#------------------------------------------------------------------------------ #$Date: 2013-08-29 16:37:19 +0100 (Thu, 29 Aug 2013) $ #$Revision: 88064 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/23/2202357.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_2202357 loop_ _publ_author_name 'Ejsmont, Krzysztof' 'Zaleski, Jacek' 'Sporzy\'nski, Andrzej' 'Lewandowski, Micha\/l' _publ_section_title ; 5-Formyl-2-furanboronic acid at 100K ; _journal_issue 9 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first o1324 _journal_page_last o1326 _journal_volume 59 _journal_year 2003 _chemical_formula_moiety 'C5 H5 B O4' _chemical_formula_sum 'C5 H5 B O4' _chemical_formula_weight 139.90 _chemical_name_systematic ; ? ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 91.31(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 3.7550(8) _cell_length_b 7.758(2) _cell_length_c 20.694(4) _cell_measurement_reflns_used 3391 _cell_measurement_temperature 100.0(2) _cell_measurement_theta_max 25.48 _cell_measurement_theta_min 3.28 _cell_volume 602.7(2) _computing_cell_refinement 'CrysAlisRED (Oxford Diffraction, 2002)' _computing_data_collection 'CrysAlisCCD (Oxford Diffraction, 2002)' _computing_data_reduction CrysAlisRED _computing_molecular_graphics SHELXTL _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXTL (Sheldrick, 1990)' _diffrn_ambient_temperature 100.0(2) _diffrn_detector_area_resol_mean '1024 x 1024 with blocks 2 x 2' _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type Xcalibur _diffrn_measurement_method '\w 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 0.0889 _diffrn_reflns_av_sigmaI/netI 0.0613 _diffrn_reflns_limit_h_max 3 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 3391 _diffrn_reflns_theta_full 25.48 _diffrn_reflns_theta_max 25.48 _diffrn_reflns_theta_min 3.28 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.131 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.542 _exptl_crystal_density_method 'not measured' _exptl_crystal_description cube _exptl_crystal_F_000 288 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _refine_diff_density_max 0.162 _refine_diff_density_min -0.207 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.945 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 111 _refine_ls_number_reflns 1126 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.945 _refine_ls_R_factor_all 0.0673 _refine_ls_R_factor_gt 0.0474 _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^)+(0.0811P)^2^] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1197 _refine_ls_wR_factor_ref 0.1324 _reflns_number_gt 764 _reflns_number_total 1126 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file bt6327.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P 21/n' _cod_database_code 2202357 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' 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_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol O1 0.4972(4) 0.36605(18) 0.16766(6) 0.0377(5) Uani d . 1 . . O C2 0.3680(6) 0.3652(3) 0.10461(10) 0.0370(6) Uani d . 