Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Phalguni Chaudhuri' _publ_contact_author_address ; Max-Planck-Institut-Fur Bioanorganische Chemie Postfach 10 13 65 Mulheim an der Ruhr D-45413 GERMANY ; _publ_contact_author_email CHAUDH@MPI-MUELHEIM.MPG.DE _publ_section_title ; Effect of the Substituents on the Spin Coupling Between Iminosemiquinone ?-Radicals Mediated by Diamagnetic Metal Ions: l.s. Co(III) vs Ga(III). ; loop_ _publ_author_name 'Phalguni Chaudhuri' 'Biplab Biswas' 'Ulrich Pieper' 'Rita Wagner' 'Thomas Weyhermuller' data_2 _database_code_depnum_ccdc_archive 'CCDC 665848' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H92 Co N3 O9.50' _chemical_formula_weight 1162.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 12.9603(6) _cell_length_b 22.0793(12) _cell_length_c 22.8771(12) _cell_angle_alpha 90.00 _cell_angle_beta 95.07(1) _cell_angle_gamma 90.00 _cell_volume 6520.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 123864 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.88 _exptl_crystal_description 'opaque block' _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.184 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2496 _exptl_absorpt_coefficient_mu 0.320 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method '929 images at 1 deg in \w and 6 sec.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 108636 _diffrn_reflns_av_R_equivalents 0.0443 _diffrn_reflns_av_sigmaI/netI 0.0277 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 27.86 _reflns_number_total 15482 _reflns_number_gt 12943 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO, Nonius Collect Software' _computing_cell_refinement 'DENZO, Nonius Collect Software' _computing_data_reduction 'DENZO, Nonius Collect Software' _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0341P)^2^+4.0936P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15482 _refine_ls_number_parameters 745 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0478 _refine_ls_R_factor_gt 0.0363 _refine_ls_wR_factor_ref 0.0899 _refine_ls_wR_factor_gt 0.0840 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.066960(13) 0.237772(8) 0.794620(8) 0.01201(5) Uani 1 d . . . O1 O -0.03971(7) 0.29730(4) 0.79070(4) 0.01479(19) Uani 1 d . . . C2 C -0.11536(10) 0.28261(6) 0.75186(6) 0.0144(3) Uani 1 d . . . C3 C -0.09253(10) 0.23823(6) 0.70865(6) 0.0144(2) Uani 1 d . . . C4 C -0.16568(10) 0.22496(6) 0.66019(6) 0.0165(3) Uani 1 d . . . H4 H -0.1479 0.1983 0.6301 0.020 Uiso 1 calc R . . C5 C -0.26198(10) 0.25109(6) 0.65738(6) 0.0172(3) Uani 1 d . . . C6 C -0.28666(10) 0.29037(6) 0.70413(6) 0.0184(3) Uani 1 d . . . H6 H -0.3551 0.3061 0.7028 0.022 Uiso 1 calc R . . C7 C -0.21754(10) 0.30692(6) 0.75100(6) 0.0155(3) Uani 1 d . . . N8 N 0.00162(8) 0.21314(5) 0.71955(5) 0.0142(2) Uani 1 d . . . C9 C 0.03566(10) 0.16641(6) 0.68292(6) 0.0159(3) Uani 1 d . . . C10 C -0.00636(11) 0.10847(6) 0.68604(6) 0.0182(3) Uani 1 d . . . H10 H -0.0582 0.1001 0.7118 0.022 Uiso 1 calc R . . C11 C 0.02963(11) 0.06309(7) 0.65044(7) 0.0215(3) Uani 1 d . . . C12 C 0.10447(12) 0.07614(7) 0.61236(7) 0.0243(3) Uani 1 d . . . H12 H 0.1283 0.0452 0.5880 0.029 Uiso 1 calc R . . C13 C 0.14453(11) 0.13435(7) 0.60991(7) 0.0230(3) Uani 1 d . . . C14 C 0.11211(11) 0.18019(7) 0.64598(6) 0.0190(3) Uani 1 d . . . H14 H 0.1413 0.2196 0.6454 0.023 Uiso 1 calc R . . O15 O -0.00575(9) 0.00465(5) 0.64958(5) 0.0282(2) Uani 1 d . . . C16 C -0.06318(13) -0.01377(7) 0.69709(8) 0.0297(4) Uani 1 d . . . H16A H -0.0842 -0.0562 0.6917 0.045 Uiso 1 calc R . . H16B H -0.1249 0.0117 0.6980 0.045 Uiso 1 calc R . . H16C H -0.0198 -0.0095 0.7342 0.045 Uiso 1 calc R . . O17 O 0.21756(9) 0.14239(6) 0.57069(5) 0.0320(3) Uani 1 d . . . C18 C 0.26903(13) 0.19952(8) 0.57103(8) 0.0335(4) Uani 1 d . . . H18A H 0.3189 0.1995 0.5413 0.050 Uiso 1 calc R . . H18B H 0.3056 0.2066 0.6098 0.050 Uiso 1 calc R . . H18C H 0.2180 0.2317 0.5623 0.050 Uiso 1 calc R . . C19 C -0.24794(10) 0.34570(6) 0.80250(6) 0.0173(3) Uani 1 d . . . C20 C -0.36041(11) 0.36796(7) 0.79250(7) 0.0233(3) Uani 1 d . . . H20A H -0.3772 0.3925 0.8261 0.035 Uiso 1 calc R . . H20B H -0.4072 0.3330 0.7883 0.035 Uiso 1 calc R . . H20C H -0.3686 0.3926 0.7567 0.035 Uiso 1 calc R . . C21 C -0.23837(11) 0.30610(7) 0.85834(6) 0.0210(3) Uani 1 d . . . H21A H -0.2575 0.3301 0.8918 0.031 Uiso 1 calc R . . H21B H -0.1668 0.2920 0.8660 0.031 Uiso 1 calc R . . H21C H -0.2848 0.2712 0.8527 0.031 Uiso 1 calc R . . C22 C -0.17751(11) 0.40171(6) 0.81247(7) 0.0209(3) Uani 1 d . . . H22A H -0.1992 0.4253 0.8456 0.031 Uiso 1 calc R . . H22B H -0.1830 0.4269 0.7770 0.031 Uiso 1 calc R . . H22C H -0.1055 0.3886 0.8211 0.031 Uiso 1 calc R . . C23 C -0.34641(11) 0.23667(7) 0.60781(7) 0.0222(3) Uani 1 d . . . C24 C -0.43177(13) 0.19872(8) 0.63430(8) 0.0325(4) Uani 1 d . . . H24A H -0.4598 0.2216 0.6660 0.049 Uiso 1 calc R . . H24B H -0.4019 0.1606 0.6499 0.049 Uiso 1 calc R . . H24C H -0.4875 0.1899 0.6037 0.049 Uiso 1 calc R . . C25 C -0.30518(13) 0.19950(9) 0.55869(8) 0.0332(4) Uani 1 d . . . H25A H -0.2742 0.1620 0.5750 0.050 Uiso 1 calc R . . H25B H -0.2526 0.2230 0.5403 0.050 Uiso 1 calc R . . H25C H -0.3623 0.1897 0.5292 0.050 Uiso 1 calc R . . C26 C -0.39468(14) 0.29495(8) 0.58180(8) 0.0358(4) Uani 1 d . . . H26A H -0.4213 0.3192 0.6131 0.054 Uiso 1 calc R . . H26B H -0.4517 0.2848 0.5524 0.054 Uiso 1 calc R . . H26C H -0.3421 0.3182 0.5632 0.054 Uiso 1 calc R . . O31 O 0.16153(7) 0.28727(4) 0.75825(4) 0.01484(19) Uani 1 d . . . C32 C 0.20660(10) 0.32741(6) 0.79374(6) 0.0143(3) Uani 1 d . . . C33 C 0.18254(10) 0.32560(6) 0.85401(6) 0.0147(3) Uani 1 d . . . C34 C 0.22677(10) 0.36858(6) 0.89530(6) 0.0172(3) Uani 1 d . . . H34 H 0.2099 0.3675 0.9349 0.021 Uiso 1 calc R . . C35 C 0.29428(11) 0.41170(6) 0.87755(6) 0.0183(3) Uani 1 d . . . C36 C 0.31997(11) 0.41100(6) 0.81801(6) 0.0187(3) Uani 1 d . . . H36 H 0.3683 0.4402 0.8067 0.022 Uiso 1 calc R . . C37 C 0.27943(10) 0.37083(6) 0.77578(6) 0.0158(3) Uani 1 d . . . N38 N 0.12183(8) 0.27826(5) 0.86543(5) 0.0139(2) Uani 1 d . . . C39 C 0.08253(10) 0.27005(6) 0.92068(6) 0.0151(3) Uani 1 d . . . C40 C 0.09947(11) 0.21449(6) 0.94865(6) 0.0172(3) Uani 1 d . . . H40 H 0.1402 0.1842 0.9323 0.021 Uiso 1 calc R . . C41 C 0.05522(11) 0.20434(6) 1.00121(6) 0.0199(3) Uani 1 d . . . C42 C -0.00336(12) 0.24882(7) 1.02566(6) 0.0225(3) Uani 1 d . . . H42 H -0.0333 0.2414 1.0614 0.027 Uiso 1 calc R . . C43 C -0.01789(11) 0.30422(7) 0.99746(6) 0.0207(3) Uani 1 d . . . C44 C 0.02389(11) 0.31551(6) 0.94439(6) 0.0181(3) Uani 1 d . . . H44 H 0.0127 0.3532 0.9248 0.022 Uiso 1 calc R . . O45 O 0.06649(9) 0.15151(5) 1.03251(5) 0.0277(2) Uani 1 d . . . C46 C 0.12320(15) 0.10420(7) 1.00800(7) 0.0308(4) Uani 1 d . . . H46A H 0.1259 0.0690 1.0342 0.046 Uiso 1 calc R . . H46B H 0.1938 0.1181 1.0033 0.046 Uiso 1 calc R . . H46C H 0.0891 0.0928 0.9696 0.046 Uiso 1 calc R . . O47 O -0.07585(9) 0.34537(5) 1.02520(5) 0.0281(2) Uani 1 d . . . C48 C -0.08953(15) 0.40378(8) 0.99935(8) 0.0352(4) Uani 1 d . . . H48A H -0.1322 0.4287 1.0232 0.053 Uiso 1 calc R . . H48B H -0.1240 0.3998 0.9597 0.053 Uiso 1 calc R . . H48C H -0.0218 0.4231 0.9974 0.053 Uiso 1 calc R . . C49 C 0.30945(11) 0.37091(7) 0.71251(6) 0.0190(3) Uani 1 d . . . C50 C 0.36320(12) 0.31068(7) 0.70009(7) 0.0242(3) Uani 1 d . . . H50A H 0.3825 0.3106 0.6596 0.036 Uiso 1 calc R . . H50B H 0.3157 0.2770 0.7055 0.036 Uiso 1 calc R . . H50C H 0.4255 0.3061 0.7273 0.036 Uiso 1 calc R . . C51 C 0.21176(12) 0.37833(8) 0.66967(7) 0.0275(3) Uani 1 d . . . H51A H 0.2314 0.3784 0.6293 0.041 Uiso 1 calc R . . H51B H 0.1776 0.4167 0.6776 0.041 Uiso 1 calc R . . H51C H 0.1642 0.3447 0.6749 0.041 Uiso 1 calc R . . C52 C 0.38428(12) 0.42296(7) 0.70162(7) 0.0250(3) Uani 1 d . . . H52A H 0.4018 0.4216 0.6608 0.037 Uiso 1 calc R . . H52B H 0.4476 0.4187 0.7281 0.037 Uiso 1 calc R . . H52C H 0.3512 0.4618 0.7090 0.037 Uiso 1 calc R . . C53 C 0.34693(11) 0.45838(7) 0.91994(7) 0.0222(3) Uani 1 d . . . C54 C 0.34155(16) 0.52210(7) 0.89282(8) 0.0363(4) Uani 1 d . . . H54A H 0.3738 0.5217 0.8557 0.054 Uiso 1 calc R . . H54B H 0.3784 0.5507 0.9199 0.054 Uiso 1 calc R . . H54C H 0.2690 0.5345 0.8856 0.054 Uiso 1 calc R . . C55 C 0.29563(14) 0.46144(8) 0.97768(8) 0.0330(4) Uani 1 d . . . H55A H 0.3313 0.4916 1.0036 0.050 Uiso 1 calc R . . H55B H 0.3000 0.4217 0.9968 0.050 Uiso 1 calc R . . H55C H 0.2227 0.4730 0.9696 0.050 Uiso 1 calc R . . C56 C 0.46095(13) 0.43965(8) 0.93282(8) 0.0328(4) Uani 1 d . . . H56A H 0.4940 0.4376 0.8960 0.049 Uiso 1 calc R . . H56B H 0.4645 0.3998 0.9518 0.049 Uiso 1 calc R . . H56C H 0.4970 0.4696 0.9589 0.049 Uiso 1 calc R . . O61 O -0.02727(7) 0.18730(4) 0.82974(4) 0.01470(19) Uani 1 d . . . C62 C 0.00641(10) 0.13194(6) 0.83770(6) 0.0139(2) Uani 1 d . . . C63 C 0.11141(10) 0.12053(6) 0.82528(6) 0.0139(2) Uani 1 d . . . C64 C 0.15736(10) 0.06298(6) 0.83797(6) 0.0163(3) Uani 1 d . . . H64 H 0.2277 0.0561 0.8312 0.020 Uiso 1 calc R . . C65 C 0.10004(11) 0.01739(6) 0.85999(6) 0.0167(3) Uani 1 d . . . C66 C -0.00601(11) 0.02914(6) 0.86938(6) 0.0171(3) Uani 1 d . . . H66 H -0.0455 -0.0032 0.8834 0.020 Uiso 1 calc R . . C67 C -0.05458(10) 0.08446(6) 0.85932(6) 0.0156(3) Uani 1 d . . . N68 N 0.15836(8) 0.16945(5) 0.80428(5) 0.0142(2) Uani 1 d . . . C69 C 0.26515(10) 0.16672(6) 0.79384(6) 0.0156(3) Uani 1 d . . . C70 C 0.33479(10) 0.20217(6) 0.82860(6) 0.0178(3) Uani 1 d . . . H70 H 0.3116 0.2281 0.8579 0.021 Uiso 1 calc R . . C71 C 0.43957(11) 0.19874(7) 0.81936(7) 0.0218(3) Uani 1 d . . . C72 C 0.47386(11) 0.16072(7) 0.77691(7) 0.0247(3) Uani 1 d . . . H72 H 0.5454 0.1590 0.7709 0.030 Uiso 1 calc R . . C73 C 0.40296(11) 0.12515(7) 0.74321(7) 0.0222(3) Uani 1 d . . . C74 C 0.29716(11) 0.12814(6) 0.75055(6) 0.0184(3) Uani 1 d . . . H74 H 0.2485 0.1046 0.7268 0.022 Uiso 1 calc R . . O75 O 0.51558(8) 0.23125(5) 0.85120(5) 0.0301(3) Uani 1 d . . . C76 C 0.48327(13) 0.27279(8) 0.89358(8) 0.0327(4) Uani 1 d . . . H76A H 0.5441 0.2931 0.9132 0.049 Uiso 1 calc R . . H76B H 0.4466 0.2508 0.9227 0.049 Uiso 1 calc R . . H76C H 0.4369 0.3031 0.8740 0.049 Uiso 1 calc R . . O77 O 0.44490(8) 0.08792(5) 0.70347(5) 0.0310(3) Uani 1 d . . . C78 C 0.37632(14) 0.04807(9) 0.67029(9) 0.0400(4) Uani 1 d . . . H78A H 0.4153 0.0242 0.6436 0.060 Uiso 1 calc R . . H78B H 0.3229 0.0717 0.6475 0.060 Uiso 1 calc R . . H78C H 0.3435 0.0208 0.6969 0.060 Uiso 1 calc R . . C79 C 0.14769(11) -0.04441(6) 0.87706(6) 0.0191(3) Uani 1 d . . . C80 C 0.25756(12) -0.05108(7) 0.85739(7) 0.0240(3) Uani 1 d . . . H80A H 0.2854 -0.0910 0.8691 0.036 Uiso 1 calc R . . H80B H 0.3023 -0.0194 0.8759 0.036 Uiso 1 calc R . . H80C H 0.2550 -0.0471 0.8146 0.036 Uiso 1 calc R . . C81 C 0.15531(13) -0.05031(7) 0.94426(7) 0.0277(3) Uani 1 d . . . H81A H 0.1857 -0.0896 0.9558 0.042 Uiso 1 calc R . . H81B H 0.0859 -0.0473 0.9579 0.042 Uiso 1 calc R . . H81C H 0.1991 -0.0178 0.9619 0.042 Uiso 1 calc R . . C82 C 0.07999(12) -0.09614(6) 0.84971(7) 0.0241(3) Uani 1 d . . . H82A H 0.1117 -0.1352 0.8612 0.036 Uiso 1 calc R . . H82B H 0.0744 -0.0924 0.8069 0.036 Uiso 1 calc R . . H82C H 0.0108 -0.0938 0.8637 0.036 Uiso 1 calc R . . C83 C -0.16770(10) 0.09706(6) 0.87029(6) 0.0177(3) Uani 1 d . . . C84 C -0.22878(12) 0.11586(8) 0.81236(7) 0.0278(3) Uani 1 d . . . H84A H -0.3010 0.1239 0.8194 0.042 Uiso 1 calc R . . H84B H -0.2262 0.0831 0.7836 0.042 Uiso 1 calc R . . H84C H -0.1980 0.1525 0.7972 0.042 Uiso 1 calc R . . C85 C -0.17295(12) 0.14778(7) 0.91622(7) 0.0223(3) Uani 1 d . . . H85A H -0.2454 0.1554 0.9229 0.033 Uiso 1 calc R . . H85B H -0.1421 0.1848 0.9018 0.033 Uiso 1 calc R . . H85C H -0.1346 0.1353 0.9531 0.033 Uiso 1 calc R . . C86 C -0.22023(11) 0.04080(7) 0.89360(7) 0.0240(3) Uani 1 d . . . H86A H -0.2921 0.0505 0.9001 0.036 Uiso 1 calc R . . H86B H -0.1830 0.0281 0.9307 0.036 Uiso 1 calc R . . H86C H -0.2192 0.0079 0.8649 0.036 Uiso 1 calc R . . O90 O 0.5219(5) 0.0016(3) 0.9965(5) 0.0874(16) Uani 0.50 d PD . . C91 C 0.5004(7) -0.0434(4) 1.0338(5) 0.118(3) Uani 0.50 d PD . . H91A H 0.4296 -0.0585 1.0224 0.142 Uiso 0.50 calc PR . . H91B H 0.5008 -0.0263 1.0738 0.142 Uiso 0.50 calc PR . . C92 C 0.5732(8) -0.0953(4) 1.0355(6) 0.135(3) Uani 0.50 d PD . . H92A H 0.5506 -0.1264 1.0622 0.203 Uiso 0.50 calc PR . . H92B H 0.6429 -0.0815 1.0496 0.203 Uiso 0.50 calc PR . . H92C H 0.5743 -0.1124 0.9961 0.203 Uiso 0.50 calc PR . . C93 C 0.4613(8) 0.0527(4) 0.9951(5) 0.118(3) Uani 0.50 d PD . . H93A H 0.4689 0.0723 1.0342 0.142 Uiso 0.50 calc PR . . H93B H 0.3878 0.0409 0.9868 0.142 Uiso 0.50 calc PR . . C94 C 0.4889(8) 0.0966(4) 0.9503(6) 0.135(3) Uani 0.50 d PD . . H94A H 0.4423 0.1316 0.9501 0.203 Uiso 0.50 calc PR . . H94B H 0.4823 0.0773 0.9116 0.203 Uiso 0.50 calc PR . . H94C H 0.5606 0.1102 0.9596 0.203 Uiso 0.50 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 Co1 0.01042(8) 0.01262(8) 0.01303(9) 0.00034(7) 0.00129(6) 0.00005(6) O1 0.0129(4) 0.0146(4) 0.0168(5) -0.0001(4) 0.0008(4) 0.0005(3) C2 0.0144(6) 0.0143(6) 0.0144(6) 0.0029(5) 0.0016(5) -0.0012(5) C3 0.0131(6) 0.0151(6) 0.0154(6) 0.0027(5) 0.0030(5) -0.0001(5) C4 0.0162(6) 0.0185(6) 0.0151(7) -0.0006(5) 0.0023(5) -0.0012(5) C5 0.0156(6) 0.0186(7) 0.0173(7) 0.0010(5) -0.0002(5) -0.0010(5) C6 0.0133(6) 0.0199(7) 0.0219(7) 0.0010(6) 0.0019(5) 0.0022(5) C7 0.0137(6) 0.0149(6) 0.0183(7) 0.0005(5) 0.0030(5) 0.0006(5) N8 0.0136(5) 0.0156(5) 0.0136(5) -0.0009(4) 0.0017(4) 0.0005(4) C9 0.0148(6) 0.0198(7) 0.0125(6) -0.0015(5) -0.0014(5) 0.0040(5) C10 0.0167(6) 0.0204(7) 0.0173(7) -0.0017(5) 0.0007(5) 0.0013(5) C11 0.0217(7) 0.0204(7) 0.0214(7) -0.0033(6) -0.0032(6) 0.0025(6) C12 0.0252(7) 0.0267(8) 0.0209(7) -0.0086(6) 0.0006(6) 0.0067(6) C13 0.0196(7) 0.0326(8) 0.0172(7) -0.0016(6) 0.0042(6) 0.0048(6) C14 0.0169(6) 0.0226(7) 0.0175(7) 0.0003(5) 0.0018(5) 0.0020(5) O15 0.0324(6) 0.0198(5) 0.0326(6) -0.0079(5) 0.0025(5) -0.0002(4) C16 0.0275(8) 0.0210(7) 0.0405(10) -0.0034(7) 0.0026(7) -0.0041(6) O17 0.0305(6) 0.0407(7) 0.0270(6) -0.0072(5) 0.0150(5) 0.0005(5) C18 0.0264(8) 0.0443(10) 0.0319(9) 0.0023(8) 0.0140(7) 0.0022(7) C19 0.0130(6) 0.0189(6) 0.0199(7) -0.0022(5) 0.0016(5) 0.0017(5) C20 0.0160(7) 0.0272(8) 0.0269(8) -0.0049(6) 0.0031(6) 0.0049(6) C21 0.0179(7) 0.0244(7) 0.0211(7) -0.0008(6) 0.0045(6) -0.0003(6) C22 0.0196(7) 0.0190(7) 0.0240(8) -0.0034(6) 0.0024(6) 0.0017(5) C23 0.0160(7) 0.0279(8) 0.0219(7) -0.0039(6) -0.0031(5) 0.0016(6) C24 0.0225(8) 0.0371(9) 0.0378(10) -0.0066(8) 0.0018(7) -0.0060(7) C25 0.0236(8) 0.0479(10) 0.0269(9) -0.0095(8) -0.0043(7) 0.0015(7) C26 0.0347(9) 0.0358(9) 0.0340(10) 0.0004(7) -0.0122(8) 0.0025(7) O31 0.0135(4) 0.0168(4) 0.0144(5) 0.0007(4) 0.0022(4) -0.0006(4) C32 0.0121(6) 0.0134(6) 0.0173(7) 0.0016(5) 0.0008(5) 0.0016(5) C33 0.0119(6) 0.0145(6) 0.0177(7) 0.0019(5) 0.0014(5) 0.0011(5) C34 0.0158(6) 0.0188(6) 0.0169(7) -0.0004(5) 0.0015(5) -0.0008(5) C35 0.0165(6) 0.0166(6) 0.0217(7) -0.0011(5) 0.0001(5) -0.0019(5) C36 0.0141(6) 0.0175(6) 0.0247(7) 0.0038(5) 0.0027(5) -0.0026(5) C37 0.0120(6) 0.0168(6) 0.0185(7) 0.0045(5) 0.0015(5) 0.0013(5) N38 0.0128(5) 0.0144(5) 0.0147(5) 0.0002(4) 0.0011(4) -0.0005(4) C39 0.0137(6) 0.0184(6) 0.0129(6) -0.0014(5) 0.0006(5) -0.0036(5) C40 0.0192(7) 0.0170(6) 0.0152(7) -0.0016(5) 0.0008(5) -0.0025(5) C41 0.0239(7) 0.0199(7) 0.0155(7) 0.0012(5) -0.0002(6) -0.0059(6) C42 0.0230(7) 0.0297(8) 0.0153(7) -0.0019(6) 0.0050(6) -0.0060(6) C43 0.0168(7) 0.0262(7) 0.0193(7) -0.0057(6) 0.0034(5) -0.0023(6) C44 0.0163(6) 0.0196(7) 0.0184(7) -0.0008(5) 0.0010(5) -0.0010(5) O45 0.0442(7) 0.0222(5) 0.0174(5) 0.0043(4) 0.0064(5) -0.0023(5) C46 0.0474(10) 0.0221(8) 0.0224(8) 0.0044(6) 0.0013(7) 0.0016(7) O47 0.0271(6) 0.0326(6) 0.0262(6) -0.0058(5) 0.0105(5) 0.0042(5) C48 0.0396(10) 0.0349(9) 0.0316(9) -0.0063(7) 0.0054(8) 0.0152(8) C49 0.0164(6) 0.0242(7) 0.0163(7) 0.0056(5) 0.0011(5) -0.0024(5) C50 0.0226(7) 0.0295(8) 0.0216(7) -0.0003(6) 0.0073(6) -0.0005(6) C51 0.0241(8) 0.0345(9) 0.0227(8) 0.0124(7) -0.0043(6) -0.0060(6) C52 0.0207(7) 0.0316(8) 0.0228(8) 0.0086(6) 0.0026(6) -0.0056(6) C53 0.0213(7) 0.0208(7) 0.0247(8) -0.0044(6) 0.0036(6) -0.0074(6) C54 0.0490(11) 0.0207(8) 0.0389(10) -0.0049(7) 0.0026(8) -0.0102(7) C55 0.0360(9) 0.0326(9) 0.0321(9) -0.0143(7) 0.0121(7) -0.0152(7) C56 0.0244(8) 0.0378(9) 0.0354(10) -0.0123(7) -0.0016(7) -0.0057(7) O61 0.0124(4) 0.0151(4) 0.0169(5) 0.0011(4) 0.0025(4) 0.0002(3) C62 0.0147(6) 0.0153(6) 0.0114(6) -0.0012(5) -0.0006(5) 0.0003(5) C63 0.0134(6) 0.0150(6) 0.0132(6) -0.0008(5) 0.0000(5) -0.0009(5) C64 0.0147(6) 0.0176(6) 0.0164(7) -0.0008(5) 0.0011(5) 0.0018(5) C65 0.0190(7) 0.0162(6) 0.0147(6) -0.0016(5) -0.0002(5) 0.0012(5) C66 0.0184(7) 0.0159(6) 0.0170(7) -0.0003(5) 0.0023(5) -0.0032(5) C67 0.0146(6) 0.0185(6) 0.0134(6) -0.0016(5) 0.0008(5) -0.0014(5) N68 0.0119(5) 0.0158(5) 0.0149(5) 0.0008(4) 0.0015(4) 0.0005(4) C69 0.0124(6) 0.0155(6) 0.0190(7) 0.0047(5) 0.0022(5) 0.0023(5) C70 0.0144(6) 0.0193(7) 0.0197(7) 0.0013(5) 0.0016(5) 0.0013(5) C71 0.0143(6) 0.0234(7) 0.0271(8) 0.0019(6) -0.0013(6) -0.0007(5) C72 0.0128(6) 0.0300(8) 0.0319(9) 0.0022(7) 0.0052(6) 0.0037(6) C73 0.0196(7) 0.0240(7) 0.0238(8) 0.0014(6) 0.0069(6) 0.0051(6) C74 0.0155(6) 0.0192(7) 0.0207(7) 0.0005(5) 0.0023(5) 0.0014(5) O75 0.0131(5) 0.0366(6) 0.0400(7) -0.0091(5) -0.0017(5) -0.0027(4) C76 0.0204(8) 0.0392(10) 0.0378(10) -0.0106(8) -0.0017(7) -0.0046(7) O77 0.0209(5) 0.0363(6) 0.0372(7) -0.0109(5) 0.0112(5) 0.0044(5) C78 0.0302(9) 0.0440(11) 0.0468(11) -0.0212(9) 0.0090(8) 0.0063(8) C79 0.0219(7) 0.0151(6) 0.0202(7) 0.0023(5) 0.0024(6) 0.0022(5) C80 0.0226(7) 0.0188(7) 0.0308(8) 0.0019(6) 0.0039(6) 0.0059(6) C81 0.0343(9) 0.0257(8) 0.0231(8) 0.0060(6) 0.0025(7) 0.0066(7) C82 0.0258(8) 0.0165(7) 0.0305(8) -0.0020(6) 0.0049(6) 0.0010(6) C83 0.0139(6) 0.0185(7) 0.0211(7) 0.0010(5) 0.0033(5) -0.0018(5) C84 0.0155(7) 0.0382(9) 0.0290(9) 0.0066(7) -0.0020(6) -0.0022(6) C85 0.0218(7) 0.0196(7) 0.0269(8) 0.0006(6) 0.0105(6) 0.0000(6) C86 0.0186(7) 0.0212(7) 0.0332(9) 0.0000(6) 0.0071(6) -0.0044(6) O90 0.084(5) 0.066(2) 0.121(4) -0.017(2) 0.053(5) -0.017(4) C91 0.103(6) 0.126(5) 0.129(8) 0.068(5) 0.026(4) 0.011(4) C92 0.142(8) 0.085(3) 0.188(8) 0.020(4) 0.064(6) 0.006(5) C93 0.103(6) 0.126(5) 0.129(8) 0.068(5) 0.026(4) 0.011(4) C94 0.142(8) 0.085(3) 0.188(8) 0.020(4) 0.064(6) 0.006(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 Co1 O61 1.8848(9) . ? Co1 O31 1.8893(9) . ? Co1 O1 1.9039(9) . ? Co1 N68 1.9187(11) . ? Co1 N8 1.9249(11) . ? Co1 N38 1.9302(11) . ? O1 C2 1.3046(16) . ? C2 C7 1.4274(18) . ? C2 C3 1.4411(19) . ? C3 N8 1.3432(17) . ? C3 C4 1.4240(19) . ? C4 C5 1.3714(19) . ? C5 C6 1.435(2) . ? C5 C23 1.5380(19) . ? C6 C7 1.384(2) . ? C7 C19 1.5357(19) . ? N8 C9 1.4236(17) . ? C9 C14 1.3917(19) . ? C9 C10 1.395(2) . ? C10 C11 1.397(2) . ? C11 O15 1.3689(18) . ? C11 C12 1.390(2) . ? C12 C13 1.389(2) . ? C13 O17 1.3720(18) . ? C13 C14 1.394(2) . ? O15 C16 1.430(2) . ? O17 C18 1.427(2) . ? C19 C20 1.5361(19) . ? C19 C22 1.5420(19) . ? C19 C21 1.544(2) . ? C23 C25 1.526(2) . ? C23 