#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:49:54 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179209 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/40/4314011.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_4314011
loop_
_publ_author_name
'Changsheng Cao'
'S. Dahal'
'Mayou Shang'
'Alicia M. Beatty'
'Wendy Hibbs'
'Charles E. Schulz'
'W. Robert Scheidt'
_publ_section_title
;
 Effect of the Sixth Axial Ligand in CS-Ligated
 Iron(II)octaethylporphyrinates: Structural and Mössbauer Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5202
_journal_page_last               5210
_journal_paper_doi               10.1021/ic030043r
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         'C38 H52 Fe N4 O S'
_chemical_formula_sum            'C38 H52 Fe N4 O S'
_chemical_formula_weight         668.75
_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                90.2610(10)
_cell_angle_beta                 100.3620(10)
_cell_angle_gamma                114.6640(10)
_cell_formula_units_Z            1
_cell_length_a                   9.0599(5)
_cell_length_b                   9.4389(5)
_cell_length_c                   11.0676(6)
_cell_measurement_reflns_used    6525
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.384
_cell_volume                     842.72(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0189
_diffrn_reflns_av_sigmaI/netI    0.0278
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9096
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    0.546
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             358
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.450
_refine_diff_density_min         -0.566
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.283
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         4178
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.283
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0587
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0278P)²+1.5067P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1395
_refine_ls_wR_factor_ref         0.1403
_reflns_number_gt                3956
_reflns_number_total             4178
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic030043r_3.cif
_cod_data_source_block           meoh
_cod_database_code               4314011
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe -0.5000 -0.5000 0.5000 0.02162(15) Uani 1 2 d S . .
N1 N -0.3870(3) -0.6345(2) 0.56181(19) 0.0172(4) Uani 1 1 d . A .
CA1 C -0.2738(3) -0.6644(3) 0.5107(2) 0.0185(5) Uani 1 1 d . . .
S1 S -0.1665(3) -0.2321(2) 0.69425(19) 0.0256(4) Uani 0.50 1 d P A 1
C19 C -0.3231(14) -0.3514(9) 0.6006(11) 0.0194(16) Uani 0.50 1 d P A 1
O51 O -0.3028(10) -0.2978(6) 0.5926(7) 0.0209(13) Uani 0.50 1 d P A 2
H51 H -0.2293 -0.2690 0.5322 0.025 Uiso 1 1 d R A 2
C51 C -0.2022(10) -0.2942(10) 0.7054(8) 0.0295(17) Uani 0.50 1 d P A 2
H51A H -0.1220 -0.2055 0.7609 0.035 Uiso 1 1 d R A 2
H51B H -0.1647 -0.3693 0.6890 0.035 Uiso 1 1 d R A 2
H51C H -0.2764 -0.3553 0.7543 0.035 Uiso 1 1 d R A 2
CB1 C -0.2188(3) -0.7679(3) 0.5829(2) 0.0193(5) Uani 1 1 d . A .
N2 N -0.6124(3) -0.5419(2) 0.64366(19) 0.0181(4) Uani 1 1 d . A .
CB2 C -0.2961(3) -0.7972(3) 0.6801(2) 0.0196(5) Uani 1 1 d . . .
CA2 C -0.3981(3) -0.7115(3) 0.6680(2) 0.0189(5) Uani 1 1 d . A .
CM1 C -0.4920(3) -0.7058(3) 0.7518(2) 0.0199(5) Uani 1 1 d . . .
HM1 H -0.4819 -0.7604 0.8228 0.024 Uiso 1 1 d R A .
CA3 C -0.5920(3) -0.6272(3) 0.7410(2) 0.0192(5) Uani 1 1 d . A .
CB3 C -0.6928(3) -0.6263(3) 0.8288(2) 0.0213(5) Uani 1 1 d . . .
CB4 C -0.7771(3) -0.5419(3) 0.7829(2) 0.0209(5) Uani 1 1 d . A .
CA4 C -0.7259(3) -0.4888(3) 0.6682(2) 0.0194(5) Uani 1 1 d . . .
C11 C -0.1044(3) -0.8323(3) 0.5481(3) 0.0240(5) Uani 1 1 d . . .
H11A H -0.0227 -0.7544 0.5244 0.029 Uiso 1 1 d R A .
H11B H -0.0779 -0.8782 0.6177 0.029 Uiso 1 1 d R . .
