Modelling the binding of cytotoxic dinuclear nickel complexes to two neighboring phosphate esters of DNA using dicarboxylate ligands.
Riediger, Thomas; Böhm, Maximilian; Kapiza, Michael; Stammler, Anja; Oldengott, Jan; Glaser, Thorsten; Dalton transactions (Cambridge, England : 2003) 54 (2025) 9984–9991; doi:10.1039/d5dt00941c

data_7718819
_publ_section_title
;
 Modelling the binding of cytotoxic dinuclear nickel complexes to two
 neighboring phosphate esters of DNA using dicarboxylate ligands.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9984
_journal_page_last               9991
_journal_paper_doi               10.1039/d5dt00941c
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C45 H47 N6 Ni2 O6, C24 H20 B, 2(C2 H3 N)'
_chemical_formula_sum            'C73 H73 B N8 Ni2 O6'
_chemical_formula_weight         1286.62
_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   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-04-17
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-04-19 deposited with the CCDC.	2025-06-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.945(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.6053(8)
_cell_length_b                   24.5063(10)
_cell_length_c                   14.9770(7)
_cell_measurement_reflns_used    9777
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.914
_cell_measurement_theta_min      2.224
_cell_volume                     6288.4(5)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2019)'
_computing_data_collection       'APEX4 v2021.10-0 (Bruker AXS, 2021)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2019)'
_computing_molecular_graphics    'DIAMOND 2/4 (Crystal Impact, 2022)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker APEX II area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker KAPPA APEX Duo'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'graphite monochromator'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0427
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            311779
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.347
_diffrn_reflns_theta_min         1.662
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_type              'Bruker KAPPA APEX Duo'
_diffrn_source_voltage           40.0
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_exptl_absorpt_coefficient_mu    0.660
_exptl_absorpt_correction_T_max  0.6706
_exptl_absorpt_correction_T_min  0.6029
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0534 before and 0.0501 after correction.
The Ratio of minimum to maximum transmission is 0.8990.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2704
_exptl_crystal_preparation
'Crystal selected from oil dispersion and mounted via cryoloop.'
_exptl_crystal_recrystallization_method
;
A solution of the complex in MeCN/H2O was filtered. Single-crystals were 
obtained by slow vapour diffusion of methyl tert-butyl ether into this solution.
;
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.966
_refine_diff_density_min         -0.713
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    hetero
_refine_ls_matrix_type           full
_refine_ls_number_parameters     821
_refine_ls_number_reflns         24173
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0410
_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^)+(0.0521P)^2^+3.3377P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0999
_refine_ls_wR_factor_ref         0.1102
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19402
_reflns_number_total             24173
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00941c2.cif
_cod_data_source_block           g2850
_cod_depositor_comments
'Adding full bibliography for 7718818--7718819.cif.'
_cod_database_code               7718819
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.863
_shelx_estimated_absorpt_t_min   0.769
_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 C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C22(H22A,H22B), C31(H31A,H31B), C32(H32A,
 H32B), C42(H42A,H42B), C62(H62A,H62B), C63(H63A,H63B), C64(H64A,H64B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C9(H9), C10(H10), C14(H14), C15(H15), C16(H16), C24(H24),
 C25(H25), C26(H26), C34(H34), C35(H35), C36(H36), C44(H44), C45(H45), C46(H46),
  C102(H102), C103(H103), C104(H104), C105(H105), C106(H106), C108(H108),
 C109(H109), C110(H110), C111(H111), C112(H112), C114(H114), C115(H115),
 C116(H116), C117(H117), C118(H118), C120(H120), C121(H121), C122(H122),
 C123(H123), C124(H124)
2.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C28(H28A,H28B,H28C), C38(H38A,H38B,H38C), C48(H48A,H48B,
 H48C), C4S(H4SA,H4SB,H4SC), C2S(H2SA,H2SB,H2SC)
;
_shelx_res_checksum              30038
_shelx_hkl_checksum              22471
_olex2_submission_special_instructions 'No special instructions were received'