Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 #------------------ AUDIT DETAILS -------------------------------------------# _audit_creation_date 2006-01-09 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _audit_update_record ? _publ_contact_author_name 'M. Weller' _publ_contact_author_address ; Department of Chemistry The University Southampton SO9 5NH UNITED KINGDOM ; _publ_contact_author_email MTW@SOTON.AC.UK _publ_section_title ; Iron Arsenate Frameworks ; _publ_section_references ; Allen, F.H., Kennard, O. & Taylor, R. (1983). Acc. Chem. Res. 16, 146-153. Altomare, A., Cascarano, G., Giacovazzo, C. & Guagliardi, A. (1993) J. Appl. Cryst. 26, 343-350. Altomare, A. Burla, M. C., Camalli, M., Cascarano, G. L., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G. & Spagna, R. (1999) J. Appl. Cryst. 32, 115-119. Blessing, R. H. (1995) Acta Cryst., A51, 33-38. Blessing, R. H. (1987) Cryst. Rev. 1, 3-58. Blessing, R. H. (1989) J. Appl. Cryst. 22, 396-397. Beurskens, P.T., Beurskens, G., de Gelder, R., Garci\'ia-Granda, S., Gould, R.O., Israel, R. & Smits, J.M.M. (1999) The DIRDIF-99 program system, Technical Report of the Crystallography Laboratory, University of Nijmegen, The Netherlands. Cremer, D. & Pople, J.A. (1975). J. Am. Chem. Soc. 97, 1354-1358. Enraf-Nonius (1994). CAD4Express Software. Enraf-Nonius, Delft, The Netherlands. Farrugia, L. J. (1997) ORTEP-3 for Windows, J. Appl. Cryst. 30, 565. Farrugia, L. J. (1999) WinGX, J. Appl. Cryst. 32, 837-838. Flack, H.D. (1983). Acta Cryst. A39, 876-881. Harms, K. & Wocadlo, S. (1995) XCAD-4. Program for Processing CAD-4 Diffractometer Data. University of Marburg, Germany. Johnson, C.K. (1965). ORTEP. Report ORNL-3794. Oak Ridge National Laboratory, Tennessee, USA. Lehman, M. S. and Larsen, F. K. (1974) Acta. Cryst. A30, 580 LePage, Y. (1987). J. Appl. Cryst. 20, 264-269. North, A. C. T., Phillips, D. C. & Mathews, F. S. (1968) Acta Cryst, A24, 351-359 Orpen, A. G., Brammer, L., Allen, F. H., Kennard, O., Watson, D. G., & Taylor, R. (1992). International Tables for Crystallography, Volume C. Sheldrick, G.M. (1993) SHELXL93. Program for crystal structure refinement. University of G\"ottingen, Germany. Sheldrick, G.M. (1997) SHELXL97. Program for crystal structure refinement. University of G\"ottingen, Germany. Sheldrick, G.M. (1985). SHELXS86. In Crystallographic Computing 3, edited by G. M. Sheldrick, C. Kruger & R. Goddard, pp. 175-189. Oxford University Press. Sheldrick, G.M. (1997) SHELXS97. Program for Crystal Structure solution. University of G\"ottingen, Germany. Spek, A.L. (1990). Acta Cryst. A46, C34 Streltsov, V. A. & Zavodnik, V. E. (1989) Sov. Phys. Crystallogr. 34, 824-828 Streltsov, V. A. & Zavodnik, V. E. (1990) Sov. Phys. Crystallogr. 35, 281. Walker, N. & Stuart, D. (1983). Acta Cryst., A39, 158 - 166. Wilson, A.J.C. (1992) Ed. International Tables for Crystallography, Volume C, Kluwer Academic Publishers, Dordrecht, The Netherlands. ; _publ_section_figure_captions ; Figure 1. View of (I) (50% probability displacement ellipsoids) ; _publ_section_acknowledgements ; ? ; _publ_section_table_legends ; Table 1. Fractional atomic coordinates and equivalent isotropic displacement parameters (\%A^2^) Table 2. Selected geometric parameters (\%A ,\% ) ; loop_ _publ_author_name 'M. Weller' 'Robert W. Hughes' 'Daniel J. Price' 'Seth B. Wiggin' #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_1 _database_code_depnum_ccdc_archive 'CCDC 639058' _audit_creation_date 2006-01-09T13:21:33-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #------------------ CHEMICAL INFORMATION ------------------------------------# _chemical_formula_moiety 'As2 Fe2 H4 O9' _chemical_formula_sum 'As2 Fe2 H4 O9' _chemical_formula_weight 409.57 #------------------ UNIT CELL INFORMATION -----------------------------------# _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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' _cell_length_a 6.6108(2) _cell_length_b 14.3741(5) _cell_length_c 7.6321(2) _cell_angle_alpha 90 _cell_angle_beta 95.830(2) _cell_angle_gamma 90 _cell_volume 721.48(4) _cell_measurement_reflns_used 3604 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) #------------------ CRYSTAL INFORMATION -------------------------------------# _exptl_crystal_description fragment _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 3.771 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 776 _exptl_absorpt_coefficient_mu 13.148 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SORTAV _exptl_absorpt_correction_T_min 0.0838 _exptl_absorpt_correction_T_max 0.2684 #------------------ DATA COLLECTION INFORMATION -----------------------------# _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_reflns_number 7380 _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius KappaCCD area-detector' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_av_R_equivalents 0.0856 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.997 _reflns_number_total 1648 _reflns_number_gt 1551 _reflns_threshold_expression >2sigma(I) #------------------ COMPUTER PROGRAMS USED ----------------------------------# _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) &COLLECT (Hooft, R.W.W., 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_molecular_graphics 'DIAMOND V2.1a (Brandenburg, K., 1999)' #------------------ REFINEMENT INFORMATION ----------------------------------# _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+0.1974P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.0154(10) _refine_ls_number_reflns 1648 _refine_ls_number_parameters 131 _refine_ls_number_restraints 6 _refine_ls_R_factor_gt 0.0326 _refine_ls_wR_factor_ref 0.0833 _refine_ls_goodness_of_fit_ref 1.08 _refine_ls_restrained_S_all 1.08 _refine_ls_shift/su_max 0 _refine_diff_density_max 1.312 _refine_diff_density_min -1.879 #------------------ ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS --------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source As As 0.0499 2.0058 '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' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_group _atom_site_disorder_assembly As1 As 0.23900(5) 0.08107(2) 0.35033(5) 0.00310(15) Uani 1 d . . . As2 As 0.43797(5) 0.18495(2) 0.06443(5) 0.00312(15) Uani 1 d . . . Fe1 Fe 0.73874(7) 0.11359(4) 0.41513(7) 0.00385(17) Uani 1 d . . . Fe2 Fe 0.45455(8) 0.24630(4) 0.64761(7) 0.00428(17) Uani 1 d . . . O1 O 0.4314(4) 0.12533(18) 0.4838(3) 0.0053(5) Uani 1 d . . . O2 O 0.1783(4) -0.02992(17) 0.3743(4) 0.0071(5) Uani 1 d . . . O1W O 0.7557(4) 0.00045(19) 0.2348(4) 0.0101(6) Uani 1 d D . . O3 O 0.0337(4) 0.14981(18) 0.3425(3) 0.0058(5) Uani 1 d . . . O2W O 0.4295(4) 0.3453(2) 0.4361(4) 0.0122(6) Uani 1 d D . . O4 O 0.3302(4) 0.08326(17) 0.1426(3) 0.0060(5) Uani 1 d . . . O5 O 0.2701(4) 0.26984(18) 0.0922(3) 0.0063(5) Uani 1 d . . . O6 O 0.6532(4) 0.20373(19) 0.1951(3) 0.0072(5) Uani 1 d . . . O7 O 0.4688(4) 0.15536(18) -0.1411(3) 0.0071(5) Uani 1 d . . . H1W H 0.867(4) -0.028(3) 0.243(6) 0.009 Uiso 1 d D . . H2W H 0.667(4) -0.038(2) 0.193(5) 0.009 Uiso 1 d D . . H3W H 0.340(6) 0.387(2) 0.448(6) 0.009 Uiso 1 d D . . H4W H 0.430(6) 0.325(3) 0.331(3) 0.009 Uiso 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 As1 0.0030(2) 0.0041(2) 0.0022(2) 0.00019(13) -0.00027(15) -0.00008(13) As2 0.0033(2) 0.0043(2) 0.0017(2) -0.00001(13) -0.00019(15) 0.00013(13) Fe1 0.0041(3) 0.0051(3) 0.0022(3) 0.00060(19) 0.0001(2) 0.00021(18) Fe2 0.0047(3) 0.0051(3) 0.0028(3) -0.00005(19) -0.0004(2) -0.00003(18) O1 0.0054(12) 0.0076(12) 0.0026(12) -0.0037(10) -0.0005(9) 0.0004(10) O2 0.0087(12) 0.0048(12) 0.0075(13) 0.0000(10) -0.0010(10) -0.0005(10) O1W 0.0078(13) 0.0072(13) 0.0149(15) -0.0056(12) -0.0004(11) 0.0009(11) O3 0.0041(11) 0.0066(13) 0.0066(13) 0.0023(10) 0.0003(10) 0.0008(10) O2W 0.0110(14) 0.0181(16) 0.0073(14) 0.0040(12) 0.0000(11) 0.0008(12) O4 0.0068(12) 0.0057(13) 0.0056(13) 0.0006(10) 0.0010(10) -0.0023(10) O5 0.0044(12) 0.0051(12) 0.0096(13) 0.0016(10) 0.0016(10) 0.0027(10) O6 0.0054(12) 0.0108(13) 0.0047(12) 0.0009(11) -0.0025(9) -0.0017(11) O7 0.0105(13) 0.0081(12) 0.0026(12) -0.0018(10) -0.0002(10) 0.0005(11) #------------------ MOLECULAR GEOMETRY --------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 As1 O2 1.660(3) . ? As1 O1 1.672(3) . ? As1 O3 1.675(2) . ? As1 O4 1.752(3) . ? As2 O7 1.657(2) . ? As2 O6 1.675(2) . ? As2 O5 1.677(2) . ? As2 O4 1.757(2) . ? Fe1 O2 2.037(3) 3_656 ? Fe1 O1W 2.141(3) . ? Fe1 O3 2.145(2) 1_655 ? Fe1 O5 2.149(3) 4_666 ? Fe1 O6 2.150(3) . ? Fe1 O1 2.156(3) . ? Fe2 O7 2.071(3) 1_556 ? Fe2 O3 2.135(3) 4_666 ? Fe2 O1 2.138(3) . ? Fe2 O2W 2.146(3) . ? Fe2 O6 2.182(2) 4_566 ? Fe2 O5 2.182(2) 4_666 ? O2 Fe1 2.037(3) 3_656 ? O1W H1W 0.837(19) . ? O1W H2W 0.840(19) . ? O3 Fe2 2.135(3) 4_565 ? O3 Fe1 2.145(2) 1_455 ? O2W H3W 0.851(19) . ? O2W H4W 0.852(19) . ? O5 Fe1 2.149(3) 4_565 ? O5 Fe2 2.182(2) 4_565 ? O6 Fe2 2.182(2) 4_665 ? O7 Fe2 2.071(3) 1_554 ? 