# Supplementary Material (ESI) for Organic & Biomolecular Chemistry # This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full Org.Biomol.Chem. _journal_coden_Cambridge 0177 _publ_contact_author_name 'ProfD Hidemitsu Uno' _publ_contact_author_address ; INCS Ehime University Matsuyama 790-8577 JAPAN ; _publ_contact_author_email UNO@DPC.EHIME-U.AC.JP _publ_section_title ; Extremely large cavity assembled by self-interlocking of distorted biconcave porphyrins ; loop_ _publ_author_name 'Hidemitsu Uno' 'Noboru Ono' 'Hikaru Watanabe' 'Yuko Yamashita' #============================================================================== data_TPTAP-Zn-7PhMe(TPTAP-Zn) _database_code_depnum_ccdc_archive 'CCDC 248905' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C149 H116 N4 Zn ' _chemical_formula_moiety 'C100 H60 N4 Zn, 7(C7 H8) ' _chemical_formula_weight 2027.96 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _cell_length_a 10.263(1) _cell_length_b 16.066(2) _cell_length_c 16.779(2) _cell_angle_alpha 82.544(5) _cell_angle_beta 85.022(6) _cell_angle_gamma 80.666(6) _cell_volume 2700.8(5) _cell_formula_units_Z 1 _cell_measurement_reflns_used 11247 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 173.1 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.247 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1068 _exptl_absorpt_coefficient_mu 0.286 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8586 _exptl_absorpt_correction_T_max 0.9450 _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoKa _diffrn_radiation_source '6kW rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ccd _diffrn_measurement_method w _diffrn_detector_area_resol_mean 14.6199 _diffrn_reflns_number 27419 _diffrn_reflns_av_R_equivalents 0.0304 _diffrn_reflns_av_sigmaI/netI 0.0461 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.966 _reflns_number_total 11968 _reflns_number_gt 9800 _reflns_threshold_expression >2sigma(I) _computing_data_collection CRYSTALCLEAR _computing_cell_refinement CRYSTALCLEAR _computing_data_reduction CrystalStructure _computing_structure_solution SIR97 _computing_structure_refinement ; SHELXL-97 (Sheldrick, 1997) and PLATON SQUEEZE ; _computing_publication_material 'CrystalStructure 3.6.0' _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^)+(0.1093P)^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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 11968 _refine_ls_number_parameters 476 _refine_ls_number_restraints 484 _refine_ls_R_factor_all 0.0554 _refine_ls_R_factor_gt 0.0484 _refine_ls_wR_factor_ref 0.1515 _refine_ls_wR_factor_gt 0.1467 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 0.980 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.320 _refine_diff_density_min -0.316 _refine_diff_density_rms 0.065 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 Zn1 Zn 0.5000 0.5000 0.5000 0.01742(9) Uani 1 2 d SU . . N1 N 0.42378(12) 0.39621(8) 0.56014(8) 0.0173(3) Uani 1 1 d U . . N2 N 0.44242(12) 0.47379(8) 0.39280(8) 0.0174(3) Uani 1 1 d U . . C1 C 0.41170(14) 0.37477(10) 0.64187(9) 0.0170(3) Uani 1 1 d U . . C2 C 0.33713(15) 0.30437(10) 0.66037(9) 0.0186(3) Uani 1 1 d U . . C3 C 0.30550(14) 0.28412(10) 0.58846(9) 0.0177(3) Uani 1 1 d U . . C4 C 0.35957(14) 0.34198(10) 0.52561(9) 0.0170(3) Uani 1 1 d U . . C5 C 0.34285(14) 0.34471(10) 0.44327(9) 0.0167(3) Uani 1 1 d U . . C6 C 0.38218(15) 0.40568(10) 0.38215(9) 0.0176(3) Uani 1 1 d U . . C7 C 0.37068(15) 0.40484(10) 0.29676(9) 0.0184(3) Uani 1 1 d U . . C8 C 0.42501(15) 0.47163(10) 0.25707(9) 0.0182(3) Uani 1 1 d U . . C9 C 0.47080(14) 0.51459(10) 0.31743(9) 0.0163(3) Uani 1 1 d U . . C10 C 0.53753(14) 0.58548(10) 0.30065(9) 0.0170(3) Uani 1 1 d U . . C11 C 0.26862(16) 0.25929(11) 0.73392(10) 0.0228(3) Uani 1 1 d U . . H1 H 0.2919 0.2744 0.7863 0.027 Uiso 1 1 calc R . . C12 C 0.30176(16) 0.16437(11) 0.72549(11) 0.0258(4) Uani 1 1 d U . . C13 C 0.3567(2) 0.10119(13) 0.78309(13) 0.0384(5) Uani 1 1 d U . . H2 H 0.3775 0.1151 0.8334 0.046 Uiso 1 1 calc R . . C14 C 0.3806(2) 0.01820(14) 0.76620(16) 0.0494(6) Uani 1 1 d U . . H3 H 0.4184 -0.0252 0.8052 0.059 Uiso 1 1 calc R . . C15 C 0.3505(2) -0.00293(13) 0.69378(15) 0.0468(5) Uani 1 1 d U . . H4 H 0.3674 -0.0606 0.6835 0.056 Uiso 1 1 calc R . . C16 C 0.29510(18) 0.06004(12) 0.63480(13) 0.0324(4) Uani 1 1 d U . . H5 H 0.2746 0.0457 0.5846 0.039 Uiso 1 1 calc R . . C17 C 0.27093(16) 0.14404(11) 0.65178(10) 0.0233(3) Uani 1 1 d U . . C18 C 0.20946(15) 0.21974(10) 0.59659(10) 0.0193(3) Uani 1 1 d U . . H6 H 0.1874 0.2049 0.5438 0.023 Uiso 1 1 calc R . . C19 C 0.08972(15) 0.26268(10) 0.64533(10) 0.0219(3) Uani 1 1 d U . . C20 C -0.03751(17) 0.28288(12) 0.62103(11) 0.0289(4) Uani 1 1 d U . . H7 H -0.0588 0.2678 0.5714 0.035 Uiso 1 1 calc R . . C21 C -0.13452(19) 0.32591(14) 0.67063(14) 0.0399(5) Uani 1 1 d U . . H8 H -0.2223 0.3415 0.6542 0.048 Uiso 1 1 calc R . . C22 C -0.1034(2) 0.34604(15) 0.74401(14) 0.0437(5) Uani 1 1 d U . . H9 H -0.1705 0.3743 0.7779 0.052 Uiso 1 1 calc R . . C23 C 0.02436(19) 0.32530(14) 0.76822(12) 0.0353(4) Uani 1 1 d U . . H10 H 0.0452 0.3397 0.8183 0.042 Uiso 1 1 calc R . . C24 C 0.12188(16) 0.28343(11) 0.71897(10) 0.0244(3) Uani 1 1 d U . . C25 C 0.27966(15) 0.27570(10) 0.41898(9) 0.0187(3) Uani 1 1 d U . . C26 C 0.14581(16) 0.28914(11) 0.40489(11) 0.0256(4) Uani 1 1 d U . . H11 H 0.0945 0.3433 0.4093 0.031 Uiso 1 1 calc R . . C27 C 0.08690(19) 0.22334(13) 0.38438(13) 0.0365(4) Uani 1 1 d U . . H12 H -0.0047 0.2326 0.3754 0.044 Uiso 1 1 calc R . . C28 C 0.1611(2) 0.14482(13) 0.37714(14) 0.0420(5) Uani 1 1 d U . . H13 H 0.1205 0.1001 0.3632 0.050 Uiso 1 1 calc R . . C29 C 0.2944(2) 0.13093(12) 0.39005(13) 0.0367(4) Uani 1 1 d U . . H14 H 0.3457 0.0769 0.3846 0.044 Uiso 1 1 calc R . . C30 C 0.35310(17) 0.19623(11) 0.41108(11) 0.0261(4) Uani 1 1 d U . . H15 H 0.4447 0.1865 0.4202 0.031 Uiso 1 1 calc R . . C31 C 0.32696(16) 0.34691(10) 0.24209(9) 0.0221(3) Uani 1 1 d U . . H16 H 0.2872 0.2981 0.2720 0.026 Uiso 1 1 calc R . . C32 C 0.45164(18) 0.32026(11) 0.18887(10) 0.0254(3) Uani 1 1 d U . . C33 C 0.5100(2) 0.23865(13) 0.17958(12) 0.0350(4) Uani 1 1 d U . . H17 H 0.4710 0.1918 0.2059 0.042 Uiso 1 1 calc R . . C34 C 0.6269(2) 0.22521(14) 0.13111(14) 0.0452(5) Uani 1 1 d U . . H18 H 0.6680 0.1689 0.1246 0.054 Uiso 1 1 calc R . . C35 C 0.6830(2) 0.29278(15) 0.09267(13) 0.0421(5) Uani 1 1 d U . . H19 H 0.7635 0.2827 0.0605 0.050 Uiso 1 1 calc R . . C36 C 0.62349(18) 0.37612(13) 0.10019(11) 0.0325(4) Uani 1 1 d U . . H20 H 0.6618 0.4227 0.0726 0.039 Uiso 1 1 calc R . . C37 C 0.50777(17) 0.38960(11) 0.14857(10) 0.0236(3) Uani 1 1 d U . . C38 C 0.43109(16) 0.47560(11) 0.16557(9) 0.0214(3) Uani 1 1 d U . . H21 H 0.4707 0.5250 0.1367 0.026 Uiso 1 1 calc R . . C39 C 0.28903(16) 0.47456(11) 0.14530(9) 0.0221(3) Uani 1 1 d U . . C40 C 0.21625(18) 0.53410(12) 0.09273(10) 0.0279(4) Uani 1 1 d U . . H22 H 0.2541 0.5808 0.0650 0.034 Uiso 1 1 calc R . . C41 C 0.08609(19) 0.52486(14) 0.08078(11) 0.0356(4) Uani 1 1 d U . . H23 H 0.0352 0.5656 0.0450 0.043 Uiso 1 1 calc R . . C42 C 0.03156(19) 0.45635(15) 0.12111(12) 0.0385(5) Uani 1 1 d U . . H24 H -0.0563 0.4499 0.1123 0.046 Uiso 1 1 calc R . . C43 C 0.10483(18) 0.39694(14) 0.17443(11) 0.0331(4) Uani 1 1 d U . . H25 H 0.0668 0.3505 0.2026 0.040 Uiso 1 1 calc R . . C44 C 0.23357(16) 0.40603(11) 0.18609(10) 0.0233(3) Uani 1 1 d U . . C45 C 0.55818(15) 0.61903(10) 0.21399(9) 0.0190(3) Uani 1 1 d U . . C46 C 0.66983(16) 0.58697(12) 0.16700(10) 0.0252(3) Uani 1 1 d U . . H26 H 0.7368 0.5459 0.1911 0.030 Uiso 1 1 calc R . . C47 C 0.68316(18) 0.61508(13) 0.08514(11) 0.0310(4) Uani 1 1 d U . . H27 H 0.7596 0.5933 0.0537 0.037 Uiso 1 1 calc R . . C48 C 0.5870(2) 0.67395(14) 0.04934(11) 0.0353(4) Uani 1 1 d U . . H28 H 0.5956 0.6916 -0.0069 0.042 Uiso 1 1 calc R . . C49 C 0.4770(2) 0.70763(13) 0.09562(11) 0.0354(4) Uani 1 1 d U . . H29 H 0.4111 0.7492 0.0712 0.043 Uiso 1 1 calc R . . C50 C 0.46321(17) 0.68061(11) 0.17797(10) 0.0255(3) Uani 1 1 d U . . H30 H 0.3885 0.7045 0.2095 0.031 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.02552(15) 0.01736(15) 0.01096(14) 0.00036(9) -0.00300(9) -0.00866(9) N1 0.0223(7) 0.0183(7) 0.0131(6) -0.0017(5) -0.0015(5) -0.0079(5) N2 0.0239(7) 0.0175(7) 0.0121(6) -0.0015(5) -0.0012(5) -0.0078(5) C1 0.0200(7) 0.0173(8) 0.0139(7) -0.0010(6) -0.0016(5) -0.0041(5) C2 0.0228(8) 0.0193(8) 0.0142(7) 0.0003(6) -0.0011(5) -0.0064(6) C3 0.0207(8) 0.0169(8) 0.0156(7) 0.0001(6) -0.0001(5) -0.0051(5) C4 0.0209(7) 0.0156(7) 0.0153(7) -0.0029(6) 0.0000(5) -0.0049(5) C5 0.0193(7) 0.0162(7) 0.0148(7) -0.0016(6) -0.0012(5) -0.0036(5) C6 0.0217(8) 0.0184(8) 0.0142(7) -0.0038(6) -0.0025(5) -0.0056(6) C7 0.0242(8) 0.0192(8) 0.0128(7) -0.0022(6) -0.0025(5) -0.0059(6) C8 0.0219(8) 0.0180(8) 0.0150(7) -0.0010(6) -0.0040(5) -0.0032(5) C9 0.0190(7) 0.0173(7) 0.0128(7) -0.0010(6) -0.0026(5) -0.0027(5) C10 0.0198(7) 0.0182(8) 0.0131(7) 0.0005(6) -0.0026(5) -0.0042(5) C11 0.0306(9) 0.0245(9) 0.0148(8) 0.0003(6) -0.0002(6) -0.0116(6) C12 0.0283(9) 0.0249(9) 0.0239(9) 0.0051(7) -0.0003(6) -0.0106(6) C13 0.0490(12) 0.0343(11) 0.0323(11) 0.0109(8) -0.0086(8) -0.0159(8) C14 0.0610(14) 0.0292(11) 0.0538(15) 0.0159(10) -0.0158(11) -0.0047(9) C15 0.0598(14) 0.0207(10) 0.0579(15) 0.0047(10) -0.0071(11) -0.0064(9) C16 0.0378(10) 0.0206(9) 0.0391(11) -0.0030(8) 0.0016(8) -0.0077(7) C17 0.0257(8) 0.0194(8) 0.0255(9) 0.0008(7) 0.0013(6) -0.0094(6) C18 0.0218(8) 0.0189(8) 0.0183(8) -0.0025(6) 0.0012(6) -0.0074(6) C19 0.0248(8) 0.0210(8) 0.0210(8) -0.0046(6) 0.0022(6) -0.0072(6) C20 0.0291(9) 0.0305(10) 0.0289(9) -0.0062(8) -0.0017(7) -0.0082(7) C21 0.0272(10) 0.0470(13) 0.0461(13) -0.0136(10) 0.0000(8) -0.0019(8) C22 0.0349(11) 0.0535(14) 0.0449(13) -0.0238(11) 0.0115(9) -0.0061(9) C23 0.0402(11) 0.0446(12) 0.0250(10) -0.0148(9) 0.0078(7) -0.0148(8) C24 0.0315(9) 0.0264(9) 0.0177(8) -0.0046(7) 0.0041(6) -0.0127(7) C25 0.0270(8) 0.0189(8) 0.0118(7) -0.0020(6) 0.0001(6) -0.0087(6) C26 0.0271(9) 0.0248(9) 0.0255(9) -0.0005(7) -0.0068(6) -0.0051(6) C27 0.0336(10) 0.0371(11) 0.0436(12) -0.0024(9) -0.0118(8) -0.0169(8) C28 0.0571(13) 0.0307(11) 0.0463(13) -0.0069(9) -0.0136(10) -0.0235(9) C29 0.0570(12) 0.0184(9) 0.0360(11) -0.0057(8) -0.0022(9) -0.0080(8) C30 0.0295(9) 0.0233(9) 0.0262(9) -0.0053(7) -0.0004(6) -0.0053(6) C31 0.0340(9) 0.0208(8) 0.0142(7) -0.0030(6) -0.0048(6) -0.0099(6) C32 0.0403(9) 0.0231(9) 0.0145(8) -0.0047(7) -0.0047(6) -0.0068(7) C33 0.0545(12) 0.0247(10) 0.0257(10) -0.0061(8) -0.0049(8) -0.0024(8) C34 0.0619(14) 0.0331(11) 0.0366(12) -0.0105(9) 0.0011(9) 0.0077(9) C35 0.0436(11) 0.0466(13) 0.0316(11) -0.0108(9) 0.0054(8) 0.0068(9) C36 0.0387(10) 0.0375(11) 0.0216(9) -0.0084(8) 0.0017(7) -0.0050(8) C37 0.0342(9) 0.0249(9) 0.0135(7) -0.0043(6) -0.0034(6) -0.0072(6) C38 0.0310(8) 0.0238(8) 0.0109(7) -0.0017(6) -0.0030(6) -0.0085(6) C39 0.0322(9) 0.0231(8) 0.0125(7) -0.0045(6) -0.0044(6) -0.0050(6) C40 0.0405(10) 0.0298(10) 0.0136(8) -0.0048(7) -0.0051(6) -0.0019(7) C41 0.0377(10) 0.0484(12) 0.0200(9) -0.0099(8) -0.0092(7) 0.0043(8) C42 0.0314(10) 0.0594(14) 0.0276(10) -0.0125(9) -0.0087(7) -0.0059(9) C43 0.0365(10) 0.0451(12) 0.0219(9) -0.0084(8) -0.0043(7) -0.0133(8) C44 0.0314(9) 0.0284(9) 0.0133(7) -0.0069(7) -0.0044(6) -0.0088(7) C45 0.0241(8) 0.0197(8) 0.0153(7) -0.0024(6) -0.0037(6) -0.0082(6) C46 0.0239(8) 0.0321(10) 0.0194(8) -0.0022(7) 0.0003(6) -0.0054(6) C47 0.0354(10) 0.0401(11) 0.0197(9) -0.0058(8) 0.0057(7) -0.0143(8) C48 0.0499(11) 0.0451(12) 0.0124(8) 0.0036(8) -0.0012(7) -0.0172(9) C49 0.0447(11) 0.0373(11) 0.0224(9) 0.0085(8) -0.0094(7) -0.0061(8) C50 0.0322(9) 0.0242(9) 0.0200(8) 0.0013(7) -0.0045(6) -0.0058(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 Zn1 N2 2.0552(12) . ? Zn1 N2 2.0552(12) 2_666 ? Zn1 N1 2.0641(13) . ? Zn1 N1 2.0641(13) 2_666 ? N1 C1 1.3698(19) . ? N1 C4 1.3829(18) . ? N2 C9 1.3772(19) . ? N2 C6 1.3787(19) . ? C1 C10 1.402(2) 2_666 ? C1 C2 1.453(2) . ? C2 C3 1.368(2) . ? C2 C11 1.525(2) . ? C3 C4 1.448(2) . ? C3 C18 1.527(2) . ? C4 C5 1.401(2) . ? C5 C6 1.403(2) . ? C5 C25 1.487(2) . ? C6 C7 1.450(2) . ? C7 C8 1.360(2) . ? C7 C31 1.529(2) . ? C8 C9 1.447(2) . ? C8 C38 1.525(2) . ? C9 C10 1.408(2) . ? C10 C1 1.402(2) 2_666 ? C10 C45 1.493(2) . ? C11 C24 1.527(2) . ? C11 C12 1.530(2) . ? C11 H1 1.0000 . ? C12 C13 1.392(3) . ? C12 C17 1.394(2) . ? C13 C14 1.378(3) . ? C13 H2 0.9500 . ? C14 C15 1.376(3) . ? C14 H3 0.9500 . ? C15 C16 1.406(3) . ? C15 H4 0.9500 . ? C16 C17 1.394(2) . ? C16 H5 0.9500 . ? C17 C18 1.515(2) . ? C18 C19 1.534(2) . ? C18 H6 1.0000 . ? C19 C20 1.377(2) . ? C19 C24 1.400(2) . ? C20 C21 1.394(3) . ? C20 H7 0.9500 . ? C21 C22 1.388(3) . ? C21 H8 0.9500 . ? C22 C23 1.382(3) . ? C22 H9 0.9500 . ? C23 C24 1.385(2) . ? C23 H10 0.9500 . ? C25 C30 1.389(2) . ? C25 C26 1.392(2) . ? C26 C27 1.393(2) . ? C26 H11 0.9500 . ? C27 C28 1.378(3) . ? C27 H12 0.9500 . ? C28 C29 1.381(3) . ? C28 H13 0.9500 . ? C29 C30 1.388(2) . ? C29 H14 0.9500 . ? C30 H15 0.9500 . ? C31 C44 1.527(2) . ? C31 C32 1.530(2) . ? C31 H16 1.0000 . ? C32 C33 1.373(3) . ? C32 C37 1.405(2) . ? C33 C34 1.393(3) . ? C33 H17 0.9500 . ? C34 C35 1.372(3) . ? C34 H18 0.9500 . ? C35 C36 1.395(3) . ? C35 H19 0.9500 . ? C36 C37 1.382(2) . ? C36 H20 0.9500 . ? C37 C38 1.523(2) . ? C38 C39 1.529(2) . ? C38 H21 1.0000 . ? C39 C40 1.384(2) . ? C39 C44 1.394(2) . ? C40 C41 1.402(3) . ? C40 H22 0.9500 . ? C41 C42 1.387(3) . ? C41 H23 0.9500 . ? C42 C43 1.393(3) . ? C42 H24 0.9500 . ? C43 C44 1.386(2) . ? C43 H25 0.9500 . ? C45 C50 1.389(2) . ? C45 C46 1.399(2) . ? C46 C47 1.391(2) . ? C46 H26 0.9500 . ? C47 C48 1.372(3) . ? C47 H27 0.9500 . ? C48 C49 1.389(3) . ? C48 H28 0.9500 . ? C49 C50 1.396(2) . ? C49 H29 0.9500 . ? C50 H30 0.9500 . ? 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 N2 Zn1 N2 180.000(1) . 2_666 ? N2 Zn1 N1 90.44(5) . . ? N2 Zn1 N1 89.56(5) 2_666 . ? N2 Zn1 N1 89.56(5) . 2_666 ? N2 Zn1 N1 90.44(5) 2_666 2_666 ? N1 Zn1 N1 180.00(4) . 2_666 ? C1 N1 C4 107.19(12) . . ? C1 N1 Zn1 126.62(10) . . ? C4 N1 Zn1 125.70(10) . . ? C9 N2 C6 107.20(12) . . ? C9 N2 Zn1 126.39(10) . . ? C6 N2 Zn1 125.99(10) . . ? N1 C1 C10 125.63(14) . 2_666 ? N1 C1 C2 109.56(13) . . ? C10 C1 C2 124.81(14) 2_666 . ? C3 C2 C1 106.88(13) . . ? C3 C2 C11 114.05(13) . . ? C1 C2 C11 138.09(14) . . ? C2 C3 C4 107.10(13) . . ? C2 C3 C18 114.13(13) . . ? C4 C3 C18 137.88(14) . . ? N1 C4 C5 125.87(14) . . ? N1 C4 C3 109.27(13) . . ? C5 C4 C3 124.79(14) . . ? C4 C5 C6 125.85(14) . . ? C4 C5 C25 116.56(13) . . ? C6 C5 C25 117.58(13) . . ? N2 C6 C5 125.97(14) . . ? N2 C6 C7 108.92(13) . . ? C5 C6 C7 125.06(14) . . ? C8 C7 C6 107.46(13) . . ? C8 C7 C31 114.61(14) . . ? C6 C7 C31 137.66(14) . . ? C7 C8 C9 107.01(13) . . ? C7 C8 C38 114.06(13) . . ? C9 C8 C38 138.66(14) . . ? N2 C9 C10 125.86(13) . . ? N2 C9 C8 109.40(13) . . ? C10 C9 C8 124.71(14) . . ? C1 C10 C9 125.42(14) 2_666 . ? C1 C10 C45 117.96(13) 2_666 . ? C9 C10 C45 116.60(13) . . ? C2 C11 C24 103.43(13) . . ? C2 C11 C12 105.89(13) . . ? C24 C11 C12 105.40(13) . . ? C2 C11 H1 113.7 . . ? C24 C11 H1 113.7 . . ? C12 C11 H1 113.7 . . ? C13 C12 C17 120.52(17) . . ? C13 C12 C11 126.17(17) . . ? C17 C12 C11 113.31(15) . . ? C14 C13 C12 119.1(2) . . ? C14 C13 H2 120.5 . . ? C12 C13 H2 120.5 . . ? C15 C14 C13 121.1(2) . . ? C15 C14 H3 119.4 . . ? C13 C14 H3 119.4 . . ? C14 C15 C16 120.6(2) . . ? C14 C15 H4 119.7 . . ? C16 C15 H4 119.7 . . ? C17 C16 C15 118.35(19) . . ? C17 C16 H5 120.8 . . ? C15 C16 H5 120.8 . . ? C12 C17 C16 120.31(17) . . ? C12 C17 C18 113.91(14) . . ? C16 C17 C18 125.77(16) . . ? C17 C18 C3 105.90(12) . . ? C17 C18 C19 106.10(13) . . ? C3 C18 C19 102.91(12) . . ? C17 C18 H6 113.7 . . ? C3 C18 H6 113.7 . . ? C19 C18 H6 113.7 . . ? C20 C19 C24 121.13(15) . . ? C20 C19 C18 125.72(15) . . ? C24 C19 C18 113.12(14) . . ? C19 C20 C21 118.82(17) . . ? C19 C20 H7 120.6 . . ? C21 C20 H7 120.6 . . ? C22 C21 C20 120.27(18) . . ? C22 C21 H8 119.9 . . ? C20 C21 H8 119.9 . . ? C23 C22 C21 120.63(17) . . ? C23 C22 H9 119.7 . . ? C21 C22 H9 119.7 . . ? C22 C23 C24 119.57(17) . . ? C22 C23 H10 120.2 . . ? C24 C23 H10 120.2 . . ? C23 C24 C19 119.55(16) . . ? C23 C24 C11 126.79(15) . . ? C19 C24 C11 113.59(14) . . ? C30 C25 C26 118.86(15) . . ? C30 C25 C5 120.44(14) . . ? C26 C25 C5 120.69(14) . . ? C25 C26 C27 120.18(17) . . ? C25 C26 H11 119.9 . . ? C27 C26 H11 119.9 . . ? C28 C27 C26 120.19(17) . . ? C28 C27 H12 119.9 . . ? C26 C27 H12 119.9 . . ? C27 C28 C29 120.20(17) . . ? C27 C28 H13 119.9 . . ? C29 C28 H13 119.9 . . ? C28 C29 C30 119.70(18) . . ? C28 C29 H14 120.2 . . ? C30 C29 H14 120.2 . . ? C29 C30 C25 120.87(16) . . ? C29 C30 H15 119.6 . . ? C25 C30 H15 119.6 . . ? C44 C31 C7 104.81(13) . . ? C44 C31 C32 105.34(13) . . ? C7 C31 C32 104.18(12) . . ? C44 C31 H16 113.8 . . ? C7 C31 H16 113.8 . . ? C32 C31 H16 113.8 . . ? C33 C32 C37 120.37(17) . . ? C33 C32 C31 126.52(17) . . ? C37 C32 C31 113.11(15) . . ? C32 C33 C34 119.32(19) . . ? C32 C33 H17 120.3 . . ? C34 C33 H17 120.3 . . ? C35 C34 C33 120.43(19) . . ? C35 C34 H18 119.8 . . ? C33 C34 H18 119.8 . . ? C34 C35 C36 120.93(19) . . ? C34 C35 H19 119.5 . . ? C36 C35 H19 119.5 . . ? C37 C36 C35 118.72(19) . . ? C37 C36 H20 120.6 . . ? C35 C36 H20 120.6 . . ? C36 C37 C32 120.21(17) . . ? C36 C37 C38 126.09(16) . . ? C32 C37 C38 113.69(15) . . ? C37 C38 C8 103.94(13) . . ? C37 C38 C39 105.65(13) . . ? C8 C38 C39 105.11(13) . . ? C37 C38 H21 113.7 . . ? C8 C38 H21 113.7 . . ? C39 C38 H21 113.7 . . ? C40 C39 C44 120.40(15) . . ? C40 C39 C38 125.96(16) . . ? C44 C39 C38 113.64(14) . . ? C39 C40 C41 119.35(18) . . ? C39 C40 H22 120.3 . . ? C41 C40 H22 120.3 . . ? C42 C41 C40 120.07(18) . . ? C42 C41 H23 120.0 . . ? C40 C41 H23 120.0 . . ? C41 C42 C43 120.38(18) . . ? C41 C42 H24 119.8 . . ? C43 C42 H24 119.8 . . ? C44 C43 C42 119.51(19) . . ? C44 C43 H25 120.2 . . ? C42 C43 H25 120.2 . . ? C43 C44 C39 120.29(17) . . ? C43 C44 C31 126.14(16) . . ? C39 C44 C31 113.57(14) . . ? C50 C45 C46 118.90(15) . . ? C50 C45 C10 120.01(15) . . ? C46 C45 C10 121.04(15) . . ? C47 C46 C45 120.21(17) . . ? C47 C46 H26 119.9 . . ? C45 C46 H26 119.9 . . ? C48 C47 C46 120.63(17) . . ? C48 C47 H27 119.7 . . ? C46 C47 H27 119.7 . . ? C47 C48 C49 119.74(17) . . ? C47 C48 H28 120.1 . . ? C49 C48 H28 120.1 . . ? C48 C49 C50 120.15(18) . . ? C48 C49 H29 119.9 . . ? C50 C49 H29 119.9 . . ? C45 C50 C49 120.32(17) . . ? C45 C50 H30 119.8 . . ? C49 C50 H30 119.8 . . ? 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 N2 Zn1 N1 C1 -172.38(13) . . . . ? N2 Zn1 N1 C1 7.62(13) 2_666 . . . ? N2 Zn1 N1 C4 -1.54(12) . . . . ? N2 Zn1 N1 C4 178.46(12) 2_666 . . . ? N1 Zn1 N2 C9 -173.88(13) . . . . ? N1 Zn1 N2 C9 6.12(13) 2_666 . . . ? N1 Zn1 N2 C6 -2.27(13) . . . . ? N1 Zn1 N2 C6 177.73(13) 2_666 . . . ? C4 N1 C1 C10 -179.69(14) . . . 2_666 ? Zn1 N1 C1 C10 -7.5(2) . . . 2_666 ? C4 N1 C1 C2 -0.02(17) . . . . ? Zn1 N1 C1 C2 172.20(10) . . . . ? N1 C1 C2 C3 0.21(17) . . . . ? C10 C1 C2 C3 179.88(15) 2_666 . . . ? N1 C1 C2 C11 -167.14(18) . . . . ? C10 C1 C2 C11 12.5(3) 2_666 . . . ? C1 C2 C3 C4 -0.30(17) . . . . ? C11 C2 C3 C4 170.48(13) . . . . ? C1 C2 C3 C18 -171.49(13) . . . . ? C11 C2 C3 C18 -0.72(19) . . . . ? C1 N1 C4 C5 176.79(14) . . . . ? Zn1 N1 C4 C5 4.5(2) . . . . ? C1 N1 C4 C3 -0.17(17) . . . . ? Zn1 N1 C4 C3 -172.48(10) . . . . ? C2 C3 C4 N1 0.30(17) . . . . ? C18 C3 C4 N1 168.28(17) . . . . ? C2 C3 C4 C5 -176.70(15) . . . . ? C18 C3 C4 C5 -8.7(3) . . . . ? N1 C4 C5 C6 -3.6(3) . . . . ? C3 C4 C5 C6 172.90(15) . . . . ? N1 C4 C5 C25 175.31(14) . . . . ? C3 C4 C5 C25 -8.2(2) . . . . ? C9 N2 C6 C5 176.68(14) . . . . ? Zn1 N2 C6 C5 3.7(2) . . . . ? C9 N2 C6 C7 -0.94(17) . . . . ? Zn1 N2 C6 C7 -173.88(10) . . . . ? C4 C5 C6 N2 -0.9(3) . . . . ? C25 C5 C6 N2 -179.76(14) . . . . ? C4 C5 C6 C7 176.40(15) . . . . ? C25 C5 C6 C7 -2.5(2) . . . . ? N2 C6 C7 C8 0.58(17) . . . . ? C5 C6 C7 C8 -177.07(15) . . . . ? N2 C6 C7 C31 173.86(17) . . . . ? C5 C6 C7 C31 -3.8(3) . . . . ? C6 C7 C8 C9 0.01(17) . . . . ? C31 C7 C8 C9 -175.02(13) . . . . ? C6 C7 C8 C38 175.22(13) . . . . ? C31 C7 C8 C38 0.2(2) . . . . ? C6 N2 C9 C10 -177.23(14) . . . . ? Zn1 N2 C9 C10 -4.3(2) . . . . ? C6 N2 C9 C8 0.95(17) . . . . ? Zn1 N2 C9 C8 173.85(10) . . . . ? C7 C8 C9 N2 -0.59(18) . . . . ? C38 C8 C9 N2 -173.97(17) . . . . ? C7 C8 C9 C10 177.61(14) . . . . ? C38 C8 C9 C10 4.2(3) . . . . ? N2 C9 C10 C1 1.3(3) . . . 2_666 ? C8 C9 C10 C1 -176.65(14) . . . 2_666 ? N2 C9 C10 C45 179.62(14) . . . . ? C8 C9 C10 C45 1.7(2) . . . . ? C3 C2 C11 C24 -56.03(17) . . . . ? C1 C2 C11 C24 110.7(2) . . . . ? C3 C2 C11 C12 54.57(18) . . . . ? C1 C2 C11 C12 -138.70(19) . . . . ? C2 C11 C12 C13 126.76(18) . . . . ? C24 C11 C12 C13 -124.04(18) . . . . ? C2 C11 C12 C17 -53.45(17) . . . . ? C24 C11 C12 C17 55.75(17) . . . . ? C17 C12 C13 C14 0.1(3) . . . . ? C11 C12 C13 C14 179.92(18) . . . . ? C12 C13 C14 C15 -0.2(3) . . . . ? C13 C14 C15 C16 0.3(4) . . . . ? C14 C15 C16 C17 -0.3(3) . . . . ? C13 C12 C17 C16 -0.1(2) . . . . ? C11 C12 C17 C16 -179.94(15) . . . . ? C13 C12 C17 C18 178.88(16) . . . . ? C11 C12 C17 C18 -0.93(19) . . . . ? C15 C16 C17 C12 0.2(3) . . . . ? C15 C16 C17 C18 -178.68(17) . . . . ? C12 C17 C18 C3 54.56(17) . . . . ? C16 C17 C18 C3 -126.49(17) . . . . ? C12 C17 C18 C19 -54.34(17) . . . . ? C16 C17 C18 C19 124.60(17) . . . . ? C2 C3 C18 C17 -54.02(17) . . . . ? C4 C3 C18 C17 138.58(19) . . . . ? C2 C3 C18 C19 57.15(17) . . . . ? C4 C3 C18 C19 -110.3(2) . . . . ? C17 C18 C19 C20 -127.52(18) . . . . ? C3 C18 C19 C20 121.46(17) . . . . ? C17 C18 C19 C24 54.58(17) . . . . ? C3 C18 C19 C24 -56.43(17) . . . . ? C24 C19 C20 C21 1.0(3) . . . . ? C18 C19 C20 C21 -176.73(18) . . . . ? C19 C20 C21 C22 -1.5(3) . . . . ? C20 C21 C22 C23 1.3(3) . . . . ? C21 C22 C23 C24 -0.5(3) . . . . ? C22 C23 C24 C19 0.0(3) . . . . ? C22 C23 C24 C11 176.96(19) . . . . ? C20 C19 C24 C23 -0.3(3) . . . . ? C18 C19 C24 C23 177.74(16) . . . . ? C20 C19 C24 C11 -177.60(16) . . . . ? C18 C19 C24 C11 0.4(2) . . . . ? C2 C11 C24 C23 -121.35(19) . . . . ? C12 C11 C24 C23 127.69(19) . . . . ? C2 C11 C24 C19 55.77(18) . . . . ? C12 C11 C24 C19 -55.20(18) . . . . ? C4 C5 C25 C30 -79.92(19) . . . . ? C6 C5 C25 C30 99.09(18) . . . . ? C4 C5 C25 C26 99.18(18) . . . . ? C6 C5 C25 C26 -81.81(19) . . . . ? C30 C25 C26 C27 0.9(3) . . . . ? C5 C25 C26 C27 -178.20(16) . . . . ? C25 C26 C27 C28 -0.6(3) . . . . ? C26 C27 C28 C29 -0.1(3) . . . . ? C27 C28 C29 C30 0.6(3) . . . . ? C28 C29 C30 C25 -0.3(3) . . . . ? C26 C25 C30 C29 -0.4(3) . . . . ? C5 C25 C30 C29 178.68(16) . . . . ? C8 C7 C31 C44 -54.99(18) . . . . ? C6 C7 C31 C44 132.06(19) . . . . ? C8 C7 C31 C32 55.44(18) . . . . ? C6 C7 C31 C32 -117.5(2) . . . . ? C44 C31 C32 C33 -125.41(18) . . . . ? C7 C31 C32 C33 124.55(18) . . . . ? C44 C31 C32 C37 55.81(17) . . . . ? C7 C31 C32 C37 -54.22(17) . . . . ? C37 C32 C33 C34 1.3(3) . . . . ? C31 C32 C33 C34 -177.36(18) . . . . ? C32 C33 C34 C35 -0.3(3) . . . . ? C33 C34 C35 C36 -1.0(3) . . . . ? C34 C35 C36 C37 1.3(3) . . . . ? C35 C36 C37 C32 -0.3(3) . . . . ? C35 C36 C37 C38 178.39(17) . . . . ? C33 C32 C37 C36 -1.0(2) . . . . ? C31 C32 C37 C36 177.82(15) . . . . ? C33 C32 C37 C38 -179.85(15) . . . . ? C31 C32 C37 C38 -0.99(19) . . . . ? C36 C37 C38 C8 -122.63(17) . . . . ? C32 C37 C38 C8 56.10(17) . . . . ? C36 C37 C38 C39 126.97(17) . . . . ? C32 C37 C38 C39 -54.29(17) . . . . ? C7 C8 C38 C37 -56.07(17) . . . . ? C9 C8 C38 C37 117.0(2) . . . . ? C7 C8 C38 C39 54.72(18) . . . . ? C9 C8 C38 C39 -132.22(19) . . . . ? C37 C38 C39 C40 -125.47(17) . . . . ? C8 C38 C39 C40 124.96(17) . . . . ? C37 C38 C39 C44 55.04(17) . . . . ? C8 C38 C39 C44 -54.52(17) . . . . ? C44 C39 C40 C41 0.0(3) . . . . ? C38 C39 C40 C41 -179.50(15) . . . . ? C39 C40 C41 C42 -0.3(3) . . . . ? C40 C41 C42 C43 0.8(3) . . . . ? C41 C42 C43 C44 -0.9(3) . . . . ? C42 C43 C44 C39 0.6(3) . . . . ? C42 C43 C44 C31 179.97(16) . . . . ? C40 C39 C44 C43 -0.1(2) . . . . ? C38 C39 C44 C43 179.44(15) . . . . ? C40 C39 C44 C31 -179.56(15) . . . . ? C38 C39 C44 C31 -0.04(19) . . . . ? C7 C31 C44 C43 -125.17(17) . . . . ? C32 C31 C44 C43 125.24(18) . . . . ? C7 C31 C44 C39 54.27(17) . . . . ? C32 C31 C44 C39 -55.32(17) . . . . ? C1 C10 C45 C50 -92.12(18) 2_666 . . . ? C9 C10 C45 C50 89.39(19) . . . . ? C1 C10 C45 C46 90.49(19) 2_666 . . . ? C9 C10 C45 C46 -88.00(18) . . . . ? C50 C45 C46 C47 -1.6(2) . . . . ? C10 C45 C46 C47 175.82(15) . . . . ? C45 C46 C47 C48 -0.4(3) . . . . ? C46 C47 C48 C49 1.8(3) . . . . ? C47 C48 C49 C50 -1.1(3) . . . . ? C46 C45 C50 C49 2.3(2) . . . . ? C10 C45 C50 C49 -175.17(15) . . . . ? C48 C49 C50 C45 -0.9(3) . . . . ? #============================================================================== data_12-9PhBrsqueezed(12-4PhBr) _database_code_depnum_ccdc_archive 'CCDC 248906' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C162 H107 Br9 N4 ' _chemical_formula_moiety 'C108 H62 N4, 9(C6 H5 Br)' _chemical_formula_weight 2829.80 _chemical_melting_point ? # CRYSTAL DATA _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 42/n ' _symmetry_space_group_name_Hall '-P 4bc' _symmetry_Int_Tables_number 86 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' Br Br -0.2901 2.4595 '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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x+1/2, z+1/2' '-x+1/2, -y+1/2, z' 'y+1/2, -x, z+1/2' '-x, -y, -z' 'y, -x-1/2, -z-1/2' 'x-1/2, y-1/2, -z' '-y-1/2, x, -z-1/2' _cell_length_a 22.6270(13) _cell_length_b 22.6270(13) _cell_length_c 12.7634(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6534.6(7) _cell_formula_units_Z 2 _cell_measurement_reflns_used 10488 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 123.1 _exptl_crystal_description Platelet _exptl_crystal_colour Red _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.438 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2846 _exptl_absorpt_coefficient_mu 2.816 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details Coppens_numerical _exptl_absorpt_correction_T_min 0.2828 _exptl_absorpt_correction_T_max 0.7660 _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoKa _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type MERCURY _diffrn_measurement_method w _diffrn_detector_area_resol_mean 14.62 _diffrn_reflns_number 52854 _diffrn_reflns_av_R_equivalents 0.0858 _diffrn_reflns_av_sigmaI/netI 0.0731 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.990 _reflns_number_total 7430 _reflns_number_gt 4697 _reflns_threshold_expression >2sigma(I) _computing_data_collection CRYSTALCLEAR _computing_cell_refinement CRYSTALCLEAR _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement 'Shelxh-97 and PLATON SQUEEZE' _computing_publication_material 'CrystalStructure Ver. 3.5.1' _computing_molecular_graphics ? _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. Disordered solvent molecules are removed by the PLATON SQUEEZE method. ; _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^)+(0.1000P)^2^+2.0000P] 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 noref _refine_ls_number_reflns 7430 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1168 _refine_ls_R_factor_gt 0.0890 _refine_ls_wR_factor_ref 0.2378 _refine_ls_wR_factor_gt 0.2291 _refine_ls_goodness_of_fit_ref 1.242 _refine_ls_restrained_S_all 1.242 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.284 _refine_diff_density_min -0.713 _refine_diff_density_rms 0.095 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 Br1 Br 0.34776(3) 0.55719(3) 0.34218(4) 0.0554(2) Uani 1 1 d . . . N1 N 0.66684(14) 0.71132(13) 0.7501(2) 0.0236(7) Uani 1 1 d . . . C1 C 0.61469(17) 0.74156(17) 0.7448(3) 0.0256(8) Uani 1 1 d . . . C2 C 0.56862(18) 0.69859(18) 0.7281(3) 0.0324(9) Uani 1 1 d . . . C3 C 0.59356(18) 0.64459(17) 0.7235(3) 0.0284(8) Uani 1 1 d . . . C4 C 0.65596(17) 0.65197(17) 0.7379(3) 0.0274(8) Uani 1 1 d . . . C5 C 0.69841(17) 0.60741(16) 0.7442(3) 0.0246(7) Uani 1 1 d . . . C6 C 0.50265(16) 0.70012(17) 0.7088(3) 0.0252(8) Uani 1 1 d . . . C7 C 0.47655(19) 0.65572(18) 0.7856(3) 0.0321(9) Uani 1 1 d . . . C8 C 0.43235(18) 0.66744(19) 0.8565(3) 0.0313(9) Uani 1 1 d . . . C9 C 0.41216(18) 0.62241(19) 0.9270(3) 0.0331(9) Uani 1 1 d . . . C10 C 0.3663(2) 0.6316(2) 0.9985(3) 0.0435(11) Uani 1 1 d . . . C11 C 0.3461(2) 0.5879(3) 1.0616(3) 0.0489(12) Uani 1 1 d . . . C12 C 0.3695(2) 0.5303(2) 1.0521(3) 0.0475(12) Uani 1 1 d . . . C13 C 0.4150(2) 0.5190(2) 0.9845(3) 0.0413(11) Uani 1 1 d . . . C14 C 0.43682(19) 0.5648(2) 0.9189(3) 0.0358(10) Uani 1 1 d . . . C15 C 0.4834(2) 0.55490(19) 0.8442(3) 0.0370(10) Uani 1 1 d . . . C16 C 0.50280(17) 0.59873(18) 0.7802(3) 0.0299(9) Uani 1 1 d . . . C17 C 0.55271(19) 0.59526(18) 0.6991(3) 0.0328(9) Uani 1 1 d . . . C18 C 0.52434(19) 0.61431(19) 0.5955(3) 0.0329(9) Uani 1 1 d . . . C19 C 0.52746(18) 0.58450(18) 0.5027(3) 0.0288(8) Uani 1 1 d . . . C20 C 0.5029(2) 0.60880(19) 0.4105(3) 0.0358(9) Uani 1 1 d . . . C21 C 0.5100(2) 0.5838(2) 0.3097(4) 0.0446(11) Uani 1 1 d . . . C22 C 0.4886(3) 0.6095(3) 0.2217(4) 0.0631(16) Uani 1 1 d . . . C23 C 0.4603(3) 0.6649(3) 0.2290(4) 0.0624(16) Uani 1 1 d . . . C24 C 0.4527(3) 0.6927(2) 0.3229(4) 0.0512(13) Uani 1 1 d . . . C25 C 0.4756(2) 0.6660(2) 0.4157(3) 0.0382(10) Uani 1 1 d . . . C26 C 0.4725(2) 0.6958(2) 0.5147(3) 0.0377(10) Uani 1 1 d . . . C27 C 0.49703(16) 0.67082(17) 0.6011(3) 0.0259(8) Uani 1 1 d . . . C28 C 0.3389(2) 0.5352(3) 0.4839(4) 0.0561(14) Uani 1 1 d . . . C29 C 0.3044(3) 0.4872(3) 0.5077(4) 0.0700(18) Uani 1 1 d . . . C30 C 0.2976(3) 0.4707(4) 0.6129(5) 0.082(2) Uani 1 1 d . . . C31 C 0.3286(4) 0.5016(5) 0.6907(5) 0.094(3) Uani 1 1 d . . . C32 C 0.3600(3) 0.5523(4) 0.6631(5) 0.087(3) Uani 1 1 d . . . C33 C 0.3673(3) 0.5658(3) 0.5612(6) 0.0758(19) Uani 1 1 d . . . H1 H 0.7010 0.7269 0.7599 0.028 Uiso 0.50 1 d P . . H2 H 0.6846 0.5687 0.7406 0.029 Uiso 1 1 c . . . H3 H 0.4852 0.7397 0.7131 0.030 Uiso 1 1 c . . . H4 H 0.4154 0.7049 0.8589 0.037 Uiso 1 1 c . . . H5 H 0.3492 0.6688 1.0028 0.052 Uiso 1 1 c . . . H6 H 0.3170 0.5957 1.1113 0.058 Uiso 1 1 c . . . H7 H 0.3540 0.4997 1.0920 0.057 Uiso 1 1 c . . . H8 H 0.4314 0.4814 0.9810 0.048 Uiso 1 1 c . . . H9 H 0.5007 0.5176 0.8394 0.044 Uiso 1 1 c . . . H10 H 0.5721 0.5566 0.6959 0.039 Uiso 1 1 c . . . H11 H 0.5458 0.5478 0.5004 0.034 Uiso 1 1 c . . . H12 H 0.5298 0.5479 0.3036 0.053 Uiso 1 1 c . . . H13 H 0.4924 0.5909 0.1572 0.074 Uiso 1 1 c . . . H14 H 0.4465 0.6830 0.1682 0.074 Uiso 1 1 c . . . H15 H 0.4326 0.7284 0.3267 0.061 Uiso 1 1 c . . . H16 H 0.4533 0.7320 0.5198 0.045 Uiso 1 1 c . . . H17 H 0.2858 0.4660 0.4544 0.082 Uiso 1 1 c . . . H18 H 0.2729 0.4392 0.6307 0.097 Uiso 1 1 c . . . H19 H 0.3282 0.4889 0.7596 0.111 Uiso 1 1 c . . . H20 H 0.3758 0.5766 0.7147 0.103 Uiso 1 1 c . . . H21 H 0.3926 0.5965 0.5426 0.089 Uiso 1 1 c . . . 