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_7715099
_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
'0.67(C68 H59 N4 O14 Ru2), 0.33(C68 H56 N4 O14 Ru2), 1.33(C3 O0.75)'
_chemical_formula_sum            'C72 H58 N4 O15 Ru2'
_chemical_formula_weight         1421.36
_space_group_crystal_system      tetragonal
_space_group_IT_number           84
_space_group_name_Hall           '-P 4c'
_space_group_name_H-M_alt        'P 42/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-11-25
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            6
_cell_length_a                   17.6693(7)
_cell_length_b                   17.6693(7)
_cell_length_c                   32.9554(14)
_cell_measurement_reflns_used    9560
_cell_measurement_temperature    102
_cell_measurement_theta_max      28.3580
_cell_measurement_theta_min      1.6790
_cell_volume                     10288.8(7)
_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 0.987
_diffrn_measured_fraction_theta_max 0.987
_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     -5.00  21.00   0.50   14.18    --    4.13   5.00 -40.00   52
  2  \w     10.00  36.00   0.50   14.18    --    4.13 -99.00  90.00   52
  3  \w     -2.00  72.00   0.50   14.18    --    4.13  57.00-150.00  148
;
_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      0.0258445000
_diffrn_orient_matrix_UB_12      -0.0306805000
_diffrn_orient_matrix_UB_13      0.0009353000
_diffrn_orient_matrix_UB_21      0.0306686000
_diffrn_orient_matrix_UB_22      0.0258372000
_diffrn_orient_matrix_UB_23      0.0009594000
_diffrn_orient_matrix_UB_31      -0.0023970000
_diffrn_orient_matrix_UB_32      0.0001660000
_diffrn_orient_matrix_UB_33      0.0214621000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1099
_diffrn_reflns_av_unetI/netI     0.0665
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            34899
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.025
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         2.578
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.508
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.23055
_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    1.376
_exptl_crystal_description       block
_exptl_crystal_F_000             4356
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.557
_refine_diff_density_min         -1.815
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     681
_refine_ls_number_reflns         9143
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.1290
_refine_ls_R_factor_gt           0.0885
_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^)+(0.1354P)^2^+34.2001P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2181
_refine_ls_wR_factor_ref         0.2576
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6202
_reflns_number_total             9143
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03535b2.cif
_cod_data_source_block           Ru-ph(OMe)
_cod_original_cell_volume        10288.8(9)
_cod_database_code               7715099
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ru2 C68 H72 O14 N4'
_shelx_estimated_absorpt_t_max   0.995
_shelx_estimated_absorpt_t_min   0.985
_diffrn_oxdiff_digest_frames
;
013a90126e6446757bb6c6548ad7d4028b00025a422
;
_diffrn_oxdiff_digest_hkl
;
01911aa63da6058ff0117d9413d0c0525a18dc
;
_reflns_odcompleteness_completeness 99.75
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O7-C31
 1.54 with sigma of 0.01
 C56-C57
 1.54 with sigma of 0.01
 O12-C57
 1.54 with sigma of 0.01
 C54-C55
 1.54 with sigma of 0.01
 O13-C60
 1.54 with sigma of 0.01
 C53-C61
 3.3 with sigma of 0.01
3. Rigid bond restraints
 O13, C60, C61
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 Ru3, O12, C54, C55, C56, C57
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 Ru1, O7, C31, C32, C33, C34
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 Ru2, O8, C35, C36, C37, C38
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
O13 \\sim C60 \\sim C61: within 1A with sigma of 0.004 and sigma for terminal
atoms of 0.008
Ru3 \\sim O12 \\sim C54 \\sim C55 \\sim C56 \\sim C57: within 1A with sigma of
0.004 and sigma for terminal atoms of 0.008
Ru1 \\sim O7 \\sim C31 \\sim C32 \\sim C33 \\sim C34: within 1A with sigma of
0.004 and sigma for terminal atoms of 0.008
Ru2 \\sim O8 \\sim C35 \\sim C36 \\sim C37 \\sim C38: within 1A with sigma of
0.004 and sigma for terminal atoms of 0.008
Uanis(O14) \\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C56)
\\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C57) \\sim Ueq,
Uanis(C32) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(O6)
\\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(C60) \\sim Ueq, Uanis(C61) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: C31(0.5) H31A(0.5) H31B(0.5) C32(0.5) H32(0.5) H34A(0.5) H34B(0.5)
 H38A(0.5) H38B(0.5) C56(0.5) H56(0.5) O13(0.375) C60(0.75) C61(0.75)
 O14(0.375) C58(0.75) C59(0.75)
6.a Ternary CH refined with riding coordinates:
 C32(H32), C33(H33), C55(H55), C56(H56), C57(H57)
6.b Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C34(H34A,H34B), C38(H38A,H38B)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C8(H8), C9(H9), C12(H12), C13(H13), C14(H14),
 C15(H15), C18(H18), C19(H19), C21(H21), C23(H23), C24(H24), C27(H27), C28(H28),
  C29(H29), C30(H30), C35(H35), C36(H36), C37(H37), C41(H41), C42(H42),
 C44(H44), C46(H46), C47(H47), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54)
6.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C26(H26A,H26B,H26C), C49(H49A,H49B,H49C)
;
_shelx_res_checksum              56864
_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 3.139
_oxdiff_exptl_absorpt_empirical_full_min 0.618