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 O2 As1 O1 118.42(13) . . ? O2 As1 O3 111.53(12) . . ? O1 As1 O3 111.13(13) . . ? O2 As1 O4 103.07(12) . . ? O1 As1 O4 103.54(12) . . ? O3 As1 O4 108.00(12) . . ? O7 As2 O6 115.23(12) . . ? O7 As2 O5 116.93(13) . . ? O6 As2 O5 109.91(13) . . ? O7 As2 O4 101.60(13) . . ? O6 As2 O4 106.33(12) . . ? O5 As2 O4 105.42(12) . . ? O2 Fe1 O1W 91.79(11) 3_656 . ? O2 Fe1 O3 99.68(10) 3_656 1_655 ? O1W Fe1 O3 84.83(10) . 1_655 ? O2 Fe1 O5 87.89(10) 3_656 4_666 ? O1W Fe1 O5 171.27(10) . 4_666 ? O3 Fe1 O5 86.62(9) 1_655 4_666 ? O2 Fe1 O6 179.11(11) 3_656 . ? O1W Fe1 O6 89.00(11) . . ? O3 Fe1 O6 79.97(9) 1_655 . ? O5 Fe1 O6 91.27(10) 4_666 . ? O2 Fe1 O1 92.25(10) 3_656 . ? O1W Fe1 O1 109.15(10) . . ? O3 Fe1 O1 161.42(10) 1_655 . ? O5 Fe1 O1 79.58(9) 4_666 . ? O6 Fe1 O1 87.88(10) . . ? O7 Fe2 O3 84.85(10) 1_556 4_666 ? O7 Fe2 O1 86.38(10) 1_556 . ? O3 Fe2 O1 166.95(10) 4_666 . ? O7 Fe2 O2W 176.91(11) 1_556 . ? O3 Fe2 O2W 93.14(11) 4_666 . ? O1 Fe2 O2W 95.98(11) . . ? O7 Fe2 O6 92.78(10) 1_556 4_566 ? O3 Fe2 O6 79.47(10) 4_666 4_566 ? O1 Fe2 O6 110.63(10) . 4_566 ? O2W Fe2 O6 84.54(10) . 4_566 ? O7 Fe2 O5 96.60(10) 1_556 4_666 ? O3 Fe2 O5 92.17(9) 4_666 4_666 ? O1 Fe2 O5 79.25(10) . 4_666 ? O2W Fe2 O5 85.81(10) . 4_666 ? O6 Fe2 O5 166.85(10) 4_566 4_666 ? As1 O1 Fe2 132.11(14) . . ? As1 O1 Fe1 119.95(13) . . ? Fe2 O1 Fe1 101.09(11) . . ? As1 O2 Fe1 127.28(15) . 3_656 ? Fe1 O1W H1W 115(3) . . ? Fe1 O1W H2W 131(3) . . ? H1W O1W H2W 107(3) . . ? As1 O3 Fe2 125.30(13) . 4_565 ? As1 O3 Fe1 127.03(14) . 1_455 ? Fe2 O3 Fe1 100.65(10) 4_565 1_455 ? Fe2 O2W H3W 113(3) . . ? Fe2 O2W H4W 118(3) . . ? H3W O2W H4W 114(4) . . ? As1 O4 As2 120.72(14) . . ? As2 O5 Fe1 120.69(13) . 4_565 ? As2 O5 Fe2 127.22(14) . 4_565 ? Fe1 O5 Fe2 99.89(10) 4_565 4_565 ? As2 O6 Fe1 120.53(14) . . ? As2 O6 Fe2 133.53(14) . 4_665 ? Fe1 O6 Fe2 98.98(10) . 4_665 ? As2 O7 Fe2 125.08(15) . 1_554 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA O1W H1W O2 1_655 0.837(19) 2.20(3) 2.920(4) 145(4) O1W H2W O7 3_655 0.840(19) 1.94(2) 2.741(4) 160(4) O1W H2W O4 3_655 0.840(19) 2.65(4) 3.120(4) 117(3) O2W H3W O7 4_566 0.851(19) 2.55(4) 3.043(4) 118(4) O2W H4W O5 . 0.852(19) 2.16(3) 2.935(4) 151(4) O2W H4W O6 . 0.852(19) 2.57(3) 3.204(4) 132(3) #Diamino data_2 _database_code_depnum_ccdc_archive 'CCDC 639059' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H22 As8 Fe6 N2 O34' _chemical_formula_weight 1576.70 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' 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' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n 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' _cell_length_a 10.1348(1) _cell_length_b 10.8220(2) _cell_length_c 14.3264(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.158(3) _cell_angle_gamma 90.00 _cell_volume 1571.30(4) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 3787 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Rod _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.332 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1504 _exptl_absorpt_coefficient_mu 11.189 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1577 _exptl_absorpt_correction_T_max 0.6366 _exptl_absorpt_process_details ; SADABS V2.10 (Sheldrick, G.M., 2003) ; _exptl_special_details ; SADABS was used to perform the Absorption correction Parameter refinement on 30382 reflections reduced R(int) from 0.1097 to 0.0393 Ratio of minimum to maximum apparent transmission: 0.569603 The given Tmin and Tmax were generated using the SHELX SIZE command ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker Nonius FR591 Rotating Anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans to fill the asymmetric unit' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34093 _diffrn_reflns_av_R_equivalents 0.0406 _diffrn_reflns_av_sigmaI/netI 0.0243 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3589 _reflns_number_gt 3376 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CAMERON (Watkin, et al., 1993)' _computing_publication_material 'WINGX (Farrugia, 1998)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0118P)^2^+4.9366P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00082(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3589 _refine_ls_number_parameters 252 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0227 _refine_ls_R_factor_gt 0.0205 _refine_ls_wR_factor_ref 0.0490 _refine_ls_wR_factor_gt 0.0480 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.086 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 C1 C 0.6890(3) 1.0080(3) 0.4956(2) 0.0151(6) Uani 1 1 d . . . H1D H 0.7000 1.0969 0.5102 0.018 Uiso 1 1 calc R . . H1E H 0.7053 0.9603 0.5535 0.018 Uiso 1 1 calc R . . C2 C 0.5497(3) 0.9845(3) 0.4615(2) 0.0141(6) Uani 1 1 d . . . H2A H 0.5403 0.8967 0.4433 0.017 Uiso 1 1 calc R . . H2B H 0.5316 1.0360 0.4058 0.017 Uiso 1 1 calc R . . N1 N 0.7861(2) 0.9707(2) 0.42272(17) 0.0136(5) Uani 1 1 d . . . H1A H 0.7825 0.8875 0.4143 0.020 Uiso 1 1 calc R . . H1B H 0.8688 0.9926 0.4413 0.020 Uiso 1 1 calc R . . H1C H 0.7663 1.0094 0.3681 0.020 Uiso 1 1 calc R . . O1W O 0.4551(2) 0.5663(2) 0.08516(16) 0.0220(5) Uani 1 1 d D . . H1 H 0.413(4) 0.534(3) 0.133(2) 0.030 Uiso 1 1 d D . . H2 H 0.459(4) 0.6455(17) 0.091(3) 0.030 Uiso 1 1 d D . . O5 O -0.47103(18) 0.62986(18) 0.27973(13) 0.0074(4) Uani 1 1 d . . . O7 O -0.27819(18) 0.80521(17) 0.24063(13) 0.0072(4) Uani 1 1 d . . . O8 O -0.29438(18) 0.71502(17) 0.41489(13) 0.0064(4) Uani 1 1 d . . . O9 O -0.07669(18) 0.56764(17) 0.43721(13) 0.0058(4) Uani 1 1 d . . . O10 O 0.08262(18) 0.68864(17) 0.56707(13) 0.0063(4) Uani 1 1 d . . . O16 O 0.57772(18) 0.54942(17) 0.56968(13) 0.0059(4) Uani 1 1 d . . . O1 O 0.03320(18) 0.42616(18) 0.26584(13) 0.0078(4) Uani 1 1 d . . . O2 O 0.20232(19) 0.30926(17) 0.38821(13) 0.0066(4) Uani 1 1 d . . . O3 O 0.22111(18) 0.25968(18) 0.20243(13) 0.0073(4) Uani 1 1 d . . . O4 O 0.29965(18) 0.48380(18) 0.25680(13) 0.0069(4) Uani 1 1 d . . . O6 O -0.20665(18) 0.57194(17) 0.26070(13) 0.0062(4) Uani 1 1 d . . . O11 O 0.0539(2) 0.77803(18) 0.38876(14) 0.0106(4) Uani 1 1 d . . . H11 H -0.0113 0.8203 0.4057 0.016 Uiso 1 1 calc R . . O12 O 0.19124(18) 0.56242(17) 0.41614(13) 0.0054(4) Uani 1 1 d . . . O13 O 0.41696(18) 0.69980(17) 0.46096(13) 0.0065(4) Uani 1 1 d . . . O14 O 0.30770(18) 0.53879(17) 0.59083(13) 0.0055(4) Uani 1 1 d . . . O15 O 0.4510(2) 0.74092(19) 0.64865(14) 0.0112(4) Uani 1 1 d . . . H15 H 0.3768 0.7723 0.6594 0.017 Uiso 1 1 calc R . . Fe5 Fe 0.24987(4) 0.40704(3) 0.49300(3) 0.00418(9) Uani 1 1 d . . . Fe6 Fe 0.36517(4) 0.61077(3) 0.34399(3) 0.00475(9) Uani 1 1 d . . . Fe7 Fe -0.12963(4) 0.43143(4) 0.33085(3) 0.00463(9) Uani 1 1 d . . . As1 As 0.18761(3) 0.37262(2) 0.280261(18) 0.00451(7) Uani 1 1 d . . . As2 As -0.31634(3) 0.67625(2) 0.301050(18) 0.00438(7) Uani 1 1 d . . . As3 As 0.06421(3) 0.64881(2) 0.455591(19) 0.00473(7) Uani 1 1 d . . . As4 As 0.43606(3) 0.63225(2) 0.564090(19) 0.00469(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0163(15) 0.0151(15) 0.0140(15) -0.0042(12) -0.0023(12) 0.0010(12) C2 0.0149(15) 0.0109(14) 0.0164(15) -0.0019(12) -0.0016(12) -0.0016(12) N1 0.0158(13) 0.0109(12) 0.0140(13) -0.0004(10) -0.0018(10) 0.0006(10) O1W 0.0279(13) 0.0194(12) 0.0188(12) 0.0006(10) -0.0002(10) -0.0025(10) O5 0.0045(9) 0.0097(10) 0.0080(9) 0.0017(8) 0.0015(7) -0.0020(7) O7 0.0082(9) 0.0052(9) 0.0084(9) 0.0029(7) 0.0013(7) -0.0011(7) O8 0.0076(9) 0.0063(9) 0.0052(9) -0.0005(7) 0.0005(7) 0.0010(7) O9 0.0064(9) 0.0064(9) 0.0047(9) -0.0006(7) 0.0015(7) -0.0011(7) O10 0.0076(9) 0.0062(9) 0.0050(9) -0.0013(7) 0.0001(7) 0.0009(7) O16 0.0053(9) 0.0058(9) 0.0065(9) 0.0008(7) 0.0007(7) 0.0014(7) O1 0.0051(9) 0.0105(10) 0.0079(9) 0.0008(8) 0.0011(7) 0.0017(7) O2 0.0086(9) 0.0071(9) 0.0039(9) 0.0000(7) -0.0003(7) -0.0004(7) O3 0.0070(9) 0.0070(9) 0.0078(9) -0.0040(7) 0.0020(7) -0.0006(7) O4 0.0064(9) 0.0074(9) 0.0068(9) 0.0000(7) 0.0006(7) -0.0026(7) O6 0.0067(9) 0.0063(9) 0.0057(9) 0.0002(7) 0.0014(7) 0.0017(7) O11 0.0132(10) 0.0048(9) 0.0137(10) 0.0052(8) 0.0029(8) 0.0032(8) O12 0.0058(9) 0.0048(9) 0.0056(9) 0.0002(7) 0.0013(7) 0.0009(7) O13 0.0084(9) 0.0053(9) 0.0057(9) 0.0015(7) 0.0004(7) -0.0002(7) O14 0.0047(9) 0.0058(9) 0.0060(9) 0.0006(7) 0.0019(7) -0.0014(7) O15 0.0108(10) 0.0098(10) 0.0129(10) -0.0071(8) 0.0028(8) -0.0009(8) Fe5 0.00472(19) 0.00397(18) 0.00384(18) -0.00003(14) 0.00056(14) 0.00012(14) Fe6 0.00494(19) 0.00444(18) 0.00486(18) 0.00062(14) 0.00049(14) -0.00033(14) Fe7 0.00503(18) 0.00418(18) 0.00468(18) -0.00046(14) 0.00038(14) 0.00026(14) As1 0.00457(14) 0.00450(13) 0.00445(14) -0.00104(10) 0.00057(10) -0.00007(10) As2 0.00469(13) 0.00413(13) 0.00433(13) 0.00075(10) 0.00066(10) 0.00010(10) As3 0.00444(13) 0.00408(13) 0.00569(14) -0.00022(10) 