Crystal Environments Probed by EPR Spectroscopy. Variations in the EPR Spectra of CoII(octaethylporphyrin) Doped in Crystalline Diamagnetic Hosts and a Reassessment of the Electronic Structure of Four-Coordinate Cobalt(II)
Andrew Ozarowski; Hon Man Lee; Alan L. Balch; Journal of the American Chemical Society 125 (2003) 12606–12614; doi:10.1021/ja030221f

data_4114249
_publ_section_title
;
 Crystal Environments Probed by EPR Spectroscopy. Variations in the EPR
 Spectra of CoII(octaethylporphyrin) Doped in Crystalline Diamagnetic
 Hosts and a Reassessment of the Electronic Structure of Four-Coordinate
 Cobalt(II)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12606
_journal_page_last               12614
_journal_paper_doi               10.1021/ja030221f
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C46 H54 N6 Zn'
_chemical_formula_weight         756.32
_chemical_name_common            Zn(OEP)(py)2
_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                98.970(5)
_cell_angle_beta                 90.724(4)
_cell_angle_gamma                114.565(5)
_cell_formula_units_Z            1
_cell_length_a                   9.8564(9)
_cell_length_b                   10.3391(10)
_cell_length_c                   10.4252(11)
_cell_measurement_reflns_used    964
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      20.0
_cell_measurement_theta_min      2.4
_cell_volume                     950.87(17)
_computing_cell_refinement       'SMART 5.054 (Bruker, 2002)'
_computing_data_collection       'SMART 5.054 (Bruker, 2002)'
_computing_data_reduction        'SAINT 6.35 (Bruker, 2002)'
_computing_molecular_graphics    'SHELXTL 5.1 (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.892
_diffrn_measured_fraction_theta_max 0.892
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_sigmaI/netI    0.0466
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9043
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    0.688
_exptl_absorpt_correction_T_max  0.836
_exptl_absorpt_correction_T_min  0.652
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.03 (Sheldrick, 2002)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_description       prism
_exptl_crystal_F_000             402
_exptl_crystal_size_max          0.68
_exptl_crystal_size_mid          0.57
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.398
_refine_diff_density_min         -0.700
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         4211
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0420
_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^)+(0.0919P)^2^+0.4235P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1385
_refine_ls_wR_factor_ref         0.1426
_reflns_number_gt                3980
_reflns_number_total             4211
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja030221f_3.cif
_cod_data_source_block           hml35
_cod_original_cell_volume        950.87(16)
_cod_database_code               4114249