Ru(III) complexes with pyrazolopyrimidines as anticancer agents: bioactivities and the underlying mechanisms.
Gu, Yun-Qiong; Shen, Wen-Ying; Yang, Qi-Yuan; Chen, Zhen-Feng; Liang, Hong; Dalton transactions (Cambridge, England : 2003) 51 (2022) 1333–1343; doi:10.1039/d1dt02765d

data_7709253
_publ_section_title
;
 Ru(III) complexes with pyrazolopyrimidines as anticancer agents:
 bioactivities and the underlying mechanisms.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1333
_journal_page_last               1343
_journal_paper_doi               10.1039/d1dt02765d
_journal_volume                  51
_journal_year                    2022
_chemical_formula_moiety         '2(C25 H36 Cl3 N6 O Ru), 0.5(H2 O)'
_chemical_formula_sum            'C50 H73 Cl6 N12 O2.5 Ru2'
_chemical_formula_weight         1297.04
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-11-25
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2021-11-29 deposited with the CCDC.	2021-12-20 downloaded from the CCDC.
;
_cell_angle_alpha                78.483(2)
_cell_angle_beta                 83.943(2)
_cell_angle_gamma                81.607(2)
_cell_formula_units_Z            2
_cell_length_a                   13.3340(3)
_cell_length_b                   14.3744(3)
_cell_length_c                   15.7555(4)
_cell_measurement_reflns_used    12968
_cell_measurement_temperature    292(5)
_cell_measurement_theta_max      76.5910
_cell_measurement_theta_min      2.8560
_cell_volume                     2918.24(12)
_computing_cell_refinement       'CrysAlisPro 1.171.40.80a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.80a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.80a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      292(5)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.970
_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  12.00   0.50    2.32    --  -46.81  19.00 -30.00   54
  2  \w    -12.00  16.00   0.50    2.32    --  -46.81  19.00-150.00   56
  3  \w    -48.00 -16.00   0.50    4.00    --  -88.50  45.00 -60.00   64
  4  \w    -49.00 -17.00   0.50    4.00    --  -88.50  45.00 -30.00   64
  5  \w    -53.00 -22.00   0.50    4.00    --  -88.50 125.00 -90.00   62
  6  \w    -79.00  17.00   0.50    2.32    --  -46.81 101.00  21.00  192
  7  \w    -50.00 -16.00   0.50    4.00    --  -88.50  45.00-120.00   68
  8  \w    -76.00 -47.00   0.50    4.00    --  -88.50 101.00  21.00   58
  9  \w    -50.00 -16.00   0.50    4.00    --  -88.50  45.00 120.00   68
 10  \w    -61.00  22.00   0.50    2.32    --  -46.81  77.00 150.00  166
 11  \w    -28.00  25.00   0.50    2.32    --   46.81 -19.00   0.00  106
 12  \w    -20.00  59.00   0.50    2.32    --   46.81 -57.00 -30.00  158
 13  \w      4.00  60.00   0.50    2.32    --   46.81-101.00 -83.00  112
 14  \w     79.00 106.00   0.50    4.00    --  108.56-101.00 -83.00   54
 15  \w     64.00  98.00   0.50    4.00    --  108.56 -94.00  30.00   68
 16  \w     58.00 104.00   0.50    4.00    --  108.56 -94.00 120.00   92
 17  \w     75.00 102.00   0.50    4.00    --  108.56 -94.00 150.00   54
 18  \w     48.00 109.00   0.50    4.00    --  108.56-112.00 122.79  122
 19  \w     45.00 111.00   0.50    4.00    --  108.56-125.00   0.00  132
 20  \w     58.00 107.00   0.50    4.00    --  108.56-109.00 -79.17   98
 21  \w     51.00  92.00   0.50    4.00    --  108.56 -94.00-150.00   82
 22  \w     40.00 104.00   0.50    4.00    --  108.56 -94.00-180.00  128
 23  \w     43.00  77.00   0.50    4.00    --  108.56 -94.00 -60.00   68
 24  \w     39.00 110.00   0.50    4.00    --  108.56-125.00 -90.00  142
 25  \w     43.00 107.00   0.50    4.00    --  108.56-106.00  36.59  128
 26  \w     37.00  68.00   0.50    4.00    --  108.56 -61.00 120.00   62
 27  \w     37.00  62.00   0.50    4.00    --  108.56 -94.00 150.00   50
 28  \w     36.00 111.00   0.50    4.00    --  108.56-125.00 120.00  150
 29  \w     41.00  69.00   0.50    4.00    --  108.56 -61.00  90.00   56
 30  \w     36.00  63.00   0.50    4.00    --  108.56 -61.00  30.00   54
 31  \w     36.00  71.00   0.50    4.00    --  108.56 -61.00 -30.00   70
 32  \w     91.00 176.00   0.50    4.00    --  108.56  15.00  30.00  170
 33  \w    152.00 178.00   0.50    4.00    --  108.56  15.00 120.00   52
 34  \w    111.00 159.00   0.50    4.00    --  108.56 101.00  21.00   96
 35  \w     98.00 147.00   0.50    4.00    --  108.56  15.00 120.00   98
 36  \w     95.00 151.00   0.50    4.00    --  108.56 125.00  30.00  112
 37  \w     95.00 154.00   0.50    4.00    --  108.56 125.00 -60.00  118
 38  \w    103.00 128.00   0.50    4.00    --  108.56 125.00-120.00   50
