Electronic Configuration of Five-Coordinate High-Spin Pyrazole-Ligated Iron(II) Porphyrinates
Chuanjiang Hu; Bruce C. Noll; Charles E. Schulz; W. Robert Scheidt; Inorganic Chemistry 49 (2010) 10984–10991; doi:10.1021/ic101469e

data_4317157
_publ_section_title
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 Electronic Configuration of Five-Coordinate High-Spin Pyrazole-Ligated
 Iron(II) Porphyrinates
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10984
_journal_page_last               10991
_journal_paper_doi               10.1021/ic101469e
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C53 H44 Fe N6 O4, C7 H8'
_chemical_formula_sum            'C60 H52 Fe N6 O4'
_chemical_formula_weight         976.93
_chemical_melting_point          ?
_chemical_name_common            Fe(TOCH3PP)(Hdmpz)
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 106.9490(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.9585(3)
_cell_length_b                   35.4853(9)
_cell_length_c                   11.9857(3)
_cell_measurement_reflns_used    9013
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.2861
_cell_measurement_theta_min      2.4082
_cell_volume                     4865.2(2)
_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 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0488
_diffrn_reflns_av_sigmaI/netI    0.0308
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            86053
_diffrn_reflns_theta_full        28.46
_diffrn_reflns_theta_max         28.46
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    0.367
_exptl_absorpt_correction_T_max  0.9303
_exptl_absorpt_correction_T_min  0.8322
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Sheldrick, G. M. (2007) SADABS. University of G\"ottingen, Germany.'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.625
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     692
_refine_ls_number_reflns         12075
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0428
_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^)+(0.0548P)^2^+3.1845P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1046
_refine_ls_wR_factor_ref         0.1132
_reflns_number_gt                10028
_reflns_number_total             12075
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101469e_si_001_2.cif
_cod_data_source_block           Fe(TOCH3PP)(Hdmpz)
_cod_depositor_comments
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The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
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_cod_database_code               4317157