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#$Date: 2016-03-21 17:29:04 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178784 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/38/4103891.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_4103891
loop_
_publ_author_name
'Masaaki Okazaki'
'Masato Takano'
'Fumiyuki Ozawa'
_publ_contact_author_address
'Institute for Chemical Research, Kyoto University'
_publ_contact_author_email       mokazaki@scl.kyoto-u.ac.jp
_publ_contact_author_fax         81-774-38-3039
_publ_contact_author_name        'Masaaki Okazaki'
_publ_contact_author_phone       81-774-38-3029
_publ_section_title
;
 Redox-Responsive Recombination of Carbon-Carbon Bonds on Flexible
 Tetrairon Cores
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1684
_journal_page_last               1685
_journal_paper_doi               10.1021/ja809540w
_journal_volume                  131
_journal_year                    2009
_chemical_absolute_configuration unk
_chemical_formula_sum            'C38 H48 F12 Fe4 P2 Si2'
_chemical_formula_weight         1074.28
_chemical_properties_physical    air-sensitive
_space_group_IT_number           152
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      152
_symmetry_space_group_name_Hall  'P 31 2"'
_symmetry_space_group_name_H-M   'P 31 2 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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   11.366(10)
_cell_length_b                   11.366(10)
_cell_length_c                   29.309(27)
_cell_measurement_reflns_used    9067
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      3.4647
_cell_volume                     3279(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0679
_diffrn_reflns_av_sigmaI/netI    0.0525
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            26788
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.47
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.508
_exptl_absorpt_correction_T_max  0.9284
_exptl_absorpt_correction_T_min  0.8166
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   Higashi
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1638
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.148
_refine_diff_density_min         -0.522
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.26(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         5006
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_gt           0.0608
_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)+(0.0955P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1589
_refine_ls_wR_factor_ref         0.1663
_reflns_number_gt                4443
_reflns_number_total             5006
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja809540w_si_002.cif
_cod_data_source_block           okazaki
_cod_database_code               4103891
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
'x-y, -y, -z+2/3'
'-x, -x+y, -z+1/3'
'y, x, -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
Fe1 Fe 0.10416(7) 0.32218(7) 0.14252(2) 0.03222(19) Uani 1 1 d .
Fe2 Fe -0.09640(7) 0.10389(7) 0.11874(2) 0.0342(2) Uani 1 1 d .
C1 C 0.0633(5) 0.1312(5) 0.15197(15) 0.0351(10) Uani 1 1 d .
C2 C -0.0829(5) 0.2714(5) 0.12676(16) 0.0351(10) Uani 1 1 d .
C3 C -0.1326(5) 0.3420(6) 0.10300(19) 0.0387(12) Uani 1 1 d .
C4 C -0.1753(6) 0.4015(6) 0.08044(19) 0.0429(12) Uani 1 1 d .
Si1 Si -0.23168(17) 0.50536(17) 0.04833(6) 0.0463(4) Uani 1 1 d .
C5 C -0.0768(7) 0.6731(7) 0.0403(3) 0.0638(19) Uani 1 1 d .
H1 H -0.0214 0.6979 0.0680 0.096 Uiso 1 1 calc R
H2 H -0.1028 0.7417 0.0340 0.096 Uiso 1 1 calc R
H3 H -0.0242 0.6683 0.0145 0.096 Uiso 1 1 calc R
C6 C -0.3605(7) 0.5184(8) 0.0840(3) 0.074(2) Uani 1 1 d .
H4 H -0.4435 0.4294 0.0856 0.111 Uiso 1 1 calc R
H5 H -0.3815 0.5845 0.0703 0.111 Uiso 1 1 calc R
H6 H -0.3244 0.5482 0.1148 0.111 Uiso 1 1 calc R
C7 C -0.3032(10) 0.4201(9) -0.0077(3) 0.080(2) Uani 1 1 d .
H7 H -0.2413 0.3942 -0.0218 0.120 Uiso 1 1 calc R
H8 H -0.3139 0.4829 -0.0279 0.120 Uiso 1 1 calc R
H9 H -0.3919 0.3388 -0.0027 0.120 Uiso 1 1 calc R
C8 C 0.2111(6) 0.5305(6) 0.1197(2) 0.0456(13) Uani 1 1 d .
C9 C 0.2984(5) 0.5007(6) 0.1455(2) 0.0460(14) Uani 1 1 d .
H10 H 0.3477 0.5484 0.1739 0.055 Uiso 1 1 calc R
C10 C 0.3081(6) 0.3950(7) 0.1231(2) 0.0522(15) Uani 1 1 d .