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 Br1 0.0477(4) 0.0495(4) 0.0690(4) -0.0038(2) -0.0063(2) -0.0054(3) N1 0.0213(16) 0.0220(16) 0.0275(15) -0.0023(12) -0.0022(11) -0.0021(12) C1 0.025(2) 0.027(2) 0.0252(17) 0.0010(14) -0.0018(14) 0.0001(15) C2 0.026(2) 0.028(2) 0.043(2) 0.0007(16) -0.0038(16) -0.0016(17) C3 0.026(2) 0.021(2) 0.039(2) -0.0037(15) -0.0055(15) 0.0033(16) C4 0.024(2) 0.026(2) 0.0323(18) -0.0007(15) -0.0013(14) -0.0031(16) C5 0.0231(19) 0.0148(18) 0.0360(19) 0.0004(14) -0.0023(14) -0.0019(14) C6 0.0197(19) 0.0198(19) 0.0361(19) -0.0025(14) -0.0038(14) -0.0053(15) C7 0.029(2) 0.026(2) 0.042(2) -0.0017(16) -0.0074(16) -0.0026(17) C8 0.025(2) 0.033(2) 0.036(2) -0.0076(16) -0.0033(15) 0.0005(17) C9 0.026(2) 0.035(2) 0.038(2) 0.0003(17) -0.0055(16) -0.0037(18) C10 0.032(3) 0.050(3) 0.049(3) 0.002(2) -0.0004(18) 0.002(2) C11 0.047(3) 0.067(4) 0.033(2) 0.001(2) 0.0000(19) -0.007(3) C12 0.047(3) 0.057(3) 0.038(2) 0.005(2) -0.004(2) -0.013(3) C13 0.040(3) 0.037(3) 0.047(2) 0.0058(19) -0.0110(19) -0.004(2) C14 0.033(2) 0.037(2) 0.037(2) 0.0002(17) -0.0063(17) -0.0099(19) C15 0.031(2) 0.027(2) 0.052(2) -0.0027(18) -0.0116(18) -0.0025(18) C16 0.0188(19) 0.028(2) 0.043(2) -0.0082(16) -0.0047(15) 0.0017(16) C17 0.029(2) 0.023(2) 0.046(2) -0.0064(16) -0.0051(17) 0.0029(17) C18 0.031(2) 0.030(2) 0.038(2) -0.0030(16) -0.0059(16) -0.0026(18) C19 0.024(2) 0.023(2) 0.038(2) -0.0020(15) 0.0026(15) -0.0022(16) C20 0.036(2) 0.028(2) 0.044(2) -0.0051(17) -0.0011(17) -0.0054(19) C21 0.052(3) 0.038(3) 0.044(2) -0.0062(19) -0.003(2) -0.003(2) C22 0.082(4) 0.060(4) 0.048(3) -0.013(2) -0.009(3) -0.015(3) C23 0.078(4) 0.057(4) 0.052(3) 0.013(2) -0.018(3) -0.014(3) C24 0.072(4) 0.035(3) 0.047(3) 0.0022(19) -0.021(2) -0.006(3) C25 0.041(3) 0.035(2) 0.039(2) 0.0030(17) -0.0053(18) -0.004(2) C26 0.032(2) 0.031(2) 0.051(2) -0.0040(18) -0.0074(18) 0.0022(19) C27 0.0189(19) 0.025(2) 0.0338(19) -0.0006(14) -0.0055(14) -0.0062(15) C28 0.034(3) 0.060(4) 0.075(4) 0.006(3) 0.002(2) -0.008(3) C29 0.077(5) 0.069(4) 0.064(3) -0.007(3) 0.011(3) -0.003(4) C30 0.090(5) 0.103(6) 0.053(3) 0.003(3) 0.022(3) -0.017(4) C31 0.075(5) 0.149(8) 0.058(4) -0.005(4) 0.000(3) 0.007(5) C32 0.068(5) 0.134(8) 0.059(4) -0.018(4) 0.005(3) -0.026(5) C33 0.053(4) 0.088(5) 0.087(5) -0.015(4) -0.002(3) -0.016(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 C28 1.886(6) . ? N1 C1 1.366(5) . ? N1 C4 1.374(5) . ? N1 H1 0.858 . ? C1 C5 1.375(5) 6_577 ? C1 C2 1.441(5) . ? C2 C3 1.347(6) . ? C2 C6 1.513(6) . ? C3 C4 1.434(6) . ? C3 C17 1.482(6) . ? C4 C5 1.395(5) . ? C5 C1 1.375(5) 8_757 ? C5 H2 0.931 . ? C6 C7 1.523(5) . ? C6 C27 1.531(5) . ? C6 H3 0.979 . ? C7 C8 1.374(6) . ? C7 C16 1.421(6) . ? C8 C9 1.434(6) . ? C8 H4 0.931 . ? C9 C10 1.397(6) . ? C9 C14 1.422(6) . ? C10 C11 1.356(7) . ? C10 H5 0.928 . ? C11 C12 1.413(8) . ? C11 H6 0.931 . ? C12 C13 1.366(7) . ? C12 H7 0.929 . ? C13 C14 1.420(6) . ? C13 H8 0.930 . ? C14 C15 1.440(6) . ? C15 C16 1.357(6) . ? C15 H9 0.931 . ? C16 C17 1.534(6) . ? C17 C18 1.532(6) . ? C17 H10 0.980 . ? C18 C19 1.365(5) . ? C18 C27 1.422(6) . ? C19 C20 1.412(6) . ? C19 H11 0.929 . ? C20 C21 1.415(6) . ? C20 C25 1.437(6) . ? C21 C22 1.354(7) . ? C21 H12 0.932 . ? C22 C23 1.412(9) . ? C22 H13 0.928 . ? C23 C24 1.364(8) . ? C23 H14 0.931 . ? C24 C25 1.427(6) . ? C24 H15 0.929 . ? C25 C26 1.434(6) . ? C26 C27 1.358(6) . ? C26 H16 0.929 . ? C28 C33 1.365(9) . ? C28 C29 1.372(9) . ? C29 C30 1.402(8) . ? C29 H17 0.932 . ? C30 C31 1.400(11) . ? C30 H18 0.935 . ? C31 C32 1.396(11) . ? C31 H19 0.925 . ? C32 C33 1.346(10) . ? C32 H20 0.930 . ? C33 H21 0.933 . ? 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 C1 N1 C4 109.2(3) . . ? C1 N1 H1 125.5 . . ? C4 N1 H1 125.3 . . ? N1 C1 C5 126.4(3) . 6_577 ? N1 C1 C2 107.1(3) . . ? C5 C1 C2 126.5(4) 6_577 . ? C3 C2 C1 108.4(4) . . ? C3 C2 C6 115.3(4) . . ? C1 C2 C6 136.2(4) . . ? C2 C3 C4 107.5(4) . . ? C2 C3 C17 115.5(4) . . ? C4 C3 C17 136.8(3) . . ? N1 C4 C5 125.2(3) . . ? N1 C4 C3 107.8(3) . . ? C5 C4 C3 127.0(4) . . ? C1 C5 C4 126.8(3) 8_757 . ? C1 C5 H2 116.6 8_757 . ? C4 C5 H2 116.5 . . ? C2 C6 C7 105.2(3) . . ? C2 C6 C27 102.6(3) . . ? C7 C6 C27 105.1(3) . . ? C2 C6 H3 114.1 . . ? C7 C6 H3 114.2 . . ? C27 C6 H3 114.4 . . ? C8 C7 C16 120.7(4) . . ? C8 C7 C6 125.4(4) . . ? C16 C7 C6 113.9(4) . . ? C7 C8 C9 120.5(4) . . ? C7 C8 H4 119.8 . . ? C9 C8 H4 119.7 . . ? C10 C9 C14 118.4(4) . . ? C10 C9 C8 122.7(4) . . ? C14 C9 C8 118.8(4) . . ? C11 C10 C9 122.0(5) . . ? C11 C10 H5 119.0 . . ? C9 C10 H5 119.0 . . ? C10 C11 C12 119.7(5) . . ? C10 C11 H6 120.4 . . ? C12 C11 H6 119.9 . . ? C13 C12 C11 120.6(5) . . ? C13 C12 H7 119.5 . . ? C11 C12 H7 119.9 . . ? C12 C13 C14 119.9(5) . . ? C12 C13 H8 120.1 . . ? C14 C13 H8 120.0 . . ? C13 C14 C9 119.3(4) . . ? C13 C14 C15 122.2(4) . . ? C9 C14 C15 118.5(4) . . ? C16 C15 C14 121.4(4) . . ? C16 C15 H9 119.2 . . ? C14 C15 H9 119.4 . . ? C15 C16 C7 119.9(4) . . ? C15 C16 C17 127.3(4) . . ? C7 C16 C17 112.8(4) . . ? C3 C17 C18 103.3(3) . . ? C3 C17 C16 106.2(3) . . ? C18 C17 C16 105.1(3) . . ? C3 C17 H10 113.7 . . ? C18 C17 H10 113.8 . . ? C16 C17 H10 113.8 . . ? C19 C18 C27 120.7(4) . . ? C19 C18 C17 126.0(4) . . ? C27 C18 C17 113.1(3) . . ? C18 C19 C20 120.7(4) . . ? C18 C19 H11 119.5 . . ? C20 C19 H11 119.8 . . ? C19 C20 C21 123.9(4) . . ? C19 C20 C25 118.8(4) . . ? C21 C20 C25 116.8(4) . . ? C22 C21 C20 122.9(5) . . ? C22 C21 H12 118.5 . . ? C20 C21 H12 118.6 . . ? C21 C22 C23 119.3(5) . . ? C21 C22 H13 120.5 . . ? C23 C22 H13 120.2 . . ? C24 C23 C22 121.6(5) . . ? C24 C23 H14 119.2 . . ? C22 C23 H14 119.2 . . ? C23 C24 C25 119.2(5) . . ? C23 C24 H15 120.5 . . ? C25 C24 H15 120.2 . . ? C24 C25 C26 121.0(4) . . ? C24 C25 C20 120.0(4) . . ? C26 C25 C20 119.0(4) . . ? C27 C26 C25 120.0(4) . . ? C27 C26 H16 120.1 . . ? C25 C26 H16 119.9 . . ? C26 C27 C18 120.7(4) . . ? C26 C27 C6 125.6(4) . . ? C18 C27 C6 113.5(3) . . ? C33 C28 C29 120.6(6) . . ? C33 C28 Br1 120.6(5) . . ? C29 C28 Br1 118.8(4) . . ? C28 C29 C30 119.0(6) . . ? C28 C29 H17 120.2 . . ? C30 C29 H17 120.8 . . ? C31 C30 C29 119.5(7) . . ? C31 C30 H18 120.5 . . ? C29 C30 H18 120.1 . . ? C32 C31 C30 119.1(7) . . ? C32 C31 H19 119.9 . . ? C30 C31 H19 121.0 . . ? C33 C32 C31 119.5(7) . . ? C33 C32 H20 120.2 . . ? C31 C32 H20 120.3 . . ? C32 C33 C28 121.8(7) . . ? C32 C33 H21 119.3 . . ? C28 C33 H21 118.9 . . ? 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 C4 N1 C1 C5 178.5(4) . . . 6_577 ? C4 N1 C1 C2 -0.1(4) . . . . ? N1 C1 C2 C3 -0.2(4) . . . . ? C5 C1 C2 C3 -178.8(4) 6_577 . . . ? N1 C1 C2 C6 -175.7(4) . . . . ? C5 C1 C2 C6 5.7(7) 6_577 . . . ? C1 C2 C3 C4 0.4(4) . . . . ? C6 C2 C3 C4 176.9(3) . . . . ? C1 C2 C3 C17 -175.9(3) . . . . ? C6 C2 C3 C17 0.7(5) . . . . ? C1 N1 C4 C5 -176.6(3) . . . . ? C1 N1 C4 C3 0.3(4) . . . . ? C2 C3 C4 N1 -0.4(4) . . . . ? C17 C3 C4 N1 174.6(4) . . . . ? C2 C3 C4 C5 176.4(4) . . . . ? C17 C3 C4 C5 -8.6(7) . . . . ? N1 C4 C5 C1 -5.6(6) . . . 8_757 ? C3 C4 C5 C1 178.1(4) . . . 8_757 ? C3 C2 C6 C7 53.4(4) . . . . ? C1 C2 C6 C7 -131.3(5) . . . . ? C3 C2 C6 C27 -56.3(4) . . . . ? C1 C2 C6 C27 119.0(5) . . . . ? C2 C6 C7 C8 126.1(4) . . . . ? C27 C6 C7 C8 -126.0(4) . . . . ? C2 C6 C7 C16 -53.0(4) . . . . ? C27 C6 C7 C16 54.9(4) . . . . ? C16 C7 C8 C9 0.5(6) . . . . ? C6 C7 C8 C9 -178.5(4) . . . . ? C7 C8 C9 C10 -178.3(4) . . . . ? C7 C8 C9 C14 -2.8(6) . . . . ? C14 C9 C10 C11 1.7(7) . . . . ? C8 C9 C10 C11 177.2(4) . . . . ? C9 C10 C11 C12 -3.2(7) . . . . ? C10 C11 C12 C13 4.2(7) . . . . ? C11 C12 C13 C14 -3.6(7) . . . . ? C12 C13 C14 C9 2.1(6) . . . . ? C12 C13 C14 C15 -178.1(4) . . . . ? C10 C9 C14 C13 -1.1(6) . . . . ? C8 C9 C14 C13 -176.7(4) . . . . ? C10 C9 C14 C15 179.1(4) . . . . ? C8 C9 C14 C15 3.4(6) . . . . ? C13 C14 C15 C16 178.4(4) . . . . ? C9 C14 C15 C16 -1.8(6) . . . . ? C14 C15 C16 C7 -0.6(6) . . . . ? C14 C15 C16 C17 178.4(4) . . . . ? C8 C7 C16 C15 1.3(6) . . . . ? C6 C7 C16 C15 -179.7(3) . . . . ? C8 C7 C16 C17 -177.9(3) . . . . ? C6 C7 C16 C17 1.2(5) . . . . ? C2 C3 C17 C18 55.9(5) . . . . ? C4 C3 C17 C18 -118.9(5) . . . . ? C2 C3 C17 C16 -54.4(5) . . . . ? C4 C3 C17 C16 130.8(5) . . . . ? C15 C16 C17 C3 -126.7(4) . . . . ? C7 C16 C17 C3 52.4(4) . . . . ? C15 C16 C17 C18 124.2(4) . . . . ? C7 C16 C17 C18 -56.7(4) . . . . ? C3 C17 C18 C19 119.4(4) . . . . ? C16 C17 C18 C19 -129.4(4) . . . . ? C3 C17 C18 C27 -55.5(4) . . . . ? C16 C17 C18 C27 55.6(4) . . . . ? C27 C18 C19 C20 -0.8(6) . . . . ? C17 C18 C19 C20 -175.4(4) . . . . ? C18 C19 C20 C21 172.8(4) . . . . ? C18 C19 C20 C25 1.1(6) . . . . ? C19 C20 C21 C22 -176.5(5) . . . . ? C25 C20 C21 C22 -4.6(7) . . . . ? C20 C21 C22 C23 2.8(9) . . . . ? C21 C22 C23 C24 -1.5(10) . . . . ? C22 C23 C24 C25 2.0(9) . . . . ? C23 C24 C25 C26 175.3(5) . . . . ? C23 C24 C25 C20 -3.9(8) . . . . ? C19 C20 C25 C24 177.4(4) . . . . ? C21 C20 C25 C24 5.1(7) . . . . ? C19 C20 C25 C26 -1.9(6) . . . . ? C21 C20 C25 C26 -174.2(4) . . . . ? C24 C25 C26 C27 -176.9(5) . . . . ? C20 C25 C26 C27 2.4(7) . . . . ? C25 C26 C27 C18 -2.0(7) . . . . ? C25 C26 C27 C6 173.3(4) . . . . ? C19 C18 C27 C26 1.3(6) . . . . ? C17 C18 C27 C26 176.5(4) . . . . ? C19 C18 C27 C6 -174.6(4) . . . . ? C17 C18 C27 C6 0.6(5) . . . . ? C2 C6 C27 C26 -121.8(4) . . . . ? C7 C6 C27 C26 128.4(4) . . . . ? C2 C6 C27 C18 53.8(4) . . . . ? C7 C6 C27 C18 -56.0(4) . . . . ? C33 C28 C29 C30 1.3(11) . . . . ? Br1 C28 C29 C30 -180.0(6) . . . . ? C28 C29 C30 C31 -3.2(11) . . . . ? C29 C30 C31 C32 7.4(12) . . . . ? C30 C31 C32 C33 -9.7(13) . . . . ? C31 C32 C33 C28 8.0(12) . . . . ? C29 C28 C33 C32 -3.7(11) . . . . ? Br1 C28 C33 C32 177.5(6) . . . . ? #============================================================================== data_13-10PhClsqueezed(13) _database_code_depnum_ccdc_archive 'CCDC 248907' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C168 H110 Cl10 N4 Zn ' _chemical_formula_moiety ; C108 H60 N4 Zn, 4(C6 H5 Cl), 4(C3 H2.5 Cl0.5), 4(C3 H2.5 Cl0.5), 4(C3 H2.5 Cl0.5) ; _chemical_formula_weight 2602.47 _chemical_melting_point ? # CRYSTAL DATA _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 42/n ' _symmetry_space_group_name_Hall '-P 4bc ' _symmetry_Int_Tables_number 86 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x+1/2, z+1/2' '-x+1/2, -y+1/2, z' 'y+1/2, -x, z+1/2' '-x, -y, -z' 'y, -x-1/2, -z-1/2' 'x-1/2, y-1/2, -z' '-y-1/2, x, -z-1/2' _cell_length_a 22.4739(8) _cell_length_b 22.4739(8) _cell_length_c 12.8564(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 6493.5(4) _cell_formula_units_Z 2 _cell_measurement_reflns_used 69823 _cell_measurement_theta_min 1.3 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 123.2 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.250 _exptl_crystal_density_diffrn 1.332 _exptl_crystal_F_000 2688.0 _exptl_absorpt_coefficient_mu 0.453 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_absorpt_correction_T_min 0.750 _exptl_absorpt_correction_T_max 0.893 # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo Ka' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-IV Imaging Plate' _diffrn_measurement_method w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 22899 _diffrn_reflns_av_R_equivalents 0.027 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.883 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.883 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _reflns_number_total 6591 _reflns_number_gt 3535 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution SIR-97 _computing_structure_refinement ; SHELXL-97 (Sheldrick, 1997) and PLATON SQUEEZE ; _computing_publication_material 'CrystalStructure Ver. 3.6.0' _computing_molecular_graphics ? _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^)+(0.1000P)^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 noref _refine_ls_number_reflns 6591 _refine_ls_number_parameters 255 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0851 _refine_ls_R_factor_gt 0.0684 _refine_ls_wR_factor_ref 0.1987 _refine_ls_wR_factor_gt 0.1946 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.478 _refine_diff_density_min -0.526 _refine_diff_density_rms 0.115 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 Zn1 Zn 0.2500 0.2500 0.2500 0.0346(2) Uani 1 4 d S . . N1 N 0.28780(10) 0.16768(10) 0.25388(18) 0.0329(5) Uani 1 1 d . . . C1 C 0.34817(12) 0.15567(13) 0.2644(2) 0.0316(6) Uani 1 1 d . . . C2 C 0.35529(13) 0.09204(13) 0.2748(2) 0.0356(7) Uani 1 1 d . . . C3 C 0.30056(13) 0.06702(13) 0.2693(2) 0.0367(7) Uani 1 1 d . . . C4 C 0.25812(12) 0.11360(12) 0.2557(2) 0.0327(6) Uani 1 1 d . . . C5 C 0.19701(12) 0.10732(12) 0.2419(2) 0.0328(6) Uani 1 1 d . . . C6 C 0.29926(14) 0.00060(14) 0.2889(2) 0.0392(7) Uani 1 1 d . . . C7 C 0.32769(14) -0.00492(14) 0.3968(3) 0.0415(7) Uani 1 1 d . . . C8 C 0.30249(15) -0.03058(15) 0.4806(3) 0.0461(8) Uani 1 1 d . . . C9 C 0.33311(17) -0.02874(17) 0.5781(3) 0.0533(9) Uani 1 1 d . . . C10 C 0.30583(19) -0.0524(2) 0.6710(3) 0.0647(11) Uani 1 1 d . . . C11 C 0.3340(2) -0.0470(2) 0.7647(4) 0.0770(13) Uani 1 1 d . . . C12 C 0.3892(2) -0.0180(2) 0.7732(3) 0.0759(13) Uani 1 1 d . . . C13 C 0.41737(19) 0.0038(2) 0.6859(3) 0.0692(12) Uani 1 1 d . . . C14 C 0.38920(17) -0.00097(18) 0.5840(3) 0.0572(10) Uani 1 1 d . . . C15 C 0.41569(15) 0.02402(15) 0.4924(3) 0.0457(8) Uani 1 1 d . . . C16 C 0.38564(15) 0.02206(15) 0.4022(3) 0.0435(8) Uani 1 1 d . . . C17 C 0.40519(14) 0.04972(14) 0.2981(3) 0.0400(7) Uani 1 1 d . . . C18 C 0.40073(14) 0.00057(14) 0.2169(2) 0.0404(7) Uani 1 1 d . . . C19 C 0.44652(15) -0.01762(15) 0.1540(3) 0.0465(8) Uani 1 1 d . . . C20 C 0.43471(15) -0.06377(15) 0.0789(3) 0.0433(8) Uani 1 1 d . . . C21 C 0.48028(17) -0.08459(16) 0.0118(3) 0.0542(9) Uani 1 1 d . . . C22 C 0.46779(18) -0.12841(18) -0.0595(3) 0.0565(9) Uani 1 1 d . . . C23 C 0.41120(19) -0.15187(16) -0.0685(3) 0.0570(10) Uani 1 1 d . . . C24 C 0.36587(17) -0.13440(17) -0.0053(3) 0.0551(9) Uani 1 1 d . . . C25 C 0.37692(16) -0.08928(15) 0.0706(3) 0.0462(8) Uani 1 1 d . . . C26 C 0.33137(16) -0.06953(14) 0.1398(3) 0.0456(8) Uani 1 1 d . . . C27 C 0.34382(15) -0.02571(15) 0.2109(3) 0.0426(8) Uani 1 1 d . . . H1 H 0.1824 0.0678 0.2362 0.039 Uiso 1 1 c . . . H2 H 0.2606 -0.0163 0.2845 0.047 Uiso 1 1 c . . . H3 H 0.2649 -0.0496 0.4751 0.055 Uiso 1 1 c . . . H4 H 0.2683 -0.0717 0.6670 0.078 Uiso 1 1 c . . . H5 H 0.3160 -0.0632 0.8253 0.092 Uiso 1 1 c . . . H6 H 0.4072 -0.0134 0.8396 0.091 Uiso 1 1 c . . . H7 H 0.4553 0.0221 0.6921 0.083 Uiso 1 1 c . . . H8 H 0.4540 0.0417 0.4955 0.055 Uiso 1 1 c . . . H9 H 0.4432 0.0682 0.3008 0.048 Uiso 1 1 c . . . H10 H 0.4849 -0.0003 0.1598 0.056 Uiso 1 1 c . . . H11 H 0.5192 -0.0683 0.0161 0.065 Uiso 1 1 c . . . H12 H 0.4986 -0.1428 -0.1034 0.068 Uiso 1 1 c . . . H13 H 0.4037 -0.1811 -0.1203 0.068 Uiso 1 1 c . . . H14 H 0.3276 -0.1519 -0.0116 0.066 Uiso 1 1 c . . . H15 H 0.2927 -0.0866 0.1367 0.055 Uiso 1 1 c . . . 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 Zn1 0.0298(3) 0.0298(3) 0.0444(4) 0.000 0.000 0.000 N1 0.0300(12) 0.0318(12) 0.0369(12) 0.0015(11) -0.0004(11) -0.0014(10) C1 0.0302(15) 0.0307(15) 0.0340(15) 0.0053(11) -0.0029(11) -0.0006(12) C2 0.0294(15) 0.0321(16) 0.0453(17) 0.0053(12) -0.0061(11) 0.0010(13) C3 0.0337(16) 0.0289(15) 0.0475(18) 0.0061(12) -0.0018(12) -0.0016(13) C4 0.0302(14) 0.0307(14) 0.0371(14) 0.0030(12) -0.0022(12) -0.0030(11) C5 0.0289(14) 0.0280(14) 0.0413(15) -0.0021(12) -0.0043(12) -0.0019(11) C6 0.0311(17) 0.0275(16) 0.0591(18) 0.0064(13) -0.0057(13) 0.0002(13) C7 0.0332(17) 0.0270(16) 0.064(2) 0.0055(14) -0.0040(14) 0.0051(14) C8 0.0376(19) 0.0426(19) 0.0581(19) 0.0118(15) -0.0063(15) -0.0045(15) C9 0.042(2) 0.050(2) 0.068(2) 0.0134(17) -0.0039(16) -0.0004(17) C10 0.054(2) 0.071(3) 0.069(2) 0.017(2) -0.0066(19) 0.006(2) C11 0.058(3) 0.092(4) 0.080(3) 0.023(2) -0.007(2) 0.001(2) C12 0.058(3) 0.093(4) 0.076(3) 0.017(2) -0.016(2) -0.007(2) C13 0.052(2) 0.071(3) 0.085(3) 0.020(2) -0.018(2) -0.001(2) C14 0.046(2) 0.051(2) 0.075(2) 0.0085(18) -0.0158(18) 0.0026(18) C15 0.0342(18) 0.0413(19) 0.062(2) 0.0105(15) -0.0064(15) 0.0011(15) C16 0.0343(18) 0.0352(18) 0.061(2) 0.0087(14) -0.0067(14) 0.0025(14) C17 0.0300(17) 0.0338(17) 0.0563(18) 0.0086(14) -0.0048(13) -0.0036(14) C18 0.0331(17) 0.0339(17) 0.0543(18) 0.0103(13) -0.0047(13) 0.0001(14) C19 0.0366(19) 0.0359(19) 0.067(2) 0.0104(15) -0.0044(15) 0.0053(15) C20 0.0391(19) 0.0386(19) 0.0522(19) 0.0093(14) -0.0039(14) 0.0038(15) C21 0.051(2) 0.039(2) 0.073(2) 0.0088(17) 0.0041(18) 0.0029(17) C22 0.053(2) 0.051(2) 0.065(2) 0.0059(18) 0.0037(18) 0.0046(19) C23 0.060(3) 0.036(2) 0.075(2) 0.0048(17) 0.0013(19) 0.0081(18) C24 0.051(2) 0.043(2) 0.071(2) 0.0067(17) -0.0029(18) 0.0017(18) C25 0.046(2) 0.0320(18) 0.061(2) 0.0034(15) -0.0035(15) 0.0043(15) C26 0.0401(19) 0.0289(17) 0.068(2) 0.0053(15) -0.0052(15) 0.0013(15) C27 0.0364(18) 0.0362(18) 0.0551(18) 0.0067(14) -0.0057(14) 0.0026(14) _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 Zn1 N1 2.036(2) 8_656 ? Zn1 N1 2.036(2) 6_566 ? Zn1 N1 2.036(2) 3 ? Zn1 N1 2.036(2) . ? N1 C4 1.387(3) . ? N1 C1 1.390(3) . ? C1 C5 1.368(4) 8_656 ? C1 C2 1.445(4) . ? C2 C3 1.354(4) . ? C2 C17 1.501(4) . ? C3 C4 1.427(4) . ? C3 C6 1.514(4) . ? C4 C5 1.392(4) . ? C5 C1 1.368(4) 6_566 ? C5 H1 0.950 . ? C6 C7 1.533(4) . ? C6 C27 1.536(5) . ? C6 H2 0.950 . ? C7 C8 1.347(4) . ? C7 C16 1.438(5) . ? C8 C9 1.431(5) . ? C8 H3 0.950 . ? C9 C14 1.409(5) . ? C9 C10 1.445(5) . ? C10 C11 1.367(6) . ? C10 H4 0.949 . ? C11 C12 1.406(6) . ? C11 H5 0.949 . ? C12 C13 1.380(6) . ? C12 H6 0.950 . ? C13 C14 1.459(5) . ? C13 H7 0.950 . ? C14 C15 1.434(5) . ? C15 C16 1.342(5) . ? C15 H8 0.950 . ? C16 C17 1.540(5) . ? C17 C18 1.523(5) . ? C17 H9 0.950 . ? C18 C19 1.371(5) . ? C18 C27 1.411(4) . ? C19 C20 1.442(5) . ? C19 H10 0.950 . ? C20 C21 1.418(5) . ? C20 C25 1.424(5) . ? C21 C22 1.374(5) . ? C21 H11 0.950 . ? C22 C23 1.382(6) . ? C22 H12 0.950 . ? C23 C24 1.361(5) . ? C23 H13 0.951 . ? C24 C25 1.429(5) . ? C24 H14 0.950 . ? C25 C26 1.427(5) . ? C26 C27 1.372(5) . ? C26 H15 0.950 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Zn1 N1 177.20(13) 8_656 6_566 ? N1 Zn1 N1 90.034(3) 8_656 3 ? N1 Zn1 N1 90.034(3) 6_566 3 ? N1 Zn1 N1 90.034(3) 8_656 . ? N1 Zn1 N1 90.034(3) 6_566 . ? N1 Zn1 N1 177.20(13) 3 . ? C4 N1 C1 107.3(2) . . ? C4 N1 Zn1 126.59(19) . . ? C1 N1 Zn1 125.88(19) . . ? C5 C1 N1 125.2(3) 8_656 . ? C5 C1 C2 126.6(3) 8_656 . ? N1 C1 C2 108.0(2) . . ? C3 C2 C1 107.8(3) . . ? C3 C2 C17 115.2(3) . . ? C1 C2 C17 136.7(3) . . ? C2 C3 C4 108.0(3) . . ? C2 C3 C6 114.7(3) . . ? C4 C3 C6 137.0(3) . . ? N1 C4 C5 124.1(3) . . ? N1 C4 C3 108.9(2) . . ? C5 C4 C3 126.9(3) . . ? C1 C5 C4 127.1(3) 6_566 . ? C1 C5 H1 116.4 6_566 . ? C4 C5 H1 116.5 . . ? C3 C6 C7 102.8(2) . . ? C3 C6 C27 105.0(2) . . ? C7 C6 C27 106.8(3) . . ? C3 C6 H2 113.8 . . ? C7 C6 H2 113.7 . . ? C27 C6 H2 113.7 . . ? C8 C7 C16 121.5(3) . . ? C8 C7 C6 125.7(3) . . ? C16 C7 C6 112.8(3) . . ? C7 C8 C9 119.1(3) . . ? C7 C8 H3 120.5 . . ? C9 C8 H3 120.4 . . ? C14 C9 C8 119.4(3) . . ? C14 C9 C10 119.9(3) . . ? C8 C9 C10 120.7(3) . . ? C11 C10 C9 120.0(4) . . ? C11 C10 H4 120.0 . . ? C9 C10 H4 120.0 . . ? C10 C11 C12 121.2(4) . . ? C10 C11 H5 119.4 . . ? C12 C11 H5 119.4 . . ? C13 C12 C11 120.4(4) . . ? C13 C12 H6 119.8 . . ? C11 C12 H6 119.8 . . ? C12 C13 C14 120.4(4) . . ? C12 C13 H7 119.8 . . ? C14 C13 H7 119.8 . . ? C9 C14 C15 120.1(3) . . ? C9 C14 C13 118.0(4) . . ? C15 C14 C13 121.9(4) . . ? C16 C15 C14 119.2(3) . . ? C16 C15 H8 120.4 . . ? C14 C15 H8 120.4 . . ? C15 C16 C7 120.8(3) . . ? C15 C16 C17 126.4(3) . . ? C7 C16 C17 112.7(3) . . ? C2 C17 C18 105.9(2) . . ? C2 C17 C16 102.5(3) . . ? C18 C17 C16 106.5(3) . . ? C2 C17 H9 113.7 . . ? C18 C17 H9 113.6 . . ? C16 C17 H9 113.7 . . ? C19 C18 C27 121.5(3) . . ? C19 C18 C17 124.8(3) . . ? C27 C18 C17 113.7(3) . . ? C18 C19 C20 118.1(3) . . ? C18 C19 H10 120.9 . . ? C20 C19 H10 121.0 . . ? C21 C20 C25 118.7(3) . . ? C21 C20 C19 120.8(3) . . ? C25 C20 C19 120.5(3) . . ? C22 C21 C20 119.6(4) . . ? C22 C21 H11 120.2 . . ? C20 C21 H11 120.1 . . ? C21 C22 C23 121.1(4) . . ? C21 C22 H12 119.5 . . ? C23 C22 H12 119.4 . . ? C24 C23 C22 122.0(4) . . ? C24 C23 H13 119.0 . . ? C22 C23 H13 119.0 . . ? C23 C24 C25 118.8(4) . . ? C23 C24 H14 120.6 . . ? C25 C24 H14 120.6 . . ? C20 C25 C26 118.9(3) . . ? C20 C25 C24 119.7(3) . . ? C26 C25 C24 121.5(3) . . ? C27 C26 C25 119.5(3) . . ? C27 C26 H15 120.3 . . ? C25 C26 H15 120.3 . . ? C26 C27 C18 121.5(3) . . ? C26 C27 C6 125.3(3) . . ? C18 C27 C6 113.2(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Zn1 N1 C4 -178.8(3) 8_656 . . . ? N1 Zn1 N1 C4 -1.59(17) 6_566 . . . ? N1 Zn1 N1 C1 7.26(16) 8_656 . . . ? N1 Zn1 N1 C1 -175.5(3) 6_566 . . . ? C4 N1 C1 C5 174.6(3) . . . 8_656 ? Zn1 N1 C1 C5 -10.4(4) . . . 8_656 ? C4 N1 C1 C2 -1.0(3) . . . . ? Zn1 N1 C1 C2 173.90(18) . . . . ? C5 C1 C2 C3 -174.9(3) 8_656 . . . ? N1 C1 C2 C3 0.7(3) . . . . ? C5 C1 C2 C17 11.5(5) 8_656 . . . ? N1 C1 C2 C17 -173.0(3) . . . . ? C1 C2 C3 C4 -0.1(3) . . . . ? C17 C2 C3 C4 175.1(3) . . . . ? C1 C2 C3 C6 -174.6(2) . . . . ? C17 C2 C3 C6 0.6(4) . . . . ? C1 N1 C4 C5 -176.6(3) . . . . ? Zn1 N1 C4 C5 8.5(4) . . . . ? C1 N1 C4 C3 0.9(3) . . . . ? Zn1 N1 C4 C3 -173.93(19) . . . . ? C2 C3 C4 N1 -0.5(3) . . . . ? C6 C3 C4 N1 172.1(3) . . . . ? C2 C3 C4 C5 177.0(3) . . . . ? C6 C3 C4 C5 -10.4(6) . . . . ? N1 C4 C5 C1 -7.5(5) . . . 6_566 ? C3 C4 C5 C1 175.4(3) . . . 6_566 ? C2 C3 C6 C7 56.8(3) . . . . ? C4 C3 C6 C7 -115.5(4) . . . . ? C2 C3 C6 C27 -54.7(3) . . . . ? C4 C3 C6 C27 133.0(4) . . . . ? C3 C6 C7 C8 123.2(4) . . . . ? C27 C6 C7 C8 -126.6(3) . . . . ? C3 C6 C7 C16 -55.4(3) . . . . ? C27 C6 C7 C16 54.9(3) . . . . ? C16 C7 C8 C9 2.6(5) . . . . ? C6 C7 C8 C9 -175.8(3) . . . . ? C7 C8 C9 C14 -0.9(6) . . . . ? C7 C8 C9 C10 176.1(4) . . . . ? C14 C9 C10 C11 1.0(6) . . . . ? C8 C9 C10 C11 -175.9(4) . . . . ? C9 C10 C11 C12 0.8(7) . . . . ? C10 C11 C12 C13 -2.5(8) . . . . ? C11 C12 C13 C14 2.3(7) . . . . ? C8 C9 C14 C15 -1.3(6) . . . . ? C10 C9 C14 C15 -178.3(4) . . . . ? C8 C9 C14 C13 175.8(4) . . . . ? C10 C9 C14 C13 -1.2(6) . . . . ? C12 C13 C14 C9 -0.4(6) . . . . ? C12 C13 C14 C15 176.6(4) . . . . ? C9 C14 C15 C16 1.9(6) . . . . ? C13 C14 C15 C16 -175.1(4) . . . . ? C14 C15 C16 C7 -0.3(5) . . . . ? C14 C15 C16 C17 176.1(3) . . . . ? C8 C7 C16 C15 -2.0(5) . . . . ? C6 C7 C16 C15 176.6(3) . . . . ? C8 C7 C16 C17 -178.9(3) . . . . ? C6 C7 C16 C17 -0.3(4) . . . . ? C3 C2 C17 C18 53.9(3) . . . . ? C1 C2 C17 C18 -132.8(3) . . . . ? C3 C2 C17 C16 -57.6(3) . . . . ? C1 C2 C17 C16 115.8(4) . . . . ? C15 C16 C17 C2 -120.5(4) . . . . ? C7 C16 C17 C2 56.1(3) . . . . ? C15 C16 C17 C18 128.5(4) . . . . ? C7 C16 C17 C18 -54.9(3) . . . . ? C2 C17 C18 C19 127.1(3) . . . . ? C16 C17 C18 C19 -124.3(3) . . . . ? C2 C17 C18 C27 -52.8(3) . . . . ? C16 C17 C18 C27 55.8(3) . . . . ? C27 C18 C19 C20 1.5(5) . . . . ? C17 C18 C19 C20 -178.3(3) . . . . ? C18 C19 C20 C21 -179.8(3) . . . . ? C18 C19 C20 C25 0.2(5) . . . . ? C25 C20 C21 C22 0.3(5) . . . . ? C19 C20 C21 C22 -179.7(3) . . . . ? C20 C21 C22 C23 1.2(6) . . . . ? C21 C22 C23 C24 -2.3(6) . . . . ? C22 C23 C24 C25 1.7(6) . . . . ? C21 C20 C25 C26 178.4(3) . . . . ? C19 C20 C25 C26 -1.7(5) . . . . ? C21 C20 C25 C24 -0.8(5) . . . . ? C19 C20 C25 C24 179.1(3) . . . . ? C23 C24 C25 C20 -0.2(5) . . . . ? C23 C24 C25 C26 -179.3(3) . . . . ? C20 C25 C26 C27 1.4(5) . . . . ? C24 C25 C26 C27 -179.4(3) . . . . ? C25 C26 C27 C18 0.2(5) . . . . ? C25 C26 C27 C6 179.0(3) . . . . ? C19 C18 C27 C26 -1.8(5) . . . . ? C17 C18 C27 C26 178.1(3) . . . . ? C19 C18 C27 C6 179.3(3) . . . . ? C17 C18 C27 C6 -0.9(4) . . . . ? C3 C6 C27 C26 -125.0(3) . . . . ? C7 C6 C27 C26 126.3(3) . . . . ? C3 C6 C27 C18 53.9(3) . . . . ? C7 C6 C27 C18 -54.8(3) . . . . ? #============================================================================== data_12-12PhH _database_code_depnum_ccdc_archive 'CCDC 248908' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C180 H134 N4 ' _chemical_formula_moiety 'C108 H62 N4, 12(C6 H6)' _chemical_formula_weight 2352.91 _chemical_melting_point ? # CRYSTAL DATA _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 41/a ' _symmetry_space_group_name_Hall '-I 4ad ' _symmetry_Int_Tables_number 88 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2-y,z 3/4-y,1/4+x,1/4+z 1/4+y,1/4-x,1/4+z -x,-y,-z x,1/2+y,-z 3/4+y,1/4-x,1/4-z 1/4-y,1/4+x,1/4-z 1/2+x,1/2+y,1/2+z 1/2-x,-y,1/2+z 1/4-y,3/4+x,3/4+z 3/4+y,3/4-x,3/4+z 1/2-x,1/2-y,1/2-z 1/2+x,y,1/2-z 1/4+y,3/4-x,3/4-z 3/4-y,3/4+x,3/4-z _cell_length_a 19.390(1) _cell_length_b 19.390(1) _cell_length_c 36.077(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 13564(1) _cell_formula_units_Z 4 _cell_measurement_reflns_used 12512 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 173.2 _exptl_crystal_description Prism _exptl_crystal_colour Red _exptl_crystal_size_max 0.600 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.152 _exptl_crystal_F_000 4968 _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.066 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details Coppens_numerical _exptl_absorpt_correction_T_max 0.9886 _exptl_absorpt_correction_T_min 0.9805 # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo Ka' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method w _diffrn_detector_area_resol_mean 14.62 _diffrn_reflns_number 55742 _diffrn_reflns_av_R_equivalents 0.062 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9938 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.9938 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 37 # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 7742 _reflns_number_gt 4343 _reflns_threshold_expression F^2^>2.0s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0650 _refine_ls_wR_factor_ref 0.1587 _refine_ls_hydrogen_treatment mixed _refine_ls_number_reflns 7742 _refine_ls_number_parameters 419 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[s^2^(Fo^2^) + (0.05000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0002 _refine_diff_density_max 0.45 _refine_diff_density_min -0.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.47093(8) -0.14736(8) 0.12389(5) 0.0287(4) Uani 1.00 d . . . C1 C 0.51523(9) -0.09201(9) 0.12279(5) 0.0275(5) Uani 1.00 d . . . C2 C 0.47429(9) -0.03031(9) 0.12202(5) 0.0286(5) Uani 1.00 d . . . C3 C 0.40707(9) -0.04889(9) 0.12307(5) 0.0289(5) Uani 1.00 d . . . C4 C 0.40447(9) -0.12285(9) 0.12454(5) 0.0274(5) Uani 1.00 d . . . C5 C 0.34549(9) -0.16340(9) 0.12639(5) 0.0286(5) Uani 1.00 d . . . C6 C 0.48754(9) 0.04665(9) 0.12286(6) 0.0309(5) Uani 1.00 d . . . C7 C 0.45033(10) 0.07096(9) 0.15769(6) 0.0311(5) Uani 1.00 d . . . C8 C 0.4784(1) 0.10675(10) 0.18639(6) 0.0356(6) Uani 1.00 d . . . C9 C 0.4372(1) 0.1258(1) 0.21741(6) 0.0388(6) Uani 1.00 d . . . C10 C 0.4639(1) 0.1632(1) 0.24775(7) 0.0502(7) Uani 1.00 d . . . C11 C 0.4231(1) 0.1825(1) 0.27665(7) 0.0606(9) Uani 1.00 d . . . C12 C 0.3529(1) 0.1647(1) 0.27688(7) 0.0585(8) Uani 1.00 d . . . C13 C 0.3255(1) 0.1284(1) 0.24838(7) 0.0487(7) Uani 1.00 d . . . C14 C 0.3661(1) 0.1082(1) 0.21757(6) 0.0385(6) Uani 1.00 d . . . C15 C 0.33843(10) 0.07067(10) 0.18746(6) 0.0352(6) Uani 1.00 d . . . C16 C 0.37918(10) 0.05195(9) 0.15863(6) 0.0307(5) Uani 1.00 d . . . C17 C 0.35681(9) 0.01068(9) 0.12457(6) 0.0312(5) Uani 1.00 d . . . C18 C 0.37462(10) 0.05691(9) 0.09170(6) 0.0318(6) Uani 1.00 d . . . C19 C 0.3301(1) 0.0808(1) 0.06554(6) 0.0387(6) Uani 1.00 d . . . C20 C 0.3542(1) 0.1223(1) 0.03591(6) 0.0432(7) Uani 1.00 d . . . C21 C 0.3102(1) 0.1466(1) 0.00746(7) 0.0603(8) Uani 1.00 d . . . C22 C 0.3356(2) 0.1819(1) -0.02198(8) 0.074(1) Uani 1.00 d . . . C23 C 0.4059(2) 0.1962(1) -0.02469(8) 0.0724(10) Uani 1.00 d . . . C24 C 0.4501(1) 0.1747(1) 0.00242(7) 0.0587(8) Uani 1.00 d . . . C25 C 0.4256(1) 0.1380(1) 0.03343(6) 0.0430(7) Uani 1.00 d . . . C26 C 0.4706(1) 0.11440(10) 0.06205(6) 0.0368(6) Uani 1.00 d . . . C27 C 0.44592(10) 0.07548(9) 0.09038(6) 0.0312(5) Uani 1.00 d . . . C28 C 0.8950(2) 0.0896(2) 0.13411(9) 0.088(1) Uani 1.00 d . . . C29 C 0.9226(2) 0.0400(1) 0.1120(1) 0.075(1) Uani 1.00 d . . . C30 C 0.9288(1) 0.0505(2) 0.0752(1) 0.075(1) Uani 1.00 d . . . C31 C 0.9064(2) 0.1105(2) 0.05942(9) 0.085(1) Uani 1.00 d . . . C32 C 0.8783(2) 0.1615(2) 0.0815(1) 0.092(1) Uani 1.00 d . . . C33 C 0.8734(2) 0.1510(2) 0.1187(1) 0.095(1) Uani 1.00 d . . . C34 C 0.7220(2) -0.0807(3) 0.2802(1) 0.110(2) Uani 1.00 d . . . C35 C 0.7250(3) -0.1376(3) 0.2601(2) 0.160(3) Uani 1.00 d . . . C36 C 0.6792(5) -0.1485(5) 0.2332(3) 0.229(5) Uani 1.00 d . . . C37 C 0.6303(4) -0.0957(7) 0.2244(2) 0.230(5) Uani 1.00 d . . . C38 C 0.6308(3) -0.0385(4) 0.2459(2) 0.171(3) Uani 1.00 d . . . C39 C 0.6765(2) -0.0316(3) 0.2738(1) 0.124(2) Uani 1.00 d . . . C40 C 0.0158(3) -0.1289(3) 0.0949(2) 0.134(2) Uani 1.00 d . . . C41 C 0.0560(5) -0.1019(4) 0.0696(2) 0.170(3) Uani 1.00 d . . . C42 C 0.1185(6) -0.0678(4) 0.0763(4) 0.270(6) Uani 1.00 d . . . C43 C 0.1261(3) -0.0660(2) 0.1161(3) 0.173(3) Uani 1.00 d . . . C44 C 0.0837(4) -0.0931(3) 0.1415(2) 0.155(2) Uani 1.00 d . . . C45 C 0.0287(3) -0.1266(3) 0.1306(2) 0.144(2) Uani 1.00 d . . . H1N H 0.481(2) -0.189(2) 0.1243(10) 0.024(9) Uiso 0.50 d P . . H5 H 0.3013 -0.1423 0.1268 0.0344 Uiso 1.00 calc . . . H6 H 0.5350 0.0586 0.1222 0.0370 Uiso 1.00 calc . . . H8 H 0.5258 0.1191 0.1857 0.0427 Uiso 1.00 calc . . . H10 H 0.5114 0.1752 0.2480 0.0603 Uiso 1.00 calc . . . H11 H 0.4421 0.2081 0.2967 0.0727 Uiso 1.00 calc . . . H12 H 0.3245 0.1782 0.2971 0.0702 Uiso 1.00 calc . . . H13 H 0.2780 0.1162 0.2491 0.0584 Uiso 1.00 calc . . . H15 H 0.2910 0.0585 0.1874 0.0423 Uiso 1.00 calc . . . H17 H 0.3098 -0.0032 0.1252 0.0374 Uiso 1.00 calc . . . H19 H 0.2825 0.0696 0.0671 0.0465 Uiso 1.00 calc . . . H21 H 0.2620 0.1380 0.0090 0.0724 Uiso 1.00 calc . . . H22 H 0.3052 0.1972 -0.0409 0.0889 Uiso 1.00 calc . . . H23 H 0.4231 0.2209 -0.0455 0.0868 Uiso 1.00 calc . . . H24 H 0.4979 0.1847 0.0003 0.0704 Uiso 1.00 calc . . . H26 H 0.5182 0.1260 0.0613 0.0442 Uiso 1.00 calc . . . H28 H 0.8905 0.0820 0.1600 0.1058 Uiso 1.00 calc . . . H29 H 0.9376 -0.0023 0.1226 0.0903 Uiso 1.00 calc . . . H30 H 0.9491 0.0159 0.0601 0.0905 Uiso 1.00 calc . . . H31 H 0.9100 0.1171 0.0334 0.1023 Uiso 1.00 calc . . . H32 H 0.8627 0.2035 0.0709 0.1109 Uiso 1.00 calc . . . H33 H 0.8549 0.1862 0.1342 0.1141 Uiso 1.00 calc . . . H34 H 0.7537 -0.0750 0.3000 0.1315 Uiso 1.00 calc . . . H35 H 0.7599 -0.1709 0.2648 0.1920 Uiso 1.00 calc . . . H36 H 0.6789 -0.1909 0.2200 0.2753 Uiso 1.00 calc . . . H37 H 0.5989 -0.1006 0.2043 0.2755 Uiso 1.00 calc . . . H38 H 0.5984 -0.0027 0.2413 0.2058 Uiso 1.00 calc . . . H39 H 0.6759 0.0086 0.2888 0.1489 Uiso 1.00 calc . . . H40 H -0.0251 -0.1514 0.0869 0.1602 Uiso 1.00 calc . . . H41 H 0.0415 -0.1056 0.0445 0.2035 Uiso 1.00 calc . . . H42 H 0.1494 -0.0497 0.0584 0.3235 Uiso 1.00 calc . . . H43 H 0.1657 -0.0428 0.1253 0.2074 Uiso 1.00 calc . . . H44 H 0.0935 -0.0882 0.1672 0.1855 Uiso 1.00 calc . . . H45 H -0.0009 -0.1485 0.1480 0.1728 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 N1 0.0237(8) 0.0233(9) 0.0391(10) -0.0006(7) 0.0010(7) -0.0001(8) C1 0.0269(10) 0.0237(9) 0.032(1) 0.0006(8) 0.0008(8) 0.0001(8) C2 0.0256(10) 0.0231(9) 0.037(1) 0.0003(8) -0.0009(8) 0.0001(8) C3 0.0260(10) 0.0216(9) 0.039(1) 0.0011(8) 0.0001(9) -0.0013(8) C4 0.0259(10) 0.0229(9) 0.033(1) 0.0021(8) -0.0001(9) 0.0004(8) C5 0.0246(10) 0.0257(10) 0.036(1) 0.0027(8) 0.0000(8) 0.0001(8) C6 0.0227(9) 0.0229(9) 0.047(1) -0.0004(8) -0.0030(9) 0.0014(9) C7 0.028(1) 0.0195(9) 0.046(1) 0.0027(8) -0.0043(9) 0.0015(8) C8 0.030(1) 0.028(1) 0.048(1) -0.0019(9) -0.0056(10) 0.0012(9) C9 0.040(1) 0.030(1) 0.046(1) 0.0021(9) -0.006(1) -0.0014(10) C10 0.050(1) 0.047(1) 0.054(2) -0.003(1) -0.010(1) -0.007(1) C11 0.069(2) 0.063(2) 0.049(2) 0.002(1) -0.008(1) -0.017(1) C12 0.062(2) 0.060(2) 0.053(2) 0.010(1) 0.003(1) -0.013(1) C13 0.048(1) 0.046(1) 0.052(1) 0.004(1) 0.004(1) -0.005(1) C14 0.041(1) 0.028(1) 0.046(1) 0.0053(9) -0.001(1) -0.0001(9) C15 0.026(1) 0.027(1) 0.052(1) 0.0023(9) -0.0003(9) -0.0007(9) C16 0.028(1) 0.0200(9) 0.044(1) 0.0029(8) -0.0027(9) 0.0014(9) C17 0.0216(9) 0.0222(9) 0.050(1) 0.0003(8) -0.0020(9) -0.0009(9) C18 0.031(1) 0.0188(9) 0.046(1) 0.0013(8) -0.0037(9) -0.0029(9) C19 0.034(1) 0.030(1) 0.052(1) 0.0003(9) -0.0097(10) -0.0031(10) C20 0.048(1) 0.030(1) 0.051(1) -0.001(1) -0.015(1) -0.001(1) C21 0.066(2) 0.052(2) 0.063(2) -0.007(1) -0.029(1) 0.012(1) C22 0.093(2) 0.063(2) 0.066(2) -0.014(2) -0.040(2) 0.019(1) C23 0.098(2) 0.064(2) 0.055(2) -0.022(2) -0.021(2) 0.019(1) C24 0.071(2) 0.048(1) 0.056(2) -0.012(1) -0.007(1) 0.013(1) C25 0.053(1) 0.030(1) 0.046(1) -0.006(1) -0.007(1) 0.0024(10) C26 0.035(1) 0.027(1) 0.049(1) -0.0041(9) -0.0016(10) 0.0037(9) C27 0.029(1) 0.0199(10) 0.044(1) 0.0012(8) -0.0028(9) -0.0022(8) C28 0.114(3) 0.064(2) 0.087(2) -0.003(2) 0.014(2) -0.003(2) C29 0.072(2) 0.052(2) 0.102(3) -0.007(1) -0.001(2) -0.010(2) C30 0.060(2) 0.063(2) 0.103(3) -0.018(2) 0.018(2) -0.024(2) C31 0.089(2) 0.089(3) 0.077(2) -0.020(2) 0.020(2) -0.003(2) C32 0.106(3) 0.070(2) 0.101(3) 0.008(2) 0.028(2) 0.016(2) C33 0.128(3) 0.069(2) 0.089(3) 0.020(2) 0.041(2) 0.004(2) C34 0.088(3) 0.113(3) 0.127(3) -0.020(3) 0.012(2) -0.014(3) C35 0.151(5) 0.097(4) 0.233(7) -0.039(3) 0.131(5) -0.021(4) C36 0.27(1) 0.247(9) 0.175(9) -0.198(9) 0.155(9) -0.125(7) C37 0.183(7) 0.44(2) 0.062(3) -0.188(9) 0.017(4) -0.030(7) C38 0.114(4) 0.268(8) 0.132(5) -0.035(5) -0.026(4) 0.041(5) C39 0.094(3) 0.128(4) 0.151(4) -0.013(3) -0.016(3) -0.019(3) C40 0.094(3) 0.116(4) 0.191(6) 0.038(3) -0.073(4) -0.063(4) C41 0.238(9) 0.108(5) 0.163(5) 0.115(5) 0.036(6) 0.018(4) C42 0.29(1) 0.099(5) 0.42(2) 0.076(6) 0.14(1) 0.145(8) C43 0.098(4) 0.057(3) 0.36(1) -0.035(2) -0.016(6) 0.035(5) C44 0.148(5) 0.087(4) 0.229(6) 0.031(3) -0.098(5) -0.024(4) C45 0.106(4) 0.108(4) 0.219(7) 0.042(3) -0.009(4) -0.011(4) _computing_data_collection CRYSTALCLEAR _computing_cell_refinement CRYSTALCLEAR _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SAPI91 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C1 1.375(2) . . yes N1 C4 1.374(2) . . yes N1 H1N 0.84(4) . . no C1 C2 1.436(2) . . yes C1 C5 1.386(3) . 