#------------------------------------------------------------------------------ #$Date: 2013-02-20 17:18:43 +0200 (Wed, 20 Feb 2013) $ #$Revision: 73524 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/11/70/4117094.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_4117094 loop_ _publ_author_name 'Dirk Wiechert' 'Dietrich Mootz' 'Thomas Dahlems' _publ_contact_author ; Prof. Dr. Dietrich Mootz Institut f\"ur Anorganische Chemie und Strukturchemie Heinrich-Heine-Universit\"at D\"usseldorf Universit\"atsstr. 1 D-40225 D\"usseldorf Federal Republic of Germany ; _publ_contact_author_email mootz@uni-duesseldorf.de _publ_contact_author_fax '049 211 8114146' _publ_contact_author_phone '049 211 8113135' _publ_section_title ; The Formic Acid 1D Array with H Bonds All Reversed: Structure of a Cocrystal with Hydrogen Fluoride1,2 ; _journal_name_full 'Journal of the American Chemical Society' _journal_page_first 12665 _journal_page_last 12666 _journal_volume 119 _journal_year 1997 _chemical_formula_moiety 'H F.C H2 O2' _chemical_formula_sum 'C H3 F O2' _chemical_formula_weight 66.03 _chemical_melting_point 242 _chemical_name_systematic ; Formic acid - hydrogen fluoride (1/1) ; _space_group_IT_number 62 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2n' _symmetry_space_group_name_H-M 'P n m a' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 6.551(3) _cell_length_b 5.651(3) _cell_length_c 7.347(4) _cell_measurement_reflns_used 32 _cell_measurement_temperature 123(2) _cell_measurement_theta_max 13.122 _cell_measurement_theta_min 11.066 _cell_volume 272.0(2) _computing_cell_refinement 'Stoe DIF4' _computing_data_collection 'Stoe DIF4' _computing_data_reduction 'Stoe X-RED' _computing_molecular_graphics SHELXTL-PLUS _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _diffrn_ambient_temperature 123(2) _diffrn_measurement_device 'Siemens-Stoe AED 2' _diffrn_measurement_method \W/\Q-scan _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 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0080 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_l_max 1 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 638 _diffrn_reflns_theta_max 34.90 _diffrn_reflns_theta_min 4.17 _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.191 _exptl_absorpt_correction_type none _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.613 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_description ; grown by miniature zone-melting with the sample sealed in a PE tubing of 0.8 mm inner diameter, which in turn was enclosed in a thin-walled glass capillary for mechanical fixation ; _exptl_crystal_F_000 136 _refine_diff_density_max 0.231 _refine_diff_density_min -0.443 _refine_diff_density_rms 0.087 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 1.203 _refine_ls_goodness_of_fit_obs 1.165 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 34 _refine_ls_number_reflns 635 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.232 _refine_ls_restrained_S_obs 1.165 _refine_ls_R_factor_all 0.0450 _refine_ls_R_factor_obs 0.0386 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0638P)^2^+0.0737P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_wR_factor_all 0.1281 _refine_ls_wR_factor_obs 0.1139 _reflns_number_observed 566 _reflns_number_total 638 _reflns_observed_criterion >2sigma(I) _journal_paper_doi 10.1021/ja972337f _[local]_cod_data_source_file ja972337f.cif _[local]_cod_data_source_block hcooh/hf _cod_database_code 4117094 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' 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 F 0.0410(6) 0.0416(6) 0.0168(4) 0.000 0.0046(3) 0.000 O1 0.0166(4) 0.0302(5) 0.0173(4) 0.000 0.0009(3) 0.000 O2 0.0158(4) 0.0333(5) 0.0155(4) 0.000 0.0002(3) 0.000 C 0.0148(5) 0.0234(5) 0.0172(5) 0.000 -0.0010(3) 0.000 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags F F 0.1109(2) 0.2500 0.8174(1) 0.0332(3) Uani 1 d S O1 O 0.0989(1) 0.2500 0.4697(1) 0.0214(2) Uani 1 d S O2 O 0.2422(1) 0.2500 0.2001(1) 0.0216(2) Uani 1 d S C C 0.2552(2) 0.2500 0.3765(2) 0.0185(2) Uani 1 d S H1 H 0.381(4) 0.2500 0.434(3) 0.027(6) Uiso 1 d S H2 H 0.365(5) 0.2500 0.144(4) 0.040(7) Uiso 1 d S H3 H 0.104(5) 0.2500 0.708(5) 0.047(8) Uiso 1 d S 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -1,-3,3 1,-3,3 2,-2,2 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 O1 C O2 120.0(1) . . H1 C O1 119(2) . . H1 C O2 121(2) . . H2 O2 C 114(2) . . F H3 O1 178(3) . . C O1 H3 123(1) . . C H1 F 157(2) . 6_657 C H1 O2 130(2) . 6_656 O2 H2 O1 179(3) . 6_656 C O1 H2 118(1) . 6_556 H2 O1 H3 120(2) 6_556 . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 O1 C 1.232(2) . O2 C 1.298(2) . C H1 0.92(2) . O2 H2 0.91(2) . F H3 0.81(4) . F O1 2.556(2) . O1 H3 1.75(4) . O1 O2 2.649(2) 6_556 O1 H2 1.74(3) 6_556 O2 C 3.240(2) 6_556 O2 H1 2.57(2) 6_556 F C 3.238(2) 6_557 F H1 2.37(3) 6_557