Observation of Deuteration Effect in Co-Crystal System: Hexamethylenetetraminium 3,5-Dinitrobenzoate Hemideuterated Water
Chen, Li-Zhuang; Zhao, Hong; Ge, Jia-Zhen; Xiong, Ren-Gen; Hu, Hong-Wen; Crystal Growth & Design 9 (2009) 3828–; doi:10.1021/cg900348x

data_4509560
_publ_section_title
;
 Observation of Deuteration Effect in Co-Crystal System:
 Hexamethylenetetraminium 3,5-Dinitrobenzoate Hemideuterated Water
;
_journal_issue                   9
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              3828
_journal_paper_doi               10.1021/cg900348x
_journal_volume                  9
_journal_year                    2009
_chemical_formula_sum            'C13 H15 D2 N6 O6.5'
_chemical_formula_weight         363.34
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                103.27(3)
_cell_angle_beta                 98.38(3)
_cell_angle_gamma                105.94(3)
_cell_formula_units_Z            2
_cell_length_a                   6.9911(14)
_cell_length_b                   10.748(2)
_cell_length_c                   11.428(2)
_cell_measurement_temperature    293(2)
_cell_volume                     783.4(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0297
_diffrn_reflns_av_sigmaI/netI    0.0407
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8172
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.11
_exptl_absorpt_coefficient_mu    0.125
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8116
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             378
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.272
_refine_diff_density_min         -0.255
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         3553
_refine_ls_number_restraints     333
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0864
_refine_ls_R_factor_gt           0.0560
_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^)+(0.0534P)^2^+0.3228P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1258
_refine_ls_wR_factor_ref         0.1403
_reflns_number_gt                2458
_reflns_number_total             3553
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg900348xsup3.cif
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      p-1
_cod_original_formula_sum        'C13 H15 D2 N6 O6.50'
_cod_database_code               4509560