#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:37:44 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179854 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/50/7015041.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_7015041
loop_
_publ_author_name
'Pushkarevsky, Nikolay A.'
'Konchenko, Sergey N.'
'Zabel, Manfred'
'Bodensteiner, Michael'
'Scheer, Manfred'
_publ_section_title
;
 Dimerization of pentanuclear clusters [Fe(3)Q(AsMe)(CO)(9)] (Q = Se,
 Te) as a conversion pathway to novel cubane-like aggregates.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2067
_journal_page_last               2074
_journal_paper_doi               10.1039/c0dt01587c
_journal_volume                  40
_journal_year                    2011
_chemical_formula_sum            'C15 H8 As2 Cl2 Fe4 O12 Se2'
_chemical_formula_weight         982.27
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 92.02(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.397(2)
_cell_length_b                   17.966(4)
_cell_length_c                   15.416(3)
_cell_measurement_reflns_used    987
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.91
_cell_measurement_theta_min      2.07
_cell_volume                     2877.8(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  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'STOE IPDS'
_diffrn_measurement_method       rotation
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56087
_diffrn_reflns_av_R_equivalents  0.1064
_diffrn_reflns_av_sigmaI/netI    0.0852
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24851
_diffrn_reflns_theta_full        25.91
_diffrn_reflns_theta_max         25.91
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    3.686
_exptl_absorpt_correction_T_max  0.6930
_exptl_absorpt_correction_T_min  0.4721
_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       route
_exptl_crystal_F_000             1864
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.787
_refine_diff_density_min         -2.417
_refine_diff_density_rms         0.267
_refine_ls_extinction_coef       0.0050(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.252
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         10996
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.264
_refine_ls_R_factor_all          0.1395
_refine_ls_R_factor_gt           0.0778
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1985
_refine_ls_wR_factor_ref         0.2399
_reflns_number_gt                6218
_reflns_number_total             10996
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0DT01587C.TXT
_cod_data_source_block           2a_CH2Cl2
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7015041
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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
As2 As 0.22007(7) 0.21507(4) 0.00030(5) 0.03289(18) Uani 1 1 d . . .
As1 As 0.28010(7) 0.17508(4) 0.18030(5) 0.03155(18) Uani 1 1 d . . .
Se1 Se 0.41825(7) 0.08807(4) 0.03669(5) 0.03451(18) Uani 1 1 d . . .
Se2 Se 0.10790(7) 0.06763(4) 0.06898(5) 0.03386(18) Uani 1 1 d . . .
Fe1 Fe 0.42385(11) 0.22171(6) 0.07609(8) 0.0333(2) Uani 1 1 d . . .
Fe2 Fe 0.30068(11) 0.04443(6) 0.16296(8) 0.0350(2) Uani 1 1 d . . .
Fe3 Fe 0.22719(11) 0.09403(6) -0.06256(7) 0.0356(2) Uani 1 1 d . . .
Fe4 Fe 0.07296(11) 0.19850(6) 0.11404(7) 0.0327(2) Uani 1 1 d . . .
C1 C 0.5063(9) 0.2474(5) -0.0214(6) 0.0451(19) Uani 1 1 d . . .
O1 O 0.5540(8) 0.2677(5) -0.0818(6) 0.075(2) Uani 1 1 d . . .
C2 C 0.3928(9) 0.3149(5) 0.1091(7) 0.047(2) Uani 1 1 d . . .
O2 O 0.3739(9) 0.3742(4) 0.1317(7) 0.082(3) Uani 1 1 d . . .
C3 C 0.5658(9) 0.2095(5) 0.1487(6) 0.0439(18) Uani 1 1 d . . .
O3 O 0.6516(8) 0.2059(5) 0.1940(6) 0.068(2) Uani 1 1 d . . .
C4 C 0.4479(9) 0.0440(5) 0.2289(7) 0.048(2) Uani 1 1 d . . .
O4 O 0.5385(9) 0.0450(5) 0.2695(6) 0.075(2) Uani 1 1 d . . .
C5 C 0.1963(11) 0.0303(5) 0.2519(6) 0.050(2) Uani 1 1 d . . .
O5 O 0.1324(9) 0.0274(4) 0.3087(5) 0.070(2) Uani 1 1 d . . .
C6 C 0.3109(9) -0.0533(4) 0.1303(7) 0.046(2) Uani 1 1 d . . .
O6 O 0.3181(8) -0.1145(4) 0.1115(6) 0.067(2) Uani 1 1 d . . .
C7 C 0.2388(8) -0.0073(5) -0.0856(6) 0.0445(19) Uani 1 1 d . . .
O7 O 0.2429(8) -0.0666(4) -0.1030(6) 0.069(2) Uani 1 1 d . . .
C8 C 0.0781(9) 0.1092(5) -0.1229(6) 0.0448(18) Uani 1 1 d . . .
O8 O -0.0131(8) 0.1205(5) -0.1628(5) 0.070(2) Uani 1 1 d . . .
C9 C 0.3278(10) 0.1283(6) -0.1465(6) 0.053(2) Uani 1 1 d . . .