0.00060(10) 0.00011(10) As4 0.00433(14) 0.00391(13) 0.00584(14) 0.00016(10) 0.00070(10) 0.00002(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 C1 N1 1.493(4) . ? C1 C2 1.514(4) . ? C1 H1D 0.9900 . ? C1 H1E 0.9900 . ? C2 C2 1.533(6) 3_676 ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? N1 H1A 0.9100 . ? N1 H1B 0.9100 . ? N1 H1C 0.9100 . ? O1W H1 0.889(18) . ? O1W H2 0.863(18) . ? O5 As2 1.6735(19) . ? O5 Fe6 1.9117(19) 1_455 ? O7 As2 1.6877(19) . ? O7 Fe7 1.9447(19) 2_455 ? O8 As2 1.6980(19) . ? O8 Fe5 1.9200(19) 3_566 ? O9 As3 1.6965(19) . ? O9 Fe5 2.0408(19) 3_566 ? O9 Fe7 2.1859(19) . ? O10 As3 1.6642(19) . ? O10 Fe7 2.0126(19) 3_566 ? O16 As4 1.6943(18) . ? O16 Fe5 2.0224(19) 3_666 ? O16 Fe6 2.2059(19) 3_666 ? O1 As1 1.6809(19) . ? O1 Fe7 1.8980(19) . ? O2 As1 1.6980(19) . ? O2 Fe5 1.8979(19) . ? O3 As1 1.6895(18) . ? O3 Fe6 1.9496(19) 2_545 ? O4 As1 1.6888(18) . ? O4 Fe6 1.9709(19) . ? O6 As2 1.6876(18) . ? O6 Fe7 1.9817(19) . ? O11 As3 1.6979(19) . ? O11 H11 0.8400 . ? O12 As3 1.6896(18) . ? O12 Fe5 2.0951(19) . ? O12 Fe6 2.1117(19) . ? O13 As4 1.6593(18) . ? O13 Fe6 2.0017(19) . ? O14 As4 1.6926(18) . ? O14 Fe5 2.0823(19) . ? O14 Fe7 2.1520(18) 3_566 ? O15 As4 1.6948(19) . ? O15 H15 0.8400 . ? Fe5 O8 1.9200(19) 3_566 ? Fe5 O16 2.0224(19) 3_666 ? Fe5 O9 2.0408(19) 3_566 ? Fe6 O5 1.9117(19) 1_655 ? Fe6 O3 1.9496(19) 2 ? Fe6 O16 2.2059(19) 3_666 ? Fe7 O7 1.9447(19) 2_445 ? Fe7 O10 2.0126(19) 3_566 ? Fe7 O14 2.1520(18) 3_566 ? 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 N1 C1 C2 110.2(2) . . ? N1 C1 H1D 109.6 . . ? C2 C1 H1D 109.6 . . ? N1 C1 H1E 109.6 . . ? C2 C1 H1E 109.6 . . ? H1D C1 H1E 108.1 . . ? C1 C2 C2 110.2(3) . 3_676 ? C1 C2 H2A 109.6 . . ? C2 C2 H2A 109.6 3_676 . ? C1 C2 H2B 109.6 . . ? C2 C2 H2B 109.6 3_676 . ? H2A C2 H2B 108.1 . . ? C1 N1 H1A 109.5 . . ? C1 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? C1 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? H1 O1W H2 110(3) . . ? As2 O5 Fe6 139.37(12) . 1_455 ? As2 O7 Fe7 137.78(11) . 2_455 ? As2 O8 Fe5 121.33(10) . 3_566 ? As3 O9 Fe5 125.39(10) . 3_566 ? As3 O9 Fe7 131.47(10) . . ? Fe5 O9 Fe7 102.84(8) 3_566 . ? As3 O10 Fe7 123.76(10) . 3_566 ? As4 O16 Fe5 126.07(10) . 3_666 ? As4 O16 Fe6 131.55(10) . 3_666 ? Fe5 O16 Fe6 101.91(8) 3_666 3_666 ? As1 O1 Fe7 139.51(12) . . ? As1 O2 Fe5 121.12(10) . . ? As1 O3 Fe6 137.09(11) . 2_545 ? As1 O4 Fe6 126.59(11) . . ? As2 O6 Fe7 126.76(10) . . ? As3 O11 H11 109.5 . . ? As3 O12 Fe5 118.91(10) . . ? As3 O12 Fe6 131.64(10) . . ? Fe5 O12 Fe6 102.72(8) . . ? As4 O13 Fe6 124.27(11) . . ? As4 O14 Fe5 118.16(10) . . ? As4 O14 Fe7 132.43(10) . 3_566 ? Fe5 O14 Fe7 102.63(8) . 3_566 ? As4 O15 H15 109.5 . . ? O2 Fe5 O8 102.63(8) . 3_566 ? O2 Fe5 O16 89.80(8) . 3_666 ? O8 Fe5 O16 105.30(8) 3_566 3_666 ? O2 Fe5 O9 104.21(8) . 3_566 ? O8 Fe5 O9 87.50(8) 3_566 3_566 ? O16 Fe5 O9 158.67(8) 3_666 3_566 ? O2 Fe5 O14 169.92(8) . . ? O8 Fe5 O14 86.75(8) 3_566 . ? O16 Fe5 O14 84.11(7) 3_666 . ? O9 Fe5 O14 79.58(7) 3_566 . ? O2 Fe5 O12 87.75(8) . . ? O8 Fe5 O12 168.28(8) 3_566 . ? O16 Fe5 O12 79.85(7) 3_666 . ? O9 Fe5 O12 84.65(7) 3_566 . ? O14 Fe5 O12 83.29(7) . . ? O5 Fe6 O3 97.79(8) 1_655 2 ? O5 Fe6 O4 93.53(8) 1_655 . ? O3 Fe6 O4 102.13(8) 2 . ? O5 Fe6 O13 97.18(8) 1_655 . ? O3 Fe6 O13 90.23(8) 2 . ? O4 Fe6 O13 162.40(8) . . ? O5 Fe6 O12 171.75(8) 1_655 . ? O3 Fe6 O12 89.86(7) 2 . ? O4 Fe6 O12 81.79(7) . . ? O13 Fe6 O12 85.81(7) . . ? O5 Fe6 O16 97.36(8) 1_655 3_666 ? O3 Fe6 O16 163.26(7) 2 3_666 ? O4 Fe6 O16 83.97(8) . 3_666 ? O13 Fe6 O16 80.86(7) . 3_666 ? O12 Fe6 O16 75.46(7) . 3_666 ? O1 Fe7 O7 97.91(8) . 2_445 ? O1 Fe7 O6 96.66(8) . . ? O7 Fe7 O6 94.81(8) 2_445 . ? O1 Fe7 O10 97.63(8) . 3_566 ? O7 Fe7 O10 92.38(8) 2_445 3_566 ? O6 Fe7 O10 162.95(8) . 3_566 ? O1 Fe7 O14 172.70(8) . 3_566 ? O7 Fe7 O14 88.71(8) 2_445 3_566 ? O6 Fe7 O14 79.62(7) . 3_566 ? O10 Fe7 O14 85.12(7) 3_566 3_566 ? O1 Fe7 O9 98.64(8) . . ? O7 Fe7 O9 163.21(8) 2_445 . ? O6 Fe7 O9 86.08(7) . . ? O10 Fe7 O9 82.63(7) 3_566 . ? O14 Fe7 O9 74.94(7) 3_566 . ? O1 As1 O4 110.87(9) . . ? O1 As1 O3 110.91(9) . . ? O4 As1 O3 104.34(9) . . ? O1 As1 O2 109.30(9) . . ? O4 As1 O2 114.30(9) . . ? O3 As1 O2 106.96(9) . . ? O5 As2 O6 110.76(9) . . ? O5 As2 O7 111.73(9) . . ? O6 As2 O7 103.03(9) . . ? O5 As2 O8 111.69(9) . . ? O6 As2 O8 114.18(9) . . ? O7 As2 O8 104.99(9) . . ? O10 As3 O12 112.39(9) . . ? O10 As3 O9 112.03(9) . . ? O12 As3 O9 107.66(9) . . ? O10 As3 O11 109.53(10) . . ? O12 As3 O11 108.24(9) . . ? O9 As3 O11 106.76(10) . . ? O13 As4 O14 112.14(9) . . ? O13 As4 O16 111.83(9) . . ? O14 As4 O16 108.96(9) . . ? O13 As4 O15 109.92(10) . . ? O14 As4 O15 108.67(9) . . ? O16 As4 O15 105.03(10) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A O8 0.91 2.02 2.887(3) 158.3 1_655 N1 H1B O1W 0.91 1.99 2.822(4) 150.8 2_655 N1 H1B O1W 0.91 2.33 2.913(4) 122.1 4_676 N1 H1C O6 0.91 2.05 2.957(3) 171.1 2 O1W H2 O2 0.863(18) 2.43(3) 3.100(3) 135(3) 2 O1W H1 O4 0.889(18) 2.18(2) 3.057(3) 171(3) . O1W H2 O10 0.863(18) 2.22(2) 2.962(3) 145(3) 4_675 O11 H11 N1 0.84 2.63 3.458(3) 168.0 1_455 O15 H15 O7 0.84 2.13 2.720(3) 127.1 4_676 O15 H15 O6 0.84 2.38 3.041(3) 135.9 4_676 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.880 _refine_diff_density_min -0.927 _refine_diff_density_rms 0.119 _audit_creation_date 2006-07-13T13:26:20-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #Pip1 data_3 _database_code_depnum_ccdc_archive 'CCDC 639060' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H12 As6 Fe4 N2 O22' _chemical_formula_weight 1113.08 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' As As 0.0499 2.0058 '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' N N 0.0061 0.0033 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.7503(2) _cell_length_b 7.7757(3) _cell_length_c 11.2924(3) _cell_angle_alpha 72.396(2) _cell_angle_beta 80.801(2) _cell_angle_gamma 79.085(2) _cell_volume 551.40(3) _cell_formula_units_Z 1 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 7194 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.352 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 528 _exptl_absorpt_coefficient_mu 11.623 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2046 _exptl_absorpt_correction_T_max 0.8926 _exptl_absorpt_process_details ; SADABS V2.10 (Sheldrick, G.M., 2003) ; _exptl_special_details ; SADABS was used to perform the Absorption correction Parameter refinement on 30382 reflections reduced R(int) from 0.1097 to 0.0393 Ratio of minimum to maximum apparent transmission: 0.569603 The given Tmin and Tmax were generated using the SHELX SIZE command ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker Nonius FR591 Rotating Anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans to fill the asymmetric unit' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11483 _diffrn_reflns_av_R_equivalents 0.0644 _diffrn_reflns_av_sigmaI/netI 0.0414 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 27.46 _reflns_number_total 2516 _reflns_number_gt 2245 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CAMERON (Watkin, et al., 1993)' _computing_publication_material 'WINGX (Farrugia, 1998)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0196P)^2^+3.8020P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0063(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2516 _refine_ls_number_parameters 169 _refine_ls_number_restraints 60 _refine_ls_R_factor_all 0.0366 _refine_ls_R_factor_gt 0.0308 _refine_ls_wR_factor_ref 0.0726 _refine_ls_wR_factor_gt 0.0702 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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 C1 C -0.1819(8) 0.0991(7) 0.0498(4) 0.0120(7) Uani 1 1 d U . . H1A H -0.3038 0.1934 0.0366 0.040 Uiso 1 1 d R . . H1B H -0.1803 0.0423 0.1410 0.040 Uiso 1 1 d R . . C2 C 0.1939(7) 0.0444(7) 0.0113(4) 0.0120(7) Uani 1 1 d U . . H2A H 0.3187 0.0997 -0.0246 0.018(15) Uiso 1 1 d R . . H2B H 0.2030 -0.0139 0.1019 0.005(12) Uiso 1 1 d R . . As1 As 0.14128(7) 0.11140(6) 0.35074(4) 0.00638(13) Uani 1 1 d U . . As2 As 0.49029(7) 0.53450(6) 0.20804(4) 0.00700(13) Uani 1 1 d U . . As3 As 0.34220(7) 0.26805(6) 0.62588(4) 0.00554(12) Uani 1 1 d U . . Fe4 Fe 0.63718(10) 0.13614(9) 0.40193(6) 0.00717(15) Uani 1 1 d . . . Fe5 Fe 0.14988(10) -0.33035(9) 0.43255(6) 0.00640(15) Uani 1 1 d . . . N1 N 0.0035(8) 0.1874(7) -0.0037(5) 0.0319(12) Uani 1 1 d U . . H1C H 0.0119 0.2704 0.0382 0.060 Uiso 1 1 d R . . H1D H -0.0013 0.2483 -0.0872 0.060 Uiso 1 1 d R . . O1 O 0.1700(5) 0.2846(4) 0.2147(3) 0.0100(7) Uani 1 1 d . . . O2 O 0.3310(5) 0.0953(4) 0.4379(3) 0.0073(6) Uani 1 1 d . . . O3 O 0.1469(5) -0.0740(4) 0.3063(3) 0.0098(7) Uani 1 1 d U . . O4 O -0.0814(5) 0.1803(4) 0.4271(3) 0.0094(7) Uani 1 1 d U . . O5 O 0.1424(5) 0.4108(4) 0.5679(3) 0.0085(6) Uani 1 1 d U . . O6 O 0.5547(5) 0.2968(4) 0.5257(3) 0.0072(6) Uani 1 1 d U . . O7 O 0.3727(5) 0.3181(5) 0.7620(3) 