Ru(II)-arene azole complexes as anti-amyloid-β agents.
Hacker, Ryan M.; Grimard, Daniela M.; Morgan, Katie A.; Saleh, Eaman; Wrublik, Morgan M.; Meiss, Cade J.; Kant, Caitlyn C.; Jones, Marjorie A.; Brennessel, William W.; Webb, Michael I.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 18845–18855; doi:10.1039/d4dt01740d

data_7716797
_publ_section_title
;
 Ru(II)-arene azole complexes as anti-amyloid-&#x3b2; agents.
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18845
_journal_page_last               18855
_journal_paper_doi               10.1039/d4dt01740d
_journal_volume                  53
_journal_year                    2024
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C13 H18 Cl2 N2 Ru S'
_chemical_formula_sum            'C13 H18 Cl2 N2 Ru S'
_chemical_formula_weight         406.32
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-11-17
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-05-18 deposited with the CCDC.	2024-07-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.01050(10)
_cell_length_b                   12.05820(10)
_cell_length_c                   14.31010(10)
_cell_measurement_reflns_used    13528
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      79.7460
_cell_measurement_theta_min      4.7820
_cell_volume                     1554.80(2)
_computing_cell_refinement       'CrysAlisPro 1.171.42.101a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.101a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.101a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2015a)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_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    -63.00 -19.00   0.50    0.06    --  -91.75  61.00-150.00   88
  2  \w   -162.00 -84.00   0.50    0.06    --  -91.75-104.00 -46.00  156
  3  \w   -119.00 -25.00   0.50    0.05    --  -47.33 -77.00 -60.00  188
  4  \w   -121.00 -34.00   0.50    0.05    --  -47.33 -33.00 156.00  174
  5  \w   -119.00 -65.00   0.50    0.05    --  -47.33   0.00  60.00  108
  6  \w     -9.00  28.00   0.50    0.05    --  -47.33  19.00 150.00   74
  7  \w    -31.00  26.00   0.50    0.05    --  -47.33  38.00 -30.00  114
  8  \w     -9.00  28.00   0.50    0.05    --  -47.33  19.00-180.00   74
  9  \w     -9.00  28.00   0.50    0.05    --  -47.33  19.00  60.00   74
 10  \w   -119.00 -65.00   0.50    0.05    --  -47.33   0.00   0.00  108
 11  \w     44.00 111.00   0.50    0.06    --  113.25-125.00 -30.00  134
 12  \w     42.00 106.00   0.50    0.06    --  113.25 -94.00   0.00  128
 13  \w     41.00 178.00   0.50    0.06    --  113.25   0.00 -90.00  274
 14  \w     91.00 178.00   0.50    0.06    --  113.25  77.00  30.00  174
 15  \w    100.00 178.00   0.50    0.06    --  113.25  33.00 -44.00  156
 16  \w    100.00 178.00   0.50    0.06    --  113.25  15.00 120.00  156
 17  \w     42.00  83.00   0.50    0.06    --  113.25 -61.00  60.00   82
 18  \w     42.00  83.00   0.50    0.06    --  113.25 -61.00 120.00   82
 19  \w     42.00  83.00   0.50    0.06    --  113.25 -61.00 150.00   82
 20  \w     42.00  83.00   0.50    0.06    --  113.25 -61.00 -60.00   82
 21  \w    107.00 178.00   0.50    0.06    --  113.25  99.00 152.00  142
 22  \w     95.00 178.00   0.50    0.06    --  113.25 125.00-150.00  166
 23  \w    -71.00 -45.00   0.50    0.06    --  -91.75 104.00  54.00   52
 24  \w     55.00  81.00   0.50    0.06    --  113.25 -61.00-180.00   52
 25  \w    110.00 156.00   0.50    0.06    --  113.25 125.00-180.00   92
 26  \w     57.00  83.00   0.50    0.06    --  113.25 -61.00 -30.00   52
 27  \w     51.00  99.00   0.50    0.06    --  113.25-125.00  90.00   96
;
_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      0.0400291000
_diffrn_orient_matrix_UB_12      -0.1225611000
_diffrn_orient_matrix_UB_13      0.0169451000
_diffrn_orient_matrix_UB_21      0.0600976000
_diffrn_orient_matrix_UB_22      -0.0086619000
_diffrn_orient_matrix_UB_23      -0.1004632000
_diffrn_orient_matrix_UB_31      0.1550779000
_diffrn_orient_matrix_UB_32      0.0350590000
_diffrn_orient_matrix_UB_33      0.0345782000
_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  0.0402
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17298
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         80.227
_diffrn_reflns_theta_min         4.796
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.471
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48907
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.101a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.736
_exptl_crystal_description       block
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.204
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_min          0.066
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.648
_refine_diff_density_rms         0.100
_refine_ls_abs_structure_details
;
 Flack x determined using 1386 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.004(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         3359
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0254
_refine_ls_R_factor_gt           0.0252
_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^)+(0.0173P)^2^+3.7196P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0624
_refine_ls_wR_factor_ref         0.0624
_reflns_Friedel_coverage         0.726
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.974
_reflns_number_gt                3344
_reflns_number_total             3359
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01740d2.cif
_cod_data_source_block           genmw06
_cod_depositor_comments
'Adding full bibliography for 7716796--7716798.cif.'
_cod_database_code               7716797
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.493
_shelx_estimated_absorpt_t_min   0.185
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C6) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.006
3.a Ternary CH refined with riding coordinates:
 C7(H7)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C12(H12), C13(H13)
3.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              97912
_shelx_hkl_checksum              69385
_olex2_submission_original_sample_id genmw06
_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 1.517
_oxdiff_exptl_absorpt_empirical_full_min 0.789