.9155(6) 0.3999(5) 0.2402(6) 0.057(3) Uani 1 1 d . . . C6 C 0.4292(9) 0.5296(7) 0.3246(10) 0.077(5) Uani 1 1 d . . . H6 H 0.3951 0.5612 0.3421 0.092 Uiso 1 1 calc R . . N7 N 0.0804(5) 0.1084(4) 0.2493(5) 0.036(2) Uani 1 1 d . . . C7 C 0.4345(10) 0.5299(8) 0.2562(10) 0.088(6) Uani 1 1 d . . . H7 H 0.4033 0.5617 0.2278 0.106 Uiso 1 1 calc R . . N8 N 0.1656(5) 0.1867(4) 0.1855(5) 0.033(2) Uani 1 1 d . . . C8 C 0.4825(8) 0.4862(7) 0.2299(8) 0.065(4) Uani 1 1 d . . . N9 N 0.2925(5) 0.0020(4) 0.3944(4) 0.031(2) Uani 1 1 d . . . C9 C 0.5760(7) 0.3875(6) 0.3892(6) 0.041(3) Uani 1 1 d . . . H9 H 0.6312 0.3871 0.3769 0.050 Uiso 1 1 calc R . . N10 N 0.2969(6) -0.0848(5) 0.2806(5) 0.044(2) Uani 1 1 d . . . C10 C 0.5422(8) 0.3143(6) 0.3785(7) 0.056(4) Uani 1 1 d . . . H10A H 0.5780 0.2827 0.4064 0.084 Uiso 1 1 calc R . . H10B H 0.5390 0.3012 0.3314 0.084 Uiso 1 1 calc R . . H10C H 0.4882 0.3123 0.3908 0.084 Uiso 1 1 calc R . . N11 N 0.4737(5) -0.0073(5) 0.3383(5) 0.035(2) Uani 1 1 d . . . C11 C 0.5863(9) 0.4059(8) 0.4626(7) 0.067(4) Uani 1 1 d . . . H11A H 0.5333 0.4069 0.4769 0.100 Uiso 1 1 calc R . . H11B H 0.6119 0.4511 0.4700 0.100 Uiso 1 1 calc R . . H11C H 0.6203 0.3718 0.4885 0.100 Uiso 1 1 calc R . . N12 N 0.4148(6) 0.0954(5) 0.2389(6) 0.051(3) Uani 1 1 d . . . C12 C 0.4938(10) 0.4922(10) 0.1595(9) 0.088(5) Uani 1 1 d DU . . H12 H 0.5339 0.4578 0.1491 0.106 Uiso 1 1 calc R . . C13 C 0.4181(11) 0.4870(11) 0.1098(9) 0.113(8) Uani 1 1 d D . . H13A H 0.3720 0.4996 0.1312 0.169 Uiso 1 1 calc R . . H13B H 0.4111 0.4399 0.0928 0.169 Uiso 1 1 calc R . . H13C H 0.4215 0.5180 0.0727 0.169 Uiso 1 1 calc R . . C14 C 0.5213(19) 0.5632(11) 0.1459(16) 0.188(13) Uani 1 1 d DU . . H14A H 0.5611 0.5608 0.1156 0.282 Uiso 1 1 calc R . . H14B H 0.5460 0.5852 0.1879 0.282 Uiso 1 1 calc R . . H14C H 0.4748 0.5900 0.1252 0.282 Uiso 1 1 calc R . . C15 C 0.7146(7) 0.2706(6) 0.1477(5) 0.035(3) Uani 1 1 d . . . C16 C 0.7589(7) 0.2149(5) 0.1770(6) 0.037(3) Uani 1 1 d . . . C17 C 0.8076(8) 0.1777(7) 0.1406(7) 0.050(3) Uani 1 1 d . . . H17 H 0.8372 0.1400 0.1610 0.060 Uiso 1 1 calc R . . C18 C 0.8137(9) 0.1943(8) 0.0762(7) 0.065(4) Uani 1 1 d . . . H18 H 0.8470 0.1687 0.0517 0.078 Uiso 1 1 calc R . . C19 C 0.7699(10) 0.2492(7) 0.0482(7) 0.063(4) Uani 1 1 d . . . H19 H 0.7731 0.2605 0.0033 0.075 Uiso 1 1 calc R . . C20 C 0.7216(9) 0.2888(7) 0.0822(7) 0.060(4) Uani 1 1 d . . . C21 C 0.7517(8) 0.1940(7) 0.2487(7) 0.057(4) Uani 1 1 d . . . H21 H 0.7463 0.2374 0.2740 0.069 Uiso 1 1 calc R . . C22 C 0.6766(11) 0.1527(10) 0.2515(9) 0.091(5) Uani 1 1 d U . . H22A H 0.6290 0.1796 0.2334 0.137 Uiso 1 1 calc R . . H22B H 0.6742 0.1409 0.2980 0.137 Uiso 1 1 calc R . . H22C H 0.6776 0.1108 0.2250 0.137 Uiso 1 1 calc R . . C23 C 0.8268(7) 0.1571(6) 0.2861(6) 0.044(3) Uani 1 1 d . . . H23A H 0.8330 0.1131 0.2642 0.066 Uiso 1 1 calc R . . H23B H 0.8200 0.1494 0.3325 0.066 Uiso 1 1 calc R . . H23C H 0.8749 0.1854 0.2853 0.066 Uiso 1 1 calc R . . C24 C 0.6727(13) 0.3501(9) 0.0477(8) 0.092(6) Uani 1 1 d . . . H24 H 0.6577 0.3809 0.0832 0.110 Uiso 1 1 calc R . . C25 C 0.5944(12) 0.3247(10) 0.0032(10) 0.095(6) Uani 1 1 d U . . H25A H 0.6076 0.2894 -0.0277 0.143 Uiso 1 1 calc R . . H25B H 0.5681 0.3631 -0.0222 0.143 Uiso 1 1 calc R . . H25C H 0.5579 0.3055 0.0314 0.143 Uiso 1 1 calc R . . C26 C 0.7248(11) 0.3917(9) 0.0055(9) 0.090(5) Uani 1 1 d U . . H26A H 0.7743 0.4074 0.0342 0.136 Uiso 1 1 calc R . . H26B H 0.6942 0.4312 -0.0138 0.136 Uiso 1 1 calc R . . H26C H 0.7388 0.3626 -0.0303 0.136 Uiso 1 1 calc R . . C27 C 0.7284(7) 0.5728(5) 0.3057(6) 0.043(3) Uani 1 1 d . . . H27 H 0.6801 0.5945 0.2855 0.052 Uiso 1 1 calc R . . C28 C 0.7252(6) 0.5337(5) 0.3594(6) 0.035(3) Uani 1 1 d . . . H28 H 0.6752 0.5294 0.3752 0.042 Uiso 1 1 calc R . . C29 C 0.8104(8) 0.6460(5) 0.2441(6) 0.046(3) Uani 1 1 d . . . C30 C 0.8119(8) 0.6460(7) 0.1741(7) 0.054(3) Uani 1 1 d . . . C31 C 0.8214(8) 0.7074(7) 0.1430(8) 0.062(4) Uani 1 1 d . . . H31 H 0.8230 0.7073 0.0964 0.075 Uiso 1 1 calc R . . C32 C 0.8286(12) 0.7680(8) 0.1767(9) 0.088(6) Uani 1 1 d . . . H32 H 0.8308 0.8098 0.1536 0.106 Uiso 1 1 calc R . . C33 C 0.8325(13) 0.7679(8) 0.2462(11) 0.098(6) Uani 1 1 d . . . H33 H 0.8413 0.8096 0.2707 0.117 Uiso 1 1 calc R . . C34 C 0.8235(11) 0.7066(7) 0.2799(8) 0.071(4) Uani 1 1 d . . . C35 C 0.8040(11) 0.5801(8) 0.1345(8) 0.079(5) Uani 1 1 d D . . H35 H 0.8065 0.5408 0.1660 0.094 Uiso 1 1 calc R . . C36 C 0.7267(14) 0.5758(17) 0.0859(14) 0.180(12) Uani 1 1 d DU . . H36A H 0.7201 0.6175 0.0591 0.270 Uiso 1 1 calc R . . H36B H 0.6813 0.5710 0.1103 0.270 Uiso 1 1 calc R . . H36C H 0.7281 0.5361 0.0564 0.270 Uiso 1 1 calc R . . C37 C 0.8702(13) 0.5731(14) 0.0936(12) 0.148(10) Uani 1 1 d DU . . H37A H 0.8814 0.5246 0.0875 0.221 Uiso 1 1 calc R . . H37B H 0.9190 0.5961 0.1167 0.221 Uiso 1 1 calc R . . H37C H 0.8534 0.5942 0.0499 0.221 Uiso 1 1 calc R . . C38 C 0.8282(11) 0.7089(9) 0.3539(9) 0.081(5) Uani 1 