Mixed-Valence Dinitrogen-Bridged Fe(0)/Fe(II) Complex
Leslie D. Field; Ruth W. Guest; Peter Turner; Inorganic Chemistry 49 (2010) 9086–9093; doi:10.1021/ic101646p

data_4316686
_publ_section_title
;
 Mixed-Valence Dinitrogen-Bridged Fe(0)/Fe(II) Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9086
_journal_page_last               9093
_journal_paper_doi               10.1021/ic101646p
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C88 H86 B2 F48 Fe2 N2 P8'
_chemical_formula_weight         2464.67
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                106.01(3)
_cell_angle_beta                 92.18(3)
_cell_angle_gamma                93.96(3)
_cell_formula_units_Z            1
_cell_length_a                   13.091(3)
_cell_length_b                   14.036(3)
_cell_length_c                   14.726(3)
_cell_measurement_reflns_used    7657
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.68
_cell_measurement_theta_min      2.39
_cell_volume                     2590.1(11)
_computing_cell_refinement       'SAINT (Bruker,1995)'
_computing_data_collection       'SMART (Bruker,1995)'
_computing_data_reduction        'SAINT and XPREP (Bruker 1995)'
_computing_molecular_graphics
;
  xtal 3.6 (Hall,du Boulay, D.J. & Olthof-Hazekamp, R. 1999)
  ORTEPII  (Johnson,C.K., 1976). 
  WinGX (Farrugia, 1999)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrcik, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_crystal_treatment
;
attached with Exxon Paratone N, to a short length 
of fibre supported on a thin piece of copper wire 
inserted in a copper mounting pin.  The crystal was 
quenched in a cold nitrogen gas stream from an 
Oxford Cryosystems Cryostream. 
;
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0792
_diffrn_reflns_av_sigmaI/netI    0.0882
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25893
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.06
_diffrn_reflns_theta_min         1.44
_diffrn_standards_decay_%        0.28
_diffrn_standards_number         151
_exptl_absorpt_coefficient_mu    0.5350
_exptl_absorpt_correction_T_max  0.9044
_exptl_absorpt_correction_T_min  0.7048
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
  Gaussian (Coppens et al., 1965)
  WinGX  (Bruker, 1995)
  PLATON (Spek, 1990)
  A grid of  8 x  8 x  8 =   512 sampling points was used
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular prism'
_exptl_crystal_F_000             1242
_exptl_crystal_size_max          0.337
_exptl_crystal_size_mid          0.313
_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.744
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     725
_refine_ls_number_reflns         11999
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0762
_refine_ls_R_factor_gt           0.0479
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+0.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.1013
_reflns_number_gt                7958
_reflns_number_total             11999
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101646p_si_001_1.cif
_cod_data_source_block           ldf05sh4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Gaussian'
changed to 'gaussian' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

data name '_atom_site_symetry_multiplicity' was replaced with
'_atom_site_symmetry_multiplicity' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_cell_volume        2590.2(9)
_cod_database_code               4316686
_exptl_absorpt_correction_t_ave  0.8577