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_7715095
_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         'C42 H32 F12 O12 Ru2'
_chemical_formula_sum            'C42 H32 F12 O12 Ru2'
_chemical_formula_weight         1158.81
_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     dual
_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                63.049(7)
_cell_angle_beta                 86.323(5)
_cell_angle_gamma                84.182(5)
_cell_formula_units_Z            1
_cell_length_a                   9.2598(5)
_cell_length_b                   10.9329(8)
_cell_length_c                   11.6726(8)
_cell_measurement_reflns_used    7749
_cell_measurement_temperature    102
_cell_measurement_theta_max      29.5210
_cell_measurement_theta_min      1.9450
_cell_volume                     1047.71(14)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      102.0
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.856
_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     54.00  80.00   0.50    1.82    --   17.03  57.00-180.00   52
  2  \w    -13.00  45.00   0.50    1.82    --   17.03  57.00-180.00  116
  3  \w     46.00  88.00   0.50    1.82    --   17.03  57.00 120.00   84
  4  \w     -1.00  27.00   0.50    1.82    --   17.03  57.00 120.00   56
  5  \w    -48.00  61.00   0.50    1.82    --  -16.56  57.00  30.00  218
  6  \w    -63.00 -35.00   0.50    1.82    --  -16.56 106.00  41.00   56
  7  \w   -107.00 -49.00   0.50    1.82    --  -16.56-179.00-150.00  116
  8  \w    -61.00  48.00   0.50    1.82    --   17.03 -57.00-150.00  218
  9  \w      3.00  71.00   0.50    1.82    --   17.03-106.00 -57.00  136
 10  \w    -60.00  48.00   0.50    1.82    --   17.03 -57.00 120.00  216
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_av_unetI/netI     0.0549
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.856
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13617
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.856
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.614
_diffrn_reflns_theta_min         1.958
_exptl_absorpt_coefficient_mu    0.839
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81368
_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    1.837
_exptl_crystal_description       block
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.115
_exptl_crystal_size_mid          0.112
_exptl_crystal_size_min          0.094
_refine_diff_density_max         0.717
_refine_diff_density_min         -0.906
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         5043
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0517
_refine_ls_R_factor_gt           0.0369
_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^)+(0.0462P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0848
_refine_ls_wR_factor_ref         0.0902
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4040
_reflns_number_total             5043
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03535b2.cif
_cod_data_source_block           Hete-Ru-p-CHO
_cod_original_cell_volume        1047.71(13)
_cod_database_code               7715095
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.925
_shelx_estimated_absorpt_t_min   0.910
_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:
 C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C13(H13), C14(H14), C15(H15)
;
_shelx_res_checksum              60041
_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
;