C26 1.528(2) . ? C23 C24 1.553(2) . ? O31 C32 1.3047(16) . ? C32 C37 1.4308(18) . ? C32 C33 1.4408(19) . ? C33 N38 1.3477(17) . ? C33 C34 1.4231(19) . ? C34 C35 1.3782(19) . ? C35 C36 1.431(2) . ? C35 C53 1.5333(19) . ? C36 C37 1.381(2) . ? C37 C49 1.5316(19) . ? N38 C39 1.4154(17) . ? C39 C40 1.3921(19) . ? C39 C44 1.3972(19) . ? C40 C41 1.395(2) . ? C41 O45 1.3697(17) . ? C41 C42 1.389(2) . ? C42 C43 1.388(2) . ? C43 O47 1.3699(17) . ? C43 C44 1.395(2) . ? O45 C46 1.421(2) . ? O47 C48 1.423(2) . ? C49 C52 1.5381(19) . ? C49 C50 1.539(2) . ? C49 C51 1.540(2) . ? C53 C55 1.532(2) . ? C53 C54 1.537(2) . ? C53 C56 1.538(2) . ? O61 C62 1.3053(16) . ? C62 C67 1.4274(18) . ? C62 C63 1.4368(18) . ? C63 N68 1.3489(17) . ? C63 C64 1.4222(18) . ? C64 C65 1.3729(19) . ? C65 C66 1.4335(19) . ? C65 C79 1.5340(19) . ? C66 C67 1.3841(19) . ? C67 C83 1.5345(19) . ? N68 C69 1.4264(16) . ? C69 C70 1.3903(19) . ? C69 C74 1.3967(19) . ? C70 C71 1.3946(19) . ? C71 O75 1.3745(18) . ? C71 C72 1.386(2) . ? C72 C73 1.389(2) . ? C73 O77 1.3729(18) . ? C73 C74 1.3977(19) . ? O75 C76 1.424(2) . ? O77 C78 1.422(2) . ? C79 C81 1.537(2) . ? C79 C80 1.538(2) . ? C79 C82 1.539(2) . ? C83 C86 1.5346(19) . ? C83 C84 1.540(2) . ? C83 C85 1.541(2) . ? O90 C91 1.353(7) . ? O90 C93 1.373(7) . ? C91 C92 1.484(8) . ? C93 C94 1.478(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 O61 Co1 O31 178.90(4) . . ? O61 Co1 O1 86.16(4) . . ? O31 Co1 O1 94.39(4) . . ? O61 Co1 N68 84.42(4) . . ? O31 Co1 N68 95.02(4) . . ? O1 Co1 N68 170.58(4) . . ? O61 Co1 N8 87.86(4) . . ? O31 Co1 N8 91.25(4) . . ? O1 Co1 N8 83.84(4) . . ? N68 Co1 N8 95.69(5) . . ? O61 Co1 N38 96.93(4) . . ? O31 Co1 N38 84.06(4) . . ? O1 Co1 N38 86.10(4) . . ? N68 Co1 N38 95.13(5) . . ? N8 Co1 N38 168.54(5) . . ? C2 O1 Co1 111.07(8) . . ? O1 C2 C7 123.81(12) . . ? O1 C2 C3 116.66(12) . . ? C7 C2 C3 119.52(12) . . ? N8 C3 C4 126.23(12) . . ? N8 C3 C2 113.04(12) . . ? C4 C3 C2 120.73(12) . . ? C5 C4 C3 119.36(13) . . ? C4 C5 C6 118.77(13) . . ? C4 C5 C23 122.18(13) . . ? C6 C5 C23 118.93(12) . . ? C7 C6 C5 124.43(13) . . ? C6 C7 C2 116.58(12) . . ? C6 C7 C19 123.31(12) . . ? C2 C7 C19 119.98(12) . . ? C3 N8 C9 120.88(11) . . ? C3 N8 Co1 111.71(9) . . ? C9 N8 Co1 126.52(9) . . ? C14 C9 C10 122.26(13) . . ? C14 C9 N8 118.25(12) . . ? C10 C9 N8 119.47(12) . . ? C9 C10 C11 118.43(13) . . ? O15 C11 C12 115.96(13) . . ? O15 C11 C10 123.76(14) . . ? C12 C11 C10 120.27(14) . . ? C13 C12 C11 120.07(13) . . ? O17 C13 C12 115.35(13) . . ? O17 C13 C14 123.67(14) . . ? C12 C13 C14 120.97(14) . . ? C9 C14 C13 117.95(14) . . ? C11 O15 C16 116.96(12) . . ? C13 O17 C18 117.40(12) . . ? C7 C19 C20 111.63(12) . . ? C7 C19 C22 111.84(11) . . ? C20 C19 C22 107.87(11) . . ? C7 C19 C21 108.17(11) . . ? C20 C19 C21 108.07(12) . . ? C22 C19 C21 109.18(12) . . ? C25 C23 C26 108.90(14) . . ? C25 C23 C5 112.44(12) . . ? C26 C23 C5 110.66(13) . . ? C25 C23 C24 107.76(13) . . ? C26 C23 C24 108.97(13) . . ? C5 C23 C24 108.00(13) . . ? C32 O31 Co1 113.02(8) . . ? O31 C32 C37 123.15(12) . . ? O31 C32 C33 117.00(11) . . ? C37 C32 C33 119.83(12) . . ? N38 C33 C34 126.61(13) . . ? N38 C33 C32 112.73(12) . . ? C34 C33 C32 120.53(12) . . ? C35 C34 C33 119.61(13) . . ? C34 C35 C36 118.70(13) . . ? C34 C35 C53 122.46(13) . . ? C36 C35 C53 118.77(12) . . ? C37 C36 C35 124.54(13) . . ? C36 C37 C32 116.70(13) . . ? C36 C37 C49 123.21(12) . . ? C32 C37 C49 120.09(12) . . ? C33 N38 C39 122.32(11) . . ? C33 N38 Co1 112.00(9) . . ? C39 N38 Co1 123.72(9) . . ? C40 C39 C44 121.58(13) . . ? C40 C39 N38 117.95(12) . . ? C44 C39 N38 120.38(12) . . ? C39 C40 C41 118.52(13) . . ? O45 C41 C42 115.38(13) . . ? O45 C41 C40 123.66(13) . . ? C42 C41 C40 120.96(13) . . ? C43 C42 C41 119.51(13) . . ? O47 C43 C42 115.26(13) . . ? O47 C43 C44 123.74(14) . . ? C42 C43 C44 120.99(13) . . ? C43 C44 C39 118.42(13) . . ? C41 O45 C46 117.05(12) . . ? C43 O47 C48 117.51(12) . . ? C37 C49 C52 111.74(12) . . ? C37 C49 C50 109.29(11) . . ? C52 C49 C50 108.26(12) . . ? C37 C49 C51 109.78(12) . . ? C52 C49 C51 108.19(12) . . ? C50 C49 C51 109.54(13) . . ? C55 C53 C35 111.85(12) . . ? C55 C53 C54 107.46(14) . . ? C35 C53 C54 111.00(13) . . ? C55 C53 C56 109.25(14) . . ? C35 C53 C56 107.87(12) . . ? C54 C53 C56 109.40(14) . . ? C62 O61 Co1 113.07(8) . . ? O61 C62 C67 123.19(12) . . ? O61 C62 C63 116.59(11) . . ? C67 C62 C63 120.20(12) . . ? N68 C63 C64 126.45(12) . . ? N68 C63 C62 113.27(11) . . ? C64 C63 C62 120.20(12) . . ? C65 C64 C63 119.97(12) . . ? C64 C65 C66 118.65(12) . . ? C64 C65 C79 121.79(12) . . ? C66 C65 C79 119.51(12) . . ? C67 C66 C65 124.25(12) . . ? C66 C67 C62 116.62(12) . . ? C66 C67 C83 124.04(12) . . ? C62 C67 C83 119.34(12) . . ? C63 N68 C69 120.05(11) . . ? C63 N68 Co1 112.16(9) . . ? C69 N68 Co1 127.75(9) . . ? C70 C69 C74 122.03(12) . . ? C70 C69 N68 118.09(12) . . ? C74 C69 N68 119.86(12) . . ? C69 C70 C71 118.32(13) . . ? O75 C71 C72 115.35(13) . . ? O75 C71 C70 123.59(14) . . ? C72 C71 C70 121.05(14) . . ? C71 C72 C73 119.59(13) . . ? O77 C73 C72 115.14(13) . . ? O77 C73 C74 123.92(14) . . ? C72 C73 C74 120.95(14) . . ? C69 C74 C73 118.04(13) . . ? C71 O75 C76 117.19(12) . . ? C73 O77 C78 117.30(12) . . ? C65 C79 C81 108.59(12) . . ? C65 C79 C80 111.91(12) . . ? C81 C79 C80 107.77(12) . . ? C65 C79 C82 110.76(12) . . ? C81 C79 C82 109.12(12) . . ? C80 C79 C82 108.62(12) . . ? C67 C83 C86 111.70(11) . . ? C67 C83 C84 109.51(12) . . ? C86 C83 C84 107.89(12) . . ? C67 C83 C85 110.09(11) . . ? C86 C83 C85 107.68(12) . . ? C84 C83 C85 109.92(12) . . ? C91 O90 C93 118.0(6) . . ? O90 C91 C92 114.8(6) . . ? O90 C93 C94 112.5(6) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 27.86 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.575 _refine_diff_density_min -0.391 _refine_diff_density_rms 0.046 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 665849' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H123 Co N3 O3' _chemical_formula_weight 1281.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 16.1355(4) _cell_length_b 14.5516(4) _cell_length_c 34.0664(8) _cell_angle_alpha 90.00 _cell_angle_beta 97.77(1) _cell_angle_gamma 90.00 _cell_volume 7925.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'opaque parallelepiped' _exptl_crystal_colour black _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.074 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2796 _exptl_absorpt_coefficient_mu 0.263 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.9141 _exptl_absorpt_correction_T_max 0.9774 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method '2014 images at 0.5 deg. in\w and 20 sec.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 86147 _diffrn_reflns_av_R_equivalents 0.0676 _diffrn_reflns_av_sigmaI/netI 0.0523 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.50 _reflns_number_total 18094 _reflns_number_gt 14435 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO, Nonius Collect Software' _computing_cell_refinement 'DENZO, Nonius Collect Software' _computing_data_reduction 'DENZO, Nonius Collect Software' _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0267P)^2^+5.4393P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18094 _refine_ls_number_parameters 856 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0674 _refine_ls_R_factor_gt 0.0480 _refine_ls_wR_factor_ref 0.1027 _refine_ls_wR_factor_gt 0.0954 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.742157(13) 0.773696(15) 0.094718(7) 0.01268(6) Uani 1 d . . . O1 O 0.63937(7) 0.77098(8) 0.11503(3) 0.0148(2) Uani 1 d . . . C1 C 0.63107(10) 0.69913(11) 0.13688(5) 0.0149(3) Uani 1 d . . . C2 C 0.55751(10) 0.68073(12) 0.15435(5) 0.0186(4) Uani 1 d . . . C3 C 0.55978(11) 0.60572(12) 0.17904(5) 0.0214(4) Uani 1 d . . . H3 H 0.5112 0.5924 0.1909 0.026 Uiso 1 calc R . . C4 C 0.63056(11) 0.54654(12) 0.18793(5) 0.0190(4) Uani 1 d . . . C5 C 0.69970(10) 0.56240(11) 0.16967(5) 0.0171(3) Uani 1 d . . . H5 H 0.7471 0.5234 0.1749 0.021 Uiso 1 calc R . . C6 C 0.70074(10) 0.63681(11) 0.14302(5) 0.0151(3) Uani 1 d . . . N7 N 0.76301(8) 0.65926(9) 0.12221(4) 0.0141(3) Uani 1 d . . . C8 C 0.84002(10) 0.60896(11) 0.12857(5) 0.0157(3) Uani 1 d . . . C9 C 0.90736(10) 0.64700(12) 0.15315(5) 0.0181(3) Uani 1 d . . . H9 H 0.9019 0.7058 0.1646 0.022 Uiso 1 calc R . . C10 C 0.98256(10) 0.59947(12) 0.16096(5) 0.0200(4) Uani 1 d . . . C11 C 0.98769(10) 0.51303(12) 0.14385(5) 0.0210(4) Uani 1 d . . . H11 H 1.0390 0.4803 0.1487 0.025 Uiso 1 calc R . . C12 C 0.92095(11) 0.47255(12) 0.11994(5) 0.0184(4) Uani 1 d . . . C13 C 0.84657(10) 0.52286(11) 0.11199(5) 0.0169(3) Uani 1 d . . . H13 H 0.8004 0.4978 0.0951 0.020 Uiso 1 calc R . . C14 C 0.48159(11) 0.74460(13) 0.14539(6) 0.0257(4) Uani 1 d . . . C15 C 0.50533(13) 0.84170(14) 0.16024(6) 0.0313(5) Uani 1 d . . . H15A H 0.5499 0.8656 0.1462 0.047 Uiso 1 calc R . . H15B H 0.5249 0.8397 0.1887 0.047 Uiso 1 calc R . . H15C H 0.4563 0.8819 0.1553 0.047 Uiso 1 calc R . . C16 C 0.45277(12) 0.74624(15) 0.10058(6) 0.0311(5) Uani 1 d . . . H16A H 0.4975 0.7714 0.0870 0.047 Uiso 1 calc R . . H16B H 0.4028 0.7848 0.0950 0.047 Uiso 1 calc R . . H16C H 0.4396 0.6836 0.0912 0.047 Uiso 1 calc R . . C17 C 0.40826(13) 0.71136(17) 0.16596(8) 0.0489(7) Uani 1 d . . . H17A H 0.3604 0.7525 0.1592 0.073 Uiso 1 calc R . . H17B H 0.4248 0.7115 0.1947 0.073 Uiso 1 calc R . . H17C H 0.3927 0.6489 0.1571 0.073 Uiso 1 calc R . . C18 C 0.62478(11) 0.46579(12) 0.21631(6) 0.0235(4) Uani 1 d . . . C19 C 0.59439(16) 0.49890(15) 0.25474(7) 0.0416(6) Uani 1 d . . . H19A H 0.5931 0.4469 0.2729 0.062 Uiso 1 calc R . . H19B H 0.5381 0.5248 0.2486 0.062 Uiso 1 calc R . . H19C H 0.6326 0.5461 0.2672 0.062 Uiso 1 calc R . . C20 C 0.70959(12) 0.41903(13) 0.22736(6) 0.0256(4) Uani 1 d . . . H20A H 0.7286 0.3936 0.2035 0.038 Uiso 1 calc R . . H20B H 0.7042 0.3694 0.2463 0.038 Uiso 1 calc R . . H20C H 0.7504 0.4642 0.2394 0.038 Uiso 1 calc R . . C21 C 0.56293(12) 0.39509(14) 0.19569(7) 0.0351(5) Uani 1 d . . . H21A H 0.5837 0.3723 0.1718 0.053 Uiso 1 calc R . . H21B H 0.5083 0.4242 0.1884 0.053 Uiso 1 calc R . . H21C H 0.5574 0.3437 0.2137 0.053 Uiso 1 calc R . . C22 C 1.05841(11) 0.63992(13) 0.18725(6) 0.0262(4) Uani 1 d . . . C23 C 1.09895(13) 0.56664(15) 0.21592(6) 0.0335(5) Uani 1 d . . . H23A H 1.1228 0.5181 0.2009 0.050 Uiso 1 calc R . . H23B H 1.0566 0.5401 0.2307 0.050 Uiso 1 calc R . . H23C H 1.1434 0.5948 0.2345 0.050 Uiso 1 calc R . . C24 C 1.12154(14) 0.6726(2) 0.16086(8) 0.0506(7) Uani 1 d . . . H24A H 1.1703 0.6988 0.1773 0.076 Uiso 1 calc R . . H24B H 1.0957 0.7195 0.1425 0.076 Uiso 1 calc R . . H24C H 1.1392 0.6204 0.1458 0.076 Uiso 1 calc R . . C25 C 1.03461(14) 0.72094(16) 0.21208(8) 0.0467(6) Uani 1 d . . . H25A H 0.9920 0.7013 0.2282 0.070 Uiso 1 calc R . . H25B H 1.0124 0.7710 0.1945 0.070 Uiso 1 calc R . . H25C H 1.0842 0.7424 0.2294 0.070 Uiso 1 calc R . . C26 C 0.92567(11) 0.37335(12) 0.10528(6) 0.0216(4) Uani 1 d . . . C27 C 1.01529(12) 0.33575(13) 0.11059(7) 0.0292(4) Uani 1 d . . . H27A H 1.0158 0.2751 0.0982 0.044 Uiso 1 calc R . . H27B H 1.0359 0.3305 0.1389 0.044 Uiso 1 calc R . . H27C H 1.0514 0.3777 0.0981 0.044 Uiso 1 calc R . . C28 C 0.87331(12) 0.31287(13) 0.12953(6) 0.0283(4) Uani 1 d . . . H28A H 0.8152 0.3342 0.1257 0.042 Uiso 1 calc R . . H28B H 0.8959 0.3168 0.1577 0.042 Uiso 1 calc R . . H28C H 0.8754 0.2489 0.1207 0.042 Uiso 1 calc R . . C29 C 0.89117(15) 0.36645(14) 0.06135(6) 0.0365(5) Uani 1 d . . . H29A H 0.9261 0.4030 0.0458 0.055 Uiso 1 calc R . . H29B H 0.8337 0.3899 0.0571 0.055 Uiso 1 calc R . . H29C H 0.8916 0.3021 0.0529 0.055 Uiso 1 calc R . . O31 O 0.84330(7) 0.77546(8) 0.07332(3) 0.0159(2) Uani 1 d . . . C31 C 0.89811(10) 0.83044(11) 0.09256(5) 0.0151(3) Uani 1 d . . . C32 C 0.97526(10) 0.85303(11) 0.07910(5) 0.0176(3) Uani 1 d . . . C33 C 1.02751(11) 0.91084(12) 0.10292(5) 0.0206(4) Uani 1 d . . . H33 H 1.0789 0.9279 0.0942 0.025 Uiso 1 calc R . . C34 C 1.00974(11) 0.94696(12) 0.13989(5) 0.0192(4) Uani 1 d . . . C35 C 0.93507(10) 0.92611(11) 0.15223(5) 0.0180(3) Uani 1 d . . . H35 H 0.9217 0.9501 0.1765 0.022 Uiso 1 calc R . . C36 C 0.87747(10) 0.86861(11) 0.12879(5) 0.0154(3) Uani 1 d . . . N37 N 0.80296(8) 0.84023(9) 0.13769(4) 0.0146(3) Uani 1 d . . . C38 C 0.76879(10) 0.87728(11) 0.17056(5) 0.0149(3) Uani 1 d . . . C39 C 0.76242(10) 0.82193(12) 0.20321(5) 0.0172(3) Uani 1 d . . . H39 H 0.7810 0.7600 0.2034 0.021 Uiso 1 calc R . . C40 C 0.72883(11) 0.85704(12) 0.23565(5) 0.0185(4) Uani 1 d . . . C41 C 0.70165(10) 0.94823(12) 0.23389(5) 0.0186(4) Uani 1 d . . . H41 H 0.6785 0.9727 0.2559 0.022 Uiso 1 calc R . . C42 C 0.70699(10) 1.00475(11) 0.20148(5) 0.0163(3) Uani 1 d . . . C43 C 0.74092(10) 0.96755(11) 0.16938(5) 0.0163(3) Uani 1 d . . . H43 H 0.7449 1.0042 0.1466 0.020 Uiso 1 calc R . . C44 C 0.99581(11) 0.81407(13) 0.03977(5) 0.0223(4) Uani 1 d . . . C45 C 0.99419(12) 0.70827(13) 0.04109(6) 0.0259(4) Uani 1 d . . . H45A H 1.0335 0.6866 0.0637 0.039 Uiso 1 calc R . . H45B H 1.0105 0.6836 0.0165 0.039 Uiso 1 calc R . . H45C H 0.9376 0.6873 0.0440 0.039 Uiso 1 calc R . . C46 C 0.93142(13) 0.84901(15) 0.00576(6) 0.0314(5) Uani 1 d . . . H46A H 0.8753 0.8294 0.0102 0.047 Uiso 1 calc R . . H46B H 0.9443 0.8237 -0.0194 0.047 Uiso 1 calc R . . H46C H 0.9335 0.9163 0.0048 0.047 Uiso 1 calc R . . C47 C 1.08301(12) 0.84390(14) 0.03168(6) 0.0313(5) Uani 1 d . . . H47A H 1.0852 0.9111 0.0301 0.047 Uiso 1 calc R . . H47B H 1.0946 0.8173 0.0066 0.047 Uiso 1 calc R . . H47C H 1.1250 0.8224 0.0532 0.047 Uiso 1 calc R . . C48 C 1.07380(11) 1.01051(13) 0.16322(6) 0.0240(4) Uani 1 d . . . C49 C 1.07097(12) 1.10256(13) 0.14106(7) 0.0308(5) Uani 1 d . . . H49A H 1.0831 1.0923 0.1140 0.046 Uiso 1 calc R . . H49B H 1.1128 1.1444 0.1548 0.046 Uiso 1 calc R . . H49C H 1.0152 1.1298 0.1402 0.046 Uiso 1 calc R . . C50 C 1.05346(13) 1.02749(16) 0.20524(6) 0.0365(5) Uani 1 d . . . H50A H 0.9990 1.0580 0.2039 0.055 Uiso 1 calc R . . H50B H 1.0967 1.0667 0.2196 0.055 Uiso 1 calc R . . H50C H 1.0516 0.9687 0.2191 0.055 Uiso 1 calc R . . C51 C 1.16171(12) 0.96888(14) 0.16662(7) 0.0308(5) Uani 1 d . . . H51A H 1.1621 0.9092 0.1800 0.046 Uiso 1 calc R . . H51B H 1.2017 1.0102 0.1820 0.046 Uiso 1 calc R . . H51C H 1.1776 0.9606 0.1401 0.046 Uiso 1 calc R . . C52 C 0.71918(12) 0.79792(12) 0.27190(5) 0.0230(4) Uani 1 d . . . C53 C 0.62600(13) 0.77700(16) 0.27158(7) 0.0375(5) Uani 1 d . . . H53A H 0.5952 0.8347 0.2731 0.056 Uiso 1 calc R . . H53B H 0.6186 0.7383 0.2944 0.056 Uiso 1 calc R . . H53C H 0.6046 0.7446 0.2471 0.056 Uiso 1 calc R . . C54 C 0.76541(14) 0.70638(14) 0.27108(6) 0.0353(5) Uani 1 d . . . H54A H 0.7421 0.6714 0.2476 0.053 Uiso 1 calc R . . H54B H 0.7588 0.6711 0.2950 0.053 Uiso 1 calc R . . H54C H 0.8249 0.7180 0.2702 0.053 Uiso 1 calc R . . C55 C 0.75313(18) 0.84836(16) 0.30993(6) 0.0462(6) Uani 1 d . . . H55A H 0.8123 0.8630 0.3096 0.069 Uiso 1 calc R . . H55B H 0.7473 0.8092 0.3328 0.069 Uiso 1 calc R . . H55C H 0.7216 0.9053 0.3118 0.069 Uiso 1 calc R . . C56 C 0.67387(11) 1.10341(12) 0.19912(5) 0.0205(4) Uani 1 d . . . C57 C 0.73634(14) 1.16787(13) 0.18290(7) 0.0336(5) Uani 1 d . . . H57A H 0.7440 1.1486 0.1561 0.050 Uiso 1 calc R . . H57B H 0.7901 1.1653 0.2001 0.050 Uiso 1 calc R . . H57C H 0.7148 1.2309 0.1822 0.050 Uiso 1 calc R . . C58 C 0.65731(13) 1.13945(13) 0.23944(6) 0.0265(4) Uani 1 d . . . H58A H 0.6391 1.2037 0.2368 0.040 Uiso 1 calc R . . H58B H 0.7087 1.1354 0.2583 0.040 Uiso 1 calc R . . H58C H 0.6135 1.1024 0.2490 0.040 Uiso 1 calc R . . C59 C 0.59114(13) 1.10443(15) 0.17118(6) 0.0331(5) Uani 1 d . . . H59A H 0.5509 1.0638 0.1816 0.050 Uiso 1 calc R . . H59B H 0.6007 1.0830 0.1449 0.050 Uiso 1 calc R . . H59C H 0.5689 1.1672 0.1691 0.050 Uiso 1 calc R . . O61 O 0.71458(7) 0.89065(8) 0.07262(3) 0.0156(2) Uani 1 d . . . C61 C 0.69535(10) 0.88804(11) 0.03444(5) 0.0152(3) Uani 1 d . . . C62 C 0.68654(11) 0.96849(11) 0.01058(5) 0.0179(3) Uani 1 d . . . C63 C 0.66845(11) 0.95621(11) -0.02960(5) 0.0187(4) Uani 1 d . . . H63 H 0.6636 1.0093 -0.0460 0.022 Uiso 1 calc R . . C64 C 0.65644(10) 0.86877(11) -0.04825(5) 0.0164(3) Uani 1 d . . . C65 C 0.66235(10) 0.79144(11) -0.02511(5) 0.0153(3) Uani 1 d . . . H65 H 0.6521 0.7328 -0.0370 0.018 Uiso 1 calc R . . C66 C 0.68365(10) 0.79855(11) 0.01653(5) 0.0142(3) Uani 1 d . . . N67 N 0.69337(8) 0.72939(9) 0.04305(4) 0.0143(3) Uani 1 d . . . C68 C 0.69130(10) 0.63639(11) 0.03073(5) 0.0150(3) Uani 1 d . . . C69 C 0.73872(10) 0.60546(11) 0.00239(5) 0.0164(3) Uani 1 d . . . H69 H 0.7750 0.6469 -0.0085 0.020 Uiso 1 calc R . . C70 C 0.73377(10) 0.51400(11) -0.01036(5) 0.0169(3) Uani 1 d . . . C71 C 0.68237(10) 0.45459(11) 0.00764(5) 0.0185(4) Uani 1 d . . . H71 H 0.6793 0.3920 -0.0003 0.022 Uiso 1 calc R . . C72 C 0.63526(10) 0.48360(11) 0.03694(5) 0.0163(3) Uani 1 d . . . C73 C 0.64028(10) 0.57518(11) 0.04831(5) 0.0160(3) Uani 1 d . . . H73 H 0.6089 0.5966 0.0682 0.019 Uiso 1 calc R . . C74 C 0.69672(13) 1.06360(12) 0.03006(5) 0.0240(4) Uani 1 d . . . C75 C 0.62889(14) 1.07644(13) 0.05711(6) 0.0326(5) Uani 1 d . . . H75A H 0.5736 1.0745 0.0412 0.049 Uiso 1 calc R . . H75B H 0.6366 1.1359 0.0706 0.049 Uiso 1 calc R . . H75C H 0.6331 1.0271 0.0768 0.049 Uiso 1 calc R . . C76 C 0.78403(13) 1.07310(13) 0.05407(6) 0.0313(5) Uani 1 d . . . H76A H 0.7917 1.0253 0.0745 0.047 Uiso 1 calc R . . H76B H 0.7893 1.1338 0.0666 0.047 Uiso 1 calc R . . H76C H 0.8267 1.0663 0.0364 0.047 Uiso 1 calc R . . C77 C 0.68732(15) 1.14094(13) -0.00090(6) 0.0329(5) Uani 1 d . . . H77A H 0.7290 1.1329 -0.0190 0.049 Uiso 1 calc R . . H77B H 0.6959 1.2005 0.0125 0.049 Uiso 1 calc R . . H77C H 0.6311 1.1388 -0.0159 0.049 Uiso 1 calc R . . C78 C 0.64486(11) 0.86157(12) -0.09346(5) 0.0193(4) Uani 1 d . . . C79 C 0.58862(13) 0.78079(13) -0.10820(6) 0.0274(4) Uani 1 d . . . H79A H 0.5340 0.7880 -0.0990 0.041 Uiso 1 calc R . . H79B H 0.6145 0.7233 -0.0978 0.041 Uiso 1 calc R . . H79C H 0.5813 0.7793 -0.1372 0.041 Uiso 1 calc R . . C80 C 0.73184(13) 0.84697(16) -0.10583(6) 0.0353(5) Uani 1 d . . . H80A H 0.7274 0.8458 -0.1348 0.053 Uiso 1 calc R . . H80B H 0.7549 0.7884 -0.0951 0.053 Uiso 1 calc R . . H80C H 0.7689 0.8973 -0.0955 0.053 Uiso 1 calc R . . C81 C 0.60690(14) 0.94879(14) -0.11355(6) 0.0332(5) Uani 1 d . . . H81A H 0.5544 0.9632 -0.1034 0.050 Uiso 1 calc R . . H81B H 0.5959 0.9390 -0.1422 0.050 Uiso 1 calc R . . H81C H 0.6461 1.0000 -0.1078 0.050 Uiso 1 calc R . . C82 C 0.78090(11) 0.48396(12) -0.04437(5) 0.0210(4) Uani 1 d . . . C83 C 0.77710(12) 0.37976(13) -0.05093(6) 0.0283(4) Uani 1 d . . . H83A H 0.8024 0.3485 -0.0268 0.042 Uiso 1 calc R . . H83B H 0.8078 0.3637 -0.0729 0.042 Uiso 1 calc R . . H83C H 0.7186 0.3605 -0.0573 0.042 Uiso 1 calc R . . C84 C 0.87313(11) 0.51239(13) -0.03613(6) 0.0266(4) Uani 1 d . . . H84A H 0.8770 0.5794 -0.0339 0.040 Uiso 1 calc R . . H84B H 0.9024 0.4917 -0.0579 0.040 Uiso 1 calc R . . H84C H 0.8989 0.4842 -0.0113 0.040 Uiso 1 calc R . . C85 C 0.74073(14) 0.53138(15) -0.08256(6) 0.0347(5) Uani 1 d . . . H85A H 0.6820 