# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2004 data_global _journal_coden_Cambridge 1145 loop_ _publ_author_name 'Michael J. Cook' 'Aurelien Auger' 'Paul M. Burnham' 'Isabelle Chambrier' 'David L. Hughes' _publ_contact_author_name 'Dr Michael J Cook' _publ_contact_author_address ; Wolfson Materials and Catalysis Centre University of East Anglia School of Chemical Sciences Norwich NR4 7TJ UNITED KINGDOM ; _publ_contact_author_email M.COOK@UEA.AC.UK _publ_requested_journal 'Journal of Materials Chemistry' _publ_section_title ; X-Ray crystallographic studies of three substituted indium(III) phthalocyanines: effect of ring substitution and the axial ligand on molecular geometry and packing ; data_paulb _database_code_depnum_ccdc_archive 'CCDC 248916' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common 'Compound 1' _chemical_formula_moiety 'C80 H112 Cl In N8' _chemical_formula_structural '[InCl(octa-hexyl-phthal)]' _chemical_formula_analytical ? _chemical_formula_sum 'C80 H112 Cl In N8' _chemical_formula_weight 1336.05 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 29.331(2) _cell_length_b 12.1280(10) _cell_length_c 41.706(3) _cell_angle_alpha 90.00 _cell_angle_beta 108.896(2) _cell_angle_gamma 90.00 _cell_volume 14036.4(18) _cell_formula_units_Z 8 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'very fine, long needles' _exptl_crystal_colour 'dark blue' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.264 _exptl_crystal_density_method ? _exptl_crystal_F_000 5712 _exptl_absorpt_coefficient_mu 0.425 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.945 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'SADABS, (Sheldrick et al, 1977)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Bruker Smart APEX CCD' _diffrn_measurement_method 'CCD detector' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 76057 _diffrn_reflns_av_R_equivalents 0.0320 _diffrn_reflns_av_sigmaI/netI 0.0325 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 49 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 25.03 _reflns_number_total 12398 _reflns_number_observed 11232 _reflns_observed_criterion I>2sigma(I) _computing_data_collection 'SMART (Sparks, 1993)' _computing_cell_refinement 'SMART (Sparks, 1993)' _computing_data_reduction 'SAINT (Sparks, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0616P)^2^+58.3135P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12398 _refine_ls_number_parameters 807 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0640 _refine_ls_R_factor_gt 0.0577 _refine_ls_wR_factor_ref 0.1432 _refine_ls_wR_factor_gt 0.1393 _refine_ls_goodness_of_fit_ref 1.164 _refine_ls_restrained_S_all 1.164 _refine_ls_shift/su_max 0.070 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group In In 0.604362(9) 0.33368(2) 0.561520(6) 0.02081(10) Uani 1 1 d . . . Cl Cl 0.66008(3) 0.20521(8) 0.55390(3) 0.0294(2) Uani 1 1 d . . . N1 N 0.53455(11) 0.2590(3) 0.54438(8) 0.0232(7) Uani 1 1 d . . . C2 C 0.50779(13) 0.2516(3) 0.51080(9) 0.0218(8) Uani 1 1 d . . . C3 C 0.47478(13) 0.1578(3) 0.50611(10) 0.0220(8) Uani 1 1 d . . . C4 C 0.44202(13) 0.1125(3) 0.47690(9) 0.0214(8) Uani 1 1 d . . . C5 C 0.41820(13) 0.0188(3) 0.48210(10) 0.0254(8) Uani 1 1 d . . . H5 H 0.3968 -0.0161 0.4634 0.031 Uiso 1 1 calc R . . C6 C 0.42479(14) -0.0250(3) 0.51388(10) 0.0261(8) Uani 1 1 d . . . H6 H 0.4075 -0.0879 0.5156 0.031 Uiso 1 1 calc R . . C7 C 0.45610(13) 0.0207(3) 0.54343(10) 0.0229(8) Uani 1 1 d . . . C8 C 0.48187(13) 0.1134(3) 0.53869(9) 0.0218(8) Uani 1 1 d . . . C9 C 0.52003(13) 0.1800(3) 0.56251(9) 0.0215(8) Uani 1 1 d . . . N10 N 0.53615(11) 0.1646(3) 0.59589(8) 0.0245(7) Uani 1 1 d . . . N11 N 0.59927(11) 0.3044(3) 0.61064(8) 0.0226(7) Uani 1 1 d . . . C12 C 0.57094(13) 0.2241(3) 0.61802(10) 0.0234(8) Uani 1 1 d . . . C13 C 0.58522(14) 0.2120(3) 0.65475(10) 0.0255(8) Uani 1 1 d . . . C14 C 0.56806(15) 0.1427(3) 0.67545(10) 0.0302(9) Uani 1 1 d . . . C15 C 0.59192(17) 0.1526(4) 0.71005(11) 0.0378(10) Uani 1 1 d . . . H15 H 0.5832 0.1059 0.7247 0.045 Uiso 1 1 calc R . . C16 C 0.62818(16) 0.2292(4) 0.72366(11) 0.0363(10) Uani 1 1 d . . . H16 H 0.6424 0.2321 0.7471 0.044 Uiso 1 1 calc R . . C17 C 0.64423(15) 0.3018(3) 0.70390(10) 0.0297(9) Uani 1 1 d . . . C18 C 0.62252(14) 0.2887(3) 0.66868(10) 0.0261(8) Uani 1 1 d . . . C19 C 0.63085(13) 0.3457(3) 0.64018(10) 0.0239(8) Uani 1 1 d . . . N20 N 0.66327(11) 0.4262(2) 0.64328(8) 0.0230(7) Uani 1 1 d . . . N21 N 0.64101(11) 0.4807(2) 0.58430(8) 0.0213(7) Uani 1 1 d . . . C22 C 0.66743(13) 0.4891(3) 0.61811(10) 0.0237(8) Uani 1 1 d . . . C23 C 0.69830(13) 0.5865(3) 0.62259(10) 0.0252(8) Uani 1 1 d . . . C24 C 0.73350(14) 0.6307(3) 0.65139(10) 0.0296(9) Uani 1 1 d . . . C25 C 0.75363(15) 0.7294(3) 0.64610(11) 0.0346(10) Uani 1 1 d . . . H25 H 0.7769 0.7618 0.6644 0.041 Uiso 1 1 calc R . . C26 C 0.74097(15) 0.7829(3) 0.61497(11) 0.0329(9) Uani 1 1 d . . . H26 H 0.7553 0.8501 0.6134 0.039 Uiso 1 1 calc R . . C27 C 0.70746(14) 0.7390(3) 0.58595(10) 0.0270(8) Uani 1 1 d . . . C28 C 0.68702(13) 0.6380(3) 0.59069(10) 0.0234(8) Uani 1 1 d . . . C29 C 0.65089(13) 0.5677(3) 0.56680(10) 0.0235(8) Uani 1 1 d . . . N30 N 0.63200(10) 0.5889(2) 0.53372(8) 0.0217(7) Uani 1 1 d . . . N31 N 0.57516(10) 0.4367(2) 0.51830(8) 0.0213(7) Uani 1 1 d . . . C32 C 0.59721(13) 0.5307(3) 0.51166(10) 0.0235(8) Uani 1 1 d . . . C33 C 0.57525(13) 0.5593(3) 0.47574(9) 0.0228(8) Uani 1 1 d . . . C34 C 0.58585(14) 0.6425(3) 0.45590(10) 0.0254(8) Uani 1 1 d . . . C35 C 0.55706(15) 0.6435(3) 0.42221(10) 0.0303(9) Uani 1 1 d . . . H35 H 0.5628 0.6967 0.4079 0.036 Uiso 1 1 calc R . . C36 C 0.51978(14) 0.5680(3) 0.40875(10) 0.0302(9) Uani 1 1 d . . . H36 H 0.5012 0.5745 0.3861 0.036 Uiso 1 1 calc R . . C37 C 0.50937(14) 0.4838(3) 0.42775(10) 0.0263(8) Uani 1 1 d . . . C38 C 0.53862(13) 0.4808(3) 0.46188(9) 0.0223(8) Uani 1 1 d . . . C39 C 0.53950(13) 0.4049(3) 0.48934(9) 0.0221(8) Uani 1 1 d . . . N40 N 0.50983(11) 0.3181(2) 0.48573(8) 0.0223(7) Uani 1 1 d . . . C41 C 0.43275(14) 0.1592(3) 0.44188(10) 0.0257(8) Uani 1 1 d . . . H41A H 0.4635 0.1683 0.4381 0.031 Uiso 1 1 calc R . . H41B H 0.4186 0.2319 0.4411 0.031 Uiso 1 1 calc R . . C42 C 0.39991(14) 0.0907(3) 0.41295(10) 0.0265(8) Uani 1 1 d . . . H42A H 0.4140 0.0181 0.4135 0.032 Uiso 1 1 calc R . . H42B H 0.3691 0.0815 0.4165 0.032 Uiso 1 1 calc R . . C43 C 0.39146(15) 0.1412(3) 0.37808(10) 0.0307(9) Uani 1 1 d . . . H43A H 0.4223 0.1538 0.3748 0.037 Uiso 1 1 calc R . . H43B H 0.3756 0.2119 0.3770 0.037 Uiso 1 1 calc R . . C44 C 0.36063(16) 0.0672(4) 0.34975(11) 0.0391(11) Uani 1 1 d . . . H44A H 0.3738 -0.0068 0.3533 0.047 Uiso 1 1 calc R . . H44B H 0.3284 0.0639 0.3513 0.047 Uiso 1 1 calc R . . C45 C 0.35706(18) 0.1038(4) 0.31415(11) 0.0445(12) Uani 1 1 d . . . H45A H 0.3893 0.1163 0.3133 0.053 Uiso 1 1 calc R . . H45B H 0.3427 0.0448 0.2984 0.053 Uiso 1 1 calc R . . C46 C 0.3275(2) 0.2079(5) 0.30272(13) 0.0537(13) Uani 1 1 d . . . H46A H 0.3273 0.2273 0.2803 0.081 Uiso 1 1 calc R . . H46B H 0.3415 0.2669 0.3181 0.081 Uiso 1 1 calc R . . H46C H 0.2951 0.1953 0.3025 0.081 Uiso 1 1 calc R . . C71 C 0.46087(14) -0.0272(3) 0.57787(10) 0.0261(8) Uani 1 1 d . . . H71A H 0.4524 0.0293 0.5914 0.031 Uiso 1 1 calc R . . H71B H 0.4944 -0.0466 0.5891 0.031 Uiso 1 1 calc R . . C72 C 0.42980(15) -0.1288(3) 0.57708(10) 0.0296(9) Uani 1 1 d . . . H72A H 0.3969 -0.1122 0.5634 0.035 Uiso 1 1 calc R . . H72B H 0.4410 -0.1884 0.5660 0.035 Uiso 1 1 calc R . . C73 C 0.42998(16) -0.1679(4) 0.61154(11) 0.0382(10) Uani 1 1 d . . . H73A H 0.4151 -0.1125 0.6216 0.046 Uiso 1 1 calc R . . H73B H 0.4630 -0.1775 0.6262 0.046 Uiso 1 1 calc R . . C74 C 0.40287(17) -0.2769(4) 0.60904(12) 0.0398(11) Uani 1 1 d . . . H74A H 0.3707 -0.2677 0.5930 0.048 Uiso 1 1 calc R . . H74B H 0.4191 -0.3324 0.5999 0.048 Uiso 1 1 calc R . . C75 C 0.39852(19) -0.3195(4) 0.64191(14) 0.0512(13) Uani 1 1 d . . . H75A H 0.3815 -0.2655 0.6509 0.061 Uiso 1 1 calc R . . H75B H 0.4305 -0.3285 0.6582 0.061 Uiso 1 1 calc R . . C76 C 0.3719(2) -0.4293(5) 0.63754(18) 0.0724(19) Uani 1 1 d . . . H76A H 0.3403 -0.4210 0.6213 0.109 Uiso 1 1 calc R . . H76B H 0.3692 -0.4521 0.6589 0.109 Uiso 1 1 calc R . . H76C H 0.3894 -0.4840 0.6297 0.109 Uiso 1 1 calc R . . C141 C 0.52712(16) 0.0626(4) 0.66166(11) 0.0363(10) Uani 1 1 d . . . C142 C 0.4765(3) 0.1308(7) 0.6545(2) 0.049(2) Uiso 0.60 1 d P . . C143 C 0.4706(4) 0.2012(8) 0.6827(2) 0.058(2) Uiso 0.60 1 d P . . C144 C 0.4190(4) 0.2539(9) 0.6722(3) 0.059(2) Uiso 0.60 1 d P . . C145 C 0.4118(4) 0.3193(10) 0.7002(3) 0.072(3) Uiso 0.60 1 d P . . C146 C 0.4457(5) 0.4209(12) 0.7111(3) 0.095(4) Uiso 0.60 1 d P . . C642 C 0.5079(4) 0.0080(9) 0.6846(3) 0.034(2) Uiso 0.40 1 d P . . C643 C 0.4801(5) 0.0907(11) 0.7000(3) 0.049(3) Uiso 0.40 1 d P . . C644 C 0.4392(7) 0.1480(15) 0.6733(5) 0.076(5) Uiso 0.40 1 d P . . C645 C 0.4104(8) 0.2173(19) 0.6926(6) 0.097(6) Uiso 0.40 1 d P . . C646 C 0.3773(9) 0.292(2) 0.6670(6) 0.117(7) Uiso 0.40 1 d P . . C171 C 0.68098(15) 0.3898(4) 0.71916(10) 0.0322(9) Uani 1 1 d . . . H17A H 0.6708 0.4574 0.7065 0.039 Uiso 1 1 calc R . . H17B H 0.7114 0.3679 0.7165 0.039 Uiso 1 1 calc R . . C172 C 0.68939(16) 0.4136(4) 0.75651(10) 0.0341(10) Uani 1 1 d . . . H17C H 0.6585 0.4227 0.7600 0.041 Uiso 1 1 calc R . . H17D H 0.7054 0.3508 0.7699 0.041 Uiso 1 1 calc R . . C173 C 0.71975(16) 0.5165(4) 0.76900(11) 0.0345(10) Uani 1 1 d . . . H17E H 0.7514 0.5055 0.7668 0.041 Uiso 1 1 calc R . . H17F H 0.7048 0.5784 0.7547 0.041 Uiso 1 1 calc R . . C174 C 0.72550(16) 0.5443(4) 0.80557(11) 0.0353(10) Uani 1 1 d . . . H17G H 0.6938 0.5536 0.8077 0.042 Uiso 1 1 calc R . . H17H H 0.7408 0.4826 0.8198 0.042 Uiso 1 1 calc R . . C175 C 0.75478(18) 0.6474(4) 0.81858(11) 0.0406(11) Uani 1 1 d . . . H17I H 0.7396 0.7093 0.8044 0.049 Uiso 1 1 calc R . . H17J H 0.7867 0.6381 0.8167 0.049 Uiso 1 1 calc R . . C176 C 0.7598(2) 0.6738(4) 0.85513(13) 0.0540(14) Uani 1 1 d . . . H17K H 0.7775 0.7413 0.8617 0.081 Uiso 1 1 calc R . . H17L H 0.7767 0.6150 0.8695 0.081 Uiso 1 1 calc R . . H17M H 0.7284 0.6820 0.8573 0.081 Uiso 1 1 calc R . . C241 C 0.75100(18) 0.5745(4) 0.68551(11) 0.0446(12) Uani 1 1 d . . . C242 C 0.7941(3) 0.4925(7) 0.6819(2) 0.0397(18) Uiso 0.60 1 d P . . C243 C 0.8242(3) 0.4489(7) 0.7167(2) 0.0407(18) Uiso 0.60 1 d P . . C244 C 0.8732(5) 0.3885(13) 0.7224(4) 0.041(3) Uiso 0.35 1 d P . . C245 C 0.9112(5) 0.4562(11) 0.7094(3) 0.084(3) Uiso 0.60 1 d P . . C246 C 0.9578(4) 0.3835(10) 0.7224(3) 0.073(3) Uiso 0.60 1 d P . . C742 C 0.7795(4) 0.4801(9) 0.6928(3) 0.033(2) Uiso 0.40 1 d P . . C743 C 0.8279(5) 0.5142(10) 0.6899(3) 0.042(3) Uiso 0.40 1 d P . . C744 C 0.8651(8) 0.4170(19) 0.6991(6) 0.049(5) Uiso 0.25 1 d P . . C944 C 0.8613(6) 0.3619(14) 0.7086(4) 0.055(4) Uiso 0.40 1 d P . . C945 C 0.8967(6) 0.3217(14) 0.7384(4) 0.068(4) Uiso 0.40 1 d P . . C946 C 0.9296(5) 0.2458(12) 0.7297(4) 0.057(3) Uiso 0.40 1 d P . . C271 C 0.69286(14) 0.7965(3) 0.55220(10) 0.0284(9) Uani 1 1 d . . . H27A H 0.6579 0.7961 0.5431 0.034 Uiso 1 1 calc R . . H27B H 0.7046 0.7531 0.5370 0.034 Uiso 1 1 calc R . . C272 C 0.70993(14) 0.9155(3) 0.55134(11) 0.0288(9) Uani 1 1 d . . . H27C H 0.6870 0.9529 0.5323 0.035 Uiso 1 1 calc R . . H27D H 0.7093 0.9524 0.5718 0.035 Uiso 1 1 calc R . . C273 C 0.76000(14) 0.9289(3) 0.54839(11) 0.0309(9) Uani 1 1 d . . . H27E H 0.7630 0.8811 0.5306 0.037 Uiso 1 1 calc R . . H27F H 0.7839 0.9063 0.5695 0.037 Uiso 1 1 calc R . . C274 C 0.76988(15) 1.0477(3) 0.54056(11) 0.0316(9) Uani 1 1 d . . . H27G H 0.7436 1.0730 0.5211 0.038 Uiso 1 1 calc R . . H27H H 0.7705 1.0938 0.5597 0.038 Uiso 1 1 calc R . . C275 C 0.81703(16) 1.0625(4) 0.53317(12) 0.0368(10) Uani 1 1 d . . . H27I H 0.8436 1.0472 0.5537 0.044 Uiso 1 1 calc R . . H27J H 0.8184 1.0090 0.5162 0.044 Uiso 1 1 calc R . . C276 C 0.82326(19) 1.1765(4) 0.52077(13) 0.0493(13) Uani 1 1 d . . . H27K H 0.7999 1.1882 0.4988 0.074 Uiso 1 1 calc R . . H27L H 0.8551 1.1836 0.5192 0.074 Uiso 1 1 calc R . . H27M H 0.8188 1.2304 0.5364 0.074 Uiso 1 1 calc R . . C341 C 0.62606(14) 0.7257(3) 0.46901(10) 0.0276(9) Uani 1 1 d . . . H34A H 0.6549 0.6871 0.4824 0.033 Uiso 1 1 calc R . . H34B H 0.6173 0.7767 0.4840 0.033 Uiso 1 1 calc R . . C342 C 0.63767(14) 0.7915(3) 0.44172(10) 0.0286(9) Uani 1 1 d . . . H34C H 0.6089 0.8303 0.4284 0.034 Uiso 1 1 calc R . . H34D H 0.6464 0.7406 0.4267 0.034 Uiso 1 1 calc R . . C343 C 0.67813(15) 0.8746(3) 0.45509(10) 0.0306(9) Uani 1 1 d . . . H34E H 0.7075 0.8359 0.4675 0.037 Uiso 1 1 calc R . . H34F H 0.6702 0.9240 0.4708 0.037 Uiso 1 1 calc R . . C344 C 0.68707(15) 0.9426(3) 0.42683(11) 0.0313(9) Uani 1 1 d . . . H34G H 0.6981 0.8937 0.4124 0.038 Uiso 1 1 calc R . . H34H H 0.6568 0.9748 0.4130 0.038 Uiso 1 1 calc R . . C345 C 0.72370(16) 1.0338(4) 0.43954(11) 0.0370(10) Uani 1 1 d . . . H34I H 0.7549 1.0014 0.4512 0.044 Uiso 1 1 calc R . . H34J H 0.7145 1.0785 0.4557 0.044 Uiso 1 1 calc R . . C346 C 0.72804(17) 1.1076(4) 0.41109(12) 0.0415(11) Uani 1 1 d . . . H34K H 0.7511 1.1649 0.4205 0.062 Uiso 1 1 calc R . . H34L H 0.6973 1.1398 0.3994 0.062 Uiso 1 1 calc R . . H34M H 0.7386 1.0644 0.3955 0.062 Uiso 1 1 calc R . . C371 C 0.46939(14) 0.4025(3) 0.41275(10) 0.0291(9) Uani 1 1 d . . . H37A H 0.4467 0.4075 0.4252 0.035 Uiso 1 1 calc R . . H37B H 0.4830 0.3289 0.4162 0.035 Uiso 1 1 calc R . . C372 C 0.44173(14) 0.4171(3) 0.37519(10) 0.0298(9) Uani 1 1 d . . . H37C H 0.4353 0.4950 0.3706 0.036 Uiso 1 1 calc R . . H37D H 0.4110 0.3797 0.3700 0.036 Uiso 1 1 calc R . . C373 C 0.4681(2) 0.3729(5) 0.35166(14) 0.0534(14) Uani 1 1 d . . . C374 C 0.4362(3) 0.4226(8) 0.3114(2) 0.0366(17) Uiso 0.60 1 d P . . C375 C 0.4542(4) 0.3667(9) 0.2856(3) 0.061(2) Uiso 0.60 1 d P . . C376 C 0.4256(4) 0.4115(10) 0.2491(3) 0.076(3) Uiso 0.60 1 d P . . C874 C 0.4500(4) 0.3605(10) 0.3186(3) 0.039(3) Uiso 0.40 1 d P . . C875 C 0.4385(5) 0.4798(12) 0.3031(3) 0.045(3) Uiso 0.40 1 d P . . C876 C 0.4813(6) 0.5441(13) 0.3056(4) 0.065(4) Uiso 0.40 1 d P . . 