Control of Dominant Conduction Orbitals by Peripheral Substituents in Paddle-Wheel Diruthenium Alkynyl Molecular Junctions
Ogawa, Shiori; Chattopadhyay, Swarup; Tanaka, Yuya; Ohto, Tatsuhiko; Tada, Tomofumi; Tada, Hirokazu; Fujii, Shintaro; Nishino, Tomoaki; Akita, Munetaka; Chemical Science  (2021) –; doi:10.1039/D1SC02407H

data_1564070
_publ_section_title
;
 Control of Dominant Conduction Orbitals by Peripheral Substituents in
 Paddle-Wheel Diruthenium Alkynyl Molecular Junctions
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC02407H
_journal_year                    2021
_chemical_formula_moiety         'C70 H58 N8 Ru2 S2'
_chemical_formula_sum            'C70 H58 N8 Ru2 S2'
_chemical_formula_weight         1277.50
_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
_audit_creation_date             2020-10-06
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-01-19 deposited with the CCDC.	2021-07-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.800(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.1130(4)
_cell_length_b                   15.1675(3)
_cell_length_c                   16.6699(3)
_cell_measurement_reflns_used    22488
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      74.5160
_cell_measurement_theta_min      3.4340
_cell_volume                     5894.48(19)
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_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      93(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.969
_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     13.00  72.00   0.50    0.05    --   42.05  77.00  60.00  118
  2  \w     13.00 116.00   0.50    0.05    --   42.05  77.00 -60.00  206
  3  \w     13.00 116.00   0.50    0.05    --   42.05  77.00-180.00  206
  4  \w    -35.00  44.00   0.50    0.05    --   42.05 -37.00-180.00  158
  5  \w    -38.00  28.00   0.50    0.05    --   42.05 -19.00  60.00  132
  6  \w     89.00 178.00   0.50    0.18    --  106.13 104.00  41.00  178
  7  \w     83.00 178.00   0.50    0.18    --  106.13  61.00   0.00  190
  8  \w     84.00 178.00   0.50    0.18    --  106.13  45.00  30.00  188
  9  \w     83.00 178.00   0.50    0.18    --  106.13  30.00 150.00  190
 10  \w     32.00  73.00   0.50    0.18    --  106.13 -61.00  60.00   82
 11  \w     32.00 108.00   0.50    0.18    --  106.13 -77.00 -60.00  152
 12  \w     32.00  73.00   0.50    0.18    --  106.13 -61.00 -90.00   82
 13  \w     32.00  73.00   0.50    0.18    --  106.13 -61.00 -60.00   82
 14  \w      2.00  84.00   0.50    0.05    --   42.05-104.00 -59.00  164
 15  \w     31.00 106.00   0.50    0.18    --  106.13-104.00 -59.00  150
 16  \w    -24.00  39.00   0.50    0.05    --  -42.05  19.00 -60.00  126
 17  \w    -24.00  39.00   0.50    0.05    --  -42.05  19.00  30.00  126
 18  \w    -69.00 -28.00   0.50    0.18    -- -102.00  61.00  30.00   82
 19  \w    -69.00 -28.00   0.50    0.18    -- -102.00  61.00  60.00   82
 20  \w    -69.00 -28.00   0.50    0.18    -- -102.00  61.00 -90.00   82
 21  \w    -69.00 -28.00   0.50    0.18    -- -102.00  61.00-150.00   82
 22  \w    -84.00   2.00   0.50    0.05    --  -42.05 104.00  41.00  172
 23  \w   -106.00 -27.00   0.50    0.18    -- -102.00 104.00  41.00  158
 24  \w   -175.00 -85.00   0.50    0.18    -- -102.00-104.00 -59.00  180
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0099711000
_diffrn_orient_matrix_UB_12      0.0968049000
_diffrn_orient_matrix_UB_13      -0.0277956000
_diffrn_orient_matrix_UB_21      0.0347036000
_diffrn_orient_matrix_UB_22      -0.0148550000
_diffrn_orient_matrix_UB_23      -0.0646356000
_diffrn_orient_matrix_UB_31      -0.0553393000
_diffrn_orient_matrix_UB_32      -0.0268462000
_diffrn_orient_matrix_UB_33      -0.0647644000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_unetI/netI     0.0209
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            28645
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.820
_diffrn_reflns_theta_min         3.476
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.202
_exptl_absorpt_correction_T_max  0.458
_exptl_absorpt_correction_T_min  0.451
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark violet'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.440
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2616
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.664
_refine_diff_density_min         -0.889
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         6061
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0307
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0488P)^2^+10.4170P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0833
_refine_ls_wR_factor_ref         0.0839
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5665
_reflns_number_total             6061
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc02407h2.cif
_cod_data_source_block           201006_so85
_cod_database_code               1564070
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ru S N C H'
_shelx_estimated_absorpt_t_max   0.509
_shelx_estimated_absorpt_t_min   0.423
_diffrn_oxdiff_digest_frames
;
01a65b2b01ffc7b21796f166acd14b757100097a5de
;
_diffrn_oxdiff_digest_hkl
;
01099f343e9282ddb24154a1ae6ae308b14cd0
;
_reflns_odcompleteness_completeness 99.84
_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:
 C7(H7), C13(H13), C20(H20), C25(H25), C15(H15), C19(H19), C9(H9), C10(H10),
 C22(H22), C26(H26), C24(H24), C31(H31), C12(H12), C30(H30), C6(H6), C2(H2),
 C11(H11), C34(H34), C16(H16), C18(H18), C33(H33), C23(H23), C17(H17), C3(H3),
 C4(H4), C5(H5)
2.b Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C)
;
_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 1.749
_oxdiff_exptl_absorpt_empirical_full_min 0.495