Synthesis and Characterization of Iron N-Confused Porphyrins: Structural Evidences of Agostic Interaction
Wan-Chin Chen; Chen-Hsiung Hung; Inorganic Chemistry 40 (2001) 5070–5071; doi:10.1021/ic0155333

data_4320336
_publ_section_title
;
 Synthesis and Characterization of Iron N-Confused Porphyrins: Structural
 Evidences of Agostic Interaction
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5070
_journal_page_last               5071
_journal_paper_doi               10.1021/ic0155333
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C59 H52 Fe N4 O2 S'
_chemical_formula_weight         936.96
_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                72.921(2)
_cell_angle_beta                 83.036(2)
_cell_angle_gamma                77.615(2)
_cell_formula_units_Z            2
_cell_length_a                   13.4489(15)
_cell_length_b                   13.6169(15)
_cell_length_c                   14.3453(15)
_cell_measurement_temperature    293(2)
_cell_volume                     2448.0(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0265
_diffrn_reflns_av_sigmaI/netI    0.1409
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15631
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    0.398
_exptl_absorpt_correction_T_max  0.9486
_exptl_absorpt_correction_T_min  0.7572
_exptl_absorpt_correction_type   'Empirical Used SADABS'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.451
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.716
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     641
_refine_ls_number_reflns         10859
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.716
_refine_ls_R_factor_all          0.1205
_refine_ls_R_factor_gt           0.0464
_refine_ls_shift/su_max          1.095
_refine_ls_shift/su_mean         0.012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0474P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1003
_refine_ls_wR_factor_ref         0.1138
_reflns_number_gt                4231
_reflns_number_total             10859
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0155333-2_s3.cif
_cod_data_source_block           h0621m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 
;
_cod_database_code               4320336