Low-Coordinate Iron(II) Amido Complexes of β-Diketiminates: Synthesis, Structure, and Reactivity
Nathan A. Eckert; Jeremy M. Smith; Rene J. Lachicotte; Patrick L. Holland; Inorganic Chemistry 43 (2004) 3306–3321; doi:10.1021/ic035483x

data_4311033
_publ_section_title
;
 Low-Coordinate Iron(II) Amido Complexes of \b-Diketiminates: Synthesis,
 Structure, and Reactivity
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3306
_journal_page_last               3321
_journal_paper_doi               10.1021/ic035483x
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C39 H63 Fe N3'
_chemical_formula_weight         629.77
_chemical_name_common            holne02
_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                 96.464(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.7000(11)
_cell_length_b                   17.906(2)
_cell_length_c                   21.821(3)
_cell_measurement_temperature    192(2)
_cell_volume                     3766.0(8)
_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      192(2)
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.955
_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
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_diffrn_reflns_av_R_equivalents  0.0734
_diffrn_reflns_av_sigmaI/netI    0.1245
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
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_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14136
_diffrn_reflns_theta_full        23.32
_diffrn_reflns_theta_max         23.32
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    0.429
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.111
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.310
_refine_diff_density_min         -2.473
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
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_refine_ls_number_reflns         5218
_refine_ls_number_restraints     0
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_refine_ls_R_factor_all          0.2373
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_refine_ls_shift/su_mean         0.031
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4248
_refine_ls_wR_factor_ref         0.4496
_reflns_number_gt                2937
_reflns_number_total             5218
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035483xsi20031224_095602_15.cif
_cod_data_source_block           L(tBu)FeNHtBu
_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.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

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 
;
_cod_original_cell_volume        3766.0(7)
_cod_database_code               4311033