#------------------------------------------------------------------------------ #$Date: 2017-10-13 06:28:26 +0100 (Fri, 13 Oct 2017) $ #$Revision: 201972 $ #$URL: svn://www.crystallography.net/cod/cif/2/10/37/2103788.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2103788 loop_ _publ_author_name 'Clemente, Dore Augusto' 'Marzotto, Armando' _publ_section_title ; 22 Space-group changes ; _journal_issue 1 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 43 _journal_page_last 50 _journal_paper_doi 10.1107/S0108768102022668 _journal_volume 59 _journal_year 2003 _chemical_formula_moiety 'C22 N2 O6' _chemical_formula_sum 'C22 N2 O6' _chemical_formula_weight 388.24 _chemical_name_systematic ;1,1'-Dihydroxy-2,2'-(1,4,7,10-tetraoxadeca-1,10-diyl)-6,6'-(2,5-diazahexa-1,5- -diene-1,6-diyl)dibenzene ; _space_group_IT_number 19 _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M 'P 21 21 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 12.148(2) _cell_length_b 8.251(2) _cell_length_c 21.690(2) _cell_measurement_temperature 293(2) _cell_volume 2174.1(7) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.382 _diffrn_measured_fraction_theta_max 0.382 _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71070 _diffrn_reflns_av_R_equivalents 0.0212 _diffrn_reflns_av_sigmaI/netI 0.0872 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 12290 _diffrn_reflns_theta_full 32.87 _diffrn_reflns_theta_max 32.87 _diffrn_reflns_theta_min 1.88 _exptl_absorpt_coefficient_mu 0.090 _exptl_crystal_density_diffrn 1.186 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 776 _refine_diff_density_max 0.588 _refine_diff_density_min -0.577 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.1(6) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.631 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 121 _refine_ls_number_reflns 3081 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.631 _refine_ls_R_factor_all 0.0195 _refine_ls_R_factor_gt 0.0193 _refine_ls_shift/su_max 0.745 _refine_ls_shift/su_mean 0.006 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0178P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0699 _refine_ls_wR_factor_ref 0.0767 _reflns_number_gt 3050 _reflns_number_total 3081 _reflns_threshold_expression >2sigma(I) _cod_data_source_file an0613.cif _cod_data_source_block nohned _cod_database_code 2103788 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_type_symbol O1 0.48470(7) 0.01990(11) 0.07400(5) 0.0200(2) Uiso d 1 O O2 0.49230(7) -0.11310(11) -0.09220(5) 0.0200(2) Uiso d 1 O O3 0.64660(7) 0.02390(11) -0.16910(5) 0.0200(2) Uiso d 1 O O4 0.81390(7) 0.02970(11) -0.07060(5) 0.0200(2) Uiso d 1 O O5 0.85960(7) 0.04990(11) 0.06020(5) 0.0200(2) Uiso d 1 O O6 0.67100(7) 0.04800(11) 0.13490(5) 0.0200(2) Uiso d 1 O C1 0.60760(11) -0.14270(15) 0.21420(8) 0.0200(3) Uiso d 1 C C2 0.52320(10) -0.24260(15) 0.23560(8) 0.0200(3) Uiso d 1 C C3 