#------------------------------------------------------------------------------ #$Date: 2009-11-14 13:09:05 +0000 (Sat, 14 Nov 2009) $ #$Revision: 846 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003287.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_2003287 _journal_name_full 'Acta Crystallographica C' _journal_volume 51 _journal_year 1995 _journal_page_first 543 _journal_page_last 544 _publ_section_title ; 1-[4-(N,N-Dimethylamino)phenyl]-3-(1-pyrenyl)hexamethyltrisilane ; _chemical_formula_sum 'C30 H37 N Si3' _chemical_formula_weight 495.88 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' _symmetry_space_group_name_H-M 'P 21/n' _cell_length_a 7.8980(10) _cell_length_b 26.463(4) _cell_length_c 14.099(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.69(2) _cell_angle_gamma 90.00 _cell_volume 2904.7(7) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.134 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 23 _exptl_absorpt_coefficient_mu 1.626 _cell_measurement_temperature 289(2) _exptl_crystal_description blocks _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_colour yellow _chemical_compound_source ? _diffrn_measurement_device 'Siemens P4/PC' _diffrn_measurement_method '\q-2\q scans' _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.479 _exptl_absorpt_correction_T_max 0.991 _diffrn_reflns_number 4081 _reflns_number_total 3030 _reflns_number_observed 1827 _reflns_observed_criterion >2sigma(I) _diffrn_reflns_av_R_equivalents 0.0520 _diffrn_reflns_theta_max 50.41 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.0640 _refine_ls_wR_factor_obs 0.1480 _refine_ls_wR_factor_all 0.1746 _refine_ls_goodness_of_fit_obs 1.191 _refine_ls_goodness_of_fit_all 1.058 _refine_ls_number_reflns 3030 _refine_ls_number_parameters 308 _refine_ls_hydrogen_treatment ? _refine_ls_weighting_scheme ; w = 1/[\s^2^(F~o~^2^) + (0.0748P)^2^ + 0.5736P] where P = (F~o~^2^ + 2F~c~^2^)/3 ; _refine_ls_shift/esd_max 0.063 _refine_diff_density_max 0.308 _refine_diff_density_min -0.204 _refine_ls_extinction_method 'F~c~^*^ = kF~c~[1 + 0.001xF~c~^2^\l^3^/sin(2\q)' _refine_ls_extinction_coef 0.00023(11) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag 'C' 'C' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0181 0.009 'H' 'H' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0000 0.000 'N' 'N' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0311 0.018 'Si' 'Si' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.2541 0.3 _computing_data_collection ; P3/PC Data Collection Program (Siemens, 1989) ; loop_ _atom_site_label _atom_site_occupancy _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv Si1 1 0.0343(2) 0.28680(5) 0.93410(9) 0.0625(4) Si2 1 -0.0069(2) 0.34352(5) 0.80437(8) 0.0564(4) Si3 1 -0.2972(2) 0.35587(5) 0.74315(8) 0.0555(4) C1 1 -0.0999(5) 0.2287(2) 0.9023(3) 0.0559(14) C2 1 -0.2453(6) 0.2204(2) 0.9452(3) 0.068(2) H2A 1 -0.2659(6) 0.2421(2) 0.9938(3) 0.082 C3 1 -0.3594(6) 0.1813(2) 0.9185(3) 0.075(2) H3A 1 -0.4520(6) 0.1769(2) 0.9507(3) 0.091 C4 1 -0.4560(6) 0.1079(2) 0.8128(3) 0.081(2) H4A 1 -0.5515(6) 0.1032(2) 0.8424(3) 0.097 C5 1 -0.4322(7) 0.0767(2) 0.7416(4) 0.095(2) H5A 1 -0.5117(7) 0.0513(2) 0.7220(4) 0.113 C6 1 -0.2623(8) 0.0488(2) 0.6205(4) 0.109(2) H6A 1 -0.3422(8) 0.0235(2) 0.6002(4) 0.131 C7 1 -0.1176(9) 0.0546(2) 0.5780(4) 0.118(3) H7A 1 -0.0993(9) 0.0322(2) 0.5299(4) 0.141 C8 1 -0.0009(8) 0.0924(2) 0.6047(3) 0.108(2) H8A 1 0.0932(8) 0.0958(2) 0.5734(3) 0.130 C9 1 0.0953(7) 0.1652(2) 0.7097(3) 0.088(2) H9A 1 0.1918(7) 0.1688(2) 0.6806(3) 0.106 C10 1 0.0722(6) 0.1976(2) 0.7804(3) 0.071(2) H10A 1 0.1538(6) 0.2227(2) 0.7987(3) 0.086 C11 1 -0.3391(6) 0.1487(2) 0.8455(3) 0.0670(15) C12 1 -0.2852(7) 0.0822(2) 0.6954(3) 0.085(2) C13 1 -0.0218(7) 0.1261(2) 0.6787(3) 0.077(2) C14 1 -0.0742(6) 0.1947(2) 0.8282(3) 0.0579(14) C15 1 -0.1925(6) 0.1547(2) 0.8006(3) 0.0598(14) C16 1 -0.1660(7) 0.1210(2) 0.7251(3) 0.068(2) C17 1 -0.0438(7) 0.3195(2) 1.0367(3) 0.085(2) H17A 1 -0.1634(7) 0.3276(2) 1.0186(3) 0.102 H17B 1 0.0206(7) 0.3500(2) 1.0523(3) 0.102 H17C 1 -0.0287(7) 0.2976(2) 1.0918(3) 0.102 C18 1 0.2670(6) 0.2726(2) 0.9758(3) 0.092(2) H18A 1 0.3129(6) 0.2558(2) 0.9254(3) 0.110 H18B 1 0.2792(6) 0.2512(2) 1.0315(3) 0.110 H18C 1 0.3283(6) 0.3036(2) 0.9919(3) 0.110 C19 1 0.0880(6) 0.4057(2) 0.8513(3) 0.082(2) H19A 1 0.0356(6) 0.4164(2) 0.9046(3) 0.099 H19B 1 0.0673(6) 0.4306(2) 0.8011(3) 0.099 H19C 1 0.2095(6) 0.4019(2) 0.8720(3) 0.099 C20 1 0.0965(6) 0.3229(2) 0.6996(3) 0.080(2) H20A 1 0.0485(6) 0.2911(2) 0.6755(3) 0.095 H20B 1 0.2180(6) 0.3191(2) 0.7204(3) 0.095 H20C 1 0.0758(6) 0.3478(2) 0.6496(3) 0.095 C21 1 -0.4093(6) 0.3860(2) 0.8354(3) 0.089(2) H21A 1 -0.4070(6) 0.3635(2) 0.8889(3) 0.107 H21B 1 -0.5263(6) 0.3931(2) 0.8074(3) 0.107 H21C 1 -0.3521(6) 0.4170(2) 0.8571(3) 0.107 C22 1 -0.4021(6) 0.2945(2) 0.7023(3) 0.080(2) H22A 1 -0.3988(6) 0.2724(2) 0.7566(3) 0.096 H22B 1 -0.3421(6) 0.2792(2) 0.6560(3) 0.096 H22C 1 -0.5194(6) 0.3005(2) 0.6735(3) 0.096 C23 1 -0.3017(5) 0.3996(2) 0.6394(3) 0.0522(13) C24 1 -0.3470(6) 0.3851(2) 0.5431(3) 0.0595(14) H24A 1 -0.3833(6) 0.3520(2) 0.5299(3) 0.071 C25 1 -0.3410(6) 0.4167(2) 0.4674(3) 0.0591(14) H25A 1 -0.3717(6) 0.4045(2) 0.4050(3) 0.071 C26 1 -0.2900(6) 0.4667(2) 0.4812(3) 0.0585(14) C27 