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 In 0.01920(15) 0.01821(15) 0.02291(15) -0.00137(10) 0.00391(10) -0.00127(10) Cl 0.0260(5) 0.0239(5) 0.0390(6) -0.0039(4) 0.0112(4) 0.0009(4) N1 0.0176(15) 0.0226(16) 0.0271(17) -0.0014(13) 0.0043(13) -0.0030(13) C2 0.0189(18) 0.0193(18) 0.027(2) -0.0012(15) 0.0073(15) 0.0023(15) C3 0.0175(18) 0.0195(19) 0.029(2) -0.0014(15) 0.0083(15) 0.0013(14) C4 0.0185(18) 0.0213(19) 0.0241(19) -0.0027(15) 0.0066(15) 0.0014(15) C5 0.0232(19) 0.024(2) 0.027(2) -0.0079(16) 0.0051(16) -0.0040(16) C6 0.025(2) 0.0191(19) 0.035(2) -0.0028(16) 0.0103(17) -0.0025(15) C7 0.0189(18) 0.0200(19) 0.030(2) -0.0002(15) 0.0079(16) 0.0014(15) C8 0.0188(18) 0.0190(18) 0.028(2) -0.0015(15) 0.0080(15) 0.0018(15) C9 0.0192(18) 0.0169(18) 0.0261(19) -0.0012(15) 0.0043(15) 0.0034(14) N10 0.0224(16) 0.0207(16) 0.0282(17) -0.0016(13) 0.0052(14) -0.0014(13) N11 0.0218(16) 0.0221(16) 0.0228(16) -0.0023(13) 0.0057(13) -0.0004(13) C12 0.0223(19) 0.0195(19) 0.028(2) -0.0004(15) 0.0068(16) 0.0027(15) C13 0.026(2) 0.0235(19) 0.0233(19) 0.0010(16) 0.0033(16) 0.0024(16) C14 0.033(2) 0.027(2) 0.028(2) -0.0008(17) 0.0061(18) -0.0011(17) C15 0.048(3) 0.033(2) 0.029(2) 0.0057(18) 0.009(2) -0.005(2) C16 0.042(3) 0.037(3) 0.025(2) 0.0012(18) 0.0038(19) -0.003(2) C17 0.031(2) 0.027(2) 0.027(2) -0.0011(17) 0.0048(17) 0.0018(17) C18 0.025(2) 0.023(2) 0.028(2) -0.0020(16) 0.0055(16) 0.0042(16) C19 0.0238(19) 0.0181(19) 0.027(2) -0.0024(15) 0.0049(16) 0.0028(15) N20 0.0221(16) 0.0195(16) 0.0245(17) -0.0023(13) 0.0034(13) 0.0033(13) N21 0.0209(16) 0.0141(15) 0.0265(17) -0.0042(12) 0.0043(13) -0.0022(12) C22 0.0202(19) 0.0197(19) 0.030(2) -0.0050(16) 0.0056(16) 0.0009(15) C23 0.0197(19) 0.0222(19) 0.032(2) -0.0047(16) 0.0057(16) -0.0001(15) C24 0.027(2) 0.023(2) 0.033(2) -0.0053(17) 0.0025(17) 0.0002(16) C25 0.033(2) 0.031(2) 0.033(2) -0.0098(18) 0.0009(18) -0.0093(18) C26 0.033(2) 0.026(2) 0.037(2) -0.0049(18) 0.0063(19) -0.0096(18) C27 0.023(2) 0.023(2) 0.035(2) -0.0034(17) 0.0095(17) 0.0010(16) C28 0.0197(19) 0.0213(19) 0.029(2) -0.0050(15) 0.0074(16) 0.0009(15) C29 0.0182(18) 0.023(2) 0.030(2) -0.0059(16) 0.0082(16) 0.0009(15) N30 0.0172(15) 0.0204(16) 0.0262(17) -0.0024(13) 0.0053(13) -0.0006(12) N31 0.0175(15) 0.0204(16) 0.0230(16) -0.0009(13) 0.0024(13) -0.0011(12) C32 0.0205(19) 0.0225(19) 0.029(2) -0.0019(16) 0.0095(16) 0.0018(15) C33 0.0203(19) 0.0220(19) 0.026(2) 0.0009(15) 0.0069(15) 0.0035(15) C34 0.025(2) 0.0204(19) 0.031(2) 0.0003(16) 0.0087(17) 0.0009(15) C35 0.032(2) 0.027(2) 0.032(2) 0.0048(17) 0.0101(18) 0.0001(17) C36 0.029(2) 0.029(2) 0.027(2) 0.0037(17) 0.0015(17) -0.0002(17) C37 0.023(2) 0.025(2) 0.029(2) -0.0001(16) 0.0044(16) 0.0011(16) C38 0.0171(18) 0.0214(19) 0.028(2) -0.0009(15) 0.0072(15) 0.0020(14) C39 0.0222(19) 0.0179(18) 0.027(2) 0.0011(15) 0.0086(16) 0.0038(15) N40 0.0190(16) 0.0185(16) 0.0277(17) -0.0021(13) 0.0052(13) -0.0006(12) C41 0.026(2) 0.022(2) 0.028(2) -0.0066(16) 0.0082(16) -0.0024(16) C42 0.027(2) 0.024(2) 0.028(2) -0.0069(16) 0.0076(16) -0.0021(16) C43 0.028(2) 0.032(2) 0.030(2) -0.0051(17) 0.0069(17) -0.0026(17) C44 0.037(2) 0.042(3) 0.034(2) -0.012(2) 0.0040(19) 0.000(2) C45 0.042(3) 0.052(3) 0.032(2) -0.010(2) 0.002(2) 0.006(2) C46 0.053(3) 0.058(3) 0.043(3) -0.003(2) 0.006(2) 0.011(3) C71 0.025(2) 0.022(2) 0.030(2) -0.0013(16) 0.0085(17) -0.0005(16) C72 0.027(2) 0.025(2) 0.034(2) 0.0025(17) 0.0057(17) -0.0039(17) C73 0.035(2) 0.036(2) 0.038(2) 0.009(2) 0.004(2) -0.0019(19) C74 0.037(2) 0.034(2) 0.044(3) 0.013(2) 0.008(2) -0.003(2) C75 0.045(3) 0.057(3) 0.057(3) 0.020(3) 0.024(3) 0.005(2) C76 0.083(4) 0.056(4) 0.096(5) 0.029(3) 0.055(4) 0.000(3) C141 0.033(2) 0.033(2) 0.037(2) 0.0081(19) 0.0048(19) -0.0088(19) C171 0.034(2) 0.032(2) 0.026(2) -0.0008(17) 0.0036(18) -0.0019(18) C172 0.037(2) 0.033(2) 0.028(2) -0.0016(18) 0.0056(18) -0.0025(19) C173 0.037(2) 0.033(2) 0.031(2) -0.0010(18) 0.0072(19) -0.0031(19) C174 0.040(2) 0.033(2) 0.030(2) -0.0028(18) 0.0080(19) -0.0044(19) C175 0.047(3) 0.036(3) 0.037(3) -0.004(2) 0.011(2) -0.008(2) C176 0.065(4) 0.054(3) 0.041(3) -0.019(2) 0.015(3) -0.021(3) C241 0.050(3) 0.031(2) 0.033(2) 0.0012(19) -0.013(2) -0.003(2) C271 0.026(2) 0.026(2) 0.034(2) -0.0035(17) 0.0108(17) -0.0057(16) C272 0.029(2) 0.023(2) 0.036(2) 0.0003(17) 0.0132(18) 0.0003(16) C273 0.027(2) 0.025(2) 0.043(2) -0.0024(18) 0.0135(18) -0.0017(17) C274 0.030(2) 0.026(2) 0.040(2) -0.0066(18) 0.0125(19) -0.0034(17) C275 0.036(2) 0.034(2) 0.047(3) -0.006(2) 0.022(2) -0.0073(19) C276 0.052(3) 0.052(3) 0.048(3) 0.001(2) 0.022(2) -0.021(2) C341 0.025(2) 0.023(2) 0.033(2) 0.0014(16) 0.0075(17) -0.0016(16) C342 0.027(2) 0.025(2) 0.033(2) 0.0025(17) 0.0084(17) -0.0012(17) C343 0.030(2) 0.028(2) 0.034(2) -0.0003(18) 0.0113(18) -0.0023(17) C344 0.032(2) 0.028(2) 0.035(2) -0.0010(18) 0.0134(18) -0.0041(17) C345 0.036(2) 0.035(2) 0.041(3) -0.002(2) 0.014(2) -0.0099(19) C346 0.042(3) 0.030(2) 0.055(3) 0.002(2) 0.020(2) -0.008(2) C371 0.023(2) 0.027(2) 0.033(2) 0.0002(17) 0.0026(17) -0.0011(16) C372 0.028(2) 0.028(2) 0.032(2) -0.0053(17) 0.0066(17) -0.0032(17) C373 0.063(3) 0.052(3) 0.057(3) -0.024(3) 0.037(3) -0.011(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag In N11 2.132(3) . ? In N31 2.132(3) . ? In N1 2.139(3) . ? In N21 2.140(3) . ? In Cl 2.3528(10) . ? N1 C2 1.368(5) . ? N1 C9 1.371(5) . ? C2 N40 1.337(5) . ? C2 C3 1.465(5) . ? C3 C4 1.397(5) . ? C3 C8 1.413(5) . ? C4 C5 1.388(5) . ? C4 C41 1.507(5) . ? C5 C6 1.382(6) . ? C5 H5 0.9300 . ? C6 C7 1.392(5) . ? C6 H6 0.9300 . ? C7 C8 1.403(5) . ? C7 C71 1.513(5) . ? C8 C9 1.474(5) . ? C9 N10 1.331(5) . ? N10 C12 1.343(5) . ? N11 C19 1.374(5) . ? N11 C12 1.378(5) . ? C12 C13 1.459(5) . ? C13 C18 1.410(5) . ? C13 C14 1.410(6) . ? C14 C15 1.390(6) . ? C14 C141 1.506(6) . ? C15 C16 1.387(6) . ? C15 H15 0.9300 . ? C16 C17 1.388(6) . ? C16 H16 0.9300 . ? C17 C18 1.408(5) . ? C17 C171 1.503(6) . ? C18 C19 1.463(6) . ? C19 N20 1.339(5) . ? N20 C22 1.335(5) . ? N21 C29 1.366(5) . ? N21 C22 1.375(5) . ? C22 C23 1.463(5) . ? C23 C28 1.409(5) . ? C23 C24 1.411(5) . ? C24 C25 1.384(6) . ? C24 C241 1.510(6) . ? C25 C26 1.389(6) . ? C25 H25 0.9300 . ? C26 C27 1.394(6) . ? C26 H26 0.9300 . ? C27 C28 1.405(5) . ? C27 C271 1.504(6) . ? C28 C29 1.469(5) . ? C29 N30 1.334(5) . ? N30 C32 1.333(5) . ? N31 C39 1.373(5) . ? N31 C32 1.382(5) . ? C32 C33 1.468(5) . ? C33 C34 1.402(5) . ? C33 C38 1.412(5) . ? C34 C35 1.385(6) . ? C34 C341 1.513(5) . ? C35 C36 1.397(6) . ? C35 H35 0.9300 . ? C36 C37 1.386(6) . ? C36 H36 0.9300 . ? C37 C38 1.404(5) . ? C37 C371 1.504(5) . ? C38 C39 1.463(5) . ? C39 N40 1.343(5) . ? C41 C42 1.524(5) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C43 1.522(6) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 C44 1.525(6) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 C45 1.521(6) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 C46 1.518(7) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C71 C72 1.527(5) . ? C71 H71A 0.9700 . ? C71 H71B 0.9700 . ? C72 C73 1.512(6) . ? C72 H72A 0.9700 . ? C72 H72B 0.9700 . ? C73 C74 1.528(6) . ? C73 H73A 0.9700 . ? C73 H73B 0.9700 . ? C74 C75 1.509(6) . ? C74 H74A 0.9700 . ? C74 H74B 0.9700 . ? C75 C76 1.525(8) . ? C75 H75A 0.9700 . ? C75 H75B 0.9700 . ? C76 H76A 0.9600 . ? C76 H76B 0.9600 . ? C76 H76C 0.9600 . ? C141 C642 1.421(12) . ? C141 C142 1.639(10) . ? C142 C143 1.507(13) . ? C142 C644 1.554(19) . ? C142 C643 1.928(16) . ? C142 C642 1.972(14) . ? C143 C644 1.089(19) . ? C143 C643 1.503(16) . ? C143 C144 1.569(14) . ? C143 C645 1.95(2) . ? C144 C645 1.06(2) . ? C144 C646 1.26(3) . ? C144 C644 1.41(2) . ? C144 C145 1.483(15) . ? C145 C645 1.27(2) . ? C145 C646 1.46(3) . ? C145 C146 1.556(17) . ? C642 C643 1.559(17) . ? C643 C644 1.51(2) . ? C644 C645 1.58(3) . ? C645 C646 1.50(3) . ? C171 C172 1.524(6) . ? C171 H17A 0.9700 . ? C171 H17B 0.9700 . ? C172 C173 1.524(6) . ? C172 H17C 0.9700 . ? C172 H17D 0.9700 . ? C173 C174 1.517(6) . ? C173 H17E 0.9700 . ? C173 H17F 0.9700 . ? C174 C175 1.514(6) . ? C174 H17G 0.9700 . ? C174 H17H 0.9700 . ? C175 C176 1.518(6) . ? C175 H17I 0.9700 . ? C175 H17J 0.9700 . ? C176 H17K 0.9600 . ? C176 H17L 0.9600 . ? C176 H17M 0.9600 . ? C241 C742 1.392(12) . ? C241 C242 1.653(10) . ? C242 C742 0.732(11) . ? C242 C743 0.975(13) . ? C242 C243 1.527(11) . ? C243 C743 1.403(14) . ? C243 C742 1.417(13) . ? C243 C244 1.563(16) . ? C243 C944 1.628(17) . ? C243 C744 1.64(2) . ? C244 C944 0.652(18) . ? C244 C744 0.98(3) . ? C244 C945 1.13(2) . ? C244 C245 1.612(19) . ? C245 C744 1.37(2) . ? C245 C246 1.566(16) . ? C245 C944 1.85(2) . ? C246 C946 1.929(18) . ? C742 C743 1.521(16) . ? C743 C744 1.57(2) . ? C744 C944 0.80(2) . ? C744 C945 1.97(3) . ? C944 C945 1.42(2) . ? C945 C946 1.46(2) . ? C271 C272 1.532(5) . ? C271 H27A 0.9700 . ? C271 H27B 0.9700 . ? C272 C273 1.522(5) . ? C272 H27C 0.9700 . ? C272 H27D 0.9700 . ? C273 C274 1.525(6) . ? C273 H27E 0.9700 . ? C273 H27F 0.9700 . ? C274 C275 1.522(6) . ? C274 H27G 0.9700 . ? C274 H27H 0.9700 . ? C275 C276 1.509(6) . ? C275 H27I 0.9700 . ? C275 H27J 0.9700 . ? C276 H27K 0.9600 . ? C276 H27L 0.9600 . ? C276 H27M 0.9600 . ? C341 C342 1.516(5) . ? C341 H34A 0.9700 . ? C341 H34B 0.9700 . ? C342 C343 1.519(6) . ? C342 H34C 0.9700 . ? C342 H34D 0.9700 . ? C343 C344 1.529(6) . ? C343 H34E 0.9700 . ? C343 H34F 0.9700 . ? C344 C345 1.513(6) . ? C344 H34G 0.9700 . ? C344 H34H 0.9700 . ? C345 C346 1.524(6) . ? C345 H34I 0.9700 . ? C345 H34J 0.9700 . ? C346 H34K 0.9600 . ? C346 H34L 0.9600 . ? C346 H34M 0.9600 . ? C371 C372 1.523(5) . ? C371 H37A 0.9700 . ? C371 H37B 0.9700 . ? C372 C373 1.531(6) . ? C372 H37C 0.9700 . ? C372 H37D 0.9700 . ? C373 C874 1.314(12) . ? C373 C374 1.746(10) . ? C374 C875 0.785(13) . ? C374 C874 0.863(12) . ? C374 C375 1.505(12) . ? C375 C874 1.427(15) . ? C375 C376 1.576(15) . ? C375 C875 1.689(16) . ? C874 C875 1.576(17) . ? C875 C876 1.45(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N11 In N31 140.91(12) . . ? N11 In N1 83.87(12) . . ? N31 In N1 83.50(12) . . ? N11 In N21 83.89(12) . . ? N31 In N21 83.86(11) . . ? N1 In N21 142.22(12) . . ? N11 In Cl 106.71(9) . . ? N31 In Cl 112.37(9) . . ? N1 In Cl 107.81(9) . . ? N21 In Cl 109.94(8) . . ? C2 N1 C9 109.9(3) . . ? C2 N1 In 122.6(2) . . ? C9 N1 In 123.1(2) . . ? N40 C2 N1 127.2(3) . . ? N40 C2 C3 124.0(3) . . ? N1 C2 C3 108.8(3) . . ? C4 C3 C8 122.3(3) . . ? C4 C3 C2 131.3(3) . . ? C8 C3 C2 106.4(3) . . ? C5 C4 C3 115.1(3) . . ? C5 C4 C41 121.2(3) . . ? C3 C4 C41 123.7(3) . . ? C6 C5 C4 122.9(4) . . ? C6 C5 H5 118.5 . . ? C4 C5 H5 118.5 . . ? C5 C6 C7 122.9(4) . . ? C5 C6 H6 118.6 . . ? C7 C6 H6 118.6 . . ? C6 C7 C8 115.2(3) . . ? C6 C7 C71 121.3(3) . . ? C8 C7 C71 123.5(3) . . ? C7 C8 C3 121.5(3) . . ? C7 C8 C9 132.1(3) . . ? C3 C8 C9 106.4(3) . . ? N10 C9 N1 127.3(3) . . ? N10 C9 C8 124.3(3) . . ? N1 C9 C8 108.4(3) . . ? C9 N10 C12 125.3(3) . . ? C19 N11 C12 109.7(3) . . ? C19 N11 In 124.4(3) . . ? C12 N11 In 124.6(2) . . ? N10 C12 N11 127.2(3) . . ? N10 C12 C13 124.3(3) . . ? N11 C12 C13 108.5(3) . . ? C18 C13 C14 121.6(4) . . ? C18 C13 C12 106.7(3) . . ? C14 C13 C12 131.7(4) . . ? C15 C14 C13 115.1(4) . . ? C15 C14 C141 121.6(4) . . ? C13 C14 C141 123.3(4) . . ? C16 C15 C14 123.0(4) . . ? C16 C15 H15 118.5 . . ? C14 C15 H15 118.5 . . ? C15 C16 C17 123.0(4) . . ? C15 C16 H16 118.5 . . ? C17 C16 H16 118.5 . . ? C16 C17 C18 114.9(4) . . ? C16 C17 C171 122.2(4) . . ? C18 C17 C171 122.8(4) . . ? C17 C18 C13 122.2(4) . . ? C17 C18 C19 131.0(4) . . ? C13 C18 C19 106.8(3) . . ? N20 C19 N11 127.1(3) . . ? N20 C19 C18 124.5(3) . . ? N11 C19 C18 108.3(3) . . ? C22 N20 C19 125.7(3) . . ? C29 N21 C22 110.1(3) . . ? C29 N21 In 124.7(2) . . ? C22 N21 In 123.5(2) . . ? N20 C22 N21 126.8(3) . . ? N20 C22 C23 124.9(3) . . ? N21 C22 C23 108.1(3) . . ? C28 C23 C24 121.3(4) . . ? C28 C23 C22 106.9(3) . . ? C24 C23 C22 131.8(4) . . ? C25 C24 C23 115.1(4) . . ? C25 C24 C241 120.5(4) . . ? C23 C24 C241 124.2(4) . . ? C24 C25 C26 123.6(4) . . ? C24 C25 H25 118.2 . . ? C26 C25 H25 118.2 . . ? C25 C26 C27 122.2(4) . . ? C25 C26 H26 118.9 . . ? C27 C26 H26 118.9 . . ? C26 C27 C28 115.0(4) . . ? C26 C27 C271 122.9(4) . . ? C28 C27 C271 122.1(3) . . ? C27 C28 C23 122.6(3) . . ? C27 C28 C29 131.1(4) . . ? C23 C28 C29 106.3(3) . . ? N30 C29 N21 127.7(3) . . ? N30 C29 C28 123.8(3) . . ? N21 C29 C28 108.5(3) . . ? C32 N30 C29 125.5(3) . . ? C39 N31 C32 109.2(3) . . ? C39 N31 In 124.2(2) . . ? C32 N31 In 124.6(2) . . ? N30 C32 N31 127.0(3) . . ? N30 C32 C33 124.4(3) . . ? N31 C32 C33 108.7(3) . . ? C34 C33 C38 121.9(3) . . ? C34 C33 C32 131.6(4) . . ? C38 C33 C32 106.4(3) . . ? C35 C34 C33 115.2(4) . . ? C35 C34 C341 120.6(4) . . ? C33 C34 C341 124.2(3) . . ? C34 C35 C36 122.8(4) . . ? C34 C35 H35 118.6 . . ? C36 C35 H35 118.6 . . ? C37 C36 C35 122.8(4) . . ? C37 C36 H36 118.6 . . ? C35 C36 H36 118.6 . . ? C36 C37 C38 115.0(4) . . ? C36 C37 C371 122.1(4) . . ? C38 C37 C371 122.9(3) . . ? C37 C38 C33 122.1(3) . . ? C37 C38 C39 131.3(3) . . ? C33 C38 C39 106.6(3) . . ? N40 C39 N31 126.9(3) . . ? N40 C39 C38 124.0(3) . . ? N31 C39 C38 109.1(3) . . ? C2 N40 C39 125.2(3) . . ? C4 C41 C42 115.6(3) . . ? C4 C41 H41A 108.4 . . ? C42 C41 H41A 108.4 . . ? C4 C41 H41B 108.4 . . ? C42 C41 H41B 108.4 . . ? H41A C41 H41B 107.4 . . ? C43 C42 C41 113.8(3) . . ? C43 C42 H42A 108.8 . . ? C41 C42 H42A 108.8 . . ? C43 C42 H42B 108.8 . . ? C41 C42 H42B 108.8 . . ? H42A C42 H42B 107.7 . . ? C42 C43 C44 112.1(4) . . ? C42 C43 H43A 109.2 . . ? C44 C43 H43A 109.2 . . ? C42 C43 H43B 109.2 . . ? C44 C43 H43B 109.2 . . ? H43A C43 H43B 107.9 . . ? C45 C44 C43 114.9(4) . . ? C45 C44 H44A 108.5 . . ? C43 C44 H44A 108.5 . . ? C45 C44 H44B 108.5 . . ? C43 C44 H44B 108.5 . . ? H44A C44 H44B 107.5 . . ? C46 C45 C44 113.7(4) . . ? C46 C45 H45A 108.8 . . ? C44 C45 H45A 108.8 . . ? C46 C45 H45B 108.8 . . ? C44 C45 H45B 108.8 . . ? H45A C45 H45B 107.7 . . ? 