1 d U . . H38 H 0.8320 0.6605 0.3695 0.097 Uiso 1 1 calc R . . C39 C 0.7507(13) 0.7371(11) 0.3711(10) 0.106(6) Uani 1 1 d U . . H39A H 0.7402 0.7820 0.3506 0.159 Uiso 1 1 calc R . . H39B H 0.7555 0.7417 0.4198 0.159 Uiso 1 1 calc R . . H39C H 0.7060 0.7059 0.3544 0.159 Uiso 1 1 calc R . . C40 C 0.9050(13) 0.7458(11) 0.3888(11) 0.110(7) Uani 1 1 d U . . H40A H 0.9022 0.7944 0.3771 0.165 Uiso 1 1 calc R . . H40B H 0.9524 0.7254 0.3742 0.165 Uiso 1 1 calc R . . H40C H 0.9092 0.7412 0.4373 0.165 Uiso 1 1 calc R . . C41 C 0.7922(6) 0.4789(5) 0.4604(6) 0.034(3) Uani 1 1 d . . . C42 C 0.8191(7) 0.4140(5) 0.4821(6) 0.037(3) Uani 1 1 d . . . C43 C 0.8116(8) 0.3937(6) 0.5461(7) 0.049(3) Uani 1 1 d . . . H43 H 0.8293 0.3493 0.5602 0.059 Uiso 1 1 calc R . . C44 C 0.7796(7) 0.4351(7) 0.5901(6) 0.049(3) Uani 1 1 d . . . H44 H 0.7720 0.4192 0.6328 0.059 Uiso 1 1 calc R . . C45 C 0.7590(7) 0.5010(7) 0.5696(7) 0.053(4) Uani 1 1 d . . . H45 H 0.7398 0.5315 0.6000 0.064 Uiso 1 1 calc R . . C46 C 0.7656(6) 0.5242(6) 0.5051(6) 0.038(3) Uani 1 1 d . . . C47 C 0.8543(7) 0.3629(5) 0.4377(6) 0.041(3) Uani 1 1 d . . . H47 H 0.8661 0.3882 0.3978 0.049 Uiso 1 1 calc R . . C48 C 0.7932(8) 0.3068(6) 0.4129(7) 0.050(3) Uani 1 1 d . . . H48A H 0.7727 0.2867 0.4509 0.076 Uiso 1 1 calc R . . H48B H 0.8193 0.2713 0.3898 0.076 Uiso 1 1 calc R . . H48C H 0.7483 0.3263 0.3820 0.076 Uiso 1 1 calc R . . C49 C 0.9337(8) 0.3309(6) 0.4719(6) 0.049(3) Uani 1 1 d . . . H49A H 0.9708 0.3671 0.4916 0.074 Uiso 1 1 calc R . . H49B H 0.9582 0.3052 0.4388 0.074 Uiso 1 1 calc R . . H49C H 0.9226 0.2999 0.5070 0.074 Uiso 1 1 calc R . . C50 C 0.7510(7) 0.5994(6) 0.4923(7) 0.044(3) Uani 1 1 d . . . H50 H 0.7603 0.6088 0.4458 0.053 Uiso 1 1 calc R . . C51 C 0.6622(8) 0.6208(7) 0.4969(8) 0.063(4) Uani 1 1 d . . . H51A H 0.6247 0.5963 0.4625 0.095 Uiso 1 1 calc R . . H51B H 0.6563 0.6702 0.4900 0.095 Uiso 1 1 calc R . . H51C H 0.6500 0.6092 0.5411 0.095 Uiso 1 1 calc R . . C52 C 0.8118(8) 0.6425(6) 0.5402(7) 0.057(4) Uani 1 1 d . . . H52A H 0.8033 0.6349 0.5862 0.085 Uiso 1 1 calc R . . H52B H 0.8041 0.6910 0.5293 0.085 Uiso 1 1 calc R . . H52C H 0.8668 0.6291 0.5356 0.085 Uiso 1 1 calc R . . C53 C 0.9911(8) 0.5105(7) 0.4109(6) 0.051(3) Uani 1 1 d . . . H53A H 0.9725 0.4685 0.4299 0.077 Uiso 1 1 calc R . . H53B H 0.9628 0.5498 0.4261 0.077 Uiso 1 1 calc R . . H53C H 1.0493 0.5160 0.4257 0.077 Uiso 1 1 calc R . . C54 C 0.9920(8) 0.5737(7) 0.3119(8) 0.063(4) Uani 1 1 d . . . H54A H 1.0493 0.5845 0.3258 0.095 Uiso 1 1 calc R . . H54B H 0.9592 0.6085 0.3296 0.095 Uiso 1 1 calc R . . H54C H 0.9792 0.5730 0.2630 0.095 Uiso 1 1 calc R . . C55 C 1.0285(8) 0.4553(8) 0.3150(7) 0.059(4) Uani 1 1 d . . . H55A H 1.0341 0.4159 0.3456 0.071 Uiso 1 1 calc R . . H55B H 1.0826 0.4761 0.3163 0.071 Uiso 1 1 calc R . . C56 C 0.9976(8) 0.4310(8) 0.2462(8) 0.070(5) Uani 1 1 d . . . H56A H 1.0353 0.3968 0.2328 0.084 Uiso 1 1 calc R . . H56B H 0.9957 0.4700 0.2151 0.084 Uiso 1 1 calc R . . C57 C 0.8839(10) 0.3915(8) 0.1666(7) 0.069(4) Uani 1 1 d . . . H57A H 0.9139 0.3552 0.1481 0.104 Uiso 1 1 calc R . . H57B H 0.8908 0.4346 0.1438 0.104 Uiso 1 1 calc R . . H57C H 0.8265 0.3793 0.1602 0.104 Uiso 1 1 calc R . . C58 C 0.9162(9) 0.3304(7) 0.2703(7) 0.058(4) Uani 1 1 d . . . H58A H 0.9444 0.2986 0.2447 0.087 Uiso 1 1 calc R . . H58B H 0.8606 0.3145 0.2693 0.087 Uiso 1 1 calc R . . H58C H 0.9441 0.3325 0.3166 0.087 Uiso 1 1 calc R . . C59 C 0.0385(7) 0.1587(7) 0.2100(6) 0.050(3) Uani 1 1 d . . . H59 H -0.0183 0.1638 0.2062 0.060 Uiso 1 1 calc R . . C60 C 0.0844(8) 0.2006(7) 0.1772(7) 0.055(3) Uani 1 1 d . . . H60 H 0.0613 0.2371 0.1502 0.066 Uiso 1 1 calc R . . C61 C 0.0307(7) 0.0599(6) 0.2776(7) 0.045(3) Uani 1 1 d . . . C62 C -0.0118(9) 0.0091(8) 0.2367(8) 0.071(5) Uani 1 1 d . . . C63 C -0.0625(9) -0.0338(8) 0.2656(10) 0.087(6) Uani 1 1 d . . . H63 H -0.0927 -0.0678 0.2384 0.105 Uiso 1 1 calc R . . C64 C -0.0707(10) -0.0296(7) 0.3299(10) 0.083(6) Uani 1 1 d . . . H64 H -0.1079 -0.0586 0.3471 0.099 Uiso 1 1 calc R . . C65 C -0.0254(8) 0.0167(6) 0.3706(8) 0.055(4) Uani 1 1 d . . . H65 H -0.0289 0.0177 0.4168 0.066 Uiso 1 1 calc R . . C66 C 0.0268(7) 0.0631(5) 0.3457(6) 0.040(3) Uani 1 1 d . . . C67 C 0.0004(12) -0.0032(10) 0.1641(10) 0.092(5) Uani 1 1 d U . . H67 H 0.0463 0.0258 0.1545 0.111 Uiso 1 1 calc R . . C68 C -0.0731(14) 0.0132(12) 0.1162(10) 0.128(9) Uani 1 1 d . . . H68A H -0.1206 -0.0057 0.1322 0.191 Uiso 1 1 calc R . . H68B H -0.0691 -0.0067 0.0725 0.191 Uiso 1 1 calc R . . H68C H -0.0784 0.0630 0.1123 0.191 Uiso 1 1 calc R . . C69 C 0.0212(13) -0.0812(11) 0.1555(11) 0.114(7) Uani 1 1 d U . . H69A H -0.0280 -0.1088 0.1532 0.170 Uiso 1 1 calc R . . H69B H 0.0608 -0.0956 0.1937 0.170 Uiso 1 1 calc R . . H69C H 0.0437 -0.0874 0.1143 0.170 Uiso 1 1 calc R . . C70 C 0.0765(7) 0.1140(6) 0.3917(6) 0.043(3) Uani 1 1 d . . . H70 H 0.1312 0.1154 0.3783 0.052 Uiso 1 1 calc R . . C71 C 0.0412(8) 0.1868(6) 