#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:44:04 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178913 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/42/4114248.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_4114248
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            'C76 H96 N8 O2 Zn2'
_chemical_formula_weight         1284.35
_chemical_name_common            (dioxane)[Zn(OEP)]2
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 90.021(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.9979(11)
_cell_length_b                   9.7677(9)
_cell_length_c                   22.9303(17)
_cell_measurement_reflns_used    928
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      28.5
_cell_measurement_theta_min      2.7
_cell_volume                     3359.2(5)
_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 8.3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0601
_diffrn_reflns_av_sigmaI/netI    0.0514
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            39309
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         0.89
_exptl_absorpt_coefficient_mu    0.767
_exptl_absorpt_correction_T_max  0.934
_exptl_absorpt_correction_T_min  0.887
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.03 (Sheldrick, 2002)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_description       prism
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.075
_refine_diff_density_min         -0.599
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         8313
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0415
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0589P)²+0.9075P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0971
_refine_ls_wR_factor_ref         0.1065
_reflns_number_gt                6726
_reflns_number_total             8314
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ja030221f_2.cif
_cod_data_source_block           hml55
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4114248
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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 0.98329(2) 0.82914(3) 0.538034(16) 0.01071(8) Uani 1 1 d .
O1 O 0.96469(11) 0.60158(18) 0.53770(10) 0.0167(4) Uani 1 1 d .
N1 N 0.98550(16) 0.8472(2) 0.44891(9) 0.0112(5) Uani 1 1 d .
N2 N 0.84823(13) 0.8583(2) 0.53738(12) 0.0120(4) Uani 1 1 d .
N3 N 0.98393(17) 0.8365(2) 0.62702(10) 0.0116(4) Uani 1 1 d .
N4 N 1.12011(13) 0.8173(2) 0.53864(12) 0.0110(4) Uani 1 1 d .
C1 C 1.0580(2) 0.8280(3) 0.41368(13) 0.0114(5) Uani 1 1 d .
C2 C 1.0303(2) 0.8208(3) 0.35269(12) 0.0119(6) Uani 1 1 d .
C3 C 0.93943(19) 0.8354(3) 0.35238(13) 0.0123(5) Uani 1 1 d .
C4 C 0.9119(2) 0.8510(3) 0.41238(13) 0.0109(6) Uani 1 1 d .
C5 C 0.8237(2) 0.8637(3) 0.43161(13) 0.0134(6) Uani 1 1 d .
H5A H 0.7792 0.8710 0.4022 0.016 Uiso 1 1 calc R
C6 C 0.7941(2) 0.8669(3) 0.48917(14) 0.0120(6) Uani 1 1 d .
C7 C 0.70100(18) 0.8790(3) 0.50728(13) 0.0128(6) Uani 1 1 d .
C8 C 0.70103(18) 0.8762(3) 0.56657(13) 0.0131(6) Uani 1 1 d .
C9 C 0.79351(19) 0.8649(3) 0.58528(13) 0.0129(6) Uani 1 1 d .
C10 C 0.82309(19) 0.8620(3) 0.64269(12) 0.0136(6) Uani 1 1 d .
H10A H 0.7785 0.8689 0.6719 0.016 Uiso 1 1 calc R
C11 C 0.9108(2) 0.8500(3) 0.66232(13) 0.0127(6) Uani 1 1 d .
C12 C 0.9383(2) 0.8482(3) 0.72293(13) 0.0156(6) Uani 1 1 d .
C13 C 1.0286(2) 0.8314(3) 0.72371(12) 0.0138(6) Uani 1 1 d .
C14 C 1.0563(2) 0.8255(3) 0.66319(13) 0.0133(5) Uani 1 1 d .
C15 C 1.1444(2) 0.8108(3) 0.64398(13) 0.0135(6) Uani 1 1 d .
H15A H 1.1888 0.8037 0.6734 0.016 Uiso 1 1 calc R
C16 C 1.17387(19) 0.8055(3) 0.58643(13) 0.0129(6) Uani 1 1 d .
C17 C 1.26623(18) 0.7859(3) 0.56854(13) 0.0126(6) Uani 1 1 d .
