#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:34:58 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179252 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/72/4317224.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_4317224
loop_
_publ_author_name
'Jeremy M. Smith'
'Jeffrey R. Long'
_publ_section_title
;
 First-Row Transition Metal Complexes of the Strongly Donating
 Pentadentate Ligand PY4Im
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11223
_journal_page_last               11230
_journal_paper_doi               10.1021/ic1018407
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C31 H29 F20 Fe N9 P3'
_chemical_formula_weight         1056.39
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2010-08-07 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.868(3)
_cell_length_b                   21.448(4)
_cell_length_c                   14.278(3)
_cell_measurement_temperature    293(2)
_cell_volume                     4553.1(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0327
_diffrn_reflns_av_sigmaI/netI    0.0307
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18420
_diffrn_reflns_theta_full        25.39
_diffrn_reflns_theta_max         25.39
_diffrn_reflns_theta_min         2.74
_exptl_absorpt_coefficient_mu    0.554
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6939
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2116
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.033
_refine_diff_density_min         -0.884
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         4276
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0796
_refine_ls_R_factor_gt           0.0626
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1218P)²+4.4331P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1867
_refine_ls_wR_factor_ref         0.2000
_reflns_number_gt                3241
_reflns_number_total             4276
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1018407_si_002_7.cif
_cod_data_source_block           jms8b
_cod_original_cell_volume        4552.9(16)
_cod_database_code               4317224
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, 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
Fe Fe 0.91569(4) 0.2500 0.99500(4) 0.0246(2) Uani 1 2 d S . .
P1 P 0.51217(11) 0.2500 0.08689(11) 0.0419(4) Uani 1 2 d S . .
P2 P 0.79316(9) 0.05390(5) 0.16995(8) 0.0490(4) Uani 1 1 d . . .
F7 F 0.7257(2) 0.10974(15) 0.1492(2) 0.0790(10) Uani 1 1 d . A .
N12 N 0.83922(19) 0.17997(13) 0.94279(19) 0.0280(6) Uani 1 1 d . . .
F10 F 0.8615(3) -0.00026(18) 0.1937(2) 0.1022(14) Uani 1 1 d . A .
N11 N 1.0009(2) 0.20064(16) 0.8314(2) 0.0381(8) Uani 1 1 d . . .
N14 N 0.8514(3) 0.2500 1.1174(3) 0.0290(9) Uani 1 2 d S . .
N13 N 0.99694(19) 0.32138(14) 1.0322(2) 0.0318(7) Uani 1 1 d . . .
C12 C 0.7515(2) 0.17478(16) 0.9627(3) 0.0311(8) Uani 1 1 d . . .
H12 H 0.7261 0.2023 1.0055 0.037 Uiso 1 1 calc R . .
F1 F 0.4793(5) 0.2500 0.1838(5) 0.263(10) Uani 1 2 d S . .
C24 C 0.7654(5) 0.2500 1.2745(4) 0.0536(17) Uani 1 2 d S . .
H24A H 0.7980 0.2260 1.3200 0.080 Uiso 0.50 1 calc PR . .
H24B H 0.7070 0.2320 1.2653 0.080 Uiso 0.50 1 calc PR . .
H24C H 0.7590 0.2921 1.2966 0.080 Uiso 0.50 1 calc PR . .
C13 C 1.0290(3) 0.32794(19) 1.1192(3) 0.0394(9) Uani 1 1 d . . .
H13 H 1.0119 0.2992 1.1645 0.047 Uiso 1 1 calc R . .
C1 C 0.9773(3) 0.14022(19) 0.8720(3) 0.0400(9) Uani 1 1 d . . .
C23 C 1.0863(3) 0.3756(2) 1.1445(3) 0.0524(11) Uani 1 1 d . . .
H23 H 1.1089 0.3777 1.2052 0.063 Uiso 1 1 calc R . .
C11 C 0.9781(3) 0.2500 0.8798(4) 0.0319(11) Uani 1 2 d S . .
C52 C 0.8760(3) 0.13726(17) 0.8844(3) 0.0348(8) Uani 1 1 d . . .
C14 C 0.8145(3) 0.2500 1.1860(4) 0.0316(11) Uani 1 2 d S . .
C42 C 0.8257(3) 0.09138(19) 0.8426(3) 0.0444(10) Uani 1 1 d . . .
H42 H 0.8530 0.0626 0.8030 0.053 Uiso 1 1 calc R . .
C22 C 0.6977(3) 0.13016(19) 0.9221(3) 0.0405(9) Uani 1 1 d . . .
H22 H 0.6369 0.1283 0.9369 0.049 Uiso 1 1 calc R . .
C21 C 1.0395(3) 0.2190(2) 0.7476(3) 0.0527(11) Uani 1 1 d . . .
