#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:44:04 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178913 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/42/4114247.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4114247
loop_
_publ_author_name
'Andrew Ozarowski'
'Hon Man Lee'
'Alan L. Balch'
_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       ω
_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/[σ²(Fo²)+(0.0308P)²+0.5306P] where P=(Fo²+2Fc²)/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>2σ(I)
_cod_data_source_file            ja030221f_1.cif
_cod_data_source_block           hml88a
_cod_original_cell_volume        750.1(10)
_cod_database_code               4114247
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Zn1 Zn 0.5000 0.5000 0.5000 0.01305(8) Uani 1 2 d S
N1 N 0.4099(3) 0.36745(14) 0.35432(14) 0.0136(3) Uani 1 1 d .
N2 N 0.1977(4) 0.44162(14) 0.57342(14) 0.0137(3) Uani 1 1 d .
C1 C 0.5405(4) 0.34450(17) 0.25710(17) 0.0147(4) Uani 1 1 d .
C2 C 0.4285(4) 0.23894(17) 0.17431(17) 0.0157(4) Uani 1 1 d .
C3 C 0.2281(4) 0.19919(16) 0.22424(16) 0.0157(4) Uani 1 1 d .
C4 C 0.2171(4) 0.28117(17) 0.33642(17) 0.0143(4) Uani 1 1 d .
C5 C 0.0345(4) 0.27313(17) 0.41414(17) 0.0152(4) Uani 1 1 d .
H5A H -0.0985 0.2111 0.3897 0.018 Uiso 1 1 calc R
C6 C 0.0270(4) 0.34691(17) 0.52425(17) 0.0143(4) Uani 1 1 d .
C7 C -0.1558(4) 0.33130(17) 0.60422(18) 0.0153(4) Uani 1 1 d .
C8 C -0.0908(4) 0.41891(17) 0.70251(17) 0.0150(4) Uani 1 1 d .
C9 C 0.1288(4) 0.48753(17) 0.68139(17) 0.0147(4) Uani 1 1 d .
C10 C 0.2482(4) 0.58728(17) 0.75944(17) 0.0153(4) Uani 1 1 d .
H10A H 0.1784 0.6115 0.8317 0.018 Uiso 1 1 calc R
C11 C 0.5185(5) 0.18734(18) 0.05750(18) 0.0187(4) Uani 1 1 d .
H11A H 0.4678 0.1066 0.0267 0.022 Uiso 1 1 calc R
H11B H 0.7286 0.1969 0.0565 0.022 Uiso 1 1 calc R
C12 C 0.3801(5) 0.2375(2) -0.01571(19) 0.0224(4) Uani 1 1 d .
H12A H 0.4470 0.2009 -0.0908 0.034 Uiso 1 1 calc R
H12B H 0.4324 0.3172 0.0134 0.034 Uiso 1 1 calc R
H12C H 0.1721 0.2265 -0.0167 0.034 Uiso 1 1 calc R
C13 C 0.0619(5) 0.08987(18) 0.17818(18) 0.0195(4) Uani 1 1 d .
H13A H 0.0652 0.0582 0.0967 0.023 Uiso 1 1 calc R
H13B H -0.1394 0.1018 0.1991 0.023 Uiso 1 1 calc R
C14 C 0.1816(6) 0.0070(2) 0.2196(2) 0.0267(5) Uani 1 1 d .
H14A H 0.0673 -0.0633 0.1873 0.040 Uiso 1 1 calc R
H14B H 0.1743 0.0371 0.3001 0.040 Uiso 1 1 calc R
H14C H 0.3799 -0.0061 0.1981 0.040 Uiso 1 1 calc R
C15 C -0.3616(5) 0.23475(19) 0.58130(19) 0.0203(4) Uani 1 1 d .
