16-[(<i>E</i>)-Benzylidene]-13-hydroxy-4-methyl-2-phenyl-4,14-diazapentacyclo-[12.3.1.0^1,5^.0^5,13^.0^7,12^]octadeca-7(12),8,10-triene-6,17-dione
Kumar, Raju Suresh; Osman, Hasnah; Ali, Mohamed Ashraf; Quah, Ching Kheng; Fun, Hoong-Kun; Acta Crystallographica Section E 66 (2010) o1540–o1541; doi:10.1107/S1600536810020271

data_2226649
_publ_section_title
;
 16-[(<i>E</i>)-Benzylidene]-13-hydroxy-4-methyl-2-phenyl-4,14-diazapentacyclo-[12.3.1.0^1,5^.0^5,13^.0^7,12^]octadeca-7(12),8,10-triene-6,17-dione
;
_journal_coeditor_code           RZ2455
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1540
_journal_page_last               o1541
_journal_paper_doi               10.1107/S1600536810020271
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C30 H26 N2 O3'
_chemical_formula_moiety         'C30 H26 N2 O3'
_chemical_formula_sum            'C30 H26 N2 O3'
_chemical_formula_weight         462.53
_chemical_name_systematic
;16-[(<i>E</i>)-Benzylidene]-13-hydroxy-4-methyl-2-phenyl-4,14-
diazapentacyclo-[12.3.1.0^1,5^.0^5,13^.0^7,12^]octadeca-
7(12),8,10-triene-6,17-dione
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                80.943(2)
_cell_angle_beta                 78.0340(10)
_cell_angle_gamma                80.5780(10)
_cell_formula_units_Z            2
_cell_length_a                   9.0333(5)
_cell_length_b                   9.4222(5)
_cell_length_c                   14.0290(7)
_cell_measurement_reflns_used    9987
_cell_measurement_temperature    100
_cell_measurement_theta_max      35.79
_cell_measurement_theta_min      2.82
_cell_volume                     1142.88(10)
_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
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type
;
Bruker APEXII DUO CCD area-detector diffractometer
;
_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  0.0257
_diffrn_reflns_av_sigmaI/netI    0.0188
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21768
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_T_max  0.9910
_exptl_absorpt_correction_T_min  0.9569
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Bruker, 2009)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.394
_exptl_crystal_size_min          0.104
_refine_diff_density_max         0.579
_refine_diff_density_min         -0.287
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         4213
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0429
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_max_lt       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^)+(0.0728P)^2^+0.7251P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1235
_refine_ls_wR_factor_ref         0.1296
_reflns_number_gt                3812
_reflns_number_total             4213
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            rz2455.cif
_cod_data_source_block           I
_cod_database_code               2226649
_cod_database_fobs_code          2226649