Methyl 9-hydroxy-15-methyl-2-oxo-11-(pyren-1-yl)-10-oxa-15-azatetracyclo[7.6.0.0^1,12^.0^3,8^]pentadeca-3(8),4,6-triene-12-carboxylate
Sharmila, P.; Jagadeesan, G.; Raju, Rajesh; Raghavachary, Raghunathan; Aravindhan, S.; Acta Crystallographica Section E 69 (2013) o1569–; doi:10.1107/S1600536813024951

data_2238600
_publ_section_title
;
 Methyl
 9-hydroxy-15-methyl-2-oxo-11-(pyren-1-yl)-10-oxa-15-azatetracyclo[7.6.0.0^1,12^.0^3,8^]pentadeca-3(8),4,6-triene-12-carboxylate
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1569
_journal_paper_doi               10.1107/S1600536813024951
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C32 H25 N O5'
_chemical_formula_moiety         'C32 H25 N O5'
_chemical_formula_sum            'C32 H25 N O5'
_chemical_formula_weight         503.53
_chemical_name_common
'Methyl 9-hydroxy-15-methyl-2-oxo-11-(pyren-1-yl)-10-oxa-15-azatetracyclo[7.6.0.0^1,12^.0^3,8^]pentadeca-3(8),4,6-triene-12-carboxylate'
_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                90.00
_cell_angle_beta                 96.5030(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   31.6964(6)
_cell_length_b                   11.0325(2)
_cell_length_c                   14.1965(3)
_cell_measurement_reflns_used    8834
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.20
_cell_measurement_theta_min      2.05
_cell_volume                     4932.44(17)
_computing_cell_refinement       'APEX2 and SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT and XPREP (Bruker, 2004)'
_computing_molecular_graphics    '<i>ORTEP-3 for Windows</i> (Farrugia, 2012)'
_computing_publication_material  '<i>PLATON</i> (Spek, 2009)'
_computing_structure_refinement  '<i>SHELXL97</i> (Sheldrick, 2008)'
_computing_structure_solution    '<i>SHELXS97</i> (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Kappa APEXII CCD'
_diffrn_measurement_method       '\w and \f scan'
_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  0.0312
_diffrn_reflns_av_sigmaI/netI    0.0295
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20953
_diffrn_reflns_theta_full        25.66
_diffrn_reflns_theta_max         25.66
_diffrn_reflns_theta_min         1.96
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.092
_exptl_absorpt_correction_T_max  0.9831
_exptl_absorpt_correction_T_min  0.9790
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.150
_refine_diff_density_min         -0.177
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         4661
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0413
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0547P)^2^+1.5070P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1013
_refine_ls_wR_factor_ref         0.1142
_reflns_number_gt                3280
_reflns_number_total             4661
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt6925.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2238600