H15A H -0.4628 0.2160 0.5094 0.024 Uiso 1 1 calc R
H15B H -0.5055 0.2556 0.6388 0.024 Uiso 1 1 calc R
C16 C -0.2127(6) 0.1324(2) 0.5789(3) 0.0329(6) Uani 1 1 d .
H16A H -0.3548 0.0711 0.5637 0.049 Uiso 1 1 calc R
H16B H -0.1152 0.1501 0.6504 0.049 Uiso 1 1 calc R
H16C H -0.0728 0.1105 0.5210 0.049 Uiso 1 1 calc R
C17 C -0.2109(4) 0.43865(19) 0.81184(18) 0.0183(4) Uani 1 1 d .
H17A H -0.4137 0.4115 0.8007 0.022 Uiso 1 1 calc R
H17B H -0.2038 0.5195 0.8579 0.022 Uiso 1 1 calc R
C18 C -0.0495(6) 0.3807(2) 0.8727(2) 0.0291(5) Uani 1 1 d .
H18A H -0.1358 0.3963 0.9436 0.044 Uiso 1 1 calc R
H18B H 0.1506 0.4083 0.8852 0.044 Uiso 1 1 calc R
H18C H -0.0596 0.3004 0.8282 0.044 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N2 Zn1 N2 180.000(1) . 2_666
N2 Zn1 N1 89.86(8) . 2_666
N2 Zn1 N1 90.14(8) . .
N1 Zn1 N1 180.0 2_666 .
C4 N1 C1 106.62(17) . .
C4 N1 Zn1 126.50(14) . .
C1 N1 Zn1 126.80(14) . .
C9 N2 C6 106.36(17) . .
C9 N2 Zn1 127.07(15) . .
C6 N2 Zn1 126.57(14) . .
N1 C1 C10 124.69(19) . 2_666
N1 C1 C2 110.14(18) . .
C10 C1 C2 125.2(2) 2_666 .
C3 C2 C1 106.44(19) . .
C3 C2 C11 128.3(2) . .
C1 C2 C11 125.26(19) . .
C2 C3 C4 106.55(18) . .
C2 C3 C13 128.46(19) . .
C4 C3 C13 124.87(18) . .
N1 C4 C5 125.13(19) . .
N1 C4 C3 110.25(17) . .
C5 C4 C3 124.6(2) . .
C4 C5 C6 126.5(2) . .
N2 C6 C5 125.01(19) . .
N2 C6 C7 110.43(18) . .
C5 C6 C7 124.5(2) . .
C8 C7 C6 106.27(19) . .
C8 C7 C15 128.22(19) . .
C6 C7 C15 125.46(19) . .
C7 C8 C9 106.52(18) . .
C7 C8 C17 127.2(2) . .
C9 C8 C17 126.21(19) . .
N2 C9 C10 124.60(19) . .
N2 C9 C8 110.42(19) . .
C10 C9 C8 124.96(19) . .
C9 C10 C1 126.9(2) . 2_666
C2 C11 C12 113.00(18) . .
C3 C13 C14 112.23(19) . .
C7 C15 C16 112.1(2) . .
C8 C17 C18 112.60(18) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 N2 2.035(2) .
Zn1 N1 2.036(2) .
N1 C4 1.365(3) .
N1 C1 1.366(3) .
N2 C9 1.363(3) .
N2 C6 1.367(3) .
C1 C10 1.394(3) 2_666
C1 C2 1.450(3) .
C2 C3 1.367(3) .
C2 C11 1.497(3) .
C3 C4 1.447(3) .
C3 C13 1.497(3) .
C4 C5 1.389(3) .
C5 C6 1.392(3) .
C6 C7 1.452(3) .
C7 C8 1.366(3) .
C7 C15 1.492(3) .
C8 C9 1.451(3) .
C8 C17 1.494(3) .
C9 C10 1.390(3) .
C11 C12 1.528(3) .
C13 C14 1.528(3) .
C15 C16 1.532(4) .
C17 C18 1.526(3) .
