#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/24/7012425.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_7012425
loop_
_publ_author_name
'Konchenko, Sergei N.'
'Pushkarevsky, Nikolai A.'
'Virovets, Alexander V.'
'Scheer, Manfred'
_publ_section_title
;
 Reactions of [Fe3(µ3-Q)(CO)9]2-- (Q = Se, Te) with organic and
 organometallic dihalides of group 15 elements -- an approach to
 functionalised clusters
;
_journal_issue                   4
_journal_name_full               'Dalton Transactions'
_journal_page_first              581
_journal_paper_doi               10.1039/b210839a
_journal_year                    2003
_chemical_formula_sum            'C20 H13 Fe4 O11 Sb Te'
_chemical_formula_weight         902.05
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 103.56(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.0904(18)
_cell_length_b                   16.776(3)
_cell_length_c                   17.831(4)
_cell_measurement_reflns_used    1278
_cell_measurement_temperature    200(1)
_cell_measurement_theta_max      24.04
_cell_measurement_theta_min      1.69
_cell_volume                     2643.4(10)
_computing_cell_refinement       'STOE IPDS software'
_computing_data_collection       'STOE IPDS software'
_computing_data_reduction        'STOE IPDS software'
_computing_molecular_graphics    SIEMENS-XP
_computing_publication_material  SHEXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(1)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'STOE IPDS'
_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  0.0387
_diffrn_reflns_av_sigmaI/netI    0.0292
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10723
_diffrn_reflns_theta_full        24.04
_diffrn_reflns_theta_max         24.04
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    4.288
_exptl_absorpt_correction_T_max  0.8978
_exptl_absorpt_correction_T_min  0.6458
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'program faceit'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.267
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.741
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         4030
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.966
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0249
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0437P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0623
_refine_ls_wR_factor_ref         0.0632
_reflns_number_gt                3422
_reflns_number_total             4030
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b210839a.txt
_cod_data_source_block           new2
_cod_original_cell_volume        2643.3(9)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7012425
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-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
Sb Sb 0.92088(3) 0.753167(11) 0.103482(14) 0.02454(9) Uani 1 1 d . . .
Te Te 0.71386(3) 0.747796(11) -0.073624(14) 0.03015(9) Uani 1 1 d . . .
Fe1 Fe 0.63785(5) 0.72766(3) 0.05264(3) 0.02634(13) Uani 1 1 d . . .
Fe2 Fe 0.78488(6) 0.86392(3) 0.02122(3) 0.02844(13) Uani 1 1 d . . .
Fe3 Fe 0.86641(6) 0.63958(3) 0.01021(3) 0.02881(13) Uani 1 1 d . . .
Fe4 Fe 1.09357(6) 0.74242(2) 0.23631(3) 0.02869(13) Uani 1 1 d . . .
C1 C 0.9899(4) 0.8186(2) 0.2708(2) 0.0328(8) Uani 1 1 d . . .
O1 O 0.9204(3) 0.86539(16) 0.29402(17) 0.0468(7) Uani 1 1 d . . .
C2 C 0.9814(4) 0.6659(2) 0.2628(2) 0.0371(9) Uani 1 1 d . . .
O2 O 0.9142(4) 0.61570(17) 0.28329(19) 0.0573(8) Uani 1 1 d . . .
C3 C 0.9441(5) 0.8971(2) -0.0128(2) 0.0374(9) Uani 1 1 d . . .
O3 O 1.0464(3) 0.91777(16) -0.03512(18) 0.0508(7) Uani 1 1 d . . .
C4 C 0.7961(4) 0.9301(2) 0.1022(2) 0.0350(8) Uani 1 1 d . . .
O4 O 0.8020(3) 0.97389(15) 0.15164(17) 0.0486(7) Uani 1 1 d . . .
C5 C 0.6359(5) 0.9230(2) -0.0385(2) 0.0389(9) Uani 1 1 d . . .
O5 O 0.5427(4) 0.96030(17) -0.07620(19) 0.0591(8) Uani 1 1 d . . .
C6 C 0.9261(4) 0.5700(2) 0.0875(2) 0.0383(9) Uani 1 1 d . . .
O6 O 0.9680(4) 0.52594(16) 0.13681(19) 0.0559(8) Uani 1 1 d . . .
