# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_d1245 #TrackingRef 'web_deposit_cif_file_0_ProfDrTimothyPBender_1352857284.BsubPc compound 3b_d1245.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; Boron subphthalocyanine compound 3b ; _chemical_melting_point ? _chemical_formula_moiety 'C66 H24 B F5 N6 O13, 2(C4 H8 O)' _chemical_formula_sum 'C74 H40 B F5 N6 O15' _chemical_formula_weight 1358.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.0798(5) _cell_length_b 20.9681(8) _cell_length_c 23.1817(11) _cell_angle_alpha 90.00 _cell_angle_beta 91.723(3) _cell_angle_gamma 90.00 _cell_volume 5869.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 9904 _cell_measurement_theta_min 2.84 _cell_measurement_theta_max 65.43 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.538 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2784 _exptl_absorpt_coefficient_mu 1.009 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8800 _exptl_absorpt_correction_T_max 0.9607 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'Bruker Triumph' _diffrn_measurement_device_type 'Bruker APEX-DUO' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38252 _diffrn_reflns_av_R_equivalents 0.0747 _diffrn_reflns_av_sigmaI/netI 0.0569 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_max 66.07 _reflns_number_total 10022 _reflns_number_gt 6944 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 (Bruker, 2007)' _computing_cell_refinement APEX2 _computing_data_reduction 'SAINT (Bruker, 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2009)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^)+(0.0825P)^2^] 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 10022 _refine_ls_number_parameters 910 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0696 _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_ref 0.1430 _refine_ls_wR_factor_gt 0.1333 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _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 F1 F 1.02664(14) 0.81955(7) 0.11033(9) 0.0693(6) Uani 1 1 d . . . F2 F 1.14267(15) 0.84708(8) 0.01622(10) 0.0828(6) Uani 1 1 d . . . F3 F 1.22014(14) 0.75135(10) -0.05041(8) 0.0788(6) Uani 1 1 d . . . F4 F 1.17804(14) 0.62843(9) -0.02197(8) 0.0698(5) Uani 1 1 d . . . F5 F 1.05560(13) 0.60131(6) 0.06988(8) 0.0567(5) Uani 1 1 d . . . O1 O 0.74634(16) 0.79111(8) -0.08742(7) 0.0447(4) Uani 1 1 d . . . O2 O 0.66905(15) 0.91929(8) -0.09951(8) 0.0445(4) Uani 1 1 d . . . O3 O 0.64349(16) 0.99167(7) -0.00816(8) 0.0445(4) Uani 1 1 d . . . O4 O 0.68886(14) 0.94376(7) 0.10529(7) 0.0372(4) Uani 1 1 d . . . O5 O 0.64250(13) 0.85160(7) 0.28608(7) 0.0357(4) Uani 1 1 d . . . O6 O 0.51933(15) 0.79153(7) 0.37430(7) 0.0409(4) Uani 1 1 d . . . O7 O 0.52005(15) 0.66791(7) 0.38670(7) 0.0405(4) Uani 1 1 d . . . O8 O 0.62866(14) 0.58729(7) 0.30671(7) 0.0358(4) Uani 1 1 d . . . O9 O 0.66493(13) 0.45909(7) 0.14946(7) 0.0362(4) Uani 1 1 d . . . O10 O 0.57264(14) 0.39970(7) 0.04814(8) 0.0400(4) Uani 1 1 d . . . O11 O 0.59170(14) 0.45206(7) -0.05343(7) 0.0410(4) Uani 1 1 d . . . O12 O 0.70054(13) 0.57202(7) -0.06633(7) 0.0378(4) Uani 1 1 d . . . O13 O 0.97466(12) 0.69789(7) 0.13852(7) 0.0352(4) Uani 1 1 d . . . N1 N 0.81131(15) 0.75108(8) 0.09169(8) 0.0292(4) Uani 1 1 d . . . N2 N 0.74938(15) 0.81494(8) 0.16897(8) 0.0292(4) Uani 1 1 d . . . N3 N 0.79473(15) 0.70500(8) 0.18394(8) 0.0280(4) Uani 1 1 d . . . N4 N 0.74247(15) 0.59561(8) 0.18884(9) 0.0304(4) Uani 1 1 d . . . N5 N 0.80749(15) 0.63948(8) 0.10143(8) 0.0289(4) Uani 1 1 d . . . N6 N 0.78374(15) 0.68645(8) 0.00850(8) 0.0318(5) Uani 1 1 d . . . C1 C 0.79171(19) 0.74410(10) 0.03408(10) 0.0310(5) Uani 1 1 d . . . C2 C 0.75614(19) 0.80649(10) 0.01366(10) 0.0312(5) Uani 1 1 d . . . C3 C 0.7296(2) 0.82957(11) -0.04087(11) 0.0342(6) Uani 1 1 d . . . C4 C 0.7324(2) 0.81991(12) -0.14104(11) 0.0411(6) Uani 1 1 d . . . C5 C 0.7558(2) 0.78453(14) -0.18860(12) 0.0527(7) Uani 1 1 d . . . H5A H 0.7846 0.7426 -0.1844 0.063 Uiso 1 1 calc R . . C6 C 0.7372(3) 0.81017(17) -0.24274(14) 0.0690(9) Uani 1 1 d . . . H6A H 0.7523 0.7856 -0.2761 0.083 Uiso 1 1 calc R . . C7 C 0.6971(4) 0.87078(19) -0.24862(15) 0.0807(11) Uani 1 1 d . . . H7A H 0.6841 0.8881 -0.2861 0.097 Uiso 1 1 calc R . . C8 C 0.6751(3) 0.90750(15) -0.20019(13) 0.0619(8) Uani 1 1 d . . . H8A H 0.6480 0.9498 -0.2044 0.074 Uiso 1 1 calc R . . C9 C 0.6929(2) 0.88165(12) -0.14658(11) 0.0435(6) Uani 1 1 d . . . C10 C 0.6916(2) 0.89192(11) -0.04636(11) 0.0360(6) Uani 1 1 d . . . C11 C 0.67892(19) 0.93013(10) 0.00185(11) 0.0348(6) Uani 1 1 d . . . C12 C 0.6350(2) 1.02990(10) 0.04048(11) 0.0368(6) Uani 1 1 d . . . C13 C 0.6042(2) 1.09277(12) 0.03269(13) 0.0458(7) Uani 1 1 d . . . H13A H 0.5906 1.1091 -0.0051 0.055 Uiso 1 1 calc R . . C14 C 0.5932(2) 1.13185(12) 0.08015(13) 0.0473(7) Uani 1 1 d . . . H14A H 0.5724 1.1752 0.0749 0.057 Uiso 1 1 calc R . . C15 C 0.6123(2) 1.10852(11) 0.13470(13) 0.0442(7) Uani 1 1 d . . . H15A H 0.6037 1.1356 0.1671 0.053 Uiso 1 1 calc R . . C16 C 0.6442(2) 1.04535(11) 0.14285(12) 0.0380(6) Uani 1 1 d . . . H16A H 0.6578 1.0292 0.1807 0.046 Uiso 1 1 calc R . . C17 C 0.65577(19) 1.00664(10) 0.09563(11) 0.0347(6) Uani 1 1 d . . . C18 C 0.70284(19) 0.90758(10) 0.05696(10) 0.0313(5) Uani 1 1 d . . . C19 C 0.74313(18) 0.84571(10) 0.06318(10) 0.0302(5) Uani 1 1 d . . . C20 C 0.77249(18) 0.80745(10) 0.11359(10) 0.0289(5) Uani 1 1 d . . . C21 C 0.75313(18) 0.76241(10) 0.20222(10) 0.0284(5) Uani 1 1 d . . . C22 C 0.69488(18) 0.74855(10) 0.25450(10) 0.0287(5) Uani 1 1 d . . . C23 C 0.63822(19) 0.78655(10) 0.29216(10) 0.0293(5) Uani 1 1 d . . . C24 C 0.57927(19) 0.88629(10) 0.32403(10) 0.0321(5) Uani 1 1 d . . . C25 C 0.5781(2) 0.95175(11) 0.31815(11) 0.0372(6) Uani 1 1 d . . . H25A H 0.6212 0.9719 0.2897 0.045 Uiso 1 1 calc R . . C26 C 0.5136(2) 0.98767(11) 0.35408(13) 0.0437(7) Uani 1 1 d . . . H26A H 0.5123 1.0328 0.3504 0.052 Uiso 1 1 calc R . . C27 C 0.4512(2) 0.95851(11) 0.39504(13) 0.0461(7) Uani 1 1 d . . . H27A H 0.4067 0.9836 0.4194 0.055 Uiso 1 1 calc R . . C28 C 0.4526(2) 0.89297(11) 0.40115(12) 0.0404(6) Uani 1 1 d . . . H28A H 0.4092 0.8729 0.4294 0.048 Uiso 1 1 calc R . . C29 C 0.5178(2) 0.85716(10) 0.36568(11) 0.0342(6) Uani 1 1 d . . . C30 C 0.57917(19) 0.75772(11) 0.33540(10) 0.0322(5) Uani 1 1 d . . . C31 C 0.57729(19) 0.69139(10) 0.34129(10) 0.0316(5) Uani 1 1 d . . . C32 C 0.5140(2) 0.60201(10) 0.38975(11) 0.0339(6) Uani 1 1 d . . . C33 C 0.4536(2) 0.57587(11) 0.43319(12) 0.0392(6) Uani 1 1 d . . . H33A H 0.4199 0.6027 0.4607 0.047 Uiso 1 1 calc R . . C34 C 0.4421(2) 0.51053(12) 0.43664(13) 0.0505(7) Uani 1 1 d . . . H34A H 0.3981 0.4923 0.4656 0.061 Uiso 1 1 calc R . . C35 C 0.4945(3) 0.47175(12) 0.39793(13) 0.0534(8) Uani 1 1 d . . . H35A H 0.4876 0.4267 0.4008 0.064 Uiso 1 1 calc R . . C36 C 0.5568(2) 0.49789(11) 0.35505(12) 0.0433(6) Uani 1 1 d . . . H36A H 0.5930 0.4710 0.3286 0.052 Uiso 1 1 calc R . . C37 C 0.5665(2) 0.56300(11) 0.35075(10) 0.0333(5) Uani 1 1 d . . . C38 C 0.63183(19) 0.65266(10) 0.30335(10) 0.0295(5) Uani 1 1 d . . . C39 C 0.69269(18) 0.68065(10) 0.26001(10) 0.0284(5) Uani 1 1 d . . . C40 C 0.74963(18) 0.65414(10) 0.21195(10) 0.0283(5) Uani 1 1 d . . . C41 C 0.76430(18) 0.59052(10) 0.13270(10) 0.0298(5) Uani 1 1 d . . . C42 C 0.72460(18) 0.54441(10) 0.09021(10) 0.0293(5) Uani 1 1 d . . . C43 C 0.67186(18) 0.48578(10) 0.09583(10) 0.0308(5) Uani 1 1 d . . . C44 C 0.61036(19) 0.40050(10) 0.15150(11) 0.0348(6) Uani 1 1 d . . . C45 C 0.6004(2) 0.37220(11) 0.20435(12) 0.0393(6) Uani 1 1 d . . . H45A H 0.6315 0.3920 0.2380 0.047 Uiso 1 1 calc R . . C46 C 0.5449(2) 0.31456(12) 0.20859(13) 0.0453(7) Uani 1 1 d . . . H46A H 0.5374 0.2948 0.2451 0.054 Uiso 1 1 calc R . . C47 C 0.5003(2) 0.28599(12) 0.15935(13) 0.0471(7) Uani 1 1 d . . . H47A H 0.4629 0.2463 0.1621 0.057 Uiso 1 1 calc R . . C48 C 0.5100(2) 0.31500(11) 0.10619(13) 0.0445(7) Uani 1 1 d . . . H48A H 0.4783 0.2957 0.0725 0.053 Uiso 1 1 calc R . . C49 C 0.5658(2) 0.37202(11) 0.10242(11) 0.0360(6) Uani 1 1 d . . . C50 C 0.62851(19) 0.45701(10) 0.04676(11) 0.0328(5) Uani 1 1 d . . . C51 C 0.63809(19) 0.48500(10) -0.00731(11) 0.0332(5) Uani 1 1 d . . . C52 C 0.6037(2) 0.48042(11) -0.10713(11) 0.0367(6) Uani 1 1 d . . . C53 C 0.5590(2) 0.44962(13) -0.15471(12) 0.0460(7) Uani 1 1 d . . . H53A H 0.5200 0.4106 -0.1505 0.055 Uiso 1 1 calc R . . C54 C 0.5714(2) 0.47589(13) -0.20863(13) 0.0517(7) Uani 1 1 d . . . H54A H 0.5408 0.4547 -0.2417 0.062 Uiso 1 1 calc R . . C55 C 0.6276(2) 0.53236(13) -0.21522(12) 0.0493(7) Uani 1 1 d . . . H55A H 0.6365 0.5497 -0.2527 0.059 Uiso 1 1 calc R . . C56 C 0.6710(2) 0.56391(12) -0.16720(11) 0.0410(6) Uani 1 1 d . . . H56A H 0.7091 0.6032 -0.1715 0.049 Uiso 1 1 calc R . . C57 C 0.65873(19) 0.53804(11) -0.11343(11) 0.0344(6) Uani 1 1 d . . . C58 C 0.69111(18) 0.54299(10) -0.01380(10) 0.0308(5) Uani 1 1 d . . . C59 C 0.73525(18) 0.57267(10) 0.03486(10) 0.0306(5) Uani 1 1 d . . . C60 C 0.78329(18) 0.63579(10) 0.04369(10) 0.0311(5) Uani 1 1 d . . . C61 C 1.03617(18) 0.70993(10) 0.09192(11) 0.0325(5) Uani 1 1 d . . . C62 C 1.0623(2) 0.77143(11) 0.07649(13) 0.0453(7) Uani 1 1 d . . . C63 C 1.1207(2) 0.78637(13) 0.02992(15) 0.0524(8) Uani 1 1 d . . . C64 C 1.1589(2) 0.73868(15) -0.00448(13) 0.0531(8) Uani 1 1 d . . . C65 C 1.1387(2) 0.67527(13) 0.00973(13) 0.0459(7) Uani 1 1 d . . . C66 C 1.07648(19) 0.66208(10) 0.05774(11) 0.0360(6) Uani 1 1 d . . . B1 B 0.8537(2) 0.69842(12) 0.12937(12) 0.0301(6) Uani 1 1 d . . . O1S O 0.55768(16) 0.69609(9) 0.12299(10) 0.0622(6) Uani 1 1 d . . . C1S C 0.5296(3) 0.70411(17) 0.06357(16) 0.0673(9) Uani 1 1 d . . . H1SA H 0.5436 0.6641 0.0424 0.081 Uiso 1 1 calc R . . H1SB H 0.5756 0.7382 0.0470 0.081 Uiso 1 1 calc R . . C2S C 0.4103(2) 0.72144(15) 0.05764(13) 0.0566(8) Uani 1 1 d . . . H2SA H 0.3699 0.6909 0.0322 0.068 Uiso 1 1 calc R . . H2SB H 0.4013 0.7649 0.0415 0.068 Uiso 1 1 calc R . . C3S C 0.3687(3) 0.71843(17) 0.11821(14) 0.0636(9) Uani 1 1 d . . . H3SA H 0.3319 0.6772 0.1256 0.076 Uiso 1 1 calc R . . H3SB H 0.3163 0.7536 0.1255 0.076 Uiso 1 1 calc R . . C4S C 0.4735(3) 0.72545(16) 0.15471(15) 0.0668(9) Uani 1 1 d . . . H4SA H 0.4908 0.7711 0.1615 0.080 Uiso 1 1 calc R . . H4SB H 0.4658 0.7041 0.1925 0.080 Uiso 1 1 calc R . . O2S O 0.2839(3) 0.86756(15) 0.18629(16) 0.1113(10) Uani 1 1 d . . . C5S C 0.2939(4) 0.9047(2) 0.1364(2) 0.126(2) Uani 1 1 d . . . H5SA H 0.2649 0.9482 0.1425 0.151 Uiso 1 1 calc R . . H5SB H 0.2529 0.8850 0.1034 0.151 Uiso 1 1 calc R . . C6S C 0.4166(3) 0.9064(2) 0.12576(17) 0.0961(14) Uani 1 1 d . . . H6SA H 0.4411 0.8674 0.1058 0.115 Uiso 1 1 calc R . . H6SB H 0.4367 0.9443 0.1028 0.115 Uiso 1 1 calc R . . C7S C 0.4643(3) 0.91010(16) 0.18485(16) 0.0722(10) Uani 1 1 d . . . H7SA H 0.4774 0.9550 0.1965 0.087 Uiso 1 1 calc R . . H7SB H 0.5352 0.8864 0.1881 0.087 Uiso 1 1 calc R . . C8S C 0.3779(3) 0.87972(18) 0.22111(17) 0.0735(10) Uani 1 1 d . . . H8SA H 0.4067 0.8394 0.2379 0.088 Uiso 1 1 calc R . . H8SB H 0.3589 0.9086 0.2531 0.088 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 F1 0.0555(11) 0.0300(8) 0.1228(17) -0.0146(9) 0.0082(10) -0.0046(7) F2 0.0640(12) 0.0570(10) 0.1272(18) 0.0465(11) -0.0003(12) -0.0192(9) F3 0.0449(10) 0.1302(16) 0.0621(12) 0.0387(11) 0.0129(9) -0.0115(10) F4 0.0510(10) 0.0892(12) 0.0703(13) -0.0192(10) 0.0214(9) 0.0143(9) F5 0.0572(10) 0.0265(7) 0.0877(13) 0.0048(7) 0.0252(9) 0.0053(6) O1 0.0615(12) 0.0429(9) 0.0301(10) -0.0038(8) 0.0074(8) -0.0020(8) O2 0.0566(12) 0.0432(10) 0.0338(11) 0.0031(8) 0.0028(9) -0.0011(8) O3 0.0599(12) 0.0335(9) 0.0403(11) 0.0049(8) 0.0026(9) 0.0038(8) O4 0.0484(11) 0.0274(8) 0.0359(10) -0.0009(7) 0.0040(8) 0.0016(7) O5 0.0426(10) 0.0262(8) 0.0391(10) -0.0017(7) 0.0165(8) 0.0031(7) O6 0.0523(11) 0.0283(8) 0.0435(11) 0.0021(7) 0.0219(9) 0.0092(7) O7 0.0509(11) 0.0294(9) 0.0422(11) 0.0044(7) 0.0177(9) 0.0044(7) O8 0.0459(10) 0.0241(8) 0.0377(10) 0.0001(7) 0.0064(8) 0.0023(7) O9 0.0404(10) 0.0310(8) 0.0373(10) -0.0019(7) 0.0030(8) -0.0032(7) O10 0.0450(10) 0.0340(9) 0.0413(11) -0.0059(8) 0.0042(8) -0.0105(7) O11 0.0465(11) 0.0409(9) 0.0357(10) -0.0071(8) 0.0016(8) -0.0083(8) O12 0.0399(10) 0.0402(9) 0.0336(10) -0.0060(8) 0.0066(8) -0.0044(7) O13 0.0243(8) 0.0412(9) 