Chiroptical switching behavior of heteroleptic ruthenium complexes bearing acetylacetonato and tropolonato ligands
Yoshida, Jun; Yamazaki, Kana; Tateyama, Kazunori; Yuge, Hidetaka; Sato, Hisako; Dalton Transactions  (2021) –; doi:10.1039/D1DT02592A

data_7708289
_publ_section_title
;
 Chiroptical switching behavior of heteroleptic ruthenium complexes
 bearing acetylacetonato and tropolonato ligands
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02592A
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C19 H17 O6 Ru'
_chemical_formula_sum            'C19 H17 O6 Ru'
_chemical_formula_weight         442.39
_chemical_name_systematic        L-Ru(acac)(trop)2
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-02-09
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2021-07-27 deposited with the CCDC.	2021-09-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.9110(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.5743(4)
_cell_length_b                   7.39860(10)
_cell_length_c                   8.17530(10)
_cell_measurement_reflns_used    7917
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.4640
_cell_measurement_theta_min      5.4220
_cell_volume                     1728.12(4)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Rigaku HyPix-6000 area detector'
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.961
_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     50.00  75.00   0.50    3.82    --   47.45  66.00 -96.00   50
  2  \w     88.00 176.00   0.50   15.29    --  105.24  66.00 -96.00  176
  3  \w    141.00 168.00   0.50   15.29    --  105.24 125.00-150.00   54
  4  \w    135.00 176.00   0.50   15.29    --  105.24  77.00 -60.00   82
  5  \w    126.00 174.00   0.50   15.29    --  105.24  45.00  30.00   96
  6  \w    131.00 175.00   0.50   15.29    --  105.24  45.00   0.00   88
  7  \w    100.00 134.00   0.50   15.29    --  105.24 125.00-150.00   68
  8  \w     99.00 169.00   0.50   15.29    --  105.24  61.00-180.00  140
  9  \w     89.00 168.00   0.50   15.29    --  105.24  61.00 -30.00  158
 10  \w     94.00 126.00   0.50   15.29    --  105.24  45.00   0.00   64
 11  \w     83.00 123.00   0.50   15.29    --  105.24  77.00 -60.00   80
 12  \w     94.00 161.00   0.50   15.29    --  105.24  30.00-180.00  134
 13  \w     44.00  70.00   0.50   15.29    --  105.24 -61.00 -60.00   52
 14  \w     35.00  61.00   0.50   15.29    --  105.24 -61.00 -90.00   52
 15  \w     34.00 103.00   0.50   15.29    --  105.24 -77.00-150.00  138
 16  \w     34.00  67.00   0.50   15.29    --  105.24 -61.00-150.00   66
 17  \w     34.00  59.00   0.50   15.29    --  105.24 -61.00-180.00   50
 18  \w     40.00  65.00   0.50   15.29    --  105.24 -61.00  30.00   50
 19  \w     41.00  68.00   0.50   15.29    --  105.24 -61.00  60.00   54
 20  \w     47.00  76.00   0.50   15.29    --  105.24 -66.00 128.00   58
 21  \w     46.00  80.00   0.50   15.29    --  105.24 -77.00 150.00   68
 22  \w      3.00  65.00   0.50    3.82    --   47.45 -66.00 128.00  124
 23  \w    -25.00  14.00   0.50    3.82    --  -47.45  19.00 -90.00   78
 24  \w    -46.00 -16.00   0.50   15.29    --  -86.25  45.00  30.00   60
 25  \w    -41.00 -16.00   0.50   15.29    --  -86.25  45.00  60.00   50
 26  \w    -61.00  25.00   0.50    3.82    --  -47.45  66.00 -96.00  172
 27  \w    -70.00 -45.00   0.50   15.29    --  -86.25  66.00 -96.00   50
 28  \w   -122.00 -73.00   0.50   15.29    --  -86.25 -45.00  30.00   98
 29  \w   -113.00 -74.00   0.50   15.29    --  -86.25 -45.00   0.00   78
 30  \w   -117.00 -92.00   0.50    3.82    --  -47.45-125.00 -30.00   50
 31  \w   -140.00 -73.00   0.50   15.29    --  -86.25 -45.00  60.00  134
 32  \w   -110.00 -34.00   0.50    3.82    --  -47.45 -66.00 128.00  152
 33  \w   -156.00-131.00   0.50   15.29    --  -86.25 -94.00-120.00   50
 34  \w   -112.00 -87.00   0.50   15.29    --  -86.25 -94.00-120.00   50
 35  \w   -119.00 -90.00   0.50    3.82    --  -47.45-125.00-150.00   58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-S'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0329700000
_diffrn_orient_matrix_UB_12      -0.1531620000
_diffrn_orient_matrix_UB_13      -0.0530461000
_diffrn_orient_matrix_UB_21      0.0119336000
_diffrn_orient_matrix_UB_22      -0.0404731000
_diffrn_orient_matrix_UB_23      0.1807845000
_diffrn_orient_matrix_UB_31      -0.0409636000
_diffrn_orient_matrix_UB_32      -0.1350589000
_diffrn_orient_matrix_UB_33      0.0061373000
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            9684
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.409
_diffrn_reflns_theta_min         3.094
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.648
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65963
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.700
_exptl_crystal_description       block
_exptl_crystal_F_000             892
_exptl_crystal_recrystallization_method
'Slow evaporation from the benzene solution.'
_exptl_crystal_size_max          0.047
_exptl_crystal_size_mid          0.038
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.415
_refine_diff_density_min         -0.402
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details
;
 Flack x determined using 1453 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.019(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         3411
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0208
_refine_ls_R_factor_gt           0.0199
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0241P)^2^+1.2898P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0512
_refine_ls_wR_factor_ref         0.0515
_reflns_Friedel_coverage         0.808
_reflns_Friedel_fraction_full    0.989
_reflns_Friedel_fraction_max     0.912
_reflns_number_gt                3316
_reflns_number_total             3411
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02592a2.cif
_cod_data_source_block           exp_978
_cod_database_code               7708289
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ru O6 C17 H19'
_chemical_oxdiff_usercomment     L-Ru(acac)(trop)2
_shelx_estimated_absorpt_t_max   0.862
_shelx_estimated_absorpt_t_min   0.715
_reflns_odcompleteness_completeness 99.05
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.a Aromatic/amide H refined with riding coordinates:
 C009(H009), C00C(H00C), C00G(H00G), C00K(H00K), C00O(H00O), C00Q(H00Q),
 C3(H3), C4(H4), C7(H7), C8(H8), C1(H1)
2.b Idealised Me refined as rotating group:
 C00I(H00A,H00B,H00D), C00R(H00E,H00F,H00H)
;
_shelx_res_checksum              71676
_shelx_hkl_checksum              92647
_olex2_exptl_crystal_mounting_method loop
_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 1.471
_oxdiff_exptl_absorpt_empirical_full_min 0.618