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 . . ? C7 C71 C72 114.7(3) . . ? C7 C71 H71A 108.6 . . ? C72 C71 H71A 108.6 . . ? C7 C71 H71B 108.6 . . ? C72 C71 H71B 108.6 . . ? H71A C71 H71B 107.6 . . ? C73 C72 C71 114.5(3) . . ? C73 C72 H72A 108.6 . . ? C71 C72 H72A 108.6 . . ? C73 C72 H72B 108.6 . . ? C71 C72 H72B 108.6 . . ? H72A C72 H72B 107.6 . . ? C72 C73 C74 111.4(4) . . ? C72 C73 H73A 109.3 . . ? C74 C73 H73A 109.3 . . ? C72 C73 H73B 109.3 . . ? C74 C73 H73B 109.3 . . ? H73A C73 H73B 108.0 . . ? C75 C74 C73 115.4(4) . . ? C75 C74 H74A 108.4 . . ? C73 C74 H74A 108.4 . . ? C75 C74 H74B 108.4 . . ? C73 C74 H74B 108.4 . . ? H74A C74 H74B 107.5 . . ? C74 C75 C76 112.4(5) . . ? C74 C75 H75A 109.1 . . ? C76 C75 H75A 109.1 . . ? C74 C75 H75B 109.1 . . ? C76 C75 H75B 109.1 . . ? H75A C75 H75B 107.9 . . ? C75 C76 H76A 109.5 . . ? C75 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C75 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C642 C141 C14 119.0(6) . . ? C642 C141 C142 79.9(6) . . ? C14 C141 C142 107.9(4) . . ? C143 C142 C644 41.6(7) . . ? C143 C142 C141 118.0(7) . . ? C644 C142 C141 136.1(9) . . ? C143 C142 C643 50.1(6) . . ? C644 C142 C643 50.2(8) . . ? C141 C142 C643 86.4(6) . . ? C143 C142 C642 94.6(7) . . ? C644 C142 C642 92.3(9) . . ? C141 C142 C642 45.2(4) . . ? C643 C142 C642 47.1(5) . . ? C644 C143 C643 69.4(12) . . ? C644 C143 C142 71.5(11) . . ? C643 C143 C142 79.6(8) . . ? C644 C143 C144 60.9(11) . . ? C643 C143 C144 120.6(9) . . ? C142 C143 C144 110.8(8) . . ? C644 C143 C645 54.3(12) . . ? C643 C143 C645 91.5(10) . . ? C142 C143 C645 124.2(10) . . ? C144 C143 C645 32.9(7) . . ? C645 C144 C646 79.7(17) . . ? C645 C144 C644 78.3(16) . . ? C646 C144 C644 135.8(17) . . ? C645 C144 C145 57.3(13) . . ? C646 C144 C145 63.8(13) . . ? C644 C144 C145 128.8(11) . . ? C645 C144 C143 93.5(15) . . ? C646 C144 C143 173.2(15) . . ? C644 C144 C143 42.5(8) . . ? C145 C144 C143 111.5(9) . . ? C645 C145 C646 65.9(15) . . ? C645 C145 C144 44.5(11) . . ? C646 C145 C144 50.7(11) . . ? C645 C145 C146 143.9(15) . . ? C646 C145 C146 129.5(14) . . ? C144 C145 C146 114.5(10) . . ? C141 C642 C643 110.6(9) . . ? C141 C642 C142 54.9(5) . . ? C643 C642 C142 65.0(7) . . ? C143 C643 C644 42.3(8) . . ? C143 C643 C642 114.5(10) . . ? C644 C643 C642 112.8(11) . . ? C143 C643 C142 50.3(6) . . ? C644 C643 C142 52.0(8) . . ? C642 C643 C142 67.9(7) . . ? C143 C644 C144 76.7(13) . . ? C143 C644 C643 68.3(12) . . ? C144 C644 C643 131.9(15) . . ? C143 C644 C142 66.9(11) . . ? C144 C644 C142 117.5(13) . . ? C643 C644 C142 77.9(10) . . ? C143 C644 C645 91.8(15) . . ? C144 C644 C645 41.1(10) . . ? C643 C644 C645 107.2(14) . . ? C142 C644 C645 155.0(16) . . ? C144 C645 C145 78.2(17) . . ? C144 C645 C646 56.0(15) . . ? C145 C645 C646 63.1(15) . . ? C144 C645 C644 60.6(14) . . ? C145 C645 C644 131.4(19) . . ? C646 C645 C644 106.9(18) . . ? C144 C645 C143 53.5(12) . . ? C145 C645 C143 101.0(15) . . ? C646 C645 C143 109.5(17) . . ? C644 C645 C143 33.9(8) . . ? C144 C646 C145 65.5(14) . . ? C144 C646 C645 44.3(12) . . ? C145 C646 C645 51.0(12) . . ? C17 C171 C172 115.1(4) . . ? C17 C171 H17A 108.5 . . ? C172 C171 H17A 108.5 . . ? C17 C171 H17B 108.5 . . ? C172 C171 H17B 108.5 . . ? H17A C171 H17B 107.5 . . ? C173 C172 C171 112.8(4) . . ? C173 C172 H17C 109.0 . . ? C171 C172 H17C 109.0 . . ? C173 C172 H17D 109.0 . . ? C171 C172 H17D 109.0 . . ? H17C C172 H17D 107.8 . . ? C174 C173 C172 112.9(4) . . ? C174 C173 H17E 109.0 . . ? C172 C173 H17E 109.0 . . ? C174 C173 H17F 109.0 . . ? C172 C173 H17F 109.0 . . ? H17E C173 H17F 107.8 . . ? C175 C174 C173 114.2(4) . . ? C175 C174 H17G 108.7 . . ? C173 C174 H17G 108.7 . . ? C175 C174 H17H 108.7 . . ? C173 C174 H17H 108.7 . . ? H17G C174 H17H 107.6 . . ? C174 C175 C176 113.2(4) . . ? C174 C175 H17I 108.9 . . ? C176 C175 H17I 108.9 . . ? C174 C175 H17J 108.9 . . ? C176 C175 H17J 108.9 . . ? H17I C175 H17J 107.8 . . ? C175 C176 H17K 109.5 . . ? C175 C176 H17L 109.5 . . ? H17K C176 H17L 109.5 . . ? C175 C176 H17M 109.5 . . ? H17K C176 H17M 109.5 . . ? H17L C176 H17M 109.5 . . ? C742 C241 C24 125.0(6) . . ? C742 C241 C242 26.1(5) . . ? C24 C241 C242 102.9(5) . . ? C742 C242 C743 125.4(16) . . ? C742 C242 C243 67.4(12) . . ? C743 C242 C243 63.8(9) . . ? C742 C242 C241 56.6(11) . . ? C743 C242 C241 122.0(10) . . ? C243 C242 C241 110.2(6) . . ? C743 C243 C742 65.3(7) . . ? C743 C243 C242 38.6(6) . . ? C742 C243 C242 28.5(5) . . ? C743 C243 C244 94.6(9) . . ? C742 C243 C244 145.9(10) . . ? C242 C243 C244 121.8(8) . . ? C743 C243 C944 88.3(9) . . ? C742 C243 C944 123.8(9) . . ? C242 C243 C944 104.3(8) . . ? C244 C243 C944 23.5(7) . . ? C743 C243 C744 61.3(10) . . ? C742 C243 C744 113.1(11) . . ? C242 C243 C744 86.5(9) . . ? C244 C243 C744 35.7(9) . . ? C944 C243 C744 28.4(8) . . ? C944 C244 C744 54(2) . . ? C944 C244 C945 103(3) . . ? C744 C244 C945 138(2) . . ? C944 C244 C243 84(2) . . ? C744 C244 C243 76.5(16) . . ? C945 C244 C243 141.3(15) . . ? C944 C244 C245 101(2) . . ? C744 C244 C245 57.6(16) . . ? C945 C244 C245 102.0(14) . . ? C243 C244 C245 114.4(11) . . ? C744 C245 C246 125.2(14) . . ? C744 C245 C244 37.5(11) . . ? C246 C245 C244 102.5(10) . . ? C744 C245 C944 23.3(11) . . ? C246 C245 C944 104.7(10) . . ? C244 C245 C944 20.3(7) . . ? C245 C246 C946 99.9(9) . . ? C242 C742 C241 97.3(13) . . ? C242 C742 C243 84.1(13) . . ? C241 C742 C243 136.6(9) . . ? C242 C742 C743 31.5(10) . . ? C241 C742 C743 105.6(9) . . ? C243 C742 C743 56.9(7) . . ? C242 C743 C243 77.6(10) . . ? C242 C743 C742 23.1(7) . . ? C243 C743 C742 57.8(7) . . ? C242 C743 C744 115.5(14) . . ? C243 C743 C744 66.9(10) . . ? C742 C743 C744 111.6(12) . . ? C944 C744 C244 41.3(17) . . ? C944 C744 C245 114(3) . . ? C244 C744 C245 84.9(19) . . ? C944 C744 C743 124(3) . . ? C244 C744 C743 116(2) . . ? C245 C744 C743 110.8(17) . . ? C944 C744 C243 75(2) . . ? C244 C744 C243 67.8(15) . . ? C245 C744 C243 124.8(16) . . ? C743 C744 C243 51.8(8) . . ? C944 C744 C945 37.4(19) . . ? C244 C744 C945 22.6(12) . . ? C245 C744 C945 77.9(12) . . ? C743 C744 C945 138.4(15) . . ? C243 C744 C945 89.0(12) . . ? C244 C944 C744 84(3) . . ? C244 C944 C945 51(2) . . ? C744 C944 C945 123(3) . . ? C244 C944 C243 73(2) . . ? C744 C944 C243 77(2) . . ? C945 C944 C243 113.0(13) . . ? C244 C944 C245 59(2) . . ? C744 C944 C245 42.3(19) . . ? C945 C944 C245 81.2(11) . . ? C243 C944 C245 100.1(10) . . ? C244 C945 C944 26.6(10) . . ? C244 C945 C946 129.0(17) . . ? C944 C945 C946 110.6(14) . . ? C244 C945 C744 19.5(11) . . ? C944 C945 C744 20.0(9) . . ? C946 C945 C744 109.5(13) . . ? C945 C946 C246 81.1(10) . . ? C27 C271 C272 117.6(3) . . ? C27 C271 H27A 107.9 . . ? C272 C271 H27A 107.9 . . ? C27 C271 H27B 107.9 . . ? C272 C271 H27B 107.9 . . ? H27A C271 H27B 107.2 . . ? C273 C272 C271 115.7(3) . . ? C273 C272 H27C 108.4 . . ? C271 C272 H27C 108.4 . . ? C273 C272 H27D 108.4 . . ? C271 C272 H27D 108.4 . . ? H27C C272 H27D 107.4 . . ? C272 C273 C274 111.9(3) . . ? C272 C273 H27E 109.2 . . ? C274 C273 H27E 109.2 . . ? C272 C273 H27F 109.2 . . ? C274 C273 H27F 109.2 . . ? H27E C273 H27F 107.9 . . ? C275 C274 C273 113.7(3) . . ? C275 C274 H27G 108.8 . . ? C273 C274 H27G 108.8 . . ? C275 C274 H27H 108.8 . . ? C273 C274 H27H 108.8 . . ? H27G C274 H27H 107.7 . . ? C276 C275 C274 113.3(4) . . ? C276 C275 H27I 108.9 . . ? C274 C275 H27I 108.9 . . ? C276 C275 H27J 108.9 . . ? C274 C275 H27J 108.9 . . ? H27I C275 H27J 107.7 . . ? C275 C276 H27K 109.5 . . ? C275 C276 H27L 109.5 . . ? H27K C276 H27L 109.5 . . ? C275 C276 H27M 109.5 . . ? H27K C276 H27M 109.5 . . ? H27L C276 H27M 109.5 . . ? C34 C341 C342 114.7(3) . . ? C34 C341 H34A 108.6 . . ? C342 C341 H34A 108.6 . . ? C34 C341 H34B 108.6 . . ? C342 C341 H34B 108.6 . . ? H34A C341 H34B 107.6 . . ? C341 C342 C343 114.3(3) . . ? C341 C342 H34C 108.7 . . ? C343 C342 H34C 108.7 . . ? C341 C342 H34D 108.7 . . ? C343 C342 H34D 108.7 . . ? H34C C342 H34D 107.6 . . ? C342 C343 C344 112.6(3) . . ? C342 C343 H34E 109.1 . . ? C344 C343 H34E 109.1 . . ? C342 C343 H34F 109.1 . . ? C344 C343 H34F 109.1 . . ? H34E C343 H34F 107.8 . . ? C345 C344 C343 113.8(4) . . ? C345 C344 H34G 108.8 . . ? C343 C344 H34G 108.8 . . ? C345 C344 H34H 108.8 . . ? C343 C344 H34H 108.8 . . ? H34G C344 H34H 107.7 . . ? C344 C345 C346 112.7(4) . . ? C344 C345 H34I 109.1 . . ? C346 C345 H34I 109.1 . . ? C344 C345 H34J 109.1 . . ? C346 C345 H34J 109.1 . . ? H34I C345 H34J 107.8 . . ? C345 C346 H34K 109.5 . . ? C345 C346 H34L 109.5 . . ? H34K C346 H34L 109.5 . . ? C345 C346 H34M 109.5 . . ? H34K C346 H34M 109.5 . . ? H34L C346 H34M 109.5 . . ? C37 C371 C372 115.8(3) . . ? C37 C371 H37A 108.3 . . ? C372 C371 H37A 108.3 . . ? C37 C371 H37B 108.3 . . ? C372 C371 H37B 108.3 . . ? H37A C371 H37B 107.4 . . ? C371 C372 C373 114.0(4) . . ? C371 C372 H37C 108.8 . . ? C373 C372 H37C 108.8 . . ? C371 C372 H37D 108.8 . . ? C373 C372 H37D 108.8 . . ? H37C C372 H37D 107.6 . . ? C874 C373 C372 126.5(7) . . ? C874 C373 C374 28.6(6) . . ? C372 C373 C374 105.7(4) . . ? C875 C374 C874 145.9(17) . . ? C875 C374 C375 89.3(13) . . ? C874 C374 C375 67.9(10) . . ? C875 C374 C373 129.1(13) . . ? C874 C374 C373 46.7(9) . . ? C375 C374 C373 109.2(7) . . ? C874 C375 C374 34.1(5) . . ? C874 C375 C376 139.9(10) . . ? C374 C375 C376 109.5(8) . . ? C874 C375 C875 60.1(7) . . ? C374 C375 C875 27.7(5) . . ? C376 C375 C875 90.2(8) . . ? C374 C874 C373 104.7(13) . . ? C374 C874 C375 77.9(11) . . ? C373 C874 C375 151.0(11) . . ? C374 C874 C875 16.2(8) . . ? C373 C874 C875 106.5(9) . . ? C375 C874 C875 68.2(8) . . ? C374 C875 C876 129.4(17) . . ? C374 C875 C874 17.9(9) . . ? C876 C875 C874 113.4(11) . . ? C374 C875 C375 63.0(11) . . ? C876 C875 C375 96.6(10) . . ? C874 C875 C375 51.7(7) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.830 _refine_diff_density_min -0.434 _refine_diff_density_rms 0.093 # #===END # data_paulb3 _database_code_depnum_ccdc_archive 'CCDC 248917' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common 'Compound 2' _chemical_formula_moiety 'C86 H116 F In N8' _chemical_formula_structural '[In(C6H4F)(octahexyl-phthalocyanine)]' _chemical_formula_analytical ? _chemical_formula_sum 'C86 H116 F In N8' _chemical_formula_weight 1395.69 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.873(3) _cell_length_b 17.910(4) _cell_length_c 17.642(4) _cell_angle_alpha 102.92(3) _cell_angle_beta 93.73(3) _cell_angle_gamma 90.50(3) _cell_volume 3955.0(14) _cell_formula_units_Z 2 _cell_measurement_temperature 293(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'very thin flat needles' _exptl_crystal_colour blue-green _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.001 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.172 _exptl_crystal_density_method ? _exptl_crystal_F_000 1492 _exptl_absorpt_coefficient_mu 0.349 _exptl_absorpt_correction_type 'not applied' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku R-Axis-IIc' _diffrn_measurement_method 'image-plate oscillation photos' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 12642 _diffrn_reflns_av_R_equivalents 0.1039 _diffrn_reflns_av_sigmaI/netI 0.1756 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 20.00 _reflns_number_total 6866 _reflns_number_observed 3217 _reflns_observed_criterion I>2sigma(I) _computing_data_collection 'MSC R-Axis-II control software' _computing_cell_refinement 'DENZO/CELL (Otwinowski and Minor, 1985)' _computing_data_reduction 'DENZO, SCALEPACK (Otwinowski and Minor, 1985)' _computing_structure_solution 'SHELXS (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL (Sheldrick, 1997)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0620P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6866 _refine_ls_number_parameters 844 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1582 _refine_ls_R_factor_gt 0.0645 _refine_ls_wR_factor_ref 0.1596 _refine_ls_wR_factor_gt 0.1279 _refine_ls_goodness_of_fit_ref 0.935 _refine_ls_restrained_S_all 0.935 _refine_ls_shift/su_max 0.067 _refine_ls_shift/su_mean 0.003 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 In In 0.19816(6) 0.32026(5) 0.36593(6) 0.0851(4) Uani 1 1 d . . . N1 N 0.2588(7) 0.4390(5) 0.4054(8) 0.079(3) Uani 1 1 d . . . C2 C 0.2554(10) 0.4812(7) 0.4787(10) 0.084(4) Uani 1 1 d . . . C3 C 0.3392(10) 0.5393(7) 0.4909(10) 0.083(4) Uani 1 1 d . . . C4 C 0.3709(10) 0.5954(8) 0.5583(9) 0.085(3) Uani 1 1 d . . . C5 C 0.4596(11) 0.6399(7) 0.5497(10) 0.104(4) Uani 1 1 d . . . H5 H 0.4849 0.6780 0.5919 0.125 Uiso 1 1 calc R . . C6 C 0.5094(9) 0.6289(8) 0.4818(12) 0.110(5) Uani 1 1 d . . . H6 H 0.5681 0.6593 0.4809 0.132 Uiso 1 1 calc R . . C7 C 0.4776(10) 0.5751(7) 0.4145(9) 0.085(4) Uani 1 1 d . . . C8 C 0.3897(9) 0.5293(7) 0.4228(10) 0.079(4) Uani 1 1 d . . . C9 C 0.3384(10) 0.4676(7) 0.3682(11) 0.079(4) Uani 1 1 d . . . N10 N 0.3601(7) 0.4437(6) 0.2944(9) 0.085(3) Uani 1 1 d . . . N11 N 0.2288(7) 0.3391(6) 0.2524(6) 0.080(3) Uani 1 1 d . . . C12 C 0.3090(9) 0.3877(9) 0.2420(10) 0.081(4) Uani 1 1 d . . . C13 C 0.3324(9) 0.3657(8) 0.1593(10) 0.081(4) Uani 1 1 d . . . C14 C 0.4006(9) 0.3970(7) 0.1127(11) 0.092(4) Uani 1 1 d . . . C15 C 0.4037(11) 0.3569(10) 0.0348(11) 0.115(5) Uani 1 1 d . . . H15 H 0.4463 0.3753 0.0021 0.137 Uiso 1 1 calc R . . C16 C 0.3451(13) 0.2908(9) 0.0058(9) 0.118(5) Uani 1 1 d . . . H16 H 0.3541 0.2648 -0.0452 0.141 Uiso 1 1 calc R . . C17 C 0.2756(11) 0.2609(10) 0.0455(11) 0.112(6) Uani 1 1 d . . . C18 C 0.2695(9) 0.3009(9) 0.1217(12) 0.093(5) Uani 1 1 d . . . C19 C 0.2036(10) 0.2883(7) 0.1812(10) 0.088(4) Uani 1 1 d . . . N20 N 0.1227(9) 0.2394(5) 0.1690(6) 0.083(3) Uani 1 1 d . . . N21 N 0.0582(7) 0.2652(5) 0.2983(8) 0.083(3) Uani 1 1 d . . . C22 C 0.0552(10) 0.2310(7) 0.2197(10) 0.079(4) Uani 1 1 d . . . C23 C -0.0410(9) 0.1816(7) 0.2028(13) 0.088(4) Uani 1 1 d . . . C24 C -0.0843(12) 0.1383(9) 0.1343(12) 0.103(4) Uani 1 1 d . . . C25 C -0.1784(12) 0.0975(7) 0.1388(11) 0.111(5) Uani 1 1 d . . . H25 H -0.2117 0.0682 0.0934 0.133 Uiso 1 1 calc R . . C26 C -0.2204(10) 0.1004(9) 0.2079(14) 0.108(5) Uani 1 1 d . . . H26 H -0.2791 0.0696 0.2077 0.130 Uiso 1 1 calc R . . C27 C -0.1834(11) 0.1447(8) 0.2769(13) 0.100(4) Uani 1 1 d . . . C28 C -0.0889(11) 0.1875(7) 0.2721(11) 0.088(4) Uani 1 1 d . . . C29 C -0.0259(10) 0.2425(8) 0.3325(10) 0.081(4) Uani 1 1 d . . . N30 N -0.0516(7) 0.2690(7) 0.4056(9) 0.087(3) Uani 1 1 d . . . N31 N 0.0879(7) 0.3640(6) 0.4513(6) 0.084(3) Uani 1 1 d . . . C32 C -0.0050(10) 0.3272(8) 0.4609(10) 0.083(4) Uani 1 1 d . . . C33 C -0.0441(10) 0.3626(8) 0.5352(9) 0.083(4) Uani 1 1 d . . . C34 C -0.1351(10) 0.3443(8) 0.5713(11) 0.093(4) Uani 1 1 d . . . C35 C -0.1480(10) 0.3940(11) 0.6405(11) 0.114(5) Uani 1 1 d . . . H35 H -0.2061 0.3860 0.6667 0.137 Uiso 1 1 calc R . . C36 C -0.0824(12) 0.4553(8) 0.6752(8) 0.108(4) Uani 1 1 d . . . H36 H -0.0978 0.4854 0.7231 0.129 Uiso 1 1 calc R . . C37 C 0.0059(11) 0.4734(9) 0.6410(11) 0.098(4) Uani 1 1 d . . . C38 C 0.0233(10) 0.4246(8) 0.5690(10) 0.079(4) Uani 1 1 d . . . C39 C 0.1052(10) 0.4229(8) 0.5153(9) 0.081(4) Uani 1 1 d . . . N40 N 0.1826(9) 0.4744(5) 0.5283(6) 0.086(3) Uani 1 1 d . . . C41 C 0.3173(8) 0.6100(7) 0.6346(8) 0.097(4) Uani 1 1 d . . . H41A H 0.3082 0.5613 0.6492 0.117 Uiso 1 1 calc R . . H41B H 0.2484 0.6291 0.6254 0.117 Uiso 1 1 calc R . . C42 C 0.3731(9) 0.6662(7) 0.7039(10) 0.120(5) Uani 1 1 d . . . H42A H 0.4434 0.6487 0.7113 0.144 Uiso 1 1 calc R . . H42B H 0.3785 0.7157 0.6905 0.144 Uiso 1 1 calc R . . C43 C 0.3232(10) 0.6769(7) 0.7796(10) 0.119(5) Uani 1 1 d . . . H43A H 0.3196 0.6277 0.7940 0.143 Uiso 1 1 calc R . . H43B H 0.2523 0.6932 0.7721 0.143 Uiso 1 1 calc R . . C44 C 0.3787(9) 0.7348(7) 0.8472(9) 0.109(4) Uani 1 1 d . . . H44A H 0.4503 0.7199 0.8541 0.131 Uiso 1 1 calc R . . H44B H 0.3794 0.7848 0.8345 0.131 Uiso 1 1 calc R . . C45 C 0.3277(10) 0.7401(8) 0.9208(10) 0.134(5) Uani 1 1 d . . . H45A H 0.3317 0.6913 0.9359 0.161 Uiso 1 1 calc R . . H45B H 0.2548 0.7516 0.9133 0.161 Uiso 1 1 calc R . . C46 C 0.3801(10) 0.8018(8) 0.9843(9) 0.151(6) Uani 1 1 d . . . H46A H 0.3464 0.8047 1.0318 0.227 Uiso 1 1 calc R . . H46B H 0.3753 0.8502 0.9695 0.227 Uiso 1 1 calc R . . H46C H 0.4521 0.7900 0.9921 0.227 Uiso 1 1 calc R . . C71 C 0.5324(8) 0.5692(6) 0.3429(8) 0.094(4) Uani 1 1 d . . . H71A H 0.4847 0.5831 0.3037 0.113 Uiso 1 1 calc R . . H71B H 0.5498 0.5160 0.3238 0.113 Uiso 1 1 calc R . . C72 C 0.6321(8) 