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_4120960
_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), 1.8(C2H5OH)'
_chemical_formula_sum            'C71.6 H80.8 Fe N10 O7.8'
_chemical_formula_weight         1262.11
_chemical_name_common            '[Fe(TpivPP)(2-MeIm)(O2)],1.8EtOH '
_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                 91.5980(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.7058(5)
_cell_length_b                   19.4848(6)
_cell_length_c                   17.8094(5)
_cell_measurement_temperature    100(2)
_cell_volume                     6488.6(3)
_computing_cell_refinement       'Brucker APEX2/SAINT'
_computing_data_collection       'Brucker APEX2'
_computing_data_reduction        'Brucker SAINT/SHELXTL'
_computing_molecular_graphics    Ortep3
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Smart Apex CCD area detector'
_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  0.0211
_diffrn_reflns_av_sigmaI/netI    0.0172
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            37542
_diffrn_reflns_theta_full        27.96
_diffrn_reflns_theta_max         27.96
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    0.297
_exptl_absorpt_correction_T_max  0.9653
_exptl_absorpt_correction_T_min  0.9084
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_description       diamond
_exptl_crystal_F_000             2675
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.751
_refine_diff_density_min         -0.836
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.205
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     537
_refine_ls_number_reflns         7772
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.212
_refine_ls_R_factor_all          0.0813
_refine_ls_R_factor_gt           0.0760
_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^)+(0.0389P)^2^+36.0082P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1828
_refine_ls_wR_factor_ref         0.1854
_reflns_number_gt                7074
_reflns_number_total             7772
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja408431z_si_001_6.cif
_cod_data_source_block           B_TpivPP2-MeHIm_O2_100K
_cod_original_formula_sum        'C71.60 H80.80 Fe N10 O7.80'
_cod_database_code               4120960