# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _publ_contact_author_email ZALESKI@INDIANA.EDU _publ_contact_author_name 'Dr Jeffrey Zaleski' _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name J.Zaleski J.C.Huffman M.Nath data_02084 _database_code_CSD 200680 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H30 N4' _chemical_formula_weight 662.76 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.4177(5) _cell_length_b 10.0068(4) _cell_length_c 23.8356(9) _cell_angle_alpha 90.00 _cell_angle_beta 97.5350(10) _cell_angle_gamma 90.00 _cell_volume 3409.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 114(2) _cell_measurement_reflns_used 7809 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 30.1 _exptl_crystal_description 'hexagonal plate' _exptl_crystal_colour black _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.291 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1384 _exptl_absorpt_coefficient_mu 0.076 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 114(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_method '\w scans' _diffrn_measurement_device 'three-circle goniometer with fixed chi' _diffrn_measurement_device_type 'Bruker Platform goniometer' _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker SMART 6000' _diffrn_detector_area_resol_mean 44.52 _diffrn_standards_number 328 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0016 _diffrn_reflns_number 46218 _diffrn_reflns_av_R_equivalents 0.0519 _diffrn_reflns_av_sigmaI/netI 0.0474 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 30.02 _reflns_number_total 9941 _reflns_number_gt 6558 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1999)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT (Bruker, 1999), XTEL (local package)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0779P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9941 _refine_ls_number_parameters 589 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0809 _refine_ls_R_factor_gt 0.0500 _refine_ls_wR_factor_ref 0.1356 _refine_ls_wR_factor_gt 0.1228 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_restrained_S_all 0.983 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.50740(8) 0.92017(11) 0.10520(5) 0.0229(2) Uani 1 1 d . . . C2 C 0.44370(9) 0.86360(13) 0.06458(6) 0.0218(3) Uani 1 1 d . . . C3 C 0.34855(9) 0.88662(14) 0.07736(6) 0.0232(3) Uani 1 1 d . . . C4 C 0.35680(9) 0.96476(14) 0.12509(6) 0.0233(3) Uani 1 1 d . . . C5 C 0.45730(9) 0.98106(14) 0.14285(6) 0.0225(3) Uani 1 1 d . . . C6 C 0.49584(9) 1.04657(14) 0.19288(6) 0.0236(3) Uani 1 1 d . . . C7 C 0.59112(9) 1.05437(14) 0.21370(6) 0.0244(3) Uani 1 1 d . . . C8 C 0.63006(10) 1.12484(15) 0.26347(6) 0.0286(3) Uani 1 1 d . . . C9 C 0.72509(10) 1.11263(15) 0.26898(6) 0.0278(3) Uani 1 1 d . . . C10 C 0.74805(9) 1.03192(14) 0.22285(6) 0.0238(3) Uani 1 1 d . . . N11 N 0.66507(8) 0.99898(12) 0.19068(5) 0.0242(2) Uani 1 1 d . . . C12 C 0.83799(9) 0.99759(14) 0.21138(6) 0.0233(3) Uani 1 1 d . . . C13 C 0.85781(9) 0.93132(14) 0.16212(6) 0.0229(3) Uani 1 1 d . . . C14 C 0.95179(9) 0.89207(15) 0.15227(6) 0.0259(3) Uani 1 1 d . . . C15 C 0.94357(10) 0.83812(15) 0.10017(6) 0.0266(3) Uani 1 1 d . . . C16 C 0.84431(9) 0.84322(14) 0.07775(6) 0.0239(3) Uani 1 1 d . . . N17 N 0.79338(8) 0.89775(12) 0.11690(5) 0.0234(2) Uani 1 1 d . . . C18 C 0.80818(9) 0.79830(14) 0.02354(6) 0.0229(3) Uani 1 1 d . . . C19 C 0.71285(9) 0.79024(14) 0.00269(6) 0.0230(3) Uani 1 1 d . . . C20 C 0.67309(10) 0.74333(14) -0.05185(6) 0.0254(3) Uani 1 1 d . . . C21 C 0.57819(10) 0.74070(14) -0.05311(6) 0.0247(3) Uani 1 1 d . . . C22 C 0.55622(9) 0.78743(13) 0.00035(6) 0.0224(3) Uani 1 1 d . . . N23 N 0.63960(8) 0.81879(12) 0.03240(5) 0.0227(2) Uani 1 1 d . . . C24 C 0.46595(9) 0.79882(13) 0.01566(5) 0.0222(3) Uani 1 1 d . . . C25 C 0.25974(11) 0.83524(15) 0.04932(6) 0.0321(3) Uani 1 1 d . . . C26 C 0.18942(13) 0.7938(2) 0.03164(8) 0.0448(4) Uani 1 1 d . . . C27 C 0.27684(11) 1.01995(15) 0.14853(6) 0.0291(3) Uani 1 1 d . . . C28 C 0.20997(12) 1.06131(18) 0.16220(7) 0.0382(4) Uani 1 1 d . . . C29 C 0.43142(9) 1.11123(15) 0.22916(6) 0.0248(3) Uani 1 1 d . . . C30 C 0.40452(11) 1.04254(17) 0.27527(6) 0.0321(3) Uani 1 1 d . . . C31 C 0.34324(11) 1.10159(18) 0.30827(7) 0.0371(4) Uani 1 1 d . . . C32 C 0.31019(10) 1.22882(17) 0.29654(7) 0.0353(4) Uani 1 1 d . . . C33 C 0.33765(10) 1.29916(17) 0.25147(7) 0.0335(3) Uani 1 1 d . . . C34 C 0.39838(10) 1.24058(16) 0.21781(6) 0.0292(3) Uani 1 1 d . . . C35 C 0.91787(9) 1.04040(14) 0.25398(6) 0.0245(3) Uani 1 1 d . . . C36 C 0.98564(10) 1.12940(16) 0.23907(7) 0.0302(3) Uani 1 1 d . . . C37 C 1.06015(11) 1.16855(17) 0.27851(7) 0.0346(3) Uani 1 1 d . . . C38 C 1.06742(11) 1.12196(16) 0.33357(7) 0.0339(3) Uani 1 1 d . . . C39 C 0.99915(11) 1.03846(16) 0.34922(7) 0.0338(3) Uani 1 1 d . . . C40 C 0.92555(10) 0.99593(16) 0.30990(6) 0.0285(3) Uani 1 1 d . . . C41 C 0.87521(9) 0.75162(15) -0.01526(6) 0.0254(3) Uani 1 1 d . . . C42 C 0.88190(11) 0.61687(17) -0.02830(7) 0.0355(4) Uani 1 1 d . . . C43 C 0.94457(12) 0.5742(2) -0.06431(7) 0.0414(4) Uani 1 1 d . . . C44 C 1.00021(11) 0.6661(2) -0.08761(7) 0.0396(4) Uani 1 1 d . . . C45 C 0.99406(11) 0.7991(2) -0.07505(7) 0.0379(4) Uani 1 1 d . . . C46 C 0.93162(10) 0.84288(18) -0.03907(6) 0.0321(3) Uani 1 1 d . . . C47 C 0.39046(9) 0.73540(13) -0.02486(6) 0.0224(3) Uani 1 1 d . . . C48 C 0.33694(11) 0.80908(16) -0.06657(6) 0.0322(3) Uani 1 1 d . . . C49 C 0.26817(11) 0.74754(17) -0.10413(7) 0.0341(3) Uani 1 1 d . . . C50 C 0.25323(10) 0.61151(16) -0.10075(7) 0.0307(3) Uani 1 1 d . . . C51 C 0.30680(11) 0.53727(16) -0.05985(7) 0.0344(3) Uani 1 1 d . . . C52 C 0.37499(10) 0.59859(15) -0.02193(7) 0.0301(3) Uani 1 1 d . . . H53 H 0.5926(11) 1.1703(17) 0.2886(7) 0.035(4) Uiso 1 1 d . . . H54 H 0.7731(11) 1.1536(15) 0.2999(7) 0.029(4) Uiso 1 1 d . . . H55 H 0.6586(13) 0.949(2) 0.1590(8) 0.052(6) Uiso 1 1 d . . . H56 H 1.0083(11) 0.9000(16) 0.1807(7) 0.032(4) Uiso 1 1 d . . . H57 H 0.9956(11) 0.8011(15) 0.0789(7) 0.027(4) Uiso 1 1 d . . . H58 H 0.7107(11) 0.7195(16) -0.0823(7) 0.031(4) Uiso 1 1 d . . . H59 H 0.5311(10) 0.7198(14) -0.0853(6) 0.021(4) Uiso 1 1 d . . . H60 H 0.6452(13) 0.8447(19) 0.0678(9) 0.048(6) Uiso 1 1 d . . . H61 H 0.1279(17) 0.760(2) 0.0117(10) 0.077(7) Uiso 1 1 d . . . H62 H 0.1497(19) 1.111(3) 0.1761(12) 0.106(9) Uiso 1 1 d . . . H63 H 0.4268(11) 0.9546(18) 0.2822(7) 0.032(4) Uiso 1 1 d . . . H64 H 0.3272(12) 1.0510(19) 0.3398(8) 0.046(5) Uiso 1 1 d . . . H65 H 0.2692(12) 1.2707(17) 0.3214(7) 0.041(5) Uiso 1 1 d . . . H66 H 0.3142(12) 1.3916(19) 0.2413(8) 0.044(5) Uiso 1 1 d . . . H67 H 0.4165(12) 1.2908(18) 0.1869(8) 0.039(5) Uiso 1 1 d . . . H68 H 0.9804(11) 1.1632(16) 0.1997(8) 0.034(4) Uiso 1 1 d . . . H69 H 1.1075(13) 1.2284(18) 0.2654(7) 0.043(5) Uiso 1 1 d . . . H70 H 1.1211(12) 1.1476(17) 0.3619(7) 0.034(4) Uiso 1 1 d . . . H71 H 1.0017(13) 1.0109(19) 0.3879(9) 0.052(6) Uiso 1 1 d . . . H72 H 0.8829(12) 0.9348(18) 0.3208(7) 0.040(5) Uiso 1 1 d . . . H73 H 0.8436(12) 0.5521(18) -0.0118(7) 0.041(5) Uiso 1 1 d . . . H74 H 0.9527(13) 0.479(2) -0.0704(8) 0.056(6) Uiso 1 1 d . . . H75 H 1.0408(13) 0.6331(19) -0.1135(8) 0.049(5) Uiso 1 1 d . . . H76 H 1.0319(13) 0.867(2) -0.0918(8) 0.051(5) Uiso 1 1 d . . . H77 H 0.9250(12) 0.941(2) -0.0318(7) 0.043(5) Uiso 1 1 d . . . H78 H 0.3473(13) 0.908(2) -0.0691(8) 0.051(5) Uiso 1 1 d . . . H79 H 0.2275(14) 0.803(2) -0.1324(9) 0.057(6) Uiso 1 1 d . . . H80 H 0.2041(11) 0.5690(16) -0.1285(7) 0.030(4) Uiso 1 1 d . . . H81 H 0.2970(12) 0.4420(19) -0.0577(8) 0.045(5) Uiso 1 1 d . . . H82 H 0.4138(12) 0.5493(19) 0.0077(8) 0.044(5) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0226(5) 0.0244(6) 0.0222(6) 0.0007(4) 0.0046(4) 0.0015(4) C2 0.0210(6) 0.0217(7) 0.0229(6) 0.0046(5) 0.0039(5) 0.0015(5) C3 0.0215(6) 0.0239(7) 0.0244(7) 0.0040(5) 0.0037(5) 0.0029(5) C4 0.0223(6) 0.0234(7) 0.0247(7) 0.0035(5) 0.0044(5) 0.0010(5) C5 0.0205(6) 0.0232(7) 0.0245(7) 0.0034(5) 0.0057(5) 0.0011(5) C6 0.0224(6) 0.0248(7) 0.0242(7) 0.0006(5) 0.0056(5) 0.0016(5) C7 0.0225(6) 0.0271(7) 0.0241(7) 0.0000(5) 0.0050(5) 0.0025(5) C8 0.0259(7) 0.0319(8) 0.0282(7) -0.0054(6) 0.0046(6) 0.0025(6) C9 0.0245(7) 0.0325(8) 0.0262(7) -0.0052(6) 0.0026(5) 0.0018(6) C10 0.0217(6) 0.0271(7) 0.0226(7) 0.0007(5) 0.0027(5) 0.0008(5) N11 0.0200(5) 0.0291(7) 0.0234(6) -0.0018(5) 0.0032(4) 0.0027(4) C12 0.0209(6) 0.0257(7) 0.0232(7) 0.0031(5) 0.0030(5) 0.0010(5) C13 0.0197(6) 0.0253(7) 0.0239(7) 0.0039(5) 0.0039(5) 0.0021(5) C14 0.0205(6) 0.0321(8) 0.0251(7) 0.0026(6) 0.0031(5) 0.0032(5) C15 0.0214(6) 0.0315(8) 0.0274(7) 0.0021(6) 0.0050(5) 0.0032(5) C16 0.0224(6) 0.0251(7) 0.0246(7) 0.0032(5) 0.0050(5) 0.0020(5) N17 0.0230(5) 0.0252(6) 0.0224(6) 0.0012(4) 0.0046(4) 0.0028(4) C18 0.0231(6) 0.0228(7) 0.0234(7) 0.0025(5) 0.0057(5) 0.0035(5) C19 0.0248(6) 0.0217(7) 0.0229(6) 0.0029(5) 0.0048(5) 0.0028(5) C20 0.0275(7) 0.0276(7) 0.0216(7) 0.0017(5) 0.0050(5) 0.0024(6) C21 0.0267(7) 0.0250(7) 0.0223(7) 0.0014(5) 0.0034(5) 0.0008(5) C22 0.0249(6) 0.0205(7) 0.0221(6) 0.0024(5) 0.0035(5) 0.0020(5) N23 0.0218(5) 0.0254(6) 0.0213(6) -0.0003(5) 0.0040(4) 0.0027(4) C24 0.0235(6) 0.0208(7) 0.0223(6) 0.0035(5) 0.0024(5) 0.0010(5) C25 0.0390(9) 0.0306(8) 0.0292(8) -0.0020(6) 0.0133(6) 0.0041(7) C26 0.0363(9) 0.0620(12) 0.0363(9) -0.0089(8) 0.0055(7) 0.0118(9) C27 0.0367(8) 0.0265(7) 0.0235(7) 0.0003(6) 0.0014(6) -0.0066(6) C28 0.0330(8) 0.0416(10) 0.0384(9) 0.0018(7) -0.0013(7) -0.0042(7) C29 0.0183(6) 0.0318(8) 0.0242(7) -0.0041(6) 0.0023(5) 0.0009(5) C30 0.0310(8) 0.0352(9) 0.0312(8) 0.0013(6) 0.0082(6) 0.0036(6) C31 0.0340(8) 0.0473(10) 0.0323(8) -0.0017(7) 0.0128(7) -0.0015(7) C32 0.0234(7) 0.0463(10) 0.0372(9) -0.0128(7) 0.0081(6) -0.0005(6) C33 0.0265(7) 0.0337(8) 0.0396(9) -0.0079(7) 0.0022(6) 0.0041(6) C34 0.0252(7) 0.0329(8) 0.0296(8) -0.0033(6) 0.0040(6) 0.0000(6) C35 0.0206(6) 0.0282(7) 0.0247(7) -0.0012(5) 0.0032(5) 0.0032(5) C36 0.0275(7) 0.0360(8) 0.0275(8) 0.0010(6) 0.0049(6) -0.0014(6) C37 0.0290(7) 0.0357(9) 0.0392(9) -0.0055(7) 0.0054(6) -0.0057(6) C38 0.0300(8) 0.0369(9) 0.0330(8) -0.0115(7) -0.0019(6) 0.0013(6) C39 0.0405(9) 0.0360(9) 0.0236(7) -0.0026(6) -0.0004(6) 0.0054(7) C40 0.0274(7) 0.0317(8) 0.0266(7) 0.0011(6) 0.0049(6) 0.0013(6) C41 0.0213(6) 0.0338(8) 0.0212(7) 0.0006(5) 0.0035(5) 0.0049(5) C42 0.0340(8) 0.0352(9) 0.0393(9) 0.0007(7) 0.0123(7) 0.0057(7) C43 0.0425(9) 0.0427(10) 0.0402(9) -0.0065(8) 0.0097(7) 0.0122(8) C44 0.0286(8) 0.0624(12) 0.0287(8) -0.0043(8) 0.0074(6) 0.0103(8) C45 0.0302(8) 0.0560(11) 0.0293(8) 0.0044(7) 0.0106(6) -0.0007(7) C46 0.0290(7) 0.0392(9) 0.0288(8) 0.0014(6) 0.0067(6) 0.0005(6) C47 0.0218(6) 0.0235(7) 0.0229(6) 0.0009(5) 0.0061(5) -0.0004(5) C48 0.0395(8) 0.0249(8) 0.0302(8) 0.0041(6) -0.0035(6) -0.0047(6) C49 0.0356(8) 0.0354(9) 0.0291(8) 0.0041(6) -0.0036(6) -0.0015(7) C50 0.0246(7) 0.0357(8) 0.0329(8) -0.0070(6) 0.0083(6) -0.0054(6) C51 0.0324(8) 0.0226(8) 0.0492(10) -0.0008(7) 0.0086(7) -0.0030(6) C52 0.0278(7) 0.0248(7) 0.0377(8) 0.0067(6) 0.0047(6) 0.0028(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 C2 1.3667(17) . ? N1 C5 1.3668(17) . ? C2 C24 1.4073(18) . ? C2 C3 1.4621(18) . ? C3 C4 1.3727(19) . ? C3 C25 1.458(2) . ? C4 C27 1.454(2) . ? C4 C5 1.4643(18) . ? C5 C6 1.4095(19) . ? C6 C7 1.4003(18) . ? C6 C29 1.4967(18) . ? C7 N11 1.3779(17) . ? C7 C8 1.430(2) . ? C8 C9 1.365(2) . ? C9 C10 1.4375(19) . ? C10 N11 1.3739(17) . ? C10 C12 1.4027(18) . ? C12 C13 1.4098(19) . ? C12 C35 1.4947(19) . ? C13 N17 1.3694(17) . ? C13 C14 1.4590(18) . ? C14 C15 1.345(2) . ? C15 C16 1.4614(19) . ? C16 N17 1.3738(17) . ? C16 C18 1.4022(19) . ? C18 C19 1.4012(18) . ? C18 C41 1.4974(18) . ? C19 N23 1.3766(17) . ? C19 C20 1.4295(19) . ? C20 C21 1.3649(19) . ? C21 C22 1.4314(18) . ? C22 N23 1.3735(17) . ? C22 C24 1.4015(18) . ? C24 C47 1.4981(19) . ? C25 C26 1.125(2) . ? C27 C28 1.136(2) . ? C29 C34 1.393(2) . ? C29 C30 1.394(2) . ? C30 C31 1.389(2) . ? C31 C32 1.375(2) . ? C32 C33 1.385(2) . ? C33 C34 1.392(2) . ? C35 C40 1.396(2) . ? C35 C36 1.402(2) . ? C36 C37 1.388(2) . ? C37 C38 1.384(2) . ? C38 C39 1.379(2) . ? C39 C40 1.387(2) . ? C41 C42 1.390(2) . ? C41 C46 1.392(2) . ? C42 C43 1.393(2) . ? C43 C44 1.384(3) . ? C44 C45 1.370(3) . ? C45 C46 1.393(2) . ? C47 C48 1.388(2) . ? C47 C52 1.390(2) . ? C48 C49 1.390(2) . ? C49 C50 1.382(2) . ? C50 C51 1.379(2) . ? C51 C52 1.388(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 