C7 C 1.0398(5) 0.6519(2) -0.0169(2) 0.0383(9) Uani 1 1 d . . .
O7 O 1.1532(3) 0.65990(18) -0.03383(19) 0.0580(8) Uani 1 1 d . . .
C8 C 0.7777(4) 0.5636(2) -0.0582(2) 0.0373(9) Uani 1 1 d . . .
O8 O 0.7272(3) 0.51497(15) -0.10134(18) 0.0515(7) Uani 1 1 d . . .
C9 C 0.4775(4) 0.7925(2) 0.0261(2) 0.0343(8) Uani 1 1 d . . .
O9 O 0.3696(3) 0.82955(16) 0.00957(17) 0.0496(7) Uani 1 1 d . . .
C10 C 0.6448(4) 0.7219(2) 0.1527(2) 0.0382(9) Uani 1 1 d . . .
O10 O 0.6393(3) 0.7162(2) 0.21616(19) 0.0588(8) Uani 1 1 d . . .
C11 C 0.5413(5) 0.6346(2) 0.0304(2) 0.0396(9) Uani 1 1 d . . .
O11 O 0.4723(4) 0.57762(16) 0.0189(2) 0.0659(10) Uani 1 1 d . . .
C12 C 1.3005(4) 0.8073(2) 0.2448(2) 0.0326(8) Uani 1 1 d . . .
C13 C 1.2775(4) 0.75219(19) 0.1826(3) 0.0380(9) Uani 1 1 d . . .
H13 H 1.2692 0.7654 0.1299 0.046 Uiso 1 1 calc R . .
C14 C 1.2689(4) 0.6740(2) 0.2121(3) 0.0496(11) Uani 1 1 d . . .
H14 H 1.2536 0.6261 0.1828 0.059 Uiso 1 1 calc R . .
C15 C 1.2873(5) 0.6804(2) 0.2930(3) 0.0511(11) Uani 1 1 d . . .
H15 H 1.2882 0.6375 0.3279 0.061 Uiso 1 1 calc R . .
C16 C 1.3039(4) 0.7617(2) 0.3127(3) 0.0422(10) Uani 1 1 d . . .
H16 H 1.3156 0.7829 0.3631 0.051 Uiso 1 1 calc R . .
C17 C 1.3337(4) 0.8959(2) 0.2406(2) 0.0357(8) Uani 1 1 d . . .
C18 C 1.2225(5) 0.9348(2) 0.1726(3) 0.0506(11) Uani 1 1 d . . .
H18A H 1.2484 0.9912 0.1695 0.076 Uiso 1 1 calc R . .
H18B H 1.1194 0.9303 0.1802 0.076 Uiso 1 1 calc R . .
H18C H 1.2283 0.9079 0.1246 0.076 Uiso 1 1 calc R . .
C19 C 1.4943(4) 0.9030(2) 0.2275(3) 0.0436(9) Uani 1 1 d . . .
H19A H 1.5237 0.9593 0.2290 0.065 Uiso 1 1 calc R . .
H19B H 1.4965 0.8804 0.1771 0.065 Uiso 1 1 calc R . .
H19C H 1.5652 0.8739 0.2681 0.065 Uiso 1 1 calc R . .
C20 C 1.3287(5) 0.9377(2) 0.3155(3) 0.0574(12) Uani 1 1 d . . .
H20A H 1.3465 0.9949 0.3106 0.086 Uiso 1 1 calc R . .
H20B H 1.4073 0.9156 0.3576 0.086 Uiso 1 1 calc R . .
H20C H 1.2292 0.9295 0.3266 0.086 Uiso 1 1 calc 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'
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'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Te Te -0.5308 1.6751 '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 Sb Te 49.50(3) . . ?
Fe2 Sb Te 50.455(18) . . ?
Fe2 Sb Fe1 66.36(2) . . ?
Fe2 Sb Fe4 135.68(2) . . ?
Fe3 Sb Te 50.116(15) . . ?
Fe3 Sb Fe1 67.09(2) . . ?
Fe3 Sb Fe2 100.49(3) . . ?
Fe3 Sb Fe4 123.54(2) . . ?
Fe4 Sb Te 173.396(14) . . ?
Fe4 Sb Fe1 132.39(3) . . ?
Fe1 Te Sb 50.240(18) . . ?
Fe1 Te Fe2 65.969(19) . . ?
