2-Hydroxy-11-methyl-16-[(<i>E</i>)-4-methylbenzylidene]-13-(4-methylphenyl)-1,11-diazapentacyclo[12.3.1.0^2,10^.0^3,8^.0^10,14^]octadeca-3(8),4,6-triene-9,15-dione
Kumar, Raju Suresh; Osman, Hasnah; Ali, Mohamed Ashraf; Yeap, Chin Sing; Fun, Hoong-Kun; Acta Crystallographica Section E 66 (2010) o2370–o2371; doi:10.1107/S1600536810033064

data_2227316
_publ_section_title
;
 2-Hydroxy-11-methyl-16-[(<i>E</i>)-4-methylbenzylidene]-13-(4-methylphenyl)-1,11-diazapentacyclo[12.3.1.0^2,10^.0^3,8^.0^10,14^]octadeca-3(8),4,6-triene-9,15-dione
;
_journal_coeditor_code           CI5154
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2370
_journal_page_last               o2371
_journal_paper_doi               10.1107/S1600536810033064
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C32 H30 N2 O3'
_chemical_formula_moiety         'C32 H30 N2 O3'
_chemical_formula_sum            'C32 H30 N2 O3'
_chemical_formula_weight         490.58
_chemical_name_systematic
;
2-Hydroxy-11-methyl-16-[(<i>E</i>)-4-methylbenzylidene]-13-(4-methylphenyl)-
1,11-diazapentacyclo[12.3.1.0^2,10^.0^3,8^.0^10,14^]octadeca-3(8),4,6-triene-
9,15-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                67.480(2)
_cell_angle_beta                 86.093(2)
_cell_angle_gamma                69.475(2)
_cell_formula_units_Z            2
_cell_length_a                   9.3252(6)
_cell_length_b                   12.1781(8)
_cell_length_c                   12.9821(8)
_cell_measurement_reflns_used    9995
_cell_measurement_temperature    100
_cell_measurement_theta_max      67.75
_cell_measurement_theta_min      5.75
_cell_volume                     1271.68(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
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'Bruker APEXII DUO CCD area-detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_av_sigmaI/netI    0.0226
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13699
_diffrn_reflns_theta_full        64.99
_diffrn_reflns_theta_max         64.99
_diffrn_reflns_theta_min         6.05
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.653
_exptl_absorpt_correction_T_max  0.8511
_exptl_absorpt_correction_T_min  0.7127
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Bruker, 2009)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.317
_refine_diff_density_min         -0.396
_refine_ls_extinction_coef       0.069(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXTL (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.205
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         4121
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.205
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0444
_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^)+(0.0743P)^2^+0.3694P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1232
_refine_ls_wR_factor_ref         0.1338
_reflns_number_gt                4004
_reflns_number_total             4121
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ci5154.cif
_cod_data_source_block           I
_cod_database_code               2227316
_cod_database_fobs_code          2227316