Synthesis of 2'-deoxyadenosine nucleosides bearing bipyridine-type ligands and their Ru-complexes in position 8 through cross-coupling reactions.
Vrábel, Milan; Pohl, Radek; Klepetárová, Blanka; Votruba, Ivan; Hocek, Michal; Organic & biomolecular chemistry 5 (2007) 2849–2857; doi:10.1039/b709245h

data_7151160
_publ_section_title
;
 Synthesis of 2'-deoxyadenosine nucleosides bearing bipyridine-type
 ligands and their Ru-complexes in position 8 through cross-coupling
 reactions.
;
_journal_issue                   17
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              2849
_journal_page_last               2857
_journal_paper_doi               10.1039/b709245h
_journal_volume                  5
_journal_year                    2007
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C28 H23 N7 O3, C28 H22 N7 O3'
_chemical_formula_sum            'C28 H23 N7 O3'
_chemical_formula_weight         505.53
_chemical_name_common
8-((1'',10'''-phenantroline-2''-yl)phenyl)-2'-deoxyadenosine
_chemical_name_systematic
8-[(1'',10'''-phenantroline-2''-yl]phenyl]-2'-deoxyadenosine
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      1
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             07-06-15
_audit_creation_method           CRYSTALS_ver_12.84
_cell_angle_alpha                96.79(3)
_cell_angle_beta                 106.00(3)
_cell_angle_gamma                105.90(3)
_cell_formula_units_Z            2
_cell_length_a                   10.790(4)
_cell_length_b                   10.800(3)
_cell_length_c                   13.163(4)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    150
_cell_measurement_theta_max      77
_cell_measurement_theta_min      4
_cell_volume                     1386.6(9)
_computing_cell_refinement       'CrysAlis RED, (Oxford Diffraction, 2002)'
_computing_data_collection       'Xcalibur, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis RED, (Oxford Diffraction, 2002)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Oxford Diffraction XCALIBUR'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.056
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5801
_diffrn_reflns_theta_full        71.623
_diffrn_reflns_theta_max         77.851
_diffrn_reflns_theta_min         4.353
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.671
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_correction_T_min  0.88
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
Analytical Absorption (De Meulenaer & Tompa, 1965)
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_description       prism
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_exptl_crystal_size_max          0.63
_exptl_crystal_size_mid          0.19
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_platon_squeeze_details
;
The methanol solvent molecules were not modelled and the disordered
density was taken into account using the SQUEEZE/PLATON procedure.
;
_refine_diff_density_max         0.43
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_refine_ls_extinction_method     None
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     685
_refine_ls_number_reflns         2973
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0894
_refine_ls_R_factor_gt           0.0576
_refine_ls_shift/su_max          0.003747
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
17.3 5.05 15.0
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0920
_refine_ls_wR_factor_gt          0.0712
_refine_ls_wR_factor_ref         0.0712
_reflns_limit_h_max              12
_reflns_limit_h_min              -13
_reflns_limit_k_max              13
_reflns_limit_k_min              -13
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                2973
_reflns_number_total             5801
_reflns_threshold_expression     I>2.0\s(I)
_cod_data_source_file            b709245h.txt
_cod_data_source_block           9c
_cod_original_cell_volume        1386.5(9)
_cod_database_code               7151160