0.6182(6) 0.3500(8) 0.107(4) Uani 1 1 d . . . H72A H 0.6173 0.6711 0.3731 0.128 Uiso 1 1 calc R . . H72B H 0.6838 0.6009 0.3844 0.128 Uiso 1 1 calc R . . C73 C 0.6757(9) 0.6136(7) 0.2719(9) 0.121(5) Uani 1 1 d . . . H73A H 0.6244 0.6314 0.2376 0.145 Uiso 1 1 calc R . . H73B H 0.6901 0.5607 0.2486 0.145 Uiso 1 1 calc R . . C74 C 0.7752(10) 0.6619(8) 0.2795(10) 0.151(6) Uani 1 1 d . . . H74A H 0.7649 0.7120 0.3126 0.182 Uiso 1 1 calc R . . H74B H 0.8309 0.6378 0.3043 0.182 Uiso 1 1 calc R . . C75 C 0.8059(12) 0.6712(10) 0.2021(13) 0.207(9) Uani 1 1 d . . . H75A H 0.8098 0.6211 0.1673 0.248 Uiso 1 1 calc R . . H75B H 0.7534 0.6998 0.1795 0.248 Uiso 1 1 calc R . . C76 C 0.9076(19) 0.7116(13) 0.2092(14) 0.354(17) Uani 1 1 d . . . H76A H 0.9256 0.7168 0.1586 0.531 Uiso 1 1 calc R . . H76B H 0.9599 0.6829 0.2307 0.531 Uiso 1 1 calc R . . H76C H 0.9035 0.7615 0.2428 0.531 Uiso 1 1 calc R . . C141 C 0.4670(8) 0.4708(8) 0.1438(7) 0.108(4) Uani 1 1 d . . . H14A H 0.4772 0.4790 0.2001 0.129 Uiso 1 1 calc R . . H14B H 0.5349 0.4635 0.1229 0.129 Uiso 1 1 calc R . . C142 C 0.4215(15) 0.5404(10) 0.1243(13) 0.212(10) Uani 1 1 d . . . H14C H 0.4670 0.5824 0.1520 0.254 Uiso 1 1 calc R . . H14D H 0.4313 0.5355 0.0694 0.254 Uiso 1 1 calc R . . C143 C 0.3308(13) 0.5642(11) 0.1334(15) 0.244(13) Uani 1 1 d . . . H14E H 0.3189 0.5674 0.1878 0.293 Uiso 1 1 calc R . . H14F H 0.2844 0.5238 0.1034 0.293 Uiso 1 1 calc R . . C144 C 0.2915(16) 0.6387(12) 0.1148(13) 0.219(10) Uani 1 1 d . . . H14G H 0.3455 0.6780 0.1323 0.263 Uiso 1 1 calc R . . H14H H 0.2808 0.6312 0.0586 0.263 Uiso 1 1 calc R . . C145 C 0.2026(16) 0.6649(13) 0.1466(13) 0.236(11) Uani 1 1 d . . . H14I H 0.2104 0.6693 0.2025 0.283 Uiso 1 1 calc R . . H14J H 0.1462 0.6284 0.1255 0.283 Uiso 1 1 calc R . . C146 C 0.1762(16) 0.7400(11) 0.1307(14) 0.283(13) Uani 1 1 d . . . H14K H 0.1127 0.7570 0.1541 0.424 Uiso 1 1 calc R . . H14L H 0.1672 0.7356 0.0754 0.424 Uiso 1 1 calc R . . H14M H 0.2314 0.7765 0.1523 0.424 Uiso 1 1 calc R . . C171 C 0.2137(10) 0.1852(8) 0.0052(8) 0.132(5) Uani 1 1 d . . . C172 C 0.281(2) 0.1188(16) -0.0030(19) 0.117(9) Uiso 0.50 1 d P . . C672 C 0.259(3) 0.1152(18) 0.055(3) 0.141(12) Uiso 0.50 1 d P . . C173 C 0.325(3) 0.1143(18) 0.088(2) 0.119(12) Uiso 0.50 1 d P . . C673 C 0.363(3) 0.107(2) 0.057(2) 0.148(15) Uiso 0.50 1 d P . . C174 C 0.3862(12) 0.0413(10) 0.0856(11) 0.160(6) Uiso 1 1 d . . . C175 C 0.4165(19) 0.0386(13) 0.1564(18) 0.114(8) Uiso 0.50 1 d P . . C675 C 0.494(2) 0.0410(16) 0.1277(18) 0.142(10) Uiso 0.50 1 d P . . C176 C 0.5107(15) -0.0265(12) 0.1563(13) 0.235(8) Uiso 1 1 d . . . C241 C -0.0365(9) 0.1330(6) 0.0574(10) 0.109(5) Uani 1 1 d . . . H24A H -0.0254 0.1847 0.0509 0.131 Uiso 1 1 calc R . . H24B H 0.0315 0.1106 0.0610 0.131 Uiso 1 1 calc R . . C242 C -0.0944(9) 0.0888(7) -0.0143(10) 0.124(5) Uani 1 1 d . . . H24C H -0.1084 0.0374 -0.0075 0.149 Uiso 1 1 calc R . . H24D H -0.1610 0.1125 -0.0201 0.149 Uiso 1 1 calc R . . C243 C -0.0409(10) 0.0829(8) -0.0869(10) 0.137(5) Uani 1 1 d . . . H24E H 0.0261 0.0595 -0.0816 0.165 Uiso 1 1 calc R . . H24F H -0.0285 0.1339 -0.0951 0.165 Uiso 1 1 calc R . . C244 C -0.1068(12) 0.0337(10) -0.1600(12) 0.159(6) Uani 1 1 d . . . H24G H -0.1208 -0.0161 -0.1495 0.190 Uiso 1 1 calc R . . H24H H -0.1733 0.0581 -0.1640 0.190 Uiso 1 1 calc R . . C245 C -0.0656(13) 0.0220(11) -0.2323(13) 0.187(8) Uani 1 1 d . . . H24I H 0.0020 -0.0009 -0.2286 0.225 Uiso 1 1 calc R . . H24J H -0.0547 0.0714 -0.2447 0.225 Uiso 1 1 calc R . . C246 C -0.1335(12) -0.0299(9) -0.3008(9) 0.193(7) Uani 1 1 d . . . H24K H -0.0991 -0.0348 -0.3483 0.289 Uiso 1 1 calc R . . H24L H -0.2000 -0.0071 -0.3063 0.289 Uiso 1 1 calc R . . H24M H -0.1433 -0.0796 -0.2901 0.289 Uiso 1 1 calc R . . C271 C -0.2305(10) 0.1407(9) 0.3511(12) 0.131(5) Uani 1 1 d . . . H27A H -0.3025 0.1234 0.3387 0.158 Uiso 1 1 calc R . . H27B H -0.2307 0.1921 0.3836 0.158 Uiso 1 1 calc R . . C272 C -0.1777(15) 0.0891(14) 0.3982(12) 0.195(8) Uani 1 1 d . . . H27C H -0.1039 0.1022 0.4057 0.234 Uiso 1 1 calc R . . H27D H -0.2055 0.0989 0.4492 0.234 Uiso 1 1 calc R . . C273 C -0.190(2) 0.0105(13) 0.3637(15) 0.243(13) Uani 1 1 d . . . H27E H -0.1641 -0.0003 0.3122 0.291 Uiso 1 1 calc R . . H27F H -0.2635 -0.0043 0.3585 0.291 Uiso 1 1 calc R . . C274 C -0.130(2) -0.0349(14) 0.4152(16) 0.251(13) Uani 1 1 d . . . H27G H -0.0617 -0.0108 0.4287 0.301 Uiso 1 1 calc R . . H27H H -0.1650 -0.0287 0.4633 0.301 Uiso 1 1 calc R . . C275 C -0.1167(18) -0.1090(15) 0.3890(14) 0.230(9) Uani 1 1 d . . . H27I H -0.0860 -0.1152 0.3393 0.276 Uiso 1 1 calc R . . H27J H -0.1854 -0.1333 0.3784 0.276 Uiso 1 1 calc R . . C276 C -0.0521(14) -0.1551(12) 0.4371(12) 0.259(12) Uani 1 1 d . . . H27K H -0.0510 -0.2076 0.4091 0.388 Uiso 1 1 calc R . . H27L H -0.0823 -0.1523 0.4859 0.388 Uiso 1 1 calc R . . H27M H 0.0178 -0.1343 0.4465 0.388 Uiso 1 1 calc R . . C341 C -0.2064(9) 0.2759(7) 0.5364(8) 0.115(5) Uani 1 1 d . . . C342 C -0.2715(12) 0.2534(10) 0.6019(11) 0.199(8) Uani 1 1 d . . . C343 C -0.348(2) 0.1942(16) 0.5575(17) 0.115(9) Uiso 0.50 1 d P . . C843 C -0.293(3) 0.175(2) 0.587(3) 0.198(16) Uiso 0.50 1 d P . . C344 C -0.413(3) 0.157(3) 0.621(3) 0.184(15) Uiso 0.50 1 d P . . C844 C -0.354(4) 0.144(3) 0.655(4) 0.25(2) Uiso 0.50 1 d P . . C345 C -0.395(4) 0.187(3) 0.689(3) 0.23(2) Uiso 0.50 1 d P . . C845 C -0.466(2) 0.2100(18) 0.659(2) 0.153(11) Uiso 0.50 1 d P . . C346 C -0.5216(19) 0.1781(14) 0.7208(16) 0.300(11) Uiso 1 1 d . . . C371 C 0.0766(9) 0.5402(8) 0.6790(8) 0.100(4) Uani 1 1 d . . . H37A H 0.0741 0.5766 0.6457 0.121 Uiso 1 1 calc R . . H37B H 0.1472 0.5219 0.6807 0.121 Uiso 1 1 calc R . . C372 C 0.0549(8) 0.5830(7) 0.7604(10) 0.101(4) Uani 1 1 d . . . H37C H 0.0894 0.6330 0.7707 0.121 Uiso 1 1 calc R . . H37D H -0.0194 0.5911 0.7621 0.121 Uiso 1 1 calc R . . C373 C 0.0891(10) 0.5442(8) 0.8244(10) 0.126(5) Uani 1 1 d . . . H37E H 0.1638 0.5376 0.8239 0.152 Uiso 1 1 calc R . . H37F H 0.0564 0.4935 0.8133 0.152 Uiso 1 1 calc R . . C374 C 0.0641(12) 0.5862(10) 0.9065(11) 0.158(6) Uani 1 1 d . . . H37G H 0.1060 0.5657 0.9444 0.189 Uiso 1 1 calc R . . H37H H 0.0831 0.6400 0.9139 0.189 Uiso 1 1 calc R . . C375 C -0.0454(15) 0.5795(11) 0.9208(12) 0.210(9) Uani 1 1 d . . . H37I H -0.0864 0.6019 0.8838 0.252 Uiso 1 1 calc R . . H37J H -0.0646 0.5254 0.9103 0.252 Uiso 1 1 calc R . . C376 C -0.0733(14) 0.6146(12) 0.9976(12) 0.240(10) Uani 1 1 d . . . H37K H -0.1466 0.6069 1.0010 0.361 Uiso 1 1 calc R . . H37L H -0.0571 0.6685 1.0083 0.361 Uiso 1 1 calc R . . H37M H -0.0350 0.5920 1.0349 0.361 Uiso 1 1 calc R . . C51 C 0.2965(10) 0.2332(6) 0.3892(11) 0.091(4) Uani 1 1 d . . . C52 C 0.3693(12) 0.2006(8) 0.3380(9) 0.108(4) Uani 1 1 d . . . H52 H 0.3753 0.2177 0.2924 0.130 Uiso 1 1 calc R . . C53 C 0.4325(17) 0.1438(14) 0.3530(14) 0.155(8) Uani 1 1 d . . . H53 H 0.4834 0.1259 0.3188 0.186 Uiso 1 1 calc R . . C54 C 0.424(2) 0.1140(16) 0.413(2) 0.22(2) Uani 1 1 d . . . C55 C 0.3560(19) 0.1415(14) 0.4673(16) 0.189(11) Uani 1 1 d . . . H55 H 0.3521 0.1217 0.5115 0.227 Uiso 1 1 calc R . . C56 C 0.2908(10) 0.2016(10) 0.4541(11) 0.128(5) Uani 1 1 d . . . H56 H 0.2424 0.2204 0.4902 0.154 Uiso 1 1 calc R . . F57 F 0.4868(9) 0.0584(6) 0.4295(8) 0.297(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 In 0.0774(5) 0.0753(6) 0.0997(8) 0.0194(5) -0.0111(4) -0.0139(4) N1 0.078(7) 0.062(7) 0.099(11) 0.031(8) -0.019(6) -0.022(5) C2 0.093(11) 0.057(9) 0.083(14) -0.017(9) -0.032(9) -0.007(9) C3 0.085(8) 0.054(9) 0.088(13) -0.023(9) -0.018(10) -0.018(8) C4 0.090(9) 0.079(10) 0.084(13) 0.018(10) -0.001(9) 0.004(8) C5 0.097(10) 0.084(10) 0.116(16) 0.000(10) -0.025(9) -0.033(8) C6 0.098(9) 0.107(12) 0.120(16) 0.014(12) 0.017(11) -0.020(8) C7 0.089(9) 0.072(9) 0.081(13) -0.006(9) -0.016(9) -0.014(8) C8 0.071(8) 0.066(10) 0.092(14) 0.004(9) -0.016(9) -0.014(8) C9 0.080(9) 0.055(10) 0.094(14) 0.008(11) -0.012(10) -0.007(7) N10 0.080(6) 0.081(8) 0.088(10) 0.012(8) -0.011(8) -0.018(6) N11 0.060(5) 0.084(7) 0.100(10) 0.027(7) 0.002(6) -0.024(5) C12 0.074(9) 0.116(13) 0.055(12) 0.020(10) -0.002(8) 0.017(9) C13 0.061(7) 0.076(10) 0.110(16) 0.038(10) -0.018(9) -0.022(7) C14 0.089(9) 0.070(10) 0.111(15) 0.012(10) -0.015(9) -0.016(8) C15 0.150(12) 0.103(13) 0.087(15) 0.010(11) 0.029(10) -0.019(10) C16 0.148(12) 0.098(12) 0.087(13) -0.024(10) 0.011(11) -0.003(9) C17 0.093(10) 0.184(18) 0.076(14) 0.053(14) 0.043(10) 0.034(11) C18 0.070(9) 0.111(13) 0.112(16) 0.044(12) 0.037(10) -0.004(9) C19 0.078(9) 0.058(9) 0.109(14) -0.006(10) -0.036(10) -0.017(7) N20 0.087(7) 0.077(7) 0.083(10) 0.020(6) -0.006(7) -0.014(6) N21 0.070(6) 0.077(7) 0.104(11) 0.028(8) -0.001(7) -0.023(5) C22 0.090(10) 0.061(9) 0.078(14) 0.005(9) -0.024(9) -0.012(8) C23 0.079(9) 0.063(10) 0.115(17) 0.015(10) -0.023(12) -0.009(8) C24 0.103(12) 0.099(12) 0.104(17) 0.024(12) -0.018(11) 0.000(10) C25 0.111(12) 0.083(10) 0.123(17) 0.008(10) -0.041(10) -0.040(9) C26 0.094(10) 0.101(12) 0.124(17) 0.024(13) -0.024(12) -0.043(8) C27 0.090(10) 0.081(10) 0.124(17) 0.023(11) -0.022(11) -0.025(8) C28 0.098(10) 0.070(10) 0.094(14) 0.019(9) -0.023(11) -0.011(9) C29 0.084(10) 0.085(10) 0.071(12) 0.020(10) -0.016(10) -0.008(8) N30 0.088(7) 0.073(8) 0.104(11) 0.036(8) -0.009(8) -0.016(6) N31 0.071(6) 0.091(8) 0.089(9) 0.020(7) -0.011(6) -0.019(6) C32 0.079(9) 0.071(10) 0.101(14) 0.027(10) -0.008(9) 0.001(8) C33 0.089(9) 0.074(10) 0.086(13) 0.021(9) 0.009(9) 0.002(9) C34 0.098(11) 0.094(12) 0.105(14) 0.059(11) 0.007(10) 0.005(9) C35 0.102(10) 0.130(14) 0.112(16) 0.024(12) 0.026(10) -0.006(10) C36 0.111(11) 0.100(12) 0.115(14) 0.034(10) -0.001(11) -0.003(9) C37 0.101(11) 0.094(12) 0.102(15) 0.033(12) -0.004(11) 0.004(10) C38 0.082(9) 0.070(10) 0.085(13) 0.024(10) -0.016(10) -0.005(8) C39 0.070(8) 0.089(11) 0.080(12) 0.018(9) -0.004(9) -0.021(8) N40 0.076(7) 0.088(8) 0.096(10) 0.026(7) -0.009(6) -0.005(6) C41 0.089(8) 0.095(10) 0.101(13) 0.016(9) -0.012(9) -0.012(7) C42 0.109(9) 0.095(10) 0.134(15) -0.010(10) -0.017(10) -0.015(8) C43 0.133(11) 0.100(11) 0.120(15) 0.016(11) 0.008(11) 0.003(9) C44 0.118(9) 0.083(10) 0.107(14) -0.015(10) -0.018(10) -0.006(8) C45 0.143(11) 0.126(13) 0.117(15) -0.009(12) 0.019(11) -0.006(10) C46 0.164(12) 0.130(12) 0.126(15) -0.041(11) 0.002(10) 0.002(10) C71 0.084(8) 0.093(10) 0.100(13) 0.012(8) -0.004(8) -0.028(7) C72 0.094(8) 0.100(10) 0.123(14) 0.020(9) 0.003(8) -0.020(7) C73 0.101(9) 0.100(10) 0.164(17) 0.032(10) 0.017(9) -0.020(8) C74 0.127(12) 0.171(15) 0.170(19) 0.065(13) 0.028(11) -0.026(10) C75 0.169(14) 0.189(17) 0.26(3) 0.027(17) 0.059(16) -0.082(13) C76 0.37(3) 0.32(3) 0.33(4) -0.05(3) 0.17(3) -0.16(3) C141 0.112(9) 0.116(12) 0.093(11) 0.018(10) 0.013(8) -0.023(9) C142 0.199(18) 0.106(16) 0.33(3) 0.086(16) -0.08(2) -0.047(14) C143 0.125(13) 0.128(17) 0.48(4) 0.075(19) -0.03(2) 0.011(12) C144 0.21(2) 0.21(2) 0.25(3) 0.082(19) -0.042(18) 0.041(18) C145 0.21(2) 0.25(3) 0.27(3) 0.11(2) 0.003(19) 0.070(19) C146 0.34(3) 0.19(2) 0.37(3) 0.13(2) 0.08(2) 0.12(2) C171 0.150(11) 0.107(11) 0.110(13) -0.027(10) -0.022(9) -0.070(10) C241 0.116(10) 0.063(9) 0.123(14) -0.009(9) -0.073(11) -0.031(7) C242 0.114(10) 0.093(11) 0.148(17) -0.001(11) -0.021(12) 0.011(8) C243 0.105(10) 0.147(13) 0.131(16) -0.017(12) -0.038(11) 0.011(9) C244 0.160(14) 0.167(16) 0.134(19) 0.008(15) -0.008(15) 0.006(12) C245 0.171(16) 0.23(2) 0.14(2) -0.004(17) 0.004(15) -0.007(13) C246 0.213(15) 0.228(18) 0.093(14) -0.040(13) -0.043(12) -0.066(13) C271 0.110(10) 0.136(14) 0.146(18) 0.030(12) -0.002(12) -0.041(9) C272 0.213(17) 0.22(2) 0.19(2) 0.11(2) 0.011(16) -0.030(18) C273 0.38(3) 0.11(2) 0.26(3) 0.06(2) 0.06(3) -0.03(2) C274 0.36(3) 0.108(19) 0.28(4) 0.03(2) 0.06(3) 0.00(2) C275 0.27(2) 0.23(3) 0.20(3) 0.07(2) 0.03(2) 0.00(2) C276 0.24(2) 0.28(2) 0.27(3) 0.14(2) -0.140(19) -0.044(17) C341 0.098(8) 0.089(10) 0.158(14) 0.027(9) 0.022(8) -0.044(8) C342 0.172(13) 0.144(15) 0.25(2) -0.039(14) 0.082(14) -0.096(12) C371 0.109(9) 0.100(11) 0.088(13) 0.015(9) -0.006(9) 0.005(8) C372 0.097(8) 0.098(10) 0.107(14) 0.021(11) 0.008(9) 0.001(7) C373 0.137(11) 0.134(13) 0.117(15) 0.047(12) 0.011(11) 0.016(9) C374 0.148(14) 0.191(17) 0.133(18) 0.036(14) 0.004(12) 0.009(12) C375 0.192(19) 0.27(2) 0.18(2) 0.060(19) 0.064(16) 0.135(16) C376 0.23(2) 0.32(3) 0.18(2) 0.08(2) 0.063(18) 0.114(18) C51 0.096(9) 0.069(9) 0.105(14) 0.021(10) -0.016(9) -0.023(7) C52 0.104(10) 0.087(11) 0.120(14) 0.001(10) -0.017(10) 0.000(8) C53 0.124(12) 0.13(2) 0.19(3) -0.004(14) -0.029(15) 0.031(15) C54 0.17(2) 0.074(17) 0.38(7) 0.04(2) -0.11(3) 0.022(15) C55 0.21(2) 0.15(2) 0.23(3) 0.11(2) -0.11(2) -0.019(16) C56 0.115(10) 0.125(14) 0.146(18) 0.047(12) -0.032(11) -0.030(10) F57 0.301(12) 0.135(8) 0.427(19) 0.048(10) -0.131(12) 0.078(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag In C51 2.111(12) . ? In N31 2.160(9) . ? In N11 2.165(9) . ? In N21 2.191(9) . ? In N1 2.203(9) . ? N1 C2 1.349(13) . ? N1 C9 1.404(14) . ? C2 N40 1.345(14) . ? C2 C3 1.463(16) . ? C3 C8 1.381(14) . ? C3 C4 1.409(15) . ? C4 C5 1.422(14) . ? C4 C41 1.525(14) . ? C5 C6 1.372(15) . ? C5 H5 0.9300 . ? C6 C7 1.387(15) . ? C6 H6 0.9300 . ? C7 C8 1.426(15) . ? C7 C71 1.470(14) . ? C8 C9 1.419(15) . ? C9 N10 1.326(14) . ? N10 C12 1.337(14) . ? N11 C12 1.391(14) . ? N11 C19 1.394(13) . ? C12 C13 1.476(15) . ? C13 C18 1.419(16) . ? C13 C14 1.432(15) . ? C14 C15 1.405(16) . ? C14 C141 1.541(14) . ? C15 C16 1.376(15) . ? C15 H15 0.9300 . ? C16 C17 1.350(15) . ? C16 H16 0.9300 . ? C17 C18 1.383(17) . ? C17 C171 1.565(18) . ? C18 C19 1.445(16) . ? C19 N20 1.329(13) . ? N20 C22 1.318(13) . ? N21 C29 1.376(13) . ? N21 C22 1.383(13) . ? C22 C23 1.490(16) . ? C23 C24 1.363(17) . ? C23 C28 1.389(15) . ? C24 C25 1.425(17) . ? C24 C241 1.509(16) . ? C25 C26 1.356(16) . ? C25 H25 0.9300 . ? C26 C27 1.351(17) . ? C26 H26 0.9300 . ? C27 C28 1.449(16) . ? C27 C271 1.493(17) . ? C28 C29 1.472(16) . ? C29 N30 1.335(14) . ? N30 C32 1.361(14) . ? N31 C39 1.367(13) . ? N31 C32 1.399(13) . ? C32 C33 1.447(15) . ? C33 C38 1.401(14) . ? C33 C34 1.438(15) . ? C34 C35 1.362(15) . ? C34 C341 1.514(16) . ? C35 C36 1.382(16) . ? C35 H35 0.9300 . ? C36 C37 1.389(15) . ? C36 H36 0.9300 . ? C37 C38 1.406(16) . ? C37 C371 1.500(16) . ? C38 C39 1.458(15) . ? C39 N40 1.325(13) . ? C41 C42 1.531(15) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C43 1.495(15) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 C44 1.527(15) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 C45 1.478(15) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 C46 1.507(15) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C71 C72 1.530(13) . ? C71 H71A 0.9700 . ? C71 H71B 0.9700 . ? C72 C73 1.507(14) . ? C72 H72A 0.9700 . ? C72 H72B 0.9700 . ? C73 C74 1.521(15) . ? C73 H73A 0.9700 . ? C73 H73B 0.9700 . ? C74 C75 