1 . . C C3 0.2287(6) 0.5230(3) 0.09057(11) 0.0435(6) Uani d . 1 . . C C4 0.2760(6) 0.6270(3) 0.14538(11) 0.0439(6) Uani d . 1 . . C C5 0.4390(6) 0.5284(3) 0.19130(10) 0.0368(5) Uani d . 1 . . C B6 0.4052(7) 0.2001(3) 0.06251(12) 0.0404(6) Uani d . 1 . . B O7 0.2772(5) 0.2141(2) 0.00177(7) 0.0545(6) Uani d . 1 . . O O8 0.5605(5) 0.0522(2) 0.08392(8) 0.0516(6) Uani d . 1 . . O C9 0.5554(6) 0.5719(3) 0.25553(11) 0.0442(6) Uani d . 1 . . C O10 0.7116(5) 0.4754(2) 0.29327(7) 0.0550(5) Uani d . 1 . . O H9 0.502(6) 0.697(4) 0.2692(11) 0.058(7) Uiso d . 1 . . H H3 0.128(5) 0.556(3) 0.0477(11) 0.046(6) Uiso d . 1 . . H H4 0.209(7) 0.745(4) 0.1508(13) 0.070(8) Uiso d . 1 . . H H7 0.325(9) 0.114(5) -0.0258(16) 0.094(11) Uiso d . 1 . . H H8 0.617(7) 0.048(4) 0.1224(14) 0.065(8) Uiso d . 1 . . H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O1 0.0528(9) 0.0329(8) 0.0270(8) 0.0032(7) -0.0068(6) -0.0006(6) C2 0.0429(12) 0.0398(12) 0.0280(11) -0.0003(10) -0.0049(9) -0.0004(9) C3 0.0530(14) 0.0414(13) 0.0357(13) 0.0039(11) -0.0082(10) 0.0020(10) C4 0.0522(14) 0.0354(12) 0.0439(13) 0.0038(11) -0.0056(11) 0.0002(10) C5 0.0446(12) 0.0320(12) 0.0338(12) -0.0012(9) -0.0002(9) -0.0044(9) B6 0.0509(15) 0.0411(14) 0.0289(13) 0.0032(12) -0.0022(10) 0.0002(10) O7 0.0849(13) 0.0459(10) 0.0319(9) 0.0161(9) -0.0150(8) -0.0052(7) O8 0.0854(13) 0.0411(10) 0.0276(9) 0.0128(9) -0.0132(8) -0.0028(7) C9 0.0568(15) 0.0404(13) 0.0353(13) -0.0046(11) -0.0015(11) -0.0054(10) O10 0.0816(13) 0.0501(11) 0.0326(9) -0.0018(9) -0.0123(8) 0.0002(7) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag O1 C5 . 1.371(2) y O1 C2 . 1.382(2) y C2 C3 . 1.360(3) y C2 B6 . 1.557(3) y C3 C4 . 1.400(3) y C3 H3 . 0.99(2) ? C4 C5 . 1.355(3) y C4 H4 . 0.95(3) ? C5 C9 . 1.430(3) y B6 O7 . 1.340(3) y B6 O8 . 1.357(3) y O7 H7 . 0.98(4) ? O8 H8 . 0.82(3) ? C9 O10 . 1.222(3) y C9 H9 . 1.03(3) ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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_publ_flag C5 O1 C2 106.6(2) y C3 C2 O1 108.8(2) y C3 C2 B6 131.3(2) y O1 C2 B6 119.9(2) y C2 C3 C4 107.7(2) y C2 C3 H3 124.0(14) ? C4 C3 H3 128.2(14) ? C5 C4 C3 106.8(2) y C5 C4 H4 125.0(16) ? C3 C4 H4 128.1(17) ? C4 C5 O1 110.0(2) y C4 C5 C9 130.0(2) y O1 C5 C9 120.0(2) y O7 B6 O8 121.1(2) y O7 B6 C2 115.1(2) y O8 B6 C2 123.8(2) y B6 O7 H7 114.5(19) ? B6 O8 H8 116.8(19) ? O10 C9 C5 125.6(2) y O10 C9 H9 119.5(14) ? C5 C9 H9 114.9(14) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA O7 H7 O8 3_655 0.98(4) 1.82(4) 2.799(2) 173(3) O8 H8 O10 2_645 0.82(3) 1.93(3) 2.729(2) 164(3) C3 H3 O7 3_565 0.99(2) 2.55(2) 3.355(3) 139(2) 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_publ_flag C5 O1 C2 C3 -1.0(2) ? C5 O1 C2 B6 177.8(2) y O1 C2 C3 C4 1.0(3) ? B6 C2 C3 C4 -177.6(2) y C2 C3 C4 C5 -0.7(3) ? C3 C4 C5 O1 0.1(3) ? C3 C4 C5 C9 178.4(2) ? C2 O1 C5 C4 0.5(2) ? C2 O1 C5 C9 -178.0(2) ? C3 C2 B6 O7 -0.3(4) ? O1 C2 B6 O7 -178.8(2) y C3 C2 B6 O8 178.4(2) y O1 C2 B6 O8 -0.1(4) ? C4 C5 C9 O10 -177.5(2) ? O1 C5 C9 O10 0.7(4) ? _cod_database_fobs_code 2202357