H11 H 0.3661 0.3564 0.1329 0.063 Uiso 1 1 calc R
C11 C 0.2265(6) 0.3582(7) 0.0833(2) 0.0514(15) Uani 1 1 d .
H12 H 0.2162 0.2890 0.0601 0.062 Uiso 1 1 calc R
C12 C 0.1655(6) 0.4406(6) 0.08159(19) 0.0441(12) Uani 1 1 d .
H13 H 0.1031 0.4383 0.0571 0.053 Uiso 1 1 calc R
C13 C 0.1772(8) 0.6405(6) 0.1290(2) 0.0623(18) Uani 1 1 d .
H14 H 0.2494 0.7270 0.1169 0.093 Uiso 1 1 calc R
H15 H 0.1693 0.6488 0.1620 0.093 Uiso 1 1 calc R
H16 H 0.0909 0.6173 0.1143 0.093 Uiso 1 1 calc R
C14 C -0.2789(6) -0.0763(6) 0.0977(2) 0.0492(14) Uani 1 1 d .
C15 C -0.1633(7) -0.0885(7) 0.0903(2) 0.0574(16) Uani 1 1 d .
H17 H -0.1481 -0.1603 0.1041 0.069 Uiso 1 1 calc R
C16 C -0.0724(7) 0.0137(8) 0.0599(2) 0.0577(17) Uani 1 1 d .
H18 H 0.0148 0.0246 0.0478 0.069 Uiso 1 1 calc R
C17 C -0.1316(7) 0.0944(7) 0.0485(2) 0.0576(17) Uani 1 1 d .
H19 H -0.0935 0.1730 0.0269 0.069 Uiso 1 1 calc R
C18 C -0.2573(6) 0.0397(6) 0.07241(19) 0.0462(13) Uani 1 1 d .
H20 H -0.3218 0.0753 0.0708 0.055 Uiso 1 1 calc R
C19 C -0.4011(7) -0.1685(7) 0.1247(2) 0.0632(18) Uani 1 1 d .
H21 H -0.4714 -0.2348 0.1043 0.095 Uiso 1 1 calc R
H22 H -0.4355 -0.1154 0.1402 0.095 Uiso 1 1 calc R
H23 H -0.3772 -0.2163 0.1474 0.095 Uiso 1 1 calc R
P1 P 0.35181(17) 0.04665(17) 0.06919(6) 0.0506(4) Uani 1 1 d .
F1 F 0.2785(8) 0.0922(7) 0.0315(2) 0.124(2) Uani 1 1 d .
F2 F 0.4232(6) -0.0011(6) 0.10398(19) 0.1102(19) Uani 1 1 d .
F3 F 0.2873(8) -0.0954(6) 0.0460(2) 0.127(2) Uani 1 1 d .
F4 F 0.4071(11) 0.1828(6) 0.0930(2) 0.182(4) Uani 1 1 d .
F5 F 0.4734(7) 0.0997(9) 0.0355(3) 0.156(3) Uani 1 1 d .
F6 F 0.2255(8) -0.0142(8) 0.1015(3) 0.160(3) Uani 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'
F F 0.0171 0.0103 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 '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
C2 Fe1 C2 93.7(2) 5 .
C2 Fe1 C1 95.0(2) 5 .
C2 Fe1 C1 94.8(2) . .
C2 Fe1 C10 113.6(2) 5 .
C2 Fe1 C10 150.2(2) . .
C1 Fe1 C10 94.4(2) . .
C2 Fe1 C9 87.1(2) 5 .
C2 Fe1 C9 138.3(2) . .
C1 Fe1 C9 126.7(2) . .
C10 Fe1 C9 39.2(2) . .
C2 Fe1 C12 136.1(2) 5 .
C2 Fe1 C12 87.3(2) . .
C1 Fe1 C12 128.8(2) . .
C10 Fe1 C12 65.1(2) . .
C9 Fe1 C12 64.9(2) . .
C2 Fe1 C11 151.4(2) 5 .
C2 Fe1 C11 111.8(2) . .
C1 Fe1 C11 95.5(2) . .
C10 Fe1 C11 39.0(2) . .
C9 Fe1 C11 65.4(3) . .
C12 Fe1 C11 38.8(2) . .
C2 Fe1 C8 98.5(2) 5 .
C2 Fe1 C8 100.6(2) . .
C1 Fe1 C8 158.8(2) . .
C10 Fe1 C8 65.2(3) . .
C9 Fe1 C8 38.6(2) . .
C12 Fe1 C8 38.8(2) . .
C11 Fe1 C8 65.3(2) . .
C2 Fe1 Fe2 108.59(16) 5 .