O9 O 0.3867(9) 0.1517(6) -0.1992(6) 0.086(3) Uani 1 1 d . . .
C10 C -0.0173(8) 0.1685(5) 0.2071(6) 0.0391(16) Uani 1 1 d . . .
O10 O -0.0730(7) 0.1517(4) 0.2649(5) 0.0591(18) Uani 1 1 d . . .
C11 C -0.0655(8) 0.2078(5) 0.0411(6) 0.0411(17) Uani 1 1 d . . .
O11 O -0.1507(8) 0.2152(4) -0.0047(6) 0.0642(19) Uani 1 1 d . . .
C12 C 0.0821(9) 0.2951(5) 0.1419(6) 0.0433(18) Uani 1 1 d . . .
O12 O 0.0869(8) 0.3554(4) 0.1606(6) 0.072(2) Uani 1 1 d . . .
C13 C 0.3102(10) 0.2111(6) 0.2995(6) 0.051(2) Uani 1 1 d . . .
H13A H 0.2873 0.2639 0.3026 0.077 Uiso 1 1 calc R . .
H13B H 0.4013 0.2047 0.3166 0.077 Uiso 1 1 calc R . .
H13C H 0.2571 0.1825 0.3389 0.077 Uiso 1 1 calc R . .
C14 C 0.1776(11) 0.2982(3) -0.0826(4) 0.059(3) Uani 1 1 d . . .
H14A H 0.2454 0.3023 -0.1249 0.088 Uiso 1 1 calc R . .
H14B H 0.1714 0.3450 -0.0504 0.088 Uiso 1 1 calc R . .
H14C H 0.0952 0.2878 -0.1130 0.088 Uiso 1 1 calc R . .
C15 C 0.1999(5) 0.0469(2) -0.4775(4) 0.32(6) Uani 0.50 1 d PRD A 1
Cl1 Cl 0.1368(5) -0.0191(2) -0.4088(4) 0.182(8) Uani 0.50 1 d PRD A 1
Cl2 Cl 0.3437(5) 0.0163(3) -0.5150(4) 0.109(3) Uani 0.50 1 d PRD A 1
C16 C 0.2802(5) 0.0481(2) -0.4227(4) 0.53(12) Uani 0.50 1 d PRD D 2
Cl3 Cl 0.2420(5) 0.1310(2) -0.4016(4) 0.115(4) Uani 0.50 1 d PRD D 2
Cl4 Cl 0.1732(5) -0.0045(2) -0.3632(4) 0.43(3) Uani 0.50 1 d PRD D 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0015 0.0009 '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 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.2886 0.5448 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.2758 1.3314 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se 0.2367 1.4831 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.0998 0.0984 '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
C14 As2 Fe3 115.46(17) . . ?
C14 As2 Fe4 115.4(3) . . ?
Fe3 As2 Fe4 102.41(5) . . ?
C14 As2 Fe1 116.5(3) . . ?
Fe3 As2 Fe1 101.83(5) . . ?
Fe4 As2 Fe1 103.15(5) . . ?
C14 As2 As1 145.69(17) . . ?
Fe3 As2 As1 98.84(4) . . ?
Fe4 As2 As1 52.44(4) . . ?
Fe1 As2 As1 52.35(4) . . ?
C13 As1 Fe2 114.8(3) . . ?
C13 As1 Fe1 115.6(3) . . ?
Fe2 As1 Fe1 102.15(5) . . ?
C13 As1 Fe4 117.0(3) . . ?
Fe2 As1 Fe4 102.10(5) . . ?
Fe1 As1 Fe4 103.13(5) . . ?
C13 As1 As2 146.4(3) . . ?
Fe2 As1 As2 98.85(4) . . ?
Fe1 As1 As2 52.40(4) . . ?
Fe4 As1 As2 52.37(4) . . ?
Fe2 Se1 Fe3 95.32(5) . . ?
Fe2 Se1 Fe1 97.05(4) . . ?
Fe3 Se1 Fe1 96.97(5) . . ?
Fe3 Se2 Fe2 95.38(5) . . ?
Fe3 Se2 Fe4 97.53(4) . . ?
Fe2 Se2 Fe4 96.87(5) . . ?
C2 Fe1 C1 95.3(4) . . ?
C2 Fe1 C3 95.1(4) . . ?
C1 Fe1 C3 98.2(4) . . ?
C2 Fe1 As1 90.8(3) . . ?
C1 Fe1 As1 166.5(3) . . ?
C3 Fe1 As1 93.3(3) . . ?
C2 Fe1 As2 91.2(3) . . ?
C1 Fe1 As2 92.5(3) . . ?
C3 Fe1 As2 167.0(3) . . ?
As1 Fe1 As2 75.26(4) . . ?
C2 Fe1 Se1 167.8(3) . . ?
C1 Fe1 Se1 92.9(3) . . ?
C3 Fe1 Se1 92.6(3) . . ?
As1 Fe1 Se1 79.33(4) . . ?
As2 Fe1 Se1 79.55(4) . . ?
C5 Fe2 C4 95.3(5) . . ?
C5 Fe2 C6 96.7(4) . . ?