1.491(19) . ? C74 H74A 0.9700 . ? C74 H74B 0.9700 . ? C75 C76 1.47(2) . ? C75 H75A 0.9700 . ? C75 H75B 0.9700 . ? C76 H76A 0.9600 . ? C76 H76B 0.9600 . ? C76 H76C 0.9600 . ? C141 C142 1.481(17) . ? C141 H14A 0.9700 . ? C141 H14B 0.9700 . ? C142 C143 1.255(18) . ? C142 H14C 0.9700 . ? C142 H14D 0.9700 . ? C143 C144 1.53(2) . ? C143 H14E 0.9700 . ? C143 H14F 0.9700 . ? C144 C145 1.35(2) . ? C144 H14G 0.9700 . ? C144 H14H 0.9700 . ? C145 C146 1.47(2) . ? C145 H14I 0.9700 . ? C145 H14J 0.9700 . ? C146 H14K 0.9600 . ? C146 H14L 0.9600 . ? C146 H14M 0.9600 . ? C171 C172 1.47(3) . ? C171 C672 1.77(4) . ? C172 C672 1.10(4) . ? C172 C673 1.49(4) . ? C172 C173 1.69(5) . ? C672 C173 0.99(4) . ? C672 C673 1.34(5) . ? C173 C673 0.75(4) . ? C173 C174 1.53(4) . ? C673 C174 1.40(3) . ? C174 C175 1.30(3) . ? C174 C675 1.54(3) . ? C175 C675 1.16(3) . ? C175 C176 1.69(3) . ? C675 C176 1.42(3) . ? C241 C242 1.483(15) . ? C241 H24A 0.9700 . ? C241 H24B 0.9700 . ? C242 C243 1.478(16) . ? C242 H24C 0.9700 . ? C242 H24D 0.9700 . ? C243 C244 1.579(18) . ? C243 H24E 0.9700 . ? C243 H24F 0.9700 . ? C244 C245 1.385(18) . ? C244 H24G 0.9700 . ? C244 H24H 0.9700 . ? C245 C246 1.561(19) . ? C245 H24I 0.9700 . ? C245 H24J 0.9700 . ? C246 H24K 0.9600 . ? C246 H24L 0.9600 . ? C246 H24M 0.9600 . ? C271 C272 1.513(19) . ? C271 H27A 0.9700 . ? C271 H27B 0.9700 . ? C272 C273 1.41(2) . ? C272 H27C 0.9700 . ? C272 H27D 0.9700 . ? C273 C274 1.53(3) . ? C273 H27E 0.9700 . ? C273 H27F 0.9700 . ? C274 C275 1.32(2) . ? C274 H27G 0.9700 . ? C274 H27H 0.9700 . ? C275 C276 1.52(2) . ? C275 H27I 0.9700 . ? C275 H27J 0.9700 . ? C276 H27K 0.9600 . ? C276 H27L 0.9600 . ? C276 H27M 0.9600 . ? C341 C342 1.589(18) . ? C342 C843 1.38(4) . ? C342 C343 1.49(3) . ? C343 C843 0.96(4) . ? C343 C344 1.69(4) . ? C843 C844 1.67(6) . ? C843 C344 1.74(6) . ? C344 C844 1.00(6) . ? C344 C345 1.22(6) . ? C344 C845 1.28(5) . ? C844 C345 1.04(6) . ? C844 C845 1.87(6) . ? C345 C845 1.15(6) . ? C345 C346 1.78(5) . ? C845 C346 1.55(3) . ? C371 C372 1.514(14) . ? C371 H37A 0.9700 . ? C371 H37B 0.9700 . ? C372 C373 1.497(15) . ? C372 H37C 0.9700 . ? C372 H37D 0.9700 . ? C373 C374 1.532(17) . ? C373 H37E 0.9700 . ? C373 H37F 0.9700 . ? C374 C375 1.457(18) . ? C374 H37G 0.9700 . ? C374 H37H 0.9700 . ? C375 C376 1.43(2) . ? C375 H37I 0.9700 . ? C375 H37J 0.9700 . ? C376 H37K 0.9600 . ? C376 H37L 0.9600 . ? C376 H37M 0.9600 . ? C51 C52 1.385(15) . ? C51 C56 1.392(16) . ? C52 C53 1.37(2) . ? C52 H52 0.9300 . ? C53 C54 1.29(3) . ? C53 H53 0.9300 . ? C54 F57 1.36(3) . ? C54 C55 1.36(3) . ? C55 C56 1.42(2) . ? C55 H55 0.9300 . ? C56 H56 0.9300 . ? 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 C51 In N31 116.9(6) . . ? C51 In N11 108.1(6) . . ? N31 In N11 134.9(3) . . ? C51 In N21 108.0(4) . . ? N31 In N21 82.8(5) . . ? N11 In N21 80.3(4) . . ? C51 In N1 116.6(3) . . ? N31 In N1 80.6(5) . . ? N11 In N1 82.7(5) . . ? N21 In N1 135.3(3) . . ? C2 N1 C9 109.7(12) . . ? C2 N1 In 124.3(10) . . ? C9 N1 In 121.8(10) . . ? N40 C2 N1 125.6(13) . . ? N40 C2 C3 127.1(16) . . ? N1 C2 C3 107.1(13) . . ? C8 C3 C4 122.6(14) . . ? C8 C3 C2 107.8(13) . . ? C4 C3 C2 129.5(18) . . ? C3 C4 C5 113.9(12) . . ? C3 C4 C41 125.0(14) . . ? C5 C4 C41 121.1(14) . . ? C6 C5 C4 122.8(13) . . ? C6 C5 H5 118.6 . . ? C4 C5 H5 118.6 . . ? C5 C6 C7 123.9(13) . . ? C5 C6 H6 118.0 . . ? C7 C6 H6 118.0 . . ? C6 C7 C8 113.8(13) . . ? C6 C7 C71 120.7(13) . . ? C8 C7 C71 125.6(14) . . ? C3 C8 C9 107.3(13) . . ? C3 C8 C7 123.0(15) . . ? C9 C8 C7 129.7(17) . . ? N10 C9 N1 126.6(13) . . ? N10 C9 C8 125.4(15) . . ? N1 C9 C8 108.0(13) . . ? C9 N10 C12 125.5(11) . . ? C12 N11 C19 108.0(11) . . ? C12 N11 In 122.2(10) . . ? C19 N11 In 125.7(10) . . ? N10 C12 N11 129.2(14) . . ? N10 C12 C13 123.6(14) . . ? N11 C12 C13 107.2(13) . . ? C18 C13 C14 117.6(15) . . ? C18 C13 C12 108.9(14) . . ? C14 C13 C12 133.5(14) . . ? C15 C14 C13 116.2(12) . . ? C15 C14 C141 120.4(16) . . ? C13 C14 C141 123.4(15) . . ? C16 C15 C14 121.4(13) . . ? C16 C15 H15 119.3 . . ? C14 C15 H15 119.3 . . ? C17 C16 C15 125.0(15) . . ? C17 C16 H16 117.5 . . ? C15 C16 H16 117.5 . . ? C16 C17 C18 114.2(16) . . ? C16 C17 C171 119.7(16) . . ? C18 C17 C171 126.0(14) . . ? C17 C18 C13 125.2(14) . . ? C17 C18 C19 130.6(16) . . ? C13 C18 C19 104.2(15) . . ? N20 C19 N11 123.2(14) . . ? N20 C19 C18 125.0(14) . . ? N11 C19 C18 111.6(12) . . ? C22 N20 C19 127.0(12) . . ? C29 N21 C22 111.3(12) . . ? C29 N21 In 122.7(11) . . ? C22 N21 In 123.8(8) . . ? N20 C22 N21 127.8(12) . . ? N20 C22 C23 126.1(16) . . ? N21 C22 C23 106.1(14) . . ? C24 C23 C28 121.3(14) . . ? C24 C23 C22 131(2) . . ? C28 C23 C22 107.9(16) . . ? C23 C24 C25 116.1(15) . . ? C23 C24 C241 122.8(17) . . ? C25 C24 C241 121.1(18) . . ? C26 C25 C24 121.5(15) . . ? C26 C25 H25 119.2 . . ? C24 C25 H25 119.2 . . ? C27 C26 C25 124.8(15) . . ? C27 C26 H26 117.6 . . ? C25 C26 H26 117.6 . . ? C26 C27 C28 113.7(16) . . ? C26 C27 C271 121.2(15) . . ? C28 C27 C271 124.7(17) . . ? C23 C28 C27 122.4(15) . . ? C23 C28 C29 106.9(15) . . ? C27 C28 C29 130.7(19) . . ? N30 C29 N21 126.9(13) . . ? N30 C29 C28 125.2(15) . . ? N21 C29 C28 107.7(13) . . ? C29 N30 C32 128.1(11) . . ? C39 N31 C32 106.6(11) . . ? C39 N31 In 126.4(9) . . ? C32 N31 In 125.7(10) . . ? N30 C32 N31 123.5(14) . . ? N30 C32 C33 126.6(13) . . ? N31 C32 C33 109.8(13) . . ? C38 C33 C34 122.8(15) . . ? C38 C33 C32 106.7(13) . . ? C34 C33 C32 130.4(15) . . ? C35 C34 C33 112.6(14) . . ? C35 C34 C341 124.3(15) . . ? C33 C34 C341 123.1(16) . . ? C34 C35 C36 125.6(14) . . ? C34 C35 H35 117.2 . . ? C36 C35 H35 117.2 . . ? C35 C36 C37 122.3(15) . . ? C35 C36 H36 118.8 . . ? C37 C36 H36 118.8 . . ? C36 C37 C38 114.9(14) . . ? C36 C37 C371 122.0(17) . . ? C38 C37 C371 123.1(15) . . ? C33 C38 C37 121.7(14) . . ? C33 C38 C39 105.9(14) . . ? C37 C38 C39 132.4(15) . . ? N40 C39 N31 126.6(13) . . ? N40 C39 C38 122.5(14) . . ? N31 C39 C38 110.8(12) . . ? C39 N40 C2 126.2(11) . . ? C4 C41 C42 116.3(11) . . ? C4 C41 H41A 108.2 . . ? C42 C41 H41A 108.2 . . ? C4 C41 H41B 108.2 . . ? C42 C41 H41B 108.2 . . ? H41A C41 H41B 107.4 . . ? C43 C42 C41 116.0(12) . . ? C43 C42 H42A 108.3 . . ? C41 C42 H42A 108.3 . . ? C43 C42 H42B 108.3 . . ? C41 C42 H42B 108.3 . . ? H42A C42 H42B 107.4 . . ? C42 C43 C44 115.0(12) . . ? C42 C43 H43A 108.5 . . ? C44 C43 H43A 108.5 . . ? C42 C43 H43B 108.5 . . ? C44 C43 H43B 108.5 . . ? H43A C43 H43B 107.5 . . ? C45 C44 C43 112.0(12) . . ? C45 C44 H44A 109.2 . . ? C43 C44 H44A 109.2 . . ? C45 C44 H44B 109.2 . . ? C43 C44 H44B 109.2 . . ? H44A C44 H44B 107.9 . . ? C44 C45 C46 110.2(12) . . ? C44 C45 H45A 109.6 . . ? C46 C45 H45A 109.6 . . ? C44 C45 H45B 109.6 . . ? C46 C45 H45B 109.6 . . ? H45A C45 H45B 108.1 . . ? 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 . . ? C7 C71 C72 116.4(11) . . ? C7 C71 H71A 108.2 . . ? C72 C71 H71A 108.2 . . ? C7 C71 H71B 108.2 . . ? C72 C71 H71B 108.2 . . ? H71A C71 H71B 107.3 . . ? C73 C72 C71 111.8(11) . . ? C73 C72 H72A 109.3 . . ? C71 C72 H72A 109.3 . . ? C73 C72 H72B 109.3 . . ? C71 C72 H72B 109.3 . . ? H72A C72 H72B 107.9 . . ? C72 C73 C74 111.4(12) . . ? C72 C73 H73A 109.3 . . ? C74 C73 H73A 109.3 . . ? C72 C73 H73B 109.3 . . ? C74 C73 H73B 109.3 . . ? H73A C73 H73B 108.0 . . ? C75 C74 C73 111.5(14) . . ? C75 C74 H74A 109.3 . . ? C73 C74 H74A 109.3 . . ? C75 C74 H74B 109.3 . . ? C73 C74 H74B 109.3 . . ? H74A C74 H74B 108.0 . . ? C76 C75 C74 111.1(18) . . ? C76 C75 H75A 109.4 . . ? C74 C75 H75A 109.4 . . ? C76 C75 H75B 109.4 . . ? C74 C75 H75B 109.4 . . ? H75A C75 H75B 108.0 . . ? C75 C76 H76A 109.5 . . ? C75 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C75 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C142 C141 C14 114.4(11) . . ? C142 C141 H14A 108.7 . . ? C14 C141 H14A 108.7 . . ? C142 C141 H14B 108.7 . . ? C14 C141 H14B 108.7 . . ? H14A C141 H14B 107.6 . . ? C143 C142 C141 128.0(19) . . ? C143 C142 H14C 105.3 . . ? C141 C142 H14C 105.3 . . ? C143 C142 H14D 105.3 . . ? C141 C142 H14D 105.3 . . ? H14C C142 H14D 106.0 . . ? C142 C143 C144 125(2) . . ? C142 C143 H14E 106.2 . . ? C144 C143 H14E 106.2 . . ? C142 C143 H14F 106.2 . . ? C144 C143 H14F 106.2 . . ? H14E C143 H14F 106.4 . . ? C145 C144 C143 116(2) . . ? C145 C144 H14G 108.3 . . ? C143 C144 H14G 108.3 . . ? C145 C144 H14H 108.3 . . ? C143 C144 H14H 108.3 . . ? H14G C144 H14H 107.4 . . ? C144 C145 C146 112(2) . . ? C144 C145 H14I 109.3 . . ? C146 C145 H14I 109.3 . . ? C144 C145 H14J 109.3 . . ? C146 C145 H14J 109.3 . . ? H14I C145 H14J 108.0 . . ? C145 C146 H14K 109.5 . . ? C145 C146 H14L 109.5 . . ? H14K C146 H14L 109.5 . . ? C145 C146 H14M 109.5 . . ? H14K C146 H14M 109.5 . . ? H14L C146 H14M 109.5 . . ? C172 C171 C17 111.0(14) . . ? C172 C171 C672 38.3(14) . . ? C17 C171 C672 105.5(15) . . ? C672 C172 C171 86(3) . . ? C672 C172 C673 60(3) . . ? C171 C172 C673 125(3) . . ? C672 C172 C173 34(2) . . ? C171 C172 C173 106(2) . . ? C673 C172 C173 26.5(17) . . ? C173 C672 C172 107(4) . . ? C173 C672 C673 34(3) . . ? C172 C672 C673 75(3) . . ? C173 C672 C171 130(4) . . ? C172 C672 C171 56(2) . . ? C673 C672 C171 114(3) . . ? C673 C173 C672 99(6) . . ? C673 C173 C172 62(5) . . ? C672 C173 C172 39(3) . . ? C673 C173 C174 66(4) . . ? C672 C173 C174 122(4) . . ? C172 C173 C174 110(2) . . ? C173 C673 C174 85(5) . . ? C173 C673 C672 47(4) . . ? C174 C673 C672 108(3) . . ? C173 C673 C172 92(5) . . ? C174 C673 C172 131(3) . . ? C672 C673 C172 45(2) . . ? C175 C174 C673 127(3) . . ? C175 C174 C675 47.3(14) . . ? C673 C174 C675 116(2) . . ? C175 C174 C173 108(2) . . ? C673 C174 C173 29.4(18) . . ? C675 C174 C173 123(2) . . ? C675 C175 C174 77(2) . . ? C675 C175 C176 56.2(18) . . ? C174 C175 C176 110(2) . . ? C175 C675 C176 81(2) . . ? C175 C675 C174 55.4(19) . . ? C176 C675 C174 113(2) . . ? C675 C176 C175 42.6(13) . . ? C242 C241 C24 118.1(13) . . ? C242 C241 H24A 107.8 . . ? C24 C241 H24A 107.8 . . ? C242 C241 H24B 107.8 . . ? C24 C241 H24B 107.8 . . ? H24A C241 H24B 107.1 . . ? C243 C242 C241 115.2(13) . . ? C243 C242 H24C 108.5 . . ? C241 C242 H24C 108.5 . . ? C243 C242 H24D 108.5 . . ? C241 C242 H24D 108.5 . . ? H24C C242 H24D 107.5 . . ? C242 C243 C244 111.9(13) . . ? C242 C243 H24E 109.2 . . ? C244 C243 H24E 109.2 . . ? C242 C243 H24F 109.2 . . ? C244 C243 H24F 109.2 . . ? H24E C243 H24F 107.9 . . ? C245 C244 C243 118.5(16) . . ? C245 C244 H24G 107.7 . . ? C243 C244 H24G 107.7 . . ? C245 C244 H24H 107.7 . . ? C243 C244 H24H 107.7 . . ? H24G C244 H24H 107.1 . . ? C244 C245 C246 115.3(16) . . ? C244 C245 H24I 108.5 . . ? C246 C245 H24I 108.5 . . ? C244 C245 H24J 108.5 . . ? C246 C245 H24J 108.5 . . ? H24I C245 H24J 107.5 . . ? C245 C246 H24K 109.5 . . ? C245 C246 H24L 109.5 . . ? H24K C246 H24L 109.5 . . ? C245 C246 H24M 109.5 . . ? H24K C246 H24M 109.5 . . ? H24L C246 H24M 109.5 . . ? C27 C271 C272 116.2(14) . . ? C27 C271 H27A 108.2 . . ? C272 C271 H27A 108.2 . . ? C27 C271 H27B 108.2 . . ? C272 C271 H27B 108.2 . . ? H27A C271 H27B 107.4 . . ? C273 C272 C271 114(2) . . ? C273 C272 H27C 108.8 . . ? C271 C272 H27C 108.8 . . ? C273 C272 H27D 108.8 . . ? C271 C272 H27D 108.8 . . ? H27C C272 H27D 107.7 . . ? C272 C273 C274 109(3) . . ? C272 C273 H27E 109.9 . . ? C274 C273 H27E 109.9 . . ? C272 C273 H27F 109.9 . . ? C274 C273 H27F 109.9 . . ? H27E C273 H27F 108.3 . . ? C275 C274 C273 120(3) . . ? C275 C274 H27G 107.4 . . ? C273 C274 H27G 107.4 . . ? C275 C274 H27H 107.4 . . ? C273 C274 H27H 107.4 . . ? H27G C274 H27H 106.9 . . ? C274 C275 C276 121(3) . . ? C274 C275 H27I 107.1 . . ? C276 C275 H27I 107.1 . . ? C274 C275 H27J 107.1 . . ? C276 C275 H27J 107.1 . . ? H27I C275 H27J 106.8 . . ? C275 C276 H27K 109.5 . . ? C275 C276 H27L 109.5 . . ? H27K C276 H27L 109.5 . . ? C275 C276 H27M 109.5 . . ? H27K C276 H27M 109.5 . . ? H27L C276 H27M 109.5 . . ? C34 C341 C342 110.3(12) . . ? C843 C342 C343 38.6(18) . . ? C843 C342 C341 112(2) . . ? C343 C342 C341 104.0(16) . . ? C843 C343 C342 65(3) . . ? C843 C343 C344 77(4) . . ? C342 C343 C344 109(2) . . ? C343 C843 C342 77(3) . . ? C343 C843 C844 104(5) . . ? C342 C843 C844 116(4) . . ? C343 C843 C344 71(4) . . ? C342 C843 C344 111(3) . . ? C844 C843 C344 34(2) . . ? C844 C344 C345 55(4) . . ? C844 C344 C845 110(6) . . ? C345 C344 C845 55(4) . . ? C844 C344 C343 101(5) . . ? C345 C344 C343 115(4) . . ? C845 C344 C343 107(4) . . ? C844 C344 C843 69(4) . . ? C345 C344 C843 98(4) . . ? C845 C344 C843 122(3) . . ? C343 C344 C843 32.3(17) . . ? C344 C844 C345 73(5) . . ? C344 C844 C843 77(5) . . ? C345 C844 C843 111(6) . . ? C344 C844 C845 40(4) . . ? C345 C844 C845 33(4) . . ? C843 C844 C845 96(3) . . ? C844 C345 C845 117(7) . . ? C844 C345 C344 52(4) . . ? C845 C345 C344 65(4) . . ? C844 C345 C346 125(6) . . ? C845 C345 C346 59(3) . . ? C344 C345 C346 98(4) . . ? C345 C845 C344 60(3) . . ? C345 C845 C346 81(3) . . ? C344 C845 C346 108(3) . . ? C345 C845 C844 30(4) . . ? C344 C845 C844 30(3) . . ? C346 C845 C844 95(3) . . ? C845 C346 C345 40(2) . . ? C37 C371 C372 117.5(12) . . ? C37 C371 H37A 107.9 . . ? C372 C371 H37A 107.9 . . ? C37 C371 H37B 107.9 . . ? C372 C371 H37B 107.9 . . ? H37A C371 H37B 107.2 . . ? C373 C372 C371 115.4(11) . . ? C373 C372 H37C 108.4 . . ? C371 C372 H37C 108.4 . . ? C373 C372 H37D 108.4 . . ? C371 C372 H37D 108.4 . . ? H37C C372 H37D 107.5 . . ? C372 C373 C374 115.4(12) . . ? C372 C373 H37E 108.4 . . ? C374 C373 H37E 108.4 . . ? C372 C373 H37F 108.4 . . ? C374 C373 H37F 108.4 . . ? H37E C373 H37F 107.5 . . ? C375 C374 C373 113.0(15) . . ? C375 C374 H37G 109.0 . . ? C373 C374 H37G 109.0 . . ? C375 C374 H37H 109.0 . . ? C373 C374 H37H 109.0 . . ? H37G C374 H37H 107.8 . . ? C376 C375 C374 116(2) . . ? C376 C375 H37I 108.3 . . ? C374 C375 H37I 108.3 . . ? C376 C375 H37J 108.3 . . ? C374 C375 H37J 108.3 . . ? H37I C375 H37J 107.4 . . ? C375 C376 H37K 109.5 . . ? C375 C376 H37L 109.5 . . ? H37K C376 H37L 109.5 . . ? C375 C376 H37M 109.5 . . ? H37K C376 H37M 109.5 . . ? H37L C376 H37M 109.5 . . ? C52 C51 C56 114.8(13) . . ? C52 C51 In 121.6(13) . . ? C56 C51 In 123.5(13) . . ? C53 C52 C51 121.5(16) . . ? C53 C52 H52 119.3 . . ? C51 C52 H52 119.3 . . ? C54 C53 C52 123(3) . . ? C54 C53 H53 118.7 . . ? C52 C53 H53 118.6 . . ? C53 C54 F57 124(4) . . ? C53 C54 C55 121(3) . . ? F57 C54 C55 115(4) . . ? C54 C55 C56 118(3) . . ? C54 C55 H55 121.2 . . ? C56 C55 H55 121.2 . . ? C51 C56 C55 122.4(17) . . ? C51 C56 H56 118.8 . . ? C55 C56 H56 118.8 . . ? _diffrn_measured_fraction_theta_max 0.930 _diffrn_reflns_theta_full 20.00 _diffrn_measured_fraction_theta_full 0.930 _refine_diff_density_max 0.264 _refine_diff_density_min -0.197 _refine_diff_density_rms 0.053 # #===END # data_aura3 _database_code_depnum_ccdc_archive 'CCDC 248918' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Compound 3' _chemical_melting_point ? _chemical_formula_moiety 'C76 H103 Br Cl In N8 O2' _chemical_formula_structural '[InCl(hexa-hexyl-dibutoxy,Br-phthalocyanine)]' _chemical_formula_sum 'C76 H103 Br Cl In N8 O2' _chemical_formula_weight 1390.