0.0096(7) Uani 1 1 d . . . O8 O 0.2997(5) 0.0538(4) 0.6914(3) 0.0096(7) Uani 1 1 d U . . O9 O 0.6252(5) 0.3283(5) 0.2390(3) 0.0138(7) Uani 1 1 d U . . O10 O 0.4854(5) 0.6209(5) 0.0522(3) 0.0154(7) Uani 1 1 d U . . O11 O 0.2579(5) 0.5555(4) 0.2823(3) 0.0095(7) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0178(17) 0.0151(18) 0.0052(15) -0.0036(13) -0.0025(13) -0.0056(14) C2 0.0178(17) 0.0151(18) 0.0052(15) -0.0036(13) -0.0025(13) -0.0056(14) As1 0.0066(2) 0.0067(2) 0.0059(2) -0.00191(17) -0.00161(17) -0.00023(17) As2 0.0084(2) 0.0072(2) 0.0061(2) -0.00218(17) -0.00190(17) -0.00128(17) As3 0.0057(2) 0.0050(2) 0.0063(2) -0.00164(17) -0.00194(16) -0.00072(16) Fe4 0.0076(3) 0.0064(3) 0.0086(3) -0.0031(2) -0.0031(2) -0.0002(2) Fe5 0.0074(3) 0.0058(3) 0.0065(3) -0.0018(2) -0.0011(2) -0.0018(2) N1 0.044(3) 0.025(3) 0.028(3) -0.003(2) -0.007(2) -0.014(2) O1 0.0125(16) 0.0105(17) 0.0053(15) 0.0017(12) -0.0021(12) -0.0029(13) O2 0.0069(15) 0.0068(16) 0.0077(15) -0.0009(12) -0.0026(12) -0.0002(12) O3 0.0142(16) 0.0072(16) 0.0093(16) -0.0040(13) -0.0012(13) -0.0022(13) O4 0.0083(15) 0.0099(17) 0.0094(16) -0.0023(13) -0.0009(12) -0.0003(13) O5 0.0054(15) 0.0070(16) 0.0112(16) 0.0005(13) -0.0029(12) 0.0002(12) O6 0.0046(14) 0.0086(16) 0.0080(15) -0.0023(12) -0.0017(12) 0.0008(12) O7 0.0117(16) 0.0127(17) 0.0072(15) -0.0052(13) 0.0004(12) -0.0062(13) O8 0.0120(16) 0.0077(16) 0.0095(16) -0.0016(13) -0.0010(13) -0.0042(13) O9 0.0135(17) 0.0099(17) 0.0192(18) -0.0054(14) -0.0070(14) 0.0019(14) O10 0.0173(18) 0.021(2) 0.0076(16) -0.0015(14) -0.0029(14) -0.0048(15) O11 0.0097(16) 0.0103(17) 0.0096(16) -0.0037(13) -0.0001(13) -0.0032(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 C1 N1 1.495(7) . ? C1 C2 1.498(7) 2 ? C1 H1A 0.9911 . ? C1 H1B 0.9917 . ? C2 C1 1.498(7) 2 ? C2 N1 1.527(7) . ? C2 H2A 0.9915 . ? C2 H2B 0.9916 . ? As1 O3 1.656(3) . ? As1 O4 1.688(3) . ? As1 O2 1.701(3) . ? As1 O1 1.722(3) . ? As2 O9 1.653(3) . ? As2 O11 1.660(3) . ? As2 O10 1.686(3) . ? As2 O7 1.738(3) 2_666 ? As3 O5 1.660(3) . ? As3 O8 1.665(3) . ? As3 O6 1.685(3) . ? As3 O7 1.746(3) . ? Fe4 O9 1.991(4) . ? Fe4 O8 2.009(3) 2_656 ? Fe4 O4 2.070(3) 1_655 ? Fe4 O6 2.090(3) . ? Fe4 O2 2.107(3) . ? Fe4 O2 2.137(3) 2_656 ? Fe5 O3 2.069(3) . ? Fe5 O11 2.114(3) 1_545 ? Fe5 O5 2.131(3) 1_545 ? Fe5 O5 2.181(3) 2_556 ? Fe5 O4 2.184(3) 2_556 ? Fe5 O6 2.200(3) 2_656 ? N1 H1C 0.9219 . ? N1 H1D 0.9215 . ? O2 Fe4 2.137(3) 2_656 ? O4 Fe4 2.070(3) 1_455 ? O4 Fe5 2.184(3) 2_556 ? O5 Fe5 2.131(3) 1_565 ? O5 Fe5 2.181(3) 2_556 ? O6 Fe5 2.200(3) 2_656 ? O7 As2 1.738(3) 2_666 ? O8 Fe4 2.009(3) 2_656 ? O11 Fe5 2.114(3) 1_565 ? 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 N1 C1 C2 110.8(4) . 2 ? N1 C1 H1A 109.1 . . ? C2 C1 H1A 109.6 2 . ? N1 C1 H1B 110.3 . . ? C2 C1 H1B 109.1 2 . ? H1A C1 H1B 108.0 . . ? C1 C2 N1 110.4(4) 2 . ? C1 C2 H2A 109.4 2 . ? N1 C2 H2A 111.7 . . ? C1 C2 H2B 108.9 2 . ? N1 C2 H2B 108.4 . . ? H2A C2 H2B 107.9 . . ? O3 As1 O4 114.94(16) . . ? O3 As1 O2 113.47(16) . . ? O4 As1 O2 108.51(15) . . ? O3 As1 O1 105.60(16) . . ? O4 As1 O1 105.16(16) . . ? O2 As1 O1 108.63(15) . . ? O9 As2 O11 117.05(17) . . ? O9 As2 O10 109.51(18) . . ? O11 As2 O10 110.80(17) . . ? O9 As2 O7 108.30(16) . 2_666 ? O11 As2 O7 109.13(16) . 2_666 ? O10 As2 O7 100.79(16) . 2_666 ? O5 As3 O8 114.21(16) . . ? O5 As3 O6 111.65(15) . . ? O8 As3 O6 116.33(16) . . ? O5 As3 O7 106.47(16) . . ? O8 As3 O7 97.70(15) . . ? O6 As3 O7 108.96(15) . . ? O9 Fe4 O8 88.93(14) . 2_656 ? O9 Fe4 O4 93.56(13) . 1_655 ? O8 Fe4 O4 104.45(13) 2_656 1_655 ? O9 Fe4 O6 100.44(13) . . ? O8 Fe4 O6 169.91(13) 2_656 . ? O4 Fe4 O6 78.90(12) 1_655 . ? O9 Fe4 O2 99.21(13) . . ? O8 Fe4 O2 89.88(13) 2_656 . ? O4 Fe4 O2 161.00(13) 1_655 . ? O6 Fe4 O2 84.96(12) . . ? O9 Fe4 O2 172.16(14) . 2_656 ? O8 Fe4 O2 83.45(13) 2_656 2_656 ? O4 Fe4 O2 86.59(12) 1_655 2_656 ? O6 Fe4 O2 87.29(12) . 2_656 ? O2 Fe4 O2 82.66(13) . 2_656 ? O3 Fe5 O11 88.54(13) . 1_545 ? O3 Fe5 O5 177.39(13) . 1_545 ? O11 Fe5 O5 93.81(13) 1_545 1_545 ? O3 Fe5 O5 105.78(13) . 2_556 ? O11 Fe5 O5 87.17(12) 1_545 2_556 ? O5 Fe5 O5 73.23(13) 1_545 2_556 ? O3 Fe5 O4 84.28(12) . 2_556 ? O11 Fe5 O4 169.43(12) 1_545 2_556 ? O5 Fe5 O4 93.55(12) 1_545 2_556 ? O5 Fe5 O4 102.22(12) 2_556 2_556 ? O3 Fe5 O6 86.52(12) . 2_656 ? O11 Fe5 O6 97.71(12) 1_545 2_656 ? O5 Fe5 O6 94.29(12) 1_545 2_656 ? O5 Fe5 O6 166.94(12) 2_556 2_656 ? O4 Fe5 O6 74.17(12) 2_556 2_656 ? C1 N1 C2 110.3(4) . . ? C1 N1 H1C 109.4 . . ? C2 N1 H1C 108.5 . . ? C1 N1 H1D 111.0 . . ? C2 N1 H1D 109.1 . . ? H1C N1 H1D 108.4 . . ? As1 O2 Fe4 136.22(17) . . ? As1 O2 Fe4 116.82(16) . 2_656 ? Fe4 O2 Fe4 97.34(13) . 2_656 ? As1 O3 Fe5 122.26(17) . . ? As1 O4 Fe4 124.98(18) . 1_455 ? As1 O4 Fe5 131.11(17) . 2_556 ? Fe4 O4 Fe5 103.91(13) 1_455 2_556 ? As3 O5 Fe5 125.93(17) . 1_565 ? As3 O5 Fe5 124.37(17) . 2_556 ? Fe5 O5 Fe5 106.77(13) 1_565 2_556 ? As3 O6 Fe4 118.81(17) . . ? As3 O6 Fe5 127.01(17) . 2_656 ? Fe4 O6 Fe5 102.71(13) . 2_656 ? As2 O7 As3 133.30(19) 2_666 . ? As3 O8 Fe4 122.62(17) . 2_656 ? As2 O9 Fe4 128.6(2) . . ? As2 O11 Fe5 129.04(18) . 1_565 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1C O1 0.92 2.45 3.202(6) 139.3 . _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.171 _refine_diff_density_min -1.017 _refine_diff_density_rms 0.191 #Pip2 data_4 _database_code_depnum_ccdc_archive 'CCDC 639061' _audit_creation_date 2006-01-11T16:09:14-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #------------------ CHEMICAL INFORMATION ------------------------------------# _chemical_formula_moiety 'As5 Fe5 H6 O24, C4 H12 N2, 2(H2 O)' _chemical_formula_sum 'C4 H22 As5 Fe5 N2 O26' _chemical_formula_weight 1168.09 #------------------ UNIT CELL INFORMATION -----------------------------------# _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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' _cell_length_a 6.6375(18) _cell_length_b 22.195(6) _cell_length_c 17.312(6) _cell_angle_alpha 90 _cell_angle_beta 94.14(2) _cell_angle_gamma 90 _cell_volume 2543.7(13) _cell_measurement_reflns_used 5504 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) #------------------ CRYSTAL INFORMATION -------------------------------------# _exptl_crystal_description fragment _exptl_crystal_colour green _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 3.05 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2252 _exptl_absorpt_coefficient_mu 9.355 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, 2003)' _exptl_absorpt_correction_T_min 0.6037 _exptl_absorpt_correction_T_max 0.8350 _exptl_special_details ; SADABS was used to perform the Absorption correction Parameter refinement on 17401 reflections reduced R(int) from 0.1425 to 0.0619 Ratio of minimum to maximum apparent transmission: 0.697285 The given Tmin and Tmax were generated using the SHELX SIZE command ; #------------------ DATA COLLECTION INFORMATION -----------------------------# _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_reflns_number 29453 _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius KappaCCD area-detector' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_av_R_equivalents 0.0781 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 27.53 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measured_fraction_theta_full 0.992 _reflns_number_total 5819 _reflns_number_gt 4008 _reflns_threshold_expression >2sigma(I) #------------------ COMPUTER PROGRAMS USED ----------------------------------# _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) &COLLECT (Hooft, R.W.W., 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_molecular_graphics 'DIAMOND V2.1a (Brandenburg, K., 1999)' #------------------ REFINEMENT INFORMATION ----------------------------------# _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0463P)^2^+28.8788P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 5819 _refine_ls_number_parameters 397 _refine_ls_number_restraints 9 _refine_ls_R_factor_gt 0.0541 _refine_ls_wR_factor_ref 0.1317 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.001 _refine_diff_density_max 2.093 _refine_diff_density_min -1.33 #------------------ ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS --------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source As As 0.0499 2.0058 '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' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 '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' 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_group _atom_site_disorder_assembly As1 As -0.36673(12) 0.32703(4) 0.44437(4) 0.01253(19) Uani 1 d . . . As2 As 0.04801(12) 0.26027(4) 0.29074(4) 0.01052(19) Uani 1 d . . . As3 As 0.36433(12) 0.16971(4) 0.45980(4) 0.01108(19) Uani 1 d . . . As4 As 0.45223(12) 0.26337(4) 0.11394(4) 0.01048(19) Uani 1 d . . . As5 As 0.75029(12) 0.11769(4) 0.19979(5) 0.01121(18) Uani 1 d . . . Fe1 Fe 0.25042(15) 0.14511(5) 