Tricyclanos: conformationally constrained nucleoside analogues with a new heterotricycle obtained from a d-ribofuranose unit.
Kicsák, Máté; Mándi, Attila; Varga, Szabolcs; Herczeg, Mihály; Batta, Gyula; Bényei, Attila; Borbás, Anikó; Herczegh, Pál; Organic & biomolecular chemistry 16 (2018) 393–401; doi:10.1039/c7ob02296d

data_7155930
_publ_section_title
;
 Tricyclanos: conformationally constrained nucleoside analogues with a new
 heterotricycle obtained from a d-ribofuranose unit.
;
_journal_issue                   3
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              393
_journal_page_last               401
_journal_paper_doi               10.1039/c7ob02296d
_journal_volume                  16
_journal_year                    2018
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C35  H33  N5  O7, C3 H8 O1'
_chemical_formula_sum            'C38 H41 N5 O8'
_chemical_formula_weight         695.75
_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'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-08-20T15:52:18-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2017-08-28 deposited with the CCDC.
2017-10-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.8476(3)
_cell_length_b                   17.3220(4)
_cell_length_c                   37.2345(9)
_cell_measurement_reflns_used    10049
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      76.946
_cell_measurement_theta_min      4.215
_cell_volume                     6996.4(3)
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Synergy, Dualflex, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0563
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            43348
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 0.97
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.221
_diffrn_reflns_theta_min         4.245
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.771
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.62257
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro 1.171.39.6a (Rigaku Oxford Diffraction, 2015)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2944
_exptl_crystal_size_max          0.112
_exptl_crystal_size_mid          0.029
_exptl_crystal_size_min          0.018
_refine_diff_density_max         0.643
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details
;
 Flack x determined using 4034 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.03(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     933
_refine_ls_number_reflns         14689
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0862
_refine_ls_R_factor_gt           0.0669
_refine_ls_shift/su_max          0.067
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0997P)^2^+2.3782P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1861
_reflns_number_gt                11384
_reflns_number_total             14689
_reflns_threshold_expression     'I > 2\s(I)'
_publcif_datablock.id            {4e2d3392-8d40-4e69-b307-088a64c6c2a0}
_cod_data_source_file            c7ob02296d2.cif
_cod_data_source_block           18b
_cod_depositor_comments
;

2018-02-16
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel

 Adding full bibliography for 7155930.cif.
;
_cod_original_formula_moiety     '2(C35  H33  N5  O7), 2(C3 H8 O1)'
_cod_original_formula_sum        'C76 H82 N10 O16'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     1391.51
_cod_database_code               7155930
_publcif_funding_html
;
;