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_7719635
_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         'C34 H40 Cl2 N2 O Ru S, C H4 O'
_chemical_formula_sum            'C35 H44 Cl2 N2 O2 Ru S'
_chemical_formula_weight         728.75
_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
_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                 107.429(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.4880(5)
_cell_length_b                   12.7523(4)
_cell_length_c                   19.7959(6)
_cell_measurement_reflns_used    15079
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      26.6350
_cell_measurement_theta_min      1.9210
_cell_volume                     3489.5(2)
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      113.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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     -4.00  22.00   0.50   59.50    --   10.60  82.00 -90.00   52
  2  \w    -17.00  99.00   0.50   59.50    --   10.60  82.00   0.00  232
  3  \w     66.00  92.00   0.50   59.50    --   10.60 -19.00 -90.00   52
  4  \w    -14.00  21.00   0.50   59.50    --   10.60 -19.00 -90.00   70
  5  \w    -58.00  22.00   0.50   59.50    --   10.60 -82.00 -60.00  160
  6  \w    -32.00  36.00   0.50   59.50    --   10.60 -77.00-150.00  136
  7  \w    -99.00 -34.00   0.50   59.50    --  -10.90 -77.00-180.00  130
  8  \w    -61.00  15.00   0.50   59.50    --  -10.90 -77.00 150.00  152
  9  \w    -73.00 -48.00   0.50   59.50    --  -10.90 -77.00-120.00   50
;
_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  0.0376
_diffrn_reflns_av_unetI/netI     0.0386
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            28115
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.995
_diffrn_reflns_theta_max         24.995
_diffrn_reflns_theta_min         1.927
_exptl_absorpt_coefficient_mu    0.695
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65852
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_description       plate
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.405
_refine_diff_density_min         -1.023
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         6130
_refine_ls_number_restraints     1243
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0623
_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^)+(0.0756P)^2^+17.1661P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1596
_refine_ls_wR_factor_ref         0.1652
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5177
_reflns_number_total             6130
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01959a2.cif
_cod_data_source_block           k11107-sodio-d_auto
_cod_depositor_comments
'Adding full bibliography for 7719633--7719636.cif.'
_cod_database_code               7719635
_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, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Rigid bond restraints
 C8, C10
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 9.8
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33
\\sim C34 \\sim C35 \\sim N1 \\sim N2 \\sim O1 \\sim O2 \\sim S1 \\sim Cl1
\\sim Cl2 \\sim Ru1: within 3.8A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 3.8A
4.a Ternary CH refined with riding coordinates:
 C8(H8), C15(H15), C17(H17), C19(H19)
4.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C16(H16A,H16B), C18(H18A,H18B), C20(H20A,H20B), C21(H21A,
 H21B), C22(H22A,H22B)
4.c Aromatic/amide H refined with riding coordinates:
 N1(H1), C3(H3), C4(H4), C6(H6), C7(H7), C24(H24), C25(H25), C26(H26),
 C27(H27), C28(H28), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34)
4.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C35(H35A,H35B,H35C)
4.e Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_shelx_res_checksum              59264
_shelx_hkl_checksum              524
_shelx_fab_checksum              51331
_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 1.368
_oxdiff_exptl_absorpt_empirical_full_min 0.729