Switching of Charge Transport Pathways via Delocalization Changes in Single-molecule Metallacycles Junctions.
Li, Ruihao; Lu, Zhengyu; Cai, Yuanting; Jiang, Feng; Tang, Chun; Chen, Zhixin; Zheng, Jueting; Pi, Jiuchan; Zhang, Rui; Liu, Junyang; Chen, Zhao-Bin; Yang, Yang; Shi, Jia; Hong, Wenjing; Xia, Haiping; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b06400

data_4126381
_publ_section_title
;
 Switching of Charge Transport Pathways via Delocalization Changes in
 Single-molecule Metallacycles Junctions.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b06400
_journal_year                    2017
_chemical_formula_moiety         'C57 H44 O3 Os P2 S2, 5(C4 H8 O2)'
_chemical_formula_sum            'C77 H84 O13 Os P2 S2'
_chemical_formula_weight         1533.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-01-21
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_cell_angle_alpha                90
_cell_angle_beta                 103.7050(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7051(2)
_cell_length_b                   18.7402(2)
_cell_length_c                   24.2360(3)
_cell_measurement_reflns_used    16652
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      71.7870
_cell_measurement_theta_min      4.7130
_cell_volume                     6929.97(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4741
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
  1 omega  113.00  162.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      103.3446  125.0000   60.0000 49

  2 omega   78.00  178.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      103.3446   30.0000   90.0000 100

  3 omega   79.00  105.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      103.3446  -94.0000   60.0000 26

  4 omega   53.00  122.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      103.3446  -61.0000   90.0000 69

  5 omega   56.00  109.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      103.3446  -94.0000    0.0000 53

  6 omega   83.00  108.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      103.3446  -94.0000  -90.0000 25

  7 omega   38.00   90.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      103.3446  -30.0000  -60.0000 52

  8 omega   31.00   66.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      103.3446  -30.0000   60.0000 35

  9 omega   34.00   59.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      103.3446  -94.0000   60.0000 25

 10 omega   23.00   98.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       40.5672 -125.0000 -120.0000 75

 11 omega   29.00   63.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      103.3446  -30.0000 -180.0000 34

 12 omega  -37.00    1.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5672   37.0000 -180.0000 38

 13 omega  -37.00   41.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5672   19.0000  -60.0000 78

 14 omega  -49.00  -12.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5672   37.0000   30.0000 37
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0429571000
_diffrn_orient_matrix_UB_12      0.0636840000
_diffrn_orient_matrix_UB_13      -0.0231995000
_diffrn_orient_matrix_UB_21      -0.0458290000
_diffrn_orient_matrix_UB_22      0.0517145000
_diffrn_orient_matrix_UB_23      0.0330703000
_diffrn_orient_matrix_UB_31      0.0789566000
_diffrn_orient_matrix_UB_32      -0.0044488000
_diffrn_orient_matrix_UB_33      0.0515552000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_av_unetI/netI     0.0398
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            26083
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        65.000
_diffrn_reflns_theta_max         65.000
_diffrn_reflns_theta_min         3.736
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.000
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50571
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_description       block
_exptl_crystal_F_000             3152
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.942
_refine_diff_density_min         -1.617
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     860
_refine_ls_number_reflns         11776
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0435
_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^)+(0.0750P)^2^+13.4088P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1146
_refine_ls_wR_factor_ref         0.1165
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11122
_reflns_number_total             11776
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b06400_si_003.cif
_cod_data_source_block           3
_cod_database_code               4126381
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_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
 C15S-C16S
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C15S) \\sim Ueq, Uanis(C16S) \\sim Ueq, Uanis(C14S) \\sim Ueq,
Uanis(C17S) \\sim Ueq, Uanis(C20S) \\sim Ueq, Uanis(C11) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Uiso: H(-0.001)
5.a Secondary CH2 refined with riding coordinates:
 C6S(H6SA,H6SB), C5S(H5SA,H5SB), C9S(H9SA,H9SB), C10S(H10A,H10B), C7S(H7SA,
 H7SB), C8S(H8SA,H8SB), C3S(H3SA,H3SB), C4S(H4SA,H4SB), C2S(H2SA,H2SB),
 C19S(H19A,H19B), C1S(H1SA,H1SB), C11S(H11D,H11E), C12S(H12A,H12B), C18S(H18A,
 H18B), C13S(H13A,H13B), C14S(H14A,H14B), C16S(H16A,H16B), C15S(H15A,H15B),
 C17S(H17A,H17B), C20S(H20A,H20B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C14(H14), C9(H9), C5(H5), C13(H13), C131(H131), C16(H16),
 C225(H225), C135(H135), C111(H111), C125(H125), C221(H221), C231(H231),
 C20(H20), C232(H232), C112(H112), C224(H224), C215(H215), C235(H235),
 C115(H115), C234(H234), C233(H233), C18(H18), C132(H132), C121(H121),
 C211(H211), C21(H21), C134(H134), C133(H133), C122(H122), C124(H124),
 C212(H212), C214(H214), C213(H213), C222(H222), C113(H113), C223(H223),
 C114(H114), C123(H123)
5.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C)
;
_olex2_submission_special_instructions 'No special instructions were received'