Mononuclear (Nitrido)iron(V) and (Oxo)iron(IV) Complexes via Photolysis of [(cyclam-acetato)FeIII(N3)]+ and Ozonolysis of [(cyclam-acetato)FeIII(O3SCF3)]+ in Water/Acetone Mixtures
Craig A. Grapperhaus; Bernd Mienert; Eckhard Bill; Thomas Weyhermüller; Karl Wieghardt; Inorganic Chemistry 39 (2000) 5306–5317; doi:10.1021/ic0005238

data_4321553
_publ_section_title
;
 Mononuclear (Nitrido)iron(V) and (Oxo)iron(IV) Complexes via Photolysis
 of [(cyclam-acetato)FeIII(N3)]+ and Ozonolysis of
 [(cyclam-acetato)FeIII(O3SCF3)]+ in Water/Acetone Mixtures
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5306
_journal_page_last               5317
_journal_paper_doi               10.1021/ic0005238
_journal_volume                  39
_journal_year                    2000
_chemical_formula_structural     '[C12 H25 Fe N7 O2]+, (C24 H20 B)-, CH3CN'
_chemical_formula_sum            'C38 H48 B Fe N8 O2'
_chemical_formula_weight         715.50
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 102.20(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.945(2)
_cell_length_b                   12.599(2)
_cell_length_c                   24.455(4)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    100(2)
_cell_volume                     3597.2(11)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SAINT'
_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      100(2)
_diffrn_measurement_device       'Siemens SMART CCD-Detector'
_diffrn_measurement_method       '\w-scan, 0.3 deg./frame'
_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  0.0519
_diffrn_reflns_av_sigmaI/netI    0.0634
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            33835
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    0.465
_exptl_absorpt_correction_T_max  0.927
_exptl_absorpt_correction_T_min  0.798
_exptl_absorpt_correction_type   'SADABS, G.M. Sheldrick 1994'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_description       transparent
_exptl_crystal_F_000             1516
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.417
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.052
_refine_ls_goodness_of_fit_obs   1.152
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         10115
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_restrained_S_obs      1.152
_refine_ls_R_factor_all          0.0856
_refine_ls_R_factor_obs          0.0465
_refine_ls_shift/esd_max         -0.024
_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^+0.2661P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1102
_refine_ls_wR_factor_obs         0.0976
_reflns_number_observed          6926
_reflns_number_total             10179
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0005238.cif
_cod_data_source_block           2b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+0.2661P] 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^+0.2661P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3597.2(10)
_cod_database_code               4321553