Search for new biologically active compounds: <i>in vitro</i> studies of antitumor and antimicrobial activity of dirhodium(II,II) paddlewheel complexes.
Mitrović, Marina; Djukić, Maja B; Vukić, Milena; Nikolić, Ivana; Radovanović, Marko D; Luković, Jovan; Filipović, Ignjat P; Matić, Sanja; Marković, Tijana; Klisurić, Olivera R; Popović, Suzana; Matović, Zoran D; Ristić, Marija S; Dalton transactions (Cambridge, England : 2003) 53 (2024) 9330–9349; doi:10.1039/d4dt01082e

data_7716074
_publ_section_title
;
 Search for new biologically active compounds: <i>in vitro</i> studies of
 antitumor and antimicrobial activity of dirhodium(II,II) paddlewheel
 complexes.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9330
_journal_page_last               9349
_journal_paper_doi               10.1039/d4dt01082e
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         '2(C11 H18 N2 O4 Rh), 1[C7 H8]'
_chemical_formula_sum            'C29 H44 N4 O8 Rh2'
_chemical_formula_weight         782.506
_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
_audit_creation_date             2024-05-08
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2019.10.09 svn.r3662 for OlexSys, GUI svn.r5959)
;
_audit_update_record
;
2024-05-09 deposited with the CCDC.	2024-05-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.366(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7537(6)
_cell_length_b                   13.5490(5)
_cell_length_c                   17.3153(7)
_cell_measurement_reflns_used    6505
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.3020
_cell_measurement_theta_min      2.6400
_cell_volume                     3464.9(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'Sheldrick, G. M. (2015). Acta Cryst. A71, 3-8'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.3280
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.851
_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    -32.00   7.00   1.00   44.23    --  -15.69 -77.00 150.00   39
  2  \w    -40.00  14.00   1.00   44.23    --  -15.69  77.00 120.00   54
  3  \w    -52.00  36.00   1.00   44.23    --   16.71 -37.00-150.00   88
  4  \w      0.00  53.00   1.00   44.23    --   16.71  57.00   0.00   53
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_unetI/netI     0.0503
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.851
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            17655
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.851
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.335
_diffrn_reflns_theta_min         2.040
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.002
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94444
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_description       prism
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.398
_exptl_crystal_size_mid          0.269
_exptl_crystal_size_min          0.245
_platon_squeeze_details
;
A platon squeeze results showed that 160 electrons were 
found in a volume of 996\%A^3^. 
This is consistent with the presence of 1 toluene [C7H8] per formula moety 
which account for 200 electrons per unit cell.
;
_refine_diff_density_max         1.111
_refine_diff_density_min         -0.604
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         8088
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0898
_refine_ls_R_factor_gt           0.0629
_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^)+(0.0579P)^2^+8.8336P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1502
_refine_ls_wR_factor_ref         0.1645
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5710
_reflns_number_total             8088
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01082e2.cif
_cod_data_source_block           mj1_auto_sq
_cod_depositor_comments          'Adding full bibliography for 7716074.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7716074
_shelx_shelxl_version_number     2018/3
_oxdiff_exptl_absorpt_empirical_full_min 0.932
_oxdiff_exptl_absorpt_empirical_full_max 1.064
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_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. Restrained distances
 C19-C20 \\sim C21-C22
 with sigma of 0.02
 C8-C9 \\sim C10-C11
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C19, C20, C21, C22
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C8, C9, C10, C11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C19(H19A,H19B), C9(H9A,H9B), C10(H10A,H10B), C20(H20A,H20B),
 C21(H21A,H21B)
4.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C17(H17), C18(H18), C16(H16), C7(H7), C6(H6)
4.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C4(H4A,H4B,H4C), C3(H3A,H3B,H3C), C15(H15A,H15B,H15C),
 C11(H11A,H11B,H11C), C22(H22A,H22B,H22C)
;
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              41142
_shelx_fab_checksum              47631