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.694(3) _cell_length_b 17.033(3) _cell_length_c 17.996(4) _cell_angle_alpha 108.54(3) _cell_angle_beta 103.32(3) _cell_angle_gamma 92.96(3) _cell_volume 3556.8(12) _cell_formula_units_Z 2 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour 'fine, green' _exptl_crystal_size_max 1.4 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.299 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1464 _exptl_absorpt_coefficient_mu 0.982 _exptl_absorpt_correction_type 'not applied' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku R-Axis-IIc' _diffrn_measurement_method 'image-plate oscillation photos' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 19249 _diffrn_reflns_av_R_equivalents 0.0935 _diffrn_reflns_av_sigmaI/netI 0.1490 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.24 _diffrn_reflns_theta_max 25.35 _reflns_number_total 11790 _reflns_number_gt 6567 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'MSC R-Axis-II control software' _computing_cell_refinement 'DENZO/CELL (Otwinowski and Minor, 1985)' _computing_data_reduction 'DENZO, SCALEPACK (Otwinowski and Minor, 1985)' _computing_structure_solution 'SHELXS (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL (Sheldrick, 1997)' _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^)+(0.0900P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11790 _refine_ls_number_parameters 803 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1258 _refine_ls_R_factor_gt 0.0682 _refine_ls_wR_factor_ref 0.1885 _refine_ls_wR_factor_gt 0.1707 _refine_ls_goodness_of_fit_ref 0.936 _refine_ls_restrained_S_all 0.936 _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 In In 0.24757(4) 0.46986(3) 0.30812(3) 0.03957(17) Uani 1 1 d . . . Cl Cl 0.14493(17) 0.56855(14) 0.27023(13) 0.0684(6) Uani 1 1 d . . . Br5 Br 0.51161(7) 0.33033(6) -0.10171(5) 0.0658(3) Uani 0.95 1 d P . . N1 N 0.3511(4) 0.4391(3) 0.2266(3) 0.0411(13) Uani 1 1 d . . . C2 C 0.3168(5) 0.3823(4) 0.1485(4) 0.0400(16) Uani 1 1 d . B . C3 C 0.3990(5) 0.3935(4) 0.1067(4) 0.0424(16) Uani 1 1 d . . . C4 C 0.4068(5) 0.3516(5) 0.0257(4) 0.0460(17) Uani 1 1 d . . . C5 C 0.4973(6) 0.3806(5) 0.0069(4) 0.0512(19) Uani 1 1 d . . . C6 C 0.5788(6) 0.4423(5) 0.0596(4) 0.0468(18) Uani 1 1 d . . . H6 H 0.6384 0.4568 0.0425 0.056 Uiso 1 1 calc R . . C7 C 0.5732(5) 0.4841(4) 0.1400(4) 0.0454(17) Uani 1 1 d . . . C8 C 0.4804(5) 0.4580(4) 0.1616(4) 0.0408(16) Uani 1 1 d . . . C9 C 0.4485(5) 0.4858(4) 0.2391(4) 0.0372(15) Uani 1 1 d . . . N10 N 0.5079(4) 0.5449(3) 0.3070(3) 0.0421(14) Uani 1 1 d . . . N11 N 0.3963(4) 0.5336(3) 0.3976(3) 0.0382(13) Uani 1 1 d . . . C12 C 0.4854(5) 0.5665(4) 0.3802(4) 0.0394(16) Uani 1 1 d . . . C13 C 0.5542(5) 0.6268(4) 0.4535(4) 0.0393(16) Uani 1 1 d . . . C14 C 0.6505(5) 0.6801(4) 0.4680(4) 0.0431(16) Uani 1 1 d . . . C15 C 0.6959(5) 0.7284(4) 0.5485(4) 0.0475(17) Uani 1 1 d . . . H15 H 0.7603 0.7640 0.5608 0.057 Uiso 1 1 calc R . . C16 C 0.6514(5) 0.7274(4) 0.6127(4) 0.0460(17) Uani 1 1 d . . . H16 H 0.6883 0.7605 0.6654 0.055 Uiso 1 1 calc R . . C17 C 0.5540(5) 0.6784(4) 0.5999(4) 0.0376(15) Uani 1 1 d . . . C18 C 0.5060(5) 0.6264(4) 0.5184(4) 0.0414(16) Uani 1 1 d . . . C19 C 0.4058(5) 0.5682(4) 0.4796(4) 0.0379(15) Uani 1 1 d . . . N20 N 0.3354(4) 0.5511(3) 0.5208(3) 0.0354(12) Uani 1 1 d . . . N21 N 0.2082(4) 0.4424(3) 0.4071(3) 0.0366(12) Uani 1 1 d . . . C22 C 0.2451(5) 0.4941(4) 0.4882(4) 0.0378(15) Uani 1 1 d . . . C23 C 0.1730(5) 0.4750(4) 0.5329(4) 0.0367(15) Uani 1 1 d . . . C24 C 0.1686(5) 0.5126(4) 0.6146(4) 0.0385(15) Uani 1 1 d . . . C25 C 0.0820(5) 0.4775(4) 0.6350(4) 0.0451(17) Uani 1 1 d . . . H25 H 0.0758 0.5000 0.6879 0.054 Uiso 1 1 calc R . . C26 C 0.0055(5) 0.4118(5) 0.5815(4) 0.0473(18) Uani 1 1 d . . . H26 H -0.0507 0.3931 0.5996 0.057 Uiso 1 1 calc R . . C27 C 0.0085(5) 0.3724(4) 0.5018(4) 0.0400(16) Uani 1 1 d . . . C28 C 0.0952(5) 0.4076(4) 0.4788(4) 0.0402(16) Uani 1 1 d . . . C29 C 0.1214(5) 0.3869(4) 0.3992(4) 0.0398(15) Uani 1 1 d . . . N30 N 0.0695(4) 0.3218(4) 0.3333(3) 0.0410(13) Uani 1 1 d . . . N31 N 0.1659(4) 0.3447(3) 0.2380(3) 0.0407(13) Uani 1 1 d . . . C32 C 0.0921(5) 0.3012(4) 0.2612(4) 0.0406(16) Uani 1 1 d . . . C33 C 0.0384(5) 0.2267(4) 0.1898(4) 0.0434(17) Uani 1 1 d . B . C34 C -0.0380(5) 0.1593(5) 0.1816(4) 0.0485(17) Uani 1 1 d . . . C35 C -0.0721(6) 0.0998(5) 0.1035(4) 0.0554(19) Uani 1 1 d . B . H35 H -0.1216 0.0534 0.0945 0.067 Uiso 1 1 calc R . . C36 C -0.0343(6) 0.1073(5) 0.0382(5) 0.056(2) Uani 1 1 d . . . H36 H -0.0611 0.0662 -0.0125 0.068 Uiso 1 1 calc R A 1 Br36 Br -0.0990(18) 0.0494(16) -0.0677(15) 0.102(7) Uiso 0.05 1 d P B 1 C37 C 0.0401(5) 0.1724(5) 0.0460(4) 0.0468(17) Uani 1 1 d . B . C38 C 0.0789(5) 0.2315(5) 0.1249(4) 0.0464(17) Uani 1 1 d . . . C39 C 0.1627(5) 0.3047(4) 0.1571(4) 0.0433(16) Uani 1 1 d . B . N40 N 0.2315(4) 0.3241(4) 0.1180(3) 0.0422(13) Uani 1 1 d . . . O4 O 0.3225(4) 0.2927(3) -0.0299(3) 0.0530(12) Uani 1 1 d . . . C41 C 0.3468(6) 0.2078(5) -0.0462(5) 0.069(2) Uani 1 1 d . D . H41A H 0.3187 0.1827 -0.0120 0.082 Uiso 1 1 calc R . . H41B H 0.4251 0.2071 -0.0350 0.082 Uiso 1 1 calc R . . C42 C 0.2927(8) 0.1596(6) -0.1349(6) 0.091(3) Uani 1 1 d . . . H42A H 0.3217 0.1814 -0.1709 0.109 Uiso 0.50 1 calc PR C 1 H42B H 0.2139 0.1577 -0.1478 0.109 Uiso 0.50 1 calc PR C 1 H54A H 0.2144 0.1597 -0.1440 0.109 Uiso 0.50 1 calc PR C 2 H54B H 0.3171 0.1889 -0.1674 0.109 Uiso 0.50 1 calc PR C 2 C43 C 0.337(2) 0.0535(16) -0.1362(16) 0.104(8) Uiso 0.50 1 d P D 1 H43A H 0.4128 0.0597 -0.1054 0.124 Uiso 0.50 1 calc PR D 1 H43B H 0.2909 0.0242 -0.1149 0.124 Uiso 0.50 1 calc PR D 1 C44 C 0.3245(17) 0.0110(15) -0.2222(14) 0.099(6) Uiso 0.50 1 d P D 1 H44A H 0.3700 0.0422 -0.2417 0.148 Uiso 0.50 1 calc PR D 1 H44B H 0.2495 0.0066 -0.2511 0.148 Uiso 0.50 1 calc PR D 1 H44C H 0.3453 -0.0439 -0.2307 0.148 Uiso 0.50 1 calc PR D 1 C543 C 0.3133(18) 0.0761(16) -0.1627(15) 0.092(7) Uiso 0.50 1 d P D 2 H54C H 0.2751 0.0432 -0.1394 0.110 Uiso 0.50 1 calc PR D 2 H54D H 0.3909 0.0741 -0.1446 0.110 Uiso 0.50 1 calc PR D 2 C544 C 0.2748(19) 0.0368(16) -0.2589(15) 0.120(8) Uiso 0.50 1 d P D 2 H54E H 0.3117 0.0698 -0.2821 0.180 Uiso 0.50 1 calc PR D 2 H54F H 0.1973 0.0362 -0.2768 0.180 Uiso 0.50 1 calc PR D 2 H54G H 0.2921 -0.0193 -0.2760 0.180 Uiso 0.50 1 calc PR D 2 O7 O 0.6495(4) 0.5463(3) 0.1951(3) 0.0517(12) Uani 1 1 d . . . C71 C 0.7402(6) 0.5737(5) 0.1673(5) 0.055(2) Uani 1 1 d . . . H71A H 0.7119 0.5881 0.1193 0.066 Uiso 1 1 calc R . . H71B H 0.7838 0.5287 0.1535 0.066 Uiso 1 1 calc R . . C72 C 0.8093(6) 0.6479(5) 0.2333(5) 0.059(2) Uani 1 1 d . . . H72A H 0.8339 0.6334 0.2819 0.071 Uiso 1 1 calc R . . H72B H 0.7651 0.6927 0.2457 0.071 Uiso 1 1 calc R . . C73 C 0.9069(6) 0.6785(6) 0.2116(5) 0.074(3) Uani 1 1 d . . . H73A H 0.8822 0.6923 0.1626 0.089 Uiso 1 1 calc R . . H73B H 0.9515 0.6338 0.1999 0.089 Uiso 1 1 calc R . . C74 C 0.9773(7) 0.7556(6) 0.2791(5) 0.090(3) Uani 1 1 d . . . H74A H 1.0388 0.7719 0.2621 0.135 Uiso 1 1 calc R . . H74B H 1.0028 0.7422 0.3275 0.135 Uiso 1 1 calc R . . H74C H 0.9344 0.8007 0.2897 0.135 Uiso 1 1 calc R . . C141 C 0.6997(5) 0.6914(5) 0.4021(4) 0.0492(18) Uani 1 1 d . . . H14A H 0.6775 0.6417 0.3541 0.059 Uiso 1 1 calc R . . H14B H 0.7788 0.6994 0.4208 0.059 Uiso 1 1 calc R . . C142 C 0.6606(6) 0.7685(5) 0.3809(5) 0.061(2) Uani 1 1 d . . . H14C H 0.6762 0.8164 0.4305 0.073 Uiso 1 1 calc R . . H14D H 0.7019 0.7808 0.3459 0.073 Uiso 1 1 calc R . . C143 C 0.5393(7) 0.7562(6) 0.3389(5) 0.072(2) Uani 1 1 d . . . H14E H 0.5226 0.7054 0.2919 0.086 Uiso 1 1 calc R . . H14F H 0.4979 0.7486 0.3758 0.086 Uiso 1 1 calc R . . C144 C 0.5021(8) 0.8281(6) 0.3117(5) 0.079(3) Uani 1 1 d . . . H14G H 0.5343 0.8308 0.2685 0.095 Uiso 1 1 calc R . . H14H H 0.5269 0.8802 0.3567 0.095 Uiso 1 1 calc R . . C145 C 0.3699(10) 0.8160(7) 0.2795(7) 0.131(5) Uani 1 1 d . . . H14I H 0.3451 0.7622 0.2368 0.158 Uiso 1 1 calc R . . H14J H 0.3380 0.8165 0.3237 0.158 Uiso 1 1 calc R . . C146 C 0.3325(15) 0.8819(10) 0.2484(9) 0.198(8) Uani 1 1 d . . . H14K H 0.2541 0.8756 0.2342 0.297 Uiso 1 1 calc R . . H14L H 0.3577 0.8779 0.2012 0.297 Uiso 1 1 calc R . . H14M H 0.3610 0.9354 0.2894 0.297 Uiso 1 1 calc R . . C171 C 0.5014(5) 0.6773(4) 0.6666(4) 0.0449(17) Uani 1 1 d . . . H17A H 0.4995 0.6217 0.6704 0.054 Uiso 1 1 calc R . . H17B H 0.4264 0.6878 0.6515 0.054 Uiso 1 1 calc R . . C172 C 0.5585(5) 0.7413(4) 0.7513(4) 0.0486(17) Uani 1 1 d . . . H17C H 0.5361 0.7235 0.7922 0.058 Uiso 1 1 calc R . . H17D H 0.6369 0.7411 0.7605 0.058 Uiso 1 1 calc R . . C173 C 0.5339(6) 0.8299(5) 0.7622(4) 0.0531(18) Uani 1 1 d . . . H17E H 0.4554 0.8285 0.7446 0.064 Uiso 1 1 calc R . . H17F H 0.5662 0.8504 0.7269 0.064 Uiso 1 1 calc R . . C174 C 0.5747(6) 0.8917(5) 0.8482(6) 0.074(2) Uani 1 1 d . . . H17G H 0.5391 0.8730 0.8830 0.089 Uiso 1 1 calc R . . H17H H 0.5524 0.9454 0.8486 0.089 Uiso 1 1 calc R . . C175 C 0.6979(7) 0.9039(6) 0.8843(5) 0.073(2) Uani 1 1 d . . . H17I H 0.7152 0.9420 0.9399 0.087 Uiso 1 1 calc R . . H17J H 0.7206 0.8507 0.8854 0.087 Uiso 1 1 calc R . . C176 C 0.7614(7) 0.9380(6) 0.8379(6) 0.083(3) Uani 1 1 d . . . H17K H 0.8382 0.9429 0.8624 0.125 Uiso 1 1 calc R . . H17L H 0.7421 0.9920 0.8389 0.125 Uiso 1 1 calc R . . H17M H 0.7446 0.9008 0.7827 0.125 Uiso 1 1 calc R . . C241 C 0.2510(5) 0.5849(4) 0.6765(4) 0.0452(17) Uani 1 1 d . . . H24A H 0.2608 0.6271 0.6522 0.054 Uiso 1 1 calc R . . H24B H 0.3208 0.5648 0.6892 0.054 Uiso 1 1 calc R . . C242 C 0.2193(5) 0.6256(4) 0.7555(4) 0.0457(17) Uani 1 1 d . . . H24C H 0.1467 0.6415 0.7429 0.055 Uiso 1 1 calc R . . H24D H 0.2165 0.5851 0.7829 0.055 Uiso 1 1 calc R . . C243 C 0.2979(5) 0.7017(5) 0.8120(4) 0.0501(18) Uani 1 1 d . . . H24E H 0.2957 0.7440 0.7863 0.060 Uiso 1 1 calc R . . H24F H 0.3713 0.6868 0.8203 0.060 Uiso 1 1 calc R . . C244 C 0.2737(6) 0.7394(5) 0.8950(4) 0.0522(19) Uani 1 1 d . . . H24G H 0.1978 0.7487 0.8864 0.063 Uiso 1 1 calc R . . H24H H 0.2835 0.6991 0.9231 0.063 Uiso 1 1 calc R . . C245 C 0.3447(6) 0.8207(5) 0.9490(5) 0.066(2) Uani 1 1 d . . . H24I H 0.3278 0.8635 0.9248 0.079 Uiso 1 1 calc R . . H24J H 0.4208 0.8137 0.9522 0.079 Uiso 1 1 calc R . . C246 C 0.3282(7) 0.8498(6) 1.0349(5) 0.080(3) Uani 1 1 d . . . H24K H 0.3744 0.9017 1.0667 0.120 Uiso 1 1 calc R . . H24L H 0.3468 0.8084 1.0597 0.120 Uiso 1 1 calc R . . H24M H 0.2532 0.8576 1.0320 0.120 Uiso 1 1 calc R . . C271 C -0.0742(5) 0.2987(4) 0.4456(4) 0.0484(18) Uani 1 1 d . . . H27A H -0.0359 0.2508 0.4296 0.058 Uiso 1 1 calc R . . H27B H -0.1072 0.3108 0.3969 0.058 Uiso 1 1 calc R . . C272 C -0.1645(5) 0.2747(4) 0.4793(4) 0.0474(17) Uani 1 1 d . . . H27C H -0.2058 0.3213 0.4920 0.057 Uiso 1 1 calc R . . H27D H -0.1314 0.2662 0.5299 0.057 Uiso 1 1 calc R . . C273 C -0.2433(5) 0.1974(5) 0.4247(5) 0.0535(19) Uani 1 1 d . . . H27E H -0.2036 0.1495 0.4156 0.064 Uiso 1 1 calc R . . H27F H -0.2730 0.2037 0.3725 0.064 Uiso 1 1 calc R . . C274 C -0.3381(5) 0.1802(5) 0.4597(5) 0.0543(19) Uani 1 1 d . . . H27G H -0.3079 0.1847 0.5158 0.065 Uiso 1 1 calc R . . H27H H -0.3844 0.2237 0.4598 0.065 Uiso 1 1 calc R . . C275 C -0.4076(6) 0.0980(5) 0.4169(5) 0.062(2) Uani 1 1 d . . . H27I H -0.3632 0.0540 0.4204 0.075 Uiso 1 1 calc R . . H27J H -0.4345 0.0914 0.3599 0.075 Uiso 1 1 calc R . . C276 C -0.5046(7) 0.0876(6) 0.4510(6) 0.086(3) Uani 1 1 d . . . H27K H -0.5464 0.0336 0.4207 0.128 Uiso 1 1 calc R . . H27L H -0.5498 0.1303 0.4469 0.128 Uiso 1 1 calc R . . H27M H -0.4787 0.0924 0.5070 0.128 Uiso 1 1 calc R . . C341 C -0.0789(6) 0.1460(5) 0.2467(4) 0.0569(19) Uani 1 1 d . . . H34A H -0.1463 0.1075 0.2223 0.068 Uiso 1 1 calc R . . H34B H -0.0966 0.1988 0.2786 0.068 Uiso 1 1 calc R . . C342 C -0.0005(8) 0.1114(6) 0.3052(6) 0.084(3) Uani 1 1 d . . . H34C H 0.0680 0.1487 0.3282 0.101 Uiso 1 1 calc R . . H34D H -0.0322 0.1122 0.3496 0.101 Uiso 1 1 calc R . . C343 C 0.0219(9) 0.0300(8) 0.2694(7) 0.109(4) Uani 1 1 d . . . H34E H 0.0474 0.0276 0.2220 0.130 Uiso 1 1 calc R . . H34F H -0.0453 -0.0084 0.2513 0.130 Uiso 1 1 calc R . . C344 C 0.1113(13) 0.0002(9) 0.3294(10) 0.166(6) Uani 1 1 d . F . H34G H 0.1212 -0.0567 0.3015 0.199 Uiso 1 1 calc R . . H34H H 0.1806 0.0353 0.3433 0.199 Uiso 1 1 calc R . . C345 C 0.0818(14) 0.0039(11) 0.4039(10) 0.184(8) Uani 1 1 d . . . H34I H 0.0146 -0.0325 0.3929 0.221 Uiso 0.60 1 calc PR E 1 H34J H 0.0746 0.0605 0.4351 0.221 Uiso 0.60 1 calc PR E 1 H84A H 0.0053 -0.0197 0.3856 0.221 Uiso 0.40 1 calc PR E 2 H84B H 0.0829 0.0631 0.4315 0.221 Uiso 0.40 1 calc PR E 2 C346 C 0.1892(19) -0.0301(16) 0.4509(16) 0.147(9) Uiso 0.60 1 d P F 1 H34K H 0.1802 -0.0307 0.5022 0.221 Uiso 0.60 1 calc PR F 1 H34L H 0.2544 0.0064 0.4595 0.221 Uiso 0.60 1 calc PR F 1 H34M H 0.1949 -0.0857 0.4180 0.221 Uiso 0.60 1 calc PR F 1 C846 C 0.128(3) -0.029(3) 0.472(3) 0.161(15) Uiso 0.40 1 d P F 2 H84C H 0.0869 -0.0140 0.5113 0.241 Uiso 0.40 1 calc PR F 2 H84D H 0.2031 -0.0043 0.4965 0.241 Uiso 0.40 1 calc PR F 2 H84E H 0.1241 -0.0883 0.4500 0.241 Uiso 0.40 1 calc PR F 2 C371 C 0.0674(6) 0.1819(5) -0.0273(4) 0.057(2) Uani 1 1 d . B 2 H37A H 0.0755 0.1277 -0.0631 0.069 Uiso 1 1 calc R B 2 H37B H 0.1364 0.2178 -0.0109 0.069 Uiso 1 1 calc R B 2 C372 C -0.0210(6) 0.2192(5) -0.0727(5) 0.062(2) Uani 1 1 d . B 2 H37C H -0.0023 0.2217 -0.1213 0.074 Uiso 1 1 calc R B 2 H37D H -0.0895 0.1824 -0.0897 0.074 Uiso 1 1 calc R B 2 C373 C -0.0369(6) 0.3051(6) -0.0236(5) 0.070(2) Uani 1 1 d . B 2 H37E H 0.0336 0.3399 -0.0024 0.084 Uiso 1 1 calc R B 2 H37F H -0.0615 0.3012 0.0224 0.084 Uiso 1 1 calc R B 2 C374 C -0.1169(6) 0.3487(6) -0.0680(5) 0.070(2) Uani 1 1 d . B 2 H37G H -0.1862 0.3126 -0.0935 0.084 Uiso 1 1 calc R B 2 H37H H -0.0890 0.3590 -0.1105 0.084 Uiso 1 1 calc R B 2 C375 C -0.1348(8) 0.4329(7) -0.0091(6) 0.091(3) Uani 1 1 d . B 2 H37I H -0.1706 0.4219 0.0295 0.109 Uiso 1 1 calc R B 2 H37J H -0.0645 0.4661 0.0212 0.109 Uiso 1 1 calc R B 2 C376 C -0.2040(7) 0.4819(7) -0.0543(6) 0.092(3) Uani 1 1 d . B 2 H37K H -0.2138 0.5333 -0.0161 0.138 Uiso 1 1 calc R B 2 H37L H -0.2739 0.4495 -0.0837 0.138 Uiso 1 1 calc R B 2 H37M H -0.1679 0.4940 -0.0915 0.138 Uiso 1 1 calc R 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 In 0.0437(3) 0.0478(3) 0.0327(3) 0.0157(2) 0.0162(2) 0.0131(2) Cl 0.0825(13) 0.0908(17) 0.0667(14) 0.0506(13) 0.0441(11) 0.0504(12) Br5 0.0755(6) 0.0745(7) 0.0489(5) 0.0128(5) 0.0305(4) 0.0091(5) N1 0.047(3) 0.043(4) 0.039(3) 0.017(3) 0.018(3) 0.012(3) C2 0.046(4) 0.044(4) 0.033(4) 0.013(3) 0.015(3) 0.010(3) C3 0.053(4) 0.045(5) 0.034(4) 0.014(3) 0.017(3) 0.018(3) C4 0.047(4) 