H21 H 1.0612 0.1931 0.7005 0.063 Uiso 1 1 calc R . .
C53 C 1.0198(3) 0.36545(18) 0.9680(3) 0.0370(9) Uani 1 1 d . . .
C32 C 0.7340(3) 0.0883(2) 0.8596(3) 0.0456(10) Uani 1 1 d . . .
H32 H 0.6981 0.0589 0.8298 0.055 Uiso 1 1 calc R . .
F4 F 0.6079(5) 0.2500 0.1188(5) 0.238(7) Uani 1 2 d S . .
F3 F 0.5528(8) 0.2500 -0.0145(7) 0.244(9) Uani 1 2 d S . .
F2 F 0.4192(4) 0.2500 0.0522(5) 0.210(6) Uani 1 2 d S . .
C33 C 1.1093(3) 0.4191(2) 1.0807(4) 0.0627(14) Uani 1 1 d . . .
H33 H 1.1479 0.4516 1.0968 0.075 Uiso 1 1 calc R . .
C43 C 1.0747(3) 0.4149(2) 0.9903(4) 0.0561(13) Uani 1 1 d . . .
H43 H 1.0885 0.4450 0.9457 0.067 Uiso 1 1 calc R . .
N1S N 0.0038(3) 0.9336(2) 0.3385(3) 0.0698(12) Uani 1 1 d . . .
C2S C 0.0027(3) 0.9851(3) 0.3590(3) 0.0550(12) Uani 1 1 d . . .
C1S C 0.0000(5) 1.0511(3) 0.3827(5) 0.0843(18) Uani 1 1 d . . .
H1S1 H -0.0059 1.0753 0.3265 0.126 Uiso 1 1 calc R . .
H1S2 H 0.0546 1.0625 0.4143 0.126 Uiso 1 1 calc R . .
H1S3 H -0.0504 1.0590 0.4230 0.126 Uiso 1 1 calc R . .
F5 F 0.5290(11) 0.3074(5) 0.0387(10) 0.320(7) Uani 1 1 d . . .
F6 F 0.5008(17) 0.3019(5) 0.1428(11) 0.478(16) Uani 1 1 d . . .
F8 F 0.8490(8) 0.0670(6) 0.0801(8) 0.089(4) Uani 0.543(19) 1 d P A .
F9 F 0.7398(8) 0.0075(7) 0.1142(18) 0.176(9) Uani 0.543(19) 1 d P A .
F11 F 0.7343(17) 0.0392(7) 0.2551(15) 0.172(11) Uani 0.543(19) 1 d P A .
F12 F 0.8529(12) 0.1027(6) 0.2211(12) 0.133(7) Uani 0.543(19) 1 d P A .
F8A F 0.8699(10) 0.0997(10) 0.162(2) 0.193(13) Uani 0.457(19) 1 d P A 1
F11A F 0.7902(13) 0.0637(9) 0.2773(8) 0.116(8) Uani 0.457(19) 1 d P A 1
F12A F 0.791(2) 0.0372(11) 0.0648(8) 0.172(13) Uani 0.457(19) 1 d P A 1
F9A F 0.7096(11) 0.0105(9) 0.1873(18) 0.139(10) Uani 0.457(19) 1 d P A 1
H3 H 1.001(3) 0.1075(19) 0.831(3) 0.035(10) Uiso 1 1 d . . .
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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
C11 Fe N14 179.3(2) . . ?
C11 Fe N13 86.31(13) . . ?
N14 Fe N13 93.21(12) . . ?
C11 Fe N13 86.31(13) . 8_565 ?
N14 Fe N13 93.21(12) . 8_565 ?
N13 Fe N13 98.47(18) . 8_565 ?
C11 Fe N12 87.42(13) . . ?
N14 Fe N12 93.08(12) . . ?
N13 Fe N12 173.56(12) . . ?
N13 Fe N12 82.57(12) 8_565 . ?
C11 Fe N12 87.42(13) . 8_565 ?
N14 Fe N12 93.08(11) . 8_565 ?
N13 Fe N12 82.57(12) . 8_565 ?
N13 Fe N12 173.56(12) 8_565 8_565 ?
N12 Fe N12 95.70(16) . 8_565 ?
F6 P1 F6 107.5(12) . 8_565 ?
F6 P1 F5 66.8(6) . . ?
F6 P1 F5 172.9(12) 8_565 . ?
F6 P1 F5 172.9(12) . 8_565 ?
F6 P1 F5 66.8(6) 8_565 8_565 ?
F5 P1 F5 118.5(12) . 8_565 ?
F6 P1 F1 54.1(6) . . ?
F6 P1 F1 54.1(6) 8_565 . ?
F5 P1 F1 120.7(6) . . ?
