Just a Proton: Distinguishing the Two Electronic States of Five-Coordinate High-Spin Iron(II) Porphyrinates with Imidazole/ate Coordination
Chuanjiang Hu; Corinne D. Sulok; Florian Paulat; Nicolai Lehnert; Anna I. Twigg; Michael P. Hendrich; Charles E. Schulz; W. Robert Scheidt; Journal of the American Chemical Society 132 (2010) 3737–3750; doi:10.1021/ja907584x

data_4102099
_publ_section_title
;
 Just a Proton: Distinguishing the Two Electronic States of
 Five-Coordinate High-Spin Iron(II) Porphyrinates with Imidazole/ate
 Coordination
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3737
_journal_page_last               3750
_journal_paper_doi               10.1021/ja907584x
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety
'C44 H28 Cl Fe N4, C18 H36 N2 Na O6, 3(C H2 Cl2)'
_chemical_formula_sum            'C65 H70 Cl7 Fe N6 Na O6'
_chemical_formula_weight         1358.26
_chemical_name_common            Na(222)[Fe(TPP)Cl]
_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                85.756(8)
_cell_angle_beta                 83.340(7)
_cell_angle_gamma                63.273(7)
_cell_formula_units_Z            2
_cell_length_a                   12.720(2)
_cell_length_b                   12.902(2)
_cell_length_c                   22.267(4)
_cell_measurement_reflns_used    8538
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.7296
_cell_measurement_theta_min      2.4799
_cell_volume                     3240.9(9)
_computing_cell_refinement       'APEX2/SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_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      100(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Bruker d8 Apex II 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  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0228
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            94826
_diffrn_reflns_theta_full        30.88
_diffrn_reflns_theta_max         30.88
_diffrn_reflns_theta_min         0.92
_exptl_absorpt_coefficient_mu    0.584
_exptl_absorpt_correction_T_max  0.8444
_exptl_absorpt_correction_T_min  0.7209
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Sheldrick, G. M. (2007) SADABS. University of G\"ottingen, Germany.'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1412
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.488
_refine_diff_density_min         -0.870
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     838
_refine_ls_number_reflns         19830
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0383
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+2.2459P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1032
_refine_ls_wR_factor_ref         0.1190
_reflns_number_gt                17903
_reflns_number_total             19830
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja907584x_si_002.cif
_cod_data_source_block           fetppclna222
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        3241.0(9)
_cod_database_code               4102099