Hydrogen-Bond Symmetry in Difluoromaleate Monoanion
Charles L. Perrin; Phaneendrasai Karri; Curtis Moore; Arnold L. Rheingold; Journal of the American Chemical Society 134 (2012) 7766–7772; doi:10.1021/ja2117848

data_4117902
_publ_section_title
;
 Hydrogen-Bond Symmetry in Difluoromaleate Monoanion
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7766
_journal_page_last               7772
_journal_paper_doi               10.1021/ja2117848
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C4 H F2 K O4'
_chemical_formula_weight         190.15
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           57
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2c 2b'
_symmetry_space_group_name_H-M   'P b c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   4.6377(3)
_cell_length_b                   8.0574(6)
_cell_length_c                   15.4299(12)
_cell_measurement_reflns_used    1260
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      63.55
_cell_measurement_theta_min      9.57
_cell_volume                     576.58(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_sigmaI/netI    0.0433
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            1942
_diffrn_reflns_theta_full        55.00
_diffrn_reflns_theta_max         64.21
_diffrn_reflns_theta_min         9.57
_exptl_absorpt_coefficient_mu    8.306
_exptl_absorpt_correction_T_max  0.6815
_exptl_absorpt_correction_T_min  0.2874
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.190
_exptl_crystal_description       Plate
_exptl_crystal_F_000             376
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.559
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.111
_refine_ls_extinction_coef       0.0027(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     55
_refine_ls_number_reflns         490
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0427
_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^)+(0.0523P)^2^+3.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1120
_refine_ls_wR_factor_ref         0.1143
_reflns_number_gt                434
_reflns_number_total             490
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2117848_si_002.cif
_cod_data_source_block           per18
_cod_database_code               4117902