C18 C 1.26642(19) 0.7853(3) 0.50922(13) 0.0122(6) Uani 1 1 d .
C19 C 1.1747(2) 0.8069(3) 0.49097(13) 0.0115(6) Uani 1 1 d .
C20 C 1.1449(2) 0.8118(3) 0.43320(14) 0.0120(6) Uani 1 1 d .
H20A H 1.1894 0.8031 0.4039 0.014 Uiso 1 1 calc R
C21 C 1.0902(2) 0.7944(3) 0.30178(13) 0.0168(6) Uani 1 1 d .
H21A H 1.1463 0.8463 0.3073 0.020 Uiso 1 1 calc R
H21B H 1.0611 0.8291 0.2659 0.020 Uiso 1 1 calc R
C22 C 1.1126(2) 0.6428(3) 0.29351(15) 0.0260(7) Uani 1 1 d .
H22A H 1.1531 0.6324 0.2603 0.039 Uiso 1 1 calc R
H22B H 1.0576 0.5914 0.2861 0.039 Uiso 1 1 calc R
H22C H 1.1413 0.6076 0.3289 0.039 Uiso 1 1 calc R
C23 C 0.8776(2) 0.8295(3) 0.30083(14) 0.0192(7) Uani 1 1 d .
H23A H 0.9096 0.8612 0.2656 0.023 Uiso 1 1 calc R
H23B H 0.8267 0.8922 0.3075 0.023 Uiso 1 1 calc R
C24 C 0.8423(2) 0.6847(4) 0.29043(16) 0.0285(8) Uani 1 1 d .
H24A H 0.8023 0.6849 0.2566 0.043 Uiso 1 1 calc R
H24B H 0.8095 0.6537 0.3250 0.043 Uiso 1 1 calc R
H24C H 0.8924 0.6227 0.2831 0.043 Uiso 1 1 calc R
C25 C 0.62257(17) 0.8868(3) 0.46628(15) 0.0154(5) Uani 1 1 d .
H25A H 0.6387 0.9452 0.4326 0.019 Uiso 1 1 calc R
H25B H 0.5720 0.9309 0.4867 0.019 Uiso 1 1 calc R
C26 C 0.5927(2) 0.7468(3) 0.44383(13) 0.0209(7) Uani 1 1 d .
H26A H 0.5418 0.7583 0.4175 0.031 Uiso 1 1 calc R
H26B H 0.5752 0.6891 0.4768 0.031 Uiso 1 1 calc R
H26C H 0.6420 0.7033 0.4228 0.031 Uiso 1 1 calc R
C27 C 0.62234(19) 0.8803(3) 0.60728(13) 0.0167(6) Uani 1 1 d .
H27A H 0.5708 0.9212 0.5866 0.020 Uiso 1 1 calc R
H27B H 0.6368 0.9401 0.6408 0.020 Uiso 1 1 calc R
C28 C 0.5962(2) 0.7397(4) 0.62977(15) 0.0248(7) Uani 1 1 d .
H28A H 0.5466 0.7487 0.6573 0.037 Uiso 1 1 calc R
H28B H 0.6473 0.6978 0.6495 0.037 Uiso 1 1 calc R
H28C H 0.5779 0.6819 0.5970 0.037 Uiso 1 1 calc R
C29 C 0.8769(2) 0.8575(3) 0.77459(14) 0.0200(7) Uani 1 1 d .
H29A H 0.8249 0.9151 0.7643 0.024 Uiso 1 1 calc R
H29B H 0.9086 0.9023 0.8073 0.024 Uiso 1 1 calc R
C30 C 0.8443(2) 0.7179(4) 0.79413(16) 0.0301(9) Uani 1 1 d .
H30A H 0.8050 0.7285 0.8280 0.045 Uiso 1 1 calc R
H30B H 0.8955 0.6608 0.8048 0.045 Uiso 1 1 calc R
H30C H 0.8114 0.6742 0.7622 0.045 Uiso 1 1 calc R
C31 C 1.0889(2) 0.8145(3) 0.77570(13) 0.0160(6) Uani 1 1 d .
