2-Methyl-4-(4-methylpiperazin-1-yl)-10<i>H</i>-thieno[2,3-<i>b</i>][1,5]benzodiazepine methanol solvate monohydrate
Capuano, Ben; Crosby, Ian T.; Fallon, Gary D.; Lloyd, Edward J.; Yuriev, Elizabeth; Acta Crystallographica Section E 59 (2003) o1367–o1369; doi:10.1107/S1600536803017744

data_2202933
_publ_section_title
;2-Methyl-4-(4-methylpiperazin-1-yl)-10<i>H</i>-thieno[2,3-<i>b</i>][1,5]benzodiazepine
 methanol solvate monohydrate
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1367
_journal_page_last               o1369
_journal_paper_doi               10.1107/S1600536803017744
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          'C17 H20 N4 S, C H4 O, H2 O'
_chemical_formula_moiety         'C17 H20 N4 S, C H4 O, H2 O'
_chemical_formula_sum            'C18 H26 N4 O2 S'
_chemical_formula_weight         362.49
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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
_cell_angle_beta                 127.5820(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.3587(2)
_cell_length_b                   11.9729(2)
_cell_length_c                   15.6010(2)
_cell_measurement_reflns_used    21650
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      28.3
_cell_measurement_theta_min      2.6
_cell_volume                     3753.77(10)
_computing_cell_refinement       'HKL SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL DENZO (Otwinowski & Minor, 1997) and SCALEPACK'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method
'CCD rotation images in \f and \w, thick slices'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.041
_diffrn_reflns_av_sigmaI/netI    0.049
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20806
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         28.3
_diffrn_reflns_theta_min         2.6
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.192
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.40
_refine_diff_density_min         -0.32
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.03
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         4643
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.03
_refine_ls_R_factor_all          0.065
_refine_ls_R_factor_gt           0.044
_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^)+(0.0341P)^2^+3.6138P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.086
_refine_ls_wR_factor_ref         0.092
_reflns_number_gt                3683
_reflns_number_total             4643
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            tk6132.cif
_cod_data_source_block           I
_cod_original_cell_volume        3753.77(8)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2202933
_cod_database_fobs_code          2202933