Organometallic single-molecule electronics: tuning electron transport through X(diphosphine)2FeC4Fe(diphosphine)2X building blocks by varying the Fe-X-Au anchoring scheme from coordinative to covalent.
Lissel, Franziska; Schwarz, Florian; Blacque, Olivier; Riel, Heike; Lörtscher, Emanuel; Venkatesan, Koushik; Berke, Heinz; Journal of the American Chemical Society 136 (2014) 14560–14569; doi:10.1021/ja507672g

data_4129267
_publ_section_title
;
 Organometallic single-molecule electronics: tuning electron transport
 through X(diphosphine)2FeC4Fe(diphosphine)2X building blocks by varying
 the Fe-X-Au anchoring scheme from coordinative to covalent.
;
_journal_issue                   41
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14560
_journal_page_last               14569
_journal_paper_doi               10.1021/ja507672g
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'C46 H96 Fe2 N2 P8 Se2, 3(C6 H6)'
_chemical_formula_sum            'C64 H114 Fe2 N2 P8 Se2'
_chemical_formula_weight         1428.95
_chemical_name_systematic
'(\m^2^-Buta-1,3-diyne-1,4-diyl){tetrakis[ethane-1,2-diylbis(diethylphosphane-\k<i>P</i>)]}bis(selenocyanato-\k<i>N</i>)diiron benzene solvate (1:2)'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2013-11-20
_audit_creation_method
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4709)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.994(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.0294(7)
_cell_length_b                   19.4329(7)
_cell_length_c                   18.4637(10)
_cell_measurement_reflns_used    4815
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      32.9
_cell_measurement_theta_min      2.9
_cell_volume                     3571.8(3)
_computing_cell_refinement
;
CrysAlisPro, Version 1.171.33.55 (Oxford Diffraction Ltd., 2010)
;
_computing_data_collection
;
CrysAlisPro, Version 1.171.33.55 (Oxford Diffraction Ltd., 2010)
;
_computing_data_reduction
;
CrysAlisPro, Version 1.171.33.55 (Oxford Diffraction Ltd., 2010)
;
_computing_molecular_graphics    'Mercury (Macrae et al., 2006)'
_computing_publication_material
;
Mercury (Macrae et al., 2006)
Olex2 (Dolomanov et al., 2009)
PLATON for Windows (Spek, 2003)
PublCIF (Westrip, 2010)
ShelXL2013 (Sheldrick, 2008) 
WinGX (Farrugia, 1999)
;
_computing_structure_refinement  'ShelXL2013 (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      183(2)
_diffrn_detector_area_resol_mean 10.4498
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0157037000
_diffrn_orient_matrix_UB_12      -0.0050669000
_diffrn_orient_matrix_UB_13      -0.0360274000
_diffrn_orient_matrix_UB_21      0.0631045000
_diffrn_orient_matrix_UB_22      0.0161810000
_diffrn_orient_matrix_UB_23      0.0095069000
_diffrn_orient_matrix_UB_31      0.0291156000
_diffrn_orient_matrix_UB_32      -0.0323452000
_diffrn_orient_matrix_UB_33      0.0104070000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0827
_diffrn_reflns_av_unetI/netI     0.0888
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            26409
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.930
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.642
_exptl_absorpt_correction_T_max  0.905
_exptl_absorpt_correction_T_min  0.799
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
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            orange
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_description       prism
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.788
_refine_diff_density_min         -0.718
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         6537
_refine_ls_number_restraints     124
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0999
_refine_ls_R_factor_gt           0.0628
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0691P)^2^+1.0536P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1413
_refine_ls_wR_factor_ref         0.1682
_reflns_number_gt                4341
_reflns_number_total             6537
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja507672g_si_002.cif
_cod_data_source_block           7
_cod_database_code               4129267
_shelxl_version_number           2013-4
_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
 C10A-C11A \\sim C10B-C11B
 with sigma of 0.005
 P1-C4A \\sim P1-C4B \\sim P2-C5A \\sim P2-C5B
 with sigma of 0.005
 C4A-C5A \\sim C4B-C5B
 with sigma of 0.005
 P4-C20A \\sim P4-C20B
 with sigma of 0.005
 C20A-C21A \\sim C20B-C21B
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
C20B \\sim C21B \\sim C20A \\sim C21A: within 3A with sigma of 0.01 and sigma
for terminal atoms of 0.02
C10A \\sim C10B \\sim C11A \\sim C11B: within 1.7A with sigma of 0.005 and
sigma for terminal atoms of 0.01
C4A \\sim C4B \\sim C5A \\sim C5B: within 3A with sigma of 0.005 and sigma for
terminal atoms of 0.01
C14 \\sim C15: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01
4. Others
 Sof(C10B)=Sof(H10C)=Sof(H10D)=Sof(C11B)=Sof(H11D)=Sof(H11E)=Sof(H11F)=
 Sof(C12B)=Sof(H12C)=Sof(H12D)=Sof(C13B)=Sof(H13D)=Sof(H13E)=Sof(H13F)=1-FVAR(1)
 Sof(C10A)=Sof(H10A)=Sof(H10B)=Sof(C11A)=Sof(H11A)=Sof(H11B)=Sof(H11C)=
 Sof(C12A)=Sof(H12A)=Sof(H12B)=Sof(C13A)=Sof(H13A)=Sof(H13B)=Sof(H13C)=FVAR(1)
 Sof(C5B)=Sof(H5BA)=Sof(H5BB)=Sof(C4B)=Sof(H4BA)=Sof(H4BB)=1-FVAR(2)
 Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=FVAR(2)
 Sof(C20B)=Sof(H20A)=Sof(H20B)=Sof(C21B)=Sof(H21A)=Sof(H21B)=Sof(H21C)=1-FVAR(3)
 Sof(C20A)=Sof(H20C)=Sof(H20D)=Sof(C21A)=Sof(H21D)=Sof(H21E)=Sof(H21F)=FVAR(3)
5.a Secondary CH2 refined with riding coordinates:
 C4A(H4AA,H4AB), C5B(H5BA,H5BB), C6(H6A,H6B), C8(H8A,H8B), C10A(H10A,H10B),
 C10B(H10C,H10D), C12A(H12A,H12B), C12B(H12C,H12D), C14(H14A,H14B), C15(H15A,
 H15B), C16(H16A,H16B), C18(H18A,H18B), C22(H22A,H22B), C4B(H4BA,H4BB),
 C5A(H5AA,H5AB), C20B(H20A,H20B), C20A(H20C,H20D)
5.b Aromatic/amide H refined with riding coordinates:
 C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30),
 C31(H31), C32(H32)
5.c Fitted hexagon refined as free rotating group:
 C24(C25,C26,C27,C28,C29)
5.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C11A(H11A,H11B,H11C), C11B(H11D,H11E,H11F),
 C13A(H13A,H13B,H13C), C13B(H13D,H13E,H13F), C17(H17A,H17B,H17C), C19(H19A,H19B,
 H19C), C23(H23A,H23B,H23C), C21B(H21A,H21B,H21C), C21A(H21D,H21E,H21F)
;