Towards proton transfer in hydrogen bonded molecular complexes: joint experimental and theoretical modelling and an energy scale for polymorphism
Schmidtmann, Marc; Gutmann, Matthias J.; Middlemiss, Derek S.; Wilson, Chick C.; CrystEngComm 9 (2007) 743–; doi:10.1039/b709136m

data_7203050
_publ_section_title
;
 Towards proton transfer in hydrogen bonded molecular complexes: joint
 experimental and theoretical modelling and an energy scale for
 polymorphism
;
_journal_issue                   9
_journal_name_full               CrystEngComm
_journal_page_first              743
_journal_paper_doi               10.1039/b709136m
_journal_volume                  9
_journal_year                    2007
_chemical_formula_sum            'C14 H14 N4 O6'
_chemical_formula_weight         334.29
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                85.638(9)
_cell_angle_beta                 87.856(10)
_cell_angle_gamma                84.221(10)
_cell_formula_units_Z            1
_cell_length_a                   3.6811(7)
_cell_length_b                   7.5912(14)
_cell_length_c                   12.455(2)
_cell_measurement_reflns_used    3240
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.81
_cell_measurement_theta_min      3.06
_cell_volume                     345.11(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0223
_diffrn_reflns_av_sigmaI/netI    0.0239
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8148
_diffrn_reflns_theta_full        33.92
_diffrn_reflns_theta_max         33.92
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    0.128
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       stick
_exptl_crystal_F_000             174
_refine_diff_density_max         0.614
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         2759
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0405
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+0.0400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1153
_refine_ls_wR_factor_ref         0.1212
_reflns_number_gt                2340
_reflns_number_total             2759
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b709136m.txt
_cod_data_source_block           oxaiso6
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7203050