#------------------------------------------------------------------------------ #$Date: 2016-03-20 23:21:50 +0000 (Sun, 20 Mar 2016) $ #$Revision: 178377 $ #$URL: svn://www.crystallography.net/cod/cif/4/00/03/4000393.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4000393 _journal_name_full 'Chemistry of Materials' _journal_paper_doi 10.1021/cm035379d _journal_year 2004 _chemical_formula_sum 'C50 H42 N6 Si' _chemical_formula_weight 754.99 _chemical_name_common j38a _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 81.055(5) _cell_angle_beta 87.709(6) _cell_angle_gamma 75.893(6) _cell_formula_units_Z 2 _cell_length_a 9.804(3) _cell_length_b 10.381(3) _cell_length_c 20.723(6) _cell_measurement_reflns_used ? _cell_measurement_temperature 297(2) _cell_measurement_theta_max ? _cell_measurement_theta_min ? _cell_volume 2020.5(10) _diffrn_ambient_temperature 297(2) _diffrn_detector_area_resol_mean ? _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0602 _diffrn_reflns_av_sigmaI/netI 0.3669 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 14725 _diffrn_reflns_theta_max 28.33 _diffrn_reflns_theta_min 2.05 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _exptl_absorpt_coefficient_mu 0.102 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.856 _exptl_absorpt_correction_type Empirical(SADABS) _exptl_absorpt_process_details ? _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.241 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 796 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.700 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 594 _refine_ls_number_reflns 9317 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.700 _refine_ls_R_factor_all 0.2767 _refine_ls_R_factor_gt 0.0644 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0361P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0964 _refine_ls_wR_factor_ref 0.1289 _reflns_number_gt 2132 _reflns_number_total 9317 _reflns_threshold_expression >2sigma(I) _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_original_sg_symbol_H-M P-1 _cod_database_code 4000393 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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 Si1 Si 0.23398(12) 0.85367(11) 0.12151(6) 0.0541(4) Uani 1 1 d . . . N1 N 0.2808(3) 0.9378(4) -0.21336(16) 0.0589(9) Uani 1 1 d . . . N2 N 0.3439(4) 0.7088(4) -0.18154(17) 0.0753(11) Uani 1 1 d . . . N3 N 0.3957(4) 1.0301(4) -0.3015(2) 0.0940(14) Uani 1 1 d . . . N4 N 0.183(3) 0.8130(17) 0.4623(12) 