Effect of Particle Size and Morphology on the Dehydration Mechanism of a Non-Stoichiometric Hydrate
Kang, Feirong; Vogt, Frederick G.; Brum, Jeffrey; Forcino, Rachel; Copley, Royston C. B.; Williams, Glenn; Carlton, Robert; Crystal Growth & Design 12 (2012) 60–; doi:10.1021/cg200768x

data_4502739
_publ_section_title
;
 Effect of Particle Size and Morphology on the Dehydration Mechanism of a
 Non-Stoichiometric Hydrate
;
_journal_issue                   1
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              60
_journal_paper_doi               10.1021/cg200768x
_journal_volume                  12
_journal_year                    2012
_chemical_formula_moiety         'C19 H15 F3 N4 O, H2 O'
_chemical_formula_sum            'C19 H17 F3 N4 O2'
_chemical_formula_weight         390.37
_chemical_name_systematic
;
1-Methyl-7-(methyloxy)-5-[4-(trifluoromethyl)phenyl]
[1,2,4]triazolo[4,3-a]quinolin-4-amine, monohydrate
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                102.09(4)
_cell_angle_beta                 102.70(5)
_cell_angle_gamma                94.86(8)
_cell_formula_units_Z            4
_cell_length_a                   8.473(6)
_cell_length_b                   12.542(7)
_cell_length_c                   17.476(9)
_cell_measurement_temperature    150(2)
_cell_volume                     1754.8(19)
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Nonius, 1997-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs, 1990-2000)'
_computing_molecular_graphics    'SHELXTL V6.10 [NT] (Bruker, 2001)'
_computing_publication_material  'SHELXTL V6.10 [NT] (Bruker, 2001)'
_computing_structure_refinement  'SHELXTL V6.10 [NT] (Bruker, 2001)'
_computing_structure_solution    'SHELXTL V6.10 [NT] (Bruker, 2001)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_collimation    '0.6 mm double-pinhole'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'normal focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0861
_diffrn_reflns_av_sigmaI/netI    0.0837
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22146
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         4.44
_exptl_absorpt_coefficient_mu    0.120
_exptl_absorpt_correction_T_max  0.986
_exptl_absorpt_correction_T_min  0.954
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.288
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       0.0052(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     538
_refine_ls_number_reflns         6097
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.1046
_refine_ls_R_factor_gt           0.0599
_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^)+(0.0749P)^2^+1.2629P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1431
_refine_ls_wR_factor_ref         0.1654
_reflns_number_gt                3967
_reflns_number_total             6097
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg200768x_si_002.cif
_cod_data_source_block           x4284i1
_cod_original_cell_volume        1754.8(18)
_cod_database_code               4502739