<i>rac</i>-(6<i>S</i>)-6-Hydroxy-6-{2-[2-(propan-2-ylidene)hydrazinylidene]propyl}indolo[2,1-<i>b</i>]quinazolin-12(6<i>H</i>)-one
Rodstein, Matthew E.; Steffen, Paul D.; Krivogorsky, Bogdana; Grundt, Peter; Acta Crystallographica Section E 67 (2011) o2695–o2696; doi:10.1107/S1600536811037408

data_2231970
_publ_section_title
;
 <i>rac</i>-(6<i>S</i>)-6-Hydroxy-6-{2-[2-(propan-2-ylidene)hydrazinylidene]propyl}indolo[2,1-<i>b</i>]quinazolin-12(6<i>H</i>)-one
;
_journal_coeditor_code           LD2027
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2695
_journal_page_last               o2696
_journal_paper_doi               10.1107/S1600536811037408
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C21 H20 N4 O2'
_chemical_formula_moiety         'C21 H20 N4 O2'
_chemical_formula_sum            'C21 H20 N4 O2'
_chemical_formula_weight         360.42
_chemical_name_systematic
;
<i>rac</i>-(6<i>S</i>)-6-Hydroxy-6-{2-[2-(propan-2-
ylidene)hydrazinylidene]propyl}indolo[2,1-<i>b</i>]quinazolin-12(6<i>H</i>)-one
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 99.58(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.6788(17)
_cell_length_b                   15.117(3)
_cell_length_c                   13.283(3)
_cell_measurement_reflns_used    1820
_cell_measurement_temperature    100
_cell_measurement_theta_max      2
_cell_measurement_theta_min      25
_cell_volume                     1718.4(6)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'CrystalClear (Rigaku Americas, 2009)'
_computing_data_reduction        'CrystalClear (Rigaku Americas, 2009)'
_computing_molecular_graphics    'CAMERON (Watkin <i>et al.</i>, 1996)'
_computing_publication_material  'CRYSTALS (Betteridge <i>et al.</i>, 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge <i>et al.</i>, 2003)'
_computing_structure_solution
;
CrystalStructure (Rigaku Americas, 2009) and
SIR2004 (Burla <i>et al.</i>, 2005)
;
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'image plate'
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID II image-plate'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Mo Sealed tube tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.096
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11165
_diffrn_reflns_theta_full        24.711
_diffrn_reflns_theta_max         24.711
_diffrn_reflns_theta_min         3.053
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.98
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.59
_refine_diff_density_min         -0.48
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0129
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_constraints    13
_refine_ls_number_parameters     244
_refine_ls_number_reflns         2899
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0980
_refine_ls_R_factor_gt           0.0624
_refine_ls_shift/su_max          0.0001471
_refine_ls_shift/su_mean         0.0000159
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial,(Watkin, 1994; Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
5.56 6.74 1.72
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1605
_refine_ls_wR_factor_gt          0.1284
_refine_ls_wR_factor_ref         0.1605
_reflns_number_gt                1850
_reflns_number_total             2914
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ld2027.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2231970
_cod_database_fobs_code          2231970