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_4128948
_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_absolute_configuration ad
_chemical_formula_moiety         'C64 H44 N14 Ru2, 4(F6 P), 2(C H3 N O2)'
_chemical_formula_sum            'C66 H50 F24 N16 O4 P4 Ru2'
_chemical_formula_weight         1913.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-09-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.257(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.4658(7)
_cell_length_b                   16.2947(9)
_cell_length_c                   21.7440(12)
_cell_measurement_reflns_used    9754
_cell_measurement_temperature    100
_cell_measurement_theta_max      23.953
_cell_measurement_theta_min      2.184
_cell_volume                     4381.4(4)
_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 0.999
_diffrn_measured_fraction_theta_max 0.997
_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  0.0879
_diffrn_reflns_av_unetI/netI     0.0750
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            132518
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.637
_diffrn_reflns_theta_min         1.566
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.520
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6474
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0717 before and 0.0606 after correction. The Ratio of minimum to maximum transmission is 0.8683. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_description       block
_exptl_crystal_F_000             1908
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.378
_refine_diff_density_min         -0.798
_refine_diff_density_rms         0.126
_refine_ls_abs_structure_details
;
 Flack x determined using 5490 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.065(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1105
_refine_ls_number_reflns         20322
_refine_ls_number_restraints     1190
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.1063
_refine_ls_R_factor_gt           0.0710
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0995P)^2^+7.7694P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1717
_refine_ls_wR_factor_ref         0.1900
_reflns_Friedel_coverage         0.928
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                14801
_reflns_number_total             20322
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b12280_si_003.cif
_cod_data_source_block           iaj674k_2_0m
_cod_database_code               4128948
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.912
_shelx_estimated_absorpt_t_min   0.781
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 P4B-F20B \\sim P4B-F24B \\sim P4B-F22B \\sim P4B-F23B \\sim P4B-F19B \\sim
P4B-F21B
 with sigma of 0.02
 N2S-C2S \\sim N1S-C1S
 with sigma of 0.02
 O1S-N1S \\sim O2S-N1S \\sim O4S-N2S \\sim O3S-N2S
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C1S) = Uanis(C2S)
4. 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
5. Others
 Sof(P4B)=Sof(F19B)=Sof(F20B)=Sof(F21B)=Sof(F22B)=Sof(F23B)=Sof(F24B)=1-FVAR(1)
 Sof(F19A)=Sof(F20A)=Sof(F21A)=Sof(F22A)=Sof(F23A)=Sof(F24A)=Sof(P4A)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C8(H8), C9(H9), C10(H10), C14(H14), C15(H15),
 C16(H16), C19(H19), C20(H20), C21(H21), C25(H25), C26(H26), C27(H27), C28(H28),
  C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C37(H37),
 C38(H38), C41(H41), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), C47(H47),
  C48(H48), C51(H51), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56),
 C57(H57), C58(H58), C61(H61), C62(H62), C63(H63), C64(H64)
6.b Idealised Me refined as rotating group:
 C1S(H1SA,H1SB,H1SC), C2S(H2SA,H2SB,H2SC)
;
_shelx_res_checksum              33337
_shelx_hkl_checksum              35795
_shelx_fab_checksum              15701
_olex2_exptl_crystal_mounting_method 'MiTiGen microloop in fomblin oil'
_olex2_submission_special_instructions 'No special instructions were received'