Triaza-tricyclanos - synthesis of a new class of tricyclic nucleoside analogues by stereoselective cascade cyclocondensation.
Bege, Miklós; Herczeg, Mihály; Bereczki, Ilona; Debreczeni, Nóra; Bényei, Attila; Herczegh, Pál; Borbás, Anikó; Organic & biomolecular chemistry 21 (2023) 2213–2219; doi:10.1039/d3ob00154g

data_7159164
_publ_section_title
;
 Triaza-tricyclanos - synthesis of a new class of tricyclic nucleoside
 analogues by stereoselective cascade cyclocondensation.
;
_journal_issue                   10
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              2213
_journal_page_last               2219
_journal_paper_doi               10.1039/d3ob00154g
_journal_volume                  21
_journal_year                    2023
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C27 H30 N8 O2'
_chemical_formula_sum            'C27 H30 N8 O2'
_chemical_formula_weight         498.59
_chemical_name_common            'Borbasa ERJ750'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2023-01-13 deposited with the CCDC.	2023-02-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.2246(3)
_cell_length_b                   14.0455(7)
_cell_length_c                   24.2928(11)
_cell_measurement_reflns_used    123
_cell_measurement_temperature    291.(2)
_cell_measurement_theta_max      22.4517
_cell_measurement_theta_min      3.1791
_cell_volume                     2465.1(2)
_computing_cell_refinement       'APEX3 v2019.11-0 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service vV6.2.6'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_molecular_graphics    Mercury
_computing_publication_material  'WinGX, PublCIF'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      291.(2)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Bruker APEX-II CCD'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\w and \p scan'
_diffrn_radiation_monochromator  'multilayer mirror INCOATEC'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           ' Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0583
_diffrn_reflns_av_unetI/netI     0.0436
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            23730
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         26.04
_diffrn_reflns_theta_min         2.22
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'INCOATEC I\mS 3.0'
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.405
_exptl_crystal_size_mid          0.283
_exptl_crystal_size_min          0.084
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.371
_refine_ls_abs_structure_details
;

Flack x determined using 1615 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.3(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.151
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         4840
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.151
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0455
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0723P)^2^+0.1787P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1206
_refine_ls_wR_factor_ref         0.1299
_reflns_Friedel_coverage         0.744
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                4326
_reflns_number_total             4840
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ob00154g2.cif
_cod_data_source_block           33
_cod_depositor_comments
'Adding full bibliography for 7159162--7159165.cif.'
_cod_database_code               7159164
_publcif_datablock.id            {39f6acfa-fb16-4660-a28f-ec63ea8b564e}
_shelx_res_checksum              51899
_publcif_funding_html
;
;