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_4120965
_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         'C69 H72 Fe N10 O6, C6 H6'
_chemical_formula_sum            'C75 H78 Fe N10 O6'
_chemical_formula_weight         1271.32
_chemical_name_common            '[Fe(TpivPP)(1-EtIm)(O2)], benzene'
_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                 90.359(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.5288(9)
_cell_length_b                   19.2070(10)
_cell_length_c                   18.4449(8)
_cell_measurement_reflns_used    7397
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24.3522
_cell_measurement_theta_min      2.3910
_cell_volume                     6564.1(5)
_computing_cell_refinement       'APEX2/SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2007; Sheldrick, 2008)'
_computing_molecular_graphics    'XP (Sheldrick, 2008)'
_computing_publication_material  'XCIF (Sheldrick, 2008)/enCIFer (CCDC, 2005)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Brucker d8 ApexII CCD diffractometer'
_diffrn_measurement_method       '\f and \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  0.0387
_diffrn_reflns_av_sigmaI/netI    0.0517
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            32729
_diffrn_reflns_theta_full        28.66
_diffrn_reflns_theta_max         28.66
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    0.292
_exptl_absorpt_correction_T_max  0.9658
_exptl_absorpt_correction_T_min  0.8847
_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    1.286
_exptl_crystal_description       block
_exptl_crystal_F_000             2688
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.727
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         8170
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.1255
_refine_ls_R_factor_gt           0.0601
_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^)+(0.0697P)^2^+9.8681P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1492
_refine_ls_wR_factor_ref         0.1849
_reflns_number_gt                4618
_reflns_number_total             8170
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja408431z_si_003_2.cif
_cod_data_source_block           FeTpivPP1-EtImO2-200
_cod_database_code               4120965