Structural and Electronic Variations of sp/sp2Carbon-Based Bridges in Di- and Trinuclear Redox-Active Iron Complexes Bearing Fe(diphosphine)2X (X = I, NCS) Moieties
Lissel, Franziska; Blacque, Olivier; Venkatesan, Koushik; Berke, Heinz; Organometallics 34 (2015) 408–; doi:10.1021/om500602m

data_4085285
_publ_section_title
;
 Structural and Electronic Variations of sp/sp2Carbon-Based Bridges in Di-
 and Trinuclear Redox-Active Iron Complexes Bearing Fe(diphosphine)2X (X =
 I, NCS) Moieties
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              408
_journal_paper_doi               10.1021/om500602m
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C50 H98 Fe2 N2 P8 S3'
_chemical_formula_sum            'C50 H98 Fe2 N2 P8 S3'
_chemical_formula_weight         1182.98
_chemical_name_systematic
(\m^2^-2,5-Thiophenediethynyl)-tetrakis(ethane-1,2-diylbis(diethylphosphine))-bis(isothiocyanato)-diiron
_space_group_IT_number           14
_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   geom
_audit_creation_date             2014-09-09
_audit_creation_method
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 117.489(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.8328(4)
_cell_length_b                   20.0399(4)
_cell_length_c                   18.9596(4)
_cell_measurement_reflns_used    16749
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      28.71
_cell_measurement_theta_min      2.28
_cell_volume                     6010.6(3)
_computing_cell_refinement
;
CrysAlisPro, version 1.171.36.20 ((Agilent Technologies, 2012)
;
_computing_data_collection
;
CrysAlisPro, version 1.171.36.20 (Agilent Technologies, 2012)
;
_computing_data_reduction
;
CrysAlisPro, version 1.171.36.20 (Agilent Technologies, 2012)
;
_computing_molecular_graphics
;
<i>ORTEP-3 for Windows</i> (Farrugia, 1997) and/or <i>Mercury</i> (Macrae et
al.,
2006)
;
_computing_publication_material
; 
<i>WinGX</i> (Farrugia, 1999), <i>PLATON for Windows</i> (Spek, 2003) and
<i>publCIF</i> (Westrip, 2010)
;
_computing_structure_refinement  ' SHELXL2013 (Sheldrick, 2008)'
_computing_structure_solution    ' SHELXS97 (Sheldrick, 2008) '
_diffrn_ambient_temperature      183(1)
_diffrn_detector                 'Atlas CCD camera on \k goniostat'
_diffrn_detector_area_resol_mean 10.3801
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.889
_diffrn_measurement_device_type
'Oxford Diffraction SuperNova, dual radiation diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0582
_diffrn_reflns_av_sigmaI/netI    0.0529
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            69260
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.78
_diffrn_reflns_theta_min         2.37
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.834
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_correction_T_min  0.851
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Version 1.171.36.20 (Agilent Technologies, 2012)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid (1995).
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2528
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.126
_refine_diff_density_min         -1.421
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     578
_refine_ls_number_reflns         13916
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.1383
_refine_ls_R_factor_gt           0.1044
_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^)+(0.0099P)^2^+64.1384P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2110
_refine_ls_wR_factor_ref         0.2259
_reflns_number_gt                10152
_reflns_number_total             13916
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500602m_si_002.cif
_cod_data_source_block           9
_cod_depositor_comments
'Adding full bibliography for 4085279--4085285.cif.'
_cod_original_cell_volume        6010.6(2)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4085285
_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
 Fe2-P5A = Fe2-P5B = Fe2-P6A = Fe2-P6B
 2.25025 with sigma of 0.005
 Fe2-P7A = Fe2-P7B = Fe2-P8A = Fe2-P8B
 2.25025 with sigma of 0.005
