#------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (чт, 18 лют 2016) $
#$Revision: 176729 $
#$URL: svn://crystallography.net/cod/cif/1/50/27/1502740.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_1502740
_journal_issue                   51
_journal_name_full               'The journal of physical chemistry. A'
_journal_page_first              13418
_journal_page_last               13433
_journal_paper_doi               10.1021/jp1098624
_journal_volume                  114
_journal_year                    2010
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C12 H4 Fe3 O11'
_chemical_formula_sum            'C12 H4 Fe3 O11'
_chemical_formula_weight         491.7
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             '30-Sep-09 T18:02:13-00:00'
_audit_creation_method           'XD routine XDCIF'
_cell_angle_alpha                90
_cell_angle_beta                 103.9270(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.46720(10)
_cell_length_b                   16.4731(2)
_cell_length_c                   13.74140(10)
_cell_measurement_reflns_used    84907
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      55.734
_cell_measurement_theta_min      2
_cell_measurement_wavelength     0.71073
_cell_volume                     1640.61(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.835814E-1
_diffrn_orient_matrix_UB_12      0.27222E-2
_diffrn_orient_matrix_UB_13      0.468772E-1
_diffrn_orient_matrix_UB_21      0.875286E-1
_diffrn_orient_matrix_UB_22      -0.349279E-1
_diffrn_orient_matrix_UB_23      0.490164E-1
_diffrn_orient_matrix_UB_31      0.662568E-1
_diffrn_orient_matrix_UB_32      0.495755E-1
_diffrn_orient_matrix_UB_33      0.319599E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            131757
_diffrn_reflns_reduction_process
;
 Scaled and merged with SORTAV
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        50.04
_diffrn_reflns_theta_max         50.04
_diffrn_reflns_theta_min         2.47
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    2.674
_exptl_absorpt_correction_T_max  0.636
_exptl_absorpt_correction_T_min  0.433
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
   P. Coppens, L. Leiserowitz, D Rabinovich, Acta Cryst.
   (1965), 18, 1035-1038
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.991
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.405
_refine_diff_density_min         -0.402
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.412
_refine_ls_matrix_type           full
_refine_ls_number_parameters     721
_refine_ls_number_reflns         14316
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.035
