Cytotoxic (<i>cis</i>,<i>cis</i>-1,3,5-triaminocyclohexane)ruthenium(II)-diphosphine complexes; evidence for covalent binding <i>and</i> intercalation with DNA.
Wise, Dan E.; Gamble, Aimee J.; Arkawazi, Sham W.; Walton, Paul H.; Galan, M. Carmen; O'Hagan, Michael P; Hogg, Karen G.; Marrison, Joanne L.; O'Toole, Peter J; Sparkes, Hazel A.; Lynam, Jason M.; Pringle, Paul G.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 15219–15230; doi:10.1039/d0dt02612c

data_7705548
_publ_section_title
;
 Cytotoxic
 (<i>cis</i>,<i>cis</i>-1,3,5-triaminocyclohexane)ruthenium(II)-diphosphine
 complexes; evidence for covalent binding <i>and</i> intercalation with
 DNA.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15219
_journal_page_last               15230
_journal_paper_doi               10.1039/d0dt02612c
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C38 H39 Cl N5 P2 Ru, F6 P'
_chemical_formula_sum            'C38 H39 Cl F6 N5 P3 Ru'
_chemical_formula_weight         909.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-05-31
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-10-15 deposited with the CCDC.	2020-09-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.3870(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9014(6)
_cell_length_b                   19.6282(9)
_cell_length_c                   14.2188(6)
_cell_measurement_reflns_used    5713
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.66
_cell_measurement_theta_min      2.22
_cell_volume                     3838.2(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'Bruker Apex suite'
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Bruker area detector'
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Bruker Apex II kappa CCD area detector'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_unetI/netI     0.0516
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            34855
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.874
_diffrn_reflns_theta_min         1.781
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.669
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6063
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0636 before and 0.0495 after correction. The Ratio of minimum to maximum transmission is 0.8132. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_description       block
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.392
_exptl_crystal_size_mid          0.288
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.495
_refine_diff_density_min         -0.548
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     560
_refine_ls_number_reflns         9143
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0350
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0259P)^2^+2.1027P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0695
_refine_ls_wR_factor_ref         0.0762
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7108
_reflns_number_total             9143
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02612c2.cif
_cod_data_source_block           testm1
_cod_depositor_comments          'Adding full bibliography for 7705548.cif.'
_cod_database_code               7705548
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.912
_shelx_estimated_absorpt_t_min   0.780
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All N(H,H) groups
2. Restrained distances
 P3-F1 \\sim P3-F1A \\sim P3-F2 \\sim P3-F3 \\sim P3-F3A \\sim P3-F2A \\sim
P3-F6 \\sim P3-F6A \\sim P3-F4 ~
 P3-F4A
 with sigma of 0.01
 N3-H3A \\sim N3-H3B \\sim N4-H4A \\sim N4-H4B \\sim N5-H5B \\sim N5-H5A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
F1 \\sim F2 \\sim F3 \\sim F4 \\sim F5 \\sim F6 \\sim F1A \\sim F2A \\sim F3A
\\sim F6A \\sim F4A \\sim F5A: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(F6A)=Sof(F4A)=Sof(F5A)=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C33(H33), C35(H35), C37(H37)
5.b Secondary CH2 refined with riding coordinates:
 C34(H34A,H34B), C36(H36A,H36B), C38(H38A,H38B)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C15(H15), C16(H16), C17(H17), C18(H18), C22(H22), C23(H23), C24(H24),
  C25(H25), C26(H26), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32)
;
_shelx_res_checksum              75399
_olex2_submission_special_instructions 'No special instructions were received'