0.0405(10) -0.0012(8) 0.0049(7) -0.0008(7) N1 0.0266(10) 0.0291(9) 0.0322(12) -0.0044(8) 0.0074(8) -0.0011(8) N2 0.0285(10) 0.0279(10) 0.0314(12) -0.0037(8) 0.0041(8) -0.0022(8) N3 0.0254(10) 0.0281(9) 0.0306(11) -0.0037(8) 0.0027(8) 0.0021(7) N4 0.0286(10) 0.0288(10) 0.0339(12) -0.0034(8) 0.0019(8) 0.0041(8) N5 0.0273(10) 0.0287(9) 0.0311(12) -0.0047(8) 0.0056(8) 0.0017(8) N6 0.0296(10) 0.0324(10) 0.0339(12) -0.0039(9) 0.0088(9) -0.0012(8) C1 0.0266(12) 0.0335(12) 0.0334(14) -0.0037(10) 0.0090(10) -0.0021(9) C2 0.0290(12) 0.0317(12) 0.0331(14) -0.0038(10) 0.0083(10) -0.0055(9) C3 0.0357(13) 0.0337(12) 0.0335(15) -0.0033(11) 0.0077(11) -0.0075(10) C4 0.0416(15) 0.0503(15) 0.0319(15) 0.0008(12) 0.0092(12) -0.0102(12) C5 0.0567(19) 0.0630(18) 0.0390(17) -0.0060(14) 0.0134(14) -0.0038(14) C6 0.092(3) 0.081(2) 0.0358(19) -0.0070(16) 0.0168(17) 0.0072(19) C7 0.107(3) 0.099(3) 0.036(2) 0.0102(19) 0.0100(19) 0.009(2) C8 0.077(2) 0.0682(19) 0.0405(19) 0.0087(15) 0.0078(16) 0.0005(17) C9 0.0442(15) 0.0538(16) 0.0328(15) 0.0023(13) 0.0065(12) -0.0108(12) C10 0.0351(14) 0.0402(13) 0.0327(14) 0.0058(11) 0.0018(11) -0.0074(10) C11 0.0343(13) 0.0296(12) 0.0406(16) 0.0026(11) 0.0025(11) -0.0028(10) C12 0.0375(14) 0.0306(12) 0.0427(16) -0.0017(11) 0.0072(11) -0.0022(10) C13 0.0465(16) 0.0391(14) 0.0518(18) 0.0085(13) 0.0041(13) -0.0014(12) C14 0.0470(16) 0.0325(13) 0.063(2) -0.0022(13) 0.0074(14) 0.0014(11) C15 0.0411(15) 0.0379(14) 0.0538(19) -0.0068(13) 0.0061(13) -0.0022(11) C16 0.0346(14) 0.0344(13) 0.0451(16) -0.0045(12) 0.0025(11) -0.0022(10) C17 0.0297(13) 0.0290(12) 0.0458(16) 0.0009(11) 0.0049(11) -0.0021(9) C18 0.0298(12) 0.0323(12) 0.0323(14) -0.0026(11) 0.0062(10) -0.0056(10) C19 0.0279(12) 0.0289(12) 0.0342(14) 0.0004(10) 0.0072(10) -0.0052(9) C20 0.0253(12) 0.0264(11) 0.0352(14) -0.0040(10) 0.0041(10) -0.0034(9) C21 0.0266(12) 0.0250(11) 0.0336(14) -0.0050(10) 0.0008(10) -0.0006(9) C22 0.0261(12) 0.0285(11) 0.0315(14) -0.0028(10) 0.0006(10) 0.0014(9) C23 0.0335(13) 0.0245(11) 0.0300(13) -0.0016(10) 0.0031(10) 0.0024(9) C24 0.0312(13) 0.0297(12) 0.0358(14) -0.0066(10) 0.0066(11) 0.0030(9) C25 0.0349(14) 0.0300(12) 0.0474(16) -0.0037(11) 0.0096(12) -0.0040(10) C26 0.0399(15) 0.0261(12) 0.066(2) -0.0102(12) 0.0168(13) -0.0030(10) C27 0.0402(15) 0.0342(13) 0.065(2) -0.0155(13) 0.0207(14) -0.0020(11) C28 0.0363(14) 0.0367(13) 0.0491(17) -0.0034(12) 0.0162(12) -0.0002(11) C29 0.0359(13) 0.0275(12) 0.0394(15) -0.0021(10) 0.0066(11) 0.0012(10) C30 0.0327(13) 0.0319(12) 0.0326(14) -0.0021(10) 0.0066(10) 0.0053(10) C31 0.0324(13) 0.0314(12) 0.0312(14) 0.0029(10) 0.0055(10) 0.0027(10) C32 0.0335(13) 0.0287(12) 0.0393(15) 0.0035(11) -0.0026(11) 0.0025(10) C33 0.0364(14) 0.0370(13) 0.0446(17) 0.0080(11) 0.0062(12) 0.0018(10) C34 0.0516(17) 0.0434(15) 0.0568(19) 0.0109(14) 0.0087(14) -0.0046(13) C35 0.065(2) 0.0326(14) 0.062(2) 0.0108(14) 0.0051(16) -0.0084(13) C36 0.0519(17) 0.0306(13) 0.0473(17) -0.0028(12) -0.0005(13) -0.0013(11) C37 0.0348(13) 0.0345(12) 0.0305(14) 0.0061(11) -0.0017(11) -0.0017(10) C38 0.0330(13) 0.0257(11) 0.0297(13) -0.0003(10) -0.0008(10) 0.0019(9) C39 0.0286(12) 0.0281(11) 0.0284(13) -0.0011(9) -0.0005(10) 0.0021(9) C40 0.0252(12) 0.0277(11) 0.0320(13) 0.0004(10) -0.0002(10) 0.0030(9) C41 0.0234(11) 0.0304(12) 0.0358(14) -0.0014(10) 0.0024(10) 0.0054(9) C42 0.0265(12) 0.0285(11) 0.0331(14) -0.0054(10) 0.0052(10) 0.0038(9) C43 0.0279(12) 0.0290(11) 0.0359(15) -0.0030(10) 0.0062(10) 0.0038(9) C44 0.0283(12) 0.0276(12) 0.0487(17) -0.0020(11) 0.0059(11) 0.0029(9) C45 0.0360(14) 0.0372(13) 0.0449(17) 0.0005(12) 0.0019(12) 0.0053(11) C46 0.0377(15) 0.0421(14) 0.0561(19) 0.0112(13) 0.0026(13) 0.0007(11) C47 0.0418(16) 0.0362(14) 0.063(2) 0.0038(14) 0.0052(14) -0.0062(11) C48 0.0392(15) 0.0380(14) 0.0566(19) -0.0063(13) 0.0042(13) -0.0063(11) C49 0.0328(13) 0.0324(12) 0.0429(16) -0.0013(11) 0.0056(11) 0.0030(10) C50 0.0307(13) 0.0284(11) 0.0395(15) -0.0056(11) 0.0053(11) 0.0001(9) C51 0.0301(13) 0.0332(12) 0.0363(15) -0.0108(11) 0.0042(11) 0.0003(10) C52 0.0344(13) 0.0402(13) 0.0359(15) -0.0055(11) 0.0043(11) 0.0045(11) C53 0.0464(16) 0.0448(14) 0.0462(18) -0.0086(13) -0.0077(13) 0.0045(12) C54 0.0580(18) 0.0560(17) 0.0404(17) -0.0119(14) -0.0090(14) 0.0065(14) C55 0.0523(17) 0.0577(17) 0.0377(17) -0.0030(13) -0.0008(13) 0.0088(14) C56 0.0381(14) 0.0461(14) 0.0388(16) -0.0046(12) 0.0033(12) 0.0053(11) C57 0.0295(13) 0.0405(13) 0.0333(14) -0.0078(11) 0.0038(11) 0.0058(10) C58 0.0280(12) 0.0334(12) 0.0316(14) -0.0034(10) 0.0083(10) 0.0038(9) C59 0.0271(12) 0.0300(12) 0.0352(14) -0.0075(10) 0.0080(10) 0.0036(9) C60 0.0256(12) 0.0338(12) 0.0345(14) -0.0054(11) 0.0090(10) 0.0031(9) C61 0.0230(12) 0.0281(12) 0.0465(16) 0.0012(11) 0.0040(11) -0.0003(9) C62 0.0303(14) 0.0328(13) 0.073(2) 0.0065(13) 0.0032(13) -0.0024(10) C63 0.0365(15) 0.0411(15) 0.079(2) 0.0216(15) 0.0006(15) -0.0019(12) C64 0.0312(15) 0.079(2) 0.0490(18) 0.0304(16) 0.0045(13) -0.0105(14) C65 0.0301(14) 0.0585(17) 0.0493(18) -0.0052(14) 0.0082(12) 0.0097(12) C66 0.0296(13) 0.0268(12) 0.0520(17) 0.0059(11) 0.0090(12) 0.0027(9) B1 0.0253(13) 0.0289(13) 0.0362(16) -0.0022(12) 0.0038(11) 0.0009(10) O1S 0.0426(12) 0.0595(12) 0.0833(17) -0.0075(11) -0.0165(11) 0.0095(9) C1S 0.0386(17) 0.085(2) 0.079(3) 0.0064(19) 0.0046(16) -0.0015(15) C2S 0.0442(17) 0.0681(18) 0.058(2) -0.0036(15) 0.0014(15) 0.0131(14) C3S 0.0457(18) 0.089(2) 0.056(2) 0.0009(17) -0.0006(15) 0.0189(16) C4S 0.061(2) 0.071(2) 0.067(2) -0.0140(17) -0.0150(17) 0.0196(16) O2S 0.090(2) 0.117(2) 0.129(3) -0.028(2) 0.022(2) -0.0231(17) C5S 0.084(3) 0.124(4) 0.166(5) 0.073(4) -0.060(3) -0.030(3) C6S 0.067(3) 0.150(4) 0.070(3) 0.051(3) -0.018(2) -0.014(2) C7S 0.058(2) 0.068(2) 0.091(3) 0.0209(19) 0.0058(19) 0.0003(16) C8S 0.057(2) 0.083(2) 0.081(3) -0.017(2) 0.0111(19) -0.0113(17) _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 F1 C62 1.356(3) . ? F2 C63 1.340(3) . ? F3 C64 1.341(3) . ? F4 C65 1.324(3) . ? F5 C66 1.331(3) . ? O1 C3 1.367(3) . ? O1 C4 1.388(3) . ? O2 C10 1.379(3) . ? O2 C9 1.384(3) . ? O3 C11 1.377(3) . ? O3 C12 1.390(3) . ? O4 C18 1.368(3) . ? O4 C17 1.394(3) . ? O5 C23 1.372(3) . ? O5 C24 1.388(3) . ? O6 C30 1.370(3) . ? O6 C29 1.391(3) . ? O7 C31 1.368(3) . ? O7 C32 1.386(3) . ? O8 C38 1.374(3) . ? O8 C37 1.383(3) . ? O9 C43 1.368(3) . ? O9 C44 1.396(3) . ? O10 C50 1.379(3) . ? O10 C49 1.390(3) . ? O11 C51 1.378(3) . ? O11 C52 1.391(3) . ? O12 C58 1.369(3) . ? O12 C57 1.386(3) . ? O13 C61 1.353(3) . ? O13 B1 1.470(3) . ? N1 C1 1.357(3) . ? N1 C20 1.374(3) . ? N1 B1 1.489(3) . ? N2 C20 1.331(3) . ? N2 C21 1.344(3) . ? N3 C40 1.370(3) . ? N3 C21 1.376(3) . ? N3 B1 1.477(3) . ? N4 C41 1.340(3) . ? N4 C40 1.341(3) . ? N5 C60 1.364(3) . ? N5 C41 1.369(3) . ? N5 B1 1.495(3) . ? N6 C60 1.340(3) . ? N6 C1 1.349(3) . ? C1 C2 1.452(3) . ? C2 C3 1.382(3) . ? C2 C19 1.425(3) . ? C3 C10 1.390(3) . ? C4 C5 1.365(4) . ? C4 C9 1.384(4) . ? C5 C6 1.378(4) . ? C5 H5A 0.9500 . ? C6 C7 1.365(5) . ? C6 H6A 0.9500 . ? C7 C8 1.394(5) . ? C7 H7A 0.9500 . ? C8 C9 1.367(4) . ? C8 H8A 0.9500 . ? C10 C11 1.387(4) . ? C11 C18 1.384(3) . ? C12 C13 1.380(3) . ? C12 C17 1.384(4) . ? C13 C14 1.381(4) . ? C13 H13A 0.9500 . ? C14 C15 1.369(4) . ? C14 H14A 0.9500 . ? C15 C16 1.391(3) . ? C15 H15A 0.9500 . ? C16 C17 1.373(3) . ? C16 H16A 0.9500 . ? C18 C19 1.392(3) . ? C19 C20 1.453(3) . ? C21 C22 1.449(3) . ? C22 C23 1.379(3) . ? C22 C39 1.430(3) . ? C23 C30 1.386(3) . ? C24 C29 1.379(3) . ? C24 C25 1.379(3) . ? C25 C26 1.381(3) . ? C25 H25A 0.9500 . ? C26 C27 1.373(4) . ? C26 H26A 0.9500 . ? C27 C28 1.382(3) . ? C27 H27A 0.9500 . ? C28 C29 1.378(3) . ? C28 H28A 0.9500 . ? C30 C31 1.398(3) . ? C31 C38 1.379(3) . ? C32 C33 1.375(3) . ? C32 C37 1.387(3) . ? C33 C34 1.380(3) . ? C33 H33A 0.9500 . ? C34 C35 1.379(4) . ? C34 H34A 0.9500 . ? C35 C36 1.379(4) . ? C35 H35A 0.9500 . ? C36 C37 1.374(3) . ? C36 H36A 0.9500 . ? C38 C39 1.392(3) . ? C39 C40 1.439(3) . ? C41 C42 1.451(3) . ? C42 C43 1.393(3) . ? C42 C59 1.423(3) . ? C43 C50 1.377(3) . ? C44 C45 1.370(4) . ? C44 C49 1.380(3) . ? C45 C46 1.387(3) . ? C45 H45A 0.9500 . ? C46 C47 1.384(4) . ? C46 H46A 0.9500 . ? C47 C48 1.382(4) . ? C47 H47A 0.9500 . ? C48 C49 1.377(3) . ? C48 H48A 0.9500 . ? C50 C51 1.392(3) . ? C51 C58 1.385(3) . ? C52 C53 1.375(4) . ? C52 C57 1.389(3) . ? C53 C54 1.378(4) . ? C53 H53A 0.9500 . ? C54 C55 1.375(4) . ? C54 H54A 0.9500 . ? C55 C56 1.385(4) . ? C55 H55A 0.9500 . ? C56 C57 1.372(3) . ? C56 H56A 0.9500 . ? C58 C59 1.381(3) . ? C59 C60 1.457(3) . ? C61 C66 1.377(3) . ? C61 C62 1.377(3) . ? C62 C63 1.345(4) . ? C63 C64 1.368(4) . ? C64 C65 1.393(4) . ? C65 C66 1.389(4) . ? O1S C4S 1.413(4) . ? O1S C1S 1.419(4) . ? C1S C2S 1.488(4) . ? C1S H1SA 0.9900 . ? C1S H1SB 0.9900 . ? C2S C3S 1.507(4) . ? C2S H2SA 0.9900 . ? C2S H2SB 0.9900 . ? C3S C4S 1.509(4) . ? C3S H3SA 0.9900 . ? C3S H3SB 0.9900 . ? C4S H4SA 0.9900 . ? C4S H4SB 0.9900 . ? O2S C8S 1.397(4) . ? O2S C5S 1.402(5) . ? C5S C6S 1.511(6) . ? C5S H5SA 0.9900 . ? C5S H5SB 0.9900 . ? C6S C7S 1.472(5) . ? C6S H6SA 0.9900 . ? C6S H6SB 0.9900 . ? C7S C8S 1.501(5) . ? C7S H7SA 0.9900 . ? C7S H7SB 0.9900 . ? C8S H8SA 0.9900 . ? C8S H8SB 0.9900 . ? 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 C3 O1 C4 115.71(19) . . ? C10 O2 C9 115.27(19) . . ? C11 O3 C12 115.71(19) . . ? C18 O4 C17 115.77(19) . . ? C23 O5 C24 115.64(18) . . ? C30 O6 C29 115.00(18) . . ? C31 O7 C32 115.27(18) . . ? C38 O8 C37 115.22(18) . . ? C43 O9 C44 115.63(18) . . ? C50 O10 C49 115.30(19) . . ? C51 O11 C52 115.43(18) . . ? C58 O12 C57 115.72(18) . . ? C61 O13 B1 116.78(19) . . ? C1 N1 C20 113.88(19) . . ? C1 N1 B1 122.95(18) . . ? C20 N1 B1 122.4(2) . . ? C20 N2 C21 116.86(18) . . ? C40 N3 C21 112.39(18) . . ? C40 N3 B1 122.82(18) . . ? C21 N3 B1 122.38(19) . . ? C41 N4 C40 116.66(19) . . ? C60 N5 C41 113.78(18) . . ? C60 N5 B1 122.57(19) . . ? C41 N5 B1 122.2(2) . . ? C60 N6 C1 116.4(2) . . ? N6 C1 N1 122.5(2) . . ? N6 C1 C2 130.4(2) . . ? N1 C1 C2 105.36(18) . . ? C3 C2 C19 120.4(2) . . ? C3 C2 C1 132.2(2) . . ? C19 C2 C1 107.2(2) . . ? O1 C3 C2 118.7(2) . . ? O1 C3 C10 122.6(2) . . ? C2 C3 C10 118.7(2) . . ? C5 C4 C9 120.8(3) . . ? C5 C4 O1 117.7(2) . . ? C9 C4 O1 121.5(2) . . ? C4 C5 C6 119.4(3) . . ? C4 C5 H5A 120.3 . . ? C6 C5 H5A 120.3 . . ? C7 C6 C5 120.1(3) . . ? C7 C6 H6A 119.9 . . ? C5 C6 H6A 119.9 . . ? C6 C7 C8 120.6(3) . . ? C6 C7 H7A 119.7 . . ? C8 C7 H7A 119.7 . . ? C9 C8 C7 119.0(3) . . ? C9 C8 H8A 120.5 . . ? C7 C8 H8A 120.5 . . ? C8 C9 O2 117.4(2) . . ? C8 C9 C4 120.0(3) . . ? O2 C9 C4 122.6(2) . . ? O2 C10 C11 117.1(2) . . ? O2 C10 C3 121.9(2) . . ? C11 C10 C3 120.9(2) . . ? O3 C11 C18 122.1(2) . . ? O3 C11 C10 116.5(2) . . ? C18 C11 C10 121.4(2) . . ? C13 C12 C17 119.9(2) . . ? C13 C12 O3 118.1(2) . . ? C17 C12 O3 122.0(2) . . ? C12 C13 C14 119.6(3) . . ? C12 C13 H13A 120.2 . . ? C14 C13 H13A 120.2 . . ? C15 C14 C13 120.4(2) . . ? C15 C14 H14A 119.8 . . ? C13 C14 H14A 119.8 . . ? C14 C15 C16 120.3(3) . . ? C14 C15 H15A 119.9 . . ? C16 C15 H15A 119.9 . . ? C17 C16 C15 119.3(3) . . ? C17 C16 H16A 120.4 . . ? C15 C16 H16A 120.4 . . ? C16 C17 C12 120.5(2) . . ? C16 C17 O4 117.8(2) . . ? C12 C17 O4 121.7(2) . . ? O4 C18 C11 122.6(2) . . ? O4 C18 C19 118.9(2) . . ? C11 C18 C19 118.5(2) . . ? C18 C19 C2 120.1(2) . . ? C18 C19 C20 132.4(2) . . ? C2 C19 C20 107.41(19) . . ? N2 C20 N1 122.8(2) . . ? N2 C20 C19 131.1(2) . . ? N1 C20 C19 104.80(19) . . ? N2 C21 N3 123.1(2) . . ? N2 C21 C22 129.4(2) . . ? N3 C21 C22 105.85(18) . . ? C23 C22 C39 120.5(2) . . ? C23 C22 C21 132.6(2) . . ? C39 C22 C21 106.56(19) . . ? O5 C23 C22 119.2(2) . . ? O5 C23 C30 122.0(2) . . ? C22 C23 C30 118.8(2) . . ? C29 C24 C25 120.4(2) . . ? C29 C24 O5 122.01(19) . . ? C25 C24 O5 117.6(2) . . ? C24 C25 C26 119.1(2) . . ? C24 C25 H25A 120.4 . . ? C26 C25 H25A 120.4 . . ? C27 C26 C25 120.4(2) . . ? C27 C26 H26A 119.8 . . ? C25 C26 H26A 119.8 . . ? C26 C27 C28 120.6(2) . . ? C26 C27 H27A 119.7 . . ? C28 C27 H27A 119.7 . . ? C29 C28 C27 119.1(2) . . ? C29 C28 H28A 120.5 . . ? C27 C28 H28A 120.5 . . ? C28 C29 C24 120.4(2) . . ? C28 C29 O6 117.3(2) . . ? C24 C29 O6 122.3(2) . . ? O6 C30 C23 122.9(2) . . ? O6 C30 C31 116.1(2) . . ? C23 C30 C31 121.0(2) . . ? O7 