A conformationally locked tricyclic nucleoside. Synthesis, crystal structure and incorporation into oligonucleotides
Ravn, Jacob; Thorup, Niels; Nielsen, Poul; Journal of the Chemical Society, Perkin Transactions 1  (2001) 1855–; doi:10.1039/b104438a

data_7213494
_publ_section_title
;
 A conformationally locked tricyclic nucleoside. Synthesis, crystal
 structure and incorporation into oligonucleotides
;
_journal_issue                   16
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 1'
_journal_page_first              1855
_journal_paper_doi               10.1039/b104438a
_journal_year                    2001
_chemical_formula_moiety         '(C12 H14 N2 O7), 2(H2 O1)'
_chemical_formula_sum            'C12 H18 N2 O9'
_chemical_formula_weight         334.28
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'manual editing of SHELXL-97 cif'
_cell_angle_alpha                90.00
_cell_angle_beta                 98.416(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.555(3)
_cell_length_b                   8.5576(11)
_cell_length_c                   6.7140(8)
_cell_measurement_reflns_used    964
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.44
_cell_measurement_theta_min      2.52
_cell_volume                     1395.6(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.921
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_device_type  'Siemens/Bruker SMART 1K)'
_diffrn_measurement_method       'omega scan, frame data integration'
_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  0.0145
_diffrn_reflns_av_sigmaI/netI    0.0157
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            8619
_diffrn_reflns_theta_full        29.79
_diffrn_reflns_theta_max         29.79
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    0.138
_exptl_absorpt_correction_T_max  0.9743
_exptl_absorpt_correction_T_min  0.9406
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2000)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.232
_refine_diff_density_min         -0.225
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.2(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         3464
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0270
_refine_ls_R_factor_gt           0.0262
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0510P)^2^+0.1632P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0685
_refine_ls_wR_factor_ref         0.0690
_reflns_number_gt                3370
_reflns_number_total             3464
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b104438asup1.cif
_cod_data_source_block           pn2ak
_cod_database_code               7213494