Concomitant Hydrate Polymorphism in the Precipitation of Sparfloxacin from Aqueous Solution
Llinàs, Antonio; Burley, Jonathan C.; Prior, Timothy J.; Glen, Robert C.; Goodman, Jonathan M.; Crystal Growth & Design 8 (2008) 114–; doi:10.1021/cg700908m

data_4503266
_publ_section_title
;
 Concomitant Hydrate Polymorphism in the Precipitation of Sparfloxacin
 from Aqueous Solution
;
_journal_issue                   1
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              114
_journal_paper_doi               10.1021/cg700908m
_journal_volume                  8
_journal_year                    2008
_chemical_formula_moiety         'C19 H22 F2 N4 O3, 3(H2 O)'
_chemical_formula_sum            'C19 H28 F2 N4 O6'
_chemical_formula_weight         446.45
_chemical_name_common            'Sparfloxamine trihydrate'
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 109.207(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.1250(13)
_cell_length_b                   10.3010(15)
_cell_length_c                   11.8890(17)
_cell_measurement_reflns_used    8341
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      39.975
_cell_measurement_theta_min      5.321
_cell_volume                     1055.3(3)
_computing_cell_refinement       'Bruker APEX2 v2.0-2'
_computing_data_collection       'Bruker APEX2 v2.0-2'
_computing_data_reduction        'Bruker APEX2 v2.0-2'
_computing_molecular_graphics    PLATON
_computing_publication_material  'vi (http://www.vim.org)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker D8 with APEX-2 area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'SRS Daresbury Station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.69040
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0510
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2016
_diffrn_reflns_theta_full        24.60
_diffrn_reflns_theta_max         24.60
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    0.116
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  .663
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2004/1 from Bruker Nonius was used for area detector scaling, absorption
correction, and to apply a correction for decay of the incident beam.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelopiped
_exptl_crystal_F_000             472
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.238
_refine_diff_density_min         -0.277
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.6(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         2016
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.0782
_refine_ls_R_factor_gt           0.0571
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1074P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1377
_refine_ls_wR_factor_ref         0.1511
_reflns_number_gt                1542
_reflns_number_total             2016
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg700908m-file003.cif
_cod_data_source_block           sparfloxacin_Synchrotron
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4503266