C31 C38 122.7(2) . . ? O7 C31 C30 116.3(2) . . ? C38 C31 C30 120.9(2) . . ? C33 C32 O7 117.7(2) . . ? C33 C32 C37 120.4(2) . . ? O7 C32 C37 121.9(2) . . ? C32 C33 C34 119.6(3) . . ? C32 C33 H33A 120.2 . . ? C34 C33 H33A 120.2 . . ? C35 C34 C33 119.9(3) . . ? C35 C34 H34A 120.0 . . ? C33 C34 H34A 120.0 . . ? C36 C35 C34 120.4(2) . . ? C36 C35 H35A 119.8 . . ? C34 C35 H35A 119.8 . . ? C37 C36 C35 119.8(3) . . ? C37 C36 H36A 120.1 . . ? C35 C36 H36A 120.1 . . ? C36 C37 O8 117.9(2) . . ? C36 C37 C32 119.8(2) . . ? O8 C37 C32 122.2(2) . . ? O8 C38 C31 122.5(2) . . ? O8 C38 C39 118.5(2) . . ? C31 C38 C39 119.0(2) . . ? C38 C39 C22 119.7(2) . . ? C38 C39 C40 132.2(2) . . ? C22 C39 C40 107.76(19) . . ? N4 C40 N3 123.0(2) . . ? N4 C40 C39 129.5(2) . . ? N3 C40 C39 105.81(17) . . ? N4 C41 N5 122.94(19) . . ? N4 C41 C42 129.9(2) . . ? N5 C41 C42 105.3(2) . . ? C43 C42 C59 120.4(2) . . ? C43 C42 C41 131.9(2) . . ? C59 C42 C41 107.32(19) . . ? O9 C43 C50 122.6(2) . . ? O9 C43 C42 119.1(2) . . ? C50 C43 C42 118.2(2) . . ? C45 C44 C49 120.5(2) . . ? C45 C44 O9 117.8(2) . . ? C49 C44 O9 121.7(2) . . ? C44 C45 C46 119.8(3) . . ? C44 C45 H45A 120.1 . . ? C46 C45 H45A 120.1 . . ? C47 C46 C45 119.7(3) . . ? C47 C46 H46A 120.1 . . ? C45 C46 H46A 120.1 . . ? C48 C47 C46 120.2(2) . . ? C48 C47 H47A 119.9 . . ? C46 C47 H47A 119.9 . . ? C49 C48 C47 119.6(3) . . ? C49 C48 H48A 120.2 . . ? C47 C48 H48A 120.2 . . ? C48 C49 C44 120.2(2) . . ? C48 C49 O10 117.6(2) . . ? C44 C49 O10 122.2(2) . . ? C43 C50 O10 122.5(2) . . ? C43 C50 C51 121.3(2) . . ? O10 C50 C51 116.2(2) . . ? O11 C51 C58 122.3(2) . . ? O11 C51 C50 116.4(2) . . ? C58 C51 C50 121.3(2) . . ? C53 C52 C57 120.1(2) . . ? C53 C52 O11 117.9(2) . . ? C57 C52 O11 121.9(2) . . ? C52 C53 C54 119.3(3) . . ? C52 C53 H53A 120.4 . . ? C54 C53 H53A 120.4 . . ? C55 C54 C53 120.8(3) . . ? C55 C54 H54A 119.6 . . ? C53 C54 H54A 119.6 . . ? C54 C55 C56 119.9(3) . . ? C54 C55 H55A 120.1 . . ? C56 C55 H55A 120.1 . . ? C57 C56 C55 119.5(3) . . ? C57 C56 H56A 120.2 . . ? C55 C56 H56A 120.2 . . ? C56 C57 O12 117.8(2) . . ? C56 C57 C52 120.3(2) . . ? O12 C57 C52 121.9(2) . . ? O12 C58 C59 119.1(2) . . ? O12 C58 C51 122.6(2) . . ? C59 C58 C51 118.4(2) . . ? C58 C59 C42 120.4(2) . . ? C58 C59 C60 131.8(2) . . ? C42 C59 C60 107.3(2) . . ? N6 C60 N5 123.2(2) . . ? N6 C60 C59 130.1(2) . . ? N5 C60 C59 105.21(19) . . ? O13 C61 C66 122.4(2) . . ? O13 C61 C62 121.2(2) . . ? C66 C61 C62 116.4(2) . . ? C63 C62 F1 118.3(2) . . ? C63 C62 C61 123.8(3) . . ? F1 C62 C61 117.8(2) . . ? F2 C63 C62 121.6(3) . . ? F2 C63 C64 118.9(3) . . ? C62 C63 C64 119.5(2) . . ? F3 C64 C63 121.4(3) . . ? F3 C64 C65 118.8(3) . . ? C63 C64 C65 119.7(3) . . ? F4 C65 C66 120.6(2) . . ? F4 C65 C64 120.5(3) . . ? C66 C65 C64 118.9(3) . . ? F5 C66 C61 120.2(2) . . ? F5 C66 C65 118.1(2) . . ? C61 C66 C65 121.7(2) . . ? O13 B1 N3 112.3(2) . . ? O13 B1 N1 114.39(19) . . ? N3 B1 N1 105.48(18) . . ? O13 B1 N5 114.38(19) . . ? N3 B1 N5 105.36(19) . . ? N1 B1 N5 104.0(2) . . ? C4S O1S C1S 107.4(2) . . ? O1S C1S C2S 108.7(3) . . ? O1S C1S H1SA 109.9 . . ? C2S C1S H1SA 109.9 . . ? O1S C1S H1SB 109.9 . . ? C2S C1S H1SB 109.9 . . ? H1SA C1S H1SB 108.3 . . ? C1S C2S C3S 104.6(3) . . ? C1S C2S H2SA 110.8 . . ? C3S C2S H2SA 110.8 . . ? C1S C2S H2SB 110.8 . . ? C3S C2S H2SB 110.8 . . ? H2SA C2S H2SB 108.9 . . ? C2S C3S C4S 102.8(3) . . ? C2S C3S H3SA 111.2 . . ? C4S C3S H3SA 111.2 . . ? C2S C3S H3SB 111.2 . . ? C4S C3S H3SB 111.2 . . ? H3SA C3S H3SB 109.1 . . ? O1S C4S C3S 105.7(3) . . ? O1S C4S H4SA 110.6 . . ? C3S C4S H4SA 110.6 . . ? O1S C4S H4SB 110.6 . . ? C3S C4S H4SB 110.6 . . ? H4SA C4S H4SB 108.7 . . ? C8S O2S C5S 106.6(3) . . ? O2S C5S C6S 105.0(3) . . ? O2S C5S H5SA 110.8 . . ? C6S C5S H5SA 110.8 . . ? O2S C5S H5SB 110.8 . . ? C6S C5S H5SB 110.8 . . ? H5SA C5S H5SB 108.8 . . ? C7S C6S C5S 102.0(4) . . ? C7S C6S H6SA 111.4 . . ? C5S C6S H6SA 111.4 . . ? C7S C6S H6SB 111.4 . . ? C5S C6S H6SB 111.4 . . ? H6SA C6S H6SB 109.2 . . ? C6S C7S C8S 103.9(3) . . ? C6S C7S H7SA 111.0 . . ? C8S C7S H7SA 111.0 . . ? C6S C7S H7SB 111.0 . . ? C8S C7S H7SB 111.0 . . ? H7SA C7S H7SB 109.0 . . ? O2S C8S C7S 108.7(3) . . ? O2S C8S H8SA 109.9 . . ? C7S C8S H8SA 109.9 . . ? O2S C8S H8SB 109.9 . . ? C7S C8S H8SB 109.9 . . ? H8SA C8S H8SB 108.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C60 N6 C1 N1 7.5(3) . . . . ? C60 N6 C1 C2 -155.0(2) . . . . ? C20 N1 C1 N6 -154.3(2) . . . . ? B1 N1 C1 N6 16.0(3) . . . . ? C20 N1 C1 C2 12.0(2) . . . . ? B1 N1 C1 C2 -177.71(19) . . . . ? N6 C1 C2 C3 -18.5(4) . . . . ? N1 C1 C2 C3 176.7(2) . . . . ? N6 C1 C2 C19 157.4(2) . . . . ? N1 C1 C2 C19 -7.4(2) . . . . ? C4 O1 C3 C2 -171.6(2) . . . . ? C4 O1 C3 C10 5.5(3) . . . . ? C19 C2 C3 O1 178.1(2) . . . . ? C1 C2 C3 O1 -6.4(4) . . . . ? C19 C2 C3 C10 0.9(3) . . . . ? C1 C2 C3 C10 176.3(2) . . . . ? C3 O1 C4 C5 175.5(2) . . . . ? C3 O1 C4 C9 -6.4(3) . . . . ? C9 C4 C5 C6 -1.6(4) . . . . ? O1 C4 C5 C6 176.4(3) . . . . ? C4 C5 C6 C7 0.8(5) . . . . ? C5 C6 C7 C8 0.3(6) . . . . ? C6 C7 C8 C9 -0.8(6) . . . . ? C7 C8 C9 O2 -179.3(3) . . . . ? C7 C8 C9 C4 0.0(5) . . . . ? C10 O2 C9 C8 -178.1(2) . . . . ? C10 O2 C9 C4 2.6(3) . . . . ? C5 C4 C9 C8 1.2(4) . . . . ? O1 C4 C9 C8 -176.8(3) . . . . ? C5 C4 C9 O2 -179.5(2) . . . . ? O1 C4 C9 O2 2.5(4) . . . . ? C9 O2 C10 C11 174.0(2) . . . . ? C9 O2 C10 C3 -3.5(3) . . . . ? O1 C3 C10 O2 -0.6(4) . . . . ? C2 C3 C10 O2 176.6(2) . . . . ? O1 C3 C10 C11 -178.0(2) . . . . ? C2 C3 C10 C11 -0.9(4) . . . . ? C12 O3 C11 C18 1.0(3) . . . . ? C12 O3 C11 C10 -177.9(2) . . . . ? O2 C10 C11 O3 0.8(3) . . . . ? C3 C10 C11 O3 178.4(2) . . . . ? O2 C10 C11 C18 -178.0(2) . . . . ? C3 C10 C11 C18 -0.4(4) . . . . ? C11 O3 C12 C13 177.4(2) . . . . ? C11 O3 C12 C17 -2.9(3) . . . . ? C17 C12 C13 C14 -0.7(4) . . . . ? O3 C12 C13 C14 179.0(2) . . . . ? C12 C13 C14 C15 -0.3(4) . . . . ? C13 C14 C15 C16 0.8(4) . . . . ? C14 C15 C16 C17 -0.3(4) . . . . ? C15 C16 C17 C12 -0.6(4) . . . . ? C15 C16 C17 O4 179.4(2) . . . . ? C13 C12 C17 C16 1.1(4) . . . . ? O3 C12 C17 C16 -178.5(2) . . . . ? C13 C12 C17 O4 -178.9(2) . . . . ? O3 C12 C17 O4 1.4(4) . . . . ? C18 O4 C17 C16 -177.9(2) . . . . ? C18 O4 C17 C12 2.1(3) . . . . ? C17 O4 C18 C11 -4.1(3) . . . . ? C17 O4 C18 C19 175.6(2) . . . . ? O3 C11 C18 O4 2.7(4) . . . . ? C10 C11 C18 O4 -178.6(2) . . . . ? O3 C11 C18 C19 -177.0(2) . . . . ? C10 C11 C18 C19 1.7(3) . . . . ? O4 C18 C19 C2 178.59(19) . . . . ? C11 C18 C19 C2 -1.7(3) . . . . ? O4 C18 C19 C20 2.5(4) . . . . ? C11 C18 C19 C20 -177.8(2) . . . . ? C3 C2 C19 C18 0.4(3) . . . . ? C1 C2 C19 C18 -176.1(2) . . . . ? C3 C2 C19 C20 177.4(2) . . . . ? C1 C2 C19 C20 0.9(2) . . . . ? C21 N2 C20 N1 -7.6(3) . . . . ? C21 N2 C20 C19 157.2(2) . . . . ? C1 N1 C20 N2 156.9(2) . . . . ? B1 N1 C20 N2 -13.5(3) . . . . ? C1 N1 C20 C19 -11.4(2) . . . . ? B1 N1 C20 C19 178.24(19) . . . . ? C18 C19 C20 N2 15.4(4) . . . . ? C2 C19 C20 N2 -161.0(2) . . . . ? C18 C19 C20 N1 -177.7(2) . . . . ? C2 C19 C20 N1 5.9(2) . . . . ? C20 N2 C21 N3 9.9(3) . . . . ? C20 N2 C21 C22 -153.6(2) . . . . ? C40 N3 C21 N2 -153.7(2) . . . . ? B1 N3 C21 N2 9.1(3) . . . . ? C40 N3 C21 C22 13.0(2) . . . . ? B1 N3 C21 C22 175.9(2) . . . . ? N2 C21 C22 C23 -15.3(4) . . . . ? N3 C21 C22 C23 179.1(2) . . . . ? N2 C21 C22 C39 157.8(2) . . . . ? N3 C21 C22 C39 -7.8(2) . . . . ? C24 O5 C23 C22 177.2(2) . . . . ? C24 O5 C23 C30 -3.3(3) . . . . ? C39 C22 C23 O5 179.52(19) . . . . ? C21 C22 C23 O5 -8.1(4) . . . . ? C39 C22 C23 C30 0.0(3) . . . . ? C21 C22 C23 C30 172.3(2) . . . . ? C23 O5 C24 C29 1.0(3) . . . . ? C23 O5 C24 C25 -177.8(2) . . . . ? C29 C24 C25 C26 -0.7(4) . . . . ? O5 C24 C25 C26 178.1(2) . . . . ? C24 C25 C26 C27 -0.1(4) . . . . ? C25 C26 C27 C28 0.4(4) . . . . ? C26 C27 C28 C29 0.2(4) . . . . ? C27 C28 C29 C24 -1.1(4) . . . . ? C27 C28 C29 O6 178.2(2) . . . . ? C25 C24 C29 C28 1.4(4) . . . . ? O5 C24 C29 C28 -177.5(2) . . . . ? C25 C24 C29 O6 -177.9(2) . . . . ? O5 C24 C29 O6 3.3(4) . . . . ? C30 O6 C29 C28 175.6(2) . . . . ? C30 O6 C29 C24 -5.1(3) . . . . ? C29 O6 C30 C23 2.9(3) . . . . ? C29 O6 C30 C31 -176.8(2) . . . . ? O5 C23 C30 O6 1.3(4) . . . . ? C22 C23 C30 O6 -179.2(2) . . . . ? O5 C23 C30 C31 -179.1(2) . . . . ? C22 C23 C30 C31 0.5(4) . . . . ? C32 O7 C31 C38 -4.3(3) . . . . ? C32 O7 C31 C30 176.5(2) . . . . ? O6 C30 C31 O7 -2.8(3) . . . . ? C23 C30 C31 O7 177.6(2) . . . . ? O6 C30 C31 C38 178.0(2) . . . . ? C23 C30 C31 C38 -1.7(4) . . . . ? C31 O7 C32 C33 -177.4(2) . . . . ? C31 O7 C32 C37 2.6(3) . . . . ? O7 C32 C33 C34 177.7(2) . . . . ? C37 C32 C33 C34 -2.3(4) . . . . ? C32 C33 C34 C35 2.4(4) . . . . ? C33 C34 C35 C36 -1.2(4) . . . . ? C34 C35 C36 C37 -0.2(4) . . . . ? C35 C36 C37 O8 -179.2(2) . . . . ? C35 C36 C37 C32 0.3(4) . . . . ? C38 O8 C37 C36 177.7(2) . . . . ? C38 O8 C37 C32 -1.9(3) . . . . ? C33 C32 C37 C36 0.9(4) . . . . ? O7 C32 C37 C36 -179.1(2) . . . . ? C33 C32 C37 O8 -179.5(2) . . . . ? O7 C32 C37 O8 0.4(4) . . . . ? C37 O8 C38 C31 0.2(3) . . . . ? C37 O8 C38 C39 -179.9(2) . . . . ? O7 C31 C38 O8 3.0(4) . . . . ? C30 C31 C38 O8 -177.8(2) . . . . ? O7 C31 C38 C39 -176.8(2) . . . . ? C30 C31 C38 C39 2.4(3) . . . . ? O8 C38 C39 C22 178.25(19) . . . . ? C31 C38 C39 C22 -1.9(3) . . . . ? O8 C38 C39 C40 6.2(4) . . . . ? C31 C38 C39 C40 -174.0(2) . . . . ? C23 C22 C39 C38 0.7(3) . . . . ? C21 C22 C39 C38 -173.4(2) . . . . ? C23 C22 C39 C40 174.6(2) . . . . ? C21 C22 C39 C40 0.5(2) . . . . ? C41 N4 C40 N3 -11.0(3) . . . . ? C41 N4 C40 C39 152.3(2) . . . . ? C21 N3 C40 N4 153.9(2) . . . . ? B1 N3 C40 N4 -8.8(3) . . . . ? C21 N3 C40 C39 -12.7(2) . . . . ? B1 N3 C40 C39 -175.5(2) . . . . ? C38 C39 C40 N4 14.4(4) . . . . ? C22 C39 C40 N4 -158.4(2) . . . . ? C38 C39 C40 N3 179.9(2) . . . . ? C22 C39 C40 N3 7.1(2) . . . . ? C40 N4 C41 N5 9.4(3) . . . . ? C40 N4 C41 C42 -152.7(2) . . . . ? C60 N5 C41 N4 -155.0(2) . . . . ? B1 N5 C41 N4 11.8(3) . . . . ? C60 N5 C41 C42 10.8(2) . . . . ? B1 N5 C41 C42 177.61(19) . . . . ? N4 C41 C42 C43 -14.7(4) . . . . ? N5 C41 C42 C43 -179.1(2) . . . . ? N4 C41 C42 C59 157.7(2) . . . . ? N5 C41 C42 C59 -6.7(2) . . . . ? C44 O9 C43 C50 -0.2(3) . . . . ? C44 O9 C43 C42 179.67(19) . . . . ? C59 C42 C43 O9 178.61(19) . . . . ? C41 C42 C43 O9 -9.8(4) . . . . ? C59 C42 C43 C50 -1.5(3) . . . . ? C41 C42 C43 C50 170.1(2) . . . . ? C43 O9 C44 C45 -179.4(2) . . . . ? C43 O9 C44 C49 -0.5(3) . . . . ? C49 C44 C45 C46 -0.2(4) . . . . ? O9 C44 C45 C46 178.7(2) . . . . ? C44 C45 C46 C47 0.3(4) . . . . ? C45 C46 C47 C48 -0.7(4) . . . . ? C46 C47 C48 C49 1.0(4) . . . . ? C47 C48 C49 C44 -0.9(4) . . . . ? C47 C48 C49 O10 -179.5(2) . . . . ? C45 C44 C49 C48 0.5(4) . . . . ? O9 C44 C49 C48 -178.3(2) . . . . ? C45 C44 C49 O10 179.0(2) . . . . ? O9 C44 C49 O10 0.2(3) . . . . ? C50 O10 C49 C48 179.5(2) . . . . ? C50 O10 C49 C44 0.9(3) . . . . ? O9 C43 C50 O10 1.4(3) . . . . ? C42 C43 C50 O10 -178.5(2) . . . . ? O9 C43 C50 C51 -179.2(2) . . . . ? C42 C43 C50 C51 0.9(3) . . . . ? C49 O10 C50 C43 -1.7(3) . . . . ? C49 O10 C50 C51 178.89(19) . . . . ? C52 O11 C51 C58 1.2(3) . . . . ? C52 O11 C51 C50 -179.07(19) . . . . ? C43 C50 C51 O11 180.0(2) . . . . ? O10 C50 C51 O11 -0.6(3) . . . . ? C43 C50 C51 C58 -0.3(3) . . . . ? O10 C50 C51 C58 179.1(2) . . . . ? C51 O11 C52 C53 180.0(2) . . . . ? C51 O11 C52 C57 0.0(3) . . . . ? C57 C52 C53 C54 1.3(4) . . . . ? O11 C52 C53 C54 -178.7(2) . . . . ? C52 C53 C54 C55 -0.1(4) . . . . ? C53 C54 C55 C56 -0.9(4) . . . . ? C54 C55 C56 C57 0.8(4) . . . . ? C55 C56 C57 O12 -178.1(2) . . . . ? C55 C56 C57 C52 0.4(4) . . . . ? C58 O12 C57 C56 -177.01(19) . . . . ? C58 O12 C57 C52 4.5(3) . . . . ? C53 C52 C57 C56 -1.4(4) . . . . ? O11 C52 C57 C56 178.6(2) . . . . ? C53 C52 C57 O12 177.0(2) . . . . ? O11 C52 C57 O12 -3.0(3) . . . . ? C57 O12 C58 C59 177.18(19) . . . . ? C57 O12 C58 C51 -3.3(3) . . . . ? O11 C51 C58 O12 0.5(3) . . . . ? C50 C51 C58 O12 -179.2(2) . . . . ? O11 C51 C58 C59 -180.0(2) . . . . ? C50 C51 C58 C59 0.3(3) . . . . ? O12 C58 C59 C42 178.58(19) . . . . ? C51 C58 C59 C42 -0.9(3) . . . . ? O12 C58 C59 C60 7.8(4) . . . . ? C51 C58 C59 C60 -171.7(2) . . . . ? C43 C42 C59 C58 1.5(3) . . . . ? C41 C42 C59 C58 -171.9(2) . . . . ? C43 C42 C59 C60 174.4(2) . . . . ? C41 