N1 C5 106.62(11) . . ? N1 C2 C24 124.94(12) . . ? N1 C2 C3 110.41(11) . . ? C24 C2 C3 124.57(12) . . ? C4 C3 C25 123.80(12) . . ? C4 C3 C2 106.31(12) . . ? C25 C3 C2 129.82(12) . . ? C3 C4 C27 123.21(12) . . ? C3 C4 C5 106.13(11) . . ? C27 C4 C5 130.61(13) . . ? N1 C5 C6 125.39(12) . . ? N1 C5 C4 110.40(12) . . ? C6 C5 C4 124.17(12) . . ? C7 C6 C5 125.82(12) . . ? C7 C6 C29 115.18(12) . . ? C5 C6 C29 118.97(12) . . ? N11 C7 C6 127.65(13) . . ? N11 C7 C8 106.77(12) . . ? C6 C7 C8 125.56(12) . . ? C9 C8 C7 108.40(13) . . ? C8 C9 C10 107.81(13) . . ? N11 C10 C12 126.30(12) . . ? N11 C10 C9 106.90(11) . . ? C12 C10 C9 126.75(13) . . ? C10 N11 C7 110.11(12) . . ? C10 C12 C13 124.83(12) . . ? C10 C12 C35 116.55(12) . . ? C13 C12 C35 118.57(11) . . ? N17 C13 C12 125.47(12) . . ? N17 C13 C14 110.84(12) . . ? C12 C13 C14 123.68(12) . . ? C15 C14 C13 106.58(12) . . ? C14 C15 C16 106.68(12) . . ? N17 C16 C18 125.89(12) . . ? N17 C16 C15 110.51(12) . . ? C18 C16 C15 123.60(12) . . ? C13 N17 C16 105.33(11) . . ? C19 C18 C16 125.02(12) . . ? C19 C18 C41 116.45(12) . . ? C16 C18 C41 118.51(12) . . ? N23 C19 C18 126.06(12) . . ? N23 C19 C20 107.03(12) . . ? C18 C19 C20 126.81(12) . . ? C21 C20 C19 107.91(12) . . ? C20 C21 C22 108.21(12) . . ? N23 C22 C24 127.70(12) . . ? N23 C22 C21 106.86(11) . . ? C24 C22 C21 125.44(12) . . ? C22 N23 C19 109.94(12) . . ? C22 C24 C2 124.99(12) . . ? C22 C24 C47 114.75(11) . . ? C2 C24 C47 120.26(11) . . ? C26 C25 C3 174.77(17) . . ? C28 C27 C4 173.87(16) . . ? C34 C29 C30 119.20(13) . . ? C34 C29 C6 120.77(13) . . ? C30 C29 C6 120.02(13) . . ? C31 C30 C29 119.99(15) . . ? C32 C31 C30 120.52(16) . . ? C31 C32 C33 120.10(14) . . ? C32 C33 C34 119.90(15) . . ? C33 C34 C29 120.27(15) . . ? C40 C35 C36 118.29(13) . . ? C40 C35 C12 121.00(12) . . ? C36 C35 C12 120.69(12) . . ? C37 C36 C35 120.73(14) . . ? C38 C37 C36 120.20(15) . . ? C39 C38 C37 119.51(15) . . ? C38 C39 C40 120.86(15) . . ? C39 C40 C35 120.35(14) . . ? C42 C41 C46 118.94(14) . . ? C42 C41 C18 120.67(13) . . ? C46 C41 C18 120.39(13) . . ? C41 C42 C43 120.34(16) . . ? C44 C43 C42 120.02(17) . . ? C45 C44 C43 120.06(15) . . ? C44 C45 C46 120.37(16) . . ? C41 C46 C45 120.27(16) . . ? C48 C47 C52 118.77(13) . . ? C48 C47 C24 121.70(12) . . ? C52 C47 C24 119.50(12) . . ? C47 C48 C49 120.58(14) . . ? C50 C49 C48 120.16(15) . . ? C51 C50 C49 119.65(14) . . ? C50 C51 C52 120.36(15) . . ? C51 C52 C47 120.47(14) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.02 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.555 _refine_diff_density_min -0.217 _refine_diff_density_rms 0.052 data_02098 _database_code_CSD 200681 _exptl_crystal_id MSC02098 _audit_creation_date 09/14/2002 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety Zn(C48H28N4) _chemical_formula_sum 'C48 H28 N4 Ni' _chemical_formula_weight 719.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ni Ni 0.3393 1.1124 '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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2(1)/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 24.5972(12) _cell_length_b 10.4576(5) _cell_length_c 13.3721(6) _cell_angle_alpha 90.00 _cell_angle_beta 94.1010(10) _cell_angle_gamma 90.00 _cell_volume 3430.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 114(2) _cell_measurement_reflns_used 9202 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 26.43 _exptl_crystal_description teardrop _exptl_crystal_colour reddish-orange _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.393 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1488 _exptl_absorpt_coefficient_mu 0.608 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 114(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_method '\w scans' _diffrn_measurement_device 'three-circle goniometer with fixed chi' _diffrn_measurement_device_type 'Bruker Platform goniometer' _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker SMART 6000' _diffrn_detector_area_resol_mean 44.52 _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 38662 _diffrn_reflns_av_R_equivalents 0.0860 _diffrn_reflns_av_sigmaI/netI 0.0832 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 27.53 _reflns_number_total 7901 _reflns_number_gt 4764 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1999)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT (Bruker, 1999), XTEL (local package)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Reciprocal Net' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0703P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7901 _refine_ls_number_parameters 630 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0989 _refine_ls_R_factor_gt 0.0538 _refine_ls_wR_factor_ref 0.1409 _refine_ls_wR_factor_gt 0.1262 _refine_ls_goodness_of_fit_ref 0.963 _refine_ls_restrained_S_all 0.963 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.243814(17) 0.97818(4) 0.27905(3) 0.02979(13) Uani 1 1 d . . . N2 N 0.31141(10) 0.9627(2) 0.35824(17) 0.0278(6) Uani 1 1 d . . . C3 C 0.33181(13) 1.0490(3) 0.4298(2) 0.0305(7) Uani 1 1 d . . . C4 C 0.38782(14) 1.0196(3) 0.4588(2) 0.0361(7) Uani 1 1 d . . . C5 C 0.40002(13) 0.9084(3) 0.4114(2) 0.0324(7) Uani 1 1 d . . . C6 C 0.35282(12) 0.8760(3) 0.3467(2) 0.0285(7) Uani 1 1 d . . . C7 C 0.35069(13) 0.7788(3) 0.2748(2) 0.0294(7) Uani 1 1 d . . . C8 C 0.31243(13) 0.7811(3) 0.1939(2) 0.0318(7) Uani 1 1 d . . . C9 C 0.31586(14) 0.7075(3) 0.1035(2) 0.0364(8) Uani 1 1 d . . . C10 C 0.28031(14) 0.7569(3) 0.0344(3) 0.0384(8) Uani 1 1 d . . . C11 C 0.25097(13) 0.8552(3) 0.0823(2) 0.0326(7) Uani 1 1 d . . . N12 N 0.27119(10) 0.8693(2) 0.18019(18) 0.0297(6) Uani 1 1 d . . . C13 C 0.20612(14) 0.9182(3) 0.0372(2) 0.0340(7) Uani 1 1 d . . . C14 C 0.16935(14) 0.9821(3) 0.0946(2) 0.0355(7) Uani 1 1 d . . . C15 C 0.11544(15) 1.0168(4) 0.0601(3) 0.0493(10) Uani 1 1 d . . . C16 C 0.08915(17) 1.0509(5) 0.1422(3) 0.0602(12) Uani 1 1 d . . . C17 C 0.12840(15) 1.0420(4) 0.2266(3) 0.0493(10) Uani 1 1 d . . . N18 N 0.17751(11) 1.0015(2) 0.19696(19) 0.0353(7) Uani 1 1 d . . . C19 C 0.11803(16) 1.0755(5) 0.3251(3) 0.0583(12) Uani 1 1 d . . . C20 C 0.16071(15) 1.0975(4) 0.3960(3) 0.0455(9) Uani 1 1 d . . . C21 C 0.15600(18) 1.1647(4) 0.4891(3) 0.0557(11) Uani 1 1 d . . . C22 C 0.20672(17) 1.1939(4) 0.5269(3) 0.0465(9) Uani 1 1 d . . . C23 C 0.24402(14) 1.1375(3) 0.4604(2) 0.0365(8) Uani 1 1 d . . . N24 N 0.21517(11) 1.0787(3) 0.38132(19) 0.0365(7) Uani 1 1 d . . . C25 C 0.29974(14) 1.1355(3) 0.4783(2) 0.0330(7) Uani 1 1 d . . . C26 C 0.4255(3) 1.1068(6) 0.5103(4) 0.0332(15) Uani 0.50 1 d P . . C27 C 0.4579(3) 1.1817(7) 0.5537(6) 0.0462(19) Uani 0.50 1 d P . . C28 C 0.4520(3) 0.8535(5) 0.4182(4) 0.0269(13) Uani 0.50 1 d P . . C29 C 0.4965(3) 0.8023(6) 0.4286(5) 0.0343(15) Uani 0.50 1 d P . . C30 C 0.39450(13) 0.6798(3) 0.2809(2) 0.0303(7) Uani 1 1 d . . . C31 C 0.39844(16) 0.5957(3) 0.3614(3) 0.0423(9) Uani 1 1 d . . . C32 C 0.44013(19) 0.5055(4) 0.3698(3) 0.0542(11) Uani 1 1 d . . . C33 C 0.47744(18) 0.4991(4) 0.2981(3) 0.0517(11) Uani 1 1 d . . . C34 C 0.47370(16) 0.5819(4) 0.2177(3) 0.0439(9) Uani 1 1 d . . . C35 C 0.43284(14) 0.6718(3) 0.2087(3) 0.0354(8) Uani 1 1 d . . . C36 C 0.19608(14) 0.9132(4) -0.0747(2) 0.0405(8) Uani 1 1 d . . . C37 C 0.1730(2) 0.8113(5) -0.1241(4) 0.0705(14) Uani 1 1 d . . . C38 C 0.1667(3) 0.8148(7) -0.2311(4) 0.085(2) Uani 1 1 d . . . C39 C 0.1826(2) 0.9159(7) -0.2811(4) 0.0830(18) Uani 1 1 d . . . C40 C 0.2051(3) 1.0203(8) -0.2316(4) 0.107(2) Uani 1 1 d . . . C41 C 0.2118(2) 1.0166(6) -0.1292(3) 0.0752(15) Uani 1 1 d . . . C42 C 0.0555(8) 1.067(2) 0.3522(13) 0.057(5) Uani 0.50 1 d P . . C43 C 0.0339(7) 1.1766(19) 0.3735(12) 0.096(7) Uani 0.50 1 d P . . C44 C -0.0307(4) 1.1774(13) 0.3963(6) 0.133(5) Uani 1 1 d . . . C45 C -0.0516(7) 1.070(4) 0.3994(10) 0.173(16) Uani 0.50 1 d P . . C46 C -0.0280(4) 0.9481(16) 0.3743(6) 0.090(4) Uani 0.50 1 d P . . C47 C 0.0287(5) 0.9444(13) 0.3491(8) 0.059(3) Uani 0.50 1 d P . . C48 C 0.32635(14) 1.2199(3) 0.5577(2) 0.0358(8) Uani 1 1 d . . . C49 C 0.33834(15) 1.3453(3) 0.5358(3) 0.0364(8) Uani 1 1 d . . . C50 C 0.36592(16) 1.4229(4) 0.6056(3) 0.0434(9) Uani 1 1 d . . . C51 C 0.38036(17) 1.3763(4) 0.6994(3) 0.0493(10) Uani 1 1 d . . . C52 C 0.3671(2) 1.2541(4) 0.7240(3) 0.0712(15) Uani 1 1 d . . . C53 C 0.3394(2) 1.1749(4) 0.6545(3) 0.0634(14) Uani 1 1 d . . . H63 H 0.3368(14) 0.630(3) 0.097(2) 0.045(10) Uiso 1 1 d . . . H64 H 0.2700(14) 0.726(3) -0.036(3) 0.048(10) Uiso 1 1 d . . . H65 H 0.1193(15) 1.179(4) 0.522(3) 0.055(11) Uiso 1 1 d . . . H66 H 0.2237(15) 1.238(4) 0.599(3) 0.065(12) Uiso 1 1 d . . . H67 H 0.3681(14) 0.595(3) 0.403(2) 0.040(10) Uiso 1 1 d . . . H68 H 0.4405(16) 0.457(4) 0.428(3) 0.064(13) Uiso 1 1 d . . . H69 H 0.5023(17) 0.452(4) 0.303(3) 0.055(13) Uiso 1 1 d . . . H70 H 0.4973(13) 0.581(3) 0.170(2) 0.033(9) Uiso 1 1 d . . . H71 H 0.4316(13) 0.738(3) 0.152(2) 0.037(9) Uiso 1 1 d . . . H72 H 0.1588(14) 0.746(3) -0.086(3) 0.038(10) Uiso 1 1 d . . . H73 H 0.150(3) 0.752(6) -0.251(5) 0.13(3) Uiso 1 1 d . . . H74 H 0.190(2) 0.926(6) -0.353(5) 0.14(2) Uiso 1 1 d . . . H75 H 0.226(3) 1.085(7) -0.293(5) 0.16(2) Uiso 1 1 d . . . H76 H 0.2297(19) 1.084(4) -0.095(3) 0.079(15) Uiso 1 1 d . . . H77 H 0.3309(13) 1.367(3) 0.475(3) 0.041(10) Uiso 1 1 d . . . H78 H 0.3742(15) 1.507(4) 0.590(3) 0.053(12) Uiso 1 1 d . . . H79 H 0.3990(14) 1.428(4) 0.748(3) 0.046(10) Uiso 1 1 d . . . H80 H 0.3764(18) 1.220(4) 0.794(3) 0.080(14) Uiso 1 1 d . . . H81 H 0.3300(15) 1.097(4) 0.672(3) 0.054(12) Uiso 1 1 d . . . C54A C 0.0909(4) 1.0041(10) -0.0371(7) 0.075(3) Uani 0.50 1 d P . . C55A C 0.0660(4) 0.9869(15) -0.1213(7) 0.107(5) Uani 0.50 1 d P . . C56A C 0.0360(4) 1.0970(13) 0.1389(6) 0.092(4) Uani 0.50 1 d P . . C57A C -0.0120(6) 1.1347(19) 0.1287(9) 0.157(8) Uani 0.50 1 d P . . C58A C 0.0662(7) 1.1255(18) 0.3487(13) 0.054(5) Uani 0.50 1 d P . . C59A C 0.0513(7) 1.2547(14) 0.3662(12) 0.077(5) Uani 0.50 1 d P . . C60A C -0.0037(5) 1.2802(14) 0.3929(8) 0.086(4) Uani 0.50 1 d P . . C61A C -0.0315(8) 1.0532(18) 0.3792(12) 0.091(5) Uiso 0.50 1 d P . . C62A C 0.0273(6) 1.0276(16) 0.3529(9) 0.060(3) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0343(2) 0.0307(2) 0.0250(2) -0.00161(18) 0.00645(15) 0.00305(19) N2 0.0373(15) 0.0256(13) 0.0212(12) -0.0014(11) 0.0068(10) -0.0013(12) C3 0.0404(19) 0.0277(17) 0.0240(15) 0.0028(13) 0.0073(13) -0.0027(14) C4 0.043(2) 0.0390(18) 0.0269(16) -0.0021(15) 0.0054(14) 0.0002(16) C5 0.0389(19) 0.0353(18) 0.0234(16) 0.0042(14) 0.0047(13) 0.0005(15) C6 0.0336(18) 0.0260(16) 0.0265(16) 0.0056(13) 0.0069(13) -0.0002(13) C7 0.0341(18) 0.0252(16) 0.0299(17) -0.0008(13) 0.0087(13) -0.0005(13) C8 0.0361(19) 0.0266(16) 0.0333(18) -0.0029(13) 0.0070(14) -0.0018(14) C9 0.039(2) 0.0349(19) 0.0358(19) -0.0110(15) 0.0035(15) 0.0027(16) C10 0.038(2) 0.041(2) 0.0363(19) -0.0116(16) 0.0022(15) -0.0022(16) C11 0.0357(19) 0.0337(18) 0.0288(17) -0.0051(14) 0.0053(14) -0.0029(14) N12 0.0330(15) 0.0310(14) 0.0257(13) -0.0023(11) 0.0066(11) -0.0013(12) C13 0.0382(19) 0.0349(18) 0.0293(17) -0.0056(14) 0.0055(14) -0.0065(15) C14 0.0403(19) 0.0373(18) 0.0289(17) 0.0022(14) 0.0033(14) 0.0017(15) C15 0.048(2) 0.066(3) 0.0339(19) -0.0028(18) 0.0014(16) 0.017(2) C16 0.046(2) 0.095(3) 0.039(2) -0.006(2) 0.0002(17) 0.024(2) C17 0.043(2) 0.074(3) 0.0308(18) -0.0028(18) 0.0008(15) 0.019(2) N18 0.0379(16) 0.0402(17) 0.0283(14) -0.0010(12) 0.0065(11) 0.0073(12) C19 0.047(2) 0.094(3) 0.034(2) -0.004(2) 0.0035(17) 0.028(2) C20 0.045(2) 0.061(3) 0.0314(19) -0.0016(17) 0.0083(16) 0.0174(18) C21 0.055(3) 0.081(3) 0.033(2) -0.0068(19) 0.0141(18) 0.026(2) C22 0.056(3) 0.054(2) 0.0303(19) -0.0060(17) 0.0073(17) 0.0154(19) C23 0.048(2) 0.0349(18) 0.0271(17) 0.0002(14) 0.0062(15) 0.0062(16) N24 0.0425(17) 0.0428(16) 0.0248(14) -0.0012(12) 0.0065(12) 0.0088(13) C25 0.048(2) 0.0267(16) 0.0245(16) 0.0011(13) 0.0045(14) 0.0003(15) C26 0.038(4) 0.038(4) 0.024(3) 0.002(3) 0.002(3) 0.015(3) C27 0.042(5) 0.046(4) 0.049(5) -0.010(4) -0.005(4) 0.021(4) C28 0.045(4) 0.020(3) 0.016(3) -0.003(2) 0.000(3) -0.003(3) C29 0.037(4) 0.028(3) 0.036(4) -0.003(3) -0.007(3) -0.003(3) C30 0.0347(18) 0.0256(16) 0.0308(17) -0.0043(13) 0.0027(13) -0.0021(13) C31 0.052(2) 0.0307(19) 0.046(2) 0.0026(16) 0.0100(18) 0.0014(16) C32 0.072(3) 0.034(2) 0.056(3) 0.0090(19) 0.004(2) 0.0113(19) C33 0.051(3) 0.033(2) 0.072(3) -0.0040(19) 0.003(2) 0.0184(18) C34 0.043(2) 