Iron-Mediated Cleavage of Coordinated 1,1,1,5,5,5-Hexafluoropentane-2,4-dione by the 2,2,6,6-Tetramethylpiperidine-1-oxyl Nitroxyl Radical
Caroline Ahlers; Michael H. Dickman; Inorganic Chemistry 37 (1998) 6337–6340; doi:10.1021/ic980489l

data_4323185
_publ_section_title
;
 Iron-Mediated Cleavage of Coordinated
 1,1,1,5,5,5-Hexafluoropentane-2,4-dione by the
 2,2,6,6-Tetramethylpiperidine-1-oxyl Nitroxyl Radical
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6337
_journal_page_last               6340
_journal_paper_doi               10.1021/ic980489l
_journal_volume                  37
_journal_year                    1998
_chemical_compound_source        synthesized
_chemical_formula_sum            'C39 H44 F24 Fe2 N2 O12'
_chemical_formula_weight         1300.46
_chemical_name_systematic
; 
 ? 
;
_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   'difmap except geom for disordered'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.9380(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.60790(10)
_cell_length_b                   12.4155(2)
_cell_length_c                   22.4199(4)
_cell_measurement_reflns_used    7504
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      1.37
_cell_volume                     5457.21(13)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens SMART CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0550
_diffrn_reflns_av_sigmaI/netI    0.0521
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            53092
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         1.37
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.669
_exptl_absorpt_correction_T_max  0.921
_exptl_absorpt_correction_T_min  0.766
_exptl_absorpt_correction_type   Blessing
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             2624
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.827
_refine_diff_density_min         -0.651
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.129
_refine_ls_goodness_of_fit_obs   1.152
_refine_ls_hydrogen_treatment    'refall except noref for disordered'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     965
_refine_ls_number_reflns         12993
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.133
_refine_ls_restrained_S_obs      1.157
_refine_ls_R_factor_all          0.1030
_refine_ls_R_factor_obs          0.0646
_refine_ls_shift/esd_max         0.013
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+7.4600P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1559
_refine_ls_wR_factor_obs         0.1312
_reflns_number_observed          9107
_reflns_number_total             12993
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980489l_1.cif
_cod_data_source_block           vbn
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+7.4600P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+7.4600P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4323185