C42 C59 C60 0.9(2) . . . . ? C1 N6 C60 N5 -10.6(3) . . . . ? C1 N6 C60 C59 153.3(2) . . . . ? C41 N5 C60 N6 157.0(2) . . . . ? B1 N5 C60 N6 -9.7(3) . . . . ? C41 N5 C60 C59 -10.3(2) . . . . ? B1 N5 C60 C59 -176.98(19) . . . . ? C58 C59 C60 N6 10.9(4) . . . . ? C42 C59 C60 N6 -160.8(2) . . . . ? C58 C59 C60 N5 177.0(2) . . . . ? C42 C59 C60 N5 5.3(2) . . . . ? B1 O13 C61 C66 -93.7(3) . . . . ? B1 O13 C61 C62 86.7(3) . . . . ? O13 C61 C62 C63 -178.3(2) . . . . ? C66 C61 C62 C63 2.1(4) . . . . ? O13 C61 C62 F1 1.6(4) . . . . ? C66 C61 C62 F1 -178.0(2) . . . . ? F1 C62 C63 F2 -0.9(4) . . . . ? C61 C62 C63 F2 179.0(2) . . . . ? F1 C62 C63 C64 179.1(2) . . . . ? C61 C62 C63 C64 -1.0(4) . . . . ? F2 C63 C64 F3 1.9(4) . . . . ? C62 C63 C64 F3 -178.1(3) . . . . ? F2 C63 C64 C65 178.8(2) . . . . ? C62 C63 C64 C65 -1.2(4) . . . . ? F3 C64 C65 F4 -0.8(4) . . . . ? C63 C64 C65 F4 -177.8(3) . . . . ? F3 C64 C65 C66 179.2(2) . . . . ? C63 C64 C65 C66 2.2(4) . . . . ? O13 C61 C66 F5 0.0(4) . . . . ? C62 C61 C66 F5 179.6(2) . . . . ? O13 C61 C66 C65 179.4(2) . . . . ? C62 C61 C66 C65 -1.0(4) . . . . ? F4 C65 C66 F5 -1.7(4) . . . . ? C64 C65 C66 F5 178.4(2) . . . . ? F4 C65 C66 C61 178.9(2) . . . . ? C64 C65 C66 C61 -1.1(4) . . . . ? C61 O13 B1 N3 -162.09(18) . . . . ? C61 O13 B1 N1 -41.9(3) . . . . ? C61 O13 B1 N5 77.9(3) . . . . ? C40 N3 B1 O13 -99.4(2) . . . . ? C21 N3 B1 O13 99.5(2) . . . . ? C40 N3 B1 N1 135.32(19) . . . . ? C21 N3 B1 N1 -25.7(3) . . . . ? C40 N3 B1 N5 25.7(3) . . . . ? C21 N3 B1 N5 -135.3(2) . . . . ? C1 N1 B1 O13 94.5(2) . . . . ? C20 N1 B1 O13 -96.0(2) . . . . ? C1 N1 B1 N3 -141.6(2) . . . . ? C20 N1 B1 N3 27.9(3) . . . . ? C1 N1 B1 N5 -30.9(3) . . . . ? C20 N1 B1 N5 138.6(2) . . . . ? C60 N5 B1 O13 -97.6(3) . . . . ? C41 N5 B1 O13 96.8(3) . . . . ? C60 N5 B1 N3 138.5(2) . . . . ? C41 N5 B1 N3 -27.1(3) . . . . ? C60 N5 B1 N1 27.8(3) . . . . ? C41 N5 B1 N1 -137.8(2) . . . . ? C4S O1S C1S C2S -17.1(3) . . . . ? O1S C1S C2S C3S -3.8(4) . . . . ? C1S C2S C3S C4S 21.6(3) . . . . ? C1S O1S C4S C3S 31.2(3) . . . . ? C2S C3S C4S O1S -32.6(3) . . . . ? C8S O2S C5S C6S 33.9(5) . . . . ? O2S C5S C6S C7S -37.4(5) . . . . ? C5S C6S C7S C8S 26.0(4) . . . . ? C5S O2S C8S C7S -17.0(5) . . . . ? C6S C7S C8S O2S -7.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 66.07 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.574 _refine_diff_density_min -0.421 _refine_diff_density_rms 0.051 _iucr_refine_instructions_details ; TITL cu_d1245_0m in P2(1)/n CELL 1.54178 12.0798 20.9681 23.1817 90.000 91.723 90.000 ZERR 4.00 0.0005 0.0008 0.0011 0.000 0.003 0.000 LATT 1 SYMM -x+1/2, y+1/2, -z+1/2 SFAC C H N O B F UNIT 296 160 24 60 4 20 TEMP -123.160 SIZE 0.040 0.120 0.130 ACTA L.S. 4 FMAP 2 PLAN 20 HTAB BOND $H CONF WGHT 0.0825 0.0000 FVAR 0.13361 F1 6 1.026639 0.819551 0.110329 11.00000 0.05547 0.02996 = 0.12279 -0.01461 0.00822 -0.00459 F2 6 1.142669 0.847085 0.016221 11.00000 0.06403 0.05702 = 0.12712 0.04653 -0.00027 -0.01923 F3 6 1.220143 0.751349 -0.050412 11.00000 0.04490 0.13015 = 0.06213 0.03872 0.01286 -0.01155 F4 6 1.178045 0.628428 -0.021966 11.00000 0.05097 0.08916 = 0.07033 -0.01923 0.02143 0.01430 F5 6 1.055597 0.601308 0.069881 11.00000 0.05725 0.02646 = 0.08765 0.00477 0.02520 0.00533 O1 4 0.746336 0.791115 -0.087422 11.00000 0.06152 0.04289 = 0.03009 -0.00378 0.00741 -0.00198 O2 4 0.669048 0.919286 -0.099511 11.00000 0.05664 0.04321 = 0.03381 0.00310 0.00280 -0.00107 O3 4 0.643489 0.991671 -0.008165 11.00000 0.05985 0.03347 = 0.04030 0.00493 0.00265 0.00384 O4 4 0.688857 0.943757 0.105293 11.00000 0.04839 0.02738 = 0.03589 -0.00093 0.00401 0.00157 O5 4 0.642497 0.851596 0.286078 11.00000 0.04260 0.02623 = 0.03911 -0.00170 0.01647 0.00306 O6 4 0.519326 0.791535 0.374301 11.00000 0.05225 0.02830 = 0.04349 0.00214 0.02192 0.00919 O7 4 0.520047 0.667909 0.386701 11.00000 0.05089 0.02943 = 0.04224 0.00443 0.01775 0.00441 O8 4 0.628664 0.587289 0.306711 11.00000 0.04595 0.02407 = 0.03769 0.00012 0.00636 0.00235 O9 4 0.664933 0.459094 0.149460 11.00000 0.04037 0.03100 = 0.03725 -0.00189 0.00302 -0.00319 O10 4 0.572636 0.399696 0.048142 11.00000 0.04497 0.03396 = 0.04130 -0.00588 0.00424 -0.01046 O11 4 0.591704 0.452062 -0.053427 11.00000 0.04648 0.04086 = 0.03569 -0.00708 0.00165 -0.00832 O12 4 0.700539 0.572017 -0.066329 11.00000 0.03991 0.04020 = 0.03361 -0.00602 0.00665 -0.00439 O13 4 0.974662 0.697891 0.138523 11.00000 0.02427 0.04117 = 0.04050 -0.00118 0.00493 -0.00084 N1 3 0.811309 0.751081 0.091689 11.00000 0.02662 0.02906 = 0.03218 -0.00442 0.00742 -0.00114 N2 3 0.749378 0.814936 0.168973 11.00000 0.02849 0.02788 = 0.03137 -0.00374 0.00412 -0.00223 N3 3 0.794730 0.705003 0.183941 11.00000 0.02541 0.02810 = 0.03065 -0.00373 0.00271 0.00215 N4 3 0.742473 0.595607 0.188843 11.00000 0.02862 0.02883 = 0.03392 -0.00336 0.00190 0.00410 N5 3 0.807489 0.639483 0.101434 11.00000 0.02732 0.02870 = 0.03108 -0.00469 0.00557 0.00166 N6 3 0.783740 0.686455 0.008496 11.00000 0.02963 0.03236 = 0.03386 -0.00393 0.00878 -0.00117 C1 1 0.791708 0.744103 0.034083 11.00000 0.02660 0.03346 = 0.03341 -0.00371 0.00896 -0.00206 C2 1 0.756140 0.806486 0.013663 11.00000 0.02904 0.03174 = 0.03315 -0.00384 0.00827 -0.00554 C3 1 0.729629 0.829565 -0.040870 11.00000 0.03566 0.03376 = 0.03347 -0.00328 0.00766 -0.00748 C4 1 0.732397 0.819909 -0.141038 11.00000 0.04160 0.05028 = 0.03195 0.00081 0.00922 -0.01021 C5 1 0.755752 0.784526 -0.188596 11.00000 0.05668 0.06305 = 0.03902 -0.00601 0.01335 -0.00381 AFIX 43 H5A 2 0.784568 0.742572 -0.184385 11.00000 -1.20000 AFIX 0 C6 1 0.737180 0.810172 -0.242744 11.00000 0.09164 0.08059 = 0.03577 -0.00702 0.01678 0.00718 AFIX 43 H6A 2 0.752292 0.785640 -0.276050 11.00000 -1.20000 AFIX 0 C7 1 0.697097 0.870780 -0.248623 11.00000 0.10708 0.09908 = 0.03637 0.01020 0.00996 0.00868 AFIX 43 H7A 2 0.684108 0.888087 -0.286090 11.00000 -1.20000 AFIX 0 C8 1 0.675055 0.907500 -0.200194 11.00000 0.07723 0.06817 = 0.04053 0.00867 0.00783 0.00047 AFIX 43 H8A 2 0.648014 0.949844 -0.204371 11.00000 -1.20000 AFIX 0 C9 1 0.692945 0.881649 -0.146583 11.00000 0.04416 0.05382 = 0.03280 0.00227 0.00647 -0.01075 C10 1 0.691591 0.891924 -0.046360 11.00000 0.03511 0.04020 = 0.03267 0.00581 0.00184 -0.00742 C11 1 0.678920 0.930129 0.001852 11.00000 0.03432 0.02956 = 0.04059 0.00262 0.00253 -0.00279 C12 1 0.634962 1.029899 0.040482 11.00000 0.03753 0.03062 = 0.04267 -0.00166 0.00715 -0.00219 C13 1 0.604186 1.092770 0.032689 11.00000 0.04652 0.03914 = 0.05184 0.00854 0.00411 -0.00138 AFIX 43 H13A 2 0.590610 1.109079 -0.005098 11.00000 -1.20000 AFIX 0 C14 1 0.593234 1.131848 0.080153 11.00000 0.04702 0.03246 = 0.06275 -0.00218 0.00739 0.00143 AFIX 43 H14A 2 0.572349 1.175189 0.074902 11.00000 -1.20000 AFIX 0 C15 1 0.612283 1.108523 0.134701 11.00000 0.04113 0.03787 = 0.05384 -0.00685 0.00606 -0.00217 AFIX 43 H15A 2 0.603690 1.135594 0.167121 11.00000 -1.20000 AFIX 0 C16 1 0.644167 1.045349 0.142853 11.00000 0.03455 0.03443 = 0.04514 -0.00450 0.00255 -0.00225 AFIX 43 H16A 2 0.657770 1.029152 0.180676 11.00000 -1.20000 AFIX 0 C17 1 0.655772 1.006635 0.095629 11.00000 0.02974 0.02896 = 0.04577 0.00087 0.00491 -0.00205 C18 1 0.702835 0.907582 0.056957 11.00000 0.02977 0.03225 = 0.03232 -0.00264 0.00621 -0.00557 C19 1 0.743133 0.845708 0.063179 11.00000 0.02787 0.02892 = 0.03421 0.00036 0.00715 -0.00519 C20 1 0.772485 0.807454 0.113591 11.00000 0.02531 0.02636 = 0.03520 -0.00396 0.00411 -0.00336 C21 1 0.753132 0.762406 0.202219 11.00000 0.02661 0.02499 = 0.03363 -0.00502 0.00077 -0.00063 C22 1 0.694879 0.748551 0.254499 11.00000 0.02606 0.02846 = 0.03152 -0.00279 0.00064 0.00144 C23 1 0.638217 0.786553 0.292156 11.00000 0.03354 0.02453 = 0.03000 -0.00158 0.00311 0.00242 C24 1 0.579274 0.886294 0.324035 11.00000 0.03122 0.02974 = 0.03579 -0.00663 0.00664 0.00296 C25 1 0.578136 0.951749 0.318147 11.00000 0.03486 0.02997 = 0.04741 -0.00369 0.00956 -0.00403 AFIX 43 H25A 2 0.621192 0.971871 0.289749 11.00000 -1.20000 AFIX 0 C26 1 0.513581 0.987666 0.354079 11.00000 0.03986 0.02611 = 0.06608 -0.01019 0.01679 -0.00300 AFIX 43 H26A 2 0.512324 1.032790 0.350434 11.00000 -1.20000 AFIX 0 C27 1 0.451207 0.958513 0.395043 11.00000 0.04022 0.03418 = 0.06507 -0.01551 0.02065 -0.00196 AFIX 43 H27A 2 0.406743 0.983629 0.419385 11.00000 -1.20000 AFIX 0 C28 1 0.452569 0.892969 0.401153 11.00000 0.03626 0.03672 = 0.04910 -0.00344 0.01622 -0.00022 AFIX 43 H28A 2 0.409165 0.872867 0.429416 11.00000 -1.20000 AFIX 0 C29 1 0.517757 0.857161 0.365684 11.00000 0.03595 0.02747 = 0.03941 -0.00213 0.00660 0.00119 C30 1 0.579171 0.757721 0.335396 11.00000 0.03266 0.03187 = 0.03255 -0.00207 0.00660 0.00525 C31 1 0.577294 0.691394 0.341295 11.00000 0.03245 0.03142 = 0.03123 0.00291 0.00551 0.00269 C32 1 0.513988 0.602012 0.389755 11.00000 0.03349 0.02873 = 0.03932 0.00354 -0.00259 0.00252 C33 1 0.453563 0.575874 0.433194 11.00000 0.03636 0.03703 = 0.04457 0.00795 0.00625 0.00181 AFIX 43 H33A 2 0.419910 0.602668 0.460680 11.00000 -1.20000 AFIX 0 C34 1 0.442079 0.510530 0.436640 11.00000 0.05158 0.04341 = 0.05681 0.01095 0.00874 -0.00463 AFIX 43 H34A 2 0.398099 0.492271 0.465648 11.00000 -1.20000 AFIX 0 C35 1 0.494509 0.471751 0.397931 11.00000 0.06533 0.03254 = 0.06247 0.01077 0.00514 -0.00836 AFIX 43 H35A 2 0.487635 0.426741 0.400834 11.00000 -1.20000 AFIX 0 C36 1 0.556835 0.497890 0.355047 11.00000 0.05186 0.03064 = 0.04727 -0.00278 -0.00045 -0.00134 AFIX 43 H36A 2 0.592985 0.470976 0.328553 11.00000 -1.20000 AFIX 0 C37 1 0.566499 0.563002 0.350750 11.00000 0.03476 0.03447 = 0.03047 0.00613 -0.00173 -0.00168 C38 1 0.631832 0.652663 0.303352 11.00000 0.03301 0.02574 = 0.02969 -0.00033 -0.00077 0.00193 C39 1 0.692689 0.680645 0.260007 11.00000 0.02864 0.02807 = 0.02838 -0.00111 -0.00047 0.00206 C40 1 0.749629 0.654141 0.211946 11.00000 0.02519 0.02773 = 0.03200 0.00035 -0.00019 0.00303 C41 1 0.764299 0.590521 0.132703 11.00000 0.02341 0.03037 = 0.03584 -0.00144 0.00241 0.00537 C42 1 0.724599 0.544413 0.090207 11.00000 0.02654 0.02850 = 0.03309 -0.00539 0.00519 0.00383 C43 1 0.671860 0.485776 0.095825 11.00000 0.02788 0.02901 = 0.03590 -0.00299 0.00624 0.00382 C44 1 0.610360 0.400499 0.151502 11.00000 0.02827 0.02763 = 0.04865 -0.00200 0.00594 0.00287 C45 1 0.600431 0.372197 0.204348 11.00000 0.03600 0.03718 = 0.04491 0.00049 0.00188 0.00532 AFIX 43 H45A 2 0.631489 0.391960 0.237973 11.00000 -1.20000 AFIX 0 C46 1 0.544854 0.314562 0.208591 11.00000 0.03774 0.04209 = 0.05610 0.01116 0.00265 0.00075 AFIX 43 H46A 2 0.537437 0.294793 0.245145 11.00000 -1.20000 AFIX 0 C47 1 0.500265 0.285992 0.159346 11.00000 0.04183 0.03624 = 0.06343 0.00379 0.00522 -0.00615 AFIX 43 H47A 2 0.462862 0.246302 0.162085 11.00000 -1.20000 AFIX 0 C48 1 0.509952 0.314996 0.106187 11.00000 0.03923 0.03795 = 0.05658 -0.00632 0.00423 -0.00632 AFIX 43 H48A 2 0.478302 0.295707 0.072476 11.00000 -1.20000 AFIX 0 C49 1 0.565764 0.372018 0.102416 11.00000 0.03281 0.03242 = 0.04289 -0.00128 0.00560 0.00302 C50 1 0.628514 0.457010 0.046763 11.00000 0.03065 0.02845 = 0.03948 -0.00557 0.00532 0.00015 C51 1 0.638084 0.484997 -0.007305 11.00000 0.03014 0.03322 = 0.03632 -0.01084 0.00425 0.00025 C52 1 0.603696 0.480423 -0.107135 11.00000 0.03436 0.04017 = 0.03589 -0.00553 0.00435 0.00452 C53 1 0.559004 0.449615 -0.154710 11.00000 0.04640 0.04477 = 0.04618 -0.00861 -0.00773 0.00449 AFIX 43 H53A 2 0.519992 0.410637 -0.150472 11.00000 -1.20000 AFIX 0 C54 1 0.571404 0.475885 -0.208629 11.00000 0.05803 0.05605 = 0.04037 -0.01188 -0.00895 0.00647 AFIX 43 H54A 2 0.540785 0.454731 -0.241650 11.00000 -1.20000 AFIX 0 C55 1 0.627567 0.532356 -0.215217 11.00000 0.05232 0.05774 = 0.03770 -0.00298 -0.00082 0.00878 AFIX 43 H55A 2 0.636530 0.549682 -0.252653 11.00000 -1.20000 AFIX 0 C56 1 0.671019 0.563911 -0.167201 11.00000 0.03809 0.04615 = 0.03882 -0.00457 0.00333 0.00528 AFIX 43 H56A 2 0.709072 0.603200 -0.171469 11.00000 -1.20000 AFIX 0 C57 1 0.658727 0.538038 -0.113434 11.00000 0.02949 0.04050 = 0.03330 -0.00780 0.00380 0.00577 C58 1 0.691109 0.542992 -0.013804 11.00000 0.02801 0.03342 = 0.03156 -0.00340 0.00831 0.00383 C59 1 0.735246 0.572675 0.034857 11.00000 0.02707 0.03005 = 0.03517 -0.00753 0.00798 0.00364 C60 1 0.783288 0.635788 0.043695 