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_4114247
_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            'C36 H44 N4 Zn'
_chemical_formula_weight         598.12
_chemical_name_common            Zinc(II)octaethylporphyrin
_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                113.94(3)
_cell_angle_beta                 91.177(15)
_cell_angle_gamma                92.157(14)
_cell_formula_units_Z            1
_cell_length_a                   4.692(4)
_cell_length_b                   13.185(10)
_cell_length_c                   13.287(10)
_cell_measurement_reflns_used    936
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      30.4
_cell_measurement_theta_min      3.1
_cell_volume                     750.2(10)
_computing_cell_refinement       'SMART (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        'SAINT (Bruker, 2002)'
_computing_molecular_graphics    'SHELXL 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 8.3
_diffrn_measured_fraction_theta_full 0.916
_diffrn_measured_fraction_theta_max 0.916
_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  0.0270
_diffrn_reflns_av_sigmaI/netI    0.0355
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8457
_diffrn_reflns_theta_full        30.50
_diffrn_reflns_theta_max         30.50
_diffrn_reflns_theta_min         1.69
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.851
_exptl_absorpt_correction_T_max  0.8975
_exptl_absorpt_correction_T_min  0.5795
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.03 (Sheldrick, 2001)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_description       rod
_exptl_crystal_F_000             318
_exptl_crystal_size_max          0.72
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.740
_refine_diff_density_min         -0.574
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.167
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         4192
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.167
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0349
_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^)+(0.0308P)^2^+0.5306P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0868
_refine_ls_wR_factor_ref         0.0897
_reflns_number_gt                4067
_reflns_number_total             4192
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja030221f_1.cif
_cod_data_source_block           hml88a
_cod_original_cell_volume        750.1(10)
_cod_database_code               4114247