A dinuclear ruthenium(II) phototherapeutic that targets duplex and quadruplex DNA
Archer, Stuart; Raza, Ahtasham; Dröge, Fabian; Robertson, Craig C.; Auty, Alexander J.; Chekulaev, Dimitri M.; Weinstein, Julia; Keane, Theo; Meijer, Anthony J. H. M.; Haycock, John; MacNeil, Sheila; Thomas, Jim A.; Chemical Science  (2019) –; doi:10.1039/C8SC05084H

data_1550599
_publ_section_title
;
 A dinuclear ruthenium(II) phototherapeutic that targets duplex and
 quadruplex DNA
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C8SC05084H
_journal_year                    2019
_chemical_formula_moiety         'C64 H36 N22 Ru2, 4(Cl)'
_chemical_formula_sum            'C64 H36 Cl4 N22 Ru2'
_chemical_formula_weight         1457.09
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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     dual
_audit_creation_date             2017-09-06
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-11-01 deposited with the CCDC.    2019-02-15 downloaded from the CCDC.
;
_cell_angle_alpha                89.440(6)
_cell_angle_beta                 81.175(5)
_cell_angle_gamma                87.749(6)
_cell_formula_units_Z            2
_cell_length_a                   12.9007(13)
_cell_length_b                   14.8064(14)
_cell_length_c                   18.5391(16)
_cell_measurement_reflns_used    9966
_cell_measurement_temperature    100
_cell_measurement_theta_max      66.67
_cell_measurement_theta_min      2.41
_cell_volume                     3496.6(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      99.99
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker Venture Photon 100'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1466
_diffrn_reflns_av_unetI/netI     0.1128
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            47487
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        66.802
_diffrn_reflns_theta_max         66.802
_diffrn_reflns_theta_min         2.987
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.351
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.4748
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1234 before and 0.0877 after correction. The Ratio of minimum to maximum transmission is 0.6307. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_description       block
_exptl_crystal_F_000             1460
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.486
_refine_diff_density_min         -1.730
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     843
_refine_ls_number_reflns         12184
_refine_ls_number_restraints     124
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1383
_refine_ls_R_factor_gt           0.0927
_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^)+(0.1190P)^2^+20.8430P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2250
_refine_ls_wR_factor_ref         0.2553
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7793
_reflns_number_total             12184
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc05084h2.cif
_cod_data_source_block           iaj641v(2)
_cod_database_code               1550599
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.901
_shelx_estimated_absorpt_t_min   0.430
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid bond restraints
 C55, C56, C57, C58, C59, C60, C61, C62, C63, C64
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C1, C2, C3, C4, C5, C6, C7, C8, C9, C10
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C55 \\sim C56 \\sim C57 \\sim C58 \\sim C59 \\sim C60 \\sim C61 \\sim C62 \\sim
C63 \\sim C64: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(N4) = Uanis(N3)
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C7(H7), C8(H8), C11(H11), C12(H12), C14(H14),
 C15(H15), C17(H17), C18(H18), C21(H21), C22(H22), C23(H23), C28(H28), C29(H29),
  C30(H30), C36(H36), C37(H37), C38(H38), C41(H41), C42(H42), C43(H43),
 C45(H45), C46(H46), C48(H48), C49(H49), C51(H51), C52(H52), C55(H55), C56(H56),
  C58(H58), C59(H59), C61(H61), C62(H62)
;
_shelx_res_checksum              18353
_shelx_fab_checksum              841
_olex2_exptl_crystal_mounting_method 'mitigen holder in oil'
_olex2_submission_special_instructions 'No special instructions were received'