0.5127 -0.0884 0.052 Uiso 1 calc R . . H85B H 0.7707 0.5135 -0.1046 0.052 Uiso 1 calc R . . H85C H 0.7439 0.5982 -0.0791 0.052 Uiso 1 calc R . . C86 C 0.58108(10) 0.41438(11) 0.05618(5) 0.0197(4) Uani 1 d . . . C87 C 0.51682(12) 0.46268(13) 0.07826(7) 0.0312(5) Uani 1 d . . . H87A H 0.4817 0.5030 0.0599 0.047 Uiso 1 calc R . . H87B H 0.5460 0.4993 0.1000 0.047 Uiso 1 calc R . . H87C H 0.4816 0.4166 0.0890 0.047 Uiso 1 calc R . . C88 C 0.53424(12) 0.35085(13) 0.02495(6) 0.0284(4) Uani 1 d . . . H88A H 0.5746 0.3164 0.0117 0.043 Uiso 1 calc R . . H88B H 0.4984 0.3876 0.0054 0.043 Uiso 1 calc R . . H88C H 0.4997 0.3078 0.0378 0.043 Uiso 1 calc R . . C89 C 0.63892(11) 0.35658(12) 0.08596(6) 0.0230(4) Uani 1 d . . . H89A H 0.6057 0.3111 0.0982 0.034 Uiso 1 calc R . . H89B H 0.6678 0.3967 0.1065 0.034 Uiso 1 calc R . . H89C H 0.6802 0.3250 0.0722 0.034 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.01491(10) 0.01111(11) 0.01260(11) 0.00116(9) 0.00393(8) -0.00008(8) O1 0.0152(5) 0.0139(6) 0.0161(6) 0.0035(5) 0.0050(4) 0.0015(4) C1 0.0187(8) 0.0130(8) 0.0131(8) 0.0029(6) 0.0027(6) 0.0009(6) C2 0.0173(8) 0.0184(9) 0.0210(9) 0.0037(7) 0.0055(7) 0.0025(7) C3 0.0202(8) 0.0216(9) 0.0248(10) 0.0074(7) 0.0112(7) 0.0030(7) C4 0.0233(9) 0.0158(8) 0.0188(9) 0.0056(7) 0.0062(7) 0.0009(7) C5 0.0194(8) 0.0138(8) 0.0182(9) 0.0024(7) 0.0031(7) 0.0036(6) C6 0.0164(8) 0.0152(8) 0.0141(8) 0.0002(6) 0.0030(6) -0.0004(6) N7 0.0151(6) 0.0123(7) 0.0152(7) 0.0004(5) 0.0037(5) 0.0019(5) C8 0.0161(8) 0.0150(8) 0.0168(9) 0.0050(7) 0.0057(6) 0.0021(6) C9 0.0199(8) 0.0169(8) 0.0179(9) 0.0017(7) 0.0034(7) 0.0013(6) C10 0.0180(8) 0.0210(9) 0.0208(9) 0.0044(7) 0.0015(7) -0.0003(7) C11 0.0164(8) 0.0205(9) 0.0265(10) 0.0063(7) 0.0049(7) 0.0055(7) C12 0.0212(8) 0.0170(8) 0.0184(9) 0.0037(7) 0.0074(7) 0.0031(7) C13 0.0176(8) 0.0159(8) 0.0176(9) 0.0013(7) 0.0036(7) -0.0006(6) C14 0.0200(9) 0.0272(10) 0.0321(11) 0.0137(8) 0.0120(8) 0.0084(7) C15 0.0386(11) 0.0291(11) 0.0285(11) 0.0070(9) 0.0126(9) 0.0188(9) C16 0.0188(9) 0.0360(11) 0.0374(12) 0.0099(9) -0.0004(8) 0.0032(8) C17 0.0262(11) 0.0546(15) 0.0722(18) 0.0365(13) 0.0297(11) 0.0213(10) C18 0.0259(9) 0.0200(9) 0.0265(10) 0.0115(8) 0.0102(8) 0.0040(7) C19 0.0602(15) 0.0346(12) 0.0364(13) 0.0212(10) 0.0301(11) 0.0160(11) C20 0.0300(10) 0.0193(9) 0.0275(11) 0.0119(8) 0.0041(8) 0.0033(7) C21 0.0280(10) 0.0278(11) 0.0493(14) 0.0191(10) 0.0051(9) -0.0040(8) C22 0.0204(9) 0.0255(10) 0.0306(11) 0.0040(8) -0.0036(8) -0.0003(7) C23 0.0299(10) 0.0346(11) 0.0327(12) 0.0012(9) -0.0077(9) 0.0045(9) C24 0.0348(12) 0.0696(18) 0.0449(15) 0.0110(13) -0.0037(11) -0.0265(12) C25 0.0384(12) 0.0351(13) 0.0584(16) -0.0168(12) -0.0227(11) 0.0060(10) C26 0.0246(9) 0.0164(9) 0.0241(10) 0.0009(7) 0.0037(7) 0.0064(7) C27 0.0278(10) 0.0188(9) 0.0430(13) 0.0026(9) 0.0115(9) 0.0074(8) C28 0.0269(10) 0.0200(9) 0.0383(12) 0.0024(8) 0.0057(9) -0.0007(8) C29 0.0546(14) 0.0270(11) 0.0269(11) -0.0049(9) 0.0019(10) 0.0162(10) O31 0.0177(5) 0.0153(6) 0.0158(6) -0.0015(5) 0.0059(5) -0.0014(5) C31 0.0169(8) 0.0117(8) 0.0171(9) 0.0020(6) 0.0033(6) 0.0008(6) C32 0.0188(8) 0.0155(8) 0.0197(9) 0.0024(7) 0.0070(7) 0.0012(6) C33 0.0186(8) 0.0184(9) 0.0267(10) 0.0019(7) 0.0092(7) -0.0020(7) C34 0.0201(8) 0.0160(8) 0.0215(9) 0.0006(7) 0.0024(7) -0.0023(6) C35 0.0213(8) 0.0155(8) 0.0175(9) -0.0020(7) 0.0037(7) -0.0017(6) C36 0.0173(8) 0.0127(8) 0.0169(9) 0.0029(6) 0.0053(6) 0.0000(6) N37 0.0168(7) 0.0136(7) 0.0141(7) 0.0000(5) 0.0042(5) -0.0003(5) C38 0.0150(7) 0.0171(8) 0.0128(8) -0.0014(6) 0.0025(6) -0.0013(6) C39 0.0192(8) 0.0155(8) 0.0171(9) 0.0014(7) 0.0033(7) 0.0023(6) C40 0.0209(8) 0.0216(9) 0.0130(8) 0.0029(7) 0.0027(7) 0.0021(7) C41 0.0206(8) 0.0215(9) 0.0146(9) -0.0015(7) 0.0057(7) 0.0020(7) C42 0.0164(8) 0.0163(8) 0.0160(9) 0.0000(7) 0.0016(6) 0.0013(6) C43 0.0179(8) 0.0162(8) 0.0152(8) 0.0020(7) 0.0036(7) -0.0004(6) C44 0.0240(9) 0.0235(9) 0.0217(10) -0.0024(7) 0.0119(7) -0.0017(7) C45 0.0249(9) 0.0239(10) 0.0309(11) -0.0073(8) 0.0114(8) -0.0005(7) C46 0.0349(11) 0.0395(12) 0.0224(10) 0.0025(9) 0.0127(8) 0.0031(9) C47 0.0300(10) 0.0327(11) 0.0354(12) -0.0069(9) 0.0201(9) -0.0069(8) C48 0.0217(9) 0.0223(9) 0.0279(10) -0.0030(8) 0.0032(8) -0.0059(7) C49 0.0240(9) 0.0199(9) 0.0479(13) -0.0013(9) 0.0032(9) -0.0058(7) C50 0.0353(11) 0.0416(13) 0.0330(12) -0.0151(10) 0.0061(9) -0.0186(10) C51 0.0240(10) 0.0270(10) 0.0393(12) -0.0011(9) -0.0028(9) -0.0033(8) C52 0.0342(10) 0.0213(9) 0.0151(9) 0.0041(7) 0.0089(8) 0.0050(7) C53 0.0395(12) 0.0407(12) 0.0363(12) 0.0187(10) 0.0189(10) 0.0070(10) C54 0.0505(13) 0.0326(11) 0.0254(11) 0.0142(9) 0.0147(10) 0.0165(10) C55 0.0850(19) 0.0355(13) 0.0165(11) 0.0055(9) 0.0012(11) -0.0065(12) C56 0.0263(9) 0.0170(9) 0.0185(9) 0.0004(7) 0.0038(7) 0.0048(7) C57 0.0472(12) 0.0177(9) 0.0395(13) 0.0004(9) 0.0193(10) 0.0017(8) C58 0.0363(11) 0.0205(9) 0.0233(10) -0.0031(8) 0.0066(8) 0.0081(8) C59 0.0358(11) 0.0321(11) 0.0290(11) -0.0029(9) -0.0043(9) 0.0152(9) O61 0.0217(6) 0.0121(6) 0.0133(6) 0.0015(5) 0.0040(5) 0.0000(4) C61 0.0159(8) 0.0147(8) 0.0157(9) 0.0014(7) 0.0044(6) 0.0000(6) C62 0.0234(9) 0.0121(8) 0.0190(9) 0.0011(7) 0.0060(7) 0.0000(6) C63 0.0252(9) 0.0136(8) 0.0183(9) 0.0048(7) 0.0062(7) 0.0013(7) C64 0.0161(8) 0.0186(8) 0.0148(8) 0.0021(7) 0.0028(6) 0.0006(6) C65 0.0169(8) 0.0138(8) 0.0154(8) 0.0000(6) 0.0031(6) -0.0005(6) C66 0.0148(7) 0.0123(8) 0.0159(8) 0.0019(6) 0.0034(6) -0.0009(6) N67 0.0159(6) 0.0124(7) 0.0148(7) 0.0014(6) 0.0029(5) -0.0007(5) C68 0.0169(8) 0.0120(8) 0.0153(8) 0.0018(6) -0.0006(6) 0.0001(6) C69 0.0171(8) 0.0149(8) 0.0173(9) 0.0022(7) 0.0023(6) -0.0013(6) C70 0.0178(8) 0.0151(8) 0.0173(9) -0.0006(7) 0.0007(7) 0.0022(6) C71 0.0191(8) 0.0118(8) 0.0238(10) -0.0008(7) 0.0003(7) 0.0003(6) C72 0.0149(8) 0.0135(8) 0.0199(9) 0.0040(7) -0.0001(6) -0.0005(6) C73 0.0165(8) 0.0160(8) 0.0154(8) 0.0017(7) 0.0017(6) 0.0006(6) C74 0.0427(11) 0.0119(8) 0.0183(9) 0.0014(7) 0.0080(8) -0.0007(7) C75 0.0550(13) 0.0169(9) 0.0288(11) 0.0004(8) 0.0158(10) 0.0089(9) C76 0.0503(13) 0.0188(10) 0.0247(11) -0.0013(8) 0.0044(9) -0.0121(9) C77 0.0629(14) 0.0130(9) 0.0239(11) 0.0025(8) 0.0096(10) 0.0013(9) C78 0.0262(9) 0.0174(8) 0.0143(9) 0.0026(7) 0.0030(7) -0.0012(7) C79 0.0399(11) 0.0240(10) 0.0170(9) 0.0018(8) -0.0009(8) -0.0072(8) C80 0.0355(11) 0.0514(14) 0.0212(11) -0.0034(10) 0.0115(9) -0.0045(10) C81 0.0546(13) 0.0241(10) 0.0183(10) 0.0040(8) -0.0048(9) -0.0007(9) C82 0.0256(9) 0.0177(9) 0.0205(9) -0.0006(7) 0.0062(7) 0.0030(7) C83 0.0319(10) 0.0217(10) 0.0327(11) -0.0092(8) 0.0098(9) 0.0004(8) C84 0.0284(10) 0.0225(9) 0.0317(11) -0.0006(8) 0.0148(8) -0.0013(8) C85 0.0444(12) 0.0393(12) 0.0213(10) 0.0005(9) 0.0081(9) 0.0157(10) C86 0.0188(8) 0.0141(8) 0.0262(10) 0.0031(7) 0.0034(7) -0.0023(6) C87 0.0280(10) 0.0203(9) 0.0491(13) 0.0079(9) 0.0191(9) -0.0011(8) C88 0.0259(10) 0.0263(10) 0.0312(11) 0.0045(8) -0.0022(8) -0.0110(8) C89 0.0247(9) 0.0194(9) 0.0245(10) 0.0060(7) 0.0018(7) -0.0034(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 Co1 O31 1.8754(11) . ? Co1 O1 1.8818(11) . ? Co1 O61 1.8896(11) . ? Co1 N37 1.9118(14) . ? Co1 N7 1.9177(13) . ? Co1 N67 1.9389(14) . ? O1 C1 1.3007(19) . ? C1 C2 1.423(2) . ? C1 C6 1.438(2) . ? C2 C3 1.375(2) . ? C2 C14 1.535(2) . ? C3 C4 1.430(2) . ? C4 C5 1.369(2) . ? C4 C18 1.532(2) . ? C5 C6 1.415(2) . ? C6 N7 1.346(2) . ? N7 C8 1.433(2) . ? C8 C13 1.384(2) . ? C8 C9 1.394(2) . ? C9 C10 1.391(2) . ? C10 C11 1.394(3) . ? C10 C22 1.533(2) . ? C11 C12 1.390(2) . ? C12 C13 1.401(2) . ? C12 C26 1.533(2) . ? C14 C15 1.532(3) . ? C14 C17 1.533(3) . ? C14 C16 1.534(3) . ? C18 C20 1.529(2) . ? C18 C21 1.536(3) . ? C18 C19 1.536(3) . ? C22 C24 1.523(3) . ? C22 C25 1.530(3) . ? C22 C23 1.532(3) . ? C26 C29 1.528(3) . ? C26 C27 1.534(2) . ? C26 C28 1.536(3) . ? O31 C31 1.3020(19) . ? C31 C32 1.422(2) . ? C31 C36 1.433(2) . ? C32 C33 1.375(2) . ? C32 C44 1.532(2) . ? C33 C34 1.429(2) . ? C34 C35 1.363(2) . ? C34 C48 1.527(2) . ? C35 C36 1.415(2) . ? C36 N37 1.344(2) . ? N37 C38 1.420(2) . ? C38 C43 1.387(2) . ? C38 C39 1.388(2) . ? C39 C40 1.392(2) . ? C40 C41 1.396(2) . ? C40 C52 1.530(2) . ? C41 C42 1.389(2) . ? C42 C43 1.397(2) . ? C42 C56 1.530(2) . ? C44 C47 1.533(2) . ? C44 C46 1.534(3) . ? C44 C45 1.541(3) . ? C48 C50 1.531(3) . ? C48 C51 1.532(3) . ? C48 C49 1.535(3) . ? C52 C55 1.525(3) . ? C52 C54 1.529(3) . ? C52 C53 1.533(3) . ? C56 C58 1.527(2) . ? C56 C59 1.531(3) . ? C56 C57 1.534(3) . ? O61 C61 1.296(2) . ? C61 C62 1.421(2) . ? C61 C66 1.440(2) . ? C62 C63 1.372(2) . ? C62 C74 1.534(2) . ? C63 C64 1.424(2) . ? C64 C65 1.370(2) . ? C64 C78 1.530(2) . ? C65 C66 1.417(2) . ? C66 N67 1.347(2) . ? N67 C68 1.416(2) . ? C68 C69 1.386(2) . ? C68 C73 1.401(2) . ? C69 C70 1.399(2) . ? C70 C71 1.396(2) . ? C70 C82 1.533(2) . ? C71 C72 1.399(2) . ? C72 C73 1.387(2) . ? C72 C86 1.537(2) . ? C74 C75 1.534(3) . ? C74 C77 1.536(2) . ? C74 C76 1.537(3) . ? C78 C79 1.528(2) . ? C78 C81 1.530(3) . ? C78 C80 1.534(3) . ? C82 C83 1.533(2) . ? C82 C84 1.533(2) . ? C82 C85 1.537(3) . ? C86 C88 1.530(3) . ? C86 C87 1.532(3) . ? C86 C89 1.533(2) . ? 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 O31 Co1 O1 178.65(5) . . ? O31 Co1 O61 90.19(5) . . ? O1 Co1 O61 89.64(5) . . ? O31 Co1 N37 84.68(5) . . ? O1 Co1 N37 96.64(5) . . ? O61 Co1 N37 85.28(5) . . ? O31 Co1 N7 95.58(5) . . ? O1 Co1 N7 84.69(5) . . ? O61 Co1 N7 173.17(5) . . ? N37 Co1 N7 91.59(6) . . ? O31 Co1 N67 85.39(5) . . ? O1 Co1 N67 93.26(5) . . ? O61 Co1 N67 83.86(5) . . ? N37 Co1 N67 165.24(6) . . ? N7 Co1 N67 100.22(6) . . ? C1 O1 Co1 113.04(10) . . ? O1 C1 C2 123.14(14) . . ? O1 C1 C6 116.83(14) . . ? C2 C1 C6 120.03(14) . . ? C3 C2 C1 116.76(15) . . ? C3 C2 C14 123.83(15) . . ? C1 C2 C14 119.41(15) . . ? C2 C3 C4 124.20(16) . . ? C5 C4 C3 118.62(15) . . ? C5 C4 C18 122.62(15) . . ? C3 C4 C18 118.72(15) . . ? C4 C5 C6 120.14(15) . . ? N7 C6 C5 126.75(15) . . ? N7 C6 C1 113.27(14) . . ? C5 C6 C1 119.96(15) . . ? C6 N7 C8 119.35(13) . . ? C6 N7 Co1 111.95(10) . . ? C8 N7 Co1 127.49(11) . . ? C13 C8 C9 120.56(15) . . ? C13 C8 N7 120.87(15) . . ? C9 C8 N7 118.53(15) . . ? C10 C9 C8 120.44(16) . . ? C9 C10 C11 117.93(16) . . ? C9 C10 C22 121.86(16) . . ? C11 C10 C22 120.20(15) . . ? C12 C11 C10 122.85(16) . . ? C11 C12 C13 117.87(16) . . ? C11 C12 C26 121.42(15) . . ? C13 C12 C26 120.54(16) . . ? C8 C13 C12 120.31(16) . . ? C15 C14 C17 108.30(17) . . ? C15 C14 C16 110.05(16) . . ? C17 C14 C16 108.11(17) . . ? C15 C14 C2 109.60(16) . . ? C17 C14 C2 111.26(15) . . ? C16 C14 C2 109.49(16) . . ? C20 C18 C4 111.58(14) . . ? C20 C18 C21 108.61(16) . . ? C4 C18 C21 108.44(15) . . ? C20 C18 C19 107.93(17) . . ? C4 C18 C19 110.54(15) . . ? C21 C18 C19 109.71(17) . . ? C24 C22 C25 108.91(19) . . ? C24 C22 C23 109.36(17) . . ? C25 C22 C23 107.55(17) . . ? C24 C22 C10 108.64(17) . . ? C25 C22 C10 112.24(16) . . ? C23 C22 C10 110.09(15) . . ? C29 C26 C12 110.70(15) . . ? C29 C26 C27 107.75(16) . . ? C12 C26 C27 112.65(15) . . ? C29 C26 C28 109.58(17) . . ? C12 C26 C28 108.02(15) . . ? C27 C26 C28 108.09(15) . . ? C31 O31 Co1 112.35(10) . . ? O31 C31 C32 122.98(15) . . ? O31 C31 C36 116.78(14) . . ? C32 C31 C36 120.25(15) . . ? C33 C32 C31 116.39(15) . . ? C33 C32 C44 123.68(15) . . ? C31 C32 C44 119.93(15) . . ? C32 C33 C34 124.39(16) . . ? C35 C34 C33 118.75(16) . . ? C35 C34 C48 122.59(16) . . ? C33 C34 C48 118.62(15) . . ? C34 C35 C36 119.90(16) . . ? N37 C36 C35 126.43(15) . . ? N37 C36 C31 113.23(14) . . ? C35 C36 C31 120.26(15) . . ? C36 N37 C38 121.06(14) . . ? C36 N37 Co1 111.40(11) . . ? C38 N37 Co1 125.63(10) . . ? C43 C38 C39 120.91(15) . . ? C43 C38 N37 119.72(15) . . ? C39 C38 N37 119.36(15) . . ? C38 C39 C40 120.14(16) . . ? C39 C40 C41 117.93(16) . . ? C39 C40 C52 121.83(15) . . ? C41 C40 C52 120.22(15) . . ? C42 C41 C40 122.96(16) . . ? C41 C42 C43 117.77(15) . . ? C41 C42 C56 122.59(15) . . ? C43 C42 C56 119.58(15) . . ? C38 C43 C42 120.28(15) . . ? C32 C44 C47 111.40(15) . . ? C32 C44 C46 109.47(15) . . ? C47 C44 C46 108.35(16) . . ? C32 C44 C45 109.73(15) . . ? C47 C44 C45 107.93(15) . . ? C46 C44 C45 109.92(16) . . ? C34 C48 C50 111.63(15) . . ? C34 C48 C51 110.75(15) . . ? C50 C48 C51 107.85(17) . . ? C34 C48 C49 107.41(15) . . ? C50 C48 C49 108.84(17) . . ? C51 C48 C49 110.35(16) . . ? C55 C52 C54 108.34(17) . . ? C55 C52 C40 110.55(16) . . ? C54 C52 C40 111.84(15) . . ? C55 C52 C53 109.94(18) . . ? C54 C52 C53 107.90(17) . . ? C40 C52 C53 108.23(15) . . ? C58 C56 C42 112.17(15) . . ? C58 C56 C59 108.18(15) . . ? C42 C56 C59 108.09(15) . . ? C58 C56 C57 108.51(16) . . ? C42 C56 C57 110.55(14) . . ? C59 C56 C57 109.28(17) . . ? C61 O61 Co1 112.64(10) . . ? O61 C61 C62 122.79(15) . . ? O61 C61 C66 116.85(14) . . ? C62 C61 C66 120.35(15) . . ? C63 C62 C61 117.04(15) . . ? C63 C62 C74 123.03(15) . . ? C61 C62 C74 119.93(15) . . ? C62 C63 C64 124.01(16) . . ? C65 C64 C63 118.87(16) . . ? C65 C64 C78 120.84(15) . . ? C63 C64 C78 120.08(15) . . ? C64 C65 C66 120.29(15) . . ? N67 C66 C65 127.37(15) . . ? N67 C66 C61 113.25(14) . . ? C65 C66 C61 119.37(14) . . ? C66 N67 C68 121.28(14) . . ? C66 N67 Co1 110.88(11) . . ? C68 N67 Co1 125.26(11) . . ? C69 C68 C73 120.20(15) . . ? C69 C68 N67 121.59(14) . . ? C73 C68 N67 118.20(15) . . ? C68 C69 C70 120.77(15) . . ? C71 C70 C69 117.72(16) . . ? C71 C70 C82 122.71(15) . . ? C69 C70 C82 119.51(15) . . ? C70 C71 C72 122.61(15) . . ? C73 C72 C71 118.17(15) . . ? C73 C72 C86 121.71(15) . . ? C71 C72 C86 120.11(15) . . ? C72 C73 C68 120.47(16) . . ? C62 C74 C75 109.04(15) . . ? C62 C74 C77 111.66(15) . . ? C75 C74 C77 108.12(16) . . ? C62 C74 C76 110.38(15) . . ? C75 C74 C76 110.28(16) . . ? C77 C74 C76 107.32(16) . . ? C79 C78 C64 111.71(14) . . ? C79 C78 C81 107.89(15) . . ? C64 C78 C81 112.36(15) . . ? C79 C78 C80 109.15(16) . . ? C64 C78 C80 107.12(14) . . ? C81 C78 C80 108.53(16) . . ? C83 C82 C70 112.22(15) . . ? C83 C82 C84 108.20(15) . . ? C70 C82 C84 110.68(15) . . ? C83 C82 C85 108.46(16) . . ? C70 C82 C85 108.44(14) . . ? C84 C82 C85 108.76(16) . . ? C88 C86 C87 108.38(15) . . ? C88 C86 C89 109.14(15) . . ? C87 C86 C89 108.59(16) . . ? C88 C86 C72 110.82(15) . . ? C87 C86 C72 111.75(14) . . ? C89 C86 C72 108.12(14) . . ? _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.957 _refine_diff_density_max 0.341 _refine_diff_density_min -0.496 _refine_diff_density_rms 0.049 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 665850' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H69 Co F18 N3 O3' _chemical_formula_weight 1353.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/n ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.3974(3) _cell_length_b 22.8936(9) _cell_length_c 21.4790(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.494(5) _cell_angle_gamma 90.00 _cell_volume 6587.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'transparent parallelepiped' _exptl_crystal_colour 'P2(1)/n, No.14' _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.364 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2796 _exptl_absorpt_coefficient_mu 0.358 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.8981 _exptl_absorpt_correction_T_max 0.9424 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method '363 images at 1.0 deg. in phi and 206 images at 1.0 deg. in \w, 20 sec./frame' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 93422 _diffrn_reflns_av_R_equivalents 0.0495 _diffrn_reflns_av_sigmaI/netI 0.0361 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.34 _diffrn_reflns_theta_max 30.00 _reflns_number_total 19130 _reflns_number_gt 15672 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect Software' _computing_cell_refinement 'Nonius Collect Software' _computing_data_reduction 'Nonius Collect Software' _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0482P)^2^+6.2167P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 19130 _refine_ls_number_parameters 892 _refine_ls_number_restraints 72 _refine_ls_R_factor_all 0.0656 _refine_ls_R_factor_gt 0.0503 _refine_ls_wR_factor_ref 0.1218 _refine_ls_wR_factor_gt 0.1137 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.001 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.653418(16) 0.259178(9) 0.516980(10) 0.01236(5) Uani 1 d . . . O1 O 0.60949(9) 0.20799(5) 0.45361(5) 0.0154(2) Uani 1 d . . . C1 C 0.62904(12) 0.22652(7) 0.39788(7) 0.0145(3) Uani 1 d . . . O2 O 0.61509(8) 0.20193(5) 0.57608(5) 0.0156(2) Uani 1 d . . . C2 C 0.61274(12) 0.19176(7) 0.34315(8) 0.0164(3) Uani 1 d . . . O3 O 0.69708(8) 0.30873(5) 0.58201(5) 0.0146(2) Uani 1 d . . . C3 C 0.63156(13) 0.21819(7) 0.28693(8) 0.0183(3) Uani 1 d . . . H3 H 0.6226 0.1956 0.2502 0.022 Uiso 1 calc R . . C4 C 0.66383(13) 0.27763(7) 0.28001(8) 0.0171(3) Uani 1 d . . . C5 C 0.68212(12) 0.31027(7) 0.33254(7) 0.0167(3) Uani 1 d . . . H5 H 0.7035 0.3497 0.3290 0.020 Uiso 1 calc R . . C6 C 0.66883(12) 0.28470(7) 0.39235(7) 0.0141(3) Uani 1 d . . . N7 N 0.68608(10) 0.31029(6) 0.44837(6) 0.0134(2) Uani 1 d . . . C8 C 0.72864(12) 0.36668(7) 0.45280(7) 0.0140(3) Uani 1 d . . . C9 C 0.81853(12) 0.38002(7) 0.42316(7) 0.0154(3) Uani 1 d . . . H9 H 0.8510 0.3513 0.3986 0.018 Uiso 1 calc R . . C10 C 0.86011(12) 0.43543(7) 0.42973(8) 0.0167(3) Uani 1 d . . . C11 C 0.81502(13) 0.47783(7) 0.46647(8) 0.0177(3) Uani 1 d . . . H11 H 0.8446 0.5152 0.4716 0.021 Uiso 1 calc R . . C12 C 0.72581(13) 0.46422(7) 0.49551(7) 0.0170(3) Uani 1 d . . . C13 C 0.68191(13) 0.40950(7) 0.48863(7) 0.0160(3) Uani 1 d . . . H13 H 0.6202 0.4012 0.5083 0.019 Uiso 1 calc R . . C14 C 0.57670(13) 0.12841(7) 0.34904(8) 0.0193(3) Uani 1 d . . . C15 C 0.47434(14) 0.12694(9) 0.38107(10) 0.0277(4) Uani 1 d . . . H15A H 0.4508 0.0865 0.3836 0.042 Uiso 1 calc R . . H15B H 0.4264 0.1502 0.3569 0.042 Uiso 1 calc R . . H15C H 0.4806 0.1432 0.4231 0.042 Uiso 1 calc R . . C16 C 0.65303(15) 0.09293(8) 0.38761(9) 0.0248(4) Uani 1 d . . . H16A H 0.6307 0.0523 0.3905 0.037 Uiso 1 calc R . . H16B H 0.6587 0.1097 0.4295 0.037 Uiso 1 calc R . . H16C H 0.7182 0.0943 0.3673 0.037 Uiso 1 calc R . . C17 C 0.56492(14) 0.09958(8) 0.28485(9) 0.0243(4) Uani 1 d . . . H17A H 0.5428 0.0591 0.2900 0.037 Uiso 1 calc R . . H17B H 0.6292 0.1001 0.2634 0.037 Uiso 1 calc R . . H17C H 0.5153 0.1211 0.2602 0.037 Uiso 1 calc R . . C18 C 0.67640(14) 0.30154(8) 0.21395(8) 0.0206(3) Uani 1 d . . . C19 C 0.75763(16) 0.26635(9) 0.18017(9) 0.0280(4) Uani 1 d . . . H19A H 0.7382 0.2251 0.1784 0.042 Uiso 1 calc R . . H19B H 0.8211 0.2701 0.2029 0.042 Uiso 1 calc R . . H19C H 0.7653 0.2814 0.1378 0.042 Uiso 1 calc R . . C20 C 0.70729(16) 0.36612(8) 0.21383(9) 0.0259(4) Uani 1 d . . . H20A H 0.7123 0.3799 0.1708 0.039 Uiso 1 calc R . . H20B H 0.7721 0.3704 0.2348 0.039 Uiso 1 calc R . . H20C H 0.6571 0.3892 0.2358 0.039 Uiso 1 calc R . . C21 C 0.57658(15) 0.29552(9) 0.17840(9) 0.0272(4) Uani 1 d . . . H21A H 0.5565 0.2544 0.1774 0.041 Uiso 1 calc R . . H21B H 0.5845 0.3099 0.1357 0.041 Uiso 1 calc R . . H21C H 0.5252 0.3185 0.1994 0.041 Uiso 1 calc R . . C22 C 0.95317(14) 