Fe1 Te Fe3 66.85(2) . . ?
Fe2 Te Sb 48.989(15) . . ?
Fe3 Te Sb 48.930(18) . . ?
Fe3 Te Fe2 97.84(3) . . ?
Sb Fe1 Fe2 55.965(16) . . ?
Sb Fe1 Fe3 55.527(18) . . ?
Te Fe1 Sb 80.26(3) . . ?
Te Fe1 Fe2 57.596(18) . . ?
Te Fe1 Fe3 56.88(2) . . ?
Fe2 Fe1 Fe3 87.53(2) . . ?
C9 Fe1 Sb 132.95(11) . . ?
C9 Fe1 Te 93.39(12) . . ?
C9 Fe1 Fe2 81.20(11) . . ?
C9 Fe1 Fe3 149.35(12) . . ?
C10 Fe1 Sb 81.78(12) . . ?
C10 Fe1 Te 161.97(12) . . ?
C10 Fe1 Fe2 110.08(13) . . ?
C10 Fe1 Fe3 112.99(12) . . ?
C10 Fe1 C9 97.66(17) . . ?
C10 Fe1 C11 94.30(18) . . ?
C11 Fe1 Sb 128.71(13) . . ?
C11 Fe1 Te 98.16(13) . . ?
C11 Fe1 Fe2 155.51(13) . . ?
C11 Fe1 Fe3 80.56(12) . . ?
C11 Fe1 C9 98.32(17) . . ?
Sb Fe2 Te 80.56(3) . . ?
Sb Fe2 Fe1 57.67(2) . . ?
Te Fe2 Fe1 56.44(2) . . ?
C3 Fe2 Sb 95.85(11) . . ?
C3 Fe2 Te 96.40(12) . . ?
C3 Fe2 Fe1 142.57(11) . . ?
C3 Fe2 C4 100.50(17) . . ?
C3 Fe2 C5 100.59(16) . . ?
C4 Fe2 Sb 93.47(11) . . ?
C4 Fe2 Te 162.58(11) . . ?
C4 Fe2 Fe1 106.57(11) . . ?
C4 Fe2 C5 91.57(17) . . ?
C5 Fe2 Sb 161.62(12) . . ?
C5 Fe2 Te 89.45(13) . . ?
C5 Fe2 Fe1 103.96(12) . . ?
Sb Fe3 Te 80.95(3) . . ?
Sb Fe3 Fe1 57.38(2) . . ?
Te Fe3 Fe1 56.27(2) . . ?
C6 Fe3 Sb 90.45(12) . . ?
C6 Fe3 Te 160.39(12) . . ?
C6 Fe3 Fe1 104.29(12) . . ?
C6 Fe3 C8 93.78(17) . . ?
C7 Fe3 Sb 92.41(12) . . ?
C7 Fe3 Te 98.86(12) . . ?
C7 Fe3 Fe1 141.26(11) . . ?
C7 Fe3 C6 99.08(17) . . ?
C7 Fe3 C8 100.54(17) . . ?
C8 Fe3 Sb 165.54(11) . . ?
C8 Fe3 Te 90.65(12) . . ?
C8 Fe3 Fe1 108.16(11) . . ?
C1 Fe4 Sb 90.55(12) . . ?
C1 Fe4 C12 97.90(14) . . ?
C1 Fe4 C13 129.64(14) . . ?
C1 Fe4 C14 163.07(16) . . ?
C1 Fe4 C15 130.10(19) . . ?
C1 Fe4 C16 98.11(17) . . ?
C2 Fe4 Sb 91.80(12) . . ?
C2 Fe4 C1 92.52(17) . . ?
C2 Fe4 C12 153.92(16) . . ?
C2 Fe4 C13 137.82(15) . . ?
C2 Fe4 C14 99.86(16) . . ?
C2 Fe4 C15 89.01(16) . . ?
C2 Fe4 C16 115.70(16) . . ?
C12 Fe4 Sb 111.84(11) . . ?
C13 Fe4 Sb 87.31(12) . . ?
C13 Fe4 C12 38.93(14) . . ?
C14 Fe4 Sb 100.48(14) . . ?
C14 Fe4 C12 66.15(14) . . ?
C14 Fe4 C13 39.51(15) . . ?
C14 Fe4 C15 39.64(19) . . ?
