#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:12:28 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179050 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/12/4301297.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_4301297
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]'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                82.25(2)
_cell_angle_beta                 65.78(2)
_cell_angle_gamma                69.44(2)
_cell_formula_units_Z            1
_cell_length_a                   9.754(2)
_cell_length_b                   9.943(2)
_cell_length_c                   10.394(3)
_cell_measurement_temperature    90(2)
_cell_volume                     860.7(4)
_computing_cell_refinement       'APEX2/SAINT (Bruker, 2004)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2004; Sheldrick, 2001)'
_computing_molecular_graphics    'Platon (Spek, 2004)'
_computing_publication_material  'XCIF (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full .968
_diffrn_measured_fraction_theta_max .968
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       'ω and φ 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0795
_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       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4337
_diffrn_reflns_theta_full        27.71
_diffrn_reflns_theta_max         27.71
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    0.481
_exptl_absorpt_correction_T_max  0.9625
_exptl_absorpt_correction_T_min  0.9057
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Blessing, R.H. ACTA Cryst. (1995) A51, 33-38'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'square bipyramid'
_exptl_crystal_F_000             361
_exptl_crystal_recrystallization_method
'liquid diffusion (chloroform/methanol)'
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.08
_refine_diff_density_max         .498
_refine_diff_density_min         -.358
_refine_diff_density_rms         .067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.949
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         4337
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.949
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_gt           0.0476
_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)+(0.0648P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1084
_refine_ls_wR_factor_ref         0.1174
_reflns_number_gt                2843
_reflns_number_total             4337
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801617q_si_002_02.cif
_cod_data_source_block           90_cryst_1
_cod_database_code               4301297
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 0.4801(5) 0.4983(7) 0.4996(7) 0.0196(5) Uani 0.50 1 d P . .
N1 N 0.4632(2) 0.68161(18) 0.39282(19) 0.0200(4) Uani 1 1 d . . .
N2 N 0.3569(2) 0.60885(18) 0.67908(19) 0.0200(4) Uani 1 1 d . . .
C(M1 C 0.6311(3) 0.5886(2) 0.1495(2) 0.0207(5) Uani 1 1 d . . .
C(M2 C 0.2809(3) 0.8545(2) 0.5876(2) 0.0204(5) Uani 1 1 d . . .
C(A1 C 0.5269(3) 0.6981(2) 0.2478(2) 0.0216(5) Uani 1 1 d . . .
C(A2 C 0.3685(3) 0.8177(2) 0.4459(2) 0.0214(5) Uani 1 1 d . . .
C(A3 C 0.2780(3) 0.7553(2) 0.6961(2) 0.0223(5) Uani 1 1 d . . .
C(A4 C 0.3168(3) 0.5555(2) 0.8143(2) 0.0220(5) Uani 1 1 d . . .
C(B1 C 0.4713(3) 0.8458(2) 0.2116(2) 0.0255(5) Uani 1 1 d . . .
H(BA H 0.4984 0.8845 0.1192 0.031 Uiso 1 1 calc R . .
C(B2 C 0.3731(3) 0.9198(2) 0.3333(2) 0.0239(5) Uani 1 1 d . . .
H(BB H 0.3177 1.0202 0.3428 0.029 Uiso 1 1 calc R . .
C(B3 C 0.1902(3) 0.7928(2) 0.8432(2) 0.0270(6) Uani 1 1 d . . .
H(BC H 0.1281 0.8867 0.8818 0.032 Uiso 1 1 calc R . .
C(B4 C 0.2127(3) 0.6696(2) 0.9164(2) 0.0253(5) Uani 1 1 d . . .
H(BD H 0.1683 0.6600 1.0160 0.030 Uiso 1 1 calc R . .
C10 C 0.6911(3) 0.6278(2) -0.0037(2) 0.0212(5) Uani 1 1 d . . .
C11 C 0.8386(3) 0.6462(3) -0.0685(3) 0.0283(6) Uani 1 1 d . . .
H11A H 0.9013 0.6346 -0.0153 0.034 Uiso 1 1 calc R . .
C12 C 0.8962(3) 0.6813(2) -0.2102(3) 0.0296(6) Uani 1 1 d . . .
H12A H 0.9976 0.6938 -0.2536 0.036 Uiso 1 1 calc R . .
C13 C 0.8053(3) 0.6981(2) -0.2885(2) 0.0273(6) Uani 1 1 d . . .
H13A H 0.8448 0.7207 -0.3858 0.033 Uiso 1 1 calc R . .
C14 C 0.6577(3) 0.6817(3) -0.2243(3) 0.0334(6) Uani 1 1 d . . .
H14A H 0.5945 0.6946 -0.2772 0.040 Uiso 1 1 calc R . .
C15 C 0.6005(3) 0.6464(3) -0.0822(3) 0.0311(6) Uani 1 1 d . . .
H15A H 0.4985 0.6350 -0.0387 0.037 Uiso 1 1 calc R . .