0.45097(8) 0.39461(9) 0.0226(3) Uani 1 d . . . F23 F 1.00664(10) 0.40498(6) 0.37847(8) 0.0489(4) Uani 1 d . . . F24 F 0.93152(11) 0.47897(8) 0.34204(8) 0.0591(5) Uani 1 d . . . F25 F 1.01302(12) 0.48643(8) 0.42655(8) 0.0643(5) Uani 1 d . . . C26 C 0.67332(15) 0.51031(8) 0.53322(9) 0.0235(4) Uani 1 d . . . F27 F 0.61630(11) 0.48849(5) 0.57716(6) 0.0401(3) Uani 1 d . . . F28 F 0.61606(15) 0.54430(7) 0.49813(7) 0.0625(5) Uani 1 d . . . F29 F 0.73765(13) 0.54573(7) 0.56202(9) 0.0655(5) Uani 1 d . . . C31 C 0.68463(12) 0.16352(7) 0.58687(7) 0.0151(3) Uani 1 d . . . C32 C 0.67257(13) 0.11464(7) 0.62771(8) 0.0172(3) Uani 1 d . . . C33 C 0.75316(13) 0.07788(7) 0.63427(8) 0.0185(3) Uani 1 d . . . H33 H 0.7463 0.0452 0.6612 0.022 Uiso 1 calc R . . C34 C 0.84667(13) 0.08532(7) 0.60348(8) 0.0172(3) Uani 1 d . . . C35 C 0.85921(12) 0.13271(7) 0.56525(8) 0.0165(3) Uani 1 d . . . H35 H 0.9211 0.1391 0.5451 0.020 Uiso 1 calc R . . C36 C 0.77854(12) 0.17219(7) 0.55605(7) 0.0143(3) Uani 1 d . . . N37 N 0.77916(10) 0.21959(6) 0.51951(6) 0.0141(2) Uani 1 d . . . C38 C 0.86802(11) 0.23894(7) 0.49127(7) 0.0138(3) Uani 1 d . . . C39 C 0.89161(12) 0.22190(7) 0.43107(7) 0.0150(3) Uani 1 d . . . H39 H 0.8495 0.1955 0.4091 0.018 Uiso 1 calc R . . C40 C 0.97731(12) 0.24380(7) 0.40318(8) 0.0166(3) Uani 1 d . . . C41 C 1.03951(12) 0.28265(7) 0.43463(8) 0.0176(3) Uani 1 d . . . H41 H 1.0971 0.2981 0.4151 0.021 Uiso 1 calc R . . C42 C 1.01586(12) 0.29851(7) 0.49510(8) 0.0180(3) Uani 1 d . . . C43 C 0.93076(12) 0.27735(7) 0.52381(8) 0.0172(3) Uani 1 d . . . H43 H 0.9153 0.2888 0.5651 0.021 Uiso 1 calc R . . C44 C 0.57320(14) 0.10492(8) 0.66120(9) 0.0222(3) Uani 1 d . . . C45 C 0.57856(17) 0.05189(9) 0.70496(11) 0.0343(5) Uani 1 d . . . H45A H 0.5144 0.0471 0.7260 0.052 Uiso 1 calc R . . H45B H 0.6314 0.0581 0.7361 0.052 Uiso 1 calc R . . H45C H 0.5932 0.0167 0.6807 0.052 Uiso 1 calc R . . C46 C 0.54813(16) 0.15868(9) 0.70102(9) 0.0287(4) Uani 1 d . . . H46A H 0.4860 0.1516 0.7236 0.043 Uiso 1 calc R . . H46B H 0.5399 0.1928 0.6740 0.043 Uiso 1 calc R . . H46C H 0.6025 0.1659 0.7309 0.043 Uiso 1 calc R . . C47 C 0.49024(15) 0.09416(10) 0.61278(11) 0.0326(4) Uani 1 d . . . H47A H 0.4264 0.0890 0.6340 0.049 Uiso 1 calc R . . H47B H 0.5056 0.0589 0.5888 0.049 Uiso 1 calc R . . H47C H 0.4857 0.1277 0.5846 0.049 Uiso 1 calc R . . C48 C 0.92845(14) 0.03997(7) 0.61505(8) 0.0210(3) Uani 1 d . . . C49 C 0.88897(16) -0.02096(8) 0.59613(10) 0.0281(4) Uani 1 d . . . H49A H 0.8299 -0.0304 0.6208 0.042 Uiso 1 calc R . . H49B H 0.9409 -0.0503 0.6038 0.042 Uiso 1 calc R . . H49C H 0.8710 -0.0208 0.5518 0.042 Uiso 1 calc R . . C50 C 0.95618(16) 0.04010(9) 0.68470(9) 0.0289(4) Uani 1 d . . . H50A H 0.8976 0.0293 0.7092 0.043 Uiso 1 calc R . . H50B H 0.9787 0.0792 0.6969 0.043 Uiso 1 calc R . . H50C H 1.0099 0.0119 0.6924 0.043 Uiso 1 calc R . . C51 C 1.02256(15) 0.05269(8) 0.57752(10) 0.0272(4) Uani 1 d . . . H51A H 1.0719 0.0219 0.5851 0.041 Uiso 1 calc R . . H51B H 1.0505 0.0904 0.5904 0.041 Uiso 1 calc R . . H51C H 1.0056 0.0539 0.5331 0.041 Uiso 1 calc R . . C52 C 1.00038(13) 0.22376(9) 0.33840(8) 0.0232(4) Uani 1 d . . . F53 F 0.92670(9) 0.23615(7) 0.29838(6) 0.0421(3) Uani 1 d . . . F54 F 1.08374(9) 0.24789(6) 0.31610(5) 0.0329(3) Uani 1 d . . . F55 F 1.01324(11) 0.16558(6) 0.33591(6) 0.0381(3) Uani 1 d . . . C56 C 1.08273(14) 0.33964(8) 0.53062(9) 0.0256(4) Uani 1 d D . . F57 F 1.0440(6) 0.3935(2) 0.5288(4) 0.0423(17) Uani 0.50 d PD A 1 F58 F 1.1722(5) 0.3453(4) 0.5088(5) 0.081(4) Uani 0.50 d PD A 1 F59 F 1.0897(10) 0.3280(4) 0.5901(3) 0.074(4) Uani 0.50 d PD A 1 F57X F 1.0380(7) 0.3839(4) 0.5548(7) 0.064(5) Uani 0.32 d PD A 2 F58X F 1.1543(8) 0.3614(6) 0.4951(5) 0.051(3) Uani 0.32 d PD A 2 F59X F 1.1300(12) 0.3110(5) 0.5746(6) 0.100(8) Uani 0.32 d PD A 2 F57Y F 1.0898(18) 0.3909(5) 0.5070(9) 0.068(7) Uani 0.18 d PD A 3 F58Y F 1.1740(8) 0.3176(9) 0.5345(10) 0.079(9) Uani 0.18 d PD A 3 F59Y F 1.0576(12) 0.3468(10) 0.5902(4) 0.038(4) Uani 0.18 d PD A 3 C61 C 0.62306(12) 0.33415(7) 0.61042(7) 0.0134(3) Uani 1 d . . . C62 C 0.63481(12) 0.36887(7) 0.66512(7) 0.0147(3) Uani 1 d . . . C63 C 0.55045(12) 0.39693(7) 0.68610(7) 0.0160(3) Uani 1 d . . . H63 H 0.5568 0.4205 0.7223 0.019 Uiso 1 calc R . . C64 C 0.45347(12) 0.39312(7) 0.65706(7) 0.0149(3) Uani 1 d . . . C65 C 0.44166(12) 0.35797(7) 0.60572(7) 0.0150(3) Uani 1 d . . . H65 H 0.3779 0.3536 0.5866 0.018 Uiso 1 calc R . . C66 C 0.52557(12) 0.32823(7) 0.58156(7) 0.0136(3) Uani 1 d . . . N67 N 0.52784(10) 0.29573(6) 0.52966(6) 0.0146(3) Uani 1 d . . . C68 C 0.44364(12) 0.28463(7) 0.49112(7) 0.0150(3) Uani 1 d . . . C69 C 0.38167(12) 0.23740(7) 0.50348(8) 0.0178(3) Uani 1 d . . . H69 H 0.3899 0.2156 0.5408 0.021 Uiso 1 calc R . . C70 C 0.30738(12) 0.22240(8) 0.46065(8) 0.0191(3) Uani 1 d . . . C71 C 0.29449(12) 0.25392(8) 0.40580(8) 0.0194(3) Uani 1 d . . . H71 H 0.2450 0.2427 0.3762 0.023 Uiso 1 calc R . . C72 C 0.35523(13) 0.30215(8) 0.39494(8) 0.0194(3) Uani 1 d . . . C73 C 0.42968(12) 0.31777(7) 0.43708(8) 0.0180(3) Uani 1 d . . . H73 H 0.4708 0.3507 0.4293 0.022 Uiso 1 calc R . . C74 C 0.73772(12) 0.37380(7) 0.69677(8) 0.0171(3) Uani 1 d . . . C75 C 0.73262(14) 0.41034(9) 0.75663(9) 0.0271(4) Uani 1 d . . . H75A H 0.7989 0.4120 0.7762 0.041 Uiso 1 calc R . . H75B H 0.6854 0.3923 0.7854 0.041 Uiso 1 calc R . . H75C H 0.7103 0.4500 0.7464 0.041 Uiso 1 calc R . . C76 C 0.77606(13) 0.31243(8) 0.71434(8) 0.0224(3) Uani 1 d . . . H76A H 0.8417 0.3158 0.7345 0.034 Uiso 1 calc R . . H76B H 0.7817 0.2886 0.6766 0.034 Uiso 1 calc R . . H76C H 0.7291 0.2939 0.7430 0.034 Uiso 1 calc R . . C77 C 0.81207(13) 0.40374(8) 0.65249(9) 0.0225(3) Uani 1 d . . . H77A H 0.8782 0.4051 0.6722 0.034 Uiso 1 calc R . . H77B H 0.7894 0.4436 0.6436 0.034 Uiso 1 calc R . . H77C H 0.8158 0.3816 0.6136 0.034 Uiso 1 calc R . . C78 C 0.36866(12) 0.43063(7) 0.68254(7) 0.0159(3) Uani 1 d . . . C79 C 0.26916(12) 0.41823(8) 0.64936(8) 0.0186(3) Uani 1 d . . . H79A H 0.2169 0.4430 0.6671 0.028 Uiso 1 calc R . . H79B H 0.2513 0.3771 0.6549 0.028 Uiso 1 calc R . . H79C H 0.2756 0.4267 0.6049 0.028 Uiso 1 calc R . . C80 C 0.35463(13) 0.41897(8) 0.75236(8) 0.0205(3) Uani 1 d . . . H80A H 0.3046 0.4460 0.7689 0.031 Uiso 1 calc R . . H80B H 0.4182 0.4249 0.7743 0.031 Uiso 1 calc R . . H80C H 0.3321 0.3787 0.7584 0.031 Uiso 1 calc R . . C81 C 0.39522(14) 0.49542(7) 0.67170(9) 0.0217(3) Uani 1 d . . . H81A H 0.3423 0.5203 0.6885 0.032 Uiso 1 calc R . . H81B H 0.4017 0.5027 0.6269 0.032 Uiso 1 calc R . . H81C H 0.4585 0.5045 0.6928 0.032 Uiso 1 calc R . . C82 C 0.24128(14) 0.17093(8) 0.47436(10) 0.0260(4) Uani 1 d . . . F83 F 0.17168(11) 0.18433(6) 0.51625(7) 0.0455(4) Uani 1 d . . . F84 F 0.29161(10) 0.12597(6) 0.49663(9) 0.0546(5) Uani 1 d . . . F85 F 0.19079(12) 0.15317(7) 0.42432(7) 0.0530(4) Uani 1 d . . . C86 C 0.34037(16) 0.33642(9) 0.33600(9) 0.0303(4) Uani 1 d . . . F87 F 0.39431(12) 0.38469(7) 0.33401(7) 0.0482(4) Uani 1 d . . . F88 F 0.36223(17) 0.30563(8) 0.28602(6) 0.0679(5) Uani 1 d . . . F89 F 0.24579(12) 0.35377(9) 0.32927(9) 0.0707(6) Uani 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.01308(10) 0.01079(9) 0.01324(10) -0.00069(7) 0.00128(7) -0.00055(7) O1 0.0173(5) 0.0129(5) 0.0159(5) -0.0022(4) 0.0015(4) -0.0028(4) C1 0.0130(7) 0.0124(7) 0.0180(7) -0.0016(5) 0.0005(5) 0.0006(5) O2 0.0161(5) 0.0140(5) 0.0167(5) 0.0010(4) 0.0032(4) -0.0007(4) C2 0.0152(7) 0.0143(7) 0.0198(8) -0.0043(6) 0.0005(6) 0.0002(6) O3 0.0138(5) 0.0149(5) 0.0152(5) -0.0020(4) 0.0012(4) -0.0005(4) C3 0.0202(8) 0.0167(7) 0.0180(7) -0.0043(6) 0.0000(6) 0.0000(6) C4 0.0190(8) 0.0159(7) 0.0163(7) -0.0004(6) 0.0001(6) 0.0018(6) C5 0.0198(8) 0.0141(7) 0.0161(7) 0.0002(6) -0.0004(6) 0.0004(6) C6 0.0144(7) 0.0121(7) 0.0158(7) -0.0019(5) -0.0006(5) 0.0006(5) N7 0.0147(6) 0.0106(6) 0.0148(6) -0.0017(5) -0.0001(5) -0.0004(5) C8 0.0173(7) 0.0112(7) 0.0136(7) 0.0011(5) -0.0014(5) -0.0006(5) C9 0.0181(7) 0.0127(7) 0.0154(7) 0.0004(5) -0.0005(6) 0.0008(6) C10 0.0172(7) 0.0146(7) 0.0184(7) 0.0031(6) -0.0001(6) -0.0017(6) C11 0.0227(8) 0.0117(7) 0.0187(7) 0.0015(6) -0.0009(6) -0.0020(6) C12 0.0235(8) 0.0120(7) 0.0154(7) -0.0008(5) 0.0009(6) 0.0003(6) C13 0.0202(8) 0.0126(7) 0.0153(7) 0.0008(5) 0.0020(6) -0.0003(6) C14 0.0210(8) 0.0145(7) 0.0225(8) -0.0054(6) 0.0046(6) -0.0038(6) C15 0.0243(9) 0.0265(9) 0.0325(10) -0.0121(8) 0.0096(7) -0.0103(7) C16 0.0327(10) 0.0140(8) 0.0279(9) -0.0014(7) 0.0039(7) 0.0002(7) C17 0.0267(9) 0.0205(8) 0.0259(9) -0.0100(7) 0.0049(7) -0.0074(7) C18 0.0285(9) 0.0183(8) 0.0150(7) -0.0004(6) -0.0012(6) -0.0001(7) C19 0.0357(11) 0.0285(10) 0.0201(8) 0.0000(7) 0.0063(7) 0.0051(8) C20 0.0379(11) 0.0205(8) 0.0192(8) 0.0025(7) -0.0012(7) -0.0028(7) C21 0.0337(10) 0.0270(9) 0.0209(8) 0.0010(7) -0.0072(7) 0.0005(8) C22 0.0209(8) 0.0165(8) 0.0306(9) 0.0032(7) 0.0043(7) -0.0014(6) F23 0.0340(7) 0.0239(6) 0.0894(12) 0.0098(7) 0.0316(7) 0.0057(5) F24 0.0423(8) 0.0799(12) 0.0554(9) 0.0446(9) 0.0249(7) 0.0242(8) F25 0.0458(9) 0.0773(12) 0.0703(11) -0.0284(9) 0.0224(8) -0.0408(9) C26 0.0356(10) 0.0132(7) 0.0219(8) -0.0011(6) 0.0078(7) -0.0015(7) F27 0.0638(9) 0.0201(6) 0.0368(7) -0.0006(5) 0.0300(6) 0.0021(6) F28 0.1053(14) 0.0510(9) 0.0315(7) 0.0072(6) 0.0142(8) 0.0558(10) F29 0.0570(10) 0.0493(9) 0.0907(13) -0.0530(9) 0.0276(9) -0.0231(8) C31 0.0185(7) 0.0124(7) 0.0143(7) -0.0018(5) 0.0014(6) -0.0018(6) C32 0.0208(8) 0.0142(7) 0.0166(7) 0.0000(6) 0.0040(6) -0.0036(6) C33 0.0247(8) 0.0118(7) 0.0190(7) 0.0034(6) 0.0033(6) -0.0016(6) C34 0.0215(8) 0.0131(7) 0.0170(7) 0.0005(6) 0.0016(6) 0.0006(6) C35 0.0169(7) 0.0139(7) 0.0186(7) 0.0008(6) 0.0031(6) 0.0007(6) C36 0.0172(7) 0.0118(7) 0.0138(7) 0.0006(5) 0.0017(5) -0.0011(5) N37 0.0147(6) 0.0120(6) 0.0156(6) 0.0016(5) 0.0031(5) -0.0013(5) C38 0.0130(7) 0.0106(6) 0.0177(7) 0.0022(5) 0.0026(5) 0.0013(5) C39 0.0146(7) 0.0140(7) 0.0165(7) 0.0007(6) 0.0000(6) 0.0003(6) C40 0.0152(7) 0.0176(7) 0.0169(7) 0.0029(6) 0.0020(6) 0.0024(6) C41 0.0127(7) 0.0153(7) 0.0248(8) 0.0041(6) 0.0023(6) 0.0008(6) C42 0.0158(7) 0.0127(7) 0.0255(8) -0.0008(6) -0.0011(6) -0.0012(6) C43 0.0183(8) 0.0147(7) 0.0186(7) -0.0006(6) 0.0012(6) -0.0008(6) C44 0.0230(9) 0.0188(8) 0.0251(9) 0.0035(7) 0.0095(7) -0.0037(7) C45 0.0379(11) 0.0262(10) 0.0393(11) 0.0120(9) 0.0189(9) -0.0021(8) C46 0.0339(10) 0.0271(9) 0.0255(9) 0.0003(7) 0.0147(8) 0.0009(8) C47 0.0239(9) 0.0339(11) 0.0399(11) 0.0003(9) 0.0054(8) -0.0109(8) C48 0.0240(8) 0.0141(7) 0.0250(8) 0.0048(6) 0.0016(7) 0.0023(6) C49 0.0353(11) 0.0139(8) 0.0350(10) 0.0010(7) 0.0049(8) 0.0013(7) C50 0.0317(10) 0.0264(9) 0.0287(10) 0.0100(8) -0.0050(8) 0.0014(8) C51 0.0249(9) 0.0202(8) 0.0368(10) 0.0078(7) 0.0064(8) 0.0063(7) C52 0.0177(8) 0.0337(10) 0.0182(8) 0.0007(7) 0.0028(6) 0.0012(7) F53 0.0249(6) 0.0818(11) 0.0196(6) 0.0028(6) -0.0025(5) 0.0075(6) F54 0.0230(6) 0.0529(8) 0.0229(6) 0.0018(5) 0.0104(4) -0.0051(5) F55 0.0505(8) 0.0339(7) 0.0301(6) -0.0124(5) 0.0114(6) 0.0020(6) C56 0.0227(9) 0.0221(9) 0.0321(10) -0.0026(7) 0.0001(7) -0.0075(7) F57 0.052(4) 0.0164(15) 0.058(5) -0.011(3) -0.020(3) -0.004(2) F58 0.020(2) 0.087(7) 0.136(10) -0.085(7) 0.018(4) -0.021(3) F59 0.111(8) 0.056(6) 0.055(4) 0.033(4) -0.059(4) -0.057(5) F57X 0.035(4) 0.068(9) 0.089(11) -0.062(8) 0.015(6) -0.013(5) F58X 0.038(6) 0.070(7) 0.044(3) -0.007(4) 0.013(4) -0.042(5) F59X 0.158(19) 0.041(6) 0.098(9) 0.028(7) -0.109(11) -0.044(8) F57Y 0.103(17) 0.039(8) 0.060(10) 0.027(7) -0.032(9) -0.057(10) F58Y 0.023(6) 0.063(13) 0.15(2) -0.074(14) -0.033(9) 0.017(8) F59Y 0.041(6) 0.066(11) 0.005(4) -0.012(5) 0.005(4) -0.029(6) C61 0.0155(7) 0.0118(7) 0.0130(7) 0.0006(5) 0.0017(5) -0.0010(5) C62 0.0166(7) 0.0143(7) 0.0132(7) -0.0007(5) -0.0001(5) -0.0017(6) C63 0.0192(8) 0.0150(7) 0.0137(7) -0.0023(5) 0.0004(6) -0.0009(6) C64 0.0155(7) 0.0141(7) 0.0150(7) 0.0004(5) 0.0018(5) -0.0001(6) C65 0.0150(7) 0.0143(7) 0.0158(7) -0.0004(5) 0.0009(5) 0.0002(6) C66 0.0155(7) 0.0119(7) 0.0135(7) 0.0005(5) 0.0006(5) -0.0008(5) N67 0.0133(6) 0.0145(6) 0.0159(6) -0.0032(5) -0.0006(5) -0.0009(5) C68 0.0135(7) 0.0152(7) 0.0162(7) -0.0037(6) 0.0000(5) 0.0015(6) C69 0.0173(7) 0.0178(7) 0.0182(7) -0.0011(6) 0.0016(6) -0.0011(6) C70 0.0151(7) 0.0180(8) 0.0241(8) -0.0047(6) 0.0004(6) -0.0009(6) C71 0.0145(7) 0.0234(8) 0.0201(8) -0.0056(6) -0.0015(6) 0.0012(6) C72 0.0171(8) 0.0215(8) 0.0196(8) -0.0017(6) -0.0016(6) 0.0032(6) C73 0.0170(8) 0.0169(7) 0.0201(8) -0.0008(6) -0.0001(6) -0.0004(6) C74 0.0150(7) 0.0199(8) 0.0165(7) -0.0032(6) -0.0016(6) -0.0013(6) C75 0.0205(9) 0.0376(11) 0.0231(9) -0.0138(8) -0.0051(7) 0.0021(8) C76 0.0198(8) 0.0256(9) 0.0218(8) 0.0021(7) -0.0032(6) 0.0020(7) C77 0.0170(8) 0.0250(9) 0.0256(9) -0.0001(7) -0.0007(6) -0.0064(6) C78 0.0161(7) 0.0150(7) 0.0166(7) -0.0017(6) 0.0016(6) 0.0016(6) C79 0.0166(8) 0.0190(8) 0.0204(8) -0.0015(6) 0.0003(6) 0.0032(6) C80 0.0202(8) 0.0242(8) 0.0171(8) -0.0012(6) 0.0031(6) 0.0026(6) C81 0.0262(9) 0.0147(7) 0.0241(8) -0.0023(6) 0.0002(7) 0.0010(6) C82 0.0201(9) 0.0238(9) 0.0341(10) -0.0010(7) -0.0023(7) -0.0061(7) F83 0.0391(8) 0.0413(8) 0.0566(9) 0.0014(7) 0.0213(7) -0.0137(6) F84 0.0307(7) 0.0250(7) 0.1079(14) 0.0214(8) -0.0136(8) -0.0069(5) F85 0.0635(10) 0.0505(9) 0.0447(8) -0.0019(7) -0.0144(7) -0.0381(8) C86 0.0318(10) 0.0328(10) 0.0260(9) 0.0042(8) -0.0085(8) -0.0026(8) F87 0.0627(10) 0.0440(8) 0.0375(7) 0.0201(6) -0.0173(7) -0.0197(7) F88 0.1346(17) 0.0514(10) 0.0176(6) -0.0006(6) -0.0009(8) 0.0032(10) F89 0.0357(8) 0.0982(15) 0.0778(12) 0.0531(11) -0.0169(8) 0.0069(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 1.8865(11) . ? Co1 O3 1.8885(11) . ? Co1 O2 1.8984(11) . ? Co1 N67 1.9007(14) . ? Co1 N37 1.9133(14) . ? Co1 N7 1.9348(13) . ? O1 C1 1.2987(19) . ? C1 C2 1.435(2) . ? C1 C6 1.440(2) . ? O2 C31 1.301(2) . ? C2 C3 1.376(2) . ? C2 C14 1.534(2) . ? O3 C61 1.3058(19) . ? C3 C4 1.436(2) . ? C4 C5 1.374(2) . ? C4 C18 1.531(2) . ? C5 C6 1.424(2) . ? C6 N7 1.356(2) . ? N7 C8 1.414(2) . ? C8 C13 1.398(2) . ? C8 C9 1.401(2) . ? C9 C10 1.392(2) . ? C10 C11 1.392(2) . ? C10 C22 1.505(2) . ? C11 C12 1.388(2) . ? C12 C13 1.391(2) . ? C12 C26 1.508(2) . ? C14 C17 1.535(2) . ? C14 C15 1.540(2) . ? C14 C16 1.542(3) . ? C18 C20 1.535(3) . ? C18 C21 1.540(3) . ? C18 C19 1.541(3) . ? C22 F23 1.321(2) . ? C22 F25 1.328(2) . ? C22 F24 1.328(2) . ? C26 F27 1.318(2) . ? C26 F28 1.324(2) . ? C26 F29 1.332(2) . ? C31 C32 1.432(2) . ? C31 C36 1.440(2) . ? C32 C33 1.375(2) . ? C32 C44 1.535(2) . ? C33 C34 1.432(2) . ? C34 C35 1.372(2) . ? C34 C48 1.528(2) . ? C35 C36 1.421(2) . ? C36 N37 1.339(2) . ? N37 C38 1.412(2) . ? C38 C39 1.390(2) . ? C38 C43 1.399(2) . ? C39 C40 1.393(2) . ? C40 C41 1.390(2) . ? C40 C52 1.500(2) . ? C41 C42 1.388(2) . ? C42 C43 1.388(2) . ? C42 C56 1.503(2) . ? C44 C47 1.535(3) . ? C44 C45 1.537(3) . ? C44 C46 1.538(3) . ? C48 C51 1.530(3) . ? C48 C50 1.538(3) . ? C48 C49 1.545(3) . ? C52 F53 1.334(2) . ? C52 F54 1.338(2) . ? C52 F55 1.344(2) . ? C56 F57Y 1.282(6) . ? C56 F57X 1.288(6) . ? C56 F58 1.297(5) . ? C56 F59X 1.308(6) . ? C56 F59 1.308(5) . ? C56 F58Y 1.325(7) . ? C56 F58X 1.327(6) . ? C56 F59Y 1.335(6) . ? C56 F57 1.339(4) . ? C61 C62 1.426(2) . ? C61 C66 1.447(2) . ? C62 C63 1.379(2) . ? C62 C74 1.536(2) . ? C63 C64 1.439(2) . ? C64 C65 1.373(2) . ? C64 C78 1.529(2) . ? C65 C66 1.416(2) . ? C66 N67 1.341(2) . ? N67 C68 1.416(2) . ? C68 C69 1.390(2) . ? C68 C73 1.398(2) . ? C69 C70 1.392(2) . ? C70 C71 1.391(2) . ? C70 C82 1.505(2) . ? C71 C72 1.392(2) . ? C72 C73 1.388(2) . ? C72 C86 1.501(3) . ? C74 C75 1.536(2) . ? C74 C76 1.542(2) . ? C74 C77 1.544(2) . ? C78 C79 1.533(2) . ? C78 C80 1.536(2) . ? C78 C81 1.544(2) . ? C82 F84 1.318(2) . ? C82 F85 1.329(2) . ? C82 F83 1.337(2) . ? C86 F88 1.319(3) . ? C86 F87 1.321(2) . ? C86 F89 1.335(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 O3 178.43(5) . . ? O1 Co1 O2 88.23(5) . . ? O3 Co1 O2 90.23(5) . . ? O1 Co1 N67 96.08(5) . . ? O3 Co1 N67 84.17(5) . . ? O2 Co1 N67 87.90(5) . . ? O1 Co1 N37 89.73(5) . . ? O3 Co1 N37 89.80(5) . . ? O2 Co1 N37 84.10(5) . . ? N67 Co1 N37 169.96(6) . . ? O1 Co1 N7 84.11(5) . . ? O3 Co1 N7 97.44(5) . . ? O2 Co1 N7 172.34(5) . . ? N67 Co1 N7 92.82(6) . . ? N37 Co1 N7 95.92(6) . . ? C1 O1 Co1 113.45(10) . . ? O1 C1 C2 122.92(14) . . ? O1 C1 C6 117.13(14) . . ? C2 C1 C6 119.95(14) . . ? C31 O2 Co1 112.86(10) . . ? C3 C2 C1 116.58(15) . . ? C3 C2 C14 123.25(15) . . ? C1 C2 C14 120.17(15) . . ? C61 O3 Co1 112.44(10) . . ? C2 C3 C4 124.42(15) . . ? C5 C4 C3 118.82(15) . . ? C5 C4 C18 123.11(15) . . ? C3 C4 C18 118.06(14) . . ? C4 C5 C6 119.65(15) . . ? N7 C6 C5 126.95(14) . . ? N7 C6 C1 112.75(14) . . ? C5 C6 C1 120.24(14) . . ? C6 N7 C8 121.29(13) . . ? C6 N7 Co1 112.12(10) . . ? C8 N7 Co1 126.49(10) . . ? C13 C8 C9 119.23(14) . . ? C13 C8 N7 119.67(14) . . ? C9 C8 N7 121.08(14) . . ? C10 C9 C8 119.83(15) . . ? C9 C10 C11 121.17(15) . . ? C9 C10 C22 119.80(15) . . ? C11 C10 C22 118.98(15) . . ? C12 C11 C10 118.53(15) . . ? C11 C12 C13 121.28(15) . . ? C11 C12 C26 119.44(15) . . ? C13 C12 C26 119.24(15) . . ? C12 C13 C8 119.94(15) . . ? C2 C14 C17 111.25(14) . . ? C2 C14 C15 109.86(14) . . ? C17 C14 C15 107.86(14) . . ? C2 C14 C16 109.55(14) . . ? C17 C14 C16 108.58(15) . . ? C15 C14 C16 109.72(16) . . ? C4 C18 C20 112.19(14) . . ? C4 C18 C21 108.99(15) . . ? C20 C18 C21 108.56(15) . . ? C4 C18 C19 109.46(14) . . ? C20 C18 C19 108.14(16) . . ? C21 C18 C19 109.48(15) . . ? F23 C22 F25 107.23(17) . . ? F23 C22 F24 106.05(17) . . ? F25 C22 F24 105.71(18) . . ? F23 C22 C10 113.35(15) . . ? F25 C22 C10 112.62(16) . . ? F24 C22 C10 111.36(15) . . ? F27 C26 F28 107.09(17) . . ? F27 C26 F29 105.95(16) . . ? F28 C26 F29 106.04(18) . . ? F27 C26 C12 113.29(14) . . ? F28 C26 C12 112.09(15) . . ? F29 C26 C12 111.88(16) . . ? O2 C31 C32 123.58(15) . . ? O2 C31 C36 116.88(14) . . ? C32 C31 C36 119.53(15) . . ? C33 C32 C31 116.64(15) . . ? C33 C32 C44 123.13(15) . . ? C31 C32 C44 120.23(15) . . ? C32 C33 C34 124.69(15) . . ? C35 C34 C33 118.86(15) . . ? C35 C34 C48 122.90(15) . . ? C33 C34 C48 118.24(14) . . ? C34 C35 C36 119.28(15) . . ? N37 C36 C35 126.02(15) . . ? N37 C36 C31 113.01(14) . . ? C35 C36 C31 120.98(14) . . ? C36 N37 C38 121.03(14) . . ? C36 N37 Co1 112.99(11) . . ? C38 N37 Co1 125.77(10) . . ? C39 C38 C43 120.05(15) . . ? C39 C38 N37 120.73(14) . . ? C43 C38 N37 119.19(14) . . ? C38 C39 C40 119.61(15) . . ? C41 C40 C39 120.94(15) . . ? C41 C40 C52 121.27(15) . . ? C39 C40 C52 117.78(15) . . ? C42 C41 C40 118.78(15) . . ? C41 C42 C43 121.29(15) . . ? C41 C42 C56 119.93(15) . . ? C43 C42 C56 118.78(16) . . ? C42 C43 C38 119.31(15) . . ? C32 C44 C47 109.36(15) . . ? C32 C44 C45 111.42(16) . . ? C47 C44 C45 108.50(17) . . ? C32 C44 C46 109.83(15) . . ? C47 C44 C46 110.17(17) . . ? C45 C44 C46 107.54(16) . . ? C34 C48 C51 112.21(14) . . ? C34 C48 C50 108.89(15) . . ? C51 C48 C50 108.59(16) . . ? C34 C48 C49 109.10(15) . . ? C51 C48 C49 108.36(16) . . ? C50 C48 C49 109.68(15) . . ? F53 C52 F54 107.26(15) . . ? F53 C52 F55 106.23(16) . . ? F54 C52 F55 106.69(15) . . ? F53 