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_7719634
_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         '0.33(C26 H40 Cl2 N2 O Ru S)'
_chemical_formula_sum            'C8.67 H13.33 Cl0.67 N0.67 O0.33 Ru0.33 S0.33'
_chemical_formula_weight         200.21
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-07-17
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2025-04-30 deposited with the CCDC.	2025-10-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.976(2)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   14.9144(2)
_cell_length_b                   11.48480(10)
_cell_length_c                   17.1011(3)
_cell_measurement_reflns_used    75835
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      26.9300
_cell_measurement_theta_min      2.1840
_cell_volume                     2696.85(8)
_computing_cell_refinement       'CrysAlisPro 1.171.41.56a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.56a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.56a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_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    -79.00  49.00   0.50    6.19    --   10.60 -36.00  94.00  256
  2  \w    -28.00 100.00   0.50    6.19    --   10.60  36.00-109.00  256
  3  \w   -100.00  27.00   0.50    6.19    --  -10.90 -36.00  94.00  254
  4  \w    -49.00  78.00   0.50    6.19    --  -10.90  36.00-109.00  254
  5  \w    -20.00 100.00   0.50    6.19    --   10.60  57.00   0.00  240
  6  \w    -15.00 100.00   0.50    6.19    --   10.60  77.00   0.00  230
  7  \w    -79.00  36.00   0.50    6.19    --   10.60 -77.00  60.00  230
  8  \w    -15.00 100.00   0.50    6.19    --   10.60  77.00 -90.00  230
  9  \w    -15.00 100.00   0.50    6.19    --   10.60  77.00 -60.00  230
 10  \w   -100.00  15.00   0.50    6.19    --  -10.90 -77.00 150.00  230
 11  \w    -79.00  38.00   0.50    6.19    --   10.60 -82.00  90.00  234
 12  \w    -79.00  38.00   0.50    6.19    --   10.60 -82.00   0.00  234
 13  \w    -79.00  38.00   0.50    6.19    --   10.60 -82.00-120.00  234
 14  \w    -79.00  38.00   0.50    6.19    --   10.60 -82.00 120.00  234
 15  \w    -79.00  38.00   0.50    6.19    --   10.60 -82.00-180.00  234
 16  \w    -17.00 100.00   0.50    6.19    --   10.60  82.00  90.00  234
 17  \w    -79.00  38.00   0.50    6.19    --   10.60 -82.00 -60.00  234
 18  \w    -79.00  38.00   0.50    6.19    --   10.60 -82.00  30.00  234
 19  \w   -100.00  17.00   0.50    6.19    --  -10.90 -82.00  60.00  234
 20  \w    -41.00  79.00   0.50    6.19    --  -10.90  57.00 -30.00  240
 21  \w    -79.00  38.00   0.50    6.19    --   10.60 -82.00 150.00  234
 22  \w    -79.00  38.00   0.50    6.19    --   10.60 -82.00 -30.00  234
 23  \w    -79.00 -54.00   0.50    6.19    --   10.60 -82.00 -90.00   50
 24  \w    -79.00  38.00   0.50    6.19    --   10.60 -82.00-150.00  234
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro II AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0416894000
_diffrn_orient_matrix_UB_12      -0.0351584000
_diffrn_orient_matrix_UB_13      0.0206833000
_diffrn_orient_matrix_UB_21      0.0303181000
_diffrn_orient_matrix_UB_22      0.0458625000
_diffrn_orient_matrix_UB_23      -0.0029970000
_diffrn_orient_matrix_UB_31      0.0034282000
_diffrn_orient_matrix_UB_32      0.0216720000
_diffrn_orient_matrix_UB_33      0.0399320000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0797
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_Laue_measured_fraction_full 0.999
_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       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            117196
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.195
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.879
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34789
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.56a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_description       block
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.794
_refine_diff_density_min         -0.816
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         4748
_refine_ls_number_restraints     918
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0264
_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^)+(0.0292P)^2^+3.5714P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0649
_refine_ls_wR_factor_ref         0.0662
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4432
_reflns_number_total             4748
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01959a2.cif
_cod_data_source_block           k11007-sodio-d
_cod_depositor_comments
'Adding full bibliography for 7719633--7719636.cif.'
_cod_original_cell_volume        2696.85(7)
_cod_database_code               7719634
_shelx_shelxl_version_number     2018/3
_diffrn_oxdiff_digest_frames
;
010e34e102277e76fdbaa54dc9f9d4d0a200025af86
;
_diffrn_oxdiff_digest_hkl
;
01bc1d740902a1df712e009f40213263850026
;
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
2. 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 N1 \\sim N2 \\sim O1 \\sim S1 \\sim Cl1 \\sim Cl2 \\sim Ru1:
within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Ternary CH refined with riding coordinates:
 C5(H5), C7(H7), C9(H9), C24(H24)
3.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C6(H6A,H6B), C8(H8A,H8B), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B), C13(H13A,H13B), C15(H15A,H15B)
3.c Aromatic/amide H refined with riding coordinates:
 N1(H1), C19(H19), C20(H20), C22(H22), C23(H23)
3.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C25(H25A,H25B,
 H25C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              54694
_shelx_hkl_checksum              95712
_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 1.905
_oxdiff_exptl_absorpt_empirical_full_min 0.527