Characterization of the Bis(azido)(meso-tetraphenylporphinato)ferrate(III) Anion. An Unusual Spin-Equilibrium System
Mary K. Ellison; Habib Nasri; Y.-M. Xia; Jean-Claude Marchon; Charles E. Schulz; Peter G. Debrunner; W. Robert Scheidt; Inorganic Chemistry 36 (1997) 4804–4811; doi:10.1021/ic970527l

data_4323630
_publ_section_title
;
 Characterization of the
 Bis(azido)(meso-tetraphenylporphinato)ferrate(III) Anion. An Unusual
 Spin-Equilibrium System
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4804
_journal_page_last               4811
_journal_paper_doi               10.1021/ic970527l
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C68 H66 Cl2 Fe N10 Na O8'
_chemical_formula_weight         1301.05
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                64.30(2)
_cell_angle_beta                 77.18(3)
_cell_angle_gamma                77.67(2)
_cell_formula_units_Z            1
_cell_length_a                   11.417(2)
_cell_length_b                   12.371(4)
_cell_length_c                   12.628(2)
_cell_measurement_reflns_used    247
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      20.5
_cell_measurement_theta_min      -20.5
_cell_volume                     1553.0(7)
_computing_cell_refinement       MADNES
_computing_data_collection       MADNES
_computing_data_reduction        'MADNES (Messerschmitt & Pflugrath, 1987)'
_computing_molecular_graphics    'ORTEP-III (Burnett, Johnson, 1996)'
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      130(2)
_diffrn_measurement_device       'Enraf-Nonius FAST area-detector'
_diffrn_measurement_method       'Ellipsoid-mask fitting'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0472
_diffrn_reflns_av_sigmaI/netI    0.0359
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14065
_diffrn_reflns_theta_max         29.90
_diffrn_reflns_theta_min         2.34
_diffrn_standards_decay_%        'No measurable crystal decay'
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.402
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.68
_exptl_absorpt_correction_type   refdelf
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'asymmetrical block'
_exptl_crystal_F_000             679
_exptl_crystal_size_max          0.73
_exptl_crystal_size_mid          0.67
_exptl_crystal_size_min          0.53
_refine_diff_density_max         0.436
_refine_diff_density_min         -0.713
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.111
_refine_ls_goodness_of_fit_obs   1.119
_refine_ls_hydrogen_treatment
;
Idealized with riding model, Aromatic C-H = 0.95 \%A, Aliphatic C-H = 0.99 \%A.
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         7603
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.116
_refine_ls_restrained_S_obs      1.119
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_obs          0.0417
_refine_ls_shift/esd_max         -0.007
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0477P)^2^+1.0781P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1082
_refine_ls_wR_factor_obs         0.1021
_reflns_number_observed          6778
_reflns_number_total             7608
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic970527l_1.cif
_cod_data_source_block           sd:fetppn3lt
_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^)+(0.0477P)^2^+1.0781P] 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^)+(0.0477P)^2^+1.0781P] 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        1553.0(6)
_cod_database_code               4323630