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#$Date: 2016-03-22 23:13:32 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179051 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/13/4301303.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_4301303
loop_
_publ_author_name
'Nathan J. Silvernail'
'Marilyn M. Olmstead'
'Bruce C. Noll'
_publ_contact_author_address
;University of Notre Dame
Department of Chemistry and Biochemistry
251 Nieuwland Science Hall
Notre Dame, IN 46556-5670
;
_publ_contact_author_email       W.R.Scheidt.1@nd.edu
_publ_contact_author_fax         1(574)6316652
_publ_contact_author_name        'Professor W. Robert Scheidt'
_publ_contact_author_phone       1(574)6315939
_publ_section_title
;
Tetragonal to Triclinic-A Phase Change for [Fe(TPP)(NO)]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              971
_journal_page_last               977
_journal_paper_doi               10.1021/ic801617q
_journal_volume                  48
_journal_year                    2009
_chemical_compound_source        synthesized
_chemical_formula_moiety         'C44 H28 Fe N5 O'
_chemical_formula_sum            'C44 H28 Fe N5 O'
_chemical_formula_weight         698.56
_chemical_name_common            '[Fe(TPP)(NO)]'
_space_group_IT_number           87
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      87
_symmetry_space_group_name_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 4/m'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.4152(2)
_cell_length_b                   13.4152(2)
_cell_length_c                   9.7151(3)
_cell_measurement_reflns_used    4123
_cell_measurement_temperature    272(2)
_cell_measurement_theta_max      26.4586
_cell_measurement_theta_min      2.5885
_cell_volume                     1748.40(7)
_computing_cell_refinement       'APEX2/SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2007; Sheldrick, 2003)'
_computing_molecular_graphics    'XP (Sheldrick, 1998)'
_computing_publication_material  'XCIF (Sheldrick, 2001)/enCIFer (CCDC, 2005)'
_computing_structure_refinement  'XL (Sheldrick, 2001)'
_computing_structure_solution    'XS (Sheldrick, 2001)'
_diffrn_ambient_temperature      272(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker X8-Apex II CCD diffractometer'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_av_sigmaI/netI    0.0112
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            11545
_diffrn_reflns_theta_full        27.87
_diffrn_reflns_theta_max         27.87
_diffrn_reflns_theta_min         2.15
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Siemens KFFMO2K-90'
_exptl_absorpt_coefficient_mu    0.474
_exptl_absorpt_correction_T_max  0.8783
_exptl_absorpt_correction_T_min  0.8783
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Sheldrick, G. M. (2007). SADABS. University of Göttingen. Germany.'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       octahedron
_exptl_crystal_F_000             722
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.287
_refine_diff_density_min         -0.141
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     82
_refine_ls_number_reflns         1101
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0391
_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)+(0.0698P)²+0.5801P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1132
_refine_ls_wR_factor_ref         0.1239
_reflns_number_gt                918
_reflns_number_total             1101
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801617q_si_002_08.cif
_cod_data_source_block           273_cryst_4
_cod_database_code               4301303
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+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
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.5000 0.5000 0.02458(14) 0.0458(5) Uani 0.50 4 d SP . .
N1 N 0.35686(13) 0.53668(13) 0.0000 0.0489(4) Uani 1 2 d S . .
N2 N 0.5000 0.5000 0.1998(6) 0.0494(11) Uani 0.50 4 d SP . .
O1 O 0.516(6) 0.4625(10) 0.2967(10) 0.095(15) Uani 0.13 1 d P . .
C(A1 C 0.27652(16) 0.47339(17) 0.0000 0.0513(5) Uani 1 2 d S . .
C(B1 C 0.18567(18) 0.52908(18) 0.0000 0.0617(6) Uani 1 2 d S . .
H(B1 H 0.1214 0.5030 0.0000 0.074 Uiso 1 2 calc SR . .