0.3809(7) 0.055(3) Uani 1 1 d . . . H71A H -0.0149 0.1867 0.3885 0.082 Uiso 1 1 calc R . . H71B H 0.0432 0.2012 0.3350 0.082 Uiso 1 1 calc R . . H71C H 0.0731 0.2188 0.4123 0.082 Uiso 1 1 calc R . . C72 C 0.0895(9) 0.0974(8) 0.4657(7) 0.063(4) Uani 1 1 d . . . H72A H 0.0382 0.1015 0.4825 0.095 Uiso 1 1 calc R . . H72B H 0.1290 0.1294 0.4900 0.095 Uiso 1 1 calc R . . H72C H 0.1096 0.0506 0.4723 0.095 Uiso 1 1 calc R . . C73 C 0.2156(6) 0.2265(6) 0.1491(5) 0.036(3) Uani 1 1 d . . . C74 C 0.2588(7) 0.2820(6) 0.1792(6) 0.037(3) Uani 1 1 d . . . C75 C 0.3087(7) 0.3194(6) 0.1424(7) 0.049(3) Uani 1 1 d . . . H75 H 0.3387 0.3575 0.1627 0.059 Uiso 1 1 calc R . . C76 C 0.3144(9) 0.3019(7) 0.0783(7) 0.059(4) Uani 1 1 d . . . H76 H 0.3484 0.3271 0.0541 0.071 Uiso 1 1 calc R . . C77 C 0.2703(9) 0.2472(7) 0.0493(7) 0.062(4) Uani 1 1 d . . . H77 H 0.2733 0.2355 0.0042 0.075 Uiso 1 1 calc R . . C78 C 0.2216(8) 0.2086(7) 0.0835(7) 0.054(3) Uani 1 1 d . . . C79 C 0.2540(6) 0.3034(7) 0.2510(7) 0.061(4) Uani 1 1 d D . . H79 H 0.2502 0.2599 0.2758 0.073 Uiso 1 1 calc R . . C80 C 0.3270(6) 0.3404(6) 0.2877(6) 0.046(3) Uani 1 1 d D . . H80A H 0.3248 0.3886 0.2750 0.069 Uiso 1 1 calc R . . H80B H 0.3759 0.3197 0.2761 0.069 Uiso 1 1 calc R . . H80C H 0.3277 0.3368 0.3359 0.069 Uiso 1 1 calc R . . C81 C 0.1781(8) 0.3412(9) 0.2558(9) 0.088(5) Uani 1 1 d DU . . H81A H 0.1779 0.3844 0.2316 0.133 Uiso 1 1 calc R . . H81B H 0.1752 0.3507 0.3028 0.133 Uiso 1 1 calc R . . H81C H 0.1315 0.3134 0.2360 0.133 Uiso 1 1 calc R . . C82 C 0.1750(14) 0.1464(9) 0.0502(8) 0.093(6) Uani 1 1 d . . . H82 H 0.1615 0.1157 0.0861 0.112 Uiso 1 1 calc R . . C83 C 0.2242(12) 0.1053(9) 0.0061(8) 0.089(6) Uani 1 1 d . . . H83A H 0.2259 0.1302 -0.0354 0.134 Uiso 1 1 calc R . . H83B H 0.1987 0.0605 -0.0044 0.134 Uiso 1 1 calc R . . H83C H 0.2793 0.0992 0.0300 0.134 Uiso 1 1 calc R . . C84 C 0.0944(11) 0.1706(11) 0.0072(10) 0.100(7) Uani 1 1 d . . . H84A H 0.0574 0.1863 0.0366 0.150 Uiso 1 1 calc R . . H84B H 0.0696 0.1324 -0.0206 0.150 Uiso 1 1 calc R . . H84C H 0.1057 0.2083 -0.0216 0.150 Uiso 1 1 calc R . . C85 C 0.2236(7) -0.0337(5) 0.3625(6) 0.037(3) Uani 1 1 d . . . H85 H 0.1746 -0.0294 0.3797 0.044 Uiso 1 1 calc R . . C86 C 0.2249(7) -0.0739(5) 0.3081(6) 0.041(3) Uani 1 1 d . . . H86 H 0.1762 -0.0956 0.2876 0.049 Uiso 1 1 calc R . . C87 C 0.2929(6) 0.0226(5) 0.4617(6) 0.034(3) Uani 1 1 d . . . C88 C 0.2657(6) -0.0213(6) 0.5100(6) 0.038(3) Uani 1 1 d . . . C89 C 0.2602(7) 0.0043(7) 0.5716(6) 0.047(3) Uani 1 1 d . . . H89 H 0.2398 -0.0248 0.6024 0.057 Uiso 1 1 calc R . . C90 C 0.2825(7) 0.0695(7) 0.5917(6) 0.047(3) Uani 1 1 d . . . H90 H 0.2763 0.0858 0.6347 0.057 Uiso 1 1 calc R . . C91 C 0.3144(7) 0.1110(6) 0.5477(6) 0.045(3) Uani 1 1 d . . . H91 H 0.3320 0.1559 0.5613 0.054 Uiso 1 1 calc R . . C92 C 0.3212(6) 0.0880(5) 0.4834(5) 0.032(3) Uani 1 1 d . . . C93 C 0.2497(7) -0.0968(6) 0.4967(7) 0.046(3) Uani 1 1 d . . . H93 H 0.2575 -0.1063 0.4497 0.055 Uiso 1 1 calc R . . C94 C 0.3104(8) -0.1405(7) 0.5422(7) 0.054(3) Uani 1 1 d . . . H94A H 0.3654 -0.1266 0.5377 0.082 Uiso 1 1 calc R . . H94B H 0.3020 -0.1888 0.5295 0.082 Uiso 1 1 calc R . . H94C H 0.3027 -0.1341 0.5887 0.082 Uiso 1 1 calc R . . C95 C 0.1614(8) -0.1173(7) 0.5019(7) 0.055(3) Uani 1 1 d . . . H95A H 0.1536 -0.1143 0.5487 0.083 Uiso 1 1 calc R . . H95B H 0.1509 -0.1643 0.4855 0.083 Uiso 1 1 calc R . . H95C H 0.1240 -0.0862 0.4749 0.083 Uiso 1 1 calc R . . C96 C 0.3581(7) 0.1376(5) 0.4381(6) 0.037(3) Uani 1 1 d . . . H96 H 0.3698 0.1110 0.3986 0.045 Uiso 1 1 calc R . . C97 C 0.4359(8) 0.1700(6) 0.4718(6) 0.046(3) Uani 1 1 d . . . H97A H 0.4628 0.1923 0.4383 0.070 Uiso 1 1 calc R . . H97B H 0.4713 0.1347 0.4945 0.070 Uiso 1 1 calc R . . H97C H 0.4244 0.2040 0.5046 0.070 Uiso 1 1 calc R . . C98 C 0.2969(8) 0.1934(6) 0.4125(6) 0.050(3) Uani 1 1 d . . . H98A H 0.2821 0.2187 0.4505 0.075 Uiso 1 1 calc R . . H98B H 0.2485 0.1722 0.3867 0.075 Uiso 1 1 calc R . . H98C H 0.3211 0.2249 0.3840 0.075 Uiso 1 1 calc R . . C99 C 0.3059(8) -0.1479(6) 0.2441(8) 0.057(4) Uani 1 1 d . . . C100 C 0.3119(9) -0.1487(7) 0.1789(8) 0.060(4) Uani 1 1 d . . . C101 C 0.3204(9) -0.2121(8) 0.1478(8) 0.068(4) Uani 1 1 d . . . H101 H 0.3243 -0.2129 0.1017 0.082 Uiso 1 1 calc R . . C102 C 0.3232(13) -0.2717(9) 0.1808(9) 0.097(6) Uani 1 1 d . . . H102 H 0.3260 -0.3143 0.1584 0.116 Uiso 1 1 calc R . . C103 C 0.3218(11) -0.2685(9) 0.2475(9) 0.088(5) Uani 1 1 d U . . H103 H 0.3270 -0.3103 0.2714 0.105 Uiso 1 1 calc R . . C104 C 0.3133(13) -0.2083(7) 0.2840(9) 0.088(6) Uani 1 1 d . . . C105 C 0.3110(10) -0.0831(7) 0.1410(8) 0.079(5) Uani 1 1 d D . . H105 H 0.3272 -0.0455 0.1743 0.095 Uiso 1 1 calc R . . C106 C 0.3673(13) -0.0804(12) 0.0908(10) 0.126(8) Uani 1 1 d DU . . H10D H 0.3455 -0.1088 0.0520 0.189 Uiso 1 1 calc R . . H10E H 0.4203 -0.0977 0.1110 0.189 Uiso 1 1 calc R . . H10F H 0.3728 -0.0331 0.0767 0.189 Uiso 1 1 calc R . . C107 C 