Screening for Pharmaceutical Cocrystal Hydrates via Neat and Liquid-Assisted Grinding
Karki, Shyam; Friščić, Tomislav; Jones, William; Motherwell, W. D. Samuel; Molecular Pharmaceutics 4 (2007) 347–; doi:10.1021/mp0700054

data_1505185
_publ_section_title
;
 Screening for Pharmaceutical Cocrystal Hydrates via Neat and
 Liquid-Assisted Grinding
;
_journal_issue                   3
_journal_name_full               'Molecular Pharmaceutics'
_journal_page_first              347
_journal_paper_doi               10.1021/mp0700054
_journal_volume                  4
_journal_year                    2007
_chemical_formula_sum            'C13 H18 N4 O10'
_chemical_formula_weight         390.31
_chemical_name_common            2
_chemical_name_systematic
;
 theophylline-citric acid-water 1/1/1 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 105.2120(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.9217(2)
_cell_length_b                   6.17660(10)
_cell_length_c                   15.3751(3)
_cell_measurement_reflns_used    41307
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      32.03
_cell_measurement_theta_min      1.02
_cell_volume                     1642.32(5)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius B.V. 1998)'
_computing_data_reduction
;
 HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_publication_material  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_solution    'SIR-92 (Altomare et al. 1994)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.698
_diffrn_measured_fraction_theta_max 0.698
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Thin slice \w and \f scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0206
_diffrn_reflns_av_sigmaI/netI    0.0419
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6458
_diffrn_reflns_theta_full        31.50
_diffrn_reflns_theta_max         31.50
_diffrn_reflns_theta_min         3.57
_exptl_absorpt_coefficient_mu    0.137
_exptl_absorpt_correction_T_max  0.972
_exptl_absorpt_correction_T_min  0.838
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.347
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         3811
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0393
_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^)+(0.0564P)^2^+0.6598P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1155
_refine_ls_wR_factor_ref         0.1189
_reflns_number_gt                3490
_reflns_number_total             3811
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            mp0700054si20070319_094943.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               1505185