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_4088815
_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         'C90 H94 N2 O4 P2 Pt'
_chemical_formula_sum            'C90 H94 N2 O4 P2 Pt'
_chemical_formula_weight         1524.70
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-06-20
_audit_creation_method
;
  Olex2 1.2-beta
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                71.273(5)
_cell_angle_beta                 86.786(4)
_cell_angle_gamma                71.249(4)
_cell_formula_units_Z            1
_cell_length_a                   9.5706(4)
_cell_length_b                   13.1673(6)
_cell_length_c                   16.6608(9)
_cell_measurement_reflns_used    4629
_cell_measurement_temperature    120
_cell_measurement_theta_max      24.3260
_cell_measurement_theta_min      3.1600
_cell_volume                     1880.28(17)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 16.1511
_diffrn_measured_fraction_theta_full 0.9993
_diffrn_measured_fraction_theta_max 0.9022
_diffrn_measurement_details
;
  1 omega  -57.00   41.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.3337   77.0000    0.0000 98

  2 omega  -79.00  -38.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.3337  116.0000 -159.0000 41

  3 omega  -50.00   25.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.3337   38.0000 -150.0000 75

  4 omega  -84.00  -14.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.3337  -57.0000   60.0000 70

  5 omega -101.00   -5.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.3337  -38.0000 -150.0000 96

  6 omega   36.00   79.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       28.9587 -116.0000  112.0000 43

  7 omega   -2.00   64.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       28.9587   19.0000   30.0000 66
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0288938000
_diffrn_orient_matrix_UB_12      -0.0140337000
_diffrn_orient_matrix_UB_13      0.0407650000
_diffrn_orient_matrix_UB_21      0.0714466000
_diffrn_orient_matrix_UB_22      -0.0359897000
_diffrn_orient_matrix_UB_23      0.0176096000
_diffrn_orient_matrix_UB_31      0.0142517000
_diffrn_orient_matrix_UB_32      0.0459839000
_diffrn_orient_matrix_UB_33      0.0073796000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0719
_diffrn_reflns_av_unetI/netI     0.1127
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17913
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.54
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.962
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.756
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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)
;
_exptl_crystal_colour            'dull light yellow'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             788
_exptl_crystal_size_max          0.2302
_exptl_crystal_size_mid          0.0751
_exptl_crystal_size_min          0.0466
_refine_diff_density_max         1.373
_refine_diff_density_min         -0.697
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     450
_refine_ls_number_reflns         8632
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0535
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0340P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0994
_refine_ls_wR_factor_ref         0.1048
_reflns_number_gt                7746
_reflns_number_total             8632
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00472_si_001.cif
_cod_data_source_block           7_13srv186
_cod_original_cell_volume        1880.29(16)
_cod_database_code               4088815
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.44
_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.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,
 H20B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B),
 C26(H26A,H26B)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C12(H12), C13(H13), C14(H14), C15(H15), 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)
2.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C27(H27A,H27B,H27C)
;