Hyphenation of lipophilic ruthenium(II)-diphosphine core with 5-fluorouracil: an effective metallodrug against glioblastoma brain cancer cells.
Saha, Abhijit; Mondal, Indranil; Kumari, Anuj; Sonkar, Avinash Kumar; Mishra, Ramranjan; Kulshreshtha, Ritu; Patra, Ashis K.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 1551–1567; doi:10.1039/d3dt02941g

data_7714639
_publ_section_title
;
 Hyphenation of lipophilic ruthenium(II)-diphosphine core with
 5-fluorouracil: an effective metallodrug against glioblastoma brain
 cancer cells.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1551
_journal_page_last               1567
_journal_paper_doi               10.1039/d3dt02941g
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C56 H50 F N2 O2 P4 Ru, F6 P, C2 H6 O S'
_chemical_formula_sum            'C58 H56 F7 N2 O3 P5 Ru S'
_chemical_formula_weight         1250.02
_chemical_name_systematic        abhijeet
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-11-20
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-11-28 deposited with the CCDC.	2023-11-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.6410(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.5354(4)
_cell_length_b                   20.8155(6)
_cell_length_c                   17.9751(5)
_cell_measurement_reflns_used    9844
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.52
_cell_measurement_theta_min      2.41
_cell_volume                     5427.6(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_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 SMART CCD 1K area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 1K area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            72419
_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         26.049
_diffrn_reflns_theta_min         2.772
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.547
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6226
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1866 before and 0.0663 after correction.
The Ratio of minimum to maximum transmission is 0.8345.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic light yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_description       block
_exptl_crystal_F_000             2560
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.220
_refine_diff_density_min         -1.614
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     697
_refine_ls_number_reflns         10709
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0740
_refine_ls_R_factor_gt           0.0581
_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^)+(0.0781P)^2^+20.9923P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1537
_refine_ls_wR_factor_ref         0.1691
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8769
_reflns_number_total             10709
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02941g2.cif
_cod_data_source_block           abhijeet_0m_a
_cod_depositor_comments          'Adding full bibliography for 7714639.cif.'
_cod_database_code               7714639
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.918
_shelx_estimated_absorpt_t_min   0.898
_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, All O(H) groups
2. Restrained distances
 C2-O2
 1.5 with sigma of 0.02
3. Rigid bond restraints
 N1, C4, C3, C2, N2, C1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C4) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(N2) \\sim
Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
5.a Secondary CH2 refined with riding coordinates:
 C43(H43A,H43B), C44(H44A,H44B), C18(H18A,H18B), C17(H17A,H17B)
5.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C38(H38), C16(H16), C6(H6), C39(H39), C40(H40), C26(H26), C52(H52),
 C15(H15), C54(H54), C12(H12), C46(H46), C35(H35), C34(H34), C55(H55), C36(H36),
  C7(H7), C42(H42), C48(H48), C9(H9), C14(H14), C13(H13), C56(H56), C20(H20),
 C53(H53), C41(H41), C8(H8), C50(H50), C33(H33), C32(H32), C22(H22), C47(H47),
 C49(H49), C24(H24), C27(H27), C21(H21), C30(H30), C23(H23), C28(H28), C29(H29),
  C4(H4)
5.c Idealised Me refined as rotating group:
 C57(H57A,H57B,H57C), C58(H58A,H58B,H58C)
5.d Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_shelx_res_checksum              60328
_olex2_submission_special_instructions 'No special instructions were received'