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_7153826
_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 ad
_chemical_formula_moiety
'C48 H38 N11 O3 Ru, C48 H37 N11 O3 Ru, 4(F6 P)'
_chemical_formula_sum            'C48 H39 F12 N11 O3 P2 Ru'
_chemical_formula_weight         1208.90
_chemical_name_common
;
8((1'',10'''-phenantroline-2''-yl)phenyl-(bis (2,2')-
bipyridine)ruthenium)-2'-deoxyadenosine-dihexafluorophosphate
;
_chemical_name_systematic
;8{(1'',10'''-phenantroline-2''-yl)phenyl-(bis
[2,2']-bipyridine)ruthenium}-2'-deoxyadenosine-
dihexafluorophosphate
;
_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                89.02(3)
_cell_angle_beta                 71.32(3)
_cell_angle_gamma                89.82(4)
_cell_formula_units_Z            2
_cell_length_a                   13.291(5)
_cell_length_b                   13.669(5)
_cell_length_c                   16.242(5)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    150
_cell_measurement_theta_max      77
_cell_measurement_theta_min      4
_cell_volume                     2794.9(18)
_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 0.995
_diffrn_measured_fraction_theta_max 0.973
_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  0.059
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21182
_diffrn_reflns_theta_full        71.196
_diffrn_reflns_theta_max         78.237
_diffrn_reflns_theta_min         3.758
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.606
_exptl_absorpt_correction_T_max  0.52
_exptl_absorpt_correction_T_min  0.36
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
Analytical Absorption (De Meulenaer & Tompa, 1965)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_description       prism
_exptl_crystal_F_000             1217
_exptl_crystal_size_max          0.71
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.18
_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         1.87
_refine_diff_density_min         -0.95
_refine_ls_abs_structure_details 'Flack (1983), 18175 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.014(3)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1358
_refine_ls_number_reflns         14870
_refine_ls_number_restraints     25
_refine_ls_R_factor_all          0.0727
_refine_ls_R_factor_gt           0.0585
_refine_ls_shift/su_max          0.022687
_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:
26.0 -9.77 22.3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0778
_refine_ls_wR_factor_gt          0.0689
_refine_ls_wR_factor_ref         0.0689
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              17
_reflns_limit_k_min              -15
_reflns_limit_l_max              20
_reflns_limit_l_min              -20
_reflns_number_gt                14870
_reflns_number_total             21182
_reflns_threshold_expression     I>2.0\s(I)
_cod_data_source_file            b709245h.txt
_cod_data_source_block           13c
_cod_database_code               7153826
_cod_duplicate_entry 7151161