Investigating the DNA binding properties of two new Ru<sup>II</sup>(dppz) complexes incorporating the facially coordinated ligands tris(pyridin-2-yl)methylamine and di(pyridin-2-yl)methylamine.
Andrews, Thomas S.; Robertson, Craig; Meijer, Anthony J. H. M.; Thomas, Jim A.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 14587–14596; doi:10.1039/d5dt01159k

data_7719579
_publ_section_title
;
 Investigating the DNA binding properties of two new Ru<sup>II</sup>(dppz)
 complexes incorporating the facially coordinated ligands
 tris(pyridin-2-yl)methylamine and di(pyridin-2-yl)methylamine.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14587
_journal_page_last               14596
_journal_paper_doi               10.1039/d5dt01159k
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C34 H26 N8 Ru, 2(F6 P), 0.5[CH3NO2]'
_chemical_formula_sum            'C34.5 H27.5 F12 N8.5 O P2 Ru'
_chemical_formula_weight         968.16
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-08-27
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_audit_update_record
;
2025-09-05 deposited with the CCDC.	2025-09-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.450(15)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.11(3)
_cell_length_b                   13.85(2)
_cell_length_c                   31.10(5)
_cell_measurement_reflns_used    391
_cell_measurement_temperature    100
_cell_measurement_theta_max      10.820
_cell_measurement_theta_min      2.366
_cell_volume                     7519(2)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.997
_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  0.2943
_diffrn_reflns_av_unetI/netI     0.1606
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            23454
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        16.009
_diffrn_reflns_theta_max         16.009
_diffrn_reflns_theta_min         1.166
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.605
_exptl_absorpt_correction_T_max  0.7438
_exptl_absorpt_correction_T_min  0.5993
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0968 before and 0.0668 after correction. The Ratio of minimum to maximum transmission is 0.8057. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'dark orange'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.710
_exptl_crystal_description       plate
_exptl_crystal_F_000             3872
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.961
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.528
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     848
_refine_ls_number_reflns         3667
_refine_ls_number_restraints     1320
_refine_ls_restrained_S_all      1.287
_refine_ls_R_factor_all          0.3047
_refine_ls_R_factor_gt           0.1753
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4219
_refine_ls_wR_factor_ref         0.4967
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1464
_reflns_number_total             3667
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01159k2.cif
_cod_data_source_block           iaj667s_0m
_cod_original_cell_volume        7520(20)
_cod_original_formula_sum        'C34.50 H27.50 F12 N8.50 O P2 Ru'
_cod_database_code               7719579
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.970
_shelx_estimated_absorpt_t_min   0.889
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
2. Restrained distances
 Ru1B-C33B
 2.7 with sigma of 0.02
 P2-F3 \\sim P2-F1 \\sim P2-F5 \\sim P2-F7 \\sim P2-F10 \\sim P2-F11
 with sigma of 0.02
 F3-F1 \\sim F3-F7 \\sim F3-F10 \\sim F3-F11 \\sim F5-F1 \\sim F5-F7 \\sim
F5-F10 \\sim F5-F11 \\sim F7-F3 ~
 F7-F5 \\sim F1-F5 \\sim F1-F3
 with sigma of 0.04
 F3-F5 \\sim F1-F7 \\sim F11-F10
 with sigma of 0.05
 P1-F2 \\sim P1-F4 \\sim P1-F6 \\sim P1-F8 \\sim P1-F17 \\sim P1-F18
 with sigma of 0.02
 F2-F4 \\sim F2-F8 \\sim F2-F17 \\sim F2-F18 \\sim F6-F4 \\sim F6-F8 \\sim
F6-F17 \\sim F6-F18 \\sim F8-F2 ~
 F8-F6 \\sim F4-F6 \\sim F4-F2
 with sigma of 0.04
 F2-F6 \\sim F4-F8 \\sim F18-F17
 with sigma of 0.05
 P4-F9 \\sim P4-F13 \\sim P4-F15 \\sim P4-F16 \\sim P4-F19 \\sim P4-F1A
 with sigma of 0.02
 F9-F13 \\sim F9-F16 \\sim F9-F19 \\sim F9-F1A \\sim F15-F13 \\sim F15-F16
\\sim F15-F19 \\sim F15-F1A ~
 F16-F9 \\sim F16-F15 \\sim F13-F15 \\sim F13-F9
 with sigma of 0.04
 F9-F15 \\sim F13-F16 \\sim F1A-F19
 with sigma of 0.05
3. Rigid bond restraints
 N6B, C28B, C27B, C26B, C25B, C24B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N7A, C33A, C32A, C31A, C30A, C29A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
P2 \\sim F1 \\sim F3 \\sim F5 \\sim F7 \\sim F10 \\sim F11: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
P1 \\sim F2 \\sim F4 \\sim F6 \\sim F8 \\sim F17 \\sim F18: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
P4 \\sim F1A \\sim F9 \\sim F13 \\sim F15 \\sim F16 \\sim F19: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
N6B \\sim C24B \\sim C25B \\sim C26B \\sim C27B \\sim C28B: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
N7A \\sim C29A \\sim C30A \\sim C31A \\sim C32A \\sim C33A: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
5. 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
6.a Ternary CH refined with riding coordinates:
 C34A(H34A), C34B(H34B)
6.b Secondary CH2 refined with riding coordinates:
 N8A(H8AA,H8AB), N8B(H8BA,H8BB)
6.c Aromatic/amide H refined with riding coordinates:
 C19A(H19A), C20A(H20A), C21A(H21A), C22A(H22A), C23A(H23A), C3A(H3A),
 C1A(H1A), C2A(H2A), C10A(H10A), C8A(H8A), C9A(H9A), C13A(H13A), C14A(H14A),
 C15A(H15A), C16A(H16A), C27A(H27A), C26A(H26A), C25A(H25A), C24A(H24A),
 C32A(H32A), C29A(H29A), C30A(H30A), C31A(H31A), C32B(H32B), C31B(H31B),
 C30B(H30B), C29B(H29B), C8B(H8B), C9B(H9B), C10B(H10B), C1B(H1B), C2B(H2B),
 C3B(H3B), C9AA(H9AA), C16B(H16B), C14B(H14B), C15B(H15B), C21B(H21B),
 C20B(H20B), C19B(H19B), C23B(H23B), C22B(H22B), C24B(H24B), C27B(H27B),
 C26B(H26B), C25B(H25B)
6.d Fitted hexagon refined as free rotating group:
 N5A(C19A,C20A,C21A,C22A,C23A), C3A(C4A,C5A,N1A,C1A,C2A), C10A(N2A,C6A,C7A,C8A,
 C9A), C12A(C13A,C14A,C15A,C16A,C17A), C28A(C27A,C26A,C25A,C24A,N6A), C32A(C33A,
 N7A,C29A,C30A,C31A), N7B(C33B,C32B,C31B,C30B,C29B), N11B(C6B,C7B,C8B,C9B,C10B),
  C1B(C2B,C3B,C4B,C5B,N1B), C9AA(C16B,C17B,C13B,C14B,C15B), C21B(C20B,C19B,N5B,
 C23B,C22B), C24B(N6B,C28B,C27B,C26B,C25B)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              62131
_shelx_hkl_checksum              29778
_shelx_fab_checksum              84296
_olex2_exptl_crystal_mounting_method 'MiTiGen microloop in fomblin oil'
_olex2_submission_special_instructions 'No special instructions were received'