C12 C -0.1922(4) -0.9640(3) 0.4440(3) 0.0272(6) Uani 1 1 d . A .
H12A H -0.2954 -1.0522 0.4611 0.033 Uiso 1 1 d R . .
H12B H -0.2137 -0.9283 0.3745 0.033 Uiso 1 1 d R . .
H12C H -0.1162 -0.9948 0.4262 0.033 Uiso 1 1 d R . .
C21 C -0.2860(3) -0.9006(3) 0.7810(2) 0.0235(5) Uani 1 1 d . A .
H21A H -0.2597 -0.8492 0.8584 0.028 Uiso 1 1 d R . .
H21B H -0.1971 -0.9169 0.7793 0.028 Uiso 1 1 d R . .
C22 C -0.4352(4) -1.0590(3) 0.7631(3) 0.0325(7) Uani 1 1 d . . .
H22A H -0.4259 -1.1195 0.8312 0.039 Uiso 1 1 d R A .
H22B H -0.4574 -1.1215 0.6764 0.039 Uiso 1 1 d R . .
H22C H -0.5224 -1.0412 0.7756 0.039 Uiso 1 1 d R . .
C31 C -0.7019(4) -0.7090(4) 0.9447(3) 0.0285(6) Uani 1 1 d . A .
H31A H -0.5880 -0.6802 0.9873 0.034 Uiso 1 1 d R . .
H31B H -0.7368 -0.6613 0.9989 0.034 Uiso 1 1 d R . .
C32 C -0.8111(4) -0.8840(4) 0.9213(3) 0.0364(7) Uani 1 1 d . . .
H32A H -0.7552 -0.9291 0.8759 0.044 Uiso 1 1 d R A .
H32B H -0.8218 -0.9555 0.9719 0.044 Uiso 1 1 d R . .
H32C H -0.9325 -0.9117 0.8775 0.044 Uiso 1 1 d R . .
C41 C -0.8991(3) -0.5043(3) 0.8363(3) 0.0256(6) Uani 1 1 d . . .
H41A H -0.9455 -0.5756 0.8798 0.031 Uiso 1 1 d R A .
H41B H -0.9801 -0.5186 0.7852 0.031 Uiso 1 1 d R . .
C42 C -0.8232(4) -0.3408(4) 0.9039(3) 0.0352(7) Uani 1 1 d . A .
H42A H -0.8995 -0.3207 0.9356 0.042 Uiso 1 1 d R . .
H42B H -0.7640 -0.2677 0.8603 0.042 Uiso 1 1 d R . .
H42C H -0.7555 -0.3425 0.9544 0.042 Uiso 1 1 d R . .
CM2 C -0.7798(3) -0.3948(3) 0.5952(2) 0.0201(5) Uani 1 1 d . . .
HM2 H -0.8545 -0.3696 0.6188 0.024 Uiso 1 1 d 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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 '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'
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
_geom_angle_publ_flag
C19 Fe1 C19 180.0(5) . 2_446 ?
C19 Fe1 N1 97.5(3) . 2_446 ?
C19 Fe1 N1 82.5(3) 2_446 2_446 ?
C19 Fe1 N1 82.4(3) . . ?
C19 Fe1 N1 97.6(3) 2_446 . ?
N1 Fe1 N1 180.0 2_446 . ?
C19 Fe1 N2 92.9(3) . 2_446 ?
C19 Fe1 N2 87.1(3) 2_446 2_446 ?
N1 Fe1 N2 89.72(8) 2_446 2_446 ?
N1 Fe1 N2 90.28(8) . 2_446 ?
C19 Fe1 N2 87.1(3) . . ?
C19 Fe1 N2 92.9(3) 2_446 . ?
N1 Fe1 N2 90.28(8) 2_446 . ?
N1 Fe1 N2 89.72(8) . . ?
N2 Fe1 N2 180.00(11) 2_446 . ?
C19 Fe1 O51 168.8(4) . 2_446 ?
C19 Fe1 O51 11.2(4) 2_446 2_446 ?
N1 Fe1 O51 92.34(19) 2_446 2_446 ?
N1 Fe1 O51 87.67(19) . 2_446 ?
N2 Fe1 O51 92.4(2) 2_446 2_446 ?
N2 Fe1 O51 87.6(2) . 2_446 ?
