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_4302050
_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         'C42 H62 Fe N6'
_chemical_formula_sum            'C42 H62 Fe N6'
_chemical_formula_weight         706.83
_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                 96.083(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.3610(9)
_cell_length_b                   13.2578(8)
_cell_length_c                   18.1805(9)
_cell_measurement_reflns_used    2401
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      20.07
_cell_measurement_theta_min      3.05
_cell_volume                     3921.3(4)
_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 0.999
_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  0.0583
_diffrn_reflns_av_sigmaI/netI    0.0541
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17487
_diffrn_reflns_theta_full        20.82
_diffrn_reflns_theta_max         20.82
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    0.421
_exptl_absorpt_correction_T_max  0.9591
_exptl_absorpt_correction_T_min  0.8496
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    1.197
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.214
_refine_diff_density_min         -0.247
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     611
_refine_ls_number_reflns         4096
_refine_ls_number_restraints     1146
_refine_ls_restrained_S_all      0.965
_refine_ls_R_factor_all          0.0796
_refine_ls_R_factor_gt           0.0598
_refine_ls_shift/su_max          0.589
_refine_ls_shift/su_mean         0.032
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0459P)^2^+5.1279P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1173
_refine_ls_wR_factor_ref         0.1263
_reflns_number_gt                3342
_reflns_number_total             4096
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801623m_si_004_2.cif
_cod_data_source_block           at1
_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_sg_symbol_H-M      P2(1)/n
_cod_database_code               4302050