C52 C40 112.06(15) . . ? F54 C52 C40 112.65(15) . . ? F55 C52 C40 111.57(15) . . ? F57Y C56 F57X 58.5(9) . . ? F57Y C56 F58 72.2(9) . . ? F57X C56 F58 120.1(7) . . ? F57Y C56 F59X 135.0(9) . . ? F57X C56 F59X 109.0(6) . . ? F58 C56 F59X 82.4(8) . . ? F57Y C56 F59 124.7(8) . . ? F57X C56 F59 78.2(5) . . ? F58 C56 F59 108.3(5) . . ? F59X C56 F59 33.1(7) . . ? F57Y C56 F58Y 107.6(6) . . ? F57X C56 F58Y 134.9(10) . . ? F58 C56 F58Y 37.4(8) . . ? F59X C56 F58Y 47.4(10) . . ? F59 C56 F58Y 78.6(8) . . ? F57Y C56 F58X 51.2(10) . . ? F57X C56 F58X 106.2(5) . . ? F58 C56 F58X 23.1(7) . . ? F59X C56 F58X 104.8(6) . . ? F59 C56 F58X 126.3(8) . . ? F58Y C56 F58X 60.5(10) . . ? F57Y C56 F59Y 106.7(6) . . ? F57X C56 F59Y 52.8(7) . . ? F58 C56 F59Y 125.1(8) . . ? F59X C56 F59Y 59.7(9) . . ? F59 C56 F59Y 26.6(7) . . ? F58Y C56 F59Y 103.1(6) . . ? F58X C56 F59Y 133.9(9) . . ? F57Y C56 F57 34.4(10) . . ? F57X C56 F57 26.7(5) . . ? F58 C56 F57 104.8(4) . . ? F59X C56 F57 131.9(6) . . ? F59 C56 F57 104.0(4) . . ? F58Y C56 F57 135.2(9) . . ? F58X C56 F57 85.4(6) . . ? F59Y C56 F57 79.3(8) . . ? F57Y C56 C42 114.7(6) . . ? F57X C56 C42 114.8(5) . . ? F58 C56 C42 115.3(4) . . ? F59X C56 C42 109.6(6) . . ? F59 C56 C42 113.9(4) . . ? F58Y C56 C42 109.9(7) . . ? F58X C56 C42 111.9(6) . . ? F59Y C56 C42 114.1(7) . . ? F57 C56 C42 109.4(3) . . ? O3 C61 C62 123.67(14) . . ? O3 C61 C66 116.38(13) . . ? C62 C61 C66 119.87(14) . . ? C63 C62 C61 116.35(14) . . ? C63 C62 C74 123.79(14) . . ? C61 C62 C74 119.86(14) . . ? C62 C63 C64 124.71(15) . . ? C65 C64 C63 118.76(15) . . ? C65 C64 C78 122.39(14) . . ? C63 C64 C78 118.78(14) . . ? C64 C65 C66 119.31(15) . . ? N67 C66 C65 126.52(14) . . ? N67 C66 C61 112.41(14) . . ? C65 C66 C61 120.94(14) . . ? C66 N67 C68 124.17(14) . . ? C66 N67 Co1 112.95(11) . . ? C68 N67 Co1 122.60(10) . . ? C69 C68 C73 120.32(15) . . ? C69 C68 N67 120.13(15) . . ? C73 C68 N67 119.21(14) . . ? C68 C69 C70 119.36(16) . . ? C71 C70 C69 120.96(16) . . ? C71 C70 C82 120.19(16) . . ? C69 C70 C82 118.84(16) . . ? C70 C71 C72 118.99(15) . . ? C73 C72 C71 120.85(16) . . ? C73 C72 C86 120.31(16) . . ? C71 C72 C86 118.83(16) . . ? C72 C73 C68 119.47(16) . . ? C75 C74 C62 111.36(14) . . ? C75 C74 C76 107.97(14) . . ? C62 C74 C76 109.71(13) . . ? C75 C74 C77 107.90(15) . . ? C62 C74 C77 109.97(13) . . ? C76 C74 C77 109.89(14) . . ? C64 C78 C79 112.05(13) . . ? C64 C78 C80 110.45(13) . . ? C79 C78 C80 107.97(14) . . ? C64 C78 C81 108.22(13) . . ? C79 C78 C81 107.97(14) . . ? C80 C78 C81 110.15(14) . . ? F84 C82 F85 108.05(18) . . ? F84 C82 F83 107.00(18) . . ? F85 C82 F83 105.16(16) . . ? F84 C82 C70 112.49(15) . . ? F85 C82 C70 112.20(17) . . ? F83 C82 C70 111.54(16) . . ? F88 C86 F87 107.17(19) . . ? F88 C86 F89 106.75(19) . . ? F87 C86 F89 105.47(19) . . ? F88 C86 C72 112.22(18) . . ? F87 C86 C72 113.32(16) . . ? F89 C86 C72 111.45(18) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.934 _refine_diff_density_min -0.608 _refine_diff_density_rms 0.064 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 665851' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H69 Co F6 N3 O3' _chemical_formula_weight 1053.11 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6439(3) _cell_length_b 14.7847(4) _cell_length_c 17.7515(6) _cell_angle_alpha 96.64(1) _cell_angle_beta 94.02(1) _cell_angle_gamma 94.25(1) _cell_volume 2758.39(14) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'opaque parallelepiped' _exptl_crystal_colour black _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.268 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1110 _exptl_absorpt_coefficient_mu 0.378 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.8877 _exptl_absorpt_correction_T_max 0.9582 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method '984 images at 1.0 deg. in \w and 15 sec.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 70658 _diffrn_reflns_av_R_equivalents 0.0465 _diffrn_reflns_av_sigmaI/netI 0.0466 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 31.06 _reflns_number_total 17661 _reflns_number_gt 14099 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO, Nonius Collect Software' _computing_cell_refinement 'DENZO, Nonius Collect Software' _computing_data_reduction 'DENZO, Nonius Collect Software' _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0324P)^2^+1.6633P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17661 _refine_ls_number_parameters 676 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0647 _refine_ls_R_factor_gt 0.0457 _refine_ls_wR_factor_ref 0.1017 _refine_ls_wR_factor_gt 0.0946 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co -0.244561(17) 0.757450(13) 0.745018(10) 0.01277(5) Uani 1 d . . . O1 O -0.35690(9) 0.72732(7) 0.65683(5) 0.01551(19) Uani 1 d . . . C1 C -0.30030(13) 0.69677(9) 0.59762(8) 0.0152(2) Uani 1 d . . . C2 C -0.36352(13) 0.67454(10) 0.52336(8) 0.0171(3) Uani 1 d . . . C3 C -0.28939(14) 0.64915(10) 0.46500(8) 0.0190(3) Uani 1 d . . . H3 H -0.3295 0.6353 0.4150 0.023 Uiso 1 calc R . . C4 C -0.15615(13) 0.64239(10) 0.47495(8) 0.0172(3) Uani 1 d . . . C5 C -0.09661(13) 0.66035(10) 0.54650(8) 0.0166(3) Uani 1 d . . . H5 H -0.0086 0.6543 0.5543 0.020 Uiso 1 calc R . . C6 C -0.16692(13) 0.68813(9) 0.60907(8) 0.0151(2) Uani 1 d . . . N7 N -0.12069(11) 0.70797(8) 0.68213(6) 0.0148(2) Uani 1 d . . . C8 C 0.01092(13) 0.71983(10) 0.70055(8) 0.0156(3) Uani 1 d . . . C9 C 0.06717(14) 0.66714(10) 0.75152(8) 0.0194(3) Uani 1 d . . . H9 H 0.0178 0.6244 0.7756 0.023 Uiso 1 calc R . . C10 C 0.19659(15) 0.67889(11) 0.76591(9) 0.0245(3) Uani 1 d . . . C11 C 0.27324(14) 0.74056(11) 0.73373(10) 0.0249(3) Uani 1 d . . . H11 H 0.3624 0.7466 0.7442 0.030 Uiso 1 calc R . . C12 C 0.21276(14) 0.79290(10) 0.68544(9) 0.0209(3) Uani 1 d . . . C13 C 0.08408(13) 0.78497(10) 0.66781(8) 0.0187(3) Uani 1 d . . . H13 H 0.0461 0.8227 0.6344 0.022 Uiso 1 calc R . . C14 C -0.50539(14) 0.68294(11) 0.51090(8) 0.0216(3) Uani 1 d . . . C15 C -0.57801(15) 0.62107(13) 0.56021(9) 0.0278(3) Uani 1 d . . . H15A H -0.5632 0.5572 0.5449 0.042 Uiso 1 calc R . . H15B H -0.6686 0.6286 0.5532 0.042 Uiso 1 calc R . . H15C H -0.5484 0.6381 0.6139 0.042 Uiso 1 calc R . . C16 C -0.53260(16) 0.78305(12) 0.53190(9) 0.0283(3) Uani 1 d . . . H16A H -0.5015 0.8032 0.5849 0.042 Uiso 1 calc R . . H16B H -0.6239 0.7883 0.5257 0.042 Uiso 1 calc R . . H16C H -0.4897 0.8215 0.4985 0.042 Uiso 1 calc R . . C17 C -0.55487(16) 0.65439(15) 0.42763(9) 0.0340(4) Uani 1 d . . . H17A H -0.5102 0.6928 0.3949 0.051 Uiso 1 calc R . . H17B H -0.6456 0.6618 0.4217 0.051 Uiso 1 calc R . . H17C H -0.5404 0.5903 0.4130 0.051 Uiso 1 calc R . . C18 C -0.08446(14) 0.61818(11) 0.40453(8) 0.0213(3) Uani 1 d . . . C19 C -0.14276(18) 0.52783(13) 0.35982(10) 0.0343(4) Uani 1 d . . . H19A H -0.0972 0.5139 0.3144 0.051 Uiso 1 calc R . . H19B H -0.2319 0.5335 0.3446 0.051 Uiso 1 calc R . . H19C H -0.1364 0.4785 0.3920 0.051 Uiso 1 calc R . . C20 C -0.09413(18) 0.69509(13) 0.35375(10) 0.0326(4) Uani 1 d . . . H20A H -0.0586 0.7530 0.3824 0.049 Uiso 1 calc R . . H20B H -0.1831 0.6999 0.3375 0.049 Uiso 1 calc R . . H20C H -0.0469 0.6814 0.3089 0.049 Uiso 1 calc R . . C21 C 0.05557(16) 0.60861(14) 0.42509(9) 0.0302(4) Uani 1 d . . . H21A H 0.0637 0.5607 0.4585 0.045 Uiso 1 calc R . . H21B H 0.0953 0.6667 0.4514 0.045 Uiso 1 calc R . . H21C H 0.0974 0.5923 0.3786 0.045 Uiso 1 calc R . . F22 F 0.25117(10) 0.62556(8) 0.81350(7) 0.0423(3) Uani 1 d . . . F23 F 0.28323(9) 0.85544(7) 0.65303(6) 0.0296(2) Uani 1 d . . . O31 O -0.19993(9) 0.86962(7) 0.71029(6) 0.01631(19) Uani 1 d . . . C31 C -0.29427(13) 0.92133(9) 0.71092(8) 0.0153(2) Uani 1 d . . . C32 C -0.29857(13) 0.99888(10) 0.67041(8) 0.0185(3) Uani 1 d . . . C33 C -0.40205(14) 1.04838(10) 0.67874(8) 0.0196(3) Uani 1 d . . . H33 H -0.4076 1.0998 0.6515 0.024 Uiso 1 calc R . . C34 C -0.50214(13) 1.02793(10) 0.72556(8) 0.0169(3) Uani 1 d . . . C35 C -0.49426(13) 0.95569(9) 0.76726(8) 0.0156(3) Uani 1 d . . . H35 H -0.5568 0.9431 0.8011 0.019 Uiso 1 calc R . . C36 C -0.39212(13) 0.89999(9) 0.75940(7) 0.0147(2) Uani 1 d . . . N37 N -0.37538(11) 0.82285(8) 0.79270(6) 0.0139(2) Uani 1 d . . . C38 C -0.42660(12) 0.80877(9) 0.86176(7) 0.0144(2) Uani 1 d . . . C39 C -0.47640(13) 0.72095(10) 0.87142(8) 0.0160(3) Uani 1 d . . . H39 H -0.4797 0.6723 0.8312 0.019 Uiso 1 calc R . . C40 C -0.52051(14) 0.70681(10) 0.94056(8) 0.0189(3) Uani 1 d . . . C41 C -0.51813(15) 0.77415(11) 1.00120(8) 0.0215(3) Uani 1 d . . . H41 H -0.5491 0.7624 1.0483 0.026 Uiso 1 calc R . . C42 C -0.46802(15) 0.85981(10) 0.98937(8) 0.0198(3) Uani 1 d . . . C43 C -0.42219(13) 0.87973(10) 0.92198(8) 0.0169(3) Uani 1 d . . . H43 H -0.3886 0.9397 0.9164 0.020 Uiso 1 calc R . . C44 C -0.19117(14) 1.02276(11) 0.62085(9) 0.0240(3) Uani 1 d . . . C45 C -0.17940(16) 0.94246(13) 0.55928(9) 0.0303(4) Uani 1 d . . . H45A H -0.1583 0.8886 0.5835 0.045 Uiso 1 calc R . . H45B H -0.1126 0.9589 0.5269 0.045 Uiso 1 calc R . . H45C H -0.2598 0.9287 0.5282 0.045 Uiso 1 calc R . . C46 C -0.06639(15) 1.04410(12) 0.67120(11) 0.0300(4) Uani 1 d . . . H46A H -0.0474 0.9906 0.6964 0.045 Uiso 1 calc R . . H46B H -0.0745 1.0960 0.7097 0.045 Uiso 1 calc R . . H46C H 0.0022 1.0593 0.6396 0.045 Uiso 1 calc R . . C47 C -0.21637(18) 1.10670(14) 0.58051(13) 0.0400(5) Uani 1 d . . . H47A H -0.1466 1.1200 0.5492 0.060 Uiso 1 calc R . . H47B H -0.2230 1.1594 0.6185 0.060 Uiso 1 calc R . . H47C H -0.2956 1.0944 0.5481 0.060 Uiso 1 calc R . . C48 C -0.61401(14) 1.08738(10) 0.72570(8) 0.0189(3) Uani 1 d . . . C49 C -0.67369(15) 1.08499(11) 0.64402(9) 0.0235(3) Uani 1 d . . . H49A H -0.7455 1.1228 0.6442 0.035 Uiso 1 calc R . . H49B H -0.7030 1.0219 0.6238 0.035 Uiso 1 calc R . . H49C H -0.6107 1.1088 0.6120 0.035 Uiso 1 calc R . . C50 C -0.56678(17) 1.18633(11) 0.75685(10) 0.0273(3) Uani 1 d . . . H50A H -0.5300 1.1883 0.8092 0.041 Uiso 1 calc R . . H50B H -0.6378 1.2249 0.7560 0.041 Uiso 1 calc R . . H50C H -0.5024 1.2089 0.7252 0.041 Uiso 1 calc R . . C51 C -0.71624(15) 1.05515(11) 0.77538(9) 0.0232(3) Uani 1 d . . . H51A H -0.6803 1.0580 0.8280 0.035 Uiso 1 calc R . . H51B H -0.7479 0.9921 0.7565 0.035 Uiso 1 calc R . . H51C H -0.7860 1.0948 0.7734 0.035 Uiso 1 calc R . . F52 F -0.56941(10) 0.62173(6) 0.94950(5) 0.0285(2) Uani 1 d . . . F53 F -0.46302(10) 0.92765(6) 1.04794(5) 0.0279(2) Uani 1 d . . . O61 O -0.28638(9) 0.63973(7) 0.77133(5) 0.01554(19) Uani 1 d . . . C61 C -0.24172(13) 0.62852(9) 0.83932(7) 0.0146(2) Uani 1 d . . . C62 C -0.26621(13) 0.54544(9) 0.87128(8) 0.0159(3) Uani 1 d . . . C63 C -0.23298(13) 0.54808(10) 0.94784(8) 0.0170(3) Uani 1 d . . . H63 H -0.2522 0.4945 0.9711 0.020 Uiso 1 calc R . . C64 C -0.17131(13) 0.62626(10) 0.99474(8) 0.0164(3) Uani 1 d . . . C65 C -0.13614(13) 0.70275(10) 0.96163(8) 0.0164(3) Uani 1 d . . . H65 H -0.0906 0.7540 0.9912 0.020 Uiso 1 calc R . . C66 C -0.16836(12) 0.70465(9) 0.88265(7) 0.0141(2) Uani 1 d . . . N67 N -0.14392(11) 0.77494(8) 0.84175(6) 0.0146(2) Uani 1 d . . . C68 C -0.05970(13) 0.85075(10) 0.87163(8) 0.0169(3) Uani 1 d . . . C69 C -0.09541(15) 0.93924(10) 0.86803(8) 0.0206(3) Uani 1 d . . . H69 H -0.1767 0.9492 0.8465 0.025 Uiso 1 calc R . . C70 C -0.00991(17) 1.01178(11) 0.89645(9) 0.0255(3) Uani 1 d . . . C71 C 0.10943(16) 1.00260(12) 0.92807(9) 0.0274(3) Uani 1 d . . . H71 H 0.1665 1.0539 0.9471 0.033 Uiso 1 calc R . . C72 C 0.14085(15) 0.91450(12) 0.93035(10) 0.0273(3) Uani 1 d . . . C73 C 0.06074(14) 0.83790(11) 0.90338(9) 0.0221(3) Uani 1 d . . . H73 H 0.0868 0.7782 0.9063 0.027 Uiso 1 calc R . . C74 C -0.32543(14) 0.45980(10) 0.82069(8) 0.0191(3) Uani 1 d . . . C75 C -0.45771(15) 0.47495(11) 0.78545(9) 0.0246(3) Uani 1 d . . . H75A H -0.5112 0.4944 0.8260 0.037 Uiso 1 calc R . . H75B H -0.4958 0.4178 0.7567 0.037 Uiso 1 calc R . . H75C H -0.4501 0.5223 0.7513 0.037 Uiso 1 calc R . . C76 C -0.23894(15) 0.43574(11) 0.75673(9) 0.0228(3) Uani 1 d . . . H76A H -0.2298 0.4869 0.7264 0.034 Uiso 1 calc R . . H76B H -0.2762 0.3810 0.7240 0.034 Uiso 1 calc R . . H76C H -0.1557 0.4240 0.7790 0.034 Uiso 1 calc R . . C77 C -0.33935(19) 0.37857(11) 0.86664(9) 0.0300(4) Uani 1 d . . . H77A H -0.2566 0.3685 0.8906 0.045 Uiso 1 calc R . . H77B H -0.3725 0.3237 0.8327 0.045 Uiso 1 calc R . . H77C H -0.3978 0.3916 0.9060 0.045 Uiso 1 calc R . . C78 C -0.15039(14) 0.62166(10) 1.08024(8) 0.0189(3) Uani 1 d . . . C79 C -0.28010(17) 0.61027(13) 1.11244(9) 0.0295(4) Uani 1 d . . . H79A H -0.2685 0.6071 1.1673 0.044 Uiso 1 calc R . . H79B H -0.3266 0.5539 1.0874 0.044 Uiso 1 calc R . . H79C H -0.3280 0.6626 1.1032 0.044 Uiso 1 calc R . . C80 C -0.0776(2) 0.70756(13) 1.12199(9) 0.0344(4) Uani 1 d . . . H80A H 0.0057 0.7154 1.1022 0.052 Uiso 1 calc R . . H80B H -0.0671 0.7019 1.1765 0.052 Uiso 1 calc R . . H80C H -0.1245 0.7607 1.1142 0.052 Uiso 1 calc R . . C81 C -0.07741(18) 0.53885(13) 1.09533(10) 0.0312(4) Uani 1 d . . . H81A H 0.0061 0.5455 1.0757 0.047 Uiso 1 calc R . . H81B H -0.1243 0.4829 1.0697 0.047 Uiso 1 calc R . . H81C H -0.0675 0.5354 1.1502 0.047 Uiso 1 calc R . . F82 F -0.04680(12) 1.09721(7) 0.89407(7) 0.0398(3) Uani 1 d . . . F83 F 0.25731(10) 0.90152(8) 0.96127(8) 0.0458(3) Uani 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.01391(9) 0.01470(9) 0.00995(8) 0.00287(6) 0.00036(6) 0.00126(6) O1 0.0146(4) 0.0216(5) 0.0103(4) 0.0017(4) 0.0000(3) 0.0024(4) C1 0.0168(6) 0.0167(6) 0.0124(6) 0.0033(5) 0.0009(5) 0.0013(5) C2 0.0170(6) 0.0215(7) 0.0131(6) 0.0041(5) -0.0007(5) 0.0030(5) C3 0.0205(7) 0.0233(7) 0.0126(6) 0.0011(5) -0.0010(5) 0.0027(5) C4 0.0199(6) 0.0180(6) 0.0142(6) 0.0020(5) 0.0030(5) 0.0032(5) C5 0.0168(6) 0.0185(6) 0.0150(6) 0.0024(5) 0.0021(5) 0.0038(5) C6 0.0173(6) 0.0159(6) 0.0124(6) 0.0026(5) 0.0005(5) 0.0020(5) N7 0.0136(5) 0.0180(6) 0.0129(5) 0.0024(4) 0.0002(4) 0.0022(4) C8 0.0157(6) 0.0179(6) 0.0126(6) -0.0013(5) 0.0001(5) 0.0024(5) C9 0.0191(7) 0.0192(7) 0.0197(7) 0.0025(5) -0.0022(5) 0.0028(5) C10 0.0212(7) 0.0232(8) 0.0284(8) 0.0029(6) -0.0080(6) 0.0057(6) C11 0.0151(7) 0.0270(8) 0.0301(8) -0.0030(6) -0.0043(6) 0.0018(6) C12 0.0183(7) 0.0212(7) 0.0215(7) -0.0024(6) 0.0031(5) -0.0021(5) C13 0.0177(6) 0.0211(7) 0.0172(6) 0.0024(5) 0.0002(5) 0.0018(5) C14 0.0161(6) 0.0348(8) 0.0137(6) 0.0033(6) -0.0020(5) 0.0043(6) C15 0.0187(7) 0.0397(10) 0.0237(8) 0.0033(7) -0.0009(6) -0.0035(7) C16 0.0255(8) 0.0403(10) 0.0224(7) 0.0100(7) 0.0014(6) 0.0155(7) C17 0.0221(8) 0.0613(13) 0.0172(7) 0.0007(8) -0.0050(6) 0.0058(8) C18 0.0234(7) 0.0265(8) 0.0146(6) 0.0010(6) 0.0048(5) 0.0060(6) C19 0.0389(10) 0.0350(10) 0.0266(8) -0.0098(7) 0.0076(7) 0.0038(8) C20 0.0388(10) 0.0423(10) 0.0208(8) 0.0123(7) 0.0102(7) 0.0099(8) C21 0.0260(8) 0.0470(11) 0.0196(7) 0.0022(7) 0.0081(6) 0.0122(7) F22 0.0271(5) 0.0418(6) 0.0591(7) 0.0239(6) -0.0185(5) 0.0028(5) F23 0.0223(5) 0.0338(5) 0.0317(5) 0.0042(4) 0.0050(4) -0.0076(4) O31 0.0153(4) 0.0180(5) 0.0169(5) 0.0064(4) 0.0026(4) 0.0023(4) C31 0.0147(6) 0.0176(6) 0.0138(6) 0.0036(5) 0.0001(5) 0.0019(5) C32 0.0175(6) 0.0199(7) 0.0193(6) 0.0090(5) 0.0002(5) 0.0008(5) C33 0.0199(7) 0.0190(7) 0.0211(7) 0.0096(6) -0.0007(5) 0.0003(5) C34 0.0174(6) 0.0167(6) 0.0163(6) 0.0027(5) -0.0025(5) 0.0017(5) C35 0.0159(6) 0.0168(6) 0.0143(6) 0.0025(5) 0.0004(5) 0.0014(5) C36 0.0173(6) 0.0151(6) 0.0117(6) 0.0033(5) -0.0007(5) 0.0003(5) N37 0.0155(5) 0.0147(5) 0.0122(5) 0.0034(4) 0.0016(4) 0.0022(4) C38 0.0143(6) 0.0178(6) 0.0118(6) 0.0039(5) 0.0005(5) 0.0027(5) C39 0.0173(6) 0.0173(6) 0.0134(6) 0.0028(5) 0.0010(5) 0.0007(5) C40 0.0217(7) 0.0180(7) 0.0178(6) 0.0064(5) 0.0029(5) -0.0009(5) C41 0.0269(7) 0.0259(8) 0.0133(6) 0.0061(6) 0.0057(5) 0.0033(6) C42 0.0256(7) 0.0215(7) 0.0124(6) 0.0004(5) 0.0006(5) 0.0060(6) C43 0.0198(6) 0.0164(6) 0.0147(6) 0.0023(5) 0.0011(5) 0.0023(5) C44 0.0185(7) 0.0281(8) 0.0295(8) 0.0179(7) 0.0048(6) 0.0032(6) C45 0.0273(8) 0.0448(10) 0.0226(8) 0.0154(7) 0.0072(6) 0.0057(7) C46 0.0195(7) 0.0299(9) 0.0422(10) 0.0150(8) 0.0026(7) -0.0029(6) C47 0.0289(9) 0.0460(11) 0.0555(12) 0.0388(10) 0.0149(8) 0.0093(8) C48 0.0200(7) 0.0186(7) 0.0183(6) 0.0032(5) -0.0006(5) 0.0040(5) C49 0.0226(7) 0.0282(8) 0.0210(7) 0.0073(6) -0.0012(6) 0.0069(6) C50 0.0327(9) 0.0183(7) 0.0303(8) 0.0009(6) 0.0002(7) 0.0037(6) C51 0.0215(7) 0.0266(8) 0.0230(7) 0.0053(6) 0.0032(6) 0.0076(6) F52 0.0415(6) 0.0217(5) 0.0230(5) 0.0073(4) 0.0095(4) -0.0069(4) F53 0.0465(6) 0.0235(5) 0.0134(4) -0.0025(3) 0.0044(4) 0.0058(4) O61 0.0179(5) 0.0168(5) 0.0118(4) 0.0031(4) -0.0007(4) 0.0007(4) C61 0.0149(6) 0.0172(6) 0.0116(6) 0.0017(5) 0.0003(5) 0.0025(5) C62 0.0180(6) 0.0149(6) 0.0145(6) 0.0021(5) 0.0007(5) -0.0003(5) C63 0.0209(7) 0.0159(6) 0.0142(6) 0.0034(5) 0.0009(5) 0.0000(5) C64 0.0188(6) 0.0179(6) 0.0124(6) 0.0018(5) -0.0002(5) 0.0017(5) C65 0.0190(6) 0.0166(6) 0.0129(6) 0.0010(5) -0.0013(5) 0.0003(5) C66 0.0145(6) 0.0150(6) 0.0127(6) 0.0020(5) 0.0006(5) 0.0015(5) N67 0.0161(5) 0.0147(5) 0.0125(5) 0.0011(4) 0.0000(4) 0.0000(4) C68 0.0191(6) 0.0187(7) 0.0123(6) 0.0017(5) 0.0012(5) -0.0023(5) C69 0.0261(7) 0.0174(7) 0.0177(7) 0.0033(5) -0.0009(5) -0.0023(6) C70 0.0368(9) 0.0177(7) 0.0211(7) 0.0033(6) 0.0026(6) -0.0046(6) C71 0.0291(8) 0.0268(8) 0.0232(8) -0.0011(6) 0.0025(6) -0.0121(6) C72 0.0170(7) 0.0358(9) 0.0267(8) -0.0006(7) -0.0015(6) -0.0043(6) C73 0.0196(7) 0.0237(7) 0.0221(7) 0.0004(6) -0.0003(6) 0.0009(6) C74 0.0258(7) 0.0172(7) 0.0133(6) 0.0015(5) -0.0003(5) -0.0036(5) C75 0.0234(7) 0.0253(8) 0.0228(7) -0.0012(6) 0.0008(6) -0.0057(6) C76 0.0289(8) 0.0201(7) 0.0180(7) -0.0026(6) 0.0001(6) 0.0016(6) C77 0.0496(11) 0.0181(7) 0.0200(7) 0.0032(6) -0.0019(7) -0.0093(7) C78 0.0257(7) 0.0198(7) 0.0106(6) 0.0027(5) -0.0012(5) -0.0006(6) C79 0.0338(9) 0.0386(10) 0.0163(7) 0.0031(7) 0.0057(6) 0.0013(7) C80 0.0529(11) 0.0321(9) 0.0147(7) 0.0039(6) -0.0062(7) -0.0138(8) C81 0.0401(10) 0.0347(9) 0.0199(7) 0.0084(7) -0.0048(7) 0.0094(8) F82 0.0562(7) 0.0157(5) 0.0445(6) 0.0032(4) -0.0077(5) -0.0051(5) F83 0.0207(5) 0.0485(7) 0.0616(8) -0.0076(6) -0.0132(5) -0.0033(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 Co1 O31 1.8753(10) . ? Co1 O61 1.8836(10) . ? Co1 O1 1.8911(10) . ? Co1 N7 1.9184(12) . ? Co1 N67 1.9394(12) . ? Co1 N37 1.9406(12) . ? O1 C1 1.3005(16) . ? C1 C2 1.4288(19) . ? C1 C6 1.4372(19) . ? C2 C3 1.380(2) . ? C2 C14 1.527(2) . ? C3 C4 1.429(2) . ? C4 C5 1.3673(19) . ? C4 C18 1.531(2) . ? C5 C6 1.4210(19) . ? C6 N7 1.3459(17) . ? N7 C8 1.4092(18) . ? C8 C9 1.3929(19) . ? C8 C13 1.398(2) . ? C9 C10 1.378(2) . ? C10 F22 1.3515(18) . ? C10 C11 1.378(2) . ? C11 C12 1.378(2) . ? C12 F23 1.3525(17) . ? C12 C13 1.377(2) . ? C14 C17 1.534(2) . ? C14 C16 1.538(2) . ? C14 C15 1.541(2) . ? C18 C21 1.530(2) . ? C18 C20 1.535(2) . ? C18 C19 1.537(2) . ? O31 C31 1.3062(17) . ? C31 C32 1.4238(19) . ? C31 C36 1.4369(18) . ? C32 C33 1.374(2) . ? C32 C44 1.536(2) . ? C33 C34 1.432(2) . ? C34 C35 1.3722(19) . ? C34 C48 1.532(2) . ? C35 C36 1.4166(19) . ? C36 N37 1.3615(17) . ? N37 C38 1.4068(17) . ? C38 C39 1.3994(19) . ? C38 C43 1.4042(19) . ? C39 C40 1.3770(19) . ? C40 F52 1.3560(16) . ? C40 C41 1.377(2) . ? C41 C42 1.382(2) . ? C42 F53 1.3538(17) . ? C42 C43 1.3776(19) . ? C44 C47 1.534(2) . ? C44 C45 1.537(3) . ? C44 C46 1.539(2) . ? C48 C51 1.531(2) . ? C48 C49 1.537(2) . ? C48 C50 1.537(2) . ? O61 C61 1.2990(16) . ? C61 C62 1.4259(19) . ? C61 C66 1.4331(19) . ? C62 C63 1.3755(19) . ? C62 C74 1.532(2) . ? C63 C64 1.431(2) . ? C64 C65 1.3734(19) . ? C64 C78 1.5286(19) . ? C65 C66 1.4237(18) . ? C66 N67 1.3548(17) . ? N67 C68 1.4099(18) . ? C68 C69 1.396(2) . ? C68 C73 1.399(2) . ? C69 C70 1.378(2) . ? C70 F82 1.3544(19) . ? C70 C71 1.375(2) . ? C71 C72 1.373(3) . ? C72 F83 1.3561(19) . ? C72 C73 1.383(2) . ? C74 C77 1.532(2) . ? C74 C76 1.538(2) . ? C74 C75 1.543(2) . ? C78 C80 1.523(2) . ? C78 C79 1.536(2) . ? C78 C81 1.537(2) . ? 