Iron-Porphyrin NO Complexes with Covalently Attached N-Donor Ligands: Formation of a Stable Six-Coordinate Species in Solution
Timothy C. Berto; V. K. K. Praneeth; Lauren E. Goodrich; Nicolai Lehnert; Journal of the American Chemical Society 131 (2009) 17116–17126; doi:10.1021/ja904368n

data_4105399
_publ_section_title
;
 Iron-Porphyrin NO Complexes with Covalently Attached N-Donor Ligands:
 Formation of a Stable Six-Coordinate Species in Solution
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17116
_journal_page_last               17126
_journal_paper_doi               10.1021/ja904368n
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C55 H31 F6 N7 O Zn, C H2 Cl2'
_chemical_formula_sum            'C56 H33 Cl2 F6 N7 O Zn'
_chemical_formula_weight         1070.16
_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                103.955(1)
_cell_angle_beta                 101.557(1)
_cell_angle_gamma                100.116(1)
_cell_formula_units_Z            2
_cell_length_a                   10.5223(8)
_cell_length_b                   13.2057(10)
_cell_length_c                   19.7516(15)
_cell_measurement_reflns_used    9862
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.58
_cell_volume                     2536.1(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART-APEX'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      85(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0460
_diffrn_reflns_av_sigmaI/netI    0.0406
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            54977
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    0.659
_exptl_absorpt_correction_T_max  0.9370
_exptl_absorpt_correction_T_min  0.9134
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  Blessing, R. Acta Cryst. (1995) A51 33-38.
  Sheldrick, G.  SADABS (Version 2008/1) Bruker AXS area
  detector absorption and other corrections, University of
  Gottingen, Germany 2008.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_description       block
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.301
_refine_diff_density_min         -0.655
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     749
_refine_ls_number_reflns         12597
_refine_ls_number_restraints     153
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0570
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1026P)^2^+1.5178P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1630
_refine_ls_wR_factor_ref         0.1770
_reflns_number_gt                9535
_reflns_number_total             12597
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja904368n_si_002.cif
_cod_data_source_block           znbzim
_cod_database_code               4105399