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_4129266
_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         'C54 H114 Fe2 P8 Sn2, C6 H6'
_chemical_formula_sum            'C60 H120 Fe2 P8 Sn2'
_chemical_formula_weight         1438.39
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90.9394(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.0064(3)
_cell_length_b                   18.7974(4)
_cell_length_c                   19.7398(3)
_cell_measurement_reflns_used    25295
_cell_measurement_temperature    183(1)
_cell_measurement_theta_max      30.6
_cell_measurement_theta_min      2.3
_cell_volume                     7051.5(2)
_computing_cell_refinement
;
CrysAlisPro, version 1.171.36.20 (Agilent Technologies, 2012)
;
_computing_data_collection
;
CrysAlisPro, version 1.171.36.24a (Agilent Technologies, 2012)
;
_computing_data_reduction
;
CrysAlisPro, version 1.171.36.20 (Agilent Technologies, 2012)
;
_computing_molecular_graphics    'Mercury (Macrae et al., 2006)'
_computing_publication_material
;
Mercury (Macrae et al., 2006)
PLATON for Windows (Spek, 2003)
PublCIF (Westrip, 2010)
ShelXL97 (Sheldrick, 2008) 
WinGX (Farrugia, 1999)
;
_computing_structure_refinement  'ShelXL97 (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      183(1)
_diffrn_detector_area_resol_mean 10.3801
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0105968000
_diffrn_orient_matrix_UB_12      -0.0286963000
_diffrn_orient_matrix_UB_13      0.0211442000
_diffrn_orient_matrix_UB_21      -0.0334136000
_diffrn_orient_matrix_UB_22      -0.0162490000
_diffrn_orient_matrix_UB_23      -0.0048620000
_diffrn_orient_matrix_UB_31      0.0127492000
_diffrn_orient_matrix_UB_32      -0.0184170000
_diffrn_orient_matrix_UB_33      -0.0286331000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0576
_diffrn_reflns_av_unetI/netI     0.0466
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            65475
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         2.310
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.319
_exptl_absorpt_correction_T_max  0.913
_exptl_absorpt_correction_T_min  0.800
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
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            yellow
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_description       plate
_exptl_crystal_F_000             3008
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.881
_refine_diff_density_min         -0.956
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     758
_refine_ls_number_reflns         15409
_refine_ls_number_restraints     236
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0799
_refine_ls_R_factor_gt           0.0647
_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^)+(0.0638P)^2^+40.1507P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1661
_refine_ls_wR_factor_ref         0.1769
_reflns_number_gt                12244
_reflns_number_total             15409
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja507672g_si_002.cif
_cod_data_source_block           5
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4129266
_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
 C20-C21A \\sim C20-C21B
 with sigma of 0.005
 C49-C50A \\sim C49-C50B
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
C16 \\sim C17: within 3A with sigma of 0.01 and sigma for terminal atoms of 0.02
C20 \\sim C21A \\sim C21B: within 3A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C49 \\sim C50A \\sim C50B: within 3A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Sn1A \\sim Sn1B: within 3A with sigma of 0.002 and sigma for terminal atoms of
0.004
Sn2A \\sim Sn2B: within 3A with sigma of 0.002 and sigma for terminal atoms of
0.004
C55 \\sim C56 \\sim C57 \\sim C58 \\sim C59 \\sim C60: within 3A with sigma of
0.02 and sigma for terminal atoms of 0.04
C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65 \\sim C66: within 3A with sigma of
0.02 and sigma for terminal atoms of 0.04
4. Others
 Sof(Sn1B)=1-FVAR(1)
 Sof(Sn1A)=FVAR(1)
 Sof(Sn2B)=1-FVAR(2)
 Sof(Sn2A)=FVAR(2)
 Sof(H20C)=Sof(H20D)=Sof(C21B)=Sof(H21D)=Sof(H21E)=Sof(H21F)=1-FVAR(3)
 Sof(H20A)=Sof(H20B)=Sof(C21A)=Sof(H21A)=Sof(H21B)=Sof(H21C)=FVAR(3)
 Sof(H49C)=Sof(H49D)=Sof(C50B)=Sof(H50D)=Sof(H50E)=Sof(H50F)=1-FVAR(4)
 Sof(H49A)=Sof(H49B)=Sof(C50A)=Sof(H50A)=Sof(H50B)=Sof(H50C)=FVAR(4)
 Sof(C66)=Sof(H66)=Sof(C61)=Sof(H61)=Sof(C62)=Sof(H62)=Sof(C63)=Sof(H63)=
 Sof(C64)=Sof(H64)=Sof(C65)=Sof(H65)=1-FVAR(5)
 Sof(C55)=Sof(H55)=Sof(C56)=Sof(H56)=Sof(C57)=Sof(H57)=Sof(C58)=Sof(H58)=
 Sof(C59)=Sof(H59)=Sof(C60)=Sof(H60)=FVAR(5)
5.a :
 C55(C56,C57,C58,C59,C60), C66(C61,C62,C63,C64,C65)
5.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C12(H12A,H12B), C14(H14A,H14B),
 C16(H16A,H16B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C22(H22A,H22B),
  C24(H24A,H24B), C26(H26A,H26B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,
 H37B), C39(H39A,H39B), C41(H41A,H41B), C43(H43A,H43B), C45(H45A,H45B),
 C46(H46A,H46B), C47(H47A,H47B), C49(H49A,H49B), C51(H51A,H51B), C53(H53A,H53B)
5.c Aromatic/amide H refined with riding coordinates:
 C55(H55), C56(H56), C57(H57), C58(H58), C59(H59), C60(H60), C66(H66),
 C61(H61), C62(H62), C63(H63), C64(H64), C65(H65)
5.d Idealised Me refined as rotating group:
 C5A(H5AA,H5AB,H5AC), C6A(H6AA,H6AB,H6AC), C7A(H7AA,H7AB,H7AC), C11(H11A,H11B,
 H11C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C),
 C21A(H21A,H21B,H21C), C21B(H21D,H21E,H21F), C23(H23A,H23B,H23C), C25(H25A,H25B,
 H25C), C27(H27A,H27B,H27C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,
 H34B,H34C), C38(H38A,H38B,H38C), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C),
 C44(H44A,H44B,H44C), C48(H48A,H48B,H48C), C50A(H50A,H50B,H50C), C50B(H50D,H50E,
 H50F), C52(H52A,H52B,H52C), C54(H54A,H54B,H54C)
;