Synthesis and Characterization of Two Intensely Colored Tris(benzoylcyanoxime)iron(II) Anionic Complexes
Travis Owen; Fernande Grandjean; Gary J. Long; Konstantin V. Domasevitch; Nikolay Gerasimchuk; Inorganic Chemistry 47 (2008) 8704–8713; doi:10.1021/ic8004322

data_4305449
_publ_contact_author_address
; 
 Department of Chemistry, 
 Temple Hall 456, 
 Missouri State University, 
 Springfield, MO 65897, USA. 
;
_publ_contact_author_email       NNGerasimchuk@missouristate.edu
_publ_contact_author_fax         '1 417 836 5507'
_publ_contact_author_name        'Prof. Nikolay Gerasimchuk'
_publ_contact_author_phone       '1 417 836 5165'
_publ_section_title
;
Synthesis and Characterization of Two Intensely Colored
Tris(benzoylcyanoxime)iron(II) Anionic Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8704
_journal_page_last               8713
_journal_paper_doi               10.1021/ic8004322
_journal_volume                  47
_journal_year                    2008
_chemical_compound_source        'synthesized new Fe(II) complex'
_chemical_formula_moiety         'C27 H15 Fe N6 O6, C24 H20 P'
_chemical_formula_sum            'C51 H35 Fe N6 O6 P'
_chemical_formula_weight         914.67
_chemical_melting_point          'oxidizes upon heating on air up to 100 C'
_chemical_name_common            'tris[benzoylcyanoximato]iron(II)}, PPh4 salt'
_chemical_name_systematic
; 
 Tetraphenylphosphonium salt of fac{tris[benzoylcyanoximato{Iron(II)]}
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                 92.4370(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.2043(12)
_cell_length_b                   25.991(3)
_cell_length_c                   13.8507(13)
_cell_measurement_reflns_used    317
_cell_measurement_temperature    155(2)
_cell_measurement_theta_max      27.021
_cell_measurement_theta_min      2.182
_cell_volume                     4389.5(8)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics    'ORTEP-III (Burnett & Johnson, 1996)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      155(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX2 CCD area detector'
_diffrn_measurement_method       '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  0.0480
_diffrn_reflns_av_sigmaI/netI    0.0350
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            45003
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.57
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    0.439
_exptl_absorpt_correction_T_max  0.9370
_exptl_absorpt_correction_T_min  0.7633
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2005)'
_exptl_crystal_colour            blue-purple
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       plate
_exptl_crystal_F_000             1888
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.371
_refine_diff_density_min         -0.385
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         9000
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0329
_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^)+(0.0308P)^2^+2.2454P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0759
_refine_ls_wR_factor_ref         0.0837
_reflns_number_gt                7255
_reflns_number_total             9000
_reflns_threshold_expression     >4sigma(I)
_cod_data_source_file            ic8004322_si_003.cif
_cod_data_source_block           febco3-155k-1
_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        4389.4(8)
_cod_original_sg_symbol_Hall     '-P 2yn '
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               4305449