Organometallic Ru(II), Rh(III) and Re(I) complexes of sterane-based bidentate ligands: synthesis, solution speciation, interaction with biomolecules and anticancer activity.
Pivarcsik, Tamás; Kiss, Márton A; Rapuš, Uroš; Kljun, Jakob; Spengler, Gabriella; Frank, Éva; Turel, Iztok; Enyedy, Éva A; Dalton transactions (Cambridge, England : 2003) 53 (2024) 4984–5000; doi:10.1039/d3dt04138g

data_7715157
_publ_section_title
;
 Organometallic Ru(II), Rh(III) and Re(I) complexes of sterane-based
 bidentate ligands: synthesis, solution speciation, interaction with
 biomolecules and anticancer activity.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4984
_journal_page_last               5000
_journal_paper_doi               10.1039/d3dt04138g
_journal_volume                  53
_journal_year                    2024
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C31 H36 Cl N2 O4 Re'
_chemical_formula_sum            'C31 H36 Cl N2 O4 Re'
_chemical_formula_weight         722.27
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-10-19
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-10-19 deposited with the CCDC.	2024-02-12 downloaded from the CCDC.
;
_cell_angle_alpha                110.232(3)
_cell_angle_beta                 107.742(3)
_cell_angle_gamma                91.611(3)
_cell_formula_units_Z            2
_cell_length_a                   8.9975(3)
_cell_length_b                   12.9898(4)
_cell_length_c                   13.9898(5)
_cell_measurement_reflns_used    9903
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      29.1430
_cell_measurement_theta_min      6.5190
_cell_volume                     1444.82(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_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    'ShelXS n/a (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4933
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.876
_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    -44.00  21.00   1.00   55.31    --  -11.01  77.00 -90.00   65
  2  \w    -35.00  63.00   1.00   55.31    --  -11.01  37.00 150.00   98
  3  \w    -15.00  30.00   1.00   55.31    --  -11.01 -99.00 150.00   45
  4  \w    -84.00  17.00   1.00   55.31    --  -11.01 -57.00  30.00  101
  5  \w    -39.00  62.00   1.00   55.31    --  -11.01  57.00  30.00  101
  6  \w    -42.00 -17.00   1.00   55.31    --  -11.01 -77.00 -90.00   25
  7  \w    -44.00  21.00   1.00   55.31    --  -11.01  77.00-150.00   65
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0480348000
_diffrn_orient_matrix_UB_12      -0.0263592000
_diffrn_orient_matrix_UB_13      -0.0550177000
_diffrn_orient_matrix_UB_21      -0.0685436000
_diffrn_orient_matrix_UB_22      0.0067559000
_diffrn_orient_matrix_UB_23      0.0151791000
_diffrn_orient_matrix_UB_31      -0.0012857000
_diffrn_orient_matrix_UB_32      0.0521874000
_diffrn_orient_matrix_UB_33      -0.0056763000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_unetI/netI     0.0656
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.876
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20202
_diffrn_reflns_point_group_measured_fraction_full 0.923
_diffrn_reflns_point_group_measured_fraction_max 0.756
_diffrn_reflns_theta_full        25.214
_diffrn_reflns_theta_max         29.456
_diffrn_reflns_theta_min         2.401
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.336
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92776
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.660
_exptl_crystal_description       plate
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.259
_refine_diff_density_min         -1.346
_refine_diff_density_rms         0.108
_refine_ls_abs_structure_details
;
 Flack x determined using 4157 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.036(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     651
_refine_ls_number_reflns         12182
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0320
_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^)+(0.0139P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0578
_refine_ls_wR_factor_ref         0.0603
_reflns_Friedel_coverage         0.727
_reflns_Friedel_fraction_full    0.847
_reflns_Friedel_fraction_max     0.637
_reflns_number_gt                10632
_reflns_number_total             12182
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt04138g2.cif
_cod_data_source_block           moc625
_cod_depositor_comments          'Adding full bibliography for 7715157.cif.'
_cod_database_code               7715157
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C31 H36 Cl1 Re1 N2 O4'
_shelx_estimated_absorpt_t_max   0.918
_shelx_estimated_absorpt_t_min   0.671
_reflns_odcompleteness_completeness 99.95
_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
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N6) = Uanis(C51) = Uanis(C44) = Uanis(C35) = Uanis(C32) = Uanis(C23)
Uanis(N12) = Uanis(C11) = Uanis(C19)
Uanis(O17) = Uanis(C7)
Uanis(Re2) = Uanis(C21) = Uanis(C30)
3.a Ternary CH refined with riding coordinates:
 C26(H26), C31(H31), C50(H50), C67(H67), C70(H70), C71(H71), C79(H79),
 C82(H82), C12(H12), C6(H6)
3.b Secondary CH2 refined with riding coordinates:
 C40(H40A,H40B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B), C52(H52A,
 H52B), C56(H56A,H56B), C59(H59A,H59B), C60(H60A,H60B), C104(H10A,H10B), C5(H5A,
 H5B), C2(H2A,H2B), C17(H17A,H17B), C15(H15A,H15B), C24(H24A,H24B), C18(H18A,
 H18B), C1(H1A,H1B)
3.c Aromatic/amide H refined with riding coordinates:
 C19(H19), C20(H20), C27(H27), C32(H32), C34(H34), C35(H35), C43(H43),
 C44(H44), C49(H49), C51(H51)
3.d Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C42(H42A,H42B,H42C), C62(H62A,H62B,H62C), C3(H3A,H3B,
 H3C), C45(H45A,H45B,H45C), C4(H4A,H4B,H4C)
3.e Idealised tetrahedral OH refined as rotating group:
 O4(H4), O5(H5)
;
_shelx_res_checksum              29896
_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 1.294
_oxdiff_exptl_absorpt_empirical_full_min 0.855