Thermal, X-ray Structural, and Dissolution Characteristics of Solid Forms Derived from the Anticancer Agents 2-Methoxyestradiol and 2-Methoxyestradiol-3,17-O,O-Bis-Sulfamate
Mino R. Caira; Susan A. Bourne; Halima Samsodien; Journal of Pharmaceutical Sciences 104 (2015) 3418–3425; doi:10.1002/jps.24545

data_1548358
_publ_section_title
;
 Thermal, X-ray Structural, and Dissolution Characteristics of Solid Forms
 Derived from the Anticancer Agents 2-Methoxyestradiol and
 2-Methoxyestradiol-3,17-O,O-Bis-Sulfamate
;
_journal_name_full               'Journal of Pharmaceutical Sciences'
_journal_page_first              3418
_journal_page_last               3425
_journal_paper_doi               10.1002/jps.24545
_journal_volume                  104
_journal_year                    2015
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C19 H26 O3, 2(C1 H1 Cl3)'
_chemical_formula_sum            'C21 H28 Cl6 O3'
_chemical_formula_weight         541.13
_chemical_name_common            '2-methoxyestradiol chloroform solvate 1:2'
_chemical_name_systematic
; 
 17beta-2-methoxyestra-1,3,5(10)-triene-3,17-diol chloroform solvate 1:2'
;
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                104.386(2)
_cell_angle_beta                 95.464(2)
_cell_angle_gamma                107.774(2)
_cell_formula_units_Z            1
_cell_length_a                   6.3150(2)
_cell_length_b                   9.3352(3)
_cell_length_c                   11.1622(5)
_cell_measurement_reflns_used    1639
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.02
_cell_measurement_theta_min      1.00
_cell_volume                     596.44(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean n/a
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Nonius Kappa CCD diffractometer'
_diffrn_measurement_method       'phi- and omega-scans'
_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  0.0347
_diffrn_reflns_av_sigmaI/netI    0.0393
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            17745
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         3.99
_diffrn_standards_decay_%        n/a
_diffrn_standards_interval_count n/a
_diffrn_standards_interval_time  n/a
_diffrn_standards_number         n/a
_exptl_absorpt_coefficient_mu    0.742
_exptl_absorpt_correction_T_max  0.8780
_exptl_absorpt_correction_T_min  0.6137
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             280
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.280
_refine_diff_density_min         -0.376
_refine_diff_density_rms         '0.055 '
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(4)
_refine_ls_extinction_coef       0.029(4)
_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   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     279
_refine_ls_number_reflns         5178
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0296
_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^)+(0.0386P)^2^+0.1166P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0682
_refine_ls_wR_factor_ref         0.0715
_reflns_number_gt                4690
_reflns_number_total             5178
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jps24545-sup-0001-S1.CIF
_cod_data_source_block           2meclors
_cod_depositor_comments
;
 Updating space group information.

 Antanas Vaitkus,
 2018-06-07
;
_cod_original_sg_symbol_H-M      P1
_cod_database_code               1548358