Powder X-ray diffraction as an emerging method to structurally characterize organic solids.
Karki, Shyam; Fábián, László; Friscić, Tomislav; Jones, William; Organic letters 9 (2007) 3133–3136; doi:10.1021/ol071329t

data_1505484
_publ_section_title
;
 Powder X-ray diffraction as an emerging method to structurally
 characterize organic solids.
;
_journal_issue                   16
_journal_name_full               'Organic letters'
_journal_page_first              3133
_journal_page_last               3136
_journal_paper_doi               10.1021/ol071329t
_journal_volume                  9
_journal_year                    2007
_chemical_formula_moiety         'C7 H8 N4 O2, C2 H F3 O2'
_chemical_formula_sum            'C9 H9 F3 N4 O4'
_chemical_formula_weight         294.20
_chemical_name_common            'theobromine trifluoroacetic acid'
_chemical_name_systematic
;
theobromine trifluoroacetic acid
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                90.1645(18)
_cell_angle_beta                 95.5873(17)
_cell_angle_gamma                99.7283(22)
_cell_formula_units_Z            2
_cell_length_a                   5.09253(14)
_cell_length_b                   8.33537(37)
_cell_length_c                   14.89683(42)
_cell_measurement_temperature    298
_cell_volume                     620.17(4)
_computing_cell_refinement       'Topas V3 (Bruker AXS, 2005)'
_computing_structure_refinement  'Topas V3 (Bruker AXS, 2005)'
_computing_structure_solution    'DASH 3.0 (David et al., 2004)'
_diffrn_ambient_temperature      298
_diffrn_radiation_type           'Cu K\a~1~'
_diffrn_radiation_wavelength     1.54056
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Cu
_exptl_absorpt_coefficient_mu    1.360
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.576
_pd_block_diffractogram_id       tbtfac
_pd_instr_location               ' ?'
_pd_meas_2theta_range_inc        0.004187
_pd_meas_2theta_range_max        59.9881
_pd_meas_2theta_range_min        5.0021
_pd_meas_number_of_points        13135
_pd_prep_pressure                100
_pd_prep_temperature             298
_pd_proc_2theta_range_inc        0.004187
_pd_proc_2theta_range_max        59.9881
_pd_proc_2theta_range_min        5.0021
_pd_proc_info_data_reduction     none
_pd_proc_info_excluded_regions   none
_pd_proc_ls_background_function  'Chebyshev polynomial, 15 terms'
_pd_proc_ls_pref_orient_corr
;
March (1932), along the -114 axis, ratio = 0.9062(11)
;
_pd_proc_ls_profile_function     'double-Voigt (Balzar, 1999)'
_pd_proc_ls_prof_R_factor        0.04426
_pd_proc_ls_prof_wR_expected     0.02279
_pd_proc_ls_prof_wR_factor       0.05726
_pd_proc_wavelength              1.54056
_pd_spec_mounting                ' ?'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.585
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           sparse
_refine_ls_number_constraints    1
_refine_ls_number_parameters     118
_refine_ls_number_restraints     78
_refine_ls_R_I_factor            0.03122
_refine_ls_weighting_scheme      sigma
_cod_data_source_file            ol071329t-file004.cif
_cod_data_source_block           tbtfac
_cod_original_cell_volume        620.168(37)
_cod_database_code               1505484