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_1505186
_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_moiety         '(C8 H10 N4 O2), (C6 H8 O7)'
_chemical_formula_sum            'C14 H18 N4 O9'
_chemical_formula_weight         386.32
_chemical_name_common            3
_chemical_name_systematic
;
 caffeine-citric acid 1/1
;
_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                91.3330(10)
_cell_angle_beta                 99.0400(10)
_cell_angle_gamma                99.5880(10)
_cell_formula_units_Z            2
_cell_length_a                   7.38740(10)
_cell_length_b                   8.3967(2)
_cell_length_c                   13.5053(3)
_cell_measurement_reflns_used    12399
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      34.97
_cell_measurement_theta_min      1.00
_cell_volume                     814.72(3)
_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 0.929
_diffrn_measured_fraction_theta_max 0.929
_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  0.0269
_diffrn_reflns_av_sigmaI/netI    0.0310
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14491
_diffrn_reflns_theta_full        34.92
_diffrn_reflns_theta_max         34.92
_diffrn_reflns_theta_min         3.61
_exptl_absorpt_coefficient_mu    0.133
_exptl_absorpt_correction_T_max  0.959
_exptl_absorpt_correction_T_min  0.892
_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    1.575
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             404
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.422
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         6642
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0382
_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^)+(0.0565P)^2^+0.1876P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1055
_refine_ls_wR_factor_ref         0.1102
_reflns_number_gt                5931
_reflns_number_total             6642
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            mp0700054si20070319_094943.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1505186