#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:44:04 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178913 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/42/4114249.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_4114249
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            '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       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  0.0329
_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/[σ²(Fo²)+(0.0919P)²+0.4235P] where P=(Fo²+2Fc²)/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>2σ(I)
_cod_data_source_file            ja030221f_3.cif
_cod_data_source_block           hml35
_cod_original_cell_volume        950.87(16)
_cod_database_code               4114249
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 0.01219(13) Uani 1 2 d S
N1 N 0.43488(18) 0.55395(17) 0.33472(15) 0.0124(3) Uani 1 1 d .
N2 N 0.33240(17) 0.29321(17) 0.44939(15) 0.0115(3) Uani 1 1 d .
N3 N 0.33516(18) 0.58437(17) 0.61652(15) 0.0143(3) Uani 1 1 d .
C1 C 0.4921(2) 0.6880(2) 0.30121(17) 0.0120(3) Uani 1 1 d .
C2 C 0.4110(2) 0.68511(19) 0.18273(17) 0.0122(3) Uani 1 1 d .
C3 C 0.3055(2) 0.5463(2) 0.14485(17) 0.0121(3) Uani 1 1 d .
C4 C 0.3208(2) 0.4655(2) 0.24255(17) 0.0128(3) Uani 1 1 d .
C5 C 0.23059(19) 0.31895(19) 0.24436(17) 0.0114(3) Uani 1 1 d .
H5 H 0.1574 0.2684 0.1727 0.014 Uiso 1 1 calc R
C6 C 0.2357(2) 0.23891(19) 0.33888(18) 0.0124(3) Uani 1 1 d .
C7 C 0.1440(2) 0.08475(19) 0.33319(17) 0.0122(3) Uani 1 1 d .
C8 C 0.19093(19) 0.04794(19) 0.44051(17) 0.0117(3) Uani 1 1 d .
C9 C 0.3091(2) 0.18015(19) 0.51239(18) 0.0123(3) Uani 1 1 d .
C10 C 0.6107(2) 0.8102(2) 0.37207(17) 0.0130(3) Uani 1 1 d .
H10 H 0.6400 0.8967 0.3375 0.016 Uiso 1 1 calc R
C11 C 0.4398(2) 0.8128(2) 0.11685(18) 0.0148(3) Uani 1 1 d .
H11A H 0.4561 0.8979 0.1842 0.018 Uiso 1 1 calc R
H11B H 0.3497 0.7920 0.0595 0.018 Uiso 1 1 calc R
C12 C 0.5750(2) 0.8502(2) 0.03557(19) 0.0182(4) Uani 1 1 d .
H12A H 0.6655 0.8748 0.0922 0.027 Uiso 1 1 calc R
H12B H 0.5866 0.9329 -0.0055 0.027 Uiso 1 1 calc R
H12C H 0.5594 0.7669 -0.0320 0.027 Uiso 1 1 calc R
C13 C 0.1972(2) 0.4856(2) 0.02530(18) 0.0150(4) Uani 1 1 d .
H13A H 0.1754 0.5635 -0.0008 0.018 Uiso 1 1 calc R
H13B H 0.1021 0.4105 0.0460 0.018 Uiso 1 1 calc R
C14 C 0.2581(3) 0.4196(2) -0.08880(19) 0.0219(4) Uani 1 1 d .
H14A H 0.3508 0.4942 -0.1113 0.033 Uiso 1 1 calc R
H14B H 0.1838 0.3807 -0.1643 0.033 Uiso 1 1 calc R
H14C H 0.2787 0.3416 -0.0638 0.033 Uiso 1 1 calc R
C15 C 0.0221(2) -0.0119(2) 0.22858(18) 0.0149(3) Uani 1 1 d .
H15A H -0.0273 0.0449 0.1975 0.018 Uiso 1 1 calc R
H15B H -0.0540 -0.0903 0.2667 0.018 Uiso 1 1 calc R
C16 C 0.0783(2) -0.0791(2) 0.1122(2) 0.0232(4) Uani 1 1 d .
H16A H 0.1512 -0.0023 0.0720 0.035 Uiso 1 1 calc R
H16B H -0.0063 -0.1412 0.0482 0.035 Uiso 1 1 calc R
H16C H 0.1260 -0.1368 0.1419 0.035 Uiso 1 1 calc R
C17 C 0.1408(2) -0.09911(19) 0.47579(18) 0.0144(3) Uani 1 1 d .
H17A H 0.0378 -0.1610 0.4356 0.017 Uiso 1 1 calc R
H17B H 0.1383 -0.0907 0.5716 0.017 Uiso 1 1 calc R
C18 C 0.2443(2) -0.1708(2) 0.4302(2) 0.0201(4) Uani 1 1 d .
H18A H 0.2398 -0.1875 0.3347 0.030 Uiso 1 1 calc R
H18B H 0.2120 -0.2633 0.4606 0.030 Uiso 1 1 calc R
H18C H 0.3473 -0.1074 0.4660 0.030 Uiso 1 1 calc R
C19 C 0.1862(2) 0.5056(2) 0.6041(2) 0.0185(4) Uani 1 1 d .