0.2273(13) -0.0684(14) 0.1067(13) 0.153(10) Uani 1 1 d DU . . H10G H 0.1885 -0.0825 0.1352 0.230 Uiso 1 1 calc R . . H10H H 0.2165 -0.0937 0.0643 0.230 Uiso 1 1 calc R . . H10I H 0.2219 -0.0192 0.0981 0.230 Uiso 1 1 calc R . . C108 C 0.3134(13) -0.2102(11) 0.3580(10) 0.100(6) Uani 1 1 d U . . H108 H 0.3202 -0.1620 0.3748 0.120 Uiso 1 1 calc R . . C109 C 0.3845(14) -0.2507(11) 0.3947(11) 0.122(7) Uani 1 1 d U . . H10J H 0.3676 -0.2982 0.3997 0.183 Uiso 1 1 calc R . . H10K H 0.4024 -0.2302 0.4389 0.183 Uiso 1 1 calc R . . H10L H 0.4291 -0.2497 0.3690 0.183 Uiso 1 1 calc R . . C110 C 0.2316(14) -0.2350(11) 0.3710(11) 0.119(7) Uani 1 1 d U . . H11D H 0.2300 -0.2325 0.4190 0.179 Uiso 1 1 calc R . . H11E H 0.2229 -0.2824 0.3554 0.179 Uiso 1 1 calc R . . H11F H 0.1892 -0.2061 0.3469 0.179 Uiso 1 1 calc R . . C111 C 0.4929(8) -0.0100(6) 0.4119(6) 0.049(3) Uani 1 1 d . . . H11G H 0.5508 -0.0180 0.4255 0.073 Uiso 1 1 calc R . . H11H H 0.4622 -0.0473 0.4281 0.073 Uiso 1 1 calc R . . H11I H 0.4784 0.0335 0.4310 0.073 Uiso 1 1 calc R . . C112 C 0.4880(8) -0.0776(7) 0.3139(8) 0.063(4) Uani 1 1 d . . . H11J H 0.5443 -0.0902 0.3293 0.095 Uiso 1 1 calc R . . H11K H 0.4768 -0.0786 0.2650 0.095 Uiso 1 1 calc R . . H11L H 0.4521 -0.1100 0.3314 0.095 Uiso 1 1 calc R . . C113 C 0.5286(7) 0.0426(7) 0.3131(7) 0.055(4) Uani 1 1 d . . . H11M H 0.5354 0.0834 0.3427 0.066 Uiso 1 1 calc R . . H11N H 0.5823 0.0216 0.3141 0.066 Uiso 1 1 calc R . . C114 C 0.4963(8) 0.0638(8) 0.2441(8) 0.066(4) Uani 1 1 d . . . H11O H 0.4928 0.0234 0.2141 0.079 Uiso 1 1 calc R . . H11P H 0.5340 0.0971 0.2291 0.079 Uiso 1 1 calc R . . C115 C 0.4202(9) 0.1648(7) 0.2706(7) 0.062(4) Uani 1 1 d . . . H11Q H 0.4458 0.1614 0.3174 0.093 Uiso 1 1 calc R . . H11R H 0.3659 0.1836 0.2682 0.093 Uiso 1 1 calc R . . H11S H 0.4525 0.1949 0.2469 0.093 Uiso 1 1 calc R . . C116 C 0.3819(8) 0.1038(7) 0.1661(6) 0.055(3) Uani 1 1 d . . . H11T H 0.4188 0.1324 0.1454 0.082 Uiso 1 1 calc R . . H11U H 0.3288 0.1255 0.1612 0.082 Uiso 1 1 calc R . . H11V H 0.3765 0.0588 0.1441 0.082 Uiso 1 1 calc R . . C117 C 0.557(2) 0.0930(19) 0.062(2) 0.106(13) Uiso 0.50 1 d PD . . H11W H 0.5459 0.1139 0.1035 0.159 Uiso 0.50 1 calc PR . . H11$ H 0.5088 0.0675 0.0405 0.159 Uiso 0.50 1 calc PR . . H11 H 0.5696 0.1288 0.0318 0.159 Uiso 0.50 1 calc PR . . C118 C 0.6267(19) 0.0450(16) 0.0770(12) 0.085(10) Uiso 0.50 1 d PD . . H3 H 0.6230 0.0103 0.0408 0.102 Uiso 0.50 1 calc PR . . H4 H 0.6775 0.0711 0.0776 0.102 Uiso 0.50 1 calc PR . . C119 C 0.6984(14) -0.0305(14) 0.1539(12) 0.066(8) Uiso 0.50 1 d PD . . H8 H 0.7475 -0.0030 0.1516 0.079 Uiso 0.50 1 calc PR . . H13 H 0.6955 -0.0677 0.1202 0.079 Uiso 0.50 1 calc PR . . C120 C 0.704(2) -0.0607(17) 0.2218(13) 0.079(9) Uiso 0.50 1 d PD . . H12A H 0.6985 -0.0244 0.2543 0.119 Uiso 0.50 1 calc PR . . H12B H 0.7567 -0.0828 0.2340 0.119 Uiso 0.50 1 calc PR . . H12C H 0.6610 -0.0947 0.2217 0.119 Uiso 0.50 1 calc PR . . C121 C 1.202(2) 0.557(2) 0.2192(16) 0.111(13) Uiso 0.50 1 d PD . . H12D H 1.1630 0.5907 0.2310 0.166 Uiso 0.50 1 calc PR . . H12E H 1.2560 0.5772 0.2271 0.166 Uiso 0.50 1 calc PR . . H12F H 1.2004 0.5164 0.2468 0.166 Uiso 0.50 1 calc PR . . C122 C 1.179(2) 0.5378(18) 0.1472(16) 0.121(15) Uiso 0.50 1 d PD . . H12G H 1.1537 0.5777 0.1225 0.145 Uiso 0.50 1 calc PR . . H12H H 1.2292 0.5274 0.1293 0.145 Uiso 0.50 1 calc PR . . C123 C 1.122(3) 0.439(2) 0.0769(18) 0.144(19) Uiso 0.50 1 d PD . . H12I H 1.1750 0.4165 0.0795 0.173 Uiso 0.50 1 calc PR . . H12J H 1.1160 0.4696 0.0379 0.173 Uiso 0.50 1 calc PR . . C124 C 1.059(2) 0.3839(18) 0.0607(19) 0.101(12) Uiso 0.50 1 d PD . . H12K H 1.0517 0.3603 0.1018 0.152 Uiso 0.50 1 calc PR . . H12L H 1.0763 0.3509 0.0294 0.152 Uiso 0.50 1 calc PR . . H12M H 1.0077 0.4044 0.0404 0.152 Uiso 0.50 1 calc PR . . C125 C 0.582(3) 0.740(2) 0.2103(18) 0.146(19) Uiso 0.50 1 d PD . . H12N H 0.6408 0.7388 0.2273 0.175 Uiso 0.50 1 calc PR . . H12O H 0.5665 0.6956 0.1876 0.175 Uiso 0.50 1 calc PR . . C126 C 0.537(2) 0.7488(18) 0.2674(15) 0.094(11) Uiso 0.50 1 d PD . . H12P H 0.5754 0.7622 0.3075 0.141 Uiso 0.50 1 calc PR . . H12Q H 0.5110 0.7056 0.2756 0.141 Uiso 0.50 1 calc PR . . H12R H 0.4966 0.7844 0.2568 0.141 Uiso 0.50 1 calc PR . . C127 C 0.589(3) 0.781(3) 0.1006(17) 0.18(2) Uiso 0.50 1 d PD . . H12S H 0.5771 0.7323 0.0875 0.212 Uiso 0.50 1 calc PR . . H12T H 0.6475 0.7886 0.1038 0.212 Uiso 0.50 1 calc PR . . C128 C 0.544(4) 0.826(3) 0.0483(17) 0.19(3) Uiso 0.50 1 d PD . . H12U H 0.4903 0.8355 0.0586 0.288 Uiso 0.50 1 calc PR . . H12V H 0.5395 0.8038 0.0045 0.288 Uiso 0.50 1 calc PR . . H12W H 0.5740 0.8695 0.0477 0.288 Uiso 0.50 1 calc PR . . C129 C 0.077(3) -0.295(2) 0.2147(18) 0.153(18) Uiso 0.50 1 d PDU . . H10 H 0.1354 -0.3002 0.2306 0.184 Uiso 0.50 1 calc PR . . H14 H 0.0513 -0.3410 0.2157 0.184 Uiso 0.50 1 calc PR . . C130 C 0.042(3) -0.248(2) 0.2602(18) 0.137(17) Uiso 0.50 1 d PDU . . H13D H 0.0453 -0.2006 0.2446 0.205 Uiso 0.50 1 calc PR . . H13E H 0.0719 -0.2513 0.3056 0.205 Uiso 0.50 1 calc PR . . H13F H -0.0150 -0.2597 0.2602 0.205 Uiso 0.50 1 calc PR . . C131 C 0.089(3) -0.315(3) 0.100(2) 0.26(3) Uiso 0.50 1 d PDU . . H13G H 0.0990 -0.3614 0.1198 0.307 Uiso 0.50 1 calc PR . . H13H H 0.1408 -0.2981 0.0887 0.307 Uiso 0.50 1 calc PR . . C132 C 0.027(4) -0.320(3) 0.039(2) 0.21(3) Uiso 0.50 1 d PDU . . H13I H -0.0267 -0.3244 0.0514 0.312 Uiso 0.50 1 calc PR . . H13J H 0.0377 -0.3596 0.0121 0.312 Uiso 0.50 1 calc PR . . H13K H 0.0290 -0.2781 0.0125 0.312 Uiso 0.50 1 calc PR . . 