C2 Fe1 Fe2 47.27(15) . .
C1 Fe1 Fe2 49.91(15) . .
C10 Fe1 Fe2 126.5(2) . .
C9 Fe1 Fe2 163.80(17) . .
C12 Fe1 Fe2 104.02(17) . .
C11 Fe1 Fe2 98.49(19) . .
C8 Fe1 Fe2 137.80(17) . .
C2 Fe1 Fe1 50.57(16) 5 5
C2 Fe1 Fe1 50.25(14) . 5
C1 Fe1 Fe1 75.86(15) . 5
C10 Fe1 Fe1 159.25(18) . 5
C9 Fe1 Fe1 135.81(17) . 5
C12 Fe1 Fe1 135.11(16) . 5
C11 Fe1 Fe1 158.01(19) . 5
C8 Fe1 Fe1 125.28(16) . 5
Fe2 Fe1 Fe1 60.38(5) . 5
C2 Fe1 Fe2 46.99(16) 5 5
C2 Fe1 Fe2 107.64(14) . 5
C1 Fe1 Fe2 50.01(13) . 5
C10 Fe1 Fe2 99.94(18) . 5
C9 Fe1 Fe2 103.07(16) . 5
C12 Fe1 Fe2 164.98(16) . 5
C11 Fe1 Fe2 129.25(19) . 5
C8 Fe1 Fe2 135.52(17) . 5
Fe2 Fe1 Fe2 85.60(5) . 5
Fe1 Fe1 Fe2 59.71(5) 5 5
C2 Fe2 C1 100.5(2) . .
C2 Fe2 C1 99.8(2) . 5
C1 Fe2 C1 45.7(3) . 5
C2 Fe2 C17 95.4(3) . .
C1 Fe2 C17 129.9(2) . .
C1 Fe2 C17 164.7(3) 5 .
C2 Fe2 C16 130.2(3) . .
C1 Fe2 C16 98.7(2) . .
C1 Fe2 C16 125.8(3) 5 .
C17 Fe2 C16 39.8(3) . .
C2 Fe2 C18 92.9(2) . .
C1 Fe2 C18 164.5(2) . .
C1 Fe2 C18 139.5(2) 5 .
C17 Fe2 C18 39.8(2) . .
C16 Fe2 C18 66.4(2) . .
C2 Fe2 C15 157.8(2) . .
C1 Fe2 C15 100.9(2) . .
C1 Fe2 C15 99.3(3) 5 .
C17 Fe2 C15 66.1(3) . .
C16 Fe2 C15 39.6(3) . .
C18 Fe2 C15 65.2(2) . .
C2 Fe2 C14 124.2(2) . .
C1 Fe2 C14 132.4(2) . .
C1 Fe2 C14 105.4(2) 5 .
C17 Fe2 C14 66.4(2) . .
C16 Fe2 C14 66.2(3) . .
C18 Fe2 C14 39.1(2) . .
C15 Fe2 C14 38.6(3) . .
C2 Fe2 Fe1 51.20(16) . .
C1 Fe2 Fe1 51.91(16) . .
C1 Fe2 Fe1 76.68(16) 5 .
C17 Fe2 Fe1 112.58(19) . .
C16 Fe2 Fe1 116.2(2) . .
C18 Fe2 Fe1 137.27(18) . .
C15 Fe2 Fe1 145.69(19) . .
C14 Fe2 Fe1 175.37(18) . .
C2 Fe2 Fe1 50.56(15) . 5
C1 Fe2 Fe1 76.49(15) . 5
C1 Fe2 Fe1 51.49(16) 5 5
C17 Fe2 Fe1 143.4(2) . 5
C16 Fe2 Fe1 175.03(19) . 5
C18 Fe2 Fe1 118.47(18) . 5
C15 Fe2 Fe1 142.0(2) . 5
C14 Fe2 Fe1 117.94(17) . 5
Fe1 Fe2 Fe1 59.91(3) . 5
C1 C1 Fe2 67.6(4) 5 .
C1 C1 Fe2 66.7(3) 5 5
Fe2 C1 Fe2 120.7(3) . 5
C1 C1 Fe1 104.14(15) 5 .
Fe2 C1 Fe1 78.19(19) . .
Fe2 C1 Fe1 78.49(19) 5 .
C3 C2 Fe2 133.5(4) . .
C3 C2 Fe1 130.1(4) . 5
Fe2 C2 Fe1 82.4(2) . 5
C3 C2 Fe1 130.4(4) . .
Fe2 C2 Fe1 81.5(2) . .
Fe1 C2 Fe1 79.18(19) 5 .