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 O31 Co1 O61 174.89(4) . . ? O31 Co1 O1 88.55(4) . . ? O61 Co1 O1 88.28(4) . . ? O31 Co1 N7 86.47(5) . . ? O61 Co1 N7 89.25(5) . . ? O1 Co1 N7 84.68(5) . . ? O31 Co1 N67 99.23(5) . . ? O61 Co1 N67 84.16(5) . . ? O1 Co1 N67 171.70(4) . . ? N7 Co1 N67 98.61(5) . . ? O31 Co1 N37 84.08(5) . . ? O61 Co1 N37 99.85(5) . . ? O1 Co1 N37 88.66(5) . . ? N7 Co1 N37 168.57(5) . . ? N67 Co1 N37 89.26(5) . . ? C1 O1 Co1 112.68(9) . . ? O1 C1 C2 123.23(12) . . ? O1 C1 C6 116.83(12) . . ? C2 C1 C6 119.92(12) . . ? C3 C2 C1 116.70(13) . . ? C3 C2 C14 123.08(13) . . ? C1 C2 C14 120.18(12) . . ? C2 C3 C4 124.16(13) . . ? C5 C4 C3 119.04(13) . . ? C5 C4 C18 122.31(13) . . ? C3 C4 C18 118.62(12) . . ? C4 C5 C6 119.74(13) . . ? N7 C6 C5 126.01(13) . . ? N7 C6 C1 113.61(12) . . ? C5 C6 C1 120.37(12) . . ? C6 N7 C8 120.13(11) . . ? C6 N7 Co1 111.57(9) . . ? C8 N7 Co1 124.78(9) . . ? C9 C8 C13 120.42(13) . . ? C9 C8 N7 119.94(13) . . ? C13 C8 N7 119.64(12) . . ? C10 C9 C8 117.93(14) . . ? F22 C10 C9 117.73(14) . . ? F22 C10 C11 118.39(14) . . ? C9 C10 C11 123.87(14) . . ? C12 C11 C10 115.98(14) . . ? F23 C12 C13 117.79(14) . . ? F23 C12 C11 118.51(13) . . ? C13 C12 C11 123.70(14) . . ? C12 C13 C8 118.05(14) . . ? C2 C14 C17 111.88(13) . . ? C2 C14 C16 109.26(13) . . ? C17 C14 C16 107.75(14) . . ? C2 C14 C15 110.12(12) . . ? C17 C14 C15 107.78(14) . . ? C16 C14 C15 110.01(13) . . ? C21 C18 C4 112.19(12) . . ? C21 C18 C20 108.25(14) . . ? C4 C18 C20 108.36(13) . . ? C21 C18 C19 108.40(14) . . ? C4 C18 C19 110.35(13) . . ? C20 C18 C19 109.23(14) . . ? C31 O31 Co1 111.29(8) . . ? O31 C31 C32 123.04(12) . . ? O31 C31 C36 116.43(12) . . ? C32 C31 C36 120.40(12) . . ? C33 C32 C31 116.25(13) . . ? C33 C32 C44 123.85(13) . . ? C31 C32 C44 119.89(13) . . ? C32 C33 C34 124.63(13) . . ? C35 C34 C33 118.75(13) . . ? C35 C34 C48 123.16(13) . . ? C33 C34 C48 118.09(12) . . ? C34 C35 C36 119.46(13) . . ? N37 C36 C35 126.52(12) . . ? N37 C36 C31 113.08(12) . . ? C35 C36 C31 120.39(12) . . ? C36 N37 C38 121.64(12) . . ? C36 N37 Co1 109.64(9) . . ? C38 N37 Co1 127.15(9) . . ? C39 C38 C43 119.88(12) . . ? C39 C38 N37 118.82(12) . . ? C43 C38 N37 121.21(12) . . ? C40 C39 C38 118.42(13) . . ? F52 C40 C41 118.01(12) . . ? F52 C40 C39 118.21(13) . . ? C41 C40 C39 123.78(13) . . ? C40 C41 C42 115.98(13) . . ? F53 C42 C43 118.41(13) . . ? F53 C42 C41 117.71(13) . . ? C43 C42 C41 123.87(14) . . ? C42 C43 C38 118.06(13) . . ? C47 C44 C32 111.40(13) . . ? C47 C44 C45 107.66(15) . . ? C32 C44 C45 109.87(13) . . ? C47 C44 C46 108.25(14) . . ? C32 C44 C46 109.47(13) . . ? C45 C44 C46 110.16(14) . . ? C51 C48 C34 112.37(12) . . ? C51 C48 C49 108.42(12) . . ? C34 C48 C49 109.51(12) . . ? C51 C48 C50 108.03(13) . . ? C34 C48 C50 109.21(12) . . ? C49 C48 C50 109.26(13) . . ? C61 O61 Co1 113.36(9) . . ? O61 C61 C62 122.31(12) . . ? O61 C61 C66 117.13(12) . . ? C62 C61 C66 120.54(12) . . ? C63 C62 C61 116.18(12) . . ? C63 C62 C74 123.82(12) . . ? C61 C62 C74 120.00(12) . . ? C62 C63 C64 124.25(13) . . ? C65 C64 C63 118.94(12) . . ? C65 C64 C78 122.77(13) . . ? C63 C64 C78 118.27(12) . . ? C64 C65 C66 119.52(13) . . ? N67 C66 C65 127.07(12) . . ? N67 C66 C61 113.05(12) . . ? C65 C66 C61 119.75(12) . . ? C66 N67 C68 121.16(11) . . ? C66 N67 Co1 111.15(9) . . ? C68 N67 Co1 127.60(9) . . ? C69 C68 C73 119.68(13) . . ? C69 C68 N67 119.94(13) . . ? C73 C68 N67 120.37(13) . . ? C70 C69 C68 118.43(15) . . ? F82 C70 C71 118.21(14) . . ? F82 C70 C69 117.79(15) . . ? C71 C70 C69 123.99(15) . . ? C72 C71 C70 115.71(14) . . ? F83 C72 C71 118.15(15) . . ? F83 C72 C73 117.80(16) . . ? C71 C72 C73 124.05(15) . . ? C72 C73 C68 118.13(15) . . ? C62 C74 C77 110.79(12) . . ? C62 C74 C76 108.93(12) . . ? C77 C74 C76 108.46(13) . . ? C62 C74 C75 111.33(12) . . ? C77 C74 C75 107.93(13) . . ? C76 C74 C75 109.35(12) . . ? C80 C78 C64 112.29(12) . . ? C80 C78 C79 108.68(14) . . ? C64 C78 C79 108.36(12) . . ? C80 C78 C81 108.61(14) . . ? C64 C78 C81 110.35(12) . . ? C79 C78 C81 108.48(13) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 31.06 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.424 _refine_diff_density_min -0.508 _refine_diff_density_rms 0.057 #===END data_6 _database_code_depnum_ccdc_archive 'CCDC 665852' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C84 H123 Ga N3 O3' _chemical_formula_weight 1292.57 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' _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 16.4504(3) _cell_length_b 14.6410(3) _cell_length_c 33.8237(6) _cell_angle_alpha 90.00 _cell_angle_beta 96.57(1) _cell_angle_gamma 90.00 _cell_volume 8092.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 233803 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 28.28 _exptl_crystal_description 'opaque block' _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.061 _exptl_crystal_density_method ? _exptl_crystal_F_000 2812 _exptl_absorpt_coefficient_mu 0.385 _exptl_absorpt_correction_type None _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius Kappa-CCD' _diffrn_measurement_method '2267 images at 0.5 deg. in /w and 22 sec.' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 72722 _diffrn_reflns_av_R_equivalents 0.0616 _diffrn_reflns_av_sigmaI/netI 0.0458 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 28.35 _reflns_number_total 19839 _reflns_number_observed 16827 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Nonius Collect Software' _computing_cell_refinement 'Nonius Collect Software' _computing_data_reduction 'Nonius Collect Software' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 29 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0388P)^2^+5.6927P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 19810 _refine_ls_number_parameters 820 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0554 _refine_ls_R_factor_obs 0.0443 _refine_ls_wR_factor_all 0.1089 _refine_ls_wR_factor_obs 0.1029 _refine_ls_goodness_of_fit_all 1.031 _refine_ls_goodness_of_fit_obs 1.064 _refine_ls_restrained_S_all 1.034 _refine_ls_restrained_S_obs 1.064 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ga1 Ga 0.265782(10) 1.282835(11) -0.091894(5) 0.01281(5) Uani 1 d . . O1 O 0.30241(7) 1.39980(7) -0.06706(3) 0.0162(2) Uani 1 d . . C1 C 0.31997(9) 1.39481(10) -0.02884(4) 0.0153(3) Uani 1 d . . C2 C 0.33233(10) 1.47362(11) -0.00420(5) 0.0198(3) Uani 1 d . . C3 C 0.35022(10) 1.45959(11) 0.03611(5) 0.0212(3) Uani 1 d . . H3 H 0.35776(10) 1.51175(11) 0.05283(5) 0.025 Uiso 1 calc R . C4 C 0.35816(9) 1.37170(11) 0.05437(4) 0.0169(3) Uani 1 d . . C5 C 0.34751(9) 1.29573(10) 0.03072(4) 0.0163(3) Uani 1 d . . H5 H 0.35402(9) 1.23676(10) 0.04237(4) 0.020 Uiso 1 calc R . C6 C 0.32683(9) 1.30420(10) -0.01106(4) 0.0147(3) Uani 1 d . . N7 N 0.31363(8) 1.23608(8) -0.03741(4) 0.0141(2) Uani 1 d . . C8 C 0.31583(9) 1.14277(10) -0.02634(4) 0.0157(3) Uani 1 d . . C9 C 0.27177(10) 1.10833(11) 0.00296(5) 0.0185(3) Uani 1 d . . H9 H 0.23871(10) 1.14816(11) 0.01650(5) 0.022 Uiso 1 calc R . C10 C 0.27563(10) 1.01526(11) 0.01277(5) 0.0201(3) Uani 1 d . . C11 C 0.32325(10) 0.95868(11) -0.00827(5) 0.0203(3) Uani 1 d . . H11 H 0.32599(10) 0.89544(11) -0.00197(5) 0.024 Uiso 1 calc R . C12 C 0.36741(9) 0.99147(10) -0.03843(5) 0.0178(3) Uani 1 d . . C13 C 0.36283(9) 1.08397(10) -0.04726(5) 0.0164(3) Uani 1 d . . H13 H 0.39185(9) 1.10773(10) -0.06770(5) 0.020 Uiso 1 calc R . C14 C 0.32653(13) 1.56935(11) -0.02283(5) 0.0294(4) Uani 1 d . . C15 C 0.3388(2) 1.64450(13) 0.00901(6) 0.0509(7) Uani 1 d . . H15A H 0.3924(2) 1.63690(13) 0.02457(6) 0.076 Uiso 1 calc R . H15B H 0.2958(2) 1.64004(13) 0.02669(6) 0.076 Uiso 1 calc R . H15C H 0.3362(2) 1.70449(13) -0.00393(6) 0.076 Uiso 1 calc R . C16 C 0.39412(14) 1.57954(13) -0.05038(6) 0.0357(5) Uani 1 d . . H16A H 0.44767(14) 1.57016(13) -0.03501(6) 0.054 Uiso 1 calc R . H16B H 0.39173(14) 1.64094(13) -0.06199(6) 0.054 Uiso 1 calc R . H16C H 0.38602(14) 1.53400(13) -0.07171(6) 0.054 Uiso 1 calc R . C17 C 0.24262(14) 1.58374(13) -0.04627(6) 0.0378(5) Uani 1 d . . H17A H 0.23988(14) 1.64506(13) -0.05796(6) 0.057 Uiso 1 calc R . H17B H 0.20010(14) 1.57734(13) -0.02840(6) 0.057 Uiso 1 calc R . H17C H 0.23399(14) 1.53805(13) -0.06751(6) 0.057 Uiso 1 calc R . C18 C 0.37211(10) 1.36293(11) 0.09973(5) 0.0201(3) Uani 1 d . . C19 C 0.28851(12) 1.3445(2) 0.11415(6) 0.0397(5) Uani 1 d . . H19A H 0.25115(12) 1.3949(2) 0.10592(6) 0.060 Uiso 1 calc R . H19B H 0.29499(12) 1.3396(2) 0.14323(6) 0.060 Uiso 1 calc R . H19C H 0.26600(12) 1.2873(2) 0.10249(6) 0.060 Uiso 1 calc R . C20 C 0.4071(2) 1.45005(14) 0.11989(6) 0.0396(5) Uani 1 d . . H20A H 0.3708(2) 1.50154(14) 0.11193(6) 0.059 Uiso 1 calc R . H20B H 0.4614(2) 1.46196(14) 0.11182(6) 0.059 Uiso 1 calc R . H20C H 0.4114(2) 1.44255(14) 0.14885(6) 0.059 Uiso 1 calc R . C21 C 0.42985(13) 1.28412(14) 0.11268(5) 0.0319(4) Uani 1 d . . H21A H 0.40843(13) 1.22749(14) 0.10002(5) 0.048 Uiso 1 calc R . H21B H 0.43411(13) 1.27743(14) 0.14167(5) 0.048 Uiso 1 calc R . H21C H 0.48410(13) 1.29685(14) 0.10465(5) 0.048 Uiso 1 calc R . C22 C 0.23049(12) 0.98093(12) 0.04716(6) 0.0274(4) Uani 1 d . . C23 C 0.23356(13) 0.87627(13) 0.05108(6) 0.0341(4) Uani 1 d . . H23A H 0.20771(13) 0.84848(13) 0.02643(6) 0.051 Uiso 1 calc R . H23B H 0.20425(13) 0.85737(13) 0.07337(6) 0.051 Uiso 1 calc R . H23C H 0.29069(13) 0.85628(13) 0.05595(6) 0.051 Uiso 1 calc R . C24 C 0.2712(2) 1.0222(2) 0.08604(6) 0.0476(6) Uani 1 d . . H24A H 0.3288(2) 1.0037(2) 0.09013(6) 0.071 Uiso 1 calc R . H24B H 0.2432(2) 1.0004(2) 0.10830(6) 0.071 Uiso 1 calc R . H24C H 0.2677(2) 1.0890(2) 0.08459(6) 0.071 Uiso 1 calc R . C25 C 0.14038(13) 1.01000(15) 0.04083(7) 0.0420(5) Uani 1 d . . H25A H 0.11420(13) 0.98360(15) 0.01594(7) 0.063 Uiso 1 calc R . H25B H 0.13693(13) 1.07676(15) 0.03939(7) 0.063 Uiso 1 calc R . H25C H 0.11243(13) 0.98820(15) 0.06311(7) 0.063 Uiso 1 calc R . C26 C 0.41955(10) 0.92555(11) -0.06020(5) 0.0208(3) Uani 1 d . . C27 C 0.47364(12) 0.86777(14) -0.03010(6) 0.0336(4) Uani 1 d . . H27A H 0.43926(12) 0.83496(14) -0.01299(6) 0.050 Uiso 1 calc R . H27B H 0.51178(12) 0.90758(14) -0.01374(6) 0.050 Uiso 1 calc R . H27C H 0.50455(12) 0.82372(14) -0.04429(6) 0.050 Uiso 1 calc R . C28 C 0.36269(12) 0.86234(13) -0.08685(6) 0.0304(4) Uani 1 d . . H28A H 0.32703(12) 0.82905(13) -0.07054(6) 0.046 Uiso 1 calc R . H28B H 0.39553(12) 0.81874(13) -0.10024(6) 0.046 Uiso 1 calc R . H28C H 0.32917(12) 0.89884(13) -0.10682(6) 0.046 Uiso 1 calc R . C29 C 0.47401(13) 0.97612(13) -0.08658(7) 0.0370(5) Uani 1 d . . H29A H 0.43993(13) 1.01342(13) -0.10601(7) 0.055 Uiso 1 calc R . H29B H 0.50492(13) 0.93177(13) -0.10061(7) 0.055 Uiso 1 calc R . H29C H 0.51215(13) 1.01563(13) -0.07006(7) 0.055 Uiso 1 calc R . O31 O 0.36553(6) 1.27306(7) -0.11774(3) 0.0158(2) Uani 1 d . . C31 C 0.36797(9) 1.20432(10) -0.14177(4) 0.0141(3) Uani 1 d . . C32 C 0.43513(9) 1.18745(11) -0.16360(5) 0.0174(3) Uani 1 d . . C33 C 0.42808(10) 1.11474(11) -0.18988(5) 0.0191(3) Uani 1 d . . H33 H 0.47278(10) 1.10263(11) -0.20456(5) 0.023 Uiso 1 calc R . C34 C 0.35805(10) 1.05664(10) -0.19640(5) 0.0173(3) Uani 1 d . . C35 C 0.29444(9) 1.07119(10) -0.17458(4) 0.0161(3) Uani 1 d . . H35 H 0.24759(9) 1.03286(10) -0.17828(4) 0.019 Uiso 1 calc R . C36 C 0.29786(9) 1.14333(10) -0.14635(4) 0.0144(3) Uani 1 d . . N37 N 0.24027(7) 1.16363(9) -0.12294(4) 0.0148(2) Uani 1 d . . C38 C 0.16503(9) 1.11341(10) -0.12803(4) 0.0155(3) Uani 1 d . . C39 C 0.15928(10) 1.02722(11) -0.11151(5) 0.0194(3) Uani 1 d . . H39 H 0.20493(10) 1.00178(11) -0.09551(5) 0.023 Uiso 1 calc R . C40 C 0.08602(10) 0.97761(11) -0.11844(5) 0.0217(3) Uani 1 d . . C41 C 0.02036(10) 1.01825(12) -0.14123(5) 0.0236(3) Uani 1 d . . H41 H -0.02975(10) 0.98559(12) -0.14568(5) 0.028 Uiso 1 calc R . C42 C 0.02475(10) 1.10521(12) -0.15793(5) 0.0213(3) Uani 1 d . . C43 C 0.09823(9) 1.15247(11) -0.15096(5) 0.0191(3) Uani 1 d . . H43 H 0.10295(9) 1.21174(11) -0.16190(5) 0.023 Uiso 1 calc R . C44 C 0.51045(10) 1.24984(12) -0.15764(5) 0.0233(3) Uani 1 d . . C45 C 0.54740(11) 1.24707(14) -0.11389(6) 0.0315(4) Uani 1 d . . H45A H 0.50613(11) 1.26637(14) -0.09690(6) 0.047 Uiso 1 calc R . H45B H 0.59451(11) 1.28837(14) -0.10999(6) 0.047 Uiso 1 calc R . H45C H 0.56515(11) 1.18468(14) -0.10684(6) 0.047 Uiso 1 calc R . C46 C 0.57625(12) 1.21937(15) -0.18346(7) 0.0376(5) Uani 1 d . . H46A H 0.62347(12) 1.26041(15) -0.17902(7) 0.056 Uiso 1 calc R . H46B H 0.55390(12) 1.22135(15) -0.21158(7) 0.056 Uiso 1 calc R . H46C H 0.59344(12) 1.15687(15) -0.17629(7) 0.056 Uiso 1 calc R . C47 C 0.48557(12) 1.34813(12) -0.16965(6) 0.0287(4) Uani 1 d . . H47A H 0.44343(12) 1.36933(12) -0.15353(6) 0.043 Uiso 1 calc R . H47B H 0.46392(12) 1.34956(12) -0.19786(6) 0.043 Uiso 1 calc R . H47C H 0.53352(12) 1.38812(12) -0.16519(6) 0.043 Uiso 1 calc R . C48 C 0.35745(10) 0.97977(11) -0.22709(5) 0.0209(3) Uani 1 d . . C49 C 0.27585(11) 0.92885(12) -0.23228(5) 0.0258(4) Uani 1 d . . H49A H 0.27793(11) 0.88035(12) -0.25211(5) 0.039 Uiso 1 calc R . H49B H 0.23175(11) 0.97162(12) -0.24127(5) 0.039 Uiso 1 calc R . H49C H 0.26554(11) 0.90193(12) -0.20680(5) 0.039 Uiso 1 calc R . C50 C 0.37093(12) 1.01961(13) -0.26797(5) 0.0290(4) Uani 1 d . . H50A H 0.42294(12) 1.05289(13) -0.26574(5) 0.044 Uiso 1 calc R . H50B H 0.32605(12) 1.06144(13) -0.27692(5) 0.044 Uiso 1 calc R . H50C H 0.37236(12) 0.96987(13) -0.28726(5) 0.044 Uiso 1 calc R . C51 C 0.42631(12) 0.91204(12) -0.21345(6) 0.0308(4) Uani 1 d . . H51A H 0.47882(12) 0.94434(12) -0.21007(6) 0.046 Uiso 1 calc R . H51B H 0.42796(12) 0.86398(12) -0.23351(6) 0.046 Uiso 1 calc R . H51C H 0.41607(12) 0.88457(12) -0.18806(6) 0.046 Uiso 1 calc R . C52 C 0.08183(12) 0.87890(12) -0.10338(6) 0.0301(4) Uani 1 d . . C53 C -0.00567(14) 0.8436(2) -0.10548(10) 0.0548(7) Uani 1 d . . H53A H -0.03725(14) 0.8828(2) -0.08939(10) 0.082 Uiso 1 calc R . H53B H -0.00530(14) 0.7810(2) -0.09522(10) 0.082 Uiso 1 calc R . H53C H -0.03075(14) 0.8443(2) -0.13320(10) 0.082 Uiso 1 calc R . C54 C 0.13008(15) 0.81800(15) -0.12830(8) 0.0463(6) Uani 1 d . . H54A H 0.18646(15) 0.84039(15) -0.12707(8) 0.069 Uiso 1 calc R . H54B H 0.10479(15) 0.81873(15) -0.15598(8) 0.069 Uiso 1 calc R . H54C H 0.13025(15) 0.75542(15) -0.11801(8) 0.069 Uiso 1 calc R . C55 C 0.1185(2) 0.8728(2) -0.05952(8) 0.0726(10) Uani 1 d . . H55A H 0.0874(2) 0.9122(2) -0.04329(8) 0.109 Uiso 1 calc R . H55B H 0.1757(2) 0.8929(2) -0.05701(8) 0.109 Uiso 1 calc R . H55C H 0.1159(2) 0.8095(2) -0.05033(8) 0.109 Uiso 1 calc R . C56 C -0.04963(10) 1.14362(13) -0.18395(6) 0.0286(4) Uani 1 d . . C57 C -0.12014(14) 1.1560(2) -0.15854(8) 0.0616(8) Uani 1 d . . H57A H -0.13220(14) 1.0975(2) -0.14644(8) 0.092 Uiso 1 calc R . H57B H -0.16882(14) 1.1776(2) -0.17537(8) 0.092 Uiso 1 calc R . H57C H -0.10453(14) 1.2009(2) -0.13756(8) 0.092 Uiso 1 calc R . C58 C -0.03178(15) 1.2354(2) -0.20253(9) 0.0562(7) Uani 1 d . . H58A H -0.01523(15) 1.2797(2) -0.18141(9) 0.084 Uiso 1 calc R . H58B H -0.08110(15) 1.2574(2) -0.21873(9) 0.084 Uiso 1 calc R . H58C H 0.01245(15) 1.2280(2) -0.21937(9) 0.084 Uiso 1 calc R . C59 C -0.07519(13) 1.0765(2) -0.21778(6) 0.0398(5) Uani 1 d . . H59A H -0.08703(13) 1.0169(2) -0.20661(6) 0.060 Uiso 1 calc R . H59B H -0.03068(13) 1.0702(2) -0.23453(6) 0.060 Uiso 1 calc R . H59C H -0.12423(13) 1.0995(2) -0.23388(6) 0.060 Uiso 1 calc R . O61 O 0.16020(6) 1.28294(7) -0.06962(3) 0.0168(2) Uani 1 d . . C61 C 0.10633(9) 1.33764(10) -0.08763(4) 0.0158(3) Uani 1 d . . C62 C 0.03008(10) 1.35593(11) -0.07308(5) 0.0200(3) Uani 1 d . . C63 C -0.02294(10) 1.41350(12) -0.09546(5) 0.0240(3) Uani 1 d . . H63 H -0.07378(10) 1.42680(12) -0.08594(5) 0.029 Uiso 1 calc R . C64 C -0.00665(10) 1.45462(11) -0.13206(5) 0.0223(3) Uani 1 d . . C65 C 0.06698(10) 1.43853(11) -0.14572(5) 0.0197(3) Uani 1 d . . H65 H 0.07906(10) 1.46583(11) -0.16985(5) 0.024 Uiso 1 calc R . C66 C 0.12554(9) 1.38111(10) -0.12394(4) 0.0154(3) Uani 1 d . . N67 N 0.19883(8) 1.35954(9) -0.13419(4) 0.0149(2) Uani 1 d . . C68 C 0.22737(9) 1.39720(10) -0.16886(4) 0.0148(3) Uani 1 d . . C69 C 0.22698(9) 1.34312(10) -0.20256(5) 0.0170(3) Uani 1 d . . H69 H 0.20548(9) 1.28289(10) -0.20257(5) 0.020 Uiso 1 calc R . C70 C 0.25792(9) 1.37657(11) -0.23642(5) 0.0176(3) Uani 1 d . . C71 C 0.28915(10) 1.46520(11) -0.23497(5) 0.0189(3) Uani 1 d . . H71 H 0.31005(10) 1.48903(11) -0.25790(5) 0.023 Uiso 1 calc R . C72 C 0.29097(9) 1.52036(10) -0.20123(5) 0.0172(3) Uani 1 d . . C73 C 0.25952(9) 1.48523(10) -0.16784(5) 0.0168(3) Uani 1 d . . H73 H 0.26001(9) 1.52125(10) -0.14445(5) 0.020 Uiso 1 calc R . C74 C 0.01059(11) 1.31150(12) -0.03425(5) 0.0260(4) Uani 1 d . . C75 C 0.01107(12) 1.20677(12) -0.03857(6) 0.0316(4) Uani 1 d . . H75A H -0.00142(12) 1.17861(12) -0.01369(6) 0.047 Uiso 1 calc R . H75B H 0.06520(12) 1.18665(12) -0.04448(6) 0.047 Uiso 1 calc R . H75C H -0.03027(12) 1.18844(12) -0.06031(6) 0.047 Uiso 1 calc R . C76 C -0.07428(14) 1.3399(2) -0.02404(7) 0.0447(6) Uani 1 d . . H76A H -0.08506(14) 1.3106(2) 0.00087(7) 0.067 Uiso 1 calc R . H76B H -0.11592(14) 1.3210(2) -0.04552(7) 0.067 Uiso 1 calc R . H76C H -0.07608(14) 1.4064(2) -0.02094(7) 0.067 Uiso 1 calc R . C77 C 0.07413(13) 1.34120(15) 0.00017(6) 0.0360(5) Uani 1 d . . H77A H 0.06140(13) 1.31261(15) 0.02493(6) 0.054 Uiso 1 calc R . H77B H 0.07276(13) 1.40779(15) 0.00296(6) 0.054 Uiso 1 calc R . H77C H 0.12878(13) 1.32215(15) -0.00540(6) 0.054 Uiso 1 calc R . C78 C -0.07169(11) 1.51729(13) -0.15377(6) 0.0289(4) Uani 1 d . . C79 C -0.05031(14) 1.5432(2) -0.19531(7) 0.0458(6) Uani 1 d . . H79A H 0.00288(14) 1.5741(2) -0.19287(7) 0.069 Uiso 1 calc R . H79B H -0.09241(14) 1.5843(2) -0.20816(7) 0.069 Uiso 1 calc R . H79C H -0.04773(14) 1.4879(2) -0.21142(7) 0.069 Uiso 1 calc R . C80 C -0.15487(12) 1.46942(15) -0.15897(7) 0.0379(5) Uani 1 d . . H80A H -0.19587(12) 1.51021(15) -0.17288(7) 0.057 Uiso 1 calc R . H80B H -0.17097(12) 1.45386(15) -0.13278(7) 0.057 Uiso 1 calc R . H80C H -0.15107(12) 1.41350(15) -0.17458(7) 0.057 Uiso 1 calc R . C81 C -0.07606(12) 1.60412(14) -0.12884(7) 0.0377(5) Uani 1 d . . H81A H -0.02247(12) 1.63415(14) -0.12572(7) 0.056 Uiso 1 calc R . H81B H -0.09151(12) 1.58807(14) -0.10258(7) 0.056 Uiso 1 calc R . H81C H -0.11700(12) 1.64569(14) -0.14227(7) 