Tetranuclear Ru2Cu2 and Ru2Ni2 complexes with nanomolar anticancer activity
Alguacil, Andrés; Scalambra, Franco; Lorenzo Luiz, Pablo; Puerta, Adrián; González-Bakker , Aday; Mendoza, Zenaida; Padrón, José M.; Romerosa-Nievas, Antonio Manuel; Dalton Transactions  (2023) –; doi:10.1039/D3DT01284K

data_7713278
_publ_section_title
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 Tetranuclear Ru2Cu2 and Ru2Ni2 complexes with nanomolar anticancer
 activity
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01284K
_journal_year                    2023
_chemical_formula_moiety         'C96 H103 Cl3 N6 Ni2 O P6 Ru2'
_chemical_formula_sum            'C96 H103 Cl3 N6 Ni2 O P6 Ru2'
_chemical_formula_weight         1968.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2022-06-30
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-06-09 deposited with the CCDC.	2023-06-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.105(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.9347(10)
_cell_length_b                   14.1345(7)
_cell_length_c                   32.7675(15)
_cell_measurement_reflns_used    9795
_cell_measurement_temperature    293
_cell_measurement_theta_max      63.92
_cell_measurement_theta_min      2.70
_cell_volume                     10606.7(9)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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    'XT (Sheldrick, 2015'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1488
_diffrn_reflns_av_unetI/netI     0.0810
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            79421
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        64.673
_diffrn_reflns_theta_max         64.673
_diffrn_reflns_theta_min         2.701
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.547
_exptl_absorpt_correction_T_max  0.3158
_exptl_absorpt_correction_T_min  0.1870
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1181 before and 0.0933 after correction.
The Ratio of minimum to maximum transmission is 0.5921.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'light orange'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_description       block
_exptl_crystal_F_000             4056
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.004
_refine_diff_density_min         -0.596
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.159
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         8835
_refine_ls_number_restraints     512
_refine_ls_restrained_S_all      1.136
_refine_ls_R_factor_all          0.1479
_refine_ls_R_factor_gt           0.0952
_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^)+(0.0707P)^2^+117.3230P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2005
_refine_ls_wR_factor_ref         0.2252
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5695
_reflns_number_total             8835
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01284k2.cif
_cod_data_source_block           zm801_5_0m_sq
_cod_database_code               7713278
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.956
_shelx_estimated_absorpt_t_min   0.956
_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. Restrained distances
 H1-O1
 0.98 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C16) = Uanis(C14) = Uanis(C15) = Uanis(C17) = Uanis(C18) = Uanis(C19)
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. Others
 Sof(Cl2B)=1-FVAR(1)
 Sof(Cl2A)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C1(H1A,H1B), C5(H5A,H5B), C3(H3A,H3B), C2(H2A,H2B)
6.b Aromatic/amide H refined with riding coordinates:
 C48(H48), C47(H47), C43(H43), C13(H13), C46(H46), C44(H44), C45(H45), C9(H9),
 C40(H40), C10(H10), C37(H37), C19(H19), C18(H18), C21(H21), C15(H15), C41(H41),
  C31(H31), C36(H36), C33(H33), C27(H27), C39(H39), C42(H42), C17(H17),
 C35(H35), C12(H12), C28(H28), C11(H11), C22(H22), C16(H16), C29(H29), C34(H34),
  C30(H30), C23(H23), C25(H25), C24(H24)
6.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C6(H6A,H6B,H6C)
;
_shelx_res_checksum              3156
_shelx_hkl_checksum              52478
_shelx_fab_checksum              18904
_platon_squeeze_special_details
;
A solvent mask was calculated and 565 electrons were 
found in a volume of 2788\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
2[CF3SO3] per Asymmetric Unit 
which account for 584 electrons 
per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'