Physical, Crystallographic, and Spectroscopic Characterization of a Crystalline Pharmaceutical Hydrate: Understanding the Role of Water
Vogt, Frederick G.; Brum, Jeffrey; Katrincic, Lee M.; Flach, Agnes; Socha, Jerome M.; Goodman, Richard M.; Haltiwanger, R. Curtis; Crystal Growth & Design 6 (2006) 2333–; doi:10.1021/cg060324k

data_4508811
_publ_section_title
;
 Physical, Crystallographic, and Spectroscopic Characterization of a
 Crystalline Pharmaceutical Hydrate:&#x2009; Understanding the Role of
 Water
;
_journal_issue                   10
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              2333
_journal_paper_doi               10.1021/cg060324k
_journal_volume                  6
_journal_year                    2006
_chemical_formula_sum            'C13 H15 Cl3 N3 Na O7 S'
_chemical_formula_weight         486.68
_chemical_melting_point          205
_chemical_name_systematic
; 
 Sodium N-(3-(aminosulfonyl)-4-chloro-2-hydroxyphenyl)-N'-
 (2,3-dichlorophenyl) urea trihydrate 
;
_space_group_IT_number           14
_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                 91.04(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.110(8)
_cell_length_b                   6.863(3)
_cell_length_c                   13.555(3)
_cell_measurement_temperature    173(2)
_cell_volume                     1870.5(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0566
_diffrn_reflns_av_sigmaI/netI    0.0626
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5306
_diffrn_reflns_theta_full        22.98
_diffrn_reflns_theta_max         22.98
_diffrn_reflns_theta_min         1.01
_exptl_absorpt_coefficient_mu    0.669
_exptl_absorpt_correction_T_max  0.9673
_exptl_absorpt_correction_T_min  0.6897
_exptl_crystal_density_diffrn    1.728
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.327
_refine_diff_density_min         -0.509
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.871
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         2607
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0729
_refine_ls_R_factor_gt           0.0372
_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^)+(0.0918P)^2^+4.2371P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1029
_refine_ls_wR_factor_ref         0.1352
_reflns_number_gt                1844
_reflns_number_total             2607
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg060324ksup1.cif
_cod_data_source_block           trihydrate
_cod_database_code               4508811