0.094(7) Uani 0.50 1 d P . . N4A N 0.182(2) 0.752(2) 0.4599(10) 0.105(7) Uani 0.50 1 d P . . N5A N 0.090(2) 0.748(2) 0.5636(11) 0.110(7) Uani 0.50 1 d P . . N5 N 0.083(2) 0.6791(17) 0.5532(12) 0.087(6) Uani 0.50 1 d P . . N6 N 0.2176(14) 0.9765(17) 0.5097(6) 0.139(5) Uiso 0.33 1 d P . . N6B N 0.4003(14) 0.5809(16) 0.4946(6) 0.093(4) Uiso 0.33 1 d P . . N6A N 0.4311(17) 0.6745(17) 0.4875(6) 0.116(5) Uiso 0.33 1 d P . . C1 C 0.0927(3) 0.7629(3) 0.12425(17) 0.0667(12) Uani 1 1 d . . . H1A H 0.0029 0.8252 0.1261 0.100 Uiso 1 1 calc R . . H1B H 0.1043 0.6955 0.1623 0.100 Uiso 1 1 calc R . . H1C H 0.0975 0.7211 0.0858 0.100 Uiso 1 1 calc R . . C2 C 0.4036(3) 0.7284(3) 0.11876(18) 0.0795(13) Uani 1 1 d . . . H2B H 0.4795 0.7723 0.1177 0.119 Uiso 1 1 calc R . . H2C H 0.4072 0.6868 0.0803 0.119 Uiso 1 1 calc R . . H2A H 0.4122 0.6612 0.1568 0.119 Uiso 1 1 calc R . . C3 C 0.2292(3) 0.9998(4) 0.05623(18) 0.0445(10) Uani 1 1 d . . . C4 C 0.2192(4) 0.9610(4) 0.18629(19) 0.0502(11) Uani 1 1 d . . . C5 C 0.2311(3) 1.1065(4) 0.08531(19) 0.0443(10) Uani 1 1 d . . . C6 C 0.2173(3) 1.0879(4) 0.15828(19) 0.0465(10) Uani 1 1 d . . . C7 C 0.2451(4) 1.2395(4) 0.05037(17) 0.0424(10) Uani 1 1 d . . . C8 C 0.1521(4) 1.3114(4) 0.00123(19) 0.0611(12) Uani 1 1 d . . . H8A H 0.0795 1.2756 -0.0097 0.073 Uiso 1 1 calc R . . C9 C 0.1642(5) 1.4339(5) -0.0317(2) 0.0812(15) Uani 1 1 d . . . H9A H 0.1013 1.4792 -0.0649 0.097 Uiso 1 1 calc R . . C10 C 0.2688(5) 1.4885(5) -0.0154(2) 0.0875(16) Uani 1 1 d . . . H10A H 0.2777 1.5715 -0.0371 0.105 Uiso 1 1 calc R . . C11 C 0.3614(5) 1.4191(5) 0.0336(2) 0.0745(14) Uani 1 1 d . . . H11A H 0.4323 1.4566 0.0451 0.089 Uiso 1 1 calc R . . C12 C 0.3511(4) 1.2961(4) 0.06557(18) 0.0568(11) Uani 1 1 d . . . H12A H 0.4159 1.2504 0.0978 0.068 Uiso 1 1 calc R . . C13 C 0.2038(4) 1.2051(4) 0.19197(18) 0.0472(11) Uani 1 1 d . . . C14 C 0.0872(4) 1.3109(4) 0.18381(17) 0.0569(12) Uani 1 1 d . . . H14A H 0.0157 1.3075 0.1565 0.068 Uiso 1 1 calc R . . C15 C 0.0726(5) 1.4219(4) 0.2147(2) 0.0713(13) Uani 1 1 d . . . H15A H -0.0086 1.4909 0.2090 0.086 Uiso 1 1 calc R . . C16 C 0.1788(6) 1.4295(5) 0.2541(2) 0.0814(15) Uani 1 1 d . . . H16A H 0.1716 1.5045 0.2746 0.098 Uiso 1 1 calc R . . C17 C 0.2952(5) 1.3251(6) 0.2625(2) 0.0780(15) Uani 1 1 d . . . H17A H 0.3677 1.3300 0.2889 0.094 Uiso 1 1 calc R . . C18 C 0.3083(4) 1.2128(4) 0.23296(19) 0.0674(13) Uani 1 1 d . . . H18A H 0.3877 1.1420 0.2406 0.081 Uiso 1 1 calc R . . C19 C 0.2442(4) 0.9891(4) -0.01424(18) 