Synthesis and characterization of a semiconducting and solution-processable ruthenium-based polymetallayne
Ho, Po-Yuen; Komber, Hartmut; Horatz, Kilian; Tsuda, Takuya; Mannsfeld, Stefan C. B.; Dmitrieva, Evgenia; Blacque, Olivier; Kraft, Ulrike; Sirringhaus, Henning; Lissel, Franziska; Polymer Chemistry 11 (2020) 472–479; doi:10.1039/C9PY01090D

data_1552372
_publ_section_title
;
 Synthesis and characterization of a semiconducting and
 solution-processable ruthenium-based polymetallayne
;
_journal_issue                   2
_journal_name_full               'Polymer Chemistry'
_journal_page_first              472
_journal_page_last               479
_journal_paper_doi               10.1039/C9PY01090D
_journal_volume                  11
_journal_year                    2020
_chemical_formula_moiety         'C64 H52 Br2 P4 Ru S2'
_chemical_formula_sum            'C64 H52 Br2 P4 Ru S2'
_chemical_formula_weight         1269.94
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-03-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-07-22 deposited with the CCDC.    2019-10-03 downloaded from the CCDC.
;
_cell_angle_alpha                117.037(2)
_cell_angle_beta                 96.017(2)
_cell_angle_gamma                103.315(2)
_cell_formula_units_Z            1
_cell_length_a                   9.3882(2)
_cell_length_b                   12.9082(2)
_cell_length_c                   13.5032(3)
_cell_measurement_reflns_used    23521
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      78.2110
_cell_measurement_theta_min      3.7930
_cell_volume                     1376.31(6)
_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 0.998
_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    -43.00  25.00   0.50    1.00    --  -51.70  38.00 -90.00  136
  2  \w    -35.00  -6.00   0.50    4.00    --  -84.25  30.00-150.00   58
  3  \w    -66.00  21.00   0.50    1.00    --  -51.70  57.00  30.00  174
  4  \w    -26.00  28.00   0.50    1.00    --  -51.70  19.00 150.00  108
  5  \w     30.00  98.00   0.50    1.00    --   51.70-125.00 -90.00  136
  6  \w     83.00 108.00   0.50    4.00    --  105.75 -94.00-150.00   50
  7  \w     90.00 126.00   0.50    4.00    --  105.75 -84.00-126.45   72
  8  \w     83.00 112.00   0.50    4.00    --  105.75-111.00 -90.00   58
  9  \w     79.00 108.00   0.50    4.00    --  105.75-111.00-150.00   58
 10  \w     59.00  96.00   0.50    4.00    --  105.75 -77.00-180.00   74
 11  \w     47.00  74.00   0.50    4.00    --  105.75-111.00 -90.00   54
 12  \w     73.00 102.00   0.50    4.00    --  105.75 -94.00 -60.00   58
 13  \w     78.00 104.00   0.50    4.00    --  105.75-111.00  30.00   52
 14  \w     60.00 109.00   0.50    4.00    --  105.75 -94.00  30.00   98
 15  \w     73.00 112.00   0.50    4.00    --  105.75-111.00 120.00   78
 16  \w     77.00 111.00   0.50    4.00    --  105.75-111.00 150.00   68
 17  \w     57.00  82.00   0.50    4.00    --  105.75 -94.00 150.00   50
 18  \w     43.00  70.00   0.50    4.00    --  105.75 -61.00 150.00   54
 19  \w     43.00  69.00   0.50    4.00    --  105.75 -61.00 120.00   52
 20  \w     48.00 109.00   0.50    4.00    --  105.75 -94.00  60.00  122
 21  \w     39.00  76.00   0.50    4.00    --  105.75 -77.00 -30.00   74
 22  \w     35.00  71.00   0.50    4.00    --  105.75 -61.00 -30.00   72
 23  \w     29.00 112.00   0.50    4.00    --  105.75-111.00   0.00  166
 24  \w     35.00  71.00   0.50    4.00    --  105.75 -61.00  90.00   72
 25  \w     33.00 105.00   0.50    4.00    --  105.75 -77.00  30.00  144
 26  \w     96.00 178.00   0.50    4.00    --  105.75  15.00  90.00  164
 27  \w    125.00 175.00   0.50    4.00    --  105.75  45.00   0.00  100
 28  \w    133.00 177.00   0.50    4.00    --  105.75  30.00 -30.00   88
 29  \w    133.00 178.00   0.50    4.00    --  105.75  77.00 -90.00   90
 30  \w    139.00 164.00   0.50    4.00    --  105.75 111.00-150.00   50
 31  \w    108.00 133.00   0.50    4.00    --  105.75 111.00-150.00   50
 32  \w    106.00 153.00   0.50    4.00    --  105.75 111.00-120.00   94
 33  \w    106.00 132.00   0.50    4.00    --  105.75  77.00-180.00   52
 34  \w     94.00 141.00   0.50    4.00    --  105.75 124.00-148.47   94
