Correlated Ligand Dynamics in Oxyiron Picket Fence Porphyrins: Structural and Mössbauer Investigations
Jianfeng Li; Bruce C. Noll; Allen G. Oliver; Charles E. Schulz; W. Robert Scheidt; Journal of the American Chemical Society 135 (2013) 15627–15641; doi:10.1021/ja408431z

data_4120969
_publ_section_title
;
 Correlated Ligand Dynamics in Oxyiron Picket Fence Porphyrins: Structural
 and M\"ossbauer Investigations
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15627
_journal_page_last               15641
_journal_paper_doi               10.1021/ja408431z
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety
'C68 H70 Fe N10 O6, C2.88 H2.4 Cl0.48, C1.12 H1.68 N0.56 '
_chemical_formula_sum            'C72 H74.08 Cl0.48 Fe N10.56 O6'
_chemical_formula_weight         1256.23
_chemical_name_common
'[Fe(TpivPP)(1-MeIm)(O2)]1-MeIm, 0.48(PhCl), 0.28(1-MeIm)'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 91.2670(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.7509(16)
_cell_length_b                   19.4484(17)
_cell_length_c                   18.6503(16)
_cell_measurement_reflns_used    4475
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      24.4990
_cell_measurement_theta_min      2.9281
_cell_volume                     6799.6(10)
_computing_cell_refinement       'Bruker SAINT v7.34A'
_computing_data_collection       'Bruker APEX2 v2.1-4'
_computing_data_reduction        'Bruker SAINT v7.34A'
_computing_molecular_graphics    'Bruker SHELXTL v6.14'
_computing_publication_material  'Bruker SHELXTL v6.14'
_computing_structure_refinement  'Bruker SHELXTL v6.14'
_computing_structure_solution    'Bruker SHELXTL v6.14'
_diffrn_ambient_temperature      300(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'Si-<111> channel cut crystal'
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77490
_diffrn_reflns_av_R_equivalents  0.0741
_diffrn_reflns_av_sigmaI/netI    0.0471
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            32920
_diffrn_reflns_theta_full        27.22
_diffrn_reflns_theta_max         27.22
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    0.300
_exptl_absorpt_correction_T_max  0.9593
_exptl_absorpt_correction_T_min  0.9129
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Sheldrick, G. M. (2008) SADABS. University of G\"ottingen, Germany.'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_description       block
_exptl_crystal_F_000             2633
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.611
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         5813
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0920
_refine_ls_R_factor_gt           0.0642
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1202P)^2^+3.3309P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1822
_refine_ls_wR_factor_ref         0.2070
_reflns_number_gt                4011
_reflns_number_total             5813
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja408431z_si_004_3.cif
_cod_data_source_block           FeTpivPP1-MeImO2-300
_cod_database_code               4120969