0.041(2) 0.049(2) -0.0130(18) 0.0125(18) 0.0028(17) C35 0.037(2) 0.0303(18) 0.0390(19) -0.0062(15) 0.0043(15) -0.0028(15) C36 0.041(2) 0.050(2) 0.0301(18) -0.0064(16) 0.0032(15) 0.0049(17) C37 0.101(4) 0.052(3) 0.054(3) -0.008(2) -0.023(3) 0.007(3) C38 0.110(5) 0.072(4) 0.067(4) -0.034(3) -0.037(3) 0.041(4) C39 0.087(4) 0.125(5) 0.037(3) 0.001(3) 0.009(3) 0.046(4) C40 0.094(4) 0.182(7) 0.043(3) 0.020(4) -0.001(3) -0.032(4) C41 0.085(4) 0.101(4) 0.039(2) 0.010(3) -0.002(2) -0.031(3) C42 0.022(8) 0.118(18) 0.032(5) 0.000(9) 0.002(6) -0.009(9) C43 0.065(11) 0.17(2) 0.050(7) -0.019(11) 0.010(7) 0.063(12) C44 0.106(8) 0.243(16) 0.048(4) 0.002(7) 0.001(4) 0.006(7) C45 0.065(10) 0.44(5) 0.016(5) 0.011(13) 0.004(6) 0.106(18) C46 0.038(5) 0.210(16) 0.021(4) 0.003(6) -0.003(3) 0.012(7) C47 0.034(6) 0.107(9) 0.035(5) 0.003(7) 0.003(4) -0.018(7) C48 0.051(2) 0.0323(18) 0.0249(17) -0.0022(14) 0.0069(15) 0.0072(15) C49 0.051(2) 0.0318(18) 0.0260(18) 0.0014(15) -0.0019(15) 0.0044(16) C50 0.054(2) 0.036(2) 0.040(2) -0.0063(17) 0.0035(17) 0.0004(18) C51 0.060(3) 0.049(2) 0.037(2) -0.0198(19) -0.0074(18) 0.016(2) C52 0.137(5) 0.050(3) 0.025(2) -0.0073(19) -0.012(2) 0.034(3) C53 0.129(4) 0.029(2) 0.031(2) -0.0013(17) 0.000(2) 0.006(2) C54A 0.056(6) 0.120(9) 0.050(5) -0.006(5) 0.013(4) 0.029(6) C55A 0.063(6) 0.213(15) 0.044(5) -0.027(7) -0.002(5) 0.036(8) C56A 0.076(7) 0.165(11) 0.035(5) -0.025(6) 0.002(5) 0.039(7) C57A 0.096(10) 0.30(2) 0.072(8) -0.086(11) -0.029(7) 0.099(12) C58A 0.025(8) 0.115(15) 0.023(5) -0.008(8) 0.007(4) -0.002(8) C59A 0.069(10) 0.104(11) 0.054(7) -0.031(8) -0.023(7) 0.057(8) C60A 0.058(7) 0.151(12) 0.046(6) -0.033(7) -0.012(5) 0.038(7) C62A 0.039(7) 0.101(11) 0.040(5) 0.001(8) -0.001(5) -0.003(11) _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 N24 1.900(3) . ? Ni1 N12 1.904(2) . ? Ni1 N2 1.913(3) . ? Ni1 N18 1.915(3) . ? N2 C6 1.380(4) . ? N2 C3 1.383(4) . ? C3 C25 1.391(4) . ? C3 C4 1.437(5) . ? C4 C5 1.368(4) . ? C4 C26 1.440(8) . ? C5 C28 1.398(7) . ? C5 C6 1.438(4) . ? C6 C7 1.398(4) . ? C7 C8 1.382(4) . ? C7 C30 1.493(4) . ? C8 N12 1.373(4) . ? C8 C9 1.441(4) . ? C9 C10 1.331(5) . ? C10 C11 1.433(5) . ? C11 N12 1.375(4) . ? C11 C13 1.385(5) . ? C13 C14 1.398(4) . ? C13 C36 1.500(4) . ? C14 N18 1.384(4) . ? C14 C15 1.420(5) . ? C15 C16 1.361(5) . ? C15 C54A 1.399(10) . ? C16 C56A 1.392(11) . ? C16 C17 1.436(5) . ? C17 N18 1.365(4) . ? C17 C19 1.403(5) . ? C19 C20 1.383(5) . ? C19 C58A 1.43(2) . ? C19 C42 1.608(18) . ? C20 N24 1.382(4) . ? C20 C21 1.441(5) . ? C21 C22 1.347(6) . ? C22 C23 1.448(5) . ? C23 C25 1.374(5) . ? C23 N24 1.376(4) . ? C25 C48 1.496(4) . ? C26 C27 1.232(10) . ? C27 C29 1.143(9) 3_676 ? C28 C29 1.217(9) . ? C29 C27 1.143(9) 3_676 ? C30 C31 1.388(5) . ? C30 C35 1.399(4) . ? C31 C32 1.392(5) . ? C32 C33 1.375(6) . ? C33 C34 1.379(6) . ? C34 C35 1.376(5) . ? C36 C37 1.356(6) . ? C36 C41 1.374(6) . ? C37 C38 1.430(7) . ? C38 C39 1.325(9) . ? C39 C40 1.372(9) . ? C40 C41 1.368(7) . ? C42 C43 1.30(3) . ? C42 C47 1.44(2) . ? C43 C44 1.64(2) . ? C44 C45 1.23(4) . ? C44 C60A 1.266(15) . ? C44 C61A 1.319(19) . ? C45 C46 1.45(4) . ? C46 C47 1.458(16) . ? C48 C49 1.381(5) . ? C48 C53 1.392(5) . ? C49 C50 1.378(5) . ? C50 C51 1.369(5) . ? C51 C52 1.365(6) . ? C52 C53 1.387(6) . ? C54A C55A 1.256(13) . ? C55A C57A 1.84(2) 3_575 ? C56A C57A 1.243(14) . ? C57A C55A 1.84(2) 3_575 ? C58A C62A 1.405(19) . ? C58A C59A 1.42(3) . ? C59A C60A 1.45(2) . ? C61A C62A 1.53(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N24 Ni1 N12 176.85(12) . . ? N24 Ni1 N2 90.05(11) . . ? N12 Ni1 N2 89.83(10) . . ? N24 Ni1 N18 89.86(11) . . ? N12 Ni1 N18 90.41(11) . . ? N2 Ni1 N18 177.10(11) . . ? C6 N2 C3 105.8(3) . . ? C6 N2 Ni1 127.8(2) . . ? C3 N2 Ni1 125.8(2) . . ? N2 C3 C25 123.9(3) . . ? N2 C3 C4 109.9(3) . . ? C25 C3 C4 125.3(3) . . ? C5 C4 C3 107.1(3) . . ? C5 C4 C26 127.2(4) . . ? C3 C4 C26 124.4(4) . . ? C4 C5 C28 123.3(4) . . ? C4 C5 C6 106.5(3) . . ? C28 C5 C6 129.5(3) . . ? N2 C6 C7 124.2(3) . . ? N2 C6 C5 110.4(3) . . ? C7 C6 C5 125.1(3) . . ? C8 C7 C6 121.0(3) . . ? C8 C7 C30 120.3(3) . . ? C6 C7 C30 118.4(3) . . ? N12 C8 C7 124.9(3) . . ? N12 C8 C9 109.5(3) . . ? C7 C8 C9 124.7(3) . . ? C10 C9 C8 107.5(3) . . ? C9 C10 C11 107.1(3) . . ? N12 C11 C13 125.9(3) . . ? N12 C11 C10 110.1(3) . . ? C13 C11 C10 123.9(3) . . ? C8 N12 C11 105.6(2) . . ? C8 N12 Ni1 127.1(2) . . ? C11 N12 Ni1 127.1(2) . . ? C11 C13 C14 121.0(3) . . ? C11 C13 C36 119.1(3) . . ? C14 C13 C36 119.8(3) . . ? N18 C14 C13 124.0(3) . . ? N18 C14 C15 110.5(3) . . ? C13 C14 C15 124.7(3) . . ? C16 C15 C54A 125.1(5) . . ? C16 C15 C14 106.9(3) . . ? C54A C15 C14 127.5(5) . . ? C15 C16 C56A 124.4(5) . . ? C15 C16 C17 106.6(3) . . ? C56A C16 C17 128.7(5) . . ? N18 C17 C19 125.0(3) . . ? N18 C17 C16 110.5(3) . . ? C19 C17 C16 124.4(3) . . ? C17 N18 C14 105.3(3) . . ? C17 N18 Ni1 127.4(2) . . ? C14 N18 Ni1 127.3(2) . . ? C20 C19 C17 120.3(3) . . ? C20 C19 C58A 115.5(8) . . ? C17 C19 C58A 121.5(8) . . ? C20 C19 C42 123.1(7) . . ? C17 C19 C42 116.1(7) . . ? C58A C19 C42 24.4(10) . . ? N24 C20 C19 125.1(3) . . ? N24 C20 C21 109.3(3) . . ? C19 C20 C21 124.7(3) . . ? C22 C21 C20 107.8(3) . . ? C21 C22 C23 106.7(3) . . ? C25 C23 N24 125.4(3) . . ? C25 C23 C22 124.6(3) . . ? N24 C23 C22 109.8(3) . . ? C23 N24 C20 106.2(3) . . ? C23 N24 Ni1 127.1(2) . . ? C20 N24 Ni1 126.5(2) . . ? C23 C25 C3 121.4(3) . . ? C23 C25 C48 119.6(3) . . ? C3 C25 C48 118.7(3) . . ? C27 C26 C4 179.4(7) . . ? C29 C27 C26 141.6(8) 3_676 . ? C29 C28 C5 176.5(6) . . ? C27 C29 C28 145.2(7) 3_676 . ? C31 C30 C35 119.0(3) . . ? C31 C30 C7 119.5(3) . . ? C35 C30 C7 121.5(3) . . ? C30 C31 C32 120.1(4) . . ? C33 C32 C31 120.1(4) . . ? C32 C33 C34 120.2(4) . . ? C35 C34 C33 120.3(4) . . ? C34 C35 C30 120.3(3) . . ? C37 C36 C41 119.0(4) . . ? C37 C36 C13 123.1(4) . . ? C41 C36 C13 117.9(3) . . ? C36 C37 C38 118.6(5) . . ? C39 C38 C37 120.7(6) . . ? C38 C39 C40 121.0(5) . . ? C41 C40 C39 118.4(6) . . ? C40 C41 C36 122.3(5) . . ? C43 C42 C47 126.6(18) . . ? C43 C42 C19 114.5(16) . . ? C47 C42 C19 118.8(15) . . ? C42 C43 C44 117.5(17) . . ? C45 C44 C60A 172.9(19) . . ? C45 C44 C61A 27.3(10) . . ? C60A C44 C61A 146.2(16) . . ? C45 C44 C43 114.4(18) . . ? C60A C44 C43 58.6(9) . . ? C61A C44 C43 88.0(15) . . ? C44 C45 C46 128.1(17) . . ? C45 C46 C47 118.8(17) . . ? C42 C47 C46 114.3(14) . . ? C49 C48 C53 118.7(3) . . ? C49 C48 C25 119.9(3) . . ? C53 C48 C25 121.4(3) . . ? C50 C49 C48 121.2(3) . . ? C51 C50 C49 119.6(4) . . ? C52 C51 C50 120.2(4) . . ? C51 C52 C53 120.8(4) . . ? C52 C53 C48 119.4(4) . . ? C55A C54A C15 175.4(12) . . ? C54A C55A C57A 116.8(11) . 3_575 ? C57A C56A C16 175.2(9) . . ? C56A C57A C55A 117.7(15) . 3_575 ? C62A C58A C59A 120.0(17) . . ? C62A C58A C19 111.2(16) . . ? C59A C58A C19 128.7(12) . . ? C58A C59A C60A 118.1(14) . . ? C44 C60A C59A 110.8(12) . . ? C44 C61A C62A 102.1(16) . . ? C58A C62A C61A 122.5(17) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.408 _refine_diff_density_min -0.410 _refine_diff_density_rms 0.065 data_02120 _database_code_CSD 200682 _exptl_crystal_id MSC02120 _audit_creation_date 09/30/2002 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety Ni(C48H26N4) _chemical_formula_sum 'C48 H26 N4 Ni' _chemical_formula_weight 717.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ni Ni 0.3393 1.1124 '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' 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 2(1)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 7.3141(9) _cell_length_b 21.308(3) _cell_length_c 20.088(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3130.6(7) _cell_formula_units_Z 4 _cell_measurement_temperature 128(2) _cell_measurement_reflns_used 6569 _cell_measurement_theta_min 2.79 _cell_measurement_theta_max 27.54 _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.522 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1480 _exptl_absorpt_coefficient_mu 0.667 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; _diffrn_ambient_temperature 128(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_details ' 0.30 degree frames measured for 10.15 seconds each' _diffrn_measurement_method '\w scans' _diffrn_measurement_device 'three-circle goniometer with fixed chi' _diffrn_measurement_device_type 'Bruker Platform goniometer' _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker SMART 6000' _diffrn_detector_area_resol_mean 44.52 _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 66044 _diffrn_reflns_av_R_equivalents 0.1003 _diffrn_reflns_av_sigmaI/netI 0.0437 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 27.56 _reflns_number_total 7221 _reflns_number_gt 6442 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1999)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT (Bruker, 1999), XTEL (local package)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0478P)^2^+0.2636P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00 _refine_ls_number_reflns 7221 _refine_ls_number_parameters 582 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0408 _refine_ls_R_factor_gt 0.0321 _refine_ls_wR_factor_ref 0.0840 _refine_ls_wR_factor_gt 0.0782 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.31955(3) 0.352021(12) 0.506239(14) 0.01573(7) Uani 1 1 d . . . N2 N 0.3558(3) 0.41017(10) 0.43442(10) 0.0181(4) Uani 1 1 d . . . C3 C 0.3239(3) 0.39907(12) 0.36796(13) 0.0209(5) Uani 1 1 d . . . C4 C 0.3592(4) 0.45458(13) 0.32986(13) 0.0248(5) Uani 1 1 d . . . C5 C 0.4098(4) 0.50019(13) 0.37327(13) 0.0244(5) Uani 1 1 d . . . C6 C 0.4041(3) 0.47270(11) 0.43860(12) 0.0198(5) Uani 1 1 d . . . C7 C 0.4271(3) 0.50608(10) 0.49798(12) 0.0197(4) Uani 1 1 d . . . C8 C 0.3950(3) 0.48005(11) 0.56042(12) 0.0185(5) Uani 1 1 d . . . C9 C 0.4125(3) 0.51387(12) 0.62176(12) 0.0211(5) Uani 1 1 d . . . C10 C 0.3441(3) 0.47697(12) 0.67011(13) 0.0206(5) Uani 1 1 d . . . C11 C 0.2865(3) 0.41970(11) 0.63922(12) 0.0181(5) Uani 1 1 d . . . N12 N 0.3277(3) 0.42013(10) 0.57243(10) 0.0169(4) Uani 1 1 d . . . C13 C 0.2102(3) 0.36661(11) 0.67158(12) 0.0179(4) Uani 1 1 d . . . C14 C 0.2233(3) 0.30984(12) 0.63905(12) 0.0192(5) Uani 1 1 d . . . C15 C 0.1931(3) 0.25376(12) 0.67543(12) 0.0195(5) Uani 1 1 d . . . C16 C 0.2421(3) 0.20500(11) 0.63531(12) 0.0187(5) Uani 1 1 d . . . C17 C 0.2922(3) 0.23097(12) 0.57293(13) 0.0200(5) Uani 1 1 d . . . N18 N 0.2813(3) 0.29539(10) 0.57546(10) 0.0175(4) Uani 1 1 d . . . C19 C 0.3198(3) 0.19098(10) 0.52028(10) 0.0174(5) Uani 1 1 d . . . C20 C 0.3056(3) 0.21731(12) 0.45574(13) 0.0189(5) Uani 1 1 d . . . C21 C 0.2587(3) 0.18299(12) 0.39637(12) 0.0223(5) Uani 1 1 d . . . C22 C 0.2330(3) 0.22541(12) 0.34831(12) 0.0217(5) Uani 1 1 d . . . C23 C 0.2672(3) 0.28645(12) 0.37643(12) 0.0209(5) Uani 1 1 d . . . N24 N 0.3066(3) 0.28058(11) 0.44377(10) 0.0186(5) Uani 1 1 d . . . C25 C 0.2706(3) 0.34164(12) 0.34066(12) 0.0210(5) Uani 1 1 d . . . C26 C 0.4561(3) 0.57564(10) 0.49419(11) 0.0200(5) Uani 1 1 d . . . C27 C 0.6035(3) 0.60293(12) 0.46093(13) 0.0233(5) Uani 1 1 d . . . C28 C 0.6187(4) 0.66765(13) 0.45671(13) 0.0268(5) Uani 1 1 d . . . C29 C 0.4888(3) 0.70616(12) 0.48588(12) 0.0264(5) Uani 1 1 d . . . C30 C 0.3439(3) 0.67996(11) 0.52026(11) 0.0231(5) Uani 1 1 d . . . C31 C 0.3263(3) 0.61494(11) 0.52328(11) 0.0210(5) Uani 1 1 d . . . C32 C 0.1299(3) 0.36476(12) 0.73936(11) 0.0195(5) Uani 1 1 d . . . C33 C 0.0739(3) 0.42004(12) 0.77144(12) 0.0228(5) Uani 1 1 d . . . C34 C -0.0033(3) 0.41990(13) 0.83410(12) 0.0258(5) Uani 1 1 d . . . C35 C -0.0331(4) 0.36351(13) 0.86737(13) 0.0283(6) Uani 1 1 d . . . C36 C 0.0127(3) 0.30796(13) 0.83637(12) 0.0236(5) Uani 1 1 d . . . C37 C 0.0936(3) 0.30645(11) 0.77310(11) 0.0204(5) Uani 1 1 d . . . C38 C 0.1321(3) 0.24712(11) 0.73977(11) 0.0197(5) Uani 1 1 d . . . C39 C 0.1172(3) 0.18341(11) 0.76075(12) 0.0217(5) Uani 1 1 d . . . C40 C 0.1657(3) 0.13328(12) 0.71931(12) 0.0209(5) Uani 1 1 d . . . C41 C 0.2322(3) 0.14271(11) 0.65321(12) 0.0191(5) Uani 1 1 d . . . C42 C 0.2964(3) 0.09968(11) 0.60236(12) 0.0202(5) Uani 1 1 d . . . C43 C 0.3255(3) 0.03522(12) 0.61535(13) 0.0226(5) Uani 1 1 d . . . C44 C 0.3948(4) -0.00470(12) 0.56786(14) 0.0257(5) Uani 1 1 d . . . C45 C 0.4415(3) 0.01855(10) 0.50535(16) 0.0246(4) Uani 1 1 d . . . C46 C 0.4162(3) 0.08153(11) 0.49106(12) 0.0218(5) Uani 1 1 d . . . C47 C 0.3397(3) 0.12327(11) 0.53719(12) 0.0189(5) Uani 1 1 d . . . C48 C 0.2188(4) 0.33963(12) 0.26840(12) 0.0227(5) Uani 1 1 d . . . C49 C 0.0551(4) 0.36564(13) 0.24797(13) 0.0295(6) Uani 1 1 d . . . C50 C 0.0016(4) 0.36253(14) 0.18117(15) 0.0345(6) Uani 1 1 d . . . C51 C 0.1131(4) 0.33409(13) 0.13502(13) 0.0317(6) Uani 1 1 d . . . C52 C 0.2772(4) 0.30879(15) 0.15449(13) 0.0353(6) Uani 1 1 d . . . C53 C 0.3295(4) 0.31095(15) 0.22106(14) 0.0327(6) Uani 1 1 d . . . H54 H 0.339(4) 0.4551(16) 0.2851(18) 0.036(9) Uiso 1 1 d . . . H55 H 0.449(4) 0.5404(14) 0.3637(15) 0.028(8) Uiso 1 1 d . . . H56 H 0.454(4) 0.5557(13) 0.6279(14) 0.022(7) Uiso 1 1 d . . . H57 H 0.352(4) 0.4854(15) 0.7149(18) 0.041(9) Uiso 1 1 d . . . H58 H 0.241(4) 0.1366(13) 0.3921(15) 0.028(8) Uiso 1 1 d . . . H59 H 0.192(4) 0.2203(14) 0.3040(17) 0.032(8) Uiso 1 1 d . . . H60 H 0.689(3) 0.5792(12) 0.4420(13) 0.014(6) Uiso 1 1 d . . . H61 H 0.717(4) 0.6852(14) 0.4338(15) 0.024(7) Uiso 1 1 d . . . H62 H 0.504(4) 0.7506(12) 0.4822(12) 0.020(6) Uiso 1 1 d . . . H63 H 0.250(4) 0.7060(13) 0.5394(13) 0.018(6) Uiso 1 1 d . . . H64 H 0.217(3) 0.5958(11) 0.5429(11) 0.007(5) Uiso 1 1 d . . . H65 H 0.079(4) 0.4568(13) 0.7521(14) 0.021(7) Uiso 1 1 d . . . H66 H -0.045(4) 0.4566(13) 0.8524(13) 0.022(7) Uiso 1 1 d . . . H67 H -0.093(4) 0.3663(13) 0.9143(15) 0.024(7) Uiso 1 1 d . . . H68 H -0.011(4) 0.2702(13) 0.8534(14) 0.026(7) Uiso 1 1 d . . . H69 H 0.080(4) 0.1743(13) 0.8024(15) 0.022(7) Uiso 1 1 d . . . H70 H 0.149(3) 0.0922(12) 0.7332(13) 0.013(6) Uiso 1 1 d . . . H71 H 0.298(4) 0.0227(13) 0.6548(16) 0.022(7) Uiso 1 1 d . . . H72 H 0.412(4) -0.0446(14) 0.5773(14) 0.029(8) Uiso 1 1 d . . . H73 H 0.500(3) -0.0092(12) 0.4739(13) 0.017(6) Uiso 1 1 d . . . H74 H 0.466(4) 0.0963(13) 0.4487(14) 0.022(7) Uiso 1 1 d . . . H75 H 0.431(5) 0.2925(15) 0.2324(16) 0.038(9) Uiso 1 1 d . . . H76 H 0.361(5) 0.2928(16) 0.1230(18) 0.048(10) Uiso 1 1 d . . . H77 H 0.088(4) 0.3295(13) 0.0892(16) 0.028(7) Uiso 1 1 d . . . H78 H -0.101(5) 0.3836(16) 0.1650(18) 0.046(9) Uiso 1 1 d . . . H79 H -0.027(4) 0.3829(13) 0.2781(14) 0.020(6) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.01722(12) 0.01792(12) 0.01204(12) 0.00029(13) 0.00035(13) 0.00165(10) N2 0.0200(9) 0.0200(10) 0.0144(10) 0.0008(8) 0.0008(8) 0.0023(8) C3 0.0208(12) 0.0244(13) 0.0176(11) 0.0010(10) -0.0022(9) 0.0041(9) C4 0.0296(13) 0.0287(13) 0.0161(12) 0.0017(10) -0.0008(10) 0.0026(11) C5 0.0324(13) 0.0221(12) 0.0188(12) 0.0048(9) 0.0001(11) 0.0012(11) C6 0.0199(12) 0.0216(12) 0.0180(12) 0.0023(9) 0.0015(9) 0.0037(10) C7 0.0176(9) 0.0194(10) 0.0220(12) 0.0024(9) 0.0007(10) 0.0025(8) C8 0.0181(11) 0.0189(11) 0.0187(11) 0.0006(9) -0.0012(9) 0.0019(9) C9 0.0203(12) 0.0218(12) 0.0214(12) -0.0017(9) -0.0037(10) 0.0027(10) C10 0.0240(12) 0.0213(12) 0.0164(11) -0.0033(10) -0.0030(10) 0.0035(9) C11 0.0156(10) 0.0220(12) 0.0167(11) -0.0003(9) -0.0004(9) 0.0043(9) N12 0.0185(10) 0.0174(10) 0.0148(10) 0.0007(8) -0.0001(7) 0.0012(7) C13 0.0157(10) 0.0237(11) 0.0144(10) -0.0008(9) -0.0016(8) 0.0028(9) C14 0.0172(10) 0.0243(12) 0.0160(11) 0.0029(9) 0.0014(9) 0.0023(9) C15 0.0168(10) 0.0214(11) 0.0205(11) 0.0026(9) -0.0012(9) 0.0007(9) C16 0.0190(11) 0.0219(12) 0.0152(11) 0.0017(9) -0.0004(9) 0.0007(9) C17 0.0184(11) 0.0223(12) 0.0193(12) 0.0044(10) 0.0001(9) -0.0005(9) N18 0.0184(9) 0.0192(10) 0.0150(10) 0.0005(8) 0.0017(8) -0.0008(8) C19 0.0173(9) 0.0174(10) 0.0173(13) 0.0015(8) -0.0006(8) -0.0013(8) C20 0.0146(11) 0.0232(13) 0.0190(12) -0.0038(10) 0.0020(9) -0.0002(9) C21 0.0202(11) 0.0260(12) 0.0206(12) -0.0027(10) -0.0006(10) 0.0007(10) C22 0.0214(12) 0.0261(13) 0.0178(12) -0.0043(10) -0.0032(10) -0.0014(10) C23 0.0182(11) 0.0279(13) 0.0166(11) -0.0017(9) 0.0000(10) 0.0014(10) N24 0.0199(10) 0.0244(11) 0.0115(10) -0.0001(8) 0.0000(7) 0.0015(8) C25 0.0200(12) 0.0292(13) 0.0138(10) -0.0007(9) -0.0016(9) 0.0021(9) C26 0.0205(9) 0.0226(10) 0.0168(12) 0.0002(8) -0.0043(9) 0.0018(8) C27 0.0235(11) 0.0249(12) 0.0216(11) 0.0012(9) 0.0007(10) 0.0021(10) C28 0.0279(12) 0.0289(13) 0.0235(12) 0.0037(10) 0.0000(11) -0.0040(11) C29 0.0330(12) 0.0217(11) 0.0245(12) 0.0018(9) -0.0077(10) 0.0000(10) C30 0.0275(12) 0.0233(11) 0.0183(13) -0.0032(8) -0.0050(9) 0.0050(9) C31 0.0229(11) 0.0218(11) 0.0182(13) -0.0001(8) -0.0019(9) 0.0002(9) C32 0.0144(10) 0.0293(12) 0.0147(11) -0.0008(9) -0.0005(9) 0.0036(9) C33 0.0220(11) 0.0269(12) 0.0194(11) -0.0010(10) -0.0016(9) 0.0030(10) C34 0.0246(12) 0.0328(13) 0.0200(11) -0.0054(10) -0.0001(10) 0.0050(10) C35 0.0252(13) 0.0446(16) 0.0152(11) -0.0015(11) -0.0003(10) 0.0033(11) C36 0.0206(11) 0.0351(14) 0.0151(11) 0.0035(10) -0.0001(9) -0.0017(10) C37 0.0149(10) 0.0293(12) 0.0169(11) 0.0004(9) -0.0017(9) 0.0014(9) C38 0.0150(10) 0.0281(12) 0.0160(11) 0.0002(9) -0.0035(9) 0.0008(9) C39 0.0179(10) 0.0297(13) 0.0174(11) 0.0056(9) -0.0012(9) -0.0022(9) C40 0.0186(11) 0.0240(12) 0.0202(12) 0.0055(9) -0.0033(9) -0.0037(9) C41 0.0147(10) 0.0218(11) 0.0207(12) 0.0018(9) -0.0033(9) -0.0021(8) C42 0.0165(10) 0.0229(12) 0.0213(11) 0.0015(9) -0.0042(9) -0.0021(9) C43 0.0205(12) 0.0239(12) 0.0234(13) 0.0022(10) -0.0041(10) -0.0032(9) C44 0.0239(12) 0.0182(12) 0.0350(14) 0.0006(10) -0.0059(11) -0.0013(10) C45 0.0192(9) 0.0241(10) 0.0306(12) -0.0062(13) -0.0039(13) 0.0000(8) C46 0.0196(10) 0.0229(11) 0.0230(13) -0.0019(9) -0.0009(9) -0.0026(9) C47 0.0157(10) 0.0186(11) 0.0225(12) 0.0013(9) -0.0030(9) -0.0012(9) C48 0.0262(12) 0.0261(12) 0.0157(11) 0.0009(9) -0.0031(10) -0.0043(10) C49 0.0311(14) 0.0376(14) 0.0198(12) 0.0047(11) -0.0008(11) 0.0039(11) C50 0.0353(16) 0.0447(17) 0.0235(14) 0.0060(12) -0.0093(12) 0.0034(13) C51 0.0515(17) 0.0268(13) 0.0167(12) 0.0026(10) -0.0091(12) -0.0056(12) C52 0.0442(16) 0.0428(16) 0.0190(13) -0.0057(11) -0.0006(12) 0.0028(13) C53 0.0312(14) 0.0423(16) 0.0246(13) -0.0039(11) -0.0048(11) 0.0078(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N18 1.862(2) . ? Ni1 N2 1.920(2) . ? Ni1 N12 1.969(2) . ? Ni1 N24 1.975(2) . ? N2 C3 1.376(3) . ? N2 C6 1.381(3) . ? C3 C25 1.396(3) . ? C3 C4 1.432(4) . ? C4 C5 1.357(4) . ? C5 C6 1.438(3) . ? C6 C7 1.399(3) . ? C7 C8 1.391(3) . ? C7 C26 1.499(3) . ? C8 N12 1.390(3) . ? C8 C9 1.433(3) . ? C9 C10 1.346(4) . ? C10 C11 1.432(3) . ? C11 N12 1.375(3) . ? C11 C13 1.419(3) . ? C13 C14 1.378(3) . ? C13 C32 1.483(3) . ? C14 N18 1.381(3) . ? C14 C15 1.418(3) . ? C15 C16 1.363(3) . ? C15 C38 1.375(3) . ? C16 C41 1.377(3) . ? C16 C17 1.418(3) . ? C17 C19 1.373(3) . ? C17 N18 1.376(3) . ? C19 C20 1.416(3) . ? C19 C47 1.489(3) . ? C20 N24 1.369(3) . ? C20 C21 1.440(4) . ? C21 C22 1.336(3) . ? C22 C23 1.440(3) . ? C23 C25 1.378(3) . ? C23 N24 1.389(3) . ? C25 C48 1.501(3) . ? C26 C31 1.394(3) . ? C26 C27 1.395(3) . ? C27 C28 1.386(4) . ? C28 C29 1.386(4) . ? C29 C30 1.383(4) . ? C30 C31 1.393(3) . ? C32 C33 1.404(3) . ? C32 C37 1.440(3) . ? C33 C34 1.379(3) . ? C34 C35 1.392(4) . ? C35 C36 1.379(4) . ? C36 C37 1.403(3) . ? C37 C38 1.458(3) . ? C38 C39 1.425(3) . ? C39 C40 1.400(4) . ? C40 C41 1.428(3) . ? C41 C42 1.451(3) . ? C42 C43 1.414(3) . ? C42 C47 1.438(3) . ? C43 C44 1.375(4) . ? C44 C45 1.392(4) . ? C45 C46 1.385(3) . ? C46 C47 1.401(3) . ? C48 C49 1.382(4) . ? C48 C53 1.391(4) . ? C49 C50 1.399(4) . ? C50 C51 1.376(4) . ? C51 C52 1.372(4) . ? C52 C53 1.392(4) . ? 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 N18 Ni1 N2 179.23(10) . . ? N18 Ni1 N12 88.74(9) . . ? N2 Ni1 N12 91.58(8) . . ? N18 Ni1 N24 88.15(9) . . ? N2 Ni1 N24 91.53(9) . . ? N12 Ni1 N24 176.84(9) . . ? C3 N2 C6 105.6(2) . . ? C3 N2 Ni1 126.49(18) . . ? C6 N2 Ni1 127.75(16) . . ? N2 C3 C25 125.4(2) . . ? N2 C3 C4 110.2(2) . . ? C25 C3 C4 124.3(2) . . ? C5 C4 C3 107.3(2) . . ? C4 C5 C6 106.7(2) . . ? N2 C6 C7 125.0(2) . . ? N2 C6 C5 110.2(2) . . ? C7 C6 C5 124.6(2) . . ? C8 C7 C6 123.08(19) . . ? C8 C7 C26 117.6(2) . . ? C6 C7 C26 118.4(2) . . ? N12 C8 C7 125.6(2) . . ? N12 C8 C9 110.1(2) . . ? C7 C8 C9 124.0(2) . . ? C10 C9 C8 107.1(2) . . ? C9 C10 C11 107.1(2) . . ? N12 C11 C13 122.6(2) . . ? N12 C11 C10 110.6(2) . . ? C13 C11 C10 126.6(2) . . ? C11 N12 C8 104.7(2) . . ? C11 N12 Ni1 130.33(17) . . ? C8 N12 Ni1 124.80(16) . . ? C14 C13 C11 117.1(2) . . ? C14 C13 C32 116.1(2) . . ? C11 C13 C32 126.7(2) . . ? C13 C14 N18 131.0(2) . . ? C13 C14 C15 119.0(2) . . ? N18 C14 C15 109.7(2) . . ? C16 C15 C38 124.3(2) . . ? C16 C15 C14 107.3(2) . . ? C38 C15 C14 128.5(2) . . ? C15 C16 C41 124.5(2) . . ? C15 C16 C17 107.0(2) . . ? C41 C16 C17 128.3(2) . . ? C19 C17 N18 131.0(2) . . ? C19 C17 C16 118.5(2) . . ? N18 C17 C16 110.0(2) . . ? C17 N18 C14 105.9(2) . . ? C17 N18 Ni1 127.60(17) . . ? C14 N18 Ni1 126.33(17) . . ? C17 C19 C20 116.6(2) . . ? C17 C19 C47 116.1(2) . . ? C20 C19 C47 126.8(2) . . ? N24 C20 C19 123.4(2) . . ? N24 C20 C21 110.8(2) . . ? C19 C20 C21 125.0(2) . . ? C22 C21 C20 106.8(2) . . ? C21 C22 C23 107.7(2) . . ? C25 C23 N24 125.5(2) . . ? C25 C23 C22 124.7(2) . . ? N24 C23 C22 109.7(2) . . ? C20 N24 C23 105.0(2) . . ? C20 N24 Ni1 130.36(17) . . ? C23 N24 Ni1 124.01(17) . . ? C23 C25 C3 123.2(2) . . ? C23 C25 C48 118.4(2) . . ? C3 C25 C48 118.4(2) . . ? C31 C26 C27 118.4(2) . . ? C31 C26 C7 118.4(2) . . ? C27 C26 C7 123.1(2) . . ? C28 C27 C26 120.4(2) . . ? C29 C28 C27 120.6(2) . . ? C30 C29 C28 119.9(2) . . ? C29 C30 C31 119.6(2) . . ? C30 C31 C26 121.1(2) . . ? C33 C32 C37 117.0(2) . . ? C33 C32 C13 121.0(2) . . ? C37 C32 C13 121.9(2) . . ? C34 C33 C32 122.4(2) . . ? C33 C34 C35 120.3(3) . . ? C36 C35 C34 119.1(2) . . ? C35 C36 C37 122.1(2) . . ? C36 C37 C32 119.0(2) . . ? C36 C37 C38 121.2(2) . . ? C32 C37 C38 119.8(2) . . ? C15 C38 C39 113.6(2) . . ? C15 C38 C37 113.9(2) . . ? C39 C38 C37 132.5(2) . . ? C40 C39 C38 122.1(2) . . ? C39 C40 C41 122.1(2) . . ? C16 C41 C40 113.3(2) . . ? C16 C41 C42 114.1(2) . . ? C40 C41 C42 132.5(2) . . ? C43 C42 C47 118.3(2) . . ? C43 C42 C41 122.2(2) . . ? C47 C42 C41 119.4(2) . . ? C44 C43 C42 121.9(2) . . ? C43 C44 C45 119.7(2) . . ? C46 C45 C44 119.9(2) . . ? C45 C46 C47 122.1(2) . . ? C46 C47 C42 117.9(2) . . ? C46 C47 C19 120.2(2) . . ? C42 C47 C19 121.7(2) . . ? C49 C48 C53 118.5(2) . . ? C49 C48 C25 119.7(2) . . ? C53 C48 C25 121.8(2) . . ? C48 C49 C50 120.6(3) . . ? C51 C50 C49 120.1(3) . . ? C52 C51 C50 120.0(2) . . ? C51 C52 C53 120.1(3) . . ? C48 C53 C52 120.8(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.606 _refine_diff_density_min -0.428 _refine_diff_density_rms 0.061 data_02141 _database_code_CSD 200683 _exptl_crystal_id MSC02141 _audit_creation_date 10/27/2002 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety C54H46N4Si2 _chemical_formula_sum 'C54 H46 N4 Si2' _chemical_formula_weight 807.13 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.5229(13) _cell_length_b 13.1739(14) _cell_length_c 15.3064(16) _cell_angle_alpha 115.102(3) _cell_angle_beta 104.733(3) _cell_angle_gamma 93.997(3) _cell_volume 2165.