#------------------------------------------------------------------------------ #$Date: 2016-02-16 20:30:59 +0000 (Tue, 16 Feb 2016) $ #$Revision: 176467 $ #$URL: svn://www.crystallography.net/cod/cif/4/00/02/4000295.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_4000295 _journal_name_full 'Chemistry of Materials' _journal_paper_doi 10.1021/cm0340532 _journal_year 2003 _chemical_formula_sum 'C20 H20.6 N2 O6.3' _chemical_formula_weight 389.78 _space_group_IT_number 33 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'P 2c -2n' _symmetry_space_group_name_H-M 'P n a 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 6.5798(10) _cell_length_b 16.699(2) _cell_length_c 17.630(3) _cell_measurement_reflns_used 2422 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 24.68 _cell_measurement_theta_min 2.31 _cell_volume 1937.2(5) _diffrn_ambient_temperature 100(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 0.0646 _diffrn_reflns_av_sigmaI/netI 0.0792 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 8922 _diffrn_reflns_theta_max 24.77 _diffrn_reflns_theta_min 1.68 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _exptl_absorpt_coefficient_mu 0.101 _exptl_absorpt_correction_T_max 0.9960 _exptl_absorpt_correction_T_min 0.9821 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Sadabs (Bruker)' _exptl_crystal_colour light _exptl_crystal_density_diffrn 1.336 _exptl_crystal_density_meas 0 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 820 _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.5(17) _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 267 _refine_ls_number_reflns 3040 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.051 _refine_ls_R_factor_all 0.0982 _refine_ls_R_factor_gt 0.0468 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0476P)^2^+0.2790P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0945 _refine_ls_wR_factor_ref 0.1159 _reflns_number_gt 2052 _reflns_number_total 3040 _reflns_threshold_expression >2sigma(I) _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' 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 Pna2(1) _cod_original_formula_sum 'C20 H20.60 N2 O6.30' _cod_database_code 4000295 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' 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 0.8992(5) 0.31917(19) 0.38213(18) 0.0190(8) Uani 1 1 d . . . N2 N 0.8815(5) 0.3050(2) 0.45682(19) 0.0198(7) Uani 1 1 d . . . O1 O 0.9527(4) 0.19198(15) 0.17877(16) 0.0262(7) Uani 1 1 d . . . O2 O 0.9560(5) 0.31261(16) 0.12224(16) 0.0281(7) Uani 1 1 d . . . O3 O 1.1291(5) 0.46976(15) 0.19907(16) 0.0314(7) Uani 1 1 d . . . O4 O 0.7891(5) 0.48427(15) 0.18983(17) 0.0308(7) Uani 1 1 d . . . O5 O 0.9432(4) 0.53103(14) 0.35010(15) 0.0252(7) Uani 1 1 d . . . O6 O 0.8379(4) 0.47376(16) 0.46042(16) 0.0294(7) Uani 1 1 d . . . C1 C 0.8745(6) 0.2270(2) 0.4753(2) 0.0204(10) Uani 1 1 d . . . C2 C 0.8542(7) 0.2102(3) 0.5549(3) 0.0303(11) Uani 1 1 d . . . H2 H 0.8511 0.2522 0.5912 0.036 Uiso 1 1 calc R . . C3 C 0.8396(7) 0.1323(3) 0.5769(3) 0.0320(12) Uani 1 1 d . . . H3 H 0.8269 0.1202 0.6293 0.038 Uiso 1 1 calc R . . C4 C 0.8428(7) 0.0686(3) 0.5234(3) 0.0335(12) Uani 1 1 d . . . H4 H 0.8277 0.0152 0.5410 0.040 Uiso 1 1 calc R . . C5 C 0.8664(6) 0.0816(2) 0.4489(3) 0.0291(11) Uani 1 1 d . . . H5 H 0.8721 0.0379 0.4144 0.035 Uiso 1 1 calc R . . C6 C 0.8833(6) 0.1632(2) 0.4216(3) 0.0223(10) Uani 1 1 d . . . C7 C 0.9060(6) 0.1814(2) 0.3457(3) 0.0233(10) Uani 1 1 d . . . H7 H 0.9158 0.1401 0.3088 0.028 Uiso 1 1 calc R . . C8 C 0.9142(6) 0.2618(2) 0.3243(2) 