_refine_ls_R_factor_gt           0.02
_refine_ls_shift/su_max          0.00004
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
        calc w1 = 1/[s²(Fo)]
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.016
_reflns_number_gt                14317
_reflns_number_total             17081
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jp1098624_si_002.cif
_cod_data_source_block           multipole
_cod_database_code               1502740
loop_
_atom_rho_multipole_atom_label
_atom_rho_multipole_coeff_Pv
_atom_rho_multipole_coeff_P00
_atom_rho_multipole_coeff_P11
_atom_rho_multipole_coeff_P1-1
_atom_rho_multipole_coeff_P10
_atom_rho_multipole_coeff_P20
_atom_rho_multipole_coeff_P21
_atom_rho_multipole_coeff_P2-1
_atom_rho_multipole_coeff_P22
_atom_rho_multipole_coeff_P2-2
_atom_rho_multipole_coeff_P30
_atom_rho_multipole_coeff_P31
_atom_rho_multipole_coeff_P3-1
_atom_rho_multipole_coeff_P32
_atom_rho_multipole_coeff_P3-2
_atom_rho_multipole_coeff_P33
_atom_rho_multipole_coeff_P3-3
_atom_rho_multipole_coeff_P40
_atom_rho_multipole_coeff_P41
_atom_rho_multipole_coeff_P4-1
_atom_rho_multipole_coeff_P42
_atom_rho_multipole_coeff_P4-2
_atom_rho_multipole_coeff_P43
_atom_rho_multipole_coeff_P4-3
_atom_rho_multipole_coeff_P44
_atom_rho_multipole_coeff_P4-4
_atom_rho_multipole_kappa
_atom_rho_multipole_kappa_prime0
_atom_rho_multipole_kappa_prime1
_atom_rho_multipole_kappa_prime2
_atom_rho_multipole_kappa_prime3
_atom_rho_multipole_kappa_prime4
Fe(1) 5.429(17) 0 -0.058(10) -0.089(10) -0.110(11) -0.003(14) 0.042(12)
-0.011(12) 0.130(13) -0.035(13) -0.044(10) -0.037(9) -0.035(9) 0.002(8)
-0.016(9) 0.017(8) 0.027(8) -0.135(15) -0.058(13) 0.056(13) -0.053(13)
-0.014(14) 0.035(12) -0.007(13) -0.164(11) 0.058(11) 1.01239 1.075384 1.075384
1.075384 1.075384 1.075384
Fe(2) 5.418(16) 0 -0.014(10) -0.015(10) 0.027(10) 0.059(13) 0.002(12) 0.034(12)
0.015(12) -0.011(12) 0.010(8) 0.005(8) 0.024(8) 0.002(8) -0.022(8) -0.020(8)
-0.010(8) -0.247(13) 0.028(12) -0.036(12) -0.048(12) 0.020(12) -0.025(12)
-0.053(12) -0.190(11) -0.091(11) 1.01239 1.075384 1.075384 1.075384 1.075384
1.075384
Fe(3) 5.408(16) 0 -0.014(10) -0.036(10) 0.070(10) 0.053(13) 0.005(12) 0.004(13)
-0.021(12) -0.011(12) 0.047(9) -0.024(8) 0.000(9) -0.003(8) 0.005(8) 0.022(8)
0.002(8) -0.226(14) -0.035(13) -0.023(13) -0.052(13) 0.014(13) 0.005(12)
-0.025(12) -0.184(11) 0.040(11) 1.01239 1.075384 1.075384 1.075384 1.075384
1.075384
O(1) 5.99(2) 0 0.018(14) -0.083(15) 0.009(13) 0.056(14) 0.020(14) 0.058(14)
0.033(15) 0.030(15) 0.052(10) -0.009(9) -0.003(10) 0.056(10) 0.015(10)
