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_4085279
_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 H100 Fe2 I2 P8'
_chemical_formula_sum            'C50 H100 Fe2 I2 P8'
_chemical_formula_weight         1314.56
_chemical_name_systematic
(\m^2^-1,4-Benzenediethynyl)-tetrakis(ethane-1,2-diylbis(diethylphosphine))-diiodo-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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.748(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.5189(4)
_cell_length_b                   9.9102(2)
_cell_length_c                   18.2717(3)
_cell_measurement_reflns_used    18605
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      32.43
_cell_measurement_theta_min      2.86
_cell_volume                     2963.87(11)
_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
;
<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  ' SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    ' SHELXS97 (Sheldrick, 2008) '
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 10.4498
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_sigmaI/netI    0.0314
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            47537
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         3.05
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.779
_exptl_absorpt_correction_T_max  0.890
_exptl_absorpt_correction_T_min  0.633
_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.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             1356
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.722
_refine_diff_density_min         -1.061
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         8570
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0375
_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^)+(0.0396P)^2^+6.3761P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0902
_refine_ls_wR_factor_ref         0.0985
_reflns_number_gt                7514
_reflns_number_total             8570
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500602m_si_002.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 4085279--4085285.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4085279
_shelx_hkl_checksum              9892