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_4128949
_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)'
_chemical_formula_sum            'C64 H44 F24 N14 P4 Ru2'
_chemical_formula_weight         1791.14
_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             2018-09-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.129(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.5327(14)
_cell_length_b                   16.3645(19)
_cell_length_c                   21.809(3)
_cell_measurement_reflns_used    9640
_cell_measurement_temperature    100
_cell_measurement_theta_max      22.73
_cell_measurement_theta_min      2.18
_cell_volume                     4438.3(9)
_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 0.997
_diffrn_measured_fraction_theta_max 0.992
_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  0.1023
_diffrn_reflns_av_unetI/netI     0.1197
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       14
_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       -24
_diffrn_reflns_number            77631
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.579
_diffrn_reflns_theta_min         1.560
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.504
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6325
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0851 before and 0.0774 after correction. The Ratio of minimum to maximum transmission is 0.8483. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'reddish orange'
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_description       block
_exptl_crystal_F_000             1780
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.104
_refine_diff_density_max         1.155
_refine_diff_density_min         -0.884
_refine_diff_density_rms         0.155
_refine_ls_abs_structure_details
;
 Flack x determined using 4853 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.086(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     973
_refine_ls_number_reflns         20302
_refine_ls_number_restraints     1151
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.1158
_refine_ls_R_factor_gt           0.0758
_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^)+(0.1312P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1894
_refine_ls_wR_factor_ref         0.2114
_reflns_Friedel_coverage         0.923
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.982
_reflns_number_gt                13917
_reflns_number_total             20302
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b12280_si_002.cif
_cod_data_source_block           iaj672k_0m
_cod_depositor_comments
;

2020-09-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C32 H22 F12 N7 P2 Ru'
_cod_original_formula_weight         895.57
_cod_original_formula_moiety         '0.5(C64 H44 N14 Ru2), 2(F6 P)'
_cod_original_formula_units_Z            4
_cod_database_code               4128949
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.949
_shelx_estimated_absorpt_t_min   0.783
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 P4-F21 \\sim P4-F22 \\sim P4-F23 \\sim P4-F24 \\sim P4-F20 \\sim P4-F19
 with sigma of 0.02
 F21-F22 \\sim F21-F24 \\sim F21-F20 \\sim F21-F19 \\sim F23-F22 \\sim F23-F24
\\sim F23-F20 \\sim F23-F19
 \\sim F24-F21 \\sim F24-F23 \\sim F22-F23 \\sim F22-F21
 with sigma of 0.04
 F21-F23 \\sim F22-F24 \\sim F19-F20
 with sigma of 0.05
3. Uiso/Uaniso restraints and constraints
P4 \\sim F19 \\sim F20 \\sim F21 \\sim F22 \\sim F23 \\sim F24: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
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.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), C20(H20), C21(H21), C22(H22), 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)
;
_shelx_res_checksum              69367
_shelx_hkl_checksum              62175
_shelx_fab_checksum              12487
_olex2_exptl_crystal_mounting_method 'MiTiGen microloop in fomblin oil'
_olex2_submission_special_instructions 'No special instructions were received'