-0.002(10) -0.030(10) 0.016(13) -0.019(11) -0.011(12) 0.009(12) -0.007(12)
-0.014(12) -0.002(12) -0.016(12) 0.039(12) 0.996583 1.020057 1.020057 1.020057
1.020057 1.020057
O(11) 5.81(3) 0 -0.029(16) 0.013(16) -0.066(17) 0.066(18) -0.004(16) -0.005(16)
-0.005(16) -0.010(16) 0.004(12) -0.006(11) -0.006(12) -0.019(11) -0.018(11)
-0.040(11) -0.041(11) 0 0 0 0 0 0 0 0 0 1.003297 1.007294 1.007294 1.007294
1.007294 1.007294
O(12) 5.97(3) 0 -0.048(16) -0.027(14) 0.027(17) 0.120(17) 0.040(16) -0.001(15)
-0.016(15) 0.026(15) 0.028(11) 0.008(11) 0.003(10) 0.005(11) 0.004(11)
-0.027(10) -0.006(10) 0 0 0 0 0 0 0 0 0 1.003297 1.007294 1.007294 1.007294
1.007294 1.007294
O(13) 5.99(4) 0 0.07(2) -0.02(3) 0.10(2) 0.17(2) -0.02(2) 0.01(2) 0.06(3)
0.02(3) -0.050(15) -0.035(13) 0.022(15) -0.037(15) 0.064(15) 0.079(16)
-0.013(16) 0 0 0 0 0 0 0 0 0 1.003297 1.007294 1.007294 1.007294 1.007294
1.007294
O(14) 6.01(4) 0 -0.09(2) 0.032(19) 0.12(2) 0.15(2) -0.01(2) 0.02(2) 0.01(2)
0.10(2) 0.022(16) 0.053(15) -0.001(13) 0.039(15) -0.015(15) -0.028(13)
-0.003(13) 0 0 0 0 0 0 0 0 0 1.003297 1.007294 1.007294 1.007294 1.007294
1.007294
O(21) 5.90(2) 0 0.001(14) 0.019(13) -0.014(16) 0.150(16) 0.006(15) 0.021(14)
-0.030(14) 0.014(14) 0.031(11) -0.005(10) -0.003(10) -0.011(10) -0.004(10)
0.028(10) 0.029(10) 0 0 0 0 0 0 0 0 0 1.003297 1.007294 1.007294 1.007294
1.007294 1.007294
O(22) 5.94(3) 0 0.012(17) 0.043(18) -0.086(18) 0.113(19) -0.010(17) 0.009(18)
0.005(18) 0.000(18) 0.022(13) -0.023(12) 0.011(12) 0.020(12) -0.011(12)
-0.011(12) 0.026(12) 0 0 0 0 0 0 0 0 0 1.003297 1.007294 1.007294 1.007294
1.007294 1.007294
O(23) 5.95(3) 0 0.028(15) 0.006(15) 0.017(16) 0.121(17) -0.018(16) 0.002(15)
-0.009(16) -0.005(15) 0.022(11) -0.023(11) 0.022(11) -0.014(11) 0.016(11)
-0.023(10) -0.012(10) 0 0 0 0 0 0 0 0 0 1.003297 1.007294 1.007294 1.007294
1.007294 1.007294
O(31) 6.05(4) 0 0.02(2) -0.01(2) 0.07(2) 0.14(2) 0.04(2) 0.05(2) 0.04(2)
-0.03(2) 0.001(15) 0.024(14) -0.013(15) -0.012(14) 0.033(14) 0.025(14)
0.079(14) 0 0 0 0 0 0 0 0 0 1.003297 1.007294 1.007294 1.007294 1.007294
1.007294
O(32) 5.93(3) 0 -0.04(2) 0.051(17) 0.046(19) 0.14(2) -0.02(2) -0.039(17)
-0.04(2) -0.01(2) -0.002(14) 0.015(13) -0.040(12) 0.017(13) -0.012(13)
-0.038(13) 0.079(13) 0 0 0 0 0 0 0 0 0 1.003297 1.007294 1.007294 1.007294
1.007294 1.007294
O(33) 5.91(3) 0 -0.028(18) 0.02(2) -0.014(19) 0.08(2) 0.000(18) -0.038(19)
-0.04(2) 0.00(2) -0.080(13) 0.015(12) -0.040(13) -0.055(13) 0.117(13)
-0.048(14) -0.073(13) 0 0 0 0 0 0 0 0 0 1.003297 1.007294 1.007294 1.007294
1.007294 1.007294
C(1) 4.48(2) 0 0.035(16) 0.030(16) -0.24(2) 0.20(2) -0.053(16) 0.029(17)
