5,7-Diacetyl-13-benzyl-7,8-dihydro-5<i>H</i>,8a<i>H</i>,13<i>H</i>-diindolo[2,3-<i>c</i>;2,3-<i>d</i>]pyrimidin-8-yl acetate, the result of an intramolecular cycloaddition between an <i>N</i>-benzylindole and a 1,2,4,5-tetrazine
Madeleine Helliwell; Steven Corden; John A. Joule; Acta Crystallographica Section E 63 (2007) o1993–o1995; doi:10.1107/S1600536807011166

data_2212996
_publ_section_title
;5,7-Diacetyl-13-benzyl-7,8-dihydro-5<i>H</i>,8a<i>H</i>,13<i>H</i>-diindolo[2,3-<i>c</i>;2,3-<i>d</i>]pyrimidin-8-yl
 acetate, the result of an intramolecular cycloaddition between an
 <i>N</i>-benzylindole and a 1,2,4,5-tetrazine
;
_journal_coeditor_code           SG2145
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1993
_journal_page_last               o1995
_journal_paper_doi               10.1107/S1600536807011166
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C29 H26 N4 O4'
_chemical_formula_moiety         'C29 H26 N4 O4'
_chemical_formula_sum            'C29 H26 N4 O4'
_chemical_formula_weight         494.54
_chemical_name_systematic
;
5,7-diacetyl-13-benzyl-7,8-dihydro-5H,8aH,13H-diindolo[2,3-c;2,3-d]pyrimidin-
8-yl acetate
;
_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
_cell_angle_alpha                109.371(2)
_cell_angle_beta                 95.624(2)
_cell_angle_gamma                93.782(2)
_cell_formula_units_Z            2
_cell_length_a                   9.8170(12)
_cell_length_b                   11.2404(14)
_cell_length_c                   11.5762(14)
_cell_measurement_reflns_used    2177
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.00
_cell_measurement_theta_min      2.19
_cell_volume                     1192.7(3)
_computing_cell_refinement       SMART
_computing_data_collection
'SMART [PLEASE PROVIDE YEAR/VERSION NUMBER/REFERENCE]'
_computing_data_reduction
'SAINT [PLEASE PROVIDE YEAR/VERSION NUMBER/REFERENCE]'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution
'SHELXTL [PLEASE PROVIDE YEAR/VERSION NUMBER/REFERENCE]'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.889
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.0200
_diffrn_reflns_av_sigmaI/netI    0.0452
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7514
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_T_max  0.9907
_exptl_absorpt_correction_T_min  0.9460
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.415
_refine_diff_density_min         -0.233
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         5269
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0452
_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^)+(0.0523P)^2^+0.4497P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1065
_refine_ls_wR_factor_ref         0.1154
_reflns_number_gt                4159
_reflns_number_total             5269
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sg2145.cif
_cod_data_source_block           3
_cod_database_code               2212996
_cod_database_fobs_code          2212996