Two Anhydrous and a Trihydrate Form of Tilorone Dihydrochloride: Hydrogen-Bonding Patterns and Reversible Hydration/Dehydration Solid-State Transformation
Chernyshev, Vladimir V.; Yatsenko, Alexandr V.; Pirogov, Sergey V.; Nikulenkova, Tamara F.; Tumanova, Ekaterina V.; Lonin, Ivan S.; Paseshnichenko, Ksenia A.; Mironov, Andrei V.; Velikodny, Yurii A.; Crystal Growth & Design 12 (2012) 6118–; doi:10.1021/cg3012475

data_4507021
_publ_section_title
;
 Two Anhydrous and a Trihydrate Form of Tilorone Dihydrochloride:
 Hydrogen-Bonding Patterns and Reversible Hydration/Dehydration
 Solid-State Transformation
;
_journal_issue                   12
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              6118
_journal_paper_doi               10.1021/cg3012475
_journal_volume                  12
_journal_year                    2012
_chemical_formula_moiety         'C25 H36 N2 O3 2+, 2 (Cl -), 3 (H2 O)'
_chemical_formula_sum            'C25 H42 Cl2 N2 O6'
_chemical_formula_weight         537.51
_chemical_name_systematic
; 
2,7-Bis[2-(diethylamino)ethoxy]-9-fluorenone dihydrochloride  
trihydrate
;
_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'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.39(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.7102(19)
_cell_length_b                   13.3601(17)
_cell_length_c                   12.1598(16)
_cell_measurement_reflns_used    1737
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      39.98
_cell_measurement_theta_min      2.51
_cell_volume                     2859.3(6)
_computing_cell_refinement       'MRIA (Zlokazov & Chernyshev, 1992)'
_computing_data_collection
'<i>G670 Imaging Plate Guinier Camera Software</i> (Huber, 2002)'
_computing_data_reduction
'<i>G670 Imaging Plate Guinier Camera Software</i>'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'MRIA, SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  MRIA
_computing_structure_solution    'simulated annealing (Zhukov et al., 2001)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_type            'Imaging Plate'
_diffrn_measurement_device       'Guinier camera G670'
_diffrn_radiation_monochromator  'Curved Germanium (111)'
_diffrn_radiation_source         'line-focus sealed tube'
_diffrn_radiation_type           CuK\a~1~
_diffrn_radiation_wavelength     1.54059
_diffrn_source                   'Fine focus X-ray tube'
_diffrn_source_target            Cu
_exptl_absorpt_coefficient_mu    2.368
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.249
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1152
_pd_block_diffractogram_id       Form_IIIh_pattern
_pd_char_colour                  orange
_pd_char_particle_morphology     'no specific habit'
_pd_instr_location
;
Dept. of Chemistry, Moscow State University, 119991 Moscow, Russia
;
_pd_meas_2theta_range_inc        0.01
_pd_meas_2theta_range_max        80.00
_pd_meas_2theta_range_min        3.00
_pd_meas_number_of_points        7701
_pd_meas_scan_method             cont
_pd_prep_pressure                101
_pd_prep_temperature             298(2)
_pd_proc_2theta_range_inc        0.01
_pd_proc_2theta_range_max        80.00
_pd_proc_2theta_range_min        3.00
_pd_proc_info_excluded_regions   none
_pd_proc_ls_background_function  'Chebyshev polynomial up to the 5th order'
_pd_proc_ls_pref_orient_corr
;
March-Dollase (1986) texture correction
;
_pd_proc_ls_profile_function     'split-type pseudo-Voigt (Toraya, 1986)'
_pd_proc_ls_prof_R_factor        0.028
_pd_proc_ls_prof_wR_expected     0.020
_pd_proc_ls_prof_wR_factor       0.036
_pd_proc_wavelength              1.54059
_pd_spec_mounting
; 
thin layer in the specimen holder of the camera
;
_pd_spec_mount_mode              transmission
_pd_spec_shape                   flat_sheet
_pd_spec_size_axial              15
_pd_spec_size_equat              1
_pd_spec_size_thick              1
_refine_diff_density_max         0.52
_refine_diff_density_min         -0.36
_refine_diff_density_rms         0.27
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.695
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           fullcycle
_refine_ls_number_constraints    0
_refine_ls_number_parameters     172
_refine_ls_number_restraints     110
_refine_ls_R_I_factor            0.061
_refine_ls_shift/su_max          .003
_refine_ls_shift/su_mean         .001
_refine_ls_structure_factor_coef Inet
_refine_ls_weighting_scheme      sigma
_cod_data_source_file            cg3012475_si_001.cif
_cod_data_source_block           Tiloron_IIIh
_cod_original_cell_volume        2859.2(6)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4507021