 35  \w     94.00 178.00   0.50    4.00    --  105.75  45.00 -60.00  168
 36  \w    115.00 153.00   0.50    4.00    --  105.75  30.00   0.00   76
 37  \w    113.00 139.00   0.50    4.00    --  105.75  61.00  30.00   52
 38  \w    106.00 178.00   0.50    4.00    --  105.75  30.00  30.00  144
 39  \w    110.00 160.00   0.50    4.00    --  105.75 111.00 150.00  100
 40  \w    114.00 139.00   0.50    4.00    --  105.75 178.00  30.00   50
 41  \w     59.00 150.00   0.50    4.00    --  105.75 178.00 -60.00  182
 42  \w     85.00 129.00   0.50    4.00    --  105.75  77.00 -90.00   88
 43  \w     92.00 142.00   0.50    4.00    --  105.75  61.00 -60.00  100
 44  \w     35.00  71.00   0.50    4.00    --  105.75 -61.00-180.00   72
 45  \w     29.00 112.00   0.50    4.00    --  105.75-111.00-180.00  166
 46  \w     33.00 105.00   0.50    4.00    --  105.75 -77.00-150.00  144
 47  \w     35.00  71.00   0.50    4.00    --  105.75 -61.00 -60.00   72
 48  \w     30.00 109.00   0.50    4.00    --  105.75 -94.00 -90.00  158
 49  \w     33.00 105.00   0.50    4.00    --  105.75 -77.00   0.00  144
 50  \w     35.00  68.00   0.50    4.00    --  105.75 -61.00-120.00   66
 51  \w     31.00  58.00   0.50    4.00    --  105.75-111.00-150.00   54
 52  \w     34.00  59.00   0.50    4.00    --  105.75 -94.00-150.00   50
 53  \w     33.00  65.00   0.50    4.00    --  105.75 -84.00-126.45   64
 54  \w     30.00 109.00   0.50    4.00    --  105.75 -94.00  90.00  158
 55  \w     30.00 109.00   0.50    4.00    --  105.75 -94.00 120.00  158
 56  \w     33.00 105.00   0.50    4.00    --  105.75 -77.00  90.00  144
 57  \w     86.00 114.00   0.50    4.00    --  105.75  77.00 150.00   56
 58  \w   -125.00 -30.00   0.50    1.00    --  -51.70 -77.00 150.00  190
 59  \w   -130.00 -43.00   0.50    1.00    --  -51.70 -19.00  30.00  174
 60  \w   -127.00 -82.00   0.50    1.00    --  -51.70 -99.00 150.00   90
 61  \w   -127.00 -82.00   0.50    1.00    --  -51.70 -99.00   0.00   90
 62  \w   -125.00 -76.00   0.50    1.00    --  -51.70 -86.00-172.00   98
;
_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      -0.1680880000
_diffrn_orient_matrix_UB_12      -0.0250220000
_diffrn_orient_matrix_UB_13      -0.0478069000
_diffrn_orient_matrix_UB_21      0.0366779000
_diffrn_orient_matrix_UB_22      0.0022619000
_diffrn_orient_matrix_UB_23      -0.1076993000
_diffrn_orient_matrix_UB_31      -0.0245335000
_diffrn_orient_matrix_UB_32      -0.1388648000
_diffrn_orient_matrix_UB_33      -0.0594966000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_av_unetI/netI     0.0194
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            29985
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.489
_diffrn_reflns_theta_min         3.787
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.129
_exptl_absorpt_correction_T_max  0.892
_exptl_absorpt_correction_T_min  0.628
_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            yellow
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_description       plate
_exptl_crystal_F_000             642
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.293
_refine_diff_density_min         -1.441
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         5629
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0312
_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^)+(0.0500P)^2^+1.2715P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0833
_refine_ls_wR_factor_ref         0.0837
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5455
_reflns_number_total             5629
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9py01090d2.cif
_cod_data_source_block           fran1203
_cod_depositor_comments
;Adding full bibliography for 1552372.cif.

 Adding full bibliography for 1552372.cif.
;
_cod_original_cell_volume        1376.31(5)
_cod_database_code               1552372
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.887
_shelx_estimated_absorpt_t_min   0.481
_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:
 C7(H7A,H7B), C8(H8A,H8B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), 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              79019