0.056 Uiso 1 calc R . C82 C 0.26172(11) 1.31789(11) -0.27367(5) 0.0216(3) Uani 1 d . . C83 C 0.2270(2) 1.36954(15) -0.31100(6) 0.0434(5) Uani 1 d . . H83A H 0.2567(2) 1.42713(15) -0.31273(6) 0.065 Uiso 1 calc R . H83B H 0.1689(2) 1.38243(15) -0.30969(6) 0.065 Uiso 1 calc R . H83C H 0.2330(2) 1.33225(15) -0.33455(6) 0.065 Uiso 1 calc R . C84 C 0.35172(12) 1.29265(15) -0.27645(6) 0.0364(5) Uani 1 d . . H84A H 0.37365(12) 1.25952(15) -0.25239(6) 0.055 Uiso 1 calc R . H84B H 0.38363(12) 1.34847(15) -0.27891(6) 0.055 Uiso 1 calc R . H84C H 0.35518(12) 1.25390(15) -0.29982(6) 0.055 Uiso 1 calc R . C85 C 0.21412(13) 1.22867(13) -0.27186(6) 0.0334(4) Uani 1 d . . H85A H 0.23554(13) 1.19437(13) -0.24804(6) 0.050 Uiso 1 calc R . H85B H 0.22019(13) 1.19211(13) -0.29561(6) 0.050 Uiso 1 calc R . H85C H 0.15609(13) 1.24229(13) -0.27076(6) 0.050 Uiso 1 calc R . C86 C 0.33012(11) 1.61578(11) -0.20144(5) 0.0231(3) Uani 1 d . . C87 C 0.42102(12) 1.60367(15) -0.20925(7) 0.0368(5) Uani 1 d . . H87A H 0.42317(12) 1.57119(15) -0.23444(7) 0.055 Uiso 1 calc R . H87B H 0.45041(12) 1.56840(15) -0.18750(7) 0.055 Uiso 1 calc R . H87C H 0.44666(12) 1.66381(15) -0.21072(7) 0.055 Uiso 1 calc R . C88 C 0.3293(2) 1.66594(15) -0.16249(7) 0.0455(6) Uani 1 d . . H88A H 0.3565(2) 1.62872(15) -0.14081(7) 0.068 Uiso 1 calc R . H88B H 0.2725(2) 1.67743(15) -0.15766(7) 0.068 Uiso 1 calc R . H88C H 0.3581(2) 1.72422(15) -0.16372(7) 0.068 Uiso 1 calc R . C89 C 0.28804(13) 1.67272(13) -0.23534(6) 0.0357(4) Uani 1 d . . H89A H 0.28890(13) 1.63965(13) -0.26048(6) 0.054 Uiso 1 calc R . H89B H 0.31685(13) 1.73101(13) -0.23674(6) 0.054 Uiso 1 calc R . H89C H 0.23123(13) 1.68422(13) -0.23067(6) 0.054 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ga1 0.01432(8) 0.01232(8) 0.01216(8) -0.00103(6) 0.00314(5) 0.00010(6) O1 0.0216(5) 0.0139(5) 0.0135(5) -0.0005(4) 0.0032(4) 0.0009(4) C1 0.0167(7) 0.0161(7) 0.0138(7) -0.0011(5) 0.0049(5) 0.0003(5) C2 0.0289(8) 0.0148(7) 0.0169(7) -0.0012(6) 0.0077(6) -0.0008(6) C3 0.0316(9) 0.0162(7) 0.0168(7) -0.0047(6) 0.0069(6) -0.0027(6) C4 0.0194(7) 0.0192(7) 0.0126(7) -0.0010(6) 0.0043(5) 0.0002(6) C5 0.0178(7) 0.0155(7) 0.0159(7) 0.0003(6) 0.0037(5) 0.0010(5) C6 0.0147(7) 0.0147(7) 0.0152(7) -0.0013(5) 0.0040(5) 0.0010(5) N7 0.0162(6) 0.0123(6) 0.0139(6) -0.0020(5) 0.0015(5) 0.0009(5) C8 0.0176(7) 0.0129(7) 0.0160(7) -0.0012(5) -0.0006(5) 0.0009(5) C9 0.0204(7) 0.0164(7) 0.0189(7) -0.0018(6) 0.0034(6) 0.0009(6) C10 0.0232(8) 0.0167(7) 0.0208(8) 0.0008(6) 0.0038(6) -0.0021(6) C11 0.0242(8) 0.0135(7) 0.0226(8) -0.0002(6) 0.0007(6) 0.0010(6) C12 0.0191(7) 0.0140(7) 0.0193(7) -0.0037(6) -0.0013(6) 0.0027(6) C13 0.0176(7) 0.0156(7) 0.0156(7) -0.0026(6) -0.0002(5) 0.0004(5) C14 0.0575(12) 0.0132(8) 0.0184(8) -0.0017(6) 0.0090(8) -0.0018(7) C15 0.116(2) 0.0129(9) 0.0245(10) -0.0031(7) 0.0098(12) -0.0049(11) C16 0.0569(13) 0.0259(9) 0.0254(9) 0.0020(7) 0.0091(9) -0.0176(9) C17 0.0617(14) 0.0234(9) 0.0297(10) 0.0046(8) 0.0115(9) 0.0188(9) C18 0.0269(8) 0.0207(8) 0.0132(7) -0.0019(6) 0.0040(6) 0.0022(6) C19 0.0346(10) 0.0650(15) 0.0216(9) 0.0084(9) 0.0120(8) 0.0078(10) C20 0.0678(15) 0.0301(10) 0.0186(9) -0.0052(8) -0.0051(9) -0.0030(10) C21 0.0432(11) 0.0343(10) 0.0174(8) -0.0009(7) -0.0003(7) 0.0141(8) C22 0.0358(10) 0.0206(8) 0.0278(9) 0.0013(7) 0.0127(7) -0.0033(7) C23 0.0455(11) 0.0229(9) 0.0363(11) 0.0078(8) 0.0153(9) -0.0028(8) C24 0.076(2) 0.0418(12) 0.0288(11) -0.0042(9) 0.0215(11) -0.0208(12) C25 0.0413(12) 0.0319(10) 0.0585(14) 0.0082(10) 0.0299(11) 0.0030(9) C26 0.0227(8) 0.0159(7) 0.0234(8) -0.0042(6) 0.0012(6) 0.0051(6) C27 0.0361(10) 0.0340(10) 0.0286(10) -0.0079(8) -0.0059(8) 0.0190(8) C28 0.0338(10) 0.0272(9) 0.0285(9) -0.0114(7) -0.0034(7) 0.0074(7) C29 0.0390(11) 0.0255(9) 0.0508(13) -0.0046(9) 0.0241(9) 0.0079(8) O31 0.0160(5) 0.0155(5) 0.0167(5) -0.0048(4) 0.0047(4) -0.0022(4) C31 0.0154(7) 0.0128(7) 0.0141(7) 0.0001(5) 0.0019(5) -0.0005(5) C32 0.0163(7) 0.0176(7) 0.0190(7) -0.0002(6) 0.0051(6) -0.0015(6) C33 0.0189(7) 0.0182(7) 0.0216(8) -0.0020(6) 0.0088(6) 0.0005(6) C34 0.0221(7) 0.0137(7) 0.0167(7) -0.0017(6) 0.0043(6) 0.0005(6) C35 0.0177(7) 0.0139(7) 0.0168(7) -0.0009(6) 0.0020(5) -0.0017(5) C36 0.0155(7) 0.0139(7) 0.0139(7) 0.0005(5) 0.0022(5) 0.0001(5) N37 0.0140(6) 0.0151(6) 0.0158(6) -0.0009(5) 0.0036(5) -0.0016(5) C38 0.0146(7) 0.0172(7) 0.0154(7) -0.0039(6) 0.0053(5) -0.0029(5) C39 0.0191(7) 0.0170(7) 0.0226(8) -0.0015(6) 0.0044(6) -0.0015(6) C40 0.0242(8) 0.0189(8) 0.0233(8) -0.0026(6) 0.0086(6) -0.0067(6) C41 0.0182(8) 0.0239(8) 0.0295(9) -0.0054(7) 0.0067(6) -0.0078(6) C42 0.0166(7) 0.0249(8) 0.0224(8) -0.0045(6) 0.0021(6) -0.0017(6) C43 0.0196(7) 0.0185(7) 0.0192(7) -0.0018(6) 0.0021(6) -0.0023(6) C44 0.0183(8) 0.0251(8) 0.0283(9) -0.0060(7) 0.0100(6) -0.0069(6) C45 0.0179(8) 0.0408(11) 0.0351(10) -0.0052(8) 0.0004(7) -0.0067(7) C46 0.0257(9) 0.0425(11) 0.0485(12) -0.0171(10) 0.0216(9) -0.0121(8) C47 0.0336(10) 0.0223(9) 0.0316(10) -0.0036(7) 0.0104(8) -0.0131(7) C48 0.0261(8) 0.0154(7) 0.0222(8) -0.0058(6) 0.0075(6) -0.0004(6) C49 0.0315(9) 0.0196(8) 0.0266(9) -0.0094(7) 0.0047(7) -0.0033(7) C50 0.0406(10) 0.0261(9) 0.0223(9) -0.0070(7) 0.0117(7) -0.0042(8) C51 0.0325(10) 0.0218(9) 0.0383(11) -0.0100(8) 0.0050(8) 0.0060(7) C52 0.0324(10) 0.0214(9) 0.0367(10) 0.0031(7) 0.0054(8) -0.0098(7) C53 0.0426(13) 0.0283(11) 0.098(2) 0.0086(12) 0.0293(13) -0.0102(9) C54 0.0452(13) 0.0258(10) 0.069(2) 0.0002(10) 0.0112(11) 0.0008(9) C55 0.121(3) 0.050(2) 0.0430(15) 0.0196(12) -0.008(2) -0.044(2) C56 0.0180(8) 0.0339(10) 0.0323(10) -0.0038(8) -0.0034(7) -0.0011(7) C57 0.0310(11) 0.108(2) 0.0444(14) -0.0116(14) -0.0004(10) 0.0299(13) C58 0.0414(13) 0.0374(12) 0.081(2) 0.0168(12) -0.0322(12) -0.0045(10) C59 0.0371(11) 0.0437(12) 0.0354(11) -0.0058(9) -0.0093(9) -0.0014(9) O61 0.0174(5) 0.0176(5) 0.0161(5) 0.0026(4) 0.0047(4) 0.0016(4) C61 0.0175(7) 0.0138(7) 0.0164(7) -0.0006(5) 0.0037(5) 0.0005(5) C62 0.0199(7) 0.0185(8) 0.0234(8) 0.0009(6) 0.0104(6) 0.0010(6) C63 0.0196(8) 0.0247(8) 0.0295(9) 0.0033(7) 0.0110(7) 0.0034(6) C64 0.0197(8) 0.0217(8) 0.0263(8) 0.0033(7) 0.0052(6) 0.0045(6) C65 0.0201(7) 0.0195(8) 0.0202(8) 0.0044(6) 0.0049(6) 0.0024(6) C66 0.0160(7) 0.0144(7) 0.0161(7) -0.0012(5) 0.0035(5) -0.0006(5) N67 0.0161(6) 0.0156(6) 0.0133(6) -0.0004(5) 0.0034(5) 0.0001(5) C68 0.0145(7) 0.0166(7) 0.0136(7) 0.0018(5) 0.0028(5) 0.0012(5) C69 0.0207(7) 0.0132(7) 0.0174(7) -0.0002(6) 0.0039(6) -0.0017(6) C70 0.0209(7) 0.0180(7) 0.0142(7) -0.0012(6) 0.0025(6) -0.0005(6) C71 0.0235(8) 0.0191(7) 0.0149(7) 0.0031(6) 0.0055(6) -0.0013(6) C72 0.0197(7) 0.0139(7) 0.0182(7) 0.0013(6) 0.0032(6) -0.0008(6) C73 0.0197(7) 0.0157(7) 0.0155(7) -0.0011(6) 0.0038(6) 0.0008(6) C74 0.0272(9) 0.0261(9) 0.0279(9) 0.0075(7) 0.0167(7) 0.0043(7) C75 0.0304(9) 0.0260(9) 0.0409(11) 0.0113(8) 0.0152(8) -0.0002(7) C76 0.0429(12) 0.0446(12) 0.0538(14) 0.0207(11) 0.0363(11) 0.0149(10) C77 0.0510(12) 0.0396(11) 0.0200(9) 0.0018(8) 0.0154(8) 0.0014(9) C78 0.0233(8) 0.0315(10) 0.0323(10) 0.0074(8) 0.0052(7) 0.0100(7) C79 0.0400(12) 0.0578(14) 0.0405(12) 0.0236(11) 0.0090(9) 0.0262(10) C80 0.0262(9) 0.0402(11) 0.0454(12) 0.0000(9) -0.0039(8) 0.0092(8) C81 0.0277(10) 0.0275(10) 0.0570(14) 0.0008(9) 0.0015(9) 0.0101(8) C82 0.0306(9) 0.0207(8) 0.0142(7) -0.0030(6) 0.0051(6) -0.0030(7) C83 0.078(2) 0.0313(11) 0.0187(9) -0.0035(8) -0.0039(9) 0.0096(10) C84 0.0341(10) 0.0419(11) 0.0353(11) -0.0184(9) 0.0123(8) -0.0032(8) C85 0.0433(11) 0.0308(10) 0.0275(9) -0.0124(8) 0.0100(8) -0.0119(8) C86 0.0312(9) 0.0169(8) 0.0210(8) 0.0017(6) 0.0013(7) -0.0067(6) C87 0.0306(10) 0.0357(11) 0.0438(12) 0.0077(9) 0.0020(8) -0.0078(8) C88 0.076(2) 0.0293(11) 0.0335(11) -0.0069(9) 0.0145(11) -0.0224(11) C89 0.0448(11) 0.0207(9) 0.0400(11) 0.0072(8) -0.0027(9) -0.0075(8) _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 Ga1 O31 1.9508(10) . ? Ga1 O61 1.9707(11) . ? Ga1 O1 1.9711(11) . ? Ga1 N7 2.0376(13) . ? Ga1 N67 2.0398(13) . ? Ga1 N37 2.0553(13) . ? O1 C1 1.294(2) . ? C1 C2 1.424(2) . ? C1 C6 1.456(2) . ? C2 C3 1.377(2) . ? C2 C14 1.535(2) . ? C3 C4 1.427(2) . ? C4 C5 1.370(2) . ? C4 C18 1.531(2) . ? C5 C6 1.420(2) . ? C6 N7 1.339(2) . ? N7 C8 1.416(2) . ? C8 C9 1.388(2) . ? C8 C13 1.402(2) . ? C9 C10 1.402(2) . ? C10 C11 1.390(2) . ? C10 C22 1.535(2) . ? C11 C12 1.403(2) . ? C12 C13 1.387(2) . ? C12 C26 1.534(2) . ? C14 C17 1.526(3) . ? C14 C15 1.537(2) . ? C14 C16 1.538(3) . ? C18 C21 1.526(2) . ? C18 C20 1.527(2) . ? C18 C19 1.535(2) . ? C22 C24 1.531(3) . ? C22 C25 1.533(3) . ? C22 C23 1.538(2) . ? C26 C29 1.527(3) . ? C26 C27 1.528(2) . ? C26 C28 1.533(2) . ? O31 C31 1.297(2) . ? C31 C32 1.419(2) . ? C31 C36 1.453(2) . ? C32 C33 1.383(2) . ? C32 C44 1.534(2) . ? C33 C34 1.429(2) . ? C34 C35 1.365(2) . ? C34 C48 1.530(2) . ? C35 C36 1.421(2) . ? C36 N37 1.336(2) . ? N37 C38 1.433(2) . ? C38 C39 1.388(2) . ? C38 C43 1.393(2) . ? C39 C40 1.404(2) . ? C40 C41 1.387(2) . ? C40 C52 1.537(2) . ? C41 C42 1.398(2) . ? C42 C43 1.389(2) . ? C42 C56 1.530(2) . ? C44 C46 1.533(2) . ? C44 C45 1.535(3) . ? C44 C47 1.538(3) . ? C48 C49 1.528(2) . ? C48 C51 1.536(2) . ? C48 C50 1.540(2) . ? C52 C54 1.513(3) . ? C52 C53 1.523(3) . ? C52 C55 1.539(3) . ? C56 C58 1.526(3) . ? C56 C59 1.530(3) . ? C56 C57 1.531(3) . ? O61 C61 1.294(2) . ? C61 C62 1.424(2) . ? C61 C66 1.450(2) . ? C62 C63 1.376(2) . ? C62 C74 1.532(2) . ? C63 C64 1.429(2) . ? C64 C65 1.365(2) . ? C64 C78 1.532(2) . ? C65 C66 1.420(2) . ? C66 N67 1.330(2) . ? N67 C68 1.423(2) . ? C68 C69 1.387(2) . ? C68 C73 1.392(2) . ? C69 C70 1.394(2) . ? C70 C71 1.394(2) . ? C70 C82 1.532(2) . ? C71 C72 1.396(2) . ? C72 C73 1.393(2) . ? C72 C86 1.539(2) . ? C74 C76 1.534(2) . ? C74 C77 1.536(3) . ? C74 C75 1.540(3) . ? C78 C80 1.530(3) . ? C78 C81 1.532(3) . ? C78 C79 1.535(3) . ? C82 C83 1.526(3) . ? C82 C85 1.528(2) . ? C82 C84 1.539(3) . ? C86 C88 1.510(3) . ? C86 C89 1.519(3) . ? C86 C87 1.558(3) . ? 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 O31 Ga1 O61 174.10(4) . . ? O31 Ga1 O1 91.31(4) . . ? O61 Ga1 O1 94.37(4) . . ? O31 Ga1 N7 97.06(5) . . ? O61 Ga1 N7 85.45(5) . . ? O1 Ga1 N7 80.73(5) . . ? O31 Ga1 N67 98.07(5) . . ? O61 Ga1 N67 80.74(5) . . ? O1 Ga1 N67 86.26(5) . . ? N7 Ga1 N67 160.22(5) . . ? O31 Ga1 N37 80.90(5) . . ? O61 Ga1 N37 93.36(5) . . ? O1 Ga1 N37 171.92(5) . . ? N7 Ga1 N37 102.24(5) . . ? N67 Ga1 N37 92.68(5) . . ? C1 O1 Ga1 113.52(9) . . ? O1 C1 C2 122.65(14) . . ? O1 C1 C6 117.52(13) . . ? C2 C1 C6 119.83(13) . . ? C3 C2 C1 117.30(14) . . ? C3 C2 C14 122.60(14) . . ? C1 C2 C14 120.10(14) . . ? C2 C3 C4 124.18(14) . . ? C5 C4 C3 118.70(14) . . ? C5 C4 C18 120.79(14) . . ? C3 C4 C18 120.35(14) . . ? C4 C5 C6 120.68(14) . . ? N7 C6 C5 126.83(14) . . ? N7 C6 C1 113.88(13) . . ? C5 C6 C1 119.28(13) . . ? C6 N7 C8 123.06(13) . . ? C6 N7 Ga1 111.61(10) . . ? C8 N7 Ga1 123.97(10) . . ? C9 C8 C13 120.04(14) . . ? C9 C8 N7 122.67(13) . . ? C13 C8 N7 117.26(14) . . ? C8 C9 C10 120.58(14) . . ? C11 C10 C9 118.10(15) . . ? C11 C10 C22 122.85(15) . . ? C9 C10 C22 119.00(14) . . ? C10 C11 C12 122.48(15) . . ? C13 C12 C11 118.08(14) . . ? C13 C12 C26 122.04(15) . . ? C11 C12 C26 119.87(14) . . ? C12 C13 C8 120.70(15) . . ? C17 C14 C2 110.5(2) . . ? C17 C14 C15 107.7(2) . . ? C2 C14 C15 111.67(15) . . ? C17 C14 C16 110.2(2) . . ? C2 C14 C16 108.8(2) . . ? C15 C14 C16 108.0(2) . . ? C21 C18 C20 108.2(2) . . ? C21 C18 C4 111.59(13) . . ? C20 C18 C4 112.52(14) . . ? C21 C18 C19 109.1(2) . . ? C20 C18 C19 108.1(2) . . ? C4 C18 C19 107.23(14) . . ? C24 C22 C25 109.4(2) . . ? C24 C22 C10 108.64(15) . . ? C25 C22 C10 110.3(2) . . ? C24 C22 C23 108.2(2) . . ? C25 C22 C23 108.1(2) . . ? C10 C22 C23 112.19(15) . . ? C29 C26 C27 108.8(2) . . ? C29 C26 C28 108.0(2) . . ? C27 C26 C28 109.09(15) . . ? C29 C26 C12 111.91(14) . . ? C27 C26 C12 110.08(14) . . ? C28 C26 C12 108.97(13) . . ? C31 O31 Ga1 115.19(9) . . ? O31 C31 C32 122.88(13) . . ? O31 C31 C36 117.56(13) . . ? C32 C31 C36 119.55(13) . . ? C33 C32 C31 117.09(14) . . ? C33 C32 C44 123.36(14) . . ? C31 C32 C44 119.55(14) . . ? C32 C33 C34 124.35(14) . . ? C35 C34 C33 118.57(14) . . ? C35 C34 C48 122.41(14) . . ? C33 C34 C48 119.02(13) . . ? C34 C35 C36 120.38(14) . . ? N37 C36 C35 125.98(13) . . ? N37 C36 C31 114.10(13) . . ? C35 C36 C31 119.91(13) . . ? C36 N37 C38 118.44(12) . . ? C36 N37 Ga1 111.99(10) . . ? C38 N37 Ga1 128.33(10) . . ? C39 C38 C43 120.78(14) . . ? C39 C38 N37 121.06(14) . . ? C43 C38 N37 118.14(14) . . ? C38 C39 C40 120.0(2) . . ? C41 C40 C39 118.0(2) . . ? C41 C40 C52 121.74(15) . . ? C39 C40 C52 120.1(2) . . ? C40 C41 C42 122.83(15) . . ? C43 C42 C41 118.0(2) . . ? C43 C42 C56 122.5(2) . . ? C41 C42 C56 119.49(15) . . ? C42 C43 C38 120.36(15) . . ? C46 C44 C32 111.35(14) . . ? C46 C44 C45 108.3(2) . . ? C32 C44 C45 109.63(14) . . ? C46 C44 C47 107.8(2) . . ? C32 C44 C47 109.62(14) . . ? C45 C44 C47 110.09(15) . . ? C49 C48 C34 111.97(13) . . ? C49 C48 C51 109.11(14) . . ? C34 C48 C51 108.89(14) . . ? C49 C48 C50 107.24(14) . . ? C34 C48 C50 109.88(13) . . ? C51 C48 C50 109.71(15) . . ? C54 C52 C53 109.1(2) . . ? C54 C52 C40 108.9(2) . . ? C53 C52 C40 112.4(2) . . ? C54 C52 C55 109.3(2) . . ? C53 C52 C55 106.9(2) . . ? C40 C52 C55 110.3(2) . . ? C58 C56 C59 107.9(2) . . ? C58 C56 C42 112.43(15) . . ? C59 C56 C42 109.1(2) . . ? C58 C56 C57 108.7(2) . . ? C59 C56 C57 109.6(2) . . ? C42 C56 C57 109.1(2) . . ? C61 O61 Ga1 113.99(9) . . ? O61 C61 C62 122.44(14) . . ? O61 C61 C66 117.81(13) . . ? C62 C61 C66 119.75(14) . . ? C63 C62 C61 116.93(14) . . ? C63 C62 C74 123.37(14) . . ? C61 C62 C74 119.70(14) . . ? C62 C63 C64 124.38(15) . . ? C65 C64 C63 118.81(15) . . ? C65 C64 C78 122.6(2) . . ? C63 C64 C78 118.53(14) . . ? C64 C65 C66 120.15(15) . . ? N67 C66 C65 125.93(14) . . ? N67 C66 C61 114.12(13) . . ? C65 C66 C61 119.92(13) . . ? C66 N67 C68 121.15(13) . . ? C66 N67 Ga1 112.37(10) . . ? C68 N67 Ga1 126.06(10) . . ? C69 C68 C73 120.98(14) . . ? C69 C68 N67 119.00(13) . . ? C73 C68 N67 119.91(13) . . ? C68 C69 C70 120.43(14) . . ? C69 C70 C71 117.75(14) . . ? C69 C70 C82 122.11(14) . . ? C71 C70 C82 120.09(14) . . ? C70 C71 C72 122.74(14) . . ? C73 C72 C71 118.29(14) . . ? C73 C72 C86 122.24(14) . . ? C71 C72 C86 119.44(14) . . ? C68 C73 C72 119.80(14) . . ? C62 C74 C76 111.28(15) . . ? C62 C74 C77 109.79(14) . . ? C76 C74 C77 108.1(2) . . ? C62 C74 C75 109.71(15) . . ? C76 C74 C75 107.8(2) . . ? C77 C74 C75 110.1(2) . . ? C80 C78 C64 110.3(2) . . ? C80 C78 C81 110.2(2) . . ? C64 C78 C81 107.9(2) . . ? C80 C78 C79 107.7(2) . . ? C64 C78 C79 111.50(15) . . ? C81 C78 C79 109.2(2) . . ? C83 C82 C85 108.2(2) . . ? C83 C82 C70 110.84(14) . . ? C85 C82 C70 112.16(13) . . ? C83 C82 C84 109.9(2) . . ? C85 C82 C84 107.3(2) . . ? C70 C82 C84 108.36(14) . . ? C88 C86 C89 110.0(2) . . ? C88 C86 C72 113.07(14) . . ? C89 C86 C72 110.30(14) . . ? C88 C86 C87 108.0(2) . . ? C89 C86 C87 107.3(2) . . ? C72 C86 C87 107.93(14) . . ? _refine_diff_density_max 0.874 _refine_diff_density_min -0.359 _refine_diff_density_rms 0.053 #===END data_8 _database_code_depnum_ccdc_archive 'CCDC 665853' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[C60 H69 Cl6 Ga N3 O3], 0.5 (C2H5)3N' _chemical_formula_sum 'C63 H76.50 Cl6 Ga N3.50 O3' _chemical_formula_weight 1213.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' _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 18.2999(9) _cell_length_b 19.7567(9) _cell_length_c 35.0963(15) _cell_angle_alpha 90.00 _cell_angle_beta 93.220(10) _cell_angle_gamma 90.00 _cell_volume 12668.9(10) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 115476 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 23.82 _exptl_crystal_description 'opaque block' _exptl_crystal_colour black _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.272 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5088 _exptl_absorpt_coefficient_mu 0.733 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method '1166 images at 0.6 deg. stepwise rotation in omega and phi, 204 sec./frame' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 55606 _diffrn_reflns_av_R_equivalents 0.0844 _diffrn_reflns_av_sigmaI/netI 0.0605 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 22.50 _reflns_number_total 8277 _reflns_number_gt 6560 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO, Nonius Collect Software' _computing_cell_refinement 'DENZO, Nonius Collect Software' _computing_data_reduction 'DENZO, Nonius Collect Software' _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. ; _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^)+(0.0001P)^2^+727.9327P] 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 8277 _refine_ls_number_parameters 707 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.1370 _refine_ls_R_factor_gt 0.1145 _refine_ls_wR_factor_ref 0.2994 _refine_ls_wR_factor_gt 0.2896 _refine_ls_goodness_of_fit_ref 1.248 _refine_ls_restrained_S_all 1.247 _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 Ga1 Ga 0.27040(7) 0.02204(7) 0.61641(4) 0.0164(4) Uani 1 1 d . . . O1 O 0.3095(4) 0.0886(4) 0.5826(2) 0.0159(19) Uani 1 1 d . . . C1 C 0.3773(7) 0.0782(7) 0.5733(3) 0.019(3) Uani 1 1 d . . . C2 C 0.4135(7) 0.1212(6) 0.5484(4) 0.018(3) Uani 1 1 d . . . C3 C 0.4858(7) 0.1077(7) 0.5437(4) 0.021(3) Uani 1 1 d . . . H3 H 0.5117 0.1374 0.5280 0.026 Uiso 1 1 calc R . . C4 C 0.5250(7) 0.0513(6) 0.5610(3) 0.017(3) Uani 1 1 d . . . C5 C 0.4895(6) 0.0083(6) 0.5824(3) 0.017(3) Uani 1 1 d . . . H5 H 0.5148 -0.0297 0.5932 0.021 Uiso 1 1 calc R . . C6 C 0.4136(7) 0.0181(6) 0.5897(3) 0.017(3) Uani 1 1 d . . . N7 N 0.3717(5) -0.0177(5) 0.6119(3) 0.019(2) Uani 1 1 d . . . C8 C 0.3894(6) -0.0838(6) 0.6240(3) 0.016(3) Uani 1 1 d . . . C9 C 0.3855(7) -0.1009(7) 0.6629(4) 0.021(3) Uani 1 1 d . . . H9 H 0.3749 -0.0672 0.6811 0.026 Uiso 1 1 calc R . . C10 C 0.3973(8) -0.1680(7) 0.6742(4) 0.027(3) Uani 1 1 d . . . C11 C 0.4149(7) -0.2169(8) 0.6492(4) 0.034(4) Uani 1 1 d . . . H11 H 0.4235 -0.2622 0.6575 0.040 Uiso 1 1 calc R . . C12 C 0.4199(7) -0.1989(6) 0.6111(4) 0.023(3) Uani 1 1 d . . . C13 C 0.4091(7) -0.1341(6) 0.5983(4) 0.022(3) Uani 1 1 d . . . H13 H 0.4149 -0.1233 0.5723 0.026 Uiso 1 1 calc R . . C14 C 0.3726(7) 0.1805(6) 0.5287(4) 0.020(3) Uani 1 1 d . . . C15 C 0.4205(8) 0.2161(7) 0.5005(4) 0.035(4) Uani 1 1 d . . . H15A H 0.4656 0.2320 0.5139 0.052 Uiso 1 1 calc R . . H15B H 0.3938 0.2548 0.4890 0.052 Uiso 1 1 calc R . . H15C H 0.4326 0.1843 0.4803 0.052 Uiso 1 1 calc R . . C16 C 0.3529(8) 0.2333(6) 0.5600(4) 0.028(3) Uani 1 1 d . . . H16A H 0.3980 0.2492 0.5735 0.042 Uiso 1 1 calc R . . H16B H 0.3213 0.2119 0.5781 0.042 Uiso 1 1 calc R . . H16C H 0.3273 0.2718 0.5477 0.042 Uiso 1 1 calc R . . C17 C 0.3027(7) 0.1560(7) 0.5077(4) 0.023(3) Uani 1 1 d . . . H17A H 0.2718 0.1331 0.5256 0.035 Uiso 1 1 calc R . . H17B H 0.3150 0.1242 0.4876 0.035 Uiso 1 1 calc R . . H17C H 0.2762 0.1947 0.4962 0.035 Uiso 1 1 calc R . . C18 C 0.6081(7) 0.0447(6) 0.5550(4) 0.019(3) Uani 1 1 d . . . C19 C 0.6477(8) 