Tris(tropolonato) ruthenium as a hub for connecting π-conjugated systems.
Yoshida, Jun; Tateyama, Kazunori; Yuge, Hidetaka; Dalton transactions (Cambridge, England : 2003) 49 (2020) 2102–2111; doi:10.1039/c9dt04860j

data_7703451
_publ_section_title
;
 Tris(tropolonato) ruthenium as a hub for connecting \p-conjugated
 systems.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2102
_journal_page_last               2111
_journal_paper_doi               10.1039/c9dt04860j
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C37 H23 O6 Ru, 2(C H Cl3)'
_chemical_formula_sum            'C39 H25 Cl6 O6 Ru'
_chemical_formula_weight         903.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-09-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-12-20 deposited with the CCDC.	2020-01-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.420(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.5500(4)
_cell_length_b                   10.6232(2)
_cell_length_c                   14.7279(3)
_cell_measurement_reflns_used    9906
_cell_measurement_temperature    173
_cell_measurement_theta_max      77.2390
_cell_measurement_theta_min      3.6710
_cell_volume                     3816.94(12)
_computing_cell_refinement       'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_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      173
_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 0.999
_diffrn_measured_fraction_theta_max 0.959
_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    -86.00   2.00   0.50    0.82    --  -47.94 109.00  46.00  176
  2  \w    -71.00 -13.00   0.50    3.26    --  -86.25  37.00  30.00  116
  3  \w    -85.00 -13.00   0.50    3.26    --  -86.25 109.00  46.00  144
  4  \w    -71.00 -13.00   0.50    3.26    --  -86.25  37.00-120.00  116
  5  \w    -60.00  25.00   0.50    0.82    --  -47.94  37.00-180.00  170
  6  \w     19.00  87.00   0.50    0.82    --   47.94-109.00 -49.00  136
  7  \w     35.00 111.00   0.50    3.26    --  107.75-109.00 -49.00  152
  8  \w     35.00  71.00   0.50    3.26    --  107.75 -37.00 -30.00   72
  9  \w     35.00  60.00   0.50    3.26    --  107.75 -37.00  30.00   50
 10  \w     36.00  74.00   0.50    3.26    --  107.75 -57.00  90.00   76
 11  \w     35.00 131.00   0.50    3.26    --  107.75 -77.00 150.00  192
 12  \w     83.00 116.00   0.50    3.26    --  107.75-125.00 120.00   66
 13  \w     35.00  68.00   0.50    3.26    --  107.75 -37.00 150.00   66
 14  \w     36.00  70.00   0.50    3.26    --  107.75 -37.00  90.00   68
 15  \w     38.00  67.00   0.50    3.26    --  107.75 -37.00  60.00   58
 16  \w     35.00 107.00   0.50    3.26    --  107.75 -99.00   0.00  144
 17  \w     36.00  77.00   0.50    3.26    --  107.75-125.00 120.00   82
 18  \w    141.00 166.00   0.50    3.26    --  107.75  19.00 -30.00   50
 19  \w    101.00 178.00   0.50    3.26    --  107.75 109.00  46.00  154
 20  \w    106.00 132.00   0.50    3.26    --  107.75  19.00 -30.00   52
 21  \w     36.00  71.00   0.50    3.26    --  107.75 -37.00-180.00   70
 22  \w   -120.00 -70.00   0.50    0.82    --  -47.94-125.00-180.00  100
 23  \w   -159.00 -79.00   0.50    3.26    --  -86.25-109.00 -49.00  160
 24  \w   -120.00 -70.00   0.50    0.82    --  -47.94-125.00   0.00  100
 25  \w   -120.00 -70.00   0.50    0.82    --  -47.94-125.00  90.00  100
 26  \w   -120.00 -70.00   0.50    0.82    --  -47.94-125.00 120.00  100
;
_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      -0.0005024000
_diffrn_orient_matrix_UB_12      0.1413271000
_diffrn_orient_matrix_UB_13      0.0232810000
_diffrn_orient_matrix_UB_21      -0.0628119000
_diffrn_orient_matrix_UB_22      -0.0045495000
_diffrn_orient_matrix_UB_23      -0.0012860000
_diffrn_orient_matrix_UB_31      0.0065553000
_diffrn_orient_matrix_UB_32      -0.0321513000
_diffrn_orient_matrix_UB_33      0.1026546000
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0960
_diffrn_reflns_av_unetI/netI     0.0521
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            18613
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.285
_diffrn_reflns_theta_min         3.624
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              PhotonJet-S
_exptl_absorpt_coefficient_mu    7.575
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74832
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.45i (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_description       needle
_exptl_crystal_F_000             1812
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: chloroform'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.477
_refine_diff_density_min         -1.185
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         3930
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0848
_refine_ls_R_factor_gt           0.0795
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1503P)^2^+11.5459P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2120
_refine_ls_wR_factor_ref         0.2199
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3618
_reflns_number_total             3930
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.9961\% 
 around [-0.17 -0.00 0.99] (reciprocal) or [0.00 -0.00 1.00] (direct)
;
_cod_data_source_file            c9dt04860j2.cif
_cod_data_source_block           exp_40_twin1_hklf4
_cod_depositor_comments          'Adding full bibliography for 7703451.cif.'
_cod_database_code               7703451
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         C37H23O6Cl3Ru
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Ternary CH refined with riding coordinates:
 C00L(H00L)
2.b Aromatic/amide H refined with riding coordinates:
 C00A(H00A), C00B(H00B), C00E(H00E), C00F(H00F), C00H(H00H), C00I(H00I),
 C00J(H00J), C00M(H00M), C00O(H00O), C00P(H00P), C00Q(H00Q), C00R(H00R)
;
_shelx_res_checksum              84759
_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 1.361
_oxdiff_exptl_absorpt_empirical_full_min 0.721
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2