0.0431(10) Uani 1 1 d . . . C20 C 0.1620(4) 0.9201(4) -0.0422(2) 0.0542(11) Uani 1 1 d . . . H20A H 0.0980 0.8829 -0.0159 0.065 Uiso 1 1 calc R . . C21 C 0.1716(4) 0.9049(4) -0.1066(2) 0.0575(12) Uani 1 1 d . . . H21A H 0.1132 0.8600 -0.1235 0.069 Uiso 1 1 calc R . . C22 C 0.2675(4) 0.9559(4) -0.1467(2) 0.0520(11) Uani 1 1 d . . . C23 C 0.3525(4) 1.0216(4) -0.1204(2) 0.0587(12) Uani 1 1 d . . . H23A H 0.4193 1.0547 -0.1466 0.070 Uiso 1 1 calc R . . C24 C 0.3400(4) 1.0392(4) -0.0558(2) 0.0584(12) Uani 1 1 d . . . H24A H 0.3973 1.0860 -0.0394 0.070 Uiso 1 1 calc R . . C25 C 0.2906(5) 1.0483(5) -0.2599(2) 0.0607(12) Uani 1 1 d . . . C26 C 0.1952(5) 1.1678(5) -0.2604(2) 0.0882(16) Uani 1 1 d . . . H26A H 0.1210 1.1759 -0.2308 0.106 Uiso 1 1 calc R . . C27 C 0.2086(6) 1.2755(5) -0.3043(3) 0.1092(19) Uani 1 1 d . . . H27A H 0.1440 1.3578 -0.3052 0.131 Uiso 1 1 calc R . . C28 C 0.3162(8) 1.2611(6) -0.3462(3) 0.119(2) Uani 1 1 d . . . H28A H 0.3299 1.3339 -0.3758 0.143 Uiso 1 1 calc R . . C29 C 0.4059(6) 1.1372(8) -0.3446(3) 0.132(2) Uani 1 1 d . . . H29A H 0.4781 1.1269 -0.3753 0.158 Uiso 1 1 calc R . . C30 C 0.3007(4) 0.8089(5) -0.2295(2) 0.0570(12) Uani 1 1 d . . . C31 C 0.2754(4) 0.7886(5) -0.2915(2) 0.0725(14) Uani 1 1 d . . . H31A H 0.2449 0.8611 -0.3243 0.087 Uiso 1 1 calc R . . C32 C 0.2962(5) 0.6587(6) -0.3039(2) 0.0866(16) Uani 1 1 d . . . H32A H 0.2797 0.6419 -0.3453 0.104 Uiso 1 1 calc R . . C33 C 0.3419(5) 0.5538(5) -0.2542(3) 0.0953(17) Uani 1 1 d . . . H33A H 0.3595 0.4648 -0.2610 0.114 Uiso 1 1 calc R . . C34 C 0.3597(5) 0.5863(6) -0.1953(3) 0.0946(16) Uani 1 1 d . . . H34A H 0.3857 0.5157 -0.1611 0.114 Uiso 1 1 calc R . . C35 C 0.2035(5) 0.9172(5) 0.2568(2) 0.0606(12) Uani 1 1 d . . . C36 C 0.2745(5) 0.7931(5) 0.2853(2) 0.0878(16) Uani 1 1 d . . . H36A H 0.3314 0.7357 0.2595 0.105 Uiso 1 1 calc R . . C37 C 0.2644(6) 0.7495(5) 0.3520(3) 0.0924(17) Uani 1 1 d . . . H37A H 0.3164 0.6649 0.3700 0.111 Uiso 1 1 calc R . . C38 C 0.1804(6) 0.8279(7) 0.3907(3) 0.099(2) Uani 1 1 d . . . C39 C 0.1027(6) 0.9491(7) 0.3622(3) 0.151(3) Uani 1 1 d . . . H39A H 0.0413 1.0044 0.3874 0.181 Uiso 1 1 calc R . . C40 C 0.1144(5) 0.9902(6) 0.2963(3) 0.1142(19) Uani 1 1 d . . . H40A H 0.0581 1.0725 0.2780 0.137 Uiso 1 1 calc R . . C41A C 0.0800(11) 0.7051(12) 0.4876(6) 0.046(3) Uani 0.50 1 d P . . C41 C 0.0758(19) 0.7946(18) 0.4991(10) 0.116(6) Uani 0.50 1 d P . . C42 C 0.025(2) 0.633(2) 0.4434(9) 0.090(6) Uani 0.33 1 d P . . C42A C -0.0619(15) 0.8335(16) 0.4711(6) 