Experimental and Computational Studies of the Single-Molecule Conductance of Ru(II) and Pt(II) trans-Bis(acetylide) Complexes
Al-Owaedi, Oday A.; Milan, David C.; Oerthel, Marie-Christine; Bock, Sören; Yufit, Dmitry S.; Howard, Judith A. K.; Higgins, Simon J.; Nichols, Richard J.; Lambert, Colin J.; Bryce, Martin R.; Low, Paul J.; Organometallics 35 (2016) 2944–; doi:10.1021/acs.organomet.6b00472

data_4088816
_publ_section_title
;
 Experimental and Computational Studies of the Single-Molecule Conductance
 of Ru(II) and Pt(II) trans-Bis(acetylide) Complexes
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              2944
_journal_paper_doi               10.1021/acs.organomet.6b00472
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C94 H100 O4 P2 Pt S2'
_chemical_formula_sum            'C94 H100 O4 P2 Pt S2'
_chemical_formula_weight         1614.89
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-11-12
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2014.11.07 svn.r3078 for OlexSys, GUI svn.r4941)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 118.005(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   22.659(10)
_cell_length_b                   9.469(4)
_cell_length_c                   22.765(10)
_cell_measurement_reflns_used    4368
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.84
_cell_measurement_theta_min      2.30
_cell_volume                     4312(3)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Rigaku CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'Bruker APEX2'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 0.0350
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'CrystalLogic Kappa (4 circle)'
_diffrn_measurement_device_type  'Kappa Rigaku Saturn724+'
_diffrn_measurement_method       'omega rotation'
_diffrn_radiation_collimation    '0.3 x 1.5 Double Pinhole'
_diffrn_radiation_monochromator  'focusing mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_reflns_av_R_equivalents  0.2997
_diffrn_reflns_av_unetI/netI     0.2832
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            42922
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.97
_diffrn_source                   Synchrotron
_diffrn_source_type              'Undulator, I19, DLS, RAL'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.622
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4119
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1559 before and 0.0964 after correction.
The Ratio of minimum to maximum transmission is 0.4119.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.001
_refine_diff_density_max         2.761
_refine_diff_density_min         -1.298
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         8352
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1611
_refine_ls_R_factor_gt           0.0949
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2223
_refine_ls_wR_factor_ref         0.2517
_reflns_number_gt                4614
_reflns_number_total             8352
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00472_si_001.cif
_cod_data_source_block           18_14srv183
_cod_original_cell_volume        4313(3)
_cod_database_code               4088816
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C25-C26 \\sim C25-C26A \\sim C27-C26 \\sim C27A-C26A \\sim C28-C27 \\sim
C28A-C27A \\sim C28-C29 ~
 C28A-C29A
 with sigma of 0.005
3. Others
 Fixed Sof: H25C(0.5) H25D(0.5) H25A(0.5) H25B(0.5) C26(0.4) H26A(0.4)
 H26B(0.4) C26A(0.6) H26C(0.6) H26D(0.6) C27(0.4) H27A(0.4) H27B(0.4) C27A(0.6)
 H27C(0.6) H27D(0.6) C28(0.4) H28A(0.4) H28B(0.4) C29A(0.6) H29A(0.6) H29B(0.6)
 H29C(0.6) C28A(0.6) H28C(0.6) H28D(0.6) C29(0.4) H29D(0.4) H29E(0.4) H29F(0.4)
4.a Everything fixed:
 C26, C26A, C27, C27A, C28, C29A, C28A, C29
4.b Riding coordinates:
 C29A(H29A,H29B,H29C), C29(H29D,H29E,H29F)
4.c Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,
 H22B), C24(H24A,H24B), C25(H25C,H25D), C25(H25A,H25B), C26(H26A,H26B),
 C26A(H26C,H26D), C27(H27A,H27B), C27A(H27C,H27D), C28(H28A,H28B), C28A(H28C,
 H28D)
4.d Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C12(H12), C13(H13), C15(H15), C16(H16), C32(H32), C33(H33),
 C34(H34), C35(H35), C36(H36), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46),
  C52(H52), C53(H53), C54(H54), C55(H55), C56(H56)
4.e Fitted hexagon refined as free rotating group:
 C3(C4,C5,C6,C7,C8), C11(C12,C13,C14,C15,C16), C31(C32,C33,C34,C35,C36),
 C41(C42,C43,C44,C45,C46), C51(C52,C53,C54,C55,C56)
4.f Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C23(H23A,H23B,H23C)
;