Photolysis of cis- and trans-[FeIII(cyclam)(N3)2]+ Complexes: Spectroscopic Characterization of a Nitridoiron(V) Species
Karsten Meyer; Eckhard Bill; Bernd Mienert; Thomas Weyhermüller; Karl Wieghardt; Journal of the American Chemical Society 121 (1999) 4859–4876; doi:10.1021/ja983454t

data_4116392
_publ_section_title
;
 Photolysis of cis- and trans-[FeIII(cyclam)(N3)2]+ Complexes:
 Spectroscopic Characterization of a Nitridoiron(V) Species
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4859
_journal_page_last               4876
_journal_paper_doi               10.1021/ja983454t
_journal_volume                  121
_journal_year                    1999
_chemical_formula_structural     '[C10 H24 Fe N10]+, (ClO4)-'
_chemical_formula_sum            'C10 H24 Cl Fe N10 O4'
_chemical_formula_weight         439.69
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 99.53(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.641(2)
_cell_length_b                   8.851(1)
_cell_length_c                   15.266(3)
_cell_measurement_reflns_used    7193
_cell_measurement_temperature    100(2)
_cell_volume                     1817.7(5)
_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  0.0709
_diffrn_reflns_av_sigmaI/netI    0.0419
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            14529
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.67
_exptl_absorpt_coefficient_mu    1.018
_exptl_absorpt_correction_T_max  0.903
_exptl_absorpt_correction_T_min  0.820
_exptl_absorpt_correction_type   'SADABS, G. Sheldrick 1994'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_description       'transparent octahedron '
_exptl_crystal_F_000             916
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.38
_refine_diff_density_max         0.530
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.063
_refine_ls_goodness_of_fit_obs   1.091
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         3037
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_restrained_S_obs      1.091
_refine_ls_R_factor_all          0.0535
_refine_ls_R_factor_obs          0.0396
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0279P)^2^+2.9940P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0939
_refine_ls_wR_factor_obs         0.0849
_reflns_number_observed          2654
_reflns_number_total             3199
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja983454t_2.cif
_cod_data_source_block           (2)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0279P)^2^+2.9940P] 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^)+(0.0279P)^2^+2.9940P] 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        1817.67(7)
_cod_database_code               4116392