Molecular Structure, UV/Vis Spectra, and Cyclic Voltammograms of Mn(II), Co(II), and Zn(II) 5,10,15,20-Tetraphenyl-21-oxaporphyrins
Silvio Stute; Linda Götzke; Dirk Meyer; Mohamed L. Merroun; Peter Rapta; Olga Kataeva; Wilhelm Seichter; Kerstin Gloe; Lothar Dunsch; Karsten Gloe; Inorganic Chemistry 52 (2013) 1515–1524; doi:10.1021/ic302268h

data_4333719
_publ_contact_author_email       karsten.gloe@chemie.tu-dresden.de
_publ_contact_author_name        'Karsten Gloe'
_publ_section_title
;
 Molecular Structure, UV/Vis Spectra, and Cyclic Voltammograms of Mn(II),
 Co(II), and Zn(II) 5,10,15,20-Tetraphenyl-21-oxaporphyrins
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1515
_journal_page_last               1524
_journal_paper_doi               10.1021/ic302268h
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C44 H28 Cl N3 O Zn'
_chemical_formula_sum            'C44 H28 Cl N3 O Zn'
_chemical_formula_weight         715.51
_chemical_melting_point_gt       573
_chemical_name_common            ZnClOTPP
_chemical_name_systematic
Chloro-(5,10,15,20-tetraphenyl-21-oxaporphyrinato)zinc(II)
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 90.539(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.9737(3)
_cell_length_b                   15.8831(5)
_cell_length_c                   20.9518(5)
_cell_measurement_reflns_used    6360
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      25.83
_cell_measurement_theta_min      2.27
_cell_volume                     3318.90(16)
_computing_cell_refinement       'SAINT-NT (Sheldrick, 2008)'
_computing_data_collection       'Kappa APEX 2 (Bruker-AXS)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'ORTEP-3 (Farrugia)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scan'
_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  0.0467
_diffrn_reflns_av_sigmaI/netI    0.0481
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            33379
_diffrn_reflns_theta_full        27.04
_diffrn_reflns_theta_max         27.04
_diffrn_reflns_theta_min         2.27
_diffrn_standards_decay_%        <1%
_exptl_absorpt_coefficient_mu    0.862
_exptl_absorpt_correction_T_max  0.9382
_exptl_absorpt_correction_T_min  0.7974
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1472
_exptl_crystal_recrystallization_method
'slow evaporation of the solvent (chloroform, ethyl acetate)'
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.555
_refine_diff_density_min         -0.670
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         7237
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0772
_refine_ls_R_factor_gt           0.0450
_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^)+(0.0452P)^2^+2.8128P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0987
_refine_ls_wR_factor_ref         0.1139
_reflns_number_gt                4986
_reflns_number_total             7237
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302268h_si_001_2.cif
_cod_data_source_block           ZnClOTPP
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4333719