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 Tm1 0.0313(3) 0.0225(2) 0.0430(3) -0.0009(2) 0.0203(2) -0.00159(19) Ga1 0.0307(6) 0.0260(6) 0.0439(7) 0.0000(5) 0.0152(6) 0.0014(5) N1 0.033(5) 0.040(5) 0.049(6) 0.006(5) 0.021(5) 0.008(4) C1 0.031(7) 0.059(8) 0.058(8) -0.011(7) 0.004(6) -0.016(6) Tm2 0.0330(3) 0.0222(2) 0.0453(3) 0.0044(2) 0.0233(2) 0.00436(19) Ga2 0.0320(6) 0.0256(6) 0.0442(7) 0.0000(5) 0.0169(6) 0.0007(5) N2 0.032(5) 0.024(5) 0.064(7) 0.001(4) 0.019(5) 0.002(4) C2 0.040(7) 0.057(8) 0.054(8) -0.018(6) 0.010(6) -0.016(6) N3 0.053(7) 0.031(5) 0.064(7) 0.013(5) 0.004(6) 0.002(5) C3 0.028(6) 0.033(6) 0.056(8) 0.007(5) 0.017(6) 0.001(5) N4 0.035(5) 0.029(5) 0.039(5) -0.005(4) 0.020(4) 0.000(4) C4 0.029(6) 0.026(6) 0.075(9) 0.000(6) 0.026(6) 0.004(5) N5 0.037(5) 0.031(5) 0.054(6) -0.007(4) 0.014(5) -0.007(4) C5 0.060(8) 0.050(8) 0.068(9) -0.006(7) 0.046(7) -0.004(7) N6 0.042(6) 0.044(6) 0.092(9) -0.018(6) 0.033(6) -0.002(5) C6 0.072(10) 0.035(8) 0.136(16) 0.025(9) 0.055(11) 0.029(7) N7 0.029(5) 0.034(5) 0.047(6) -0.001(4) 0.018(4) 0.002(4) C7 0.074(11) 0.066(10) 0.139(17) 0.059(11) 0.060(11) 0.045(9) N8 0.024(5) 0.032(5) 0.043(5) 0.003(4) 0.006(4) 0.008(4) C8 0.055(9) 0.060(9) 0.089(11) 0.034(8) 0.038(8) 0.028(7) N9 0.032(5) 0.017(4) 0.048(6) 0.013(4) 0.020(4) 0.005(4) C9 0.033(6) 0.047(7) 0.048(7) 0.004(6) 0.016(6) -0.006(5) N10 0.051(6) 0.036(5) 0.048(6) 0.004(5) 0.015(5) -0.004(5) C10 0.057(8) 0.042(7) 0.064(9) 0.017(6) -0.004(7) -0.010(6) N11 0.032(5) 0.037(5) 0.039(5) 0.003(4) 0.016(4) 0.001(4) C11 0.050(8) 0.086(11) 0.068(10) -0.002(8) 0.020(8) -0.018(8) N12 0.033(6) 0.053(7) 0.075(8) 0.020(6) 0.025(5) 0.011(5) C12 0.085(7) 0.096(8) 0.086(7) 0.020(6) 0.020(6) 0.013(6) C13 0.131(18) 0.121(17) 0.091(14) 0.019(12) 0.033(13) -0.056(14) C14 0.187(14) 0.191(14) 0.185(14) 0.007(5) 0.031(5) -0.005(5) C15 0.040(6) 0.042(6) 0.025(6) -0.001(5) 0.009(5) -0.002(5) C16 0.033(6) 0.030(6) 0.054(7) -0.002(5) 0.021(6) -0.001(5) C17 0.046(7) 0.050(8) 0.061(9) 0.005(6) 0.029(7) 0.005(6) C18 0.065(10) 0.077(10) 0.057(9) -0.003(8) 0.024(8) 0.018(8) C19 0.094(11) 0.066(9) 0.034(7) 0.002(7) 0.027(7) 0.017(8) C20 0.072(10) 0.052(8) 0.058(9) 0.001(7) 0.021(8) 0.011(7) C21 0.049(8) 0.070(9) 0.062(9) 0.027(7) 0.035(7) 0.014(7) C22 0.085(7) 0.097(8) 0.092(8) 0.021(6) 0.017(6) -0.005(6) C23 0.048(7) 0.046(7) 0.041(7) 0.002(6) 0.016(6) 0.008(6) C24 0.158(19) 0.074(11) 0.055(10) 0.006(8) 0.053(12) 0.037(12) C25 0.094(8) 0.101(8) 0.093(8) 0.011(6) 0.020(6) 0.016(6) C26 0.101(8) 0.087(8) 0.082(7) 0.007(6) 0.009(6) 0.001(6) C27 0.046(7) 0.021(6) 0.067(9) -0.010(6) 0.025(6) 0.002(5) C28 0.028(6) 0.026(5) 0.058(8) -0.007(5) 0.026(6) 0.000(4) C29 0.062(8) 0.020(6) 0.058(8) 0.007(5) 0.015(7) 0.005(5) C30 0.053(8) 0.046(8) 0.069(9) 0.021(7) 0.024(7) -0.005(6) C31 0.062(9) 0.059(9) 0.067(10) 0.034(8) 0.014(8) 0.000(7) C32 0.132(16) 0.052(10) 0.066(11) 0.014(8) -0.027(11) -0.041(10) C33 0.142(18) 0.028(8) 0.115(16) 0.005(9) 0.000(13) -0.019(9) C34 0.106(13) 0.029(7) 0.072(10) 0.005(7) 0.000(9) -0.001(7) C35 0.124(15) 0.058(10) 0.067(10) 0.021(8) 0.053(10) 0.025(9) C36 0.178(13) 0.180(13) 0.182(13) -0.006(5) 0.028(5) 0.002(5) C37 0.150(11) 0.148(11) 0.151(11) -0.002(7) 0.040(7) 0.005(7) C38 0.093(7) 0.065(7) 0.082(7) 0.002(6) 0.008(6) 0.002(6) C39 0.118(9) 0.097(8) 0.104(8) 0.001(6) 0.020(6) 0.010(6) C40 0.121(9) 0.099(9) 0.108(9) 0.003(6) 0.010(6) -0.004(6) C41 0.031(6) 0.025(5) 0.054(7) -0.017(5) 0.027(5) -0.006(4) C42 0.043(7) 0.032(6) 0.043(7) -0.005(5) 0.030(6) 0.001(5) C43 0.050(8) 0.036(7) 0.067(9) 0.010(6) 0.023(7) -0.012(6) C44 0.052(8) 0.055(8) 0.048(8) -0.011(6) 0.033(6) -0.020(6) C45 0.043(7) 0.057(9) 0.068(9) -0.017(7) 0.036(7) -0.010(6) C46 0.031(6) 0.038(6) 0.048(7) -0.007(5) 0.024(6) 0.002(5) C47 0.066(8) 0.017(5) 0.043(7) 0.000(5) 0.023(6) -0.004(5) C48 0.071(9) 0.026(6) 0.058(8) -0.004(6) 0.020(7) -0.003(6) C49 0.061(8) 0.036(7) 0.055(8) 0.003(6) 0.022(7) 0.003(6) C50 0.041(7) 0.037(6) 0.059(8) -0.011(6) 0.026(6) 0.007(5) C51 0.040(7) 0.062(9) 0.089(11) -0.025(8) 0.016(7) 0.014(6) C52 0.045(8) 0.042(7) 0.087(11) -0.019(7) 0.022(7) -0.002(6) C53 0.049(8) 0.051(8) 0.060(9) -0.016(6) 0.029(7) -0.019(6) C54 0.045(8) 0.061(9) 0.085(11) 0.015(8) 0.014(8) -0.022(7) C55 0.041(8) 0.073(10) 0.065(9) -0.023(8) 0.010(7) 0.009(7) C56 0.041(8) 0.077(10) 0.099(12) -0.034(9) 0.030(8) 0.000(7) C57 