#------------------------------------------------------------------------------ #$Date: 2025-03-04 21:27:02 +0200 (Tue, 04 Mar 2025) $ #$Revision: 298147 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/38/1573842.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_1573842 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 '2(C10 H6 O4)' _chemical_formula_sum 'C20 H12 O8' _chemical_formula_weight 380.30 _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 _audit_creation_date 2023-12-05 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2024-03-25 deposited with the CCDC. 2025-01-02 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 94.48(3) _cell_angle_gamma 90 _cell_formula_units_Z 1 _cell_length_a 3.313(3) _cell_length_b 6.957(7) _cell_length_c 14.228(16) _cell_measurement_reflns_used 76 _cell_measurement_temperature 273(2) _cell_measurement_theta_max 11.861 _cell_measurement_theta_min 3.579 _cell_volume 326.9(6) _computing_cell_refinement 'SAINT V8.40B (?, 2016)' _computing_data_reduction 'SAINT V8.40B (?, 2016)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _diffrn_ambient_temperature 273.15 _diffrn_measured_fraction_theta_full 0.459 _diffrn_measured_fraction_theta_max 0.285 _diffrn_measurement_device_type 'APS 13-BM-C' _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.434 _diffrn_reflns_av_unetI/netI 0.6302 _diffrn_reflns_Laue_measured_fraction_full 0.459 _diffrn_reflns_Laue_measured_fraction_max 0.285 _diffrn_reflns_number 571 _diffrn_reflns_point_group_measured_fraction_full 0.459 _diffrn_reflns_point_group_measured_fraction_max 0.285 _diffrn_reflns_theta_full 15.094 _diffrn_reflns_theta_max 23.095 _diffrn_reflns_theta_min 3.577 _exptl_absorpt_coefficient_mu 0.061 _exptl_absorpt_process_details ; TWINABS-2012/1 (Bruker,2012) was used for absorption correction. Final HKLF 4 output contains 2560 reflections, Rint = 0.9728 (570 with I > 3sig(I), Rint = 0.9750) ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.932 _exptl_crystal_description plate _exptl_crystal_F_000 196 _refine_diff_density_max 0.695 _refine_diff_density_min -0.715 _refine_diff_density_rms 0.208 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 2.297 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 29 _refine_ls_number_reflns 571 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 2.297 _refine_ls_R_factor_all 0.5162 _refine_ls_R_factor_gt 0.4104 _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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.6897 _refine_ls_wR_factor_ref 0.7248 _reflns_Friedel_coverage 0.000 _reflns_number_gt 227 _reflns_number_total 571 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc07412b2.cif _cod_data_source_block samp3_0m_4 _cod_depositor_comments 'Adding full bibliography for 1573840--1573842.cif.' _cod_database_code 1573842 _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. Fixed Uiso At 1.2 times of: All C(H) groups 2.a Aromatic/amide H refined with riding coordinates: C003(H003), C004(H004), C007(H007) ; _shelx_res_file ; TITL furil_p3_4p4gpa_crystal2_8s_0m_a.res in P2(1)/n samp3_0m_4.res created by SHELXL-2019/1 at 11:05:48 on 05-Dec-2023 CELL 0.434 3.3129 6.9569 14.2278 90 94.483 90 ZERR 1 0.003 0.0066 0.0159 0 0.033 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H O DISP C -0.0009 0.0005 5.3074 DISP H 0 0 0.6003 DISP O -0.0008 0.002 10.704 UNIT 20 12 8 L.S. 20 PLAN 3 TEMP 0 CONF BOND $H list 4 MORE -1 fmap 2 acta OMIT -2 11 4 OMIT 2 11 2 