1 -0.2447(6) 0.4822(2) 0.5768(3) 0.072(2) H27A 1 -0.2087(6) 0.5153(2) 0.5902(3) 0.086 C28 1 -0.2524(6) 0.4498(2) 0.6502(3) 0.071(2) H28A 1 -0.2224(6) 0.4621(2) 0.7126(3) 0.085 N1 1 -0.2763(5) 0.49944(14) 0.4074(3) 0.0767(14) C29 1 -0.2279(7) 0.5517(2) 0.4269(3) 0.089(2) H29A 1 -0.2246(7) 0.5690(2) 0.3674(3) 0.107 H29B 1 -0.1165(7) 0.5531(2) 0.4665(3) 0.107 H29C 1 -0.3106(7) 0.5677(2) 0.4598(3) 0.107 C30 1 -0.3514(7) 0.4865(2) 0.3104(3) 0.086(2) H30A 1 -0.3305(7) 0.5132(2) 0.2678(3) 0.104 H30B 1 -0.4730(7) 0.4819(2) 0.3065(3) 0.104 H30C 1 -0.3010(7) 0.4558(2) 0.2922(3) 0.104 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 Si1 0.0621(9) 0.0118(8) 0.0087(7) 0.0694(8) 0.0065(7) 0.0557(7) Si2 0.0525(8) 0.0023(7) 0.0098(6) 0.0599(8) 0.0064(7) 0.0569(7) Si3 0.0510(8) 0.0039(7) 0.0102(6) 0.0602(8) 0.0047(7) 0.0559(7) C1 0.056(3) 0.021(2) 0.015(2) 0.064(3) 0.014(2) 0.050(2) C2 0.066(3) 0.016(3) 0.021(3) 0.075(3) 0.008(3) 0.067(3) C3 0.062(3) 0.018(3) 0.037(3) 0.092(4) 0.019(3) 0.081(3) C4 0.062(3) -0.006(3) 0.012(3) 0.065(3) 0.024(3) 0.114(4) C5 0.104(4) 0.002(3) -0.019(4) 0.056(3) 0.003(3) 0.110(4) C6 0.160(6) 0.017(4) -0.016(4) 0.070(4) -0.007(3) 0.085(4) C7 0.186(7) 0.047(5) 0.015(4) 0.089(4) -0.002(3) 0.077(4) C8 0.169(6) 0.030(4) 0.038(4) 0.087(4) 0.006(3) 0.075(4) C9 0.110(4) 0.020(3) 0.060(3) 0.082(4) 0.021(3) 0.087(3) C10 0.074(3) 0.017(3) 0.036(3) 0.070(3) 0.011(3) 0.078(3) C11 0.064(3) 0.012(3) 0.019(3) 0.067(3) 0.018(3) 0.072(3) C12 0.102(4) 0.020(3) 0.002(3) 0.080(4) 0.014(3) 0.070(3) C13 0.115(4) 0.021(3) 0.023(3) 0.066(3) 0.008(3) 0.055(3) C14 0.068(3) 0.013(2) 0.013(2) 0.051(3) 0.017(2) 0.056(3) C15 0.075(3) 0.027(3) 0.019(2) 0.051(3) 0.017(2) 0.056(3) C16 0.083(4) 0.015(3) 0.003(3) 0.057(3) 0.018(3) 0.060(3) C17 0.107(4) 0.021(3) 0.021(3) 0.087(4) 0.000(3) 0.062(3) C18 0.076(4) 0.013(3) 0.005(3) 0.106(4) 0.018(3) 0.090(4) C19 0.077(4) -0.014(3) 0.010(3) 0.078(3) -0.007(3) 0.091(3) C20 0.084(4) 0.013(3) 0.036(3) 0.085(4) 0.015(3) 0.076(3) C21 0.079(4) 0.027(3) 0.025(3) 0.115(4) 0.007(3) 0.078(3) C22 0.073(4) -0.012(3) 0.002(3) 0.086(4) 0.012(3) 0.079(3) C23 0.049(3) 0.004(2) 0.000(2) 0.055(3) -0.002(2) 0.050(2) C24 0.073(3) -0.009(3) 0.005(3) 0.047(3) -0.003(2) 0.057(3) C25 0.072(3) -0.005(3) -0.001(2) 0.053(3) -0.002(2) 0.048(3) C26 0.057(3) 0.001(3) -0.002(2) 0.057(3) 0.007(2) 0.057(3) C27 0.097(4) -0.012(3) 0.000(3) 0.044(3) 0.003(2) 0.070(3) C28 0.093(4) 0.004(3) 0.000(3) 0.062(3) -0.008(3) 0.054(3) N1 0.094(3) -0.015(2) 0.000(2) 0.065(3) 0.016(2) 0.066(2) C29 0.109(4) -0.005(3) 0.020(3) 0.066(3) 0.024(3) 0.094(4) C30 0.103(4) 0.007(3) 0.015(3) 0.090(4) 0.016(3) 0.067(3)