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 3326 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 26.63 _exptl_crystal_description needle _exptl_crystal_colour brown/orange _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.238 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 852 _exptl_absorpt_coefficient_mu 0.125 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_max 0.9975 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_details ' 0.30 degree frames measured for 30.16 seconds each' _diffrn_measurement_method '\w scans' _diffrn_measurement_device 'three-circle goniometer with fixed chi' _diffrn_measurement_device_type 'Bruker Platform goniometer' _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker SMART 6000' _diffrn_detector_area_resol_mean 44.52 _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 32370 _diffrn_reflns_av_R_equivalents 0.1731 _diffrn_reflns_av_sigmaI/netI 0.2533 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 27.68 _reflns_number_total 10026 _reflns_number_gt 3439 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1999)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT (Bruker, 1999), XTEL (local package)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1047P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10026 _refine_ls_number_parameters 547 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2311 _refine_ls_R_factor_gt 0.0830 _refine_ls_wR_factor_ref 0.2496 _refine_ls_wR_factor_gt 0.1893 _refine_ls_goodness_of_fit_ref 0.859 _refine_ls_restrained_S_all 0.859 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N -0.1381(3) -0.2219(3) 0.3914(3) 0.0217(9) Uani 1 1 d . . . C2 C -0.2521(4) -0.2685(4) 0.3540(4) 0.0204(11) Uani 1 1 d . . . C3 C -0.3053(4) -0.2482(4) 0.2689(4) 0.0240(12) Uani 1 1 d . . . C4 C -0.2214(4) -0.1860(4) 0.2563(4) 0.0229(11) Uani 1 1 d . . . C5 C -0.1173(4) -0.1699(4) 0.3341(4) 0.0207(11) Uani 1 1 d . . . C6 C -0.0111(4) -0.1138(4) 0.3474(4) 0.0192(11) Uani 1 1 d . . . C7 C 0.0917(4) -0.1028(4) 0.4176(4) 0.0221(11) Uani 1 1 d . . . C8 C 0.1975(4) -0.0382(4) 0.4340(4) 0.0253(12) Uani 1 1 d . . . H61 H 0.2100 0.0073 0.4019 0.030 Uiso 1 1 calc R . . C9 C 0.2778(4) -0.0534(4) 0.5043(4) 0.0278(12) Uani 1 1 d . . . H62 H 0.3560 -0.0203 0.5297 0.033 Uiso 1 1 calc R . . C10 C 0.2232(4) -0.1279(4) 0.5326(4) 0.0242(12) Uani 1 1 d . . . N11 N 0.1103(3) -0.1536(3) 0.4801(3) 0.0187(9) Uani 1 1 d . . . H105 H 0.0578 -0.1963 0.4858 0.022 Uiso 1 1 calc R . . C12 C 0.2772(4) -0.1715(4) 0.5976(4) 0.0237(12) Uani 1 1 d . . . C13 C 0.2216(4) -0.2475(4) 0.6222(4) 0.0250(12) Uani 1 1 d . . . C14 C 0.2768(5) -0.2832(5) 0.6970(4) 0.0350(14) Uani 1 1 d . . . H63 H 0.3554 -0.2665 0.7315 0.042 Uiso 1 1 calc R . . C15 C 0.1957(5) -0.3440(5) 0.7080(4) 0.0324(14) Uani 1 1 d . . . H64 H 0.2061 -0.3784 0.7522 0.039 Uiso 1 1 calc R . . C16 C 0.0887(4) -0.3479(4) 0.6401(4) 0.0247(12) Uani 1 1 d . . . N17 N 0.1074(4) -0.2888(3) 0.5881(3) 0.0257(10) Uani 1 1 d . . . C18 C -0.0181(5) -0.3950(4) 0.6364(4) 0.0244(12) Uani 1 1 d . . . C19 C -0.1211(4) -0.3961(4) 0.5749(4) 0.0224(11) Uani 1 1 d . . . C20 C -0.2299(5) -0.4468(5) 0.5679(4) 0.0317(13) Uani 1 1 d . . . H65 H -0.2432 -0.4879 0.6036 0.038 Uiso 1 1 calc R . . C21 C -0.3102(5) -0.4273(5) 0.5029(4) 0.0288(13) Uani 1 1 d . . . H66 H -0.3894 -0.4508 0.4854 0.035 Uiso 1 1 calc R . . C22 C -0.2534(4) -0.3638(4) 0.4646(4) 0.0225(11) Uani 1 1 d . . . N23 N -0.1403(4) -0.3479(3) 0.5098(3) 0.0229(10) Uani 1 1 d . . . H106 H -0.0873 -0.3118 0.4989 0.027 Uiso 1 1 calc R . . C24 C -0.3066(4) -0.3288(4) 0.3934(4) 0.0224(11) Uani 1 1 d . . . C25 C -0.4208(4) -0.2952(4) 0.1967(4) 0.0252(12) Uani 1 1 d . . . C26 C -0.5129(5) -0.3337(5) 0.1321(5) 0.0341(14) Uani 1 1 d . . . Si27 Si -0.65386(14) -0.40191(14) 0.03328(12) 0.0337(4) Uani 1 1 d . . . C28 C -0.7013(5) -0.5477(4) 0.0159(5) 0.0406(15) Uani 1 1 d . . . H69 H -0.7711 -0.5854 -0.0414 0.061 Uiso 1 1 calc R . . H68 H -0.7149 -0.5424 0.0778 0.061 Uiso 1 1 calc R . . H67 H -0.6429 -0.5925 0.0020 0.061 Uiso 1 1 calc R . . C29 C -0.7585(4) -0.3128(5) 0.0760(5) 0.0409(16) Uani 1 1 d . . . H72 H -0.7405 -0.2389 0.0764 0.061 Uiso 1 1 calc R . . H70 H -0.7551 -0.3000 0.1446 0.061 Uiso 1 1 calc R . . H71 H -0.8346 -0.3528 0.0292 0.061 Uiso 1 1 calc R . . C30 C -0.6428(6) -0.4117(6) -0.0872(5) 0.0525(18) Uani 1 1 d . . . H74 H -0.6260 -0.3345 -0.0806 0.079 Uiso 1 1 calc R . . H73 H -0.7144 -0.4541 -0.1413 0.079 Uiso 1 1 calc R . . H75 H -0.5823 -0.4518 -0.1041 0.079 Uiso 1 1 calc R . . C31 C -0.2430(4) -0.1523(4) 0.1764(4) 0.0280(12) Uani 1 1 d . . . C32 C -0.2676(5) -0.1256(5) 0.1080(4) 0.0334(13) Uani 1 1 d . . . Si33 Si -0.30552(14) -0.09864(14) -0.00436(12) 0.0343(4) Uani 1 1 d . . . C34 C -0.4586(5) -0.1461(6) -0.0676(6) 0.0575(19) Uani 1 1 d . . . H76 H -0.4809 -0.2271 -0.0859 0.086 Uiso 1 1 calc R . . H78 H -0.4786 -0.1360 -0.1293 0.086 Uiso 1 1 calc R . . H77 H -0.4979 -0.1004 -0.0215 0.086 Uiso 1 1 calc R . . C35 C -0.2343(5) -0.1891(4) -0.0895(4) 0.0336(14) Uani 1 1 d . . . H80 H -0.1526 -0.1667 -0.0555 0.050 Uiso 1 1 calc R . . H81 H -0.2519 -0.1798 -0.1515 0.050 Uiso 1 1 calc R . . H79 H -0.2600 -0.2694 -0.1071 0.050 Uiso 1 1 calc R . . C36 C -0.2595(5) 0.0545(5) 0.0320(5) 0.0398(15) Uani 1 1 d . . . H84 H -0.2850 0.1019 0.0891 0.060 Uiso 1 1 calc R . . H83 H -0.2922 0.0689 -0.0260 0.060 Uiso 1 1 calc R . . H82 H -0.1771 0.0736 0.0522 0.060 Uiso 1 1 calc R . . C37 C 0.0011(4) -0.0673(4) 0.2755(3) 0.0185(11) Uani 1 1 d . . . C38 C -0.0151(4) 0.0404(4) 0.2913(4) 0.0273(12) Uani 1 1 d . . . H85 H -0.0365 0.0869 0.3485 0.033 Uiso 1 1 calc R . . C39 C -0.0005(5) 0.0825(5) 0.2244(4) 0.0363(14) Uani 1 1 d . . . H86 H -0.0135 0.1565 0.2353 0.044 Uiso 1 1 calc R . . C40 C 0.0331(4) 0.0156(5) 0.1423(4) 0.0307(13) Uani 1 1 d . . . H87 H 0.0453 0.0444 0.0976 0.037 Uiso 1 1 calc R . . C41 C 0.0487(4) -0.0921(5) 0.1255(4) 0.0284(13) Uani 1 1 d . . . H88 H 0.0695 -0.1387 0.0678 0.034 Uiso 1 1 calc R . . C42 C 0.0345(4) -0.1335(5) 0.1919(4) 0.0261(12) Uani 1 1 d . . . H89 H 0.0475 -0.2076 0.1805 0.031 Uiso 1 1 calc R . . C43 C 0.4022(4) -0.1336(4) 0.6433(4) 0.0252(12) Uani 1 1 d . . . C44 C 0.4736(4) -0.2095(5) 0.6192(4) 0.0307(13) Uani 1 1 d . . . H90 H 0.4426 -0.2884 0.5746 0.037 Uiso 1 1 calc R . . C45 C 0.5904(5) -0.1721(6) 0.6594(4) 0.0424(16) Uani 1 1 d . . . H91 H 0.6389 -0.2249 0.6434 0.051 Uiso 1 1 calc R . . C46 C 0.6351(5) -0.0560(6) 0.7233(5) 0.0474(18) Uani 1 1 d . . . H92 H 0.7144 -0.0285 0.7491 0.057 Uiso 1 1 calc R . . C47 C 0.5639(6) 0.0185(6) 0.7488(5) 0.0534(19) Uani 1 1 d . . . H93 H 0.5949 0.0972 0.7939 0.064 Uiso 1 1 calc R . . C48 C 0.4483(5) -0.0185(5) 0.7103(5) 0.0435(16) Uani 1 1 d . . . H94 H 0.4004 0.0343 0.7293 0.052 Uiso 1 1 calc R . . C49 C -0.0193(4) -0.4397(4) 0.7114(4) 0.0215(11) Uani 1 1 d . . . C50 C 0.0201(4) -0.5386(4) 0.7051(4) 0.0268(12) Uani 1 1 d . . . H95 H 0.0482 -0.5805 0.6509 0.032 Uiso 1 1 calc R . . C51 C 0.0187(5) -0.5759(4) 0.7767(4) 0.0318(13) Uani 1 1 d . . . H96 H 0.0454 -0.6434 0.7710 0.038 Uiso 1 1 calc R . . C52 C -0.0209(4) -0.5164(4) 0.8562(4) 0.0265(12) Uani 1 1 d . . . H97 H -0.0229 -0.5435 0.9044 0.032 Uiso 1 1 calc R . . C53 C -0.0577(4) -0.4171(5) 0.8653(4) 0.0280(12) Uani 1 1 d . . . H98 H -0.0835 -0.3745 0.9208 0.034 Uiso 1 1 calc R . . C54 C -0.0572(5) -0.3794(4) 0.7935(4) 0.0296(13) Uani 1 1 d . . . H99 H -0.0831 -0.3112 0.8004 0.036 Uiso 1 1 calc R . . C55 C -0.4329(4) -0.3512(4) 0.3604(4) 0.0252(12) Uani 1 1 d . . . C56 C -0.4883(4) -0.2608(5) 0.3829(4) 0.0298(13) Uani 1 1 d . . . H100 H -0.4453 -0.1847 0.4181 0.036 Uiso 1 1 calc R . . C57 C -0.6040(5) -0.2780(6) 0.3556(4) 0.0429(16) Uani 1 1 d . . . H101 H -0.6393 -0.2137 0.3708 0.051 Uiso 1 1 calc R . . C58 C -0.6691(6) -0.3854(7) 0.3072(5) 0.0515(18) Uani 1 1 d . . . H102 H -0.7489 -0.3962 0.2897 0.062 Uiso 1 1 calc R . . C59 C -0.6176(5) -0.4776(6) 0.2842(4) 0.0482(18) Uani 1 1 d . . . H103 H -0.6623 -0.5527 0.2511 0.058 Uiso 1 1 calc R . . C60 C -0.4977(5) -0.4627(5) 0.3093(4) 0.0383(15) Uani 1 1 d . . . H104 H -0.4627 -0.5270 0.2916 0.046 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 N1 0.028(2) 0.020(2) 0.027(2) 0.016(2) 0.016(2) 0.0097(19) C2 0.020(3) 0.022(3) 0.028(3) 0.016(2) 0.013(2) 0.007(2) C3 0.024(3) 0.032(3) 0.034(3) 0.027(3) 0.017(2) 0.013(2) C4 0.023(3) 0.028(3) 0.032(3) 0.023(3) 0.014(2) 0.012(2) C5 0.025(3) 0.021(3) 0.026(3) 0.014(2) 0.015(2) 0.008(2) C6 0.022(3) 0.017(3) 0.022(3) 0.011(2) 0.008(2) 0.006(2) C7 0.031(3) 0.017(3) 0.023(3) 0.011(2) 0.013(2) 0.001(2) C8 0.027(3) 0.024(3) 0.025(3) 0.017(2) 0.000(2) -0.004(2) C9 0.024(3) 0.024(3) 0.031(3) 0.014(3) 0.001(2) -0.006(2) C10 0.036(3) 0.019(3) 0.021(3) 0.011(2) 0.010(2) 0.004(2) N11 0.018(2) 0.019(2) 0.023(2) 0.0124(19) 0.0080(19) 0.0032(18) C12 0.030(3) 0.021(3) 0.024(3) 0.013(2) 0.011(2) 0.007(2) C13 0.037(3) 0.023(3) 0.025(3) 0.015(2) 0.016(3) 0.016(3) C14 0.024(3) 0.049(4) 0.048(4) 0.033(3) 0.014(3) 0.018(3) C15 0.037(3) 0.044(4) 0.041(3) 0.034(3) 0.024(3) 0.016(3) C16 0.035(3) 0.024(3) 0.025(3) 0.015(2) 0.016(2) 0.014(2) N17 0.035(3) 0.023(2) 0.030(2) 0.016(2) 0.019(2) 0.009(2) C18 0.039(3) 0.015(3) 0.025(3) 0.010(2) 0.018(3) 0.009(2) C19 0.033(3) 0.020(3) 0.021(3) 0.012(2) 0.013(2) 0.007(2) C20 0.041(3) 0.029(3) 0.031(3) 0.020(3) 0.012(3) -0.005(3) C21 0.029(3) 0.034(3) 0.026(3) 0.021(3) 0.002(2) -0.006(3) C22 0.029(3) 0.019(3) 0.022(3) 0.010(2) 0.012(2) 0.001(2) N23 0.034(3) 0.022(2) 0.024(2) 0.016(2) 0.016(2) 0.008(2) C24 0.033(3) 0.019(3) 0.022(3) 0.012(2) 0.014(2) 0.006(2) C25 0.022(3) 0.029(3) 0.030(3) 0.018(3) 0.009(2) 0.001(2) C26 0.026(3) 0.034(3) 0.049(4) 0.022(3) 0.019(3) 0.006(3) Si27 0.0345(9) 0.0260(9) 0.0373(9) 0.0123(8) 0.0118(8) -0.0017(7) C28 0.049(4) 0.022(3) 0.058(4) 0.015(3) 0.035(3) 0.004(3) C29 0.023(3) 0.027(3) 0.054(4) 0.014(3) -0.008(3) -0.002(3) C30 0.056(4) 0.058(4) 0.046(4) 0.037(4) 0.002(3) -0.011(3) C31 0.023(3) 0.027(3) 0.034(3) 0.011(3) 0.014(3) 0.004(2) C32 0.036(3) 0.034(3) 0.033(3) 0.018(3) 0.010(3) 0.004(3) Si33 0.0405(10) 0.0289(9) 0.0371(9) 0.0174(8) 0.0158(8) 0.0001(8) C34 0.035(4) 0.055(5) 0.091(6) 0.043(4) 0.020(4) 0.002(3) C35 0.041(3) 0.026(3) 0.033(3) 0.017(3) 0.005(3) 0.002(3) C36 0.042(4) 0.030(3) 0.062(4) 0.026(3) 0.028(3) 0.013(3) C37 0.014(2) 0.022(3) 0.019(2) 0.011(2) 0.001(2) 0.001(2) C38 0.041(3) 0.019(3) 0.021(3) 0.008(2) 0.009(2) 0.004(2) C39 0.058(4) 0.019(3) 0.034(3) 0.017(3) 0.010(3) 0.001(3) C40 0.030(3) 0.039(3) 0.028(3) 0.023(3) 0.005(3) -0.001(3) C41 0.022(3) 0.042(4) 0.031(3) 0.022(3) 0.013(2) 0.010(3) C42 0.026(3) 0.030(3) 0.035(3) 0.021(3) 0.017(2) 0.013(2) C43 0.029(3) 0.030(3) 0.021(3) 0.018(3) 0.006(2) 0.004(2) C44 0.020(3) 0.041(3) 0.026(3) 0.014(3) 0.002(2) 0.005(3) C45 0.037(4) 0.065(5) 0.032(3) 0.027(3) 0.011(3) 0.018(3) C46 0.019(3) 0.069(5) 0.043(4) 0.030(4) -0.010(3) -0.011(3) C47 0.047(4) 0.032(4) 0.060(4) 0.022(3) -0.013(4) -0.009(3) C48 0.038(4) 0.028(3) 0.045(4) 0.013(3) -0.010(3) 0.001(3) C49 0.022(3) 0.020(3) 0.027(3) 0.014(2) 0.010(2) 0.001(2) C50 0.040(3) 0.018(3) 0.024(3) 0.010(2) 0.013(3) 0.006(2) C51 0.050(4) 0.021(3) 0.031(3) 0.018(3) 0.013(3) 0.010(3) C52 0.026(3) 0.030(3) 0.027(3) 0.020(3) 0.004(2) 0.000(2) C53 0.030(3) 0.031(3) 0.021(3) 0.010(2) 0.011(2) 0.003(3) C54 0.039(3) 0.023(3) 0.033(3) 0.014(3) 0.019(3) 0.013(3) C55 0.028(3) 0.030(3) 0.017(3) 0.013(2) 0.004(2) -0.005(2) C56 0.020(3) 0.044(4) 0.022(3) 0.013(3) 0.008(2) 0.000(3) C57 0.037(4) 0.067(5) 0.030(3) 0.026(3) 0.012(3) 0.011(3) C58 0.039(4) 0.082(6) 0.037(4) 0.035(4) 0.006(3) 0.003(4) C59 0.039(4) 0.059(5) 0.026(3) 0.019(3) -0.009(3) -0.031(3) C60 0.058(4) 0.036(3) 0.024(3) 0.020(3) 0.008(3) -0.001(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 C2 1.380(6) . ? N1 C5 1.382(6) . ? C2 C24 1.414(6) . ? C2 C3 1.447(6) . ? C3 C4 1.387(7) . ? C3 C25 1.476(7) . ? C4 C31 1.441(7) . ? C4 C5 1.456(7) . ? C5 C6 1.397(7) . ? C6 C7 1.404(7) . ? C6 C37 1.501(6) . ? C7 N11 1.367(6) . ? C7 C8 1.427(7) . ? C8 C9 1.367(7) . ? C9 C10 1.428(7) . ? C10 N11 1.373(6) . ? C10 C12 1.405(7) . ? C12 C13 1.409(7) . ? C12 C43 1.492(7) . ? C13 N17 1.372(7) . ? C13 C14 1.452(7) . ? C14 C15 1.338(7) . ? C15 C16 1.454(7) . ? C16 N17 1.376(6) . ? C16 C18 1.411(7) . ? C18 C19 1.385(7) . ? C18 C49 1.499(6) . ? C19 N23 1.374(6) . ? C19 C20 1.433(7) . ? C20 C21 1.347(7) . ? C21 C22 1.447(7) . ? C22 N23 1.366(6) . ? C22 C24 1.395(7) . ? C24 C55 1.499(7) . ? C25 C26 1.216(7) . ? C26 Si27 1.865(6) . ? Si27 C30 1.835(6) . ? Si27 C28 1.855(5) . ? Si27 C29 1.877(6) . ? C31 C32 1.216(7) . ? C32 Si33 1.854(6) . ? Si33 C35 1.827(6) . ? Si33 C34 1.838(6) . ? Si33 C36 1.853(5) . ? C37 C38 1.374(7) . ? C37 C42 1.396(7) . ? C38 C39 1.396(7) . ? C39 C40 1.384(7) . ? C40 C41 1.368(7) . ? C41 C42 1.383(7) . ? C43 C44 1.385(7) . ? C43 C48 1.393(7) . ? C44 C45 1.395(8) . ? C45 C46 1.393(9) . ? C46 C47 1.373(9) . ? C47 C48 1.380(8) . ? C49 C54 1.394(7) . ? C49 C50 1.399(7) . ? C50 C51 1.382(7) . ? C51 C52 1.375(7) . ? C52 C53 1.381(7) . ? C53 C54 1.385(7) . ? C55 C56 1.382(7) . ? C55 C60 1.400(7) . ? C56 C57 1.375(8) . ? C57 C58 1.364(9) . ? C58 C59 1.370(9) . ? C59 C60 1.429(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 N1 C5 106.9(4) . . ? N1 C2 C24 124.0(4) . . ? N1 C2 C3 110.1(4) . . ? C24 C2 C3 125.9(4) . . ? C4 C3 C2 106.8(4) . . ? C4 C3 C25 123.4(4) . . ? C2 C3 C25 129.3(4) . . ? C3 C4 C31 122.4(4) . . ? C3 C4 C5 106.5(4) . . ? C31 C4 C5 131.0(4) . . ? N1 C5 C6 124.6(4) . . ? N1 C5 C4 109.7(4) . . ? C6 C5 C4 125.6(4) . . ? C5 C6 C7 126.9(4) . . ? C5 C6 C37 119.2(4) . . ? C7 C6 C37 113.7(4) . . ? N11 C7 C6 127.1(4) . . ? N11 C7 C8 107.4(4) . . ? C6 C7 C8 125.5(4) . . ? C9 C8 C7 107.9(4) . . ? C8 C9 C10 107.7(5) . . ? N11 C10 C12 127.0(5) . . ? N11 C10 C9 107.3(4) . . ? C12 C10 C9 125.7(5) . . ? C7 N11 C10 109.7(4) . . ? C10 C12 C13 124.6(5) . . ? C10 C12 C43 117.0(4) . . ? C13 C12 C43 118.5(4) . . ? N17 C13 C12 125.6(4) . . ? N17 C13 C14 110.1(4) . . ? C12 C13 C14 124.0(5) . . ? C15 C14 C13 106.8(5) . . ? C14 C15 C16 107.6(4) . . ? N17 C16 C18 125.5(5) . . ? N17 C16 C15 109.4(4) . . ? C18 C16 C15 124.8(4) . . ? C13 N17 C16 106.2(4) . . ? C19 