-0.284(15) -0.146(15) 0.30(3) -0.01(2) 0.05(2) 0.165(19) 0.066(19) -0.112(17)
-0.010(17) -0.09(3) 0.01(3) -0.02(3) 0.00(3) 0.05(3) -0.09(2) 0.04(2) 0.01(2)
0.03(2) 0.963612 0.733485 0.733485 0.733485 0.733485 0.733485
C(2) 4.14(6) 0 -0.053(14) -0.054(14) -0.145(18) -0.181(18) 0.030(16) -0.045(15)
0.033(15) -0.005(14) 0.50(2) -0.001(19) -0.047(17) -0.051(17) 0.069(16)
0.011(18) -0.216(18) 0.21(2) 0.03(2) 0.04(2) 0.07(2) -0.03(2) -0.06(2) 0.16(2)
-0.047(19) 0.054(18) 0.990068 0.87519 0.87519 0.87519 0.87519 0.87519
C(11) 4.18(3) 0 -0.042(13) -0.054(13) 0.08(2) 0.52(2) -0.021(15) -0.020(15)
0.006(12) 0.014(13) 0.15(2) 0.039(17) -0.006(17) 0.008(14) -0.002(15) 0.013(13)
0.021(13) 0 0 0 0 0 0 0 0 0 0.992299 0.884585 0.884585 0.884585 0.884585
0.884585
C(12) 4.13(3) 0 -0.060(14) 0.019(13) -0.11(2) 0.48(2) -0.017(15) -0.062(15)
0.021(12) -0.007(13) 0.07(2) 0.017(17) -0.005(18) 0.014(14) -0.032(16)
0.000(13) 0.025(14) 0 0 0 0 0 0 0 0 0 0.992299 0.884585 0.884585 0.884585
0.884585 0.884585
C(13) 4.21(3) 0 -0.058(14) -0.013(15) -0.07(3) 0.40(2) -0.012(16) -0.060(18)
-0.008(14) -0.017(14) 0.01(2) 0.011(18) -0.015(19) 0.000(16) 0.063(16)
0.015(15) -0.035(15) 0 0 0 0 0 0 0 0 0 0.992299 0.884585 0.884585 0.884585
0.884585 0.884585
C(14) 4.09(4) 0 -0.004(15) 0.003(14) -0.15(3) 0.45(2) 0.024(17) 0.009(16)
0.009(14) -0.038(15) 0.03(2) 0.00(2) 0.015(19) -0.022(17) 0.009(17) 0.015(14)
0.014(13) 0 0 0 0 0 0 0 0 0 0.992299 0.884585 0.884585 0.884585 0.884585
0.884585
C(21) 4.01(3) 0 -0.012(12) 0.004(12) -0.05(2) 0.510(19) -0.002(14) -0.041(14)
-0.008(12) 0.021(12) 0.07(2) 0.006(16) -0.047(17) 0.014(14) -0.021(14)
-0.012(13) -0.002(13) 0 0 0 0 0 0 0 0 0 0.992299 0.884585 0.884585 0.884585
0.884585 0.884585
C(22) 4.32(3) 0 -0.070(13) -0.027(14) 0.01(2) 0.51(2) -0.013(15) -0.003(15)
-0.036(13) 0.005(13) 0.11(2) -0.005(18) -0.021(18) -0.018(15) 0.016(15)
0.006(14) 0.004(14) 0 0 0 0 0 0 0 0 0 0.992299 0.884585 0.884585 0.884585
0.884585 0.884585
C(23) 4.22(3) 0 -0.022(13) -0.052(13) -0.06(2) 0.44(2) -0.019(14) -0.018(14)
0.010(12) 0.034(12) 0.09(2) -0.035(17) 0.030(18) -0.011(15) -0.016(14)
-0.038(13) 0.045(13) 0 0 0 0 0 0 0 0 0 0.992299 0.884585 0.884585 0.884585
0.884585 0.884585
C(31) 4.27(3) 0 0.034(14) 0.017(15) -0.08(3) 0.41(2) 0.049(16) -0.013(17)
0.040(13) 0.011(13) 0.04(2) 0.027(19) 0.05(2) -0.023(16) 0.024(16) 0.027(14)
-0.025(14) 0 0 0 0 0 0 0 0 0 0.992299 0.884585 0.884585 0.884585 0.884585
0.884585
C(32) 4.00(3) 0 0.024(14) 0.017(12) -0.11(2) 0.45(2) -0.017(16) 0.026(15)
0.007(14) -0.021(13) 0.07(2) -0.001(19) 0.034(17) 0.057(15) -0.022(15)
0.000(13) 0.000(14) 0 0 0 0 0 0 0 0 0 0.992299 0.884585 0.884585 0.884585
0.884585 0.884585