C(B2 C 0.21027(17) 0.62567(19) 0.0000 0.0610(6) Uani 1 2 d S . .
H(B2 H 0.1664 0.6793 0.0000 0.073 Uiso 1 2 calc SR . .
C(A2 C 0.31728(16) 0.63098(17) 0.0000 0.0520(5) Uani 1 2 d S . .
C(M1 C 0.37002(17) 0.71920(16) 0.0000 0.0511(5) Uani 1 2 d S . .
C10 C 0.31341(16) 0.81527(16) 0.0000 0.0535(5) Uani 1 2 d S . .
C11 C 0.28725(18) 0.86012(15) 0.1208(2) 0.0770(6) Uani 1 1 d . . .
H11 H 0.3056 0.8312 0.2040 0.092 Uiso 1 1 calc R . .
C12 C 0.2335(2) 0.94844(16) 0.1204(3) 0.0857(7) Uani 1 1 d . . .
H12 H 0.2158 0.9782 0.2033 0.103 Uiso 1 1 calc R . .
C13 C 0.2066(2) 0.99164(18) 0.0000 0.0730(7) Uani 1 2 d S . .
H13 H 0.1699 1.0505 0.0000 0.088 Uiso 1 2 calc SR . .
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'
Fe Fe 0.3463 0.8444 '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
Fe1 Fe1 N2 180.000(2) 9_665 . ?
Fe1 Fe1 N1 83.13(4) 9_665 11_565 ?
N2 Fe1 N1 96.87(4) . 11_565 ?
Fe1 Fe1 N1 83.13(4) 9_665 . ?
N2 Fe1 N1 96.87(4) . . ?
N1 Fe1 N1 89.180(10) 11_565 . ?
Fe1 Fe1 N1 83.13(4) 9_665 9_665 ?
N2 Fe1 N1 96.87(4) . 9_665 ?
N1 Fe1 N1 89.180(10) 11_565 9_665 ?
N1 Fe1 N1 166.26(8) . 9_665 ?
Fe1 Fe1 N1 83.13(4) 9_665 3_655 ?
N2 Fe1 N1 96.87(4) . 3_655 ?
N1 Fe1 N1 166.26(8) 11_565 3_655 ?
N1 Fe1 N1 89.180(10) . 3_655 ?
N1 Fe1 N1 89.180(10) 9_665 3_655 ?
Fe1 Fe1 N2 0.000(1) 9_665 9_665 ?
N2 Fe1 N2 180.000(1) . 9_665 ?
N1 Fe1 N2 83.13(4) 11_565 9_665 ?
N1 Fe1 N2 83.13(4) . 9_665 ?
N1 Fe1 N2 83.13(4) 9_665 9_665 ?
N1 Fe1 N2 83.13(4) 3_655 9_665 ?
C(A2 N1 C(A1 105.46(17) . . ?
C(A2 N1 Fe1 126.83(14) . . ?
C(A1 N1 Fe1 127.08(14) . . ?
C(A2 N1 Fe1 126.83(14) . 9_665 ?
C(A1 N1 Fe1 127.08(14) . 9_665 ?
Fe1 N1 Fe1 13.74(8) . 9_665 ?
O1 N2 O1 41.5(17) 3_655 2_665 ?
O1 N2 O1 41.5(17) 3_655 . ?
O1 N2 O1 60(3) 2_665 . ?
O1 N2 O1 60(3) 3_655 4_565 ?
O1 N2 O1 41.5(17) 2_665 4_565 ?
O1 N2 O1 41.5(17) . 4_565 ?
O1 N2 Fe1 149.9(13) 3_655 . ?
O1 N2 Fe1 149.9(13) 2_665 . ?
O1 N2 Fe1 149.9(13) . . ?
O1 N2 Fe1 149.9(13) 4_565 . ?
O1 N2 Fe1 149.9(13) 3_655 9_665 ?
O1 N2 Fe1 149.9(13) 2_665 9_665 ?