11.00000 0.02558 0.03377 = 0.03454 -0.00543 0.00897 0.00306 C61 1 1.036174 0.709933 0.091924 11.00000 0.02298 0.02813 = 0.04651 0.00125 0.00399 -0.00034 C62 1 1.062290 0.771432 0.076491 11.00000 0.03028 0.03284 = 0.07296 0.00651 0.00318 -0.00240 C63 1 1.120737 0.786373 0.029918 11.00000 0.03648 0.04116 = 0.07948 0.02161 0.00062 -0.00191 C64 1 1.158905 0.738681 -0.004485 11.00000 0.03115 0.07930 = 0.04906 0.03045 0.00448 -0.01051 C65 1 1.138653 0.675273 0.009728 11.00000 0.03014 0.05853 = 0.04931 -0.00515 0.00822 0.00974 C66 1 1.076476 0.662075 0.057738 11.00000 0.02964 0.02685 = 0.05198 0.00589 0.00896 0.00270 B1 5 0.853704 0.698416 0.129371 11.00000 0.02530 0.02886 = 0.03621 -0.00222 0.00377 0.00088 O1S 4 0.557675 0.696094 0.122993 11.00000 0.04260 0.05949 = 0.08331 -0.00752 -0.01652 0.00946 C1S 1 0.529606 0.704114 0.063567 11.00000 0.03858 0.08471 = 0.07874 0.00639 0.00458 -0.00149 AFIX 23 H1SA 2 0.543634 0.664049 0.042405 11.00000 -1.20000 H1SB 2 0.575616 0.738218 0.047028 11.00000 -1.20000 AFIX 0 C2S 1 0.410342 0.721442 0.057641 11.00000 0.04425 0.06805 = 0.05763 -0.00361 0.00134 0.01311 AFIX 23 H2SA 2 0.369928 0.690851 0.032208 11.00000 -1.20000 H2SB 2 0.401271 0.764888 0.041461 11.00000 -1.20000 AFIX 0 C3S 1 0.368741 0.718427 0.118211 11.00000 0.04571 0.08880 = 0.05617 0.00092 -0.00061 0.01894 AFIX 23 H3SA 2 0.331947 0.677161 0.125596 11.00000 -1.20000 H3SB 2 0.316272 0.753571 0.125540 11.00000 -1.20000 AFIX 0 C4S 1 0.473543 0.725450 0.154712 11.00000 0.06064 0.07141 = 0.06734 -0.01401 -0.01503 0.01964 AFIX 23 H4SA 2 0.490774 0.771050 0.161469 11.00000 -1.20000 H4SB 2 0.465801 0.704125 0.192478 11.00000 -1.20000 AFIX 0 O2S 4 0.283892 0.867556 0.186296 11.00000 0.08955 0.11651 = 0.12890 -0.02786 0.02165 -0.02308 C5S 1 0.293942 0.904665 0.136432 11.00000 0.08377 0.12427 = 0.16606 0.07284 -0.06019 -0.02989 AFIX 23 H5SA 2 0.264909 0.948221 0.142540 11.00000 -1.20000 H5SB 2 0.252909 0.885046 0.103353 11.00000 -1.20000 AFIX 0 C6S 1 0.416651 0.906436 0.125764 11.00000 0.06673 0.15008 = 0.07033 0.05081 -0.01837 -0.01430 AFIX 23 H6SA 2 0.441118 0.867397 0.105788 11.00000 -1.20000 H6SB 2 0.436652 0.944277 0.102758 11.00000 -1.20000 AFIX 0 C7S 1 0.464330 0.910100 0.184850 11.00000 0.05762 0.06830 = 0.09083 0.02094 0.00575 0.00031 AFIX 23 H7SA 2 0.477384 0.954962 0.196499 11.00000 -1.20000 H7SB 2 0.535153 0.886430 0.188117 11.00000 -1.20000 AFIX 0 C8S 1 0.377934 0.879721 0.221110 11.00000 0.05657 0.08347 = 0.08090 -0.01649 0.01109 -0.01127 AFIX 23 H8SA 2 0.406708 0.839377 0.237919 11.00000 -1.20000 H8SB 2 0.358878 0.908601 0.253106 11.00000 -1.20000 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM cu_d1245_0m in P2(1)/n REM R1 = 0.0487 for 6944 Fo > 4sig(Fo) and 0.0696 for all 10022 data REM 910 parameters refined using 0 restraints END REM Highest difference peak 0.574, deepest hole -0.421, 1-sigma level 0.051 Q1 1 0.3457 0.8618 0.1141 11.00000 0.05 0.57 Q2 1 1.2227 0.6967 -0.0642 11.00000 0.05 0.53 Q3 1 1.1610 0.8152 -0.0259 11.00000 0.05 0.48 Q4 1 1.0363 0.8262 0.0634 11.00000 0.05 0.41 Q5 1 1.1583 0.5795 -0.0095 11.00000 0.05 0.34 Q6 1 0.2844 0.9016 0.1490 11.00000 0.05 0.31 Q7 1 0.4907 0.2954 0.2631 11.00000 0.05 0.30 Q8 1 0.6744 0.9016 -0.3144 11.00000 0.05 0.23 Q9 1 0.3618 0.4655 0.4768 11.00000 0.05 0.23 Q10 1 0.6710 0.6631 0.2847 11.00000 0.05 0.20 Q11 1 0.2137 0.8222 0.1802 11.00000 0.05 0.20 Q12 1 0.4549 0.9885 0.4762 11.00000 0.05 0.19 Q13 1 0.4820 1.0607 0.3193 11.00000 0.05 0.19 Q14 1 0.4173 0.9199 0.1320 11.00000 0.05 0.19 Q15 1 0.5549 1.1390 0.1960 11.00000 0.05 0.19 Q16 1 0.3949 0.8243 0.1971 11.00000 0.05 0.19 Q17 1 0.5447 1.1985 0.0778 11.00000 0.05 0.19 Q18 1 0.6805 0.5658 -0.2931 11.00000 0.05 0.19 Q19 1 1.1007 0.7569 -0.0083 11.00000 0.05 0.18 Q20 1 0.2032 0.8407 0.1760 11.00000 0.05 0.18 ; _database_code_depnum_ccdc_archive 'CCDC 910746' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_d12296 #TrackingRef 'web_deposit_cif_file_1_ProfDrTimothyPBender_1352857284.BsubPc compound 4a_d12296.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; Boron subphthalocyanine compound 4a ; _chemical_melting_point ? _chemical_formula_moiety 'C58 H48 B F5 N6 O5, 2(C H Cl3)' _chemical_formula_sum 'C60 H50 B Cl6 F5 N6 O5' _chemical_formula_weight 1253.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.5648(4) _cell_length_b 17.6316(8) _cell_length_c 34.0701(14) _cell_angle_alpha 90.00 _cell_angle_beta 96.526(2) _cell_angle_gamma 90.00 _cell_volume 5708.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 9883 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 65.27 _exptl_crystal_description needle _exptl_crystal_colour blue _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.459 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2576 _exptl_absorpt_coefficient_mu 3.360 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6290 _exptl_absorpt_correction_T_max 0.7536 _exptl_absorpt_process_details '(Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Bruker ImuS' _diffrn_radiation_monochromator 'multi-layer optics' _diffrn_measurement_device_type 'Bruker Kappa APEX-DUO CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 36647 _diffrn_reflns_av_R_equivalents 0.0504 _diffrn_reflns_av_sigmaI/netI 0.0467 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 65.56 _reflns_number_total 9635 _reflns_number_gt 6984 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 (Bruker, 2007)' _computing_cell_refinement APEX2 _computing_data_reduction 'SAINT (Bruker, 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2009)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^)+(0.1263P)^2^+12.7487P] 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 9635 _refine_ls_number_parameters 774 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1043 _refine_ls_R_factor_gt 0.0772 _refine_ls_wR_factor_ref 0.2370 _refine_ls_wR_factor_gt 0.2137 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.045 _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 F1 F 0.3691(3) 0.36145(17) 0.17724(11) 0.0557(8) Uani 1 1 d . . . F2 F 0.2316(4) 0.3311(2) 0.23993(14) 0.0880(14) Uani 1 1 d . . . F3 F 0.1498(4) 0.4455(3) 0.28522(10) 0.0928(15) Uani 1 1 d . . . F4 F 0.2187(4) 0.5910(3) 0.26906(11) 0.0853(13) Uani 1 1 d . . . F5 F 0.3617(3) 0.62177(17) 0.20697(10) 0.0569(8) Uani 1 1 d . . . O1 O 0.6714(3) 0.36311(15) 0.01909(7) 0.0233(6) Uani 1 1 d . . . O2 O 0.6703(3) 0.44932(15) -0.05134(7) 0.0207(6) Uani 1 1 d . . . O3 O 0.6767(3) 0.60141(16) -0.04765(7) 0.0229(6) Uani 1 1 d . . . O4 O 0.6846(3) 0.67646(15) 0.02656(7) 0.0236(6) Uani 1 1 d . . . O5 O 0.4278(3) 0.50800(18) 0.15726(8) 0.0290(7) Uani 1 1 d . . . N1 N 0.6760(3) 0.6407(2) 0.11824(9) 0.0227(7) Uani 1 1 d . . . N2 N 0.6622(4) 0.5696(2) 0.17700(9) 0.0254(8) Uani 1 1 d . . . N3 N 0.7664(4) 0.4950(2) 0.23052(10) 0.0322(9) Uani 1 1 d . . . N4 N 0.6533(4) 0.4359(2) 0.17270(9) 0.0250(8) Uani 1 1 d . . . N5 N 0.6581(4) 0.3798(2) 0.10965(10) 0.0256(8) Uani 1 1 d . . . N6 N 0.6126(3) 0.51072(19) 0.11502(9) 0.0220(7) Uani 1 1 d . . . C1 C 0.6948(4) 0.6342(2) 0.15757(12) 0.0265(9) Uani 1 1 d . . . C2 C 0.7781(5) 0.6798(3) 0.18699(12) 0.0298(10) Uani 1 1 d . . . C3 C 0.8350(5) 0.7523(3) 0.18508(14) 0.0350(11) Uani 1 1 d . . . H3A H 0.8166 0.7827 0.1621 0.042 Uiso 1 1 calc R . . C4 C 0.9197(5) 0.7782(3) 0.21810(14) 0.0420(12) Uani 1 1 d . . . H4A H 0.9583 0.8278 0.2178 0.050 Uiso 1 1 calc R . . C5 C 0.9500(5) 0.7330(3) 0.25202(14) 0.0430(13) Uani 1 1 d . . . H5A H 1.0094 0.7523 0.2740 0.052 Uiso 1 1 calc R . . C6 C 0.8947(5) 0.6611(3) 0.25379(13) 0.0380(12) Uani 1 1 d . . . H6A H 0.9163 0.6302 0.2765 0.046 Uiso 1 1 calc R . . C7 C 0.8059(5) 0.6349(3) 0.22119(13) 0.0329(10) Uani 1 1 d . . . C8 C 0.7384(5) 0.5623(3) 0.21347(12) 0.0306(10) Uani 1 1 d . . . C9 C 0.7314(5) 0.4326(3) 0.20901(12) 0.0305(10) Uani 1 1 d . . . C10 C 0.7912(5) 0.3569(3) 0.21170(12) 0.0309(10) Uani 1 1 d . . . C11 C 0.8789(5) 0.3210(3) 0.24179(13) 0.0371(11) Uani 1 1 d . . . H11A H 0.9027 0.3448 0.2667 0.044 Uiso 1 1 calc R . . C12 C 0.9291(5) 0.2507(3) 0.23419(14) 0.0405(12) Uani 1 1 d . . . H12A H 0.9888 0.2254 0.2542 0.049 Uiso 1 1 calc R . . C13 C 0.8949(5) 0.2148(3) 0.19755(14) 0.0401(12) Uani 1 1 d . . . H13A H 0.9298 0.1653 0.1934 0.048 Uiso 1 1 calc R . . C14 C 0.8108(5) 0.2508(3) 0.16729(13) 0.0341(11) Uani 1 1 d . . . H14A H 0.7905 0.2275 0.1422 0.041 Uiso 1 1 calc R . . C15 C 0.7577(4) 0.3211(3) 0.17464(12) 0.0293(10) Uani 1 1 d . . . C16 C 0.6777(4) 0.3759(2) 0.14904(12) 0.0264(9) Uani 1 1 d . . . C17 C 0.6342(4) 0.4476(2) 0.09330(11) 0.0219(9) Uani 1 1 d . . . C18 C 0.6523(4) 0.4767(2) 0.05437(11) 0.0205(8) Uani 1 1 d . . . C19 C 0.6568(4) 0.5574(2) 0.05654(11) 0.0185(8) Uani 1 1 d . . . C20 C 0.6431(4) 0.5780(2) 0.09725(11) 0.0230(9) Uani 1 1 d . . . C21 C 0.6676(4) 0.4400(2) 0.01937(11) 0.0182(8) Uani 1 1 d . . . C22 C 0.6994(4) 0.3289(2) -0.01600(11) 0.0218(9) Uani 1 1 d . . . C23 C 0.7352(4) 0.2530(2) -0.01563(12) 0.0228(9) Uani 1 1 d . . . C24 C 0.7427(4) 0.2187(2) -0.05205(12) 0.0246(9) Uani 1 1 d . . . H24A H 0.7643 0.1661 -0.0527 0.030 Uiso 1 1 calc R . . C25 C 0.7201(4) 0.2579(2) -0.08767(12) 0.0250(9) Uani 1 1 d . . . C26 C 0.6970(4) 0.3356(2) -0.08663(11) 0.0229(9) Uani 1 1 d . . . H26A H 0.6873 0.3643 -0.1104 0.027 Uiso 1 1 calc R . . C27 C 0.6883(4) 0.3705(2) -0.05104(11) 0.0203(8) Uani 1 1 d . . . C28 C 0.6733(4) 0.4833(2) -0.01463(10) 0.0180(8) Uani 1 1 d . . . C29 C 0.6763(4) 0.5621(2) -0.01265(11) 0.0190(8) Uani 1 1 d . . . C30 C 0.6936(4) 0.6800(2) -0.04388(11) 0.0206(8) Uani 1 1 d . . . C31 C 0.6996(4) 0.7198(2) -0.07824(11) 0.0237(9) Uani 1 1 d . . . H31A H 0.6899 0.6939 -0.1029 0.028 Uiso 1 1 calc R . . C32 C 0.7197(4) 0.7977(2) -0.07706(12) 0.0251(9) Uani 1 1 d . . . C33 C 0.7369(4) 0.8325(2) -0.04021(12) 0.0245(9) Uani 1 1 d . . . H33A H 0.7548 0.8855 -0.0391 0.029 Uiso 1 1 calc R . . C34 C 0.7293(4) 0.7938(2) -0.00483(11) 0.0229(9) Uani 1 1 d . . . C35 C 0.7036(4) 0.7164(2) -0.00761(11) 0.0208(8) Uani 1 1 d . . . C36 C 0.6747(4) 0.5997(2) 0.02345(11) 0.0199(8) Uani 1 1 d . . . C37 C 0.7704(4) 0.2089(2) 0.02357(12) 0.0271(9) Uani 1 1 d . . . C38 C 0.6435(5) 0.2049(3) 0.04717(13) 0.0320(10) Uani 1 1 d . . . H38A H 0.5636 0.1821 0.0308 0.048 Uiso 1 1 calc R . . H38B H 0.6184 0.2561 0.0550 0.048 Uiso 1 1 calc R . . H38C H 0.6674 0.1738 0.0708 0.048 Uiso 1 1 calc R . . C39 C 0.8936(5) 0.2486(3) 0.04826(13) 0.0338(10) Uani 1 1 d . . . H39A H 0.9205 0.2195 0.0724 0.051 Uiso 1 1 calc R . . H39B H 0.8650 0.2998 0.0552 0.051 Uiso 1 1 calc R . . H39C H 0.9740 0.2519 0.0329 0.051 Uiso 1 1 calc R . . C40 C 0.8164(6) 0.1276(3) 0.01607(14) 0.0394(12) Uani 1 1 d . . . H40A H 0.7388 0.1003 0.0009 0.059 Uiso 1 1 calc R . . H40B H 0.8418 0.1019 0.0414 0.059 Uiso 1 1 calc R . . H40C H 0.8979 0.1285 0.0011 0.059 Uiso 1 1 calc R . . C41 C 0.7196(5) 0.2165(2) -0.12790(12) 0.0290(10) Uani 1 1 d . . . C42 C 0.5755(5) 0.2275(3) -0.15159(13) 0.0360(11) Uani 1 1 d . . . H42A H 0.5589 0.2816 -0.1566 0.054 Uiso 1 1 calc R . . H42B H 0.5023 0.2073 -0.1365 0.054 Uiso 1 1 calc R . . H42C H 0.5728 0.2004 -0.1768 0.054 Uiso 1 1 calc R . . C43 C 0.8341(5) 0.2495(3) -0.15016(14) 0.0413(12) Uani 1 1 d . . . H43A H 0.8183 0.3041 -0.1539 0.062 Uiso 1 1 calc R . . H43B H 0.8317 0.2247 -0.1760 0.062 Uiso 1 1 calc R . . H43C H 0.9260 0.2411 -0.1350 0.062 Uiso 1 1 calc R . . C44 C 0.7468(6) 0.1313(3) -0.12228(15) 0.0481(14) Uani 1 1 d . . . H44A H 0.7478 0.1071 -0.1481 0.072 Uiso 1 1 calc R . . H44B H 0.6720 0.1088 -0.1086 0.072 Uiso 1 1 calc R . . H44C H 0.8378 0.1235 -0.1065 0.072 Uiso 1 1 calc R . . C45 C 0.7178(5) 0.8435(3) -0.11582(13) 0.0326(10) Uani 1 1 d . . . C46 C 0.5705(6) 0.8361(4) -0.13839(17) 0.068(2) Uani 1 1 d . . . H46A H 0.5699 0.8589 -0.1646 0.101 Uiso 1 1 calc R . . H46B H 0.5022 0.8623 -0.1238 0.101 Uiso 1 1 calc R . . H46C H 0.5452 0.7823 -0.1411 0.101 Uiso 1 1 calc R . . C47 C 0.7566(12) 0.9246(4) -0.10883(18) 0.101(3) Uani 1 1 d . . . H47A H 0.8475 0.9277 -0.0924 0.151 Uiso 1 1 calc R . . H47B H 0.6844 0.9497 -0.0953 0.151 Uiso 1 1 calc R . . H47C H 0.7636 0.9497 -0.1342 0.151 Uiso 1 1 calc R . . C48 C 0.8209(6) 0.8090(4) -0.14118(16) 0.0561(16) Uani 1 1 d . . . H48A H 0.9162 0.8122 -0.1273 0.084 Uiso 1 1 