C18 C16 125.8(4) . . ? C19 C18 C49 117.6(4) . . ? C16 C18 C49 116.5(4) . . ? N23 C19 C18 127.6(5) . . ? N23 C19 C20 106.1(4) . . ? C18 C19 C20 126.3(4) . . ? C21 C20 C19 109.4(4) . . ? C20 C21 C22 107.2(5) . . ? N23 C22 C24 127.7(4) . . ? N23 C22 C21 107.0(4) . . ? C24 C22 C21 125.3(5) . . ? C22 N23 C19 110.4(4) . . ? C22 C24 C2 125.9(5) . . ? C22 C24 C55 116.8(4) . . ? C2 C24 C55 117.2(4) . . ? C26 C25 C3 175.4(5) . . ? C25 C26 Si27 176.2(5) . . ? C30 Si27 C28 109.1(3) . . ? C30 Si27 C26 108.6(3) . . ? C28 Si27 C26 110.7(3) . . ? C30 Si27 C29 111.2(3) . . ? C28 Si27 C29 108.5(3) . . ? C26 Si27 C29 108.7(3) . . ? C32 C31 C4 176.4(6) . . ? C31 C32 Si33 174.8(5) . . ? C35 Si33 C34 108.7(3) . . ? C35 Si33 C36 111.4(3) . . ? C34 Si33 C36 111.0(3) . . ? C35 Si33 C32 105.3(3) . . ? C34 Si33 C32 109.1(3) . . ? C36 Si33 C32 111.3(3) . . ? C38 C37 C42 118.5(5) . . ? C38 C37 C6 122.2(4) . . ? C42 C37 C6 119.2(4) . . ? C37 C38 C39 121.0(5) . . ? C40 C39 C38 119.5(5) . . ? C41 C40 C39 120.0(5) . . ? C40 C41 C42 120.4(5) . . ? C41 C42 C37 120.6(5) . . ? C44 C43 C48 119.2(5) . . ? C44 C43 C12 121.6(5) . . ? C48 C43 C12 119.2(5) . . ? C43 C44 C45 121.0(6) . . ? C46 C45 C44 119.1(6) . . ? C47 C46 C45 119.7(6) . . ? C46 C47 C48 121.4(6) . . ? C47 C48 C43 119.7(6) . . ? C54 C49 C50 117.6(4) . . ? C54 C49 C18 119.7(4) . . ? C50 C49 C18 122.7(4) . . ? C51 C50 C49 120.7(5) . . ? C52 C51 C50 120.9(5) . . ? C51 C52 C53 119.4(5) . . ? C52 C53 C54 120.1(5) . . ? C53 C54 C49 121.3(5) . . ? C56 C55 C60 118.3(5) . . ? C56 C55 C24 120.0(5) . . ? C60 C55 C24 121.7(5) . . ? C57 C56 C55 121.7(6) . . ? C58 C57 C56 121.3(6) . . ? C57 C58 C59 118.9(6) . . ? C58 C59 C60 121.1(6) . . ? C55 C60 C59 118.7(6) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.68 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.118 _refine_diff_density_min -0.494 _refine_diff_density_rms 0.087 data_02144 _database_code_CSD 200684 _exptl_crystal_id MSC02144 _audit_creation_date 10/27/2002 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety [Ni(C54H44N4Si2)];0.7CH2Cl2;0.3C6H6 _chemical_formula_sum 'C56.50 H47.20 Cl1.40 N4 Ni Si2' _chemical_formula_weight 946.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ni Ni 0.3393 1.1124 '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' Si Si 0.0817 0.0704 '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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 21.0116(9) _cell_length_b 17.2824(7) _cell_length_c 12.9553(5) _cell_angle_alpha 90.00 _cell_angle_beta 94.8410(10) _cell_angle_gamma 90.00 _cell_volume 4687.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 134(2) _cell_measurement_reflns_used 6993 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 30.01 _exptl_crystal_description 'trigonal prism' _exptl_crystal_colour black/red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.341 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1976 _exptl_absorpt_coefficient_mu 0.589 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 134(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_details ' 0.30 degree frames measured for 3.16 seconds each' _diffrn_measurement_method '\w scans' _diffrn_measurement_device 'three-circle goniometer with fixed chi' _diffrn_measurement_device_type 'Bruker Platform goniometer' _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker SMART 6000' _diffrn_detector_area_resol_mean 44.52 _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 105693 _diffrn_reflns_av_R_equivalents 0.0662 _diffrn_reflns_av_sigmaI/netI 0.0402 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 30.03 _reflns_number_total 13691 _reflns_number_gt 10127 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1999)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT (Bruker, 1999), XTEL (local package)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. A number of peaks located at .93, y = 0.93, z = 0.75 were modeled as overlapping benzene (70%) and dichloromethane (30%) solvent molecules. ; _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^)+(0.0581P)^2^+1.5974P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13691 _refine_ls_number_parameters 807 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0628 _refine_ls_R_factor_gt 0.0386 _refine_ls_wR_factor_ref 0.1106 _refine_ls_wR_factor_gt 0.0966 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.288 _refine_ls_shift/su_mean 0.008 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 0.582312(9) 0.899471(12) 0.557616(15) 0.01319(6) Uani 1 1 d . . . N2 N 0.66512(6) 0.91983(8) 0.63301(10) 0.0140(2) Uani 1 1 d . . . C3 C 0.71291(7) 0.96767(9) 0.60241(12) 0.0146(3) Uani 1 1 d . . . C4 C 0.75890(7) 0.98453(9) 0.68884(12) 0.0157(3) Uani 1 1 d . . . C5 C 0.74111(7) 0.94064(9) 0.77082(12) 0.0161(3) Uani 1 1 d . . . C6 C 0.68460(7) 0.89857(9) 0.73358(12) 0.0141(3) Uani 1 1 d . . . C7 C 0.65500(7) 0.84221(9) 0.78991(12) 0.0155(3) Uani 1 1 d . . . C8 C 0.59346(8) 0.81732(9) 0.76074(12) 0.0158(3) Uani 1 1 d . . . C9 C 0.55808(8) 0.76556(10) 0.82151(13) 0.0179(3) Uani 1 1 d . . . C10 C 0.49701(8) 0.76724(10) 0.78032(13) 0.0192(3) Uani 1 1 d . . . C11 C 0.49497(8) 0.81652(9) 0.69048(12) 0.0167(3) Uani 1 1 d . . . N12 N 0.55470(6) 0.84601(8) 0.67717(10) 0.0148(3) Uani 1 1 d . . . C13 C 0.44022(8) 0.82735(9) 0.62422(12) 0.0167(3) Uani 1 1 d . . . C14 C 0.44240(7) 0.86326(9) 0.52887(12) 0.0166(3) Uani 1 1 d . . . C15 C 0.38827(8) 0.86951(10) 0.45383(13) 0.0189(3) Uani 1 1 d . . . C16 C 0.40977(8) 0.89587(10) 0.36578(13) 0.0182(3) Uani 1 1 d . . . C17 C 0.47758(7) 0.90775(9) 0.38573(12) 0.0154(3) Uani 1 1 d . . . N18 N 0.49751(6) 0.88907(8) 0.48735(10) 0.0150(3) Uani 1 1 d . . . C19 C 0.51774(8) 0.92741(9) 0.31035(12) 0.0165(3) Uani 1 1 d . . . C20 C 0.58251(8) 0.94114(9) 0.33438(12) 0.0170(3) Uani 1 1 d . . . C21 C 0.62535(8) 0.96519(11) 0.26016(13) 0.0224(3) Uani 1 1 d . . . C22 C 0.68119(9) 0.98398(11) 0.31374(13) 0.0233(4) Uani 1 1 d . . . C23 C 0.67316(8) 0.97087(10) 0.42133(12) 0.0179(3) Uani 1 1 d . . . N24 N 0.61290(6) 0.94178(8) 0.43341(10) 0.0156(3) Uani 1 1 d . . . C25 C 0.71972(8) 0.98849(9) 0.50030(12) 0.0164(3) Uani 1 1 d . . . C26 C 0.81021(8) 1.03830(10) 0.69568(12) 0.0174(3) Uani 1 1 d . . . C27 C 0.85396(8) 1.08343(10) 0.70888(13) 0.0205(3) Uani 1 1 d . . . Si28 Si 0.91824(2) 1.15588(3) 0.72846(4) 0.02137(10) Uani 1 1 d . . . C29 C 0.89085(12) 1.24658(13) 0.66116(19) 0.0339(5) Uani 1 1 d . . . C30 C 0.99125(10) 1.11792(17) 0.6742(2) 0.0413(6) Uani 1 1 d . . . C31 C 0.93312(12) 1.17241(14) 0.87014(17) 0.0345(5) Uani 1 1 d . . . C32 C 0.77060(8) 0.94506(10) 0.87393(13) 0.0194(3) Uani 1 1 d . . . C33 C 0.79749(9) 0.95456(11) 0.95931(14) 0.0242(4) Uani 1 1 d . . . Si34 Si 0.83216(3) 0.98085(3) 1.08985(4) 0.02812(12) Uani 1 1 d . . . C35 C 0.78822(14) 1.06989(15) 1.12377(18) 0.0422(6) Uani 1 1 d . . . C36 C 0.91852(13) 1.0026(2) 1.0861(2) 0.0542(8) Uani 1 1 d . . . C37 C 0.82146(15) 0.90125(15) 1.18288(18) 0.0423(6) Uani 1 1 d . . . C38 C 0.69029(8) 0.80570(10) 0.88228(13) 0.0177(3) Uani 1 1 d . . . C39 C 0.74515(9) 0.76266(10) 0.86859(14) 0.0222(3) Uani 1 1 d . . . C40 C 0.77732(9) 0.72467(11) 0.95213(16) 0.0284(4) Uani 1 1 d . . . C41 C 0.75483(10) 0.72870(12) 1.04918(16) 0.0295(4) Uani 1 1 d . . . C42 C 0.70055(9) 0.77155(12) 1.06406(14) 0.0263(4) Uani 1 1 d . . . C43 C 0.66854(8) 0.81021(10) 0.98094(13) 0.0209(3) Uani 1 1 d . . . C44 C 0.37981(8) 0.79035(10) 0.65344(13) 0.0197(3) Uani 1 1 d . . . C45 C 0.35272(8) 0.81193(11) 0.74312(14) 0.0235(4) Uani 1 1 d . . . C46 C 0.30029(9) 0.77205(13) 0.77529(17) 0.0310(4) Uani 1 1 d . . . C47 C 0.27461(9) 0.71048(13) 0.71758(19) 0.0356(5) Uani 1 1 d . . . C48 C 0.30055(10) 0.68932(12) 0.62739(19) 0.0349(5) Uani 1 1 d . . . C49 C 0.35282(9) 0.72892(11) 0.59494(16) 0.0263(4) Uani 1 1 d . . . C50 C 0.49062(8) 0.93139(10) 0.19966(12) 0.0175(3) Uani 1 1 d . . . C51 C 0.44179(9) 0.98308(10) 0.16861(14) 0.0217(3) Uani 1 1 d . . . C52 C 0.41404(10) 0.98235(11) 0.06710(15) 0.0272(4) Uani 1 1 d . . . C53 C 0.43608(10) 0.93158(12) -0.00439(14) 0.0289(4) Uani 1 1 d . . . C54 C 0.48540(10) 0.88129(12) 0.02442(14) 0.0259(4) Uani 1 1 d . . . C55 C 0.51262(8) 0.88064(11) 0.12659(13) 0.0211(3) Uani 1 1 d . . . C56 C 0.77967(8) 1.02593(10) 0.47097(12) 0.0181(3) Uani 1 1 d . . . C57 C 0.77942(9) 1.10169(11) 0.43330(14) 0.0234(4) Uani 1 1 d . . . C58 C 0.83542(10) 1.13512(13) 0.40475(15) 0.0311(4) Uani 1 1 d . . . C59 C 0.89167(10) 1.09367(13) 0.41146(16) 0.0328(5) Uani 1 1 d . . . C60 C 0.89254(9) 1.01829(13) 0.44822(16) 0.0312(4) Uani 1 1 d . . . C61 C 0.83683(9) 0.98464(12) 0.47831(14) 0.0242(4) Uani 1 1 d . . . Cl62 Cl 0.92972(7) 0.83551(12) 0.67138(14) 0.0762(4) Uani 0.70 1 d P . . C63 C 0.9066(4) 0.8740(5) 0.7870(6) 0.076(3) Uani 0.70 1 d P . . H63A H 0.8597 0.8690 0.7877 0.091 Uiso 0.70 1 calc PR . . H63B H 0.9172 0.9298 0.7896 0.091 Uiso 0.70 1 calc PR . . Cl64 Cl 0.94348(6) 0.82879(8) 0.89797(10) 0.0691(3) Uani 0.70 1 d P . . C65 C 0.9312(7) 0.8966(12) 0.787(2) 0.090(7) Uani 0.30 1 d P . . H65 H 0.9360 0.9440 0.8244 0.108 Uiso 0.30 1 calc PR . . C66 C 0.9443(4) 0.8890(8) 0.6837(7) 0.056(3) Uani 0.30 1 d P . . H66 H 0.9656 0.9323 0.6574 0.068 Uiso 0.30 1 calc PR . . C67 C 0.9325(4) 0.8325(6) 0.6151(8) 0.0384(19) Uani 0.30 1 d P . . H67 H 0.9339 0.8373 0.5422 0.046 Uiso 0.30 1 calc PR . . C68 C 0.9178(6) 0.7654(9) 0.6668(13) 0.091(4) Uani 0.30 1 d P . . H68 H 0.9167 0.7167 0.6327 0.109 Uiso 0.30 1 calc PR . . C69 C 0.9048(6) 0.7715(8) 0.7708(11) 0.081(4) Uani 0.30 1 d P . . H69 H 0.8894 0.7257 0.8008 0.098 Uiso 0.30 1 calc PR . . C70 C 0.9107(6) 0.8296(11) 0.8301(13) 0.088(6) Uani 0.30 1 d P . . H70 H 0.9015 0.8269 0.9005 0.106 Uiso 0.30 1 calc PR . . H71 H 0.5758(10) 0.7368(12) 0.8790(17) 0.024(5) Uiso 1 1 d . . . H72 H 0.4607(10) 0.7390(12) 0.8041(16) 0.023(5) Uiso 1 1 d . . . H73 H 0.3452(10) 0.8563(12) 0.4663(16) 0.020(5) Uiso 1 1 d . . . H74 H 0.3869(10) 0.9028(12) 0.3012(17) 0.023(5) Uiso 1 1 d . . . H75 H 0.6154(10) 0.9663(13) 0.1890(17) 0.026(5) Uiso 1 1 d . . . H76 H 0.7218(12) 1.0023(14) 0.2837(19) 0.041(7) Uiso 1 1 d . . . H77 H 0.8525(16) 1.2668(19) 0.691(2) 0.072(10) Uiso 1 1 d . . . H78 H 0.8792(13) 1.2346(16) 0.588(2) 0.053(8) Uiso 1 1 d . . . H79 H 0.9218(15) 1.2820(19) 0.669(2) 0.068(10) Uiso 1 1 d . . . H80 H 0.9833(16) 1.1120(19) 0.597(3) 0.073(10) Uiso 1 1 d . . . H81 H 1.0292(15) 1.1504(19) 0.696(2) 0.067(9) Uiso 1 1 d . . . H82 H 1.0014(13) 1.0686(16) 0.702(2) 0.043(7) Uiso 1 1 d . . . H83 H 0.9627(16) 1.2155(19) 0.887(2) 0.071(10) Uiso 1 1 d . . . H84 H 0.9511(14) 1.1283(18) 0.903(2) 0.058(8) Uiso 1 1 d . . . H85 H 0.8946(14) 1.1838(16) 0.901(2) 0.054(8) Uiso 1 1 d . . . H86 H 0.7977(16) 1.112(2) 1.071(3) 0.074(10) Uiso 1 1 d . . . H87 H 0.7989(14) 1.0870(17) 1.197(2) 0.062(9) Uiso 1 1 d . . . H88 H 0.7381(16) 1.0601(18) 1.117(2) 0.070(10) Uiso 1 1 d . . . H89 H 0.9247(18) 1.041(2) 1.034(3) 0.093(12) Uiso 1 1 d . . . H90 H 0.9393(15) 0.9507(19) 1.061(2) 0.065(10) Uiso 1 1 d . . . H91 H 0.9319(13) 1.0267(16) 1.160(2) 0.052(8) Uiso 1 1 d . . . H92 H 0.8379(13) 0.9149(15) 1.252(2) 0.047(7) Uiso 1 1 d . . . H93 H 0.8408(14) 0.8528(19) 1.160(2) 0.060(9) Uiso 1 1 d . . . H94 H 0.7781(14) 0.8908(15) 1.185(2) 0.044(7) Uiso 1 1 d . . . H95 H 0.7598(10) 0.7585(12) 0.8031(17) 0.024(5) Uiso 1 1 d . . . H96 H 0.8154(12) 0.6974(14) 0.9420(18) 0.035(6) Uiso 1 1 d . . . H97 H 0.7776(11) 0.7031(14) 1.1050(18) 0.033(6) Uiso 1 1 d . . . H98 H 0.6867(10) 0.7758(12) 1.1283(17) 0.022(5) Uiso 1 1 d . . . H99 H 0.6303(10) 0.8404(12) 0.9882(16) 0.022(5) Uiso 1 1 d . . . H100 H 0.3697(11) 0.8535(14) 0.7817(17) 0.030(6) Uiso 1 1 d . . . H101 H 0.2811(12) 0.7882(14) 0.8352(19) 0.039(7) Uiso 1 1 d . . . H102 H 0.2414(13) 0.6813(16) 0.738(2) 0.049(8) Uiso 1 1 d . . . H103 H 0.2863(13) 0.6470(17) 0.590(2) 0.054(8) Uiso 1 1 d . . . H104 H 0.3706(11) 0.7121(14) 0.5345(18) 0.032(6) Uiso 1 1 d . . . H105 H 0.4254(10) 1.0182(13) 0.2198(17) 0.028(6) Uiso 1 1 d . . . H106 H 0.3793(12) 1.0132(14) 0.0479(18) 0.036(6) Uiso 1 1 d . . . H107 H 0.4174(11) 0.9308(14) -0.0743(19) 0.038(7) Uiso 1 1 d . . . H108 H 0.4968(11) 0.8479(15) -0.0195(19) 0.037(7) Uiso 1 1 d . . . H109 H 0.5448(10) 0.8452(12) 0.1473(17) 0.025(5) Uiso 1 1 d . . . H110 H 0.7424(10) 1.1287(12) 0.4279(16) 0.021(5) Uiso 1 1 d . . . H111 H 0.8340(12) 1.1845(15) 0.3807(19) 0.037(7) Uiso 1 1 d . . . H112 H 0.9288(12) 1.1191(14) 0.3926(19) 0.038(6) Uiso 1 1 d . . . H113 H 0.9308(12) 0.9886(14) 