OMIT 2 10 3 OMIT -2 11 5 OMIT 0 5 5 OMIT 1 7 2 OMIT -3 3 5 OMIT 0 7 4 OMIT 2 11 4 OMIT 3 2 3 OMIT 2 4 8 OMIT -2 11 -1 OMIT -2 8 7 OMIT 2 11 5 OMIT 2 11 5 OMIT 2 11 3 OMIT -2 11 6 OMIT -2 7 12 OMIT -2 11 2 OMIT 0 8 0 OMIT -3 4 6 OMIT 1 9 2 OMIT -2 2 0 OMIT -2 2 0 REM REM REM WGHT 0.200000 FVAR 1.41172 O001 3 0.540045 0.282498 0.313711 11.00000 0.02334 O002 3 0.754554 0.612301 0.414232 11.00000 0.02681 C003 1 0.265557 0.138264 0.431832 11.00000 0.02809 AFIX 43 H003 2 0.161052 0.121922 0.490098 11.00000 -1.20000 AFIX 0 C004 1 0.430062 0.105549 0.293147 11.00000 0.04016 AFIX 43 H004 2 0.457379 0.052130 0.234061 11.00000 -1.20000 AFIX 0 C005 1 0.436512 0.303125 0.401659 11.00000 0.02707 C006 1 0.557978 0.487123 0.448601 11.00000 0.02483 C007 1 0.271069 0.003563 0.364825 11.00000 0.02082 AFIX 43 H007 2 0.189720 -0.124285 0.366182 11.00000 -1.20000 AFIX 0 HKLF 4 REM furil_p3_4p4gpa_crystal2_8s_0m_a.res in P2(1)/n REM wR2 = 0.7248, GooF = S = 2.297, Restrained GooF = 2.297 for all data REM R1 = 0.4104 for 227 Fo > 4sig(Fo) and 0.5162 for all 571 data REM 29 parameters refined using 0 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 0.695, deepest hole -0.715, 1-sigma level 0.208 Q1 1 0.0823 -0.0519 0.3175 11.00000 0.05 0.69 Q2 1 -0.2138 -0.1328 0.3432 11.00000 0.05 0.68 Q3 1 0.2586 0.1170 0.4044 11.00000 0.05 0.68 ; _shelx_res_checksum 15585 _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 0.540(3) 0.2825(13) 0.3137(13) 0.023(4) Uiso 1 1 d . . . . . O002 O 0.755(3) 0.6123(12) 0.4142(14) 0.027(4) Uiso 1 1 d . . . . . C003 C 0.266(5) 0.138(2) 0.432(2) 0.028(5) Uiso 1 1 d . . . . . H003 H 0.161052 0.121922 0.490098 0.034 Uiso 1 1 calc R . . . . C004 C 0.430(6) 0.106(2) 0.293(3) 0.040(6) Uiso 1 1 d . . . . . H004 H 0.457379 0.052130 0.234061 0.048 Uiso 1 1 calc R . . . . C005 C 0.437(5) 0.3031(19) 0.402(2) 0.027(5) Uiso 1 1 d . . . . . C006 C 0.558(5) 0.4871(18) 0.449(2) 0.025(5) Uiso 1 1 d . . . . . C007 C 0.271(5) 0.0036(17) 0.365(2) 0.021(5) Uiso 1 1 d . . . . . H007 H 0.189720 -0.124285 0.366182 0.025 Uiso 1 1 calc R . . . . loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C -0.0009 0.0005 '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' O O -0.0008 0.0020 '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 C004 O001 C005 103(2) . . ? C005 C003 H003 125.2 . . ? C007 C003 H003 125.2 . . ? C007 C003 C005 110(3) . . ? O001 C004 H004 122.2 . . ? O001 C004 C007 116(3) . . ? C007 C004 H004 122.2 . . ? O001 C005 C003 110.4(19) . . ? O001 C005 C006 115.8(18) . . ? C003 C005 C006 133(3) . . ? O002 C006 C005 125(2) . . ? O002 C006 C006 118.5(18) . 3_666 ? C005 C006 C006 116.4(19) . 3_666 ? C003 C007 C004 101.2(15) . . ? C003 C007 H007 129.4 . . ? C004 C007 H007 129.4 . . ? 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 C004 1.31(2) . ? O001 C005 1.33(3) . ? O002 C006 1.21(2) . ? C003 H003 0.9300 . ? C003 C005 1.36(3) . ? C003 C007 1.34(4) . ? C004 H004 0.9300 . ? C004 C007 1.38(4) . ? C005 C006 1.48(3) . ? C006 C006 1.55(6) 3_666 ? 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 C004 C007 C003 4(2) . . . . ? O001 C005 C006 O002 -3(3) . . . . ? O001 C005 C006 C006 -179.6(19) . . . 3_666 ? C003 C005 C006 O002 170(2) . . . . ? C003 C005 C006 C006 -6(3) . . . 3_666 ? C004 O001 C005 C003 -0.2(18) . . . . ? C004 O001 C005 C006 174.8(15) . . . . ? C005 O001 C004 C007 -2.4(19) . . . . ? C005 C003 C007 C004 -4(2) . . . . ? C007 C003 C005 O001 3(2) . . . . ? C007 C003 C005 C006 -171.0(17) . . . . ?