7_555 yes C2 C3 1.353(3) . . yes C2 C6 1.515(3) . . yes C3 C4 1.436(3) . . yes C3 C17 1.512(2) . . yes C4 C5 1.389(3) . . yes C5 H5 0.950 . . no C6 C7 1.524(3) . . yes C6 C27 1.528(3) . . yes C6 H6 0.950 . . no C7 C8 1.360(3) . . yes C7 C16 1.428(3) . . yes C8 C9 1.424(3) . . yes C8 H8 0.950 . . no C9 C10 1.411(3) . . yes C9 C14 1.421(3) . . yes C10 C11 1.361(3) . . yes C10 H10 0.950 . . no C11 C12 1.405(4) . . yes C11 H11 0.950 . . no C12 C13 1.355(3) . . yes C12 H12 0.950 . . no C13 C14 1.417(3) . . yes C13 H13 0.950 . . no C14 C15 1.413(3) . . yes C15 C16 1.356(3) . . yes C15 H15 0.950 . . no C16 C17 1.529(3) . . yes C17 C18 1.526(3) . . yes C17 H17 0.950 . . no C18 C19 1.360(3) . . yes C18 C27 1.429(3) . . yes C19 C20 1.417(3) . . yes C19 H19 0.950 . . no C20 C21 1.416(3) . . yes C20 C25 1.420(3) . . yes C21 C22 1.357(4) . . yes C21 H21 0.950 . . no C22 C23 1.394(4) . . yes C22 H22 0.950 . . no C23 C24 1.365(4) . . yes C23 H23 0.950 . . no C24 C25 1.408(3) . . yes C24 H24 0.950 . . no C25 C26 1.427(3) . . yes C26 C27 1.358(3) . . yes C26 H26 0.950 . . no C28 C29 1.359(4) . . yes C28 C33 1.379(4) . . yes C28 H28 0.950 . . no C29 C30 1.351(4) . . yes C29 H29 0.950 . . no C30 C31 1.365(4) . . yes C30 H30 0.950 . . no C31 C32 1.383(4) . . yes C31 H31 0.950 . . no C32 C33 1.361(4) . . yes C32 H32 0.950 . . no C33 H33 0.950 . . no C34 C35 1.321(6) . . yes C34 C39 1.319(5) . . yes C34 H34 0.950 . . no C35 C36 1.33(1) . . yes C35 H35 0.950 . . no C36 C37 1.43(1) . . yes C36 H36 0.950 . . no C37 C38 1.35(1) . . yes C37 H37 0.950 . . no C38 C39 1.346(6) . . yes C38 H38 0.950 . . no C39 H39 0.950 . . no C40 C41 1.309(8) . . yes C40 C45 1.314(7) . . yes C40 H40 0.950 . . no C41 C42 1.40(1) . . yes C41 H41 0.950 . . no C42 C43 1.44(1) . . yes C42 H42 0.950 . . no C43 C44 1.341(9) . . yes C43 H43 0.950 . . no C44 C45 1.309(7) . . yes C44 H44 0.950 . . no C45 H45 0.950 . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 N1 C4 108.4(2) . . . yes C1 N1 H1N 128(2) . . . no C4 N1 H1N 123(2) . . . no N1 C1 C2 107.8(2) . . . yes N1 C1 C5 125.8(2) . . 7_555 yes C2 C1 C5 126.4(2) . . 7_555 yes C1 C2 C3 108.1(2) . . . yes C1 C2 C6 136.6(2) . . . yes C3 C2 C6 115.2(2) . . . yes C2 C3 C4 107.5(2) . . . yes C2 C3 C17 114.7(2) . . . yes C4 C3 C17 137.6(2) . . . yes N1 C4 C3 108.2(2) . . . yes N1 C4 C5 125.3(2) . . . yes C3 C4 C5 126.6(2) . . . yes C1 C5 C4 127.3(2) 8_545 . . yes C1 C5 H5 112.7 8_545 . . no C4 C5 H5 120.0 . . . no C2 C6 C7 103.9(2) . . . yes C2 C6 C27 104.8(1) . . . yes C2 C6 H6 113.8 . . . no C7 C6 C27 105.6(1) . . . yes C7 C6 H6 113.8 . . . no C27 C6 H6 113.8 . . . no C6 C7 C8 126.6(2) . . . yes C6 C7 C16 113.4(2) . . . yes C8 C7 C16 120.0(2) . . . yes C7 C8 C9 120.4(2) . . . yes C7 C8 H8 119.8 . . . no C9 C8 H8 119.8 . . . no C8 C9 C10 122.5(2) . . . yes C8 C9 C14 119.0(2) . . . yes C10 C9 C14 118.4(2) . . . yes C9 C10 C11 121.5(2) . . . yes C9 C10 H10 119.3 . . . no C11 C10 H10 119.3 . . . no C10 C11 C12 120.0(2) . . . yes C10 C11 H11 120.0 . . . no C12 C11 H11 120.0 . . . no C11 C12 C13 120.2(2) . . . yes C11 C12 H12 119.9 . . . no C13 C12 H12 119.9 . . . no C12 C13 C14 121.4(2) . . . yes C12 C13 H13 119.3 . . . no C14 C13 H13 119.3 . . . no C9 C14 C13 118.4(2) . . . yes C9 C14 C15 119.3(2) . . . yes C13 C14 C15 122.3(2) . . . yes C14 C15 C16 120.4(2) . . . yes C14 C15 H15 119.8 . . . no C16 C15 H15 119.8 . . . no C7 C16 C15 120.8(2) . . . yes C7 C16 C17 113.0(2) . . . yes C15 C16 C17 126.2(2) . . . yes C3 C17 C16 104.2(1) . . . yes C3 C17 C18 106.0(2) . . . yes C3 C17 H17 113.7 . . . no C16 C17 C18 104.6(1) . . . yes C16 C17 H17 113.7 . . . no C18 C17 H17 113.7 . . . no C17 C18 C19 126.5(2) . . . yes C17 C18 C27 113.1(2) . . . yes C19 C18 C27 120.3(2) . . . yes C18 C19 C20 120.5(2) . . . yes C18 C19 H19 119.8 . . . no C20 C19 H19 119.8 . . . no C19 C20 C21 122.4(2) . . . yes C19 C20 C25 119.4(2) . . . yes C21 C20 C25 118.1(2) . . . yes C20 C21 C22 121.1(2) . . . yes C20 C21 H21 119.5 . . . no C22 C21 H21 119.5 . . . no C21 C22 C23 120.7(2) . . . yes C21 C22 H22 119.7 . . . no C23 C22 H22 119.7 . . . no C22 C23 C24 120.2(2) . . . yes C22 C23 H23 119.9 . . . no C24 C23 H23 119.9 . . . no C23 C24 C25 120.7(2) . . . yes C23 C24 H24 119.6 . . . no C25 C24 H24 119.6 . . . no C20 C25 C24 119.2(2) . . . yes C20 C25 C26 118.7(2) . . . yes C24 C25 C26 122.1(2) . . . yes C25 C26 C27 120.5(2) . . . yes C25 C26 H26 119.7 . . . no C27 C26 H26 119.7 . . . no C6 C27 C18 113.1(2) . . . yes C6 C27 C26 126.5(2) . . . yes C18 C27 C26 120.4(2) . . . yes C29 C28 C33 119.7(3) . . . yes C29 C28 H28 120.1 . . . no C33 C28 H28 120.1 . . . no C28 C29 C30 120.3(3) . . . yes C28 C29 H29 119.8 . . . no C30 C29 H29 119.8 . . . no C29 C30 C31 120.7(3) . . . yes C29 C30 H30 119.7 . . . no C31 C30 H30 119.7 . . . no C30 C31 C32 119.6(3) . . . yes C30 C31 H31 120.2 . . . no C32 C31 H31 120.2 . . . no C31 C32 C33 119.3(3) . . . yes C31 C32 H32 120.3 . . . no C33 C32 H32 120.3 . . . no C28 C33 C32 120.3(3) . . . yes C28 C33 H33 119.9 . . . no C32 C33 H33 119.9 . . . no C35 C34 C39 122.5(5) . . . yes C35 C34 H34 118.8 . . . no C39 C34 H34 118.8 . . . no C34 C35 C36 120.1(7) . . . yes C34 C35 H35 120.0 . . . no C36 C35 H35 120.0 . . . no C35 C36 C37 119.5(9) . . . yes C35 C36 H36 120.2 . . . no C37 C36 H36 120.3 . . . no C36 C37 C38 116.9(8) . . . yes C36 C37 H37 121.6 . . . no C38 C37 H37 121.5 . . . no C37 C38 C39 121.0(7) . . . yes C37 C38 H38 119.5 . . . no C39 C38 H38 119.5 . . . no C34 C39 C38 119.9(5) . . . yes C34 C39 H39 120.0 . . . no C38 C39 H39 120.0 . . . no C41 C40 C45 123.9(6) . . . yes C41 C40 H40 118.0 . . . no C45 C40 H40 118.1 . . . no C40 C41 C42 125.6(9) . . . yes C40 C41 H41 117.2 . . . no C42 C41 H41 117.2 . . . no C41 C42 C43 105.8(7) . . . yes C41 C42 H42 127.1 . . . no C43 C42 H42 127.1 . . . no C42 C43 C44 127.5(7) . . . yes C42 C43 H43 116.3 . . . no C44 C43 H43 116.2 . . . no C43 C44 C45 119.2(6) . . . yes C43 C44 H44 120.4 . . . no C45 C44 H44 120.4 . . . no C40 C45 C44 117.8(6) . . . yes C40 C45 H45 121.1 . . . no C44 C45 H45 121.1 . . . no 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 N1 C1 C2 C3 0.7(2) . . . . yes N1 C1 C2 C6 175.8(2) . . . . yes N1 C4 C3 C2 -0.7(2) . . . . yes N1 C4 C3 C17 -176.4(2) . . . . yes N1 C4 C5 C1 -1.3(3) . . . 8_545 yes C1 N1 C4 C3 1.1(2) . . . . yes C1 N1 C4 C5 -178.7(2) . . . . yes C1 C2 C3 C4 0.0(2) . . . . yes C1 C2 C3 C17 176.8(2) . . . . yes C1 C2 C6 C7 -119.5(2) . . . . yes C1 C2 C6 C27 129.9(2) . . . . yes C2 C1 N1 C4 -1.1(2) . . . . yes C2 C3 C4 C5 179.2(2) . . . . yes C2 C3 C17 C16 -55.9(2) . . . . yes C2 C3 C17 C18 54.2(2) . . . . yes C2 C6 C7 C8 124.6(2) . . . . yes C2 C6 C7 C16 -54.8(2) . . . . yes C2 C6 C27 C18 54.8(2) . . . . yes C2 C6 C27 C26 -124.5(2) . . . . yes C3 C2 C1 C5 -177.3(2) . . . 7_555 yes C3 C2 C6 C7 55.3(2) . . . . yes C3 C2 C6 C27 -55.3(2) . . . . yes C3 C17 C16 C7 54.2(2) . . . . yes C3 C17 C16 C15 -126.2(2) . . . . yes C3 C17 C18 C19 128.4(2) . . . . yes C3 C17 C18 C27 -52.4(2) . . . . yes C4 N1 C1 C5 176.8(2) . . . 7_555 yes C4 C3 C2 C6 -176.3(2) . . . . yes C4 C3 C17 C16 119.5(2) . . . . yes C4 C3 C17 C18 -130.4(2) . . . . yes C5 C1 C2 C6 2.2(4) . 8_545 8_545 8_545 yes C5 C4 C3 C17 3.5(4) . . . . yes C6 C2 C3 C17 0.5(3) . . . . yes C6 C7 C8 C9 -179.7(2) . . . . yes C6 C7 C16 C15 -178.9(2) . . . . yes C6 C7 C16 C17 0.7(2) . . . . yes C6 C27 C18 C17 -1.8(2) . . . . yes C6 C27 C18 C19 177.5(2) . . . . yes C6 C27 C26 C25 -179.9(2) . . . . yes C7 C6 C27 C18 -54.6(2) . . . . yes C7 C6 C27 C26 126.0(2) . . . . yes C7 C8 C9 C10 -179.7(2) . . . . yes C7 C8 C9 C14 -1.3(3) . . . . yes C7 C16 C15 C14 -1.3(3) . . . . yes C7 C16 C17 C18 -56.9(2) . . . . yes C8 C7 C6 C27 -125.4(2) . . . . yes C8 C7 C16 C15 1.7(3) . . . . yes C8 C7 C16 C17 -178.7(2) . . . . yes C8 C9 C10 C11 178.2(2) . . . . yes C8 C9 C14 C13 -179.1(2) . . . . yes C8 C9 C14 C15 1.7(3) . . . . yes C9 C8 C7 C16 -0.3(3) . . . . yes C9 C10 C11 C12 0.6(4) . . . . yes C9 C14 C13 C12 1.2(3) . . . . yes C9 C14 C15 C16 -0.3(3) . . . . yes C10 C9 C14 C13 -0.7(3) . . . . yes C10 C9 C14 C15 -179.9(2) . . . . yes C10 C11 C12 C13 -0.1(4) . . . . yes C11 C10 C9 C14 -0.2(3) . . . . yes C11 C12 C13 C14 -0.8(4) . . . . yes C12 C13 C14 C15 -179.6(2) . . . . yes C13 C14 C15 C16 -179.6(2) . . . . yes C14 C15 C16 C17 179.1(2) . . . . yes C15 C16 C17 C18 122.7(2) . . . . yes C16 C7 C6 C27 55.2(2) . . . . yes C16 C17 C18 C19 -121.7(2) . . . . yes C16 C17 C18 C27 57.5(2) . . . . yes C17 C18 C19 C20 -178.6(2) . . . . yes C17 C18 C27 C26 177.6(2) . . . . yes C18 C19 C20 C21 178.1(2) . . . . yes C18 C19 C20 C25 0.9(3) . . . . yes C18 C27 C26 C25 0.7(3) . . . . yes C19 C18 C27 C26 -3.1(3) . . . . yes C19 C20 C21 C22 -175.1(2) . . . . yes C19 C20 C25 C24 175.1(2) . . . . yes C19 C20 C25 C26 -3.2(3) . . . . yes C20 C19 C18 C27 2.3(3) . . . . yes C20 C21 C22 C23 -0.9(4) . . . . yes C20 C25 C24 C23 1.2(4) . . . . yes C20 C25 C26 C27 2.4(3) . . . . yes C21 C20 C25 C24 -2.3(3) . . . . yes C21 C20 C25 C26 179.5(2) . . . . yes C21 C22 C23 C24 -0.2(5) . . . . yes C22 C21 C20 C25 2.2(4) . . . . yes C22 C23 C24 C25 0.0(4) . . . . yes C23 C24 C25 C26 179.4(2) . . . . yes C24 C25 C26 C27 -175.9(2) . . . . yes C28 C29 C30 C31 -1.2(5) . . . . yes C28 C33 C32 C31 -1.1(6) . . . . yes C29 C28 C33 C32 1.4(6) . . . . yes C29 C30 C31 C32 1.4(5) . . . . yes C30 C29 C28 C33 -0.2(5) . . . . yes C30 C31 C32 C33 -0.2(5) . . . . yes C34 C35 C36 C37 4.9(10) . . . . yes C34 C39 C38 C37 0.6(9) . . . . yes C35 C34 C39 C38 0.1(7) . . . . yes C35 C36 C37 C38 -4(1) . . . . yes C36 C35 C34 C39 -3.0(8) . . . . yes C36 C37 C38 C39 1(1) . . . . yes C40 C41 C42 C43 -3(1) . . . . yes C40 C45 C44 C43 -3.4(7) . . . . yes C41 C40 C45 C44 2.6(8) . . . . yes C41 C42 C43 C44 2(1) . . . . yes C42 C41 C40 C45 1.1(10) . . . . yes C42 C43 C44 C45 1.0(10) . . . . yes C42 C43 C44 C45 1.0(10) . . . . yes loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag N1 N1 2.926(2) . 8_545 ? N1 C1 3.023(2) . 8_545 ? N1 H1N 3.30(4) . 2_645 ? C4 H1N 2.92(4) . 8_545 ? C5 H1N 2.75(4) . 8_545 ? C5 C6 3.360(3) . 8_545 ? C11 C31 3.553(4) . 4_565 ? C15 C30 3.445(3) . 8_545 ? C19 C35 3.591(5) . 8_545 ? C20 C35 3.366(4) . 8_545 ? C24 C24 3.502(5) . 2_655 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_site_distance_DH _geom_hbond_site_distance_HA _geom_hbond_site_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag N1 H1N N1 . . 7_555 0.84(3) 2.44(3) 2.926(2) 117(3) no N1 H1N N1 . . 8_545 0.84(3) 2.37(3) 2.926(2) 124(3) no #============================================================================== data_12-12PhHsqueezed(12) _database_code_depnum_ccdc_archive 'CCDC 248909' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C180 H134 N4 ' _chemical_formula_moiety 'C108 H62 N4, 12(C6 H6)' _chemical_formula_weight 2352.91 _chemical_melting_point ? # CRYSTAL DATA _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 41/a ' _symmetry_space_group_name_Hall '-I 4ad ' _symmetry_Int_Tables_number 88 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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+3/4, x+1/4, z+1/4' '-x+1/2, -y, z+1/2' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-y+5/4, x+3/4, z+3/4' '-x+1, -y+1/2, z+1' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'y-3/4, -x-1/4, -z-1/4' 'x-1/2, y, -z-1/2' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'y-1/4, -x+1/4, -z+1/4' 'x, y+1/2, -z' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 19.3904(10) _cell_length_b 19.3904(10) _cell_length_c 36.077(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 13564.4(12) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 12512 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description Prism _exptl_crystal_colour Red _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_F_000 4968 _exptl_crystal_density_diffrn 1.152 _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.066 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details Coppens_numerical _exptl_absorpt_correction_T_max 0.9886 _exptl_absorpt_correction_T_min 0.9805 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_type 'Mo Ka' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method w _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 14.62 _diffrn_reflns_number 55378 _diffrn_reflns_av_R_equivalents 0.0664 _diffrn_reflns_av_sigmaI/netI 0.0530 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.994 _reflns_number_total 7742 _reflns_number_gt 4993 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR97 _computing_publication_material 'CrystalStructure Ver. 3.5.1' _computing_structure_refinement 'SHELXH-97 and PLATON SQUEEZE' _computing_molecular_graphics ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The solvent molecules are removed one by one by using PLATON SQUEEZE program. ; _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^)+(0.1210P)^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 noref _refine_ls_number_reflns 7742 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0789 _refine_ls_R_factor_gt 0.0658 _refine_ls_wR_factor_ref 0.1980 _refine_ls_wR_factor_gt 0.1910 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.384 _refine_diff_density_min -0.242 _refine_diff_density_rms 0.059 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 N1 N 0.52912(6) 0.64759(6) 0.12386(3) 0.0247(3) Uani 1 1 d . . . C1 C 0.48448(7) 0.59215(7) 0.12274(3) 0.0247(3) Uani 1 1 d . . . C2 C 0.52563(7) 0.53007(7) 0.12191(3) 0.0252(3) Uani 1 1 d . . . C3 C 0.59314(7) 0.54889(7) 0.12292(3) 0.0256(3) Uani 1 1 d . . . C4 C 0.59552(7) 0.62289(7) 0.12452(3) 0.0251(3) Uani 1 1 d . . . C5 C 0.65460(7) 0.66323(7) 0.12638(3) 0.0264(3) Uani 1 1 d . . . C6 C 0.51223(7) 0.45358(7) 0.12272(4) 0.0269(3) Uani 1 1 d . . . C7 C 0.54971(7) 0.42889(7) 0.15770(4) 0.0284(3) Uani 1 1 d . . . C8 C 0.52146(8) 0.39315(8) 0.18635(4) 0.0321(3) Uani 1 1 d . . . C9 C 0.56266(9) 0.37408(8) 0.21731(4) 0.0370(4) Uani 1 1 d . . . C10 C 0.53571(10) 0.33662(9) 0.24781(5) 0.0470(4) Uani 1 1 d . . . C11 C 0.57709(12) 0.31803(11) 0.27661(5) 0.0572(5) Uani 1 1 d . . . C12 C 0.64683(11) 0.33580(11) 0.27705(5) 0.0564(5) Uani 1 1 d . . . C13 C 0.67478(10) 0.37149(9) 0.24840(4) 0.0443(4) Uani 1 1 d . . . C14 C 0.63364(9) 0.39169(8) 0.21768(4) 0.0368(4) Uani 1 1 d . . . C15 C 0.66181(8) 0.42942(8) 0.18738(4) 0.0327(3) Uani 1 1 d . . . C16 C 0.62088(7) 0.44813(7) 0.15870(4) 0.0281(3) Uani 1 1 d . . . C17 C 0.64328(7) 0.48956(7) 0.12436(4) 0.0287(3) Uani 1 1 d . . . C18 C 0.62553(7) 0.44289(7) 0.09162(4) 0.0283(3) Uani 1 1 d . . . C19 C 0.66999(8) 0.41953(8) 0.06573(4) 0.0363(4) Uani 1 1 d . . . C20 C 0.64548(9) 0.37758(8) 0.03573(4) 0.0413(4) Uani 1 1 d . . . C21 C 0.69027(11) 0.35369(10) 0.00775(5) 0.0567(5) Uani 1 1 d . . . C22 C 0.66402(14) 0.31733(12) -0.02203(6) 0.0721(7) Uani 1 1 d . . . C23 C 0.59439(14) 0.30384(12) -0.02475(5) 0.0698(7) Uani 1 1 d . . . C24 C 0.55029(12) 0.32564(10) 0.00228(5) 0.0568(5) Uani 1 1 d . . . C25 C 0.57449(10) 0.36212(8) 0.03347(4) 0.0407(4) Uani 1 1 d . . . C26 C 0.52909(8) 0.38542(8) 0.06202(4) 0.0338(3) Uani 1 1 d . . . C27 C 0.55411(8) 0.42438(7) 0.09037(4) 0.0288(3) Uani 1 1 d . . . H1 H 0.5174 0.6903 0.1241 0.030 Uiso 0.50 1 c P . . H2 H 0.6965 0.6398 0.1271 0.032 Uiso 1 1 c . . . H3 H 0.4632 0.4413 0.1220 0.032 Uiso 1 1 c . . . H4 H 0.4750 0.3811 0.1857 0.039 Uiso 1 1 c . . . H5 H 0.4893 0.3246 0.2481 0.056 Uiso 1 1 c . . . H6 H 0.5586 0.2931 0.2963 0.069 Uiso 1 1 c . . . H7 H 0.6743 0.3231 0.2971 0.068 Uiso 1 1 c . . . H8 H 0.7214 0.3828 0.2489 0.053 Uiso 1 1 c . . . H9 H 0.7083 0.4412 0.1873 0.039 Uiso 1 1 c . . . H10 H 0.6917 0.5040 0.1250 0.034 Uiso 1 1 c . . . H11 H 0.7166 0.4306 0.0673 0.044 Uiso 1 1 c . . . H12 H 0.7374 0.3624 0.0093 0.068 Uiso 1 1 c . . . H13 H 0.6937 0.3018 -0.0405 0.086 Uiso 1 1 c . . . H14 H 0.5774 0.2798 -0.0451 0.084 Uiso 1 1 c . . . H15 H 0.5034 0.3162 0.0001 0.068 Uiso 1 1 c . . . H16 H 0.4825 0.3740 0.0612 0.041 Uiso 1 1 c . . . 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 N1 0.0217(6) 0.0198(6) 0.0325(6) -0.0012(4) -0.0002(4) 0.0008(5) C1 0.0255(7) 0.0214(7) 0.0272(6) 0.0001(5) 0.0015(5) 0.0026(6) C2 0.0215(7) 0.0211(7) 0.0328(7) -0.0002(5) 0.0011(5) 0.0013(5) C3 0.0228(7) 0.0178(7) 0.0364(7) 0.0018(5) 0.0013(5) 0.0013(5) C4 0.0254(7) 0.0213(7) 0.0285(6) 0.0009(5) -0.0021(5) 0.0025(6) C5 0.0217(7) 0.0222(7) 0.0352(7) 0.0003(5) -0.0007(5) 0.0036(6) C6 0.0200(7) 0.0197(7) 0.0411(7) -0.0023(5) 0.0031(5) -0.0007(5) C7 0.0245(7) 0.0192(7) 0.0413(7) -0.0008(5) 0.0025(6) 0.0032(6) C8 0.0275(8) 0.0270(8) 0.0419(8) -0.0023(6) 0.0061(6) -0.0021(6) C9 0.0413(9) 0.0291(8) 0.0406(8) 0.0015(6) 0.0062(6) 0.0012(7) C10 0.0468(11) 0.0434(10) 0.0508(9) 0.0054(7) 0.0121(8) -0.0007(8) C11 0.0685(14) 0.0583(13) 0.0447(10) 0.0149(8) 0.0132(9) 0.0022(11) C12 0.0599(13) 0.0596(13) 0.0496(10) 0.0112(9) -0.0019(9) 0.0107(11) C13 0.0477(10) 0.0396(10) 0.0456(9) 0.0052(7) -0.0033(7) 0.0075(8) C14 0.0367(9) 0.0276(8) 0.0463(8) 0.0007(6) 0.0005(6) 0.0053(7) C15 0.0253(8) 0.0263(8) 0.0466(8) 0.0006(6) -0.0025(6) 0.0010(6) C16 0.0242(7) 0.0194(7) 0.0408(7) 0.0027(5) 0.0040(6) 0.0022(6) C17 0.0205(7) 0.0179(7) 0.0478(8) 0.0018(6) 0.0025(6) 0.0002(5) C18 0.0255(7) 0.0165(7) 0.0430(8) 0.0037(5) 0.0035(6) 0.0009(6) C19 0.0307(8) 0.0282(8) 0.0501(9) 0.0025(6) 0.0091(6) 0.0013(7) C20 0.0474(11) 0.0278(8) 0.0485(9) 0.0000(6) 0.0143(7) -0.0002(8) C21 0.0595(13) 0.0476(11) 0.0631(11) -0.0095(9) 0.0287(9) -0.0050(10) C22 0.0932(19) 0.0575(13) 0.0656(13) -0.0197(10) 0.0424(12) -0.0125(13) C23 0.0910(18) 0.0659(14) 0.0524(11) -0.0194(10) 0.0244(11) -0.0226(13) C24 0.0720(14) 0.0473(11) 0.0510(10) -0.0129(8) 0.0059(9) -0.0113(10) C25 0.0508(11) 0.0304(9) 0.0408(8) -0.0014(6) 0.0065(7) -0.0082(8) C26 0.0314(8) 0.0242(8) 0.0458(8) -0.0035(6) 0.0019(6) -0.0040(6) C27 0.0275(8) 0.0164(7) 0.0425(8) 0.0029(5) 0.0011(6) 0.0011(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 N1 C4 1.3739(18) . ? N1 C1 1.3808(18) . ? N1 H1 0.8600 . ? C1 C5 1.383(2) 14_565 ? C1 C2 1.4444(19) . ? C2 C3 1.360(2) . ? C2 C6 1.506(2) . ? C3 C4 1.4367(19) . ? C3 C17 1.507(2) . ? C4 C5 1.389(2) . ? C5 C1 1.383(2) 12_766 ? C5 H2 0.9300 . ? C6 C27 1.5303(19) . ? C6 C7 1.5329(19) . ? C6 H3 0.9802 . ? C7 C8 1.3598(19) . ? C7 C16 1.430(2) . ? C8 C9 1.422(2) . ? C8 H4 0.9300 . ? C9 C14 1.418(2) . ? C9 C10 1.418(2) . ? C10 C11 1.362(3) . ? C10 H5 0.9300 . ? C11 C12 1.396(3) . ? C11 H6 0.9299 . ? C12 C13 1.357(2) . ? C12 H7 0.9299 . ? C13 C14 1.421(2) . ? C13 H8 0.9300 . ? C14 C15 1.424(2) . ? C15 C16 1.354(2) . ? C15 H9 0.9299 . ? C16 C17 1.5391(18) . ? C17 C18 1.5274(19) . ? C17 H10 0.9799 . ? C18 C19 1.349(2) . ? C18 C27 1.431(2) . ? C19 C20 1.435(2) . ? C19 H11 0.9300 . ? C20 C21 1.410(2) . ? C20 C25 1.411(3) . ? C21 C22 1.382(3) . ? C21 H12 0.930 . ? C22 C23 1.379(4) . ? C22 H13 0.9301 . ? C23 C24 1.364(3) . ? C23 H14 0.930 . ? C24 C25 1.410(2) . ? C24 H15 0.930 . ? C25 C26 1.428(2) . ? C26 C27 1.361(2) . ? C26 H16 0.9301 . ? 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 C4 N1 C1 108.45(11) . . ? C4 N1 H1 125.78 . . ? C1 N1 H1 125.77 . . ? N1 C1 C5 126.14(13) . 14_565 ? N1 C1 C2 107.65(11) . . ? C5 C1 C2 126.17(13) 14_565 . ? C3 C2 C1 107.91(12) . . ? C3 C2 C6 115.47(12) . . ? C1 C2 C6 136.47(13) . . ? C2 C3 C4 107.46(12) . . ? C2 C3 C17 114.66(12) . . ? C4 C3 C17 137.76(13) . . ? N1 C4 C5 125.27(13) . . ? N1 C4 C3 108.51(12) . . ? C5 C4 C3 126.22(13) . . ? C1 C5 C4 126.96(13) 12_766 . ? C1 C5 H2 116.51 12_766 . ? C4 C5 H2 116.53 . . ? C2 C6 C27 104.96(11) . . ? C2 C6 C7 103.99(11) . . ? C27 C6 C7 105.10(11) . . ? C2 C6 H3 113.92 . . ? C27 C6 H3 113.91 . . ? C7 C6 H3 113.92 . . ? C8 C7 C16 120.17(13) . . ? C8 C7 C6 126.44(13) . . ? C16 C7 C6 113.39(12) . . ? C7 C8 C9 120.21(14) . . ? C7 C8 H4 119.90 . . ? C9 C8 H4 119.89 . . ? C14 C9 C10 118.26(15) . . ? C14 C9 C8 119.35(13) . . ? C10 C9 C8 122.38(15) . . ? C11 C10 C9 120.70(17) . . ? C11 C10 H5 119.65 . . ? C9 C10 H5 119.64 . . ? C10 C11 C12 120.97(16) . . ? C10 C11 H6 119.5 . . ? C12 C11 H6 119.5 . . ? C13 C12 C11 120.28(17) . . ? C13 C12 H7 119.9 . . ? C11 C12 H7 119.86 . . ? C12 C13 C14 120.71(17) . . ? C12 C13 H8 119.64 . . ? C14 C13 H8 119.65 . . ? C9 C14 C13 119.08(14) . . ? C9 C14 C15 119.25(14) . . ? C13 C14 C15 121.67(15) . . ? C16 C15 C14 119.97(14) . . ? C16 C15 H9 120.01 . . ? C14 C15 H9 120.03 . . ? C15 C16 C7 121.01(13) . . ? C15 C16 C17 126.14(13) . . ? C7 C16 C17 112.84(12) . . ? C3 C17 C18 106.27(11) . . ? C3 C17 C16 104.13(11) . . ? C18 C17 C16 104.46(11) . . ? C3 C17 H10 113.66 . . ? C18 C17 H10 113.68 . . ? C16 C17 H10 113.69 . . ? C19 C18 C27 120.82(13) . . ? C19 C18 C17 126.17(13) . . ? C27 C18 C17 113.01(12) . . ? C18 C19 C20 120.05(14) . . ? C18 C19 H11 119.99 . . ? C20 C19 H11 119.95 . . ? C21 C20 C25 119.32(16) . . ? C21 C20 C19 121.48(16) . . ? C25 C20 C19 119.15(14) . . ? C22 C21 C20 119.81(19) . . ? C22 C21 H12 120.10 . . ? C20 C21 H12 120.09 . . ? C23 C22 C21 120.86(18) . . ? C23 C22 H13 119.6 . . ? C21 C22 H13 119.6 . . ? C24 C23 C22 120.27(19) . . ? C24 C23 H14 119.9 . . ? C22 C23 H14 119.9 . . ? C23 C24 C25 121.2(2) . . ? C23 C24 H15 119.42 . . ? C25 C24 H15 119.41 . . ? C24 C25 C20 118.52(16) . . ? C24 C25 C26 121.96(17) . . ? C20 C25 C26 119.49(14) . . ? C27 C26 C25 119.87(14) . . ? C27 C26 H16 120.08 . . ? C25 C26 H16 120.06 . . ? C26 C27 C18 120.52(14) . . ? C26 C27 C6 126.11(13) . . ? C18 C27 C6 113.38(12) . . ? 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 C4 N1 C1 C5 176.66(12) . . . 14_565 ? C4 N1 C1 C2 -1.20(13) . . . . ? N1 C1 C2 C3 0.62(14) . . . . ? C5 C1 C2 C3 -177.24(12) 14_565 . . . ? N1 C1 C2 C6 175.77(13) . . . . ? C5 C1 C2 C6 -2.1(2) 14_565 . . . ? C1 C2 C3 C4 0.18(14) . . . . ? C6 C2 C3 C4 -176.12(10) . . . . ? C1 C2 C3 C17 176.79(10) . . . . ? C6 C2 C3 C17 0.49(16) . . . . ? C1 N1 C4 C5 -178.73(12) . . . . ? C1 N1 C4 C3 1.32(13) . . . . ? C2 C3 C4 N1 -0.92(14) . . . . ? C17 C3 C4 N1 -176.35(14) . . . . ? C2 C3 C4 C5 179.13(12) . . . . ? C17 C3 C4 C5 3.7(2) . . . . ? N1 C4 C5 C1 -1.2(2) . . . 12_766 ? C3 C4 C5 C1 178.75(12) . . . 12_766 ? C3 C2 C6 C27 -54.85(14) . . . . ? C1 C2 C6 C27 130.27(15) . . . . ? C3 C2 C6 C7 55.30(14) . . . . ? C1 C2 C6 C7 -119.58(16) . . . . ? C2 C6 C7 C8 124.53(15) . . . . ? C27 C6 C7 C8 -125.43(15) . . . . ? C2 C6 C7 C16 -54.37(15) . . . . ? C27 C6 C7 C16 55.67(15) . . . . ? C16 C7 C8 C9 -0.6(2) . . . . ? C6 C7 C8 C9 -179.47(13) . . . . ? C7 C8 C9 C14 -1.1(2) . . . . ? C7 C8 C9 C10 -179.79(15) . . . . ? C14 C9 C10 C11 -0.1(3) . . . . ? C8 C9 C10 C11 178.62(17) . . . . ? C9 C10 C11 C12 0.6(3) . . . . ? C10 C11 C12 C13 -0.7(3) . . . . ? C11 C12 C13 C14 0.4(3) . . . . ? C10 C9 C14 C13 -0.2(2) . . . . ? C8 C9 C14 C13 -178.97(14) . . . . ? C10 C9 C14 C15 -179.87(14) . . . . ? C8 C9 C14 C15 1.4(2) . . . . ? C12 C13 C14 C9 0.1(3) . . . . ? C12 C13 C14 C15 179.73(17) . . . . ? C9 C14 C15 C16 0.1(2) . . . . ? C13 C14 C15 C16 -179.58(15) . . . . ? C14 C15 C16 C7 -1.8(2) . . . . ? C14 C15 C16 C17 179.18(13) . . . . ? C8 C7 C16 C15 2.1(2) . . . . ? C6 C7 C16 C15 -178.89(13) . . . . ? C8 C7 C16 C17 -178.75(12) . . . . ? C6 C7 C16 C17 0.23(16) . . . . ? C2 C3 C17 C18 53.93(14) . . . . ? C4 C3 C17 C18 -130.88(16) . . . . ? C2 C3 C17 C16 -56.06(15) . . . . ? C4 C3 C17 C16 119.14(16) . . . . ? C15 C16 C17 C3 -126.44(15) . . . . ? C7 C16 C17 C3 54.50(15) . . . . ? C15 C16 C17 C18 122.26(15) . . . . ? C7 C16 C17 C18 -56.81(15) . . . . ? C3 C17 C18 C19 128.21(15) . . . . ? C16 C17 C18 C19 -122.04(15) . . . . ? C3 C17 C18 C27 -52.06(15) . . . . ? C16 C17 C18 C27 57.69(15) . . . . ? C27 C18 C19 C20 2.2(2) . . . . ? C17 C18 C19 C20 -178.04(13) . . . . ? C18 C19 C20 C21 178.48(16) . . . . ? C18 C19 C20 C25 0.9(2) . . . . ? C25 C20 C21 C22 1.9(3) . . . . ? C19 C20 C21 C22 -175.65(19) . . . . ? C20 C21 C22 C23 -0.2(3) . . . . ? C21 C22 C23 C24 -0.7(4) . . . . ? C22 C23 C24 C25 -0.1(4) . . . . ? C23 C24 C25 C20 1.8(3) . . . . ? C23 C24 C25 C26 179.9(2) . . . . ? C21 C20 C25 C24 -2.7(2) . . . . ? C19 C20 C25 C24 174.92(16) . . . . ? C21 C20 C25 C26 179.14(16) . . . . ? C19 C20 C25 C26 -3.2(2) . . . . ? C24 C25 C26 C27 -175.66(16) . . . . ? C20 C25 C26 C27 2.4(2) . . . . ? C25 C26 C27 C18 0.7(2) . . . . ? C25 C26 C27 C6 179.51(14) . . . . ? C19 C18 C27 C26 -3.1(2) . . . . ? C17 C18 C27 C26 177.15(13) . . . . ? C19 C18 C27 C6 177.95(13) . . . . ? C17 C18 C27 C6 -1.81(16) . . . . ? C2 C6 C27 C26 -124.45(15) . . . . ? C7 C6 C27 C26 126.21(15) . . . . ? C2 C6 C27 C18 54.44(15) . . . . ? C7 C6 C27 C18 -54.90(15) . . . . ? #============================================================================== data_12-8PhCl-4IPA _database_code_depnum_ccdc_archive 'CCDC 248910' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C168 H134 Cl8 N4 O4 ' _chemical_formula_moiety 'C108 H60 N4, 8(C6 H5 Cl), 4(C3 H8 O)' _chemical_formula_weight 2556.55 _chemical_melting_point ? # CRYSTAL DATA _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 41/a' _symmetry_space_group_name_Hall '-I 4ad' _symmetry_Int_Tables_number 88 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2-y,z 3/4-y,1/4+x,1/4+z 1/4+y,1/4-x,1/4+z -x,-y,-z x,1/2+y,-z 3/4+y,1/4-x,1/4-z 1/4-y,1/4+x,1/4-z 1/2+x,1/2+y,1/2+z 1/2-x,-y,1/2+z 1/4-y,3/4+x,3/4+z 3/4+y,3/4-x,3/4+z 1/2-x,1/2-y,1/2-z 1/2+x,y,1/2-z 1/4+y,3/4-x,3/4-z 3/4-y,3/4+x,3/4-z _cell_length_a 19.720(1) _cell_length_b 19.720(1) _cell_length_c 35.239(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 13703(1) _cell_formula_units_Z 4 _cell_measurement_reflns_used 7308 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 173.2 _exptl_crystal_description Prism _exptl_crystal_colour Red _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 1.239 _exptl_crystal_F_000 5352 _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.223 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.7111 # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo Ka' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method w _diffrn_detector_area_resol_mean 14.62 _diffrn_reflns_number 56970 _diffrn_reflns_av_R_equivalents 0.097 _diffrn_reflns_theta_max 27.49 _diffrn_measured_fraction_theta_max 0.9969 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.9969 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 40 # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 7853 _reflns_number_gt 2457 _reflns_threshold_expression F^2^>2.0s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0968 _refine_ls_wR_factor_ref 0.2407 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 7853 _refine_ls_number_parameters 361 _refine_ls_goodness_of_fit_ref 1.214 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[s^2^(Fo^2^) + (0.05000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0007 _refine_diff_density_max 1.09 _refine_diff_density_min -0.