0.4524(18) 0.034(6) Uiso 1 1 d . . . H114 H 0.8364(10) 0.9324(13) 0.5062(17) 0.025(5) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.01389(9) 0.01369(10) 0.01196(10) 0.00021(7) 0.00094(7) -0.00064(7) N2 0.0147(6) 0.0146(6) 0.0129(6) 0.0006(5) 0.0020(5) 0.0010(5) C3 0.0144(7) 0.0131(7) 0.0161(7) -0.0002(5) 0.0007(5) 0.0014(5) C4 0.0154(7) 0.0151(7) 0.0165(7) -0.0016(6) 0.0011(6) 0.0013(6) C5 0.0155(7) 0.0164(8) 0.0163(7) -0.0011(6) 0.0010(6) 0.0012(6) C6 0.0134(6) 0.0146(7) 0.0144(7) -0.0010(6) 0.0015(5) 0.0019(5) C7 0.0174(7) 0.0156(7) 0.0136(7) -0.0001(6) 0.0019(5) 0.0017(6) C8 0.0185(7) 0.0149(7) 0.0141(7) -0.0002(6) 0.0020(6) 0.0005(6) C9 0.0220(8) 0.0144(7) 0.0173(8) 0.0014(6) 0.0011(6) -0.0024(6) C10 0.0212(8) 0.0171(8) 0.0193(8) 0.0015(6) 0.0022(6) -0.0037(6) C11 0.0193(7) 0.0143(7) 0.0168(7) -0.0002(6) 0.0033(6) -0.0016(6) N12 0.0148(6) 0.0145(6) 0.0152(6) -0.0002(5) 0.0015(5) -0.0007(5) C13 0.0162(7) 0.0166(7) 0.0177(7) -0.0010(6) 0.0033(6) -0.0014(6) C14 0.0163(7) 0.0156(7) 0.0178(7) -0.0022(6) 0.0014(6) 0.0008(6) C15 0.0169(7) 0.0205(8) 0.0192(8) -0.0025(6) 0.0002(6) 0.0016(6) C16 0.0161(7) 0.0198(8) 0.0185(8) -0.0034(6) 0.0001(6) 0.0025(6) C17 0.0172(7) 0.0138(7) 0.0149(7) -0.0018(5) -0.0003(5) 0.0016(5) N18 0.0166(6) 0.0152(6) 0.0132(6) -0.0008(5) 0.0020(5) 0.0005(5) C19 0.0198(7) 0.0146(7) 0.0147(7) -0.0005(6) -0.0003(6) 0.0009(6) C20 0.0211(7) 0.0161(8) 0.0136(7) 0.0012(6) 0.0006(6) -0.0010(6) C21 0.0244(8) 0.0275(9) 0.0152(8) 0.0026(7) 0.0017(6) -0.0064(7) C22 0.0238(8) 0.0306(10) 0.0156(8) 0.0035(7) 0.0026(6) -0.0068(7) C23 0.0196(7) 0.0191(8) 0.0150(7) 0.0012(6) 0.0021(6) -0.0023(6) N24 0.0169(6) 0.0160(7) 0.0137(6) 0.0002(5) 0.0013(5) -0.0011(5) C25 0.0174(7) 0.0156(7) 0.0162(7) 0.0003(6) 0.0024(6) -0.0013(6) C26 0.0172(7) 0.0184(8) 0.0164(7) -0.0001(6) 0.0010(6) 0.0030(6) C27 0.0197(8) 0.0205(8) 0.0212(8) -0.0029(6) 0.0015(6) 0.0008(6) Si28 0.0162(2) 0.0228(2) 0.0251(2) -0.00326(19) 0.00166(17) -0.00325(18) C29 0.0401(12) 0.0249(10) 0.0371(12) 0.0036(8) 0.0065(9) -0.0055(9) C30 0.0201(9) 0.0568(16) 0.0475(14) -0.0080(12) 0.0052(9) 0.0039(10) C31 0.0368(11) 0.0364(12) 0.0292(10) -0.0059(9) -0.0039(9) -0.0044(9) C32 0.0181(7) 0.0200(8) 0.0204(8) 0.0013(6) 0.0033(6) -0.0003(6) C33 0.0236(8) 0.0298(10) 0.0191(8) 0.0007(7) 0.0012(6) -0.0031(7) Si34 0.0332(3) 0.0334(3) 0.0167(2) 0.0022(2) -0.0037(2) -0.0091(2) C35 0.0654(17) 0.0351(12) 0.0260(11) -0.0042(9) 0.0024(10) -0.0066(11) C36 0.0372(13) 0.081(2) 0.0415(14) 0.0141(14) -0.0141(11) -0.0181(14) C37 0.0621(16) 0.0402(13) 0.0233(10) 0.0029(9) -0.0034(10) -0.0143(12) C38 0.0190(7) 0.0161(8) 0.0177(7) 0.0036(6) -0.0006(6) -0.0025(6) C39 0.0240(8) 0.0208(8) 0.0215(8) 0.0032(7) 0.0007(7) 0.0023(7) C40 0.0266(9) 0.0243(10) 0.0334(10) 0.0073(8) -0.0029(8) 0.0056(7) C41 0.0327(10) 0.0261(10) 0.0281(10) 0.0126(8) -0.0069(8) -0.0036(8) C42 0.0312(9) 0.0301(10) 0.0171(8) 0.0079(7) -0.0005(7) -0.0081(8) C43 0.0215(8) 0.0221(8) 0.0191(8) 0.0019(6) 0.0007(6) -0.0035(7) C44 0.0162(7) 0.0190(8) 0.0240(8) 0.0044(6) 0.0011(6) -0.0007(6) C45 0.0206(8) 0.0261(9) 0.0238(9) 0.0041(7) 0.0030(7) -0.0009(7) C46 0.0237(9) 0.0381(11) 0.0324(10) 0.0132(9) 0.0090(8) 0.0035(8) C47 0.0183(8) 0.0323(11) 0.0562(14) 0.0184(10) 0.0042(8) -0.0048(8) C48 0.0242(9) 0.0237(10) 0.0553(14) 0.0019(9) -0.0053(9) -0.0054(8) C49 0.0215(8) 0.0226(9) 0.0345(10) -0.0018(8) 0.0010(7) -0.0012(7) C50 0.0186(7) 0.0190(8) 0.0147(7) 0.0015(6) 0.0001(6) -0.0038(6) C51 0.0248(8) 0.0183(8) 0.0214(8) 0.0012(6) -0.0010(7) -0.0012(6) C52 0.0310(9) 0.0228(9) 0.0261(9) 0.0074(7) -0.0072(7) -0.0044(7) C53 0.0383(10) 0.0296(10) 0.0172(8) 0.0053(7) -0.0066(7) -0.0109(8) C54 0.0328(10) 0.0283(10) 0.0171(8) -0.0026(7) 0.0053(7) -0.0080(8) C55 0.0221(8) 0.0228(9) 0.0187(8) 0.0005(6) 0.0030(6) -0.0026(7) C56 0.0183(7) 0.0226(8) 0.0137(7) -0.0019(6) 0.0023(6) -0.0045(6) C57 0.0217(8) 0.0282(9) 0.0199(8) 0.0050(7) -0.0001(6) -0.0048(7) C58 0.0323(10) 0.0361(11) 0.0245(9) 0.0087(8) 0.0000(7) -0.0150(9) C59 0.0262(9) 0.0469(13) 0.0266(10) -0.0021(9) 0.0092(8) -0.0153(9) C60 0.0201(8) 0.0419(12) 0.0325(10) -0.0116(9) 0.0083(7) -0.0035(8) C61 0.0227(8) 0.0267(9) 0.0237(9) -0.0065(7) 0.0053(7) -0.0014(7) Cl62 0.0578(8) 0.1024(13) 0.0687(9) -0.0032(10) 0.0081(8) 0.0321(8) C63 0.062(5) 0.093(7) 0.072(4) 0.007(4) 0.011(4) 0.048(5) Cl64 0.0589(6) 0.0815(8) 0.0656(7) -0.0053(6) -0.0032(5) 0.0321(6) C65 0.058(9) 0.067(9) 0.149(16) -0.033(9) 0.036(10) -0.004(7) C66 0.042(5) 0.092(9) 0.038(5) -0.020(5) 0.017(4) -0.023(5) C67 0.026(4) 0.054(5) 0.035(4) -0.008(4) -0.003(4) 0.006(3) C68 0.067(8) 0.072(9) 0.135(14) 0.008(9) 0.009(8) -0.004(7) C69 0.065(7) 0.090(9) 0.092(9) 0.016(8) 0.027(7) 0.008(6) C70 0.043(6) 0.137(14) 0.091(11) -0.084(10) 0.036(7) -0.048(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N24 1.9265(14) . ? Ni1 N12 1.9341(13) . ? Ni1 N18 1.9396(13) . ? Ni1 N2 1.9540(13) . ? N2 C6 1.3821(19) . ? N2 C3 1.384(2) . ? C3 C25 1.390(2) . ? C3 C4 1.446(2) . ? C4 C5 1.382(2) . ? C4 C26 1.421(2) . ? C5 C32 1.426(2) . ? C5 C6 1.440(2) . ? C6 C7 1.395(2) . ? C7 C8 1.385(2) . ? C7 C38 1.493(2) . ? C8 N12 1.390(2) . ? C8 C9 1.439(2) . ? C9 C10 1.348(2) . ? C10 C11 1.440(2) . ? C11 N12 1.379(2) . ? C11 C13 1.389(2) . ? C13 C14 1.387(2) . ? C13 C44 1.498(2) . ? C14 N18 1.391(2) . ? C14 C15 1.437(2) . ? C15 C16 1.342(2) . ? C16 C17 1.441(2) . ? C17 N18 1.386(2) . ? C17 C19 1.386(2) . ? C19 C20 1.391(2) . ? C19 C50 1.499(2) . ? C20 N24 1.384(2) . ? C20 C21 1.433(2) . ? C21 C22 1.352(2) . ? C22 C23 1.436(2) . ? C23 N24 1.384(2) . ? C23 C25 1.388(2) . ? C25 C56 1.494(2) . ? C26 C27 1.207(2) . ? C27 Si28 1.8437(18) . ? Si28 C31 1.858(2) . ? Si28 C30 1.860(2) . ? Si28 C29 1.861(2) . ? C32 C33 1.210(2) . ? C33 Si34 1.8408(18) . ? Si34 C37 1.855(2) . ? Si34 C36 1.858(3) . ? Si34 C35 1.866(3) . ? C38 C43 1.395(2) . ? C38 C39 1.396(2) . ? C39 C40 1.391(2) . ? C40 C41 1.382(3) . ? C41 C42 1.387(3) . ? C42 C43 1.392(2) . ? C44 C45 1.387(3) . ? C44 C49 1.397(3) . ? C45 C46 1.393(3) . ? C46 C47 1.384(3) . ? C47 C48 1.380(3) . ? C48 C49 1.389(3) . ? C50 C51 1.394(2) . ? C50 C55 1.397(2) . ? C51 C52 1.393(2) . ? C52 C53 1.384(3) . ? C53 C54 1.379(3) . ? C54 C55 1.397(2) . ? C56 C61 1.393(2) . ? C56 C57 1.397(3) . ? C57 C58 1.389(3) . ? C58 C59 1.379(3) . ? C59 C60 1.387(3) . ? C60 C61 1.392(3) . ? Cl62 C63 1.745(8) . ? C63 Cl64 1.757(7) . ? C65 C70 1.37(3) . ? C65 C66 1.40(3) . ? C66 C67 1.330(14) . ? C67 C68 1.386(18) . ? C68 C69 1.402(19) . ? C69 C70 1.264(17) . ? 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 N24 Ni1 N12 173.68(6) . . ? N24 Ni1 N18 90.07(6) . . ? N12 Ni1 N18 90.33(6) . . ? N24 Ni1 N2 90.20(6) . . ? N12 Ni1 N2 90.02(5) . . ? N18 Ni1 N2 174.41(6) . . ? C6 N2 C3 105.34(12) . . ? C6 N2 Ni1 127.14(11) . . ? C3 N2 Ni1 126.96(10) . . ? N2 C3 C25 124.23(14) . . ? N2 C3 C4 110.62(13) . . ? C25 C3 C4 124.70(15) . . ? C5 C4 C26 124.34(15) . . ? C5 C4 C3 106.16(14) . . ? C26 C4 C3 129.37(15) . . ? C4 C5 C32 124.48(15) . . ? C4 C5 C6 106.76(14) . . ? C32 C5 C6 128.41(15) . . ? N2 C6 C7 124.70(14) . . ? N2 C6 C5 110.59(14) . . ? C7 C6 C5 124.67(14) . . ? C8 C7 C6 121.45(14) . . ? C8 C7 C38 118.46(14) . . ? C6 C7 C38 120.07(14) . . ? C7 C8 N12 125.02(15) . . ? C7 C8 C9 123.88(15) . . ? N12 C8 C9 110.61(14) . . ? C10 C9 C8 106.77(15) . . ? C9 C10 C11 107.17(15) . . ? N12 C11 C13 126.03(15) . . ? N12 C11 C10 110.75(14) . . ? C13 C11 C10 123.09(15) . . ? C11 N12 C8 104.50(13) . . ? C11 N12 Ni1 127.91(11) . . ? C8 N12 Ni1 126.76(11) . . ? C14 C13 C11 121.54(15) . . ? C14 C13 C44 120.56(14) . . ? C11 C13 C44 117.49(14) . . ? C13 C14 N18 125.39(14) . . ? C13 C14 C15 123.56(15) . . ? N18 C14 C15 110.59(14) . . ? C16 C15 C14 107.26(15) . . ? C15 C16 C17 107.14(14) . . ? N18 C17 C19 125.01(14) . . ? N18 C17 C16 110.62(14) . . ? C19 C17 C16 124.06(15) . . ? C17 N18 C14 104.33(13) . . ? C17 N18 Ni1 128.04(11) . . ? C14 N18 Ni1 127.60(11) . . ? C17 C19 C20 121.78(15) . . ? C17 C19 C50 118.72(14) . . ? C20 C19 C50 119.48(14) . . ? N24 C20 C19 125.11(15) . . ? N24 C20 C21 110.67(14) . . ? C19 C20 C21 123.88(15) . . ? C22 C21 C20 107.00(15) . . ? C21 C22 C23 107.01(15) . . ? N24 C23 C25 126.23(15) . . ? N24 C23 C22 110.54(14) . . ? C25 C23 C22 123.19(15) . . ? C23 N24 C20 104.66(13) . . ? C23 N24 Ni1 127.26(11) . . ? C20 N24 Ni1 127.66(11) . . ? C23 C25 C3 121.46(15) . . ? C23 C25 C56 117.68(14) . . ? C3 C25 C56 120.73(14) . . ? C27 C26 C4 175.44(18) . . ? C26 C27 Si28 177.49(16) . . ? C27 Si28 C31 107.49(10) . . ? C27 Si28 C30 109.05(10) . . ? C31 Si28 C30 110.63(12) . . ? C27 Si28 C29 108.27(10) . . ? C31 Si28 C29 110.67(11) . . ? C30 Si28 C29 110.62(12) . . ? C33 C32 C5 174.74(19) . . ? C32 C33 Si34 172.42(18) . . ? C33 Si34 C37 110.71(10) . . ? C33 Si34 C36 109.72(11) . . ? C37 Si34 C36 109.82(14) . . ? C33 Si34 C35 104.75(10) . . ? C37 Si34 C35 111.66(13) . . ? C36 Si34 C35 110.08(15) . . ? C43 C38 C39 118.95(15) . . ? C43 C38 C7 122.11(15) . . ? C39 C38 C7 118.88(15) . . ? C40 C39 C38 120.32(17) . . ? C41 C40 C39 120.20(18) . . ? C40 C41 C42 120.12(17) . . ? C41 C42 C43 119.89(18) . . ? C42 C43 C38 120.51(17) . . ? C45 C44 C49 118.83(17) . . ? C45 C44 C13 120.87(16) . . ? C49 C44 C13 120.09(16) . . ? C44 C45 C46 120.56(19) . . ? C47 C46 C45 120.1(2) . . ? C48 C47 C46 119.84(19) . . ? C47 C48 C49 120.3(2) . . ? C48 C49 C44 120.4(2) . . ? C51 C50 C55 118.96(15) . . ? C51 C50 C19 121.10(15) . . ? C55 C50 C19 119.89(15) . . ? C52 C51 C50 120.39(17) . . ? C53 C52 C51 120.04(18) . . ? C54 C53 C52 120.30(17) . . ? C53 C54 C55 119.98(18) . . ? C54 C55 C50 120.28(17) . . ? C61 C56 C57 118.79(16) . . ? C61 C56 C25 120.10(16) . . ? C57 C56 C25 121.09(15) . . ? C58 C57 C56 120.30(18) . . ? C59 C58 C57 120.5(2) . . ? C58 C59 C60 119.76(18) . . ? C59 C60 C61 120.11(19) . . ? C60 C61 C56 120.49(19) . . ? Cl62 C63 Cl64 113.4(4) . . ? C70 C65 C66 113.7(16) . . ? C67 C66 C65 132.1(13) . . ? C66 C67 C68 109.1(13) . . ? C67 C68 C69 118.2(14) . . ? C70 C69 C68 128.8(15) . . ? C69 C70 C65 116.4(17) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.627 _refine_diff_density_min -0.385 _refine_diff_density_rms 0.076 data_02158 _database_code_CSD 200685 _exptl_crystal_id MSC02158 _audit_creation_date 10/27/2002 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H28 N4' _chemical_formula_weight 660.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8696(9) _cell_length_b 12.4991(11) _cell_length_c 14.6985(13) _cell_angle_alpha 67.303(2) _cell_angle_beta 73.845(2) _cell_angle_gamma 73.605(2) _cell_volume 1575.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 138(2) _cell_measurement_reflns_used 3570 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 24.96 _exptl_crystal_description multifacited _exptl_crystal_colour 'metallic black' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.393 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 688 _exptl_absorpt_coefficient_mu 0.082 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 138(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_details ' 0.30 degree frames measured for 30.16 seconds each' _diffrn_measurement_method '\w scans' _diffrn_measurement_device 'three-circle goniometer with fixed chi' _diffrn_measurement_device_type 'Bruker Platform goniometer' _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker SMART 6000' _diffrn_detector_area_resol_mean 44.52 _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 15411 _diffrn_reflns_av_R_equivalents 0.1393 _diffrn_reflns_av_sigmaI/netI 0.1637 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 25.10 _reflns_number_total 5566 _reflns_number_gt 2819 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1999)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT (Bruker, 1999), XTEL (local package)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0095P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5566 _refine_ls_number_parameters 581 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1326 _refine_ls_R_factor_gt 0.0545 _refine_ls_wR_factor_ref 0.1143 _refine_ls_wR_factor_gt 0.0932 _refine_ls_goodness_of_fit_ref 0.915 _refine_ls_restrained_S_all 0.915 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.7536(3) 1.0134(2) -0.0012(2) 0.0220(7) Uani 1 1 d . . . C2 C 0.6783(4) 1.0933(3) -0.0735(2) 0.0238(8) Uani 1 1 d . . . C3 C 0.7138(4) 1.0588(3) -0.1624(3) 0.0260(9) Uani 1 1 d . . . C4 C 0.8102(4) 0.9551(3) -0.1416(3) 0.0263(9) Uani 1 1 d . . . C5 C 0.8341(4) 