Structural Investigation into the Threading Intercalation of a Chiral Dinuclear Ruthenium(II) Polypyridyl Complex through a B-DNA Oligonucleotide.
Fairbanks, Simon D.; Robertson, Craig C.; Keene, F. Richard; Thomas, Jim A.; Williamson, Mike P.; Journal of the American Chemical Society 141 (2019) 4644–4652; doi:10.1021/jacs.8b12280

data_4128950
_publ_section_title
;
 Structural Investigation into the Threading Intercalation of a Chiral
 Dinuclear Ruthenium(II) Polypyridyl Complex through a B-DNA
 Oligonucleotide.
;
_journal_issue                   11
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4644
_journal_page_last               4652
_journal_paper_doi               10.1021/jacs.8b12280
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C64 H44 N14 Ru2, 4(Cl)'
_chemical_formula_sum            'C64 H44 Cl4 N14 Ru2'
_chemical_formula_weight         1353.07
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-12-11
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                95.542(7)
_cell_angle_beta                 92.729(7)
_cell_angle_gamma                95.095(7)
_cell_formula_units_Z            1
_cell_length_a                   8.3032(16)
_cell_length_b                   11.378(2)
_cell_length_c                   18.250(4)
_cell_measurement_reflns_used    9907
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.66
_cell_measurement_theta_min      2.22
_cell_volume                     1706.6(6)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0683
_diffrn_reflns_av_unetI/netI     0.0575
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            46946
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.556
_diffrn_reflns_theta_min         1.806
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.646
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6726
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0611 before and 0.0539 after correction. The Ratio of minimum to maximum transmission is 0.9021. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_description       block
_exptl_crystal_F_000             682
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.212
_exptl_crystal_size_min          0.188
_refine_diff_density_max         1.845
_refine_diff_density_min         -0.680
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         7843
_refine_ls_number_restraints     381
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0707
_refine_ls_R_factor_gt           0.0492
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0620P)^2^+2.8990P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1183
_refine_ls_wR_factor_ref         0.1296
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6113
_reflns_number_total             7843
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b12280_si_004.cif
_cod_data_source_block           iaj646k_0m
_cod_database_code               4128950
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.888
_shelx_estimated_absorpt_t_min   0.782
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(Cl2B)=1-FVAR(1)
 Sof(Cl2A)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C8(H8), C9(H9), C10(H10), C13(H13), C14(H14),
 C15(H15), C16(H16), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24),
  C25(H25), C26(H26), C29(H29), C30(H30), C31(H31), C32(H32)
;
_shelx_res_checksum              39665
_shelx_hkl_checksum              99536
_shelx_fab_checksum              91642
_olex2_exptl_crystal_mounting_method 'Mitigen micromount in fomblyn oil'
_olex2_submission_special_instructions 'No special instructions were received'