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_4126380
_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         'C75 H58 O3 Os P3 S2, C H2 Cl2, B F4, H2 O'
_chemical_formula_sum            'C76 H63 B Cl2 F4 O4 Os P3 S2'
_chemical_formula_weight         1545.20
_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     direct
_audit_creation_date             2017-05-23
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                90
_cell_angle_beta                 100.4787(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.65604(17)
_cell_length_b                   24.1742(4)
_cell_length_c                   24.0038(4)
_cell_measurement_reflns_used    8782
_cell_measurement_temperature    197.7(6)
_cell_measurement_theta_max      62.2510
_cell_measurement_theta_min      3.6500
_cell_volume                     6650.88(19)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_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      197.7(6)
_diffrn_detector_area_resol_mean 16.1903
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
  1 omega  -94.00  -61.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -32.3066 -178.0000    0.0000 33

  2 omega -100.00  -59.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -32.3066 -178.0000  -90.0000 41

  3 omega -111.00  -59.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -32.3066 -178.0000   60.0000 52

  4 omega  -38.00   97.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       32.3066    0.0000 -120.0000 135

  5 omega -131.00 -101.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -86.0000 -112.0000   90.0000 30

  6 omega   81.00  160.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  112.0000 -180.0000 79

  7 omega   22.00   71.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  -38.0000   90.0000 49

  8 omega   40.00   66.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  -25.0000  -60.0000 26

  9 omega   22.00   80.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000 -112.0000  120.0000 58

 10 omega   41.00   67.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  -38.0000  -60.0000 26

 11 omega   69.00  125.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000   50.0000 -150.0000 56

 12 omega   27.00   90.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000 -112.0000  150.0000 63

 13 omega   67.00  112.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  -64.0000   90.0000 45

 14 omega   21.00   63.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  -25.0000  -90.0000 42

 15 omega   21.00   53.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  -25.0000 -120.0000 32

 16 omega   24.00  124.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  -77.0000 -120.0000 100
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.1045510000
_diffrn_orient_matrix_UB_12      0.0296606000
_diffrn_orient_matrix_UB_13      -0.0363370000
_diffrn_orient_matrix_UB_21      -0.0782035000
_diffrn_orient_matrix_UB_22      -0.0501693000
_diffrn_orient_matrix_UB_23      0.0063119000
_diffrn_orient_matrix_UB_31      -0.0316795000
_diffrn_orient_matrix_UB_32      0.0258597000
_diffrn_orient_matrix_UB_33      0.0538507000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_unetI/netI     0.0505
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            22601
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        62.137
_diffrn_reflns_theta_max         62.136
_diffrn_reflns_theta_min         3.657
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.146
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97993
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_description       block
_exptl_crystal_F_000             3116
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.842
_refine_diff_density_min         -0.655
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     847
_refine_ls_number_reflns         10407
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0309
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0325P)^2^+1.4488P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0718
_refine_ls_wR_factor_ref         0.0758
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9183
_reflns_number_total             10407
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b06400_si_003.cif
_cod_data_source_block           2
_cod_original_cell_volume        6650.88(18)
_cod_database_code               4126380
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     61.08
_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, All O(H,H) groups
2. Shared sites
{C21, S2A}
{S2, C21A}
3. Uiso/Uaniso restraints and constraints
Uanis(C21) = Uanis(S2A)
Uanis(S2) = Uanis(C21A)
4. Others
 Sof(H18A)=Sof(H20A)=Sof(S2A)=Sof(C21A)=Sof(H21A)=1-FVAR(1)
 Sof(S2)=Sof(C21)=Sof(H21)=Sof(H18)=Sof(H20)=FVAR(1)
5.a Free rotating group:
 O1S(H1SC,H1SD)
5.b Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C115(H115), C235(H235), C211(H211), C231(H231), C125(H125),
 C135(H135), C9(H9), C212(H212), C13(H13), C325(H325), C321(H321), C232(H232),
 C214(H214), C215(H215), C124(H124), C315(H315), C234(H234), C134(H134),
 C131(H131), C221(H221), C225(H225), C312(H312), C132(H132), C121(H121),
 C133(H133), C322(H322), C335(H335), C111(H111), C14(H14), C314(H314),
 C311(H311), C213(H213), C233(H233), C21(H21), C18(H18), C18(H18A), C112(H112),
 C313(H313), C323(H323), C114(H114), C224(H224), C16(H16), C122(H122),
 C331(H331), C113(H113), C20(H20), C20(H20A), C324(H324), C332(H332),
 C223(H223), C222(H222), C333(H333), C123(H123), C334(H334), C21A(H21A)
5.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C)
;
_olex2_submission_special_instructions 'No special instructions were received'