C19 Fe1 O51 11.2(4) . . ?
C19 Fe1 O51 168.8(4) 2_446 . ?
N1 Fe1 O51 87.66(19) 2_446 . ?
N1 Fe1 O51 92.33(19) . . ?
N2 Fe1 O51 87.6(2) 2_446 . ?
N2 Fe1 O51 92.4(2) . . ?
O51 Fe1 O51 180.0 2_446 . ?
CA1 N1 CA2 104.9(2) . . ?
CA1 N1 Fe1 127.22(17) . . ?
CA2 N1 Fe1 127.78(16) . . ?
N1 CA1 CM2 124.8(2) . 2_446 ?
N1 CA1 CB1 110.9(2) . . ?
CM2 CA1 CB1 124.3(2) 2_446 . ?
C19 S1 H51 43.8 . . ?
C19 S1 H51A 147.8 . . ?
H51 S1 H51A 168.1 . . ?
C19 S1 H51B 69.5 . . ?
H51 S1 H51B 84.3 . . ?
H51A S1 H51B 98.2 . . ?
C19 S1 H51C 67.7 . . ?
H51 S1 H51C 110.9 . . ?
H51A S1 H51C 80.3 . . ?
H51B S1 H51C 60.9 . . ?
S1 C19 Fe1 175.4(6) . . ?
S1 C19 H51 76.2 . . ?
Fe1 C19 H51 106.5 . . ?
C51 O51 Fe1 124.2(5) . . ?
C51 O51 H51 105.7 . . ?
Fe1 O51 H51 100.9 . . ?
O51 C51 H51A 129.5 . . ?
O51 C51 H51B 102.4 . . ?
H51A C51 H51B 114.4 . . ?
O51 C51 H51C 104.9 . . ?
H51A C51 H51C 104.4 . . ?
H51B C51 H51C 95.8 . . ?
CB2 CB1 CA1 106.6(2) . . ?
CB2 CB1 C11 128.8(2) . . ?
CA1 CB1 C11 124.5(2) . . ?
CA3 N2 CA4 105.1(2) . . ?
CA3 N2 Fe1 127.74(17) . . ?
CA4 N2 Fe1 127.13(17) . . ?
CB1 CB2 CA2 106.7(2) . . ?
CB1 CB2 C21 128.4(2) . . ?
CA2 CB2 C21 124.9(2) . . ?
CM1 CA2 N1 124.5(2) . . ?
CM1 CA2 CB2 124.8(2) . . ?
N1 CA2 CB2 110.8(2) . . ?
CA2 CM1 CA3 125.7(2) . . ?
CA2 CM1 HM1 114.5 . . ?
CA3 CM1 HM1 119.8 . . ?
N2 CA3 CM1 124.5(2) . . ?
N2 CA3 CB3 110.8(2) . . ?
CM1 CA3 CB3 124.6(2) . . ?
CB4 CB3 CA3 106.6(2) . . ?
CB4 CB3 C31 128.5(2) . . ?
CA3 CB3 C31 124.9(2) . . ?
CB3 CB4 CA4 106.8(2) . . ?
CB3 CB4 C41 129.0(2) . . ?
CA4 CB4 C41 124.2(2) . . ?
CM2 CA4 N2 124.7(2) . . ?
CM2 CA4 CB4 124.6(2) . . ?
N2 CA4 CB4 110.6(2) . . ?
CB1 C11 C12 112.1(2) . . ?
CB1 C11 H11A 107.2 . . ?
C12 C11 H11A 109.8 . . ?
CB1 C11 H11B 104.0 . . ?
C12 C11 H11B 106.2 . . ?
H11A C11 H11B 117.5 . . ?
C11 C12 H12A 114.1 . . ?
C11 C12 H12B 111.3 . . ?
H12A C12 H12B 110.6 . . ?
C11 C12 H12C 107.4 . . ?
H12A C12 H12C 114.1 . . ?
H12B C12 H12C 98.4 . . ?
CB2 C21 C22 113.3(2) . . ?
CB2 C21 H21A 112.2 . . ?
C22 C21 H21A 114.1 . . ?
CB2 C21 H21B 106.4 . . ?
C22 C21 H21B 107.9 . . ?
H21A C21 H21B 102.0 . . ?
C21 C22 H22A 110.5 . . ?
