Mononuclear non-heme iron(III) peroxide complexes: syntheses, characterisation, mass spectrometric and kinetic studies
Alan Hazell; Christine J. McKenzie; Lars Preuss Nielsen; Siegfried Schindler; Markus Weitzer; J. Chem. Soc., Dalton Trans.  (2002) 310–317; doi:10.1039/b103844n

data_7010791
_publ_section_title
;
 Mononuclear non-heme iron(III) peroxide complexes: syntheses,
 characterisation, mass spectrometric and kinetic studies
;
_journal_issue                   3
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              310
_journal_page_last               317
_journal_paper_doi               10.1039/b103844n
_journal_year                    2002
_chemical_formula_sum            'C27.192 H29.384 Cl1.384 F6 Fe N5 P'
_chemical_formula_weight         676.16
_chemical_name_common            '[FetpenbzCl](PF6).0.192CH2Cl2'
_chemical_name_systematic
;                                  
[FetpenbzCl](PF6).0.192CH2Cl2                  
;
_space_group_IT_number           148
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_type_scat_source           IntTabIV
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                120.0
_cell_formula_units_Z            18
_cell_length_a                   29.1500(9)
_cell_length_b                   29.1500(9)
_cell_length_c                   17.661(1)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    120
_cell_measurement_theta_max      29.84
_cell_measurement_theta_min      2.4
_cell_volume                     12996.4(9)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_molecular_graphics
;                                  
ORTEP-III (Burnett & Johnson, 1996), KRYSTAL                    
;
_computing_publication_material  KRYSTAL
_computing_structure_refinement  'modified ORFLS(1962), KRYSTAL'
_computing_structure_solution
;                                  
SIR97 (Cascarano et al., 1996) KRYSTAL                           
;
_diffrn_ambient_temperature      120
_diffrn_measurement_device       'Siemens SMART CCD diffractometer'
_diffrn_measurement_method
;
\w rotation scans with narrow frames
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'x-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.042
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            42461
_diffrn_reflns_reduction_process 42461
_diffrn_reflns_theta_max         29.84
_diffrn_reflns_theta_min         2.4
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.772
_exptl_absorpt_correction_T_max  0.886
_exptl_absorpt_correction_T_min  0.766
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'XPREP (Siemens, 1955)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       block
_exptl_crystal_F_000             6189.984
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.34
_refine_diff_density_max         1.1(1)
_refine_diff_density_min         -1.1(1)
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    6
_refine_ls_number_parameters     387
_refine_ls_number_reflns         6787
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.046
_refine_ls_shift/su_max          0.0012
_refine_ls_shift/su_mean         0.0005
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;                                  
w = 1 /{[\s~cs~(F^2^)+B+(1+A)F^2^]^1/2^-|F|}^2^                          
A = 0.03, B = 7.0
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.037
_reflns_number_gt                6585
_reflns_number_total             7899
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b103844n.txt
_cod_data_source_block           Fetpenbz
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_site_thermal_displace_type' tag value 'Uij' was replaced with
'Uani' value 43 times.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        12996(1)
_cod_original_sg_symbol_H-M      R-3
_cod_original_formula_sum        'C27.192 H29.384 Cl1.384 F6 Fe1 N5 P1'
_cod_database_code               7010791