Reduction Chemistry of Aryl- and Alkyl-Substituted Bis(imino)pyridine Iron Dihalide Compounds: Molecular and Electronic Structures of [(PDI)2Fe] Derivatives
Bradley M. Wile; Ryan J. Trovitch; Suzanne C. Bart; Aaron M. Tondreau; Emil Lobkovsky; Carsten Milsmann; Eckhard Bill; Karl Wieghardt; Paul J. Chirik; Inorganic Chemistry 48 (2009) 4190–4200; doi:10.1021/ic801623m

data_4302048
_publ_section_title
;
Reduction Chemistry of Aryl- and Alkyl-Substituted Bis(imino)pyridine Iron
Dihalide Compounds: Molecular and Electronic Structures of [(PDI)2Fe]
Derivatives
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4190
_journal_page_last               4200
_journal_paper_doi               10.1021/ic801623m
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C30 H46 Fe N6'
_chemical_formula_sum            'C30 H46 Fe N6'
_chemical_formula_weight         546.58
_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                 119.165(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.7390(5)
_cell_length_b                   16.4698(8)
_cell_length_c                   20.7204(10)
_cell_measurement_reflns_used    3544
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.93
_cell_measurement_theta_min      2.39
_cell_volume                     2902.2(3)
_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      173(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0651
_diffrn_reflns_av_sigmaI/netI    0.0679
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            26087
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    0.549
_exptl_absorpt_correction_T_max  0.9472
_exptl_absorpt_correction_T_min  0.8104
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.355
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         5867
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0999
_refine_ls_R_factor_gt           0.0491
_refine_ls_shift/su_max          0.333
_refine_ls_shift/su_mean         0.016
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0558P)^2^+0.5510P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1074
_refine_ls_wR_factor_ref         0.1269
_reflns_number_gt                3584
_reflns_number_total             5867
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801623m_si_003.cif
_cod_data_source_block           bw4
_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 
;
_cod_original_cell_volume        2902.2(2)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4302048