C21 C22 H22B 113.2 . . ?
H22A C22 H22B 112.4 . . ?
C21 C22 H22C 106.7 . . ?
H22A C22 H22C 99.7 . . ?
H22B C22 H22C 113.4 . . ?
CB3 C31 C32 113.0(2) . . ?
CB3 C31 H31A 106.7 . . ?
C32 C31 H31A 115.2 . . ?
CB3 C31 H31B 108.5 . . ?
C32 C31 H31B 111.9 . . ?
H31A C31 H31B 100.7 . . ?
C31 C32 H32A 107.0 . . ?
C31 C32 H32B 128.5 . . ?
H32A C32 H32B 88.5 . . ?
C31 C32 H32C 113.8 . . ?
H32A C32 H32C 113.1 . . ?
H32B C32 H32C 103.4 . . ?
CB4 C41 C42 113.4(2) . . ?
CB4 C41 H41A 108.7 . . ?
C42 C41 H41A 113.4 . . ?
CB4 C41 H41B 111.5 . . ?
C42 C41 H41B 111.6 . . ?
H41A C41 H41B 97.2 . . ?
C41 C42 H42A 111.8 . . ?
C41 C42 H42B 112.5 . . ?
H42A C42 H42B 115.4 . . ?
C41 C42 H42C 103.5 . . ?
H42A C42 H42C 111.6 . . ?
H42B C42 H42C 100.9 . . ?
CA4 CM2 CA1 125.7(2) . 2_446 ?
CA4 CM2 HM2 117.0 . . ?
CA1 CM2 HM2 117.2 2_446 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 C19 1.800(12) . ?
Fe1 C19 1.801(12) 2_446 ?
Fe1 N1 1.992(2) 2_446 ?
Fe1 N1 1.992(2) . ?
Fe1 N2 1.994(2) 2_446 ?
Fe1 N2 1.994(2) . ?
Fe1 O51 2.089(7) 2_446 ?
Fe1 O51 2.089(7) . ?
N1 CA1 1.379(3) . ?
N1 CA2 1.382(3) . ?
CA1 CM2 1.381(4) 2_446 ?
CA1 CB1 1.453(4) . ?
S1 C19 1.576(12) . ?
S1 H51 1.7673 . ?
S1 H51A 0.7594 . ?
S1 H51B 1.3019 . ?
S1 H51C 1.4367 . ?
C19 H51 1.2594 . ?
O51 C51 1.398(11) . ?
O51 H51 0.9870 . ?
C51 H51A 0.9663 . ?
C51 H51B 0.9339 . ?
C51 H51C 0.9419 . ?
CB1 CB2 1.356(4) . ?
CB1 C11 1.503(3) . ?
N2 CA3 1.379(3) . ?
N2 CA4 1.382(3) . ?
CB2 CA2 1.452(3) . ?
CB2 C21 1.501(4) . ?
CA2 CM1 1.381(3) . ?
CM1 CA3 1.382(4) . ?
CM1 HM1 0.9532 . ?
CA3 CB3 1.451(3) . ?
CB3 CB4 1.359(4) . ?
CB3 C31 1.502(4) . ?
CB4 CA4 1.450(3) . ?
CB4 C41 1.503(3) . ?
CA4 CM2 1.380(4) . ?
C11 C12 1.529(4) . ?
C11 H11A 0.8794 . ?
C11 H11B 0.9292 . ?
C12 H12A 1.0090 . ?
C12 H12B 0.8638 . ?
C12 H12C 0.9014 . ?
C21 C22 1.522(4) . ?
C21 H21A 0.9228 . ?
C21 H21B 0.8842 . ?
C22 H22A 0.9603 . ?
C22 H22B 1.0649 . ?
C22 H22C 0.9068 . ?
C31 C32 1.521(4) . ?
C31 H31A 0.9756 . ?
C31 H31B 0.9192 . ?
C32 H32A 0.9797 . ?
C32 H32B 0.8643 . ?
C32 H32C 1.0390 . ?
C41 C42 1.528(4) . ?
C41 H41A 0.8370 . ?
C41 H41B 0.8025 . ?
C42 H42A 0.9122 . ?
C42 H42B 0.8860 . ?
C42 H42C 0.7579 . ?
CM2 CA1 1.381(4) 2_446 ?
CM2 HM2 0.8833 . ?