O1 N2 Fe1 149.9(13) . 9_665 ?
O1 N2 Fe1 149.9(13) 4_565 9_665 ?
Fe1 N2 Fe1 0.0 . 9_665 ?
O1 O1 O1 90.00(3) 3_655 4_565 ?
O1 O1 N2 69.3(9) 3_655 . ?
O1 O1 N2 69.3(8) 4_565 . ?
O1 O1 O1 45.00(3) 3_655 2_665 ?
O1 O1 O1 45.000(12) 4_565 2_665 ?
N2 O1 O1 59.9(13) . 2_665 ?
N1 C(A1 C(M1 125.86(19) . 3_655 ?
N1 C(A1 C(B1 110.3(2) . . ?
C(M1 C(A1 C(B1 123.9(2) 3_655 . ?
C(B2 C(B1 C(A1 107.2(2) . . ?
C(B2 C(B1 H(B1 126.4 . . ?
C(A1 C(B1 H(B1 126.4 . . ?
C(B1 C(B2 C(A2 107.1(2) . . ?
C(B1 C(B2 H(B2 126.4 . . ?
C(A2 C(B2 H(B2 126.4 . . ?
N1 C(A2 C(M1 126.4(2) . . ?
N1 C(A2 C(B2 109.9(2) . . ?
C(M1 C(A2 C(B2 123.7(2) . . ?
C(A2 C(M1 C(A1 123.2(2) . 11_565 ?
C(A2 C(M1 C10 118.6(2) . . ?
C(A1 C(M1 C10 118.13(19) 11_565 . ?
C11 C10 C11 118.6(2) 10 . ?
C11 C10 C(M1 120.70(11) 10 . ?
C11 C10 C(M1 120.70(11) . . ?
C10 C11 C12 120.53(19) . . ?
C10 C11 H11 119.7 . . ?
C12 C11 H11 119.7 . . ?
C13 C12 C11 120.4(2) . . ?
C13 C12 H12 119.8 . . ?
C11 C12 H12 119.8 . . ?
C12 C13 C12 119.4(2) 10 . ?
C12 C13 H13 120.3 10 . ?
C12 C13 H13 120.3 . . ?
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 Fe1 0.478(3) 9_665 ?
Fe1 N2 1.702(5) . ?
Fe1 N1 1.9966(18) 11_565 ?
Fe1 N1 1.9966(18) . ?
Fe1 N1 1.9966(18) 9_665 ?
Fe1 N1 1.9966(18) 3_655 ?
Fe1 N2 2.180(6) 9_665 ?
N1 C(A2 1.372(3) . ?
N1 C(A1 1.372(3) . ?
N1 Fe1 1.9966(18) 9_665 ?
N2 O1 1.088(18) 3_655 ?
N2 O1 1.088(18) 2_665 ?
N2 O1 1.088(18) . ?
N2 O1 1.088(18) 4_565 ?
N2 Fe1 2.180(6) 9_665 ?
O1 O1 0.77(4) 3_655 ?
O1 O1 0.77(4) 4_565 ?
O1 O1 1.09(6) 2_665 ?
C(A1 C(M1 1.388(3) 3_655 ?
C(A1 C(B1 1.430(3) . ?
C(B1 C(B2 1.337(4) . ?
C(B1 H(B1 0.9300 . ?
C(B2 C(A2 1.437(3) . ?
C(B2 H(B2 0.9300 . ?
C(A2 C(M1 1.379(3) . ?
C(M1 C(A1 1.388(3) 11_565 ?
C(M1 C10 1.496(3) . ?
C10 C11 1.364(2) 10 ?
C10 C11 1.364(2) . ?
C11 C12 1.387(3) . ?
C11 H11 0.9300 . ?
C12 C13 1.354(3) . ?
C12 H12 0.9300 . ?
C13 C12 1.354(3) 10 ?
C13 H13 0.9300 . ?