C4 Fe2 C6 95.4(4) . . ?
C5 Fe2 As1 89.7(3) . . ?
C4 Fe2 As1 91.1(3) . . ?
C6 Fe2 As1 170.4(3) . . ?
C5 Fe2 Se1 168.0(3) . . ?
C4 Fe2 Se1 90.7(3) . . ?
C6 Fe2 Se1 93.0(3) . . ?
As1 Fe2 Se1 79.83(4) . . ?
C5 Fe2 Se2 88.4(3) . . ?
C4 Fe2 Se2 170.2(3) . . ?
C6 Fe2 Se2 93.1(3) . . ?
As1 Fe2 Se2 79.88(4) . . ?
Se1 Fe2 Se2 84.13(5) . . ?
C8 Fe3 C9 95.1(4) . . ?
C8 Fe3 C7 96.3(4) . . ?
C9 Fe3 C7 98.9(4) . . ?
C8 Fe3 As2 91.9(3) . . ?
C9 Fe3 As2 90.4(3) . . ?
C7 Fe3 As2 167.0(3) . . ?
C8 Fe3 Se2 90.3(3) . . ?
C9 Fe3 Se2 168.7(3) . . ?
C7 Fe3 Se2 90.4(3) . . ?
As2 Fe3 Se2 79.45(4) . . ?
C8 Fe3 Se1 170.8(3) . . ?
C9 Fe3 Se1 89.1(3) . . ?
C7 Fe3 Se1 91.1(3) . . ?
As2 Fe3 Se1 79.82(4) . . ?
Se2 Fe3 Se1 84.19(5) . . ?
C12 Fe4 C11 95.4(4) . . ?
C12 Fe4 C10 97.0(4) . . ?
C11 Fe4 C10 95.5(4) . . ?
C12 Fe4 As2 91.5(3) . . ?
C11 Fe4 As2 92.8(3) . . ?
C10 Fe4 As2 167.5(3) . . ?
C12 Fe4 As1 91.6(3) . . ?
C11 Fe4 As1 166.2(3) . . ?
C10 Fe4 As1 95.3(3) . . ?
As2 Fe4 As1 75.19(4) . . ?
C12 Fe4 Se2 168.2(3) . . ?
C11 Fe4 Se2 92.0(3) . . ?
C10 Fe4 Se2 91.4(3) . . ?
As2 Fe4 Se2 78.96(4) . . ?
As1 Fe4 Se2 79.29(4) . . ?
O1 C1 Fe1 175.7(9) . . ?
O2 C2 Fe1 178.7(11) . . ?
O3 C3 Fe1 176.3(8) . . ?
O4 C4 Fe2 178.9(9) . . ?
O5 C5 Fe2 174.5(9) . . ?
O6 C6 Fe2 178.7(10) . . ?
O7 C7 Fe3 176.6(10) . . ?
O8 C8 Fe3 177.3(9) . . ?
O9 C9 Fe3 177.2(11) . . ?
O10 C10 Fe4 178.5(8) . . ?
O11 C11 Fe4 178.4(9) . . ?
O12 C12 Fe4 178.9(8) . . ?
Cl2 C15 Cl1 110.0 . . ?
Cl3 C16 Cl4 103.50(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
As2 C14 2.004(5) . ?
As2 Fe3 2.3828(13) . ?
As2 Fe4 2.3859(14) . ?
As2 Fe1 2.3860(16) . ?
As2 As1 2.9126(13) . ?
As1 C13 1.963(9) . ?
As1 Fe2 2.3731(13) . ?
As1 Fe1 2.3845(14) . ?
As1 Fe4 2.3882(15) . ?
Se1 Fe2 2.4631(15) . ?
Se1 Fe3 2.4665(16) . ?
Se1 Fe1 2.4767(13) . ?
Se2 Fe3 2.4603(15) . ?
Se2 Fe2 2.4668(16) . ?
Se2 Fe4 2.4821(13) . ?
Fe1 C2 1.783(9) . ?
Fe1 C1 1.816(9) . ?
Fe1 C3 1.834(10) . ?
Fe2 C5 1.796(10) . ?
Fe2 C4 1.807(10) . ?
Fe2 C6 1.830(8) . ?
Fe3 C8 1.799(10) . ?
Fe3 C9 1.801(10) . ?
Fe3 C7 1.860(9) . ?
Fe4 C12 1.789(9) . ?
Fe4 C11 1.803(9) . ?
Fe4 C10 1.823(8) . ?
C1 O1 1.131(10) . ?
C2 O2 1.139(10) . ?
C3 O3 1.115(11) . ?
C4 O4 1.114(12) . ?
C5 O5 1.119(11) . ?
C6 O6 1.142(10) . ?
C7 O7 1.100(11) . ?
C8 O8 1.132(12) . ?
C9 O9 1.116(11) . ?
C10 O10 1.122(10) . ?
C11 O11 1.120(11) . ?
C12 O12 1.122(11) . ?
C15 Cl2 1.7117(12) . ?
C15 Cl1 1.7338 . ?
C16 Cl3 1.5782 . ?
C16 Cl4 1.7448 . ?
