Synthesis and crystal structure of <i>anti</i>-10-butyl-10,11,22,23-tetrahydro-9<i>H</i>,21<i>H</i>-5,8:15,12-bis(metheno)[1,5,11]triazacyclohexadecino[1,16-<i>a</i>:5,6-<i>a</i>']diindole
Kubono, Koji; Tani, Keita; Kashiwagi, Yukiyasu; Tani, Fumito; Matsumoto, Taisuke; Acta Crystallographica Section E 78 (2022) –; doi:10.1107/S2056989022003383

data_2244067
_publ_section_title
;
 Synthesis and crystal structure of
 <i>anti</i>-10-butyl-10,11,22,23-tetrahydro-9<i>H</i>,21<i>H</i>-5,8:15,12-bis(metheno)[1,5,11]triazacyclohexadecino[1,16-<i>a</i>:5,6-<i>a</i>']diindole
;
_journal_coeditor_code           YK2167
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2056989022003383
_journal_volume                  78
_journal_year                    2022
_chemical_formula_iupac          'C33 H33 N3'
_chemical_formula_moiety         'C33 H33 N3'
_chemical_formula_sum            'C33 H33 N3'
_chemical_formula_weight         471.64
_chemical_name_systematic
<i>anti</i>-10-Butyl-10,11,22,23-tetrahydro-9<i>H</i>,21<i>H</i>-5,8:15,12-bis(metheno)[1,5,11]triazacyclohexadecino[1,16-<i>a</i>:5,6-<i>a</i>']diindole
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                79.988(3)
_cell_angle_beta                 77.717(3)
_cell_angle_gamma                77.909(3)
_cell_formula_units_Z            2
_cell_length_a                   7.9106(3)
_cell_length_b                   10.4468(4)
_cell_length_c                   15.5735(5)
_cell_measurement_reflns_used    9429
_cell_measurement_temperature    100
_cell_measurement_theta_max      74.84
_cell_measurement_theta_min      2.85
_cell_volume                     1218.33(8)
_computing_cell_refinement
;
CrysAlisPro (Rigaku OD, 2022)
;
_computing_data_collection
;
CrysAlisPro (Rigaku OD, 2022)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku OD, 2022)
;
_computing_molecular_graphics
;
CrystalStructure (Rigaku, 2019)
;
_computing_publication_material
;
CrystalStructure (Rigaku, 2019)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
<i>SHELXT2018/2</i> (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14067
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.411
_diffrn_reflns_theta_min         2.931
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.576
_exptl_absorpt_correction_T_max  0.972
_exptl_absorpt_correction_T_min  0.451
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2022)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             504.00
_exptl_crystal_size_max          0.403
_exptl_crystal_size_mid          0.128
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.48
_refine_diff_density_min         -0.31
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     326
_refine_ls_number_reflns         4827
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0442
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0570P)^2^+0.6261P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1148
_refine_ls_wR_factor_ref         0.1180
_reflns_number_gt                4383
_reflns_number_total             4827
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            yk2167sup1.cif
_cod_data_source_block           I
_cod_database_code               2244067
_shelx_hkl_checksum              94319
_shelx_res_checksum              81960
_cod_database_fobs_code 2244067