π-Arene/Cation Structure and Bonding. Solvation versus Ligand Binding in Iron(III) Tetraphenylporphyrin Complexes of Benzene, Toluene, p-Xylene, and [60]Fullerene
Daniel R. Evans; Nathanael L. P. Fackler; Zuowei Xie; Clifton E. F. Rickard; Peter D. W. Boyd; Christopher A. Reed; Journal of the American Chemical Society 121 (1999) 8466–8474; doi:10.1021/ja9910816

data_4116538
_publ_section_title
;
 \p-Arene/Cation Structure and Bonding. Solvation versus Ligand Binding in
 Iron(III) Tetraphenylporphyrin Complexes of Benzene, Toluene, p-Xylene,
 and [60]Fullerene
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8466
_journal_page_last               8474
_journal_paper_doi               10.1021/ja9910816
_journal_volume                  121
_journal_year                    1999
_chemical_formula_sum            'C72 H61 B11 Br6 Fe N4'
_chemical_formula_weight         1636.47
_chemical_name_systematic
; 
 ? 
;
_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                106.5120(10)
_cell_angle_beta                 92.1570(10)
_cell_angle_gamma                94.5300(10)
_cell_formula_units_Z            2
_cell_length_a                   13.4685(7)
_cell_length_b                   13.7905(7)
_cell_length_c                   19.4425(10)
_cell_measurement_reflns_used    10136
_cell_measurement_temperature    158(2)
_cell_measurement_theta_max      28.36
_cell_measurement_theta_min      1.09
_cell_volume                     3444.6(3)
_computing_cell_refinement       'Siemens SMART/SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT/SADABS'
_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      158(2)
_diffrn_measurement_device       'Siemens Platform CCD'
_diffrn_measurement_method       '\w scans'
_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  0.0563
_diffrn_reflns_av_sigmaI/netI    0.0974
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            34298
_diffrn_reflns_theta_max         28.36
_diffrn_reflns_theta_min         1.09
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    3.745
_exptl_absorpt_correction_T_max  0.624898
_exptl_absorpt_correction_T_min  0.487799
_exptl_absorpt_correction_type   'Semi-empirical via SADABS'
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            'Dark red-brown'
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       Irregular
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.598
_refine_diff_density_min         -0.666
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.034
_refine_ls_goodness_of_fit_obs   1.132
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     842
_refine_ls_number_reflns         15645
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_restrained_S_obs      1.132
_refine_ls_R_factor_all          0.1080
_refine_ls_R_factor_obs          0.0565
_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^)+(0.0308P)^2^+0.2316P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1083
_refine_ls_wR_factor_obs         0.0882
_reflns_number_observed          10136
_reflns_number_total             15648
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja9910816.cif
_cod_data_source_block           de1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' 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^)+(0.0308P)^2^+0.2316P] 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^)+(0.0308P)^2^+0.2316P] 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               4116538