C(33) 4.19(3) 0 -0.006(14) 0.057(14) 0.05(2) 0.50(2) 0.038(15) 0.043(16)
-0.016(14) 0.012(13) 0.11(2) -0.029(17) 0.037(18) 0.051(15) 0.057(16) 0.060(14)
-0.006(15) 0 0 0 0 0 0 0 0 0 0.992299 0.884585 0.884585 0.884585 0.884585
0.884585
H(1) 1.296(16) 0 -0.04(4) 0.05(4) -0.01(4) 0.04(2) -0.085(19) -0.053(19)
-0.01(2) 0.011(19) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.012809 1.012809 1.012809
1.012809 1.012809 1.012809
H(2A) 0.916(19) 0 0.012(12) 0.058(12) 0.156(12) 0.032(17) 0 0 0 0 0 0 0 0 0 0 0
0 0 0 0 0 0 0 0 0 1.158107 1.158107 1.158107 1.158107 1.158107 1.158107
H(2B) 0.916(19) 0 0.012(12) 0.058(12) 0.156(12) 0.032(17) 0 0 0 0 0 0 0 0 0 0 0
0 0 0 0 0 0 0 0 0 1.158107 1.158107 1.158107 1.158107 1.158107 1.158107
H(2B) 0.916(19) 0 0.012(12) 0.058(12) 0.156(12) 0.032(17) 0 0 0 0 0 0 0 0 0 0 0
0 0 0 0 0 0 0 0 0 1.158107 1.158107 1.158107 1.158107 1.158107
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
Fe(1) Fe 0.334365(16) 0.060764(8) 0.188579(9) 0.013 Uani 1 4
Fe(2) Fe 0.174446(14) 0.056401(7) 0.340676(8) 0.011 Uani 1 4
Fe(3) Fe 0.331354(16) 0.190514(7) 0.305413(9) 0.013 Uani 1 4
O(1) O -0.06991(8) 0.17003(4) 0.21520(5) 0.018 Uani 1 4
O(11) O -0.01607(10) 0.08612(6) 0.03426(6) 0.025 Uani 1 4
O(12) O 0.66434(9) 0.03262(5) 0.35272(6) 0.023 Uani 1 4
O(13) O 0.56577(14) 0.10887(11) 0.05138(8) 0.041 Uani 1 4
O(14) O 0.31932(18) -0.11716(6) 0.16657(8) 0.037 Uani 1 4
O(21) O 0.01848(9) 0.09985(4) 0.51081(5) 0.02 Uani 1 4
O(22) O -0.12469(11) -0.04365(6) 0.22279(7) 0.028 Uani 1 4
O(23) O 0.38893(10) -0.08665(4) 0.43805(6) 0.023 Uani 1 4
O(31) O 0.19716(19) 0.31426(7) 0.42422(8) 0.038 Uani 1 4
O(32) O 0.34868(13) 0.28957(6) 0.13032(7) 0.032 Uani 1 4
O(33) O 0.72867(12) 0.21534(6) 0.40801(9) 0.034 Uani 1 4
C(1) C 0.09540(5) 0.14793(2) 0.26279(3) 0.014 Uani 1 4
C(2) C -0.09857(8) 0.24783(4) 0.16372(5) 0.026 Uani 1 4
C(11) C 0.11743(6) 0.07884(3) 0.09496(4) 0.017 Uani 1 4
C(12) C 0.53295(6) 0.04847(3) 0.29245(4) 0.018 Uani 1 4
C(13) C 0.47455(7) 0.09168(4) 0.10442(4) 0.024 Uani 1 4
C(14) C 0.32140(8) -0.04770(4) 0.17195(4) 0.022 Uani 1 4
C(21) C 0.07573(6) 0.08187(3) 0.44384(3) 0.014 Uani 1 4
C(22) C -0.00836(6) -0.00501(3) 0.27000(4) 0.017 Uani 1 4
C(23) C 0.31186(6) -0.02990(3) 0.40271(3) 0.015 Uani 1 4
C(31) C 0.25367(8) 0.26688(3) 0.37854(4) 0.021 Uani 1 4
C(32) C 0.33952(7) 0.25044(3) 0.19820(4) 0.02 Uani 1 4
C(33) C 0.57822(7) 0.20385(3) 0.36742(4) 0.021 Uani 1 4
H(1) H 0.338(3) 0.1178(14) 0.3917(15) 0.029 Uani 1 4
H(2A) H -0.247749 0.256184 0.144954 0.073 Uani 1 4
H(2B) H -0.035424 0.295676 0.215494 0.077 Uani 1 4
H(2C) H -0.038602 0.245887 0.098855 0.073 Uani 1 4
