Synthesis, Molecular and Electronic Structures of Six-Coordinate Transition Metal (Mn, Fe, Co, Ni, Cu, and Zn) Complexes with Redox-Active 9-Hydroxyphenoxazin-1-one Ligands
Eugeny P. Ivakhnenko; Andrey G. Starikov; Vladimir I. Minkin; Konstantin A. Lyssenko; Mikhail Yu. Antipin; Vladimir I. Simakov; Mikhail S. Korobov; Gennady S. Borodkin; Pavel A. Knyazev; Inorganic Chemistry 50 (2011) 7022–7032; doi:10.1021/ic2004062

data_4325764
_publ_section_title
;
 Synthesis, Molecular and Electronic Structures of Six-Coordinate
 Transition Metal (Mn, Fe, Co, Ni, Cu, and Zn) Complexes with Redox-Active
 9-Hydroxyphenoxazin-1-one Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7022
_journal_page_last               7032
_journal_paper_doi               10.1021/ic2004062
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C56 H76 N2 O6 Zn, 6(C6 H6)'
_chemical_formula_sum            'C92 H112 N2 O6 Zn'
_chemical_formula_weight         1407.21
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                   20.5359(15)
_cell_length_b                   18.5434(14)
_cell_length_c                   21.0061(15)
_cell_measurement_reflns_used    2589
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     7999.2(10)
_computing_cell_refinement       'APEX2 (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'APEX2 (Bruker, 2005)'
_computing_molecular_graphics    'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_computing_publication_material  'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_computing_structure_refinement  'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_computing_structure_solution    'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX2 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  0.0956
_diffrn_reflns_av_sigmaI/netI    0.1216
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            48019
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    0.361
_exptl_absorpt_correction_T_max  0.9151
_exptl_absorpt_correction_T_min  0.8994
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'APEX2 (Bruker, 2005)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.168
_exptl_crystal_description       prism
_exptl_crystal_F_000             3024
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.438
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.791
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         9652
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.791
_refine_ls_R_factor_all          0.1029
_refine_ls_R_factor_gt           0.0392
_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^)+(0.0185P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0601
_refine_ls_wR_factor_ref         0.0687
_reflns_number_gt                4875
_reflns_number_total             9652
_reflns_threshold_expression     I>2/s(I)
_cod_data_source_file            ic2004062_si_002_6.cif
_cod_data_source_block           Zn
_cod_database_code               4325764