Unexpected Nitrosyl-Group Bending in Six-Coordinate {M(NO)}6σ-Bonded Aryl(iron) and -(ruthenium) Porphyrins
George B. Richter-Addo; Ralph A. Wheeler; Christopher Adam Hixson; Li Chen; Masood A. Khan; Mary K. Ellison; Charles E. Schulz; W. Robert Scheidt; Journal of the American Chemical Society 123 (2001) 6314–6326; doi:10.1021/ja010276m

data_4115597
_publ_section_title
;
 Unexpected Nitrosyl-Group Bending in Six-Coordinate {M(NO)}6\s-Bonded
 Aryl(iron) and -(ruthenium) Porphyrins
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6314
_journal_page_last               6326
_journal_paper_doi               10.1021/ja010276m
_journal_volume                  123
_journal_year                    2001
_chemical_formula_sum            'C42 H48 F Fe N5 O'
_chemical_formula_weight         713.70
_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-97
_cell_angle_alpha                96.045(15)
_cell_angle_beta                 97.114(16)
_cell_angle_gamma                99.466(16)
_cell_formula_units_Z            2
_cell_length_a                   10.487(3)
_cell_length_b                   10.833(3)
_cell_length_c                   15.804(5)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      20.5
_cell_measurement_theta_min      -20.5
_cell_volume                     1742.8(9)
_computing_cell_refinement       MADNES
_computing_data_collection       MADNES
_computing_data_reduction        'MADNES (Messerschmitt & Pflugrath, 1987)'
_computing_molecular_graphics    'ORTEPIII (Burnett, Johnson, 1996)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.883
_diffrn_measured_fraction_theta_max 0.883
_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  0.0815
_diffrn_reflns_av_sigmaI/netI    0.0705
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16669
_diffrn_reflns_theta_full        29.82
_diffrn_reflns_theta_max         29.82
_diffrn_reflns_theta_min         2.22
_diffrn_standards_decay_%        'no measurable crystal decay'
_exptl_absorpt_coefficient_mu    0.480
_exptl_absorpt_correction_T_max  0.9672
_exptl_absorpt_correction_T_min  0.9101
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_description       irregular
_exptl_crystal_F_000             756
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.710
_refine_diff_density_min         -0.807
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     459
_refine_ls_number_reflns         8836
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0902
_refine_ls_R_factor_gt           0.0628
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0459P)^2^+3.7583P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1344
_refine_ls_wR_factor_ref         0.1496
_reflns_number_gt                6605
_reflns_number_total             8836
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja010276m_1.cif
_cod_data_source_block           sd:feoepnoc6h4f
_cod_original_cell_volume        1742.9(9)
_cod_database_code               4115597