Synthesis and charge transfer characteristics of a ruthenium‒acetylide complex
Kuhrt, Robert; Ho, Po-Yuen; Hantusch, Martin; Lissel, Franziska; Blacque, Olivier; Knupfer, Martin; Büchner, Bernd; RSC Advances 10 (2020) 43242–43247; doi:10.1039/D0RA08390A

data_7241630
_publ_section_title
;
 Synthesis and charge transfer characteristics of a ruthenium--acetylide
 complex
;
_journal_issue                   70
_journal_name_full               'RSC Advances'
_journal_page_first              43242
_journal_page_last               43247
_journal_paper_doi               10.1039/D0RA08390A
_journal_volume                  10
_journal_year                    2020
_chemical_formula_moiety         'C64 H54 P4 Ru S2'
_chemical_formula_sum            'C64 H54 P4 Ru S2'
_chemical_formula_weight         1112.14
_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             2019-03-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-06-16 deposited with the CCDC.	2020-11-18 downloaded from the CCDC.
;
_cell_angle_alpha                116.7842(13)
_cell_angle_beta                 100.5828(12)
_cell_angle_gamma                98.7407(12)
_cell_formula_units_Z            1
_cell_length_a                   9.46352(14)
_cell_length_b                   12.66738(18)
_cell_length_c                   12.98267(14)
_cell_measurement_reflns_used    21281
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      78.1630
_cell_measurement_theta_min      3.9550
_cell_volume                     1315.96(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015b)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015a)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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    -66.00  18.00   0.50    0.25    --  -54.70  57.00-150.00  168
  2  \w    -35.00  -6.00   0.50    1.00    --  -84.25  30.00-120.00   58
  3  \w    -71.00 -13.00   0.50    1.00    --  -84.25  61.00 -30.00  116
  4  \w    -92.00  -9.00   0.50    0.25    --  -54.70 125.00-120.00  166
  5  \w   -132.00 -46.00   0.50    0.25    --  -54.70 -38.00  90.00  172
  6  \w   -129.00 -70.00   0.50    0.25    --  -54.70-125.00 -60.00  118
  7  \w   -130.00 -82.00   0.50    0.25    --  -54.70 -99.00 -30.00   96
  8  \w   -132.00 -46.00   0.50    0.25    --  -54.70 -38.00  30.00  172
  9  \w     33.00 105.00   0.50    1.00    --  105.75 -77.00  90.00  144
 10  \w     96.00 178.00   0.50    1.00    --  105.75  15.00  30.00  164
 11  \w     96.00 178.00   0.50    1.00    --  105.75  15.00 -60.00  164
 12  \w     96.00 178.00   0.50    1.00    --  105.75  15.00   0.00  164
 13  \w     96.00 178.00   0.50    1.00    --  105.75  15.00-120.00  164
 14  \w     97.00 178.00   0.50    1.00    --  105.75  30.00-180.00  162
 15  \w     94.00 178.00   0.50    1.00    --  105.75  45.00 -90.00  168
 16  \w     96.00 178.00   0.50    1.00    --  105.75  15.00  90.00  164
 17  \w     35.00  71.00   0.50    1.00    --  105.75 -61.00 -90.00   72
 18  \w     30.00 109.00   0.50    1.00    --  105.75 -94.00-150.00  158
 19  \w     29.00 112.00   0.50    1.00    --  105.75-111.00   0.00  166
 20  \w     33.00 105.00   0.50    1.00    --  105.75 -77.00  30.00  144
 21  \w     35.00  71.00   0.50    1.00    --  105.75 -61.00 -30.00   72
 22  \w     30.00 109.00   0.50    1.00    --  105.75 -94.00  30.00  158
 23  \w     33.00  96.00   0.50    1.00    --  105.75 -74.00 -79.00  126
 24  \w     29.00 112.00   0.50    1.00    --  105.75-111.00 -30.00  166
 25  \w     30.00 109.00   0.50    1.00    --  105.75 -94.00 120.00  158
 26  \w     33.00 105.00   0.50    1.00    --  105.75 -77.00 120.00  144
 27  \w     35.00  71.00   0.50    1.00    --  105.75 -61.00  30.00   72
 28  \w     29.00 112.00   0.50    1.00    --  105.75-111.00  90.00  166
 29  \w     33.00 105.00   0.50    1.00    --  105.75 -77.00 150.00  144
 30  \w     35.00  71.00   0.50    1.00    --  105.75 -61.00 120.00   72
 31  \w     29.00 112.00   0.50    1.00    --  105.75-111.00  60.00  166
 32  \w     29.00 112.00   0.50    1.00    --  105.75-111.00 -90.00  166
 33  \w     33.00 105.00   0.50    1.00    --  105.75 -77.00-120.00  144
 34  \w     30.00 109.00   0.50    1.00    --  105.75 -94.00-180.00  158
 35  \w     34.00 101.00   0.50    1.00    --  105.75 -77.00-150.00  134
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1248562000
_diffrn_orient_matrix_UB_12      0.0265570000
_diffrn_orient_matrix_UB_13      0.1099338000
_diffrn_orient_matrix_UB_21      -0.0512531000
_diffrn_orient_matrix_UB_22      -0.1344297000
_diffrn_orient_matrix_UB_23      -0.0296087000
_diffrn_orient_matrix_UB_31      0.1064094000
_diffrn_orient_matrix_UB_32      -0.0348277000
_diffrn_orient_matrix_UB_33      -0.0792328000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            24930
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.496
_diffrn_reflns_theta_min         3.980
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.616
_exptl_absorpt_correction_T_max  0.855
_exptl_absorpt_correction_T_min  0.708
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.39a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_description       prism
_exptl_crystal_F_000             574
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.617
_refine_diff_density_min         -0.501
_refine_diff_density_rms         0.056
_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     341
_refine_ls_number_reflns         5369
_refine_ls_number_restraints     76
_refine_ls_restrained_S_all      1.204
_refine_ls_R_factor_all          0.0254
_refine_ls_R_factor_gt           0.0250
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0320P)^2^+0.6923P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0641
_refine_ls_wR_factor_ref         0.0643
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5251
_reflns_number_total             5369
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ra08390a2.cif
_cod_data_source_block           trans-[Ru(dppe)2T2]
_cod_original_cell_volume        1315.96(3)
_cod_database_code               7241630
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.837
_shelx_estimated_absorpt_t_min   0.655
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 S1A-C3 \\sim S1B-C3
 with sigma of 0.005
 C3-C4B \\sim C6-C5 \\sim C3-C4A
 with sigma of 0.005
 S1A-C3 \\sim S1A-C5 \\sim S1B-C6 \\sim S1B-C3
 with sigma of 0.005
 C5-C4B \\sim C6-C4A
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
C3 \\sim C4A \\sim C4B \\sim C5 \\sim C6 \\sim S1A \\sim S1B: within 2A with
sigma of 0.002 and sigma for terminal atoms of 0.005
4. Others
 Sof(C4B)=Sof(H4B)=Sof(H5B)=Sof(H6B)=Sof(S1B)=1-FVAR(1)
 Sof(C4A)=Sof(H4A)=Sof(H5A)=Sof(H6A)=Sof(S1A)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B)
5.b Aromatic/amide H refined with riding coordinates:
 C4A(H4A), C4B(H4B), C5(H5A), C5(H5B), C6(H6A), C6(H6B), C10(H10), C11(H11),
 C12(H12), C13(H13), C14(H14), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20),
  C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C28(H28), C29(H29),
 C30(H30), C31(H31), C32(H32)
;
_shelx_res_checksum              38917