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cl Cl 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl(1a) Cl 0.3159(3) 0.4698(5) 0.1040(2) 0.145(3) Uani 0.60 d P . . Cl(1b) Cl 0.6879(8) 0.0469(9) 0.0823(4) 0.143(6) Uani 0.30 d P . . Cl(1c) Cl 0.556(1) 0.091(1) 0.0345(7) 0.15(1) Uani 0.10 d P . . Cl(2a) Cl 0.3582(3) 0.5397(3) 0.2316(2) 0.185(3) Uani 0.50 d P . . Cl(2b) Cl 0.7626(3) 0.1144(4) 0.1998(2) 0.172(4) Uani 0.35 d P . . Cl(2c) Cl 0.4000(6) 0.5072(6) 0.2707(6) 0.179(7) Uani 0.15 d P . . O(1) O 0.5319(2) 0.6608(2) 0.1169(1) 0.108(2) Uani 1.00 d . . . N(1) N 0.1012(2) 0.2225(2) 0.1253(1) 0.032(1) Uani 1.00 d . . . C(1) C 0.1258(2) 0.1578(2) 0.1234(1) 0.033(1) Uani 1.00 d . . . C(2) C 0.1988(2) 0.1611(2) 0.1238(1) 0.033(1) Uani 1.00 d . . . C(3) C 0.2164(2) 0.2271(2) 0.1252(1) 0.034(1) Uani 1.00 d . . . C(4) C 0.1551(2) 0.2669(2) 0.1257(1) 0.033(1) Uani 1.00 d . . . C(5) C 0.1506(2) 0.3363(2) 0.1264(1) 0.036(1) Uani 1.00 d . . . C(6) C 0.2917(2) 0.2403(2) 0.1242(1) 0.036(1) Uani 1.00 d . . . C(7) C 0.3207(2) 0.1992(2) 0.1569(1) 0.034(1) Uani 1.00 d . . . C(8) C 0.3605(2) 0.2235(2) 0.1851(2) 0.046(2) Uani 1.00 d . . . C(9) C 0.3857(2) 0.1788(3) 0.2140(2) 0.050(2) Uani 1.00 d . . . C(10) C 0.4251(3) 0.2016(3) 0.2442(2) 0.075(2) Uani 1.00 d . . . C(11) C 0.4481(3) 0.1575(4) 0.2716(2) 0.092(3) Uani 1.00 d . . . C(12) C 0.4345(3) 0.0887(4) 0.2689(2) 0.093(3) Uani 1.00 d . . . C(13) C 0.3967(3) 0.0642(3) 0.2392(2) 0.070(2) Uani 1.00 d . . . C(14) C 0.3702(2) 0.1092(3) 0.2113(2) 0.053(2) Uani 1.00 d . . . C(15) C 0.3277(2) 0.0847(2) 0.1815(2) 0.046(2) Uani 1.00 d . . . C(16) C 0.3031(2) 0.1296(2) 0.1555(1) 0.037(1) Uani 1.00 d . . . C(17) C 0.2577(2) 0.1122(2) 0.1220(2) 0.041(1) Uani 1.00 d . . . C(18) C 0.2988(2) 0.1348(2) 0.0873(1) 0.038(1) Uani 1.00 d . . . C(19) C 0.3191(2) 0.0948(2) 0.0580(2) 0.047(2) Uani 1.00 d . . . C(20) C 0.3572(2) 0.1216(3) 0.0277(2) 0.056(2) Uani 1.00 d . . . C(21) C 0.3798(3) 0.0809(3) -0.0025(2) 0.078(2) Uani 1.00 d . . . C(22) C 0.4178(4) 0.1088(4) -0.0307(2) 0.108(3) Uani 1.00 d . . . C(23) C 0.4342(3) 0.1790(4) -0.0308(2) 0.100(3) Uani 1.00 d . . . C(24) C 0.4131(3) 0.2193(3) -0.0018(2) 0.073(2) Uani 1.00 d . . . C(25) C 0.3739(2) 0.1922(3) 0.0279(2) 0.058(2) Uani 1.00 d . . . C(26) C 0.3531(2) 0.2323(2) 0.0593(2) 0.048(2) Uani 1.00 d . . . C(27) C 0.3166(2) 0.2053(2) 0.0884(1) 0.038(1) Uani 1.00 d . . . C(28a) C 0.3872(3) 0.4261(4) 0.1057(2) 0.0516 Uiso 0.60 d G . . C(28b) C 0.6137(7) 0.0753(8) 0.1023(4) 0.0963 Uiso 0.40 d G . . C(29a) C 0.4229(4) 0.4147(4) 0.0721(2) 0.0683 Uiso 0.60 d G . . C(29b) C 0.5617(8) 0.1027(9) 0.0804(3) 0.0963 Uiso 0.40 d G . . C(30a) C 0.4830(4) 0.3773(4) 0.0727(2) 0.0865 Uiso 0.60 d G . . C(30b) C 0.5054(6) 0.1319(8) 0.0979(4) 0.0963 Uiso 0.40 d G . . C(31a) C 0.5073(3) 0.3513(4) 0.1069(2) 0.1002 Uiso 0.60 d G . . C(31b) C 0.5012(6) 0.1337(7) 0.1374(4) 0.0963 Uiso 0.40 d G . . C(32a) C 0.4716(4) 0.3627(4) 0.1405(2) 0.1012 Uiso 0.60 d G . . C(32b) C 0.5533(7) 0.1062(6) 0.1594(3) 0.0963 Uiso 0.40 d G . . C(33a) C 0.4116(4) 0.4001(4) 0.1399(2) 0.0917 Uiso 0.60 d G . . C(33b) C 0.6095(6) 0.0770(7) 0.1418(4) 0.0963 Uiso 0.40 d G . . C(34a) C 0.3323(4) 0.4556(3) 0.2427(2) 0.0997 Uiso 0.65 d G . . C(34b) C 0.7131(7) 0.0951(9) 0.2333(5) 0.1104 Uiso 0.35 d G . . C(35a) C 0.2800(4) 0.4241(4) 0.2227(2) 0.1068 Uiso 0.65 d G . . C(35b) C 0.6914(8) 0.0293(8) 0.2254(4) 0.1104 Uiso 0.35 d G . . C(36a) C 0.2620(3) 0.3574(4) 0.2312(2) 0.0864 Uiso 0.65 d G . . C(36b) C 0.6373(9) 0.0014(7) 0.2456(5) 0.1104 Uiso 0.35 d G . . C(37a) C 0.2963(4) 0.3222(3) 0.2597(2) 0.1012 Uiso 0.65 d G . . C(37b) C 0.6049(7) 0.0393(9) 0.2737(5) 0.1104 Uiso 0.35 d G . . C(38a) C 0.3487(4) 0.3537(4) 0.2796(2) 0.0999 Uiso 0.65 d G . . C(38b) C 0.6266(8) 0.1051(9) 0.2816(4) 0.1104 Uiso 0.35 d G . . C(39a) C 0.3666(4) 0.4204(4) 0.2711(2) 0.1415 Uiso 0.65 d G . . C(39b) C 0.6807(8) 0.1330(7) 0.2614(5) 0.1104 Uiso 0.35 d G . . C(40) C 0.5690(7) 0.6003(5) 0.1264(3) 0.2345 Uiso 1.00 d G . . C(41) C 0.5172(6) 0.5528(6) 0.1453(3) 0.2345 Uiso 1.00 d G . . C(42) C 0.5929(6) 0.5689(6) 0.0886(3) 0.2345 Uiso 1.00 d G . . H(1N) H 0.0591 0.2337 0.1261 0.0381 Uiso 0.50 calc P . . H(1O) H 0.4839 0.6488 0.1112 0.1285 Uiso 1.00 calc . . . H(5) H 0.1898 0.3625 0.1266 0.0429 Uiso 1.00 calc . . . H(6) H 0.3034 0.2885 0.1254 0.0433 Uiso 1.00 calc . . . H(8) H 0.3715 0.2694 0.1858 0.0551 Uiso 1.00 calc . . . H(10) H 0.4361 0.2474 0.2458 0.0898 Uiso 1.00 calc . . . H(11) H 0.4729 0.1739 0.2921 0.1104 Uiso 1.00 calc . . . H(12) H 0.4509 0.0591 0.2873 0.1116 Uiso 1.00 calc . . . H(13) H 0.3883 0.0179 0.2372 0.0840 Uiso 1.00 calc . . . H(15) H 0.3170 0.0389 0.1799 0.0549 Uiso 1.00 calc . . . H(17) H 0.2440 0.0644 0.1212 0.0493 Uiso 1.00 calc . . . H(19) H 0.3076 0.0491 0.0580 0.0570 Uiso 1.00 calc . . . H(21) H 0.3688 0.0350 -0.0032 0.0940 Uiso 1.00 calc . . . H(22) H 0.4333 0.0814 -0.0504 0.1293 Uiso 1.00 calc . . . H(23) H 0.4594 0.1973 -0.0506 0.1205 Uiso 1.00 calc . . . H(24) H 0.4247 0.2650 -0.0016 0.0881 Uiso 1.00 calc . . . H(26) H 0.3647 0.2780 0.0599 0.0576 Uiso 1.00 calc . . . H(28b) H 0.6520 0.0554 0.0903 0.1155 Uiso 0.20 calc P . . H(29a) H 0.4063 0.4324 0.0488 0.0840 Uiso 0.60 calc G . . H(29b) H 0.565 0.101 0.0535 0.0963 Uiso 0.20 calc G . . H(30a) H 0.5072 0.3695 0.0498 0.0840 Uiso 0.60 calc G . . H(30b) H 0.4699 0.151 0.0830 0.0963 Uiso 0.40 calc G . . H(31a) H 0.5482 0.3259 0.1073 0.0840 Uiso 0.60 calc G . . H(31b) H 0.4628 0.1535 0.1494 0.0963 Uiso 0.40 calc G . . H(32a) H 0.4882 0.3450 0.1638 0.0840 Uiso 0.60 calc G . . H(32b) H 0.5504 0.1075 0.1863 0.0963 Uiso 0.40 calc G . . H(33a) H 0.3873 0.4079 0.1627 0.0840 Uiso 0.60 calc G . . H(33b) H 0.6450 0.058 0.1568 0.0963 Uiso 0.40 calc G . . H(35a) H 0.2566 0.4481 0.2033 0.1066 Uiso 0.65 calc G . . H(35b) H 0.713 0.004 0.2063 0.1104 Uiso 0.35 calc G . . H(36a) H 0.2263 0.3359 0.2176 0.1066 Uiso 0.65 calc G . . H(36b) H 0.623 -0.0435 0.2402 0.1104 Uiso 0.35 calc G . . H(37a) H 0.2841 0.2768 0.2655 0.1066 Uiso 0.65 calc G . . H(37b) H 0.5681 0.020 0.2874 0.1104 Uiso 0.35 calc G . . H(38a) H 0.3721 0.3298 0.2990 0.1066 Uiso 0.65 calc G . . H(38b) H 0.605 0.131 0.3007 0.1104 Uiso 0.35 calc G . . H(39a) H 0.4023 0.4419 0.2847 0.1066 Uiso 0.65 calc G . . H(39b) H 0.695 0.1779 0.2668 0.1104 Uiso 0.35 calc G . . H(40) H 0.6073 0.6101 0.1432 0.2814 Uiso 1.00 calc . . . H(41a) H 0.5013 0.5731 0.1685 0.2814 Uiso 1.00 calc . . . H(41b) H 0.4796 0.5457 0.1285 0.2814 Uiso 1.00 calc . . . H(41c) H 0.5384 0.5101 0.1509 0.2814 Uiso 1.00 calc . . . H(42a) H 0.6122 0.5250 0.0934 0.2814 Uiso 1.00 calc . . . H(42b) H 0.5549 0.5643 0.0718 0.2814 Uiso 1.00 calc . . . H(42c) H 0.6264 0.5977 0.0772 0.2814 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cl(1a) 0.066(3) 0.143(5) 0.226(9) 0.069(3) 0.031(4) 0.053(6) Cl(1b) 0.097(7) 0.15(1) 0.18(1) 0.007(6) 0.046(9) -0.08(1) Cl(1c) 0.19(2) 0.12(2) 0.15(2) 0.03(2) 0.01(2) -0.02(2) Cl(2a) 0.191(6) 0.155(5) 0.209(7) 0.003(4) 0.039(5) 0.027(5) Cl(2b) 0.111(5) 0.234(8) 0.171(8) 0.006(5) 0.020(5) 0.035(6) Cl(2c) 0.094(9) 0.064(8) 0.38(3) 0.027(7) -0.13(1) -0.12(1) O(1) 0.095(3) 0.089(3) 0.140(5) 0.032(3) -0.034(3) -0.013(3) N(1) 0.030(2) 0.025(2) 0.040(2) 0.001(2) -0.002(2) -0.002(2) C(1) 0.028(2) 0.032(3) 0.039(3) -0.001(2) 0.005(2) 0.000(2) C(2) 0.028(2) 0.030(2) 0.042(3) -0.001(2) 0.002(2) -0.005(2) C(3) 0.032(3) 0.032(3) 0.039(3) -0.002(2) 0.001(2) -0.004(2) C(4) 0.024(2) 0.036(3) 0.038(3) -0.002(2) -0.008(2) -0.003(2) C(5) 0.025(2) 0.027(2) 0.055(3) -0.006(2) -0.002(2) 0.001(2) C(6) 0.024(2) 0.032(2) 0.052(3) -0.002(2) 0.000(2) -0.006(3) C(7) 0.019(2) 0.041(3) 0.043(3) -0.001(2) 0.001(2) -0.004(2) C(8) 0.034(3) 0.047(3) 0.057(4) 0.004(2) 0.001(3) 0.002(3) C(9) 0.034(3) 0.065(4) 0.051(4) -0.001(3) -0.003(3) -0.001(3) C(10) 0.067(4) 0.099(5) 0.059(4) -0.020(4) -0.018(3) 0.017(4) C(11) 0.070(5) 0.129(6) 0.077(5) -0.021(4) -0.026(4) 0.029(5) C(12) 0.065(4) 0.119(6) 0.094(6) -0.016(4) -0.023(4) 0.058(5) C(13) 0.040(3) 0.086(4) 0.084(5) 0.003(3) 0.002(3) 0.031(4) C(14) 0.031(3) 0.070(4) 0.057(4) -0.002(3) 0.001(3) 0.018(3) C(15) 0.030(3) 0.039(3) 0.068(4) 0.005(2) 0.011(3) 0.003(3) C(16) 0.020(2) 0.039(3) 0.053(4) 0.006(2) 0.007(2) 0.002(3) C(17) 0.026(2) 0.025(2) 0.073(4) 0.003(2) -0.006(3) -0.006(3) C(18) 0.025(3) 0.043(3) 0.046(3) 0.006(2) 0.003(2) 0.001(3) C(19) 0.038(3) 0.045(3) 0.060(4) -0.001(2) 0.003(3) -0.014(3) C(20) 0.044(3) 0.070(4) 0.055(4) 0.004(3) 0.008(3) -0.014(3) C(21) 0.077(4) 0.082(5) 0.076(5) -0.013(4) 0.021(4) -0.032(4) C(22) 0.096(6) 0.135(7) 0.092(6) -0.006(5) 0.031(5) -0.048(5) C(23) 0.093(5) 0.129(7) 0.079(6) -0.028(5) 0.035(4) -0.020(5) C(24) 0.064(4) 0.095(5) 0.062(4) -0.015(3) 0.024(3) -0.014(4) C(25) 0.038(3) 0.072(4) 0.064(4) 0.004(3) 0.004(3) -0.011(3) C(26) 0.038(3) 0.046(3) 0.060(4) -0.007(2) -0.003(3) 0.003(3) C(27) 0.029(3) 0.031(3) 0.055(4) 0.001(2) -0.001(2) 0.004(2) _computing_data_collection CRYSTALCLEAR _computing_cell_refinement CRYSTALCLEAR _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl(1a) C(28a) 1.651(9) . . yes Cl(1b) H(28b) 0.779 . . no Cl(1b) C(28b) 1.72(2) . . yes Cl(1c) C(29b) 1.64(3) . . yes Cl(2a) Cl(2c) 1.73(2) . . yes Cl(2a) C(34a) 1.778(9) . . yes Cl(2b) C(34b) 1.58(2) . . yes Cl(2c) C(34a) 1.95(2) . . yes Cl(2c) C(39a) 1.83(1) . . yes Cl(2c) H(39a) 1.379 . . no O(1) H(1O) 0.995 . . no O(1) C(40) 1.44(1) . . yes N(1) C(1) 1.367(5) . . yes N(1) C(4) 1.377(5) . . yes N(1) H(1N) 0.860 . . no C(1) C(2) 1.441(5) . . yes C(1) C(5) 1.390(6) . 7_455 yes C(2) C(3) 1.347(6) . . yes C(2) C(17) 1.512(6) . . yes C(3) C(4) 1.441(6) . . yes C(3) C(6) 1.507(5) . . yes C(4) C(5) 1.372(6) . . yes C(5) H(5) 0.930 . . no C(6) C(7) 1.520(6) . . yes C(6) C(27) 1.519(7) . . yes C(6) H(6) 0.980 . . no C(7) C(8) 1.355(7) . . yes C(7) C(16) 1.416(6) . . yes C(8) C(9) 1.436(7) . . yes C(8) H(8) 0.930 . . no C(9) C(10) 1.392(8) . . yes C(9) C(14) 1.408(8) . . yes C(10) C(11) 1.378(10) . . yes C(10) H(10) 0.930 . . no C(11) C(12) 1.38(1) . . yes C(11) H(11) 0.930 . . no C(12) C(13) 1.374(9) . . yes C(12) H(12) 0.930 . . no C(13) C(14) 1.424(8) . . yes C(13) H(13) 0.930 . . no C(14) C(15) 1.427(7) . . yes C(15) C(16) 1.362(7) . . yes C(15) H(15) 0.930 . . no C(16) C(17) 1.522(7) . . yes C(17) C(18) 1.535(7) . . yes C(17) H(17) 0.980 . . no C(18) C(19) 1.359(7) . . yes C(18) C(27) 1.434(6) . . yes C(19) C(20) 1.408(7) . . yes C(19) H(19) 0.930 . . no C(20) C(21) 1.407(9) . . yes C(20) C(25) 1.431(8) . . yes C(21) C(22) 1.36(1) . . yes C(21) H(21) 0.930 . . no C(22) C(23) 1.42(1) . . yes C(22) H(22) 0.930 . . no C(23) C(24) 1.359(10) . . yes C(23) H(23) 0.930 . . no C(24) C(25) 1.407(8) . . yes C(24) H(24) 0.930 . . no C(25) C(26) 1.419(8) . . yes C(26) C(27) 1.364(7) . . yes C(26) H(26) 0.930 . . no H(28b) C(28a) 1.013 . 2_655 no H(28b) C(28b) 0.950 . . no H(40) C(40) 0.980 . . no H(41a) C(41) 0.961 . . no H(41b) C(41) 0.959 . . no H(41c) C(41) 0.960 . . no H(42a) C(42) 0.961 . . no H(42b) C(42) 0.961 . . no H(42c) C(42) 0.959 . . no C(28a) C(33a) 1.395(10) . . yes C(28a) C(29a) 1.395(10) . . yes C(33a) C(32a) 1.39(1) . . yes C(33a) H(33a) 0.950 . . no C(32a) C(31a) 1.39(1) . . yes C(32a) H(32a) 0.950 . . no C(31a) C(30a) 1.39(1) . . yes C(31a) H(31a) 0.950 . . no C(30a) C(29a) 1.39(1) . . yes C(30a) H(30a) 0.950 . . no C(29a) H(29a) 0.950 . . no C(28b) C(29b) 1.39(2) . . yes C(28b) C(33b) 1.39(2) . . yes C(29b) C(30b) 1.39(2) . . yes C(29b) H(29b) 0.950 . . no C(30b) C(31b) 1.39(2) . . yes C(30b) H(30b) 0.950 . . no C(31b) C(32b) 1.39(2) . . yes C(31b) H(31b) 0.950 . . no C(32b) C(33b) 1.39(2) . . yes C(32b) H(32b) 0.950 . . no C(33b) H(33b) 0.950 . . no C(34a) C(35a) 1.39(1) . . yes C(34a) C(39a) 1.39(1) . . yes C(35a) C(36a) 1.39(1) . . yes C(35a) H(35a) 0.950 . . no C(36a) C(37a) 1.39(1) . . yes C(36a) H(36a) 0.950 . . no C(37a) C(38a) 1.39(1) . . yes C(37a) H(37a) 0.950 . . no C(38a) C(39a) 1.39(1) . . yes C(38a) H(38a) 0.950 . . no C(39a) H(39a) 0.950 . . no C(34b) C(35b) 1.39(2) . . yes C(34b) C(39b) 1.39(2) . . yes C(35b) C(36b) 1.39(2) . . yes C(35b) H(35b) 0.940 . . no C(36b) C(37b) 1.39(2) . . yes C(36b) H(36b) 0.950 . . no C(37b) C(38b) 1.39(2) . . yes C(37b) H(37b) 0.950 . . no C(38b) C(39b) 1.39(2) . . yes C(38b) H(38b) 0.950 . . no C(39b) H(39b) 0.950 . . no C(40) C(42) 1.54(2) . . yes C(40) C(41) 1.54(2) . . yes 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag H(1O) O(1) C(40) 109.5 . . . no C(1) N(1) C(4) 108.6(3) . . . yes C(1) N(1) H(1N) 125.7 . . . no C(4) N(1) H(1N) 125.7 . . . no N(1) C(1) C(2) 108.1(3) . . . yes N(1) C(1) C(5) 125.1(3) . . 7_455 yes C(2) C(1) C(5) 126.7(4) . . 7_455 yes C(1) C(2) C(3) 107.6(3) . . . yes C(1) C(2) C(17) 137.5(4) . . . yes C(3) C(2) C(17) 114.8(3) . . . yes C(2) C(3) C(4) 108.0(3) . . . yes C(2) C(3) C(6) 114.9(3) . . . yes C(4) C(3) C(6) 137.0(4) . . . yes N(1) C(4) C(3) 107.6(3) . . . yes N(1) C(4) C(5) 125.7(3) . . . yes C(3) C(4) C(5) 126.7(4) . . . yes C(1) C(5) C(4) 127.8(4) 8_555 . . yes C(1) C(5) H(5) 112.2 8_555 . . no C(4) C(5) H(5) 120.0 . . . no C(3) C(6) C(7) 105.1(3) . . . yes C(3) C(6) C(27) 105.0(4) . . . yes C(3) C(6) H(6) 113.5 . . . no C(7) C(6) C(27) 105.4(3) . . . yes C(7) C(6) H(6) 113.5 . . . no C(27) C(6) H(6) 113.5 . . . no C(6) C(7) C(8) 125.8(4) . . . yes C(6) C(7) C(16) 113.5(4) . . . yes C(8) C(7) C(16) 120.7(4) . . . yes C(7) C(8) C(9) 120.2(4) . . . yes C(7) C(8) H(8) 119.9 . . . no C(9) C(8) H(8) 119.9 . . . no C(8) C(9) C(10) 122.4(5) . . . yes C(8) C(9) C(14) 118.4(5) . . . yes C(10) C(9) C(14) 119.2(5) . . . yes C(9) C(10) C(11) 121.0(6) . . . yes C(9) C(10) H(10) 119.5 . . . no C(11) C(10) H(10) 119.5 . . . no C(10) C(11) C(12) 120.5(6) . . . yes C(10) C(11) H(11) 119.8 . . . no C(12) C(11) H(11) 119.8 . . . no C(11) C(12) C(13) 120.1(7) . . . yes C(11) C(12) H(12) 120.0 . . . no C(13) C(12) H(12) 119.9 . . . no C(12) C(13) C(14) 120.4(6) . . . yes C(12) C(13) H(13) 119.8 . . . no C(14) C(13) H(13) 119.8 . . . no C(9) C(14) C(13) 118.8(5) . . . yes C(9) C(14) C(15) 120.4(5) . . . yes C(13) C(14) C(15) 120.8(5) . . . yes C(14) C(15) C(16) 118.9(4) . . . yes C(14) C(15) H(15) 120.5 . . . no C(16) C(15) H(15) 120.6 . . . no C(7) C(16) C(15) 121.3(4) . . . yes C(7) C(16) C(17) 112.9(4) . . . yes C(15) C(16) C(17) 125.8(4) . . . yes C(2) C(17) C(16) 106.0(4) . . . yes C(2) C(17) C(18) 104.7(4) . . . yes C(2) C(17) H(17) 113.7 . . . no C(16) C(17) C(18) 104.0(3) . . . yes C(16) C(17) H(17) 113.7 . . . no C(18) C(17) H(17) 113.7 . . . no C(17) C(18) C(19) 126.3(4) . . . yes C(17) C(18) C(27) 112.9(4) . . . yes C(19) C(18) C(27) 120.8(4) . . . yes C(18) C(19) C(20) 121.0(4) . . . yes C(18) C(19) H(19) 119.5 . . . no C(20) C(19) H(19) 119.5 . . . no C(19) C(20) C(21) 122.0(5) . . . yes C(19) C(20) C(25) 118.9(5) . . . yes C(21) C(20) C(25) 119.1(5) . . . yes C(20) C(21) C(22) 119.8(6) . . . yes C(20) C(21) H(21) 120.1 . . . no C(22) C(21) H(21) 120.1 . . . no C(21) C(22) C(23) 121.3(7) . . . yes C(21) C(22) H(22) 119.3 . . . no C(23) C(22) H(22) 119.4 . . . no C(22) C(23) C(24) 119.9(7) . . . yes C(22) C(23) H(23) 120.0 . . . no C(24) C(23) H(23) 120.0 . . . no C(23) C(24) C(25) 120.4(6) . . . yes C(23) C(24) H(24) 119.8 . . . no C(25) C(24) H(24) 119.8 . . . no C(20) C(25) C(24) 119.5(5) . . . yes C(20) C(25) C(26) 118.7(5) . . . yes C(24) C(25) C(26) 121.8(5) . . . yes C(25) C(26) C(27) 121.4(4) . . . yes C(25) C(26) H(26) 119.3 . . . no C(27) C(26) H(26) 119.3 . . . no C(6) C(27) C(18) 112.6(4) . . . yes C(6) C(27) C(26) 128.3(4) . . . yes C(18) C(27) C(26) 119.1(4) . . . yes Cl(1b) H(28b) C(28b) 166.1 . . . no Cl(1a) C(28a) C(33a) 121.1(6) . . . yes Cl(1a) C(28a) C(29a) 118.9(6) . . . yes C(33a) C(28a) C(29a) 120.0(7) . . . yes C(28a) C(33a) C(32a) 120.0(6) . . . yes C(28a) C(33a) H(33a) 120.0 . . . no C(32a) C(33a) H(33a) 120.0 . . . no C(33a) C(32a) C(31a) 120.0(6) . . . yes C(33a) C(32a) H(32a) 120.0 . . . no C(31a) C(32a) H(32a) 120.0 . . . no C(32a) C(31a) C(30a) 120.0(7) . . . yes C(32a) C(31a) H(31a) 120.0 . . . no C(30a) C(31a) H(31a) 120.0 . . . no C(31a) C(30a) C(29a) 120.0(6) . . . yes C(31a) C(30a) H(30a) 120.0 . . . no C(29a) C(30a) H(30a) 120.0 . . . no C(28a) C(29a) C(30a) 120.0(6) . . . yes C(28a) C(29a) H(29a) 120.0 . . . no C(30a) C(29a) H(29a) 120.0 . . . no Cl(1b) C(28b) C(29b) 121(1) . . . yes Cl(1b) C(28b) C(33b) 117(1) . . . yes H(28b) C(28b) C(29b) 119.9 . . . no H(28b) C(28b) C(33b) 120.1 . . . no C(29b) C(28b) C(33b) 119(1) . . . yes Cl(1c) C(29b) C(28b) 122(1) . . . yes Cl(1c) C(29b) C(30b) 116(1) . . . yes C(28b) C(29b) C(30b) 120(1) . . . yes C(28b) C(29b) H(29b) 120.0 . . . no C(30b) C(29b) H(29b) 120.0 . . . no C(29b) C(30b) C(31b) 119(1) . . . yes C(29b) C(30b) H(30b) 120.0 . . . no C(31b) C(30b) H(30b) 120.0 . . . no C(30b) C(31b) C(32b) 120(1) . . . yes C(30b) C(31b) H(31b) 120.0 . . . no C(32b) C(31b) H(31b) 120.0 . . . no C(31b) C(32b) C(33b) 120.0(10) . . . yes C(31b) C(32b) H(32b) 120.0 . . . no C(33b) C(32b) H(32b) 120.0 . . . no C(28b) C(33b) C(32b) 120(1) . . . yes C(28b) C(33b) H(33b) 120.0 . . . no C(32b) C(33b) H(33b) 120.0 . . . no Cl(1c) H(29b) C(29b) 156.9 . . . no Cl(2a) C(34a) Cl(2c) 55.0(6) . . . yes Cl(2a) C(34a) C(35a) 121.2(6) . . . yes Cl(2a) C(34a) C(39a) 118.8(6) . . . yes Cl(2c) C(34a) C(35a) 174.6(7) . . . yes Cl(2c) C(34a) C(39a) 64.0(7) . . . yes C(35a) C(34a) C(39a) 120.0(6) . . . yes C(34a) C(35a) C(36a) 120.0(7) . . . yes C(34a) C(35a) H(35a) 120.0 . . . no C(36a) C(35a) H(35a) 120.0 . . . no C(35a) C(36a) C(37a) 120.0(7) . . . yes C(35a) C(36a) H(36a) 120.0 . . . no C(37a) C(36a) H(36a) 120.0 . . . no C(36a) C(37a) C(38a) 120.0(6) . . . yes C(36a) C(37a) H(37a) 120.0 . . . no C(38a) C(37a) H(37a) 120.0 . . . no C(37a) C(38a) C(39a) 120.0(7) . . . yes C(37a) C(38a) H(38a) 120.0 . . . no C(39a) C(38a) H(38a) 120.0 . . . no Cl(2c) C(39a) C(34a) 72.8(7) . . . yes Cl(2c) C(39a) C(38a) 166.7(9) . . . yes Cl(2c) C(39a) H(39a) 47.3 . . . no C(34a) C(39a) C(38a) 120.0(7) . . . yes C(34a) C(39a) H(39a) 120.0 . . . no C(38a) C(39a) H(39a) 120.0 . . . no Cl(2c) H(39a) C(39a) 102.2 . . . no Cl(2b) C(34b) C(35b) 105(1) . . . yes Cl(2b) C(34b) C(39b) 133(1) . . . yes C(35b) C(34b) C(39b) 120(1) . . . yes C(34b) C(35b) C(36b) 119(1) . . . yes C(34b) C(35b) H(35b) 120.0 . . . no C(36b) C(35b) H(35b) 120.0 . . . no C(35b) C(36b) C(37b) 120(1) . . . yes C(35b) C(36b) H(36b) 120.0 . . . no C(37b) C(36b) H(36b) 120.0 . . . no C(36b) C(37b) C(38b) 119(1) . . . yes C(36b) C(37b) H(37b) 120.0 . . . no C(38b) C(37b) H(37b) 120.0 . . . no C(37b) C(38b) C(39b) 120(1) . . . yes C(37b) C(38b) H(38b) 120.0 . . . no C(39b) C(38b) H(38b) 120.0 . . . no C(34b) C(39b) C(38b) 119(1) . . . yes C(34b) C(39b) H(39b) 120.0 . . . no C(38b) C(39b) H(39b) 120.0 . . . no O(1) C(40) H(40) 111.6 . . . no O(1) C(40) C(42) 106.7(9) . . . yes O(1) C(40) C(41) 105.5(9) . . . yes H(40) C(40) C(42) 111.5 . . . no H(40) C(40) C(41) 111.7 . . . no C(42) C(40) C(41) 109.5(9) . . . yes H(42a) C(42) H(42b) 109.3 . . . no H(42a) C(42) H(42c) 109.4 . . . no H(42a) C(42) C(40) 109.5 . . . no H(42b) C(42) H(42c) 109.5 . . . no H(42b) C(42) C(40) 109.5 . . . no H(42c) C(42) C(40) 109.6 . . . no H(41a) C(41) H(41b) 109.5 . . . no H(41a) C(41) H(41c) 109.5 . . . no H(41a) C(41) C(40) 109.4 . . . no H(41b) C(41) H(41c) 109.6 . . . no H(41b) C(41) C(40) 109.5 . . . no H(41c) C(41) C(40) 109.5 . . . no 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 Cl(1a) C(28a) C(33a) C(32a) 179.3(7) . . . . yes Cl(1a) C(28a) C(29a) C(30a) -179.3(7) . . . . yes Cl(1b) C(28b) C(29b) C(30b) -173(1) . . . . yes Cl(1b) C(28b) C(33b) C(32b) 173(1) . . . . yes Cl(1c) C(29b) C(28b) C(33b) -168(1) . . . . yes Cl(1c) C(29b) C(30b) C(31b) 169(1) . . . . yes Cl(2a) C(34a) C(35a) C(36a) 178.1(6) . . . . yes Cl(2a) C(34a) C(39a) Cl(2c) 5.8(8) . . . . yes Cl(2a) C(34a) C(39a) C(38a) -178.2(7) . . . . yes Cl(2b) C(34b) C(35b) C(36b) -168(1) . . . . yes Cl(2b) C(34b) C(39b) C(38b) 164(1) . . . . yes Cl(2c) Cl(2a) C(34a) C(35a) 175.4(10) . . . . yes Cl(2c) Cl(2a) C(34a) C(39a) -6.4(9) . . . . yes Cl(2c) C(34a) C(39a) C(38a) 176(1) . . . . yes Cl(2c) C(39a) C(34a) C(35a) -176.0(10) . . . . yes Cl(2c) C(39a) C(38a) C(37a) 163(3) . . . . yes N(1) C(1) C(2) C(3) -1.0(5) . . . . yes N(1) C(1) C(2) C(17) -179.0(5) . . . . yes N(1) C(4) C(3) C(2) 1.3(5) . . . . yes N(1) C(4) C(3) C(6) 177.9(5) . . . . yes N(1) C(4) C(5) C(1) -0.5(8) . . . 8_555 yes C(1) N(1) C(4) C(3) -2.0(5) . . . . yes C(1) N(1) C(4) C(5) 178.2(5) . . . . yes C(1) C(2) C(3) C(4) -0.2(5) . . . . yes C(1) C(2) C(3) C(6) -177.7(4) . . . . yes C(1) C(2) C(17) C(16) -128.3(6) . . . . yes C(1) C(2) C(17) C(18) 122.1(6) . . . . yes C(2) C(1) N(1) C(4) 1.8(5) . . . . yes C(2) C(3) C(4) C(5) -178.8(5) . . . . yes C(2) C(3) C(6) C(7) -55.3(5) . . . . yes C(2) C(3) C(6) C(27) 55.6(5) . . . . yes C(2) C(17) C(16) C(7) -52.4(5) . . . . yes C(2) C(17) C(16) C(15) 129.8(5) . . . . yes C(2) C(17) C(18) C(19) -127.8(5) . . . . yes C(2) C(17) C(18) C(27) 53.4(5) . . . . yes C(3) C(2) C(1) C(5) -177.2(5) . . . 7_455 yes C(3) C(2) C(17) C(16) 53.8(5) . . . . yes C(3) C(2) C(17) C(18) -55.8(5) . . . . yes C(3) C(6) C(7) C(8) -126.2(5) . . . . yes C(3) C(6) C(7) C(16) 54.7(5) . . . . yes C(3) C(6) C(27) C(18) -55.3(5) . . . . yes C(3) C(6) C(27) C(26) 126.0(5) . . . . yes C(4) N(1) C(1) C(5) 178.1(4) . . . 7_455 yes C(4) C(3) C(2) C(17) 178.3(4) . . . . yes C(4) C(3) C(6) C(7) 128.3(6) . . . . yes C(4) C(3) C(6) C(27) -120.8(6) . . . . yes C(5) C(4) C(3) C(6) -2.2(9) . . . . yes C(6) C(3) C(2) C(17) 0.8(6) . . . . yes C(6) C(7) C(8) C(9) -178.7(4) . . . . yes C(6) C(7) C(16) C(15) 176.5(4) . . . . yes C(6) C(7) C(16) C(17) -1.4(5) . . . . yes C(6) C(27) C(18) C(17) 1.3(5) . . . . yes C(6) C(27) C(18) C(19) -177.6(4) . . . . yes C(6) C(27) C(26) C(25) 178.6(4) . . . . yes C(7) C(6) C(27) C(18) 55.3(4) . . . . yes C(7) C(6) C(27) C(26) -123.3(5) . . . . yes C(7) C(8) C(9) C(10) -178.1(5) . . . . yes C(7) C(8) C(9) C(14) 2.4(7) . . . . yes C(7) C(16) C(15) C(14) 2.0(7) . . . . yes C(7) C(16) C(17) C(18) 57.7(4) . . . . yes C(8) C(7) C(6) C(27) 123.2(5) . . . . yes C(8) C(7) C(16) C(15) -2.6(7) . . . . yes C(8) C(7) C(16) C(17) 179.5(4) . . . . yes C(8) C(9) C(10) C(11) 179.4(5) . . . . yes C(8) C(9) C(14) C(13) 178.2(5) . . . . yes C(8) C(9) C(14) C(15) -2.9(7) . . . . yes C(9) C(8) C(7) C(16) 0.3(7) . . . . yes C(9) C(10) C(11) C(12) 2.4(9) . . . . yes C(9) C(14) C(13) C(12) 2.5(8) . . . . yes C(9) C(14) C(15) C(16) 0.7(7) . . . . yes C(10) C(9) C(14) C(13) -1.4(7) . . . . yes C(10) C(9) C(14) C(15) 177.5(5) . . . . yes C(10) C(11) C(12) C(13) -1.3(10) . . . . yes C(11) C(10) C(9) C(14) -1.0(8) . . . . yes C(11) C(12) C(13) C(14) -1.2(9) . . . . yes C(12) C(13) C(14) C(15) -176.4(5) . . . . yes C(13) C(14) C(15) C(16) 179.6(5) . . . . yes C(14) C(15) C(16) C(17) 179.7(4) . . . . yes C(15) C(16) C(17) C(18) -120.1(5) . . . . yes C(16) C(7) C(6) C(27) -55.9(4) . . . . yes C(16) C(17) C(18) C(19) 121.1(5) . . . . yes C(16) C(17) C(18) C(27) -57.7(4) . . . . yes C(17) C(18) C(19) C(20) -179.6(4) . . . . yes C(17) C(18) C(27) C(26) -179.9(4) . . . . yes C(18) C(19) C(20) C(21) 178.7(5) . . . . yes C(18) C(19) C(20) C(25) -0.6(7) . . . . yes C(18) C(27) C(26) C(25) 0.0(7) . . . . yes C(19) C(18) C(27) C(26) 1.2(7) . . . . yes C(19) C(20) C(21) C(22) -178.5(6) . . . . yes C(19) C(20) C(25) C(24) 178.7(5) . . . . yes C(19) C(20) C(25) C(26) 1.8(7) . . . . yes C(20) C(19) C(18) C(27) -0.9(7) . . . . yes C(20) C(21) C(22) C(23) -1(1) . . . . yes C(20) C(25) C(24) C(23) 0.9(8) . . . . yes C(20) C(25) C(26) C(27) -1.5(7) . . . . yes C(21) C(20) C(25) C(24) -0.6(8) . . . . yes C(21) C(20) C(25) C(26) -177.6(5) . . . . yes C(21) C(22) C(23) C(24) 1(1) . . . . yes C(22) C(21) C(20) C(25) 0.8(9) . . . . yes C(22) C(23) C(24) C(25) -1.2(10) . . . . yes C(23) C(24) C(25) C(26) 177.7(6) . . . . yes C(24) C(25) C(26) C(27) -178.3(5) . . . . yes C(28a) C(33a) C(32a) C(31a) 0(1) . . . . yes C(28a) C(29a) C(30a) C(31a) 0(1) . . . . yes C(33a) C(28a) C(29a) C(30a) 0(1) . . . . yes C(33a) C(32a) C(31a) C(30a) 0(1) . . . . yes C(32a) C(33a) C(28a) C(29a) 0(1) . . . . yes C(32a) C(31a) C(30a) C(29a) 0(1) . . . . yes C(28b) C(29b) C(30b) C(31b) 0(2) . . . . yes C(29b) C(30b) C(31b) C(32b) 0(2) . . . . yes C(30b) C(31b) C(32b) C(33b) 0(1) . . . . yes C(34a) Cl(2a) Cl(2c) C(39a) 4.3(6) . . . . yes C(34a) Cl(2c) C(39a) C(38a) -164(3) . . . . yes C(34a) C(35a) C(36a) C(37a) 0(1) . . . . yes C(34a) C(39a) C(38a) C(37a) 0(1) . . . . yes C(35a) C(34a) C(39a) C(38a) 0(1) . . . . yes C(35a) C(36a) C(37a) C(38a) 0(1) . . . . yes C(36a) C(35a) C(34a) C(39a) 0(1) . . . . yes C(36a) C(37a) C(38a) C(39a) 0(1) . . . . yes C(34b) C(35b) C(36b) C(37b) 0(2) . . . . yes C(34b) C(39b) C(38b) C(37b) 0(2) . . . . yes C(35b) C(34b) C(39b) C(38b) 0(2) . . . . yes C(35b) C(36b) C(37b) C(38b) 0(2) . . . . yes C(36b) C(35b) C(34b) C(39b) 0(2) . . . . yes C(36b) C(37b) C(38b) C(39b) 0(2) . . . . yes loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cl(1a) C(29a) 2.626(9) . . ? Cl(1a) C(33a) 2.655(10) . . ? Cl(1a) C(29b) 2.93(2) . 2_655 ? Cl(1a) C(32b) 3.57(1) . 2_655 ? Cl(1b) C(33b) 2.67(2) . . ? Cl(1b) C(29b) 2.72(2) . . ? Cl(1b) C(33a) 3.01(2) . 2_655 ? Cl(1b) Cl(2c) 3.17(2) . 11_644 ? Cl(1b) C(37b) 3.47(2) . 12_554 ? Cl(1b) C(36b) 3.55(2) . 12_554 ? Cl(1c) C(30b) 2.58(3) . . ? Cl(1c) C(28b) 2.66(3) . . ? Cl(1c) C(28a) 2.77(3) . 2_655 ? Cl(1c) C(31a) 3.06(3) . 2_655 ? Cl(1c) Cl(2a) 3.58(3) . 11_644 ? Cl(1c) C(22) 3.58(3) . . ? Cl(2a) C(39a) 2.74(1) . . ? Cl(2a) C(35a) 2.771(10) . . ? Cl(2a) C(34b) 3.01(2) . 2_655 ? Cl(2a) C(38b) 3.37(2) . 2_655 ? Cl(2a) C(42) 3.48(1) . 7_465 ? Cl(2b) C(37a) 2.71(1) . 2_655 ? Cl(2b) C(39b) 2.73(2) . . ? Cl(2b) C(34a) 2.77(1) . 2_655 ? Cl(2b) C(5) 3.252(9) . 2_655 ? Cl(2b) C(13) 3.548(10) . 14_555 ? Cl(2b) C(12) 3.599(9) . 14_555 ? Cl(2c) C(35b) 2.51(2) . 2_655 ? Cl(2c) C(38a) 3.21(1) . . ? Cl(2c) C(39b) 3.21(2) . 2_655 ? Cl(2c) C(34b) 3.28(2) . 2_655 ? Cl(2c) C(26) 3.29(2) . 3_555 ? Cl(2c) C(35a) 3.34(2) . . ? O(1) O(1) 2.704(6) . 7_465 ? O(1) O(1) 2.704(6) . 8_655 ? N(1) N(1) 2.924(4) . 8_555 ? N(1) C(1) 3.028(5) . 8_555 ? C(1) C(38a) 3.461(9) . 13_555 ? C(1) C(38b) 3.50(2) . 14_455 ? C(2) C(38a) 3.542(9) . 13_555 ? C(5) C(17) 3.390(6) . 8_555 ? C(5) C(38b) 3.43(2) . 11_544 ? C(8) C(37a) 3.505(9) . . ? C(9) C(36a) 3.567(9) . 13_555 ? C(10) C(10) 3.52(1) . 2_655 ? C(10) C(37a) 3.522(9) . . ? C(10) C(38a) 3.58(1) . . ? C(12) C(37b) 3.50(2) . . ? C(14) C(36a) 3.366(9) . 13_555 ? C(20) C(30a) 3.529(9) . 2_655 ? C(25) C(30a) 3.512(9) . 2_655 ? C(37a) C(37a) 3.45(1) . 13_555 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_site_distance_DH _geom_hbond_site_distance_HA _geom_hbond_site_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag N(1) H(1N) N(1) . . 8_555 0.860 2.400 2.924(4) 119.820 no N(1) H(1N) N(1) . . 7_455 0.860 2.391 2.924(4) 120.626 no #============================================================================== data___13-12PhH _database_code_depnum_ccdc_archive 'CCDC 248911' #============================================================================== _chemical_formula_sum 'C180 H132 N4 Zn ' _chemical_formula_moiety 'C108 H60 N4 Zn, 12(C6 H6)' _chemical_formula_weight 2416.29 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 41/a' _symmetry_space_group_name_Hall '-I 4ad' _symmetry_Int_Tables_number 88 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 'x, y, z' 2 '-y+3/4, x+1/4, z+1/4' 3 '-x+1/2, -y, z+1/2' 4 'y+3/4, -x+3/4, z+3/4' 5 'x+1/2, y+1/2, z+1/2' 6 '-y+5/4, x+3/4, z+3/4' 7 '-x+1, -y+1/2, z+1' 8 'y+5/4, -x+5/4, z+5/4' 9 '-x, -y, -z' 10 'y-3/4, -x-1/4, -z-1/4' 11 'x-1/2, y, -z-1/2' 12 '-y-3/4, x-3/4, -z-3/4' 13 '-x+1/2, -y+1/2, -z+1/2' 14 'y-1/4, -x+1/4, -z+1/4' 15 'x, y+1/2, -z' 16 '-y-1/4, x-1/4, -z-1/4' _cell_length_a 19.612(3) _cell_length_b 19.612(2) _cell_length_c 36.445(8) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 14018(4) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 17988 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description Prism _exptl_crystal_colour red _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.25 _exptl_crystal_density_diffrn 1.145 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5080 _exptl_absorpt_coefficient_mu 0.231 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Higashi, T. (1999). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.8835 _exptl_absorpt_correction_T_max 0.9445 _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoKa _diffrn_radiation_source '6 kW rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CCD _diffrn_measurement_method w _diffrn_reflns_number 16256 _diffrn_reflns_av_R_equivalents 0.0600 _diffrn_reflns_av_sigmaI/netI 0.0825 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 27.49 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.993 _reflns_number_total 7994 _reflns_number_gt 4242 _reflns_threshold_expression >2sigma(I) _computing_data_collection CRYSTALCLEAR _computing_cell_refinement CRYSTALCLEAR _computing_data_reduction CrystalStructure _computing_structure_solution 'DIRDIF99 (ORIENT)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'CrystalStructure 3.6.0' _computing_molecular_graphics ? _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^)+(0.0650P)^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 noref _refine_ls_number_reflns 7994 _refine_ls_number_parameters 418 _refine_ls_number_restraints 453 _refine_ls_R_factor_all 0.1355 _refine_ls_R_factor_gt 0.0592 _refine_ls_wR_factor_ref 0.1589 _refine_ls_wR_factor_gt 0.1342 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 0.998 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.829 _refine_diff_density_min -0.250 _refine_diff_density_rms 0.042 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 Zn1 Zn 0.0000 0.2500 0.1250 0.04135(16) Uani 1 4 d SU . . N1 N 0.09983(8) 0.27865(8) 0.12558(5) 0.0429(4) Uani 1 1 d U . . C1 C 0.15571(10) 0.23562(10) 0.12639(7) 0.0422(5) Uani 1 1 d U . . C2 C 0.21686(10) 0.27604(10) 0.12616(7) 0.0453(5) Uani 1 1 d U . . C3 C 0.19830(10) 0.34232(10) 0.12507(7) 0.0457(5) Uani 1 1 d U . . C4 C 0.12507(10) 0.34468(10) 0.12457(7) 0.0427(5) Uani 1 1 d U . . C5 C 0.08509(10) 0.40290(10) 0.12327(6) 0.0425(5) Uani 1 1 d U . . H1 H 0.1080 0.4444 0.1220 0.051 Uiso 1 1 calc R . . C6 C 0.29298(10) 0.26336(11) 0.12514(7) 0.0469(5) Uani 1 1 d U . . H2 H 0.3053 0.2150 0.1258 0.056 Uiso 1 1 calc R . . C7 C 0.32166(11) 0.30461(12) 0.15731(7) 0.0498(6) Uani 1 1 d U . . C8 C 0.36127(12) 0.28056(14) 0.18508(8) 0.0612(7) Uani 1 1 d U . . H3 H 0.3731 0.2347 0.1858 0.073 Uiso 1 1 calc R . . C9 C 0.38465(14) 0.32537(16) 0.21311(8) 0.0701(8) Uani 1 1 d U . . C10 C 0.42330(17) 0.3015(2) 0.24365(10) 0.0982(11) Uani 1 1 d U . . H4 H 0.4341 0.2555 0.2455 0.118 Uiso 1 1 calc R . . C11 C 0.4444(2) 0.3456(3) 0.27001(11) 0.1269(16) Uani 1 1 d U . . H5 H 0.4693 0.3294 0.2899 0.152 Uiso 1 1 calc R . . C12 C 0.4292(2) 0.4148(3) 0.26770(12) 0.1330(17) Uani 1 1 d U . . H6 H 0.4445 0.4445 0.2858 0.160 Uiso 1 1 calc R . . C13 C 0.39221(18) 0.4393(2) 0.23904(10) 0.1030(12) Uani 1 1 d U . . H7 H 0.3824 0.4856 0.2379 0.124 Uiso 1 1 calc R . . C14 C 0.36830(14) 0.39553(16) 0.21095(8) 0.0711(8) Uani 1 1 d U . . C15 C 0.32632(13) 0.41907(14) 0.18188(8) 0.0627(7) Uani 1 1 d U . . H8 H 0.3148 0.4650 0.1805 0.075 Uiso 1 1 calc R . . C16 C 0.30273(11) 0.37498(12) 0.15602(7) 0.0496(6) Uani 1 1 d U . . C17 C 0.25708(10) 0.39238(10) 0.12332(7) 0.0475(5) Uani 1 1 d U . . H9 H 0.2427 0.4402 0.1226 0.057 Uiso 1 1 calc R . . C18 C 0.29824(11) 0.37045(11) 0.08977(7) 0.0479(6) Uani 1 1 d U . . C19 C 0.31709(12) 0.41068(13) 0.06132(7) 0.0582(7) Uani 1 1 d U . . H10 H 0.3048 0.4565 0.0611 0.070 Uiso 1 1 calc R . . C20 C 0.35553(13) 0.38329(15) 0.03190(8) 0.0630(7) Uani 1 1 d U . . C21 C 0.37638(16) 0.42370(17) 0.00173(9) 0.0832(9) Uani 1 1 d U . . H11 H 0.3646 0.4696 0.0010 0.100 Uiso 1 1 calc R . . C22 C 0.41340(19) 0.3964(2) -0.02617(10) 0.1024(12) Uani 1 1 d U . . H12 H 0.4270 0.4238 -0.0457 0.123 Uiso 1 1 calc R . . C23 C 0.4310(2) 0.3282(2) -0.02572(10) 0.1036(12) Uani 1 1 d U . . H13 H 0.4560 0.3100 -0.0450 0.124 Uiso 1 1 calc R . . C24 C 0.41199(17) 0.28740(18) 0.00273(9) 0.0853(9) Uani 1 1 d U . . H14 H 0.4245 0.2417 0.0027 0.102 Uiso 1 1 calc R . . C25 C 0.37347(13) 0.31379(15) 0.03231(8) 0.0634(7) Uani 1 1 d U . . C26 C 0.35389(12) 0.27289(13) 0.06265(7) 0.0563(6) Uani 1 1 d U . . H15 H 0.3661 0.2271 0.0633 0.068 Uiso 1 1 calc R . . C27 C 0.31745(11) 0.30019(12) 0.09076(7) 0.0482(6) Uani 1 1 d U . . C28 C 0.2169(4) 0.4154(5) 0.2786(2) 0.200(3) Uani 1 1 d DU . . H16 H 0.2462 0.4197 0.2985 0.240 Uiso 1 1 calc R . . C29 C 0.1741(5) 0.4652(5) 0.2721(3) 0.226(4) Uani 1 1 d DU . . H17 H 0.1745 0.5043 0.2865 0.271 Uiso 1 1 calc R . . C30 C 0.1292(5) 0.4587(6) 0.2439(3) 0.286(5) Uani 1 1 d DU . . H18 H 0.0968 0.4925 0.2397 0.344 Uiso 1 1 calc R . . C31 C 0.1316(7) 0.4031(9) 0.2218(3) 0.344(10) Uani 1 1 d DU . . H19 H 0.1050 0.4004 0.2008 0.413 Uiso 1 1 calc R . . C32 C 0.1741(8) 0.3514(6) 0.2315(4) 0.321(8) Uani 1 1 d DU . . H20 H 0.1711 0.3098 0.2193 0.386 Uiso 1 1 calc R . . C33 C 0.2210(5) 0.3596(5) 0.2587(3) 0.253(5) Uani 1 1 d DU . . H21 H 0.2545 0.3271 0.2631 0.304 Uiso 1 1 calc R . . C34 C 0.3905(4) 0.5891(3) 0.13137(18) 0.190(3) Uani 1 1 d DU . . H22 H 0.3843 0.5811 0.1563 0.228 Uiso 1 1 calc R . . C35 C 0.3699(4) 0.6492(3) 0.11688(19) 0.200(3) Uani 1 1 d DU . . H23 H 0.3511 0.6823 0.1320 0.240 Uiso 1 1 calc R . . C36 C 0.3765(3) 0.6611(3) 0.0814(2) 0.194(3) Uani 1 1 d DU . . H24 H 0.3626 0.7025 0.0714 0.233 Uiso 1 1 calc R . . C37 C 0.4046(4) 0.6106(4) 0.05932(18) 0.174(2) Uani 1 1 d DU . . H25 H 0.4075 0.6166 0.0341 0.209 Uiso 1 1 calc R . . C38 C 0.4275(3) 0.5527(3) 0.0751(2) 0.149(2) Uani 1 1 d DU . . H26 H 0.4495 0.5200 0.0609 0.179 Uiso 1 1 calc R . . C39 C 0.4188(3) 0.5420(3) 0.1111(2) 0.151(2) Uani 1 1 d DU . . H27 H 0.4328 0.5011 0.1216 0.181 Uiso 1 1 calc R . . C40 C 0.5920(6) 0.4079(4) 0.1363(3) 0.279(6) Uani 1 1 d DU . . H28 H 0.6076 0.4136 0.1602 0.335 Uiso 1 1 calc R . . C41 C 0.6312(5) 0.4340(5) 0.1089(5) 0.348(10) Uani 1 1 d DU . . H29 H 0.6718 0.4572 0.1130 0.418 Uiso 1 1 calc R . . C42 C 0.6047(6) 0.4224(4) 0.0746(4) 0.266(6) Uani 1 1 d DU . . H30 H 0.6295 0.4365 0.0542 0.319 Uiso 1 1 calc R . . C43 C 0.5467(6) 0.3928(5) 0.0696(3) 0.201(4) Uani 1 1 d DU . . H31 H 0.5290 0.3885 0.0460 0.242 Uiso 1 1 calc R . . C44 C 0.5129(4) 0.3690(4) 0.0976(3) 0.194(4) Uani 1 1 d DU . . H32 H 0.4719 0.3466 0.0931 0.233 Uiso 1 1 calc R . . C45 C 0.5329(5) 0.3747(4) 0.1317(3) 0.215(3) Uani 1 1 d DU . . H33 H 0.5080 0.3571 0.1512 0.259 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.03290(18) 0.03290(18) 0.0583(3) 0.000 0.000 0.000 N1 0.0333(9) 0.0333(9) 0.0622(11) 0.0022(9) -0.0012(9) -0.0003(7) C1 0.0314(10) 0.0336(10) 0.0615(13) 0.0020(11) -0.0014(11) 0.0008(8) C2 0.0308(10) 0.0352(11) 0.0700(14) -0.0016(12) -0.0002(11) 0.0000(8) C3 0.0307(10) 0.0350(11) 0.0715(15) -0.0012(12) -0.0015(11) -0.0007(8) C4 0.0329(10) 0.0337(10) 0.0615(14) 0.0005(11) -0.0013(11) -0.0025(8) C5 0.0356(10) 0.0301(10) 0.0618(13) 0.0001(11) -0.0017(11) -0.0033(8) C6 0.0313(10) 0.0352(10) 0.0743(14) -0.0041(12) -0.0018(12) 0.0013(8) C7 0.0304(11) 0.0444(13) 0.0746(16) -0.0052(12) 0.0004(11) -0.0012(10) C8 0.0428(14) 0.0576(16) 0.0830(19) -0.0018(14) -0.0092(13) 0.0064(12) C9 0.0519(16) 0.081(2) 0.0771(19) -0.0147(16) -0.0096(14) 0.0085(14) C10 0.088(2) 0.111(3) 0.096(3) -0.012(2) -0.033(2) 0.023(2) C11 0.120(3) 0.161(4) 0.099(3) -0.036(3) -0.050(3) 0.034(3) C12 0.117(3) 0.157(4) 0.125(3) -0.073(3) -0.049(3) 0.034(3) C13 0.093(3) 0.104(3) 0.112(3) -0.050(2) -0.027(2) 0.013(2) C14 0.0528(16) 0.0744(19) 0.086(2) -0.0255(16) -0.0105(14) 0.0030(14) C15 0.0471(14) 0.0542(15) 0.0868(19) -0.0185(14) -0.0011(13) 0.0000(12) C16 0.0282(11) 0.0441(13) 0.0765(17) -0.0079(12) 0.0035(11) -0.0036(9) C17 0.0328(10) 0.0324(10) 0.0772(15) -0.0038(11) 0.0005(12) -0.0023(8) C18 0.0302(11) 0.0417(13) 0.0718(16) -0.0030(11) -0.0001(11) -0.0048(10) C19 0.0429(14) 0.0496(14) 0.0820(18) 0.0025(13) 0.0027(13) -0.0027(11) C20 0.0504(15) 0.0670(17) 0.0716(18) 0.0015(14) 0.0012(13) -0.0081(13) C21 0.078(2) 0.085(2) 0.086(2) 0.0145(18) 0.0093(17) -0.0030(18) C22 0.098(3) 0.121(3) 0.088(3) 0.012(2) 0.026(2) -0.008(2) C23 0.105(3) 0.121(3) 0.085(3) -0.012(2) 0.034(2) 0.003(3) C24 0.082(2) 0.090(2) 0.084(2) -0.0141(18) 0.0187(18) 0.0031(18) C25 0.0485(15) 0.0678(17) 0.0739(18) -0.0085(14) 0.0048(13) -0.0014(13) C26 0.0411(13) 0.0498(14) 0.0779(18) -0.0088(13) 0.0006(12) 0.0010(11) C27 0.0306(11) 0.0423(13) 0.0717(16) -0.0047(11) -0.0031(11) -0.0027(10) C28 0.168(7) 0.215(9) 0.218(8) -0.001(7) 0.020(6) -0.061(6) C29 0.220(11) 0.185(8) 0.272(10) -0.021(7) -0.038(7) -0.056(6) C30 0.201(9) 0.431(15) 0.227(12) 0.062(10) -0.024(8) -0.061(9) C31 0.314(15) 0.60(3) 0.123(7) -0.037(11) 0.017(8) -0.217(15) C32 0.365(19) 0.360(12) 0.239(14) -0.117(11) 0.185(10) -0.243(12) C33 0.219(9) 0.209(8) 0.331(15) -0.034(7) 0.170(8) -0.063(7) C34 0.289(9) 0.118(4) 0.163(5) -0.003(4) 0.040(5) 0.012(5) C35 0.277(8) 0.141(5) 0.181(6) 0.013(4) 0.097(6) 0.054(5) C36 0.224(7) 0.166(6) 0.193(6) 0.054(5) 0.076(6) 0.036(5) C37 0.191(7) 0.177(6) 0.154(5) -0.003(4) 0.047(4) -0.039(5) C38 0.114(4) 0.138(4) 0.196(6) -0.051(4) 0.033(4) -0.040(3) C39 0.141(5) 0.111(4) 0.200(6) -0.019(4) -0.007(4) -0.010(3) C40 0.298(13) 0.133(8) 0.407(11) -0.062(8) -0.235(11) 0.066(7) C41 0.224(9) 0.127(7) 0.69(3) 0.020(13) -0.177(12) -0.058(6) C42 0.199(9) 0.102(7) 0.496(15) 0.070(9) 0.055(10) 0.037(6) C43 0.215(10) 0.150(9) 0.240(8) -0.036(7) -0.036(7) 0.082(7) C44 0.107(5) 0.183(7) 0.293(12) -0.038(9) -0.053(6) 0.018(4) C45 0.205(9) 0.181(8) 0.260(9) -0.008(7) -0.030(6) 0.083(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 Zn1 N1 2.0370(16) 7_454 ? Zn1 N1 2.0370(16) . ? Zn1 N1 2.0370(16) 14 ? Zn1 N1 2.0370(16) 12_666 ? N1 C1 1.383(2) . ? N1 C4 1.387(2) . ? C1 C5 1.388(3) 14 ? C1 C2 1.438(3) . ? C2 C3 1.351(3) . ? C2 C6 1.514(3) . ? C3 C4 1.437(3) . ? C3 C17 1.516(3) . ? C4 C5 1.386(3) . ? C5 C1 1.388(3) 12_666 ? C5 H1 0.9300 . ? C6 C27 1.524(3) . ? C6 C7 1.531(3) . ? C6 H2 0.9800 . ? C7 C8 1.360(3) . ? C7 C16 1.430(3) . ? C8 C9 1.423(4) . ? C8 H3 0.9300 . ? C9 C14 1.415(4) . ? C9 C10 1.426(4) . ? C10 C11 1.357(5) . ? C10 H4 0.9300 . ? C11 C12 1.392(6) . ? C11 H5 0.9300 . ? C12 C13 1.359(5) . ? C12 H6 0.9300 . ? C13 C14 1.415(4) . ? C13 H7 0.9300 . ? C14 C15 1.419(4) . ? C15 C16 1.360(3) . ? C15 H8 0.9300 . ? C16 C17 1.529(3) . ? C17 C18 1.527(3) . ? C17 H9 0.9800 . ? C18 C19 1.354(3) . ? C18 C27 1.429(3) . ? C19 C20 1.417(4) . ? C19 H10 0.9300 . ? C20 C25 1.408(4) . ? C20 C21 1.416(4) . ? C21 C22 1.359(4) . ? C21 H11 0.9300 . ? C22 C23 1.382(5) . ? C22 H12 0.9300 . ? C23 C24 1.361(5) . ? C23 H13 0.9300 . ? C24 C25 1.414(4) . ? C24 H14 0.9300 . ? C25 C26 1.419(4) . ? C26 C27 1.359(3) . ? C26 H15 0.9300 . ? C28 C29 1.309(9) . ? C28 C33 1.314(9) . ? C28 H16 0.9300 . ? C29 C30 1.361(9) . ? C29 H17 0.9300 . ? C30 C31 1.355(12) . ? C30 H18 0.9300 . ? C31 C32 1.358(14) . ? C31 H19 0.9300 . ? C32 C33 1.362(12) . ? C32 H20 0.9300 . ? C33 H21 0.9300 . ? C34 C39 1.308(7) . ? C34 C35 1.352(7) . ? C34 H22 0.9300 . ? C35 C36 1.319(7) . ? C35 H23 0.9300 . ? C36 C37 1.392(7) . ? C36 H24 0.9300 . ? C37 C38 1.350(7) . ? C37 H25 0.9300 . ? C38 C39 1.339(7) . ? C38 H26 0.9300 . ? C39 H27 0.9300 . ? C40 C45 1.341(10) . ? C40 C41 1.359(13) . ? C40 H28 0.9300 . ? C41 C42 1.372(12) . ? C41 H29 0.9300 . ? C42 C43 1.290(9) . ? C42 H30 0.9300 . ? C43 C44 1.306(9) . ? C43 H31 0.9300 . ? C44 C45 1.306(9) . ? C44 H32 0.9300 . ? C45 H33 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 N1 Zn1 N1 178.82(11) 7_454 . ? N1 Zn1 N1 90.006(3) 7_454 14 ? N1 Zn1 N1 90.006(2) . 14 ? N1 Zn1 N1 90.006(3) 7_454 12_666 ? N1 Zn1 N1 90.006(2) . 12_666 ? N1 Zn1 N1 178.82(11) 14 12_666 ? C1 N1 C4 106.70(16) . . ? C1 N1 Zn1 126.40(13) . . ? C4 N1 Zn1 126.89(13) . . ? N1 C1 C5 125.33(18) . 14 ? N1 C1 C2 108.93(16) . . ? C5 C1 C2 125.73(18) 14 . ? C3 C2 C1 107.81(17) . . ? C3 C2 C6 115.04(18) . . ? C1 C2 C6 137.08(18) . . ? C2 C3 C4 107.50(17) . . ? C2 C3 C17 114.82(17) . . ? C4 C3 C17 137.63(18) . . ? C5 C4 N1 124.63(18) . . ? C5 C4 C3 126.32(18) . . ? N1 C4 C3 109.05(17) . . ? C4 C5 C1 126.70(18) . 12_666 ? C4 C5 H1 116.6 . . ? C1 C5 H1 116.6 12_666 . ? C2 C6 C27 104.64(18) . . ? C2 C6 C7 104.87(18) . . ? C27 C6 C7 105.27(17) . . ? C2 C6 H2 113.7 . . ? C27 C6 H2 113.7 . . ? C7 C6 H2 113.7 . . ? C8 C7 C16 120.5(2) . . ? C8 C7 C6 126.6(2) . . ? C16 C7 C6 112.9(2) . . ? C7 C8 C9 120.2(2) . . ? C7 C8 H3 119.9 . . ? C9 C8 H3 119.9 . . ? C14 C9 C8 119.2(3) . . ? C14 C9 C10 118.9(3) . . ? C8 C9 C10 121.9(3) . . ? C11 C10 C9 120.3(4) . . ? C11 C10 H4 119.8 . . ? C9 C10 H4 119.8 . . ? C10 C11 C12 120.9(4) . . ? C10 C11 H5 119.5 . . ? C12 C11 H5 119.5 . . ? C13 C12 C11 120.3(4) . . ? C13 C12 H6 119.9 . . ? C11 C12 H6 119.9 . . ? C12 C13 C14 121.3(4) . . ? C12 C13 H7 119.4 . . ? C14 C13 H7 119.4 . . ? C13 C14 C9 118.3(3) . . ? C13 C14 C15 122.3(3) . . ? C9 C14 C15 119.3(2) . . ? C16 C15 C14 120.5(3) . . ? C16 C15 H8 119.7 . . ? C14 C15 H8 119.7 . . ? C15 C16 C7 120.2(2) . . ? C15 C16 C17 126.7(2) . . ? C7 C16 C17 113.1(2) . . ? C3 C17 C18 104.68(18) . . ? C3 C17 C16 105.54(19) . . ? C18 C17 C16 104.58(17) . . ? C3 C17 H9 113.7 . . ? C18 C17 H9 113.7 . . ? C16 C17 H9 113.7 . . ? C19 C18 C27 120.6(2) . . ? C19 C18 C17 126.4(2) . . ? C27 C18 C17 113.0(2) . . ? C18 C19 C20 120.3(2) . . ? C18 C19 H10 119.9 . . ? C20 C19 H10 119.9 . . ? C25 C20 C21 118.6(3) . . ? C25 C20 C19 119.5(3) . . ? C21 C20 C19 122.0(3) . . ? C22 C21 C20 121.0(3) . . ? C22 C21 H11 119.5 . . ? C20 C21 H11 119.5 . . ? C21 C22 C23 120.3(3) . . ? C21 C22 H12 119.8 . . ? C23 C22 H12 119.8 . . ? C24 C23 C22 120.7(3) . . ? C24 C23 H13 119.7 . . ? C22 C23 H13 119.7 . . ? C23 C24 C25 120.8(3) . . ? C23 C24 H14 119.6 . . ? C25 C24 H14 119.6 . . ? C20 C25 C24 118.7(3) . . ? C20 C25 C26 119.2(2) . . ? C24 C25 C26 122.1(3) . . ? C27 C26 C25 120.5(2) . . ? C27 C26 H15 119.8 . . ? C25 C26 H15 119.8 . . ? C26 C27 C18 120.0(2) . . ? C26 C27 C6 126.8(2) . . ? C18 C27 C6 113.3(2) . . ? C29 C28 C33 124.1(11) . . ? C29 C28 H16 117.9 . . ? C33 C28 H16 117.9 . . ? C28 C29 C30 118.8(10) . . ? C28 C29 H17 120.6 . . ? C30 C29 H17 120.6 . . ? C31 C30 C29 120.1(11) . . ? C31 C30 H18 120.0 . . ? C29 C30 H18 120.0 . . ? C30 C31 C32 118.0(11) . . ? C30 C31 H19 121.0 . . ? C32 C31 H19 121.0 . . ? C31 C32 C33 120.9(11) . . ? C31 C32 H20 119.5 . . ? C33 C32 H20 119.5 . . ? C28 C33 C32 117.3(11) . . ? C28 C33 H21 121.3 . . ? C32 C33 H21 121.3 . . ? C39 C34 C35 121.4(7) . . ? C39 C34 H22 119.3 . . ? C35 C34 H22 119.3 . . ? C36 C35 C34 120.6(6) . . ? C36 C35 H23 119.7 . . ? C34 C35 H23 119.7 . . ? C35 C36 C37 118.6(6) . . ? C35 C36 H24 120.7 . . ? C37 C36 H24 120.7 . . ? C38 C37 C36 119.0(7) . . ? C38 C37 H25 120.5 . . ? C36 C37 H25 120.5 . . ? C39 C38 C37 120.4(6) . . ? C39 C38 H26 119.8 . . ? C37 C38 H26 119.8 . . ? C34 C39 C38 119.9(7) . . ? C34 C39 H27 120.0 . . ? C38 C39 H27 120.0 . . ? C45 C40 C41 125.4(9) . . ? C45 C40 H28 117.3 . . ? C41 C40 H28 117.3 . . ? C40 C41 C42 113.2(9) . . ? C40 C41 H29 123.4 . . ? C42 C41 H29 123.4 . . ? C43 C42 C41 122.5(10) . . ? C43 C42 H30 118.8 . . ? C41 C42 H30 118.8 . . ? C42 C43 C44 119.9(10) . . ? C42 C43 H31 120.1 . . ? C44 C43 H31 120.1 . . ? C43 C44 C45 124.1(9) . . ? C43 C44 H32 117.9 . . ? C45 C44 H32 117.9 . . ? C44 C45 C40 114.8(9) . . ? C44 C45 H33 122.6 . . ? C40 C45 H33 122.6 . . ? 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 N1 Zn1 N1 C1 -1.68(15) 14 . . . ? N1 Zn1 N1 C1 179.5(2) 12_666 . . . ? N1 Zn1 N1 C4 177.1(2) 14 . . . ? N1 Zn1 N1 C4 -1.75(15) 12_666 . . . ? C4 N1 C1 C5 -178.5(2) . . . 14 ? Zn1 N1 C1 C5 0.4(4) . . . 14 ? C4 N1 C1 C2 0.4(3) . . . . ? Zn1 N1 C1 C2 179.39(15) . . . . ? N1 C1 C2 C3 -0.2(3) . . . . ? C5 C1 C2 C3 178.7(2) 14 . . . ? N1 C1 C2 C6 -176.9(3) . . . . ? C5 C1 C2 C6 2.1(5) 14 . . . ? C1 C2 C3 C4 -0.1(3) . . . . ? C6 C2 C3 C4 177.4(2) . . . . ? C1 C2 C3 C17 -177.9(2) . . . . ? C6 C2 C3 C17 -0.4(3) . . . . ? C1 N1 C4 C5 179.5(2) . . . . ? Zn1 N1 C4 C5 0.5(3) . . . . ? C1 N1 C4 C3 -0.5(3) . . . . ? Zn1 N1 C4 C3 -179.42(16) . . . . ? C2 C3 C4 C5 -179.6(2) . . . . ? C17 C3 C4 C5 -2.5(5) . . . . ? C2 C3 C4 N1 0.3(3) . . . . ? C17 C3 C4 N1 177.5(3) . . . . ? N1 C4 C5 C1 1.6(4) . . . 12_666 ? C3 C4 C5 C1 -178.4(3) . . . 12_666 ? C3 C2 C6 C27 -55.0(3) . . . . ? C1 C2 C6 C27 121.5(3) . . . . ? C3 C2 C6 C7 55.5(3) . . . . ? C1 C2 C6 C7 -128.0(3) . . . . ? C2 C6 C7 C8 125.3(2) . . . . ? C27 C6 C7 C8 -124.6(3) . . . . ? C2 C6 C7 C16 -54.7(2) . . . . ? C27 C6 C7 C16 55.3(2) . . . . ? C16 C7 C8 C9 -0.3(4) . . . . ? C6 C7 C8 C9 179.6(2) . . . . ? C7 C8 C9 C14 -2.3(4) . . . . ? C7 C8 C9 C10 176.7(3) . . . . ? C14 C9 C10 C11 -0.5(6) . . . . ? C8 C9 C10 C11 -179.5(3) . . . . ? C9 C10 C11 C12 -0.5(7) . . . . ? C10 C11 C12 C13 0.7(8) . . . . ? C11 C12 C13 C14 -0.1(7) . . . . ? C12 C13 C14 C9 -0.8(6) . . . . ? C12 C13 C14 C15 176.3(4) . . . . ? C8 C9 C14 C13 -179.8(3) . . . . ? C10 C9 C14 C13 1.1(5) . . . . ? C8 C9 C14 C15 3.0(4) . . . . ? C10 C9 C14 C15 -176.1(3) . . . . ? C13 C14 C15 C16 -178.0(3) . . . . ? C9 C14 C15 C16 -0.9(4) . . . . ? C14 C15 C16 C7 -1.8(4) . . . . ? C14 C15 C16 C17 179.7(2) . . . . ? C8 C7 C16 C15 2.4(4) . . . . ? C6 C7 C16 C15 -177.5(2) . . . . ? C8 C7 C16 C17 -178.9(2) . . . . ? C6 C7 C16 C17 1.2(3) . . . . ? C2 C3 C17 C18 55.6(3) . . . . ? C4 C3 C17 C18 -121.4(3) . . . . ? C2 C3 C17 C16 -54.5(3) . . . . ? C4 C3 C17 C16 128.5(3) . . . . ? C15 C16 C17 C3 -128.5(2) . . . . ? C7 C16 C17 C3 52.9(2) . . . . ? C15 C16 C17 C18 121.3(3) . . . . ? C7 C16 C17 C18 -57.2(2) . . . . ? C3 C17 C18 C19 126.8(2) . . . . ? C16 C17 C18 C19 -122.4(2) . . . . ? C3 C17 C18 C27 -53.9(2) . . . . ? C16 C17 C18 C27 56.8(2) . . . . ? C27 C18 C19 C20 0.7(4) . . . . ? C17 C18 C19 C20 179.9(2) . . . . ? C18 C19 C20 C25 0.5(4) . . . . ? C18 C19 C20 C21 -179.8(3) . . . . ? C25 C20 C21 C22 -0.5(5) . . . . ? C19 C20 C21 C22 179.8(3) . . . . ? C20 C21 C22 C23 0.5(6) . . . . ? C21 C22 C23 C24 -0.5(6) . . . . ? C22 C23 C24 C25 0.5(6) . . . . ? C21 C20 C25 C24 0.5(4) . . . . ? C19 C20 C25 C24 -179.9(3) . . . . ? C21 C20 C25 C26 179.0(3) . . . . ? C19 C20 C25 C26 -1.4(4) . . . . ? C23 C24 C25 C20 -0.5(5) . . . . ? C23 C24 C25 C26 -178.9(3) . . . . ? C20 C25 C26 C27 0.9(4) . . . . ? C24 C25 C26 C27 179.3(3) . . . . ? C25 C26 C27 C18 0.4(4) . . . . ? C25 C26 C27 C6 -179.7(2) . . . . ? C19 C18 C27 C26 -1.2(3) . . . . ? C17 C18 C27 C26 179.5(2) . . . . ? C19 C18 C27 C6 178.8(2) . . . . ? C17 C18 C27 C6 -0.4(3) . . . . ? C2 C6 C27 C26 -125.5(2) . . . . ? C7 C6 C27 C26 124.2(2) . . . . ? C2 C6 C27 C18 54.4(2) . . . . ? C7 C6 C27 C18 -55.9(2) . . . . ? C33 C28 C29 C30 2.3(12) . . . . ? C28 C29 C30 C31 -3.5(15) . . . . ? C29 C30 C31 C32 8(2) . . . . ? C30 C31 C32 C33 -11(3) . . . . ? C29 C28 C33 C32 -5.3(14) . . . . ? C31 C32 C33 C28 10(2) . . . . ? C39 C34 C35 C36 1.7(11) . . . . ? C34 C35 C36 C37 0.3(10) . . . . ? C35 C36 C37 C38 -3.6(10) . . . . ? C36 C37 C38 C39 4.9(10) . . . . ? C35 C34 C39 C38 -0.5(10) . . . . ? C37 C38 C39 C34 -2.9(10) . . . . ? C45 C40 C41 C42 -0.7(13) . . . . ? C40 C41 C42 C43 3.3(13) . . . . ? C41 C42 C43 C44 -4.1(13) . . . . ? C42 C43 C44 C45 2.1(14) . . . . ? C43 C44 C45 C40 0.4(13) . . . . ? C41 C40 C45 C44 -1.0(13) . . . . ? #============================================================================== data___14-12PhH _database_code_depnum_ccdc_archive 'CCDC 248912' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C180 H132 N4 Ni ' _chemical_formula_moiety ; C108 H60 N4 Ni, 4(C6 H6), 4(C3 H3), 4(C3 H3), 4(C4.2 H4.2), 4(C1.8 H1.8) ; _chemical_formula_weight 2409.75 # CRYSTAL DATA _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 41/a ' _symmetry_space_group_name_Hall '-I 4ad ' _symmetry_Int_Tables_number 88 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2-y,z 3/4-y,1/4+x,1/4+z 1/4+y,1/4-x,1/4+z -x,-y,-z x,1/2+y,-z 3/4+y,1/4-x,1/4-z 1/4-y,1/4+x,1/4-z 1/2+x,1/2+y,1/2+z 1/2-x,-y,1/2+z 1/4-y,3/4+x,3/4+z 3/4+y,3/4-x,3/4+z 1/2-x,1/2-y,1/2-z 1/2+x,y,1/2-z 1/4+y,3/4-x,3/4-z 3/4-y,3/4+x,3/4-z _cell_length_a 19.2176(8) _cell_length_b 19.2176(8) _cell_length_c 36.142(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 13347.8(11) _cell_formula_units_Z 4 _cell_measurement_reflns_used 14532 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 123.2 _exptl_crystal_description Prism _exptl_crystal_colour Red _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.250 _exptl_crystal_density_diffrn 1.199 _exptl_crystal_F_000 5072 _exptl_absorpt_coefficient_mu 0.204 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details Coppens_numerical _exptl_absorpt_correction_T_min 0.920 _exptl_absorpt_correction_T_max 0.944 # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo Ka' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method w _diffrn_detector_area_resol_mean 14.62 _diffrn_reflns_number 54802 _diffrn_reflns_av_R_equivalents 0.056 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9962 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.9962 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 45 # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). In the unit cell, There are three benzene molecules, two of which are disordered. The disordered benzene molecules are treated as rigid models. Three independent benzene molecules are found. Two of them are disordered and they are modeled as four rigid benzene molecules with 0.5, 0.5 0.7, and 0.3 occupancies. ; _reflns_number_total 7623 _reflns_number_gt 5261 _reflns_threshold_expression F^2^>2.0s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0697 _refine_ls_wR_factor_ref 0.1730 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 7623 _refine_ls_number_parameters 352 _refine_ls_goodness_of_fit_ref 1.412 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[s^2^(Fo^2^) + (0.05000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0194 _refine_diff_density_max 1.57 _refine_diff_density_min -0.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Ni Ni 0.339 1.112 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni(1) Ni 0.5000 0.7500 0.1250 0.01481(9) Uani 1.00 d S . . N(1) N 0.47221(10) 0.65201(9) 0.12364(6) 0.0163(5) Uani 1.00 d . . . C(1) C 0.4053(1) 0.6245(1) 0.12418(7) 0.0166(6) Uani 1.00 d . . . C(2) C 0.4075(1) 0.5504(1) 0.12226(7) 0.0194(6) Uani 1.00 d . . . C(3) C 0.4749(1) 0.5318(1) 0.12110(7) 0.0198(6) Uani 1.00 d . . . C(4) C 0.5156(1) 0.5939(1) 0.12220(7) 0.0174(6) Uani 1.00 d . . . C(5) C 0.5865(1) 0.5956(1) 0.12313(7) 0.0175(6) Uani 1.00 d . . . C(6) C 0.3565(1) 0.4903(1) 0.12392(7) 0.0202(6) Uani 1.00 d . . . C(7) C 0.3746(1) 0.4437(1) 0.09101(7) 0.0208(6) Uani 1.00 d . . . C(8) C 0.3294(1) 0.4195(1) 0.06514(8) 0.0251(7) Uani 1.00 d . . . C(9) C 0.3538(1) 0.3779(1) 0.03531(8) 0.0289(8) Uani 1.00 d . . . C(10) C 0.3092(2) 0.3535(2) 0.00717(9) 0.0417(9) Uani 1.00 d . . . C(11) C 0.3347(2) 0.3177(2) -0.02248(9) 0.050(1) Uani 1.00 d . . . C(12) C 0.4057(2) 0.3041(2) -0.02527(9) 0.051(1) Uani 1.00 d . . . C(13) C 0.4505(2) 0.3253(2) 0.00181(9) 0.0383(9) Uani 1.00 d . . . C(14) C 0.4260(1) 0.3623(1) 0.03285(8) 0.0288(8) Uani 1.00 d . . . C(15) C 0.4716(1) 0.3857(1) 0.06137(8) 0.0251(7) Uani 1.00 d . . . C(16) C 0.4465(1) 0.4253(1) 0.08969(7) 0.0208(6) Uani 1.00 d . . . C(17) C 0.4888(1) 0.4542(1) 0.12192(7) 0.0204(6) Uani 1.00 d . . . C(18) C 0.4512(1) 0.4299(1) 0.15684(7) 0.0213(7) Uani 1.00 d . . . C(19) C 0.4797(1) 0.3942(1) 0.18571(8) 0.0242(7) Uani 1.00 d . . . C(20) C 0.4382(1) 0.3746(1) 0.21654(7) 0.0253(7) Uani 1.00 d . . . C(21) C 0.4657(1) 0.3371(1) 0.24685(8) 0.0324(8) Uani 1.00 d . . . C(22) C 0.4244(2) 0.3176(2) 0.27567(9) 0.0394(9) Uani 1.00 d . . . C(23) C 0.3535(2) 0.3351(2) 0.27598(9) 0.0384(9) Uani 1.00 d . . . C(24) C 0.3255(1) 0.3716(2) 0.24721(8) 0.0319(8) Uani 1.00 d . . . C(25) C 0.3665(1) 0.3922(1) 0.21692(7) 0.0259(7) Uani 1.00 d . . . C(26) C 0.3381(1) 0.4301(1) 0.18660(8) 0.0236(7) Uani 1.00 d . . . C(27) C 0.3795(1) 0.4487(1) 0.15779(7) 0.0197(6) Uani 1.00 d . . . C(28) C 0.1190(2) 0.1629(2) 0.0827(1) 0.056(1) Uani 1.00 d . . . C(29) C 0.1232(2) 0.1525(2) 0.1204(1) 0.056(1) Uani 1.00 d . . . C(30) C 0.1024(2) 0.0900(2) 0.13565(10) 0.052(1) Uani 1.00 d . . . C(31) C 0.0763(2) 0.0388(2) 0.1133(1) 0.046(1) Uani 1.00 d . . . C(32) C 0.0708(2) 0.0496(2) 0.0760(1) 0.047(1) Uani 1.00 d . . . C(33) C 0.0924(2) 0.1106(2) 0.0606(1) 0.051(1) Uani 1.00 d . . . C(34) C 0.2716(3) 0.0737(5) 0.0240(2) 0.1214 Uiso 0.50 d G . . C(35) C 0.2686(3) 0.1243(4) -0.0036(2) 0.1005 Uiso 0.50 d G . . C(36) C 0.3238(4) 0.1321(3) -0.0283(2) 0.0698 Uiso 0.50 d G . . C(37) C 0.3822(3) 0.0892(4) -0.0253(2) 0.0585 Uiso 0.50 d G . . C(38) C 0.3852(3) 0.0386(3) 0.0023(2) 0.0674 Uiso 0.50 d G . . C(39) C 0.3300(4) 0.0309(4) 0.0270(2) 0.0543 Uiso 0.50 d G . . C(40) C 0.1253(2) 0.5598(3) 0.1232(1) 0.0892 Uiso 0.70 d G . . C(41) C 0.0806(3) 0.5940(3) 0.14754(9) 0.0761 Uiso 0.70 d G . . C(42) C 0.0238(2) 0.6313(2) 0.1339(1) 0.0616 Uiso 0.70 d G . . C(43) C 0.0117(2) 0.6343(2) 0.0959(1) 0.0602 Uiso 0.70 d G . . C(44) C 0.0564(3) 0.6001(3) 0.07149(9) 0.0843 Uiso 0.70 d G . . C(45) C 0.1132(3) 0.5628(3) 0.0851(1) 0.1022 Uiso 0.70 d G . . C(46) C 0.1323(3) 0.5475(3) 0.2558(2) 0.0923 Uiso 0.50 d G . . C(47) C 0.1401(3) 0.6101(3) 0.2749(1) 0.0599 Uiso 0.50 d G . . C(48) C 0.1912(3) 0.6575(3) 0.2640(2) 0.0589 Uiso 0.50 d G . . C(49) C 0.2343(3) 0.6423(3) 0.2341(2) 0.0575 Uiso 0.50 d G . . C(50) C 0.2265(3) 0.5797(3) 0.2150(2) 0.0820 Uiso 0.50 d G . . C(51) C 0.1755(4) 0.5323(3) 0.2258(2) 0.0553 Uiso 0.50 d G . . C(52) C 0.6684(6) 0.3427(6) 0.1859(2) 0.0706 Uiso 0.30 d G . . C(53) C 0.6318(6) 0.2823(5) 0.1770(3) 0.0706 Uiso 0.30 d G . . C(54) C 0.6194(6) 0.2653(5) 0.1401(3) 0.0706 Uiso 0.30 d G . . C(55) C 0.6436(7) 0.3087(6) 0.1120(2) 0.0706 Uiso 0.30 d G . . C(56) C 0.6802(7) 0.3691(6) 0.1208(2) 0.0706 Uiso 0.30 d G . . C(57) C 0.6926(6) 0.3861(5) 0.1577(3) 0.0706 Uiso 0.30 d G . . H(5) H 0.6123 0.5534 0.1231 0.0210 Uiso 1.00 calc . . . H(6) H 0.3092 0.5044 0.1246 0.0242 Uiso 1.00 calc . . . H(8) H 0.2813 0.4305 0.0670 0.0301 Uiso 1.00 calc . . . H(10) H 0.2607 0.3621 0.0089 0.0500 Uiso 1.00 calc . . . H(11) H 0.3039 0.3020 -0.0413 0.0601 Uiso 1.00 calc . . . H(12) H 0.4232 0.2799 -0.0462 0.0612 Uiso 1.00 calc . . . H(13) H 0.4987 0.3150 -0.0003 0.0460 Uiso 1.00 calc . . . H(15) H 0.5195 0.3737 0.0607 0.0301 Uiso 1.00 calc . . . H(17) H 0.5368 0.4423 0.1212 0.0245 Uiso 1.00 calc . . . H(19) H 0.5277 0.3823 0.1852 0.0291 Uiso 1.00 calc . . . H(21) H 0.5138 0.3253 0.2471 0.0389 Uiso 1.00 calc . . . H(22) H 0.4438 0.2921 0.2957 0.0472 Uiso 1.00 calc . . . H(23) H 0.3249 0.3214 0.2962 0.0461 Uiso 1.00 calc . . . H(24) H 0.2775 0.3834 0.2477 0.0382 Uiso 1.00 calc . . . H(26) H 0.2903 0.4424 0.1865 0.0283 Uiso 1.00 calc . . . H(28) H 0.1341 0.2055 0.0721 0.0673 Uiso 1.00 calc . . . H(29) H 0.1406 0.1884 0.1360 0.0678 Uiso 1.00 calc . . . H(30) H 0.1061 0.0826 0.1616 0.0621 Uiso 1.00 calc . . . H(31) H 0.0619 -0.0043 0.1237 0.0548 Uiso 1.00 calc . . . H(32) H 0.0519 0.0142 0.0607 0.0563 Uiso 1.00 calc . . . H(33) H 0.0891 0.1172 0.0346 0.0618 Uiso 1.00 calc . . . H(34) H 0.2340 0.0684 0.0408 0.0722 Uiso 0.50 calc P . . H(35) H 0.2289 0.1535 -0.0056 0.0722 Uiso 0.50 calc G . . H(36) H 0.3218 0.1665 -0.0471 0.0722 Uiso 0.50 calc G . . H(37) H 0.4198 0.0945 -0.0421 0.0722 Uiso 0.50 calc G . . H(38) H 0.4250 0.0094 0.0043 0.0722 Uiso 0.50 calc G . . H(39) H 0.3321 -0.0036 0.0458 0.0722 Uiso 0.50 calc G . . H(40) H 0.1640 0.5345 0.1325 0.0762 Uiso 0.70 calc P . . H(41) H 0.0888 0.5920 0.1734 0.0762 Uiso 0.70 calc G . . H(42) H -0.0066 0.6545 0.1505 0.0762 Uiso 0.70 calc G . . H(43) H -0.0270 0.6596 0.0866 0.0762 Uiso 0.70 calc G . . H(44) H 0.0482 0.6021 0.0456 0.0762 Uiso 0.70 calc G . . H(45) H 0.1436 0.5396 0.0685 0.0762 Uiso 0.70 calc G . . H(46) H 0.0975 0.5152 0.2632 0.0699 Uiso 0.50 calc P . . H(47) H 0.1107 0.6204 0.2953 0.0699 Uiso 0.50 calc G . . H(48) H 0.1965 0.7001 0.2770 0.0699 Uiso 0.50 calc G . . H(49) H 0.2691 0.6746 0.2267 0.0699 Uiso 0.50 calc G . . H(50) H 0.2559 0.5694 0.1946 0.0699 Uiso 0.50 calc G . . H(51) H 0.1701 0.4897 0.2128 0.0699 Uiso 0.50 calc G . . H(52) H 0.6769 0.3542 0.2110 0.0706 Uiso 0.30 calc P . . H(53) H 0.6153 0.2527 0.1962 0.0706 Uiso 0.30 calc G . . H(54) H 0.5944 0.2241 0.1341 0.0706 Uiso 0.30 calc G . . H(55) H 0.6352 0.2971 0.0868 0.0706 Uiso 0.30 calc G . . H(56) H 0.697 0.3987 0.1017 0.0706 Uiso 0.30 calc G . . H(57) H 0.7175 0.4273 0.1638 0.0706 Uiso 0.30 calc G . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ni(1) 0.0127(2) 0.0127 0.0190(3) 0.0000 0.0000 0.0000 N(1) 0.0141(9) 0.0142(10) 0.021(1) 0.0007(7) 0.0009(9) 0.0003(9) C(1) 0.017(1) 0.014(1) 0.018(1) -0.0017(9) 0.001(1) 0.000(1) C(2) 0.018(1) 0.014(1) 0.026(1) -0.0007(9) -0.002(1) -0.001(1) C(3) 0.015(1) 0.017(1) 0.027(1) -0.0005(9) 0.000(1) -0.003(1) C(4) 0.017(1) 0.016(1) 0.020(1) 0.0017(9) 0.001(1) 0.001(1) C(5) 0.017(1) 0.015(1) 0.021(1) 0.0033(9) 0.000(1) 0.000(1) C(6) 0.016(1) 0.015(1) 0.030(1) 0.0000(9) -0.002(1) -0.001(1) C(7) 0.021(1) 0.014(1) 0.027(1) 0.0003(10) -0.001(1) 0.003(1) C(8) 0.021(1) 0.020(1) 0.034(2) 0.001(1) -0.005(1) 0.002(1) C(9) 0.034(2) 0.021(1) 0.032(2) 0.002(1) -0.008(1) -0.001(1) C(10) 0.044(2) 0.039(2) 0.042(2) 0.009(1) -0.020(2) -0.007(1) C(11) 0.064(2) 0.044(2) 0.042(2) 0.012(2) -0.024(2) -0.014(2) C(12) 0.073(3) 0.046(2) 0.034(2) 0.015(2) -0.010(2) -0.013(2) C(13) 0.048(2) 0.032(2) 0.035(2) 0.007(1) -0.001(1) -0.008(1) C(14) 0.036(2) 0.020(1) 0.030(2) 0.004(1) -0.001(1) -0.001(1) C(15) 0.025(1) 0.019(1) 0.032(1) 0.001(1) -0.001(1) -0.001(1) C(16) 0.018(1) 0.015(1) 0.030(1) -0.0002(10) -0.003(1) 0.000(1) C(17) 0.016(1) 0.014(1) 0.031(1) 0.0012(9) -0.001(1) -0.001(1) C(18) 0.020(1) 0.012(1) 0.032(1) -0.0013(10) -0.004(1) -0.003(1) C(19) 0.021(1) 0.017(1) 0.035(2) 0.000(1) -0.006(1) -0.002(1) C(20) 0.028(1) 0.018(1) 0.030(1) -0.001(1) -0.005(1) -0.001(1) C(21) 0.032(2) 0.029(2) 0.036(2) 0.001(1) -0.008(1) 0.005(1) C(22) 0.048(2) 0.037(2) 0.034(2) -0.001(1) -0.010(1) 0.010(1) C(23) 0.047(2) 0.034(2) 0.034(2) -0.006(1) 0.000(1) 0.007(1) C(24) 0.032(2) 0.032(2) 0.032(2) -0.003(1) 0.002(1) 0.001(1) C(25) 0.029(1) 0.019(1) 0.029(1) -0.005(1) -0.002(1) -0.002(1) C(26) 0.019(1) 0.018(1) 0.034(2) -0.0018(10) -0.001(1) -0.001(1) C(27) 0.018(1) 0.013(1) 0.028(1) -0.0015(10) -0.003(1) -0.002(1) C(28) 0.066(3) 0.044(2) 0.059(2) -0.005(2) -0.016(2) 0.011(2) C(29) 0.073(3) 0.038(2) 0.058(2) -0.007(2) -0.023(2) -0.004(2) C(30) 0.067(3) 0.040(2) 0.048(2) 0.001(2) -0.007(2) -0.002(2) C(31) 0.042(2) 0.032(2) 0.063(2) 0.005(1) 0.001(2) -0.005(2) C(32) 0.037(2) 0.042(2) 0.062(2) 0.013(1) -0.009(2) -0.017(2) C(33) 0.051(2) 0.055(2) 0.049(2) 0.012(2) -0.012(2) -0.002(2) _computing_data_collection CRYSTALCLEAR _computing_cell_refinement CRYSTALCLEAR _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution 'DIRDIF94 (PATTY)' _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni(1) N(1) 1.958(2) . . yes Ni(1) N(1) 1.958(2) . 7_465 yes Ni(1) N(1) 1.958(2) . 8_655 yes Ni(1) N(1) 1.958(2) . 2_665 yes N(1) C(1) 1.390(3) . . yes N(1) C(4) 1.395(3) . . yes C(1) C(2) 1.427(3) . . yes C(1) C(5) 1.374(3) . 7_465 yes C(2) C(3) 1.344(3) . . yes C(2) C(6) 1.514(3) . . yes C(3) C(4) 1.428(3) . . yes C(3) C(17) 1.514(3) . . yes C(4) C(5) 1.364(3) . . yes C(5) H(5) 0.950 . . no C(6) C(7) 1.529(4) . . yes C(6) C(27) 1.528(4) . . yes C(6) H(6) 0.950 . . no C(7) C(8) 1.358(4) . . yes C(7) C(16) 1.426(4) . . yes C(8) C(9) 1.422(4) . . yes C(8) H(8) 0.950 . . no C(9) C(10) 1.410(4) . . yes C(9) C(14) 1.422(4) . . yes C(10) C(11) 1.364(5) . . yes C(10) H(10) 0.950 . . no C(11) C(12) 1.394(6) . . yes C(11) H(11) 0.950 . . no C(12) C(13) 1.366(5) . . yes C(12) H(12) 0.950 . . no C(13) C(14) 1.409(4) . . yes C(13) H(13) 0.950 . . no C(14) C(15) 1.425(4) . . yes C(15) C(16) 1.363(4) . . yes C(15) H(15) 0.950 . . no C(16) C(17) 1.526(4) . . yes C(17) C(18) 1.528(4) . . yes C(17) H(17) 0.950 . . no C(18) C(19) 1.364(4) . . yes C(18) C(27) 1.425(3) . . yes C(19) C(20) 1.421(4) . . yes C(19) H(19) 0.950 . . no C(20) C(21) 1.414(4) . . yes C(20) C(25) 1.418(4) . . yes C(21) C(22) 1.362(4) . . yes C(21) H(21) 0.950 . . no C(22) C(23) 1.405(5) . . yes C(22) H(22) 0.950 . . no C(23) C(24) 1.365(4) . . yes C(23) H(23) 0.950 . . no C(24) C(25) 1.406(4) . . yes C(24) H(24) 0.950 . . no C(25) C(26) 1.424(4) . . yes C(26) C(27) 1.358(4) . . yes C(26) H(26) 0.950 . . no C(28) C(29) 1.379(6) . . yes C(28) C(33) 1.382(5) . . yes C(28) H(28) 0.950 . . no C(29) C(30) 1.380(5) . . yes C(29) H(29) 0.950 . . no C(30) C(31) 1.368(5) . . yes C(30) H(30) 0.950 . . no C(31) C(32) 1.369(5) . . yes C(31) H(31) 0.950 . . no C(32) C(33) 1.362(5) . . yes C(32) H(32) 0.950 . . no C(33) H(33) 0.950 . . no C(34) C(35) 1.39(1) . . yes C(34) C(39) 1.39(1) . . yes C(35) C(36) 1.395(10) . . yes C(35) H(35) 0.950 . . no C(36) C(37) 1.395(9) . . yes C(36) H(36) 0.950 . . no C(37) C(38) 1.395(9) . . yes C(37) H(37) 0.950 . . no C(38) C(39) 1.395(9) . . yes C(38) H(38) 0.950 . . no C(39) H(39) 0.950 . . no C(40) C(41) 1.395(7) . . yes C(40) C(45) 1.395(7) . . yes C(41) C(42) 1.395(7) . . yes C(41) H(41) 0.950 . . no C(42) C(43) 1.395(6) . . yes C(42) H(42) 0.950 . . no C(43) C(44) 1.395(6) . . yes C(43) H(43) 0.950 . . no C(44) C(45) 1.395(7) . . yes C(44) H(44) 0.950 . . no C(45) H(45) 0.950 . . no C(46) C(47) 1.395(9) . . yes C(46) C(51) 1.395(10) . . yes C(47) C(48) 1.395(9) . . yes C(47) H(47) 0.950 . . no C(48) C(49) 1.395(8) . . yes C(48) H(48) 0.950 . . no C(49) C(50) 1.395(9) . . yes C(49) H(49) 0.950 . . no C(50) C(51) 1.395(9) . . yes C(50) H(50) 0.950 . . no C(51) H(51) 0.950 . . no C(52) C(53) 1.39(2) . . yes C(52) C(57) 1.39(1) . . yes C(53) C(54) 1.39(2) . . yes C(53) H(53) 0.950 . . no C(54) C(55) 1.39(2) . . yes C(54) H(54) 0.950 . . no C(55) C(56) 1.39(2) . . yes C(55) H(55) 0.950 . . no C(56) C(57) 1.39(1) . . yes C(56) H(56) 0.950 . . no C(57) H(57) 0.950 . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N(1) Ni(1) N(1) 90.036(3) . . 7_465 yes N(1) Ni(1) N(1) 90.036(3) . . 8_655 yes N(1) Ni(1) N(1) 177.1(1) . . 2_665 yes N(1) Ni(1) N(1) 177.1(1) 7_465 . 8_655 yes N(1) Ni(1) N(1) 90.036(3) 7_465 . 2_665 yes N(1) Ni(1) N(1) 90.036(3) 8_655 . 