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_4333718
_publ_contact_author_address
;Department of Chemistry
Technische Universitaet Dresden 
Dresden
Germany
;
_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 Cu N3 O, C H Cl3'
_chemical_formula_sum            'C45 H29 Cl4 Cu N3 O'
_chemical_formula_weight         833.05
_chemical_melting_point_gt       573
_chemical_name_common            CuClOTPP
_chemical_name_systematic
Chloro-(5,10,15,20-tetraphenyl-21-oxaporphyrinato)copper(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                 102.7880(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.0352(3)
_cell_length_b                   21.9674(6)
_cell_length_c                   14.4403(4)
_cell_measurement_reflns_used    8009
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.86
_cell_measurement_theta_min      2.35
_cell_volume                     3723.06(17)
_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 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0649
_diffrn_reflns_av_sigmaI/netI    0.0813
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            43406
_diffrn_reflns_theta_full        28.45
_diffrn_reflns_theta_max         28.45
_diffrn_reflns_theta_min         1.72
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    0.915
_exptl_absorpt_correction_T_max  0.8942
_exptl_absorpt_correction_T_min  0.8526
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2004)'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1700
_exptl_crystal_recrystallization_method
'slow evaporation of the solvent (chloroform, ethyl acetate)'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.108
_refine_diff_density_min         -0.947
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         9297
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0971
_refine_ls_R_factor_gt           0.0571
_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^)+(0.0716P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1355
_refine_ls_wR_factor_ref         0.1452
_reflns_number_gt                5820
_reflns_number_total             9297
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302268h_si_001_1.cif
_cod_data_source_block           CuClOTPP
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4333718