H31A H 1.0583 0.8501 0.8108 0.019 Uiso 1 1 calc R
H31B H 1.1436 0.8695 0.7697 0.019 Uiso 1 1 calc R
C32 C 1.1151(2) 0.6655(3) 0.78615(15) 0.0226(7) Uani 1 1 d .
H32A H 1.1527 0.6594 0.8211 0.034 Uiso 1 1 calc R
H32B H 1.1483 0.6311 0.7524 0.034 Uiso 1 1 calc R
H32C H 1.0613 0.6102 0.7917 0.034 Uiso 1 1 calc R
C33 C 1.34338(19) 0.7634(3) 0.60915(13) 0.0152(6) Uani 1 1 d .
H33A H 1.3378 0.8268 0.6426 0.018 Uiso 1 1 calc R
H33B H 1.3994 0.7860 0.5885 0.018 Uiso 1 1 calc R
C34 C 1.3492(2) 0.6176(3) 0.63191(15) 0.0254(7) Uani 1 1 d .
H34A H 1.4008 0.6092 0.6579 0.038 Uiso 1 1 calc R
H34B H 1.3559 0.5543 0.5991 0.038 Uiso 1 1 calc R
H34C H 1.2947 0.5953 0.6535 0.038 Uiso 1 1 calc R
C35 C 1.34383(17) 0.7614(3) 0.46900(13) 0.0134(6) Uani 1 1 d .
H35A H 1.3998 0.7850 0.4896 0.016 Uiso 1 1 calc R
H35B H 1.3383 0.8228 0.4348 0.016 Uiso 1 1 calc R
C36 C 1.3492(2) 0.6125(3) 0.44776(13) 0.0229(7) Uani 1 1 d .
H36A H 1.4005 0.6020 0.4217 0.034 Uiso 1 1 calc R
H36B H 1.2944 0.5891 0.4266 0.034 Uiso 1 1 calc R
H36C H 1.3559 0.5513 0.4814 0.034 Uiso 1 1 calc R
C37 C 1.03336(19) 0.5100(3) 0.55707(11) 0.0183(6) Uani 1 1 d .
H37A H 1.0060 0.4288 0.5757 0.022 Uiso 1 1 calc R
H37B H 1.0712 0.5565 0.5864 0.022 Uiso 1 1 calc R
C38 C 0.9100(2) 0.5346(3) 0.49381(14) 0.0193(6) Uani 1 1 d .
H38A H 0.8633 0.5986 0.4801 0.023 Uiso 1 1 calc R
H38B H 0.8801 0.4539 0.5112 0.023 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'
O O 0.0106 0.0060 '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_3
N3 Zn1 N2 90.39(11) .
N3 Zn1 N1 172.96(8) .
N2 Zn1 N1 89.84(10) .
N3 Zn1 N4 89.48(11) .
N2 Zn1 N4 175.21(9) .
N1 Zn1 N4 89.71(10) .
N3 Zn1 O1 92.22(9) .
N2 Zn1 O1 90.86(7) .
N1 Zn1 O1 94.81(9) .
N4 Zn1 O1 93.93(7) .
C37 O1 C38 109.8(2) .
C37 O1 Zn1 121.89(16) .
C38 O1 Zn1 121.26(17) .
C1 N1 C4 106.2(2) .
C1 N1 Zn1 126.14(19) .
C4 N1 Zn1 126.26(19) .
C9 N2 C6 106.7(2) .
C9 N2 Zn1 126.4(2) .
C6 N2 Zn1 126.8(2) .
C11 N3 C14 106.5(2) .
C11 N3 Zn1 126.2(2) .
C14 N3 Zn1 127.3(2) .
C16 N4 C19 106.4(2) .
C16 N4 Zn1 126.8(2) .
C19 N4 Zn1 126.6(2) .
N1 C1 C20 124.9(3) .
N1 C1 C2 110.2(3) .
C20 C1 C2 124.8(3) .
C3 C2 C1 106.5(3) .
C3 C2 C21 127.7(3) .
C1 C2 C21 125.7(3) .
C2 C3 C4 106.9(3) .
C2 C3 C23 127.9(3) .
C4 C3 C23 125.2(3) .
N1 C4 C5 124.4(3) .
