Synthesis and characterization of the 5-methyl-2′-deoxycytidine glycol‒dioxoosmium‒bipyridine ternary complex in DNA
Umemoto, Tadashi; Okamoto, Akimitsu; Organic & Biomolecular Chemistry 6 (2008) 269–271; doi:10.1039/b716400a

data_7150828
_publ_section_title
;
 Synthesis and characterization of the 5-methyl-2&#x2032;-deoxycytidine
 glycol--dioxoosmium--bipyridine ternary complex in DNA
;
_journal_issue                   2
_journal_name_full               'Organic &amp;  Biomolecular Chemistry'
_journal_page_first              269
_journal_page_last               271
_journal_paper_doi               10.1039/b716400a
_journal_volume                  6
_journal_year                    2008
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C20 H22 N4 O9 Os, 4(H2 O)'
_chemical_formula_sum            'C20 H30 N4 O13 Os'
_chemical_formula_weight         724.68
_chemical_name_systematic
;
?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.2644(18)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.4747(13)
_cell_length_b                   6.7238(7)
_cell_length_c                   15.8519(19)
_cell_measurement_reflns_used    5797
_cell_measurement_temperature    90
_cell_measurement_theta_max      32.5967
_cell_measurement_theta_min      1.7890
_cell_volume                     1213.2(2)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_molecular_graphics    ORTEP-3
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-2004
_diffrn_ambient_temperature      90
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;
scan:
Number of images: 60
Slice: -10.0000 - 20.0000
Image width: 0.5000
Exp time: 16.0000
Rotation axis: Omega
Omega: 0.0000
Chi: 0.0000
Phi: 0.0000
XTD: 40.0387
2theta: 20.0786
scan:
Number of images: 60
Slice: 20.0000 - 50.0000
Image width: 0.5000
Exp time: 16.0000
Rotation axis: Omega
Omega: 0.0000
Chi: 20.0000
Phi: 0.0000
XTD: 40.0387
2theta: 20.0786
scan:
Number of images: 344
Slice: -70.0000 - 102.0000
Image width: 0.5000
Exp time: 16.0000
Rotation axis: Omega
Omega: 0.0000
Chi: 50.0000
Phi: 90.0000
XTD: 40.0387
2theta: 20.0786
scan:
Number of images: 360
Slice: -70.0000 - 110.0000
Image width: 0.5000
Exp time: 16.0000
Rotation axis: Omega
Omega: 0.0000
Chi: 50.0000
Phi: 180.0000
XTD: 40.0387
2theta: 20.0786
scan:
Number of images: 360
Slice: -70.0000 - 110.0000
Image width: 0.5000
Exp time: 16.0000
Rotation axis: Omega
Omega: 0.0000
Chi: 50.0000
Phi: 135.0000
XTD: 40.0387
2theta: 20.0786

;
_diffrn_measurement_device_details
;
AFC8: Eulerian 3-circle
;
_diffrn_measurement_device_type
;
Rigaku AFC-8 with Saturn70 CCD detector
;
_diffrn_measurement_method       \w-scan
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.0040
_diffrn_orient_matrix_UB_12      0.0482
_diffrn_orient_matrix_UB_13      0.0733
_diffrn_orient_matrix_UB_21      0.1480
_diffrn_orient_matrix_UB_22      0.0072
_diffrn_orient_matrix_UB_23      -0.0128
_diffrn_orient_matrix_UB_31      -0.0052
_diffrn_orient_matrix_UB_32      0.0571
_diffrn_orient_matrix_UB_33      -0.0276
_diffrn_radiation_monochromator  cofocal
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_sigmaI/netI    0.0531
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            21152
_diffrn_reflns_theta_full        31.00
_diffrn_reflns_theta_max         31.00
_diffrn_reflns_theta_min         1.79
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.333
_exptl_absorpt_correction_T_max  0.9489
_exptl_absorpt_correction_T_min  0.6292
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Numabs (Higashi, 1999)
Numabs, Numerical Absorption Correction,
Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.984
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             716
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.877
_refine_diff_density_min         -0.799
_refine_diff_density_rms         0.101
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.009(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     357
_refine_ls_number_reflns         7525
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0212
_refine_ls_R_factor_gt           0.0176
_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^)+(0.0069P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0450
_refine_ls_wR_factor_ref         0.0456
_reflns_number_gt                6583
_reflns_number_total             7525
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b716400a.txt
_cod_data_source_block           Os-complex
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7150828