0.19929(6) 0.0055(2) Uani 1 d . . . Fe2 Fe 0.13958(16) 0.30403(6) 0.46307(6) 0.0114(3) Uani 1 d . . . Fe3 Fe -0.14508(16) 0.19048(5) 0.44327(6) 0.0103(2) Uani 1 d . . . Fe4 Fe 0.95160(17) 0.23868(5) 0.10586(6) 0.0110(3) Uani 1 d . . . Fe5 Fe 0.54934(16) 0.23615(5) 0.29726(6) 0.0109(3) Uani 1 d . . . O1 O -0.4413(8) 0.3146(3) 0.3508(3) 0.0142(12) Uani 1 d . . . O2 O -0.3163(10) 0.3982(3) 0.4637(3) 0.0252(15) Uani 1 d . . . O1W O 0.3764(12) 0.4603(4) 0.3800(5) 0.046(2) Uani 1 d D . . O3 O -0.1573(8) 0.2841(3) 0.4661(3) 0.0142(12) Uani 1 d . . . O2W O 0.7052(12) 0.0315(4) 0.5608(4) 0.0368(18) Uani 1 d D . . O4 O -0.5589(8) 0.3029(3) 0.4980(3) 0.0140(12) Uani 1 d . . . O5 O 0.1060(9) 0.3180(3) 0.3509(3) 0.0162(12) Uani 1 d . . . O6 O -0.1491(8) 0.2198(3) 0.3210(3) 0.0117(12) Uani 1 d . . . O7 O 0.2497(8) 0.2141(3) 0.2843(3) 0.0118(11) Uani 1 d . . . O8 O -0.0226(8) 0.2879(3) 0.2018(3) 0.0136(12) Uani 1 d . . . O9 O 0.1591(8) 0.2143(3) 0.4388(3) 0.0127(12) Uani 1 d . . . O10 O 0.5536(8) 0.1903(3) 0.4040(3) 0.0149(12) Uani 1 d . . . O11 O 0.4426(8) 0.1823(3) 0.5528(3) 0.0147(12) Uani 1 d . . . O12 O 0.2981(8) 0.0982(3) 0.4419(3) 0.0165(13) Uani 1 d . . . O13 O 0.5274(8) 0.2853(3) 0.2040(3) 0.0148(12) Uani 1 d . . . O14 O 0.2467(7) 0.2172(3) 0.1177(3) 0.0099(11) Uani 1 d . . . O15 O 0.4019(8) 0.3232(3) 0.0578(3) 0.0141(12) Uani 1 d . . . O16 O 0.6492(7) 0.2221(3) 0.0809(3) 0.0106(11) Uani 1 d . . . O17 O 0.5563(8) 0.1601(3) 0.2295(3) 0.0143(12) Uani 1 d . . . O18 O 0.9422(8) 0.1614(3) 0.1713(3) 0.0144(12) Uani 1 d . . . O19 O 0.8427(9) 0.0732(3) 0.2734(3) 0.0162(12) Uani 1 d . . . H19 H 0.8455 0.0925 0.3152 0.024 Uiso 1 calc RD . . O20 O 0.6650(8) 0.0727(3) 0.1273(3) 0.0129(12) Uani 1 d . . . H20 H 0.5388 0.0758 0.1207 0.019 Uiso 1 calc R . . O21 O -0.1135(9) 0.0973(3) 0.4237(3) 0.0218(14) Uani 1 d . . . H21 H 0.0091 0.0878 0.4297 0.033 Uiso 1 calc R . . O22 O 0.1174(9) 0.3925(3) 0.4834(3) 0.0230(14) Uani 1 d . . . H22 H 0.2037 0.4025 0.519 0.035 Uiso 1 calc RD . . O23 O 0.2392(9) 0.0763(3) 0.2829(3) 0.0173(13) Uani 1 d . . . H23 H 0.2754 0.0903 0.3268 0.026 Uiso 1 calc RD . . O24 O 0.2687(9) 0.0778(3) 0.1149(3) 0.0161(12) Uani 1 d . . . H24 H 0.2203 0.0909 0.072 0.024 Uiso 1 calc RD . . C1 C 0.5919(16) 0.4268(5) 0.1956(6) 0.034(2) Uani 1 d . . . H1C H 0.4604 0.4446 0.1771 0.041 Uiso 1 calc R . . H1D H 0.5715 0.3833 0.2049 0.041 Uiso 1 calc R . . C2 C 0.7426(15) 0.4353(5) 0.1354(5) 0.030(2) Uani 1 d . . . H2C H 0.7515 0.4787 0.1225 0.036 Uiso 1 calc R . . H2D H 0.6956 0.4135 0.0876 0.036 Uiso 1 calc R . . C3 C 0.8675(15) 0.4313(4) 0.2983(6) 0.028(2) Uani 1 d . . . H3A H 0.8526 0.3878 0.3092 0.033 Uiso 1 calc R . . H3B H 0.9138 0.4516 0.3473 0.033 Uiso 1 calc R . . C4 C 1.0218(15) 0.4400(4) 0.2396(5) 0.025(2) Uani 1 d . . . H4A H 1.0464 0.4836 0.2325 0.03 Uiso 1 calc R . . H4B H 1.1509 0.421 0.2586 0.03 Uiso 1 calc R . . N1 N 0.9490(13) 0.4126(4) 0.1637(4) 0.0297(19) Uani 1 d . . . H1A H 0.9442 0.3714 0.1691 0.036 Uiso 1 calc R . . H1B H 1.0393 0.4213 0.1275 0.036 Uiso 1 calc R . . N2 N 0.6691(11) 0.4566(4) 0.2686(5) 0.0263(18) Uani 1 d . . . H2A H 0.5771 0.4517 0.3054 0.032 Uiso 1 calc RD . . H2B H 0.6829 0.4973 0.2599 0.032 Uiso 1 calc R . . H1W H 0.352(16) 0.4971(14) 0.378(5) 0.039 Uiso 1 d D . . H2W H 0.445(7) 0.446(4) 0.4180(17) 0.039 Uiso 1 d D . . H3W H 0.630(14) 0.001(3) 0.556(5) 0.039 Uiso 1 d D . . H4W H 0.751(15) 0.043(4) 0.519(3) 0.039 Uiso 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 As1 0.0096(4) 0.0158(5) 0.0122(4) 0.0016(3) 0.0007(3) 0.0001(3) As2 0.0081(4) 0.0131(5) 0.0103(4) -0.0001(3) 0.0002(3) 0.0007(3) As3 0.0095(4) 0.0130(4) 0.0107(4) -0.0003(3) 0.0006(3) 0.0004(3) As4 0.0082(4) 0.0134(5) 0.0098(4) 0.0003(3) 0.0007(3) 0.0001(3) As5 0.0098(4) 0.0112(4) 0.0126(4) 0.0002(3) 0.0007(3) 0.0001(3) Fe1 0.0030(4) 0.0058(5) 0.0075(5) 0.0004(4) -0.0001(4) -0.0001(4) Fe2 0.0073(5) 0.0185(7) 0.0083(5) -0.0016(5) -0.0003(4) 0.0022(5) Fe3 0.0068(5) 0.0155(6) 0.0084(5) -0.0014(4) -0.0005(4) 0.0016(5) Fe4 0.0107(6) 0.0124(6) 0.0098(5) 0.0001(4) 0.0003(4) 0.0001(5) Fe5 0.0073(5) 0.0146(7) 0.0107(5) 0.0006(4) -0.0001(4) -0.0003(5) O1 0.019(3) 0.012(3) 0.011(3) -0.002(2) 0.001(2) 0.000(2) O2 0.038(4) 0.017(4) 0.020(3) 0.000(3) 0.000(3) 0.000(3) O1W 0.039(5) 0.022(4) 0.077(6) 0.000(4) 0.003(4) 0.010(4) O3 0.014(3) 0.015(3) 0.013(3) 0.000(2) -0.001(2) 0.004(2) O2W 0.046(5) 0.037(5) 0.029(4) -0.001(3) 0.012(3) 0.000(4) O4 0.011(3) 0.019(3) 0.013(3) 0.000(2) 0.002(2) 0.001(2) O5 0.018(3) 0.014(3) 0.016(3) -0.003(2) 0.000(2) 0.001(2) O6 0.012(3) 0.011(3) 0.012(3) -0.001(2) -0.001(2) 0.001(2) O7 0.006(2) 0.012(3) 0.017(3) -0.001(2) -0.001(2) 0.004(2) O8 0.009(3) 0.014(3) 0.018(3) -0.002(2) 0.000(2) -0.001(2) O9 0.008(3) 0.016(3) 0.014(3) -0.001(2) 0.000(2) -0.003(2) O10 0.016(3) 0.019(3) 0.011(3) 0.005(2) 0.004(2) 0.003(2) O11 0.016(3) 0.015(3) 0.012(3) 0.004(2) -0.006(2) -0.001(2) O12 0.016(3) 0.012(3) 0.020(3) 0.004(2) -0.003(2) -0.002(2) O13 0.018(3) 0.021(3) 0.005(2) -0.003(2) 0.000(2) -0.003(3) O14 0.003(2) 0.016(3) 0.011(3) 0.002(2) -0.002(2) 0.002(2) O15 0.012(3) 0.014(3) 0.016(3) 0.007(2) -0.001(2) 0.003(2) O16 0.003(2) 0.016(3) 0.013(3) 0.003(2) -0.001(2) 0.000(2) O17 0.010(3) 0.019(3) 0.014(3) -0.003(2) 0.001(2) 0.000(2) O18 0.013(3) 0.012(3) 0.018(3) 0.001(2) 0.003(2) -0.002(2) O19 0.019(3) 0.017(3) 0.013(3) 0.001(2) -0.002(2) 0.003(3) O20 0.012(3) 0.015(3) 0.012(3) -0.003(2) 0.002(2) 0.000(2) O21 0.014(3) 0.027(4) 0.025(3) -0.001(3) 0.008(3) 0.006(3) O22 0.026(3) 0.030(4) 0.013(3) -0.004(3) 0.002(3) -0.006(3) O23 0.020(3) 0.012(3) 0.019(3) 0.002(2) 0.003(3) 0.005(3) O24 0.019(3) 0.009(3) 0.020(3) -0.006(2) -0.005(3) 0.000(2) C1 0.032(6) 0.026(6) 0.043(6) -0.010(5) 0.002(5) 0.000(5) C2 0.031(5) 0.033(6) 0.025(5) -0.009(4) -0.005(4) 0.011(5) C3 0.035(6) 0.013(5) 0.036(5) 0.004(4) 0.008(4) -0.001(4) C4 0.035(5) 0.012(5) 0.029(5) -0.002(4) 0.008(4) 0.002(4) N1 0.039(5) 0.026(5) 0.025(4) -0.003(4) 0.003(4) 0.000(4) N2 0.023(4) 0.020(4) 0.037(4) 0.001(4) 0.012(4) 0.007(3) #------------------ MOLECULAR GEOMETRY --------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 # O1 Fe5 1.972(6) 1_455 ? # O4 Fe2 2.049(5) 1_455 ? # O4 Fe4 2.079(5) 4_466 ? # O6 Fe5 2.047(5) 1_455 ? # O8 Fe4 1.986(6) 1_455 ? # O10 Fe3 2.066(6) 1_655 ? # O11 Fe4 1.979(6) 4_566 ? # O14 Fe4 2.012(5) 1_455 ? # O15 Fe3 2.007(6) 4_665 ? # O16 Fe2 2.118(5) 4_665 ? # O18 Fe1 2.100(6) 1_655 ? As1 O2 1.645(6) . ? As1 O1 1.682(5) . ? As1 O3 1.705(5) . ? As1 O4 1.717(5) . ? As2 O5 1.678(6) . ? As2 O8 1.691(5) . ? As2 O7 1.695(5) . ? As2 O6 1.701(5) . ? As3 O12 1.669(6) . ? As3 O11 1.679(5) . ? As3 O9 1.701(5) . ? As3 O10 1.702(5) . ? As4 O15 1.666(6) . ? As4 O13 1.674(5) . ? As4 O14 1.711(5) . ? As4 O16 1.727(5) . ? As5 O20 1.671(5) . ? As5 O19 1.692(6) . ? As5 O18 1.703(5) . ? As5 O17 1.705(5) . ? Fe1 O17 2.087(5) . ? Fe1 O24 2.098(6) . ? Fe1 O18 2.100(6) 1_455 ? Fe1 O23 2.109(6) . ? Fe1 O7 2.125(5) . ? Fe1 O14 2.134(5) . ? Fe2 O5 1.964(6) . ? Fe2 O22 2.002(7) . ? Fe2 O3 2.024(6) . ? Fe2 O9 2.042(6) . ? Fe2 O4 2.049(5) 1_655 ? Fe2 O16 2.118(5) 4_566 ? Fe3 O15 2.007(6) 4_566 ? Fe3 O10 2.066(6) 1_455 ? Fe3 O9 2.093(5) . ? Fe3 O21 2.109(7) . ? Fe3 O3 2.119(6) . ? Fe3 O6 2.213(5) . ? Fe4 O11 1.979(6) 4_665 ? Fe4 O8 1.986(6) 1_655 ? Fe4 O14 2.012(5) 1_655 ? Fe4 O16 2.055(5) . ? Fe4 O18 2.058(6) . ? Fe4 O4 2.079(5) 4_765 ? Fe5 O13 1.945(6) . ? Fe5 O1 1.972(6) 1_655 ? Fe5 O7 2.044(5) . ? Fe5 O6 2.047(5) 1_655 ? Fe5 O17 2.057(6) . ? Fe5 O10 2.108(5) . ? O1W H1W 0.83(2) . ? O1W H2W 0.84(2) . ? O2W H3W 0.85(2) . ? O2W H4W 0.85(2) . ? O19 H19 0.84 . ? O20 H20 0.84 . ? O21 H21 0.84 . ? O22 H22 0.84 . ? O23 H23 0.84 . ? O24 H24 0.84 . ? C1 N2 1.484(13) . ? C1 C2 1.508(14) . ? C1 H1C 0.99 . ? C1 H1D 0.99 . ? C2 N1 1.509(12) . ? C2 H2C 0.99 . ? C2 H2D 0.99 . ? C3 N2 1.489(12) . ? C3 C4 1.506(13) . ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? C4 N1 1.495(12) . ? C4 H4A 0.99 . ? C4 H4B 0.99 . ? N1 H1A 0.92 . ? N1 H1B 0.92 . ? N2 H2A 0.92 . ? N2 H2B 0.92 . ? 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 O2 As1 O1 113.3(3) . . ? O2 As1 O3 109.9(3) . . ? O1 As1 O3 107.5(3) . . ? O2 As1 O4 109.7(3) . . ? O1 As1 O4 106.9(3) . . ? O3 As1 O4 109.4(3) . . ? O5 As2 O8 108.8(3) . . ? O5 As2 O7 110.8(3) . . ? O8 As2 O7 109.1(3) . . ? O5 As2 O6 111.1(3) . . ? O8 As2 O6 107.6(3) . . ? O7 As2 O6 109.2(3) . . ? O12 As3 O11 113.3(3) . . ? O12 As3 O9 108.5(3) . . ? O11 As3 O9 107.2(3) . . ? O12 As3 O10 110.2(3) . . ? O11 As3 O10 108.1(3) . . ? O9 As3 O10 109.6(3) . . ? O15 As4 O13 110.2(3) . . ? O15 As4 O14 111.9(3) . . ? O13 As4 O14 108.9(3) . . ? O15 As4 O16 110.7(3) . . ? O13 As4 O16 106.3(3) . . ? O14 As4 O16 108.7(3) . . ? O20 As5 O19 107.6(3) . . ? O20 As5 O18 110.1(3) . . ? O19 As5 O18 108.2(3) . . ? O20 As5 O17 109.6(3) . . ? O19 As5 O17 109.6(3) . . ? O18 As5 O17 111.7(3) . . ? O17 Fe1 O24 100.6(2) . . ? O17 Fe1 O18 160.8(2) . 1_455 ? O24 Fe1 O18 93.8(2) . 