2_665 yes Ni(1) N(1) C(1) 128.1(1) . . . yes Ni(1) N(1) C(4) 127.5(1) . . . yes C(1) N(1) C(4) 104.4(2) . . . yes N(1) C(1) C(2) 110.6(2) . . . yes N(1) C(1) C(5) 124.5(2) . . 7_465 yes C(2) C(1) C(5) 124.9(2) . . 7_465 yes C(1) C(2) C(3) 107.2(2) . . . yes C(1) C(2) C(6) 137.7(2) . . . yes C(3) C(2) C(6) 114.9(2) . . . yes C(2) C(3) C(4) 107.7(2) . . . yes C(2) C(3) C(17) 115.6(2) . . . yes C(4) C(3) C(17) 136.5(2) . . . yes N(1) C(4) C(3) 110.1(2) . . . yes N(1) C(4) C(5) 125.3(2) . . . yes C(3) C(4) C(5) 124.6(2) . . . yes C(1) C(5) C(4) 124.5(2) 8_655 . . yes C(1) C(5) H(5) 115.4 8_655 . . no C(4) C(5) H(5) 120.0 . . . no C(2) C(6) C(7) 105.6(2) . . . yes C(2) C(6) C(27) 104.1(2) . . . yes C(2) C(6) H(6) 113.9 . . . no C(7) C(6) C(27) 104.5(2) . . . yes C(7) C(6) H(6) 113.9 . . . no C(27) C(6) H(6) 113.9 . . . no C(6) C(7) C(8) 126.2(2) . . . yes C(6) C(7) C(16) 113.0(2) . . . yes C(8) C(7) C(16) 120.8(2) . . . yes C(7) C(8) C(9) 120.2(2) . . . yes C(7) C(8) H(8) 119.9 . . . no C(9) C(8) H(8) 119.9 . . . no C(8) C(9) C(10) 122.2(3) . . . yes C(8) C(9) C(14) 119.2(2) . . . yes C(10) C(9) C(14) 118.5(3) . . . yes C(9) C(10) C(11) 121.1(3) . . . yes C(9) C(10) H(10) 119.4 . . . no C(11) C(10) H(10) 119.4 . . . no C(10) C(11) C(12) 120.1(3) . . . yes C(10) C(11) H(11) 119.9 . . . no C(12) C(11) H(11) 119.9 . . . no C(11) C(12) C(13) 120.7(3) . . . yes C(11) C(12) H(12) 119.7 . . . no C(13) C(12) H(12) 119.7 . . . no C(12) C(13) C(14) 120.7(3) . . . yes C(12) C(13) H(13) 119.7 . . . no C(14) C(13) H(13) 119.6 . . . no C(9) C(14) C(13) 118.8(3) . . . yes C(9) C(14) C(15) 119.2(2) . . . yes C(13) C(14) C(15) 122.0(3) . . . yes C(14) C(15) C(16) 120.1(2) . . . yes C(14) C(15) H(15) 120.0 . . . no C(16) C(15) H(15) 120.0 . . . no C(7) C(16) C(15) 120.4(2) . . . yes C(7) C(16) C(17) 113.6(2) . . . yes C(15) C(16) C(17) 126.0(2) . . . yes C(3) C(17) C(16) 104.4(2) . . . yes C(3) C(17) C(18) 103.5(2) . . . yes C(3) C(17) H(17) 114.1 . . . no C(16) C(17) C(18) 105.4(2) . . . yes C(16) C(17) H(17) 114.1 . . . no C(18) C(17) H(17) 114.1 . . . no C(17) C(18) C(19) 126.6(2) . . . yes C(17) C(18) C(27) 113.6(2) . . . yes C(19) C(18) C(27) 119.8(2) . . . yes C(18) C(19) C(20) 120.5(2) . . . yes C(18) C(19) H(19) 119.7 . . . no C(20) C(19) H(19) 119.7 . . . no C(19) C(20) C(21) 122.1(2) . . . yes C(19) C(20) C(25) 119.3(2) . . . yes C(21) C(20) C(25) 118.5(2) . . . yes C(20) C(21) C(22) 121.0(3) . . . yes C(20) C(21) H(21) 119.5 . . . no C(22) C(21) H(21) 119.5 . . . no C(21) C(22) C(23) 120.4(3) . . . yes C(21) C(22) H(22) 119.8 . . . no C(23) C(22) H(22) 119.8 . . . no C(22) C(23) C(24) 119.9(3) . . . yes C(22) C(23) H(23) 120.0 . . . no C(24) C(23) H(23) 120.0 . . . no C(23) C(24) C(25) 121.2(3) . . . yes C(23) C(24) H(24) 119.4 . . . no C(25) C(24) H(24) 119.4 . . . no C(20) C(25) C(24) 119.0(2) . . . yes C(20) C(25) C(26) 119.1(2) . . . yes C(24) C(25) C(26) 121.9(2) . . . yes C(25) C(26) C(27) 120.0(2) . . . yes C(25) C(26) H(26) 120.0 . . . no C(27) C(26) H(26) 120.0 . . . no C(6) C(27) C(18) 113.1(2) . . . yes C(6) C(27) C(26) 125.7(2) . . . yes C(18) C(27) C(26) 121.2(2) . . . yes C(29) C(28) C(33) 119.1(3) . . . yes C(29) C(28) H(28) 120.4 . . . no C(33) C(28) H(28) 120.4 . . . no C(28) C(29) C(30) 120.2(3) . . . yes C(28) C(29) H(29) 119.9 . . . no C(30) C(29) H(29) 119.9 . . . no C(29) C(30) C(31) 119.8(3) . . . yes C(29) C(30) H(30) 120.1 . . . no C(31) C(30) H(30) 120.1 . . . no C(30) C(31) C(32) 119.9(3) . . . yes C(30) C(31) H(31) 120.0 . . . no C(32) C(31) H(31) 120.0 . . . no C(31) C(32) C(33) 120.7(3) . . . yes C(31) C(32) H(32) 119.6 . . . no C(33) C(32) H(32) 119.6 . . . no C(28) C(33) C(32) 120.1(3) . . . yes C(28) C(33) H(33) 119.9 . . . no C(32) C(33) H(33) 119.9 . . . no H(34) C(34) C(35) 120.0 . . . no H(34) C(34) C(39) 120.0 . . . no C(35) C(34) C(39) 120.0(6) . . . yes C(34) C(35) C(36) 120.0(6) . . . yes C(34) C(35) H(35) 120.0 . . . no C(36) C(35) H(35) 120.0 . . . no C(35) C(36) C(37) 120.0(6) . . . yes C(35) C(36) H(36) 120.0 . . . no C(37) C(36) H(36) 120.0 . . . no C(36) C(37) C(38) 120.0(5) . . . yes C(36) C(37) H(37) 120.0 . . . no C(38) C(37) H(37) 120.0 . . . no C(37) C(38) C(39) 120.0(5) . . . yes C(37) C(38) H(38) 120.0 . . . no C(39) C(38) H(38) 120.0 . . . no C(34) C(39) C(38) 120.0(6) . . . yes C(34) C(39) H(39) 120.0 . . . no C(38) C(39) H(39) 120.0 . . . no H(40) C(40) C(41) 120.0 . . . no H(40) C(40) C(45) 120.0 . . . no C(41) C(40) C(45) 120.0(5) . . . yes C(40) C(41) C(42) 120.0(4) . . . yes C(40) C(41) H(41) 120.0 . . . no C(42) C(41) H(41) 120.0 . . . no C(41) C(42) C(43) 120.0(4) . . . yes C(41) C(42) H(42) 120.0 . . . no C(43) C(42) H(42) 120.0 . . . no C(42) C(43) C(44) 120.0(4) . . . yes C(42) C(43) H(43) 120.0 . . . no C(44) C(43) H(43) 120.0 . . . no C(43) C(44) C(45) 120.0(3) . . . yes C(43) C(44) H(44) 120.0 . . . no C(45) C(44) H(44) 120.0 . . . no C(40) C(45) C(44) 120.0(4) . . . yes C(40) C(45) H(45) 120.0 . . . no C(44) C(45) H(45) 120.0 . . . no H(46) C(46) C(47) 120.0 . . . no H(46) C(46) C(51) 120.0 . . . no C(47) C(46) C(51) 120.0(6) . . . yes C(46) C(47) C(48) 120.0(5) . . . yes C(46) C(47) H(47) 120.0 . . . no C(48) C(47) H(47) 120.0 . . . no C(47) C(48) C(49) 120.0(5) . . . yes C(47) C(48) H(48) 120.0 . . . no C(49) C(48) H(48) 120.0 . . . no C(48) C(49) C(50) 120.0(5) . . . yes C(48) C(49) H(49) 120.0 . . . no C(50) C(49) H(49) 120.0 . . . no C(49) C(50) C(51) 120.0(6) . . . yes C(49) C(50) H(50) 120.0 . . . no C(51) C(50) H(50) 120.0 . . . no C(46) C(51) C(50) 120.0(6) . . . yes C(46) C(51) H(51) 120.0 . . . no C(50) C(51) H(51) 120.0 . . . no H(52) C(52) C(53) 120.0 . . . no H(52) C(52) C(57) 120.0 . . . no C(53) C(52) C(57) 120.0(8) . . . yes C(52) C(53) C(54) 120.0(9) . . . yes C(52) C(53) H(53) 120.0 . . . no C(54) C(53) H(53) 120.0 . . . no C(53) C(54) C(55) 120.0(9) . . . yes C(53) C(54) H(54) 120.0 . . . no C(55) C(54) H(54) 120.0 . . . no C(54) C(55) C(56) 120.0(8) . . . yes C(54) C(55) H(55) 120.0 . . . no C(56) C(55) H(55) 120.0 . . . no C(55) C(56) C(57) 120.0(9) . . . yes C(55) C(56) H(56) 120.0 . . . no C(57) C(56) H(56) 120.0 . . . no C(52) C(57) C(56) 120.0(10) . . . yes C(52) C(57) H(57) 120.0 . . . no C(56) C(57) H(57) 120.0 . . . no 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 Ni(1) N(1) C(1) C(2) 179.2(2) . . . . yes Ni(1) N(1) C(1) C(5) -1.9(4) . . . 7_465 yes Ni(1) N(1) C(4) C(3) -179.3(2) . . . . yes Ni(1) N(1) C(4) C(5) 3.1(4) . . . . yes Ni(1) N(1) C(1) C(2) -179.2(2) . 7_465 7_465 7_465 yes Ni(1) N(1) C(1) C(5) 1.9(4) . 7_465 7_465 2_665 yes Ni(1) N(1) C(4) C(3) 179.3(2) . 7_465 7_465 7_465 yes Ni(1) N(1) C(4) C(5) -3.1(4) . 7_465 7_465 7_465 yes Ni(1) N(1) C(1) C(2) -179.2(2) . 8_655 8_655 8_655 yes Ni(1) N(1) C(1) C(5) 1.9(4) . 8_655 8_655 . yes Ni(1) N(1) C(4) C(3) 179.3(2) . 8_655 8_655 8_655 yes Ni(1) N(1) C(4) C(5) -3.1(4) . 8_655 8_655 8_655 yes Ni(1) N(1) C(1) C(2) 179.2(2) . 2_665 2_665 2_665 yes Ni(1) N(1) C(1) C(5) -1.9(4) . 2_665 2_665 8_655 yes N(1) Ni(1) N(1) C(1) -176.4(2) . . 7_465 7_465 yes N(1) Ni(1) N(1) C(4) 3.0(2) . . 7_465 7_465 yes N(1) Ni(1) N(1) C(1) 0.7(2) . . 8_655 8_655 yes N(1) Ni(1) N(1) C(4) -179.8(2) . . 8_655 8_655 yes N(1) C(1) C(2) C(3) 0.9(3) . . . . yes N(1) C(1) C(2) C(6) 175.5(3) . . . . yes N(1) C(1) C(5) C(4) 2.9(4) . . 7_465 7_465 yes N(1) C(4) C(3) C(2) -0.7(3) . . . . yes N(1) C(4) C(3) C(17) -175.0(3) . . . . yes N(1) C(4) C(5) C(1) 0.3(4) . . . 8_655 yes C(1) N(1) C(4) C(3) 1.2(3) . . . . yes C(1) N(1) C(4) C(5) -176.5(2) . . . . yes C(1) C(2) C(3) C(4) -0.1(3) . . . . yes C(1) C(2) C(3) C(17) 175.5(2) . . . . yes C(1) C(2) C(6) C(7) 131.7(3) . . . . yes C(1) C(2) C(6) C(27) -118.5(3) . . . . yes C(1) C(5) C(4) C(3) 177.0(2) . 7_465 7_465 7_465 yes C(2) C(1) N(1) C(4) -1.3(3) . . . . yes C(2) C(1) C(5) C(4) -178.3(2) . . 7_465 7_465 yes C(2) C(3) C(4) C(5) 177.0(2) . . . . yes C(2) C(3) C(17) C(16) 55.0(3) . . . . yes C(2) C(3) C(17) C(18) -55.1(3) . . . . yes C(2) C(6) C(7) C(8) -128.9(3) . . . . yes C(2) C(6) C(7) C(16) 52.2(3) . . . . yes C(2) C(6) C(27) C(18) -53.7(3) . . . . yes C(2) C(6) C(27) C(26) 126.4(3) . . . . yes C(3) C(2) C(1) C(5) -178.0(2) . . . 7_465 yes C(3) C(2) C(6) C(7) -54.1(3) . . . . yes C(3) C(2) C(6) C(27) 55.7(3) . . . . yes C(3) C(17) C(16) C(7) -54.5(3) . . . . yes C(3) C(17) C(16) C(15) 125.1(3) . . . . yes C(3) C(17) C(18) C(19) -124.5(3) . . . . yes C(3) C(17) C(18) C(27) 54.8(3) . . . . yes C(4) N(1) C(1) C(5) 177.6(2) . . . 7_465 yes C(4) C(3) C(2) C(6) -176.1(2) . . . . yes C(4) C(3) C(17) C(16) -131.0(3) . . . . yes C(4) C(3) C(17) C(18) 118.8(3) . . . . yes C(5) C(1) C(2) C(6) 3.5(5) . 8_655 8_655 8_655 yes C(5) C(4) C(3) C(17) 2.7(5) . . . . yes C(6) C(2) C(3) C(17) -0.4(3) . . . . yes C(6) C(7) C(8) C(9) 178.3(2) . . . . yes C(6) C(7) C(16) C(15) -177.9(2) . . . . yes C(6) C(7) C(16) C(17) 1.8(3) . . . . yes C(6) C(27) C(18) C(17) -1.1(3) . . . . yes C(6) C(27) C(18) C(19) 178.3(2) . . . . yes C(6) C(27) C(26) C(25) -178.8(2) . . . . yes C(7) C(6) C(27) C(18) 56.9(2) . . . . yes C(7) C(6) C(27) C(26) -123.0(3) . . . . yes C(7) C(8) C(9) C(10) -178.0(3) . . . . yes C(7) C(8) C(9) C(14) -0.4(4) . . . . yes C(7) C(16) C(15) C(14) -0.1(4) . . . . yes C(7) C(16) C(17) C(18) 54.2(3) . . . . yes C(8) C(7) C(6) C(27) 121.6(3) . . . . yes C(8) C(7) C(16) C(15) 3.1(4) . . . . yes C(8) C(7) C(16) C(17) -177.3(2) . . . . yes C(8) C(9) C(10) C(11) 175.5(3) . . . . yes C(8) C(9) C(14) C(13) -175.5(3) . . . . yes C(8) C(9) C(14) C(15) 3.3(4) . . . . yes C(9) C(8) C(7) C(16) -2.8(4) . . . . yes C(9) C(10) C(11) C(12) 0.5(5) . . . . yes C(9) C(14) C(13) C(12) -0.6(4) . . . . yes C(9) C(14) C(15) C(16) -3.1(4) . . . . yes C(10) C(9) C(14) C(13) 2.2(4) . . . . yes C(10) C(9) C(14) C(15) -179.0(3) . . . . yes C(10) C(11) C(12) C(13) 1.2(5) . . . . yes C(11) C(10) C(9) C(14) -2.2(4) . . . . yes C(11) C(12) C(13) C(14) -1.1(5) . . . . yes C(12) C(13) C(14) C(15) -179.4(3) . . . . yes C(13) C(14) C(15) C(16) 175.7(3) . . . . yes C(14) C(15) C(16) C(17) -179.7(2) . . . . yes C(15) C(16) C(17) C(18) -126.2(3) . . . . yes C(16) C(7) C(6) C(27) -57.3(3) . . . . yes C(16) C(17) C(18) C(19) 126.1(3) . . . . yes C(16) C(17) C(18) C(27) -54.6(3) . . . . yes C(17) C(18) C(19) C(20) -179.8(2) . . . . yes C(17) C(18) C(27) C(26) 178.9(2) . . . . yes C(18) C(19) C(20) C(21) 179.5(2) . . . . yes C(18) C(19) C(20) C(25) 0.4(4) . . . . yes C(18) C(27) C(26) C(25) 1.2(4) . . . . yes C(19) C(18) C(27) C(26) -1.8(4) . . . . yes C(19) C(20) C(21) C(22) -178.5(3) . . . . yes C(19) C(20) C(25) C(24) 178.9(2) . . . . yes C(19) C(20) C(25) C(26) -0.9(4) . . . . yes C(20) C(19) C(18) C(27) 1.0(4) . . . . yes C(20) C(21) C(22) C(23) -0.6(4) . . . . yes C(20) C(25) C(24) C(23) -0.1(4) . . . . yes C(20) C(25) C(26) C(27) 0.1(4) . . . . yes C(21) C(20) C(25) C(24) -0.3(4) . . . . yes C(21) C(20) C(25) C(26) 179.9(2) . . . . yes C(21) C(22) C(23) C(24) 0.1(5) . . . . yes C(22) C(21) C(20) C(25) 0.6(4) . . . . yes C(22) C(23) C(24) C(25) 0.2(4) . . . . yes C(23) C(24) C(25) C(26) 179.7(3) . . . . yes C(24) C(25) C(26) C(27) -179.7(3) . . . . yes C(28) C(29) C(30) C(31) -1.1(6) . . . . yes C(28) C(33) C(32) C(31) -1.1(5) . . . . yes C(29) C(28) C(33) C(32) -0.1(6) . . . . yes C(29) C(30) C(31) C(32) -0.1(5) . . . . yes C(30) C(29) C(28) C(33) 1.2(6) . . . . yes C(30) C(31) C(32) C(33) 1.2(5) . . . . yes C(34) C(35) C(36) C(37) 0(1) . . . . yes C(34) C(39) C(38) C(37) 0.0(10) . . . . yes C(35) C(34) C(39) C(38) 0(1) . . . . yes C(35) C(36) C(37) C(38) 0.0(10) . . . . yes C(36) C(35) C(34) C(39) 0(1) . . . . yes C(36) C(37) C(38) C(39) 0.0(9) . . . . yes C(40) C(41) C(42) C(43) 0.0(7) . . . . yes C(40) C(45) C(44) C(43) 0.0(8) . . . . yes C(41) C(40) C(45) C(44) 0.0(8) . . . . yes C(41) C(42) C(43) C(44) 0.0(7) . . . . yes C(42) C(41) C(40) C(45) 0.0(8) . . . . yes C(42) C(43) C(44) C(45) 0.0(8) . . . . yes C(46) C(47) C(48) C(49) 0.0(9) . . . . yes C(46) C(51) C(50) C(49) 0.0(10) . . . . yes C(47) C(46) C(51) C(50) 0.0(10) . . . . yes C(47) C(48) C(49) C(50) 0.0(9) . . . . yes C(48) C(47) C(46) C(51) 0.0(9) . . . . yes C(48) C(49) C(50) C(51) 0.0(9) . . . . yes C(52) C(53) C(54) C(55) 0(1) . . . . yes C(52) C(57) C(56) C(55) 0(1) . . . . yes C(53) C(52) C(57) C(56) 0(1) . . . . yes C(53) C(54) C(55) C(56) 0(1) . . . . yes C(54) C(53) C(52) C(57) 0(1) . . . . yes C(54) C(55) C(56) C(57) 0(1) . . . . yes loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag C(8) C(38) 3.512(7) . 6_555 ? C(8) C(48) 3.583(7) . 12_454 ? C(9) C(49) 3.315(6) . 12_454 ? C(9) C(38) 3.428(7) . 6_555 ? C(10) C(25) 3.570(4) . 12_454 ? C(10) C(49) 3.600(6) . 12_454 ? C(11) C(36) 3.580(7) . . ? C(13) C(13) 3.464(6) . 2_655 ? C(13) C(48) 3.568(7) . 8_655 ? C(14) C(49) 3.495(6) . 12_454 ? C(20) C(53) 3.60(1) . 2_655 ? C(21) C(21) 3.597(6) . 2_655 ? C(22) C(33) 3.543(5) . 4_555 ? C(26) C(32) 3.410(4) . 8_555 ? #============================================================================== data___14-8PhCl-4IPAsqueezed(14) _database_code_depnum_ccdc_archive 'CCDC 248913' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C168 H132 Cl8 N4 Ni O4' _chemical_formula_moiety 'C108 H60 N4 Ni, 8(C6 H6), 4(C3 H8 O)' _chemical_formula_weight 2613.09 _chemical_melting_point ? # CRYSTAL DATA _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 41/a ' _symmetry_space_group_name_Hall '-I 4ad ' _symmetry_Int_Tables_number 88 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+3/4, x+1/4, z+1/4' '-x+1/2, -y, z+1/2' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-y+5/4, x+3/4, z+3/4' '-x+1, -y+1/2, z+1' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'y-3/4, -x-1/4, -z-1/4' 'x-1/2, y, -z-1/2' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'y-1/4, -x+1/4, -z+1/4' 'x, y+1/2, -z' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 19.6502(10) _cell_length_b 19.6502(10) _cell_length_c 35.387(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 13663.8(16) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8974 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description Prism _exptl_crystal_colour Red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.270 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5456 _exptl_absorpt_coefficient_mu 0.358 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Jacobson, 1998)' _exptl_absorpt_correction_T_min 0.9319 _exptl_absorpt_correction_T_max 0.9651 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoKa _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 7821 _diffrn_reflns_av_R_equivalents 0.0986 _diffrn_reflns_av_sigmaI/netI 0.1985 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _reflns_number_total 7821 _reflns_number_gt 3152 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR97 _computing_publication_material 'CrystalStructure Ver. 3.5.1' _computing_structure_refinement 'SHELXH-97 and PLATON SQUEEZE' _computing_molecular_graphics ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The solvent molecules are removed one by one by using PLATON SQUEEZE program. ; _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^)+(0.0600P)^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 noref _refine_ls_number_reflns 7821 _refine_ls_number_parameters 255 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1110 _refine_ls_R_factor_gt 0.0747 _refine_ls_wR_factor_ref 0.2036 _refine_ls_wR_factor_gt 0.1976 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.447 _refine_diff_density_min -0.339 _refine_diff_density_rms 0.067 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 Ni1 Ni 0.5000 0.7500 0.1250 0.0228(2) Uani 1 4 d S . . N1 N 0.40372(13) 0.72373(14) 0.12438(9) 0.0336(7) Uani 1 1 d . . . C1 C 0.34540(17) 0.76698(17) 0.12533(12) 0.0355(8) Uani 1 1 d . . . C2 C 0.28602(18) 0.72831(18) 0.12417(12) 0.0395(9) Uani 1 1 d . . . C3 C 0.30305(16) 0.66166(16) 0.12262(11) 0.0324(8) Uani 1 1 d . . . C4 C 0.37644(17) 0.65776(17) 0.12299(11) 0.0325(8) Uani 1 1 d . . . C5 C 0.41287(18) 0.59916(17) 0.12218(11) 0.0350(9) Uani 1 1 d . . . C6 C 0.21135(17) 0.74300(17) 0.12297(13) 0.0385(9) Uani 1 1 d . . . C7 C 0.18043(19) 0.6992(2) 0.15607(11) 0.0395(10) Uani 1 1 d . . . C8 C 0.1413(2) 0.7242(2) 0.18500(13) 0.0462(11) Uani 1 1 d . . . C9 C 0.1143(2) 0.6772(2) 0.21248(13) 0.0491(11) Uani 1 1 d . . . C10 C 0.0762(3) 0.7005(3) 0.24259(16) 0.0733(15) Uani 1 1 d . . . C11 C 0.0519(3) 0.6543(4) 0.26952(17) 0.098(2) Uani 1 1 d . . . C12 C 0.0662(3) 0.5888(3) 0.26696(17) 0.0829(18) Uani 1 1 d . . . C13 C 0.1049(3) 0.5672(3) 0.23783(15) 0.0649(14) Uani 1 1 d . . . C14 C 0.1323(2) 0.6088(2) 0.21042(13) 0.0507(12) Uani 1 1 d . . . C15 C 0.1744(2) 0.5833(2) 0.18088(13) 0.0465(11) Uani 1 1 d . . . C16 C 0.19920(19) 0.62832(19) 0.15387(12) 0.0390(10) Uani 1 1 d . . . C17 C 0.24446(18) 0.61266(18) 0.12010(11) 0.0357(9) Uani 1 1 d . . . C18 C 0.20302(18) 0.6359(2) 0.08631(12) 0.0405(10) Uani 1 1 d . . . C19 C 0.1808(2) 0.5976(2) 0.05646(13) 0.0462(11) Uani 1 1 d . . . C20 C 0.1451(2) 0.6253(3) 0.02712(14) 0.0611(13) Uani 1 1 d . . . C21 C 0.1239(3) 0.5833(3) -0.00428(17) 0.0844(17) Uani 1 1 d . . . C22 C 0.0819(4) 0.6132(4) -0.0312(2) 0.112(2) Uani 1 1 d . . . C23 C 0.0672(3) 0.6809(3) -0.03118(17) 0.0847(18) Uani 1 1 d . . . C24 C 0.0888(3) 0.7201(3) -0.00197(17) 0.0807(17) Uani 1 1 d . . . C25 C 0.1280(2) 0.6939(2) 0.02782(14) 0.0505(12) Uani 1 1 d . . . C26 C 0.1472(2) 0.7333(2) 0.05888(13) 0.0473(11) Uani 1 1 d . . . C27 C 0.1844(2) 0.7068(2) 0.08683(12) 0.0449(11) Uani 1 1 d . . . H1 H 0.3890 0.5585 0.1198 0.042 Uiso 1 1 c . . . H2 H 0.2001 0.7915 0.1243 0.046 Uiso 1 1 c . . . H3 H 0.1323 0.7705 0.1869 0.055 Uiso 1 1 c . . . H4 H 0.0667 0.7467 0.2450 0.088 Uiso 1 1 c . . . H5 H 0.0254 0.6699 0.2895 0.117 Uiso 1 1 c . . . H6 H 0.0500 0.5582 0.2849 0.099 Uiso 1 1 c . . . H7 H 0.1138 0.5208 0.2361 0.078 Uiso 1 1 c . . . H8 H 0.1851 0.5373 0.1797 0.056 Uiso 1 1 c . . . H9 H 0.2586 0.5649 0.1187 0.043 Uiso 1 1 c . . . H10 H 0.1903 0.5513 0.0562 0.055 Uiso 1 1 c . . . H11 H 0.1378 0.5382 -0.0064 0.101 Uiso 1 1 c . . . H12 H 0.0631 0.5859 -0.0500 0.135 Uiso 1 1 c . . . H13 H 0.0426 0.7001 -0.0510 0.102 Uiso 1 1 c . . . H14 H 0.0772 0.7660 -0.0017 0.097 Uiso 1 1 c . . . H15 H 0.1340 0.7787 0.0601 0.057 Uiso 1 1 c . . . 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 Ni1 0.0181(3) 0.0181(3) 0.0322(5) 0.000 0.000 0.000 N1 0.0224(15) 0.0376(17) 0.0407(18) 0.0016(17) -0.0046(16) -0.0060(13) C1 0.0315(19) 0.032(2) 0.043(2) 0.002(2) -0.003(2) -0.0019(15) C2 0.034(2) 0.040(2) 0.044(2) 0.000(2) -0.002(2) -0.0055(16) C3 0.0281(18) 0.0233(18) 0.046(2) 0.0051(19) -0.001(2) -0.0012(14) C4 0.0296(19) 0.0311(19) 0.037(2) 0.0012(19) -0.001(2) 0.0034(14) C5 0.037(2) 0.0313(19) 0.037(2) 0.008(2) -0.001(2) -0.0035(16) C6 0.0260(18) 0.0279(19) 0.062(3) -0.005(2) 0.001(2) -0.0006(14) C7 0.029(2) 0.046(3) 0.044(3) -0.003(2) -0.0016(19) -0.0016(19) C8 0.041(2) 0.040(2) 0.058(3) 0.003(2) 0.008(2) 0.015(2) C9 0.032(2) 0.064(3) 0.051(3) 0.001(2) 0.006(2) -0.003(2) C10 0.071(4) 0.082(4) 0.067(4) 0.017(3) 0.007(3) 0.006(3) C11 0.060(4) 0.149(6) 0.083(5) 0.021(5) 0.020(3) 0.020(4) C12 0.072(4) 0.097(5) 0.080(4) 0.030(4) 0.016(3) 0.019(3) C13 0.058(3) 0.067(3) 0.069(4) 0.025(3) -0.006(3) 0.000(3) C14 0.042(3) 0.055(3) 0.056(3) 0.018(2) -0.004(2) -0.002(2) C15 0.038(2) 0.041(3) 0.061(3) -0.002(2) -0.005(2) -0.0016(19) C16 0.033(2) 0.030(2) 0.054(3) 0.0013(19) -0.001(2) -0.0037(17) C17 0.034(2) 0.038(2) 0.035(2) 0.0009(19) 0.0021(19) -0.0023(16) C18 0.025(2) 0.038(2) 0.059(3) 0.006(2) 0.005(2) 0.0003(17) C19 0.035(2) 0.038(2) 0.065(3) -0.011(2) -0.002(2) -0.0012(19) C20 0.044(3) 0.083(4) 0.056(3) -0.018(3) -0.010(2) -0.003(3) C21 0.081(4) 0.108(5) 0.065(4) -0.014(3) -0.013(3) 0.007(4) C22 0.102(5) 0.135(7) 0.101(5) -0.036(5) -0.027(4) -0.016(5) C23 0.110(5) 0.077(4) 0.068(4) -0.008(3) -0.005(4) 0.016(4) C24 0.075(4) 0.096(4) 0.071(4) 0.003(3) -0.024(3) 0.015(3) C25 0.035(2) 0.050(3) 0.066(3) 0.001(3) -0.006(2) 0.001(2) C26 0.041(3) 0.048(3) 0.053(3) 0.009(2) -0.006(2) -0.001(2) C27 0.044(3) 0.038(2) 0.053(3) -0.005(2) 0.016(2) -0.005(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 1.961(2) 7_564 ? Ni1 N1 1.961(2) . ? Ni1 N1 1.961(2) 14_565 ? Ni1 N1 1.961(2) 12_766 ? N1 C4 1.404(4) . ? N1 C1 1.427(4) . ? C1 C5 1.383(5) 14_565 ? C1 C2 1.393(5) . ? C2 C3 1.353(5) . ? C2 C6 1.496(5) . ? C3 C4 1.444(5) . ? C3 C17 1.504(4) . ? C4 C5 1.356(4) . ? C5 C1 1.383(5) 12_766 ? C5 H1 0.930 . ? C6 C27 1.557(6) . ? C6 C7 1.575(5) . ? C6 H2 0.980 . ? C7 C8 1.372(5) . ? C7 C16 1.444(5) . ? C8 C9 1.442(6) . ? C8 H3 0.930 . ? C9 C10 1.381(6) . ? C9 C14 1.392(6) . ? C10 C11 1.400(7) . ? C10 H4 0.930 . ? C11 C12 1.320(8) . ? C11 H5 0.930 . ? C12 C13 1.350(7) . ? C12 H6 0.930 . ? C13 C14 1.378(6) . ? C13 H7 0.930 . ? C14 C15 1.423(6) . ? C15 C16 1.390(5) . ? C15 H8 0.930 . ? C16 C17 1.521(5) . ? C17 C18 1.517(5) . ? C17 H9 0.980 . ? C18 C19 1.368(5) . ? C18 C27 1.439(5) . ? C19 C20 1.366(6) . ? C19 H10 0.930 . ? C20 C25 1.391(6) . ? C20 C21 1.445(7) . ? C21 C22 1.392(8) . ? C21 H11 0.930 . ? C22 C23 1.361(9) . ? C22 H12 0.930 . ? C23 C24 1.358(7) . ? C23 H13 0.930 . ? C24 C25 1.404(6) . ? C24 H14 0.930 . ? C25 C26 1.396(6) . ? C26 C27 1.335(6) . ? C26 H15 0.930 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 N1 178.72(18) 7_564 . ? N1 Ni1 N1 90.007(2) 7_564 14_565 ? N1 Ni1 N1 90.007(2) . 14_565 ? N1 Ni1 N1 90.007(2) 7_564 12_766 ? N1 Ni1 N1 90.007(2) . 12_766 ? N1 Ni1 N1 178.72(18) 14_565 12_766 ? C4 N1 C1 104.1(2) . . ? C4 N1 Ni1 127.7(2) . . ? C1 N1 Ni1 128.2(2) . . ? C5 C1 C2 126.2(3) 14_565 . ? C5 C1 N1 123.5(3) 14_565 . ? C2 C1 N1 110.3(3) . . ? C3 C2 C1 108.8(3) . . ? C3 C2 C6 115.4(3) . . ? C1 C2 C6 135.8(3) . . ? C2 C3 C4 107.3(3) . . ? C2 C3 C17 115.7(3) . . ? C4 C3 C17 137.0(3) . . ? C5 C4 N1 125.7(3) . . ? C5 C4 C3 124.9(3) . . ? N1 C4 C3 109.4(3) . . ? C4 C5 C1 124.8(3) . 12_766 ? C4 C5 H1 117.6 . . ? C1 C5 H1 117.6 12_766 . ? C2 C6 C27 105.6(3) . . ? C2 C6 C7 104.6(3) . . ? C27 C6 C7 103.3(3) . . ? C2 C6 H2 114.1 . . ? C27 C6 H2 114.1 . . ? C7 C6 H2 114.1 . . ? C8 C7 C16 121.9(4) . . ? C8 C7 C6 125.2(4) . . ? C16 C7 C6 112.9(3) . . ? C7 C8 C9 118.7(4) . . ? C7 C8 H3 120.7 . . ? C9 C8 H3 120.7 . . ? C10 C9 C14 119.9(5) . . ? C10 C9 C8 120.5(4) . . ? C14 C9 C8 119.4(4) . . ? C9 C10 C11 119.6(5) . . ? C9 C10 H4 120.2 . . ? C11 C10 H4 120.2 . . ? C12 C11 C10 120.9(6) . . ? C12 C11 H5 119.6 . . ? C10 C11 H5 119.6 . . ? C11 C12 C13 118.6(6) . . ? C11 C12 H6 120.7 . . ? C13 C12 H6 120.7 . . ? C12 C13 C14 124.9(5) . . ? C12 C13 H7 117.6 . . ? C14 C13 H7 117.6 . . ? C13 C14 C9 115.9(4) . . ? C13 C14 C15 122.4(4) . . ? C9 C14 C15 121.7(4) . . ? C16 C15 C14 119.0(4) . . ? C16 C15 H8 120.5 . . ? C14 C15 H8 120.5 . . ? C15 C16 C7 119.1(4) . . ? C15 C16 C17 128.1(3) . . ? C7 C16 C17 112.8(3) . . ? C3 C17 C18 105.3(3) . . ? C3 C17 C16 105.8(3) . . ? C18 C17 C16 104.1(3) . . ? C3 C17 H9 113.6 . . ? C18 C17 H9 113.6 . . ? C16 C17 H9 113.6 . . ? C19 C18 C27 117.4(4) . . ? C19 C18 C17 127.9(4) . . ? C27 C18 C17 114.7(4) . . ? C20 C19 C18 122.1(4) . . ? C20 C19 H10 118.9 . . ? C18 C19 H10 118.9 . . ? C19 C20 C25 119.7(4) . . ? C19 C20 C21 120.4(5) . . ? C25 C20 C21 119.9(5) . . ? C22 C21 C20 117.2(6) . . ? C22 C21 H11 121.4 . . ? C20 C21 H11 121.4 . . ? C23 C22 C21 122.5(6) . . ? C23 C22 H12 118.7 . . ? C21 C22 H12 118.7 . . ? C24 C23 C22 119.3(6) . . ? C24 C23 H13 120.3 . . ? C22 C23 H13 120.4 . . ? C23 C24 C25 122.4(5) . . ? C23 C24 H14 118.8 . . ? C25 C24 H14 118.8 . . ? C20 C25 C26 119.1(4) . . ? C20 C25 C24 118.4(5) . . ? C26 C25 C24 122.4(5) . . ? C27 C26 C25 121.0(4) . . ? C27 C26 H15 119.5 . . ? C25 C26 H15 119.5 . . ? C26 C27 C18 120.5(4) . . ? C26 C27 C6 128.0(4) . . ? C18 C27 C6 111.5(4) . . ? 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 N1 Ni1 N1 C4 178.6(4) 14_565 . . . ? N1 Ni1 N1 C4 -2.7(3) 12_766 . . . ? N1 Ni1 N1 C1 -1.6(3) 14_565 . . . ? N1 Ni1 N1 C1 177.2(4) 12_766 . . . ? C4 N1 C1 C5 178.2(4) . . . 14_565 ? Ni1 N1 C1 C5 -1.6(6) . . . 14_565 ? C4 N1 C1 C2 -0.6(4) . . . . ? Ni1 N1 C1 C2 179.6(3) . . . . ? C5 C1 C2 C3 -178.6(4) 14_565 . . . ? N1 C1 C2 C3 0.2(5) . . . . ? C5 C1 C2 C6 3.9(8) 14_565 . . . ? N1 C1 C2 C6 -177.3(5) . . . . ? C1 C2 C3 C4 0.3(5) . . . . ? C6 C2 C3 C4 178.4(3) . . . . ? C1 C2 C3 C17 -178.3(3) . . . . ? C6 C2 C3 C17 -0.3(6) . . . . ? C1 N1 C4 C5 -179.2(4) . . . . ? Ni1 N1 C4 C5 0.7(6) . . . . ? C1 N1 C4 C3 0.7(4) . . . . ? Ni1 N1 C4 C3 -179.4(3) . . . . ? C2 C3 C4 C5 179.2(4) . . . . ? C17 C3 C4 C5 -2.6(8) . . . . ? C2 C3 C4 N1 -0.7(5) . . . . ? C17 C3 C4 N1 177.5(4) . . . . ? N1 C4 C5 C1 3.7(7) . . . 12_766 ? C3 C4 C5 C1 -176.2(4) . . . 12_766 ? C3 C2 C6 C27 -54.3(5) . . . . ? C1 C2 C6 C27 123.0(5) . . . . ? C3 C2 C6 C7 54.3(5) . . . . ? C1 C2 C6 C7 -128.4(5) . . . . ? C2 C6 C7 C8 124.9(4) . . . . ? C27 C6 C7 C8 -124.7(4) . . . . ? C2 C6 C7 C16 -53.3(4) . . . . ? C27 C6 C7 C16 57.0(4) . . . . ? C16 C7 C8 C9 -4.4(6) . . . . ? C6 C7 C8 C9 177.6(4) . . . . ? C7 C8 C9 C10 178.3(4) . . . . ? C7 C8 C9 C14 4.2(6) . . . . ? C14 C9 C10 C11 -4.3(8) . . . . ? C8 C9 C10 C11 -178.4(5) . . . . ? C9 C10 C11 C12 1.4(9) . . . . ? C10 C11 C12 C13 0.1(10) . . . . ? C11 C12 C13 C14 1.3(9) . . . . ? C12 C13 C14 C9 -4.1(7) . . . . ? C12 C13 C14 C15 178.2(5) . . . . ? C10 C9 C14 C13 5.5(7) . . . . ? C8 C9 C14 C13 179.5(4) . . . . ? C10 C9 C14 C15 -176.9(4) . . . . ? C8 C9 C14 C15 -2.8(7) . . . . ? C13 C14 C15 C16 178.9(4) . . . . ? C9 C14 C15 C16 1.4(6) . . . . ? C14 C15 C16 C7 -1.4(6) . . . . ? C14 C15 C16 C17 -179.9(4) . . . . ? C8 C7 C16 C15 3.0(6) . . . . ? C6 C7 C16 C15 -178.7(3) . . . . ? C8 C7 C16 C17 -178.2(4) . . . . ? C6 C7 C16 C17 0.0(5) . . . . ? C2 C3 C17 C18 54.3(5) . . . . ? C4 C3 C17 C18 -123.8(5) . . . . ? C2 C3 C17 C16 -55.6(5) . . . . ? C4 C3 C17 C16 126.3(5) . . . . ? C15 C16 C17 C3 -128.1(4) . . . . ? C7 C16 C17 C3 53.3(4) . . . . ? C15 C16 C17 C18 121.1(4) . . . . ? C7 C16 C17 C18 -57.5(4) . . . . ? C3 C17 C18 C19 129.1(4) . . . . ? C16 C17 C18 C19 -119.9(4) . . . . ? C3 C17 C18 C27 -52.3(4) . . . . ? C16 C17 C18 C27 58.8(4) . . . . ? C27 C18 C19 C20 3.1(6) . . . . ? C17 C18 C19 C20 -178.3(4) . . . . ? C18 C19 C20 C25 -2.6(7) . . . . ? C18 C19 C20 C21 178.6(4) . . . . ? C19 C20 C21 C22 173.6(5) . . . . ? C25 C20 C21 C22 -5.2(8) . . . . ? C20 C21 C22 C23 7.7(10) . . . . ? C21 C22 C23 C24 -6.3(11) . . . . ? C22 C23 C24 C25 2.3(10) . . . . ? C19 C20 C25 C26 -0.6(7) . . . . ? C21 C20 C25 C26 178.2(4) . . . . ? C19 C20 C25 C24 -177.3(4) . . . . ? C21 C20 C25 C24 1.6(7) . . . . ? C23 C24 C25 C20 0.0(8) . . . . ? C23 C24 C25 C26 -176.5(5) . . . . ? C20 C25 C26 C27 3.2(7) . . . . ? C24 C25 C26 C27 179.7(4) . . . . ? C25 C26 C27 C18 -2.7(6) . . . . ? C25 C26 C27 C6 178.8(4) . . . . ? C19 C18 C27 C26 -0.5(6) . . . . ? C17 C18 C27 C26 -179.3(4) . . . . ? C19 C18 C27 C6 178.3(3) . . . . ? C17 C18 C27 C6 -0.5(5) . . . . ? C2 C6 C27 C26 -127.9(4) . . . . ? C7 C6 C27 C26 122.5(4) . . . . ? C2 C6 C27 C18 53.4(4) . . . . ? C7 C6 C27 C18 -56.2(4) . . . . ? #============================================================================== data_14-12PhHsqueezed(14-4PhH) _database_code_depnum_ccdc_archive 'CCDC 248914' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C180 H132 N4 Ni ' _chemical_formula_moiety 'C108 H60 N4 Ni, 12(C6 H6) ' _chemical_formula_weight 2409.75 _chemical_melting_point ? # CRYSTAL DATA _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 41/a ' _symmetry_space_group_name_Hall '-I 4ad' _symmetry_Int_Tables_number 88 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' Ni Ni 0.3393 1.1124 '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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+3/4, x+1/4, z+1/4' '-x+1/2, -y, z+1/2' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-y+5/4, x+3/4, z+3/4' '-x+1, -y+1/2, z+1' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'y-3/4, -x-1/4, -z-1/4' 'x-1/2, y, -z-1/2' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'y-1/4, -x+1/4, -z+1/4' 'x, y+1/2, -z' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 19.2176(8) _cell_length_b 19.2176(8) _cell_length_c 36.142(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 13347.8(11) _cell_formula_units_Z 4 _cell_measurement_reflns_used 14532 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 123.1 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_diffrn 1.259 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5250 _exptl_absorpt_coefficient_mu 0.278 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Higashi, T. (1999). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.9213 _exptl_absorpt_correction_T_max 0.9338 _exptl_special_details ; ? ; # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo Ka' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 54802 _diffrn_reflns_av_R_equivalents 0.065 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9958 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.9958 _diffrn_ambient_temperature 123(2) _diffrn_radiation_monochromator graphite _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 45 _reflns_number_total 7623 _reflns_number_gt 6282 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'DIRDIF99 (ORIENT)' _computing_structure_refinement ; SHELXL-97 (Sheldrick, 1997) and PLATON SQUEEZE ; _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. Two of three benzene molecules are removed by PLATON SQUEEZE program. ; _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^)+(0.0863P)^2^+11.9515P] 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_number_reflns 7623 _refine_ls_number_parameters 309 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0743 _refine_ls_R_factor_gt 0.0614 _refine_ls_wR_factor_ref 0.1700 _refine_ls_wR_factor_gt 0.1640 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.100 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.267 _refine_diff_density_min -0.269 _refine_diff_density_rms 0.059 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 Ni1 Ni 0.5000 0.7500 0.6250 0.01288(13) Uani 1 4 d S . . N1 N 0.47222(8) 0.65173(8) 0.62359(4) 0.0170(3) Uani 1 1 d . . . C1 C 0.51561(9) 0.59401(9) 0.62199(5) 0.0168(3) Uani 1 1 d . . . C2 C 0.47510(9) 0.53156(9) 0.62091(5) 0.0190(4) Uani 1 1 d . . . C3 C 0.40756(9) 0.55008(9) 0.62198(5) 0.0177(4) Uani 1 1 d . . . C4 C 0.40536(9) 0.62457(9) 0.62427(5) 0.0158(3) Uani 1 1 d . . . C5 C 0.34566(9) 0.66349(9) 0.62679(5) 0.0177(3) Uani 1 1 d . . . C6 C 0.48903(9) 0.45437(9) 0.62187(5) 0.0192(4) Uani 1 1 d . . . C7 C 0.44676(10) 0.42542(9) 0.58966(5) 0.0202(4) Uani 1 1 d . . . C8 C 0.47154(10) 0.38602(10) 0.56107(6) 0.0240(4) Uani 1 1 d . . . C9 C 0.42585(12) 0.36262(11) 0.53293(6) 0.0282(4) Uani 1 1 d . . . C10 C 0.45087(14) 0.32524(12) 0.50152(6) 0.0372(5) Uani 1 1 d . . . C11 C 0.40533(17) 0.30458(15) 0.47470(7) 0.0504(7) Uani 1 1 d . . . C12 C 0.33460(16) 0.31744(14) 0.47757(7) 0.0487(7) Uani 1 1 d . . . C13 C 0.30914(14) 0.35350(13) 0.50732(7) 0.0400(6) Uani 1 1 d . . . C14 C 0.35391(11) 0.37776(10) 0.53534(6) 0.0274(4) Uani 1 1 d . . . C15 C 0.32928(10) 0.41954(10) 0.56500(6) 0.0253(4) Uani 1 1 d . . . C16 C 0.37442(10) 0.44344(9) 0.59108(5) 0.0207(4) Uani 1 1 d . . . C17 C 0.35644(9) 0.49012(9) 0.62391(5) 0.0190(4) Uani 1 1 d . . . C18 C 0.37944(10) 0.44901(9) 0.65773(5) 0.0203(4) Uani 1 1 d . . . C19 C 0.33798(10) 0.43005(10) 0.68670(5) 0.0225(4) Uani 1 1 d . . . C20 C 0.36684(11) 0.39229(10) 0.71672(5) 0.0247(4) Uani 1 1 d . . . C21 C 0.32511(12) 0.37184(11) 0.74737(6) 0.0305(5) Uani 1 1 d . . . C22 C 0.35369(14) 0.33509(13) 0.77614(6) 0.0384(5) Uani 1 1 d . . . C23 C 0.42465(14) 0.31777(13) 0.77575(7) 0.0391(6) Uani 1 1 d . . . C24 C 0.46557(12) 0.33724(11) 0.74673(6) 0.0318(5) Uani 1 1 d . . . C25 C 0.43845(11) 0.37482(10) 0.71646(6) 0.0252(4) Uani 1 1 d . . . C26 C 0.48063(10) 0.39402(10) 0.68553(6) 0.0241(4) Uani 1 1 d . . . C27 C 0.45123(10) 0.42994(9) 0.65663(5) 0.0205(4) Uani 1 1 d . . . C28 C 0.16027(15) 0.35232(16) 0.61450(8) 0.0490(7) Uani 1 1 d . . . C29 C 0.09785(16) 0.37329(18) 0.62983(8) 0.0562(8) Uani 1 1 d . . . C30 C 0.08710(15) 0.36828(17) 0.66730(9) 0.0567(8) Uani 1 1 d . . . C31 C 0.13875(16) 0.34211(15) 0.68914(8) 0.0512(7) Uani 1 1 d . . . C32 C 0.20056(14) 0.32043(13) 0.67415(8) 0.0430(6) Uani 1 1 d . . . C33 C 0.21136(13) 0.32603(14) 0.63662(8) 0.0441(6) Uani 1 1 d . . . H1 H 0.3034 0.6399 0.6277 0.021 Uiso 1 1 c . . . H2 H 0.5385 0.4421 0.6212 0.023 Uiso 1 1 c . . . H3 H 0.5195 0.3743 0.5601 0.029 Uiso 1 1 c . . . H4 H 0.4979 0.3150 0.4993 0.044 Uiso 1 1 c . . . H5 H 0.4222 0.2814 0.4540 0.060 Uiso 1 1 c . . . H6 H 0.3045 0.3015 0.4593 0.058 Uiso 1 1 c . . . H7 H 0.2616 0.3621 0.5090 0.048 Uiso 1 1 c . . . H8 H 0.2823 0.4306 0.5666 0.030 Uiso 1 1 c . . . H9 H 0.3076 0.5047 0.6246 0.023 Uiso 1 1 c . . . H10 H 0.2910 0.4418 0.6867 0.027 Uiso 1 1 c . . . H11 H 0.2781 0.3835 0.7479 0.036 Uiso 1 1 c . . . H12 H 0.3259 0.3216 0.7960 0.046 Uiso 1 1 c . . . H13 H 0.4438 0.2930 0.7954 0.047 Uiso 1 1 c . . . H14 H 0.5125 0.3255 0.7469 0.038 Uiso 1 1 c . . . H15 H 0.5276 0.3823 0.6850 0.029 Uiso 1 1 c . . . H16 H 0.1674 0.3561 0.5891 0.059 Uiso 1 1 c . . . H17 H 0.0629 0.3909 0.6147 0.067 Uiso 1 1 c . . . H18 H 0.0452 0.3826 0.6777 0.068 Uiso 1 1 c . . . H19 H 0.1319 0.3389 0.7146 0.061 Uiso 1 1 c . . . H20 H 0.2351 0.3020 0.6893 0.052 Uiso 1 1 c . . . H21 H 0.2534 0.3119 0.6264 0.053 Uiso 1 1 c . . . 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 Ni1 0.01102(16) 0.01102(16) 0.0166(2) 0.000 0.000 0.000 N1 0.0146(7) 0.0135(7) 0.0229(7) 0.0026(6) 0.0019(6) 0.0014(6) C1 0.0183(9) 0.0150(8) 0.0172(8) -0.0007(6) 0.0009(7) 0.0010(7) C2 0.0156(8) 0.0154(9) 0.0260(9) -0.0027(7) -0.0010(7) -0.0004(7) C3 0.0162(8) 0.0123(8) 0.0247(9) 0.0007(7) -0.0031(7) 0.0004(6) C4 0.0168(8) 0.0131(8) 0.0176(8) 0.0009(6) -0.0023(6) -0.0007(6) C5 0.0151(8) 0.0153(8) 0.0226(8) 0.0019(7) 0.0027(7) -0.0027(6) C6 0.0162(8) 0.0122(8) 0.0292(9) -0.0018(7) -0.0021(7) 0.0016(6) C7 0.0187(9) 0.0144(8) 0.0275(9) -0.0009(7) -0.0025(7) 0.0010(7) C8 0.0217(9) 0.0186(9) 0.0318(10) -0.0028(8) 0.0011(8) 0.0005(7) C9 0.0331(11) 0.0211(10) 0.0304(10) -0.0023(8) -0.0014(9) 0.0015(8) C10 0.0473(14) 0.0312(12) 0.0329(11) -0.0090(9) -0.0032(10) 0.0071(10) C11 0.0656(19) 0.0491(16) 0.0364(13) -0.0124(11) -0.0123(12) 0.0193(14) C12 0.0662(18) 0.0420(14) 0.0381(13) -0.0114(11) -0.0232(12) 0.0085(13) C13 0.0459(14) 0.0339(12) 0.0402(12) -0.0056(10) -0.0172(11) 0.0070(10) C14 0.0309(11) 0.0207(10) 0.0307(10) -0.0016(8) -0.0066(8) 0.0021(8) C15 0.0229(10) 0.0188(9) 0.0341(10) 0.0004(8) -0.0041(8) 0.0005(7) C16 0.0212(9) 0.0113(8) 0.0295(9) 0.0019(7) 0.0008(7) -0.0004(7) C17 0.0135(8) 0.0142(8) 0.0294(9) -0.0025(7) -0.0017(7) 0.0002(6) C18 0.0183(9) 0.0133(8) 0.0293(9) -0.0007(7) -0.0016(7) -0.0047(7) C19 0.0184(9) 0.0191(9) 0.0300(10) -0.0018(7) 0.0006(7) -0.0031(7) C20 0.0266(10) 0.0196(9) 0.0280(10) -0.0035(7) -0.0004(8) -0.0055(8) C21 0.0332(12) 0.0285(11) 0.0296(10) 0.0005(8) 0.0005(9) -0.0014(9) C22 0.0510(15) 0.0338(12) 0.0305(11) 0.0074(9) 0.0003(10) -0.0052(11) C23 0.0469(14) 0.0350(13) 0.0353(12) 0.0094(10) -0.0117(10) 0.0015(11) C24 0.0344(12) 0.0280(11) 0.0331(11) 0.0056(9) -0.0071(9) -0.0010(9) C25 0.0265(10) 0.0156(9) 0.0334(10) -0.0020(8) -0.0035(8) -0.0005(7) C26 0.0212(9) 0.0168(9) 0.0341(10) -0.0007(8) -0.0042(8) 0.0004(7) C27 0.0193(9) 0.0114(8) 0.0307(10) -0.0022(7) -0.0032(7) -0.0023(7) C28 0.0416(15) 0.0593(18) 0.0462(14) 0.0049(13) 0.0003(12) -0.0045(13) C29 0.0420(15) 0.071(2) 0.0557(17) 0.0234(15) 0.0014(12) 0.0127(14) C30 0.0406(15) 0.066(2) 0.0639(18) 0.0173(15) 0.0123(13) 0.0050(14) C31 0.0559(17) 0.0523(17) 0.0454(14) 0.0125(12) -0.0039(13) -0.0127(13) C32 0.0404(14) 0.0325(12) 0.0563(15) 0.0061(11) -0.0135(12) -0.0109(10) C33 0.0293(12) 0.0408(14) 0.0623(16) -0.0042(12) -0.0037(11) -0.0044(10) _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 Ni1 N1 1.9632(15) 7_564 ? Ni1 N1 1.9632(15) 14_566 ? Ni1 N1 1.9632(15) 12_767 ? Ni1 N1 1.9632(15) . ? N1 C4 1.387(2) . ? N1 C1 1.389(2) . ? C1 C5 1.364(2) 12_767 ? C1 C2 1.431(2) . ? C2 C3 1.346(2) . ? C2 C6 1.508(2) . ? C3 C4 1.435(2) . ? C3 C17 1.516(2) . ? C4 C5 1.373(2) . ? C5 C1 1.364(2) 14_566 ? C5 H1 0.9302 . ? C6 C7 1.525(2) . ? C6 C27 1.525(3) . ? C6 H2 0.9802 . ? C7 C8 1.367(3) . ? C7 C16 1.434(3) . ? C8 C9 1.417(3) . ? C8 H3 0.9499 . ? C9 C14 1.415(3) . ? C9 C10 1.427(3) . ? C10 C11 1.365(4) . ? C10 H4 0.929 . ? C11 C12 1.385(4) . ? C11 H5 0.930 . ? C12 C13 1.369(4) . ? C12 H6 0.930 . ? C13 C14 1.408(3) . ? C13 H7 0.930 . ? C14 C15 1.420(3) . ? C15 C16 1.361(3) . ? C15 H8 0.930 . ? C16 C17 1.527(3) . ? C17 C18 1.521(3) . ? C17 H9 0.9801 . ? C18 C19 1.365(3) . ? C18 C27 1.428(3) . ? C19 C20 1.418(3) . ? C19 H10 0.9302 . ? C20 C25 1.417(3) . ? C20 C21 1.423(3) . ? C21 C22 1.372(3) . ? C21 H11 0.930 . ? C22 C23 1.404(4) . ? C22 H12 0.931 . ? C23 C24 1.363(3) . ? C23 H13 0.930 . ? C24 C25 1.411(3) . ? C24 H14 0.930 . ? C25 C26 1.429(3) . ? C26 C27 1.374(3) . ? C26 H15 0.930 . ? C28 C33 1.363(4) . ? C28 C29 1.382(4) . ? C28 H16 0.931 . ? C29 C30 1.373(4) . ? C29 H17 0.931 . ? C30 C31 1.364(4) . ? C30 H18 0.930 . ? C31 C32 1.371(4) . ? C31 H19 0.931 . ? C32 C33 1.376(4) . ? C32 H20 0.930 . ? C33 H21 0.930 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 N1 90.039(2) 7_564 14_566 ? N1 Ni1 N1 90.039(3) 7_564 12_767 ? N1 Ni1 N1 177.03(8) 14_566 12_767 ? N1 Ni1 N1 177.03(8) 7_564 . ? N1 Ni1 N1 90.039(3) 14_566 . ? N1 Ni1 N1 90.039(2) 12_767 . ? C4 N1 C1 104.86(14) . . ? C4 N1 Ni1 127.84(12) . . ? C1 N1 Ni1 127.30(12) . . ? C5 C1 N1 125.45(17) 12_767 . ? C5 C1 C2 124.34(17) 12_767 . ? N1 C1 C2 110.13(16) . . ? C3 C2 C1 107.59(16) . . ? C3 C2 C6 115.50(16) . . ? C1 C2 C6 136.70(17) . . ? C2 C3 C4 107.08(16) . . ? C2 C3 C17 115.17(16) . . ? C4 C3 C17 137.46(16) . . ? C5 C4 N1 124.78(16) . . ? C5 C4 C3 124.90(17) . . ? N1 C4 C3 110.32(15) . . ? C1 C5 C4 124.47(17) 14_566 . ? C1 C5 H1 117.74 14_566 . ? C4 C5 H1 117.78 . . ? C2 C6 C7 104.28(14) . . ? C2 C6 C27 103.73(14) . . ? C7 C6 C27 105.23(15) . . ? C2 C6 H2 114.15 . . ? C7 C6 H2 114.15 . . ? C27 C6 H2 114.14 . . ? C8 C7 C16 119.92(17) . . ? C8 C7 C6 126.43(17) . . ? C16 C7 C6 113.65(16) . . ? C7 C8 C9 120.17(18) . . ? C7 C8 H3 119.95 . . ? C9 C8 H3 119.88 . . ? C14 C9 C8 119.72(18) . . ? C14 C9 C10 118.8(2) . . ? C8 C9 C10 121.5(2) . . ? C11 C10 C9 119.7(2) . . ? C11 C10 H4 120.1 . . ? C9 C10 H4 120.2 . . ? C10 C11 C12 121.6(2) . . ? C10 C11 H5 119.1 . . ? C12 C11 H5 119.3 . . ? C13 C12 C11 120.0(2) . . ? C13 C12 H6 120.1 . . ? C11 C12 H6 120.0 . . ? C12 C13 C14 120.9(2) . . ? C12 C13 H7 119.5 . . ? C14 C13 H7 119.6 . . ? C13 C14 C9 119.0(2) . . ? C13 C14 C15 121.8(2) . . ? C9 C14 C15 119.21(18) . . ? C16 C15 C14 120.08(19) . . ? C16 C15 H8 119.9 . . ? C14 C15 H8 120.0 . . ? C15 C16 C7 120.78(17) . . ? C15 C16 C17 126.32(17) . . ? C7 C16 C17 112.90(16) . . ? C3 C17 C18 104.09(14) . . ? C3 C17 C16 105.32(15) . . ? C18 C17 C16 104.68(14) . . ? C3 C17 H9 113.91 . . ? C18 C17 H9 113.88 . . ? C16 C17 H9 113.91 . . ? C19 C18 C27 121.12(17) . . ? C19 C18 C17 125.83(17) . . ? C27 C18 C17 113.05(16) . . ? C18 C19 C20 119.67(18) . . ? C18 C19 H10 120.16 . . ? C20 C19 H10 120.16 . . ? C25 C20 C19 119.74(18) . . ? C25 C20 C21 119.16(19) . . ? C19 C20 C21 121.10(19) . . ? C22 C21 C20 120.4(2) . . ? C22 C21 H11 119.8 . . ? C20 C21 H11 119.8 . . ? C21 C22 C23 120.2(2) . . ? C21 C22 H12 119.9 . . ? C23 C22 H12 119.9 . . ? C24 C23 C22 120.2(2) . . ? C24 C23 H13 119.9 . . ? C22 C23 H13 119.9 . . ? C23 C24 C25 121.6(2) . . ? C23 C24 H14 119.2 . . ? C25 C24 H14 119.2 . . ? C24 C25 C20 118.37(19) . . ? C24 C25 C26 121.95(19) . . ? C20 C25 C26 119.67(18) . . ? C27 C26 C25 119.42(18) . . ? C27 C26 H15 120.3 . . ? C25 C26 H15 120.27 . . ? C26 C27 C18 120.34(18) . . ? C26 C27 C6 125.80(17) . . ? C18 C27 C6 113.85(16) . . ? C33 C28 C29 119.9(3) . . ? C33 C28 H16 120.0 . . ? C29 C28 H16 120.1 . . ? C30 C29 C28 120.4(3) . . ? C30 C29 H17 119.8 . . ? C28 C29 H17 119.8 . . ? C31 C30 C29 119.1(3) . . ? C31 C30 H18 120.4 . . ? C29 C30 H18 120.4 . . ? C30 C31 C32 120.9(3) . . ? C30 C31 H19 119.5 . . ? C32 C31 H19 119.5 . . ? C31 C32 C33 119.8(2) . . ? C31 C32 H20 120.1 . . ? C33 C32 H20 120.1 . . ? C28 C33 C32 119.9(3) . . ? C28 C33 H21 120.0 . . ? C32 C33 H21 120.1 . . ? 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 N1 Ni1 N1 C4 -0.95(11) 14_566 . . . ? N1 Ni1 N1 C4 176.08(18) 12_767 . . . ? N1 Ni1 N1 C1 179.62(17) 14_566 . . . ? N1 Ni1 N1 C1 -3.35(11) 12_767 . . . ? C4 N1 C1 C5 -175.61(17) . . . 12_767 ? Ni1 N1 C1 C5 3.9(3) . . . 12_767 ? C4 N1 C1 C2 1.22(19) . . . . ? Ni1 N1 C1 C2 -179.25(11) . . . . ? C5 C1 C2 C3 176.59(17) 12_767 . . . ? N1 C1 C2 C3 -0.3(2) . . . . ? C5 C1 C2 C6 2.4(3) 12_767 . . . ? N1 C1 C2 C6 -174.43(19) . . . . ? C1 C2 C3 C4 -0.8(2) . . . . ? C6 C2 C3 C4 174.79(15) . . . . ? C1 C2 C3 C17 -175.69(15) . . . . ? C6 C2 C3 C17 -0.1(2) . . . . ? C1 N1 C4 C5 178.27(16) . . . . ? Ni1 N1 C4 C5 -1.3(3) . . . . ? C1 N1 C4 C3 -1.70(19) . . . . ? Ni1 N1 C4 C3 178.77(11) . . . . ? C2 C3 C4 C5 -178.38(17) . . . . ? C17 C3 C4 C5 -5.2(3) . . . . ? C2 C3 C4 N1 1.6(2) . . . . ? C17 C3 C4 N1 174.8(2) . . . . ? N1 C4 C5 C1 1.8(3) . . . 14_566 ? C3 C4 C5 C1 -178.26(17) . . . 14_566 ? C3 C2 C6 C7 55.0(2) . . . . ? C1 C2 C6 C7 -131.1(2) . . . . ? C3 C2 C6 C27 -54.9(2) . . . . ? C1 C2 C6 C27 118.9(2) . . . . ? C2 C6 C7 C8 124.6(2) . . . . ? C27 C6 C7 C8 -126.5(2) . . . . ? C2 C6 C7 C16 -55.1(2) . . . . ? C27 C6 C7 C16 53.76(19) . . . . ? C16 C7 C8 C9 -0.3(3) . . . . ? C6 C7 C8 C9 179.98(18) . . . . ? C7 C8 C9 C14 -2.6(3) . . . . ? C7 C8 C9 C10 175.9(2) . . . . ? C14 C9 C10 C11 -0.4(4) . . . . ? C8 C9 C10 C11 -178.9(2) . . . . ? C9 C10 C11 C12 -1.7(4) . . . . ? C10 C11 C12 C13 2.0(4) . . . . ? C11 C12 C13 C14 -0.2(4) . . . . ? C12 C13 C14 C9 -1.8(4) . . . . ? C12 C13 C14 C15 175.4(2) . . . . ? C8 C9 C14 C13 -179.4(2) . . . . ? C10 C9 C14 C13 2.0(3) . . . . ? C8 C9 C14 C15 3.4(3) . . . . ? C10 C9 C14 C15 -175.2(2) . . . . ? C13 C14 C15 C16 -178.4(2) . . . . ? C9 C14 C15 C16 -1.3(3) . . . . ? C14 C15 C16 C7 -1.7(3) . . . . ? C14 C15 C16 C17 178.37(18) . . . . ? C8 C7 C16 C15 2.6(3) . . . . ? C6 C7 C16 C15 -177.72(17) . . . . ? C8 C7 C16 C17 -177.52(17) . . . . ? C6 C7 C16 C17 2.2(2) . . . . ? C2 C3 C17 C18 55.5(2) . . . . ? C4 C3 C17 C18 -117.4(2) . . . . ? C2 C3 C17 C16 -54.4(2) . . . . ? C4 C3 C17 C16 132.8(2) . . . . ? C15 C16 C17 C3 -128.27(19) . . . . ? C7 C16 C17 C3 51.81(19) . . . . ? C15 C16 C17 C18 122.3(2) . . . . ? C7 C16 C17 C18 -57.63(19) . . . . ? C3 C17 C18 C19 127.05(19) . . . . ? C16 C17 C18 C19 -122.62(19) . . . . ? C3 C17 C18 C27 -53.75(19) . . . . ? C16 C17 C18 C27 56.58(19) . . . . ? C27 C18 C19 C20 1.6(3) . . . . ? C17 C18 C19 C20 -179.24(17) . . . . ? C18 C19 C20 C25 0.2(3) . . . . ? C18 C19 C20 C21 179.89(18) . . . . ? C25 C20 C21 C22 -0.6(3) . . . . ? C19 C20 C21 C22 179.7(2) . . . . ? C20 C21 C22 C23 0.5(3) . . . . ? C21 C22 C23 C24 -0.1(4) . . . . ? C22 C23 C24 C25 -0.1(4) . . . . ? C23 C24 C25 C20 0.0(3) . . . . ? C23 C24 C25 C26 -178.5(2) . . . . ? C19 C20 C25 C24 180.00(19) . . . . ? C21 C20 C25 C24 0.4(3) . . . . ? C19 C20 C25 C26 -1.4(3) . . . . ? C21 C20 C25 C26 178.92(18) . . . . ? C24 C25 C26 C27 179.27(19) . . . . ? C20 C25 C26 C27 0.8(3) . . . . ? C25 C26 C27 C18 1.1(3) . . . . ? C25 C26 C27 C6 179.74(17) . . . . ? C19 C18 C27 C26 -2.3(3) . . . . ? C17 C18 C27 C26 178.44(16) . . . . ? C19 C18 C27 C6 178.88(17) . . . . ? C17 C18 C27 C6 -0.4(2) . . . . ? C2 C6 C27 C26 -124.50(19) . . . . ? C7 C6 C27 C26 126.25(19) . . . . ? C2 C6 C27 C18 54.24(19) . . . . ? C7 C6 C27 C18 -55.01(19) . . . . ? C33 C28 C29 C30 0.5(5) . . . . ? C28 C29 C30 C31 -0.2(5) . . . . ? C29 C30 C31 C32 -0.5(5) . . . . ? C30 C31 C32 C33 1.0(4) . . . . ? C29 C28 C33 C32 0.0(4) . . . . ? C31 C32 C33 C28 -0.8(4) . . . . ? #============================================================================== data___12-7CH2Cl2-2PhHsqueezed(12-PhH) _database_code_depnum_ccdc_archive 'CCDC 248915' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C127 H88 Cl14 N4 ' _chemical_formula_moiety 'C108 H60 N4, 2(C6 H6), 7(C H2 Cl2)' _chemical_formula_weight 2166.46 _chemical_melting_point ? # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.2354(18) _cell_length_b 18.758(3) _cell_length_c 19.2789(17) _cell_angle_alpha 78.364(9) _cell_angle_beta 63.381(6) _cell_angle_gamma 88.391(10) _cell_volume 5127.9(10) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 13684 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description platelet _exptl_crystal_colour red _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.403 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2232 _exptl_absorpt_coefficient_mu 0.432 _exptl_absorpt_correction_T_min 0.7814 _exptl_absorpt_correction_T_max 0.9580 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Higashi, T. (1999). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoKa _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method w _diffrn_detector_area_resol_mean 7.31 _diffrn_radiation_monochromator graphite _diffrn_reflns_number 104772 _diffrn_reflns_av_R_equivalents 0.066 _diffrn_reflns_av_sigmaI/netI 0.1819 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.969 _reflns_number_total 22806 _reflns_number_gt 10520 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR97 _computing_publication_material 'CrystalStructure Ver. 3.5.1' _computing_structure_refinement 'SHELXL-97 and PLATON SQUEEZE' _computing_molecular_graphics ? _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^)+(0.0600P)^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 noref _refine_ls_number_reflns 22806 _refine_ls_number_parameters 1063 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1245 _refine_ls_R_factor_gt 0.0844 _refine_ls_wR_factor_ref 0.2006 _refine_ls_wR_factor_gt 0.1909 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.473 _refine_diff_density_min -0.495 _refine_diff_density_rms 0.069 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 N1 N 0.53915(17) 0.51740(13) 0.58545(15) 0.0191(5) Uani 1 1 d . . . N2 N 0.49013(17) 0.38956(13) 0.53687(15) 0.0195(5) Uani 1 1 d . . . N3 N 0.94544(18) 0.07754(14) 0.56537(17) 0.0242(6) Uani 1 1 d . . . N4 N 0.96604(17) 0.06067(13) 0.41292(15) 0.0201(5) Uani 1 1 d . . . C1 C 0.5570(2) 0.58291(16) 0.59978(18) 0.0200(6) Uani 1 1 d . . . C2 C 0.5806(2) 0.56694(16) 0.66349(18) 0.0206(6) Uani 1 1 d . . . C3 C 0.5797(2) 0.49230(16) 0.68342(17) 0.0190(6) Uani 1 1 d . . . C4 C 0.5517(2) 0.46073(16) 0.63608(18) 0.0184(6) Uani 1 1 d . . . C5 C 0.5358(2) 0.38684(15) 0.64264(17) 0.0172(6) Uani 1 1 d . . . C6 C 0.5038(2) 0.35424(16) 0.59954(18) 0.0204(6) Uani 1 1 d . . . C7 C 0.4837(2) 0.27650(17) 0.6136(2) 0.0237(7) Uani 1 1 d . . . C8 C 0.4552(2) 0.26562(17) 0.5607(2) 0.0249(7) Uani 1 1 d . . . C9 C 0.4619(2) 0.33621(16) 0.51054(18) 0.0195(6) Uani 1 1 d . . . C10 C 0.4428(2) 0.34869(16) 0.44620(19) 0.0219(6) Uani 1 1 d . . . C11 C 0.6061(2) 0.60706(16) 0.71272(18) 0.0210(6) Uani 1 1 d . . . C12 C 0.6997(2) 0.58111(17) 0.70378(18) 0.0225(7) Uani 1 1 d . . . C13 C 0.7774(2) 0.62596(18) 0.68093(18) 0.0243(7) Uani 1 1 d . . . C14 C 0.8594(2) 0.59397(19) 0.67773(19) 0.0272(7) Uani 1 1 d . . . C15 C 0.9404(2) 0.6375(2) 0.6555(2) 0.0353(9) Uani 1 1 d . . . C16 C 1.0174(3) 0.6056(2) 0.6527(2) 0.0423(10) Uani 1 1 d . . . C17 C 1.0191(2) 0.5311(3) 0.6726(3) 0.0448(11) Uani 1 1 d . . . C18 C 0.9416(2) 0.4866(2) 0.6944(2) 0.0372(9) Uani 1 1 d . . . C19 C 0.8609(2) 0.51652(19) 0.6962(2) 0.0275(7) Uani 1 1 d . . . C20 C 0.7791(2) 0.47222(18) 0.71754(18) 0.0234(7) Uani 1 1 d . . . C21 C 0.7008(2) 0.50405(17) 0.72171(18) 0.0218(6) Uani 1 1 d . . . C22 C 0.6071(2) 0.46454(16) 0.74943(17) 0.0186(6) Uani 1 1 d . . . C23 C 0.5399(2) 0.49720(16) 0.81843(19) 0.0208(6) Uani 1 1 d . . . C24 C 0.4858(2) 0.45925(17) 0.89356(19) 0.0232(7) Uani 1 1 d . . . C25 C 0.4285(2) 0.49586(19) 0.9531(2) 0.0264(7) Uani 1 1 d . . . C26 C 0.3710(2) 0.4598(2) 1.0324(2) 0.0333(8) Uani 1 1 d . . . C27 C 0.3178(3) 0.4951(2) 1.0894(2) 0.0412(10) Uani 1 1 d . . . C28 C 0.3199(3) 0.5708(3) 1.0709(2) 0.0401(9) Uani 1 1 d . . . C29 C 0.3731(3) 0.6102(2) 0.9943(2) 0.0400(9) Uani 1 1 d . . . C30 C 0.4281(2) 0.57389(19) 0.9341(2) 0.0289(7) Uani 1 1 d . . . C31 C 0.4849(2) 0.61135(18) 0.8547(2) 0.0253(7) Uani 1 1 d . . . C32 C 0.5393(2) 0.57382(17) 0.79827(19) 0.0219(6) Uani 1 1 d . . . C33 C 0.4817(2) 0.20880(17) 0.67312(18) 0.0241(7) Uani 1 1 d . . . C34 C 0.5373(2) 0.15494(17) 0.6231(2) 0.0263(7) Uani 1 1 d . . . C35 C 0.6083(2) 0.11986(18) 0.6277(2) 0.0289(7) Uani 1 1 d . . . C36 C 0.6540(2) 0.06853(17) 0.5769(2) 0.0270(7) Uani 1 1 d . . . C37 C 0.7267(2) 0.02930(19) 0.5830(2) 0.0351(8) Uani 1 1 d . . . C38 C 0.7683(3) -0.01758(19) 0.5349(2) 0.0368(9) Uani 1 1 d . . . C39 C 0.7394(3) -0.02783(19) 0.4778(2) 0.0423(10) Uani 1 1 d . . . C40 C 0.6690(3) 0.00957(19) 0.4698(2) 0.0370(8) Uani 1 1 d . . . C41 C 0.6232(2) 0.05695(18) 0.5225(2) 0.0306(8) Uani 1 1 d . . . C42 C 0.5467(2) 0.09489(17) 0.5192(2) 0.0289(7) Uani 1 1 d . . . C43 C 0.5057(2) 0.14226(17) 0.56661(19) 0.0247(7) Uani 1 1 d . . . C44 C 0.4236(2) 0.18744(17) 0.57062(19) 0.0262(7) Uani 1 1 d . . . C45 C 0.3499(2) 0.16684(17) 0.6558(2) 0.0262(7) Uani 1 1 d . . . C46 C 0.2598(2) 0.14227(18) 0.6831(2) 0.0321(8) Uani 1 1 d . . . C47 C 0.2001(2) 0.12518(18) 0.7646(2) 0.0315(8) Uani 1 1 d . . . C48 C 0.1046(3) 0.1005(2) 0.7947(3) 0.0492(11) Uani 1 1 d . . . C49 C 0.0481(3) 0.0831(3) 0.8750(4) 0.0670(15) Uani 1 1 d . . . C50 C 0.0834(3) 0.0872(2) 0.9289(3) 0.0592(13) Uani 1 1 d . . . C51 C 0.1718(3) 0.1093(2) 0.9048(3) 0.0475(10) Uani 1 1 d . . . C52 C 0.2329(3) 0.13112(19) 0.8203(2) 0.0384(9) Uani 1 1 d . . . C53 C 0.3259(3) 0.15700(18) 0.7916(2) 0.0325(8) Uani 1 1 d . . . C54 C 0.3824(2) 0.17610(16) 0.7126(2) 0.0235(7) Uani 1 1 d . . . C55 C 0.9472(2) 0.07935(16) 0.63511(19) 0.0209(6) Uani 1 1 d . . . C56 C 0.9095(2) 0.14535(17) 0.66065(19) 0.0253(7) Uani 1 1 d . . . C57 C 0.8831(2) 0.18267(17) 0.60784(19) 0.0224(6) Uani 1 1 d . . . C58 C 0.9077(2) 0.14006(16) 0.54629(19) 0.0206(6) Uani 1 1 d . . . C59 C 0.8957(2) 0.16236(16) 0.47849(19) 0.0216(6) Uani 1 1 d . . . C60 C 0.9222(2) 0.12538(17) 0.41662(18) 0.0214(6) Uani 1 1 d . . . C61 C 0.9078(2) 0.14190(17) 0.34759(19) 0.0238(7) Uani 1 1 d . . . C62 C 0.9431(2) 0.08946(17) 0.30522(19) 0.0228(7) Uani 1 1 d . . . C63 C 0.9792(2) 0.03695(17) 0.3455(2) 0.0234(7) Uani 1 1 d . . . C64 C 1.0183(2) -0.02653(17) 0.32382(19) 0.0227(7) Uani 1 1 d . . . C65 C 0.9048(2) 0.18630(16) 0.7235(2) 0.0244(7) Uani 1 1 d . . . C66 C 0.8052(2) 0.20743(18) 0.7630(2) 0.0300(8) Uani 1 1 d . . . C67 C 0.7484(3) 0.19358(19) 0.8410(2) 0.0329(8) Uani 1 1 d . . . C68 C 0.6569(2) 0.21289(19) 0.8690(2) 0.0322(8) Uani 1 1 d . . . C69 C 0.5943(3) 0.1966(2) 0.9519(2) 0.0409(9) Uani 1 1 d . . . C70 C 0.5037(3) 0.2140(2) 0.9789(2) 0.0413(9) Uani 1 1 d . . . C71 C 0.4708(3) 0.2489(2) 0.9239(2) 0.0400(9) Uani 1 1 d . . . C72 C 0.5301(3) 0.2641(2) 0.8447(2) 0.0355(8) Uani 1 1 d . . . C73 C 0.6243(2) 0.24825(18) 0.8148(2) 0.0299(7) Uani 1 1 d . . . C74 C 0.6867(2) 0.26457(18) 0.7323(2) 0.0258(7) Uani 1 1 d . . . C75 C 0.7756(2) 0.24473(17) 0.7065(2) 0.0268(7) Uani 1 1 d . . . C76 C 0.8512(2) 0.25729(17) 0.62027(19) 0.0246(7) Uani 1 1 d . . . C77 C 0.9353(2) 0.29572(17) 0.6174(2) 0.0264(7) Uani 1 1 d . . . C78 C 0.9843(2) 0.35695(18) 0.5654(2) 0.0290(7) Uani 1 1 d . . . C79 C 1.0673(2) 0.3825(2) 0.5629(2) 0.0328(8) Uani 1 1 d . . . C80 C 1.1246(3) 0.4431(2) 0.5070(2) 0.0404(9) Uani 1 1 d . . . C81 C 1.2047(3) 0.4633(2) 0.5046(2) 0.0424(10) Uani 1 1 d . . . C82 C 1.2337(3) 0.4256(3) 0.5614(3) 0.0531(13) Uani 1 1 d . . . C83 C 1.1793(3) 0.3686(2) 0.6174(3) 0.0438(10) Uani 1 1 d . . . C84 C 1.0959(2) 0.34367(19) 0.6197(2) 0.0305(8) Uani 1 1 d . . . C85 C 1.0421(2) 0.2804(2) 0.6752(2) 0.0324(8) Uani 1 1 d . . . C86 C 0.9639(2) 0.25758(19) 0.6731(2) 0.0302(8) Uani 1 1 d . . . C87 C 0.8672(2) 0.20338(16) 0.31037(19) 0.0228(7) Uani 1 1 d . . . C88 C 0.7946(2) 0.16484(18) 0.29807(19) 0.0276(7) Uani 1 1 d . . . C89 C 0.7052(2) 0.18049(19) 0.3221(2) 0.0310(8) Uani 1 1 d . . . C90 C 0.6455(3) 0.1385(2) 0.3066(2) 0.0334(8) Uani 1 1 d . . . C91 C 0.5505(3) 0.1510(2) 0.3331(2) 0.0390(9) Uani 1 1 d . . . C92 C 0.4947(3) 0.1061(3) 0.3196(3) 0.0547(13) Uani 1 1 d . . . C93 C 0.5300(3) 0.0515(2) 0.2796(3) 0.0469(10) Uani 1 1 d . . . C94 C 0.6204(3) 0.0380(2) 0.2522(2) 0.0396(9) Uani 1 1 d . . . C95 C 0.6800(3) 0.08104(19) 0.2665(2) 0.0337(8) Uani 1 1 d . . . C96 C 0.7751(3) 0.06724(18) 0.2389(2) 0.0301(8) Uani 1 1 d . . . C97 C 0.8308(2) 0.10767(17) 0.2544(2) 0.0258(7) Uani 1 1 d . . . C98 C 0.9331(2) 0.10006(16) 0.22884(19) 0.0237(7) Uani 1 1 d . . . C99 C 0.9824(2) 0.17602(17) 0.18297(19) 0.0234(7) Uani 1 1 d . . . C100 C 1.0559(2) 0.19058(19) 0.1094(2) 0.0311(8) Uani 1 1 d . . . C101 C 1.0991(2) 0.2639(2) 0.0757(2) 0.0338(8) Uani 1 1 d . . . C102 C 1.1790(3) 0.2812(2) 0.0039(3) 0.0495(11) Uani 1 1 d . . . C103 C 1.2206(3) 0.3509(3) -0.0255(3) 0.0579(13) Uani 1 1 d . . . C104 C 1.1834(3) 0.4060(2) 0.0174(3) 0.0500(11) Uani 1 1 d . . . C105 C 1.1069(3) 0.3899(2) 0.0876(3) 0.0474(11) Uani 1 1 d . . . C106 C 1.0626(3) 0.3186(2) 0.1194(2) 0.0357(9) Uani 1 1 d . . . C107 C 0.9834(2) 0.30050(18) 0.1960(2) 0.0293(8) Uani 1 1 d . . . C108 C 0.9469(2) 0.23109(18) 0.2267(2) 0.0250(7) Uani 1 1 d . . . C109 C 0.3605(3) 0.1995(2) 0.2087(2) 0.0430(9) Uani 1 1 d . . . C110 C 0.3307(3) 0.2582(2) 0.1727(3) 0.0414(9) Uani 1 1 d . . . C111 C 0.2416(4) 0.2596(3) 0.1846(3) 0.0581(13) Uani 1 1 d . . . C112 C 0.1793(4) 0.2056(5) 0.2326(5) 0.113(3) Uani 1 1 d . . . C113 C 0.2036(5) 0.1495(5) 0.2764(5) 0.125(3) Uani 1 1 d . . . C114 C 0.2971(4) 0.1435(3) 0.2592(4) 0.090(2) Uani 1 1 d . . . H1 H 0.5208 0.5124 0.5462 0.023 Uiso 0.50 1 c P . . H2 H 0.4983 0.4406 0.5156 0.023 Uiso 0.50 1 c P . . H3 H 0.9664 0.0402 0.5358 0.029 Uiso 0.50 1 c P . . H4 H 0.9845 0.0361 0.4513 0.024 Uiso 0.50 1 c P . . H5 H 0.5484 0.3546 0.6811 0.021 Uiso 1 1 c . . . H6 H 0.6056 0.6586 0.6991 0.025 Uiso 1 1 c . . . H7 H 0.7762 0.6775 0.6676 0.029 Uiso 1 1 c . . . H8 H 0.9409 0.6892 0.6424 0.042 Uiso 1 1 c . . . H9 H 1.0718 0.6356 0.6366 0.051 Uiso 1 1 c . . . H10 H 1.0737 0.5103 0.6713 0.054 Uiso 1 1 c . . . H11 H 0.9430 0.4352 0.7083 0.045 Uiso 1 1 c . . . H12 H 0.7794 0.4206 0.7288 0.028 Uiso 1 1 c . . . H13 H 0.6070 0.4129 0.7623 0.022 Uiso 1 1 c . . . H14 H 0.4867 0.4077 0.9059 0.028 Uiso 1 1 c . . . H15 H 0.3700 0.4081 1.0459 0.040 Uiso 1 1 c . . . H16 H 0.2793 0.4687 1.1416 0.049 Uiso 1 1 c . . . H17 H 0.2842 0.5961 1.1115 0.048 Uiso 1 1 c . . . H18 H 0.3723 0.6618 0.9827 0.048 Uiso 1 1 c . . . H19 H 0.4850 0.6629 0.8407 0.030 Uiso 1 1 c . . . H20 H 0.5027 0.2181 0.7094 0.029 Uiso 1 1 c . . . H21 H 0.6290 0.1285 0.6644 0.034 Uiso 1 1 c . . . H22 H 0.7465 0.0359 0.6209 0.042 Uiso 1 1 c . . . H23 H 0.8173 -0.0439 0.5392 0.044 Uiso 1 1 c . . . H24 H 0.7693 -0.0612 0.4446 0.051 Uiso 1 1 c . . . H25 H 0.6515 0.0039 0.4303 0.044 Uiso 1 1 c . . . H26 H 0.5247 0.0866 0.4832 0.034 Uiso 1 1 c . . . H27 H 0.4029 0.1810 0.5332 0.031 Uiso 1 1 c . . . H28 H 0.2377 0.1368 0.6463 0.038 Uiso 1 1 c . . . H29 H 0.0806 0.0964 0.7588 0.059 Uiso 1 1 c . . . H30 H -0.0151 0.0682 0.8943 0.080 Uiso 1 1 c . . . H31 H 0.0433 0.0737 0.9843 0.071 Uiso 1 1 c . . . H32 H 0.1940 0.1108 0.9424 0.057 Uiso 1 1 c . . . H33 H 0.3489 0.1610 0.8281 0.039 Uiso 1 1 c . . . H34 H 0.8669 0.2067 0.4738 0.026 Uiso 1 1 c . . . H35 H 0.9250 0.1597 0.7598 0.029 Uiso 1 1 c . . . H36 H 0.7703 0.1705 0.8775 0.039 Uiso 1 1 c . . . H37 H 0.6156 0.1735 0.9889 0.049 Uiso 1 1 c . . . H38 H 0.4631 0.2030 1.0342 0.050 Uiso 1 1 c . . . H39 H 0.4085 0.2612 0.9422 0.048 Uiso 1 1 c . . . H40 H 0.5076 0.2861 0.8083 0.043 Uiso 1 1 c . . . H41 H 0.6665 0.2893 0.6951 0.031 Uiso 1 1 c . . . H42 H 0.8318 0.2822 0.5827 0.030 Uiso 1 1 c . . . H43 H 0.9628 0.3834 0.5300 0.035 Uiso 1 1 c . . . H44 H 1.1060 0.4706 0.4700 0.048 Uiso 1 1 c . . . H45 H 1.2428 0.5032 0.4645 0.051 Uiso 1 1 c . . . H46 H 1.2902 0.4405 0.5597 0.063 Uiso 1 1 c . . . H47 H 1.1971 0.3444 0.6564 0.053 Uiso 1 1 c . . . H48 H 1.0601 0.2544 0.7133 0.039 Uiso 1 1 c . . . H49 H 0.8441 0.2402 0.3403 0.027 Uiso 1 1 c . . . H50 H 0.6823 0.2192 0.3492 0.037 Uiso 1 1 c . . . H51 H 0.5252 0.1896 0.3598 0.047 Uiso 1 1 c . . . H52 H 0.4308 0.1138 0.3385 0.065 Uiso 1 1 c . . . H53 H 0.4902 0.0222 0.2709 0.056 Uiso 1 1 c . . . H54 H 0.6438 0.0003 0.2238 0.047 Uiso 1 1 c . . . H55 H 0.7995 0.0300 0.2097 0.036 Uiso 1 1 c . . . H56 H 0.9573 0.0625 0.2002 0.028 Uiso 1 1 c . . . H57 H 1.0785 0.1530 0.0805 0.037 Uiso 1 1 c . . . H58 H 1.2053 0.2442 -0.0253 0.059 Uiso 1 1 c . . . H59 H 1.2746 0.3618 -0.0751 0.069 Uiso 1 1 c . . . H60 H 1.2120 0.4541 -0.0030 0.060 Uiso 1 1 c . . . H61 H 1.0822 0.4272 0.1164 0.057 Uiso 1 1 c . . . H62 H 0.9569 0.3375 0.2249 0.035 Uiso 1 1 c . . . H63 H 0.4233 0.1980 0.1987 0.051 Uiso 1 1 c . . . H64 H 0.3732 0.2987 0.1388 0.050 Uiso 1 1 c . . . H65 H 0.2237 0.3005 0.1576 0.070 Uiso 1 1 c . . . H66 H 0.1186 0.2057 0.2371 0.134 Uiso 1 1 c . . . H67 H 0.1572 0.1153 0.3183 0.149 Uiso 1 1 c . . . H68 H 0.3158 0.1007 0.2825 0.107 Uiso 1 1 c . . . H69 H 0.4283 0.3070 0.4317 0.026 Uiso 1 1 c . . . H70 H 1.0221 -0.0354 0.2757 0.027 Uiso 1 1 c . . . 