F5 P1 F1 120.7(6) 8_565 . ?
F6 P1 F2 94.6(11) . . ?
F6 P1 F2 94.6(11) 8_565 . ?
F5 P1 F2 90.1(7) . . ?
F5 P1 F2 90.1(7) 8_565 . ?
F1 P1 F2 90.3(4) . . ?
F6 P1 F4 86.6(11) . . ?
F6 P1 F4 86.6(11) 8_565 . ?
F5 P1 F4 88.9(7) . . ?
F5 P1 F4 88.9(7) 8_565 . ?
F1 P1 F4 91.7(4) . . ?
F2 P1 F4 178.0(4) . . ?
F6 P1 F3 125.5(6) . . ?
F6 P1 F3 125.5(6) 8_565 . ?
F5 P1 F3 59.3(6) . . ?
F5 P1 F3 59.3(6) 8_565 . ?
F1 P1 F3 176.8(6) . . ?
F2 P1 F3 92.9(5) . . ?
F4 P1 F3 85.1(5) . . ?
F9 P2 F8A 142.2(13) . . ?
F9 P2 F11 89.0(10) . . ?
F8A P2 F11 128.8(14) . . ?
F9 P2 F12A 47.1(10) . . ?
F8A P2 F12A 95.3(14) . . ?
F11 P2 F12A 135.5(15) . . ?
F9 P2 F11A 126.9(10) . . ?
F8A P2 F11A 90.5(12) . . ?
F11 P2 F11A 39.2(9) . . ?
F12A P2 F11A 173.7(13) . . ?
F9 P2 F8 88.0(8) . . ?
F8A P2 F8 54.2(11) . . ?
F11 P2 F8 176.9(12) . . ?
F12A P2 F8 41.4(11) . . ?
F11A P2 F8 143.9(9) . . ?
F9 P2 F12 175.7(10) . . ?
F8A P2 F12 33.5(10) . . ?
F11 P2 F12 95.3(10) . . ?
F12A P2 F12 128.6(13) . . ?
F11A P2 F12 57.3(7) . . ?
F8 P2 F12 87.7(8) . . ?
F9 P2 F9A 43.4(8) . . ?
F8A P2 F9A 173.9(14) . . ?
F11 P2 F9A 45.6(8) . . ?
F12A P2 F9A 90.0(13) . . ?
F11A P2 F9A 84.4(9) . . ?
F8 P2 F9A 131.3(10) . . ?
F12 P2 F9A 140.9(10) . . ?
F9 P2 F10 88.1(7) . . ?
F8A P2 F10 90.5(8) . . ?
F11 P2 F10 92.6(5) . . ?
F12A P2 F10 92.9(5) . . ?
F11A P2 F10 84.6(6) . . ?
F8 P2 F10 88.1(4) . . ?
F12 P2 F10 91.5(5) . . ?
F9A P2 F10 92.3(7) . . ?
F9 P2 F7 93.9(7) . . ?
F8A P2 F7 88.4(8) . . ?
F11 P2 F7 86.7(5) . . ?
F12A P2 F7 88.9(5) . . ?
F11A P2 F7 93.7(6) . . ?
F8 P2 F7 92.7(4) . . ?
F12 P2 F7 86.6(5) . . ?
F9A P2 F7 88.6(7) . . ?
F10 P2 F7 177.9(2) . . ?
C12 N12 C52 117.9(3) . . ?
C12 N12 Fe 122.0(2) . . ?
C52 N12 Fe 120.1(2) . . ?
C11 N11 C21 109.5(4) . . ?
C11 N11 C1 116.4(3) . . ?
C21 N11 C1 134.0(3) . . ?
C14 N14 Fe 179.4(4) . . ?
C13 N13 C53 117.6(3) . . ?
C13 N13 Fe 122.5(3) . . ?
C53 N13 Fe 119.9(3) . . ?
N12 C12 C22 122.3(3) . . ?
F6 F1 F6 118.2(13) . 8_565 ?
F6 F1 P1 59.5(6) . . ?
F6 F1 P1 59.5(6) 8_565 . ?
N13 C13 C23 122.8(4) . . ?
N11 C1 C53 109.3(3) . 8_565 ?
N11 C1 C52 108.8(3) . . ?
C53 C1 C52 107.8(3) 8_565 . ?
C33 C23 C13 119.5(4) . . ?
N11 C11 N11 107.9(5) . 8_565 ?
N11 C11 Fe 126.0(2) . . ?
N11 C11 Fe 126.0(2) 8_565 . ?
N12 C52 C42 122.3(4) . . ?
N12 C52 C1 116.4(3) . . ?
C42 C52 C1 121.3(3) . . ?
N14 C14 C24 179.3(6) . . ?
C52 C42 C32 119.5(4) . . ?