 39  \w     38.00  65.00   0.50    4.00    --  108.56 -61.00-180.00   54
 40  \w   -119.00 -75.00   0.50    2.32    --  -46.81-125.00   0.00   88
 41  \w   -112.00 -76.00   0.50    2.32    --  -46.81-125.00  90.00   72
 42  \w   -107.00 -76.00   0.50    4.00    --  -88.50 -61.00  30.00   62
 43  \w   -106.00 -78.00   0.50    4.00    --  -88.50 -15.00 150.00   56
 44  \w   -159.00-113.00   0.50    4.00    --  -88.50 -15.00 150.00   92
 45  \w   -134.00 -66.00   0.50    4.00    --  -88.50 -77.00   0.00  136
 46  \w   -150.00 -88.00   0.50    4.00    --  -88.50-101.00 -83.00  124
 47  \w   -159.00-132.00   0.50    4.00    --  -88.50 -61.00 -30.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0305558000
_diffrn_orient_matrix_UB_12      -0.0292739000
_diffrn_orient_matrix_UB_13      -0.0816168000
_diffrn_orient_matrix_UB_21      -0.0007142000
_diffrn_orient_matrix_UB_22      -0.1037660000
_diffrn_orient_matrix_UB_23      0.0496399000
_diffrn_orient_matrix_UB_31      -0.1130943000
_diffrn_orient_matrix_UB_32      0.0232084000
_diffrn_orient_matrix_UB_33      0.0299070000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            38925
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.489
_diffrn_reflns_theta_min         3.164
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.115
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76369
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.80a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_description       block
_exptl_crystal_F_000             1334
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.104
_refine_diff_density_min         -0.994
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     693
_refine_ls_number_reflns         11583
_refine_ls_number_restraints     53
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0521
_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^)+(0.0754P)^2^+3.8681P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1396
_refine_ls_wR_factor_ref         0.1478
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9494
_reflns_number_total             11583
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02765d2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7709251--7709253.cif.'
_cod_original_formula_sum        'C50 H73 Cl6 N12 O2.50 Ru2'
_cod_database_code               7709253
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C  H  O N Ru'
_shelx_estimated_absorpt_t_max   0.345
_shelx_estimated_absorpt_t_min   0.232
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Restrained distances
 O2-O53
 1.38 with sigma of 0.02
 C51-C52 = C51A-C52A
 1.55 with sigma of 0.02
 C50-C51 = C50-C51A
 1.35 with sigma of 0.02
2. Rigid bond restraints
 C1, C2, O2, O53
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
3. Uiso/Uaniso restraints and constraints
Uanis(C28A) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C29A) \\sim Ueq, Uanis(C29)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C52A) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C51A) \\sim Ueq, Uanis(C52)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C28) = Uanis(C28A)
Uanis(C29) = Uanis(C29A)
Uanis(C51) = Uanis(C51A)
Uanis(C52) = Uanis(C52A)
4. Others
 Sof(H30C)=Sof(H30D)=Sof(C28A)=Sof(H28D)=Sof(H28E)=Sof(H28F)=Sof(C29A)=
 Sof(H29C)=Sof(H29D)=1-FVAR(1)
 Sof(H30A)=Sof(H30B)=Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C29)=Sof(H29A)=
 Sof(H29B)=FVAR(1)
 Sof(H50C)=Sof(H50D)=Sof(C51A)=Sof(H51C)=Sof(H51D)=Sof(C52A)=Sof(H52D)=
 Sof(H52E)=Sof(H52F)=1-FVAR(2)
 Sof(H50A)=Sof(H50B)=Sof(C51)=Sof(H51A)=Sof(H51B)=Sof(C52)=Sof(H52A)=Sof(H52B)=
 Sof(H52C)=FVAR(2)
 Fixed Sof: O53(0.5) H53A(0.5) H53B(0.5)
5.a Free rotating group:
 O53(H53A,H53B)
5.b Rotating group:
 O1(H1A,H1B), O2(H2A,H2B)
5.c Secondary CH2 refined with riding coordinates:
 C2(H2C,H2D), C3(H3A,H3B), C4(H4A,H4B), C24(H24A,H24B), C25(H25A,H25B),
 C26(H26A,H26B), C30(H30A,H30B), C30(H30C,H30D), C31(H31A,H31B), C49(H49A,H49B),
  C50(H50A,H50B), C50(H50C,H50D), C29(H29A,H29B), C51(H51A,H51B), C29A(H29C,
 H29D), C51A(H51C,H51D)
5.d Aromatic/amide H refined with riding coordinates:
 C17(H17), C43(H43)
5.e Idealised Me refined as rotating group:
 C1(H1C,H1D,H1E), C5(H5A,H5B,H5C), C9(H9A,H9B,H9C), C16(H16A,H16B,H16C),
 C19(H19A,H19B,H19C), C23(H23A,H23B,H23C), C27(H27A,H27B,H27C), C32(H32A,H32B,
 H32C), C36(H36A,H36B,H36C), C38(H38A,H38B,H38C), C44(H44A,H44B,H44C), C48(H48A,
 H48B,H48C), C28(H28A,H28B,H28C), C52(H52A,H52B,H52C), C28A(H28D,H28E,H28F),
 C52A(H52D,H52E,H52F)
;
_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 1.513
_oxdiff_exptl_absorpt_empirical_full_min 0.708