Three-Coordinate, 12-Electron Organometallic Complexes of Iron(II) Supported by a Bulky β-Diketiminate Ligand: Synthesis and Insertion of CO To Give Square-Pyramidal Complexes
Smith, Jeremy M.; Lachicotte, Rene J.; Holland, Patrick L.; Organometallics 21 (2002) 4808–; doi:10.1021/om020571v

data_4077089
_publ_section_title
;
 Three-Coordinate, 12-Electron Organometallic Complexes of Iron(II)
 Supported by a Bulky \b-Diketiminate Ligand:&#x00A0; Synthesis and
 Insertion of CO To Give Square-Pyramidal Complexes
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_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              4808
_journal_paper_doi               10.1021/om020571v
_journal_volume                  21
_journal_year                    2002
_chemical_formula_sum            'C40 H64 Fe N2'
_chemical_formula_weight         628.78
_chemical_name_systematic
; 
 2,2,6,6-tetramethyl-3,5-bis(2,6-diisopropylphenylimido)heptyl
  neopentyl iron(ii) 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 96.7710(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.7226(7)
_cell_length_b                   18.1877(12)
_cell_length_c                   21.7853(15)
_cell_measurement_temperature    293(2)
_cell_volume                     3825.5(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.946
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0151
_diffrn_reflns_av_sigmaI/netI    0.0166
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            23521
_diffrn_reflns_theta_full        28.26
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         1.46
_exptl_absorpt_coefficient_mu    0.421
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.805
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.092
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.44
_refine_diff_density_max         1.103
_refine_diff_density_min         -0.828
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         8948
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0625
_refine_ls_shift/su_max          0.130
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1082P)^2^+3.8369P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1818
_refine_ls_wR_factor_ref         0.1885
_reflns_number_gt                7720
_reflns_number_total             8948
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om020571v.cif
_cod_data_source_block           LFeCH2tBu
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'na' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
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_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4077089