 P7B-C45B = P6B-C32B = P8A-C42A = P6B-C39B
 1.82 with sigma of 0.005
 P8B-C47B = P7B-C41B = P7A-C43A = P5B-C31B = P5A-C35A
 1.82 with sigma of 0.005
 P7B-C46B
 2.78 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C31A) = Uanis(C32A) = Uanis(C33A) = Uanis(C34A) = Uanis(C35A) =
Uanis(C36A) = Uanis(C37A) = Uanis(C38A) = Uanis(C39A) = Uanis(C40A) =
Uanis(C41A) = Uanis(C42A) = Uanis(C43A) = Uanis(C44A) = Uanis(C45A) =
Uanis(C46A) = Uanis(C47A) = Uanis(C48A) = Uanis(C49A) = Uanis(C50A) =
Uanis(C31B) = Uanis(C32B) = Uanis(C33B) = Uanis(C34B) = Uanis(C35B) =
Uanis(C36B) = Uanis(C37B) = Uanis(C38B) = Uanis(C39B) = Uanis(C40B) =
Uanis(C41B) = Uanis(C42B) = Uanis(C43B) = Uanis(C44B) = Uanis(C45B) =
Uanis(C46B) = Uanis(C47B) = Uanis(C48B) = Uanis(C49B) = Uanis(C50B)
4. Same fragment restrains
{C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12, C13, C14, C15, C16, C17, C18,
C19, C20, C21}
as
{C31A, C32A, C33A, C34A, C35A, C36A, C37A, C38A, C39A, C40A, C41A, C42A, C43A,
C44A, C45A, C46A, C47A, C48A, C49A, C50A}
{C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12, C13, C14, C15, C16, C17, C18,
C19, C20, C21}
as
{C31B, C32B, C33B, C34B, C35B, C36B, C37B, C38B, C39B, C40B, C41B, C42B, C43B,
C44B, C45B, C46B, C47B, C48B, C49B, C50B}
5. Others
 Sof(C31B)=Sof(H31C)=Sof(H31D)=Sof(C32B)=Sof(H32C)=Sof(H32D)=Sof(C33B)=
 Sof(H33C)=Sof(H33D)=Sof(C34B)=Sof(H34D)=Sof(H34E)=Sof(H34F)=Sof(C35B)=
 Sof(H35C)=Sof(H35D)=Sof(C36B)=Sof(H36D)=Sof(H36E)=Sof(H36F)=Sof(C37B)=
 Sof(H37C)=Sof(H37D)=Sof(C38B)=Sof(H38D)=Sof(H38E)=Sof(H38F)=Sof(C39B)=
 Sof(H39C)=Sof(H39D)=Sof(C40B)=Sof(H40D)=Sof(H40E)=Sof(H40F)=Sof(C41B)=
 Sof(H41C)=Sof(H41D)=Sof(C42B)=Sof(H42C)=Sof(H42D)=Sof(C43B)=Sof(H43C)=
 Sof(H43D)=Sof(C44B)=Sof(H44D)=Sof(H44E)=Sof(H44F)=Sof(C45B)=Sof(H45C)=
 Sof(H45D)=Sof(C46B)=Sof(H46D)=Sof(H46E)=Sof(H46F)=Sof(C47B)=Sof(H47C)=
 Sof(H47D)=Sof(C48B)=Sof(H48D)=Sof(H48E)=Sof(H48F)=Sof(C49B)=Sof(H49C)=
 Sof(H49D)=Sof(C50B)=Sof(H50D)=Sof(H50E)=Sof(H50F)=Sof(P5B)=Sof(P6B)=Sof(P7B)=
 Sof(P8B)=1-FVAR(1)
 Sof(C31A)=Sof(H31A)=Sof(H31B)=Sof(C32A)=Sof(H32A)=Sof(H32B)=Sof(C33A)=
 Sof(H33A)=Sof(H33B)=Sof(C34A)=Sof(H34A)=Sof(H34B)=Sof(H34C)=Sof(C35A)=
 Sof(H35A)=Sof(H35B)=Sof(C36A)=Sof(H36A)=Sof(H36B)=Sof(H36C)=Sof(C37A)=
 Sof(H37A)=Sof(H37B)=Sof(C38A)=Sof(H38A)=Sof(H38B)=Sof(H38C)=Sof(C39A)=
 Sof(H39A)=Sof(H39B)=Sof(C40A)=Sof(H40A)=Sof(H40B)=Sof(H40C)=Sof(C41A)=
 Sof(H41A)=Sof(H41B)=Sof(C42A)=Sof(H42A)=Sof(H42B)=Sof(C43A)=Sof(H43A)=
 Sof(H43B)=Sof(C44A)=Sof(H44A)=Sof(H44B)=Sof(H44C)=Sof(C45A)=Sof(H45A)=
 Sof(H45B)=Sof(C46A)=Sof(H46A)=Sof(H46B)=Sof(H46C)=Sof(C47A)=Sof(H47A)=
 Sof(H47B)=Sof(C48A)=Sof(H48A)=Sof(H48B)=Sof(H48C)=Sof(C49A)=Sof(H49A)=
 Sof(H49B)=Sof(C50A)=Sof(H50A)=Sof(H50B)=Sof(H50C)=Sof(P5A)=Sof(P6A)=Sof(P7A)=
 Sof(P8A)=FVAR(1)
 1(DFIX)=1(DFIX)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C6(H6A,H6B), C8(H8A,H8B), C10(H10A,
 H10B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C16(H16A,H16B),
 C18(H18A,H18B), C20(H20A,H20B), C31A(H31A,H31B), C32A(H32A,H32B), C33A(H33A,
 H33B), C35A(H35A,H35B), C37A(H37A,H37B), C39A(H39A,H39B), C41A(H41A,H41B),
 C42A(H42A,H42B), C43A(H43A,H43B), C45A(H45A,H45B), C47A(H47A,H47B), C49A(H49A,
 H49B), C31B(H31C,H31D), C32B(H32C,H32D), C33B(H33C,H33D), C35B(H35C,H35D),
 C37B(H37C,H37D), C39B(H39C,H39D), C41B(H41C,H41D), C42B(H42C,H42D), C43B(H43C,
 H43D), C45B(H45C,H45D), C47B(H47C,H47D), C49B(H49C,H49D)
6.b Me refined with riding coordinates:
 C34A(H34A,H34B,H34C), C36A(H36A,H36B,H36C), C38A(H38A,H38B,H38C), C40A(H40A,
 H40B,H40C), C44A(H44A,H44B,H44C), C46A(H46A,H46B,H46C), C48A(H48A,H48B,H48C),
 C50A(H50A,H50B,H50C), C34B(H34D,H34E,H34F), C36B(H36D,H36E,H36F), C38B(H38D,
 H38E,H38F), C40B(H40D,H40E,H40F), C44B(H44D,H44E,H44F), C46B(H46D,H46E,H46F),
 C48B(H48D,H48E,H48F), C50B(H50D,H50E,H50F)
6.c Aromatic/amide H refined with riding coordinates:
 C25(H25), C26(H26)
6.d Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C),
 C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C21(H21A,H21B,
 H21C)
;
_shelx_res_checksum              46477
_shelx_hkl_checksum              4206