Independent Generation of C5'-Nucleosidyl Radicals in Thymidine and 2'-Deoxyguanosine
Antonio Manetto; Dimitris Georganakis; Leondios Leondiadis; Thanasis Gimisis; Peter Mayer; Thomas Carell; Chryssostomos Chatgilialoglu; Journal of Organic Chemistry 72 (2007) 3659–3666; doi:10.1021/jo062518c

data_4022814
_publ_contact_author_address
;
ISOF, Consiglio Nazionale delle Ricerche
Via P. Gobetti
40129 Bologna
Italy
;
_publ_contact_author_email       chrys@isof.cnr.it
_publ_contact_author_fax         '+39 051 639 8349'
_publ_contact_author_name        'Chryssostomos Chatgilialoglu'
_publ_section_title
;
 Independent Generation of C5'-Nucleosidyl Radicals
 in Thymidine and 2'-Deoxyguanosine
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              3659
_journal_page_last               3666
_journal_paper_doi               10.1021/jo062518c
_journal_volume                  72
_journal_year                    2007
_chemical_formula_moiety         'C23 H38 N2 O7 Si'
_chemical_formula_sum            'C23 H38 N2 O7 Si'
_chemical_formula_weight         482.643
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_author_name               'Mayer, P.'
_audit_block_code                C23H38N2O7Si_kn169_carell
_audit_creation_date             21-Apr-06
_audit_creation_method           'form98_non/compatible with shelxl97-2'
_audit_update_record             17-Aug-06
_cell_angle_alpha                90.00
_cell_angle_beta                 93.3188(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.1327(4)
_cell_length_b                   10.9042(3)
_cell_length_c                   17.7449(6)
_cell_measurement_reflns_used    5081
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      3.134
_cell_volume                     2730.01(14)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement
'SHELXL-97 (G. M. Sheldrick. University of G\"ottingen, 97-2 version)'
_computing_structure_solution
;
A. Altomare, M. C. Burla, M. Camalli, G. L. Cascarano, C. Giacovazzo, A.
Guagliardi, A. G. G. Moliterni, G. Polidori, R. Spagna: SIR97: a new tool for
crystal structure determination and refinement; J. Appl. Crystallogr. 1999,
32, 115-119.
;
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       phi/omega-scan
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.0679678
_diffrn_orient_matrix_UB_12      -0.0232128
_diffrn_orient_matrix_UB_13      0.0103358
_diffrn_orient_matrix_UB_21      0.0178766
_diffrn_orient_matrix_UB_22      0.0509454
_diffrn_orient_matrix_UB_23      -0.0438268
_diffrn_orient_matrix_UB_31      0.0091826
_diffrn_orient_matrix_UB_32      0.0726364
_diffrn_orient_matrix_UB_33      0.0340421
_diffrn_radiation_collimation    0.25
_diffrn_radiation_monochromator  'Montel graded multilayer x-ray optics'
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0624
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7119
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         3.17
_diffrn_source_current           55.00
_diffrn_source_power             3.025
_diffrn_source_type              'FR 591 generator'
_diffrn_source_voltage           55.00
_exptl_absorpt_coefficient_mu    0.127
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.17429(6)
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.763
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.1(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     593
_refine_ls_number_reflns         7119
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0839
_refine_ls_R_factor_gt           0.0621
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1088P)^2^+0.5517P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1636
_refine_ls_wR_factor_ref         0.1774
_reflns_number_gt                5632
_reflns_number_total             7119
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo062518csi20061215_053507.cif
_cod_data_source_block           kn169
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4022814