1_455 ? O17 Fe1 O23 91.5(2) . . ? O24 Fe1 O23 88.2(2) . . ? O18 Fe1 O23 101.6(2) 1_455 . ? O17 Fe1 O7 76.2(2) . . ? O24 Fe1 O7 176.7(2) . . ? O18 Fe1 O7 89.1(2) 1_455 . ? O23 Fe1 O7 92.6(2) . . ? O17 Fe1 O14 90.6(2) . . ? O24 Fe1 O14 94.1(2) . . ? O18 Fe1 O14 75.7(2) 1_455 . ? O23 Fe1 O14 176.5(2) . . ? O7 Fe1 O14 85.2(2) . . ? O5 Fe2 O22 90.8(2) . . ? O5 Fe2 O3 91.1(2) . . ? O22 Fe2 O3 97.2(2) . . ? O5 Fe2 O9 87.5(2) . . ? O22 Fe2 O9 178.2(2) . . ? O3 Fe2 O9 82.5(2) . . ? O5 Fe2 O4 109.4(2) . 1_655 ? O22 Fe2 O4 92.5(2) . 1_655 ? O3 Fe2 O4 157.2(2) . 1_655 ? O9 Fe2 O4 88.5(2) . 1_655 ? O5 Fe2 O16 171.7(2) . 4_566 ? O22 Fe2 O16 95.6(2) . 4_566 ? O3 Fe2 O16 82.9(2) . 4_566 ? O9 Fe2 O16 86.1(2) . 4_566 ? O4 Fe2 O16 75.6(2) 1_655 4_566 ? O15 Fe3 O10 113.8(2) 4_566 1_455 ? O15 Fe3 O9 89.6(2) 4_566 . ? O10 Fe3 O9 154.4(2) 1_455 . ? O15 Fe3 O21 90.0(2) 4_566 . ? O10 Fe3 O21 92.9(2) 1_455 . ? O9 Fe3 O21 97.7(2) . . ? O15 Fe3 O3 88.3(2) 4_566 . ? O10 Fe3 O3 90.9(2) 1_455 . ? O9 Fe3 O3 79.0(2) . . ? O21 Fe3 O3 176.3(2) . . ? O15 Fe3 O6 168.4(2) 4_566 . ? O10 Fe3 O6 75.0(2) 1_455 . ? O9 Fe3 O6 80.6(2) . . ? O21 Fe3 O6 97.4(2) . . ? O3 Fe3 O6 83.8(2) . . ? O11 Fe4 O8 84.2(2) 4_665 1_655 ? O11 Fe4 O14 104.7(2) 4_665 1_655 ? O8 Fe4 O14 91.2(2) 1_655 1_655 ? O11 Fe4 O16 93.7(2) 4_665 . ? O8 Fe4 O16 107.3(2) 1_655 . ? O14 Fe4 O16 155.2(2) 1_655 . ? O11 Fe4 O18 173.0(2) 4_665 . ? O8 Fe4 O18 90.1(2) 1_655 . ? O14 Fe4 O18 79.3(2) 1_655 . ? O16 Fe4 O18 84.2(2) . . ? O11 Fe4 O4 88.8(2) 4_665 4_765 ? O8 Fe4 O4 172.2(2) 1_655 4_765 ? O14 Fe4 O4 87.5(2) 1_655 4_765 ? O16 Fe4 O4 76.3(2) . 4_765 ? O18 Fe4 O4 97.1(2) . 4_765 ? O13 Fe5 O1 83.9(2) . 1_655 ? O13 Fe5 O7 91.7(2) . . ? O1 Fe5 O7 105.1(2) 1_655 . ? O13 Fe5 O6 106.2(2) . 1_655 ? O1 Fe5 O6 93.8(2) 1_655 1_655 ? O7 Fe5 O6 155.4(2) . 1_655 ? O13 Fe5 O17 89.4(2) . . ? O1 Fe5 O17 172.4(2) 1_655 . ? O7 Fe5 O17 78.7(2) . . ? O6 Fe5 O17 84.6(2) 1_655 . ? O13 Fe5 O10 173.6(2) . . ? O1 Fe5 O10 91.0(2) 1_655 . ? O7 Fe5 O10 86.1(2) . . ? O6 Fe5 O10 77.7(2) 1_655 . ? O17 Fe5 O10 96.0(2) . . ? As1 O1 Fe5 126.5(3) . 1_455 ? H1W O1W H2W 120(4) . . ? As1 O3 Fe2 130.7(3) . . ? As1 O3 Fe3 123.2(3) . . ? Fe2 O3 Fe3 99.1(2) . . ? H3W O2W H4W 115(4) . . ? As1 O4 Fe2 125.8(3) . 1_455 ? As1 O4 Fe4 130.2(3) . 4_466 ? Fe2 O4 Fe4 103.9(2) 1_455 4_466 ? As2 O5 Fe2 119.8(3) . . ? As2 O6 Fe5 127.4(3) . 1_455 ? As2 O6 Fe3 119.6(3) . . ? Fe5 O6 Fe3 100.8(2) 1_455 . ? As2 O7 Fe5 128.0(3) . . ? As2 O7 Fe1 121.5(3) . . ? Fe5 O7 Fe1 101.4(2) . . ? As2 O8 Fe4 124.3(3) . 1_455 ? As3 O9 Fe2 125.8(3) . . ? As3 O9 Fe3 127.3(3) . . ? Fe2 O9 Fe3 99.4(2) . . ? As3 O10 Fe3 123.4(3) . 1_655 ? As3 O10 Fe5 131.6(3) . . ? Fe3 O10 Fe5 103.8(2) 1_655 . ? As3 O11 Fe4 126.2(3) . 4_566 ? As4 O13 Fe5 127.5(3) . . ? As4 O14 Fe4 128.9(3) . 1_455 ? As4 O14 Fe1 120.2(3) . . ? Fe4 O14 Fe1 102.1(2) 1_455 . ? As4 O15 Fe3 117.8(3) . 4_665 ? As4 O16 Fe4 125.9(3) . . ? As4 O16 Fe2 119.5(3) . 4_665 ? Fe4 O16 Fe2 102.3(2) . 4_665 ? As5 O17 Fe5 132.4(3) . . ? As5 O17 Fe1 125.3(3) . . ? Fe5 O17 Fe1 102.3(2) . . ? As5 O18 Fe4 133.4(3) . . ? As5 O18 Fe1 124.9(3) . 1_655 ? Fe4 O18 Fe1 101.7(2) . 1_655 ? As5 O19 H19 109.5 . . ? As5 O20 H20 109.5 . . ? Fe3 O21 H21 109.5 . . ? Fe2 O22 H22 109.5 . . ? Fe1 O23 H23 109.5 . . ? Fe1 O24 H24 109.5 . . ? N2 C1 C2 109.1(8) . . ? N2 C1 H1C 109.9 . . ? C2 C1 H1C 109.9 . . ? N2 C1 H1D 109.9 . . ? C2 C1 H1D 109.9 . . ? H1C C1 H1D 108.3 . . ? C1 C2 N1 111.4(8) . . ? C1 C2 H2C 109.3 . . ? N1 C2 H2C 109.3 . . ? C1 C2 H2D 109.3 . . ? N1 C2 H2D 109.3 . . ? H2C C2 H2D 108 . . ? N2 C3 C4 110.2(8) . . ? N2 C3 H3A 109.6 . . ? C4 C3 H3A 109.6 . . ? N2 C3 H3B 109.6 . . ? C4 C3 H3B 109.6 . . ? H3A C3 H3B 108.1 . . ? N1 C4 C3 110.4(8) . . ? N1 C4 H4A 109.6 . . ? C3 C4 H4A 109.6 . . ? N1 C4 H4B 109.6 . . ? C3 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? C4 N1 C2 112.2(7) . . ? C4 N1 H1A 109.2 . . ? C2 N1 H1A 109.2 . . ? C4 N1 H1B 109.2 . . ? C2 N1 H1B 109.2 . . ? H1A N1 H1B 107.9 . . ? C1 N2 C3 111.6(8) . . ? C1 N2 H2A 109.3 . . ? C3 N2 H2A 109.3 . . ? C1 N2 H2B 109.3 . . ? C3 N2 H2B 109.3 . . ? H2A N2 H2B 108 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA O19 H19 O21 1_655 0.84 1.88 2.651(8) 151.7 O20 H20 O24 . 0.84 1.79 2.626(8) 174.4 O21 H21 O12 . 0.84 1.93 2.727(8) 158.5 O22 H22 O20 4_566 0.84 1.99 2.605(8) 129.5 O23 H23 O12 . 0.84 1.99 2.795(8) 158.9 O24 H24 O2 4_665 0.84 1.89 2.690(8) 159.5 N1 H1A O8 1_655 0.92 1.94 2.847(10) 166.4 N1 H1A O11 4_665 0.92 2.34 2.849(10) 114.7 N1 H1B O2W 4_665 0.92 1.95 2.836(11) 159.8 N2 H2A O1W . 0.92 1.93 2.836(11) 167.4 N2 H2B O19 2_655 0.92 1.78 2.686(10) 165.9 O1W H1W O24 2 0.83(2) 1.97(4) 2.785(10) 165(11) O1W H2W O2 1_655 0.84(2) 2.02(3) 2.781(10) 151(3) O2W H3W O12 3_656 0.85(2) 2.25(9) 2.880(10) 131(10) O2W H4W O21 1_655 0.85(2) 2.27(3) 3.103(9) 166(8) #DABCO data_5 _database_code_depnum_ccdc_archive 'CCDC 639062' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H21 As7 Fe6 N2 O31' _chemical_formula_weight 1476.79 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' As As 0.0499 2.0058 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.6364(3) _cell_length_b 10.8179(4) _cell_length_c 12.2213(5) _cell_angle_alpha 109.927(2) _cell_angle_beta 100.807(2) _cell_angle_gamma 101.320(2) _cell_volume 777.40(6) _cell_formula_units_Z 1 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 3476 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Plate _exptl_crystal_colour Brown _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.154 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 706 _exptl_absorpt_coefficient_mu 10.240 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4847 _exptl_absorpt_correction_T_max 0.9045 _exptl_absorpt_process_details ; SADABS V2.10 (Sheldrick, G.M., 2003) ; _exptl_special_details ; SADABS was used to perform the Absorption correction Parameter refinement on 15366 reflections reduced R(int) from 0.1650 to 0.0610 Ratio of minimum to maximum apparent transmission: 0.655226 The given Tmin and Tmax were generated using the SHELX SIZE command ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker Nonius FR591 Rotating Anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans to fill the asymmetric unit' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15229 _diffrn_reflns_av_R_equivalents 0.0590 _diffrn_reflns_av_sigmaI/netI 0.0371 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.26 _diffrn_reflns_theta_max 25.02 _reflns_number_total 2740 _reflns_number_gt 2592 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CAMERON (Watkin, et al., 1993)' _computing_publication_material 'WINGX (Farrugia, 1998)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0568P)^2^+11.9557P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2740 _refine_ls_number_parameters 272 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0464 _refine_ls_R_factor_gt 0.0441 _refine_ls_wR_factor_ref 0.1223 _refine_ls_wR_factor_gt 0.1208 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.049 _refine_ls_shift/su_mean 0.003 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 C1 C 0.413(2) 0.3583(11) 0.4125(9) 0.057(4) Uani 1 1 d . . . C2 C 0.530(3) 0.6008(12) 0.4505(9) 0.064(4) Uani 1 1 d . . . C3 C 0.186(4) 0.506(2) 0.443(2) 0.048(6) Uani 0.50 1 d P . . C4 C 0.767(5) 0.475(3) 0.430(2) 0.064(8) Uani 0.50 1 d P . . N1 N 0.538(4) 0.4631(18) 0.3867(14) 0.050(5) Uani 0.50 1 d P . . N2 N 0.367(4) 0.4805(16) 0.3925(13) 0.038(4) Uani 0.50 1 d P . . As1 As 0.03576(10) 0.28564(7) 0.08490(6) 0.0087(2) Uani 1 1 d . . . As2 As -0.42928(12) -0.03589(8) -0.16168(7) 0.0185(2) Uani 1 1 d . . . As3 As -0.27807(11) 0.59847(7) 0.15857(6) 0.0097(2) Uani 1 1 d . . . As4 As -0.0731(4) 0.0622(2) 0.3943(2) 0.0471(6) Uani 0.50 1 d P . . Fe1 Fe 0.51410(15) 0.26612(10) 0.03548(9) 0.0101(2) Uani 1 1 d . . . Fe2 Fe -0.20627(15) 0.40622(10) -0.10517(9) 0.0115(3) Uani 1 1 d . . . Fe3 Fe -0.10432(16) -0.00300(10) 0.10356(9) 0.0115(3) Uani 1 1 d . . . O1 O -0.0128(8) 0.2009(5) 0.1739(5) 0.0146(10) Uani 1 1 d . . . O2 O -0.1977(7) 0.2809(5) -0.0039(4) 0.0105(10) Uani 1 1 d . . . O3 O 0.1862(7) 0.2132(5) -0.0035(4) 0.0111(10) Uani 1 1 d . . . O4 O 0.1735(8) 0.4486(5) 0.1753(5) 0.0133(10) Uani 1 1 d . . . O5 O -0.1796(7) 0.0106(5) -0.0635(4) 0.0109(10) Uani 1 1 d . . . O6 O -0.4125(15) -0.0279(11) -0.2849(8) 0.066(2) Uani 1 1 d . . . O7 O -0.5792(8) 0.0625(5) -0.0894(4) 0.0116(10) Uani 1 1 d . . . O8 O -0.5416(8) -0.1964(5) -0.1698(5) 0.0155(11) Uani 1 1 d . . . H8 H -0.6279 -0.2609 -0.2474 0.023 Uiso 1 1 calc R . . O9 O -0.0058(9) -0.0078(6) 0.2671(5) 0.0232(12) Uani 1 1 d . . . O10 O -0.175(3) 0.1773(16) 0.4258(15) 0.056(4) Uani 0.50 1 d P . . O11 O -0.231(4) -0.0789(19) 0.4037(19) 0.082(7) Uani 0.50 1 d P . . H11 H -0.1729 -0.1428 0.3880 0.124 Uiso 0.50 1 calc PR . . O12 O 0.167(3) 0.1204(19) 0.5033(13) 0.053(4) Uani 0.50 1 d P . . O13 O -0.1327(9) 0.7162(7) 0.2919(5) 0.0314(15) Uani 