C20 C 0.1829(3) 1.0092(2) 0.6270(2) 0.0205(5) Uani 1 1 d . . .
C21 C 0.0226(3) 1.0579(2) 0.6517(3) 0.0303(6) Uani 1 1 d . . .
H21A H -0.0258 0.9928 0.6447 0.036 Uiso 1 1 calc R . .
C22 C -0.0682(3) 1.2007(3) 0.6866(3) 0.0338(6) Uani 1 1 d . . .
H22A H -0.1777 1.2328 0.7021 0.041 Uiso 1 1 calc R . .
C23 C 0.0000(3) 1.2964(2) 0.6988(2) 0.0283(6) Uani 1 1 d . . .
H23A H -0.0619 1.3943 0.7226 0.034 Uiso 1 1 calc R . .
C24 C 0.1592(3) 1.2479(3) 0.6761(3) 0.0369(7) Uani 1 1 d . . .
H24A H 0.2068 1.3126 0.6853 0.044 Uiso 1 1 calc R . .
C25 C 0.2502(3) 1.1054(3) 0.6397(3) 0.0340(6) Uani 1 1 d . . .
H25A H 0.3600 1.0736 0.6234 0.041 Uiso 1 1 calc R . .
N3 N 0.3085(5) 0.4907(4) 0.4910(4) 0.0198(8) Uani 0.50 1 d P . .
O1 O 0.1798(4) 0.5546(4) 0.5029(4) 0.0336(8) Uani 0.50 1 d P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe .3463 .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 N3 177(2) 2_666 . ?
Fe1 Fe1 N2 88.1(19) 2_666 . ?
N3 Fe1 N2 92.0(3) . . ?
Fe1 Fe1 N1 86.1(18) 2_666 . ?
N3 Fe1 N1 91.2(3) . . ?
N2 Fe1 N1 89.8(3) . . ?
Fe1 Fe1 N1 82.3(18) 2_666 2_666 ?
N3 Fe1 N1 100.5(3) . 2_666 ?
N2 Fe1 N1 89.8(3) . 2_666 ?
N1 Fe1 N1 168.35(16) . 2_666 ?
Fe1 Fe1 N2 80.2(18) 2_666 2_666 ?
N3 Fe1 N2 99.6(3) . 2_666 ?
N2 Fe1 N2 168.33(16) . 2_666 ?
N1 Fe1 N2 89.4(3) . 2_666 ?
N1 Fe1 N2 88.6(3) 2_666 2_666 ?
Fe1 Fe1 N3 2.2(17) 2_666 2_666 ?
N3 Fe1 N3 179.5(4) . 2_666 ?
N2 Fe1 N3 88.0(2) . 2_666 ?
N1 Fe1 N3 88.3(2) . 2_666 ?
N1 Fe1 N3 80.1(2) 2_666 2_666 ?
N2 Fe1 N3 80.3(2) 2_666 2_666 ?
C(A2 N1 C(A1 104.98(17) . . ?
C(A2 N1 Fe1 127.1(2) . . ?
C(A1 N1 Fe1 127.5(2) . . ?
C(A2 N1 Fe1 127.9(2) . 2_666 ?
C(A1 N1 Fe1 126.7(2) . 2_666 ?
C(A4 N2 C(A3 104.82(17) . . ?
C(A4 N2 Fe1 127.5(2) . . ?
C(A3 N2 Fe1 127.3(2) . . ?
C(A4 N2 Fe1 127.1(2) . 2_666 ?
C(A3 N2 Fe1 127.5(2) . 2_666 ?
C(A1 C(M1 C(A4 123.5(2) . 2_666 ?
C(A1 C(M1 C10 118.05(18) . . ?
C(A4 C(M1 C10 118.42(19) 2_666 . ?
C(A2 C(M2 C(A3 123.4(2) . . ?
C(A2 C(M2 C20 118.72(18) . . ?
C(A3 C(M2 C20 117.90(19) . . ?
N1 C(A1 C(M1 125.66(19) . . ?
N1 C(A1 C(B1 110.39(18) . . ?
C(M1 C(A1 C(B1 123.9(2) . . ?
N1 C(A2 C(M2 125.8(2) . . ?
N1 C(A2 C(B2 110.51(19) . . ?
C(M2 C(A2 C(B2 123.7(2) . . ?
N2 C(A3 C(M2 125.7(2) . . ?
N2 C(A3 C(B3 110.57(18) . . ?
C(M2 C(A3 C(B3 123.8(2) . . ?
N2 C(A4 C(M1 125.74(19) . 2_666 ?
N2 C(A4 C(B4 110.72(18) . . ?
C(M1 C(A4 C(B4 123.5(2) 2_666 . ?
C(B2 C(B1 C(A1 107.13(19) . . ?
C(B2 C(B1 H(BA 126.4 . . ?
C(A1 C(B1 H(BA 126.4 . . ?
