Synthesis and Anticancer Activity of [RuCl<sub>2</sub>(η<sup>6</sup>-arene)(aroylthiourea)] Complexes-High Activity against the Human Neuroblastoma (IMR-32) Cancer Cell Line.
Swaminathan, Srividya; Haribabu, Jebiti; Kalagatur, Naveen Kumar; Konakanchi, Ramaiah; Balakrishnan, Nithya; Bhuvanesh, Nattamai; Karvembu, Ramasamy; ACS omega 4 (2019) 6245–6256; doi:10.1021/acsomega.9b00349

data_4515053
_publ_section_title
;
 Synthesis and Anticancer Activity of
 [RuCl<sub>2</sub>(\h<sup>6</sup>-arene)(aroylthiourea)] Complexes-High
 Activity against the Human Neuroblastoma (IMR-32) Cancer Cell Line.
;
_journal_issue                   4
_journal_name_full               'ACS omega'
_journal_page_first              6245
_journal_page_last               6256
_journal_paper_doi               10.1021/acsomega.9b00349
_journal_volume                  4
_journal_year                    2019
_chemical_formula_moiety         'C28 H28 Cl2 N2 O Ru S'
_chemical_formula_sum            'C28 H28 Cl2 N2 O Ru S'
_chemical_formula_weight         612.55
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2016-08-18
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                84.351(2)
_cell_angle_beta                 82.004(2)
_cell_angle_gamma                82.920(2)
_cell_formula_units_Z            2
_cell_length_a                   9.5499(6)
_cell_length_b                   11.1471(6)
_cell_length_c                   12.2998(7)
_cell_measurement_reflns_used    9863
_cell_measurement_temperature    144.0
_cell_measurement_theta_max      70.073
_cell_measurement_theta_min      3.642
_cell_volume                     1282.33(13)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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      144.0
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            18873
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.159
_diffrn_reflns_theta_min         3.641
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.819
_exptl_absorpt_correction_T_max  0.4684
_exptl_absorpt_correction_T_min  0.2077
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1300 before and 0.0528 after correction.
The Ratio of minimum to maximum transmission is 0.4434.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_description       block
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.453
_exptl_crystal_size_mid          0.174
_exptl_crystal_size_min          0.153
_refine_diff_density_max         0.553
_refine_diff_density_min         -0.716
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         4827
_refine_ls_number_restraints     506
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0256
_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^)+(0.0309P)^2^+0.8179P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0630
_refine_ls_wR_factor_ref         0.0638
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4614
_reflns_number_total             4827
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao9b00349_si_005.cif
_cod_data_source_block           jhbnrup
_cod_database_code               4515053
_shelx_estimated_absorpt_t_max   0.381
_shelx_estimated_absorpt_t_min   0.126
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C27A-C25 \\sim C26A-C25
 with sigma of 0.005
 C27A-C25 \\sim C27-C25 \\sim C26-C25 \\sim C26A-C25
 with sigma of 0.005
 N2-C9 \\sim N2-C9A
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim
C17 \\sim C18 \\sim C9A \\sim C10A \\sim C11A \\sim C12A \\sim C13A \\sim C14A
\\sim C15A \\sim C16A \\sim C17A \\sim C18A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C26A) = Uanis(C26)
Uanis(C27A) = Uanis(C27)
Uanis(C27A) = Uanis(C27) = Uanis(C26) = Uanis(C26A)
4. Rigid body (RIGU) restrains
 C9, C10, C11, C12, C13, C14, C15, C16, C17, C18, C9A, C10A, C11A, C12A, C13A,
 C14A, C15A, C16A, C17A, C18A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Same fragment restrains
{C9, C10, C11, C12, C13, C14, C15, C16, C17, C18} sigma for 1-2: 0.02, 1-3: 0.04
as
{C9A, C10A, C11A, C12A, C13A, C14A, C15A, C16A, C17A, C18A}
6. Others
 Sof(H2B)=Sof(C9A)=Sof(C10A)=Sof(C11A)=Sof(C12A)=Sof(H12A)=Sof(C13A)=Sof(H13A)=
 Sof(C14A)=Sof(H14A)=Sof(C15A)=Sof(H15A)=Sof(C16A)=Sof(H16A)=Sof(C17A)=
 Sof(H17A)=Sof(C18A)=Sof(H18A)=Sof(H25A)=Sof(C26A)=Sof(H26A)=Sof(H26B)=
 Sof(H26C)=Sof(C27A)=Sof(H27A)=Sof(H27B)=Sof(H27C)=1-FVAR(1)
 Sof(H2)=Sof(C9)=Sof(C10)=Sof(C11)=Sof(C12)=Sof(H12)=Sof(C13)=Sof(H13)=
 Sof(C14)=Sof(H14)=Sof(C15)=Sof(H15)=Sof(C16)=Sof(H16)=Sof(C17)=Sof(H17)=
 Sof(C18)=Sof(H18)=Sof(H25)=Sof(C26)=Sof(H26D)=Sof(H26E)=Sof(H26F)=Sof(C27)=
 Sof(H27D)=Sof(H27E)=Sof(H27F)=FVAR(1)
7.a Ternary CH refined with riding coordinates:
 C25(H25A), C25(H25)
7.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), N2(H2B), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C12(H12),
 C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C12A(H12A),
 C13A(H13A), C14A(H14A), C15A(H15A), C16A(H16A), C17A(H17A), C18A(H18A),
 C20(H20), C21(H21), C23(H23), C24(H24)
7.c Idealised Me refined as rotating group:
 C26A(H26A,H26B,H26C), C26(H26D,H26E,H26F), C27A(H27A,H27B,H27C), C27(H27D,
 H27E,H27F), C28(H28A,H28B,H28C)
;
_shelx_res_checksum              92428
_shelx_hkl_checksum              91501
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'