0.052(5) 0.044(4) 0.018(4) 0.016(3) 0.016(3) C5 0.061(4) 0.063(5) 0.037(4) 0.017(4) 0.026(4) 0.013(4) C6 0.054(4) 0.057(5) 0.044(4) 0.024(4) 0.030(4) 0.017(4) C7 0.055(4) 0.042(5) 0.051(5) 0.021(4) 0.026(4) 0.010(3) C8 0.048(4) 0.045(4) 0.040(4) 0.018(3) 0.024(3) 0.019(3) C9 0.044(4) 0.036(4) 0.030(4) 0.009(3) 0.010(3) 0.003(3) N10 0.048(3) 0.046(4) 0.045(4) 0.021(3) 0.025(3) 0.019(3) N11 0.048(3) 0.035(3) 0.035(3) 0.009(3) 0.021(2) 0.007(2) C12 0.040(3) 0.046(5) 0.036(4) 0.016(3) 0.015(3) 0.014(3) C13 0.043(4) 0.039(4) 0.044(4) 0.017(3) 0.021(3) 0.013(3) C14 0.047(4) 0.033(4) 0.053(5) 0.015(4) 0.021(3) 0.010(3) C15 0.043(4) 0.041(5) 0.059(5) 0.017(4) 0.014(3) 0.005(3) C16 0.055(4) 0.040(4) 0.039(4) 0.011(3) 0.010(3) 0.004(3) C17 0.043(3) 0.033(4) 0.044(4) 0.021(3) 0.013(3) 0.010(3) C18 0.050(4) 0.040(4) 0.038(4) 0.015(3) 0.014(3) 0.013(3) C19 0.034(3) 0.040(4) 0.044(4) 0.015(3) 0.015(3) 0.008(3) N20 0.042(3) 0.031(3) 0.035(3) 0.012(3) 0.011(2) 0.009(2) N21 0.043(3) 0.034(3) 0.032(3) 0.009(3) 0.012(2) 0.004(2) C22 0.047(4) 0.040(4) 0.035(4) 0.019(3) 0.016(3) 0.017(3) C23 0.042(3) 0.040(4) 0.031(4) 0.012(3) 0.015(3) 0.011(3) C24 0.042(4) 0.045(4) 0.031(4) 0.015(3) 0.011(3) 0.007(3) C25 0.051(4) 0.052(5) 0.035(4) 0.016(4) 0.014(3) 0.008(3) C26 0.051(4) 0.054(5) 0.046(4) 0.021(4) 0.023(3) 0.014(4) C27 0.048(4) 0.038(4) 0.037(4) 0.015(3) 0.014(3) 0.009(3) C28 0.044(4) 0.040(4) 0.040(4) 0.013(3) 0.015(3) 0.012(3) C29 0.047(4) 0.039(4) 0.037(4) 0.015(3) 0.014(3) 0.009(3) N30 0.040(3) 0.047(4) 0.038(3) 0.014(3) 0.014(2) 0.007(3) N31 0.042(3) 0.049(4) 0.026(3) 0.006(3) 0.009(2) 0.006(3) C32 0.037(3) 0.050(5) 0.032(4) 0.012(3) 0.008(3) 0.012(3) C33 0.043(4) 0.048(5) 0.043(4) 0.017(4) 0.015(3) 0.017(3) C34 0.053(4) 0.044(5) 0.045(5) 0.014(4) 0.009(3) 0.006(3) C35 0.056(4) 0.054(5) 0.050(5) 0.011(4) 0.013(4) -0.001(4) C36 0.059(4) 0.055(5) 0.047(5) 0.013(4) 0.005(4) 0.010(4) C37 0.052(4) 0.049(5) 0.034(4) 0.010(4) 0.007(3) 0.010(4) C38 0.047(4) 0.053(5) 0.038(4) 0.016(4) 0.009(3) 0.008(3) C39 0.048(4) 0.049(5) 0.036(4) 0.015(3) 0.014(3) 0.018(3) N40 0.045(3) 0.049(4) 0.036(3) 0.016(3) 0.014(3) 0.015(3) O4 0.059(3) 0.057(4) 0.042(3) 0.013(3) 0.017(2) 0.012(3) C41 0.057(5) 0.062(6) 0.086(7) 0.020(5) 0.022(4) 0.011(4) C42 0.098(7) 0.074(7) 0.077(7) -0.016(6) 0.039(6) -0.005(5) O7 0.055(3) 0.057(3) 0.050(3) 0.019(3) 0.027(2) 0.006(2) C71 0.056(4) 0.068(6) 0.053(5) 0.028(4) 0.025(4) 0.011(4) C72 0.062(4) 0.071(6) 0.052(5) 0.026(4) 0.023(4) 0.008(4) C73 0.062(5) 0.099(8) 0.065(6) 0.029(5) 0.021(4) -0.001(5) C74 0.095(6) 0.095(8) 0.064(6) 0.018(6) 0.016(5) -0.041(6) C141 0.044(4) 0.049(5) 0.061(5) 0.023(4) 0.020(3) 0.005(3) C142 0.078(5) 0.048(5) 0.067(6) 0.024(4) 0.034(4) 0.011(4) C143 0.088(6) 0.070(6) 0.071(6) 0.035(5) 0.029(5) 0.023(5) C144 0.123(7) 0.072(7) 0.062(6) 0.040(5) 0.032(5) 0.037(6) C145 0.160(11) 0.095(9) 0.111(10) 0.043(8) -0.035(8) 0.046(8) C146 0.30(2) 0.153(15) 0.122(12) 0.039(11) 0.011(13) 0.115(15) C171 0.050(4) 0.044(5) 0.039(4) 0.012(3) 0.009(3) 0.005(3) C172 0.052(4) 0.053(5) 0.039(4) 0.016(4) 0.010(3) 0.002(3) C173 0.055(4) 0.048(5) 0.047(5) 0.007(4) 0.006(3) 0.003(3) C174 0.074(5) 0.059(6) 0.087(7) 0.020(5) 0.022(5) 0.005(4) C175 0.082(6) 0.067(6) 0.061(6) 0.009(5) 0.022(5) 0.005(5) C176 0.076(6) 0.082(7) 0.073(7) 0.008(5) 0.013(5) -0.007(5) C241 0.052(4) 0.045(5) 0.035(4) 0.011(3) 0.010(3) 0.006(3) C242 0.057(4) 0.051(5) 0.034(4) 0.015(4) 0.017(3) 0.014(3) C243 0.051(4) 0.057(5) 0.050(5) 0.021(4) 0.021(3) 0.017(4) C244 0.058(4) 0.058(5) 0.037(4) 0.009(4) 0.012(3) 0.015(4) C245 0.064(5) 0.069(6) 0.054(5) 0.009(5) 0.014(4) 0.004(4) C246 0.080(6) 0.080(7) 0.055(6) -0.007(5) 0.012(5) 0.006(5) C271 0.052(4) 0.051(5) 0.049(5) 0.018(4) 0.024(3) 0.013(3) C272 0.049(4) 0.047(5) 0.045(4) 0.014(4) 0.013(3) 0.004(3) C273 0.053(4) 0.056(5) 0.056(5) 0.023(4) 0.017(4) 0.009(4) C274 0.057(4) 0.054(5) 0.062(5) 0.029(4) 0.022(4) 0.005(4) C275 0.061(4) 0.073(6) 0.061(5) 0.038(5) 0.011(4) 0.004(4) C276 0.072(5) 0.079(7) 0.127(9) 0.049(7) 0.048(6) 0.009(5) C341 0.071(5) 0.045(5) 0.046(5) 0.007(4) 0.013(4) -0.003(4) C342 0.099(7) 0.065(7) 0.083(7) 0.014(6) 0.029(6) 0.010(5) C343 0.120(9) 0.125(11) 0.097(9) 0.047(8) 0.042(7) 0.038(8) C344 0.231(17) 0.130(13) 0.189(17) 0.104(13) 0.070(14) 0.100(12) C345 0.220(18) 0.199(18) 0.150(15) 0.074(14) 0.036(13) 0.125(15) C371 0.051(4) 0.067(6) 0.044(5) 0.007(4) 0.013(3) 0.008(4) C372 0.066(5) 0.071(6) 0.052(5) 0.022(5) 0.020(4) -0.002(4) C373 0.069(5) 0.087(7) 0.068(6) 0.034(5) 0.030(4) 0.028(5) C374 0.067(5) 0.098(7) 0.064(6) 0.045(5) 0.027(4) 0.025(5) C375 0.096(7) 0.129(10) 0.083(7) 0.063(7) 0.044(6) 0.053(6) C376 0.086(6) 0.125(9) 0.090(8) 0.058(7) 0.035(6) 0.033(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag In N21 2.134(5) . ? In N11 2.147(5) . ? In N1 2.150(5) . ? In N31 2.161(6) . ? In Cl 2.3526(19) . ? Br5 C5 1.924(7) . ? N1 C9 1.366(8) . ? N1 C2 1.382(8) . ? C2 N40 1.313(8) . ? C2 C3 1.457(8) . ? C3 C8 1.404(9) . ? C3 C4 1.435(9) . ? C4 C5 1.380(9) . ? C4 O4 1.383(8) . ? C5 C6 1.369(10) . ? C6 C7 1.416(9) . ? C6 H6 0.9300 . ? C7 O7 1.352(8) . ? C7 C8 1.414(8) . ? C8 C9 1.483(8) . ? C9 N10 1.338(8) . ? N10 C12 1.353(8) . ? N11 C19 1.377(8) . ? N11 C12 1.380(8) . ? C12 C13 1.438(9) . ? C13 C14 1.406(9) . ? C13 C18 1.441(8) . ? C14 C15 1.384(10) . ? C14 C141 1.518(9) . ? C15 C16 1.404(9) . ? C15 H15 0.9300 . ? C16 C17 1.384(9) . ? C16 H16 0.9300 . ? C17 C18 1.419(9) . ? C17 C171 1.507(8) . ? C18 C19 1.451(9) . ? C19 N20 1.359(7) . ? N20 C22 1.347(8) . ? N21 C29 1.365(8) . ? N21 C22 1.397(8) . ? C22 C23 1.438(8) . ? C23 C28 1.403(9) . ? C23 C24 1.419(8) . ? C24 C25 1.399(8) . ? C24 C241 1.520(9) . ? C25 C26 1.377(10) . ? C25 H25 0.9300 . ? C26 C27 1.387(9) . ? C26 H26 0.9300 . ? C27 C28 1.429(8) . ? C27 C271 1.507(9) . ? C28 C29 1.482(9) . ? C29 N30 1.341(8) . ? N30 C32 1.335(8) . ? N31 C32 1.381(8) . ? N31 C39 1.388(8) . ? C32 C33 1.482(9) . ? C33 C38 1.402(9) . ? C33 C34 1.411(9) . ? C34 C35 1.399(10) . ? C34 C341 1.459(9) . ? C35 C36 1.405(10) . ? C35 H35 0.9300 . ? C36 C37 1.369(10) . ? C36 Br36 1.81(3) . ? C36 H36 0.9300 . ? C37 C38 1.412(9) . ? C37 C371 1.491(9) . ? C38 C39 1.463(10) . ? C39 N40 1.330(8) . ? O4 C41 1.445(9) . ? C41 C42 1.516(12) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C543 1.41(2) . ? C42 C43 1.92(3) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C42 H54A 0.9700 . ? C42 H54B 0.9700 . ? C43 C44 1.45(3) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C543 C544 1.59(3) . ? C543 H54C 0.9700 . ? C543 H54D 0.9700 . ? C544 H54E 0.9600 . ? C544 H54F 0.9600 . ? C544 H54G 0.9600 . ? O7 C71 1.466(7) . ? C71 C72 1.493(10) . ? C71 H71A 0.9700 . ? C71 H71B 0.9700 . ? C72 C73 1.499(9) . ? C72 H72A 0.9700 . ? C72 H72B 0.9700 . ? C73 C74 1.537(11) . ? C73 H73A 0.9700 . ? C73 H73B 0.9700 . ? C74 H74A 0.9600 . ? C74 H74B 0.9600 . ? C74 H74C 0.9600 . ? C141 C142 1.554(9) . ? C141 H14A 0.9700 . ? C141 H14B 0.9700 . ? C142 C143 1.522(11) . ? C142 H14C 0.9700 . ? C142 H14D 0.9700 . ? C143 C144 1.515(11) . ? C143 H14E 0.9700 . ? C143 H14F 0.9700 . ? C144 C145 1.624(14) . ? C144 H14G 0.9700 . ? C144 H14H 0.9700 . ? C145 C146 1.459(15) . ? C145 H14I 0.9700 . ? C145 H14J 0.9700 . ? C146 H14K 0.9600 . ? C146 H14L 0.9600 . ? C146 H14M 0.9600 . ? C171 C172 1.546(9) . ? C171 H17A 0.9700 . ? C171 H17B 0.9700 . ? C172 C173 1.519(10) . ? C172 H17C 0.9700 . ? C172 H17D 0.9700 . ? C173 C174 1.519(11) . ? C173 H17E 0.9700 . ? C173 H17F 0.9700 . ? C174 C175 1.525(11) . ? C174 H17G 0.9700 . ? C174 H17H 0.9700 . ? C175 C176 1.501(11) . ? C175 H17I 0.9700 . ? C175 H17J 0.9700 . ? C176 H17K 0.9600 . ? C176 H17L 0.9600 . ? C176 H17M 0.9600 . ? C241 C242 1.527(8) . ? C241 H24A 0.9700 . ? C241 H24B 0.9700 . ? C242 C243 1.507(10) . ? C242 H24C 0.9700 . ? C242 H24D 0.9700 . ? C243 C244 1.536(9) . ? C243 H24E 0.9700 . ? C243 H24F 0.9700 . ? C244 C245 1.512(10) . ? C244 H24G 0.9700 . ? C244 H24H 0.9700 . ? C245 C246 1.534(10) . ? C245 H24I 0.9700 . ? C245 H24J 0.9700 . ? C246 H24K 0.9600 . ? C246 H24L 0.9600 . ? C246 H24M 0.9600 . ? C271 C272 1.510(8) . ? C271 H27A 0.9700 . ? C271 H27B 0.9700 . ? C272 C273 1.514(10) . ? C272 H27C 0.9700 . ? C272 H27D 0.9700 . ? C273 C274 1.537(9) . ? C273 H27E 0.9700 . ? C273 H27F 0.9700 . ? C274 C275 1.485(10) . ? C274 H27G 0.9700 . ? C274 H27H 0.9700 . ? C275 C276 1.523(10) . ? C275 H27I 0.9700 . ? C275 H27J 0.9700 . ? C276 H27K 0.9600 . ? C276 H27L 0.9600 . ? C276 H27M 0.9600 . ? C341 C342 1.556(11) . ? C341 H34A 0.9700 . ? C341 H34B 0.9700 . ? C342 C343 1.406(13) . ? C342 H34C 0.9700 . ? C342 H34D 0.9700 . ? C343 C344 1.599(15) . ? C343 H34E 0.9700 . ? C343 H34F 0.9700 . ? C344 C345 1.456(19) . ? C344 H34G 0.9700 . ? C344 H34H 0.9700 . ? C345 C846 1.51(4) . ? C345 C346 1.66(3) . ? C345 H34I 0.9700 . ? C345 H34J 0.9700 . ? C345 H84A 0.9700 . ? C345 H84B 0.9700 . ? C346 H34K 0.9600 . ? C346 H34L 0.9600 . ? C346 H34M 0.9600 . ? C846 H84C 0.9600 . ? C846 H84D 0.9600 . ? C846 H84E 0.9600 . ? C371 C372 1.521(10) . ? C371 H37A 0.9700 . ? C371 H37B 0.9700 . ? C372 C373 1.501(11) . ? C372 H37C 0.9700 . ? C372 H37D 0.9700 . ? C373 C374 1.518(10) . ? C373 H37E 0.9700 . ? C373 H37F 0.9700 . ? C374 C375 1.553(12) . ? C374 H37G 0.9700 . ? C374 H37H 0.9700 . ? C375 C376 1.520(11) . ? C375 H37I 0.9700 . ? C375 H37J 0.9700 . ? C376 H37K 0.9600 . ? C376 H37L 0.9600 . ? C376 H37M 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N21 In N11 83.39(19) . . ? N21 In N1 142.33(19) . . ? N11 In N1 84.39(19) . . ? N21 In N31 83.92(19) . . ? N11 In N31 140.44(19) . . ? N1 In N31 83.2(2) . . ? N21 In Cl 112.68(14) . . ? N11 In Cl 109.30(15) . . ? N1 In Cl 104.99(14) . . ? N31 In Cl 110.18(15) . . ? C9 N1 C2 111.7(5) . . ? C9 N1 In 123.3(4) . . ? C2 N1 In 123.5(4) . . ? N40 C2 N1 127.7(5) . . ? N40 C2 C3 125.1(6) . . ? N1 C2 C3 107.1(6) . . ? C8 C3 C4 120.7(6) . . ? C8 C3 C2 107.6(5) . . ? C4 C3 C2 131.6(7) . . ? C5 C4 O4 124.1(6) . . ? C5 C4 C3 115.1(7) . . ? O4 C4 C3 120.4(6) . . ? C6 C5 C4 125.3(6) . . ? C6 C5 Br5 116.9(5) . . ? C4 C5 Br5 117.8(6) . . ? C5 C6 C7 120.6(6) . . ? C5 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? O7 C7 C8 119.8(6) . . ? O7 C7 C6 124.0(6) . . ? C8 C7 C6 116.2(7) . . ? C3 C8 C7 122.0(6) . . ? C3 C8 C9 106.8(5) . . ? C7 C8 C9 131.2(7) . . ? N10 C9 N1 128.8(6) . . ? N10 C9 C8 124.3(6) . . ? N1 C9 C8 106.8(5) . . ? C9 N10 C12 125.5(6) . . ? C19 N11 C12 108.8(5) . . ? C19 N11 In 124.7(4) . . ? C12 N11 In 124.1(4) . . ? N10 C12 N11 126.3(6) . . ? N10 C12 C13 124.4(6) . . ? N11 C12 C13 109.2(5) . . ? C14 C13 C12 131.9(6) . . ? C14 C13 C18 121.2(6) . . ? C12 C13 C18 106.9(5) . . ? C15 C14 C13 115.0(6) . . ? C15 C14 C141 120.3(6) . . ? C13 C14 C141 124.5(6) . . ? C14 C15 C16 124.5(6) . . ? C14 C15 H15 117.8 . . ? C16 C15 H15 117.8 . . ? C17 C16 C15 121.8(7) . . ? C17 C16 H16 119.1 . . ? C15 C16 H16 119.1 . . ? C16 C17 C18 115.5(6) . . ? C16 C17 C171 123.7(6) . . ? C18 C17 C171 120.8(5) . . ? C17 C18 C13 121.9(6) . . ? C17 C18 C19 132.9(6) . . ? C13 C18 C19 105.2(6) . . ? N20 C19 N11 126.9(6) . . ? N20 C19 C18 123.3(6) . . ? N11 C19 C18 109.8(5) . . ? C22 N20 C19 125.3(5) . . ? C29 N21 C22 108.9(5) . . ? C29 N21 In 124.3(4) . . ? C22 N21 In 124.3(4) . . ? N20 C22 N21 126.2(5) . . ? N20 C22 C23 124.7(6) . . ? N21 C22 C23 109.1(6) . . ? C28 C23 C24 121.0(6) . . ? C28 C23 C22 107.1(5) . . ? C24 C23 C22 131.9(6) . . ? C25 C24 C23 114.8(6) . . ? C25 C24 C241 121.5(6) . . ? C23 C24 C241 123.6(5) . . ? C26 C25 C24 124.0(6) . . ? C26 C25 H25 118.0 . . ? C24 C25 H25 118.0 . . ? C25 C26 C27 122.8(6) . . ? C25 C26 H26 118.6 . . ? C27 C26 H26 118.6 . . ? C26 C27 C28 114.5(6) . . ? C26 C27 C271 121.5(6) . . ? C28 C27 C271 123.9(6) . . ? C23 C28 C27 122.9(6) . . ? C23 C28 C29 106.5(5) . . ? C27 C28 C29 130.6(6) . . ? N30 C29 N21 127.6(6) . . ? N30 C29 C28 124.1(6) . . ? N21 C29 C28 108.2(6) . . ? C32 N30 C29 125.3(6) . . ? C32 N31 C39 110.2(6) . . ? C32 N31 In 124.6(4) . . ? C39 N31 In 123.9(4) . . ? N30 C32 N31 127.6(6) . . ? N30 C32 C33 125.1(6) . . ? N31 C32 C33 107.3(5) . . ? C38 C33 C34 122.0(7) . . ? C38 C33 C32 107.2(6) . . ? C34 C33 C32 130.8(6) . . ? C35 C34 C33 114.8(6) . . ? C35 C34 C341 119.3(7) . . ? C33 C34 C341 125.9(7) . . ? C34 C35 C36 122.5(7) . . ? C34 C35 H35 118.7 . . ? C36 C35 H35 118.7 . . ? C37 C36 C35 123.0(7) . . ? C37 C36 Br36 110.8(9) . . ? C35 C36 Br36 124.7(10) . . ? C37 C36 H36 118.5 . . ? C35 C36 H36 118.5 . . ? Br36 C36 H36 14.6 . . ? C36 C37 C38 115.5(7) . . ? C36 C37 C371 120.3(7) . . ? C38 C37 C371 124.0(7) . . ? C33 C38 C37 122.1(7) . . ? C33 C38 C39 107.0(6) . . ? C37 C38 C39 130.9(6) . . ? N40 C39 N31 125.9(6) . . ? N40 C39 C38 125.7(6) . . ? N31 C39 C38 108.1(6) . . ? C2 N40 C39 127.0(6) . . ? C4 O4 C41 113.4(5) . . ? O4 C41 C42 107.6(7) . . ? O4 C41 H41A 110.2 . . ? C42 C41 H41A 110.2 . . ? O4 C41 H41B 110.2 . . ? C42 C41 H41B 110.2 . . ? H41A C41 H41B 108.5 . . ? C543 C42 C41 115.3(13) . . ? C543 C42 C43 18.3(13) . . ? C41 C42 C43 97.3(10) . . ? C543 C42 H42A 100.0 . . ? C41 C42 H42A 112.3 . . ? C43 C42 H42A 112.3 . . ? C543 C42 H42B 106.3 . . ? C41 C42 H42B 112.3 . . ? C43 C42 H42B 112.3 . . ? H42A C42 H42B 109.9 . . ? C543 C42 H54A 108.5 . . ? C41 C42 H54A 108.5 . . ? C43 C42 H54A 113.3 . . ? H42A C42 H54A 112.2 . . ? H42B C42 H54A 3.8 . . ? C543 C42 H54B 108.5 . . ? C41 C42 H54B 108.5 . . ? C43 C42 H54B 120.8 . . ? H42A C42 H54B 8.5 . . ? H42B C42 H54B 105.6 . . ? H54A C42 H54B 107.5 . . ? C44 C43 C42 101.7(17) . . ? C44 C43 H43A 111.4 . . ? C42 C43 H43A 111.4 . . ? C44 C43 H43B 111.4 . . ? C42 C43 H43B 111.4 . . ? H43A C43 H43B 109.3 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C42 C543 C544 111.5(19) . . ? C42 C543 H54C 109.3 . . ? C544 C543 H54C 109.3 . . ? C42 C543 H54D 109.3 . . ? C544 C543 H54D 109.3 . . ? H54C C543 H54D 108.0 . . ? C543 C544 H54E 109.5 . . ? C543 C544 H54F 109.5 . . ? H54E C544 H54F 109.5 . . ? C543 C544 H54G 109.5 . . ? H54E C544 H54G 109.5 . . ? H54F C544 H54G 109.5 . . ? C7 O7 C71 117.0(5) . . ? O7 C71 C72 109.2(6) . . ? O7 C71 H71A 109.8 . . ? C72 C71 H71A 109.8 . . ? O7 C71 H71B 109.8 . . ? C72 C71 H71B 109.8 . . ? H71A C71 H71B 108.3 . . ? C71 C72 C73 113.1(6) . . ? C71 C72 H72A 109.0 . . ? C73 C72 H72A 109.0 . . ? C71 C72 H72B 109.0 . . ? C73 C72 H72B 109.0 . . ? H72A C72 H72B 107.8 . . ? C72 C73 C74 113.1(7) . . ? C72 C73 H73A 109.0 . . ? C74 C73 H73A 109.0 . . ? C72 C73 H73B 109.0 . . ? C74 C73 H73B 109.0 . . ? H73A C73 H73B 107.8 . . ? C73 C74 H74A 109.5 . . ? C73 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C73 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C14 C141 C142 109.7(5) . . ? C14 C141 H14A 109.7 . . ? C142 C141 H14A 109.7 . . ? C14 C141 H14B 109.7 . . ? C142 C141 H14B 109.7 . . ? H14A C141 H14B 108.2 . . ? C143 C142 C141 113.6(6) . . ? C143 