C(B1 C(B2 C(A2 106.99(19) . . ?
C(B1 C(B2 H(BB 126.5 . . ?
C(A2 C(B2 H(BB 126.5 . . ?
C(B4 C(B3 C(A3 107.1(2) . . ?
C(B4 C(B3 H(BC 126.5 . . ?
C(A3 C(B3 H(BC 126.5 . . ?
C(B3 C(B4 C(A4 106.8(2) . . ?
C(B3 C(B4 H(BD 126.6 . . ?
C(A4 C(B4 H(BD 126.6 . . ?
C11 C10 C15 118.9(2) . . ?
C11 C10 C(M1 120.2(2) . . ?
C15 C10 C(M1 120.9(2) . . ?
C10 C11 C12 120.8(2) . . ?
C10 C11 H11A 119.6 . . ?
C12 C11 H11A 119.6 . . ?
C13 C12 C11 119.9(2) . . ?
C13 C12 H12A 120.1 . . ?
C11 C12 H12A 120.1 . . ?
C14 C13 C12 119.6(2) . . ?
C14 C13 H13A 120.2 . . ?
C12 C13 H13A 120.2 . . ?
C13 C14 C15 120.3(2) . . ?
C13 C14 H14A 119.8 . . ?
C15 C14 H14A 119.8 . . ?
C10 C15 C14 120.5(2) . . ?
C10 C15 H15A 119.8 . . ?
C14 C15 H15A 119.8 . . ?
C25 C20 C21 118.6(2) . . ?
C25 C20 C(M2 120.9(2) . . ?
C21 C20 C(M2 120.4(2) . . ?
C20 C21 C22 120.8(2) . . ?
C20 C21 H21A 119.6 . . ?
C22 C21 H21A 119.6 . . ?
C23 C22 C21 120.3(2) . . ?
C23 C22 H22A 119.8 . . ?
C21 C22 H22A 119.8 . . ?
C24 C23 C22 119.1(2) . . ?
C24 C23 H23A 120.4 . . ?
C22 C23 H23A 120.4 . . ?
C23 C24 C25 120.5(2) . . ?
C23 C24 H24A 119.7 . . ?
C25 C24 H24A 119.7 . . ?
C20 C25 C24 120.7(2) . . ?
C20 C25 H25A 119.7 . . ?
C24 C25 H25A 119.7 . . ?
O1 N3 Fe1 145.6(4) . . ?
O1 N3 Fe1 145.2(4) . 2_666 ?
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 0.406(5) 2_666 ?
Fe1 N3 1.740(5) . ?
Fe1 N2 1.980(7) . ?
Fe1 N1 1.994(7) . ?
Fe1 N1 2.007(7) 2_666 ?
Fe1 N2 2.008(7) 2_666 ?
Fe1 N3 2.146(5) 2_666 ?
N1 C(A2 1.376(3) . ?
N1 C(A1 1.387(3) . ?
N1 Fe1 2.007(7) 2_666 ?
N2 C(A4 1.380(3) . ?
N2 C(A3 1.384(3) . ?
N2 Fe1 2.008(7) 2_666 ?
C(M1 C(A1 1.390(3) . ?
C(M1 C(A4 1.397(3) 2_666 ?
C(M1 C10 1.503(3) . ?
C(M2 C(A2 1.388(3) . ?
C(M2 C(A3 1.393(3) . ?
C(M2 C20 1.504(3) . ?
C(A1 C(B1 1.433(3) . ?
C(A2 C(B2 1.439(3) . ?
C(A3 C(B3 1.437(3) . ?
C(A4 C(M1 1.397(3) 2_666 ?
C(A4 C(B4 1.441(3) . ?
C(B1 C(B2 1.349(3) . ?
C(B1 H(BA 0.9500 . ?
C(B2 H(BB 0.9500 . ?
C(B3 C(B4 1.351(3) . ?
C(B3 H(BC 0.9500 . ?
C(B4 H(BD 0.9500 . ?
C10 C11 1.383(3) . ?
C10 C15 1.385(3) . ?
C11 C12 1.389(3) . ?
C11 H11A 0.9500 . ?
C12 C13 1.388(3) . ?
C12 H12A 0.9500 . ?
C13 C14 1.376(4) . ?
C13 H13A 0.9500 . ?
C14 C15 1.392(3) . ?
C14 H14A 0.9500 . ?
C15 H15A 0.9500 . ?
C20 C25 1.383(3) . ?
C20 C21 1.384(3) . ?
C21 C22 1.386(3) . ?
C21 H21A 0.9500 . ?
C22 C23 1.383(4) . ?
C22 H22A 0.9500 . ?
C23 C24 1.379(4) . ?
C23 H23A 0.9500 . ?
C24 C25 1.387(3) . ?
C24 H24A 0.9500 . ?
C25 H25A 0.9500 . ?
N3 O1 1.153(4) . ?
N3 Fe1 2.146(5) 2_666 ?