0.9280(3) -0.0414(2) 0.0218(8) Uani 1 1 d . . . C6 C 0.9295(3) 0.8248(3) 0.0058(2) 0.0212(8) Uani 1 1 d . . . C7 C 0.9692(3) 0.7979(3) 0.0971(2) 0.0199(8) Uani 1 1 d . . . C8 C 1.0519(3) 0.6890(3) 0.1516(2) 0.0211(8) Uani 1 1 d . . . C9 C 1.0612(4) 0.6975(3) 0.2389(3) 0.0234(8) Uani 1 1 d . . . C10 C 0.9845(3) 0.8115(3) 0.2433(2) 0.0213(8) Uani 1 1 d . . . N11 N 0.9298(3) 0.8686(2) 0.1566(2) 0.0212(7) Uani 1 1 d . . . C12 C 0.9527(3) 0.8612(3) 0.3209(2) 0.0211(8) Uani 1 1 d . . . C13 C 0.8359(4) 0.9562(3) 0.3241(3) 0.0241(8) Uani 1 1 d . . . C14 C 0.7897(3) 0.9829(3) 0.4151(2) 0.0212(8) Uani 1 1 d . . . C15 C 0.6668(4) 1.0693(3) 0.4048(2) 0.0231(8) Uani 1 1 d . . . C16 C 0.6410(4) 1.0961(3) 0.3068(2) 0.0219(8) Uani 1 1 d . . . N17 N 0.7445(3) 1.0256(2) 0.2569(2) 0.0231(7) Uani 1 1 d . . . C18 C 0.5273(4) 1.1899(3) 0.2761(2) 0.0230(8) Uani 1 1 d . . . C19 C 0.5097(3) 1.2359(3) 0.1747(3) 0.0227(8) Uani 1 1 d . . . C20 C 0.4411(3) 1.3486(3) 0.1166(3) 0.0227(8) Uani 1 1 d . . . C21 C 0.4599(4) 1.3509(3) 0.0205(3) 0.0237(8) Uani 1 1 d . . . C22 C 0.5439(3) 1.2381(3) 0.0151(2) 0.0199(8) Uani 1 1 d . . . N23 N 0.5735(3) 1.1728(2) 0.1099(2) 0.0216(7) Uani 1 1 d . . . C24 C 0.5839(3) 1.1999(3) -0.0676(2) 0.0224(8) Uani 1 1 d . . . C25 C 0.9903(3) 0.7350(3) -0.0468(2) 0.0200(8) Uani 1 1 d . . . C26 C 0.8962(4) 0.6834(3) -0.0652(3) 0.0254(8) Uani 1 1 d . . . C27 C 0.9484(4) 0.6038(3) -0.1163(3) 0.0277(9) Uani 1 1 d . . . C28 C 1.0937(4) 0.5737(3) -0.1512(3) 0.0286(9) Uani 1 1 d . . . C29 C 1.1885(4) 0.6247(3) -0.1344(3) 0.0284(9) Uani 1 1 d . . . C30 C 1.1376(4) 0.7048(3) -0.0820(3) 0.0278(9) Uani 1 1 d . . . C31 C 1.0308(4) 0.8122(3) 0.4058(2) 0.0225(8) Uani 1 1 d . . . C32 C 1.1667(4) 0.7354(3) 0.4002(3) 0.0250(8) Uani 1 1 d . . . C33 C 1.2410(4) 0.6856(3) 0.4776(3) 0.0255(8) Uani 1 1 d . . . C34 C 1.1823(4) 0.7112(3) 0.5672(3) 0.0286(9) Uani 1 1 d . . . C35 C 1.0544(4) 0.7896(3) 0.5750(3) 0.0256(8) Uani 1 1 d . . . C36 C 0.9771(4) 0.8433(3) 0.4956(2) 0.0242(8) Uani 1 1 d . . . C37 C 0.8457(4) 0.9324(3) 0.5015(2) 0.0234(8) Uani 1 1 d . . . C38 C 0.7664(4) 0.9766(3) 0.5801(3) 0.0261(8) Uani 1 1 d . . . C39 C 0.6439(4) 1.0654(3) 0.5694(3) 0.0272(9) Uani 1 1 d . . . C40 C 0.5888(4) 1.1167(3) 0.4785(3) 0.0249(8) Uani 1 1 d . . . C41 C 0.4639(4) 1.2082(3) 0.4512(3) 0.0241(8) Uani 1 1 d . . . C42 C 0.3733(4) 1.2629(3) 0.5192(3) 0.0270(9) Uani 1 1 d . . . C43 C 0.2484(4) 1.3443(3) 0.4973(3) 0.0282(9) Uani 1 1 d . . . C44 C 0.2091(4) 1.3685(3) 0.4059(3) 0.0281(9) Uani 1 1 d . . . C45 C 0.2977(4) 1.3165(3) 0.3376(3) 0.0251(8) Uani 1 1 d . . . C46 C 0.4317(4) 1.2405(3) 0.3539(3) 0.0238(8) Uani 1 1 d . . . C47 C 0.5136(3) 1.2773(3) -0.1557(2) 0.0227(8) Uani 1 1 d . . . C48 C 0.5500(4) 1.3853(3) -0.2179(3) 0.0237(8) Uani 1 1 d . . . C49 C 0.4837(4) 1.4562(3) -0.3002(3) 0.0264(9) Uani 1 1 d . . . C50 C 0.3770(4) 1.4184(3) -0.3177(3) 0.0263(9) Uani 1 1 d . . . C51 C 0.3363(4) 1.3117(3) -0.2542(3) 0.0269(9) Uani 1 1 d . . . C52 C 0.4051(4) 1.2406(3) -0.1746(3) 0.0234(8) Uani 1 1 d . . . H53 H 0.676(3) 1.105(3) -0.229(2) 0.025(9) Uiso 1 1 d . . . H54 H 0.868(3) 0.908(3) -0.194(2) 0.040(10) Uiso 1 1 d . . . H55 H 1.094(3) 0.623(3) 0.129(2) 0.019(8) Uiso 1 1 d . . . H56 H 1.097(4) 0.634(3) 0.297(3) 0.048(11) Uiso 1 1 d . . . H57 H 0.389(3) 1.412(3) 0.144(2) 0.020(8) Uiso 1 1 d . . . H58 H 0.434(3) 1.420(3) -0.045(2) 0.033(9) Uiso 1 1 d . . . H59 H 0.793(3) 0.700(3) -0.036(2) 0.027(9) Uiso 1 1 d . . . H60 H 0.878(4) 0.563(3) -0.126(2) 0.033(9) Uiso 1 1 d . . . H61 H 1.130(3) 0.524(3) -0.188(2) 0.034(10) Uiso 1 1 d . . . H62 H 1.292(4) 0.606(3) -0.159(2) 0.030(10) Uiso 1 1 d . . . H63 H 1.211(4) 0.737(3) -0.071(2) 0.036(10) Uiso 1 1 d . . . H64 H 1.211(4) 0.724(3) 0.337(3) 0.040(11) Uiso 1 1 d . . . H65 H 1.342(4) 0.627(3) 0.473(2) 0.049(11) Uiso 1 1 d . . . H66 H 1.233(3) 0.675(3) 0.626(2) 0.036(10) Uiso 1 1 d . . . H67 H 1.011(3) 0.813(3) 0.638(2) 0.020(8) Uiso 1 1 d . . . H68 H 0.797(3) 0.944(3) 0.643(2) 0.026(9) Uiso 1 1 d . . . H69 H 0.589(3) 1.085(3) 0.630(2) 0.017(8) Uiso 1 1 d . . . H70 H 0.400(3) 1.242(3) 0.587(2) 0.033(10) Uiso 1 1 d . . . H71 H 0.177(3) 1.384(3) 0.546(2) 0.021(8) Uiso 1 1 d . . . H72 H 0.116(3) 1.418(3) 0.392(2) 0.025(9) Uiso 1 1 d . . . H73 H 0.268(3) 1.329(2) 0.281(2) 0.011(8) Uiso 1 1 d . . . H74 H 0.626(3) 1.410(3) -0.210(2) 0.018(9) Uiso 1 1 d . . . H75 H 0.514(3) 1.526(3) -0.339(2) 0.028(10) Uiso 1 1 d . . . H76 H 0.326(4) 1.472(4) -0.378(3) 0.068(13) Uiso 1 1 d . . . H77 H 0.262(4) 1.287(3) -0.268(2) 0.035(10) Uiso 1 1 d . . . H78 H 0.372(3) 1.161(3) -0.123(2) 0.029(9) Uiso 1 1 d . . . H79 H 0.642(5) 1.084(4) 0.131(4) 0.107(17) Uiso 1 1 d . . . H80 H 0.866(4) 0.948(4) 0.145(3) 0.061(13) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0273(17) 0.0170(14) 0.0221(16) -0.0067(13) -0.0081(14) -0.0013(13) C2 0.029(2) 0.0201(18) 0.025(2) -0.0087(17) -0.0063(17) -0.0059(15) C3 0.037(2) 0.0198(18) 0.020(2) -0.0035(17) -0.0094(18) -0.0043(17) C4 0.036(2) 0.0218(19) 0.023(2) -0.0089(17) -0.0059(17) -0.0058(16) C5 0.028(2) 0.0160(17) 0.023(2) -0.0073(16) -0.0069(16) -0.0036(15) C6 0.026(2) 0.0153(16) 0.023(2) -0.0067(15) -0.0059(16) -0.0043(15) C7 0.0208(19) 0.0184(17) 0.022(2) -0.0091(16) -0.0016(15) -0.0042(14) C8 0.023(2) 0.0167(17) 0.028(2) -0.0104(17) -0.0077(16) -0.0023(15) C9 0.027(2) 0.0188(18) 0.025(2) -0.0057(17) -0.0094(17) -0.0030(15) C10 0.023(2) 0.0170(17) 0.025(2) -0.0054(16) -0.0067(16) -0.0059(14) N11 0.0259(17) 0.0158(14) 0.0239(17) -0.0079(14) -0.0081(14) -0.0021(13) C12 0.024(2) 0.0172(17) 0.024(2) -0.0053(16) -0.0069(16) -0.0068(15) C13 0.029(2) 0.0190(17) 0.025(2) -0.0048(17) -0.0069(17) -0.0078(15) C14 0.025(2) 0.0198(17) 0.020(2) -0.0061(16) -0.0029(16) -0.0072(15) C15 0.027(2) 0.0197(18) 0.025(2) -0.0111(17) -0.0045(17) -0.0031(16) C16 0.028(2) 0.0192(17) 0.020(2) -0.0073(16) -0.0048(16) -0.0067(15) N17 0.0258(17) 0.0216(15) 0.0251(17) -0.0098(14) -0.0089(14) -0.0025(13) C18 0.028(2) 0.0207(18) 0.024(2) -0.0067(16) -0.0078(17) -0.0101(15) C19 0.022(2) 0.0220(18) 0.027(2) -0.0115(17) -0.0061(16) -0.0031(15) C20 0.0195(19) 0.0229(18) 0.027(2) -0.0096(17) -0.0064(16) -0.0018(15) C21 0.030(2) 0.0191(18) 0.023(2) -0.0050(16) -0.0104(17) -0.0035(15) C22 0.0220(19) 0.0171(17) 0.022(2) -0.0074(16) -0.0042(15) -0.0049(14) N23 0.0284(17) 0.0191(15) 0.0189(16) -0.0078(13) -0.0065(14) -0.0031(13) C24 0.025(2) 0.0192(17) 0.026(2) -0.0080(16) -0.0084(16) -0.0051(15) C25 0.025(2) 0.0187(17) 0.0158(19) -0.0046(15) -0.0069(15) -0.0021(15) C26 0.026(2) 0.0235(18) 0.026(2) -0.0094(17) -0.0069(17) -0.0014(16) C27 0.036(2) 0.0217(18) 0.031(2) -0.0105(17) -0.0156(18) -0.0020(17) C28 0.045(3) 0.0191(18) 0.023(2) -0.0085(17) -0.0123(18) -0.0008(17) C29 0.028(2) 0.0234(19) 0.031(2) -0.0104(18) -0.0044(18) -0.0007(17) C30 0.028(2) 0.0266(19) 0.032(2) -0.0127(18) -0.0075(18) -0.0055(17) C31 0.030(2) 0.0188(17) 0.021(2) -0.0038(16) -0.0058(16) -0.0111(15) C32 0.029(2) 0.0200(18) 0.028(2) -0.0080(18) -0.0107(18) -0.0025(16) C33 0.031(2) 0.0207(17) 0.025(2) -0.0059(17) -0.0089(18) -0.0048(16) C34 0.036(2) 0.0237(19) 0.027(2) -0.0030(17) -0.0140(19) -0.0079(17) C35 0.034(2) 0.0217(18) 0.024(2) -0.0075(17) -0.0072(18) -0.0078(16) C36 0.034(2) 0.0161(17) 0.022(2) -0.0020(16) -0.0096(17) -0.0077(15) C37 0.030(2) 0.0202(18) 0.021(2) -0.0062(16) -0.0062(17) -0.0065(16) C38 0.034(2) 0.0242(18) 0.025(2) -0.0077(18) -0.0099(18) -0.0088(17) C39 0.037(2) 0.0248(19) 0.023(2) -0.0087(18) -0.0049(18) -0.0105(17) C40 0.030(2) 0.0224(18) 0.028(2) -0.0120(17) -0.0068(17) -0.0075(16) C41 0.027(2) 0.0221(17) 0.025(2) -0.0074(16) -0.0011(16) -0.0111(15) C42 0.033(2) 0.0241(19) 0.027(2) -0.0115(18) -0.0030(18) -0.0090(16) C43 0.034(2) 0.0254(19) 0.027(2) -0.0151(18) 0.0014(18) -0.0071(17) C44 0.026(2) 0.0232(19) 0.034(2) -0.0102(18) -0.0037(18) -0.0045(17) C45 0.026(2) 0.0260(19) 0.026(2) -0.0114(18) -0.0031(18) -0.0087(16) C46 0.025(2) 0.0195(17) 0.030(2) -0.0121(17) -0.0028(17) -0.0059(15) C47 0.024(2) 0.0185(17) 0.024(2) -0.0075(16) -0.0058(16) 0.0006(15) C48 0.025(2) 0.0214(18) 0.027(2) -0.0104(17) -0.0052(17) -0.0032(16) C49 0.036(2) 0.0137(18) 0.025(2) -0.0050(17) -0.0059(18) -0.0009(16) C50 0.028(2) 0.026(2) 0.022(2) -0.0093(17) -0.0087(17) 0.0039(17) C51 0.028(2) 0.031(2) 0.025(2) -0.0138(18) -0.0062(18) -0.0046(17) C52 0.023(2) 0.0235(19) 0.022(2) -0.0074(17) -0.0044(17) -0.0009(15) _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 C5 1.365(4) . ? N1 C2 1.371(4) . ? C2 C24 1.412(4) . ? C2 C3 1.452(4) . ? C3 C4 1.357(5) . ? C4 C5 1.451(5) . ? C5 C6 1.421(4) . ? C6 C7 1.391(4) . ? C6 C25 1.500(4) . ? C7 N11 1.383(4) . ? C7 C8 1.434(4) . ? C8 C9 1.357(5) . ? C9 C10 1.430(4) . ? C10 N11 1.374(4) . ? C10 C12 1.422(4) . ? C12 C13 1.408(4) . ? C12 C31 1.485(5) . ? C13 N17 1.391(4) . ? C13 C14 1.423(4) . ? C14 C37 1.375(5) . ? C14 C15 1.378(4) . ? C15 C40 1.375(4) . ? C15 C16 1.427(4) . ? C16 N17 1.389(4) . ? C16 C18 1.402(4) . ? C18 C19 1.418(5) . ? C18 C46 1.489(4) . ? C19 N23 1.375(4) . ? C19 C20 1.424(4) . ? C20 C21 1.363(5) . ? C21 C22 1.439(4) . ? C22 N23 1.381(4) . ? C22 C24 1.393(4) . ? C24 C47 1.499(4) . ? C25 C30 1.395(5) . ? C25 C26 1.402(5) . ? C26 C27 1.375(5) . ? C27 C28 1.378(5) . ? C28 C29 1.390(5) . ? C29 C30 1.394(5) . ? C31 C32 1.414(4) . ? C31 C36 1.437(4) . ? C32 C33 1.371(5) . ? C33 C34 1.403(5) . ? C34 C35 1.369(5) . ? C35 C36 1.414(5) . ? C36 C37 1.458(4) . ? C37 C38 1.413(4) . ? C38 C39 1.390(5) . ? C39 C40 1.428(5) . ? C40 C41 1.454(5) . ? C41 C42 1.397(5) . ? C41 C46 1.429(5) . ? C42 C43 1.385(5) . ? C43 C44 1.400(5) . ? C44 C45 1.374(5) . ? C45 C46 1.414(5) . ? C47 C48 1.388(5) . ? C47 C52 1.406(5) . ? C48 C49 1.400(5) . ? C49 C50 1.388(5) . ? C50 C51 1.395(5) . ? C51 C52 1.385(5) . ? 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 C5 N1 C2 105.0(3) . . ? N1 C2 C24 125.9(3) . . ? N1 C2 C3 111.4(3) . . ? C24 C2 C3 122.7(3) . . ? C4 C3 C2 105.8(3) . . ? C3 C4 C5 106.8(3) . . ? N1 C5 C6 126.3(3) . . ? N1 C5 C4 111.0(3) . . ? C6 C5 C4 122.7(3) . . ? C7 C6 C5 126.3(3) . . ? C7 C6 C25 117.0(3) . . ? C5 C6 C25 116.7(3) . . ? N11 C7 C6 126.8(3) . . ? N11 C7 C8 105.8(3) . . ? C6 C7 C8 127.3(3) . . ? C9 C8 C7 108.5(3) . . ? C8 C9 C10 108.6(3) . . ? N11 C10 C12 122.5(3) . . ? N11 C10 C9 106.3(3) . . ? C12 C10 C9 131.0(3) . . ? C10 N11 C7 110.8(3) . . ? C13 C12 C10 120.3(3) . . ? C13 C12 C31 116.3(3) . . ? C10 C12 C31 123.2(3) . . ? N17 C13 C12 131.8(3) . . ? N17 C13 C14 110.9(3) . . ? C12 C13 C14 116.9(3) . . ? C37 C14 C15 123.5(3) . . ? C37 C14 C13 129.7(3) . . ? C15 C14 C13 106.7(3) . . ? C40 C15 C14 123.9(3) . . ? C40 C15 C16 129.2(3) . . ? C14 C15 C16 106.9(3) . . ? N17 C16 C18 132.2(3) . . ? N17 C16 C15 110.6(3) . . ? C18 C16 C15 117.0(3) . . ? C16 N17 C13 104.8(3) . . ? C16 C18 C19 120.6(3) . . ? C16 C18 C46 116.8(3) . . ? C19 C18 C46 122.5(3) . . ? N23 C19 C18 121.7(3) . . ? N23 C19 C20 106.4(3) . . ? C18 C19 C20 131.7(3) . . ? C21 C20 C19 109.1(3) . . ? C20 C21 C22 107.6(3) . . ? N23 C22 C24 126.3(3) . . ? N23 C22 C21 106.3(3) . . ? C24 C22 C21 127.3(3) . . ? C19 N23 C22 110.5(3) . . ? C22 C24 C2 125.9(3) . . ? C22 C24 C47 116.1(3) . . ? C2 C24 C47 118.0(3) . . ? C30 C25 C26 118.8(3) . . ? C30 C25 C6 122.0(3) . . ? C26 C25 C6 119.2(3) . . ? C27 C26 C25 120.5(3) . . ? C26 C27 C28 121.0(4) . . ? C27 C28 C29 119.3(3) . . ? C28 C29 C30 120.6(4) . . ? C29 C30 C25 119.9(3) . . ? C32 C31 C36 116.2(3) . . ? C32 C31 C12 121.1(3) . . ? C36 C31 C12 122.7(3) . . ? C33 C32 C31 123.1(3) . . ? C32 C33 C34 119.6(3) . . ? C35 C34 C33 119.8(3) . . ? C34 C35 C36 121.4(3) . . ? C35 C36 C31 119.6(3) . . ? C35 C36 C37 121.4(3) . . ? C31 C36 C37 119.0(3) . . ? C14 C37 C38 114.4(3) . . ? C14 C37 C36 114.3(3) . . ? C38 C37 C36 131.3(3) . . ? C39 C38 C37 122.3(3) . . ? C38 C39 C40 122.0(3) . . ? C15 C40 C39 113.9(3) . . ? C15 C40 C41 114.8(3) . . ? C39 C40 C41 131.3(3) . . ? C42 C41 C46 119.7(3) . . ? C42 C41 C40 121.1(3) . . ? C46 C41 C40 119.3(3) . . ? C43 C42 C41 122.0(3) . . ? C42 C43 C44 118.8(3) . . ? C45 C44 C43 119.9(3) . . ? C44 C45 C46 122.8(3) . . ? C45 C46 C41 116.3(3) . . ? C45 C46 C18 121.1(3) . . ? C41 C46 C18 122.4(3) . . ? C48 C47 C52 118.9(3) . . ? C48 C47 C24 122.1(3) . . ? C52 C47 C24 118.9(3) . . ? C47 C48 C49 121.4(4) . . ? C50 C49 C48 118.9(3) . . ? C49 C50 C51 120.5(3) . . ? C52 C51 C50 120.3(4) . . ? C51 C52 C47 120.1(3) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.220 _refine_diff_density_min -0.254 _refine_diff_density_rms 0.054