Electron-Deficient Iron Alkyl Complexes Supported by Diimine Ligand (Ph2CN)2C2H4: Evidence for Reversible Ethylene Binding
Volbeda, Jeroen; Meetsma, Auke; Bouwkamp, Marco W.; Organometallics 28 (2009) 209–; doi:10.1021/om8006773

data_4068309
_publ_section_related_literature
;
;
_publ_section_title
;
 Electron-Deficient Iron Alkyl Complexes Supported by Diimine Ligand
 (Ph2CN)2C2H4: Evidence for Reversible Ethylene Binding
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              209
_journal_paper_doi               10.1021/om8006773
_journal_volume                  28
_journal_year                    2009
_chemical_compound_source        'see text'
_chemical_formula_moiety
'C56 H48 Fe N4, 2(C22 H11 B F15 Si), 2(C6 H5 Br)0.5'
_chemical_formula_sum            'C106 H75 B2 Br F30 Fe N4 Si2'
_chemical_formula_weight         2188.28
_chemical_name_systematic        ?
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   direct
_audit_creation_date             '2008-05-29  16:07:39'
_audit_creation_method
;
 PLATON <TABLE ACC> option    (version :: 110308)
 SHELXL97-2 & Manual Editing 
;
_audit_update_record
;
 ?
;
_cell_angle_alpha                87.520(4)
_cell_angle_beta                 88.489(4)
_cell_angle_gamma                66.821(4)
_cell_formula_units_Z            2
_cell_length_a                   14.484(3)
_cell_length_b                   18.160(4)
_cell_length_c                   20.298(4)
_cell_measurement_reflns_used    5103
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      27.67
_cell_measurement_theta_min      2.48
_cell_volume                     4903.2(18)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2007)'
_computing_data_collection       'SMART (Bruker, 2007)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2007)'
_computing_molecular_graphics
;
 PLATON (Spek, 2003)
 PLUTO (Meetsma, 2008) 
;
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution
;
 DIRDIF-08 (Beurskens et al., 2008)
;
_diffrn_ambient_temperature      100(1)
_diffrn_detector_area_resol_mean 66.06
_diffrn_measured_fraction_theta_full 0.926
_diffrn_measured_fraction_theta_max 0.926
_diffrn_measurement_device_type
;
  Bruker Smart Apex; CCD area detector 
;
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_detector
;
  CCD area-detector
;
_diffrn_radiation_monochromator  'parallel mounted graphite'
_diffrn_radiation_source         'fine focus sealed Siemens Mo tube '
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.2796
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            14434
_diffrn_reflns_reduction_process
;
 Intensity data were corrected for Lorentz and polarization
  effects, decay and absorption and reduced to F~o~^2^
  using SAINT-Plus & SADABS (Bruker, 2007).
;
_diffrn_reflns_theta_full        24.11
_diffrn_reflns_theta_max         24.11
_diffrn_reflns_theta_min         2.48
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.694
_exptl_absorpt_correction_T_max  0.9201
_exptl_absorpt_correction_T_min  0.7743
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, (Bruker, 2007))'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2216
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.027
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.881
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1258
_refine_ls_number_reflns         14434
_refine_ls_number_restraints     1218
_refine_ls_restrained_S_all      0.857
_refine_ls_R_factor_all          0.1897
_refine_ls_R_factor_gt           0.0849
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0749P)^2^+0.0P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1790
_refine_ls_wR_factor_ref         0.2098
_reflns_number_gt                5648
_reflns_number_total             14434
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om8006773_si_007.cif
_cod_data_source_block           DATNAM
_cod_original_formula_sum        'C106 H75 B2 Br1 F30 Fe N4 Si2'
_cod_database_code               4068309
_vrn_publ_code_void_volume       574.0
_vrn_publ_code_number_frames     1800
_vrn_publ_code_frame_time_sec    10.0
_vrn_publ_code_meas_time_hour    7.8