Variable π-Bonding in Iron(II) Porphyrinates with Nitrite, CO, and tert-Butyl Isocyanide: Characterization of [Fe(TpivPP)(NO2)(CO)]-
Habib Nasri; Mary K. Ellison; Maoyu Shang; Charles E. Schulz; W. Robert Scheidt; Inorganic Chemistry 43 (2004) 2932–2942; doi:10.1021/ic035119y

data_4310902
_publ_section_title
;
 Variable \p-Bonding in Iron(II) Porphyrinates with Nitrite, CO, and
 tert-Butyl Isocyanide: Characterization of [Fe(TpivPP)(NO2)(CO)]-
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2932
_journal_page_last               2942
_journal_paper_doi               10.1021/ic035119y
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C89 H105 Cl Fe K N11 O13'
_chemical_formula_weight         1667.24
_chemical_name_common            '[Fe(TpivPP)(NO2)(CO)]-'
_chemical_name_systematic
; 
 fe2nc 
;
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.240(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   33.548(6)
_cell_length_b                   18.8172(15)
_cell_length_c                   27.187(2)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     17091(4)
_computing_cell_refinement       MADNES
_computing_data_collection       MADNES
_computing_data_reduction        'MADNES (Messerschmitt & Pflugrath, 1987)'
_computing_molecular_graphics    'ORTEP-III for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXTL-v5 (Siemens, 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      130(2)
_diffrn_detector_area_resol_mean 8.2/10.9
_diffrn_measured_fraction_theta_full 0.849
_diffrn_measured_fraction_theta_max 0.849
_diffrn_measurement_device_type  '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  0.0759
_diffrn_reflns_av_sigmaI/netI    0.0779
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            52417
_diffrn_reflns_theta_full        27.24
_diffrn_reflns_theta_max         27.24
_diffrn_reflns_theta_min         1.83
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.325
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5780
_exptl_absorpt_correction_type   refdelf
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle-like
_exptl_crystal_F_000             7056
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.012
_refine_diff_density_min         -0.926
_refine_diff_density_rms         0.094
_refine_ls_extinction_coef       0.00022(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment
;
The amide hydrogen atoms were refined with bond-length restraints, 
while others idealized with riding models.
;
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     2169
_refine_ls_number_reflns         32440
_refine_ls_number_restraints     167
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1224
_refine_ls_R_factor_gt           0.0775
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0970P)^2^+39.7447P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1850
_refine_ls_wR_factor_ref         0.2200
_reflns_number_gt                21632
_reflns_number_total             32440
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035119ysi20030923_031529.cif
_cod_data_source_block           fe2nc
_cod_database_code               4310902