0.42490(11) -0.25420(16) 0.20260(7) 0.0200(3) Uiso d 1 C C4 0.41100(10) -0.16610(16) 0.14840(8) 0.0200(3) Uiso d 1 C C5 0.49550(11) -0.06610(15) 0.12700(8) 0.0200(3) Uiso d 1 C C6 0.59380(10) -0.05450(15) 0.15990(8) 0.0200(3) Uiso d 1 C C7 0.31010(10) -0.18380(16) 0.11490(8) 0.0200(3) Uiso d 1 C N1 0.29180(9) -0.10300(13) 0.06330(6) 0.0200(2) Uiso d 1 N C8 0.18870(10) -0.12040(15) 0.02970(8) 0.0200(3) Uiso d 1 C C9 0.19740(10) -0.22580(15) -0.02480(8) 0.0200(3) Uiso d 1 C N2 0.28900(9) -0.16300(13) -0.06720(7) 0.0200(2) Uiso d 1 N C10 0.26260(11) -0.10710(15) -0.11970(8) 0.0200(3) Uiso d 1 C C11 0.31460(10) 0.01900(15) -0.21840(8) 0.0200(3) Uiso d 1 C C12 0.39290(11) 0.08680(15) -0.25770(8) 0.0200(3) Uiso d 1 C C13 0.50370(11) 0.08770(15) -0.24090(8) 0.0200(3) Uiso d 1 C C14 0.53630(10) 0.02060(15) -0.18470(8) 0.0200(3) Uiso d 1 C C15 0.45790(10) -0.04730(16) -0.14540(8) 0.0200(3) Uiso d 1 C C16 0.34710(10) -0.04800(16) -0.16230(8) 0.0200(3) Uiso d 1 C C17 0.66970(11) 0.15400(15) -0.12900(8) 0.0200(3) Uiso d 1 C C18 0.79130(11) 0.16050(15) -0.11140(8) 0.0200(3) Uiso d 1 C C19 0.92230(10) 0.03700(16) -0.04360(8) 0.0200(3) Uiso d 1 C C20 0.92130(11) 0.14000(15) 0.01580(8) 0.0200(3) Uiso d 1 C C21 0.85090(10) 0.13690(15) 0.11630(8) 0.0200(3) Uiso d 1 C C22 0.78000(10) 0.04060(16) 0.15820(8) 0.0200(3) Uiso d 1 C loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C14 O3 C17 111.04(11) C18 O4 C19 113.40(10) C21 O5 C20 110.75(10) C6 O6 C22 118.03(11) C6 C1 C2 120.07(13) C1 C2 C3 119.92(15) C4 C3 C2 120.07(12) C3 C4 C5 120.00(13) C3 C4 C7 118.61(12) C5 C4 C7 121.38(15) O1 C5 C6 118.71(12) O1 C5 C4 121.29(12) C6 C5 C4 120.00(15) O6 C6 C5 115.13(14) O6 C6 C1 124.91(12) C5 C6 C1 119.96(12) N1 C7 C4 121.47(12) C7 N1 C8 121.25(11) N1 C8 C9 113.49(11) C8 C9 N2 109.52(10) C10 N2 C9 118.50(11) N2 C10 C16 120.64(12) C16 C11 C12 119.98(12) C11 C12 C13 120.06(15) C12 C13 C14 119.99(14) O3 C14 C15 121.33(13) O3 C14 C13 118.74(13) C15 C14 C13 119.93(12) O2 C15 C16 121.65(13) O2 C15 C14 118.37(12) C16 C15 C14 119.98(14) C11 C16 C15 120.07(14) C11 C16 C10 118.97(12) C15 C16 C10 120.79(15) O3 C17 C18 111.94(11) O4 C18 C17 108.40(11) O4 C19 C20 110.78(10) O5 C20 C19 106.27(10) O5 C21 C22 107.35(11) O6 C22 C21 107.50(12) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O1 C5 1.3573(18) O2 C15 1.3420(17) O3 C14 1.3823(16) O3 C17 1.4098(18) O4 C18 1.4224(18) O4 C19 1.4425(16) O5 C21 1.4167(19) O5 C20 1.4290(17) O6 C6 1.3743(16) O6 C22 1.4186(16) C1 C6 1.395(2) C1 C2 1.3950(18) C2 C3 1.396(2) C3 C4 1.392(2) C4 C5 1.3964(18) C4 C7 1.4324(18) C5 C6 1.3944(19) C7 N1 1.322(2) N1 C8 1.4562(18) C8 C9 1.471(2) C9 N2 1.5338(18) N2 C10 1.270(2) C10 C16 1.465(2) C11 C16 1.394(2) C11 C12 1.394(2) C12 C13 1.3945(19) C13 C14 1.396(2) C14 C15 1.396(2) C15 C16 1.3950(19) C17 C18 1.5267(19) C19 C20 1.543(2) C21 C22 1.483(2) loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 ChemSpider 30654505