"Doping" of Polyyne with an Organometallic Fragment Leads to Highly Conductive Metallapolyyne Molecular Wire.
Tanaka, Yuya; Kato, Yuya; Tada, Tomofumi; Fujii, Shintaro; Kiguchi, Manabu; Akita, Munetaka; Journal of the American Chemical Society 140 (2018) 10080–10084; doi:10.1021/jacs.8b04484

data_4132521
_publ_section_title
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 &quot;Doping&quot; of Polyyne with an Organometallic Fragment Leads to
 Highly Conductive Metallapolyyne Molecular Wire.
;
_journal_issue                   32
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10080
_journal_page_last               10084
_journal_paper_doi               10.1021/jacs.8b04484
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C74 H66 P4 Ru Si2, C6 H6'
_chemical_formula_sum            'C80 H72 P4 Ru Si2'
_chemical_formula_weight         1314.51
_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'
_symmetry_Int_Tables_number      15
_audit_creation_date             2017-01-19
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5289)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.375(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.639(5)
_cell_length_b                   10.0264(17)
_cell_length_c                   25.445(4)
_cell_measurement_reflns_used    4733
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.27
_cell_measurement_theta_min      2.28
_cell_volume                     6740(2)
_computing_cell_refinement       'SAINT V8.35A (?, 2016)'
_computing_data_reduction        'SAINT V8.35A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.9975
_diffrn_measured_fraction_theta_max 0.9975
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0602
_diffrn_reflns_av_unetI/netI     0.0846
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            15107
_diffrn_reflns_theta_full        25.0253
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.54
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.407
_exptl_absorpt_correction_T_max  0.976
_exptl_absorpt_correction_T_min  0.957
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0807 before and 0.0535 after correction.
The Ratio of minimum to maximum transmission is 0.6975.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark yellow'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.2954
_exptl_crystal_description       plate
_exptl_crystal_F_000             2736.0
_exptl_crystal_recrystallization_method 'slow diffusion of Benzene/MeOH'
_exptl_crystal_size_max          0.107
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.4281
_refine_diff_density_min         -1.4960
_refine_diff_density_rms         0.2195
_refine_ls_d_res_high            0.8401
_refine_ls_d_res_low             13.2094
_refine_ls_goodness_of_fit_ref   1.1077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    99
_refine_ls_number_parameters     449
_refine_ls_number_reflns         5941
_refine_ls_number_restraints     426
_refine_ls_restrained_S_all      1.0669
_refine_ls_R_factor_all          0.1291
_refine_ls_R_factor_gt           0.0856
_refine_ls_shift/su_max          0.0005
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+140.4049P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1806
_refine_ls_wR_factor_ref         0.1996
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              31
_reflns_limit_h_min              -31
_reflns_limit_k_max              11
_reflns_limit_k_min              0
_reflns_limit_l_max              30
_reflns_limit_l_min              0
_reflns_number_gt                3988
_reflns_number_total             5941
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ja8b04484_si_004.cif
_cod_data_source_block           2^4
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4132521
_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
 C26a-P2
 1.81 with sigma of 0.02
 C25a-P1
 1.81 with sigma of 0.02
 C26a-C25a
 1.54 with sigma of 0.02
 C26a-P1
 2.86 with sigma of 0.04
 C25a-P2
 2.86 with sigma of 0.04
3. Rigid bond restraints
 C1, C2, C3, C4, C5, C6, C1a, C2a, C3a, C4a, C5a, C6a
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C19, C20, C21, C22, C23, C24, C19a, C20a, C21a, C22a, C23a, C24a
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C26, C25, C25a, C26a
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C40, C39, C38, C39, C40, C41
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C1a \\sim C2a \\sim C3a
\\sim C4a \\sim C5a \\sim C6a: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C19a \\sim C20a
\\sim C21a \\sim C22a \\sim C23a \\sim C24a: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
C26 \\sim C25 \\sim C25a \\sim C26a: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C41 \\sim C40 \\sim C39 \\sim C38 \\sim C39 \\sim C40: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C1a) \\sim Ueq, Uanis(C2a)
\\sim Ueq, Uanis(C3a) \\sim Ueq, Uanis(C4a) \\sim Ueq, Uanis(C5a) \\sim Ueq,
Uanis(C6a) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C19) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C22)
\\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C19a) \\sim Ueq,
Uanis(C20a) \\sim Ueq, Uanis(C21a) \\sim Ueq, Uanis(C22a) \\sim Ueq,
Uanis(C23a) \\sim Ueq, Uanis(C24a) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C25a) \\sim Ueq, Uanis(C26a) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C25)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C39) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C40)
\\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C38) \\sim Ueq: with sigma of 0.1 and
sigma for terminal atoms of 0.2
5. Others
 Sof(C1a)=Sof(C2a)=Sof(C3a)=Sof(C4a)=Sof(C5a)=Sof(C6a)=Sof(C25a)=Sof(C26a)=
 Sof(C19a)=Sof(C20a)=Sof(C21a)=Sof(C22a)=Sof(C23a)=Sof(C24a)=Sof(H24a)=
 Sof(H23a)=Sof(H22a)=Sof(H21a)=Sof(H20a)=Sof(H6a)=Sof(H5a)=Sof(H4a)=Sof(H3a)=
 Sof(H2a)=Sof(H25c)=Sof(H25d)=Sof(H26c)=Sof(H26d)=1-FVAR(1)
 Sof(C1)=Sof(C2)=Sof(C3)=Sof(C4)=Sof(C5)=Sof(C6)=Sof(C19)=Sof(C20)=Sof(C21)=
 Sof(C22)=Sof(C23)=Sof(C24)=Sof(C25)=Sof(C26)=Sof(H24)=Sof(H23)=Sof(H22)=
 Sof(H21)=Sof(H20)=Sof(H6)=Sof(H5)=Sof(H4)=Sof(H3)=Sof(H2)=Sof(H26a)=Sof(H26b)=
 Sof(H25a)=Sof(H25b)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C26(H26a,H26b), C25(H25a,H25b), C25a(H25c,H25d), C26a(H26c,H26d)
6.b Me refined with riding coordinates:
 C36(H36a,H36b,H36c), C35(H35a,H35b,H35c), C37(H37a,H37b,H37c)
6.c Aromatic/amide H refined with riding coordinates:
 C18(H18), C17(H17), C16(H16), C15(H15), C14(H14), C24(H24), C23(H23),
 C22(H22), C21(H21), C20(H20), C24a(H24a), C23a(H23a), C22a(H22a), C21a(H21a),
 C20a(H20a), C6(H6), C5(H5), C4(H4), C3(H3), C2(H2), C12(H12), C11(H11),
 C10(H10), C9(H9), C8(H8), C6a(H6a), C5a(H5a), C4a(H4a), C3a(H3a), C2a(H2a),
 C39(H39), C40(H40), C41(H41), C38(H38)
6.d Fitted hexagon refined as free rotating group:
 C13(C14,C15,C16,C17,C18), C7(C8,C9,C10,C11,C12), C1(C2,C3,C4,C5,C6), C19(C20,
 C21,C22,C23,C24), C1a(C2a,C3a,C4a,C5a,C6a), C19a(C20a,C21a,C22a,C23a,C24a)
;
_olex2_submission_special_instructions 'No special instructions were received'