calc R . . H48B H 0.8169 0.8368 -0.1662 0.084 Uiso 1 1 calc R . . H48C H 0.7964 0.7557 -0.1465 0.084 Uiso 1 1 calc R . . C49 C 0.7470(4) 0.8353(3) 0.03547(12) 0.0264(9) Uani 1 1 d . . . C50 C 0.7813(6) 0.9192(3) 0.03097(14) 0.0380(11) Uani 1 1 d . . . H50A H 0.7044 0.9440 0.0143 0.057 Uiso 1 1 calc R . . H50B H 0.8688 0.9242 0.0187 0.057 Uiso 1 1 calc R . . H50C H 0.7928 0.9434 0.0571 0.057 Uiso 1 1 calc R . . C51 C 0.8676(5) 0.7996(3) 0.06295(13) 0.0334(10) Uani 1 1 d . . . H51A H 0.8872 0.8309 0.0867 0.050 Uiso 1 1 calc R . . H51B H 0.9521 0.7967 0.0492 0.050 Uiso 1 1 calc R . . H51C H 0.8405 0.7485 0.0705 0.050 Uiso 1 1 calc R . . C52 C 0.6096(5) 0.8310(3) 0.05494(13) 0.0313(10) Uani 1 1 d . . . H52A H 0.5331 0.8545 0.0375 0.047 Uiso 1 1 calc R . . H52B H 0.6218 0.8579 0.0803 0.047 Uiso 1 1 calc R . . H52C H 0.5865 0.7778 0.0594 0.047 Uiso 1 1 calc R . . C53 C 0.3692(4) 0.4927(3) 0.19028(12) 0.0255(9) Uani 1 1 d . . . C54 C 0.3349(5) 0.4190(3) 0.19988(14) 0.0359(11) Uani 1 1 d . . . C55 C 0.2628(5) 0.4025(3) 0.23178(17) 0.0478(14) Uani 1 1 d . . . C56 C 0.2214(6) 0.4600(4) 0.25447(16) 0.0551(17) Uani 1 1 d . . . C57 C 0.2559(6) 0.5345(4) 0.24645(14) 0.0511(15) Uani 1 1 d . . . C58 C 0.3295(5) 0.5497(3) 0.21462(14) 0.0358(11) Uani 1 1 d . . . B1 B 0.5813(5) 0.5062(3) 0.15648(14) 0.0251(10) Uani 1 1 d . . . C1S C 1.0804(5) 0.4825(3) 0.10387(16) 0.0421(12) Uani 1 1 d . A 1 H1S H 1.1850 0.4877 0.1053 0.051 Uiso 1 1 calc R A 1 Cl1 Cl 1.00915(14) 0.48226(12) 0.05404(5) 0.0704(5) Uani 1 1 d . A 1 Cl2 Cl 1.04072(15) 0.39599(8) 0.12594(4) 0.0561(4) Uani 1 1 d . A 1 Cl3 Cl 1.01428(17) 0.55746(9) 0.12959(7) 0.0779(6) Uani 1 1 d . A 1 C2S C 0.7847(8) 0.0084(4) 0.1708(2) 0.0638(17) Uani 0.871(3) 1 d PD B 1 H2S H 0.7495 0.0437 0.1904 0.077 Uiso 0.871(3) 1 calc PR B 1 Cl4 Cl 0.6645(2) -0.06430(13) 0.16341(6) 0.0697(6) Uani 0.871(3) 1 d PD B 1 Cl5 Cl 0.7921(2) 0.06059(11) 0.12669(6) 0.0750(6) Uani 0.871(3) 1 d PD B 1 Cl6 Cl 0.9536(3) -0.01877(18) 0.18983(11) 0.1129(12) Uani 0.871(3) 1 d PD B 1 C2SA C 0.8044(13) 0.0053(7) 0.1732(4) 0.0638(17) Uani 0.129(3) 1 d PD B 2 H2SA H 0.8071 0.0015 0.2025 0.077 Uiso 0.129(3) 1 calc PR B 2 Cl4A Cl 0.6411(12) -0.0259(8) 0.1533(4) 0.0697(6) Uani 0.129(3) 1 d PD B 2 Cl5A Cl 0.8264(14) 0.1023(6) 0.1619(4) 0.0750(6) Uani 0.129(3) 1 d PD B 2 Cl6A Cl 0.9462(13) -0.0467(8) 0.1600(7) 0.1129(12) Uani 0.129(3) 1 d PD B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 F1 0.0509(17) 0.0344(17) 0.083(2) -0.0126(16) 0.0121(16) -0.0038(13) F2 0.060(2) 0.081(3) 0.127(4) 0.058(3) 0.027(2) -0.0086(19) F3 0.058(2) 0.184(5) 0.042(2) 0.045(2) 0.0310(17) 0.010(2) F4 0.082(3) 0.128(4) 0.049(2) -0.041(2) 0.0181(18) 0.023(2) F5 0.0596(19) 0.0407(19) 0.072(2) -0.0146(16) 0.0153(16) 0.0007(14) O1 0.0381(16) 0.0208(15) 0.0124(13) 0.0015(11) 0.0082(11) 0.0023(12) O2 0.0312(14) 0.0213(15) 0.0102(12) -0.0007(11) 0.0046(10) 0.0012(11) O3 0.0375(15) 0.0227(15) 0.0091(13) 0.0032(11) 0.0057(11) 0.0006(12) O4 0.0410(16) 0.0203(15) 0.0105(13) 0.0013(11) 0.0082(11) -0.0009(12) O5 0.0281(15) 0.0427(19) 0.0173(14) 0.0070(13) 0.0070(12) 0.0034(13) N1 0.0266(17) 0.0276(19) 0.0149(16) 0.0007(14) 0.0068(13) 0.0027(14) N2 0.0313(18) 0.035(2) 0.0118(16) 0.0010(15) 0.0087(14) 0.0026(15) N3 0.039(2) 0.042(2) 0.0162(18) 0.0025(16) 0.0041(15) 0.0033(17) N4 0.0300(18) 0.033(2) 0.0132(16) 0.0054(14) 0.0065(14) 0.0005(15) N5 0.0293(18) 0.032(2) 0.0162(17) 0.0073(15) 0.0048(14) -0.0008(15) N6 0.0261(17) 0.028(2) 0.0126(16) 0.0009(14) 0.0044(13) 0.0001(14) C1 0.030(2) 0.030(2) 0.020(2) -0.0021(18) 0.0062(17) 0.0061(18) C2 0.033(2) 0.037(3) 0.021(2) -0.0091(19) 0.0093(18) 0.0040(19) C3 0.040(3) 0.039(3) 0.027(2) -0.007(2) 0.011(2) -0.003(2) C4 0.046(3) 0.047(3) 0.035(3) -0.014(2) 0.013(2) -0.008(2) C5 0.045(3) 0.061(4) 0.023(2) -0.011(2) 0.003(2) -0.002(2) C6 0.041(3) 0.055(3) 0.018(2) -0.007(2) 0.0012(19) 0.001(2) C7 0.036(2) 0.043(3) 0.020(2) -0.003(2) 0.0060(18) 0.005(2) C8 0.035(2) 0.043(3) 0.014(2) -0.0004(19) 0.0052(17) 0.001(2) C9 0.032(2) 0.046(3) 0.014(2) 0.0057(19) 0.0072(17) 0.002(2) C10 0.036(2) 0.037(3) 0.021(2) 0.0095(19) 0.0079(18) 0.002(2) C11 0.039(3) 0.050(3) 0.022(2) 0.009(2) 0.0041(19) 0.005(2) C12 0.042(3) 0.050(3) 0.030(3) 0.015(2) 0.004(2) 0.008(2) C13 0.048(3) 0.038(3) 0.036(3) 0.011(2) 0.011(2) 0.009(2) C14 0.041(3) 0.038(3) 0.024(2) 0.008(2) 0.0087(19) 0.005(2) C15 0.032(2) 0.038(3) 0.019(2) 0.0106(19) 0.0071(17) -0.0002(19) C16 0.029(2) 0.030(2) 0.021(2) 0.0023(18) 0.0072(17) 0.0001(18) C17 0.026(2) 0.028(2) 0.0117(18) 0.0009(16) 0.0043(15) -0.0024(17) C18 0.0207(19) 0.024(2) 0.0165(19) 0.0041(16) 0.0034(15) 0.0023(16) C19 0.0224(19) 0.022(2) 0.0117(18) 0.0003(15) 0.0039(14) 0.0008(15) C20 0.025(2) 0.032(2) 0.0117(19) 0.0009(17) 0.0047(15) 0.0055(17) C21 0.0207(18) 0.020(2) 0.0147(19) 0.0011(15) 0.0053(15) 0.0002(15) C22 0.0210(19) 0.028(2) 0.017(2) -0.0008(17) 0.0047(15) -0.0014(16) C23 0.0228(19) 0.025(2) 0.020(2) 0.0016(17) 0.0032(16) -0.0009(16) C24 0.026(2) 0.023(2) 0.025(2) 0.0000(17) 0.0054(17) -0.0002(16) C25 0.024(2) 0.034(2) 0.019(2) -0.0044(18) 0.0065(16) -0.0029(17) C26 0.026(2) 0.027(2) 0.0154(19) -0.0010(17) 0.0048(16) -0.0016(17) C27 0.0204(18) 0.023(2) 0.018(2) -0.0005(16) 0.0040(15) -0.0008(15) C28 0.0202(18) 0.025(2) 0.0099(18) -0.0013(15) 0.0050(14) 0.0011(15) C29 0.0224(19) 0.025(2) 0.0107(18) 0.0030(15) 0.0051(15) -0.0008(15) C30 0.0239(19) 0.020(2) 0.018(2) 0.0004(16) 0.0041(15) -0.0003(16) C31 0.031(2) 0.029(2) 0.0113(18) 0.0026(16) 0.0047(16) 0.0030(17) C32 0.029(2) 0.027(2) 0.019(2) 0.0061(17) 0.0069(16) 0.0032(17) C33 0.030(2) 0.022(2) 0.023(2) 0.0045(17) 0.0083(17) 0.0009(17) C34 0.0227(19) 0.028(2) 0.019(2) 0.0029(17) 0.0062(16) 0.0009(16) C35 0.0232(19) 0.024(2) 0.0159(19) 0.0034(16) 0.0058(15) 0.0025(16) C36 0.0228(19) 0.023(2) 0.0146(19) -0.0016(16) 0.0043(15) 0.0001(16) C37 0.032(2) 0.026(2) 0.023(2) 0.0043(18) 0.0017(17) 0.0023(18) C38 0.036(2) 0.034(3) 0.026(2) 0.0100(19) 0.0041(19) 0.0002(19) C39 0.031(2) 0.041(3) 0.028(2) 0.006(2) -0.0006(19) 0.003(2) C40 0.059(3) 0.030(3) 0.030(2) 0.007(2) 0.009(2) 0.009(2) C41 0.037(2) 0.026(2) 0.024(2) -0.0087(18) 0.0043(18) 0.0016(18) C42 0.040(3) 0.044(3) 0.024(2) -0.008(2) 0.0013(19) -0.003(2) C43 0.039(3) 0.060(3) 0.026(2) -0.013(2) 0.009(2) 0.003(2) C44 0.070(4) 0.040(3) 0.033(3) -0.017(2) 0.000(2) 0.009(3) C45 0.048(3) 0.029(2) 0.021(2) 0.0084(18) 0.0044(19) 0.002(2) C46 0.057(3) 0.105(6) 0.041(3) 0.039(3) 0.006(3) 0.018(3) C47 0.224(11) 0.044(4) 0.033(3) 0.019(3) 0.011(5) -0.028(5) C48 0.062(4) 0.071(4) 0.039(3) 0.025(3) 0.020(3) 0.008(3) C49 0.032(2) 0.030(2) 0.018(2) -0.0020(17) 0.0068(17) -0.0040(18) C50 0.060(3) 0.028(3) 0.027(2) -0.005(2) 0.012(2) -0.010(2) C51 0.036(2) 0.039(3) 0.025(2) -0.004(2) 0.0002(19) -0.004(2) C52 0.038(2) 0.034(3) 0.023(2) -0.0092(19) 0.0094(18) -0.0012(19) C53 0.024(2) 0.034(3) 0.019(2) 0.0028(18) 0.0047(16) -0.0005(17) C54 0.031(2) 0.040(3) 0.037(3) 0.004(2) 0.007(2) -0.003(2) C55 0.035(3) 0.052(4) 0.057(3) 0.025(3) 0.008(2) -0.005(2) C56 0.042(3) 0.095(5) 0.030(3) 0.029(3) 0.012(2) -0.001(3) C57 0.042(3) 0.091(5) 0.022(2) -0.017(3) 0.010(2) 0.012(3) C58 0.038(2) 0.039(3) 0.031(2) -0.003(2) 0.004(2) 0.002(2) B1 0.024(2) 0.034(3) 0.018(2) 0.001(2) 0.0045(18) 0.003(2) C1S 0.029(2) 0.044(3) 0.055(3) 0.003(2) 0.011(2) -0.002(2) Cl1 0.0315(7) 0.1262(16) 0.0528(9) 0.0217(9) 0.0013(6) -0.0046(7) Cl2 0.0565(8) 0.0485(8) 0.0638(9) 0.0049(7) 0.0097(7) -0.0073(6) Cl3 0.0610(9) 0.0502(9) 0.1255(16) -0.0291(10) 0.0227(9) 0.0011(7) C2S 0.072(4) 0.075(5) 0.046(3) 0.000(3) 0.011(3) -0.009(3) Cl4 0.0882(13) 0.0654(14) 0.0549(11) 0.0054(9) 0.0053(9) -0.0190(11) Cl5 0.1049(15) 0.0585(12) 0.0597(11) 0.0145(9) 0.0018(10) -0.0009(10) Cl6 0.0708(13) 0.120(2) 0.141(3) 0.067(2) -0.0184(16) -0.0049(13) C2SA 0.072(4) 0.075(5) 0.046(3) 0.000(3) 0.011(3) -0.009(3) Cl4A 0.0882(13) 0.0654(14) 0.0549(11) 0.0054(9) 0.0053(9) -0.0190(11) Cl5A 0.1049(15) 0.0585(12) 0.0597(11) 0.0145(9) 0.0018(10) -0.0009(10) Cl6A 0.0708(13) 0.120(2) 0.141(3) 0.067(2) -0.0184(16) -0.0049(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag F1 C54 1.338(6) . ? F2 C55 1.331(7) . ? F3 C56 1.340(6) . ? F4 C57 1.333(7) . ? F5 C58 1.340(6) . ? O1 C21 1.356(5) . ? O1 C22 1.392(5) . ? O2 C28 1.384(4) . ? O2 C27 1.400(5) . ? O3 C29 1.379(4) . ? O3 C30 1.399(5) . ? O4 C36 1.360(5) . ? O4 C35 1.390(5) . ? O5 C53 1.340(5) . ? O5 B1 1.472(5) . ? N1 C20 1.335(5) . ? N1 C1 1.337(5) . ? N2 C1 1.372(6) . ? N2 C8 1.373(5) . ? N2 B1 1.488(6) . ? N3 C8 1.336(6) . ? N3 C9 1.343(6) . ? N4 C16 1.367(6) . ? N4 C9 1.372(5) . ? N4 B1 1.492(6) . ? N5 C17 1.328(5) . ? N5 C16 1.336(5) . ? N6 C17 1.365(5) . ? N6 C20 1.378(5) . ? N6 B1 1.479(6) . ? C1 C2 1.450(6) . ? C2 C3 1.394(7) . ? C2 C7 1.408(6) . ? C3 C4 1.387(7) . ? C3 H3A 0.9500 . ? C4 C5 1.406(7) . ? C4 H4A 0.9500 . ? C5 C6 1.378(8) . ? C5 H5A 0.9500 . ? C6 C7 1.398(6) . ? C6 H6A 0.9500 . ? C7 C8 1.445(7) . ? C9 C10 1.450(7) . ? C10 C11 1.400(6) . ? C10 C15 1.416(6) . ? C11 C12 1.365(7) . ? C11 H11A 0.9500 . ? C12 C13 1.405(7) . ? C12 H12A 0.9500 . ? C13 C14 1.388(6) . ? C13 H13A 0.9500 . ? C14 C15 1.372(7) . ? C14 H14A 0.9500 . ? C15 C16 1.459(6) . ? C17 C18 1.450(5) . ? C18 C21 1.379(6) . ? C18 C19 1.426(6) . ? C19 C36 1.378(5) . ? C19 C20 1.454(5) . ? C21 C28 1.393(5) . ? C22 C23 1.382(6) . ? C22 C27 1.395(6) . ? C23 C24 1.390(6) . ? C23 C37 1.549(6) . ? C24 C25 1.392(6) . ? C24 H24A 0.9500 . ? C25 C26 1.388(6) . ? C25 C41 1.553(6) . ? C26 C27 1.371(6) . ? C26 H26A 0.9500 . ? C28 C29 1.393(6) . ? C29 C36 1.398(5) . ? C30 C31 1.371(6) . ? C30 C35 1.386(5) . ? C31 C32 1.387(6) . ? C31 H31A 0.9500 . ? C32 C33 1.391(6) . ? C32 C45 1.546(6) . ? C33 C34 1.394(6) . ? C33 H33A 0.9500 . ? C34 C35 1.388(6) . ? C34 C49 1.548(6) . ? C37 C40 1.529(6) . ? C37 C38 1.532(6) . ? C37 C39 1.537(6) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C43 1.517(7) . ? C41 C42 1.529(6) . ? C41 C44 1.534(7) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C47 1.490(8) . ? C45 C48 1.510(7) . ? C45 C46 1.532(7) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 C50 1.528(6) . ? C49 C51 1.535(6) . ? C49 C52 1.540(6) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 C58 1.384(7) . ? C53 C54 1.388(7) . ? C54 C55 1.383(7) . ? C55 C56 1.361(9) . ? C56 C57 1.388(9) . ? C57 C58 1.384(7) . ? C1S Cl3 1.744(6) . ? C1S Cl1 1.756(6) . ? C1S Cl2 1.760(5) . ? C1S H1S 1.0000 . ? C2S Cl4 1.721(7) . ? C2S Cl6 1.738(8) . ? C2S Cl5 1.771(7) . ? C2S H2S 1.0000 . ? C2SA Cl4A 1.721(7) . ? C2SA Cl6A 1.738(8) . ? C2SA Cl5A 1.771(7) . ? C2SA H2SA 1.0000 . ? 