0.0195(9) Uani 1 1 d . . . C9 C 0.9328(6) 0.3039(2) 0.2553(2) 0.0190(9) Uani 1 1 d . . . C10 C 0.9499(6) 0.2724(2) 0.1790(3) 0.0217(9) Uani 1 1 d . . . C11 C 0.9598(7) 0.1540(2) 0.1040(2) 0.0299(11) Uani 1 1 d . . . H11A H 1.0737 0.1761 0.0749 0.045 Uiso 1 1 calc R . . H11B H 0.8323 0.1644 0.0770 0.045 Uiso 1 1 calc R . . H11C H 0.9782 0.0961 0.1101 0.045 Uiso 1 1 calc R . . C12 C 0.9299(6) 0.3857(2) 0.2728(2) 0.0203(10) Uani 1 1 d . . . C13 C 0.9362(7) 0.4515(2) 0.2159(2) 0.0223(10) Uani 1 1 d . . . C14 C 1.1533(9) 0.5307(3) 0.1401(3) 0.0474(15) Uani 1 1 d . . . H14A H 1.0835 0.5799 0.1555 0.071 Uiso 1 1 calc R . . H14B H 1.0945 0.5111 0.0925 0.071 Uiso 1 1 calc R . . H14C H 1.2982 0.5419 0.1326 0.071 Uiso 1 1 calc R . . C15 C 0.9074(6) 0.3957(2) 0.3508(2) 0.0197(10) Uani 1 1 d . . . C16 C 0.8920(6) 0.4694(2) 0.3953(2) 0.0229(10) Uani 1 1 d . . . C17 C 0.9163(8) 0.6147(2) 0.3777(3) 0.0358(12) Uani 1 1 d . . . C18 C 0.9748(9) 0.6626(2) 0.3074(3) 0.0513(15) Uani 1 1 d . . . H18A H 0.8786 0.6511 0.2664 0.077 Uiso 1 1 calc R . . H18B H 1.1123 0.6477 0.2914 0.077 Uiso 1 1 calc R . . H18C H 0.9711 0.7199 0.3192 0.077 Uiso 1 1 calc R . . C19 C 1.0622(9) 0.6302(3) 0.4427(3) 0.0567(17) Uani 1 1 d . . . H19A H 1.2008 0.6170 0.4267 0.085 Uiso 1 1 calc R . . H19B H 1.0243 0.5968 0.4862 0.085 Uiso 1 1 calc R . . H19C H 1.0555 0.6868 0.4572 0.085 Uiso 1 1 calc R . . C20 C 0.6950(9) 0.6279(3) 0.3982(3) 0.0573(17) Uani 1 1 d . . . H20A H 0.6601 0.5950 0.4424 0.086 Uiso 1 1 calc R . . H20B H 0.6089 0.6126 0.3552 0.086 Uiso 1 1 calc R . . H20C H 0.6731 0.6845 0.4102 0.086 Uiso 1 1 calc R . . O1W O 0.448(2) 0.5163(8) 0.2881(7) 0.061(4) Uani 0.30 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 N1 0.019(2) 0.023(2) 0.0150(19) 0.0021(15) 0.0000(15) 0.0011(15) N2 0.0178(19) 0.0235(18) 0.0180(19) 0.0070(16) -0.0003(15) -0.0019(15) O1 0.0360(17) 0.0214(15) 0.0211(16) -0.0050(13) 0.0003(14) 0.0009(14) O2 0.0394(19) 0.0242(16) 0.0206(18) -0.0003(15) 0.0022(14) -0.0019(14) O3 0.0420(19) 0.0209(15) 0.0313(18) 0.0058(14) 0.0115(14) -0.0098(13) O4 0.044(2) 0.0243(15) 0.0244(17) 0.0062(14) -0.0052(15) 0.0036(14) O5 0.0401(19) 0.0130(13) 0.0226(16) -0.0023(12) 0.0023(14) -0.0017(13) O6 0.0401(19) 0.0288(16) 0.0194(18) -0.0012(14) 0.0033(15) 0.0027(14) C1 0.011(2) 0.027(2) 0.024(3) 0.0070(19) -0.0017(18) 0.0014(18) C2 0.028(3) 0.037(3) 0.026(3) 0.009(2) -0.001(2) 0.002(2) C3 0.033(3) 0.034(3) 0.029(3) 0.011(2) 0.001(2) 0.001(2) C4 0.034(3) 0.025(2) 0.042(3) 0.018(2) -0.006(2) 0.001(2) C5 0.026(3) 0.018(2) 0.043(3) 0.009(2) 0.000(2) 0.0008(19) C6 0.019(2) 0.021(2) 0.028(3) 0.011(2) -0.0019(19) -0.0007(18) C7 0.014(2) 0.019(2) 0.038(3) 0.003(2) -0.0030(19) 0.0009(18) C8 0.014(2) 0.016(2) 0.028(2) 0.0034(19) -0.0034(18) 0.0008(17) C9 0.017(2) 0.020(2) 0.019(2) 0.003(2) -0.0008(17) -0.0002(18) C10 0.017(2) 0.021(2) 0.027(2) -0.002(2) 0.0000(19) 0.0009(19) C11 0.038(3) 0.032(3) 0.019(3) -0.011(2) 0.003(2) 0.001(2) C12 0.015(2) 0.020(2) 0.026(3) 0.0002(18) -0.0018(18) -0.0015(18) C13 0.030(3) 0.019(2) 0.018(2) -0.0033(17) 0.001(2) -0.003(2) C14 0.076(4) 0.025(3) 0.042(3) 0.011(2) 0.033(3) -0.009(3) C15 0.024(3) 0.0130(19) 0.022(2) 0.0051(17) -0.0026(18) -0.0008(17) C16 0.023(2) 0.024(2) 0.022(3) 0.0013(19) -0.0019(19) -0.0034(19) C17 0.070(4) 0.013(2) 0.025(3) -0.0006(19) 0.000(2) 0.000(2) C18 0.097(5) 0.017(2) 0.039(3) 0.001(2) -0.005(3) -0.004(3) C19 0.112(5) 0.028(3) 0.031(3) 0.003(2) -0.016(3) -0.024(3) C20 0.089(5) 0.035(3) 0.048(4) 0.001(2) 0.007(3) 0.032(3) O1W 0.059(9) 0.077(9) 0.048(8) 0.008(7) -0.003(6) -0.009(7)