5-[(<i>E</i>)-Benzylidene]-2-hydroxy-10-methyl-8-phenyl-3,10-diazahexacyclo[10.7.1.1^3,7^.0^2,11^.0^7,11^.0^16,20^]henicosa-1(19),12(20),13,15,17-pentaen-6-one ethanol 0.25-solvate 0.6-hydrate
Kumar, Raju Suresh; Osman, Hasnah; Perumal, Subbu; Hemamalini, Madhukar; Fun, Hoong-Kun; Acta Crystallographica Section E 66 (2010) o2736–o2737; doi:10.1107/S1600536810039310

data_2227526
_publ_section_title
;
 5-[(<i>E</i>)-Benzylidene]-2-hydroxy-10-methyl-8-phenyl-3,10-diazahexacyclo[10.7.1.1^3,7^.0^2,11^.0^7,11^.0^16,20^]henicosa-1(19),12(20),13,15,17-pentaen-6-one
 ethanol 0.25-solvate 0.6-hydrate
;
_journal_coeditor_code           HB5631
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2736
_journal_page_last               o2737
_journal_paper_doi               10.1107/S1600536810039310
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C33 H28 N2 O2, 0.25C2 H6 O, 0.6H2 O'
_chemical_formula_moiety         'C33 H28 N2 O2, 0.25(C2 H6 O), 0.6(H2 O)'
_chemical_formula_sum            'C33.5 H30.7 N2 O2.85'
_chemical_formula_weight         506.90
_chemical_name_systematic
;
5-[(<i>E</i>)-Benzylidene]-2-hydroxy-10-methyl-8-phenyl-3,10-
diazahexacyclo[10.7.1.1^3,7^.0^2,11^.0^7,11^.0^16,20^]henicosa-
1(19),12(20),13,15,17-pentaen-6-one ethanol 0.25-solvate 0.6-hydrate
;
_space_group_IT_number           114
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4 2n'
_symmetry_space_group_name_H-M   'P -4 21 c'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.3839(3)
_cell_length_b                   19.3839(3)
_cell_length_c                   14.0757(2)
_cell_measurement_reflns_used    5795
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.88
_cell_measurement_theta_min      2.55
_cell_volume                     5288.74(14)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD'
_diffrn_measurement_method       '\f and \w 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  0.0410
_diffrn_reflns_av_sigmaI/netI    0.0366
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23186
_diffrn_reflns_theta_full        30.05
_diffrn_reflns_theta_max         30.05
_diffrn_reflns_theta_min         1.49
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_T_max  0.9878
_exptl_absorpt_correction_T_min  0.9849
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2009)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2148
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.212
_refine_ls_abs_structure_details none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         4230
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0579
_refine_ls_shift/su_max_lt       0.001
_refine_ls_shift/su_mean         <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0762P)^2^+1.6944P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1369
_refine_ls_wR_factor_ref         0.1476
_reflns_number_gt                3388
_reflns_number_total             4230
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb5631.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C33.50 H30.70 N2 O2.85'
_cod_database_code               2227526
_cod_database_fobs_code          2227526