0.073(5) Uani 0.33 1 d P . . C42B C -0.031(2) 0.695(2) 0.4562(11) 0.079(7) Uiso 0.33 1 d P . . C43 C -0.0242(15) 0.745(2) 0.6045(7) 0.156(6) Uani 0.50 1 d P . . C43A C 0.0044(16) 0.6121(15) 0.5855(8) 0.112(6) Uani 0.50 1 d P . . C44A C -0.1695(17) 0.8272(19) 0.5117(9) 0.099(5) Uani 0.33 1 d P . . C44B C -0.143(2) 0.654(4) 0.4979(9) 0.178(14) Uani 0.33 1 d P . . C44 C -0.032(3) 0.534(3) 0.4726(13) 0.109(8) Uani 0.33 1 d P . . C45A C -0.152(3) 0.714(4) 0.5749(14) 0.138(11) Uiso 0.25 1 d P . . C45C C -0.051(3) 0.526(3) 0.5472(12) 0.081(9) Uiso 0.25 1 d P . . C45B C -0.128(3) 0.620(3) 0.5629(12) 0.096(8) Uiso 0.25 1 d P . . C45 C -0.161(2) 0.812(2) 0.5817(10) 0.083(7) Uiso 0.25 1 d P . . C46A C 0.3382(18) 0.765(2) 0.5021(7) 0.032(4) Uiso 0.33 1 d P . . C46 C 0.2551(17) 0.8478(17) 0.4920(7) 0.057(4) Uiso 0.33 1 d P . . C46B C 0.3303(16) 0.6980(19) 0.4950(6) 0.047(4) Uiso 0.33 1 d P . . C47 C 0.3700(14) 0.7897(14) 0.5132(6) 0.102(5) Uiso 0.67 1 d P . . C47A C 0.3506(17) 0.866(2) 0.5399(8) 0.087(5) Uiso 0.33 1 d P . . C48A C 0.493(2) 0.848(3) 0.5719(9) 0.119(8) Uiso 0.33 1 d P . . C48 C 0.5785(19) 0.717(2) 0.5620(8) 0.110(6) Uiso 0.33 1 d P . . C48B C 0.4785(13) 0.7847(11) 0.5529(5) 0.104(3) Uiso 0.67 1 d P . . C49B C 0.5367(16) 0.546(2) 0.5235(7) 0.106(5) Uiso 0.33 1 d P . . C49A C 0.437(2) 0.9239(19) 0.5569(8) 0.096(6) Uiso 0.33 1 d P . . C50B C 0.5663(11) 0.6456(13) 0.5408(5) 0.154(4) Uiso 0.67 1 d P . . C50 C 0.3163(18) 1.0147(17) 0.5435(7) 0.112(5) Uiso 0.33 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 Si1 0.0642(8) 0.0460(8) 0.0514(8) -0.0006(7) -0.0029(6) -0.0156(7) N1 0.084(3) 0.055(3) 0.040(3) -0.014(2) 0.001(2) -0.018(2) N2 0.096(3) 0.053(3) 0.067(3) -0.013(3) -0.013(2) 0.004(2) N3 0.085(3) 0.087(4) 0.100(4) 0.015(3) 0.029(3) -0.024(3) N4 0.140(14) 0.077(10) 0.076(11) -0.006(7) 0.072(9) -0.061(8) N4A 0.109(12) 0.20(2) 0.030(7) 0.005(12) -0.006(7) -0.086(16) N5A 0.079(9) 0.161(18) 0.072(14) 0.062(13) -0.008(9) -0.045(13) N5 0.098(11) 0.086(12) 0.071(11) 0.001(11) 0.000(7) -0.020(9) C1 0.074(3) 0.062(3) 0.063(3) 0.010(2) -0.008(2) -0.025(2) C2 0.076(3) 0.070(3) 0.091(4) -0.010(3) 0.000(3) -0.015(3) C3 0.049(3) 0.048(3) 0.039(3) -0.002(2) -0.001(2) -0.019(2) C4 0.063(3) 0.044(3) 0.042(3) 0.005(2) -0.008(2) -0.017(2) C5 0.038(2) 0.051(3) 0.044(3) -0.001(2) -0.004(2) -0.013(2) C6 0.049(3) 0.049(3) 0.043(3) -0.006(2) -0.006(2) -0.014(2) C7 0.052(3) 0.043(3) 0.034(3) -0.005(2) 0.000(2) -0.014(2) C8 0.062(3) 0.061(3) 0.060(3) 0.003(3) -0.009(2) -0.019(2) C9 