H19 H 0.1467 0.4138 0.5487 0.022 Uiso 1 1 calc R
C20 C 0.0872(2) 0.5512(2) 0.6678(2) 0.0202(4) Uani 1 1 d .
H20 H -0.0173 0.4916 0.6566 0.024 Uiso 1 1 calc R
C21 C 0.1435(2) 0.6855(2) 0.7483(2) 0.0205(4) Uani 1 1 d .
H21 H 0.0783 0.7202 0.7927 0.025 Uiso 1 1 calc R
C22 C 0.2978(2) 0.7682(2) 0.7625(2) 0.0195(4) Uani 1 1 d .
H22 H 0.3402 0.8604 0.8173 0.023 Uiso 1 1 calc R
C23 C 0.3885(2) 0.7139(2) 0.69534(19) 0.0165(4) Uani 1 1 d .
H23 H 0.4936 0.7710 0.7055 0.020 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
N1 Zn1 N1 180.0 . 2_666
N1 Zn1 N2 90.28(7) . 2_666
N1 Zn1 N2 89.72(7) 2_666 2_666
N1 Zn1 N2 89.72(7) . .
N1 Zn1 N2 90.28(7) 2_666 .
N2 Zn1 N2 180.0 2_666 .
N1 Zn1 N3 88.28(6) . .
N1 Zn1 N3 91.72(6) 2_666 .
N2 Zn1 N3 87.97(6) 2_666 .
N2 Zn1 N3 92.03(6) . .
N1 Zn1 N3 91.72(6) . 2_666
N1 Zn1 N3 88.28(6) 2_666 2_666
N2 Zn1 N3 92.03(6) 2_666 2_666
N2 Zn1 N3 87.97(6) . 2_666
N3 Zn1 N3 180.0 . 2_666
C1 N1 C4 106.93(15) . .
C1 N1 Zn1 126.16(13) . .
C4 N1 Zn1 126.79(13) . .
C9 N2 C6 106.95(15) . .
C9 N2 Zn1 125.98(13) . .
C6 N2 Zn1 126.65(13) . .
C19 N3 C23 117.21(17) . .
C19 N3 Zn1 121.64(13) . .
C23 N3 Zn1 121.14(13) . .
N1 C1 C10 124.73(17) . .
N1 C1 C2 109.97(16) . .
C10 C1 C2 125.30(17) . .
C3 C2 C1 106.76(15) . .
C3 C2 C11 127.66(17) . .
C1 C2 C11 125.57(17) . .
C2 C3 C4 106.32(16) . .
C2 C3 C13 127.70(17) . .
C4 C3 C13 125.96(17) . .
N1 C4 C5 124.42(17) . .
N1 C4 C3 110.00(16) . .
C5 C4 C3 125.57(17) . .
C6 C5 C4 127.73(17) . .
N2 C6 C5 124.58(16) . .
N2 C6 C7 109.78(16) . .
C5 C6 C7 125.60(17) . .
C8 C7 C6 106.65(16) . .
C8 C7 C15 127.74(17) . .
C6 C7 C15 125.61(16) . .
C7 C8 C9 106.41(16) . .
C7 C8 C17 128.13(17) . .
C9 C8 C17 125.35(17) . .
N2 C9 C10 124.81(17) . 2_666
N2 C9 C8 110.19(16) . .
C10 C9 C8 124.99(17) 2_666 .
C9 C10 C1 127.77(18) 2_666 .
C2 C11 C12 113.58(15) . .
C3 C13 C14 112.17(16) . .
C7 C15 C16 113.53(16) . .
C8 C17 C18 112.05(15) . .
N3 C19 C20 123.46(19) . .
C19 C20 C21 118.84(19) . .
C20 C21 C22 118.34(19) . .
C23 C22 C21 118.91(19) . .
N3 C23 C22 123.24(18) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 N1 2.0643(16) .
Zn1 N1 2.0643(16) 2_666
Zn1 N2 2.0659(16) 2_666
Zn1 N2 2.0659(16) .
Zn1 N3 2.4029(16) .
Zn1 N3 2.4029(16) 2_666
N1 C1 1.366(2) .
N1 C4 1.367(2) .
N2 C9 1.368(2) .
N2 C6 1.370(2) .
N3 C19 1.343(3) .
N3 C23 1.344(2) .
C1 C10 1.403(3) .
C1 C2 1.452(2) .
C2 C3 1.367(3) .
C2 C11 1.507(2) .
C3 C4 1.457(2) .
C3 C13 1.501(2) .
C4 C5 1.406(2) .
C5 C6 1.395(2) .
C6 C7 1.460(2) .
C7 C8 1.370(3) .
C7 C15 1.503(2) .
C8 C9 1.457(2) .
C8 C17 1.498(2) .
C9 C10 1.400(3) 2_666
C10 C9 1.400(3) 2_666
C11 C12 1.532(3) .
C13 C14 1.532(3) .
C15 C16 1.528(3) .
C17 C18 1.532(3) .
C19 C20 1.384(3) .
C20 C21 1.387(3) .
C21 C22 1.393(3) .
C22 C23 1.384(3) .
