Organoruthenium(II) complexes with adamantane-thiourea ligands: structural and biological insights.
Guo, Chi-Xin; Eshaghi Malekshah, Rahime; Chen, Tzu-Yu; Karim, Amir; Chu, Yu-Ting; Shu, En-De; Chiu, Chien-Chih; Chien, Ching-Ming; Hsu, Sodio C. N.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 17646–17661; doi:10.1039/d5dt01959a

data_7719633
_publ_section_title
;
 Organoruthenium(II) complexes with adamantane-thiourea ligands:
 structural and biological insights.
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17646
_journal_page_last               17661
_journal_paper_doi               10.1039/d5dt01959a
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C28 H44 Cl2 N2 O Ru S'
_chemical_formula_sum            'C28 H44 Cl2 N2 O Ru S'
_chemical_formula_weight         628.68
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2025-04-30
_audit_creation_method
;
Olex2 1.5
(compiled 2025.04.05 svn.rf049d14d for OlexSys, GUI svn.r7224)
;
_audit_update_record
;
2025-04-30 deposited with the CCDC.	2025-10-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   33.1654(4)
_cell_length_b                   33.1654(4)
_cell_length_c                   14.8970(3)
_cell_measurement_reflns_used    24773
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      27.1510
_cell_measurement_theta_min      1.9640
_cell_volume                     14190.6(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      130(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -15.00 100.00   0.50   18.83    --   10.60  77.00-120.00  230
  2  \w    -79.00  36.00   0.50   18.83    --   10.60 -77.00   0.00  230
  3  \w    -27.00 100.00   0.50   18.83    --   10.60  37.00-150.00  254
  4  \w    -20.00  57.00   0.50   18.83    --   10.60  57.00  60.00  154
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro II AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_unetI/netI     0.0186
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            33587
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.984
_diffrn_reflns_theta_max         24.984
_diffrn_reflns_theta_min         1.540
_exptl_absorpt_coefficient_mu    0.755
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.32468
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_description       block
_exptl_crystal_F_000             5904
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.283
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         5553
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0231
_refine_ls_R_factor_gt           0.0200
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0238P)^2^+12.6909P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0493
_refine_ls_wR_factor_ref         0.0504
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5031
_reflns_number_total             5553
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01959a2.cif
_cod_data_source_block           k11108-sodio-d_auto
_cod_depositor_comments
'Adding full bibliography for 7719633--7719636.cif.'
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7719633
_shelx_shelxl_version_number     2018/3
_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. Uiso/Uaniso restraints and constraints
N1 \\sim N2 \\sim Cl1 \\sim Cl2 \\sim S1 \\sim Ru1 \\sim O1: within 3.8A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 3.8A
3.a Ternary CH refined with riding coordinates:
 C8(H8), C12(H12), C15(H15), C21(H21), C23(H23), C25(H25)
3.b Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C22(H22A,H22B), C24(H24A,H24B), C26(H26A,H26B), C27(H27A,
 H27B), C28(H28A,H28B)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7)
3.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C13(H13A,H13B,H13C),
 C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              8516
_shelx_hkl_checksum              1318
_shelx_fab_checksum              34250
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.507
_oxdiff_exptl_absorpt_empirical_full_min 0.765