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_7159163
_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         'C46 H43 N8 O2 . C H2 Cl2'
_chemical_formula_sum            'C46 H45 Cl2 N9 O2'
_chemical_formula_weight         826.81
_chemical_name_common            'Borbasa 725'
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_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                72.678(3)
_cell_angle_beta                 89.071(3)
_cell_angle_gamma                76.638(3)
_cell_formula_units_Z            1
_cell_length_a                   9.2221(5)
_cell_length_b                   9.3018(6)
_cell_length_c                   13.1569(8)
_cell_measurement_reflns_used    5920
_cell_measurement_temperature    150.(2)
_cell_measurement_theta_max      26.0210
_cell_measurement_theta_min      2.4278
_cell_volume                     1046.59(11)
_computing_cell_refinement       'APEX3 v2017.3-0 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service vV6.2.6'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 1365)'
_computing_publication_material  'WinGX, PublCIF'
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Bruker D8 Venture'
_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  0.0788
_diffrn_reflns_av_unetI/netI     0.0763
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            26632
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         26.09
_diffrn_reflns_theta_min         2.27
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'INCOATEC I\mS 3.0'
_exptl_absorpt_coefficient_mu    0.206
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.95
_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    1.312
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             434
_exptl_crystal_size_max          0.269
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.169
_refine_diff_density_max         0.493
_refine_diff_density_min         -0.691
_refine_ls_abs_structure_details
;

Flack x determined using 2515 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.06(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     535
_refine_ls_number_reflns         8263
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.0622
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1016P)^2^+0.3520P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1590
_refine_ls_wR_factor_ref         0.1868
_reflns_Friedel_coverage         0.992
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                6360
_reflns_number_total             8263
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ob00154g2.cif
_cod_data_source_block           31
_cod_depositor_comments
'Adding full bibliography for 7159162--7159165.cif.'
_cod_database_code               7159163
_shelx_res_checksum              74201