C14 Fe4 C16 66.14(18) . . ?
C15 Fe4 Sb 139.28(15) . . ?
C15 Fe4 C12 66.03(15) . . ?
C15 Fe4 C13 65.98(18) . . ?
C15 Fe4 C16 39.30(15) . . ?
C16 Fe4 Sb 150.56(13) . . ?
C16 Fe4 C12 39.23(15) . . ?
C16 Fe4 C13 65.52(18) . . ?
O1 C1 Fe4 177.4(3) . . ?
O2 C2 Fe4 176.5(4) . . ?
O3 C3 Fe2 179.3(4) . . ?
O4 C4 Fe2 177.8(3) . . ?
O5 C5 Fe2 179.7(4) . . ?
O6 C6 Fe3 178.3(3) . . ?
O7 C7 Fe3 179.4(4) . . ?
O8 C8 Fe3 177.5(3) . . ?
O9 C9 Fe1 175.5(3) . . ?
O10 C10 Fe1 175.3(4) . . ?
O11 C11 Fe1 175.0(3) . . ?
C13 C12 Fe4 69.5(2) . . ?
C13 C12 C16 106.5(3) . . ?
C13 C12 C17 126.2(3) . . ?
C16 C12 Fe4 68.4(2) . . ?
C16 C12 C17 126.9(4) . . ?
C17 C12 Fe4 132.3(2) . . ?
C12 C13 Fe4 71.6(2) . . ?
C12 C13 C14 108.8(4) . . ?
C14 C13 Fe4 69.1(2) . . ?
C13 C14 Fe4 71.3(2) . . ?
C15 C14 Fe4 70.2(2) . . ?
C15 C14 C13 107.6(4) . . ?
C14 C15 Fe4 70.2(2) . . ?
C16 C15 Fe4 70.6(2) . . ?
C16 C15 C14 107.9(4) . . ?
C12 C16 Fe4 72.3(2) . . ?
C15 C16 Fe4 70.1(2) . . ?
C15 C16 C12 109.2(4) . . ?
C12 C17 C18 110.7(3) . . ?
C12 C17 C19 106.9(3) . . ?
C18 C17 C19 108.8(3) . . ?
C20 C17 C12 111.1(3) . . ?
C20 C17 C18 110.4(3) . . ?
C20 C17 C19 108.8(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
Sb Te 3.2764(11) . ?
Sb Fe1 2.5555(8) . ?
Sb Fe2 2.5063(7) . ?
Sb Fe3 2.5012(6) . ?
Sb Fe4 2.5224(10) . ?
Te Fe1 2.5278(8) . ?
Te Fe2 2.5612(7) . ?
Te Fe3 2.5458(7) . ?
Fe1 Fe2 2.7706(8) . ?
Fe1 Fe3 2.7946(8) . ?
Fe1 C9 1.791(4) . ?
Fe1 C10 1.773(4) . ?
Fe1 C11 1.789(4) . ?
Fe2 C3 1.784(4) . ?
Fe2 C4 1.805(4) . ?
Fe2 C5 1.809(4) . ?
Fe3 C6 1.790(4) . ?
Fe3 C7 1.765(4) . ?
Fe3 C8 1.817(4) . ?
Fe4 C1 1.781(4) . ?
Fe4 C2 1.771(4) . ?
Fe4 C12 2.148(3) . ?
Fe4 C13 2.119(4) . ?
Fe4 C14 2.090(4) . ?
Fe4 C15 2.090(4) . ?
Fe4 C16 2.096(4) . ?
C1 O1 1.145(4) . ?
C2 O2 1.149(4) . ?
C3 O3 1.148(5) . ?
C4 O4 1.139(4) . ?
C5 O5 1.138(5) . ?
C6 O6 1.144(5) . ?
C7 O7 1.149(5) . ?
C8 O8 1.141(4) . ?
C9 O9 1.140(4) . ?
C10 O10 1.148(4) . ?
C11 O11 1.135(4) . ?
C12 C13 1.422(5) . ?
C12 C16 1.425(6) . ?
C12 C17 1.522(5) . ?
C13 C14 1.423(5) . ?
C14 C15 1.418(7) . ?
C15 C16 1.408(5) . ?
C17 C18 1.531(5) . ?
C17 C19 1.536(5) . ?
C17 C20 1.518(6) . ?