0.084(11) 0.078(11) 0.057(9) -0.011(8) 0.042(8) -0.002(8) C58 0.072(10) 0.051(8) 0.052(8) -0.009(7) 0.015(7) 0.023(7) C59 0.026(6) 0.071(9) 0.059(8) 0.004(7) 0.021(6) -0.004(6) C60 0.048(8) 0.069(9) 0.051(8) 0.013(7) 0.013(7) 0.018(7) C61 0.032(6) 0.036(6) 0.074(9) -0.009(6) 0.026(6) -0.006(5) C62 0.063(9) 0.063(9) 0.093(12) -0.046(9) 0.036(9) -0.032(8) C63 0.063(10) 0.054(9) 0.155(18) -0.056(11) 0.051(11) -0.043(8) C64 0.075(11) 0.046(9) 0.146(17) -0.033(10) 0.076(12) -0.024(8) C65 0.054(8) 0.039(7) 0.083(10) 0.006(7) 0.041(8) 0.008(6) C66 0.038(7) 0.032(6) 0.055(8) -0.010(5) 0.027(6) 0.000(5) C67 0.086(7) 0.095(8) 0.097(8) -0.009(6) 0.021(6) -0.022(6) C68 0.16(2) 0.129(18) 0.105(16) -0.030(14) 0.040(15) 0.080(16) C69 0.110(9) 0.119(9) 0.114(9) -0.013(6) 0.026(6) 0.010(6) C70 0.037(7) 0.051(7) 0.047(7) 0.006(6) 0.023(6) 0.013(5) C71 0.053(8) 0.038(7) 0.072(10) -0.018(7) 0.008(7) -0.003(6) C72 0.063(9) 0.076(10) 0.058(9) 0.010(7) 0.031(7) 0.022(8) C73 0.027(6) 0.045(7) 0.037(6) 0.004(5) 0.011(5) 0.006(5) C74 0.032(6) 0.041(7) 0.043(7) 0.004(5) 0.019(5) 0.003(5) C75 0.039(7) 0.040(7) 0.071(9) 0.000(6) 0.018(7) -0.002(5) C76 0.075(10) 0.065(9) 0.044(8) 0.008(7) 0.029(7) -0.009(8) C77 0.091(11) 0.065(9) 0.040(8) -0.006(7) 0.040(8) -0.011(8) C78 0.064(9) 0.052(8) 0.052(8) 0.001(6) 0.026(7) 0.002(7) C79 0.044(8) 0.076(10) 0.073(10) -0.029(8) 0.042(7) -0.018(7) C80 0.050(7) 0.040(7) 0.054(8) 0.009(6) 0.022(6) -0.002(6) C81 0.084(7) 0.092(8) 0.089(7) -0.016(6) 0.017(6) 0.005(6) C82 0.17(2) 0.073(12) 0.043(9) -0.014(8) 0.030(11) -0.028(12) C83 0.139(17) 0.070(11) 0.060(10) -0.004(8) 0.021(11) 0.024(11) C84 0.082(13) 0.119(16) 0.101(15) -0.055(13) 0.027(12) -0.033(12) C85 0.037(6) 0.027(6) 0.053(7) 0.009(5) 0.023(6) 0.000(5) C86 0.052(7) 0.027(6) 0.048(7) 0.006(5) 0.023(6) -0.002(5) C87 0.028(6) 0.029(6) 0.052(7) 0.006(5) 0.029(5) 0.002(4) C88 0.031(6) 0.039(6) 0.048(7) 0.013(5) 0.023(5) 0.008(5) C89 0.044(7) 0.051(8) 0.053(8) 0.021(6) 0.029(6) 0.010(6) C90 0.044(7) 0.057(8) 0.047(8) 0.007(6) 0.024(6) 0.019(6) C91 0.046(7) 0.038(7) 0.054(8) 0.000(6) 0.015(6) 0.018(5) C92 0.040(6) 0.027(5) 0.038(6) 0.001(5) 0.029(5) 0.005(5) C93 0.050(7) 0.030(6) 0.064(8) 0.017(6) 0.025(6) -0.008(5) C94 0.051(8) 0.052(8) 0.064(9) 0.022(7) 0.017(7) 0.003(6) C95 0.053(8) 0.056(8) 0.058(9) 0.017(7) 0.013(7) -0.012(6) C96 0.047(7) 0.026(6) 0.045(7) 0.002(5) 0.027(6) 0.008(5) C97 0.062(8) 0.028(6) 0.055(8) -0.002(5) 0.026(7) -0.001(6) C98 0.074(9) 0.029(6) 0.048(8) 0.008(5) 0.012(7) 0.003(6) C99 0.066(9) 0.023(6) 0.084(11) -0.018(6) 0.016(8) -0.002(6) C100 0.073(10) 0.042(8) 0.074(10) -0.019(7) 0.036(8) 0.003(7) C101 0.071(10) 0.061(10) 0.077(11) -0.013(8) 0.024(9) 0.009(8) C102 0.145(18) 0.057(11) 0.085(13) -0.019(10) 0.008(12) 0.038(11) C103 0.106(8) 0.070(7) 0.084(7) -0.003(6) 0.007(6) 0.010(6) C104 0.158(18) 0.022(7) 0.081(12) -0.009(7) 0.009(12) 0.009(9) C105 0.122(15) 0.048(9) 0.086(12) -0.012(8) 0.073(11) -0.010(9) C106 0.132(10) 0.128(10) 0.124(10) 0.000(6) 0.038(7) -0.002(6) C107 0.153(12) 0.150(12) 0.158(12) 0.017(7) 0.025(7) 0.000(7) C108 0.114(8) 0.091(8) 0.094(8) -0.006(6) 0.010(6) 0.010(6) C109 0.137(10) 0.105(9) 0.121(9) -0.006(6) 0.011(7) 0.012(6) C110 0.135(9) 0.108(9) 0.115(9) 0.004(6) 0.019(7) -0.009(6) C111 0.045(7) 0.042(7) 0.062(9) 0.009(6) 0.018(6) 0.019(6) C112 0.047(8) 0.054(8) 0.083(11) -0.015(8) -0.004(8) 0.031(7) C113 0.032(7) 0.071(9) 0.065(9) 0.025(7) 0.012(6) 0.005(6) C114 0.039(8) 0.078(10) 0.088(11) 0.026(9) 0.030(8) 0.018(7) C115 0.070(10) 0.052(8) 0.072(10) 0.010(7) 0.032(8) -0.020(7) C116 0.053(8) 0.067(9) 0.051(8) 0.003(7) 0.028(7) 0.007(7) _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 Tm1 N3 2.163(10) . ? Tm1 N4 2.171(8) . ? Tm1 N5 2.481(9) . ? Tm1 N6 2.512(10) . ? Tm1 C27 2.547(11) . ? Tm1 C28 2.563(10) . ? Tm1 Ga1 2.9742(16) . ? Ga1 N2 1.904(9) . ? Ga1 N1 1.911(9) . ? O1 C119 1.415(8) . ? O1 C118 1.419(8) . ? N1 C1 1.397(15) . ? N1 C3 1.426(14) . ? C1 C2 1.349(17) . ? Tm2 N10 2.143(9) . ? Tm2 N9 2.156(8) . ? Tm2 N11 2.482(9) . ? Tm2 N12 2.506(10) . ? Tm2 C86 2.570(11) . ? Tm2 C85 2.585(10) . ? Tm2 Ga2 2.9769(16) . ? Ga2 N7 1.899(8) . ? Ga2 N8 1.932(9) . ? O2 C123 1.417(8) . ? O2 C122 1.417(8) . ? N2 C2 1.378(14) . ? N2 C15 1.439(13) . ? O3 C125 1.414(8) . ? O3 C127 1.420(8) . ? N3 C29 1.406(14) . ? N3 C27 1.452(15) . ? C3 C4 1.394(17) . ? C3 C8 1.458(17) . ? O4 C129 1.414(8) . ? O4 C131 1.420(8) . ? N4 C28 1.409(14) . ? N4 C41 1.420(14) . ? C4 C5 1.421(16) . ? C4 C9 1.519(17) . ? N5 C53 1.467(15) . ? N5 C55 1.475(15) . ? N5 C54 1.475(15) . ? C5 C6 1.36(2) . ? N6 C56 1.491(16) . ? N6 C58 1.494(17) . ? N6 C57 1.507(18) . ? C6 C7 1.41(2) . ? N7 C59 1.391(16) . ? N7 C61 1.443(14) . ? C7 C8 1.34(2) . ? N8 C60 1.375(15) . ? N8 C73 1.435(14) . ? C8 C12 1.48(2) . ? N9 C85 1.408(14) . ? N9 C87 1.421(14) . ? C9 C11 1.511(18) . ? C9 C10 1.537(16) . ? N10 C86 1.429(15) . ? N10 C99 1.455(15) . ? N11 C111 1.478(15) . ? N11 