Synthesis, Electrochemistry, and Single-Molecule Conductance of Bimetallic 2,3,5,6-Tetra(pyridine-2-yl)pyrazine-Based Complexes.
Davidson, Ross; Liang, Jing-Hong; Costa Milan, David; Mao, Bing-Wei; Nichols, Richard J.; Higgins, Simon J.; Yufit, Dmitry S.; Beeby, Andrew; Low, Paul J.; Inorganic chemistry 54 (2015) 5487–5494; doi:10.1021/acs.inorgchem.5b00507

data_4342854
_publ_section_title
;
 Synthesis, Electrochemistry, and Single-Molecule Conductance of
 Bimetallic 2,3,5,6-Tetra(pyridine-2-yl)pyrazine-Based Complexes.
;
_journal_issue                   11
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5487
_journal_page_last               5494
_journal_paper_doi               10.1021/acs.inorgchem.5b00507
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C72 H50 N12 Ru2 S2, 4(F6 P), 2(C2 H3 N)'
_chemical_formula_sum            'C76 H56 F24 N14 P4 Ru2 S2'
_chemical_formula_weight         2011.49
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-06-24
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2014.06.23 svn.r2946 for OlexSys, GUI svn.r4855)
;
_cell_angle_alpha                99.100(2)
_cell_angle_beta                 90.219(2)
_cell_angle_gamma                115.547(2)
_cell_formula_units_Z            2
_cell_length_a                   12.926(2)
_cell_length_b                   13.311(2)
_cell_length_c                   29.507(4)
_cell_measurement_reflns_used    9451
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      31.11
_cell_measurement_theta_min      2.33
_cell_volume                     4508.1(12)
_computing_cell_refinement       'APEX2 v.2013.4_1 (Bruker, 2013)'
_computing_data_collection       'APEX2 v.2013.4_1 (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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      120.0
_diffrn_detector                 'Bruker PHOTON 100 CMOS'
_diffrn_detector_type            'CMOS sensor'
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device       'Bruker D8 Venture'
_diffrn_measurement_device_type  D8Venture
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  'focusing mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0823
_diffrn_reflns_av_unetI/netI     0.1529
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            64726
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.10
_diffrn_source                   'ImuS microsource'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.550
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6212
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1164 before and 0.0896 after correction.
The Ratio of minimum to maximum transmission is 0.6212.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'dull dark black'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2012
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.27
_refine_diff_density_max         1.786
_refine_diff_density_min         -1.359
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1092
_refine_ls_number_reflns         19134
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.1399
_refine_ls_R_factor_gt           0.0961
_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^)+(0.1500P)^2^+6.6000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2575
_refine_ls_wR_factor_ref         0.2777
_reflns_number_gt                12235
_reflns_number_total             19134
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b00507_si_002.cif
_cod_data_source_block           4_14srv161
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 4342852--4342854.cif.
;
_cod_database_code               4342854
_computing.bruker_data_scaling   'SADABS V2012/1 (Bruker AXS Inc.)'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 S1-C48B
 1.71 with sigma of 0.005
 P2-F9A \\sim P2-F9B \\sim P2-F12B \\sim P2-F12A \\sim P2-F11B \\sim P2-F11A
\\sim P2-F7B \\sim P2-F7A ~
 P2-F10 \\sim P2-F8
 with sigma of 0.005
 N13-C1A \\sim N1S-C1S
 with sigma of 0.005
 C2S-C1S \\sim C1B-C1A
 with sigma of 0.005
 S1-C48B \\sim S1-C48A
 with sigma of 0.005
3. Others
 Fixed Sof: C48B(0.6) H48A(0.6) H48B(0.6) H48C(0.6) F7A(0.5) F7B(0.5) F9A(0.5)
 F9B(0.5) F11A(0.5) F11B(0.5) F12B(0.5) F12A(0.5) N1S(0.5) C1S(0.5) C2S(0.5)
 H2SA(0.5) H2SB(0.5) H2SC(0.5) N13(0.5) C1A(0.5) C1B(0.5) H1BA(0.5) H1BB(0.5)
 H1BC(0.5) C48A(0.4) H1CA(0.4) H1CB(0.4) H1CC(0.4)
4.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C11(H11), C12(H12), C13(H13), C14(H14),
 C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22), C23(H23), C24(H24),
  C25(H25), C26(H26), C27(H27), C28(H28), C31(H31), C33(H33), C36(H36),
 C37(H37), C38(H38), C39(H39), C43(H43), C44(H44), C46(H46), C47(H47), C49(H49),
  C50(H50), C51(H51), C52(H52), C55(H55), C57(H57), C60(H60), C61(H61),
 C62(H62), C63(H63), C67(H67), C68(H68), C70(H70), C71(H71)
4.b Idealised Me refined as rotating group:
 C48B(H48A,H48B,H48C), C72(H72A,H72B,H72C), C2S(H2SA,H2SB,H2SC), C4S(H4SA,H4SB,
 H4SC), C1B(H1BA,H1BB,H1BC), C48A(H1CA,H1CB,H1CC)
;