#------------------------------------------------------------------------------ #$Date: 2025-03-04 21:27:02 +0200 (Tue, 04 Mar 2025) $ #$Revision: 298147 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/38/1573841.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_1573841 loop_ _publ_author_name 'Dunning, Samuel G.' 'Hari, Anirudh' 'Zhu, Li' 'Chen, Bo' 'Cody, George D.' 'Romi, Sebastiano' 'Zhang, Dongzhou' 'Strobel, Timothy A.' _publ_section_title ; Double-core nanothread formation from α-furil via a pressure-induced planarization pathway. ; _journal_issue 9 _journal_name_full 'Chemical science' _journal_page_first 4144 _journal_page_last 4151 _journal_paper_doi 10.1039/d4sc07412b _journal_volume 16 _journal_year 2025 _chemical_formula_moiety 'C10 H6 O4' _chemical_formula_sum 'C10 H6 O4' _chemical_formula_weight 190.15 _chemical_name_common 'Furil, phase II' _chemical_name_systematic Di(furan-2-yl)ethanedione _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2023-06-29 _audit_creation_method ; Olex2 1.5 (compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748) ; _audit_update_record ; 2024-03-25 deposited with the CCDC. 2025-01-02 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 93.132(15) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 14.586(5) _cell_length_b 7.0535(14) _cell_length_c 3.4512(6) _cell_measurement_reflns_used 106 _cell_measurement_temperature 273.15 _cell_measurement_theta_max 15.235 _cell_measurement_theta_min 3.631 _cell_volume 354.54(15) _computing_cell_refinement 'SAINT V8.40B (?, 2016)' _computing_data_reduction 'SAINT V8.40B (?, 2016)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'XT (Sheldrick, 2015)' _diffrn_ambient_temperature 273.15 _diffrn_measured_fraction_theta_full 0.307 _diffrn_measured_fraction_theta_max 0.159 _diffrn_measurement_device_type Synchrotron _diffrn_radiation_type Synchrotron _diffrn_radiation_wavelength 0.434 _diffrn_reflns_av_unetI/netI 0.2943 _diffrn_reflns_Laue_measured_fraction_full 0.307 _diffrn_reflns_Laue_measured_fraction_max 0.159 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min 1 _diffrn_reflns_limit_l_max 3 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 554 _diffrn_reflns_point_group_measured_fraction_full 0.307 _diffrn_reflns_point_group_measured_fraction_max 0.159 _diffrn_reflns_theta_full 15.094 _diffrn_reflns_theta_max 23.366 _diffrn_reflns_theta_min 1.959 _diffrn_source_current 0.0 _diffrn_source_power 0.0 _diffrn_source_voltage 0.0 _exptl_absorpt_coefficient_mu 0.056 _exptl_absorpt_process_details ; TWINABS-2012/1 (Bruker,2012) was used for absorption correction. For component 1: wR2(int) was 0.1403 before and 0.0892 after correction. For component 2: wR2(int) was 0.1409 before and 0.0766 after correction. ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.781 _exptl_crystal_description plate _exptl_crystal_F_000 196 _exptl_crystal_size_max 0.025 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.005 _refine_diff_density_max 0.293 _refine_diff_density_min -0.271 _refine_diff_density_rms 0.086 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.130 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 30 _refine_ls_number_reflns 554 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.130 _refine_ls_R_factor_all 0.2663 _refine_ls_R_factor_gt 0.1550 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1856P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.3424 _refine_ls_wR_factor_ref 0.3880 _reflns_Friedel_coverage 0.000 _reflns_number_gt 228 _reflns_number_total 554 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc07412b2.cif _cod_data_source_block p2_0m_5 _cod_depositor_comments 'Adding full bibliography for 1573840--1573842.cif.' _cod_original_cell_volume 354.55(16) _cod_database_code 1573841 _shelx_shelxl_version_number 2019/1 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.609(13) 0.391(13) 2. Fixed Uiso At 1.2 times of: All C(H) groups 3.a Aromatic/amide H refined with riding coordinates: C004(H004), C006(H006), C007(H007) ; _shelx_res_file ; TITL P2_0m_5 in P2(1)/n p2_0m_5.res created by SHELXL-2019/1 at 13:33:25 on 29-Jun-2023 CELL 0.434 14.5864 7.0535 3.4512 90 93.1315 90 ZERR 2 0.0053 0.0014 0.0006 0 0.0152 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C O H DISP C 0.0001 0.0005 5.3074 DISP H 0 0 0.6003 DISP O 0.0022 0.002 10.704 UNIT 20 8 12 L.S. 10 PLAN 5 TEMP 0 CONF list 4 MORE -1 BOND $H fmap 2 acta OMIT -6 7 2 OMIT 5 6 2 OMIT 0 9 2 OMIT -5 5 1 REM REM REM WGHT 0.185600 BASF 0.39102 FVAR 0.12599 O001 2 0.683801 0.290935 0.453951 11.00000 0.02800 O002 2 0.586909 0.606463 0.251917 11.00000 0.03497 C003 1 0.546172 0.483913 0.433861 11.00000 0.03333 C004 1 0.568433 0.147252 0.722522 11.00000 0.02190 AFIX 43 H004 3 0.510067 0.128847 0.811655 11.00000 -1.20000 AFIX 0 C005 1 0.599496 0.307461 0.562078 11.00000 0.03703 C006 1 0.713528 0.111253 0.556592 11.00000 0.02939 AFIX 43 H006 3 0.770976 0.058600 0.522341 11.00000 -1.20000 AFIX 0 C007 1 0.635256 0.021151 0.731047 11.00000 0.02357 AFIX 43 H007 3 0.633094 -0.101491 0.829055 11.00000 -1.20000 AFIX 0 HKLF 5 REM P2_0m_5 in P2(1)/n REM wR2 = 0.3880, GooF = S = 1.130, Restrained GooF = 1.130 for all data REM R1 = 0.1550 for 228 Fo > 4sig(Fo) and 0.2663 for all 554 data REM 30 parameters refined using 0 restraints END WGHT 0.1864 0.0000 REM Highest difference peak 0.293, deepest hole -0.271, 1-sigma level 0.086 Q1 1 0.7511 0.2355 0.1801 11.00000 0.05 0.29 Q2 1 0.4662 0.2205 0.4160 11.00000 0.05 0.28 Q3 1 0.7404 -0.1761 0.4507 11.00000 0.05 0.28 Q4 1 0.5374 0.3211 0.8787 11.00000 0.05 0.28 Q5 1 0.6327 0.6106 0.3993 11.00000 0.05 0.27 ; _shelx_res_checksum 20333 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_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' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O001 O 0.6838(16) 0.2909(9) 0.454(3) 0.028(3) Uiso 1 1 d . . . . . O002 O 0.5869(13) 0.6065(8) 0.252(3) 0.035(3) Uiso 1 1 d . . . . . C003 C 0.546(2) 0.4839(16) 0.434(5) 0.033(4) Uiso 1 1 d . . . . . C004 C 0.568(2) 0.1473(11) 0.723(4) 0.022(3) Uiso 1 1 d . . . . . H004 H 0.510067 0.128847 0.811655 0.026 Uiso 1 1 calc R U . . . C005 C 0.599(3) 0.3075(14) 0.562(5) 0.037(5) Uiso 1 1 d . . . . . C006 C 0.714(2) 0.1113(13) 0.557(4) 0.029(3) Uiso 1 1 d . . . . . H006 H 0.770976 0.058600 0.522341 0.035 Uiso 1 1 calc R U . . . C007 C 0.635(2) 0.0212(13) 0.731(4) 0.024(3) Uiso 1 1 d . . . . . H007 H 0.633094 -0.101491 0.829055 0.028 Uiso 1 1 calc R U . . . loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0001 0.0005 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0022 0.0020 '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' 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 C005 O001 C006 107.2(15) . . ? O002 C003 C003 121.7(17) . 3_666 ? O002 C003 C005 118(3) . . ? C003 C003 C005 120(2) 3_666 . ? C005 C004 H004 126.0 . . ? C007 C004 H004 126.0 . . ? C007 C004 C005 108(3) . . ? O001 C005 C003 117.6(18) . . ? O001 C005 C004 113(2) . . ? C004 C005 C003 129(4) . . ? O001 C006 H006 127.4 . . ? O001 C006 C007 105(2) . . ? C007 C006 H006 127.4 . . ? C004 C007 C006 106.9(12) . . ? C004 C007 H007 126.6 . . ? C006 C007 H007 126.6 . . ? 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 O001 C005 1.31(4) . ? O001 C006 1.379(18) . ? O002 C003 1.24(2) . ? C003 C003 1.46(6) 3_666 ? C003 C005 1.52(3) . ? C004 H004 0.9300 . ? C004 C005 1.35(2) . ? C004 C007 1.32(4) . ? C006 H006 0.9300 . ? C006 C007 1.46(3) . ? C007 H007 0.9300 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O001 C006 C007 C004 -0.4(14) . . . . ? O002 C003 C005 O001 -4(3) . . . . ? O002 C003 C005 C004 -171.9(17) . . . . ? C003 C003 C005 O001 -176(2) 3_666 . . . ? C003 C003 C005 C004 16(4) 3_666 . . . ? C005 O001 C006 C007 1.4(18) . . . . ? C005 C004 C007 C006 -0.7(16) . . . . ? C006 O001 C005 C003 -172.0(13) . . . . ? C006 O001 C005 C004 -2(2) . . . . ? C007 C004 C005 O001 2(2) . . . . ? C007 C004 C005 C003 170.4(16) . . . . ? loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.609(13) 2 0.391(13)