Two rhenium compounds with benzimidazole ligands: synthesis and DNA interactions
Shtemenko, Nataliia; Galiana-Rosello, Cristina; Gil-Martínez, Ariadna; Blasco, Salvador; Gonzalez-García, Jorge; Velichko, Helen; Holichenko, Oleksandr; Shtemenko, Olexandr; García-España, Enrique; RSC Advances 14 (2024) 19787–19793; doi:10.1039/D4RA02669A

data_7248897
_publ_section_title
;
 Two rhenium compounds with benzimidazole ligands: synthesis and DNA
 interactions
;
_journal_issue                   28
_journal_name_full               'RSC Advances'
_journal_page_first              19787
_journal_page_last               19793
_journal_paper_doi               10.1039/D4RA02669A
_journal_volume                  14
_journal_year                    2024
_chemical_formula_moiety
'0.5(C56 H51 N16 O4 Re2), C28 H24 N8 O2 Re, 3(O4 Re), 2.238(O)'
_chemical_formula_sum            'C56 H49.5 N16 O18.24 Re5'
_chemical_formula_weight         2169.41
_space_group_crystal_system      tetragonal
_space_group_IT_number           128
_space_group_name_Hall           '-P 4 2n'
_space_group_name_H-M_alt        'P 4/m n c'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2024-03-08
_audit_creation_method
;
Olex2 1.5
(compiled 2023.11.24 svn.r209d9fb for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-03-08 deposited with the CCDC.	2024-06-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.974(3)
_cell_length_b                   15.974(3)
_cell_length_c                   27.244(7)
_cell_measurement_reflns_used    135
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      31.03455
_cell_measurement_theta_min      6.5093
_cell_volume                     6952(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_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  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_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  0.0597
_diffrn_reflns_av_unetI/netI     0.0176
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            97620
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.991
_diffrn_reflns_theta_min         2.342
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.750
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6350
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0816 before and 0.0608 after correction.
The Ratio of minimum to maximum transmissel selsion is 0.8517.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.073
_exptl_crystal_description       block
_exptl_crystal_F_000             4074
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.119
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.059
_refine_diff_density_max         2.474
_refine_diff_density_min         -3.246
_refine_diff_density_rms         0.244
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         3501
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0584
_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^)+(0.0595P)^2^+151.8831P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1556
_refine_ls_wR_factor_ref         0.1637
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3010
_reflns_number_total             3501
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ra02669a2.cif
_cod_data_source_block           mo_sb28_0m
_cod_original_formula_sum        'C56 H49.50 N16 O18.24 Re5'
_cod_database_code               7248897
_shelx_shelxl_version_number     2019/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 O11-O12 \\sim O11-O10 \\sim O11-O11_$1 \\sim O10-O12 \\sim O10-O11_$1 \\sim
O12-O11_$1
 with sigma of 0.02
 Re4-O10 \\sim Re4-O12 \\sim Re4-O11 \\sim Re4-O11_$1
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O10) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(O12) \\sim Ueq: with sigma of
0.03 and sigma for terminal atoms of 0.06
Uanis(O9) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
4. Others
 Sof(O9)=1-FVAR(1)
 Sof(O8)=0.5*FVAR(2)
 Fixed Sof: Re4(0.25) O12(0.25) O11(0.5) O10(0.25)
5.a Aromatic/amide H refined with riding coordinates:
 N2(H2), N4(H4A), C6(H6), C1(H1), C5(H5), C10(H10), C8(H8), C4(H4), C3(H3),
 C13(H13), C12(H12), C11(H11)
;
_shelx_res_checksum              20468
_shelx_hkl_checksum              48018
_olex2_submission_special_instructions 'No special instructions were received'