C4 C3 C2 177.1(6) . .
C3 C4 Si1 175.5(5) . .
C5 Si1 C4 105.4(3) . .
C5 Si1 C6 111.7(3) . .
C4 Si1 C6 107.6(3) . .
C5 Si1 C7 111.3(4) . .
C4 Si1 C7 108.3(3) . .
C6 Si1 C7 112.2(4) . .
C9 C8 C12 107.1(5) . .
C9 C8 C13 127.1(6) . .
C12 C8 C13 125.8(6) . .
C9 C8 Fe1 69.5(3) . .
C12 C8 Fe1 69.7(3) . .
C13 C8 Fe1 128.1(4) . .
C8 C9 C10 108.4(5) . .
C8 C9 Fe1 71.9(3) . .
C10 C9 Fe1 69.9(3) . .
C11 C10 C9 108.3(6) . .
C11 C10 Fe1 71.3(3) . .
C9 C10 Fe1 70.9(3) . .
C12 C11 C10 107.3(6) . .
C12 C11 Fe1 70.6(3) . .
C10 C11 Fe1 69.7(3) . .
C11 C12 C8 108.9(5) . .
C11 C12 Fe1 70.6(3) . .
C8 C12 Fe1 71.5(3) . .
C15 C14 C18 106.0(6) . .
C15 C14 C19 127.1(7) . .
C18 C14 C19 126.8(6) . .
C15 C14 Fe2 68.5(4) . .
C18 C14 Fe2 68.3(3) . .
C19 C14 Fe2 129.5(4) . .
C14 C15 C16 110.4(6) . .
C14 C15 Fe2 72.9(3) . .
C16 C15 Fe2 70.1(4) . .
C15 C16 C17 106.9(6) . .
C15 C16 Fe2 70.3(3) . .
C17 C16 Fe2 70.0(3) . .
C16 C17 C18 107.3(6) . .
C16 C17 Fe2 70.3(4) . .
C18 C17 Fe2 70.3(3) . .
C14 C18 C17 109.3(6) . .
C14 C18 Fe2 72.6(3) . .
C17 C18 Fe2 69.9(3) . .
F4 P1 F5 93.5(5) . .
F4 P1 F3 176.8(6) . .
F5 P1 F3 89.5(4) . .
F4 P1 F2 91.9(4) . .
F5 P1 F2 91.9(4) . .
F3 P1 F2 89.0(3) . .
F4 P1 F6 89.6(5) . .
F5 P1 F6 176.8(5) . .
F3 P1 F6 87.3(4) . .
F2 P1 F6 88.4(4) . .
F4 P1 F1 90.2(4) . .
F5 P1 F1 86.7(4) . .
F3 P1 F1 89.0(3) . .
F2 P1 F1 177.6(4) . .
F6 P1 F1 92.8(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 C2 1.950(5) 5
Fe1 C2 1.959(5) .
Fe1 C1 1.999(5) .
Fe1 C10 2.113(6) .
Fe1 C9 2.126(6) .
Fe1 C12 2.133(5) .
Fe1 C11 2.133(5) .
Fe1 C8 2.157(6) .
Fe1 Fe2 2.486(2) .
Fe1 Fe1 2.492(2) 5
Fe1 Fe2 2.503(2) 5
Fe2 C2 1.847(5) .
Fe2 C1 1.943(5) .
Fe2 C1 1.957(5) 5
Fe2 C17 2.089(6) .
Fe2 C16 2.093(6) .
Fe2 C18 2.094(6) .
Fe2 C15 2.096(6) .
Fe2 C14 2.152(6) .
Fe2 Fe1 2.503(2) 5
C1 C1 1.515(10) 5
C1 Fe2 1.957(5) 5
C2 C3 1.379(7) .
C2 Fe1 1.950(5) 5
C3 C4 1.207(8) .
C4 Si1 1.857(6) .
Si1 C5 1.853(7) .
Si1 C6 1.864(7) .
Si1 C7 1.874(8) .
C8 C9 1.416(8) .
C8 C12 1.426(8) .
C8 C13 1.506(9) .
C9 C10 1.420(9) .
C10 C11 1.418(9) .
C11 C12 1.418(9) .
C14 C15 1.405(9) .
C14 C18 1.422(9) .
C14 C19 1.483(9) .
C15 C16 1.419(10) .
C16 C17 1.422(10) .
C17 C18 1.425(9) .
P1 F4 1.517(6) .
P1 F5 1.553(6) .
P1 F3 1.557(6) .
P1 F2 1.560(5) .
P1 F6 1.562(6) .
P1 F1 1.615(5) .