0.1047(7) 0.5735(4) 0.031(3) Uani 1 1 d . . . H19A H 0.6278 0.1467 0.5623 0.046 Uiso 1 1 calc R . . H19B H 0.7001 0.1016 0.5691 0.046 Uiso 1 1 calc R . . H19C H 0.6409 0.1044 0.6010 0.046 Uiso 1 1 calc R . . C20 C 0.6192(7) 0.0434(7) 0.5113(4) 0.029(3) Uani 1 1 d . . . H20A H 0.5996 0.0852 0.4996 0.043 Uiso 1 1 calc R . . H20B H 0.5933 0.0044 0.4997 0.043 Uiso 1 1 calc R . . H20C H 0.6715 0.0398 0.5070 0.043 Uiso 1 1 calc R . . C21 C 0.6386(7) -0.0197(6) 0.5721(4) 0.023(3) Uani 1 1 d . . . H21A H 0.6130 -0.0585 0.5602 0.034 Uiso 1 1 calc R . . H21B H 0.6318 -0.0200 0.5996 0.034 Uiso 1 1 calc R . . H21C H 0.6909 -0.0227 0.5678 0.034 Uiso 1 1 calc R . . Cl22 Cl 0.3927(2) -0.1874(2) 0.72209(11) 0.0428(10) Uani 1 1 d . . . Cl23 Cl 0.4410(3) -0.26248(18) 0.57867(12) 0.0473(11) Uani 1 1 d . . . O31 O 0.2316(4) -0.0445(4) 0.5789(2) 0.018(2) Uani 1 1 d . . . C31 C 0.1620(7) -0.0438(6) 0.5743(3) 0.015(3) Uani 1 1 d . . . C32 C 0.1196(7) -0.0988(6) 0.5581(4) 0.022(3) Uani 1 1 d . . . C33 C 0.0453(6) -0.0907(6) 0.5553(3) 0.018(3) Uani 1 1 d . . . H33 H 0.0172 -0.1272 0.5447 0.021 Uiso 1 1 calc R . . C34 C 0.0058(7) -0.0320(6) 0.5668(3) 0.019(3) Uiso 1 1 d . . . C35 C 0.0457(7) 0.0196(7) 0.5820(3) 0.019(3) Uani 1 1 d . . . H35 H 0.0216 0.0599 0.5892 0.023 Uiso 1 1 calc R . . C36 C 0.1236(6) 0.0153(6) 0.5876(3) 0.014(3) Uani 1 1 d . . . N37 N 0.1680(5) 0.0607(5) 0.6047(3) 0.019(2) Uani 1 1 d . . . C38 C 0.1411(7) 0.1219(6) 0.6194(4) 0.019(3) Uani 1 1 d . . . C39 C 0.1549(8) 0.1827(6) 0.6024(4) 0.026(3) Uani 1 1 d . . . H39 H 0.1796 0.1843 0.5793 0.031 Uiso 1 1 calc R . . C40 C 0.1321(8) 0.2416(7) 0.6193(4) 0.030(3) Uani 1 1 d . . . C41 C 0.0990(8) 0.2419(7) 0.6530(4) 0.033(4) Uani 1 1 d . . . H41 H 0.0852 0.2832 0.6645 0.040 Uiso 1 1 calc R . . C42 C 0.0858(7) 0.1808(7) 0.6699(4) 0.029(4) Uani 1 1 d . . . C43 C 0.1056(7) 0.1201(7) 0.6541(4) 0.025(3) Uani 1 1 d . . . H43 H 0.0958 0.0783 0.6663 0.030 Uiso 1 1 calc R . . C44 C 0.1589(7) -0.1633(6) 0.5466(4) 0.025(3) Uani 1 1 d . . . C45 C 0.2166(7) -0.1472(7) 0.5163(4) 0.029(3) Uani 1 1 d . . . H45A H 0.2519 -0.1139 0.5269 0.043 Uiso 1 1 calc R . . H45B H 0.1915 -0.1289 0.4932 0.043 Uiso 1 1 calc R . . H45C H 0.2424 -0.1888 0.5100 0.043 Uiso 1 1 calc R . . C46 C 0.1993(7) -0.1961(6) 0.5818(4) 0.026(3) Uani 1 1 d . . . H46A H 0.2335 -0.1633 0.5938 0.039 Uiso 1 1 calc R . . H46B H 0.2266 -0.2359 0.5737 0.039 Uiso 1 1 calc R . . H46C H 0.1637 -0.2100 0.6000 0.039 Uiso 1 1 calc R . . C47 C 0.1061(8) -0.2151(6) 0.5283(4) 0.028(3) Uani 1 1 d . . . H47A H 0.1334 -0.2556 0.5214 0.042 Uiso 1 1 calc R . . H47B H 0.0816 -0.1956 0.5053 0.042 Uiso 1 1 calc R . . H47C H 0.0696 -0.2275 0.5464 0.042 Uiso 1 1 calc R . . C48 C -0.0766(7) -0.0322(6) 0.5626(4) 0.023(3) Uani 1 1 d . . . C49 C -0.1088(7) 0.0385(7) 0.5703(5) 0.032(4) Uani 1 1 d . . . H49A H -0.1623 0.0365 0.5674 0.048 Uiso 1 1 calc R . . H49B H -0.0905 0.0711 0.5521 0.048 Uiso 1 1 calc R . . H49C H -0.0939 0.0527 0.5964 0.048 Uiso 1 1 calc R . . C50 C -0.1040(7) -0.0537(8) 0.5221(4) 0.033(4) Uani 1 1 d . . . H50A H -0.1576 -0.0534 0.5202 0.050 Uiso 1 1 calc R . . H50B H -0.0863 -0.0995 0.5169 0.050 Uiso 1 1 calc R . . H50C H -0.0854 -0.0221 0.5035 0.050 Uiso 1 1 calc R . . C51 C -0.1080(8) -0.0810(7) 0.5922(4) 0.036(4) Uani 1 1 d . . . H51A H -0.1615 -0.0807 0.5893 0.054 Uiso 1 1 calc R . . H51B H -0.0923 -0.0661 0.6180 0.054 Uiso 1 1 calc R . . H51C H -0.0899 -0.1269 0.5879 0.054 Uiso 1 1 calc R . . Cl52 Cl 0.1510(3) 0.31831(19) 0.59755(12) 0.0585(14) Uani 1 1 d . . . Cl53 Cl 0.0447(2) 0.1796(2) 0.71340(11) 0.0449(11) Uani 1 1 d . . . O61 O 0.2313(4) -0.0382(4) 0.6545(2) 0.019(2) Uani 1 1 d . . . C61 C 0.2235(7) -0.0110(6) 0.6880(3) 0.016(3) Uiso 1 1 d . . . C62 C 0.1816(7) -0.0418(6) 0.7169(4) 0.019(3) Uani 1 1 d . . . C63 C 0.1821(7) -0.0109(7) 0.7512(4) 0.024(3) Uani 1 1 d . . . H63 H 0.1551 -0.0312 0.7705 0.029 Uiso 1 1 calc R . . C64 C 0.2211(7) 0.0508(6) 0.7604(4) 0.021(3) Uani 1 1 d . . . C65 C 0.2586(7) 0.0812(7) 0.7328(4) 0.026(3) Uani 1 1 d . . . H65 H 0.2838 0.1224 0.7384 0.031 Uiso 1 1 calc R . . C66 C 0.2609(7) 0.0529(6) 0.6962(4) 0.019(3) Uani 1 1 d . . . N67 N 0.2930(6) 0.0775(5) 0.6656(3) 0.020(2) Uani 1 1 d . . . C68 C 0.3262(7) 0.1427(6) 0.6664(3) 0.017(3) Uani 1 1 d . . . C69 C 0.3982(8) 0.1494(7) 0.6560(4) 0.028(3) Uani 1 1 d . . . H69 H 0.4259 0.1105 0.6500 0.034 Uiso 1 1 calc R . . C70 C 0.4290(8) 0.2130(8) 0.6546(4) 0.034(4) Uani 1 1 d . . . C71 C 0.3923(8) 0.2701(7) 0.6632(4) 0.029(3) Uani 1 1 d . . . H71 H 0.4147 0.3135 0.6625 0.034 Uiso 1 1 calc R . . C72 C 0.3196(8) 0.2620(7) 0.6731(4) 0.032(4) Uani 1 1 d . . . C73 C 0.2871(8) 0.2007(6) 0.6752(4) 0.027(3) Uani 1 1 d . . . H73 H 0.2382 0.1971 0.6827 0.032 Uiso 1 1 calc R . . C74 C 0.1376(7) -0.1069(7) 0.7068(4) 0.025(3) Uani 1 1 d . . . C75 C 0.1879(8) -0.1649(7) 0.6957(4) 0.034(4) Uani 1 1 d . . . H75A H 0.2162 -0.1507 0.6742 0.050 Uiso 1 1 calc R . . H75B H 0.1582 -0.2045 0.6882 0.050 Uiso 1 1 calc R . . H75C H 0.2214 -0.1765 0.7175 0.050 Uiso 1 1 calc R . . C76 C 0.0939(8) -0.1297(8) 0.7404(4) 0.037(4) Uani 1 1 d . . . H76A H 0.1275 -0.1396 0.7624 0.056 Uiso 1 1 calc R . . H76B H 0.0659 -0.1705 0.7332 0.056 Uiso 1 1 calc R . . H76C H 0.0601 -0.0936 0.7470 0.056 Uiso 1 1 calc R . . C77 C 0.0831(7) -0.0918(7) 0.6730(4) 0.030(3) Uani 1 1 d . . . H77A H 0.1099 -0.0769 0.6511 0.045 Uiso 1 1 calc R . . H77B H 0.0494 -0.0560 0.6802 0.045 Uiso 1 1 calc R . . H77C H 0.0553 -0.1328 0.6663 0.045 Uiso 1 1 calc R . . C78 C 0.2174(8) 0.0797(7) 0.8005(4) 0.029(3) Uani 1 1 d . . . C79 C 0.2607(10) 0.1448(8) 0.8068(5) 0.051(5) Uani 1 1 d . . . H79A H 0.2561 0.1605 0.8330 0.077 Uiso 1 1 calc R . . H79B H 0.2417 0.1794 0.7889 0.077 Uiso 1 1 calc R . . H79C H 0.3124 0.1363 0.8025 0.077 Uiso 1 1 calc R . . C80 C 0.1349(9) 0.0955(9) 0.8082(4) 0.046(4) Uani 1 1 d . . . H80A H 0.1056 0.0543 0.8043 0.069 Uiso 1 1 calc R . . H80B H 0.1163 0.1307 0.7905 0.069 Uiso 1 1 calc R . . H80C H 0.1317 0.1113 0.8345 0.069 Uiso 1 1 calc R . . C81 C 0.2457(9) 0.0264(7) 0.8302(4) 0.035(4) Uani 1 1 d . . . H81A H 0.2180 -0.0157 0.8263 0.053 Uiso 1 1 calc R . . H81B H 0.2392 0.0435 0.8560 0.053 Uiso 1 1 calc R . . H81C H 0.2977 0.0177 0.8270 0.053 Uiso 1 1 calc R . . Cl82 Cl 0.5184(2) 0.2206(2) 0.64110(12) 0.0511(12) Uani 1 1 d . . . Cl83 Cl 0.2680(2) 0.33428(18) 0.68265(13) 0.0510(12) Uani 1 1 d . . . N90 N 0.0000 -0.4566(9) 0.7500 0.078(8) Uani 1 2 d SD . . C91 C -0.0217(14) -0.3883(14) 0.7551(12) 0.056(12) Uani 0.50 1 d PD A . H91A H -0.0331 -0.3827 0.7821 0.068 Uiso 0.50 1 calc PR . . H91B H -0.0680 -0.3812 0.7396 0.068 Uiso 0.50 1 calc PR . . C92 C 0.0319(17) -0.3302(13) 0.7450(10) 0.046(9) Uani 0.50 1 d PD . . H92A H 0.0093 -0.2863 0.7500 0.069 Uiso 0.50 1 calc PR A . H92B H 0.0424 -0.3332 0.7180 0.069 Uiso 0.50 1 calc PR . . H92C H 0.0775 -0.3346 0.7608 0.069 Uiso 0.50 1 calc PR . . C93 C 0.040(2) -0.5045(17) 0.7296(7) 0.050(12) Uani 0.50 1 d PD A 1 H93A H 0.0199 -0.5498 0.7349 0.060 Uiso 0.50 1 calc PR A 1 H93B H 0.0912 -0.5040 0.7407 0.060 Uiso 0.50 1 calc PR A 1 C94 C 0.0437(16) -0.4978(17) 0.6855(7) 0.048(10) Uani 0.50 1 d PD A 1 H94A H 0.0735 -0.5346 0.6759 0.072 Uiso 0.50 1 calc PR A 1 H94B H 0.0657 -0.4542 0.6793 0.072 Uiso 0.50 1 calc PR A 1 H94C H -0.0059 -0.5004 0.6735 0.072 Uiso 0.50 1 calc PR A 1 C93X C 0.023(2) -0.4779(17) 0.7141(7) 0.067(16) Uani 0.50 1 d PD A 2 H93C H 0.0523 -0.4405 0.7038 0.080 Uiso 0.50 1 calc PR A 2 H93D H -0.0211 -0.4830 0.6968 0.080 Uiso 0.50 1 calc PR A 2 C94X C 0.069(2) -0.5441(17) 0.7112(11) 0.073(13) Uani 0.50 1 d PD A 2 H94D H 0.0806 -0.5516 0.6846 0.109 Uiso 0.50 1 calc PR A 2 H94E H 0.0407 -0.5825 0.7201 0.109 Uiso 0.50 1 calc PR A 2 H94F H 0.1145 -0.5398 0.7272 0.109 Uiso 0.50 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 Ga1 0.0153(7) 0.0107(7) 0.0230(8) -0.0007(6) 0.0010(6) -0.0002(6) O1 0.015(5) 0.008(4) 0.025(5) 0.004(4) 0.001(4) 0.001(4) C1 0.016(7) 0.027(8) 0.014(7) 0.001(6) -0.010(6) -0.005(6) C2 0.017(7) 0.011(7) 0.024(7) 0.004(6) -0.006(6) -0.002(6) C3 0.013(7) 0.026(8) 0.024(7) 0.000(6) -0.003(6) -0.004(6) C4 0.014(7) 0.019(7) 0.017(7) -0.003(6) -0.003(5) -0.006(6) C5 0.014(7) 0.018(7) 0.020(7) -0.002(6) 0.002(6) -0.003(6) C6 0.024(7) 0.012(7) 0.015(6) -0.003(6) 0.000(6) 0.002(6) N7 0.013(5) 0.023(6) 0.020(6) 0.005(5) 0.000(5) -0.001(5) C8 0.010(6) 0.016(7) 0.022(7) 0.003(6) 0.001(5) -0.006(5) C9 0.017(7) 0.026(8) 0.021(7) 0.000(6) 0.000(6) -0.004(6) C10 0.032(8) 0.023(8) 0.025(8) 0.014(6) 0.004(6) 0.006(6) C11 0.024(8) 0.031(9) 0.046(10) 0.013(8) 0.005(7) 0.002(7) C12 0.029(8) 0.004(7) 0.037(9) -0.009(6) 0.003(6) 0.004(6) C13 0.019(7) 0.018(8) 0.028(8) -0.007(6) 0.005(6) -0.007(6) C14 0.024(7) 0.008(7) 0.029(8) 0.000(6) -0.005(6) 0.002(6) C15 0.031(9) 0.022(8) 0.049(10) 0.026(7) -0.010(7) 0.005(7) C16 0.034(8) 0.009(7) 0.038(8) 0.001(6) -0.020(7) -0.005(6) C17 0.023(8) 0.018(7) 0.028(8) -0.001(6) -0.005(6) 0.005(6) C18 0.015(7) 0.012(7) 0.029(7) 0.005(6) -0.004(6) -0.002(5) C19 0.029(8) 0.022(8) 0.041(9) 0.003(7) -0.005(7) -0.007(6) C20 0.026(8) 0.037(9) 0.023(8) 0.005(6) 0.006(6) -0.005(7) C21 0.013(7) 0.018(7) 0.037(8) -0.004(6) 0.003(6) 0.008(6) Cl22 0.050(2) 0.045(2) 0.034(2) 0.0211(18) 0.0069(18) 0.008(2) Cl23 0.076(3) 0.018(2) 0.048(2) -0.0068(17) 0.001(2) 0.0090(19) O31 0.015(5) 0.007(4) 0.030(5) -0.004(4) 0.000(4) -0.003(4) C31 0.018(8) 0.009(7) 0.017(7) 0.004(5) -0.001(5) -0.006(5) C32 0.025(8) 0.019(7) 0.021(7) 0.001(6) 0.001(6) 0.004(6) C33 0.014(7) 0.017(7) 0.022(7) 0.007(6) 0.001(6) -0.008(6) C35 0.021(7) 0.019(7) 0.018(7) 0.006(6) -0.003(5) 0.004(6) C36 0.013(7) 0.011(6) 0.018(7) 0.003(5) 0.001(5) -0.006(5) N37 0.015(6) 0.023(6) 0.019(6) -0.004(5) -0.001(5) 0.005(5) C38 0.017(7) 0.017(7) 0.023(7) -0.008(6) 0.001(6) 0.003(6) C39 0.037(9) 0.013(7) 0.028(8) -0.001(6) 0.000(6) -0.001(6) C40 0.046(9) 0.014(8) 0.028(8) 0.002(6) -0.007(7) 0.003(7) C41 0.050(10) 0.014(8) 0.034(9) -0.002(6) -0.013(8) 0.007(7) C42 0.024(8) 0.036(9) 0.026(8) -0.003(7) -0.012(6) 0.021(7) C43 0.021(7) 0.026(8) 0.029(8) 0.008(6) 0.011(6) -0.006(6) C44 0.025(8) 0.013(7) 0.037(8) -0.001(6) 0.004(6) -0.003(6) C45 0.024(8) 0.023(8) 0.040(9) -0.014(7) 0.015(7) -0.004(6) C46 0.024(8) 0.011(7) 0.043(9) -0.002(6) 0.004(7) 0.008(6) C47 0.031(8) 0.012(7) 0.042(9) -0.007(6) 0.007(7) -0.005(6) C48 0.028(8) 0.008(7) 0.032(8) -0.006(6) 0.003(6) -0.004(6) C49 0.015(7) 0.018(8) 0.063(10) 0.000(7) -0.003(7) -0.001(6) C50 0.020(8) 0.037(9) 0.041(9) 0.001(7) -0.006(7) -0.003(7) C51 0.031(9) 0.029(9) 0.048(10) 0.007(7) 0.006(7) -0.001(7) Cl52 0.116(4) 0.013(2) 0.045(2) 0.0098(17) -0.011(2) 0.002(2) Cl53 0.041(2) 0.060(3) 0.035(2) -0.0139(19) 0.0112(18) 0.007(2) O61 0.020(5) 0.013(5) 0.025(5) 0.001(4) 0.002(4) -0.004(4) C62 0.024(7) 0.006(7) 0.027(8) 0.003(5) 0.003(6) 0.001(5) C63 0.024(8) 0.023(8) 0.026(8) 0.012(6) 0.006(6) -0.002(6) C64 0.018(7) 0.018(7) 0.027(8) 0.005(6) 0.002(6) 0.008(6) C65 0.023(8) 0.022(8) 0.031(8) 0.004(6) -0.010(6) -0.006(6) C66 0.012(7) 0.020(7) 0.025(8) 0.000(6) -0.005(6) -0.004(6) N67 0.024(6) 0.015(6) 0.019(6) -0.005(5) 0.000(5) -0.005(5) C68 0.023(8) 0.016(7) 0.013(6) -0.005(5) -0.004(6) -0.010(6) C69 0.027(8) 0.036(9) 0.021(8) 0.001(6) -0.004(6) -0.013(7) C70 0.035(9) 0.044(10) 0.024(8) -0.005(7) 0.007(7) -0.001(8) C71 0.046(10) 0.010(7) 0.028(8) 0.001(6) -0.007(7) -0.015(7) C72 0.046(10) 0.009(7) 0.039(9) 0.006(6) -0.013(7) -0.007(7) C73 0.040(9) 0.014(8) 0.025(8) -0.005(6) -0.010(7) 0.002(7) C74 0.018(7) 0.027(8) 0.030(8) 0.006(6) 0.002(6) -0.014(6) C75 0.038(9) 0.012(7) 0.050(10) 0.005(7) -0.005(7) -0.002(6) C76 0.040(9) 0.032(9) 0.040(9) 0.001(7) 0.002(7) -0.020(7) C77 0.024(8) 0.019(8) 0.045(9) 0.006(7) -0.006(7) -0.002(6) C78 0.036(9) 0.025(8) 0.026(8) 0.006(6) 0.010(7) 0.008(7) C79 0.074(13) 0.044(10) 0.036(10) -0.017(8) 0.004(9) -0.023(9) C80 0.059(11) 0.051(11) 0.028(9) 0.008(8) 0.008(8) 0.017(9) C81 0.050(10) 0.030(8) 0.027(8) 0.005(7) 0.000(7) 0.010(8) Cl82 0.047(3) 0.055(3) 0.054(3) -0.015(2) 0.017(2) -0.035(2) Cl83 0.058(3) 0.0132(19) 0.079(3) -0.0098(19) -0.022(2) 0.0047(18) N90 0.11(2) 0.038(14) 0.086(19) 0.000 0.047(17) 0.000 C91 0.04(3) 0.10(3) 0.04(2) 0.00(2) -0.01(2) 0.026(19) C92 0.04(2) 0.035(19) 0.06(2) 0.001(18) 0.007(18) 0.003(16) C93 0.05(2) 0.07(3) 0.03(2) 0.01(2) 0.00(2) -0.01(2) C94 0.034(19) 0.06(3) 0.05(2) -0.025(19) 0.023(17) -0.038(17) C93X 0.10(4) 0.07(3) 0.03(2) -0.03(2) 0.04(3) -0.05(3) C94X 0.09(3) 0.06(3) 0.06(3) 0.01(2) 0.04(3) 0.02(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 Ga1 O1 1.935(8) . ? Ga1 O61 1.956(8) . ? Ga1 O31 1.965(8) . ? Ga1 N7 2.027(10) . ? Ga1 N37 2.045(10) . ? Ga1 N67 2.068(10) . ? O1 C1 1.316(15) . ? C1 C2 1.408(17) . ? C1 C6 1.465(17) . ? C2 C3 1.368(17) . ? C2 C14 1.534(17) . ? C3 C4 1.442(18) . ? C4 C5 1.329(17) . ? C4 C18 1.553(17) . ? C5 C6 1.439(17) . ? C6 N7 1.327(16) . ? N7 C8 1.405(16) . ? C8 C13 1.404(17) . ? C8 C9 1.413(17) . ? C9 C10 1.399(18) . ? C10 C11 1.36(2) . ? C10 Cl22 1.729(13) . ? C11 C12 1.392(19) . ? C12 C13 1.367(18) . ? C12 Cl23 1.753(12) . ? C14 C17 1.520(17) . ? C14 C15 1.532(19) . ? C14 C16 1.570(18) . ? C18 C21 1.502(17) . ? C18 C19 1.515(18) . ? C18 C20 1.561(18) . ? O31 C31 1.275(14) . ? C31 C32 1.433(17) . ? C31 C36 1.453(17) . ? C32 C33 1.367(17) . ? C32 C44 1.530(18) . ? C33 C34 1.436(18) . ? C34 C35 1.347(18) . ? C34 C48 1.508(18) . ? C35 C36 1.431(17) . ? C36 N37 1.332(15) . ? N37 C38 1.412(16) . ? C38 C39 1.370(18) . ? C38 C43 1.415(17) . ? C39 C40 1.382(19) . ? C40 C41 1.36(2) . ? C40 Cl52 1.740(14) . ? C41 C42 1.37(2) . ? C42 C43 1.376(19) . ? C42 Cl53 1.741(14) . ? C44 C47 1.524(18) . ? C44 C46 1.545(19) . ? C44 C45 1.573(18) . ? C48 C50 1.540(18) . ? C48 C49 1.546(18) . ? C48 C51 1.548(19) . ? O61 C61 1.310(14) . ? C61 C62 1.437(17) . ? C61 C66 1.458(17) . ? C62 C63 1.350(18) . ? C62 C74 1.548(18) . ? C63 C64 1.440(19) . ? C64 C65 1.356(18) . ? C64 C78 1.525(19) . ? C65 C66 1.404(18) . ? C66 N67 1.344(16) . ? N67 C68 1.424(16) . ? C68 C69 1.392(18) . ? C68 C73 1.394(18) . ? C69 C70 1.38(2) . ? C70 C71 1.36(2) . ? C70 Cl82 1.736(15) . ? C71 C72 1.40(2) . ? C72 C73 1.353(19) . ? C72 Cl83 1.755(15) . ? C74 C76 1.528(19) . ? C74 C77 1.535(18) . ? C74 C75 1.534(19) . ? C78 C79 1.52(2) . ? C78 C81 1.550(18) . ? C78 C80 1.58(2) . ? N90 C93X 1.42(2) 2_556 ? N90 C93X 1.42(2) . ? N90 C93 1.42(2) 2_556 ? N90 C93 1.42(2) . ? N90 C91 1.42(2) 2_556 ? N90 C91 1.42(2) . ? C91 C92 1.56(2) . ? C93 C94 1.56(2) . ? C93X C94X 1.56(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ga1 O61 174.3(3) . . ? O1 Ga1 O31 100.1(3) . . ? O61 Ga1 O31 85.3(3) . . ? O1 Ga1 N7 81.0(4) . . ? O61 Ga1 N7 100.9(4) . . ? O31 Ga1 N7 89.2(4) . . ? O1 Ga1 N37 89.4(4) . . ? O61 Ga1 N37 89.9(4) . . ? O31 Ga1 N37 79.8(4) . . ? N7 Ga1 N37 164.0(4) . . ? O1 Ga1 N67 95.1(4) . . ? O61 Ga1 N67 79.4(4) . . ? O31 Ga1 N67 164.2(4) . . ? N7 Ga1 N67 97.4(4) . . ? N37 Ga1 N67 96.2(4) . . ? C1 O1 Ga1 115.7(7) . . ? O1 C1 C2 122.9(11) . . ? O1 C1 C6 116.2(11) . . ? C2 C1 C6 120.9(11) . . ? C3 C2 C1 116.8(11) . . ? C3 C2 C14 122.9(11) . . ? C1 C2 C14 120.3(11) . . ? C2 C3 C4 124.0(12) . . ? C5 C4 C3 119.1(12) . . ? C5 C4 C18 122.4(11) . . ? C3 C4 C18 118.4(11) . . ? C4 C5 C6 121.4(12) . . ? N7 C6 C5 128.9(11) . . ? N7 C6 C1 113.5(11) . . ? C5 C6 C1 117.4(11) . . ? C6 N7 C8 122.7(10) . . ? C6 N7 Ga1 113.7(8) . . ? C8 N7 Ga1 122.1(8) . . ? C13 C8 N7 121.9(11) . . ? C13 C8 C9 118.7(12) . . ? N7 C8 C9 119.4(11) . . ? C10 C9 C8 119.1(12) . . ? C11 C10 C9 122.1(13) . . ? C11 C10 Cl22 119.8(11) . . ? C9 C10 Cl22 118.1(11) . . ? C10 C11 C12 118.1(13) . . ? C13 C12 C11 122.6(12) . . ? C13 C12 Cl23 119.4(11) . . ? C11 C12 Cl23 118.0(10) . . ? C12 C13 C8 119.3(12) . . ? C17 C14 C15 109.1(11) . . ? C17 C14 C2 110.6(10) . . ? C15 C14 C2 111.1(11) . . ? C17 C14 C16 109.4(10) . . ? C15 C14 C16 108.0(11) . . ? C2 C14 C16 108.6(10) . . ? C21 C18 C19 109.5(11) . . ? C21 C18 C4 111.2(10) . . ? C19 C18 C4 109.0(11) . . ? C21 C18 C20 108.3(11) . . ? C19 C18 C20 110.4(11) . . ? C4 C18 C20 108.4(10) . . ? C31 O31 Ga1 113.5(7) . . ? O31 C31 C32 123.9(11) . . ? O31 C31 C36 117.8(10) . . ? C32 C31 C36 118.3(11) . . ? C33 C32 C31 117.1(12) . . ? C33 C32 C44 124.0(12) . . ? C31 C32 C44 118.9(11) . . ? C32 C33 C34 126.0(12) . . ? C35 C34 C33 116.9(11) . . ? C35 C34 C48 123.9(11) . . ? C33 C34 C48 119.1(11) . . ? C34 C35 C36 121.5(12) . . ? N37 C36 C35 126.8(11) . . ? N37 C36 C31 113.2(10) . . ? C35 C36 C31 120.0(11) . . ? C36 N37 C38 121.7(10) . . ? C36 N37 Ga1 111.5(8) . . ? C38 N37 Ga1 125.5(8) . . ? C39 C38 N37 121.0(11) . . ? C39 C38 C43 120.2(12) . . ? N37 C38 C43 118.6(11) . . ? C38 C39 C40 118.9(13) . . ? C41 C40 C39 122.5(13) . . ? C41 C40 Cl52 119.2(11) . . ? C39 C40 Cl52 118.2(11) . . ? C40 C41 C42 118.0(13) . . ? C41 C42 C43 122.4(13) . . ? C41 C42 Cl53 119.0(11) . . ? C43 C42 Cl53 118.5(11) . . ? C42 C43 C38 117.9(12) . . ? C47 C44 C32 112.0(11) . . ? C47 C44 C46 108.6(11) . . ? C32 C44 C46 110.5(11) . . ? C47 C44 C45 106.5(11) . . ? C32 C44 C45 110.7(10) . . ? C46 C44 C45 108.4(11) . . ? C34 C48 C50 111.2(11) . . ? C34 C48 C49 111.6(10) . . ? C50 C48 C49 107.7(11) . . ? C34 C48 C51 110.1(11) . . ? C50 C48 C51 109.5(11) . . ? C49 C48 C51 106.6(11) . . ? C61 O61 Ga1 115.3(7) . . ? O61 C61 C62 123.3(11) . . ? O61 C61 C66 117.3(11) . . ? C62 C61 C66 119.4(11) . . ? C63 C62 C61 117.4(11) . . ? C63 C62 C74 123.7(11) . . ? C61 C62 C74 118.9(11) . . ? C62 C63 C64 124.0(12) . . ? C65 C64 C63 118.7(12) . . ? C65 C64 C78 122.9(12) . . ? C63 C64 C78 118.4(11) . . ? C64 C65 C66 121.2(12) . . ? N67 C66 C65 128.6(12) . . ? N67 C66 C61 112.2(11) . . ? C65 C66 C61 119.2(11) . . ? C66 N67 C68 121.2(10) . . ? C66 N67 Ga1 113.5(8) . . ? C68 N67 Ga1 124.1(8) . . ? C69 C68 C73 119.1(12) . . ? C69 C68 N67 119.3(12) . . ? C73 C68 N67 121.5(11) . . ? C70 C69 C68 119.3(14) . . ? C71 C70 C69 122.8(14) . . ? C71 C70 Cl82 118.4(12) . . ? C69 C70 Cl82 118.8(12) . . ? C70 C71 C72 116.6(12) . . ? C73 C72 C71 122.8(13) . . ? C73 C72 Cl83 118.4(12) . . ? C71 C72 Cl83 118.8(10) . . ? C72 C73 C68 119.3(14) . . ? C76 C74 C77 107.9(11) . . ? C76 C74 C75 108.9(12) . . ? C77 C74 C75 108.7(11) . . ? C76 C74 C62 111.0(11) . . ? C77 C74 C62 108.7(11) . . ? C75 C74 C62 111.5(10) . . ? C79 C78 C64 113.6(12) . . ? C79 C78 C81 109.0(13) . . ? C64 C78 C81 109.6(11) . . ? C79 C78 C80 107.7(13) . . ? C64 C78 C80 109.0(12) . . ? C81 C78 C80 107.8(11) . . ? C93X N90 C93X 145(3) 2_556 . ? C93X N90 C93 33.1(17) 2_556 2_556 ? C93X N90 C93 116.2(19) . 2_556 ? C93X N90 C93 116.2(19) 2_556 . ? C93X N90 C93 33.1(17) . . ? C93 N90 C93 96(3) 2_556 . ? C93X N90 C91 119.6(19) 2_556 2_556 ? C93X N90 C91 94(2) . 2_556 ? C93 N90 C91 149(2) 2_556 2_556 ? C93 N90 C91 114(2) . 2_556 ? C93X N90 C91 94(2) 2_556 . ? C93X N90 C91 119.6(19) . . ? C93 N90 C91 114(2) 2_556 . ? C93 N90 C91 149(2) . . ? C91 N90 C91 36(2) 2_556 . ? N90 C91 C92 119.1(15) . . ? N90 C93 C94 119.7(15) . . ? N90 C93X C94X 119.7(16) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.361 _refine_diff_density_min -0.643 _refine_diff_density_rms 0.143 #===END