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 C21 O1 C22 116.6(3) . . ? C28 O2 C27 115.6(3) . . ? C29 O3 C30 115.4(3) . . ? C36 O4 C35 117.0(3) . . ? C53 O5 B1 121.6(3) . . ? C20 N1 C1 117.6(4) . . ? C1 N2 C8 112.8(4) . . ? C1 N2 B1 122.1(3) . . ? C8 N2 B1 123.3(4) . . ? C8 N3 C9 117.7(4) . . ? C16 N4 C9 112.7(4) . . ? C16 N4 B1 121.8(3) . . ? C9 N4 B1 123.4(4) . . ? C17 N5 C16 117.7(4) . . ? C17 N6 C20 114.2(3) . . ? C17 N6 B1 122.2(4) . . ? C20 N6 B1 122.9(3) . . ? N1 C1 N2 122.9(4) . . ? N1 C1 C2 130.3(4) . . ? N2 C1 C2 105.3(4) . . ? C3 C2 C7 121.0(4) . . ? C3 C2 C1 131.5(4) . . ? C7 C2 C1 107.4(4) . . ? C4 C3 C2 117.4(5) . . ? C4 C3 H3A 121.3 . . ? C2 C3 H3A 121.3 . . ? C3 C4 C5 121.8(5) . . ? C3 C4 H4A 119.1 . . ? C5 C4 H4A 119.1 . . ? C6 C5 C4 120.9(4) . . ? C6 C5 H5A 119.6 . . ? C4 C5 H5A 119.6 . . ? C5 C6 C7 118.1(5) . . ? C5 C6 H6A 121.0 . . ? C7 C6 H6A 121.0 . . ? C6 C7 C2 120.8(5) . . ? C6 C7 C8 131.0(4) . . ? C2 C7 C8 107.9(4) . . ? N3 C8 N2 122.4(4) . . ? N3 C8 C7 130.2(4) . . ? N2 C8 C7 105.2(4) . . ? N3 C9 N4 122.3(4) . . ? N3 C9 C10 130.3(4) . . ? N4 C9 C10 105.5(4) . . ? C11 C10 C15 120.5(4) . . ? C11 C10 C9 131.4(4) . . ? C15 C10 C9 107.9(4) . . ? C12 C11 C10 117.8(4) . . ? C12 C11 H11A 121.1 . . ? C10 C11 H11A 121.1 . . ? C11 C12 C13 121.8(4) . . ? C11 C12 H12A 119.1 . . ? C13 C12 H12A 119.1 . . ? C14 C13 C12 120.7(5) . . ? C14 C13 H13A 119.6 . . ? C12 C13 H13A 119.6 . . ? C15 C14 C13 118.2(4) . . ? C15 C14 H14A 120.9 . . ? C13 C14 H14A 120.9 . . ? C14 C15 C10 121.0(4) . . ? C14 C15 C16 131.9(4) . . ? C10 C15 C16 106.7(4) . . ? N5 C16 N4 122.6(4) . . ? N5 C16 C15 129.7(4) . . ? N4 C16 C15 105.9(3) . . ? N5 C17 N6 122.4(3) . . ? N5 C17 C18 132.0(4) . . ? N6 C17 C18 104.4(3) . . ? C21 C18 C19 120.5(3) . . ? C21 C18 C17 131.4(4) . . ? C19 C18 C17 108.1(3) . . ? C36 C19 C18 120.2(3) . . ? C36 C19 C20 132.7(4) . . ? C18 C19 C20 107.0(3) . . ? N1 C20 N6 121.7(3) . . ? N1 C20 C19 132.6(4) . . ? N6 C20 C19 104.5(3) . . ? O1 C21 C18 118.7(3) . . ? O1 C21 C28 122.5(3) . . ? C18 C21 C28 118.7(4) . . ? C23 C22 O1 118.9(3) . . ? C23 C22 C27 120.8(4) . . ? O1 C22 C27 120.3(4) . . ? C22 C23 C24 116.9(4) . . ? C22 C23 C37 121.6(4) . . ? C24 C23 C37 121.5(4) . . ? C23 C24 C25 122.9(4) . . ? C23 C24 H24A 118.6 . . ? C25 C24 H24A 118.6 . . ? C26 C25 C24 118.5(4) . . ? C26 C25 C41 120.1(4) . . ? C24 C25 C41 121.3(4) . . ? C27 C26 C25 119.4(4) . . ? C27 C26 H26A 120.3 . . ? C25 C26 H26A 120.3 . . ? C26 C27 C22 121.0(4) . . ? C26 C27 O2 117.3(3) . . ? C22 C27 O2 121.7(3) . . ? O2 C28 C29 118.3(3) . . ? O2 C28 C21 121.1(3) . . ? C29 C28 C21 120.6(3) . . ? O3 C29 C28 117.5(3) . . ? O3 C29 C36 121.6(4) . . ? C28 C29 C36 120.9(3) . . ? C31 C30 C35 121.3(4) . . ? C31 C30 O3 116.3(3) . . ? C35 C30 O3 122.4(3) . . ? C30 C31 C32 120.1(4) . . ? C30 C31 H31A 120.0 . . ? C32 C31 H31A 120.0 . . ? C31 C32 C33 117.7(4) . . ? C31 C32 C45 120.3(4) . . ? C33 C32 C45 122.0(4) . . ? C32 C33 C34 123.5(4) . . ? C32 C33 H33A 118.3 . . ? C34 C33 H33A 118.3 . . ? C35 C34 C33 116.7(4) . . ? C35 C34 C49 121.7(4) . . ? C33 C34 C49 121.6(4) . . ? C30 C35 C34 120.7(4) . . ? C30 C35 O4 120.7(4) . . ? C34 C35 O4 118.7(3) . . ? O4 C36 C19 119.2(3) . . ? O4 C36 C29 122.1(3) . . ? C19 C36 C29 118.6(4) . . ? C40 C37 C38 107.7(4) . . ? C40 C37 C39 107.5(4) . . ? C38 C37 C39 109.7(4) . . ? C40 C37 C23 111.4(4) . . ? C38 C37 C23 111.6(3) . . ? C39 C37 C23 108.7(3) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C43 C41 C42 110.3(4) . . ? C43 C41 C44 108.5(4) . . ? C42 C41 C44 108.6(4) . . ? C43 C41 C25 109.3(4) . . ? C42 C41 C25 108.6(3) . . ? C44 C41 C25 111.6(4) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C47 C45 C48 108.1(6) . . ? C47 C45 C46 111.1(6) . . ? C48 C45 C46 107.5(4) . . ? C47 C45 C32 112.7(4) . . ? C48 C45 C32 109.5(4) . . ? C46 C45 C32 107.8(4) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C45 C48 H48A 109.5 . . ? C45 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C45 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C50 C49 C51 107.6(4) . . ? C50 C49 C52 107.1(4) . . ? C51 C49 C52 109.6(4) . . ? C50 C49 C34 111.8(3) . . ? C51 C49 C34 110.3(3) . . ? C52 C49 C34 110.2(3) . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C49 C52 H52A 109.5 . . ? C49 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C49 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? O5 C53 C58 121.8(4) . . ? O5 C53 C54 121.3(4) . . ? C58 C53 C54 116.8(4) . . ? F1 C54 C55 118.0(5) . . ? F1 C54 C53 119.6(4) . . ? C55 C54 C53 122.3(5) . . ? F2 C55 C56 120.0(5) . . ? F2 C55 C54 120.5(6) . . ? C56 C55 C54 119.5(5) . . ? F3 C56 C55 120.6(6) . . ? F3 C56 C57 119.3(6) . . ? C55 C56 C57 120.1(5) . . ? F4 C57 C58 120.0(6) . . ? F4 C57 C56 120.6(5) . . ? C58 C57 C56 119.4(5) . . ? F5 C58 C53 119.2(4) . . ? F5 C58 C57 119.0(5) . . ? C53 C58 C57 121.8(5) . . ? O5 B1 N6 109.1(3) . . ? O5 B1 N2 116.2(4) . . ? N6 B1 N2 104.9(4) . . ? O5 B1 N4 115.5(4) . . ? N6 B1 N4 105.3(3) . . ? N2 B1 N4 104.8(3) . . ? Cl3 C1S Cl1 111.3(3) . . ? Cl3 C1S Cl2 109.5(3) . . ? Cl1 C1S Cl2 109.4(3) . . ? Cl3 C1S H1S 108.9 . . ? Cl1 C1S H1S 108.9 . . ? Cl2 C1S H1S 108.9 . . ? Cl4 C2S Cl6 115.3(5) . . ? Cl4 C2S Cl5 110.7(4) . . ? Cl6 C2S Cl5 109.5(4) . . ? Cl4 C2S H2S 107.0 . . ? Cl6 C2S H2S 107.0 . . ? Cl5 C2S H2S 107.0 . . ? Cl4A C2SA Cl6A 115.5(5) . . ? Cl4A C2SA Cl5A 110.3(5) . . ? Cl6A C2SA Cl5A 109.7(5) . . ? Cl4A C2SA H2SA 107.0 . . ? Cl6A C2SA H2SA 107.0 . . ? Cl5A C2SA H2SA 107.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C20 N1 C1 N2 -9.6(6) . . . . ? C20 N1 C1 C2 153.9(4) . . . . ? C8 N2 C1 N1 155.0(4) . . . . ? B1 N2 C1 N1 -10.5(6) . . . . ? C8 N2 C1 C2 -12.0(5) . . . . ? B1 N2 C1 C2 -177.6(4) . . . . ? N1 C1 C2 C3 17.7(8) . . . . ? N2 C1 C2 C3 -176.6(5) . . . . ? N1 C1 C2 C7 -158.1(4) . . . . ? N2 C1 C2 C7 7.6(5) . . . . ? C7 C2 C3 C4 0.0(7) . . . . ? C1 C2 C3 C4 -175.3(5) . . . . ? C2 C3 C4 C5 1.3(7) . . . . ? C3 C4 C5 C6 -0.8(8) . . . . ? C4 C5 C6 C7 -1.0(7) . . . . ? C5 C6 C7 C2 2.3(7) . . . . ? C5 C6 C7 C8 176.6(5) . . . . ? C3 C2 C7 C6 -1.8(7) . . . . ? C1 C2 C7 C6 174.5(4) . . . . ? C3 C2 C7 C8 -177.3(4) . . . . ? C1 C2 C7 C8 -1.0(5) . . . . ? C9 N3 C8 N2 7.4(6) . . . . ? C9 N3 C8 C7 -153.2(5) . . . . ? C1 N2 C8 N3 -153.4(4) . . . . ? B1 N2 C8 N3 12.0(6) . . . . ? C1 N2 C8 C7 11.4(5) . . . . ? B1 N2 C8 C7 176.8(4) . . . . ? C6 C7 C8 N3 -17.7(8) . . . . ? C2 C7 C8 N3 157.2(5) . . . . ? C6 C7 C8 N2 179.1(5) . . . . ? C2 C7 C8 N2 -6.0(5) . . . . ? C8 N3 C9 N4 -8.4(6) . . . . ? C8 N3 C9 C10 153.2(5) . . . . ? C16 N4 C9 N3 154.0(4) . . . . ? B1 N4 C9 N3 -10.0(6) . . . . ? C16 N4 C9 C10 -11.5(5) . . . . ? B1 N4 C9 C10 -175.5(4) . . . . ? N3 C9 C10 C11 16.4(8) . . . . ? N4 C9 C10 C11 -179.7(5) . . . . ? N3 C9 C10 C15 -157.6(4) . . . . ? N4 C9 C10 C15 6.3(5) . . . . ? C15 C10 C11 C12 -0.6(7) . . . . ? C9 C10 C11 C12 -174.0(5) . . . . ? C10 C11 C12 C13 0.0(7) . . . . ? C11 C12 C13 C14 1.5(8) . . . . ? C12 C13 C14 C15 -2.4(7) . . . . ? C13 C14 C15 C10 1.8(7) . . . . ? C13 C14 C15 C16 174.1(5) . . . . ? C11 C10 C15 C14 -0.3(7) . . . . ? C9 C10 C15 C14 174.5(4) . . . . ? C11 C10 C15 C16 -174.3(4) . . . . ? C9 C10 C15 C16 0.5(5) . . . . ? C17 N5 C16 N4 10.2(6) . . . . ? C17 N5 C16 C15 -152.4(4) . . . . ? C9 N4 C16 N5 -154.3(4) . . . . ? B1 N4 C16 N5 9.9(6) . . . . ? C9 N4 C16 C15 11.8(5) . . . . ? B1 N4 C16 C15 176.1(4) . . . . ? C14 C15 C16 N5 -15.4(8) . . . . ? C10 C15 C16 N5 157.7(4) . . . . ? C14 C15 C16 N4 179.8(5) . . . . ? C10 C15 C16 N4 -7.1(5) . . . . ? C16 N5 C17 N6 -8.1(6) . . . . ? C16 N5 C17 C18 157.5(4) . . . . ? C20 N6 C17 N5 156.2(4) . . . . ? B1 N6 C17 N5 -14.5(6) . . . . ? C20 N6 C17 C18 -12.7(4) . . . . ? B1 N6 C17 C18 176.6(3) . . . . ? N5 C17 C18 C21 17.7(7) . . . . ? N6 C17 C18 C21 -174.9(4) . . . . ? N5 C17 C18 C19 -160.6(4) . . . . ? N6 C17 C18 C19 6.8(4) . . . . ? C21 C18 C19 C36 0.9(5) . . . . ? C17 C18 C19 C36 179.4(3) . . . . ? C21 C18 C19 C20 -177.8(3) . . . . ? C17 C18 C19 C20 0.7(4) . . . . ? C1 N1 C20 N6 7.7(6) . . . . ? C1 N1 C20 C19 -158.1(4) . . . . ? C17 N6 C20 N1 -156.0(4) . . . . ? B1 N6 C20 N1 14.6(6) . . . . ? C17 N6 C20 C19 13.2(4) . . . . ? B1 N6 C20 C19 -176.1(3) . . . . ? C36 C19 C20 N1 -18.8(7) . . . . ? C18 C19 C20 N1 159.7(4) . . . . ? C36 C19 C20 N6 173.6(4) . . . . ? C18 C19 C20 N6 -7.9(4) . . . . ? C22 O1 C21 C18 -174.5(3) . . . . ? C22 O1 C21 C28 8.0(5) . . . . ? C19 C18 C21 O1 176.0(3) . . . . ? C17 C18 C21 O1 -2.2(6) . . . . ? C19 C18 C21 C28 -6.4(5) . . . . ? C17 C18 C21 C28 175.4(4) . . . . ? C21 O1 C22 C23 165.8(3) . . . . ? C21 O1 C22 C27 -15.6(5) . . . . ? O1 C22 C23 C24 171.2(3) . . . . ? C27 C22 C23 C24 -7.4(6) . . . . ? O1 C22 C23 C37 -10.9(5) . . . . ? C27 C22 C23 C37 170.5(4) . . . . ? C22 C23 C24 C25 1.9(6) . . . . ? C37 C23 C24 C25 -176.0(4) . . . . ? C23 C24 C25 C26 3.8(6) . . . . ? C23 C24 C25 C41 -175.9(4) . . . . ? C24 C25 C26 C27 -4.1(6) . . . . ? C41 C25 C26 C27 175.6(4) . . . . ? C25 C26 C27 C22 -1.3(6) . . . . ? C25 C26 C27 O2 177.6(3) . . . . ? C23 C22 C27 C26 7.3(6) . . . . ? O1 C22 C27 C26 -171.2(3) . . . . ? C23 C22 C27 O2 -171.5(3) . . . . ? O1 C22 C27 O2 9.9(5) . . . . ? C28 O2 C27 C26 -175.0(3) . . . . ? C28 O2 C27 C22 3.9(5) . . . . ? C27 O2 C28 C29 171.0(3) . . . . ? C27 O2 C28 C21 -11.6(5) . . . . ? O1 C21 C28 O2 5.9(5) . . . . ? C18 C21 C28 O2 -171.6(3) . . . . ? O1 C21 C28 C29 -176.8(3) . . . . ? C18 C21 C28 C29 5.7(5) . . . . ? C30 O3 C29 C28 -174.0(3) . . . . ? C30 O3 C29 C36 7.9(5) . . . . ? O2 C28 C29 O3 -0.3(5) . . . . ? C21 C28 C29 O3 -177.7(3) . . . . ? O2 C28 C29 C36 177.9(3) . . . . ? C21 C28 C29 C36 0.5(6) . . . . ? C29 O3 C30 C31 177.7(3) . . . . ? C29 O3 C30 C35 -2.5(5) . . . . ? C35 C30 C31 C32 1.8(6) . . . . ? O3 C30 C31 C32 -178.4(3) . . . . ? C30 C31 C32 C33 1.6(6) . . . . ? C30 C31 C32 C45 -176.4(4) . . . . ? C31 C32 C33 C34 -2.7(6) . . . . ? C45 C32 C33 C34 175.3(4) . . . . ? C32 C33 C34 C35 0.3(6) . . . . ? C32 C33 C34 C49 -179.1(4) . . . . ? C31 C30 C35 C34 -4.3(6) . . . . ? O3 C30 C35 C34 175.9(3) . . . . ? C31 C30 C35 O4 174.1(3) . . . . ? O3 C30 C35 O4 -5.7(6) . . . . ? C33 C34 C35 C30 3.2(6) . . . . ? C49 C34 C35 C30 -177.4(4) . . . . ? C33 C34 C35 O4 -175.2(3) . . . . ? C49 C34 C35 O4 4.1(5) . . . . ? C36 O4 C35 C30 8.4(5) . . . . ? C36 O4 C35 C34 -173.2(3) . . . . ? C35 O4 C36 C19 179.5(3) . . . . ? C35 O4 C36 C29 -3.1(5) . . . . ? C18 C19 C36 O4 -177.2(3) . . . . ? C20 C19 C36 O4 1.1(6) . . . . ? C18 C19 C36 C29 5.3(5) . . . . ? C20 C19 C36 C29 -176.4(4) . . . . ? O3 C29 C36 O4 -5.3(6) . . . . ? C28 C29 C36 O4 176.6(3) . . . . ? O3 C29 C36 C19 172.1(3) . . . . ? C28 C29 C36 C19 -6.0(6) . . . . ? C22 C23 C37 C40 -176.1(4) . . . . ? C24 C23 C37 C40 1.7(5) . . . . ? C22 C23 C37 C38 63.5(5) . . . . ? C24 C23 C37 C38 -118.7(4) . . . . ? C22 C23 C37 C39 -57.7(5) . . . . ? C24 C23 C37 C39 120.1(4) . . . . ? C26 C25 C41 C43 60.2(5) . . . . ? C24 C25 C41 C43 -120.1(4) . . . . ? C26 C25 C41 C42 -60.2(5) . . . . ? C24 C25 C41 C42 119.5(4) . . . . ? C26 C25 C41 C44 -179.9(4) . . . . ? C24 C25 C41 C44 -0.2(6) . . . . ? C31 C32 C45 C47 -173.7(6) . . . . ? C33 C32 C45 C47 8.3(7) . . . . ? C31 C32 C45 C48 -53.4(6) . . . . ? C33 C32 C45 C48 128.7(5) . . . . ? C31 C32 C45 C46 63.3(6) . . . . ? C33 C32 C45 C46 -114.7(5) . . . . ? C35 C34 C49 C50 177.3(4) . . . . ? C33 C34 C49 C50 -3.4(5) . . . . ? C35 C34 C49 C51 57.5(5) . . . . ? C33 C34 C49 C51 -123.1(4) . . . . ? C35 C34 C49 C52 -63.6(5) . . . . ? C33 C34 C49 C52 115.7(4) . . . . ? B1 O5 C53 C58 97.4(5) . . . . ? B1 O5 C53 C54 -88.0(5) . . . . ? O5 C53 C54 F1 4.5(6) . . . . ? C58 C53 C54 F1 179.2(4) . . . . ? O5 C53 C54 C55 -173.9(4) . . . . ? C58 C53 C54 C55 0.9(7) . . . . ? F1 C54 C55 F2 1.5(7) . . . . ? C53 C54 C55 F2 179.8(4) . . . . ? F1 C54 C55 C56 -177.3(4) . . . . ? C53 C54 C55 C56 1.0(7) . . . . ? F2 C55 C56 F3 0.3(8) . . . . ? C54 C55 C56 F3 179.1(5) . . . . ? F2 C55 C56 C57 178.9(5) . . . . ? C54 C55 C56 C57 -2.3(8) . . . . ? F3 C56 C57 F4 0.2(8) . . . . ? C55 C56 C57 F4 -178.4(5) . . . . ? F3 C56 C57 C58 -179.8(5) . . . . ? C55 C56 C57 C58 1.6(8) . . . . ? O5 C53 C58 F5 -6.1(6) . . . . ? C54 C53 C58 F5 179.1(4) . . . . ? O5 C53 C58 C57 173.2(4) . . . . ? C54 C53 C58 C57 -1.6(7) . . . . ? F4 C57 C58 F5 -0.3(7) . . . . ? C56 C57 C58 F5 179.7(4) . . . . ? F4 C57 C58 C53 -179.6(4) . . . . ? C56 C57 C58 C53 0.3(7) . . . . ? C53 O5 B1 N6 169.2(4) . . . . ? C53 O5 B1 N2 -72.5(5) . . . . ? C53 O5 B1 N4 51.0(5) . . . . ? C17 N6 B1 O5 -94.8(4) . . . . ? C20 N6 B1 O5 95.3(4) . . . . ? C17 N6 B1 N2 140.1(4) . . . . ? C20 N6 B1 N2 -29.8(5) . . . . ? C17 N6 B1 N4 29.8(5) . . . . ? C20 N6 B1 N4 -140.1(4) . . . . ? C1 N2 B1 O5 -92.8(5) . . . . ? C8 N2 B1 O5 103.2(5) . . . . ? C1 N2 B1 N6 27.7(5) . . . . ? C8 N2 B1 N6 -136.3(4) . . . . ? C1 N2 B1 N4 138.4(4) . . . . ? C8 N2 B1 N4 -25.7(5) . . . . ? C16 N4 B1 O5 92.9(5) . . . . ? C9 N4 B1 O5 -104.6(5) . . . . ? C16 N4 B1 N6 -27.5(5) . . . . ? C9 N4 B1 N6 135.1(4) . . . . ? C16 N4 B1 N2 -137.9(4) . . . . ? C9 N4 B1 N2 24.7(5) . . . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 65.56 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.042 _refine_diff_density_min -1.491 _refine_diff_density_rms 0.095 _iucr_refine_instructions_details ; TITL cu_d12294_0m in P2(1)/n CELL 1.54178 9.5648 17.6316 34.0701 90.000 96.526 90.000 ZERR 4.00 0.0004 0.0008 0.0014 0.000 0.002 0.000 LATT 1 SYMM -x+1/2, y+1/2, -z+1/2 SFAC C H N O B F Cl UNIT 240 200 24 20 4 20 24 TEMP -153.120 SIZE 0.060 0.060 0.260 ACTA L.S. 4 FMAP 2 PLAN 20 HTAB BOND $H EADP Cl4 Cl4A EADP Cl5 Cl5A EADP Cl6 Cl6A EADP C2S C2SA CONF WGHT 0.126300 12.748700 FVAR 0.04680 0.87125 0.99107 F1 6 0.369053 0.361448 0.177240 11.00000 0.05088 0.03444 = 0.08281 -0.01264 0.01209 -0.00382 F2 6 0.231576 0.331059 0.239935 11.00000 0.05951 0.08084 = 0.12740 0.05847 0.02707 -0.00857 F3 6 0.149779 0.445502 0.285224 11.00000 0.05829 0.18360 = 0.04237 0.04536 0.03104 0.01006 F4 6 0.218702 0.591010 0.269056 11.00000 0.08184 0.12753 = 0.04912 -0.04108 0.01808 0.02295 F5 6 0.361656 0.621775 0.206969 11.00000 0.05958 0.04074 = 0.07210 -0.01458 0.01533 0.00073 O1 4 0.671380 0.363110 0.019086 11.00000 0.03812 0.02077 = 0.01238 0.00154 0.00823 0.00229 O2 4 0.670350 0.449320 -0.051339 11.00000 0.03120 0.02127 = 0.01022 -0.00070 0.00459 0.00119 O3 4 0.676672 0.601412 -0.047650 11.00000 0.03747 0.02275 = 0.00909 0.00316 0.00570 0.00057 O4 4 0.684617 0.676455 0.026564 11.00000 0.04105 0.02032 = 0.01054 0.00134 0.00822 -0.00088 O5 4 0.427802 0.507996 0.157256 11.00000 0.02805 0.04269 = 0.01730 0.00699 0.00699 0.00344 N1 3 0.676027 0.640694 0.118239 11.00000 0.02662 0.02758 = 0.01490 0.00069 0.00675 0.00272 N2 3 0.662202 0.569577 0.177002 11.00000 0.03133 0.03466 = 0.01179 0.00098 0.00869 0.00255 N3 3 0.766433 0.494962 0.230524 11.00000 0.03893 0.04169 = 0.01621 0.00248 0.00413 0.00334 N4 3 0.653286 0.435937 0.172696 11.00000 0.03000 0.03271 = 0.01318 0.00544 0.00653 0.00051 N5 3 0.658075 0.379767 0.109647 11.00000 0.02932 0.03176 = 0.01622 0.00726 0.00476 -0.00083 N6 3 0.612591 0.510722 0.115025 11.00000 0.02608 0.02795 = 0.01262 0.00093 0.00440 0.00009 C1 1 0.694752 0.634225 0.157574 11.00000 0.02995 0.03027 = 0.02011 -0.00208 0.00620 0.00610 C2 1 0.778075 0.679766 0.186994 11.00000 0.03338 0.03676 = 0.02070 -0.00913 0.00928 0.00396 C3 1 0.835048 0.752263 0.185077 11.00000 0.04019 0.03905 = 0.02734 -0.00691 0.01064 -0.00343 AFIX 43 H3A 2 0.816602 0.782700 0.162063 11.00000 -1.20000 AFIX 0 C4 1 0.919746 0.778211 0.218104 11.00000 0.04614 0.04674 = 0.03515 -0.01375 0.01304 -0.00786 AFIX 43 H4A 2 0.958313 0.827832 0.217805 11.00000 -1.20000 AFIX 0 C5 1 0.950036 0.733012 0.252017 11.00000 0.04509 0.06062 = 0.02310 -0.01118 0.00299 -0.00231 AFIX 43 H5A 2 1.009426 0.752320 0.273994 11.00000 -1.20000 AFIX 0 C6 1 0.894731 0.661113 0.253791 11.00000 0.04062 0.05500 = 0.01798 -0.00696 0.00123 0.00062 AFIX 43 H6A 2 0.916326 0.630219 0.276517 11.00000 -1.20000 AFIX 0 C7 1 0.805930 0.634925 0.221192 11.00000 0.03599 0.04332 = 0.02012 -0.00305 0.00598 0.00465 C8 1 0.738400 0.562316 0.213466 11.00000 0.03495 0.04344 = 0.01386 -0.00040 0.00519 0.00088 C9 1 0.731366 0.432602 0.209013 11.00000 0.03235 0.04597 = 0.01427 0.00566 0.00719 0.00183 C10 1 0.791153 0.356930 0.211704 11.00000 0.03608 0.03660 = 0.02103 0.00953 0.00791 0.00230 C11 1 0.878877 0.321026 0.241792 11.00000 0.03901 0.05032 = 0.02201 0.00876 0.00406 0.00510 AFIX 43 H11A 2 0.902670 0.344815 0.266674 11.00000 -1.20000 AFIX 0 C12 1 0.929093 0.250699 0.234191 11.00000 0.04170 0.05025 = 0.02954 0.01497 0.00426 0.00839 AFIX 43 H12A 2 0.988753 0.225354 0.254221 11.00000 -1.20000 AFIX 0 C13 1 0.894924 0.214803 0.197552 11.00000 0.04838 0.03755 = 0.03600 0.01098 0.01135 0.00934 AFIX 43 H13A 2 0.929786 0.165323 0.193445 11.00000 -1.20000 AFIX 0 C14 1 0.810785 0.250840 0.167288 11.00000 0.04131 0.03831 = 0.02373 0.00781 0.00870 0.00485 AFIX 43 H14A 2 0.790451 0.227505 0.142154 11.00000 -1.20000 AFIX 0 C15 1 0.757746 0.321092 0.174645 11.00000 0.03193 0.03759 = 0.01930 0.01064 0.00710 -0.00016 C16 1 0.677747 0.375888 0.149041 11.00000 0.02897 0.02978 = 0.02147 0.00230 0.00720 0.00010 C17 1 0.634224 0.447611 0.093303 11.00000 0.02636 0.02808 = 0.01166 0.00089 0.00435 -0.00238 C18 1 0.652335 0.476671 0.054374 11.00000 0.02068 0.02445 = 0.01654 0.00405 0.00340 0.00234 C19 1 0.656822 0.557422 0.056542 11.00000 0.02245 0.02184 = 0.01167 0.00026 0.00389 0.00084 C20 1 0.643135 0.577991 0.097247 11.00000 0.02538 0.03246 = 0.01170 0.00088 0.00475 0.00554 C21 1 0.667644 0.440008 0.019367 11.00000 0.02066 0.02007 = 0.01470 0.00105 0.00534 0.00019 C22 1 0.699364 0.328911 -0.015995 11.00000 0.02102 0.02753 = 0.01731 -0.00084 0.00466 -0.00140 C23 1 0.735176 0.252986 -0.015634 11.00000 0.02276 0.02546 = 0.02045 0.00160 0.00317 -0.00089 C24 1 0.742731 0.218666 -0.052051 11.00000 0.02578 0.02331 = 0.02536 -0.00003 0.00539 -0.00022 AFIX 43 H24A 2 0.764293 0.166115 -0.052676 11.00000 -1.20000 AFIX 0 C25 1 0.720075 0.257938 -0.087667 11.00000 0.02359 0.03352 = 0.01874 -0.00438 0.00654 -0.00290 C26 1 0.696987 0.335593 -0.086632 11.00000 0.02621 0.02748 = 0.01545 -0.00101 0.00483 -0.00160 AFIX 43 H26A 2 0.687323 0.364302 -0.110382 11.00000 -1.20000 AFIX 0 C27 1 0.688252 0.370502 -0.051043 11.00000 0.02045 0.02336 = 0.01756 -0.00051 0.00403 -0.00083 C28 1 0.673283 0.483251 -0.014627 11.00000 0.02015 0.02457 = 0.00994 -0.00132 0.00505 0.00110 C29 1 0.676258 0.562131 -0.012652 11.00000 0.02243 0.02459 = 0.01071 0.00299 0.00506 -0.00082 C30 1 0.693611 0.679994 -0.043884 11.00000 0.02393 0.01998 = 0.01843 0.00039 0.00413 -0.00025 C31 1 0.699552 0.719775 -0.078236 11.00000 0.03092 0.02934 = 0.01131 0.00262 0.00466 0.00296 AFIX 43 H31A 2 0.689867 0.693949 -0.102868 11.00000 -1.20000 AFIX 0 C32 1 0.719691 0.797705 -0.077060 11.00000 0.02946 0.02734 = 0.01932 0.00612 0.00693 0.00323 C33 1 0.736902 0.832545 -0.040206 11.00000 0.02970 0.02159 = 0.02335 0.00453 0.00825 0.00090 AFIX 43 H33A 2 0.754802 0.885544 -0.039072 11.00000 -1.20000 AFIX 0 C34 1 0.729278 0.793811 -0.004830 11.00000 0.02266 0.02799 = 0.01899 0.00288 0.00622 0.00090 C35 1 0.703575 0.716392 -0.007614 11.00000 0.02316 0.02405 = 0.01588 0.00340 0.00581 0.00248 C36 1 0.674673 0.599671 0.023453 11.00000 0.02277 0.02297 = 0.01459 -0.00163 0.00429 0.00010 C37 1 0.770410 0.208887 0.023571 11.00000 0.03223 0.02608 = 0.02257 0.00432 0.00170 0.00228 C38 1 0.643545 0.204863 0.047170 11.00000 0.03599 0.03387 = 0.02639 0.01001 0.00406 0.00025 AFIX 137 H38A 2 0.563623 0.182066 0.030789 11.00000 -1.50000 H38B 2 0.618400 0.256135 0.054979 11.00000 -1.50000 H38C 2 0.667435 0.173814 0.070840 11.00000 -1.50000 AFIX 0 C39 1 0.893637 0.248612 0.048260 11.00000 0.03132 0.04126 = 0.02789 0.00635 -0.00062 0.00335 AFIX 137 H39A 2 0.920525 0.219514 0.072450 11.00000 -1.50000 H39B 2 0.864951 0.299801 0.055193 11.00000 -1.50000 H39C 2 0.974011 0.251851 0.032880 11.00000 -1.50000 AFIX 0 C40 1 0.816356 0.127621 0.016068 11.00000 0.05931 0.03031 = 0.02957 0.00695 0.00880 0.00920 AFIX 137 H40A 2 0.738799 0.100328 0.000947 11.00000 -1.50000 H40B 2 0.841825 0.101940 0.041381 11.00000 -1.50000 H40C 2 0.897898 0.128501 0.001065 11.00000 -1.50000 AFIX 0 C41 1 0.719617 0.216531 -0.127899 11.00000 0.03675 0.02630 = 0.02425 -0.00873 0.00433 0.00158 C42 1 0.575462 0.227465 -0.151589 11.00000 0.03984 0.04386 = 0.02381 -0.00846 0.00130 -0.00269 AFIX 137 H42A 2 0.558901 0.281632 -0.156615 11.00000 -1.50000 H42B 2 0.502261 0.207342 -0.136544 11.00000 -1.50000 H42C 2 0.572807 0.200429 -0.176795 11.00000 -1.50000 AFIX 0 C43 1 0.834054 0.249527 -0.150160 11.00000 0.03925 0.06000 = 0.02583 -0.01301 0.00931 0.00339 AFIX 137 H43A 2 0.818325 0.304095 -0.153929 11.00000 -1.50000 H43B 2 0.831744 0.224709 -0.175963 11.00000 -1.50000 H43C 2 0.926035 0.241097 -0.134971 11.00000 -1.50000 AFIX 0 C44 1 0.746767 0.131262 -0.122285 11.00000 0.06957 0.04035 = 0.03284 -0.01677 -0.00030 0.00922 AFIX 137 H44A 2 0.747804 0.107072 -0.148147 11.00000 -1.50000 H44B 2 0.672018 0.108780 -0.108628 11.00000 -1.50000 H44C 2 0.837822 0.123459 -0.106493 11.00000 -1.50000 AFIX 0 C45 1 0.717805 0.843467 -0.115816 11.00000 0.04812 0.02899 = 0.02066 0.00844 0.00440 0.00230 C46 1 0.570517 0.836081 -0.138390 11.00000 0.05661 0.10503 = 0.04128 0.03854 0.00608 0.01816 AFIX 137 H46A 2 0.569891 0.858851 -0.164649 11.00000 -1.50000 H46B 2 0.502248 0.862335 -0.123829 11.00000 -1.50000 H46C 2 0.545189 0.782331 -0.141132 11.00000 -1.50000 AFIX 0 C47 1 0.756628 0.924589 -0.108828 11.00000 0.22362 0.04430 = 0.03311 0.01945 0.01095 -0.02774 AFIX 137 H47A 2 0.847490 0.927684 -0.092418 11.00000 -1.50000 H47B 2 0.684350 0.949741 -0.095274 11.00000 -1.50000 H47C 2 0.763577 0.949697 -0.134195 11.00000 -1.50000 AFIX 0 C48 1 0.820875 0.809009 -0.141178 11.00000 0.06221 0.07086 = 0.03852 0.02494 0.02010 0.00828 AFIX 137 H48A 2 0.916233 0.812189 -0.127307 11.00000 -1.50000 H48B 2 0.816855 0.836755 -0.166205 11.00000 -1.50000 H48C 2 0.796412 0.755724 -0.146477 11.00000 -1.50000 AFIX 0 C49 1 0.747002 0.835297 0.035468 11.00000 0.03246 0.02962 = 0.01803 -0.00198 0.00677 -0.00397 C50 1 0.781338 0.919250 0.030975 11.00000 0.06006 0.02826 = 0.02719 -0.00480 0.01179 -0.00968 AFIX 137 H50A 2 0.704423 0.943962 0.014252 11.00000 -1.50000 H50B 2 0.868786 0.924247 0.018740 11.00000 -1.50000 H50C 2 0.792830 0.943396 0.057051 11.00000 -1.50000 AFIX 0 C51 1 0.867591 0.799625 0.062953 11.00000 0.03586 0.03874 = 0.02470 -0.00382 0.00017 -0.00380 AFIX 137 H51A 2 0.887240 0.830923 0.086711 11.00000 -1.50000 H51B 2 0.952050 0.796671 0.049214 11.00000 -1.50000 H51C 2 0.840453 0.748513 0.070480 11.00000 -1.50000 AFIX 0 C52 1 0.609638 0.830982 0.054942 11.00000 0.03805 0.03400 = 0.02309 -0.00915 0.00940 -0.00121 AFIX 137 H52A 2 0.533138 0.854501 0.037536 11.00000 -1.50000 H52B 2 0.621825 0.857934 0.080257 11.00000 -1.50000 H52C 2 0.586515 0.777765 0.059431 11.00000 -1.50000 AFIX 0 C53 1 0.369248 0.492683 0.190282 11.00000 0.02365 0.03405 = 0.01925 0.00284 0.00465 -0.00050 C54 1 0.334931 0.419034 0.199882 11.00000 0.03097 0.04036 = 0.03729 0.00369 0.00734 -0.00307 C55 1 0.262798 0.402502 0.231777 11.00000 0.03526 0.05216 = 0.05674 0.02470 0.00834 -0.00508 C56 1 0.221429 0.460039 0.254470 11.00000 0.04215 0.09462 = 0.03032 0.02887 0.01189 -0.00145 C57 1 0.255915 0.534469 0.246447 11.00000 0.04227 0.09087 = 0.02169 -0.01715 0.00969 0.01232 C58 1 0.329457 0.549713 0.214620 11.00000 0.03844 0.03855 = 0.03060 -0.00316 0.00428 0.00151 B1 5 0.581280 0.506171 0.156482 11.00000 0.02395 0.03412 = 0.01779 0.00121 0.00446 0.00309 PART 1 C1S 1 1.080447 0.482472 0.103874 11.00000 0.02865 0.04384 = 0.05520 0.00288 0.01067 -0.00195 AFIX 13 H1S 2 1.184996 0.487749 0.105291 11.00000 -1.20000 AFIX 0 CL1 7 1.009146 0.482258 0.054036 11.00000 0.03148 0.12616 = 0.05277 0.02167 0.00126 -0.00456 CL2 7 1.040723 0.395990 0.125936 11.00000 0.05653 0.04852 = 0.06377 0.00492 0.00973 -0.00727 CL3 7 1.014281 0.557465 0.129590 11.00000 0.06096 0.05018 = 0.12547 -0.02908 0.02275 0.00107 PART 1 C2S 1 0.784673 0.008368 0.170818 21.00000 0.07168 0.07459 = 0.04596 -0.00040 0.01058 -0.00858 AFIX 13 H2S 2 0.749460 0.043734 0.190433 21.00000 -1.20000 AFIX 0 CL4 7 0.664454 -0.064299 0.163414 21.00000 0.08816 0.06536 = 0.05489 0.00539 0.00533 -0.01901 CL5 7 0.792065 0.060590 0.126692 21.00000 0.10494 0.05849 = 0.05971 0.01446 0.00184 -0.00094 CL6 7 0.953595 -0.018770 0.189831 21.00000 0.07079 0.11976 = 0.14107 0.06734 -0.01845 -0.00493 PART 2 SAME 0.002 C2S > Cl6 C2SA 1 0.804427 0.005276 0.173179 -21.00000 0.07168 0.07459 = 0.04596 -0.00040 0.01058 -0.00858 AFIX 13 H2SA 2 0.807140 0.001474 0.202541 -21.00000 -1.20000 AFIX 0 CL4A 7 0.641077 -0.025887 0.153294 -21.00000 0.08816 0.06536 = 0.05489 0.00539 0.00533 -0.01901 CL5A 7 0.826388 0.102310 0.161898 -21.00000 0.10494 0.05849 = 0.05971 0.01446 0.00184 -0.00094 CL6A 7 0.946235 -0.046693 0.159958 -21.00000 0.07079 0.11976 = 0.14107 0.06734 -0.01845 -0.00493 PART 0 HKLF 4 REM cu_d12294_0m in P2(1)/n REM R1 = 0.0772 for 6984 Fo > 4sig(Fo) and 0.1043 for all 9635 data REM 774 parameters refined using 6 restraints END WGHT 0.1260 12.8147 REM Highest difference peak 1.042, deepest hole -1.491, 1-sigma level 0.095 Q1 1 0.9651 0.8837 0.2099 11.00000 0.05 0.83 Q2 1 1.0042 0.5451 0.0626 11.00000 0.05 0.75 Q3 1 0.9288 0.1176 0.1947 11.00000 0.05 0.66 Q4 1 0.5837 0.9003 -0.1191 11.00000 0.05 0.63 Q5 1 0.8182 0.8675 0.1740 11.00000 0.05 0.62 Q6 1 0.9705 0.0111 0.1613 11.00000 0.05 0.60 Q7 1 1.0030 0.5222 0.1562 11.00000 0.05 0.60 Q8 1 1.0254 0.4074 0.0988 11.00000 0.05 0.56 Q9 1 0.6920 0.7996 -0.1519 11.00000 0.05 0.56 Q10 1 0.6983 0.0126 0.1425 11.00000 0.05 0.55 Q11 1 0.6738 0.0166 0.1845 11.00000 0.05 0.53 Q12 1 0.7570 0.2363 0.0001 11.00000 0.05 0.46 Q13 1 0.6779 0.5818 -0.0312 11.00000 0.05 0.42 Q14 1 0.8555 0.8895 -0.1170 11.00000 0.05 0.41 Q15 1 0.7207 0.2376 -0.1037 11.00000 0.05 0.41 Q16 1 0.6480 0.5035 0.0539 11.00000 0.05 0.41 Q17 1 1.0039 0.4406 0.1381 11.00000 0.05 0.39 Q18 1 0.1827 0.5033 0.2898 11.00000 0.05 0.39 Q19 1 0.6720 0.4632 -0.0324 11.00000 0.05 0.39 Q20 1 0.7013 0.3589 -0.0356 11.00000 0.05 0.38 ; _database_code_depnum_ccdc_archive 'CCDC 910747'