1 1 d . . . H13 H -0.0804 0.7890 0.2842 0.047 Uiso 1 1 calc R . . O14 O -0.1202(7) 0.5682(5) 0.0644(4) 0.0106(10) Uani 1 1 d . . . O15 O -0.4820(8) 0.6495(5) 0.0972(5) 0.0152(11) Uani 1 1 d . . . O17 O -0.3868(8) 0.4511(5) 0.1703(5) 0.0166(11) Uani 1 1 d . . . O16 O -0.2736(10) 0.2492(6) -0.2742(5) 0.0260(13) Uani 1 1 d . . . H16 H -0.3322 0.1744 -0.2716 0.039 Uiso 1 1 calc R . . H1 H 0.4952 0.4390 0.3036 0.150 Uiso 0.50 1 d P . . H1A H 0.5278 0.3357 0.3797 0.150 Uiso 1 1 d . . . H1B H 0.2866 0.2789 0.3710 0.150 Uiso 1 1 d . . . H2 H 0.3262 0.4579 0.3078 0.150 Uiso 0.50 1 d P . . H2A H 0.3822 0.6084 0.4262 0.150 Uiso 1 1 d . . . H2B H 0.6220 0.6661 0.4349 0.150 Uiso 1 1 d . . . H3A H 0.0567 0.4240 0.3936 0.150 Uiso 0.50 1 d P . . H3B H 0.1479 0.5819 0.4303 0.150 Uiso 0.50 1 d P . . H4A H 0.8466 0.5516 0.4190 0.150 Uiso 0.50 1 d P . . H4B H 0.7907 0.3924 0.3821 0.150 Uiso 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.114(11) 0.027(5) 0.017(5) 0.004(4) 0.003(6) 0.011(6) C2 0.133(13) 0.033(6) 0.016(5) 0.010(4) 0.000(6) 0.023(7) C3 0.069(16) 0.043(13) 0.035(11) 0.016(10) 0.028(11) 0.011(11) C4 0.10(2) 0.054(15) 0.025(11) 0.016(11) 0.011(13) 0.009(15) N1 0.101(18) 0.025(9) 0.009(7) 0.001(6) 0.004(9) 0.011(10) N2 0.079(14) 0.020(8) 0.008(7) 0.005(6) -0.002(8) 0.008(9) As1 0.0073(4) 0.0068(4) 0.0141(4) 0.0051(3) 0.0044(3) 0.0036(3) As2 0.0085(4) 0.0148(4) 0.0246(4) -0.0022(3) 0.0032(3) 0.0060(3) As3 0.0081(4) 0.0092(4) 0.0130(4) 0.0044(3) 0.0034(3) 0.0043(3) As4 0.0539(14) 0.0469(13) 0.0331(11) 0.0068(10) 0.0202(10) 0.0060(11) Fe1 0.0073(5) 0.0088(5) 0.0163(5) 0.0061(4) 0.0050(4) 0.0031(4) Fe2 0.0087(5) 0.0083(5) 0.0213(6) 0.0079(4) 0.0071(4) 0.0040(4) Fe3 0.0103(5) 0.0080(5) 0.0199(6) 0.0073(4) 0.0072(4) 0.0046(4) O1 0.016(3) 0.017(3) 0.017(3) 0.010(2) 0.008(2) 0.006(2) O2 0.006(2) 0.010(2) 0.015(2) 0.0042(19) 0.0017(19) 0.0046(19) O3 0.009(2) 0.013(2) 0.015(2) 0.007(2) 0.0067(19) 0.0060(19) O4 0.010(2) 0.007(2) 0.018(3) 0.001(2) 0.002(2) -0.0006(19) O5 0.006(2) 0.012(2) 0.017(3) 0.006(2) 0.0059(19) 0.0055(19) O6 0.067(6) 0.083(7) 0.060(6) 0.035(5) 0.026(5) 0.025(5) O7 0.010(2) 0.012(2) 0.017(3) 0.007(2) 0.0055(19) 0.0073(19) O8 0.019(3) 0.014(3) 0.014(2) 0.004(2) 0.005(2) 0.006(2) O9 0.023(3) 0.027(3) 0.026(3) 0.014(3) 0.007(2) 0.014(2) O10 0.067(11) 0.039(9) 0.053(10) -0.006(7) 0.025(8) 0.030(8) O11 0.125(19) 0.040(10) 0.075(14) 0.010(9) 0.056(14) 0.005(11) O12 0.054(10) 0.080(12) 0.028(7) 0.019(8) 0.012(7) 0.032(9) O13 0.017(3) 0.030(3) 0.024(3) -0.009(3) 0.002(2) -0.004(2) O14 0.010(2) 0.010(2) 0.013(2) 0.0055(19) 0.0038(19) 0.0040(19) O15 0.012(2) 0.017(3) 0.022(3) 0.010(2) 0.007(2) 0.010(2) O17 0.016(3) 0.015(3) 0.023(3) 0.010(2) 0.008(2) 0.007(2) O16 0.029(3) 0.019(3) 0.033(3) 0.010(3) 0.014(3) 0.007(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 C1 N1 1.43(2) . ? C1 N2 1.50(2) . ? C1 C2 1.528(14) 2_666 ? C1 H1A 0.959 . ? C1 H1B 0.980 . ? C2 N2 1.38(2) . ? C2 N1 1.44(2) . ? C2 C1 1.528(14) 2_666 ? C2 H2A 0.999 . ? C2 H2B 0.934 . ? C3 C4 1.46(3) 2_666 ? C3 N2 1.48(3) . ? C3 H3A 1.01(2) . ? C3 H3B 0.96(2) . ? C4 C3 1.46(3) 2_666 ? C4 N1 1.47(4) . ? C4 H4A 0.95(3) . ? C4 H4B 0.95(3) . ? N1 H1 0.928(16) . ? N2 H2 0.948(14) . ? N2 H2A 1.279(16) . ? As1 O1 1.680(5) . ? As1 O4 1.681(5) . ? As1 O2 1.697(5) . ? As1 O3 1.707(5) . ? As2 O6 1.561(9) . ? As2 O8 1.710(5) . ? As2 O5 1.719(5) . ? As2 O7 1.734(5) . ? As3 O13 1.650(6) . ? As3 O17 1.681(5) . ? As3 O14 1.691(5) . ? As3 O15 1.701(5) . ? As4 O10 1.505(14) . ? As4 O9 1.667(6) . ? As4 O12 1.716(16) . ? As4 O11 1.726(19) . ? Fe1 O17 1.995(5) 1_655 ? Fe1 O8 2.021(5) 2 ? Fe1 O2 2.048(5) 1_655 ? Fe1 O3 2.056(5) . ? Fe1 O7 2.094(5) 1_655 ? Fe1 O15 2.113(5) 2_565 ? Fe2 O4 2.025(5) 2_565 ? Fe2 O15 2.069(5) 2_465 ? Fe2 O14 2.070(5) 2_565 ? Fe2 O16 2.078(6) . ? Fe2 O14 2.093(5) . ? Fe2 O2 2.126(5) . ? Fe3 O1 1.990(5) . ? Fe3 O9 2.005(6) . ? Fe3 O7 2.028(5) 2_455 ? Fe3 O5 2.044(5) 2 ? Fe3 O5 2.071(5) . ? Fe3 O3 2.082(5) 2 ? O2 Fe1 2.048(5) 1_455 ? O3 Fe3 2.082(5) 2 ? O4 Fe2 2.025(5) 2_565 ? O5 Fe3 2.044(5) 2 ? O7 Fe3 2.028(5) 2_455 ? O7 Fe1 2.094(5) 1_455 ? O8 Fe1 2.021(5) 2 ? O8 H8 0.9500 . ? O11 H11 0.8400 . ? O12 O11 1.38(3) 2_556 ? O13 H13 0.8400 . ? O14 Fe2 2.070(5) 2_565 ? O15 Fe2 2.069(5) 2_465 ? O15 Fe1 2.113(5) 2_565 ? O17 Fe1 1.995(5) 1_455 ? O16 H16 0.8400 . ? 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 N1 C1 N2 48.1(12) . . ? N1 C1 C2 108.9(11) . 2_666 ? N2 C1 C2 105.6(10) . 2_666 ? N1 C1 H1A 64.7(12) . . ? N2 C1 H1A 110.2(13) . . ? C2 C1 H1A 112.2(13) 2_666 . ? N1 C1 H1B 138.6(12) . . ? N2 C1 H1B 109.8(14) . . ? C2 C1 H1B 111.2(12) 2_666 . ? H1A C1 H1B 107.9 . . ? N2 C2 N1 50.2(12) . . ? N2 C2 C1 110.6(12) . 2_666 ? N1 C2 C1 112.2(10) . 2_666 ? N2 C2 H2A 62.8(12) . . ? N1 C2 H2A 110.3(15) . . ? C1 C2 H2A 106.1(13) 2_666 . ? N2 C2 H2B 141.7(12) . . ? N1 C2 H2B 112.6(16) . . ? C1 C2 H2B 107.7(11) 2_666 . ? H2A C2 H2B 107.6 . . ? C4 C3 N2 111(2) 2_666 . ? C4 C3 H3A 109(2) 2_666 . ? N2 C3 H3A 108.0(18) . . ? C4 C3 H3B 112(2) 2_666 . ? N2 C3 H3B 110.0(18) . . ? H3A C3 H3B 105 . . ? C3 C4 N1 108(2) 2_666 . ? C3 C4 H4A 112(2) 2_666 . ? N1 C4 H4A 108(2) . . ? C3 C4 H4B 111(2) 2_666 . ? N1 C4 H4B 107(2) . . ? H4A C4 H4B 111(3) . . ? C1 N1 C2 115.9(17) . . ? C1 N1 C4 109.4(17) . . ? C2 N1 C4 101.9(17) . . ? C1 N1 H1 107.4(17) . . ? C2 N1 H1 110.4(17) . . ? C4 N1 H1 112(2) . . ? C2 N1 H1A 151.1(15) . . ? C4 N1 H1A 79.3(16) . . ? H1 N1 H1A 95.4(13) . . ? C2 N2 C3 106.0(15) . . ? C2 N2 C1 115.7(15) . . ? C3 N2 C1 106.6(15) . . ? C2 N2 H1 86.2(13) . . ? C3 N2 H1 161.3(16) . . ? C1 N2 H1 79.7(11) . . ? C2 N2 H2 110.7(15) . . ? C3 N2 H2 110(2) . . ? C1 N2 H2 108.1(14) . . ? H1 N2 H2 52.0(10) . . ? C3 N2 H2A 71.8(13) . . ? C1 N2 H2A 153.2(13) . . ? H1 N2 H2A 110.6(12) . . ? H2 N2 H2A 97.1(12) . . ? O1 As1 O4 107.7(3) . . ? O1 As1 O2 110.2(2) . . ? O4 As1 O2 110.1(2) . . ? O1 As1 O3 109.7(2) . . ? O4 As1 O3 109.2(2) . . ? O2 As1 O3 109.8(2) . . ? O6 As2 O8 115.0(4) . . ? O6 As2 O5 110.8(4) . . ? O8 As2 O5 103.0(2) . . ? O6 As2 O7 114.8(4) . . ? O8 As2 O7 103.9(2) . . ? O5 As2 O7 108.3(2) . . ? O13 As3 O17 111.0(3) . . ? O13 As3 O14 109.1(3) . . ? O17 As3 O14 108.6(2) . . ? O13 As3 O15 111.4(3) . . ? O17 As3 O15 107.4(2) . . ? O14 As3 O15 109.2(2) . . ? O10 As4 O9 127.5(7) . . ? O10 As4 O12 105.3(9) . . ? O9 As4 O12 102.6(5) . . ? O10 As4 O11 109.1(11) . . ? O9 As4 O11 102.2(7) . . ? O12 As4 O11 109.2(10) . . ? O17 Fe1 O8 84.5(2) 1_655 2 ? O17 Fe1 O2 93.9(2) 1_655 1_655 ? O8 Fe1 O2 105.0(2) 2 1_655 ? O17 Fe1 O3 104.9(2) 1_655 . ? O8 Fe1 O3 92.3(2) 2 . ? O2 Fe1 O3 155.6(2) 1_655 . ? O17 Fe1 O7 172.8(2) 1_655 1_655 ? O8 Fe1 O7 88.4(2) 2 1_655 ? O2 Fe1 O7 86.56(19) 1_655 1_655 ? O3 Fe1 O7 76.69(19) . 1_655 ? O17 Fe1 O15 92.2(2) 1_655 2_565 ? O8 Fe1 O15 176.3(2) 2 2_565 ? O2 Fe1 O15 76.86(19) 1_655 2_565 ? O3 Fe1 O15 86.94(19) . 2_565 ? O7 Fe1 O15 94.90(19) 1_655 2_565 ? O4 Fe2 O15 109.3(2) 2_565 2_465 ? O4 Fe2 O14 90.79(19) 2_565 2_565 ? O15 Fe2 O14 158.6(2) 2_465 2_565 ? O4 Fe2 O16 92.2(2) 2_565 . ? O15 Fe2 O16 92.1(2) 2_465 . ? O14 Fe2 O16 94.8(2) 2_565 . ? O4 Fe2 O14 86.52(19) 2_565 . ? O15 Fe2 O14 91.26(19) 2_465 . ? O14 Fe2 O14 82.17(19) 2_565 . ? O16 Fe2 O14 176.6(2) . . ? O4 Fe2 O2 169.7(2) 2_565 . ? O15 Fe2 O2 76.13(18) 2_465 . ? O14 Fe2 O2 82.92(18) 2_565 . ? O16 Fe2 O2 96.4(2) . . ? O14 Fe2 O2 84.59(18) . . ? O1 Fe3 O9 91.4(2) . . ? O1 Fe3 O7 107.0(2) . 2_455 ? O9 Fe3 O7 95.4(2) . 2_455 ? O1 Fe3 O5 91.7(2) . 2 ? O9 Fe3 O5 94.4(2) . 2 ? O7 Fe3 O5 158.6(2) 2_455 2 ? O1 Fe3 O5 86.2(2) . . ? O9 Fe3 O5 175.2(2) . . ? O7 Fe3 O5 89.36(19) 2_455 . ? O5 Fe3 O5 81.5(2) 2 . ? O1 Fe3 O3 170.0(2) . 2 ? O9 Fe3 O3 97.1(2) . 2 ? O7 Fe3 O3 77.56(18) 2_455 2 ? O5 Fe3 O3 82.41(19) 2 2 ? O5 Fe3 O3 84.93(19) . 2 ? As1 O1 Fe3 119.7(3) . . ? As1 O2 Fe1 126.8(3) . 1_455 ? As1 O2 Fe2 121.4(3) . . ? Fe1 O2 Fe2 102.27(19) 1_455 . ? As1 O3 Fe1 127.2(3) . . ? As1 O3 Fe3 121.9(3) . 2 ? Fe1 O3 Fe3 101.9(2) . 2 ? As1 O4 Fe2 119.8(3) . 2_565 ? As2 O5 Fe3 128.3(3) . 2 ? As2 O5 Fe3 127.5(3) . . ? Fe3 O5 Fe3 98.5(2) 2 . ? As2 O7 Fe3 127.4(3) . 2_455 ? As2 O7 Fe1 130.2(3) . 1_455 ? Fe3 O7 Fe1 102.4(2) 2_455 1_455 ? As2 O8 Fe1 128.3(3) . 2 ? As2 O8 H8 115.9 . . ? Fe1 O8 H8 115.9 2 . ? As4 O9 Fe3 130.3(3) . . ? As4 O11 H11 109.5 . . ? O11 O12 As4 129.5(16) 2_556 . ? As3 O13 H13 109.5 . . ? As3 O14 Fe2 129.4(3) . 2_565 ? As3 O14 Fe2 125.4(3) . . ? Fe2 O14 Fe2 97.83(19) 2_565 . ? As3 O15 Fe2 125.0(3) . 2_465 ? As3 O15 Fe1 131.3(3) . 2_565 ? Fe2 O15 Fe1 102.0(2) 2_465 2_565 ? As3 O17 Fe1 125.3(3) . 1_455 ? Fe2 O16 H16 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O8 H8 N1 0.95 2.53 3.192(18) 127.1 2 O11 H11 O13 0.84 1.68 2.46(2) 152.4 1_545 O13 H13 O9 0.84 2.25 3.072(9) 168.0 1_565 O16 H16 O6 0.84 2.09 2.908(12) 164.4 . N1 H1 O17 0.928(16) 1.968(5) 2.747(18) 140.3(16) 1_655 N1 H1 O4 0.928(16) 2.444(5) 3.13(2) 130.7(16) . N2 H2 O4 0.948(14) 1.702(5) 2.596(15) 155.8(14) . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.347 _refine_diff_density_min -1.507 _refine_diff_density_rms 0.225 #LiAsO4OH data_6 _database_code_depnum_ccdc_archive 'CCDC 639063' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H2 As2 Fe2 Li2 O10' _chemical_formula_weight 437.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Li Li -0.0003 0.0001 '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' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.2652(3) _cell_length_b 5.4841(3) _cell_length_c 7.3932(4) _cell_angle_alpha 110.669(3) _cell_angle_beta 105.318(3) _cell_angle_gamma 98.160(4) _cell_volume 185.984(18) _cell_formula_units_Z 1 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 2008 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour green _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.906 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 206 _exptl_absorpt_coefficient_mu 12.770 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2503 _exptl_absorpt_correction_T_max 0.7843 _exptl_absorpt_process_details ; SADABS V2.10 (Sheldrick, G.M., 2003) ; _exptl_special_details ; SADABS was used to perform the Absorption correction Parameter refinement on 15366 reflections reduced R(int) from 0.1650 to 0.0610 Ratio of minimum to maximum apparent transmission: 0.655226 The given Tmin and Tmax were generated using the SHELX SIZE command ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker Nonius FR591 Rotating Anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans to fill the asymmetric unit' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3489 _diffrn_reflns_av_R_equivalents 0.0575 _diffrn_reflns_av_sigmaI/netI 0.0420 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 27.42 _reflns_number_total 844 _reflns_number_gt 758 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CAMERON (Watkin, et al., 1993)' _computing_publication_material 'WINGX (Farrugia, 1998)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0365P)^2^+0.8089P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 844 _refine_ls_number_parameters 80 _refine_ls_number_restraints 25 _refine_ls_R_factor_all 0.0316 _refine_ls_R_factor_gt 0.0270 _refine_ls_wR_factor_ref 0.0686 _refine_ls_wR_factor_gt 0.0662 _refine_ls_goodness_of_fit_ref 0.956 _refine_ls_restrained_S_all 0.941 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 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 Li1 Li 0.5623(15) 0.4372(15) 0.8152(12) 0.0119(15) Uani 1 1 d . . . O1 O 1.2912(6) 0.2333(6) 0.8876(4) 0.0058(6) Uani 1 1 d U . . H1 H 0.479(10) 0.727(12) 0.667(9) 0.023(15) Uiso 1 1 d D . . As1 As 0.94977(8) 0.13337(8) 0.76741(6) 0.00389(15) Uani 1 1 d U . . Fe2 Fe 0.5000 0.0000 1.0000 0.0039(2) Uani 1 2 d S . . Fe1 Fe 1.0000 0.5000 0.5000 0.0044(2) Uani 1 2 d S . . O4 O 0.8415(6) 0.3484(6) 0.6670(4) 0.0060(6) Uani 1 1 d U . . O3 O 0.8014(6) 0.1744(6) 0.9480(4) 0.0073(6) Uani 1 1 d U . . O5 O 0.3727(6) 0.6838(6) 0.7209(4) 0.0056(6) Uani 1 1 d D . . O2 O 0.8377(6) -0.1861(6) 0.5884(5) 0.0065(6) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Li1 0.008(4) 0.011(4) 0.019(4) 0.007(3) 0.006(3) 0.005(3) O1 0.0048(14) 0.0062(14) 0.0062(14) 0.0025(11) 0.0009(11) 0.0029(11) As1 0.0030(2) 0.0046(2) 0.0045(2) 0.00151(17) 0.00191(17) 0.00188(16) Fe2 0.0024(4) 0.0044(4) 0.0046(4) 0.0012(3) 0.0013(3) 0.0013(3) Fe1 0.0041(4) 0.0047(4) 0.0042(4) 0.0013(3) 0.0014(3) 0.0018(3) O4 0.0048(14) 0.0063(14) 0.0076(14) 0.0030(11) 0.0020(12) 0.0032(11) O3 0.0092(15) 0.0083(14) 0.0063(14) 0.0027(12) 0.0048(12) 0.0041(11) O5 0.0033(14) 0.0094(14) 0.0042(14) 0.0026(11) 0.0020(11) 0.0010(11) O2 0.0061(14) 0.0043(14) 0.0093(15) 0.0013(12) 0.0041(12) 0.0033(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Li1 O1 1.987(8) 1_455 ? Li1 O5 1.998(8) . ? Li1 O4 2.068(8) . ? Li1 O1 2.143(8) 2_767 ? Li1 O3 2.343(8) . ? Li1 As1 2.827(7) . ? Li1 Li1 2.850(16) 2_667 ? Li1 Fe2 3.008(7) 1_565 ? Li1 Fe2 3.170(8) . ? Li1 H1 2.26(6) . ? O1 As1 1.689(3) . ? O1 Li1 1.987(8) 1_655 ? O1 Fe2 2.050(3) 1_655 ? O1 Li1 2.143(8) 2_767 ? As1 O2 1.681(3) . ? As1 O3 1.683(3) . ? As1 O4 1.689(3) . ? Fe2 O3 1.932(3) 2_657 ? Fe2 O3 1.932(3) . ? Fe2 O5 2.031(3) 2_667 ? Fe2 O5 2.031(3) 1_545 ? Fe2 O1 2.050(3) 2_757 ? Fe2 O1 2.050(3) 1_455 ? Fe2 Li1 3.008(8) 1_545 ? Fe2 Li1 3.008(8) 2_667 ? Fe2 Li1 3.170(8) 2_657 ? Fe1 O4 1.996(3) . ? Fe1 O4 1.996(3) 2_766 ? Fe1 O2 2.010(3) 2_756 ? Fe1 O2 2.010(3) 1_565 ? Fe1 O5 2.029(3) 1_655 ? Fe1 O5 2.029(3) 2_666 ? O5 Fe1 2.029(3) 1_455 ? O5 Fe2 2.031(3) 1_565 ? O5 H1 0.83(2) . ? O2 Fe1 2.010(3) 1_545 ? 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 O1 Li1 O5 104.5(4) 1_455 . ? O1 Li1 O4 136.2(4) 1_455 . ? O5 Li1 O4 108.8(4) . . ? O1 Li1 O1 92.8(3) 1_455 2_767 ? O5 Li1 O1 85.1(3) . 2_767 ? O4 Li1 O1 117.3(4) . 2_767 ? O1 Li1 O3 76.3(3) 1_455 . ? O5 Li1 O3 175.9(4) . . ? O4 Li1 O3 72.5(3) . . ? O1 Li1 O3 90.9(3) 2_767 . ? O1 Li1 As1 105.5(3) 1_455 . ? O5 Li1 As1 145.1(4) . . ? O4 Li1 As1 36.34(15) . . ? O1 Li1 As1 110.8(3) 2_767 . ? O3 Li1 As1 36.48(13) . . ? O1 Li1 Li1 48.7(2) 1_455 2_667 ? O5 Li1 Li1 96.4(4) . 2_667 ? O4 Li1 Li1 148.0(5) . 2_667 ? O1 Li1 Li1 44.1(2) 2_767 2_667 ? O3 Li1 Li1 81.2(3) . 2_667 ? As1 Li1 Li1 116.9(4) . 2_667 ? O1 Li1 Fe2 101.2(3) 1_455 1_565 ? O5 Li1 Fe2 42.14(16) . 1_565 ? O4 Li1 Fe2 122.6(3) . 1_565 ? O1 Li1 Fe2 42.95(15) 2_767 1_565 ? O3 Li1 Fe2 133.9(3) . 1_565 ? As1 Li1 Fe2 143.6(3) . 1_565 ? Li1 Li1 Fe2 65.5(3) 2_667 1_565 ? O1 Li1 Fe2 38.97(17) 1_455 . ? O5 Li1 Fe2 143.4(3) . . ? O4 Li1 Fe2 104.6(3) . . ? O1 Li1 Fe2 92.8(3) 2_767 . ? O3 Li1 Fe2 37.36(13) . . ? As1 Li1 Fe2 69.09(16) . . ? Li1 Li1 Fe2 59.7(3) 2_667 . ? Fe2 Li1 Fe2 125.1(3) 1_565 . ? O1 Li1 H1 125.0(10) 1_455 . ? O5 Li1 H1 21.2(9) . . ? O4 Li1 H1 88.2(10) . . ? O1 Li1 H1 89.9(15) 2_767 . ? O3 Li1 H1 158.6(10) . . ? As1 Li1 H1 124.5(10) . . ? Li1 Li1 H1 113.5(12) 2_667 . ? Fe2 Li1 H1 50.6(14) 1_565 . ? Fe2 Li1 H1 163.9(11) . . ? As1 O1 Li1 126.1(3) . 1_655 ? As1 O1 Fe2 122.13(15) . 1_655 ? Li1 O1 Fe2 103.5(3) 1_655 1_655 ? As1 O1 Li1 116.1(2) . 2_767 ? Li1 O1 Li1 87.2(3) 1_655 2_767 ? Fe2 O1 Li1 91.6(2) 1_655 2_767 ? O2 As1 O3 110.92(14) . . ? O2 As1 O4 110.91(14) . . ? O3 As1 O4 101.79(14) . . ? O2 As1 O1 113.49(14) . . ? O3 As1 O1 107.82(15) . . ? O4 As1 O1 111.26(14) . . ? O2 As1 Li1 117.73(19) . . ? O3 As1 Li1 55.88(19) . . ? O4 As1 Li1 46.53(18) . . ? O1 As1 Li1 128.70(19) . . ? O3 Fe2 O3 180.000(1) 2_657 . ? O3 Fe2 O5 92.76(12) 2_657 2_667 ? O3 Fe2 O5 87.24(12) . 2_667 ? O3 Fe2 O5 87.24(12) 2_657 1_545 ? O3 Fe2 O5 92.76(12) . 1_545 ? O5 Fe2 O5 180.0 2_667 1_545 ? O3 Fe2 O1 84.93(12) 2_657 2_757 ? O3 Fe2 O1 95.07(12) . 2_757 ? O5 Fe2 O1 93.30(11) 2_667 2_757 ? O5 Fe2 O1 86.70(11) 1_545 2_757 ? O3 Fe2 O1 95.07(12) 2_657 1_455 ? O3 Fe2 O1 84.93(12) . 1_455 ? O5 Fe2 O1 86.70(11) 2_667 1_455 ? O5 Fe2 O1 93.30(11) 1_545 1_455 ? O1 Fe2 O1 180.000(1) 2_757 1_455 ? O3 Fe2 Li1 84.01(17) 2_657 1_545 ? O3 Fe2 Li1 95.99(17) . 1_545 ? O5 Fe2 Li1 138.71(17) 2_667 1_545 ? O5 Fe2 Li1 41.29(17) 1_545 1_545 ? O1 Fe2 Li1 45.42(17) 2_757 1_545 ? O1 Fe2 Li1 134.58(17) 1_455 1_545 ? O3 Fe2 Li1 95.99(17) 2_657 2_667 ? O3 Fe2 Li1 84.01(17) . 2_667 ? O5 Fe2 Li1 41.29(17) 2_667 2_667 ? O5 Fe2 Li1 138.71(17) 1_545 2_667 ? O1 Fe2 Li1 134.58(17) 2_757 2_667 ? O1 Fe2 Li1 45.42(17) 1_455 2_667 ? Li1 Fe2 Li1 180.000(2) 1_545 2_667 ? O3 Fe2 Li1 132.62(16) 2_657 . ? O3 Fe2 Li1 47.38(16) . . ? O5 Fe2 Li1 86.41(17) 2_667 . ? O5 Fe2 Li1 93.59(16) 1_545 . ? O1 Fe2 Li1 142.44(16) 2_757 . ? O1 Fe2 Li1 37.56(16) 1_455 . ? Li1 Fe2 Li1 125.1(3) 1_545 . ? Li1 Fe2 Li1 54.9(3) 2_667 . ? O3 Fe2 Li1 47.38(16) 2_657 2_657 ? O3 Fe2 Li1 132.62(16) . 2_657 ? O5 Fe2 Li1 93.59(16) 2_667 2_657 ? O5 Fe2 Li1 86.41(17) 1_545 2_657 ? O1 Fe2 Li1 37.56(16) 2_757 2_657 ? O1 Fe2 Li1 142.44(16) 1_455 2_657 ? Li1 Fe2 Li1 54.9(3) 1_545 2_657 ? Li1 Fe2 Li1 125.1(3) 2_667 2_657 ? Li1 Fe2 Li1 180.000(2) . 2_657 ? O4 Fe1 O4 180.000(1) . 2_766 ? O4 Fe1 O2 90.80(12) . 2_756 ? O4 Fe1 O2 89.20(12) 2_766 2_756 ? O4 Fe1 O2 89.20(12) . 1_565 ? O4 Fe1 O2 90.80(12) 2_766 1_565 ? O2 Fe1 O2 180.000(1) 2_756 1_565 ? O4 Fe1 O5 94.92(12) . 1_655 ? O4 Fe1 O5 85.08(12) 2_766 1_655 ? O2 Fe1 O5 84.00(12) 2_756 1_655 ? O2 Fe1 O5 96.00(12) 1_565 1_655 ? O4 Fe1 O5 85.08(12) . 2_666 ? O4 Fe1 O5 94.92(12) 2_766 2_666 ? O2 Fe1 O5 96.00(12) 2_756 2_666 ? O2 Fe1 O5 84.00(12) 1_565 2_666 ? O5 Fe1 O5 180.0 1_655 2_666 ? As1 O4 Fe1 127.65(15) . . ? As1 O4 Li1 97.1(3) . . ? Fe1 O4 Li1 134.4(3) . . ? As1 O3 Fe2 141.43(18) . . ? As1 O3 Li1 87.6(2) . . ? Fe2 O3 Li1 95.3(2) . . ? Li1 O5 Fe1 114.9(3) . 1_455 ? Li1 O5 Fe2 96.6(3) . 1_565 ? Fe1 O5 Fe2 132.06(15) 1_455 1_565 ? Li1 O5 H1 98(4) . . ? Fe1 O5 H1 108(4) 1_455 . ? Fe2 O5 H1 102(4) 1_565 . ? As1 O2 Fe1 136.07(17) . 1_545 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.42 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.652 _refine_diff_density_min -1.001 _refine_diff_density_rms 0.209