The Formic Acid 1D Array with H Bonds All Reversed: Structure of a Cocrystal with Hydrogen Fluoride1,2
Dirk Wiechert; Dietrich Mootz; Thomas Dahlems; Journal of the American Chemical Society 119 (1997) 12665–12666; doi:10.1021/ja972337f

data_4117094
_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
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_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
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 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_paper_doi               10.1021/ja972337f
_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      ?
_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_details
'w=1/[\s^2^(Fo^2^)+(0.0638P)^2^+0.0737P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_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)
_cod_data_source_file            ja972337f.cif
_cod_data_source_block           hcooh/hf
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'Not Measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0638P)^2^+0.0737P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0638P)^2^+0.0737P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4117094