C113 1.489(15) . ? N11 C112 1.491(15) . ? N12 C115 1.492(17) . ? N12 C114 1.493(15) . ? N12 C116 1.502(16) . ? C12 C13 1.491(8) . ? C12 C14 1.504(8) . ? C15 C16 1.403(16) . ? C15 C20 1.404(17) . ? C16 C17 1.393(15) . ? C16 C21 1.538(17) . ? C17 C18 1.369(18) . ? C18 C19 1.38(2) . ? C19 C20 1.384(18) . ? C20 C24 1.56(2) . ? C21 C22 1.50(2) . ? C21 C23 1.547(17) . ? C24 C25 1.54(3) . ? C24 C26 1.55(2) . ? C27 C28 1.344(16) . ? C29 C34 1.383(18) . ? C29 C30 1.424(18) . ? C30 C31 1.383(17) . ? C30 C35 1.51(2) . ? C31 C32 1.36(2) . ? C32 C33 1.40(2) . ? C33 C34 1.41(2) . ? C34 C38 1.49(2) . ? C35 C36 1.498(8) . ? C35 C37 1.499(8) . ? C38 C39 1.51(2) . ? C38 C40 1.54(2) . ? C41 C46 1.391(14) . ? C41 C42 1.400(15) . ? C42 C43 1.386(16) . ? C42 C47 1.526(14) . ? C43 C44 1.376(17) . ? C44 C45 1.385(18) . ? C45 C46 1.410(18) . ? C46 C50 1.509(16) . ? C47 C48 1.523(16) . ? C47 C49 1.536(17) . ? C50 C52 1.533(17) . ? C50 C51 1.568(16) . ? C55 C56 1.481(19) . ? C59 C60 1.370(17) . ? C61 C66 1.395(17) . ? C61 C62 1.403(17) . ? C62 C63 1.39(2) . ? C62 C67 1.54(2) . ? C63 C64 1.34(2) . ? C64 C65 1.36(2) . ? C65 C66 1.412(16) . ? C66 C70 1.510(17) . ? C67 C68 1.48(3) . ? C67 C69 1.58(3) . ? C70 C72 1.520(17) . ? C70 C71 1.549(16) . ? C73 C74 1.384(16) . ? C73 C78 1.394(16) . ? C74 C75 1.416(16) . ? C74 C79 1.528(16) . ? C75 C76 1.361(18) . ? C76 C77 1.371(19) . ? C77 C78 1.381(18) . ? C78 C82 1.53(2) . ? C79 C81 1.492(8) . ? C79 C80 1.503(7) . ? C82 C83 1.54(2) . ? C82 C84 1.56(3) . ? C85 C86 1.353(16) . ? C87 C92 1.403(14) . ? C87 C88 1.436(14) . ? C88 C89 1.361(17) . ? C88 C93 1.514(16) . ? C89 C90 1.368(18) . ? C90 C91 1.380(17) . ? C91 C92 1.400(15) . ? C92 C96 1.537(14) . ? C93 C94 1.529(17) . ? C93 C95 1.554(16) . ? C96 C97 1.506(17) . ? C96 C98 1.538(16) . ? C99 C100 1.35(2) . ? C99 C104 1.43(2) . ? C100 C101 1.405(18) . ? C100 C105 1.50(2) . ? C101 C102 1.35(2) . ? C102 C103 1.36(2) . ? C103 C104 1.41(2) . ? C104 C108 1.50(2) . ? C105 C107 1.493(8) . ? C105 C106 1.500(8) . ? C108 C110 1.52(3) . ? C108 C109 1.53(3) . ? C113 C114 1.479(19) . ? C117 C118 1.501(8) . ? C119 C120 1.493(8) . ? C121 C122 1.494(8) . ? C123 C124 1.499(8) . ? C125 C126 1.491(8) . ? C127 C128 1.496(8) . ? C129 C130 1.497(8) . ? C131 C132 1.497(8) . ? 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 N3 Tm1 N4 85.1(4) . . ? N3 Tm1 N5 92.2(4) . . ? N4 Tm1 N5 94.4(3) . . ? N3 Tm1 N6 128.3(4) . . ? N4 Tm1 N6 142.9(4) . . ? N5 Tm1 N6 71.4(3) . . ? N3 Tm1 C27 34.7(4) . . ? N4 Tm1 C27 61.1(4) . . ? N5 Tm1 C27 116.8(3) . . ? N6 Tm1 C27 156.0(4) . . ? N3 Tm1 C28 62.4(4) . . ? N4 Tm1 C28 33.3(4) . . ? N5 Tm1 C28 117.4(3) . . ? N6 Tm1 C28 167.5(3) . . ? C27 Tm1 C28 30.5(4) . . ? N3 Tm1 Ga1 109.6(3) . . ? N4 Tm1 Ga1 97.6(2) . . ? N5 Tm1 Ga1 155.9(2) . . ? N6 Tm1 Ga1 86.7(2) . . ? C27 Tm1 Ga1 87.3(3) . . ? C28 Tm1 Ga1 82.9(2) . . ? N2 Ga1 N1 84.8(4) . . ? N2 Ga1 Tm1 141.0(3) . . ? N1 Ga1 Tm1 134.2(3) . . ? C119 O1 C118 111.9(19) . . ? C1 N1 C3 116.5(9) . . ? C1 N1 Ga1 111.8(7) . . ? C3 N1 Ga1 130.9(8) . . ? C2 C1 N1 114.5(10) . . ? N10 Tm2 N9 83.7(3) . . ? N10 Tm2 N11 92.8(3) . . ? N9 Tm2 N11 94.9(3) . . ? N10 Tm2 N12 128.7(4) . . ? N9 Tm2 N12 144.2(4) . . ? N11 Tm2 N12 71.6(3) . . ? N10 Tm2 C86 33.8(4) . . ? N9 Tm2 C86 60.8(3) . . ? N11 Tm2 C86 117.3(3) . . ? N12 Tm2 C86 154.8(4) . . ? N10 Tm2 C85 61.2(4) . . ? N9 Tm2 C85 33.0(3) . . ? N11 Tm2 C85 117.6(3) . . ? N12 Tm2 C85 167.8(3) . . ? C86 Tm2 C85 30.4(3) . . ? N10 Tm2 Ga2 109.5(3) . . ? N9 Tm2 Ga2 97.3(2) . . ? N11 Tm2 Ga2 155.6(2) . . ? N12 Tm2 Ga2 86.3(2) . . ? C86 Tm2 Ga2 87.1(3) . . ? C85 Tm2 Ga2 83.0(2) . . ? N7 Ga2 N8 84.9(4) . . ? N7 Ga2 Tm2 133.3(3) . . ? N8 Ga2 Tm2 141.8(3) . . ? C123 O2 C122 123(2) . . ? C2 N2 C15 117.7(9) . . ? C2 N2 Ga1 110.9(7) . . ? C15 N2 Ga1 130.9(7) . . ? C1 C2 N2 117.9(11) . . ? C125 O3 C127 115.1(10) . . ? C29 N3 C27 119.3(10) . . ? C29 N3 Tm1 152.3(9) . . ? C27 N3 Tm1 87.3(6) . . ? C4 C3 N1 120.1(10) . . ? C4 C3 C8 120.8(11) . . ? N1 C3 C8 119.1(11) . . ? C129 O4 C131 115.2(11) . . ? C28 N4 C41 118.5(8) . . ? C28 N4 Tm1 88.8(6) . . ? C41 N4 Tm1 148.6(7) . . ? C3 C4 C5 117.0(11) . . ? C3 C4 C9 121.7(10) . . ? C5 C4 C9 121.3(12) . . ? C53 N5 C55 108.9(10) . . ? C53 N5 C54 107.4(10) . . ? C55 N5 C54 108.7(11) . . ? C53 N5 Tm1 111.1(7) . . ? C55 N5 Tm1 112.0(7) . . ? C54 N5 Tm1 108.6(8) . . ? C6 C5 C4 122.2(13) . . ? C56 N6 C58 112.9(12) . . ? C56 N6 C57 106.9(11) . . ? C58 N6 C57 107.0(10) . . ? C56 N6 Tm1 108.0(7) . . ? C58 N6 Tm1 109.3(7) . . ? C57 N6 Tm1 112.7(8) . . ? C5 C6 C7 119.8(13) . . ? C59 N7 C61 115.3(9) . . ? C59 N7 Ga2 111.8(7) . . ? C61 N7 Ga2 132.0(8) . . ? C8 C7 C6 121.6(14) . . ? C60 N8 C73 118.6(9) . . ? C60 N8 Ga2 111.0(8) . . ? C73 N8 Ga2 130.2(7) . . ? C7 C8 C3 118.6(14) . . ? C7 C8 C12 120.6(14) . . ? C3 C8 C12 120.4(12) . . ? C85 N9 C87 116.8(8) . . ? C85 N9 Tm2 90.5(6) . . ? C87 N9 Tm2 149.0(7) . . ? C11 C9 C4 115.8(11) . . ? C11 C9 C10 