N1 C4 C3 110.2(2) .
C5 C4 C3 125.4(3) .
C6 C5 C4 127.0(3) .
N2 C6 C5 125.0(3) .
N2 C6 C7 109.9(3) .
C5 C6 C7 125.1(3) .
C8 C7 C6 106.4(3) .
C8 C7 C25 128.7(3) .
C6 C7 C25 124.9(3) .
C7 C8 C9 107.2(3) .
C7 C8 C27 128.3(3) .
C9 C8 C27 124.5(3) .
N2 C9 C10 124.5(3) .
N2 C9 C8 109.7(2) .
C10 C9 C8 125.8(3) .
C9 C10 C11 127.5(3) .
N3 C11 C10 124.9(3) .
N3 C11 C12 109.7(3) .
C10 C11 C12 125.3(3) .
C13 C12 C11 107.2(3) .
C13 C12 C29 127.3(3) .
C11 C12 C29 125.5(3) .
C12 C13 C14 106.1(3) .
C12 C13 C31 128.3(3) .
C14 C13 C31 125.6(3) .
N3 C14 C15 124.4(3) .
N3 C14 C13 110.5(3) .
C15 C14 C13 125.2(3) .
C16 C15 C14 127.0(3) .
N4 C16 C15 124.7(3) .
N4 C16 C17 110.3(2) .
C15 C16 C17 125.0(3) .
C18 C17 C16 106.5(3) .
C18 C17 C33 128.2(3) .
C16 C17 C33 125.2(3) .
C17 C18 C19 106.6(3) .
C17 C18 C35 128.1(3) .
C19 C18 C35 125.3(3) .
N4 C19 C20 124.3(3) .
N4 C19 C18 110.3(3) .
C20 C19 C18 125.4(3) .
C1 C20 C19 127.5(3) .
C2 C21 C22 113.3(3) .
C3 C23 C24 111.8(3) .
C7 C25 C26 113.2(2) .
C8 C27 C28 112.8(3) .
C12 C29 C30 112.1(3) .
C13 C31 C32 112.6(3) .
C17 C33 C34 113.2(3) .
C18 C35 C36 112.5(2) .
O1 C37 C38 110.2(2) 3_766
O1 C38 C37 110.3(2) 3_766
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 N3 2.042(2) .
Zn1 N2 2.046(2) .
Zn1 N1 2.051(2) .
Zn1 N4 2.055(2) .
Zn1 O1 2.2402(18) .
O1 C37 1.434(3) .
O1 C38 1.454(4) .
N1 C1 1.368(4) .
N1 C4 1.386(4) .
N2 C9 1.373(4) .
N2 C6 1.374(4) .
N3 C11 1.370(4) .
N3 C14 1.370(4) .
N4 C16 1.365(4) .
N4 C19 1.369(4) .
C1 C20 1.387(4) .
C1 C2 1.461(4) .
C2 C3 1.370(4) .
C2 C21 1.496(4) .
C3 C4 1.444(4) .
C3 C23 1.504(4) .
C4 C5 1.401(4) .
C5 C6 1.393(4) .
C6 C7 1.462(4) .
C7 C8 1.360(3) .
C7 C25 1.507(4) .
C8 C9 1.456(4) .
C8 C27 1.506(4) .
C9 C10 1.389(4) .
C10 C11 1.395(4) .
C11 C12 1.450(4) .
C12 C13 1.365(4) .
C12 C29 1.504(4) .
C13 C14 1.450(4) .
C13 C31 1.505(4) .
C14 C15 1.400(4) .
C15 C16 1.393(4) .
C16 C17 1.457(4) .
C17 C18 1.360(3) .
C17 C33 1.501(4) .
C18 C19 1.454(4) .
C18 C35 1.501(4) .
C19 C20 1.398(4) .
C21 C22 1.530(4) .
C23 C24 1.529(5) .
C25 C26 1.528(4) .
C27 C28 1.519(4) .
C29 C30 1.515(5) .
C31 C32 1.526(4) .
C33 C34 1.519(4) .
C35 C36 1.536(4) .
C37 C38 1.508(4) 3_766
C38 C37 1.508(4) 3_766
