Synthesis of Bis(imino)pyridine Iron Di- and Monoalkyl Complexes: Stability Differences between FeCH2SiMe3and FeCH2CMe3Derivatives
Fernández, Ignacio; Trovitch, Ryan J.; Lobkovsky, Emil; Chirik, Paul J.; Organometallics 27 (2008) 109–; doi:10.1021/om700913g

data_4070656
_publ_section_title
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 Synthesis of Bis(imino)pyridine Iron Di- and Monoalkyl Complexes:
 Stability Differences between FeCH2SiMe3and FeCH2CMe3Derivatives
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_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              109
_journal_paper_doi               10.1021/om700913g
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety         'C34 H46 Fe N3'
_chemical_formula_sum            'C34 H46 Fe N3'
_chemical_formula_weight         552.59
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   32.313(5)
_cell_length_b                   9.3004(13)
_cell_length_c                   22.451(4)
_cell_measurement_reflns_used    2391
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      19.84
_cell_measurement_theta_min      2.21
_cell_volume                     6747.1(19)
_computing_cell_refinement       'Bruker SAINT+'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT+'
_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      133(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker X8 APEX II diffractometer'
_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  0.0730
_diffrn_reflns_av_sigmaI/netI    0.0650
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            25068
_diffrn_reflns_theta_full        23.29
_diffrn_reflns_theta_max         23.29
_diffrn_reflns_theta_min         1.26
_exptl_absorpt_coefficient_mu    0.471
_exptl_absorpt_correction_T_max  0.8717
_exptl_absorpt_correction_T_min  0.7988
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.088
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2376
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_platon_squeeze_details          ' ?'
_refine_diff_density_max         2.897
_refine_diff_density_min         -0.637
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         4869
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1057
_refine_ls_R_factor_gt           0.0794
_refine_ls_shift/su_max          0.347
_refine_ls_shift/su_mean         0.013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1481P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2060
_refine_ls_wR_factor_ref         0.2215
_reflns_number_gt                3314
_reflns_number_total             4869
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700913g-file003.cif
_cod_data_source_block           rt24
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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 
;
_cod_original_cell_volume        6747.1(18)
_cod_original_sg_symbol_H-M      Pbcn
_cod_database_code               4070656