109.5(11) . . ? C4 C9 C10 110.6(10) . . ? C86 N10 C99 119.5(10) . . ? C86 N10 Tm2 89.7(6) . . ? C99 N10 Tm2 148.7(8) . . ? C111 N11 C113 109.4(10) . . ? C111 N11 C112 105.9(9) . . ? C113 N11 C112 110.2(10) . . ? C111 N11 Tm2 111.8(6) . . ? C113 N11 Tm2 111.6(7) . . ? C112 N11 Tm2 107.7(7) . . ? C115 N12 C114 111.1(11) . . ? C115 N12 C116 107.7(10) . . ? C114 N12 C116 107.7(10) . . ? C115 N12 Tm2 108.6(7) . . ? C114 N12 Tm2 108.0(8) . . ? C116 N12 Tm2 113.8(7) . . ? C8 C12 C13 114.8(15) . . ? C8 C12 C14 110.5(19) . . ? C13 C12 C14 100.5(17) . . ? C16 C15 C20 119.0(10) . . ? C16 C15 N2 120.7(9) . . ? C20 C15 N2 120.2(11) . . ? C17 C16 C15 120.0(11) . . ? C17 C16 C21 120.3(11) . . ? C15 C16 C21 119.7(10) . . ? C18 C17 C16 121.5(13) . . ? C17 C18 C19 117.8(13) . . ? C18 C19 C20 123.4(13) . . ? C19 C20 C15 118.3(13) . . ? C19 C20 C24 121.2(13) . . ? C15 C20 C24 120.5(12) . . ? C22 C21 C16 112.2(13) . . ? C22 C21 C23 110.5(12) . . ? C16 C21 C23 114.2(10) . . ? C25 C24 C26 110.2(14) . . ? C25 C24 C20 110.7(15) . . ? C26 C24 C20 110.6(15) . . ? C28 C27 N3 124.3(11) . . ? C28 C27 Tm1 75.4(6) . . ? N3 C27 Tm1 58.0(5) . . ? C27 C28 N4 122.9(10) . . ? C27 C28 Tm1 74.1(6) . . ? N4 C28 Tm1 57.9(5) . . ? C34 C29 N3 120.8(12) . . ? C34 C29 C30 119.4(12) . . ? N3 C29 C30 119.7(11) . . ? C31 C30 C29 119.0(13) . . ? C31 C30 C35 120.2(14) . . ? C29 C30 C35 120.8(11) . . ? C32 C31 C30 122.2(15) . . ? C31 C32 C33 119.0(14) . . ? C32 C33 C34 120.6(15) . . ? C29 C34 C33 119.6(15) . . ? C29 C34 C38 121.8(13) . . ? C33 C34 C38 118.7(14) . . ? C36 C35 C37 105.8(19) . . ? C36 C35 C30 112.5(17) . . ? C37 C35 C30 111.4(16) . . ? C34 C38 C39 109.7(16) . . ? C34 C38 C40 112.1(16) . . ? C39 C38 C40 114.4(16) . . ? C46 C41 C42 119.6(11) . . ? C46 C41 N4 120.0(10) . . ? C42 C41 N4 120.4(9) . . ? C43 C42 C41 119.2(10) . . ? C43 C42 C47 117.8(10) . . ? C41 C42 C47 123.0(10) . . ? C44 C43 C42 122.9(12) . . ? C43 C44 C45 117.2(11) . . ? C44 C45 C46 122.1(11) . . ? C41 C46 C45 118.7(11) . . ? C41 C46 C50 124.5(10) . . ? C45 C46 C50 116.5(10) . . ? C48 C47 C42 110.8(10) . . ? C48 C47 C49 109.9(9) . . ? C42 C47 C49 113.3(10) . . ? C46 C50 C52 110.3(11) . . ? C46 C50 C51 112.6(10) . . ? C52 C50 C51 110.9(9) . . ? N5 C55 C56 111.6(11) . . ? C55 C56 N6 112.2(12) . . ? C60 C59 N7 115.8(10) . . ? C59 C60 N8 116.4(12) . . ? C66 C61 C62 120.6(11) . . ? C66 C61 N7 119.6(10) . . ? C62 C61 N7 119.8(12) . . ? C63 C62 C61 117.4(14) . . ? C63 C62 C67 120.1(13) . . ? C61 C62 C67 122.4(13) . . ? C64 C63 C62 123.2(14) . . ? C63 C64 C65 119.3(13) . . ? C64 C65 C66 121.5(14) . . ? C61 C66 C65 117.6(11) . . ? C61 C66 C70 121.8(10) . . ? C65 C66 C70 120.6(11) . . ? C68 C67 C62 111.6(16) . . ? C68 C67 C69 108.7(16) . . ? C62 C67 C69 108.4(16) . . ? C66 C70 C72 116.2(11) . . ? C66 C70 C71 110.7(10) . . ? C72 C70 C71 109.5(10) . . ? C74 C73 C78 119.8(11) . . ? C74 C73 N8 120.2(10) . . ? C78 C73 N8 120.0(11) . . ? C73 C74 C75 118.8(11) . . ? C73 C74 C79 121.6(10) . . ? C75 C74 C79 119.6(11) . . ? C76 C75 C74 121.2(12) . . ? C75 C76 C77 118.9(12) . . ? C76 C77 C78 122.0(12) . . ? C77 C78 C73 119.3(12) . . ? C77 C78 C82 120.7(12) . . ? C73 C78 C82 120.0(12) . . ? C81 C79 C80 111.6(11) . . ? C81 C79 C74 112.0(12) . . ? C80 C79 C74 115.6(9) . . ? C78 C82 C83 112.5(16) . . ? C78 C82 C84 109.5(15) . . ? C83 C82 C84 109.5(13) . . ? C86 C85 N9 122.3(10) . . ? C86 C85 Tm2 74.1(6) . . ? N9 C85 Tm2 56.5(5) . . ? C85 C86 N10 122.2(11) . . ? C85 C86 Tm2 75.4(7) . . ? N10 C86 Tm2 56.5(5) . . ? C92 C87 N9 120.0(9) . . ? C92 C87 C88 117.5(10) . . ? N9 C87 C88 122.5(9) . . ? C89 C88 C87 119.2(11) . . ? C89 C88 C93 118.6(10) . . ? C87 C88 C93 122.0(10) . . ? C88 C89 C90 123.5(11) . . ? C89 C90 C91 118.2(11) . . ? C90 C91 C92 121.1(12) . . ? C91 C92 C87 120.1(10) . . ? C91 C92 C96 117.5(10) . . ? C87 C92 C96 122.4(9) . . ? C88 C93 C94 111.3(11) . . ? C88 C93 C95 112.2(10) . . ? C94 C93 C95 111.3(10) . . ? C97 C96 C92 113.2(10) . . ? C97 C96 C98 109.8(9) . . ? C92 C96 C98 110.1(9) . . ? C100 C99 C104 122.6(12) . . ? C100 C99 N10 122.3(12) . . ? C104 C99 N10 114.9(13) . . ? C99 C100 C101 118.3(14) . . ? C99 C100 C105 120.3(11) . . ? C101 C100 C105 121.3(14) . . ? C102 C101 C100 122.7(16) . . ? C101 C102 C103 117.2(16) . . ? C102 C103 C104 125.1(18) . . ? C103 C104 C99 113.7(16) . . ? C103 C104 C108 121.0(16) . . ? C99 C104 C108 125.3(14) . . ? C107 C105 C106 109.0(18) . . ? C107 C105 C100 110.0(16) . . ? C106 C105 C100 115.1(14) . . ? C104 C108 C110 109.4(18) . . ? C104 C108 C109 112.2(18) . . ? C110 C108 C109 113.9(19) . . ? C114 C113 N11 111.3(11) . . ? C113 C114 N12 112.2(11) . . ? O1 C118 C117 113(3) . . ? O1 C119 C120 111(2) . . ? O2 C122 C121 115(2) . . ? O2 C123 C124 122(2) . . ? O3 C125 C126 111.5(10) . . ? O3 C127 C128 111.1(10) . . ? O4 C129 C130 110.9(10) . . ? O4 C131 C132 110.8(10) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 2.823 _refine_diff_density_min -2.971 _refine_diff_density_rms 0.175