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 N1 0.0246(13) 0.0123(12) 0.0244(14) -0.0042(10) -0.0144(11) 0.0013(10) N2 0.0236(13) 0.0125(12) 0.0251(14) -0.0047(10) -0.0133(11) 0.0041(10) N3 0.0235(14) 0.0197(14) 0.0371(17) -0.0074(12) -0.0199(13) 0.0039(10) N4 0.0233(13) 0.0181(13) 0.0220(14) -0.0016(10) -0.0139(11) 0.0008(10) C1 0.0244(16) 0.0201(15) 0.0219(16) -0.0061(12) -0.0155(13) 0.0042(12) C2 0.0247(16) 0.0199(16) 0.0183(16) -0.0047(12) -0.0103(13) 0.0010(12) C3 0.0189(15) 0.0214(16) 0.0146(15) -0.0014(12) -0.0066(12) 0.0015(12) C4 0.0190(14) 0.0194(15) 0.0184(15) -0.0054(12) -0.0094(12) 0.0024(11) C5 0.0258(16) 0.0110(14) 0.0180(15) -0.0020(11) -0.0134(13) 0.0038(11) C6 0.0238(16) 0.0181(15) 0.0213(16) -0.0031(12) -0.0127(13) 0.0069(12) C7 0.0275(17) 0.0177(16) 0.0326(19) -0.0037(13) -0.0200(15) 0.0010(12) C8 0.0273(17) 0.0144(15) 0.0319(19) -0.0033(13) -0.0130(15) 0.0006(12) C9 0.0229(15) 0.0155(15) 0.0200(16) 0.0019(12) -0.0119(13) -0.0017(11) C10 0.0259(16) 0.0162(15) 0.0277(18) -0.0061(13) -0.0153(14) 0.0043(12) C11 0.0319(17) 0.0117(14) 0.0169(15) -0.0014(12) -0.0096(13) 0.0008(12) C12 0.0328(17) 0.0228(16) 0.0125(15) -0.0025(12) -0.0109(13) -0.0035(13) C13 0.0300(17) 0.0272(17) 0.0147(15) -0.0039(13) -0.0091(13) -0.0040(13) C14 0.0261(17) 0.0360(19) 0.0210(17) -0.0156(15) -0.0078(14) -0.0016(14) C15 0.0303(19) 0.044(2) 0.037(2) -0.0245(18) -0.0132(16) -0.0013(16) C16 0.032(2) 0.063(3) 0.040(2) -0.032(2) -0.0145(18) 0.0060(18) C17 0.0218(19) 0.074(3) 0.052(3) -0.035(2) -0.0199(18) 0.0172(19) C18 0.0310(19) 0.051(2) 0.047(2) -0.035(2) -0.0231(18) 0.0205(17) C19 0.0276(17) 0.039(2) 0.0245(18) -0.0162(15) -0.0153(15) 0.0082(14) C20 0.0299(17) 0.0275(17) 0.0184(16) -0.0131(13) -0.0127(14) 0.0080(13) C21 0.0341(18) 0.0219(16) 0.0185(16) -0.0095(13) -0.0179(14) 0.0039(13) C22 0.0275(16) 0.0160(15) 0.0162(15) -0.0010(11) -0.0141(13) -0.0005(12) C23 0.0196(15) 0.0220(16) 0.0297(18) -0.0093(13) -0.0173(14) 0.0012(12) C24 0.0300(17) 0.0227(16) 0.0237(17) -0.0015(13) -0.0192(14) -0.0018(13) C25 0.0185(15) 0.038(2) 0.0273(18) -0.0114(15) -0.0123(14) -0.0021(13) C26 0.0292(18) 0.050(2) 0.0224(18) 0.0001(16) -0.0160(15) -0.0099(16) C27 0.033(2) 0.066(3) 0.0177(18) -0.0059(18) -0.0055(16) -0.0098(18) C28 0.033(2) 0.070(3) 0.0168(18) -0.0158(18) -0.0084(15) 0.0084(18) C29 0.040(2) 0.056(3) 0.036(2) -0.0284(19) -0.0205(18) 0.0127(18) C30 0.0294(18) 0.036(2) 0.0268(18) -0.0052(15) -0.0179(15) 0.0051(14) C31 0.0294(17) 0.0259(17) 0.0264(18) -0.0078(14) -0.0168(15) 0.0035(13) C32 0.0229(16) 0.0226(16) 0.0224(16) -0.0055(13) -0.0116(13) -0.0014(12) C33 0.0411(19) 0.0181(16) 0.0151(15) 0.0015(12) -0.0161(14) -0.0044(13) C34 0.0350(18) 0.0192(16) 0.0244(18) 0.0012(13) -0.0151(15) -0.0030(13) C35 0.0379(19) 0.0215(17) 0.033(2) -0.0003(14) -0.0231(17) -0.0027(14) C36 0.0296(18) 0.0157(16) 0.0300(19) 0.0010(13) -0.0105(15) -0.0056(13) C37 0.0338(19) 0.0240(18) 0.043(2) 0.0033(16) -0.0172(17) -0.0043(14) C38 0.038(2) 0.0187(17) 0.046(2) 0.0055(16) -0.0180(18) 0.0032(14) C39 0.048(2) 0.0183(18) 0.043(2) -0.0046(16) -0.0058(19) 0.0019(16) C40 0.050(2) 0.0182(17) 0.031(2) 0.0032(15) -0.0108(18) -0.0033(15) C41 0.0338(19) 0.0184(17) 0.035(2) -0.0009(14) -0.0129(16) 0.0003(13) C42 0.045(2) 0.0160(16) 0.0291(19) 0.0002(13) -0.0217(16) -0.0039(14) C43 0.0365(18) 0.0182(16) 0.0250(17) 0.0020(13) -0.0210(15) -0.0044(13) C44 0.045(2) 0.0187(16) 0.0240(17) -0.0019(13) -0.0240(16) 0.0020(14) C45 0.0387(19) 0.0135(15) 0.0281(18) -0.0009(13) -0.0181(16) 0.0032(13) C46 0.041(2) 0.0157(16) 0.046(2) -0.0119(15) -0.0222(18) -0.0014(14) C47 0.0292(18) 0.0213(17) 0.034(2) -0.0023(14) -0.0064(15) -0.0008(13) C48 0.039(2) 0.029(2) 0.076(3) -0.022(2) -0.019(2) 0.0073(17) C49 0.043(3) 0.039(3) 0.087(4) -0.015(3) -0.001(3) 0.004(2) C50 0.060(3) 0.040(3) 0.047(3) -0.008(2) 0.004(2) -0.010(2) C51 0.054(3) 0.029(2) 0.042(2) -0.0095(18) -0.006(2) 0.0025(18) C52 0.045(2) 0.0182(18) 0.048(2) -0.0075(16) -0.0174(19) 0.0020(15) C53 0.047(2) 0.0193(17) 0.033(2) -0.0021(14) -0.0204(17) 0.0011(15) C54 0.0337(18) 0.0117(14) 0.0324(19) -0.0036(13) -0.0219(15) 0.0048(12) C55 0.0272(16) 0.0151(15) 0.0253(17) -0.0024(12) -0.0168(14) 0.0010(12) C56 0.0353(18) 0.0192(16) 0.0223(17) -0.0014(13) -0.0148(15) -0.0005(13) C57 0.0236(16) 0.0211(16) 0.0208(16) -0.0036(13) -0.0089(13) 0.0024(12) C58 0.0214(15) 0.0182(15) 0.0258(17) -0.0027(12) -0.0147(13) 0.0010(12) C59 0.0261(16) 0.0128(14) 0.0271(17) -0.0032(12) -0.0135(14) 0.0043(12) C60 0.0251(16) 0.0215(16) 0.0196(16) -0.0023(12) -0.0127(13) 0.0066(12) C61 0.0294(17) 0.0189(16) 0.0244(17) 0.0015(13) -0.0158(14) 0.0007(12) C62 0.0252(16) 0.0220(16) 0.0283(18) -0.0043(13) -0.0187(14) 0.0030(12) C63 0.0219(16) 0.0226(16) 0.0313(18) -0.0048(13) -0.0172(14) 0.0000(12) C64 0.0215(16) 0.0242(17) 0.0245(17) -0.0092(13) -0.0107(13) 0.0053(12) C65 0.0383(19) 0.0159(15) 0.0299(18) -0.0043(13) -0.0253(16) 0.0043(13) C66 0.0347(19) 0.0249(18) 0.039(2) -0.0130(15) -0.0221(17) 0.0056(14) C67 0.041(2) 0.0313(19) 0.031(2) -0.0027(15) -0.0224(17) 0.0063(15) C68 0.0346(19) 0.0238(18) 0.038(2) -0.0040(15) -0.0169(17) 0.0032(14) C69 0.049(2) 0.044(2) 0.027(2) -0.0080(17) -0.0142(18) 0.0093(18) C70 0.050(2) 0.045(2) 0.024(2) -0.0108(17) -0.0113(18) 0.0071(18) C71 0.038(2) 0.035(2) 0.040(2) -0.0098(17) -0.0114(18) 0.0029(16) C72 0.040(2) 0.0262(19) 0.039(2) -0.0069(16) -0.0173(18) 0.0038(15) C73 0.0339(19) 0.0219(17) 0.035(2) -0.0084(15) -0.0161(16) 0.0028(14) C74 0.0272(17) 0.0228(17) 0.0282(18) -0.0056(14) -0.0132(15) 0.0023(13) C75 0.0384(19) 0.0207(16) 0.0284(18) -0.0042(14) -0.0219(16) 0.0055(14) C76 0.0315(17) 0.0232(17) 0.0263(18) -0.0114(14) -0.0169(15) 0.0069(13) C77 0.0358(18) 0.0171(16) 0.0342(19) -0.0195(14) -0.0172(16) 0.0097(13) C78 0.0381(19) 0.0240(18) 0.0289(19) -0.0130(15) -0.0159(16) 0.0088(14) C79 0.0360(19) 0.031(2) 0.0275(19) -0.0196(16) -0.0060(15) 0.0074(15) C80 0.049(2) 0.033(2) 0.031(2) -0.0187(17) -0.0053(18) -0.0033(17) C81 0.034(2) 0.043(2) 0.035(2) -0.0159(18) 0.0010(17) -0.0116(17) C82 0.030(2) 0.057(3) 0.064(3) -0.044(3) -0.001(2) -0.0075(19) C83 0.033(2) 0.056(3) 0.057(3) -0.040(2) -0.022(2) 0.0107(19) C84 0.0329(19) 0.0299(19) 0.0309(19) -0.0181(15) -0.0117(16) 0.0063(14) C85 0.0285(18) 0.036(2) 0.042(2) -0.0170(17) -0.0210(17) 0.0109(15) C86 0.0349(19) 0.0283(18) 0.034(2) -0.0161(15) -0.0178(16) 0.0113(14) C87 0.0289(17) 0.0152(15) 0.0286(18) -0.0049(13) -0.0169(14) 0.0080(12) C88 0.0348(19) 0.0273(18) 0.0216(17) 0.0036(14) -0.0169(15) -0.0001(14) C89 0.0341(19) 0.0329(19) 0.0277(19) -0.0037(15) -0.0171(16) 0.0107(15) C90 0.039(2) 0.034(2) 0.031(2) 0.0060(15) -0.0233(17) 0.0020(15) C91 0.035(2) 0.049(2) 0.032(2) -0.0032(17) -0.0160(17) 0.0036(17) C92 0.030(2) 0.086(4) 0.042(3) 0.008(2) -0.0190(19) -0.011(2) C93 0.052(3) 0.036(2) 0.054(3) 0.003(2) -0.028(2) -0.0148(19) C94 0.043(2) 0.030(2) 0.050(3) 0.0058(17) -0.030(2) -0.0071(16) C95 0.043(2) 0.0280(19) 0.034(2) 0.0091(15) -0.0264(18) -0.0060(15) C96 0.047(2) 0.0184(16) 0.033(2) 0.0016(14) -0.0279(17) 0.0010(14) C97 0.0337(18) 0.0194(16) 0.0261(18) 0.0023(13) -0.0182(15) 0.0037(13) C98 0.0364(18) 0.0166(15) 0.0254(17) -0.0014(13) -0.0218(15) 0.0056(13) C99 0.0328(18) 0.0213(16) 0.0248(17) -0.0028(13) -0.0215(15) 0.0022(13) C100 0.0346(19) 0.0300(19) 0.031(2) -0.0097(15) -0.0156(16) 0.0099(15) C101 0.0299(18) 0.036(2) 0.040(2) -0.0024(16) -0.0227(17) 0.0049(15) C102 0.044(2) 0.052(3) 0.040(2) 0.007(2) -0.016(2) 0.000(2) C103 0.046(3) 0.066(3) 0.056(3) 0.018(2) -0.029(2) -0.013(2) C104 0.047(2) 0.033(2) 0.067(3) 0.011(2) -0.030(2) -0.0123(18) C105 0.047(2) 0.037(2) 0.062(3) 0.012(2) -0.036(2) -0.0103(18) C106 0.038(2) 0.034(2) 0.041(2) 0.0027(17) -0.0270(18) -0.0037(16) C107 0.041(2) 0.0230(18) 0.035(2) -0.0102(15) -0.0251(17) 0.0075(14) C108 0.0264(17) 0.0253(17) 0.0302(18) -0.0040(14) -0.0198(15) 0.0066(13) C109 0.041(2) 0.050(3) 0.035(2) -0.0052(18) -0.0162(18) -0.0016(18) C110 0.037(2) 0.045(2) 0.050(3) -0.0090(19) -0.027(2) 0.0017(17) C111 0.063(3) 0.059(3) 0.073(4) -0.024(3) -0.045(3) 0.017(2) C112 0.054(4) 0.147(7) 0.143(7) 0.015(5) -0.068(4) -0.021(4) C113 0.102(5) 0.146(7) 0.121(6) 0.064(5) -0.077(5) -0.080(5) C114 0.094(4) 0.082(4) 0.104(5) 0.041(3) -0.076(4) -0.049(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 N1 C4 1.368(4) . ? N1 C1 1.378(4) . ? N1 H1 0.950 . ? N2 C6 1.363(4) . ? N2 C9 1.381(4) . ? N2 H2 0.950 . ? N3 C55 1.365(4) . ? N3 C58 1.369(4) . ? N3 H3 0.950 . ? N4 C63 1.383(4) . ? N4 C60 1.388(4) . ? N4 H4 0.950 . ? C1 C10 1.404(4) 2_666 ? C1 C2 1.419(4) . ? C2 C3 1.374(4) . ? C2 C11 1.515(4) . ? C3 C4 1.413(4) . ? C3 C22 1.522(4) . ? C4 C5 1.387(4) . ? C5 C6 1.395(4) . ? C5 H5 0.950 . ? C6 C7 1.447(4) . ? C7 C8 1.344(4) . ? C7 C33 1.520(4) . ? C8 C9 1.448(4) . ? C8 C44 1.514(4) . ? C9 C10 1.383(4) . ? C10 C1 1.404(4) 2_666 ? C10 H69 0.950 . ? C11 C32 1.518(4) . ? C11 C12 1.528(4) . ? C11 H6 0.950 . ? C12 C13 1.380(4) . ? C12 C21 1.418(4) . ? C13 C14 1.426(5) . ? C13 H7 0.950 . ? C14 C15 1.412(5) . ? C14 C19 1.427(5) . ? C15 C16 1.354(5) . ? C15 H8 0.950 . ? C16 C17 1.376(6) . ? C16 H9 0.950 . ? C17 C18 1.379(6) . ? C17 H10 0.950 . ? C18 C19 1.398(5) . ? C18 H11 0.950 . ? C19 C20 1.435(5) . ? C20 C21 1.366(4) . ? C20 H12 0.950 . ? C21 C22 1.525(4) . ? C22 C23 1.525(4) . ? C22 H13 0.950 . ? C23 C24 1.362(4) . ? C23 C32 1.412(4) . ? C24 C25 1.407(5) . ? C24 H14 0.950 . ? C25 C26 1.416(5) . ? C25 C30 1.436(5) . ? C26 C27 1.342(5) . ? C26 H15 0.951 . ? C27 C28 1.390(6) . ? C27 H16 0.950 . ? C28 C29 1.387(6) . ? C28 H17 0.950 . ? C29 C30 1.401(5) . ? C29 H18 0.950 . ? C30 C31 1.423(5) . ? C31 C32 1.368(4) . ? C31 H19 0.950 . ? C33 C54 1.524(5) . ? C33 C34 1.526(5) . ? C33 H20 0.950 . ? C34 C35 1.340(5) . ? C34 C43 1.455(4) . ? C35 C36 1.459(5) . ? C35 H21 0.950 . ? C36 C41 1.401(5) . ? C36 C37 1.411(5) . ? C37 C38 1.350(5) . ? C37 H22 0.950 . ? C38 C39 1.421(6) . ? C38 H23 0.950 . ? C39 C40 1.375(5) . ? C39 H24 0.950 . ? C40 C41 1.422(5) . ? C40 H25 0.949 . ? C41 C42 1.435(5) . ? C42 C43 1.348(5) . ? C42 H26 0.950 . ? C43 C44 1.539(5) . ? C44 C45 1.513(5) . ? C44 H27 0.950 . ? C45 C46 1.371(5) . ? C45 C54 1.450(4) . ? C46 C47 1.401(5) . ? C46 H28 0.950 . ? C47 C52 1.419(5) . ? C47 C48 1.442(5) . ? C48 C49 1.373(7) . ? C48 H29 0.950 . ? C49 C50 1.409(8) . ? C49 H30 0.950 . ? C50 C51 1.344(6) . ? C50 H31 0.950 . ? C51 C52 1.452(6) . ? C51 H32 0.950 . ? C52 C53 1.415(5) . ? C53 C54 1.354(5) . ? C53 H33 0.950 . ? C55 C64 1.404(4) 2_756 ? C55 C56 1.443(4) . ? C56 C57 1.341(4) . ? C56 C65 1.535(4) . ? C57 C58 1.465(4) . ? C57 C76 1.506(4) . ? C58 C59 1.387(4) . ? C59 C60 1.395(4) . ? C59 H34 0.951 . ? C60 C61 1.425(4) . ? C61 C62 1.355(4) . ? C61 C87 1.525(4) . ? C62 C63 1.408(4) . ? C62 C98 1.526(4) . ? C63 C64 1.384(4) . ? C64 C55 1.404(4) 2_756 ? C64 H70 0.950 . ? C65 C66 1.528(5) . ? C65 C86 1.538(5) . ? C65 H35 0.950 . ? C66 C67 1.338(5) . ? C66 C75 1.432(4) . ? C67 C68 1.400(5) . ? C67 H36 0.950 . ? C68 C73 1.416(5) . ? C68 C69 1.430(5) . ? C69 C70 1.378(5) . ? C69 H37 0.951 . ? C70 C71 1.431(5) . ? C70 H38 0.950 . ? C71 C72 1.364(5) . ? C71 H39 0.949 . ? C72 C73 1.419(5) . ? C72 H40 0.950 . ? C73 C74 1.424(5) . ? C74 C75 1.369(5) . ? C74 H41 0.950 . ? C75 C76 1.534(5) . ? C76 C77 1.537(4) . ? C76 H42 0.950 . ? C77 C78 1.352(5) . ? C77 C86 1.413(5) . ? C78 C79 1.420(5) . ? C78 H43 0.950 . ? C79 C80 1.409(5) . ? C79 C84 1.436(5) . ? C80 C81 1.342(5) . ? C80 H44 0.951 . ? C81 C82 1.433(7) . ? C81 H45 0.950 . ? C82 C83 1.351(6) . ? C82 H46 0.950 . ? C83 C84 1.423(5) . ? C83 H47 0.949 . ? C84 C85 1.423(5) . ? C85 C86 1.373(5) . ? C85 H48 0.950 . ? C87 C88 1.528(4) . ? C87 C108 1.541(5) . ? C87 H49 0.950 . ? C88 C89 1.354(5) . ? C88 C97 1.446(5) . ? C89 C90 1.432(5) . ? C89 H50 0.949 . ? C90 C95 1.410(5) . ? C90 C91 1.419(5) . ? C91 C92 1.393(6) . ? C91 H51 0.950 . ? C92 C93 1.365(7) . ? C92 H52 0.951 . ? C93 C94 1.354(6) . ? C93 H53 0.950 . ? C94 C95 1.427(5) . ? C94 H54 0.950 . ? C95 C96 1.424(5) . ? C96 C97 1.362(5) . ? C96 H55 0.950 . ? C97 C98 1.518(5) . ? C98 C99 1.541(4) . ? C98 H56 0.950 . ? C99 C100 1.362(5) . ? C99 C108 1.412(5) . ? C100 C101 1.445(5) . ? C100 H57 0.950 . ? C101 C102 1.392(6) . ? C101 C106 1.409(5) . ? C102 C103 1.376(6) . ? C102 H58 0.951 . ? C103 C104 1.407(7) . ? C103 H59 0.950 . ? C104 C105 1.347(6) . ? C104 H60 0.950 . ? C105 C106 1.417(5) . ? C105 H61 0.950 . ? C106 C107 1.438(5) . ? C107 C108 1.347(5) . ? C107 H62 0.950 . ? C109 C114 1.364(6) . ? C109 C110 1.376(6) . ? C109 H63 0.950 . ? C110 C111 1.359(6) . ? C110 H64 0.951 . ? C111 C112 1.322(8) . ? C111 H65 0.951 . ? C112 C113 1.375(9) . ? C112 H66 0.951 . ? C113 C114 1.408(9) . ? C113 H67 0.951 . ? C114 H68 0.949 . ? 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 C4 N1 C1 110.0(2) . . ? C4 N1 H1 125.0(2) . . ? C1 N1 H1 125.0(2) . . ? C6 N2 C9 106.2(2) . . ? C6 N2 H2 127.0 . . ? C9 N2 H2 126.9 . . ? C55 N3 C58 106.5(3) . . ? C55 N3 H3 126.8 . . ? C58 N3 H3 126.7 . . ? C63 N4 C60 110.5(2) . . ? C63 N4 H4 124.7 . . ? C60 N4 H4 124.8 . . ? N1 C1 C10 123.9(3) . 2_666 ? N1 C1 C2 107.5(3) . . ? C10 C1 C2 128.4(3) 2_666 . ? C3 C2 C1 106.7(3) . . ? C3 C2 C11 114.3(3) . . ? C1 C2 C11 139.1(3) . . ? C2 C3 C4 109.3(3) . . ? C2 C3 C22 114.4(3) . . ? C4 C3 C22 136.3(3) . . ? N1 C4 C5 127.1(3) . . ? N1 C4 C3 106.4(2) . . ? C5 C4 C3 126.4(3) . . ? C4 C5 C6 127.7(3) . . ? C4 C5 H5 116.1 . . ? C6 C5 H5 116.2 . . ? N2 C6 C5 125.8(3) . . ? N2 C6 C7 110.0(3) . . ? C5 C6 C7 124.2(3) . . ? C8 C7 C6 107.2(3) . . ? C8 C7 C33 115.8(3) . . ? C6 C7 C33 136.9(3) . . ? C7 C8 C9 106.9(3) . . ? C7 C8 C44 114.8(3) . . ? C9 C8 C44 138.3(3) . . ? N2 C9 C10 124.9(3) . . ? N2 C9 C8 109.6(2) . . ? C10 C9 C8 125.4(3) . . ? C9 C10 C1 126.2(3) . 2_666 ? C9 C10 H69 116.9 . . ? C1 C10 H69 116.9 2_666 . ? C2 C11 C32 104.9(2) . . ? C2 C11 C12 105.5(2) . . ? C32 C11 C12 104.3(2) . . ? C2 C11 H6 113.6 . . ? C32 C11 H6 113.7 . . ? C12 C11 H6 113.7 . . ? C13 C12 C21 121.4(3) . . ? C13 C12 C11 125.3(3) . . ? C21 C12 C11 113.4(3) . . ? C12 C13 C14 119.1(3) . . ? C12 C13 H7 120.5 . . ? C14 C13 H7 120.5 . . ? C15 C14 C13 121.3(3) . . ? C15 C14 C19 118.8(3) . . ? C13 C14 C19 120.0(3) . . ? C16 C15 C14 120.0(4) . . ? C16 C15 H8 120.0 . . ? C14 C15 H8 120.0 . . ? C15 C16 C17 121.9(4) . . ? C15 C16 H9 119.1 . . ? C17 C16 H9 119.0 . . ? C16 C17 C18 119.9(3) . . ? C16 C17 H10 120.1 . . ? C18 C17 H10 120.0 . . ? C17 C18 C19 120.6(4) . . ? C17 C18 H11 119.7 . . ? C19 C18 H11 119.7 . . ? C18 C19 C14 118.8(3) . . ? C18 C19 C20 122.4(3) . . ? C14 C19 C20 118.8(3) . . ? C21 C20 C19 120.3(3) . . ? C21 C20 H12 119.9 . . ? C19 C20 H12 119.9 . . ? C20 C21 C12 120.5(3) . . ? C20 C21 C22 126.2(3) . . ? C12 C21 C22 113.2(3) . . ? C3 C22 C21 105.1(2) . . ? C3 C22 C23 104.3(2) . . ? C21 C22 C23 105.3(2) . . ? C3 C22 H13 113.7 . . ? C21 C22 H13 113.7 . . ? C23 C22 H13 113.7 . . ? C24 C23 C32 121.0(3) . . ? C24 C23 C22 125.7(3) . . ? C32 C23 C22 113.3(3) . . ? C23 C24 C25 120.5(3) . . ? C23 C24 H14 119.8 . . ? C25 C24 H14 119.7 . . ? C24 C25 C26 123.4(3) . . ? C24 C25 C30 119.3(3) . . ? C26 C25 C30 117.3(3) . . ? C27 C26 C25 123.1(4) . . ? C27 C26 H15 118.4 . . ? C25 C26 H15 118.4 . . ? C26 C27 C28 119.1(3) . . ? C26 C27 H16 120.5 . . ? C28 C27 H16 120.5 . . ? C29 C28 C27 121.4(3) . . ? C29 C28 H17 119.3 . . ? C27 C28 H17 119.3 . . ? C28 C29 C30 120.1(4) . . ? C28 C29 H18 119.9 . . ? C30 C29 H18 120.0 . . ? C29 C30 C31 122.7(3) . . ? C29 C30 C25 119.0(3) . . ? C31 C30 C25 118.4(3) . . ? C32 C31 C30 120.6(3) . . ? C32 C31 H19 119.7 . . ? C30 C31 H19 119.7 . . ? C31 C32 C23 120.2(3) . . ? C31 C32 C11 126.1(3) . . ? C23 C32 C11 113.7(3) . . ? C7 C33 C54 104.6(2) . . ? C7 C33 C34 105.2(3) . . ? C54 C33 C34 104.2(2) . . ? C7 C33 H20 113.9 . . ? C54 C33 H20 113.9 . . ? C34 C33 H20 113.9 . . ? C35 C34 C43 119.9(3) . . ? C35 C34 C33 126.6(3) . . ? C43 C34 C33 113.5(3) . . ? C34 C35 C36 120.5(3) . . ? C34 C35 H21 119.7 . . ? C36 C35 H21 119.8 . . ? C41 C36 C37 119.8(3) . . ? C41 C36 C35 119.1(3) . . ? C37 C36 C35 121.2(3) . . ? C38 C37 C36 120.0(3) . . ? C38 C37 H22 120.0 . . ? C36 C37 H22 120.0 . . ? C37 C38 C39 120.5(3) . . ? C37 C38 H23 119.7 . . ? C39 C38 H23 119.8 . . ? C40 C39 C38 121.2(4) . . ? C40 C39 H24 119.4 . . ? C38 C39 H24 119.3 . . ? C39 C40 C41 118.1(4) . . ? C39 C40 H25 120.9 . . ? C41 C40 H25 121.0 . . ? C36 C41 C40 120.3(3) . . ? C36 C41 C42 119.2(3) . . ? C40 C41 C42 120.5(3) . . ? C43 C42 C41 120.7(3) . . ? C43 C42 H26 119.7 . . ? C41 C42 H26 119.6 . . ? C42 C43 C34 120.6(3) . . ? C42 C43 C44 127.5(3) . . ? C34 C43 C44 111.9(3) . . ? C45 C44 C8 104.4(3) . . ? C45 C44 C43 105.7(3) . . ? C8 C44 C43 105.5(3) . . ? C45 C44 H27 113.5 . . ? C8 C44 H27 113.5 . . ? C43 C44 H27 113.4 . . ? C46 C45 C54 119.0(3) . . ? C46 C45 C44 127.8(3) . . ? C54 C45 C44 113.1(3) . . ? C45 C46 C47 120.7(3) . . ? C45 C46 H28 119.6 . . ? C47 C46 H28 119.7 . . ? C46 C47 C52 120.2(3) . . ? C46 C47 C48 121.7(4) . . ? C52 C47 C48 118.0(4) . . ? C49 C48 C47 120.4(4) . . ? C49 C48 H29 119.8 . . ? C47 C48 H29 119.8 . . ? C48 C49 C50 120.4(4) . . ? C48 C49 H30 119.8 . . ? C50 C49 H30 119.8 . . ? C51 C50 C49 122.2(4) . . ? C51 C50 H31 119.0 . . ? C49 C50 H31 118.9 . . ? C50 C51 C52 119.3(4) . . ? C50 C51 H32 120.4 . . ? C52 C51 H32 120.3 . . ? C53 C52 C47 118.6(4) . . ? C53 C52 C51 121.7(4) . . ? C47 C52 C51 119.7(4) . . ? C54 C53 C52 120.9(3) . . ? C54 C53 H33 119.6 . . ? C52 C53 H33 119.5 . . ? C53 C54 C45 120.4(3) . . ? C53 C54 C33 126.7(3) . . ? C45 C54 C33 112.9(3) . . ? N3 C55 C64 126.2(3) . 2_756 ? N3 C55 C56 109.7(3) . . ? C64 C55 C56 124.1(3) 2_756 . ? C57 C56 C55 108.1(3) . . ? C57 C56 C65 114.7(3) . . ? C55 C56 C65 136.6(3) . . ? C56 C57 C58 105.9(3) . . ? C56 C57 C76 115.4(3) . . ? C58 C57 C76 137.9(3) . . ? N3 C58 C59 126.4(3) . . ? N3 C58 C57 109.8(3) . . ? C59 C58 C57 123.7(3) . . ? C58 C59 C60 125.7(3) . . ? C58 C59 H34 117.1 . . ? C60 C59 H34 117.2 . . ? N4 C60 C59 125.1(3) . . ? N4 C60 C61 105.5(3) . . ? C59 C60 C61 129.4(3) . . ? C62 C61 C60 108.6(3) . . ? C62 C61 C87 115.2(3) . . ? C60 C61 C87 136.1(3) . . ? C61 C62 C63 109.3(3) . . ? C61 C62 C98 114.6(3) . . ? C63 C62 C98 136.0(3) . . ? N4 C63 C64 126.3(3) . . ? N4 C63 C62 106.0(3) . . ? C64 C63 C62 127.6(3) . . ? C63 C64 C55 127.4(3) . 2_756 ? C63 C64 H70 116.3 . . ? C55 C64 H70 116.3 2_756 . ? C66 C65 C56 105.5(2) . . ? C66 C65 C86 106.1(3) . . ? C56 C65 C86 102.8(3) . . ? C66 C65 H35 113.8 . . ? C56 C65 H35 113.8 . . ? C86 C65 H35 113.8 . . ? C67 C66 C75 121.3(3) . . ? C67 C66 C65 126.3(3) . . ? C75 C66 C65 112.4(3) . . ? C66 C67 C68 120.3(3) . . ? C66 C67 H36 119.8 . . ? C68 C67 H36 119.8 . . ? C67 C68 C73 120.0(3) . . ? C67 C68 C69 121.2(3) . . ? C73 C68 C69 118.8(3) . . ? C70 C69 C68 120.9(3) . . ? C70 C69 H37 119.6 . . ? C68 C69 H37 119.5 . . ? C69 C70 C71 120.1(4) . . ? C69 C70 H38 119.9 . . ? C71 C70 H38 120.0 . . ? C72 C71 C70 119.1(3) . . ? C72 C71 H39 120.5 . . ? C70 C71 H39 120.5 . . ? C71 C72 C73 122.4(3) . . ? C71 C72 H40 118.9 . . ? C73 C72 H40 118.8 . . ? C68 C73 C72 118.7(3) . . ? C68 C73 C74 118.8(3) . . ? C72 C73 C74 122.5(3) . . ? C75 C74 C73 120.0(3) . . ? C75 C74 H41 120.0 . . ? C73 C74 H41 120.0 . . ? C74 C75 C66 119.5(3) . . ? C74 C75 C76 126.8(3) . . ? C66 C75 C76 113.7(3) . . ? C57 C76 C75 105.0(3) . . ? C57 C76 C77 102.7(2) . . ? C75 C76 C77 106.7(2) . . ? C57 C76 H42 113.8 . . ? C75 C76 H42 113.8 . . ? C77 C76 H42 113.8 . . ? C78 C77 C86 120.3(3) . . ? C78 C77 C76 126.5(3) . . ? C86 C77 C76 113.0(3) . . ? C77 C78 C79 121.2(3) . . ? C77 C78 H43 119.5 . . ? C79 C78 H43 119.4 . . ? C80 C79 C78 124.2(4) . . ? C80 C79 C84 117.6(3) . . ? C78 C79 C84 118.3(3) . . ? C81 C80 C79 122.1(4) . . ? C81 C80 H44 119.0 . . ? C79 C80 H44 118.9 . . ? C80 C81 C82 121.0(4) . . ? C80 C81 H45 119.6 . . ? C82 C81 H45 119.5 . . ? C83 C82 C81 118.8(4) . . ? C83 C82 H46 120.6 . . ? C81 C82 H46 120.6 . . ? C82 C83 C84 121.7(4) . . ? C82 C83 H47 119.1 . . ? C84 C83 H47 119.1 . . ? C85 C84 C83 121.6(3) . . ? C85 C84 C79 119.6(3) . . ? C83 C84 C79 118.8(4) . . ? C86 C85 C84 119.1(3) . . ? C86 C85 H48 120.4 . . ? C84 C85 H48 120.4 . . ? C85 C86 C77 121.5(3) . . ? C85 C86 C65 124.7(3) . . ? C77 C86 C65 113.6(3) . . ? C61 C87 C88 104.6(2) . . ? C61 C87 C108 103.4(2) . . ? C88 C87 C108 105.7(3) . . ? C61 C87 H49 114.0 . . ? C88 C87 H49 114.0 . . ? C108 C87 H49 114.0 . . ? C89 C88 C97 120.3(3) . . ? C89 C88 C87 126.6(3) . . ? C97 C88 C87 113.0(3) . . ? C88 C89 C90 119.8(3) . . ? C88 C89 H50 120.1 . . ? C90 C89 H50 120.1 . . ? C95 C90 C91 118.3(3) . . ? C95 C90 C89 119.7(3) . . ? C91 C90 C89 122.0(4) . . ? C92 C91 C90 119.4(4) . . ? C92 C91 H51 120.3 . . ? C90 C91 H51 120.3 . . ? C93 C92 C91 121.3(4) . . ? C93 C92 H52 119.4 . . ? C91 C92 H52 119.3 . . ? C94 C93 C92 121.5(4) . . ? C94 C93 H53 119.3 . . ? C92 C93 H53 119.2 . . ? C93 C94 C95 119.5(4) . . ? C93 C94 H54 120.2 . . ? C95 C94 H54 120.3 . . ? C90 C95 C96 119.7(3) . . ? C90 C95 C94 120.0(3) . . ? C96 C95 C94 120.3(4) . . ? C97 C96 C95 119.7(3) . . ? C97 C96 H55 120.1 . . ? C95 C96 H55 120.2 . . ? C96 C97 C88 120.7(3) . . ? C96 C97 C98 126.1(3) . . ? C88 C97 C98 113.2(3) . . ? C97 C98 C62 105.1(3) . . ? C97 C98 C99 106.7(2) . . ? C62 C98 C99 103.1(2) . . ? C97 C98 H56 113.7 . . ? C62 C98 H56 113.7 . . ? C99 C98 H56 113.7 . . ? C100 C99 C108 121.5(3) . . ? C100 C99 C98 125.3(3) . . ? C108 C99 C98 113.1(3) . . ? C99 C100 C101 119.3(3) . . ? C99 C100 H57 120.4 . . ? C101 C100 H57 120.4 . . ? C102 C101 C106 118.8(4) . . ? C102 C101 C100 122.2(4) . . ? C106 C101 C100 118.9(3) . . ? C103 C102 C101 121.1(5) . . ? C103 C102 H58 119.5 . . ? C101 C102 H58 119.4 . . ? C102 C103 C104 120.3(4) . . ? C102 C103 H59 119.9 . . ? C104 C103 H59 119.9 . . ? C105 C104 C103 119.4(4) . . ? C105 C104 H60 120.3 . . ? C103 C104 H60 120.3 . . ? C104 C105 C106 121.6(4) . . ? C104 C105 H61 119.1 . . ? C106 C105 H61 119.2 . . ? C101 C106 C105 118.8(4) . . ? C101 C106 C107 119.4(3) . . ? C105 C106 C107 121.7(4) . . ? C108 C107 C106 120.1(3) . . ? C108 C107 H62 120.0 . . ? C106 C107 H62 119.9 . . ? C107 C108 C99 120.8(3) . . ? C107 C108 C87 125.3(3) . . ? C99 C108 C87 113.9(3) . . ? C114 C109 C110 117.9(4) . . ? C114 C109 H63 121.1 . . ? C110 C109 H63 121.0 . . ? C111 C110 C109 121.3(4) . . ? C111 C110 H64 119.3 . . ? C109 C110 H64 119.3 . . ? C112 C111 C110 121.7(5) . . ? C112 C111 H65 119.2 . . ? C110 C111 H65 119.1 . . ? C111 C112 C113 119.0(5) . . ? C111 C112 H66 120.5 . . ? C113 C112 H66 120.6 . . ? C112 C113 C114 119.6(5) . . ? C112 C113 H67 120.0 . . ? C114 C113 H67 120.4 . . ? C109 C114 C113 119.5(5) . . ? C109 C114 H68 120.3 . . ? C113 C114 H68 120.2 . . ? 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 C4 N1 C1 C10 175.0(3) . . . 2_666 ? C4 N1 C1 C2 -0.9(3) . . . . ? N1 C1 C2 C3 2.3(3) . . . . ? C10 C1 C2 C3 -173.4(3) 2_666 . . . ? N1 C1 C2 C11 -178.4(4) . . . . ? C10 C1 C2 C11 5.9(6) 2_666 . . . ? C1 C2 C3 C4 -2.8(3) . . . . ? C11 C2 C3 C4 177.7(3) . . . . ? C1 C2 C3 C22 177.8(3) . . . . ? C11 C2 C3 C22 -1.7(4) . . . . ? C1 N1 C4 C5 176.4(3) . . . . ? C1 N1 C4 C3 -0.8(3) . . . . ? C2 C3 C4 N1 2.2(3) . . . . ? C22 C3 C4 N1 -178.6(3) . . . . ? C2 C3 C4 C5 -175.0(3) . . . . ? C22 C3 C4 C5 4.2(6) . . . . ? N1 C4 C5 C6 -0.1(5) . . . . ? C3 C4 C5 C6 176.5(3) . . . . ? C9 N2 C6 C5 177.6(3) . . . . ? C9 N2 C6 C7 -0.1(3) . . . . ? C4 C5 C6 N2 6.7(5) . . . . ? C4 C5 C6 C7 -176.0(3) . . . . ? N2 C6 C7 C8 -1.9(4) . . . . ? C5 C6 C7 C8 -179.6(3) . . . . ? N2 C6 C7 C33 -177.6(4) . . . . ? C5 C6 C7 C33 4.7(6) . . . . ? C6 C7 C8 C9 2.9(4) . . . . ? C33 C7 C8 C9 179.7(3) . . . . ? C6 C7 C8 C44 -175.4(3) . . . . ? C33 C7 C8 C44 1.3(4) . . . . ? C6 N2 C9 C10 -178.3(3) . . . . ? C6 N2 C9 C8 1.9(3) . . . . ? C7 C8 C9 N2 -3.1(4) . . . . ? C44 C8 C9 N2 174.6(4) . . . . ? C7 C8 C9 C10 177.1(3) . . . . ? C44 C8 C9 C10 -5.2(6) . . . . ? N2 C9 C10 C1 -4.3(5) . . . 2_666 ? C8 C9 C10 C1 175.4(3) . . . 2_666 ? C3 C2 C11 C32 -54.2(3) . . . . ? C1 C2 C11 C32 126.6(4) . . . . ? C3 C2 C11 C12 55.7(3) . . . . ? C1 C2 C11 C12 -123.6(4) . . . . ? C2 C11 C12 C13 127.4(3) . . . . ? C32 C11 C12 C13 -122.3(3) . . . . ? C2 C11 C12 C21 -52.8(3) . . . . ? C32 C11 C12 C21 57.5(3) . . . . ? C21 C12 C13 C14 -1.9(4) . . . . ? C11 C12 C13 C14 177.9(3) . . . . ? C12 C13 C14 C15 -179.4(3) . . . . ? C12 C13 C14 C19 1.5(4) . . . . ? C13 C14 C15 C16 -179.8(3) . . . . ? C19 C14 C15 C16 -0.6(5) . . . . ? C14 C15 C16 C17 -1.3(6) . . . . ? C15 C16 C17 C18 1.5(6) . . . . ? C16 C17 C18 C19 0.2(6) . . . . ? C17 C18 C19 C14 -2.0(5) . . . . ? C17 C18 C19 C20 179.2(3) . . . . ? C15 C14 C19 C18 2.3(5) . . . . ? C13 C14 C19 C18 -178.6(3) . . . . ? C15 C14 C19 C20 -178.9(3) . . . . ? C13 C14 C19 C20 0.2(4) . . . . ? C18 C19 C20 C21 177.3(3) . . . . ? C14 C19 C20 C21 -1.5(4) . . . . ? C19 C20 C21 C12 1.1(4) . . . . ? C19 C20 C21 C22 -175.1(3) . . . . ? C13 C12 C21 C20 0.7(4) . . . . ? C11 C12 C21 C20 -179.2(3) . . . . ? C13 C12 C21 C22 177.3(3) . . . . ? C11 C12 C21 C22 -2.6(4) . . . . ? C2 C3 C22 C21 -54.2(3) . . . . ? C4 C3 C22 C21 126.7(4) . . . . ? C2 C3 C22 C23 56.3(3) . . . . ? C4 C3 C22 C23 -122.8(4) . . . . ? C20 C21 C22 C3 -127.8(3) . . . . ? C12 C21 C22 C3 55.8(3) . . . . ? C20 C21 C22 C23 122.4(3) . . . . ? C12 C21 C22 C23 -54.0(3) . . . . ? C3 C22 C23 C24 127.0(3) . . . . ? C21 C22 C23 C24 -122.6(3) . . . . ? C3 C22 C23 C32 -54.5(3) . . . . ? C21 C22 C23 C32 55.9(3) . . . . ? C32 C23 C24 C25 -0.6(4) . . . . ? C22 C23 C24 C25 177.9(3) . . . . ? C23 C24 C25 C26 -179.6(3) . . . . ? C23 C24 C25 C30 -0.5(4) . . . . ? C24 C25 C26 C27 178.6(3) . . . . ? C30 C25 C26 C27 -0.5(5) . . . . ? C25 C26 C27 C28 -1.3(5) . . . . ? C26 C27 C28 C29 2.4(6) . . . . ? C27 C28 C29 C30 -1.7(5) . . . . ? C28 C29 C30 C31 -179.3(3) . . . . ? C28 C29 C30 C25 -0.1(5) . . . . ? C24 C25 C30 C29 -178.0(3) . . . . ? C26 C25 C30 C29 1.2(4) . . . . ? C24 C25 C30 C31 1.2(4) . . . . ? C26 C25 C30 C31 -179.6(3) . . . . ? C29 C30 C31 C32 178.3(3) . . . . ? C25 C30 C31 C32 -0.9(4) . . . . ? C30 C31 C32 C23 -0.1(4) . . . . ? C30 C31 C32 C11 -177.0(3) . . . . ? C24 C23 C32 C31 0.9(4) . . . . ? C22 C23 C32 C31 -177.7(3) . . . . ? C24 C23 C32 C11 178.2(3) . . . . ? C22 C23 C32 C11 -0.5(3) . . . . ? C2 C11 C32 C31 -128.0(3) . . . . ? C12 C11 C32 C31 121.3(3) . . . . ? C2 C11 C32 C23 55.0(3) . . . . ? C12 C11 C32 C23 -55.8(3) . . . . ? C8 C7 C33 C54 -55.5(4) . . . . ? C6 C7 C33 C54 119.9(4) . . . . ? C8 C7 C33 C34 54.0(4) . . . . ? C6 C7 C33 C34 -130.6(4) . . . . ? C7 C33 C34 C35 127.4(3) . . . . ? C54 C33 C34 C35 -122.8(4) . . . . ? C7 C33 C34 C43 -53.4(3) . . . . ? C54 C33 C34 C43 56.4(3) . . . . ? C43 C34 C35 C36 -0.4(5) . . . . ? C33 C34 C35 C36 178.8(3) . . . . ? C34 C35 C36 C41 0.6(5) . . . . ? C34 C35 C36 C37 -177.8(3) . . . . ? C41 C36 C37 C38 2.0(5) . . . . ? C35 C36 C37 C38 -179.6(3) . . . . ? C36 C37 C38 C39 0.0(5) . . . . ? C37 C38 C39 C40 0.2(6) . . . . ? C38 C39 C40 C41 -2.4(5) . . . . ? C37 C36 C41 C40 -4.2(5) . . . . ? C35 C36 C41 C40 177.3(3) . . . . ? C37 C36 C41 C42 177.4(3) . . . . ? C35 C36 C41 C42 -1.1(5) . . . . ? C39 C40 C41 C36 4.4(5) . . . . ? C39 C40 C41 C42 -177.2(3) . . . . ? C36 C41 C42 C43 1.3(5) . . . . ? C40 C41 C42 C43 -177.1(3) . . . . ? C41 C42 C43 C34 -1.1(5) . . . . ? C41 C42 C43 C44 179.8(3) . . . . ? C35 C34 C43 C42 0.6(5) . . . . ? C33 C34 C43 C42 -178.7(3) . . . . ? C35 C34 C43 C44 179.9(3) . . . . ? C33 C34 C43 C44 0.6(4) . . . . ? C7 C8 C44 C45 55.1(4) . . . . ? C9 C8 C44 C45 -122.5(4) . . . . ? C7 C8 C44 C43 -56.2(4) . . . . ? C9 C8 C44 C43 126.3(4) . . . . ? C42 C43 C44 C45 122.6(4) . . . . ? C34 C43 C44 C45 -56.6(3) . . . . ? C42 C43 C44 C8 -127.2(4) . . . . ? C34 C43 C44 C8 53.6(3) . . . . ? C8 C44 C45 C46 122.7(3) . . . . ? C43 C44 C45 C46 -126.2(3) . . . . ? C8 C44 C45 C54 -56.6(3) . . . . ? C43 C44 C45 C54 54.5(3) . . . . ? C54 C45 C46 C47 -1.0(5) . . . . ? C44 C45 C46 C47 179.8(3) . . . . ? C45 C46 C47 C52 -1.8(5) . . . . ? C45 C46 C47 C48 178.8(3) . . . . ? C46 C47 C48 C49 179.0(4) . . . . ? C52 C47 C48 C49 -0.4(5) . . . . ? C47 C48 C49 C50 -1.7(6) . . . . ? C48 C49 C50 C51 1.3(7) . . . . ? C49 C50 C51 C52 1.2(7) . . . . ? C46 C47 C52 C53 2.2(5) . . . . ? C48 C47 C52 C53 -178.4(3) . . . . ? C46 C47 C52 C51 -176.5(3) . . . . ? C48 C47 C52 C51 2.9(5) . . . . ? C50 C51 C52 C53 178.0(4) . . . . ? C50 C51 C52 C47 -3.3(6) . . . . ? C47 C52 C53 C54 0.3(5) . . . . ? C51 C52 C53 C54 179.0(3) . . . . ? C52 C53 C54 C45 -3.2(5) . . . . ? C52 C53 C54 C33 176.2(3) . . . . ? C46 C45 C54 C53 3.6(5) . . . . ? C44 C45 C54 C53 -177.1(3) . . . . ? C46 C45 C54 C33 -175.9(3) . . . . ? C44 C45 C54 C33 3.5(4) . . . . ? C7 C33 C54 C53 -128.2(3) . . . . ? C34 C33 C54 C53 121.6(3) . . . . ? C7 C33 C54 C45 51.2(3) . . . . ? C34 C33 C54 C45 -59.0(3) . . . . ? C58 N3 C55 C64 -179.0(3) . . . 2_756 ? C58 N3 C55 C56 -0.1(3) . . . . ? N3 C55 C56 C57 1.4(4) . . . . ? C64 C55 C56 C57 -179.8(3) 2_756 . . . ? N3 C55 C56 C65 -168.5(4) . . . . ? C64 C55 C56 C65 10.4(6) 2_756 . . . ? C55 C56 C57 C58 -1.9(4) . . . . ? C65 C56 C57 C58 170.4(3) . . . . ? C55 C56 C57 C76 -173.8(3) . . . . ? C65 C56 C57 C76 -1.4(4) . . . . ? C55 N3 C58 C59 177.4(3) . . . . ? C55 N3 C58 C57 -1.0(3) . . . . ? C56 C57 C58 N3 1.9(4) . . . . ? C76 C57 C58 N3 170.9(4) . . . . ? C56 C57 C58 C59 -176.6(3) . . . . ? C76 C57 C58 C59 -7.6(6) . . . . ? N3 C58 C59 C60 -1.5(5) . . . . ? C57 C58 C59 C60 176.7(3) . . . . ? C63 N4 C60 C59 177.5(3) . . . . ? C63 N4 C60 C61 0.1(3) . . . . ? C58 C59 C60 N4 -1.0(5) . . . . ? C58 C59 C60 C61 175.9(3) . . . . ? N4 C60 C61 C62 -0.9(4) . . . . ? C59 C60 C61 C62 -178.2(3) . . . . ? N4 C60 C61 C87 -178.0(3) . . . . ? C59 C60 C61 C87 4.7(6) . . . . ? C60 C61 C62 C63 1.4(4) . . . . ? C87 C61 C62 C63 179.2(3) . . . . ? C60 C61 C62 C98 -179.7(3) . . . . ? C87 C61 C62 C98 -1.9(4) . . . . ? C60 N4 C63 C64 -178.0(3) . . . . ? C60 N4 C63 C62 0.7(3) . . . . ? C61 C62 C63 N4 -1.3(4) . . . . ? C98 C62 C63 N4 -179.9(3) . . . . ? C61 C62 C63 C64 177.4(3) . . . . ? C98 C62 C63 C64 -1.1(6) . . . . ? N4 C63 C64 C55 -0.3(5) . . . 2_756 ? C62 C63 C64 C55 -178.8(3) . . . 2_756 ? C57 C56 C65 C66 55.9(4) . . . . ? C55 C56 C65 C66 -134.7(4) . . . . ? C57 C56 C65 C86 -55.1(4) . . . . ? C55 C56 C65 C86 114.3(4) . . . . ? C56 C65 C66 C67 127.3(4) . . . . ? C86 C65 C66 C67 -124.1(4) . . . . ? C56 C65 C66 C75 -52.1(3) . . . . ? C86 C65 C66 C75 56.5(3) . . . . ? C75 C66 C67 C68 2.6(5) . . . . ? C65 C66 C67 C68 -176.8(3) . . . . ? C66 C67 C68 C73 -1.0(5) . . . . ? C66 C67 C68 C69 178.1(4) . . . . ? C67 C68 C69 C70 -178.3(4) . . . . ? C73 C68 C69 C70 0.7(6) . . . . ? C68 C69 C70 C71 0.1(6) . . . . ? C69 C70 C71 C72 0.3(6) . . . . ? C70 C71 C72 C73 -1.5(6) . . . . ? C67 C68 C73 C72 177.2(3) . . . . ? C69 C68 C73 C72 -1.9(5) . . . . ? C67 C68 C73 C74 -1.0(5) . . . . ? C69 C68 C73 C74 179.9(3) . . . . ? C71 C72 C73 C68 2.4(5) . . . . ? C71 C72 C73 C74 -179.5(3) . . . . ? C68 C73 C74 C75 1.4(5) . . . . ? C72 C73 C74 C75 -176.7(3) . . . . ? C73 C74 C75 C66 0.2(5) . . . . ? C73 C74 C75 C76 179.4(3) . . . . ? C67 C66 C75 C74 -2.2(5) . . . . ? C65 C66 C75 C74 177.2(3) . . . . ? C67 C66 C75 C76 178.5(3) . . . . ? C65 C66 C75 C76 -2.1(4) . . . . ? C56 C57 C76 C75 -53.9(4) . . . . ? C58 C57 C76 C75 137.9(4) . . . . ? C56 C57 C76 C77 57.6(4) . . . . ? C58 C57 C76 C77 -110.6(4) . . . . ? C74 C75 C76 C57 -124.1(3) . . . . ? C66 C75 C76 C57 55.2(3) . . . . ? C74 C75 C76 C77 127.3(3) . . . . ? C66 C75 C76 C77 -53.4(3) . . . . ? C57 C76 C77 C78 119.8(3) . . . . ? C75 C76 C77 C78 -130.0(3) . . . . ? C57 C76 C77 C86 -55.9(3) . . . . ? C75 C76 C77 C86 54.3(3) . . . . ? C86 C77 C78 C79 2.9(5) . . . . ? C76 C77 C78 C79 -172.5(3) . . . . ? C77 C78 C79 C80 175.8(3) . . . . ? C77 C78 C79 C84 -3.0(5) . . . . ? C78 C79 C80 C81 -176.9(3) . . . . ? C84 C79 C80 C81 1.9(5) . . . . ? C79 C80 C81 C82 -2.7(6) . . . . ? C80 C81 C82 C83 0.6(6) . . . . ? C81 C82 C83 C84 2.2(6) . . . . ? C82 C83 C84 C85 175.5(3) . . . . ? C82 C83 C84 C79 -2.9(5) . . . . ? C80 C79 C84 C85 -177.6(3) . . . . ? C78 C79 C84 C85 1.3(5) . . . . ? C80 C79 C84 C83 0.8(5) . . . . ? C78 C79 C84 C83 179.7(3) . . . . ? C83 C84 C85 C86 -178.0(3) . . . . ? C79 C84 C85 C86 0.4(5) . . . . ? C84 C85 C86 C77 -0.5(5) . . . . ? C84 C85 C86 C65 173.5(3) . . . . ? C78 C77 C86 C85 -1.2(5) . . . . ? C76 C77 C86 C85 174.9(3) . . . . ? C78 C77 C86 C65 -175.8(3) . . . . ? C76 C77 C86 C65 0.3(4) . . . . ? C66 C65 C86 C85 129.6(3) . . . . ? C56 C65 C86 C85 -119.9(3) . . . . ? C66 C65 C86 C77 -56.1(3) . . . . ? C56 C65 C86 C77 54.5(3) . . . . ? C62 C61 C87 C88 56.2(4) . . . . ? C60 C61 C87 C88 -126.8(4) . . . . ? C62 C61 C87 C108 -54.2(3) . . . . ? C60 C61 C87 C108 122.8(4) . . . . ? C61 C87 C88 C89 128.3(3) . . . . ? C108 C87 C88 C89 -122.9(3) . . . . ? C61 C87 C88 C97 -53.2(3) . . . . ? C108 C87 C88 C97 55.6(3) . . . . ? C97 C88 C89 C90 2.2(5) . . . . ? C87 C88 C89 C90 -179.4(3) . . . . ? C88 C89 C90 C95 0.2(5) . . . . ? C88 C89 C90 C91 177.7(3) . . . . ? C95 C90 C91 C92 0.6(5) . . . . ? C89 C90 C91 C92 -176.9(4) . . . . ? C90 C91 C92 C93 -1.6(6) . . . . ? C91 C92 C93 C94 0.7(7) . . . . ? C92 C93 C94 C95 1.1(6) . . . . ? C91 C90 C95 C96 179.8(3) . . . . ? C89 C90 C95 C96 -2.7(5) . . . . ? C91 C90 C95 C94 1.2(5) . . . . ? C89 C90 C95 C94 178.7(3) . . . . ? C93 C94 C95 C90 -2.1(5) . . . . ? C93 C94 C95 C96 179.3(4) . . . . ? C90 C95 C96 C97 2.8(5) . . . . ? C94 C95 C96 C97 -178.6(3) . . . . ? C95 C96 C97 C88 -0.5(5) . . . . ? C95 C96 C97 C98 -179.7(3) . . . . ? C89 C88 C97 C96 -2.1(5) . . . . ? C87 C88 C97 C96 179.3(3) . . . . ? C89 C88 C97 C98 177.2(3) . . . . ? C87 C88 C97 C98 -1.4(4) . . . . ? C96 C97 C98 C62 -125.8(3) . . . . ? C88 C97 C98 C62 55.0(3) . . . . ? C96 C97 C98 C99 125.2(3) . . . . ? C88 C97 C98 C99 -54.0(3) . . . . ? C61 C62 C98 C97 -54.2(3) . . . . ? C63 C62 C98 C97 124.3(4) . . . . ? C61 C62 C98 C99 57.4(3) . . . . ? C63 C62 C98 C99 -124.1(4) . . . . ? C97 C98 C99 C100 -128.2(3) . . . . ? C62 C98 C99 C100 121.4(3) . . . . ? C97 C98 C99 C108 55.0(3) . . . . ? C62 C98 C99 C108 -55.4(3) . . . . ? C108 C99 C100 C101 0.7(5) . . . . ? C98 C99 C100 C101 -175.9(3) . . . . ? C99 C100 C101 C102 174.5(3) . . . . ? C99 C100 C101 C106 -1.4(5) . . . . ? C106 C101 C102 C103 -2.0(6) . . . . ? C100 C101 C102 C103 -177.8(4) . . . . ? C101 C102 C103 C104 1.0(6) . . . . ? C102 C103 C104 C105 0.1(6) . . . . ? C103 C104 C105 C106 -0.1(6) . . . . ? C102 C101 C106 C105 1.9(5) . . . . ? C100 C101 C106 C105 177.9(3) . . . . ? C102 C101 C106 C107 -176.2(3) . . . . ? C100 C101 C106 C107 -0.2(5) . . . . ? C104 C105 C106 C101 -0.9(6) . . . . ? C104 C105 C106 C107 177.2(4) . . . . ? C101 C106 C107 C108 2.5(5) . . . . ? C105 C106 C107 C108 -175.5(3) . . . . ? C106 C107 C108 C99 -3.3(5) . . . . ? C106 C107 C108 C87 175.1(3) . . . . ? C100 C99 C108 C107 1.6(5) . . . . ? C98 C99 C108 C107 178.6(3) . . . . ? C100 C99 C108 C87 -176.9(3) . . . . ? C98 C99 C108 C87 0.1(3) . . . . ? C61 C87 C108 C107 -124.0(3) . . . . ? C88 C87 C108 C107 126.4(3) . . . . ? C61 C87 C108 C99 54.4(3) . . . . ? C88 C87 C108 C99 -55.2(3) . . . . ? C114 C109 C110 C111 -2.4(7) . . . . ? C109 C110 C111 C112 1.8(8) . . . . ? C110 C111 C112 C113 5.2(12) . . . . ? C111 C112 C113 C114 -11.3(14) . . . . ? C110 C109 C114 C113 -3.8(9) . . . . ? C112 C113 C114 C109 10.7(12) . . . . ? #============================================================================== # End of CIF #==============================================================================