Formation of Superoxide Anion on Aerial Oxidation of Cu(II)-Porphyrinogen in the Synthesis of Tetrakis(cyclohexyl)porphyrinogenCu(III) Anion
Dibyendu Bhattacharya; Suman Maji; Kuntal Pal; Sabyasachi Sarkar; Inorganic Chemistry 47 (2008) 5036–5038; doi:10.1021/ic800282j

data_4305073
_publ_contact_author_address
;Department of Chemistry
IIT Kanpur
Kanpur
208016
;
_publ_contact_author_email       abya@iitk.ac.in
_publ_contact_author_fax         +915122597265
_publ_contact_author_name        'Sabyasachi sarkar'
_publ_contact_author_phone       +915122597265
_publ_section_title
;
Formation of Superoxide Anion on Aerial Oxidation of Cu(II)-Porphyrinogen
in the Synthesis of Tetrakis(cyclohexyl)porphyrinogenCu(III) Anion
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5036
_journal_page_last               5038
_journal_paper_doi               10.1021/ic800282j
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C40 H48 Cu N4, C8 H20 N, 3(C H2 Cl2)'
_chemical_formula_sum            'C51 H74 Cl6 Cu N5'
_chemical_formula_weight         1033.39
_chemical_name_systematic
'Tetraethylammoniumtetrakis(cyclohexyl)Copper(III)porphyrinogen DCM solvated'
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.619(5)
_cell_length_b                   18.299(5)
_cell_length_c                   20.249(5)
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.33
_cell_measurement_theta_min      2.01
_cell_volume                     5046(3)
_computing_cell_refinement       'SAINT 6.45 ( Bruker, 2003)'
_computing_data_collection       'SMART 5.628 (Bruker, 2003)'
_computing_data_reduction        'SAINT 6.45  (Bruker, 2003)'
_computing_molecular_graphics    'Diamond 3.1e, Ortep 3'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       /w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0475
_diffrn_reflns_av_sigmaI/netI    0.0704
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            34061
_diffrn_reflns_theta_full        28.33
_diffrn_reflns_theta_max         28.33
_diffrn_reflns_theta_min         2.01
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.791
_exptl_absorpt_correction_T_max  0.9415
_exptl_absorpt_correction_T_min  0.9080
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectrangular block'
_exptl_crystal_F_000             2184
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.662
_refine_diff_density_min         -0.579
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.011(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     572
_refine_ls_number_reflns         12549
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0449
_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^)+(0.0417P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0903
_refine_ls_wR_factor_ref         0.0952
_reflns_number_gt                10592
_reflns_number_total             12549
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800282j-file003.cif
_cod_data_source_block           6maybm
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Empirical' changed to 'empirical'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4305073