0.100(4) 0.062(4) 0.071(4) 0.020(3) -0.011(3) -0.016(3) C10 0.125(5) 0.057(4) 0.077(4) 0.005(3) 0.019(3) -0.028(3) C11 0.096(4) 0.068(4) 0.076(4) -0.014(3) 0.027(3) -0.053(3) C12 0.069(3) 0.060(3) 0.049(3) -0.009(2) 0.004(2) -0.028(2) C13 0.052(3) 0.050(3) 0.039(3) -0.005(2) 0.002(2) -0.013(3) C14 0.070(3) 0.055(3) 0.047(3) -0.010(3) -0.011(2) -0.014(3) C15 0.088(4) 0.059(3) 0.069(4) -0.014(3) 0.017(3) -0.021(3) C16 0.108(4) 0.075(4) 0.069(4) -0.024(3) 0.013(3) -0.031(4) C17 0.085(4) 0.108(5) 0.054(3) -0.015(3) -0.010(3) -0.044(3) C18 0.069(3) 0.080(4) 0.058(3) -0.029(3) -0.006(3) -0.015(3) C19 0.043(2) 0.047(3) 0.039(3) -0.006(2) 0.000(2) -0.013(2) C20 0.056(3) 0.059(3) 0.057(3) -0.014(2) 0.004(2) -0.028(2) C21 0.064(3) 0.063(3) 0.055(3) -0.020(3) -0.001(3) -0.026(2) C22 0.059(3) 0.054(3) 0.044(3) -0.012(2) -0.004(2) -0.013(2) C23 0.065(3) 0.068(3) 0.049(3) -0.009(3) 0.009(2) -0.030(2) C24 0.058(3) 0.072(3) 0.055(3) -0.018(3) -0.003(2) -0.028(2) C25 0.071(4) 0.060(4) 0.046(3) 0.003(3) -0.001(3) -0.014(3) C26 0.108(4) 0.071(4) 0.067(4) 0.011(3) 0.013(3) -0.001(4) C27 0.134(5) 0.077(5) 0.096(5) 0.013(4) 0.007(4) -0.004(4) C28 0.161(7) 0.085(5) 0.111(5) 0.021(5) 0.015(5) -0.052(5) C29 0.120(5) 0.126(6) 0.143(6) 0.004(5) 0.053(4) -0.039(5) C30 0.066(3) 0.065(4) 0.040(3) -0.012(3) -0.004(2) -0.013(3) C31 0.093(3) 0.083(4) 0.049(3) -0.017(3) -0.002(3) -0.030(3) C32 0.103(4) 0.112(5) 0.061(4) -0.039(4) 0.003(3) -0.041(4) C33 0.134(5) 0.068(4) 0.094(5) -0.037(4) 0.018(4) -0.032(4) C34 0.133(4) 0.067(4) 0.067(4) -0.008(3) 0.005(3) 0.006(3) C35 0.064(3) 0.068(4) 0.050(3) 0.000(3) 0.005(3) -0.022(3) C36 0.149(5) 0.071(4) 0.037(3) -0.001(3) 0.001(3) -0.019(3) C37 0.123(5) 0.095(4) 0.060(4) 0.012(4) -0.019(4) -0.039(4) C38 0.103(5) 0.141(7) 0.059(5) -0.006(4) 0.031(4) -0.052(5) C39 0.147(6) 0.175(7) 0.084(5) 0.006(5) 0.057(4) 0.023(5) C40 0.102(4) 0.147(6) 0.065(4) 0.016(4) 0.029(3) 0.002(4) C41A 0.049(7) 0.045(7) 0.039(8) 0.017(6) -0.004(5) -0.015(6) C41 0.127(15) 0.105(13) 0.109(17) 0.021(13) 0.002(12) -0.040(12) C42 0.079(14) 0.075(15) 0.131(17) -0.048(14) -0.015(11) -0.027(13) C42A 0.033(8) 0.113(15) 0.051(9) 0.017(9) 0.007(8) 0.001(9) C43 0.068(10) 0.27(2) 0.129(13) -0.016(14) 0.013(9) -0.051(13) C43A 0.098(10) 0.145(15) 0.090(11) 0.062(11) -0.020(8) -0.072(12) C44A 0.089(12) 0.125(17) 0.085(14) 0.011(12) 0.001(10) -0.043(12) C44B 0.15(2) 0.37(4) 0.043(13) 0.07(2) -0.047(13) -0.17(3) C44 0.10(2) 0.074(17) 0.15(2) 0.029(15) -0.004(15) -0.037(17)