C142 H14C 108.8 . . ? C141 C142 H14C 108.8 . . ? C143 C142 H14D 108.8 . . ? C141 C142 H14D 108.8 . . ? H14C C142 H14D 107.7 . . ? C144 C143 C142 114.0(7) . . ? C144 C143 H14E 108.7 . . ? C142 C143 H14E 108.7 . . ? C144 C143 H14F 108.7 . . ? C142 C143 H14F 108.7 . . ? H14E C143 H14F 107.6 . . ? C143 C144 C145 110.6(8) . . ? C143 C144 H14G 109.5 . . ? C145 C144 H14G 109.5 . . ? C143 C144 H14H 109.5 . . ? C145 C144 H14H 109.5 . . ? H14G C144 H14H 108.1 . . ? C146 C145 C144 111.6(12) . . ? C146 C145 H14I 109.3 . . ? C144 C145 H14I 109.3 . . ? C146 C145 H14J 109.3 . . ? C144 C145 H14J 109.3 . . ? H14I C145 H14J 108.0 . . ? C145 C146 H14K 109.5 . . ? C145 C146 H14L 109.5 . . ? H14K C146 H14L 109.5 . . ? C145 C146 H14M 109.5 . . ? H14K C146 H14M 109.5 . . ? H14L C146 H14M 109.5 . . ? C17 C171 C172 115.1(5) . . ? C17 C171 H17A 108.5 . . ? C172 C171 H17A 108.5 . . ? C17 C171 H17B 108.5 . . ? C172 C171 H17B 108.5 . . ? H17A C171 H17B 107.5 . . ? C173 C172 C171 114.1(6) . . ? C173 C172 H17C 108.7 . . ? C171 C172 H17C 108.7 . . ? C173 C172 H17D 108.7 . . ? C171 C172 H17D 108.7 . . ? H17C C172 H17D 107.6 . . ? C172 C173 C174 115.4(6) . . ? C172 C173 H17E 108.4 . . ? C174 C173 H17E 108.4 . . ? C172 C173 H17F 108.4 . . ? C174 C173 H17F 108.4 . . ? H17E C173 H17F 107.5 . . ? C173 C174 C175 115.3(7) . . ? C173 C174 H17G 108.5 . . ? C175 C174 H17G 108.5 . . ? C173 C174 H17H 108.5 . . ? C175 C174 H17H 108.5 . . ? H17G C174 H17H 107.5 . . ? C176 C175 C174 113.1(8) . . ? C176 C175 H17I 109.0 . . ? C174 C175 H17I 109.0 . . ? C176 C175 H17J 109.0 . . ? C174 C175 H17J 109.0 . . ? H17I C175 H17J 107.8 . . ? C175 C176 H17K 109.5 . . ? C175 C176 H17L 109.5 . . ? H17K C176 H17L 109.5 . . ? C175 C176 H17M 109.5 . . ? H17K C176 H17M 109.5 . . ? H17L C176 H17M 109.5 . . ? C24 C241 C242 114.5(5) . . ? C24 C241 H24A 108.6 . . ? C242 C241 H24A 108.6 . . ? C24 C241 H24B 108.6 . . ? C242 C241 H24B 108.6 . . ? H24A C241 H24B 107.6 . . ? C243 C242 C241 112.7(6) . . ? C243 C242 H24C 109.0 . . ? C241 C242 H24C 109.0 . . ? C243 C242 H24D 109.0 . . ? C241 C242 H24D 109.0 . . ? H24C C242 H24D 107.8 . . ? C242 C243 C244 113.8(6) . . ? C242 C243 H24E 108.8 . . ? C244 C243 H24E 108.8 . . ? C242 C243 H24F 108.8 . . ? C244 C243 H24F 108.8 . . ? H24E C243 H24F 107.7 . . ? C245 C244 C243 114.3(6) . . ? C245 C244 H24G 108.7 . . ? C243 C244 H24G 108.7 . . ? C245 C244 H24H 108.7 . . ? C243 C244 H24H 108.7 . . ? H24G C244 H24H 107.6 . . ? C244 C245 C246 112.4(7) . . ? C244 C245 H24I 109.1 . . ? C246 C245 H24I 109.1 . . ? C244 C245 H24J 109.1 . . ? C246 C245 H24J 109.1 . . ? H24I C245 H24J 107.9 . . ? C245 C246 H24K 109.5 . . ? C245 C246 H24L 109.5 . . ? H24K C246 H24L 109.5 . . ? C245 C246 H24M 109.5 . . ? H24K C246 H24M 109.5 . . ? H24L C246 H24M 109.5 . . ? C27 C271 C272 115.9(6) . . ? C27 C271 H27A 108.3 . . ? C272 C271 H27A 108.3 . . ? C27 C271 H27B 108.3 . . ? C272 C271 H27B 108.3 . . ? H27A C271 H27B 107.4 . . ? C271 C272 C273 115.8(6) . . ? C271 C272 H27C 108.3 . . ? C273 C272 H27C 108.3 . . ? C271 C272 H27D 108.3 . . ? C273 C272 H27D 108.3 . . ? H27C C272 H27D 107.4 . . ? C272 C273 C274 113.2(6) . . ? C272 C273 H27E 108.9 . . ? C274 C273 H27E 108.9 . . ? C272 C273 H27F 108.9 . . ? C274 C273 H27F 108.9 . . ? H27E C273 H27F 107.7 . . ? C275 C274 C273 116.2(6) . . ? C275 C274 H27G 108.2 . . ? C273 C274 H27G 108.2 . . ? C275 C274 H27H 108.2 . . ? C273 C274 H27H 108.2 . . ? H27G C274 H27H 107.4 . . ? C274 C275 C276 113.4(7) . . ? C274 C275 H27I 108.9 . . ? C276 C275 H27I 108.9 . . ? C274 C275 H27J 108.9 . . ? C276 C275 H27J 108.9 . . ? H27I C275 H27J 107.7 . . ? C275 C276 H27K 109.5 . . ? C275 C276 H27L 109.5 . . ? H27K C276 H27L 109.5 . . ? C275 C276 H27M 109.5 . . ? H27K C276 H27M 109.5 . . ? H27L C276 H27M 109.5 . . ? C34 C341 C342 116.1(7) . . ? C34 C341 H34A 108.3 . . ? C342 C341 H34A 108.3 . . ? C34 C341 H34B 108.3 . . ? C342 C341 H34B 108.3 . . ? H34A C341 H34B 107.4 . . ? C343 C342 C341 115.0(9) . . ? C343 C342 H34C 108.5 . . ? C341 C342 H34C 108.5 . . ? C343 C342 H34D 108.5 . . ? C341 C342 H34D 108.5 . . ? H34C C342 H34D 107.5 . . ? C342 C343 C344 113.3(11) . . ? C342 C343 H34E 108.9 . . ? C344 C343 H34E 108.9 . . ? C342 C343 H34F 108.9 . . ? C344 C343 H34F 108.9 . . ? H34E C343 H34F 107.7 . . ? C345 C344 C343 113.1(12) . . ? C345 C344 H34G 109.0 . . ? C343 C344 H34G 109.0 . . ? C345 C344 H34H 109.0 . . ? C343 C344 H34H 109.0 . . ? H34G C344 H34H 107.8 . . ? C344 C345 C846 133(2) . . ? C344 C345 C346 100.7(15) . . ? C846 C345 C346 33.7(16) . . ? C344 C345 H34I 111.6 . . ? C846 C345 H34I 87.4 . . ? C346 C345 H34I 111.6 . . ? C344 C345 H34J 111.6 . . ? C846 C345 H34J 100.3 . . ? C346 C345 H34J 111.6 . . ? H34I C345 H34J 109.4 . . ? C344 C345 H84A 103.9 . . ? C846 C345 H84A 103.9 . . ? C346 C345 H84A 129.7 . . ? H34I C345 H84A 18.1 . . ? H34J C345 H84A 98.9 . . ? C344 C345 H84B 103.9 . . ? C846 C345 H84B 103.9 . . ? C346 C345 H84B 110.1 . . ? H34I C345 H84B 117.3 . . ? H34J C345 H84B 8.8 . . ? H84A C345 H84B 105.4 . . ? C345 C346 H34K 109.5 . . ? C345 C346 H34L 109.5 . . ? H34K C346 H34L 109.5 . . ? C345 C346 H34M 109.5 . . ? H34K C346 H34M 109.5 . . ? H34L C346 H34M 109.5 . . ? C345 C846 H84C 109.5 . . ? C345 C846 H84D 109.5 . . ? H84C C846 H84D 109.5 . . ? C345 C846 H84E 109.5 . . ? H84C C846 H84E 109.5 . . ? H84D C846 H84E 109.5 . . ? C37 C371 C372 111.3(6) . . ? C37 C371 H37A 109.4 . . ? C372 C371 H37A 109.4 . . ? C37 C371 H37B 109.4 . . ? C372 C371 H37B 109.4 . . ? H37A C371 H37B 108.0 . . ? C373 C372 C371 113.6(7) . . ? C373 C372 H37C 108.8 . . ? C371 C372 H37C 108.8 . . ? C373 C372 H37D 108.8 . . ? C371 C372 H37D 108.8 . . ? H37C C372 H37D 107.7 . . ? C372 C373 C374 116.1(7) . . ? C372 C373 H37E 108.3 . . ? C374 C373 H37E 108.3 . . ? C372 C373 H37F 108.3 . . ? C374 C373 H37F 108.3 . . ? H37E C373 H37F 107.4 . . ? C373 C374 C375 111.2(7) . . ? C373 C374 H37G 109.4 . . ? C375 C374 H37G 109.4 . . ? C373 C374 H37H 109.4 . . ? C375 C374 H37H 109.4 . . ? H37G C374 H37H 108.0 . . ? C376 C375 C374 111.7(8) . . ? C376 C375 H37I 109.3 . . ? C374 C375 H37I 109.3 . . ? C376 C375 H37J 109.3 . . ? C374 C375 H37J 109.3 . . ? H37I C375 H37J 107.9 . . ? C375 C376 H37K 109.5 . . ? C375 C376 H37L 109.5 . . ? H37K C376 H37L 109.5 . . ? C375 C376 H37M 109.5 . . ? H37K C376 H37M 109.5 . . ? H37L C376 H37M 109.5 . . ? 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 N21 In N1 C9 -96.5(5) . . . . ? N11 In N1 C9 -25.0(5) . . . . ? N31 In N1 C9 -167.3(5) . . . . ? Cl In N1 C9 83.5(5) . . . . ? N21 In N1 C2 98.5(5) . . . . ? N11 In N1 C2 170.1(5) . . . . ? N31 In N1 C2 27.7(5) . . . . ? Cl In N1 C2 -81.4(5) . . . . ? C9 N1 C2 N40 174.7(6) . . . . ? In N1 C2 N40 -18.8(9) . . . . ? C9 N1 C2 C3 -0.2(7) . . . . ? In N1 C2 C3 166.3(4) . . . . ? N40 C2 C3 C8 -175.7(6) . . . . ? N1 C2 C3 C8 -0.6(7) . . . . ? N40 C2 C3 C4 4.1(11) . . . . ? N1 C2 C3 C4 179.2(6) . . . . ? C8 C3 C4 C5 -1.2(9) . . . . ? C2 C3 C4 C5 179.0(7) . . . . ? C8 C3 C4 O4 -175.0(6) . . . . ? C2 C3 C4 O4 5.2(11) . . . . ? O4 C4 C5 C6 176.0(7) . . . . ? C3 C4 C5 C6 2.5(10) . . . . ? O4 C4 C5 Br5 -4.4(9) . . . . ? C3 C4 C5 Br5 -177.9(5) . . . . ? C4 C5 C6 C7 -2.2(11) . . . . ? Br5 C5 C6 C7 178.3(5) . . . . ? C5 C6 C7 O7 -179.0(6) . . . . ? C5 C6 C7 C8 0.4(10) . . . . ? C4 C3 C8 C7 -0.4(10) . . . . ? C2 C3 C8 C7 179.5(6) . . . . ? C4 C3 C8 C9 -178.7(6) . . . . ? C2 C3 C8 C9 1.1(7) . . . . ? O7 C7 C8 C3 -179.8(6) . . . . ? C6 C7 C8 C3 0.8(9) . . . . ? O7 C7 C8 C9 -1.8(10) . . . . ? C6 C7 C8 C9 178.7(6) . . . . ? C2 N1 C9 N10 -178.2(6) . . . . ? In N1 C9 N10 15.3(9) . . . . ? C2 N1 C9 C8 0.9(7) . . . . ? In N1 C9 C8 -165.7(4) . . . . ? C3 C8 C9 N10 177.9(6) . . . . ? C7 C8 C9 N10 -0.3(11) . . . . ? C3 C8 C9 N1 -1.2(7) . . . . ? C7 C8 C9 N1 -179.4(6) . . . . ? N1 C9 N10 C12 4.8(10) . . . . ? C8 C9 N10 C12 -174.1(6) . . . . ? N21 In N11 C19 -27.8(5) . . . . ? N1 In N11 C19 -172.1(5) . . . . ? N31 In N11 C19 -99.9(5) . . . . ? Cl In N11 C19 83.9(5) . . . . ? N21 In N11 C12 171.8(5) . . . . ? N1 In N11 C12 27.5(5) . . . . ? N31 In N11 C12 99.7(5) . . . . ? Cl In N11 C12 -76.5(5) . . . . ? C9 N10 C12 N11 -2.1(10) . . . . ? C9 N10 C12 C13 176.0(6) . . . . ? C19 N11 C12 N10 176.6(6) . . . . ? In N11 C12 N10 -20.4(9) . . . . ? C19 N11 C12 C13 -1.7(7) . . . . ? In N11 C12 C13 161.3(4) . . . . ? N10 C12 C13 C14 5.2(11) . . . . ? N11 C12 C13 C14 -176.5(6) . . . . ? N10 C12 C13 C18 -175.3(6) . . . . ? N11 C12 C13 C18 3.0(7) . . . . ? C12 C13 C14 C15 -178.2(6) . . . . ? C18 C13 C14 C15 2.4(9) . . . . ? C12 C13 C14 C141 6.4(11) . . . . ? C18 C13 C14 C141 -172.9(6) . . . . ? C13 C14 C15 C16 -0.9(10) . . . . ? C141 C14 C15 C16 174.6(6) . . . . ? C14 C15 C16 C17 -2.1(10) . . . . ? C15 C16 C17 C18 3.3(9) . . . . ? C15 C16 C17 C171 -178.1(6) . . . . ? C16 C17 C18 C13 -1.8(9) . . . . ? C171 C17 C18 C13 179.5(6) . . . . ? C16 C17 C18 C19 -178.7(6) . . . . ? C171 C17 C18 C19 2.6(10) . . . . ? C14 C13 C18 C17 -1.1(9) . . . . ? C12 C13 C18 C17 179.4(6) . . . . ? C14 C13 C18 C19 176.5(6) . . . . ? C12 C13 C18 C19 -3.0(6) . . . . ? C12 N11 C19 N20 -179.1(6) . . . . ? In N11 C19 N20 18.0(9) . . . . ? C12 N11 C19 C18 -0.2(7) . . . . ? In N11 C19 C18 -163.1(4) . . . . ? C17 C18 C19 N20 -1.8(11) . . . . ? C13 C18 C19 N20 -179.1(6) . . . . ? C17 C18 C19 N11 179.3(6) . . . . ? C13 C18 C19 N11 2.0(7) . . . . ? N11 C19 N20 C22 2.8(10) . . . . ? C18 C19 N20 C22 -175.9(6) . . . . ? N11 In N21 C29 -169.5(5) . . . . ? N1 In N21 C29 -97.7(5) . . . . ? N31 In N21 C29 -27.1(5) . . . . ? Cl In N21 C29 82.3(5) . . . . ? N11 In N21 C22 30.5(4) . . . . ? N1 In N21 C22 102.3(5) . . . . ? N31 In N21 C22 172.9(5) . . . . ? Cl In N21 C22 -77.7(4) . . . . ? C19 N20 C22 N21 0.4(9) . . . . ? C19 N20 C22 C23 178.0(6) . . . . ? C29 N21 C22 N20 173.3(6) . . . . ? In N21 C22 N20 -24.1(8) . . . . ? C29 N21 C22 C23 -4.6(6) . . . . ? In N21 C22 C23 158.0(4) . . . . ? N20 C22 C23 C28 -174.8(6) . . . . ? N21 C22 C23 C28 3.2(7) . . . . ? N20 C22 C23 C24 7.3(10) . . . . ? N21 C22 C23 C24 -174.7(6) . . . . ? C28 C23 C24 C25 -0.3(9) . . . . ? C22 C23 C24 C25 177.4(6) . . . . ? C28 C23 C24 C241 179.2(6) . . . . ? C22 C23 C24 C241 -3.1(11) . . . . ? C23 C24 C25 C26 -0.2(9) . . . . ? C241 C24 C25 C26 -179.7(6) . . . . ? C24 C25 C26 C27 1.6(11) . . . . ? C25 C26 C27 C28 -2.3(10) . . . . ? C25 C26 C27 C271 177.8(6) . . . . ? C24 C23 C28 C27 -0.6(10) . . . . ? C22 C23 C28 C27 -178.8(5) . . . . ? C24 C23 C28 C29 177.5(5) . . . . ? C22 C23 C28 C29 -0.7(7) . . . . ? C26 C27 C28 C23 1.8(9) . . . . ? C271 C27 C28 C23 -178.3(6) . . . . ? C26 C27 C28 C29 -175.8(6) . . . . ? C271 C27 C28 C29 4.1(11) . . . . ? C22 N21 C29 N30 -172.9(6) . . . . ? In N21 C29 N30 24.5(9) . . . . ? C22 N21 C29 C28 4.2(7) . . . . ? In N21 C29 C28 -158.4(4) . . . . ? C23 C28 C29 N30 175.1(6) . . . . ? C27 C28 C29 N30 -7.0(11) . . . . ? C23 C28 C29 N21 -2.2(7) . . . . ? C27 C28 C29 N21 175.8(6) . . . . ? N21 C29 N30 C32 -2.6(10) . . . . ? C28 C29 N30 C32 -179.3(6) . . . . ? N21 In N31 C32 20.8(5) . . . . ? N11 In N31 C32 92.7(5) . . . . ? N1 In N31 C32 165.4(5) . . . . ? Cl In N31 C32 -91.1(5) . . . . ? N21 In N31 C39 -173.3(5) . . . . ? N11 In N31 C39 -101.4(5) . . . . ? N1 In N31 C39 -28.8(5) . . . . ? Cl In N31 C39 74.7(5) . . . . ? C29 N30 C32 N31 -5.1(10) . . . . ? C29 N30 C32 C33 176.7(6) . . . . ? C39 N31 C32 N30 -177.7(6) . . . . ? In N31 C32 N30 -10.2(9) . . . . ? C39 N31 C32 C33 0.8(7) . . . . ? In N31 C32 C33 168.3(4) . . . . ? N30 C32 C33 C38 175.4(6) . . . . ? N31 C32 C33 C38 -3.1(7) . . . . ? N30 C32 C33 C34 -5.7(11) . . . . ? N31 C32 C33 C34 175.8(6) . . . . ? C38 C33 C34 C35 -1.8(9) . . . . ? C32 C33 C34 C35 179.4(6) . . . . ? C38 C33 C34 C341 175.5(6) . . . . ? C32 C33 C34 C341 -3.3(12) . . . . ? C33 C34 C35 C36 -1.0(10) . . . . ? C341 C34 C35 C36 -178.5(7) . . . . ? C34 C35 C36 C37 1.3(11) . . . . ? C34 C35 C36 Br36 -163.1(11) . . . . ? C35 C36 C37 C38 1.2(10) . . . . ? Br36 C36 C37 C38 167.5(9) . . . . ? C35 C36 C37 C371 -173.1(6) . . . . ? Br36 C36 C37 C371 -6.7(12) . . . . ? C34 C33 C38 C37 4.5(10) . . . . ? C32 C33 C38 C37 -176.4(6) . . . . ? C34 C33 C38 C39 -174.9(6) . . . . ? C32 C33 C38 C39 4.1(7) . . . . ? C36 C37 C38 C33 -4.0(10) . . . . ? C371 C37 C38 C33 170.0(6) . . . . ? C36 C37 C38 C39 175.3(7) . . . . ? C371 C37 C38 C39 -10.7(11) . . . . ? C32 N31 C39 N40 -171.7(6) . . . . ? In N31 C39 N40 20.7(9) . . . . ? C32 N31 C39 C38 1.8(7) . . . . ? In N31 C39 C38 -165.8(4) . . . . ? C33 C38 C39 N40 169.7(6) . . . . ? C37 C38 C39 N40 -9.7(11) . . . . ? C33 C38 C39 N31 -3.7(7) . . . . ? C37 C38 C39 N31 176.9(6) . . . . ? N1 C2 N40 C39 -3.5(10) . . . . ? C3 C2 N40 C39 170.5(6) . . . . ? N31 C39 N40 C2 2.4(10) . . . . ? C38 C39 N40 C2 -169.9(6) . . . . ? C5 C4 O4 C41 80.4(8) . . . . ? C3 C4 O4 C41 -106.4(7) . . . . ? C4 O4 C41 C42 -145.0(6) . . . . ? O4 C41 C42 C543 176.5(12) . . . . ? O4 C41 C42 C43 -179.4(9) . . . . ? C543 C42 C43 C44 8(4) . . . . ? C41 C42 C43 C44 -160.4(15) . . . . ? C41 C42 C543 C544 -168.1(13) . . . . ? C43 C42 C543 C544 179(5) . . . . ? C8 C7 O7 C71 -176.4(6) . . . . ? C6 C7 O7 C71 3.0(9) . . . . ? C7 O7 C71 C72 174.2(6) . . . . ? O7 C71 C72 C73 177.9(6) . . . . ? C71 C72 C73 C74 179.3(7) . . . . ? C15 C14 C141 C142 -80.1(8) . . . . ? C13 C14 C141 C142 95.0(8) . . . . ? C14 C141 C142 C143 -68.3(8) . . . . ? C141 C142 C143 C144 -175.2(7) . . . . ? C142 C143 C144 C145 -171.8(8) . . . . ? C143 C144 C145 C146 -176.6(10) . . . . ? C16 C17 C171 C172 5.3(9) . . . . ? C18 C17 C171 C172 -176.2(6) . . . . ? C17 C171 C172 C173 78.2(7) . . . . ? C171 C172 C173 C174 171.2(6) . . . . ? C172 C173 C174 C175 60.3(10) . . . . ? C173 C174 C175 C176 61.7(10) . . . . ? C25 C24 C241 C242 -11.1(9) . . . . ? C23 C24 C241 C242 169.4(6) . . . . ? C24 C241 C242 C243 -174.8(6) . . . . ? C241 C242 C243 C244 -174.8(6) . . . . ? C242 C243 C244 C245 -174.0(6) . . . . ? C243 C244 C245 C246 -172.4(6) . . . . ? C26 C27 C271 C272 4.2(9) . . . . ? C28 C27 C271 C272 -175.6(6) . . . . ? C27 C271 C272 C273 -176.3(6) . . . . ? C271 C272 C273 C274 -175.6(6) . . . . ? C272 C273 C274 C275 -169.7(6) . . . . ? C273 C274 C275 C276 -175.9(7) . . . . ? C35 C34 C341 C342 100.1(8) . . . . ? C33 C34 C341 C342 -77.1(10) . . . . ? C34 C341 C342 C343 -65.7(11) . . . . ? C341 C342 C343 C344 174.5(9) . . . . ? C342 C343 C344 C345 57.0(18) . . . . ? C343 C344 C345 C846 169(3) . . . . ? C343 C344 C345 C346 -180.0(14) . . . . ? C36 C37 C371 C372 78.1(9) . . . . ? C38 C37 C371 C372 -95.6(8) . . . . ? C37 C371 C372 C373 61.5(9) . . . . ? C371 C372 C373 C374 174.8(6) . . . . ? C372 C373 C374 C375 174.4(7) . . . . ? C373 C374 C375 C376 173.2(7) . . . . ? _diffrn_measured_fraction_theta_max 0.905 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.905 _refine_diff_density_max 1.346 _refine_diff_density_min -1.101 _refine_diff_density_rms 0.101