C32 C22 C12 120.0(4) . . ?
C21 C21 N11 106.5(2) 8_565 . ?
N13 C53 C43 121.9(4) . . ?
N13 C53 C1 116.7(3) . 8_565 ?
C43 C53 C1 121.3(4) . 8_565 ?
C22 C32 C42 117.9(4) . . ?
F5 F3 F5 111.6(10) . 8_565 ?
F5 F3 P1 55.8(5) . . ?
F5 F3 P1 55.8(5) 8_565 . ?
C23 C33 C43 119.1(4) . . ?
C53 C43 C33 119.0(4) . . ?
N1S C2S C1S 178.5(6) . . ?
P1 F5 F3 64.9(7) . . ?
P1 F5 F6 55.0(5) . . ?
F3 F5 F6 119.4(9) . . ?
F1 F6 P1 66.4(6) . . ?
F1 F6 F5 124.4(9) . . ?
P1 F6 F5 58.2(6) . . ?
F12A F8 F8A 129.4(13) . . ?
F12A F8 P2 68.8(9) . . ?
F8A F8 P2 61.3(6) . . ?
F9A F9 F12A 138.4(15) . . ?
F9A F9 P2 71.6(10) . . ?
F12A F9 P2 68.2(9) . . ?
F11A F11 F9A 138.8(15) . . ?
F11A F11 P2 71.3(9) . . ?
F9A F11 P2 69.0(7) . . ?
F8A F12 F11A 131(2) . . ?
F8A F12 P2 70.4(15) . . ?
F11A F12 P2 61.1(7) . . ?
F12 F8A F8 140.6(19) . . ?
F12 F8A P2 76.1(12) . . ?
F8 F8A P2 64.5(9) . . ?
F11 F11A F12 128.6(15) . . ?
F11 F11A P2 69.4(9) . . ?
F12 F11A P2 61.6(7) . . ?
F8 F12A F9 133.0(15) . . ?
F8 F12A P2 69.8(9) . . ?
F9 F12A P2 64.6(8) . . ?
F9 F9A F11 130.2(15) . . ?
F9 F9A P2 65.0(8) . . ?
F11 F9A P2 65.4(7) . . ?
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
Fe C11 1.889(5) . ?
Fe N14 1.991(4) . ?
Fe N13 2.021(3) . ?
Fe N13 2.021(3) 8_565 ?
Fe N12 2.026(3) . ?
Fe N12 2.026(3) 8_565 ?
P1 F6 1.381(9) . ?
P1 F6 1.381(9) 8_565 ?
P1 F5 1.433(9) . ?
P1 F5 1.433(9) 8_565 ?
P1 F1 1.468(8) . ?
P1 F2 1.469(6) . ?
P1 F4 1.494(7) . ?
P1 F3 1.569(10) . ?
P2 F9 1.501(11) . ?
P2 F8A 1.509(12) . ?
P2 F11 1.530(8) . ?
P2 F12A 1.543(10) . ?
P2 F11A 1.548(11) . ?
P2 F8 1.553(7) . ?
P2 F12 1.555(11) . ?
P2 F9A 1.572(11) . ?
P2 F10 1.580(3) . ?
P2 F7 1.590(3) . ?
N12 C12 1.339(5) . ?
N12 C52 1.353(5) . ?
N11 C11 1.309(4) . ?
N11 C21 1.384(5) . ?
N11 C1 1.463(5) . ?
N14 C14 1.123(7) . ?
N13 C13 1.338(5) . ?
N13 C53 1.360(5) . ?
C12 C22 1.375(5) . ?
F1 F6 1.298(13) . ?
F1 F6 1.298(13) 8_565 ?
C24 C14 1.460(8) . ?
C13 C23 1.379(6) . ?
C1 C53 1.515(6) 8_565 ?
C1 C52 1.518(6) . ?
C23 C33 1.350(7) . ?
C11 N11 1.309(4) 8_565 ?
C52 C42 1.372(5) . ?
C42 C32 1.387(6) . ?
C22 C32 1.375(6) . ?
C21 C21 1.330(9) 8_565 ?
C53 C43 1.375(6) . ?
C53 C1 1.515(6) 8_565 ?
F3 F5 1.490(13) . ?
F3 F5 1.490(13) 8_565 ?
C33 C43 1.392(7) . ?
N1S C2S 1.144(6) . ?
C2S C1S 1.455(8) . ?
F5 F6 1.549(15) . ?
F8 F12A 1.09(3) . ?
F8 F8A 1.40(3) . ?
F9 F9A 1.14(2) . ?
F9 F12A 1.22(2) . ?
F11 F11A 1.03(2) . ?
F11 F9A 1.20(2) . ?
F12 F8A 0.88(3) . ?
F12 F11A 1.49(2) . ?
