Post-synthetic molecular modifications based on Schiff base condensation reactions for designing functional paddlewheel diruthenium(II,II) complexes.
Itoh, Chisa; Yoshino, Haruka; Kitayama, Taku; Kosaka, Wataru; Miyasaka, Hitoshi; Dalton transactions (Cambridge, England : 2003) 53 (2024) 444–448; doi:10.1039/d3dt03535b

data_7715094
_publ_section_title
;
 Post-synthetic molecular modifications based on Schiff base condensation
 reactions for designing functional paddlewheel diruthenium(II,II)
 complexes.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              444
_journal_page_last               448
_journal_paper_doi               10.1039/d3dt03535b
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C40 H36 O14 Ru2, 2(C4 H8 O)'
_chemical_formula_sum            'C48 H52 O16 Ru2'
_chemical_formula_weight         1087.03
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-07-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-12-25 deposited with the CCDC.	2024-01-12 downloaded from the CCDC.
;
_cell_angle_alpha                63.205(4)
_cell_angle_beta                 71.840(3)
_cell_angle_gamma                71.697(3)
_cell_formula_units_Z            1
_cell_length_a                   10.1030(3)
_cell_length_b                   11.3908(4)
_cell_length_c                   11.9634(5)
_cell_measurement_reflns_used    13140
_cell_measurement_temperature    102
_cell_measurement_theta_max      30.9940
_cell_measurement_theta_min      2.1650
_cell_volume                     1143.02(8)
_computing_cell_refinement       'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      102
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.981
_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    -10.00  36.00   0.50    2.26    --    4.13 -99.00-117.00   92
  2  \w    -11.00  15.00   0.50    2.26    --    4.13 -99.00 -60.00   52
  3  \w      4.00  30.00   0.50    2.26    --    4.13 -99.00 -30.00   52
  4  \w     -6.00  34.00   0.50    2.26    --    4.13 -99.00  60.00   80
  5  \w     -1.00  35.00   0.50    2.26    --    4.13 -99.00 120.00   72
  6  \w    -68.00  18.00   0.50    2.26    --    4.13 -57.00 150.00  172
  7  \w    -27.00  14.00   0.50    2.26    --    4.13 -38.00 -90.00   82
  8  \w    -64.00 -20.00   0.50    2.26    --   -3.81 -77.00 -60.00   88
  9  \w    -16.00  18.00   0.50    2.26    --   -3.81 -77.00 -60.00   68
 10  \w     -8.00  58.00   0.50    2.26    --   -3.81  19.00 120.00  132
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0183640000
_diffrn_orient_matrix_UB_12      -0.0711224000
_diffrn_orient_matrix_UB_13      0.0286528000
_diffrn_orient_matrix_UB_21      -0.0008294000
_diffrn_orient_matrix_UB_22      -0.0036205000
_diffrn_orient_matrix_UB_23      -0.0574264000
_diffrn_orient_matrix_UB_31      0.0732117000
_diffrn_orient_matrix_UB_32      0.0027635000
_diffrn_orient_matrix_UB_33      -0.0218679000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17717
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.607
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.734
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56659
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.89a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_description       needle
_exptl_crystal_F_000             556
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.624
_refine_diff_density_min         -0.838
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         5149
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0249
_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^)+(0.0312P)^2^+0.5537P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0619
_refine_ls_wR_factor_ref         0.0635
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4679
_reflns_number_total             5149
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03535b2.cif
_cod_data_source_block           Ru-p-CHO
_cod_database_code               7715094
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_usercomment     'Brown needle'
_shelx_estimated_absorpt_t_max   0.964
_shelx_estimated_absorpt_t_min   0.667
_diffrn_oxdiff_digest_frames
;
01f0c5f69b8e8e54154674dcc8802ab9a9000268959
;
_diffrn_oxdiff_digest_hkl
;
01342cea8998673802644e3d9decc4c396056b
;
_reflns_odcompleteness_completeness 99.87
_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
2.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,
 H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C11(H11), C12(H12), C14(H14),
 C15(H15), C16(H16)
;
_shelx_res_checksum              44172
_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 1.504
_oxdiff_exptl_absorpt_empirical_full_min 0.703